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Sample records for coal liquefaction product

  1. Separation of solids from coal liquefaction products using sonic waves

    SciTech Connect

    Slomka, B.J.

    1994-10-01

    Product streams containing solids are generated in both direct and indirect coal liquefaction processes. This project seeks to improve the effectiveness of coal liquefaction by novel application of sonic and ultrasonic energy to separation of solids from coal liquefaction streams.

  2. Toxicology of coal liquefaction products: an overview.

    PubMed

    Chu, L; Villeneuve, D C; Rousseaux, C G

    1994-01-01

    Repeated exposure to coal liquefaction products produces a broad range of systemic effects. Among these, growth suppression, anaemia, leucocytosis and other haematological disorders are most prominent. Bone marrow, liver and kidney are the target organs affected by treatment. The effects are more severe with heavy distillates and male rats are more sensitive than females. Other changes included increased serum transaminases, alkaline phosphatase and cholesterol. Depending on the route of administration, the skin or lung may also be affected. Inhalation exposure produces the most severe changes, and oral exposure the least. Distillates containing N-PAHs and sulphur-containing PAHs are also more biologically active. Teratological effects were only observed if animals were exposed to the heavy distillate. Similarly, heavy distillates have mutagenic or carcinogenic properties. Teratological effects, as well as mutagenicity and carcinogenicity, of the coal liquefaction distillates seem to be linked to their PAH content, especially the N-PAHs. From the data presented in this review, it should become evident that the potential effects of coal liquefaction products on human health could be severe, especially with long-term exposure. Limited information exists on the occupational effects to coal liquefaction materials because most of the work to date has been with pilot plants. Careful and good judgement is required in order to extrapolate data from pilot plants to commercial-scale production. Experience in health effects of workers in the petroleum industry and coke-oven operations can serve as a guide for the implementation of industrial hygiene programmes for coal liquefaction operations. These programmes include engineering controls, health education, personal monitoring and hygienic practices, medical surveillance and long-term epidemiology studies, and they should be implemented to make coal liquefaction a healthy and environmentally sustainable industry.

  3. Some thoughts on the strategy of direct coal liquefaction -- Partial liquefaction and utilization of heavy liquefaction products

    SciTech Connect

    Liu, Z.; Yang, J.

    1998-12-31

    Hydrogenation has long been the only goal of coal liquefaction. However, analysis show that partial hydrogenation along with carbon rejection may be a better strategy for coal liquefaction, which reduces hydrogen consumption and reaction severity, eliminates the necessity for expensive catalyst, and may results in better economy for overall liquefaction. The hydrogenation and carbon rejection approach can be called partial liquefaction of coal. This paper presents analysis supporting the strategy of partial coal liquefaction based on the point of view of mass and energy balance, chemical reaction kinetics, reactivity of coal constituents and possible use of the heavy liquefaction products.

  4. Coal liquefaction

    DOEpatents

    Schindler, Harvey D.

    1985-01-01

    In a two-stage liquefaction wherein coal, hydrogen and liquefaction solvent are contacted in a first thermal liquefaction zone, followed by recovery of an essentially ash free liquid and a pumpable stream of insoluble material, which includes 850.degree. F.+ liquid, with the essentially ash free liquid then being further upgraded in a second liquefaction zone, the liquefaction solvent for the first stage includes the pumpable stream of insoluble material from the first liquefaction stage, and 850.degree. F.+ liquid from the second liquefaction stage.

  5. Coal liquefaction and hydrogenation

    DOEpatents

    Schindler, Harvey D.; Chen, James M.

    1985-01-01

    Disclosed is a coal liquefaction process using two stages. The first stage liquefies the coal and maximizes the product while the second stage hydrocracks the remainder of the coal liquid to produce solvent.

  6. Toxicity of a coal liquefaction product to aquatic organisms

    SciTech Connect

    Giddings, J.M.; Parkhurst, B.R.; Gehrs, C.W.; Millemann, R.E.

    1980-07-01

    Using acute bioassay tests a representative coal liquefaction product was compared with a petroleum derived residual fuel oil and a diesel fuel. The acute toxicity of water soluble fractions of the oils to two freshwater algae and one freshwater crustacean was determined.

  7. Coal liquefaction quenching process

    DOEpatents

    Thorogood, Robert M.; Yeh, Chung-Liang; Donath, Ernest E.

    1983-01-01

    There is described an improved coal liquefaction quenching process which prevents the formation of coke with a minimum reduction of thermal efficiency of the coal liquefaction process. In the process, the rapid cooling of the liquid/solid products of the coal liquefaction reaction is performed without the cooling of the associated vapor stream to thereby prevent formation of coke and the occurrence of retrograde reactions. The rapid cooling is achieved by recycling a subcooled portion of the liquid/solid mixture to the lower section of a phase separator that separates the vapor from the liquid/solid products leaving the coal reactor.

  8. Cooperative research program in coal liquefaction

    SciTech Connect

    Huffman, G.P.; Sendlein, L.V.A.

    1990-01-01

    Cooperative research in coal liquefaction is presented. Topics include: Sulfate-promoted metal oxides as direct coal liquefaction catalysts; low temperature depolymerization and liquefaction of premium US coal samples; construction of continuous flow-through gas reactor for liquefaction investigations; examination of ferric sulfide as a liquefaction catalyst; generic structural characterization and liquefaction research; spectroscopic studies of coal macerals depolymerization catalyzed by iron chloride; characterization of catalysts used in coal hydrogenation systems; coal structure/liquefaction yield correlation by means of advanced NMR techniques; mass spectrometry of coal derived liquids: determination of molecular weight distributions; catalyst cracking, hydrogenation and liquefaction of coals under milder conditions; ENDOR investigations of coal liquefaction under mild conditions; direct determination of hydroaromatic structures in coal and coal conversion products by catalytic dehydrogenation; surface characterization of APCSB coals by XPS; computation chemistry of model compounds and molecular fragments of relevance to coal liquefaction; chemical characterization and hydrogenation reactions of single coal particles; the role of hydrogen during liquefaction using donor and non-donor solvents; solvent sorption and FTIR studies on the effect of catalytic depolymerization reactions in coal; bioprocessing of coal; chemical routes to breaking bonds: new approaches to low-temperature liquefaction; an investigation into the reactivity of isotetralin and tetralin using molecular orbital calculations; coal liquefaction modification for enhanced reactivity; catalytic hydropyrolysis and energized extraction of coals; gallium catalyst in mild coal liquefaction -- potential of temperature microscope in coal liquefaction; evaluation of nitride catalysts for hydrotreatment and coal liquefaction; and improved catalysts for coal liquefaction and coprocessing.

  9. Coal liquefaction to increase jet fuel production

    NASA Technical Reports Server (NTRS)

    1979-01-01

    Processing concept that increases supply of jet fuel has been developed as part of study on methods for converting coal to hydrogen, methane, and jet fuel. Concept takes advantage of high aromatic content of coal-derived liquids to make high-octane gasoline, instead of destroying aromatics to make jet fuel.

  10. System for analyzing coal liquefaction products

    DOEpatents

    Dinsmore, Stanley R.; Mrochek, John E.

    1984-01-01

    A system for analyzing constituents of coal-derived materials comprises three adsorption columns and a flow-control arrangement which permits separation of both aromatic and polar hydrocarbons by use of two eluent streams.

  11. Coal liquefaction and hydrogenation

    DOEpatents

    Schindler, Harvey D.

    1985-01-01

    The coal liquefaction process disclosed uses three stages. The first stage is a liquefaction. The second and third stages are hydrogenation stages at different temperatures and in parallel or in series. One stage is within 650.degree.-795.degree. F. and optimizes solvent production. The other stage is within 800.degree.-840.degree. F. and optimizes the C.sub.5 -850.degree. F. product.

  12. Toxicity of a coal liquefaction product to aquatic organisms

    SciTech Connect

    Giddings, J.M.; Parkhurst, B.R.; Gehrs, C.W.; Millemann, R.E.

    1980-01-01

    As coal liquefaction processes approach commercialization in the United States, there is a growing need for information on their potential environmental impacts. Past oil spill experiences will not be adequate for predicting the effects of coal-derived oils, because the latter are chemically quite different from petroleum products. Using acute bioassay tests, a representative coal liquefaction product was compared with a petroluem-derived residual fuel oil and a diesel fuel, materials whose ecological effects have been documented following actual spills over the past 15 years. The acute toxicity of water soluble fractions (WSFs) of the three oils to two freshwater algae and one freshwater crustacean was determined. The WSFs were tested instead of the whole oils because (a) the water soluble components of an oil are responsible for most of its acute toxicity; and (b) while spilled oil can be contained and often recovered, the water with which it comes in contact will affect a larger area and for a longer time.

  13. Thin layer chromatography study of heavy liquefaction products derived from two Chinese bituminous coals

    SciTech Connect

    Li, Y.; Yan, R.; Yang, J.; Liu, Z.

    1997-12-31

    Two Chinese bituminous coals, Yanzhou and Fenxi, were liquefied in the temperature range of 375--450 C and under a cold H{sub 2} pressure of 7 MPa without the presence of a solvent. An iron sulfide catalyst, prepared by in-situ precipitation, was used in the study. Heavy liquefaction products, a portion of toluene and trichloroethylene (TCE) solubles, were studied by thin layer chromatography (TLC) technique. Under most conditions, the conversions of catalytic liquefaction are about twice as much as that of thermal liquefaction. The yields to toluene solubles are similar to that of TCE solubles. The TLC results of the heavy liquefaction products are compared with petroleum derived highway asphalts and with a coal tar pitch. The results show that the liquefaction products of Yanzhou coal, under certain conditions, have similar composition as that of petroleum derived highway asphalts, but significantly different from that of coal tar pitch, paraffinic petroleum residue and building asphalt.

  14. A teratological assessment of coal liquefaction products in the rat.

    PubMed

    Chu, I; Villeneuve, D C; Valli, V E; Black, W D; Robinson, K; Beyrouty, P

    1990-12-01

    Teratogenicity of coal liquefaction products (CLP) was assessed in the pregnant rat. Three product streams of CLP (medium, hydrotreated medium and heavy fractions) were each administered dermally on Sprague-Dawley rats at doses of 125, 250 or 500 mg kg-1 day-1 from Day 6 through to Day 15 of gestation. Depressed maternal weight gain and reduced number of fetuses resulting from an increased resorption rate, decreased fetal weight and retarded ossification were observed in the group treated with the heavy fraction at a dose of 500 mg kg-1 day-1. The heavy fraction at 500 mg kg-1 day-1 also caused anaemia and increased liver and spleen weights in dams. The dams exposed to the highest dose of three CLP fractions had mild and adaptative hepatic changes consisting of increased cytoplasmic eosinophilia and nuclear anisokaryosis. No treatment-related histological changes were observed in fetuses. None of the fractions demonstrated any teratological effects.

  15. Coal liquefaction process streams characterization and evaluation: FT-IR methods for characterization of coal liquefaction products

    SciTech Connect

    Serio, M.A.; Teng, H.; Bassilakis, R.; Solomon, P.R.

    1992-04-01

    This study was designed to demonstrate the use of two FTIR techniques for the analysis of direct coal liquefaction process-derived materials. The two methods were quantitative FTIR analysis and themogravimetric (TG) analysis with FTIR analysis of evolved products (TG-FTIR). The quantitative FTIR analyses of both whole resids and THF-soluble resids provided quantitation of total hydrogen, aliphatic and aromatic hydrogen, total carbon, total oxygen, hydroxyl and etheric oxygen, and ash contents. The FTIR results were usually in agreement with values derived by other, more conventional methods. However, the accuracies of specific measurements, in comparisons with results from conventional methods, ranged from good to poor. The TG-FTIR method provided approximate analyses of coals and resids. The data provided included the time dependent evolution profiles of the volatile species and the elemental composition of the char. Reproducible data of gaseous species and pyrolysis tar yields for whole resid samples larger than 10 mg were obtainable. The yields and evolution profiles of certain volatiles (tar, CO, and methane) provided structural information on the samples. There were some experimental and interpretational difficulties associated with both techniques. Optimization of the curve-resolving routine for coal-liquefaction samples would improve the quantitative FTIR accuracy. Aerosol formation limited the full application of the TG-FTIR technique with the THF-soluble resid samples. At this time, further development of these analytical methods as process development tools will be required before their use for that purpose can be recommended. The use of FTIR as an on-line analytical technique for coal liquefaction process streams requires demonstration before it can be recommended; however, such a demonstration may be warranted.

  16. Coal liquefaction process

    DOEpatents

    Wright, C.H.

    1986-02-11

    A process is described for the liquefaction of coal wherein raw feed coal is dissolved in recycle solvent with a slurry containing recycle coal minerals in the presence of added hydrogen at elevated temperature and pressure. The highest boiling distillable dissolved liquid fraction is obtained from a vacuum distillation zone and is entirely recycled to extinction. Lower boiling distillable dissolved liquid is removed in vapor phase from the dissolver zone and passed without purification and essentially without reduction in pressure to a catalytic hydrogenation zone where it is converted to an essentially colorless liquid product boiling in the transportation fuel range. 1 fig.

  17. Coal liquefaction process

    DOEpatents

    Wright, Charles H.

    1986-01-01

    A process for the liquefaction of coal wherein raw feed coal is dissolved in recycle solvent with a slurry containing recycle coal minerals in the presence of added hydrogen at elevated temperature and pressure. The highest boiling distillable dissolved liquid fraction is obtained from a vacuum distillation zone and is entirely recycled to extinction. Lower boiling distillable dissolved liquid is removed in vapor phase from the dissolver zone and passed without purification and essentially without reduction in pressure to a catalytic hydrogenation zone where it is converted to an essentially colorless liquid product boiling in the transportation fuel range.

  18. Coal liquefaction process

    SciTech Connect

    Gorbaty, M.L.; Long, R.B.; Schlosberg, R.H.

    1981-02-24

    An integrated coal pretreatment, liquefaction and gasification process is provided in which particulate coal is contacted with a vapor phase hydrogen donor solvent to swell the coal particles. The swollen coal particles are subjected to coal liquefaction conditions at relatively low temperatures. The solid residue of the coal liquefaction stage is subjected to pyrolysis conditions at relatively high temperatures to produce an additional amount of hydrocarbonaceous oil. The solid residue of the pyrolysis stage is gasified by treatment with steam and a molecular oxygen containing gas to produce a hydrogen-containing gas.

  19. Coal liquefaction process

    DOEpatents

    Maa, Peter S.

    1978-01-01

    A process for liquefying a particulate coal feed to produce useful petroleum-like liquid products which comprises contacting; in a series of two or more coal liquefaction zones, or stages, graded with respect to temperature, an admixture of a polar compound; or compounds, a hydrogen donor solvent and particulate coal, the total effluent being passed in each instance from a low temperature zone, or stage to the next succeeding higher temperature zone, or stage, of the series. The temperature within the initial zone, or stage, of the series is maintained about 70.degree. F and 750.degree. F and the temperature within the final zone, or stage, is maintained between about 750.degree. F and 950.degree. F. The residence time within the first zone, or stage, ranges, generally, from about 20 to about 150 minutes and residence time within each of the remaining zones, or stages, of the series ranges, generally, from about 10 minutes to about 70 minutes. Further steps of the process include: separating the product from the liquefaction zone into fractions inclusive of a liquid solvent fraction; hydrotreating said liquid solvent fraction in a hydrogenation zone; and recycling the hydrogenated liquid solvent mixture to said coal liquefaction zones.

  20. Coal liquefaction process

    SciTech Connect

    Long, R.B.; Gorbaty, M.L.; Schlosberg, R.H.

    1981-02-24

    In this integrated coal pretreatment, liquefaction, and gasification process, particulate coal is contacted with a vapor-phase hydrogen-donor solvent to swell the coal particles and then subjected to coal liquefaction at relatively low temperatures. The solid residue of the liquefaction stage undergoes pyrolysis at high temperatures to produce an additional amount of oil. The solid residue of the pyrolysis stage is then gasified by treatment with steam and a molecular-oxygen-containing gas to produce a hydrogen-containing gas.

  1. Cooperative research program in coal liquefaction

    SciTech Connect

    Huffman, G.P.

    1991-01-01

    This Quarterly Report on coal liquefaction research includes discussion in the areas of (1) Iron Based Catalysts for Coal Liquefaction; (2) Exploratory Research on Coal Conversion; (3) Novel Coal Liquefaction Concepts; (4) Novel Catalysts for Coal Liquefaction. (VC)

  2. Cooperative research program in coal liquefaction

    SciTech Connect

    Huffman, G.P.

    1992-01-01

    Research continues on coal liquefaction in the following areas: (1) Iron Based Catalysts for Coal Liquefaction; (2) Exploratory Research on Coal Conversion; (3) Novel Coal Liquefaction Concepts; (4) Novel Catalysts for Coal Liquefaction. (VC)

  3. Systemic toxicity of coal liquefaction products: results of a 14-day dermal exposure

    SciTech Connect

    Yagminas, A.; De Vries, P.A.; Villeneuve, D.C.

    1988-03-01

    Increasing energy demands, coupled with rising prices and an unstable world oil market have stimulated international interest in developing alternative sources of fuel. Direct coal liquefaction processes (CLP) hold great potential for Canada because of its large coal reserves. The conversion of coal to liquefied fuels results in many fractions of differing hydrocarbon content and includes many toxic substances such as polynuclear aromatic hydrocarbons. Since the major route of occupational exposure would be via the dermal route and since studies of systemic toxicity following dermal exposure are lacking, preliminary studies were conducted on the toxicity of SRC-II process coal liquefaction products applied dermally to the rat. Samples of the light (L), intermediate (I), and heavy, (H) fractions produced during the SRC-II coal liquefaction process, were kindly provided by the Sandwell Beak Research Group (Mississauga, Ontario, Canada). Diesel Fuel (D) was purchased from an Esso Gasoline Station. Male and female Sprague-Dawley rats weighing 200 +/- 25 grams were used.

  4. Integrated coal liquefaction process

    DOEpatents

    Effron, Edward

    1978-01-01

    In a process for the liquefaction of coal in which coal liquids containing phenols and other oxygenated compounds are produced during the liquefaction step and later hydrogenated, oxygenated compounds are removed from at least part of the coal liquids in the naphtha and gas oil boiling range prior to the hydrogenation step and employed as a feed stream for the manufacture of a synthesis gas or for other purposes.

  5. Investigations into coal coprocessing and coal liquefaction

    SciTech Connect

    Guffey, F.D.; Netzel, D.A.; Miknis, F.P.; Thomas, K.P.; Zhang, Tiejun; Haynes, H.W. Jr.

    1994-06-01

    The conversion of coal to liquid suitable as feedstock to a petroleum refinery is dependent upon several process variables. These variables include temperature, pressure, coal rank, catalyst type, nature of the feed to the reactor, type of process, etc. Western Research Institute (WRI) has initiated a research program in the area of coal liquefaction to address the impact of some of these variables upon the yield and quality of the coal-derived liquid. The principal goal of this research is to improve the efficiency of the coal liquefaction process. Two different approaches are currently being investigated. These include the coprocessing of a heavy liquid, such as crude oil, and coal using a dispersed catalyst and the direct liquefaction of coal using a supported catalyst. Another important consideration in coal liquefaction is the utilization of hydrogen, including both externally- and internally-supplied hydrogen. Because the incorporation of externally-supplied hydrogen during conversion of this very aromatic fossil fuel to, for example, transportation fuels is very expensive, improved utilization of internally-supplied hydrogen can lead to reducing processing costs. The objectives of this investigation, which is Task 3.3.4, Coal Coprocessing, of the 1991--1992 Annual Research Plan, are: (1) to evaluate coal/oil pretreatment conditions that are expected to improve the liquid yield through more efficient dispersion of an oil-soluble, iron-based catalyst, (2) to characterize the coke deposits on novel, supported catalysts after coal liquefaction experiments and to correlate the carbon skeletal structure parameters of the coke deposit with catalyst performance as measured by coal liquefaction product yield, and (3) to determine the modes of hydrogen utilization during coal liquefaction and coprocessing. Experimental results are discussed in this report.

  6. Coal Liquefaction Processes.

    ERIC Educational Resources Information Center

    Yen, T. F.

    1979-01-01

    Described is a graduate level engineering course offered at the University of Southern California on coal liquefaction processes. Lecture topics and course requirements are discussed. A 64-item bibliography of papers used in place of a textbook is included. (BT)

  7. US coal liquefaction program

    SciTech Connect

    Torkos, T.M.; Lacey, J.J.; Strakey, J.P.

    1985-08-01

    The US government's complete strategy for commercializing coal liquefaction includes financial assistance for qualifying coal liquefaction projects through an independent federal entity, the US Synthetic Fuels Corporation (SFC), to private developers of commercial projects under the authority of the Energy Security Act. This potential financial assistance, along with direct technical assistance, serves to reduce overall risks both to first-of-a-kind pioneer synfuels projects and potentially to the nation itself. The authors describe the status of the technology, the needed improvements, strategies, current program activities, new initiatives, and a funding summary for each liquefaction method. An appendix identifies active US projects in the program. 3 figures.

  8. Coal liquefaction process

    SciTech Connect

    Minami, R.; Hosoi, T.; Kanou, T.; Okamura, S.; Sunami, Y.

    1984-03-20

    A coal liquefaction process and apparatus therefor are disclosed. According to this invention, a finely divided coal slurry and a solvent are contacted with molecular hydrogen in the presence of a catalyst, the slurry is separated into a gaseous component, a liquid component and a solid residue, the solid residue (which is the liquefaction residue) is then supplied to a molten metal bath together with oxygen gas to generate a gas entraining fine powdery solids, and the thus recovered fine powdery solids are returned to the liquefaction process as a catalyst.

  9. Separating liquid and solid products of liquefaction of coal or like carbonaceous materials

    DOEpatents

    Malek, John M.

    1979-06-26

    Slurryform products of coal liquefaction are treated with caustic soda in presence of H.sub.2 O in an inline static mixer and then the treated product is separated into a solids fraction and liquid fractions, including liquid hydrocarbons, by gravity settling preferably effected in a multiplate settling separator with a plurality of settling spacings.

  10. Liquefaction of Yanzhou coal and TG analysis of the heavy products

    SciTech Connect

    Cui, H.; Yang, J.; Li, Y.; Gu, Y.; Liu, Z.

    1997-12-31

    A Chinese bituminous coal, Yanzhou of Shandong province, was liquefied in the temperature range of 375--425 C and under a cold H{sub 2} pressure of 7 MPa without the presence of a solvent. An iron sulfide catalyst, prepared by in-situ precipitation, was used in the study. Heavy liquefaction products, a portion of toluene and trichloroethylene solubles, were studied by thermal gravimetric technique. The iron catalyst was very active for the liquefaction. Under most conditions, the overall liquefaction conversions increased by 100% when 1 wt% of the catalyst was added. The yields to toluene solubles are similar to that of trichloroethylene solubles. The heavy toluene solubles were subjected to TG/DTG analysis, and compared with petroleum derived highway asphalts and with a coal tar pitch. The results show that the TG patterns for the heavy toluene solubles are very similar to those of petroleum derived highway asphalts, but significantly different from that of coal tar pitch.

  11. Biosynthesis of polyhydroxyalkanoates from low-rank coal liquefaction products by Pseudomonas oleovorans and Rhodococcus ruber

    PubMed

    Fuchtenbusch; Steinbuchel

    1999-07-01

    A screening identified several bacteria that were able to use chemically heterogeneous low-rank coal liquefaction products as complex carbon sources for growth. Pseudomonas oleovorans and Rhodococcus ruber accumulated polyhydroxyalkanoic acids (PHA) amounting to 2%-8% of the cell dry weight when the cells were cultivated on these liquefaction products in the absence of any other carbon source. R. ruber accumulated, in addition to PHA, small amounts of triacylglycerols. The accumulated PHA consisted of 3-hydroxyhexanoate, 3-hydroxydecanoate, and 3-hydroxydodecanoate (P. oleovorans) or 3-hydroxybutyric acid and 3-hydroxyvaleric acid (R. ruber). Low-rank coal liquefaction products obtained from Trichoderma atroviride were better substrates for P. oleovorans than chemically produced fulvic acids.

  12. Coal liquefaction process

    SciTech Connect

    Urban, P.; Hilfman, L.

    1986-09-09

    A coal liquefaction process is described comprising reacting coal with a hydrocarbonaceous solvent at coal liquefaction conditions in the presence of an oil shale residue catalyst comprising organic and inorganic fractions. The catalyst is produced by the treatment of oil shale in the presence of an inert gas at a temperature in the range from about 500/sup 0/F to about 825/sup 0/F and at a pressure in the range of from about atmospheric to about 2000 psig for a period of time of from about 0.1 to 10 hours.

  13. Method for coal liquefaction

    DOEpatents

    Wiser, Wendell H.; Oblad, Alex G.; Shabtai, Joseph S.

    1994-01-01

    A process is disclosed for coal liquefaction in which minute particles of coal in intimate contact with a hydrogenation catalyst and hydrogen arc reacted for a very short time at a temperature in excess of 400.degree. C. at a pressure of at least 1500 psi to yield over 50% liquids with a liquid to gaseous hydrocarbon ratio in excess of 8:1.

  14. Coal liquefaction process

    DOEpatents

    Carr, Norman L.; Moon, William G.; Prudich, Michael E.

    1983-01-01

    A C.sub.5 -900.degree. F. (C.sub.5 -482.degree. C.) liquid yield greater than 50 weight percent MAF feed coal is obtained in a coal liquefaction process wherein a selected combination of higher hydrogen partial pressure, longer slurry residence time and increased recycle ash content of the feed slurry are controlled within defined ranges.

  15. Method for separating liquid and solid products of liquefaction of coal or like carbonaceous materials

    DOEpatents

    Malek, John M.

    1978-04-18

    A method of improving the quality of slurry products taken from coal liquefaction reactors comprising subjecting the slurry to treatment with an alkaline compound such as caustic soda in the presence of steam in order to decompose the phenolic and acidic materials present in the slurry, and to also lower the slurry viscosity to allow separation of solid particles by sedimentation.

  16. Surfactant-Assisted Coal Liquefaction

    NASA Technical Reports Server (NTRS)

    Hickey, Gregory S.; Sharma, Pramod K.

    1993-01-01

    Obtaining liquid fuels from coal which are economically competitive with those obtained from petroleum based sources is a significant challenge for the researcher as well as the chemical industry. Presently, the economics of coal liquefaction are not favorable because of relatively intense processing conditions (temperatures of 430 degrees C and pressures of 2200 psig), use of a costly catalyst, and a low quality product slate of relatively high boiling fractions. The economics could be made more favorable by achieving adequate coal conversions at less intense processing conditions and improving the product slate. A study has been carried out to examine the effect of a surfactant in reducing particle agglomeration and improving hydrodynamics in the coal liquefaction reactor to increase coal conversions...

  17. Method for coal liquefaction

    DOEpatents

    Wiser, W.H.; Oblad, A.G.; Shabtai, J.S.

    1994-05-03

    A process is disclosed for coal liquefaction in which minute particles of coal in intimate contact with a hydrogenation catalyst and hydrogen arc reacted for a very short time at a temperature in excess of 400 C at a pressure of at least 1500 psi to yield over 50% liquids with a liquid to gaseous hydrocarbon ratio in excess of 8:1. 1 figures.

  18. Coal liquefaction process

    DOEpatents

    Karr, Jr., Clarence

    1977-04-19

    An improved coal liquefaction process is provided which enables conversion of a coal-oil slurry to a synthetic crude refinable to produce larger yields of gasoline and diesel oil. The process is characterized by a two-step operation applied to the slurry prior to catalytic desulfurization and hydrogenation in which the slurry undergoes partial hydrogenation to crack and hydrogenate asphaltenes and the partially hydrogenated slurry is filtered to remove minerals prior to subsequent catalytic hydrogenation.

  19. Coal Liquefaction desulfurization process

    DOEpatents

    Givens, Edwin N.

    1983-01-01

    In a solvent refined coal liquefaction process, more effective desulfurization of the high boiling point components is effected by first stripping the solvent-coal reacted slurry of lower boiling point components, particularly including hydrogen sulfide and low molecular weight sulfur compounds, and then reacting the slurry with a solid sulfur getter material, such as iron. The sulfur getter compound, with reacted sulfur included, is then removed with other solids in the slurry.

  20. Method for controlling boiling point distribution of coal liquefaction oil product

    DOEpatents

    Anderson, Raymond P.; Schmalzer, David K.; Wright, Charles H.

    1982-12-21

    The relative ratio of heavy distillate to light distillate produced in a coal liquefaction process is continuously controlled by automatically and continuously controlling the ratio of heavy distillate to light distillate in a liquid solvent used to form the feed slurry to the coal liquefaction zone, and varying the weight ratio of heavy distillate to light distillate in the liquid solvent inversely with respect to the desired weight ratio of heavy distillate to light distillate in the distillate fuel oil product. The concentration of light distillate and heavy distillate in the liquid solvent is controlled by recycling predetermined amounts of light distillate and heavy distillate for admixture with feed coal to the process in accordance with the foregoing relationships.

  1. Method for controlling boiling point distribution of coal liquefaction oil product

    DOEpatents

    Anderson, R.P.; Schmalzer, D.K.; Wright, C.H.

    1982-12-21

    The relative ratio of heavy distillate to light distillate produced in a coal liquefaction process is continuously controlled by automatically and continuously controlling the ratio of heavy distillate to light distillate in a liquid solvent used to form the feed slurry to the coal liquefaction zone, and varying the weight ratio of heavy distillate to light distillate in the liquid solvent inversely with respect to the desired weight ratio of heavy distillate to light distillate in the distillate fuel oil product. The concentration of light distillate and heavy distillate in the liquid solvent is controlled by recycling predetermined amounts of light distillate and heavy distillate for admixture with feed coal to the process in accordance with the foregoing relationships. 3 figs.

  2. Iron catalyzed coal liquefaction process

    DOEpatents

    Garg, Diwakar; Givens, Edwin N.

    1983-01-01

    A process is described for the solvent refining of coal into a gas product, a liquid product and a normally solid dissolved product. Particulate coal and a unique co-catalyst system are suspended in a coal solvent and processed in a coal liquefaction reactor, preferably an ebullated bed reactor. The co-catalyst system comprises a combination of a stoichiometric excess of iron oxide and pyrite which reduce predominantly to active iron sulfide catalysts in the reaction zone. This catalyst system results in increased catalytic activity with attendant improved coal conversion and enhanced oil product distribution as well as reduced sulfide effluent. Iron oxide is used in a stoichiometric excess of that required to react with sulfur indigenous to the feed coal and that produced during reduction of the pyrite catalyst to iron sulfide.

  3. Cooperative research program in coal liquefaction

    SciTech Connect

    Huffman, G.P.; Sendlein, L.V.A.

    1991-01-01

    This report is a coordinated effort of the Consortium for Fossil Fuel Liquefaction Science. The topics concerning coal liquefaction discussed are: sulfate promoted metal oxides as direct coal liquefaction catalysts; low temperature depolymerization and liquefaction of premium R.S. coal samples; construction of continuous flow-through gas reactor for liquefaction investigations; generic structural characterization and liquefaction research; macerals, model compounds and iron catalyst dispersion; coal structure/liquefaction yield correlation by means of advanced NMR techniques; GC/MS of model compound mixtures; catalytic cracking, hydrogenation and liquefaction of coals under milder conditions; ENDOR investigations of coal liquefaction under mild conditions; catalytic dehydrogenation of model compounds in relation to direct coal liquefaction; surface characterization of catalyst added coal samples; computational chemistry of model compounds and molecular fragments of relevance to coal liquefaction; chemical characterization and hydrogenation reactions of single coal particles; thermolytic cleavage of selected coal-related linkages at mild temperatures; solvent sorption and FTIR studies on the effect of catalytic depolymerization reactions in coal; bioprocessing of coal; chemical routes to breaking bonds; novel liquefaction concepts cyclic olefins: novel new donors for coal liquefaction; better hydrogen transfer in coal liquefaction; catalytic hydropyrolysis and energized extraction of coals; gallium catalyst in mild coal liquefaction; potential of temperature microscope in coal liquefaction; evaluation of nitride catalysts for hydrotreatment and coal liquefaction; coprocessing and coal liquefaction with novel catalysts.

  4. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Winschel, R.A.; Brandes, S.D.; Robbins, G.A.; Burke, F.P.

    1991-11-01

    Consol R D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-field: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The two broad objectives have considerable overlap and together serve to provide a bridge between process development and analytical chemistry.

  5. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Brandes, S.D.; Winschel, R.A.; Burke, F.P.; Robbins, G.A.

    1991-09-01

    Consol R D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-fold: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The two broad objectives have considerable overlap and together serve to provide a bridge between process development and analytical chemistry.

  6. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1992-03-01

    CONSOL R D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-fold: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The two broad objectives have considerable overlap and together serve to provide a bridge between process development and analytical chemistry.

  7. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1991-11-01

    Consol R D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-fold: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The two broad objectives have considerable overlap and together serve to provide a bridge between process development and analytical chemistry.

  8. Mutagenicity of products from coal gasification and liquefaction in the Salmonella/microsome assay.

    PubMed

    Schoeny, R; Warshawsky, D; Hollingsworth, L; Hund, M; Moore, G

    1981-01-01

    As a first step in the assessment of their possible bio-effects, coal-related materials were tested for mutagenicity in the Salmonella/microsome assay. Of three coal gasification by-products tested, only a tar was mutagenic for any of four Salmonella strains. The following liquefaction materials were mutagenic for strains TA1538, TA98, and/or TA100: A liquefaction vehicle oil and coal hydrogenation filtered liquid, separated bottoms, vacuum overhead, and vacuum bottoms. Neither powdered coal nor water produced as a by-product of the hydrogenation process was positive in the Salmonella test. No coal-related material was mutagenic for the missense mutant TA1535 or for any strain in the absence of metabolic activation provided by rat hepatic homogenates (S9). In all but one instance Aroclor 1254-induced S9 provided the maximum activation for mutagenesis. Fractionation of all samples was undertaken by serial extraction with organic solvents of increasing polarity (hexane, toluene, methylene chloride, acetonitrile). Highly mutagenic materials were found in fractions of the hydrogenation filtered liquid, vacuum overhead, and vacuum bottoms. Thus far non-mutagenic samples have not yielded mutagenic components upon fractionation.

  9. Viscosity Depressants for Coal Liquefaction

    NASA Technical Reports Server (NTRS)

    Kalfayan, S. H.

    1983-01-01

    Proposed process modification incorporates viscosity depressants to prevent coal from solidifying during liquefaction. Depressants reduce amount of heat needed to liquefy coal. Possible depressants are metallic soaps, such as stearate, and amides, such as stearamide and dimer acid amides.

  10. Liquefaction Of Coal With Surfactant And Disposable Catalyst

    NASA Technical Reports Server (NTRS)

    Hickey, Gregory S.; Sharma, Pramod K.

    1996-01-01

    Fuels derived from coal more competitive with petroleum products. Improved coal-liquefaction process exploits synergistic effects of disposable iron oxide catalyst and cheap anionic surfactant. Efficiency of conversion achieved in significantly higher than efficiencies obtained with addition of either surfactant or catalyst alone. No costly pretreatment necessary, and increase in conversion achieved under processing conditions milder than those used heretofore in liquefaction of coal. Quality of distillates obtained after liquefaction in process expected superior to distillates obtained after liquefaction by older techniques.

  11. Coal liquefaction with preasphaltene recycle

    DOEpatents

    Weimer, Robert F.; Miller, Robert N.

    1986-01-01

    A coal liquefaction system is disclosed with a novel preasphaltene recycle from a supercritical extraction unit to the slurry mix tank wherein the recycle stream contains at least 90% preasphaltenes (benzene insoluble, pyridine soluble organics) with other residual materials such as unconverted coal and ash. This subject process results in the production of asphaltene materials which can be subjected to hydrotreating to acquire a substitute for No. 6 fuel oil. The preasphaltene-predominant recycle reduces the hydrogen consumption for a process where asphaltene material is being sought.

  12. Effect of solvent characteristics on coal liquefaction

    SciTech Connect

    Huang, He; Wang, Shaojie; Wang, Keyu; Klein, M.T.; Calkins, W.H.

    1996-12-31

    It has been known for a long time that the characteristics of the liquefaction solvent has a profound effect on direct coal liquefaction. The amount of hydrogen consumed during the liquefaction process, the degree and quantity of retrograde reactions that occur, and the quality of the liquid products are all influenced by the process solvent. A number of analytical approaches have been developed to determine the important characteristics of the solvent for coal liquefaction. The hydrogen donor ability has clearly been important. However, such other characteristics of a liquefaction solvent as solubility parameter, content and type of higher aromatic hydrocarbons, and phenolic content have also been found to be significant. Finseth et al. have shown that the bulk of the hydrogen consumed from an uncatalyzed donor solvent liquefaction above 400{degrees}C is consumed in gas generation, heteroatom removal and hydrogenolysis of the coal matrix. Wilson et al. have also shown that the major role of hydrogen in uncatalyzed liquefaction is consumed by alkyl fission and hydrogenolysis reactions and not with hydrogenating aromatic rings. McMillan et al. have postulated that a radical hydrogen transfer process along with donor solvent capping of thermally produced radicals from the coal as possible processes involved with the hydroaromatic donor solvents in coal liquefaction. With the development of a short contact time batch reactor (SCTBR), determining the influence of the processing solvent on the liquefaction rates, conversion profiles and the quality of the liquid product at a particular time became possible. The influence of type of solvent, combined with other effects, such as gas atmosphere (i.e., in hydrogen and in nitrogen) and catalyst, on the coal liquefaction is reported in this paper.

  13. Coal liquefaction with molybdenum catalysts

    SciTech Connect

    Chien, P.L.

    1983-01-01

    Coal liquefaction experiments were carried out in a stirred autoclave under nitrogen. Tetralin was employed as solvent, and the catalyst, when used, was ammonium heptamolybdate (impregnated on coal) or stannous chloride (powdered). Production of pentane soluble oil was higher in the runs with catalyst, but net hydrogen transfer from tetralin to coal was less when catalyst was used. Coal and powdered stannous chloride exhibited a marked synergistic effect on the dehydrogenation of tetralin. A free radical mechanism was suggested to explain this effect, and model experiments with bibenzyl (but no coal) gave results that were consistent with this mechanism. An apparent synergistic effect of coal and impregnated ammonium heptamolybdate was shown to be attributed simply to improved distribution (higher surface area) of the impregnated catalyst, the coal acting as a high-area support. Comparison of the results from autoclave experiments (under nitrogen) with those from tubing bomb experiments (under air) indicated major differences in coal conversion and hydrogen transfer. The conversion was 62% in the autoclave and 81% in the tubing bomb, and the hydrogen transfer was 0.7% in the autoclave and 2.93% in the tubing bomb, when 1% of Mo (based on coal) was impregnated on coal in a preliminary step.

  14. Mild coal pretreatment to improve liquefaction reactivity

    SciTech Connect

    Miller, R.L.

    1991-01-01

    This report describes work completed during the fourth quarter of a three year project to study the effects of mild chemical pretreatment on coal dissolution reactivity during low severity liquefaction or coal/oil coprocessing. The overall objective of this research is to elucidate changes in the chemical and physical structure of coal by pretreating with methanol or other simple organic solvent and a trace amount of hydrochloric acid and measure the influence of these changes on coal dissolution reactivity. This work is part of a larger effort to develop a new coal liquefaction or coal/oil coprocessing scheme consisting of three main process steps: (1) mile pretreatment of the feed coal to enhance dissolution reactivity and dry the coal, (2) low severity thermal dissolution of the pretreated coal to obtain a very reactive coal-derived residual material amenable to upgrading, and (3) catalytic upgrading of the residual products to distillate liquids.

  15. Automated apparatus for solvent separation of a coal liquefaction product stream

    DOEpatents

    Schweighardt, Frank K.

    1985-01-01

    An automated apparatus for the solvent separation of a coal liquefaction product stream that operates continuously and unattended and eliminates potential errors resulting from subjectivity and the aging of the sample during analysis. In use of the apparatus, metered amounts of one or more solvents are passed sequentially through a filter containing the sample under the direction of a microprocessor control means. The mixture in the filter is agitated by means of ultrasonic cavitation for a timed period and the filtrate is collected. The filtrate of each solvent extraction is collected individually and the residue on the filter element is collected to complete the extraction process.

  16. Cooperative research in coal liquefaction

    SciTech Connect

    Huffman, G.P.; Sendlein, L.V.A.

    1991-05-28

    Significant progress was made in the May 1990--May 1991 contract period in three primary coal liquefaction research areas: catalysis, structure-reactivity studies, and novel liquefaction processes. A brief summary of the accomplishments in the past year in each of these areas is given.

  17. Two stage liquefaction of coal

    DOEpatents

    Neuworth, Martin B.

    1981-01-01

    A two stage coal liquefaction process and apparatus comprising hydrogen donor solvent extracting, solvent deashing, and catalytic hydrocracking. Preferrably, the catalytic hydrocracking is performed in an ebullating bed hydrocracker.

  18. Coal liquefaction process with enhanced process solvent

    DOEpatents

    Givens, Edwin N.; Kang, Dohee

    1984-01-01

    In an improved coal liquefaction process, including a critical solvent deashing stage, high value product recovery is improved and enhanced process-derived solvent is provided by recycling second separator underflow in the critical solvent deashing stage to the coal slurry mix, for inclusion in the process solvent pool.

  19. EXXON donor solvent coal liquefaction process

    NASA Technical Reports Server (NTRS)

    Epperly, W. R.; Swabb, L. E., Jr.; Tauton, J. W.

    1978-01-01

    A solvent coal liquefaction process to produce low-sulfur liquid products from a wide range of coals is described. An integrated program of laboratory and engineering research and development in conjunction with operation of a 250 T/D pilot plant is discussed.

  20. Steam pretreatment for coal liquefaction

    NASA Astrophysics Data System (ADS)

    Ivanenko, Olga

    The objectives of this work are to test the application of steam pretreatment to direct coal liquefaction, to investigate the reaction of model compounds with water, and to explore the use of zeolites in these processes. Previous work demonstrated the effectiveness of steam pretreatment in a subsequent flash pyrolysis. Apparently, subcritical steam ruptures nearly all of the ether cross links, leaving a partially depolymerized structure. It was postulated that very rapid heating of the pretreated coal to liquefaction conditions would be required to preserve the effects of such treatment. Accordingly, a method was adopted in which coal slurry is injected into a hot autoclave containing solvent. Since oxygen is capable of destroying the pretreatment effect, precautions were taken for its rigorous exclusion. Tests were conducted with Illinois No. 6 coal steam treated at 340sp°C, 750 psia for 15 minutes. Both raw and pretreated samples were liquified in deoxygenated tetralin at high severity (400sp°C, 30 min.) and low severity (a: 350sp°C, 30 min., and b: 385sp°C, 15 min.) conditions under 1500 psia hydrogen. Substantial improvement in liquid product quality was obtained and the need for rapid heating and oxygen exclusion demonstrated. Under low severity conditions, the oil yield was more than doubled, going from 12.5 to 29 wt%. Also chemistry of the pretreatment process was studied using aromatic ethers as model compounds. alpha-Benzylnaphthyl ether (alpha-BNE), alpha-naphthylmethyl phenyl (alpha-NMPE), and 9-phenoxyphenanthrene were exposed to steam and inert gas at pretreatment conditions and in some cases to liquid water at 315sp°C. alpha-BNE and alpha-NMPE showed little difference in conversion in inert gas and in steam. Hence, these compounds are poor models for coal in steam pretreatment. Thermally stable 9-phenoxyphenanthrene, however, was completely converted in one hour by liquid water at 315sp°C. At pretreatment conditions mostly rearranged starting

  1. Production and Optimization of Direct Coal Liquefaction derived Low Carbon-Footprint Transportation Fuels

    SciTech Connect

    Steven Markovich

    2010-06-30

    This report summarizes works conducted under DOE Contract No. DE-FC26-05NT42448. The work scope was divided into two categories - (a) experimental program to pretreat and refine a coal derived syncrude sample to meet transportation fuels requirements; (b) system analysis of a commercial scale direct coal liquefaction facility. The coal syncrude was derived from a bituminous coal by Headwaters CTL, while the refining study was carried out under a subcontract to Axens North America. The system analysis included H{sub 2} production cost via six different options, conceptual process design, utilities requirements, CO{sub 2} emission and overall plant economy. As part of the system analysis, impact of various H{sub 2} production options was evaluated. For consistence the comparison was carried out using the DOE H2A model. However, assumptions in the model were updated using Headwaters database. Results of Tier 2 jet fuel specifications evaluation by the Fuels & Energy Branch, US Air Force Research Laboratory (AFRL/RZPF) located at Wright Patterson Air Force Base (Ohio) are also discussed in this report.

  2. Role of non-ferrous coal minerals and by-product metallic wastes in coal liquefaction. Technical progress report, 1 March 1980-31 May 1980

    SciTech Connect

    Garg, D; Schweighardt, F K; Givens, E N; Clinton, J H; Tarrer, A R; Guin, J A; Curtis, C W; Huang, S M

    1980-06-01

    This report describes work done in a study of the role of coal minerals and by-product metallic wastes in coal liquefaction. The thermal behavior of various minerals and metallic by-product wastes was evaluated by thermal gravimetric analysis and differential thermal analysis in the presence of hydrogen, nitrogen, and air. The CPDU was operated for 220 hours to obtain baseline data and provide information on the catalytic activity of Robena pyrite in solvent hydrogenation and coal liquefaction. A number of minerals were screened for catalytic activity toward coal liquefaction in a tubing-bomb reactor. The catalytic activity of the minerals was assessed by comparing the product distributions both in the presence of minerals and their absence. The use of a Bronson Sonifier was initiated in March to accelerate and improve the solvent separation technique. The addition of lime to the reaction mixture practically killed the liquefaction reaction. The addition of dolomite, rutile, illite, quartz, zircon, and calcite to the reaction mixture showed no significant improvement over that of a no additive run. The addition of zinc oxide and ilmenite showed slight improvement. Robena pyrite and Co-Mo-Al showed significant improvement in coal conversion and production of benzene solubles and gases. Iron oxide (Fe/sub 2/O/sub 3/) gave the highest conversion of coal and production of benzene solubles among all the minerals tested so far.

  3. Direct coal liquefaction process

    DOEpatents

    Rindt, J.R.; Hetland, M.D.

    1993-10-26

    An improved multistep liquefaction process for organic carbonaceous mater which produces a virtually completely solvent-soluble carbonaceous liquid product. The solubilized product may be more amenable to further processing than liquid products produced by current methods. In the initial processing step, the finely divided organic carbonaceous material is treated with a hydrocarbonaceous pasting solvent containing from 10% and 100% by weight process-derived phenolic species at a temperature within the range of 300 C to 400 C for typically from 2 minutes to 120 minutes in the presence of a carbon monoxide reductant and an optional hydrogen sulfide reaction promoter in an amount ranging from 0 to 10% by weight of the moisture- and ash-free organic carbonaceous material fed to the system. As a result, hydrogen is generated via the water/gas shift reaction at a rate necessary to prevent condensation reactions. In a second step, the reaction product of the first step is hydrogenated.

  4. Direct coal liquefaction process

    DOEpatents

    Rindt, John R.; Hetland, Melanie D.

    1993-01-01

    An improved multistep liquefaction process for organic carbonaceous mater which produces a virtually completely solvent-soluble carbonaceous liquid product. The solubilized product may be more amenable to further processing than liquid products produced by current methods. In the initial processing step, the finely divided organic carbonaceous material is treated with a hydrocarbonaceous pasting solvent containing from 10% and 100% by weight process-derived phenolic species at a temperature within the range of 300.degree. C. to 400.degree. C. for typically from 2 minutes to 120 minutes in the presence of a carbon monoxide reductant and an optional hydrogen sulfide reaction promoter in an amount ranging from 0 to 10% by weight of the moisture- and ash-free organic carbonaceous material fed to the system. As a result, hydrogen is generated via the water/gas shift reaction at a rate necessary to prevent condensation reactions. In a second step, the reaction product of the first step is hydrogenated.

  5. Coal liquefaction process

    DOEpatents

    Skinner, Ronald W.; Tao, John C.; Znaimer, Samuel

    1985-01-01

    This invention relates to an improved process for the production of liquid carbonaceous fuels and solvents from carbonaceous solid fuels, especially coal. The claimed improved process includes the hydrocracking of the light SRC mixed with a suitable hydrocracker solvent. The recycle of the resulting hydrocracked product, after separation and distillation, is used to produce a solvent for the hydrocracking of the light solvent refined coal.

  6. Coal liquefaction process employing extraneous minerals

    SciTech Connect

    Carr, N.L.; Schmid, B.K.

    1980-09-16

    In a coal liquefaction process which includes a recycle of a product slurry which contain recycle mineral residue and recycle of extraneous catalytic material to said liquefication zone, hydrocracking of the hydrocarbonaceous material from the mineral residue occurs and a mixture of hydrocarbon gases, dissolved liquid, normally solid dissolved coal, suspended mineral residue and suspended extraneous catalytic mineral results. A first portion of said residue slurry is recycled to the liquefication zone, a second portion is passed to separation means and the third portion goes to a hydroclone. Overflow from the hydroclone goes to the liquefaction zone to reduce the median diameter of the particles recycled.

  7. Fine particle clay catalysts for coal liquefaction

    SciTech Connect

    Olson, E.S.

    1991-01-01

    The efficient production of environmentally acceptable distillate fuels requires catalysts for hydrogenation and cleavage of the coal macromolecules and removal of oxygen, nitrogen, and sulfur heteroatoms. The goal of the proposed research is to develop new catalysts for the direct liquefaction of coal. This type of catalyst consists of fine clay particles that have been treated with reagents which form pillaring structures between the aluminosilicate layers of the clay. The pillars not only hold the layers apart but also constitute the active catalytic sites for hydrogenation of the coal and the solvent used in the liquefaction. The pillaring catalytic sites are composed of pyrrhotite, which has been previously demonstrated to be active for coal liquefaction. The pyrrhotite sites are generated in situ by sulfiding the corresponding oxyiron species. The size of the catalyst will be less than 40 nm in order to promote intimate contact with the coal material. Since the clays and reagents for pillaring and activating the clays are inexpensive, the catalysts can be discarded after use, rather than regenerated by a costly process. The proposed work will evaluate methods for preparing the fine particle iron-pillared clay dispersions and for activating the particles to generate the catalysts. Characterization studies of the pillared clays and activated catalysts will be performed. The effectiveness of the pillared clay dispersion for hydrogenation and coal liquefaction will be determined in several types of testing.

  8. Fine particle clay catalysts for coal liquefaction

    SciTech Connect

    Olson, E.S.

    1991-01-01

    The efficient production of environmentally acceptable distillate fuels requires catalysts for hydrogenation and cleavage of the coal macromolecules and removal of oxygen, nitrogen, and sulfur heteroatoms. The goal of the proposed research is to develop new catalysts for the direct liquefaction of coal. This type of catalyst consists of fine clay particles that have been treated with reagents which form pillaring structures between the aluminosilicate layers of the clay. The pillars not only hold the layers apart but also constitute the active catalytic sites for hydrogenation of the coal and solvent used in the liquefaction. The pillaring catalytic sites are composed of pyrrhotite, which has been previously demonstrated to be active for coal liquefaction. The pyrrhotite sites are generated in situ by sulfiding the corresponding oxyiron species. The size of the catalyst will be less than 40 nm in order to promote intimate contact with the coal material. Since the clays and reagents for pillaring and activating the clays are inexpensive, the catalysts can be discarded after use, rather than regenerated by a costly process. The proposed work will evaluate methods for preparing the fine particle iron-pillared clay dispersions and for activating the particles to generate the catalysts. Characterization studies of the pillared clays and activated catalysts will performed. The effectiveness of the pillared clay dispersion for hydrogenation and coal liquefaction will be determined in several types of testing. 5 refs., 1 tab.

  9. The characterization of coal liquefaction products obtained under an inert atmosphere and catalytic conditions. Part II: Soluble products

    SciTech Connect

    Karaca, H.

    2006-03-15

    Beypazari and Tuncbilek lignite were liquefied using two different catalyst methods physically mixing and impregnation. The liquefaction occurred under conditions of inert atmosphere and various process parameters. Solvent to coal ratio, pressure, catalyst type, catalyst concentration, temperature, and time were examined as process parameters. The most appropriate parameters for the total soluble products obtained by liquefaction of both lignites and for elemental analysis of preasphaltenes were determined as follows: 2/1 solvent to coal ratio; from 1.25 MPa to 2.50 MPa initial nitrogen pressure; Fe{sub 2}O{sub 3} and Mo(CO){sub 6} as catalyst types; 3% as catalyst concentration; 400{sup o}C as reaction temperature; and 60 min as reaction time. In general, fuel quality of both preasphaltene and total soluble products decreased as temperature increased above 400{sup o}C and reaction time exceeded 60 min. The fuel quality of the preasphaltenes and the total soluble products obtained under the catalytic conditions and in the state of impregnation of catalyst onto coal is higher than under the noncatalytic conditions and in the state of physically mixing of catalyst.

  10. Integrated coal cleaning, liquefaction, and gasification process

    DOEpatents

    Chervenak, Michael C.

    1980-01-01

    Coal is finely ground and cleaned so as to preferentially remove denser ash-containing particles along with some coal. The resulting cleaned coal portion having reduced ash content is then fed to a coal hydrogenation system for the production of desirable hydrocarbon gases and liquid products. The remaining ash-enriched coal portion is gasified to produce a synthesis gas, the ash is removed from the gasifier usually as slag, and the synthesis gas is shift converted with steam and purified to produce the high purity hydrogen needed in the coal hydrogenation system. This overall process increases the utilization of as-mined coal, reduces the problems associated with ash in the liquefaction-hydrogenation system, and permits a desirable simplification of a liquids-solids separation step otherwise required in the coal hydrogenation system.

  11. Two-stage coal liquefaction without gas-phase hydrogen

    DOEpatents

    Stephens, H.P.

    1986-06-05

    A process is provided for the production of a hydrogen-donor solvent useful in the liquefaction of coal, wherein the water-gas shift reaction is used to produce hydrogen while simultaneously hydrogenating a donor solvent. A process for the liquefaction of coal using said solvent is also provided. The process enables avoiding the use of a separate water-gas shift reactor as well as high pressure equipment for liquefaction. 3 tabs.

  12. Process for coal liquefaction employing selective coal feed

    DOEpatents

    Hoover, David S.; Givens, Edwin N.

    1983-01-01

    An improved coal liquefaction process is provided whereby coal conversion is improved and yields of pentane soluble liquefaction products are increased. In this process, selected feed coal is pulverized and slurried with a process derived solvent, passed through a preheater and one or more dissolvers in the presence of hydrogen-rich gases at elevated temperatures and pressures, following which solids, including mineral ash and unconverted coal macerals, are separated from the condensed reactor effluent. The selected feed coals comprise washed coals having a substantial amount of mineral matter, preferably from about 25-75%, by weight, based upon run-of-mine coal, removed with at least 1.0% by weight of pyritic sulfur remaining and exhibiting vitrinite reflectance of less than about 0.70%.

  13. Surfactant-assisted coal liquefaction

    NASA Technical Reports Server (NTRS)

    Hsu, G. C.

    1977-01-01

    Improved process of coal liquefaction utilizing nonaqueous surfactant has increased oil yield from 50 to about 80%. Asphaltene molecule formation of colloid particles is prevented by surfactant. Separated molecules present more surface area for hydrogenation reaction. Lower requirements for temperature, pressure, and hydrogen lead to reduction in capital and operation costs.

  14. A Characterization and Evaluation of Coal Liquefaction Process Streams

    SciTech Connect

    G. A. Robbins; R. A. Winschel; S. D. Brandes

    1998-06-09

    CONSOL characterized 38 process strea m samples from HTI Run PB- 04, in which Black Thunder Mine Coal, Hondo vacuum resid, autom obile shredder residue (ASR), and virgin plastics were used as liquefaction feedstocks with dispersed catalyst. A paper on kinetic modeling of resid reactivity was presented at the DOE Coal Lique -faction and Solid Fuels Contractors Review Conference, September 3- 4, 1997, i n Pittsburgh, PA. The paper, "The Reactivity of Direct Coal Liquefaction Resids", i s appended (Appendix 1). Three papers on characterization of samples from coal/ resid/ waste p lastics co- liquefaction were presented or submitted for presen tation at conferences. Because of their similarity, only one of the papers is appended to this report. The paper, "Characterization o f Process Samples From Co- Liquefaction of Coal and Waste Polymers", (Appendix 2) was presented at the DOE Coal Liquefaction and Solid Fuels C ontractors Review Conference, September 3- 4, 1997, in Pittsburgh, PA. The paper, "Characterization of Process Stream Samples From Bench- Scale Co -Liquefaction Runs That Utilized Waste Polymers as Feedstocks" was presented at the 214th National Meeting of the Ameri can Chemical Society, September 7- 11, 1997, in Las Vegas, NV. The paper, "Characterization of Process Oils from Coal/ Waste Co- Liquefaction" wa s submitted for presentation at the 14th Japan/ U. S. Joint Technical Meeting on Coa l Liquefaction and Materials for Coal Liquefaction on October 28, 1997, in Tokyo, Japan. A joint Burns and Roe Services Corp. and CONSOL pap er on crude oil assays of product oils from HTI Run PB- 03 was presented at the DOE Coal Liquefaction and Solid Fuel s Contractors Review Conference, September 3- 4, 1997, in Pittsburgh, PA. The paper , "Characterization of Liquid Products from All- Slurry Mode Liquefaction", is appende d (Appendix 3).

  15. Highly dispersed catalysts for coal liquefaction

    SciTech Connect

    Hirschon, A.S.; Wilson, R.B.

    1992-11-05

    The objectives of this project are to study the effect of pretreatment methods on the two-stage liquefaction process. In particular, the effects of dispersed catalysts and carbon monoxide atmospheres on a coal liquefaction process. The project is divided into three technical tasks. Task 1 and 2 deal with the analyses and liquefaction experiments, respectively, whereas Task 3 deals with the economic impact of utilizing the pretreatment methods. This quarter we concentrated on Tasks 1 and 2, which are summarized below. Samples of Black Thunder Subbituminous coal and the corresponding recycle solvent were received from Wilsonville. These particular samples were obtained from run [number sign]263. The samples were analyzed for a proximate and ultimate analysis, as well as heat content. We have also received samples of the iron oxide used in the Wilsonville coal liquefaction runs as well as Shell 324 and molyVanL for use in future runs. Base-line screening experiments were conducted in 300 mL autoclaves using 2.5 parts by weight of recycle solvent to 1 part Black Thunder coal at 425[degree]C for one hour. In preliminary results for the comparison of iron oxide and iron carbonyl, the iron carbonyl appears to give higher yields to soluble products.

  16. Pillared montmorillonite catalysts for coal liquefaction

    SciTech Connect

    Sharma, R.K.; Olson, E.S.

    1994-12-31

    Pillared clays contain large micropores and have considerable potential for catalytic hydrogenation and cleavage of coal macromolecules. Pillared montmorillonite-supported catalysts were prepared by the intercalation of polynuclear hydroxychromium cations and subsequent impregnation of nickel and molybdenum. Infrared and thermogravimetric studies of pyridine-adsorbed catalysts indicated the presence of both Lewis and Bronsted acid sites. Thus, the catalysts have both acidic properties that can aid in hydrocracking and cleavage of carbon-heteroatom bonds as well as hydrogen-activating bimetallic sites. These catalysts were applied to the hydrodesulfurization and liquefaction of coal-derived intermediates. The reactions of model organosulfur compounds and coal liquids were carried out at 300{degrees}-400{degrees}C for 3 hours in the presence of 1000 psi of molecular hydrogen. Reaction products were analyzed by GC/FT-IR/MS/AED. The catalysts have been found to be very effective in removing sulfur from model compounds as well as liquefaction products.

  17. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Robbins, G.A.; Winshel, R.A.; Burke, F.P.

    1990-10-01

    Consol R D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-fold: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The first objective will utilize analytical techniques which have not been fully demonstrated; the second objective involves more previously proven methods. This quarter, two feed coals and 39 process oils from Wilsonville Run 258 were analyzed to provide information on process performance. Run 258 was operated in the thermal/catalytic Close-Coupled Integrated Two-Stage Liquefaction (CC-ITSL) mode with ash recycle. The subbituminous feed coals were from the Spring Creek Mine (Anderson and Dietz seams) and from the Black Thunder Mine (Wyodak and Anderson seams). Shell 324 catalyst was used in the second stage. Various coal samples related to Wilsonville Run 259 were analyzed for chemical and petrographic composition. These results will be given in a future report, which covers all of Run 259. 18 figs., 24 tabs.

  18. Two-stage coal liquefaction process

    DOEpatents

    Skinner, Ronald W.; Tao, John C.; Znaimer, Samuel

    1985-01-01

    An improved SRC-I two-stage coal liquefaction process which improves the product slate is provided. Substantially all of the net yield of 650.degree.-850.degree. F. heavy distillate from the LC-Finer is combined with the SRC process solvent, substantially all of the net 400.degree.-650.degree. F. middle distillate from the SRC section is combined with the hydrocracker solvent in the LC-Finer, and the initial boiling point of the SRC process solvent is increased sufficiently high to produce a net yield of 650.degree.-850.degree. F. heavy distillate of zero for the two-stage liquefaction process.

  19. Coal liquefaction process employing multiple recycle streams

    SciTech Connect

    Carr, N.; Schleppy, R.; Shah, Y.

    1980-07-08

    A combination coal liquefaction-gasification process comprises passing hydrogen and a liquefaction zone feed slurry comprising mineral-containing feed coal, recycle dissolved liquid coal solvent, recycle dissolved coal which is solid at room temperature and recycle mineral residue to a coal liquefaction zone to dissolve hydrocarbonaceous material from mineral residue and to hydrocrack said hydrocarbonaceous material to produce a liquefaction zone effluent mixture comprising hydrocarbon gases, dissolved liquid coal, solid dissolved coal and suspended mineral residue; recycling to said liquefaction zone feed slurry a portion of said dissolved liquid coal,solid dissolved coal and mineral residue; recycling to said liquefaction zone an other portion of ssaid solid dissolved coal and mineral residue independently of said liquefaction zone feed slurry; said liquefaction zone producing a greater net yield on a weight basis after recycle of 450 to 850/sup 0/F dissolved liquid coal as compared to the net yield on a weight basis after recycle of 850/sup 0/F solid dissolved coal; separating dissolved liquid coal and hydrocarbon gases from non-recycled solid dissolved coal and mineral residue to produce a gasifier feed slurry comprising substantially the entire net yield of solid dissolved coal and mineral residue of said liquefaction zone; passing said gasifier feed slurry to a gasification zone includin G an oxidation zone for the conversion of the hydrocarbonaceous material therein to synthesis gas; converting at least a portion of said synthesis gas to a gaseous hydrogen-rich stream and passing said hydrogen-rich stream to said liquefaction zone to supply process hydrogen thereto; the amount of hydrocarbonaceous material passed to said gasification zone being sufficient to enable said gasification zone at least the entire hydrogen requirement of said liquefaction zone.

  20. Effect of coal liquefaction conditions on the composition of the product oil

    SciTech Connect

    Karaca, H.

    2006-12-15

    Two methods, catalyst physically mixing method (method I) and catalyst impregnation method (method II) were employed for Beypazari and Tuncbilek lignites liquefaction. Fe{sub 2}O{sub 3} and Mo(CO){sub 6} were used as the catalysts. Oils obtained at the end of the catalytic coal liquefaction were qualitatively analyzed by gas chromatography (GC). With solvent/coal ratio increase, compounds with straight chain and high molecular weight were formed. Likewise, as the reaction time and catalyst concentration were increased, the number and the intensity of the compounds in the oils increased partially. Due to the increase in the reaction time, temperature and catalyst concentration, the oils were enriched in straight chain alkanes and aromatic polycyclic compounds. However, alkanes with straight chain were reduced by the effect of pyrolysis at temperatures over 400{sup o}C. Retention times of the compounds obtained by method II were higher than those of the compounds obtained by method I. Respectively, the compounds in the oils obtained by method II were found to have been composed by high quantities of high molecular straight chain alkanes and aromatic polycyclic compounds. Our data gave us ground to presume that the oils from both lignites were composed by straight chain alkanes and aromatic polycyclic compounds (tetralin, naphthalene and their derivatives, phenols, xylenols, biphenyl, naphthols, etc.). The oil compositions were strongly influenced by the liquefaction conditions.

  1. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction. [High temperature soaking coal in coal liquids prior to liquefaction

    SciTech Connect

    Not Available

    1992-10-01

    Soaking coal in coal liquids at 300-400[degrees]C (high-tenperature soaking) has been studied for coal dissolution prior to liquefaction in the previous task. Two high-volatile bituminous coals, Illinois No. 6 and Pittsburgh No. 8, were examined in three different coal liquids. The high-temperature soaking was effective to solubilize more than 70 wt% cf these coals. The mechanism of disintegration of coal by the high-temperature soaking was investigated under various soaking conditions. The products was also analyzed with solvent swelling. These results were rationalized that coal is solubilized primarily by physical disintegration. The derived mechanism was consistent with the new concept of coal structure: A significant portion of coal is physically associated, not three-dimensionally cross-linked. Radically-induced scission reactions were proposed to prorate breakage of coal moleculs by the combination of the high-temperature soaking before liquefaction. In this term, the effect of radical initiators were investigated under the conditions of the high-temperature soaking and liquefaction. Illinois No. 6 coal and a coal liquid derived from the same coal were used. The first section reports the effect of radical initiators on coal disintegration, and the second section reports the effect of a radical initiator on coal liquefaction. Radical initiators had a positive effect on disintegration. However, the effect was highly temperature-dependent and had a negative effect on liquefaction at high tenperatures.

  2. EXPLORATORY RESEARCH ON NOVEL COAL LIQUEFACTION CONCEPT

    SciTech Connect

    Brandes, S.D.; Winschel, R.A.

    1998-11-30

    The report presents a summary the work performed under DOE Contract No. DE-AC22-95PC95050. Investigations performed under Task 4--Integrated Flow Sheet Testing are detailed. In this program, a novel direct coal liquefaction technology was investigated by CONSOL Inc. with the University of Kentucky Center for Applied Energy Research and LDP Associates. The process concept explored consists of a first-stage coal dissolution step in which the coal is solubilized by hydride ion donation. In the second stage, the products are catalytically upgraded to refinery feedstocks. Integrated first-stage and solids-separation steps were used to prepare feedstocks for second-stage catalytic upgrading. An engineering and economic evaluation was conducted concurrently with experimental work throughout the program. Approaches to reduce costs for a conceptual commercial plant were recommended at the conclusion of Task 3. These approaches were investigated in Task 4. The economic analysis of the process as it was defined at the conclusion of Task 4, indicates that the production of refined product (gasoline) via this novel direct liquefaction technology is higher than the cost associated with conventional two-stage liquefaction technologies.

  3. Coal liquefaction process with increased naphtha yields

    DOEpatents

    Ryan, Daniel F.

    1986-01-01

    An improved process for liquefying solid carbonaceous materials wherein the solid carbonaceous material is slurried with a suitable solvent and then subjected to liquefaction at elevated temperature and pressure to produce a normally gaseous product, a normally liquid product and a normally solid product. The normally liquid product is further separated into a naphtha boiling range product, a solvent boiling range product and a vacuum gas-oil boiling range product. At least a portion of the solvent boiling-range product and the vacuum gas-oil boiling range product are then combined and passed to a hydrotreater where the mixture is hydrotreated at relatively severe hydrotreating conditions and the liquid product from the hydrotreater then passed to a catalytic cracker. In the catalytic cracker, the hydrotreater effluent is converted partially to a naphtha boiling range product and to a solvent boiling range product. The naphtha boiling range product is added to the naphtha boiling range product from coal liquefaction to thereby significantly increase the production of naphtha boiling range materials. At least a portion of the solvent boiling range product, on the other hand, is separately hydrogenated and used as solvent for the liquefaction. Use of this material as at least a portion of the solvent significantly reduces the amount of saturated materials in said solvent.

  4. Advanced coal liquefaction research: Final report

    SciTech Connect

    Gall, W.; McIlvried, H.G. III

    1988-07-01

    This study had two objectives: (1) To enhance the fundamental understanding of observed differences in the short contact time, donor solvent liquefaction of bituminous and subbituminous coals. (2) To determine if physical refining of subbituminous coals could be used to give a better feedstock for the first stage of two-stage liquefaction processes. Liquefaction studies using microautoclaves were carried out. Results are discussed. 11 refs., 25 figs., 29 tabs.

  5. Novel supports for coal liquefaction catalysts

    SciTech Connect

    Haynes, H.W. Jr.

    1992-01-01

    This research is divided into three parts: (1) Evaluation of Alkaline-Earth-Promoted CoMo/Alumina Catalysts in a Bench Scale Hydrotreater, (2) Development of a Novel Catalytic Coal Liquefaction Microreactor (CCLM) Unit, and (3) Evaluation of Novel Catalyst Preparations for Direct Coal Liquefaction. (VC)

  6. Catalytic coal liquefaction process

    DOEpatents

    Garg, D.; Sunder, S.

    1986-12-02

    An improved process for catalytic solvent refining or hydroliquefaction of non-anthracitic coal at elevated temperatures under hydrogen pressure in a solvent comprises using as catalyst a mixture of a 1,2- or 1,4-quinone and an alkaline compound, selected from ammonium, alkali metal, and alkaline earth metal oxides, hydroxides or salts of weak acids. 1 fig.

  7. Catalytic coal liquefaction process

    DOEpatents

    Garg, Diwakar; Sunder, Swaminathan

    1986-01-01

    An improved process for catalytic solvent refining or hydroliquefaction of non-anthracitic coal at elevated temperatures under hydrogen pressure in a solvent comprises using as catalyst a mixture of a 1,2- or 1,4-quinone and an alkaline compound, selected from ammonium, alkali metal, and alkaline earth metal oxides, hydroxides or salts of weak acids.

  8. Hydrogen donor solvent coal liquefaction process

    DOEpatents

    Plumlee, Karl W.

    1978-01-01

    An indigenous hydrocarbon product stream boiling within a range of from about C.sub.1 -700.degree. F., preferably C.sub.1 -400.degree. F., is treated to produce an upgraded hydrocarbon fuel component and a component which can be recycled, with a suitable donor solvent, to a coal liquefaction zone to catalyze the reaction. In accordance therewith, a liquid hydrocarbon fraction with a high end boiling point range up to about 700.degree. F., preferably up to about 400.degree. F., is separated from a coal liquefaction zone effluent, the separated fraction is contacted with an alkaline medium to provide a hydrocarbon phase and an aqueous extract phase, the aqueous phase is neutralized, and contacted with a peroxygen compound to convert indigenous components of the aqueous phase of said hydrocarbon fraction into catalytic components, such that the aqueous stream is suitable for recycle to the coal liquefaction zone. Naturally occurring phenols and alkyl substituted phenols, found in the aqueous phase, are converted, by the addition of hydroxyl constituents to phenols, to dihydroxy benzenes which, as disclosed in copending Application Ser. Nos. 686,813 now U.S. Pat. No. 4,049,536; 686,814 now U.S. Pat. No. 4,049,537; 686,827 now U.S. Pat. No. 4,051,012 and 686,828, K. W. Plumlee et al, filed May 17, 1976, are suitable hydrogen transfer catalysts.

  9. Cooperative research program in coal liquefaction. Quarterly report, November 1, 1991--January 31, 1992

    SciTech Connect

    Huffman, G.P.

    1992-06-01

    Research continues on coal liquefaction in the following areas: (1) Iron Based Catalysts for Coal Liquefaction; (2) Exploratory Research on Coal Conversion; (3) Novel Coal Liquefaction Concepts; (4) Novel Catalysts for Coal Liquefaction. (VC)

  10. Cooperative Research Program in coal liquefaction. Technical report, May 1, 1994--October 31, 1994

    SciTech Connect

    1994-12-31

    Progress reports are presented for the following tasks: coliquefaction of coal with waste materials; catalysts for coal liquefaction to clean transportation fuels; fundamental research in coal liquefaction; and in situ analytical techniques for coal liquefaction and coal liquefaction catalysts.

  11. Cooperative research program in coal liquefaction. Quarterly report, August 1, 1991--October 31, 1991

    SciTech Connect

    Huffman, G.P.

    1991-12-31

    This Quarterly Report on coal liquefaction research includes discussion in the areas of (1) Iron Based Catalysts for Coal Liquefaction; (2) Exploratory Research on Coal Conversion; (3) Novel Coal Liquefaction Concepts; (4) Novel Catalysts for Coal Liquefaction. (VC)

  12. Case studies on direct liquefaction of low rank Wyoming coal

    SciTech Connect

    Adler, P.; Kramer, S.J.; Poddar, S.K.

    1995-12-31

    Previous Studies have developed process designs, costs, and economics for the direct liquefaction of Illinois No. 6 and Wyoming Black Thunder coals at mine-mouth plants. This investigation concerns two case studies related to the liquefaction of Wyoming Black Thunder coal. The first study showed that reducing the coal liquefaction reactor design pressure from 3300 to 1000 psig could reduce the crude oil equivalent price by 2.1 $/bbl provided equivalent performing catalysts can be developed. The second one showed that incentives may exist for locating a facility that liquifies Wyoming coal on the Gulf Coast because of lower construction costs and higher labor productivity. These incentives are dependent upon the relative values of the cost of shipping the coal to the Gulf Coast and the increased product revenues that may be obtained by distributing the liquid products among several nearby refineries.

  13. Fundamental studies of coal liquefaction

    SciTech Connect

    Not Available

    1995-01-01

    The authors have examined the pyrolysis of Argonne samples of Wyodak and Illinois No. 6 coal in argon, undecane, Tetralin, and water. The effects of the pyrolysis on individual particles of coal were monitored visually in a cell with diamond windows capable of operation to temperature and pressures in excess of 500{degrees}C and 3000 psi. The changes in the particles from ambient to 460{degrees}C were recorded in real time on video tape, and images were then taken from the tape record and analyzed. The study showed that in argon both coals developed tars at 350{degrees}-370{degrees}C. The tars then quickly evaporated, leaving core particles remarkably similar in size and shape to the initial particles. These observations suggest that coal does not melt nor become fully liquid when heated. Nor does the softened coal undergo crosslinking to generate coke. Rather the simple loss of volatiles leaves behind the core residue as coke. Contrary to the common view, there appears to be no link between the bond-breaking processes yielding tar and the interaction of the coal with H-donors leading to liquefaction. Water as a medium was surprising in its effect. Both coals began to shrink at 300{degrees}-350{degrees}C, with the effect appearing to be more of an erosion rather than a uniform loss of substance as seen in Tetralin. The Wyodak continued to shrink to 460{degrees}C to about half its initial size. With the Illinois No. 6 coal, however, the process reversed at around 420{degrees}C, and the particles appeared to grow with the evolution of a tar, continuing to 460{degrees}C. The authors submit that this final observation is evidence for hydrothermal synthesis of hydrocarbons at these conditions.

  14. Enhancing low severity coal liquefaction reactivity using mild chemical pretreatment

    SciTech Connect

    Shams, K.G.; Miller, R.L.; Baldwin, R.M.

    1992-07-13

    In this paper, we describe results from a study in which mild chemical pretreatment of coal has been used to enhance low severity liquefaction reactivity. We have found that ambient pretreatment of eight Argonne coals using methanol and a trace amount of hydrochloric acid improves THF-soluble conversions 24.5 wt% (maf basis) for Wyodak subbituminous coal and 28.4 wt% for Beulah-Zap lignite with an average increase of 14.9 wt% for liquefaction of the eight coals at 623 K (350{degree}C) reaction temperature and 30 min. reaction time. Similar enhancement results occurred using, hexane or acetone in place of methanol. Pretreatment with methanol and HCI separately indicated that both reagents were necessary to achieve maximum liquefaction improvement. Acid concentration was the most important pretreatment variable studied; liquefaction reactivity increased with increasing acid concentration up to 2 vol%. No appreciable effect on reactivity was observed at higher acid concentrations. Although vapor phase alcohol/HCI mixtures have been shown to partially alkylate bituminous coals, analysis of Wyodak and Illinois {number sign}6 coal samples indicated that no organic phase alteration occurred during pretreatment; however, over 90 wt% of the calcium was removed from each coal. Calcium is thought to catalyze retrogressive reactions during coal pyrolysis, and thus calcium removal prior to low severity liquefaction minimizes the rate of THF-insoluble product formation.

  15. Hydrogen-donor coal liquefaction process

    DOEpatents

    Wilson, Jr., Edward L.; Mitchell, Willard N.

    1980-01-01

    Improved liquid yields are obtained during the hydrogen-donor solvent liquefaction of coal and similar carbonaceous solids by maintaining a higher concentration of material having hydrogenation catalytic activity in the downstream section of the liquefaction reactor system than in the upstream section of the system.

  16. Process for coal liquefaction in staged dissolvers

    DOEpatents

    Roberts, George W.; Givens, Edwin N.; Skinner, Ronald W.

    1983-01-01

    There is described an improved liquefaction process by which coal is converted to a low ash and low sulfur carbonaceous material that can be used as a fuel in an environmentally acceptable manner without costly gas scrubbing equipment. In the process, coal is slurried with a pasting oil, passed through a preheater and at least two dissolvers in series in the presence of hydrogen-rich gases at elevated temperatures and pressures. Solids, including mineral ash and unconverted coal macerals, are separated from the condensed reactor effluent. In accordance with the improved process, the first dissolver is operated at a higher temperature than the second dissolver. This temperature sequence produces improved product selectivity and permits the incorporation of sufficient hydrogen in the solvent for adequate recycle operations.

  17. Catalytic liquefaction of coal with petroleum residues

    NASA Astrophysics Data System (ADS)

    Kotowski, W.; Jakubowski, L.; Gorski, R.

    1980-11-01

    A process combining the desulfurization of fuel oil with coal liquefaction is presented. The unit operates at 90-110 bar, and 420-490 C, with a spatial velocity of 1.2-1.3 cu m/hr. It is designed with the possibility of producing benzene and increasing the heating oil supply. Emphasis is placed on using the smallest possible number of procedures to carry out the process. The relation between temperature change and the production of benzene, light oil, and gas is discussed.

  18. Advanced liquefaction using coal swelling and catalyst dispersion techniques

    SciTech Connect

    Curtis, C.W. ); Gutterman, C. ); Chander, S. )

    1992-08-26

    Research in this project centers upon developing a new approach to the direct liquefaction of coal to produce an all-distillate product slate at a sizable cost reduction over current technology. The approach integrates all aspects of the coal liquefaction process including coal selection, pretreatment, coal swelling with catalyst impregnation, coal liquefaction experimentation, product recovery with characterization, alternate bottoms processing, and a technical assessment including an economic evaluation. The project is being carried out under contract to the United States Department of Energy. On May 28, 1992, the Department of Energy authorized starting the experimental aspects of this projects; therefore, experimentation at Amoco started late in this quarterly report period. Research contracts with Auburn University, Pennsylvania State University, and Foster Wheeler Development Corporation were signed during June, 1992, so their work was just getting underway. Their work will be summarized in future quarterly reports. A set of coal samples were sent to Hazen Research for beneficiation. The samples were received and have been analyzed. The literature search covering coal swelling has been up-dated, and preliminary coal swelling experiments were carried out. Further swelling experimentation is underway. An up-date of the literature on the liquefaction of coal using dispersed catalysts is nearing completion; it will be included in the next quarterly report.

  19. Catalyst for coal liquefaction process

    DOEpatents

    Huibers, Derk T. A.; Kang, Chia-Chen C.

    1984-01-01

    An improved catalyst for a coal liquefaction process; e.g., the H-Coal Process, for converting coal into liquid fuels, and where the conversion is carried out in an ebullated-catalyst-bed reactor wherein the coal contacts catalyst particles and is converted, in addition to liquid fuels, to gas and residual oil which includes preasphaltenes and asphaltenes. The improvement comprises a catalyst selected from the group consisting of the oxides of nickel molybdenum, cobalt molybdenum, cobalt tungsten, and nickel tungsten on a carrier of alumina, silica, or a combination of alumina and silica. The catalyst has a total pore volume of about 0.500 to about 0.900 cc/g and the pore volume comprises micropores, intermediate pores and macropores, the surface of the intermediate pores being sufficiently large to convert the preasphaltenes to asphaltenes and lighter molecules. The conversion of the asphaltenes takes place on the surface of micropores. The macropores are for metal deposition and to prevent catalyst agglomeration. The micropores have diameters between about 50 and about 200 angstroms (.ANG.) and comprise from about 50 to about 80% of the pore volume, whereas the intermediate pores have diameters between about 200 and 2000 angstroms (.ANG.) and comprise from about 10 to about 25% of the pore volume, and the macropores have diameters between about 2000 and about 10,000 angstroms (.ANG.) and comprise from about 10 to about 25% of the pore volume. The catalysts are further improved where they contain promoters. Such promoters include the oxides of vanadium, tungsten, copper, iron and barium, tin chloride, tin fluoride and rare earth metals.

  20. Coal liquefaction process streams characterization and evaluation: The application of {sup 252}Cf-plasma desorption mass spectrometry to analysis of direct coal liquefaction heavy products

    SciTech Connect

    Larsen, J.W.; Lapucha, A.R.

    1992-10-01

    This study demonstrated the feasibility of using {sup 252}Cf PDMS, GPC, and MPLC for the examination of the tetrahydrofuran (THF)-soluble portion of distillation resid materials derived from direct coal liquefaction. The {sup 252}Cf-PDMS technique was used to determine molecular weight distributions of twenty-five THF-soluble resids. In order to detemine if {sup 252}Cf-PDMS responds differently to different chemical classes of compounds, Lehigh separated five of the samples into chemically distinct fractions by MPLC, then analyzed the parent samples, their fractions, and the re-mixed fractions by {sup 252}Cf-PDMS and GPC. Irreversible alteration of the samples upon separation was noted by Lehigh. This was confirmed by use of gas chromatographic (GC) analyses. The noted irreversible alterations prevented a direct comparison of the remixed materials and the original samples. Thus, the selective response of {sup 252}Cf-PDMS to different chemical classes of compounds could not be confirmed or ruled out. The number average molecular weights (M{sub n}) obtained by {sup 252}Cf-PDMS and GPC agreed well. However, the weight average molecular weights (M{sub w}) obtained by GPC are always higher than the corresponding {sup 252}Cf-PDMS results. Number average molecular weights and weight average molecular weights obtained with {sup 252}Cf-PDMS and GPC were compared with those obtained by field ionization mass spectrometry (FIMS), previously reported by SRI International for the parent resid samples from which the Lehigh THF-soluble samples were derived.

  1. Coal liquefaction process streams characterization and evaluation: The application of [sup 252]Cf-plasma desorption mass spectrometry to analysis of direct coal liquefaction heavy products

    SciTech Connect

    Larsen, J.W.; Lapucha, A.R.

    1992-10-01

    This study demonstrated the feasibility of using [sup 252]Cf PDMS, GPC, and MPLC for the examination of the tetrahydrofuran (THF)-soluble portion of distillation resid materials derived from direct coal liquefaction. The [sup 252]Cf-PDMS technique was used to determine molecular weight distributions of twenty-five THF-soluble resids. In order to detemine if [sup 252]Cf-PDMS responds differently to different chemical classes of compounds, Lehigh separated five of the samples into chemically distinct fractions by MPLC, then analyzed the parent samples, their fractions, and the re-mixed fractions by [sup 252]Cf-PDMS and GPC. Irreversible alteration of the samples upon separation was noted by Lehigh. This was confirmed by use of gas chromatographic (GC) analyses. The noted irreversible alterations prevented a direct comparison of the remixed materials and the original samples. Thus, the selective response of [sup 252]Cf-PDMS to different chemical classes of compounds could not be confirmed or ruled out. The number average molecular weights (M[sub n]) obtained by [sup 252]Cf-PDMS and GPC agreed well. However, the weight average molecular weights (M[sub w]) obtained by GPC are always higher than the corresponding [sup 252]Cf-PDMS results. Number average molecular weights and weight average molecular weights obtained with [sup 252]Cf-PDMS and GPC were compared with those obtained by field ionization mass spectrometry (FIMS), previously reported by SRI International for the parent resid samples from which the Lehigh THF-soluble samples were derived.

  2. Experience in feeding coal into a liquefaction process development unit

    NASA Technical Reports Server (NTRS)

    Akhtar, S.; Friedman, S.; Mazzocco, N. J.; Yavorsky, P. M.

    1977-01-01

    A system for preparing coal slurry and feeding it into a high pressure liquefaction plant is described. The system was developed to provide supporting research and development for the Bureau of Mines coal liquefaction pilot plant. Operating experiences are included.

  3. Cooperative research program in coal liquefaction. Quarterly report, May 1, 1993--October 31, 1993

    SciTech Connect

    Hoffman, G.P.

    1994-07-01

    This report summarizes progress in four areas of research under the general heading of Coal Liquefaction. Results of studies concerning the coliquefaction of coal with waste organic polymers or chemical products of these polymers were reported. Secondly, studies of catalytic systems for the production of clean transportation fuels from coal were discussed. Thirdly, investigations of the chemical composition of coals and their dehydrogenated counterparts were presented. These studies were directed toward elucidation of coal liquefaction processes on the chemical level. Finally, analytical methodologies developed for in situ monitoring of coal liquefaction were reported. Techniques utilizing model reactions and methods based on XAFS, ESR, and GC/MS are discussed.

  4. Coal liquefaction process research quarterly report, October-December 1979

    SciTech Connect

    Bickel, T.C.; Curlee, R.M.; Granoff, B.; Stohl, F.V.; Thomas, M.G.

    1980-03-01

    This quarterly report summarizes the activities of Sandia's continuing program in coal liquefaction process research. The overall objectives are to: (1) provide a fundamental understanding of the chemistry of coal liquefaction; (2) determine the role of catalysts in coal liquefaction; and (3) determine the mechanism(s) of catalyst deactivation. The program is composed of three major projects: short-contact-time coal liquefaction, mineral effects, and catalyst studies. These projects are interdependent and overlap significantly.

  5. Surface Modified Coals for Enhanced Catalyst Dispersion and Liquefaction

    SciTech Connect

    Yaw D. Yeboah

    1998-12-04

    The aim of this study is to enhance catalyst loading and dispersion in coal for improved liquefaction by preadsorption of surfactants and catalysts on to the coal. During this reporting period, liquefaction experiments were conducted with the raw coal and catalyst loaded samples. Pretreatment of the coal and catalyst-loaded samples were done using the surfactants presented in previous reports. Liquefaction samples were tested using 6.6 g of solvent, 3.3 g coal, 6.9 MPa ambient hydrogen pressure, 425 0 C and 30 minutes. The liquid and solid products were removed from the reactor using tetrahydrofuran (THF). Coal conversions were calculated based on THF and heptane solubility. The results showed that in the absence of a catalyst, 33.8% heptane solubles was obtained with the parent coal compared to 27.8% and 27.3% with the SDS and DDAB surfactants. The presence of molybdenum, as expected, resulted in enhanced heptane solubles with or without surfactants. In the absence of surfactants, 50% heptane solubles was obtained compared to 40-47% with surfactants. Thus, it appears that pretreatment, unexpectedly, had a negative effect on liquefaction activity. It is unclear if the observed differences in results are significant. Clearly, additional experiments are needed before any firm deductions and conclusions can be drawn from the results.

  6. Ultrasonic characterization of coal liquefaction products. Final report, April 11, 1979-February 11, 1980

    SciTech Connect

    Leffert, C. B.; Weisman, L.; Moore, D.

    1980-02-29

    The Wayne State University ultrasonic device and technique was used successfully to calibrate coal-derived 0 to 45% wt % asphaltene-in-oil mixtures (2 wt % increments) for transmitted signal strength versus temperature (25 to 100/sup 0/C). Computer-aided cross plots of the transmitted signal strength versus concentration of asphaltene showed that a wide range of concentration and temperature exists where the viscosity-dominated (lower temperature) sound absorption is such that a single-valued number for the concentration of the asphaltene can be obtained from measurement of the sample temperature and transmitted signal strength and thus obtain a measure of the quality of the coal-derived product. Sufficient samples were not provided to obtain a complete calibration of added particulate matter of ash and undissolved coal at all asphaltene in oil concentrations; however, calibrations were made of added ash to three concentrations of asphaltene-in-oil and the data showed the greatest effect at the higher temperatures indicating (as planned) that sound attenuation from Rayleigh scattering is predominant with the suspended particles. We conclude from these two sets of measurements that there is a excellent expectation that the Wayne State ultrasonic device and technique could be used to simultaneously measure (on-line) the suspended particle concentration as well as the quality of the coal-derived product.

  7. Coal liquefaction with subsequent bottoms pyrolysis

    DOEpatents

    Walchuk, George P.

    1978-01-01

    In a coal liquefaction process wherein heavy bottoms produced in a liquefaction zone are upgraded by coking or a similar pyrolysis step, pyrolysis liquids boiling in excess of about 1000.degree. F. are further reacted with molecular hydrogen in a reaction zone external of the liquefaction zone, the resulting effluent is fractionated to produce one or more distillate fractions and a bottoms fraction, a portion of this bottoms fraction is recycled to the reaction zone, and the remaining portion of the bottoms fraction is recycled to the pyrolysis step.

  8. One-Step Coal Liquefaction

    NASA Technical Reports Server (NTRS)

    Qader, S. A.

    1984-01-01

    Steam injection improves yield and quality of product. Single step process for liquefying coal increases liquid yield and reduces hydrogen consumption. Principal difference between this and earlier processes includes injection of steam into reactor. Steam lowers viscosity of liquid product, so further upgrading unnecessary.

  9. Evaluation of the effect of solvent modification and coal pretreatment and beneficiation on liquefaction: Final report

    SciTech Connect

    Garg, D.; Miller, R.N.; Hoover, D.S.; Givens, E.N.; Schweighardt, F.K.; Tarrer, A.R.; Guin, J.A.; Curtis, C.W.; Luckie, P.

    1985-03-01

    An extensive research program was conducted to ascertain ways to improve oil yields and process economics of direct coal liquefaction. The effects of removing heteroatoms from the solvent, pretreating coal by several techniques (including solvent extraction, oxidation, grinding, and ion exchange), and beneficiating coal by removing mineral species were investigated in both catalytic and noncatalytic coal liquefaction reactions. Additionally, fundamental studies were carried out to explain the role of heteroatoms in catalytic coal liquefaction. The effects of process variables, catalysts and mode of catalyst addition, solvent properties, and recycle of SRC on oil production and coal conversion were also studied. 9 refs., 12 figs., 72 tabs.

  10. Fired heater for coal liquefaction process

    DOEpatents

    Ying, David H. S.; McDermott, Wayne T.; Givens, Edwin N.

    1985-01-01

    A fired heater for a coal liquefaction process is operated under conditions to maximize the slurry slug frequency and thereby improve the heat transfer efficiency. The operating conditions controlled are (1) the pipe diameter and pipe arrangement, (2) the minimum coal/solvent slurry velocity, (3) the maximum gas superficial velocity, and (4) the range of the volumetric flow velocity ratio of gas to coal/solvent slurry.

  11. Effect of dispersing agent in heating process for high dispersion of coal liquefaction catalyst

    SciTech Connect

    Okada, Y.; Haneda, M.; Inokuchi, K.; Aihara, Y.; Imada, K.; Kai, T.; Sakaki, T.; Shibata, M.

    1999-07-01

    This work deals with one proposal concerning the improvement of catalytic activity on coal liquefaction. It is known that pyrite (FeS{sub 2}) transform into pyrrhotite (Fe{sub 1{minus}x}S) and aggregate at the heating process on coal liquefaction. The aggregation of liquefaction catalyst decreases the specific surface area, and causes the decline in catalytic activity. The authors investigated the effects of dispersing agent on the morphological change and the dispersing state of liquefaction catalyst at the rapid heating process. For the liquefaction tests with added dispersing agent, the product yields were compared with the results of other tests.

  12. Advanced concepts in coal liquefaction: Optimization of reactor configuration in coal liquefaction. Final report

    SciTech Connect

    Pradhan, V.R.; Comolli, A.G.; Lee, L.K.

    1994-11-01

    The overall objective of this Project was to find the ways to effectively reduce the cost of coal liquids to about dollar 25 per barrel of crude oil equivalent. The work described herein is primarily concerned with the testing at the laboratory scale of three reactor configuration concepts, namely (1) a fixed-bed plug-flow reactor as a ``finishing reactor`` in coal liquefaction, (2) three-stage well-mixed reactors in series, and (3) interstage stream concentration/product separation. The three reactor configurations listed above were tested during this project using a 20 cc tubing microreactor, a fixed-bed plug flow reactor, and a two-stage modified Robinson-Mahoney reactor system. The reactor schemes were first evaluated based on theoretical modelling studies, then experimentally evaluated at the microautoclave level and laboratory scale continuous operations. The fixed-bed ``finishing reactor`` concept was evaluated in both the upflow and the downflow modes of operation using a partially converted coal-solvent slurry as feed. For most of the testing of concepts at the microautoclave level, simulated coal, recycle oil, and slurry feedstocks were either specially prepared (to represent a specific state of coal/resid conversion) and/or obtained from HRI`s other ongoing bench-scale and PDU scale coal liquefaction experiments. The three-stage continuous stirred tank reactors (CSTR) and interstage product stream separation/concentration concepts were tested using a simulated three-stage CSTR system by employing a laboratory-scale ebullated-bed system and a modified version of the HRI`s existing Robinson-Mahoney fixed catalyst basket reactor system. This testing was conducted as a fourteen day long continuous run, divided into four Conditions to allow for a comparison of the new three-stage CSTR and interstage product concentration concepts with a two-stage CSTR baseline configuration.

  13. Highly dispersed catalysts for coal liquefaction. Phase 1 final report, August 23--November 22, 1994

    SciTech Connect

    Hirschon, A.S.; Wilson, R.B.; Ghaly, O.

    1995-03-22

    The ultimate goal of this project is to develop novel processes for making the conversion of coal into distillable liquids competitive to that of petroleum products in the range of $25/bbl. The objectives of Phase 1 were to determine the utility of new precursors to highly dispersed catalysts for use of syngas atmospheres in coal liquefaction, and to estimate the effect of such implementation on the cost of the final product. The project is divided into three technical tasks. Tasks 1 and 2 are the analyses and liquefaction experiments, respectively, and Task 3 deals with the economic effects of using these methods during coal liquefaction. Results are presented on the following: Analytical Support--screening tests and second-stage conversions; Laboratory-Scale Operations--catalysts, coal conversion in synthetic solvents, Black Thunder screening studies, and two-stage liquefaction experiments; and Technical and economic Assessment--commercial liquefaction plant description, liquefaction plant cost; and economic analysis.

  14. Low severity coal liquefaction promoted by cyclic olefins

    SciTech Connect

    Curtis, C.W.

    1991-01-01

    The objective of this project is to evaluate the efficacy of low severity coal liquefaction in the presence of highly reactive hydrogen donors, cyclic olefins. The work that was performed this quarter involved performing a literature search in which different aspects of low severity coal liquefaction were examined. In addition, two new mater's graduate students learned the fundamental differences between high severity coal liquefaction and low severity coal liquefaction by examining the literature and reading texts on coal liquefaction. The literature review presented for the first quarter's work is a compilation of the material which we have found to data involving low severity coal liquefaction. Additional review of low severity liquefaction literature is being conducted this quarter and will be reported in the next quarterly report. In addition, a summary of the work involving the reactivity of cyclic olefins in the absence and presence of coal will be presented next quarter.

  15. The Dual Role of Oxygen Functions in Coal Pretreatment and Liquefaction: Crosslinking and Cleavage Reactions

    SciTech Connect

    Michael Serio; Erik Kroo; Sylvie Charpenay; Peter Solomon

    1993-09-30

    The overall objective of this project was to elucidate and model the dual role of oxygen functions in thermal pretreatment and liquefaction of low rank coals through the application of analytical techniques and theoretical models. The project was an integrated study of model polymers representative of coal structures, raw coals of primarily low rank, and selectively modified coals in order to provide specific information relevant to the reactions of real coals. The investigations included liquefaction experiments in microautoclave reactors, along with extensive analysis of intermediate solid, liquid and gaseous products. Attempts were made to incorporate the results of experiments on the different systems into a liquefaction model.

  16. SHORT CONTACT TIME DIRECT COAL LIQUEFACTION USING A NOVEL BATCH REACTOR

    SciTech Connect

    Michael T. Klein; William H. Calkins

    1997-10-29

    The overall goal of this research is to develop an understanding of the Direct Coal Liquefaction process at the molecular level. Many approaches have been used to study this process including kinetic studies, study of the liquefaction products, study of the effect of reaction variables, such as temperature, solvent type and composition, the changing nature and composition of the coal during liquefaction, and the distribution in the liquefaction products of the hydrogen consumed. While all these studies have contributed to our growing knowledge of the liquefaction process, an adequate understanding of direct liquefaction still eludes us. This is due to many reasons including: the complexity and variable nature of coal itself and the many different chemical reactions which are occurring simultaneously during direct coal liquefaction. We believe that a study of the liquefaction process at the very early stages will avoid the complexities of secondary reactions associated with free radical high temperature processes that are clearly involved in direct coal liquefaction. This prompted us to devise a reactor system which avoids long heat up and cool-down times associated with previous kinetic studies, and allows kinetic measurements even at as short as the first few seconds of the liquefaction reaction.

  17. Liquefaction of sub-bituminous coal

    DOEpatents

    Schindler, Harvey D.; Chen, James M.

    1986-01-01

    Sub-bituminous coal is directly liquefied in two stages by use of a liquefaction solvent containing insoluble material as well as 850.degree. F.+ material and 850.degree. F.- material derived from the second stage, and controlled temperature and conversion in the second stage. The process is in hydrogen balance.

  18. Fired heater for coal liquefaction process

    DOEpatents

    Ying, David H. S.

    1984-01-01

    A fired heater for a coal liquefaction process is constructed with a heat transfer tube having U-bends at regular intervals along the length thereof to increase the slug frequency of the multi-phase mixture flowing therethrough to thereby improve the heat transfer efficiency.

  19. Coal liquefaction processes and development requirements analysis for synthetic fuels production

    NASA Technical Reports Server (NTRS)

    1980-01-01

    Focus of the study is on: (1) developing a technical and programmatic data base on direct and indirect liquefaction processes which have potential for commercialization during the 1980's and beyond, and (2) performing analyses to assess technology readiness and development trends, development requirements, commercial plant costs, and projected synthetic fuel costs. Numerous data sources and references were used as the basis for the analysis results and information presented.

  20. Coal Liquefaction by Using Dielectric Barrier Discharge Plasma

    NASA Astrophysics Data System (ADS)

    Wang, Qiuying; Wu, Peng; Gu, Fan

    2013-07-01

    An innovative method for coal liquefaction by using dielectric barrier discharge (DBD) plasma in a short reaction time was developed. Using tetralin as the reaction medium, DBD plasma as the energy source, and a reaction time of 10 min at 140°C, up to 10% of coal was converted to liquid material. The results showed the feasibility of coal's liquefaction by DBD plasma under relatively moderate conditions. Simultaneously, it was clarified that the effect of DBD plasma treatment was opposed to the thermal effect of heating. An acid plasma sheath could be formed on the coal powder surface in DBD conditions, liquefied reactions could be carried out in the absence of inorganic acid, and the products were nearly neutral and with low causticity.

  1. Development of Highly Reactive Nanometer Fe-Based Catalysts for Coal Liquefaction

    SciTech Connect

    Franz, James A.; Linehan, John C.; Matson, Dean W.; Smurthwaite, Tricia D.; Bekhazi, Jacky; Alnajjar, Mikhail S.

    2008-03-01

    This paper describes research involving the liquefaction of coal and the removal of oxygen from coal product constituents. Subbituminous Coal and early stage coal liquefaction products contain a substantial fraction of hydroxy-substituted aromatic hydrocarbons (phenols). An important reaction for upgrading of coal-derived organic materials is to remove oxygen groups. This paper describes the hydro-deoxygenation of naphthols and the liquefaction of subbituminous Wyodak coal using a catalyst prepared by in-situ sulfidation of nanometer scale 6-line iron ferrihydrite. The FeS catalyst enables the conversion of naphthol in substantial yields to tetralin and naphthalene at 400 degrees C in 9,10-dihydrophenanthrene. The kinetics and procedures to observe coal liquefaction and hydro-deoxygenation, and the effects of in-situ sulfidation on conversion kinetics are described.

  2. Coal liquefaction and gas conversion: Proceedings. Volume 1

    SciTech Connect

    Not Available

    1993-12-31

    Volume I contains papers presented at the following sessions: AR-Coal Liquefaction; Gas to Liquids; and Direct Liquefaction. Selected papers have been processed separately for inclusion in the Energy Science and Technology Database.

  3. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Brandes, S.D.; Lancet, M.S.; Robbins, G.A.; Winschel, R.A.; Burke, F.P.

    1992-11-01

    This is the eleventh Quarterly Technical Progress Report under DOE Contract DE-AC22-89PC89883. Major topics reported are: (1) The results of a study designed to determine the effects of the conditions employed at the Wilsonville slurry preheater vessel on coal conversion is described. (2) Stable carbon isotope ratios were determined and used to source the carbon of three product samples from Period 49 of UOP bench-scale coprocessing Run 37. The results from this coprocessing run agree with the general trends observed in other coprocessing runs that we have studied. (3) Microautoclave tests and chemical analyses were performed to calibrate'' the reactivity of the standard coal used for determining donor solvent quality of process oils in this contract. (4) Several aspects of Wilsonville Close-Coupled Integrated Two-Stage Liquefaction (CC-ITSL) resid conversion kinetics were investigated; results are presented. Error limits associated with calculations of deactivation rate constants previously reported for Runs 258 and 261 are revised and discussed. A new procedure is described that relates the conversions of 850[degrees]F[sup +] , 1050[degrees]F[sup +], and 850 [times] 1050[degrees]F material. Resid conversions and kinetic constants previously reported for Run 260 were incorrect; corrected data and discussion are found in Appendix I of this report.

  4. Environmental risk analysis for indirect coal liquefaction

    SciTech Connect

    Barnthouse, L.W.; Suter, G.W. II; Baes, C.F. III; Bartell, S.M.; Cavendish, M.G.; Gardner, R.H.; O'Neill, R.V.; Rosen, A.E.

    1985-01-01

    This report presents an analysis of the risks to fish, water quality (due to noxious algal blooms), crops, forests, and wildlife of two technologies for the indirect liquefaction of coal: Lurgi and Koppers-Totzek gasification of coal for Fischer-Tropsch synthesis. A variety of analytical techniques were used to make maximum use of the available data to consider effects of effluents on different levels of ecological organization. The most significant toxicants to fish were found to be ammonia, cadmium, and acid gases. An analysis of whole-effluent toxicity indicated that the Lurgi effluent is more acutely toxic than the Koppers-Totzek effluent. Six effluent components appear to pose a potential threat of blue-green algal blooms, primarily because of their effects on higher trophic levels. The most important atmospheric emissions with respect to crops, forests, and wildlife were found to be the conventional combustion products SO/sub 2/ and NO/sub 2/. Of the materials deposited on the soil, arsenic, cadmium, and nickel appear of greatest concern for phytotoxicity. 147 references, 5 figures, 41 tables.

  5. A Characterization and Evaluation of Coal Liquefaction Process Streams The Kinetics of Coal Liquefaction Distillation Resid Conversion

    SciTech Connect

    Campbell, D; Nichols, D G; Pazuchanics, D J; Huang, H; Klein, M T; Winschel, R A; Brandes, S D; Wang, S; Calkins, W H

    1998-06-04

    Under subcontract from CONSOL Inc. (DOE Contract N o. DE- AC22- 94PC93054), the University of Delaware studied the mechanism and kinetics of coal liquefaction resid conversion. Th e program at Delaware was conducted be tween August 15, 1994, and April 30, 1997. It consisted of two primary tasks. The first task was to develop an empirical test to measure the reactivit y toward hydrocracking of coal- derived distillation resids. The second task was to formulate a computer model to represent the structure of the resids and a kinetic and mechanistic model of resid reactivity based on the structural representations. An Introduction and Summary of th e project authored by CONSOL and a report of the program findings authored by the University of Delaware researchers are presented here. INTRODUCTION Resid hydrocracking is a key reaction of modern (i. e., distillate- producing) coal liquefactio n processes. Coals are readily converted to resid a nd lighter products in the liquefaction process. The resid is combined with fr esh coal in a ratio often greater than 1: 1, and some vacuum gas oil and is recycled to be further converted. Understanding the chemistry of resids and resi d reactivity is important to improve direct liquefaction process design and to achieve economi c objectives for direct coal liquefaction. Computational models that predict resid conversion from the chemical characteristics of the resids and reaction conditions would be a cost- efficient way to explore process variables. Implementation of such models could aid in the design an d operation of liquefaction facilities.

  6. Mild coal pretreatment to improve liquefaction reactivity

    SciTech Connect

    Miller, R.L.

    1991-01-01

    This report describes work completed during the fifth quarter of a three year project to study the effects of mild chemical pretreatment on coal dissolution reactivity during low severity liquefaction or coal/oil coprocessing. The overall objective of this research is to elucidate changes in the chemical and physical structure of coal by pretreating with methanol or other simple organic solvent and a trace amount of hydrochloric acid and measure the influence of these changes on coal dissolution reactivity. Work this quarter focused on analytical characterization of untreated and treated Wyodak subbituminous coal and Illinois {number sign}6 bituminous coal. Mossbauer spectroscopy and x-ray diffraction techniques were used to study the effect of methanol/HCl pretreatment on the composition of each coal's inorganic phase. Results from these studies indicated that calcite is largely removed during pretreatment, but that other mineral species such as pyrite are unaffected. This finding is significant, since calcite removal appears to directly correlate with low severity liquefaction enhancement. Further work will be performed to study this phenomenon in more detail.

  7. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Campbell, J.A.; Linehan, J.C.; Robins, W.H. )

    1992-07-01

    Under contract from the DOE , and in association with CONSOL Inc., Battelle, Pacific Northwest Laboratory (PNL) evaluated four principal and several complementary techniques for the analysis of non-distillable direct coal liquefaction materials in support of process development. Field desorption mass spectrometry (FDMS) and nuclear magnetic resonance (NMR) spectroscopic methods were examined for potential usefulness as techniques to elucidate the chemical structure of residual (nondistillable) direct coal liquefaction derived materials. Supercritical fluid extraction (SFE) and supercritical fluid chromatography/mass spectrometry (SFC/MS) were evaluated for effectiveness in compound-class separation and identification of residual materials. Liquid chromatography (including microcolumn) separation techniques, gas chromatography/mass spectrometry (GC/MS), mass spectrometry/mass spectrometry (MS/MS), and GC/Fourier transform infrared (FTIR) spectroscopy methods were applied to supercritical fluid extracts. The full report authored by the PNL researchers is presented here. The following assessment briefly highlights the major findings of the project, and evaluates the potential of the methods for application to coal liquefaction materials. These results will be incorporated by CONSOL into a general overview of the application of novel analytical techniques to coal-derived materials at the conclusion of CONSOL's contract.

  8. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction

    SciTech Connect

    Song, C.; Huang, L.; Wenzel, K.; Saini, A.K.; Burgess, C.; Hatcher, P.G.; Schobert, H.H.

    1992-12-01

    During this quarterly period progress has been made in the following three subjects related to the effects of low-temperature thermal and catalytic pretreatments on coal structure and reactivity in liquefaction. First, the liquefaction behavior of three bituminous coals with a carbon content ranging from 77% to 85% was evaluated spectroscopically by [sup 13]C NMR and pyrolysis/gas chromatography/mass spectrometry to delineate the structural changes that occur in the coal during liquefaction. Complementary data includes ultimate and proximate analysis, along with optical microscopy for maceral determinations. Even though these are all bituminous coals they exhibit quite different physical and chemical characteristics. The coals vary in rank, ranging from HvC b to HvA b, in petrographic composition, different maceral percentages, and in chemical nature, percent of carbon and of volatiles. It is these variations that govern the products, their distribution, and conversion percentages. Some of the products formed can be traced to a specific maceral group. Second, pyrolysis-GC-MS and FTIR techniques were used to characterize Wyodak coal before and after drying in vacuum and in air and the residues from its thermal and catalytic liquefactions. The analysis of the air-dried coal shows a decrease in the phenolic type structures in the coal network and increase in the carbonyl structures as the oxidative drying proceeds. An enhanced decrease in the carbonyl structure is observed in the liquefaction residues from the raw coal as compared to that of the vacuum dried coal. The analyses of the liquefaction residues of the air-dried coal show an increase in the ether linkages which may have a negative impact on liquefaction. The extent of the solvent adduction also increases during liquefaction with the extent of oxidation of the coal. Finally, the effects of reaction conditions were investigated on conversion of low-rank coals using a Texas subbituminous coal.

  9. Prevention of deleterious deposits in a coal liquefaction system

    DOEpatents

    Carr, Norman L.; Prudich, Michael E.; King, Jr., William E.; Moon, William G.

    1984-07-03

    A process for preventing the formation of deleterious coke deposits on the walls of coal liquefaction reactor vessels involves passing hydrogen and a feed slurry comprising feed coal and recycle liquid solvent to a coal liquefaction reaction zone while imparting a critical mixing energy of at least 3500 ergs per cubic centimeter of reaction zone volume per second to the reacting slurry.

  10. Coal liquefaction process streams characterization and evaluation. Quarterly technical progresss report, January 1--March 31, 1991

    SciTech Connect

    Brandes, S.D.; Winschel, R.A.; Burke, F.P.; Robbins, G.A.

    1991-09-01

    Consol R&D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-fold: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The two broad objectives have considerable overlap and together serve to provide a bridge between process development and analytical chemistry.

  11. Coal liquefaction process streams characterization and evaluation. Quarterly technical progress report, April 1--June 30, 1991

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1991-11-01

    Consol R&D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-fold: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The two broad objectives have considerable overlap and together serve to provide a bridge between process development and analytical chemistry.

  12. Coal liquefaction process streams characterization and evaluation. Quarterly technical progress report, July 1--September 30, 1991

    SciTech Connect

    Winschel, R.A.; Brandes, S.D.; Robbins, G.A.; Burke, F.P.

    1991-11-01

    Consol R&D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-field: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The two broad objectives have considerable overlap and together serve to provide a bridge between process development and analytical chemistry.

  13. Coal liquefaction process streams characterization and evaluation. Quarterly technical progress report, October 1--December 31, 1991

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1992-03-01

    CONSOL R&D is conducting a three-year program to characterize process and product streams from direct coal liquefaction process development projects. The program objectives are two-fold: (1) to obtain and provide appropriate samples of coal liquids for the evaluation of analytical methodology, and (2) to support ongoing DOE-sponsored coal liquefaction process development efforts. The two broad objectives have considerable overlap and together serve to provide a bridge between process development and analytical chemistry.

  14. A Characterization and Evaluation of Coal Liquefaction Process Streams

    SciTech Connect

    1998-10-01

    An updated assessment of the physico-chemical analytical methodology applicable to coal-liquefaction product streams and a review of the literature dealing with the modeling of fossil-fuel resid conversion to product oils are presented in this document. In addition, a summary is provided for the University of Delaware program conducted under this contract to develop an empirical test to determine relative resid reactivity and to construct a computer model to describe resid structure and predict reactivity.

  15. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction

    SciTech Connect

    Song, C.; Saini, A.K.; Wenzel, K.; Huang, L.; Hatcher, P.G.; Schobert, H.H.

    1993-04-01

    This work is a fundamental study of catalytic pretreatments as a potential preconversion step to low-severity liquefaction. The ultimate goal of this work is to provide the basis for the design of an improved liquefaction process and to facilitate our understanding of those processes that occur when coals are initially dissolved. The main objectives of this project are to study the effects of low-temperature pretreatments on coal structure and their impacts on the subsequent liquefaction. The effects of pretreatment temperatures, catalyst type, coal rank and influence of solvent will be examined. We have made significant progress in the following four aspects during this quarterly period: (1) influence of drying and oxidation of coal on the conversion and product distribution in catalytic liquefaction of Wyodak subbituminous coal using a dispersed catalyst; (2) spectroscopic characterization of dried and oxidized Wyodak coal and the insoluble residues from catalytic and thermal liquefaction; (3) the structural alteration of low-rank coal in low-severity liquefaction with the emphasis on the oxygen-containing functional groups; and (4) effects of solvents and catalyst dispersion methods in temperature-programmed and non-programmed liquefaction of three low-rank coals.

  16. Coal liquefaction and gas conversion contractors review conference: Proceedings

    SciTech Connect

    1995-11-01

    This volume contains 55 papers presented at the conference. They are divided into the following topical sections: Direct liquefaction; Indirect liquefaction; Gas conversion (methane conversion); and Advanced research liquefaction. Papers in this last section deal mostly with coprocessing of coal with petroleum, plastics, and waste tires, and catalyst studies. Selected papers are indexed separately for inclusion in the Energy Science and Technology Database.

  17. STUDY OF SOLVENT AND CATALYST INTERACTIONS IN DIRECT COAL LIQUEFACTION

    SciTech Connect

    Michael T. Klein; William H. Calkins; Jasna Tomic

    2000-10-04

    To provide a better understanding of the roles of a solid catalyst and the solvent in Direct Coal Liquefaction, a small reactor was equipped with a porous-walled basket which was permeable to the solvent but was not permeable to the coal or solid catalyst. With this equipment and a high volatile bituminous coal it was found that direct contact between the catalyst in the basket and the coal outside the basket is not required for catalyzed coal liquefaction. The character of the solvent in this system makes a significant difference in the conversion of the coal, the better solvents being strong donor solvents. Because of the extensive use of thermogravimetric analysis in this laboratory, it was noted that the peak temperature for volatiles evolution from coal was a reliable measure of coal rank. Because of this observation, a variety of coals of a range of ranks was investigated. It was shown in this work that measuring the peak temperature for volatiles evolution was a quite precise indicator of rank and correlated closely with the rank value obtained by measuring vitrinite reflectance, a more difficult measurement to make. This prompted the desire to know the composition of the volatile material evolved as a function of coal rank. This was then measured by coupling a TGA to a mass spectrometer using laser activation and photoionization detection TG-PI-MS. The predominant species in volatiles of low rank coal turned out to be phenols with some alkenes. As the rank increases, the relative amounts of alkene and aromatic hydrocarbons increases and the oxygenated species decrease. It was shown that these volatiles were actually pyrolytic products and not volatilization products of the coal. Solvent extraction experiments coupled with Thermogravimetric-photoionization-mass spectrometry (TG-PI-MS) indicated that the low boiling and more extractable material are essentially similar in chemical types to the non-extractable portions but apparently higher molecular weight

  18. CAMD studies of coal structure and coal liquefaction

    SciTech Connect

    Faulon, J.L.; Carlson, G.A.

    1994-10-01

    The macromolecular structure of coal is essential to understand the mechanisms occurring during coal liquefaction. Many attempts to model coal structure can be found in the literature. More specifically for high volatile bituminous coal, the subject of interest the most commonly quoted models are the models of Given, Wiser, Solomon, and Shinn. In past work, the authors`s have used computer-aided molecular design (CAMD) to develop three-dimensional representations for the above coal models. The three-dimensional structures were energy minimized using molecular mechanics and molecular dynamics. True density and micopore volume were evaluated for each model. With the exception of Given`s model, the computed density values were found to be in agreement with the corresponding experimental results. The above coal models were constructed by a trial and error technique consisting of a manual fitting of the-analytical data. It is obvious that for each model the amount of data is small compared to the actual complexity of coal, and for all of the models more than one structure can be built. Hence, the process by which one structure is chosen instead of another is not clear. In fact, all the authors agree that the structure they derived was only intended to represent an {open_quotes}average{close_quotes} coal model rather than a unique correct structure. The purpose of this program is further develop CAMD techniques to increase the understanding of coal structure and its relationship to coal liquefaction.

  19. Fundamental studies of coal liquefaction

    SciTech Connect

    Ross, D.S.

    1993-02-04

    The results for the control run for a single particle are shown in Figure 1. The figure, which includes other thermolytic data for Illinois No. 6 coal, shows that the particle was stable in size to around 440[degree]C. At that point it contracted very rapidly to about half its size over the next 15[degrees]. Also shown are data for the same coal from SRI's field ionization mass spectrometer (FIMS), in which case a sample of the coal is heated at 2.5[degrees]C/min from ambient to 500[degrees]C and the effluent is swept into mass spectrometer. The evolution of the coal volatiles is reflected by accumulated ion count with increasing temperature, and is presented in the figure as the fraction of total volatiles. As the figure shows, the abrupt increase in volatility corresponds very closely to the equally abrupt reduction in particle size. The weight average molecular weight profile from the FIMS work is also in the figure, and shows that the coal experiences a simple loss of volatiles of increasing molecular weight up to around 440[degrees]C. At that point pyrolysis and fragmentation come about, reflected in the quick reversal and decline in molecular weight. The high rate of volatility and shrinkage are clearly associated with this second stage in the pyrolytic process. These results are further in line with the account of Eser et al. (1991) who found in studies of Illinois No. 6 coal in a high pressure microdilatometer that the coal contracted by about 40% in the same region of temperature at heating rates of around 20[degrees]C/min. At higher heating rates the contraction was followed by a swelling. Finally, in our cell work we observed the deposition of tar in the diamond windows starting at around 350[degrees]C.

  20. A study of chemical dehydration of coals and its effect on coal liquefaction yields

    SciTech Connect

    Netzel, D.A.; Miknis, F.P.; Wallace, J.C. Jr.

    1995-12-31

    Chemical dehydration of coals is a relatively unexplored technique for removing water at low temperature. 2,2-Dimethoxypropane was used as the dehydration agent to dry coal and in conjunction with {sup 1}H NMR to simultaneously determine the moisture content in coal. Coals of rank lignite to high volatile bituminous were studied. Analysis of the kinetic data suggested that chemical dehydration provides a method to discriminate quantitatively between surface and readily accessible water from tightly bound internal pore water in coals. The results indicate that high rank coals have proportionally less surface and easily accessible water than the lower rank coals. Solid-state {sup 13}C NMR CP/MAS was employed to measure the changes in coal structure caused by chemical dehydration and residue from the liquefaction of the dried coals. For the chemically dehydrated coals, the coal liquefaction conversions yields were generally greater than the premoisturized coals. This is attributed to retention of some of the solvent and reaction products by the coal, which would have the effect of preventing collapse of the pore structure enabling donor solvent penetration into the pores.

  1. Subtask 3.3 - Feasibility of Direct Coal Liquefaction in the Modern Economic Climate

    SciTech Connect

    Benjamin Oster; Joshua Strege; Marc Kurz; Anthony Snyder; Melanie Jensen

    2009-06-15

    Coal liquefaction provides an alternative to petroleum for the production of liquid hydrocarbon-based fuels. There are two main processes to liquefy coal: direct coal liquefaction (DCL) and indirect coal liquefaction (ICL). Because ICL has been demonstrated to a greater extent than DCL, ICL may be viewed as the lower-risk option when it comes to building a coal liquefaction facility. However, a closer look, based on conversion efficiencies and economics, is necessary to determine the optimal technology. This report summarizes historical DCL efforts in the United States, describes the technical challenges facing DCL, overviews Shenhua's current DCL project in China, provides a DCL conceptual cost estimate based on a literature review, and compares the carbon dioxide emissions from a DCL facility to those from an ICL facility.

  2. Coal liquefaction process streams characterization and evaluation. FIMS analysis of direct coal liquefaction process streams

    SciTech Connect

    Malhotra, R.; McMillen, D.F.

    1994-03-01

    This study was designed to apply the method of field ionization mass spectrometry (FIMS) for the analysis of direct coal liquefaction process-stream samples. The FIMS method was shown to have a high potential for application to direct coal liquefaction-derived samples in a Phase 1 project in this program. In this Phase 3 project, the FIMS method was applied to a set of samples produced in HRI bench-scale liquefaction Runs CC-15 and CC-16. FIMS was used to obtain the molecular weight profile of the samples and to identify specific prominent peaks in the low end (160--420 Da) region of the molecular weight profile. In the samples examined in this study, species were identified which previously were recognized as precursors to the formation of high molecular weight structures associated with the formation of coke in petroleum vacuum gas oils.

  3. Hydrodeoxygenation in low-rank coal liquefaction systems using novel organometallic catalyst precursors

    SciTech Connect

    Kirby, S.R.; Song, C.; Schobert, H.H.

    1996-12-31

    Oxygen functionalities, especially phenols, are undesirable components of coal derived liquids. Removal of these compounds from the products of coal liquefaction is required. A beneficial alternative would be the removal of these functionalities, or the prevention of their formation, during the liquefaction process. Organometallic precursors of Co, Ni and Mo have been studied as catalysts. To ascertain the hydrodeoxygenation properties of these catalysts under liquefaction conditions, model compounds were investigated. Anthrone, Dibutylmethyl phenol, dinaphthyl ether and xanthene were studied to provide a comparison of conversions of deoxygenated products. Studies of the deoxygenating abilities of these catalyst precursors in coal liquefaction systems have also been performed. Improvements in conversion and product quality are observed. Both these factors are dependent on the coal used.

  4. Catalysts for coal liquefaction processes

    DOEpatents

    Garg, D.

    1986-10-14

    Improved catalysts for catalytic solvent refining or hydroliquefaction of non-anthracitic coal at elevated temperatures under hydrogen pressure in a hydrogen donor solvent comprise a combination of zinc or copper, or a compound thereof, and a Group VI or non-ferrous Group VIII metal, or a compound thereof.

  5. Catalysts for coal liquefaction processes

    DOEpatents

    Garg, Diwakar

    1986-01-01

    Improved catalysts for catalytic solvent refining or hydroliquefaction of non-anthracitic coal at elevated temperatures under hydrogen pressure in a hydrogen donor solvent comprise a combination of zinc or copper, or a compound thereof, and a Group VI or non-ferrous Group VIII metal, or a compound thereof.

  6. Advanced direct coal liquefaction concepts

    SciTech Connect

    Berger, D.J.; Parker, R.J.; Simpson, P.L. )

    1992-01-01

    During the first quarter of FY 1993, the Project proceeded close to the Project Plan. The analysis of the feed material has been completed as far as possible. Some unplanned distillation was needed to correct the boiling range of the Black Thunder solvent used during the autoclave tests. Additional distillation will be required if the same solvent is to be used for the bench unit tests. A decision on this is still outstanding. The solvent to be used with Illinois No. 6 coal has not yet been defined. As a result, the procurement of the feed and the feed analysis is somewhat behind schedule. Agglomeration tests with Black Thunder coal indicates that small agglomerates can be formed. However, the ash removal is quite low (about 10%), which is not surprising in view of the low ash content of the coal. The first series of autoclave tests with Black Thunder coal was completed as planned. Also, additional runs are in progress as repeats of previous runs or at different operating conditions based on the data obtained so far. The results are promising indicating that almost complete solubilization (close to 90%) of Black Thunder coal can be achieved in a CO/H[sub 2]O environment at our anticipated process conditions. The design of the bench unit has been completed. In contrast to the originally planned modifications, the bench unit is now designed based on a computerized control and data acquisition system. All major items of equipment have been received, and prefabrication of assemblies and control panels is proceeding on schedule. Despite a slight delay in the erection of the structural steel, it is anticipated that the bench unit will be operational at the beginning of April 1993.

  7. Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama

    SciTech Connect

    Not Available

    1992-01-01

    This report presents the results of Run 260 performed at the Advanced Coal Liquefaction R D Facility in Wilsonville. The run was started on July 17, 1990 and continued until November 14, 1990, operating in the Close-Coupled Integrated Two-Stage Liquefaction mode processing Black Thunder mine subbituminous coal (Wyodak-Anderson seam from Wyoming Powder River Basin). Both thermal/catalytic and catalytic/thermal tests were performed to determine the methods for reducing solids buildup in a subbituminous coal operation, and to improve product yields. A new, smaller interstage separator was tested to reduce solids buildup by increasing the slurry space velocity in the separator. In order to obtain improved coal and resid conversions (compared to Run 258) full-volume thermal reactor and 3/4-volume catalytic reactor were used. Shell 324 catalyst, 1/16 in. cylindrical extrudate, at a replacement rate of 3 lb/ton of MF coal was used in the catalytic stage. Iron oxide was used as slurry catalyst at a rate of 2 wt % MF coal throughout the run. (TNPS was the sulfiding agent.)

  8. Coal liquefaction process streams characterization and evaluation: The preliminary evaluation of the kinetics of coal liquefaction distillation resid conversion

    SciTech Connect

    Klein, M.T.; Calkins, W.H.; Huang, He

    1994-02-01

    This study evaluated the use of a novel laboratory-scale batch reactor, designed by the University of Delaware, to study the kinetics of coal liquefaction resid reactivity. The short time batch reactor (STBR) is capable of conducting reactions at temperatures up to 450{degrees}C and pressures up to 2500 psi at well-defined reaction times from a few seconds to 30 min or longer. Sixty experiments were conducted with the STBR in this project. The products of the resid/tetralin/hydrogen reaction were separated by solubility, and several analytical procedures were used to evaluate the reaction products, including thermogravimetric analysis (TGA), gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS). Changes were monitored in the boiling ranges of the products, as a function of process conditions (time, temperature, and tetralin donor solvent-to-resid ratio), with and without catalysts. Two distillation resid samples were studied; Sample 1 is the resid of the second stage product stream from Wilsonville Run 259 which used Pittsburgh seam coal (Ireland mine) bituminous coal, and Sample 2 is the resid of the same streak from Wilsonville Run 260 which used Wyodak and Anderson (Black Thunder Mine) subbituminous coal. It was determined that the resid reactivity was different for the two samples studied. The results demonstrate that further development of this experimental method is warranted to empirically assess resid reactivity and to provide data for use in the construction of an empirical model of coal conversion in the direct liquefaction process.

  9. Fundamental studies of coal liquefaction

    SciTech Connect

    Ross, D.S.

    1992-12-04

    SRI International is conducting studies of the effects of liquid water at temperatures and pressures near its critical point on the behavior of coal. The present study involves the construction and operation of a cell for visual observation of the process. The cell is batch charged with a dispersion of coal particles in solvent; it is designed for continuous flow operation should that mode of operation become desirable. It can be electrically heated to 550[degree]C and can handle pressures to 5000 psi. Direct observation of individual particles takes place through a pair of diamond windows, a lens assembly, and a television monitoring system. A number of runs have been performed during this quarter, including runs with Wyodak and Illinois No. 6 coal with both water and tetralin. A video tape of two runs was submitted with a monthly report during this quarter, and a tape with four runs in included with this report. Unfortunately just as our experience with the cell was developing, one of the diamonds cracked and the replacement is not expected before December. Accordingly we have spent some time operating the cell with a single window and front lighting.

  10. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1992-08-01

    This is the tenth Quarterly Technical Progress Report under DOE Contract DE-AC22-89PC89883. Process oils from Wilsonville Run 262 were analyzed to provide information on process performance. Run 262 was operated from July 10 through September 30, 1991, in the thermal/catalytic Close-Coupled Integrated Two-Stage Liquefaction (CC-ITSL) configuration with ash recycle. The feed coal was Black Thunder Mine subbituminous coal. The high/low temperature sequence was used. Each reactor was operated at 50% of the available reactor volume. The interstage separator was in use throughout the run. The second-stage reactor was charged with aged Criterion 324 catalyst (Ni/Mo on 1/16 inch alumina extrudate support). Slurry catalysts and sulfiding agent were fed to the first-stage reactor. Molyvan L is an organometallic compound which contains 8.1% Mo, and is commercially available as an oil-soluble lubricant additive. It was used in Run 262 as a dispersed hydrogenation catalyst precursor, primarily to alleviate deposition problems which plagued past runs with Black Thunder coal. One test was made with little supported catalyst in the second stage. The role of phenolic groups in donor solvent properties was examined. In this study, four samples from direct liquefaction process oils were subjected to O-methylation of the phenolic groups, followed by chemical analysis and solvent quality testing.

  11. Mild coal pretreatment to improve liquefaction reactivity. Quarterly technical progress report, June--August 1991

    SciTech Connect

    Miller, R.L.

    1991-12-31

    This report describes work completed during the fourth quarter of a three year project to study the effects of mild chemical pretreatment on coal dissolution reactivity during low severity liquefaction or coal/oil coprocessing. The overall objective of this research is to elucidate changes in the chemical and physical structure of coal by pretreating with methanol or other simple organic solvent and a trace amount of hydrochloric acid and measure the influence of these changes on coal dissolution reactivity. This work is part of a larger effort to develop a new coal liquefaction or coal/oil coprocessing scheme consisting of three main process steps: (1) mile pretreatment of the feed coal to enhance dissolution reactivity and dry the coal, (2) low severity thermal dissolution of the pretreated coal to obtain a very reactive coal-derived residual material amenable to upgrading, and (3) catalytic upgrading of the residual products to distillate liquids.

  12. Liquefaction of calcium-containing subbituminous coals and coals of lower rank

    DOEpatents

    Brunson, Roy J.

    1979-01-01

    An improved process for the treatment of a calcium-containing subbituminous coal and coals of lower rank to form insoluble, thermally stable calcium salts which remain within the solids portions of the residue on liquefaction of the coal, thereby suppressing the formation of scale, made up largely of calcium carbonate which normally forms within the coal liquefaction reactor (i.e., coal liquefaction zone), e.g., on reactor surfaces, lines, auxiliary equipment and the like. An oxide of sulfur, in liquid phase, is contacted with a coal feed sufficient to impregnate the pores of the coal. The impregnated coal, in particulate form, can thereafter be liquefied in a coal liquefaction reactor (reaction zone) at coal liquefaction conditions without significant formation of scale.

  13. Coal liquefaction process streams characterization and evaluation: Analysis of coal-derived synthetic crude from HRI CTSL Run CC-15 and HRI Run CMSL-2

    SciTech Connect

    Sturm, G.P. Jr.; Kim, J.; Shay, J.

    1994-01-01

    Under subcontract from CONSOL Inc. (US DOE Contract No. DE-AC22-89PC89883), IIT Research Institute, National Institute for Petroleum and Energy Research applied a suite of petroleum inspection tests to two direct coal liquefactions net product oils produced in two direct coal liquefaction processing runs. Two technical reports, authored by NIPER, are presented here. The following assessment briefly describes the two coal liquefaction runs and highlights the major findings of the project. It generally is concluded that the methods used in these studies can help define the value of liquefaction products and the requirements for further processing. The application of these methods adds substantially to our understanding of the coal liquefaction process and the chemistry of coal-derived materials. These results will be incorporated by CONSOL into a general overview of the application of novel analytical techniques to coal-derived materials at the conclusion of this contract.

  14. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction. [Effect of pretreatment before liquefaction

    SciTech Connect

    Not Available

    1992-07-01

    The main task of this quarter was to install reactors to conduct preconversion and liquefaction of coal. Coal and coal liquids were collected. The anaerobic chamber (Model 855-AC; Plas Labs, inc.) was procured and set up to store coal samples under an inert gas. Equipment to treat products was assembled, including Soxhlet extraction units, fractionation columns, a distillation column, and a rotary evaporator. Two gas chromatographs for analysis of gases and liquid were adjusted. Two reactor systems were installed for the experimental apparatus. One was Model 4576 high-temperature and high-pressure autoclave (Parr Instrument, 500{degrees}C and 5000 psi) (see Figure 1); the other was a 27 ml of microreactors. The autoclave was obtained from the manufacturer and assembled. The experimental set-up of microreactors are shown in Figure 2.

  15. Kinetics of coal liquefaction at very short reaction times

    SciTech Connect

    Huang, H.; Wang, K.; Wang, S.

    1995-12-31

    Kinetics of direct liquefaction of Illinois No. 6 Bituminous coal in tetralin has been investigated at three temperatures (309-424{degrees}C) during the first few seconds of the reaction and up to an hour. Conversion was followed by the ash content of the coal residue as determined by TGA, and changes in the reaction were followed by changes in the TGA parameters, such as Volatile Matter (VM) and Fixed Carbon (FC). The effects of temperature on the reaction kinetics were in both catalyzed and uncatalyzed liquefaction with a large excess of tetralin, there is an initial very rapid extraction of the soluble matter by the tetralin. After extraction there is an induction period followed by a slower rate of conversion of the coal structure itself. At higher temperatures, the amount of extraction increases and the induction period becomes shorter. At least two conflicting processes are occurring in the last stage: (1) breakdown of the coal structure to liquid products, and (2) formation of retrograde material (precursor of tar and coke). Catalysts such as sulfided molybdenum naphthenate in the presence of hydrogen greatly reduce the formation of retrograde products.

  16. Application of Light Microscopy to Direct Coal Liquefaction Research

    PubMed

    Irdi; Warzinski; Booher

    1998-01-01

    : Light microscopy was used to analyze the effects of added catalyst at different conditions (temperature and reaction times) in liquefaction testing of a low pyritic sulfur bituminous coal. Quantitative changes in vitrinite/vitroplast reflectance of coal and liquefaction residues were shown to be useful markers in analyzing and understanding the role of catalyst during the initial stage of coal particle hydrogenation. Lower reflectance values corresponded to increased conversions up to about the 60 min and 375 degreesC experimental conditions. Microscopical observation of liquefaction residues also revealed the presence of "wall scales" of varying width.

  17. Gasification of residual materials from coal liquefaction: Type II preliminary pilot-plant evaluation of molten H-Coal liquefaction residue

    SciTech Connect

    Wu, C.M.; Robin, A.M.

    1982-10-01

    About 5.5 tons of vacuum tower bottoms (residue) obtained from the liquefaction of Illinois No. 6 coal from the H-Coal liquefaction process pilot plant at Catlettsburg, Kentucky were successfully gasified at Texaco's Montebello Research Laboratory on January 16-17, 1982. Two test runs with molten H-Coal liquefaction residue were completed, each at a different operating temperature. The conversions of carbon in the feed to syngas achieved during the two test runs were 99.4 and 98.6 percent, yielding 35.2 and 35.5 standard cubic feet of dry syngas per pound of residue feed. The oxygen requirement was about 0.8 pound of oxygen per pound of residue for each run. The dry syngas contained about 93.4 (vol.) percent carbon monoxide plus hydrogen. The two short pilot unit runs did confirm the operability of the Texaco Synthesis Gas Generation Process with this feedstock, and the data obtained confirm earlier predictions of performance efficiency. A comparison of the gasification efficiency of molten H-Coal liquefaction residue with the gasification efficiency of H-Coal liquefaction residue-water slurry revealed that the molten process was more efficient. The molten system required less oxygen for gasification, 0.78 versus 1.00 pounds of oxygen per pound of residue, and produced a greater volume percent carbon monoxide plus hydrogen in the product syngas, 93.4% versus 79.2%, than the residue-water slurry.

  18. STUDY OF SOLVENT AND CATALYST INTERACTIONS IN DIRECT COAL LIQUEFACTION

    SciTech Connect

    Michael T. Klein

    2000-01-01

    There are several aspects of the Direct Coal Liquefaction process which are not fully understood and which if better understood might lead to improved yields and conversions. Among these questions are the roles of the catalyst and the solvent. While the solvent is known to act by transfer of hydrogen atoms to the free radicals formed by thermal breakdown of the coal in an uncatalyzed system, in the presence of a solid catalyst as is now currently practiced, the yields and conversions are higher than in an uncatalyzed system. The role of the catalyst in this case is not completely understood. DOE has funded many projects to produce ultrafine and more active catalysts in the expectation that better contact between catalyst and coal might result. This approach has met with limited success probably because mass transfer between two solids in a fluid medium i.e. the catalyst and the coal, is very poor. It is to develop an understanding of the role of the catalyst and solvent in Direct Liquefaction that this project was initiated. Specifically it was of interest to know whether direct contact between the coal and the catalyst was important. By separating the solid catalyst in a stainless steel basket permeable to the solvent but not the coal in the liquefaction reactor, it was shown that the catalyst still maintains a catalytic effect on the liquefaction process. There is apparently transfer of hydrogen atoms from the catalyst through the basket wall to the coal via the solvent. Strong hydrogen donor solvents appear to be more effective in this respect than weak hydrogen donors. It therefore appears that intimate contact between catalyst and coal is not a requirement, and that the role of the catalyst may be to restore the hydrogen donor strength to the solvent as the reaction proceeds. A range of solvents of varying hydrogen donor strength was investigated. Because of the extensive use of thermogravimetric analysis in this laboratory in was noted that the peak

  19. High dispersed catalysts for coal liquefaction. Quarterly report No. 7, February 23, 1993--May 22, 1993

    SciTech Connect

    Hirschon, A.S.; Wilson, R.B.

    1993-08-19

    The objectives of this project are to study the effect of pretreatment methods on the two-stage liquefaction process. In particular, the effects of dispersed catalysts and carbon monoxide atmospheres on a coal liquefaction process. The project is divided into three technical tasks. Task 1 involves the analyses of the liquefaction products derived from liquefaction experiments using the catalysts Fe(CO){sub 5} and the sulfated iron catalyst, Fe{sub 2}O{sub 3}{center_dot}SO{sub 4}. We also analyzed the products derived from treating the recycle vehicle under coal liquefaction conditions with no coal or catalyst present, and found that the toluene and THF fractions had low H/C ratios. No CO or CO{sub 2} gases were detected after reaction, although considerable amount of methane gas was produced, suggesting that during the liquefaction runs the carbon oxides are produced only from the coal, as expected, but that methane gas is produced both from the recycle solvent and the coal. We now have more information about the recycle solvent from Wilsonville, who report that the residue was 63%, composed of 45% resid and 18% insoluble inorganic (CI), and a distilable portion of 37% (1050{degrees}F). During this quarter we compared coal conversions using Fe(CO){sub 5} with CO and H{sub 2}/CO atmospheres and determined the effect of using sulfated iron (Fe{sub 2}O{sub 3}{center_dot}SO{sub 4}) as a conversion catalyst. Also, the coal liquefaction recycle vehicle was subjected to coal product distribution. We found that the Fe(CO){sub 5} under a pure hydrogen atmosphere gave better conversions than under a CO/H{sub 2} atmosphere in terms of oils and asphaltenes but was equal in terms of overall conversion into soluble fractions.

  20. The role of recycle oil in direct coal liquefaction process development

    SciTech Connect

    Burke, F.P.

    1995-08-01

    It has long been recognized that use of a recycle oil is a convenient and perhaps necessary feature of a practical direct coal liquefaction process. The recycle oil performs a number of important functions. It serves as a vehicle to convey coal into the liquefaction reactor and products from the reactor. It is a medium for mass and heat transfer among the solid, liquid, and gaseous components of the reactor inventory. It can act as a reactant or intermediate in the liquefaction process. Therefore, the nature of the recycle oil can have a determining effect on process configuration and performance, and the characterization of recycle oil composition and chemistry has been the subject of considerable interest. This paper discusses recycle oil characterization and its influence on the industrial development of coal liquefaction technology,

  1. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1992-11-01

    This is the twelfth Quarterly Technical Progress Report under DOE Contract DE-AC22-89PC89883. Major topics reported are: Summaries of the final reports produced by Lehigh University, West Virginia University, and Vander Sande Associates under the Participants Program are presented. Analytical data produced by CONSOL are provided in Appendix I for all samples employed in the Participants Program and issued with the samples to research groups in the Participants Program. A paper was presented at the 1992 US Department of Energy Pittsburgh Energy Technology Center Liquefaction Contractors' Review Conference, held in Pittsburgh September 23--24, 1992, entitled The Chemical Nature of Coal Liquid Resids and the Implications for Process Development''. It appears as Appendix 2 in this report.

  2. Coal liquefaction process streams characterization and evaluation

    SciTech Connect

    Rathbone, R.F.; Hower, J.C.; Derbyshire, F.J. . Center for Applied Energy Research)

    1991-10-01

    This study demonstrated the feasibility of using fluorescence and reflectance microscopy techniques for the examination of distillation resid materials derived from direct coal liquefaction. Resid, as defined here, is the 850{degrees}F{sup +} portion of the process stream, and includes soluble organics, insoluble organics and ash. The technique can be used to determine the degree of hydrogenation and the presence of multiple phases occurring within a resid sample. It can also be used to infer resid reactivity. The technique is rapid, requiring less than one hour for sample preparation and examination, and thus has apparent usefulness for process monitoring. Additionally, the technique can distinguish differences in samples produced under various process conditions. It can, therefore, be considered a potentially useful technique for the process developer. Further development and application of this analytical method as a process development tool is justified based on these results.

  3. Coal liquefaction. Quarterly report, July-September 1979

    SciTech Connect

    1980-07-01

    The status of coal liquefaction pilot plants supported by US DOE is reviewed under the following headings: company involved, location, contract, funding, process name, process description, flowsheet, history and progress during the July-September 1979 quarter. Supporting projects such as test facilities, refining and upgrading coal liquids, catalyst development, and gasification of residues from coal gasification plants are discussed similarly. (LTN)

  4. Dermal toxicity of a high-boiling (bp 250-450 degrees C) coal liquefaction product in the rat--II.

    PubMed

    Chu, I; Villeneuve, D C; Côté, M; Secours, V; Otson, R; Valli, V E

    1988-01-01

    Coal liquefaction products have been considered as an alternate source of energy to replace conventional crude oil. The present study was designed to investigate the dermal toxicity of a heavy fraction of coal liquefaction product (CLP, bp 250-450 degrees C) in the rat. Groups of 10 male and 10 female Sprague-Dawley rats (180-200 g) were treated dermally with CLP at dose levels of 100, 200, 400, or 800 mg/kg body weight.d for 6 wk. The controls were treated with 0.4 ml/kg of normal saline, while the positive control group received 400 mg/kg diesel fuel. Growth suppression was observed in all CLP-treated groups of males; in the females this effect occurred in the two highest dose groups. Diesel fuel at 400 mg/kg also caused growth suppression of a similar magnitude to that of CLP in male rats. Male animals treated with high doses of CLP or diesel fuel had severe skin lesions. Increased liver weights were observed in the diesel fuel-treated as well as all CLP-treated groups of females. The kidney weights of females treated with 400 mg/kg and 800 mg/kg CLP were also higher than control values. Decreased red cell count, hemoglobin, and hematocrit volume occurred in some CLP and diesel fuel groups of both sexes. There was mild bone marrow hyperplasia in rats of both sexes treated with CLP or diesel fuel. Mild histological changes were observed in the thyroid, liver, bone marrow, and skin of rats of both sexes treated with CLP and diesel fuel. Based on the data presented, dermal application of CLP produced systemic toxicity at the dose levels studied, and CLP and diesel fuel possess toxic effects of similar nature and magnitude.

  5. Coal liquefaction process streams characterization and evaluation. Volume 1, Base program activities

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1994-05-01

    This 4.5-year project consisted of routine analytical support to DOE`s direct liquefaction process development effort (the Base Program), and an extensive effort to develop, demonstrate, and apply new analytical methods for the characterization of liquefaction process streams (the Participants Program). The objective of the Base Program was to support the on-going DOE direct coal liquefaction process development program. Feed, process, and product samples were used to assess process operations, product quality, and the effects of process variables, and to direct future testing. The primary objective of the Participants Program was to identify and demonstrate analytical methods for use in support of liquefaction process development, and in so doing, provide a bridge between process design, and development, and operation and analytical chemistry. To achieve this objective, novel analytical methods were evaluated for application to direct coal liquefaction-derived materials. CONSOL teamed with 24 research groups in the program. Well-defined and characterized samples of coal liquefaction process-derived materials were provided to each group. CONSOL made an evaluation of each analytical technique. During the performance of this project, we obtained analyses on samples from numerous process development and research programs and we evaluated a variety of analytical techniques for their usefulness in supporting liquefaction process development. Because of the diverse nature of this program, we provide here an annotated bibliography of the technical reports, publications, and formal presentations that resulted from this program to serve as a comprehensive summary of contract activities.

  6. Short contact time liquefaction of subbituminous coal

    SciTech Connect

    Not Available

    1984-07-01

    This report describes a series of continuous unit studies determining how pyrite addition, as well as other variables (including solvent quality, slurry recycle, temperature, residence time), affect the short contact time liquefaction of subbituminous coal. Dissolution of low-rank coal is much more strongly affected by pyrite addition than by solvent quality. Mild hydrotreatment of an SRC I solvent provided a solvent which increased conversion only slightly over that achieved with the original SRC I solvent. Addition of pyrite or pyrrhotite, however, resulted in a significant improvement in conversion. The low quality solvent was SRC I solvent while the high quality solvent was from the Lummus Integrated Two-Stage Liquefaction Process. Essentially identical conversions were obtained with the high quality and low quality solvents. Pyrite brought about the same significant improvement in conversion in each of the solvents. Although use of a lower level of a higher quality catalyst (CoMo/Al/sub 2/O/sub 3/) increased hydrogenation and increased conversion of SRC to distillate more effectively than pyrite, the pyrite was more effective in decreasing the insoluble organic matter yield. Conversion was also increased by partial slurry recycle; i.e., by recycling a fraction of the dissolver effluent (containing SRC, insoluble organic matter and mineral matter) mixed with an equal amount of distillate in place of all distillate solvent of the normal short contact time SRC I process. Over the ranges investigated, conversions increased with increasing temperature or residence time. These increasing conversions were generally accompanied by increasing hydrogen consumption and/or hydrocarbon gas make.

  7. Novel bimetallic dispersed catalysts for temperature-programmed coal liquefaction. Technical progress report, April--June 1996

    SciTech Connect

    Kirby, S.R.; Martin, S.C.; Song, Chunshan; Schobert, H.H.

    1996-08-01

    This quarterly report describes our recent work on two related subjects: effect of using organometallic catalyst precursor on hydrodeoxygenation under coal liquefaction conditions, and the effect of mineral matters in liquefaction reactions of coals. Oxygen functionalities, especially phenols, are undesirable components of coal derived liquids. Removal of these compounds from the products of coal liquefaction is required. A beneficial alternative would be the removal of these functionalities, or the prevention of their formation, during the liquefaction process. Organometallic precursors of Co, Ni and Mo have been studied as catalysts. To ascertain the hydrodeoxygenation properties of these catalysts under liquefaction conditions, model compounds were investigated. Anthrone, Dibutylmethyl phenol, dinaphthyl ether and xanthene were studied to provide a comparison of conversions to deoxygenated products. Studies of the deoxygenating abilities of these catalyst precursors in coal liquefaction systems have also been performed. Improvements in conversion and product quality are observed. Both these factors are dependent on the coal used. It is also considered that some mineral matters in coal may have catalytic actions. Demineralization by successive HCl/HF treatments of a low rank coal has demonstrated that removal of the inherent mineral matter imparts no serious detrimental effect upon low temperature liquefaction. It appears that elimination of such species allows for better access for gaseous H{sub 2}, as suggested by previous studies.

  8. Process for coal liquefaction using electrodeposited catalyst

    DOEpatents

    Moore, Raymond H.

    1978-01-01

    A process for the liquefaction of solid hydrocarbonaceous materials is disclosed. Particles of such materials are electroplated with a metal catalyst and are then suspended in a hydrocarbon oil and subjected to hydrogenolysis to liquefy the solid hydrocarbonaceous material. A liquid product oil is separated from residue solid material containing char and the catalyst metal. The catalyst is recovered from the solid material by electrolysis for reuse. A portion of the product oil can be employed as the hydrocarbon oil for suspending additional particles of catalyst coated solid carbonaceous material for hydrogenolysis.

  9. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction. Quarterly report, July 1, 1992--September 30, 1992

    SciTech Connect

    Not Available

    1992-10-01

    Soaking coal in coal liquids at 300-400{degrees}C (high-tenperature soaking) has been studied for coal dissolution prior to liquefaction in the previous task. Two high-volatile bituminous coals, Illinois No. 6 and Pittsburgh No. 8, were examined in three different coal liquids. The high-temperature soaking was effective to solubilize more than 70 wt% cf these coals. The mechanism of disintegration of coal by the high-temperature soaking was investigated under various soaking conditions. The products was also analyzed with solvent swelling. These results were rationalized that coal is solubilized primarily by physical disintegration. The derived mechanism was consistent with the new concept of coal structure: A significant portion of coal is physically associated, not three-dimensionally cross-linked. Radically-induced scission reactions were proposed to prorate breakage of coal moleculs by the combination of the high-temperature soaking before liquefaction. In this term, the effect of radical initiators were investigated under the conditions of the high-temperature soaking and liquefaction. Illinois No. 6 coal and a coal liquid derived from the same coal were used. The first section reports the effect of radical initiators on coal disintegration, and the second section reports the effect of a radical initiator on coal liquefaction. Radical initiators had a positive effect on disintegration. However, the effect was highly temperature-dependent and had a negative effect on liquefaction at high tenperatures.

  10. U.S. DOE indirect coal liquefaction program: An overview

    SciTech Connect

    Shen, J.; Schmetz, E.; Winslow, J.; Tischer, R.; Srivastava, R.

    1997-12-31

    Coal is the most abundant domestic energy resource in the United States. The Fossil Energy Organization within the US Department of Energy (DOE) has been supporting a coal liquefaction program to develop improved technologies to convert coal to clean and cost-effective liquid fuels to complement the dwindling supply of domestic petroleum crude. The goal of this program is to produce coal liquids that are competitive with crude at $20 to $25 per barrel. Indirect and direct liquefaction routes are the two technologies being pursued under the DOE coal liquefaction program. This paper will give an overview of the DOE indirect liquefaction program. More detailed discussions will be given to the F-T diesel and DME fuels which have shown great promises as clean burning alternative diesel fuels. The authors also will briefly discuss the economics of indirect liquefaction and the hurdles and opportunities for the early commercial deployment of these technologies. Discussions will be preceded by two brief reviews on the liquid versus gas phase reactors and the natural gas versus coal based indirect liquefaction.

  11. Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama

    SciTech Connect

    Not Available

    1992-09-01

    This report presents the results of Run 261 performed at the Advanced Coal Liquefaction R D Facility in Wilsonville, Alabama. The run started on January 12, 1991 and continued until May 31, 1991, operating in the Close-Coupled Integrated Two-Stage Liquefaction mode processing Illinois No. 6 seam bituminous coal (from Burning star No. 2 mine). In the first part of Run 261, a new bimodal catalyst, EXP-AO-60, was tested for its performance and attrition characteristics in the catalytic/catalytic mode of the CC-ITSL process. The main objective of this part of the run was to obtain good process performance in the low/high temperature mode of operation along with well-defined distillation product end boiling points. In the second part of Run 261, Criterion (Shell) 324 catalyst was tested. The objective of this test was to evaluate the operational stability and catalyst and process performance while processing the high ash Illinois No. 6 coal. Increasing viscosity and preasphaltenes made it difficult to operate at conditions similar to EXP-AO-60 catalyst operation, especially at lower catalyst replacement rates.

  12. Advanced liquefaction using coal swelling and catalyst dispersion techniques. Quarterly progress report, July--September 1993

    SciTech Connect

    Curtis, C.W.; Gutterman, C.; Chander, S.

    1993-12-31

    The overall objective of this project is to develop a new approach for the direct liquefaction of coal to produce an all-distillate product slate at a sizable cost reduction over current technology. The approach integrates coal selection, pretreatment, coal swelling with catalyst impregnation, liquefaction, product recovery with characterization, alternate bottoms processing, and carrying out a technical assessment including an economic evaluation. The primary coal of this program, Black Thunder subbituminous coal, can be effectively beneficiated to about 3.5 wt % ash using aqueous sulfurous acid pretreatment. This treated coal can be further beneficiated to about 2 wt % ash using commercially available procedures. All three coals used in this study (Black Thunder, Burning Star bituminous, and Martin Lake lignite) are effectively swelled by a number of solvents. The most effective solvents are those having hetero-functionality. laboratory- and bench-scale liquefaction experimentation is underway using swelled and catalyst impregnated coal samples. Higher coal conversions were observed for the SO{sub 2}-treated subbituminous coal than the raw coal, regardless of catalyst type. Conversions of swelled coal were highest when Molyvan L, molybdenum naphthenate, and nickel octoate, respectively, were added to the liquefaction solvent. The study of bottoms processing consists of combining the ASCOT process which consists of coupling solvent deasphalting with delayed coking to maximize the production of coal-derived liquids while rejecting solids within the coke drum. The asphalt production phase has been completed; representative product has been evaluated. The solvent system for the deasphalting process has been established. Two ASCOT tests produced overall liquid yields (63.3 wt % and 61.5 wt %) that exceeded the combined liquid yields from the vacuum tower and ROSE process.

  13. Coal liquefaction. Quarterly report, April-June 1979

    SciTech Connect

    1980-04-01

    DOE's program for the conversion of coal to liquid fuels was begun by two of DOE's predecessor agencies: Office of Coal Research (OCR) in 1962, and Bureau of Mines, US Department of the Interior, in the 1930's. Current work is aimed at improved process configurations for both catalytic and non-catalytic processes to provide more attractive processing economics and lower capital investment. The advantage of coal liquefaction is that the entire range of liquid products, especially boiler fuel, distillate fuel oil, and gasoline, can be produced from coal by varying the type of process and operating conditions used in the process. Furthermore, coal-derived liquids have the potential for use as chemical feedstocks. To provide efficient and practical means of utilizing coal resources, DOE is supporting the development of several conversion processes that are currently in the pilot plant stage. DOE, together with the Electric Power Research Institue, has contracted with fourteen projects are described brieflly: funding, description, status, history, and progress in the current quarter. (LTN)

  14. Corrosion coupon studies at coal liquefaction pilot plants

    SciTech Connect

    Keiser, J.R.; Baylor, V.B.; Howell, M.; Newsome, J.F.

    1983-09-01

    As part of the Fossil Energy Materials Program at Oak Ridge National Laboratory, we have supplied corrosion coupons to coal-liquefaction pilot plants for exposure in selected vessels. These vessels were chosen on the basis of previous corrosion experience, anticipated corrosion behavior (especially important when operating conditions were changed), accessibility, and availability. Alloys exposed were selected to give a series with a corrosion resistance ranging from less than to greater than that thought to be needed for each application. Corrosion rates calculated from weight changes of the exposed coupons provide information useful in selecting materials for coal-liquefaction plants. The results presented are from coupons exposed in the Wilsonville, Alabama, and Fort Lewis, Washington, Solvent Refined Coal pilot plants; the Catlettsburg, Kentucky, H-Coal Pilot Plant; and the Baytown, Texas, Exxon Coal Liquefaction Pilot Plant.

  15. Optimization of reactor configuration in coal liquefaction. Sixth quarterly report, January 1--March 31, 1993

    SciTech Connect

    Comolli, A.G.; Johanson, E.S.; Lee, L.K.; Pradhan, V.R.; Stalzer, R.M.

    1993-04-01

    The overall objective of the program is to achieve a new approach to liquefaction that generates an all distillates product slate at reduced cost of about $25 per barrel of crude oil equivalent. The quarterly report covers work on Laboratory Support, Laboratory Scale Operations, Technical Assessment, and Project Management. The experimental work undertaken in the sixth quarter was concerned mostly with microautoclave studies on: (1) the ultimate convertibility of Black Thunder Mine Coal using hexahydropyrene as solvent; (2) the reactivity of partially converted Illinois No. 6 coal; (3) the reactivity of resid from Illinois No. 6 coal; (4) the catalytic activity of tin oxide for coal liquefaction. A laboratory scale run for evaluating the three-stage liquefaction and interstage stream concentration concepts has been developed. A two-stage Robinson-Mahoney CSTR reactor system will be used to simulate the above concepts.

  16. Liquefaction of calcium-containing subbituminous coals and coals of lower rank

    DOEpatents

    Gorbaty, Martin L.; Taunton, John W.

    1980-01-01

    A process for the treatment of a calcium-containing subbituminous coal and coals of lower rank to form insoluble, thermally stable calcium salts which remain within the solids portions of the residue on liquefaction of the coal, thereby suppressing the formation scale, made up largely of calcium carbonate deposits, e.g., vaterite, which normally forms within the coal liquefaction reactor (i.e., coal liquefaction zone), e.g., on reactor surfaces, lines, auxiliary equipment and the like. A solution of a compound or salt characterized by the formula MX, where M is a Group IA metal of the Periodic Table of the Elements, and X is an anion which is capable of forming water-insoluble, thermally stable calcium compounds, is maintained in contact with a particulate coal feed sufficient to impregnate said salt or compound into the pores of the coal. On separation of the impregnated particulate coal from the solution, the coal can be liquefied in a coal liquefaction reactor (reaction zone) at coal liquefaction conditions without significant formation of vaterite or other forms of calcium carbonate on reactor surfaces, auxiliary equipment and the like; and the Group IA metal which remains within the liquefaction bottoms catalyzes the reaction when the liquefaction bottoms are subjected to a gasification reaction.

  17. Steam pretreatment for coal liquefaction. Sixth quarterly report, 1 January 1992--31 March 1992

    SciTech Connect

    Graff, R.A.; Balogh-Nair, V.

    1992-06-28

    Steam pretreatment is the reaction of coal with steam at temperatures well below those usually used for solubilization. The objective of the proposed work is to test the application of steam pretreatment to coal liquefaction. Conversion of the autoclave apparatus to rapid heating liquefaction was carried out this quarter following redesign of the coal slurry injection system. The modified equipment and procedure was tested in a simulated liquefaction run without coal. Initial tests of slurried {minus}20 mesh coal showed too rapid settling for successful operation. Coal ground to pass 200 mesh proved suitable, and a impact grinder was put into operation to grind the material under an inert atmosphere. A batch of Illinois No. 6 coal for the, first rapid heating liquefaction tests has been prepared and stored under inert gas. The steam pretreatment of {alpha}-benzylnaphthyl ether was carried out using stainless steel and glass lined reactors. A preparative scale procedure for product separation was developed. The major components were identified and the average product distribution determined for both types of reactors. Pretreatment of {alpha}-naphthylmethyl phenyl ether was also carried out using stainless steel and glass-lined reactors. Separation and analysis of the products has been started. The major components have been identified. Analyses and identification of the components will be continued next quarter.

  18. Coal liquefaction co-processing: Topical report No. 1

    SciTech Connect

    Luebke, C.P.; Nafis, D.A.; Humbach, M.J.; Gatsis, J.G.; Nelson, B.J.; Lea, C.L.

    1987-06-01

    This is the first topical report for the UOP Coal Liquefaction Co-processing Project. The UOP co-processing scheme is a single-stage slurry catalyzed process in which the petroleum vacuum resid and coal are simultaneously upgraded to a high quality synthetic oil. Hydrogen, finely ground coal, petroleum resid and catalyst are mixed, heated and then directed to a single-stage reactor where the simultaneous conversion of the resid and coal occurs. The reactor effluent is directed to a series of separators where a hydrogen-rich gas is recovered and recycled back to the reactor inlet. The balance of the material is sent to a series of separators where the light gases, light oil, vacuum gas oil (VGO), catalyst, unconverted coal, ash and residues are recovered. The catalyst is recycled back to the reactor. The UOP co-processing scheme is designed to be integrated with a conventional petroleum refinery. The hydrocarbon products from the co-processing unit will be sent to the refinery for final upgrading to finished products. 5 refs., 15 figs., 28 tabs.

  19. Exploratory Research on Novel Coal Liquefaction Concept - Task 2: Evaluation of Process Steps.

    SciTech Connect

    Brandes, S.D.; Winschel, R.A.

    1997-05-01

    A novel direct coal liquefaction technology is being investigated in a program being conducted by CONSOL Inc. with the University of Kentucky, Center for Applied Energy Research and LDP Associates under DOE Contract DE-AC22-95PC95050. The novel concept consists of a new approach to coal liquefaction chemistry which avoids some of the inherent limitations of current high-temperature thermal liquefaction processes. The chemistry employed is based on hydride ion donation to solubilize coal at temperatures (350-400{degrees}C) significantly lower than those typically used in conventional coal liquefaction. The process concept being explored consists of two reaction stages. In the first stage, the coal is solubilized by hydride ion donation. In the second, the products are catalytically upgraded to acceptable refinery feedstocks. The program explores not only the initial solubilization step, but integration of the subsequent processing steps, including an interstage solids-separation step, to produce distillate products. A unique feature of the process concept is that many of the individual reaction steps can be decoupled, because little recycle around the liquefaction system is expected. This allows for considerable latitude in the process design. Furthermore, this has allowed for each key element in the process to be explored independently in laboratory work conducted under Task 2 of the program.

  20. Progress in donor assisted coal liquefaction: Hydroaromatic compound formation

    SciTech Connect

    Kottenstette, R.J.; Stephens, H.P.

    1993-12-31

    The role of hydrogen donor compounds in coal liquefaction has been extensively investigated since the mid 1960`s using model compounds and process derived hydrogen donor solvents. Our recent research and that of other investigators have shown that two model compounds in particular have great efficacy in solvating low rank coals. 1,2,3,10b tetrahydrofluoranthene (H{sub 4}Fl) and 1,2,3,6,7,8 hexahydropyrene (H{sub 6}Py) have been used to dissolve Wyodak coal to > 95% soluble material as measured by tetrahydrofuran (THF). Although these hydrogen donors are very effective, they may not be found in any significant concentrations in actual liquefaction process recycle solvents. Therefore, studies with process derived recycle materials are necessary to understand donor solvent chemistry. The objective of this paper is to present results of solvent hydrogenation experiments using heavy distillate solvents produced during testing at the Wilsonville Advanced Coal Liquefaction Test Facility. We evaluated the impact of hydrogenation conditions upon hydrogen donor formation in process derived distillates and compared these process derived solvents with the highly effective H{sub 4}Fl and H{sub 6}Py donors in coal liquefaction tests. This paper presents data on reaction conditions used for distillate hydrotreating and subsequent coal liquefaction, with an aim toward understanding the relationship between reaction conditions and donor solvent quality in recycle distillates.

  1. Geological occurrence response to trace elemental migration in coal liquefaction based on SPSS: take no. 11 coalbed in Antaibao mine for example

    NASA Astrophysics Data System (ADS)

    Xia, Xiaohong; Qin, Yong; Yang, Weifeng

    2013-03-01

    Coal liquefaction is an adoptable method to transfer the solid fossil energy into liquid oil in large scale, but the dirty material in which will migrate to different step of liquefaction. The migration rule of some trace elements is response to the react activity of macerals in coal and the geological occurrence of the element nature of itself. In this paper, from the SPSS data correlation analysis and hierarchical clustering dendrogram about the trace elements with macerals respond to coal liquefaction yield, it shows the trace elements in No.11 Antaibao coal seam originated from some of lithophile and sulphophle elements. Correlation coefficient between liquefaction yield of three organic macerals and migration of the elements in liquefaction residue indicated that the lithophile are easy to transfer to residue, while sulphophle are apt to in the liquid products. The activated macerals are response to sulphophle trace elements. The conclusion is useful to the coal blending and environmental effects on coal direct liquefaction.

  2. Coal liquefaction: recent findings in occupational safety and health.

    PubMed

    Harris, L R; Gideon, J A; Berardinelli, S; Reed, L D; Dobbin, R D; Evans, J M; Telesca, D R; Tanita, R K

    1980-08-01

    Some coal liquefaction materials are potentially hazardous because of similarities to materials in other related coal processes that have been associated with a high cancer risk. Limited survey data obtained by NIOSH at two coal liquefaction pilot plants have shown that workers were exposed to low concentrations of certain polynuclear aromatic hydrocarbons (PNA's) and aromatic amines, some of which are suspected carcinogens. The degree of risk incurred by such exposures cannot be determined because toxicologic data allowing for the evaluation of effects at low exposure levels are unavailable. These industrial hygiene studies are discussed as well as recent health and process aspects of this technology.

  3. Novel use of residue from direct coal liquefaction process

    SciTech Connect

    Jianli Yang; Zhaixia Wang; Zhenyu Liu; Yuzhen Zhang

    2009-09-15

    Direct coal liquefaction residue (DCLR) is, commonly, designed to be used as a feed stock for gasification or combustion. Use of DCLR as a value added product is very important for improving overall economy of direct coal liquefaction processes. This study shows that the DCLR may be used as a pavement asphalt modifier. The modification ability is similar to that of Trinidad Lake Asphalt (TLA), a superior commercial modifier. Asphalts modified by two DCLRs meet the specifications of ASTM D5710 and BSI BS-3690 designated for the TLA-modified asphalts. The required addition amount for the DCLRs tested is less than that for TLA due possibly to the high content of asphaltene in DCLRs. Different compatibility was observed for the asphalts with the same penetration grade but from the different origin. Different components in the DCLR play different roles in the modification. Positive synergetic effects among the fractions were observed, which may due to the formation of the stable colloid structure. Unlike polymer-type modifier, the structure of asphalt-type modifier has a similarity with petroleum asphalts which favors the formation of a stable dispersed polar fluid (DPF) colloid structure and improves the performance of pavement asphalt. 12 refs., 1 fig., 6 tabs.

  4. STUDY OF SOLVENT AND CATALYST INTERACTIONS IN DIRECT COAL LIQUEFACTION

    SciTech Connect

    Michael T. Klein

    2000-01-01

    Using a reactor in which the coal is physically separated from the solid catalyst by a porous wall permeable to the hydrogen donor solvent, it was shown that direct contact between the catalyst and the coal is not required for catalyzed coal liquefaction. This occurs however only when there is a hydrogen atmosphere, as liquefaction with catalyst participation does not occur in a nitrogen atmosphere. Liquefaction by hydrogen transfer from the donor solvent itself does occur. This suggests that there is transfer of hydrogen from the catalyst to the coal via the solvent. The character of the solvent makes a significant difference, the better solvents being good hydrogen donors. These results indicate that the role of the catalyst may be to regenerate the spent hydrogen donor solvent during the liquefaction process. The peak temperature for volatiles evolution has been shown to be a reproducible measure of the coal rank. This was shown by an excellent correlation (R2 = 0.998) between peak volatiles temperatures (by TGA) and vitrinite reflectance. Using TG/MS, the volatiles contents of coals of a wide range of ranks was determined. The low rank coals emit largely phenols and some other oxygen compounds and olefins. The higher rank coals emit largely aromatic hydrocarbons and some olefins.

  5. Recent progress in the direct liquefaction of coal.

    PubMed

    Lumpkin, R E

    1988-02-19

    Interest in direct coal liquefaction steadily decreased during the 1980s as the price of crude oil dropped; there is now only one integrated coal liquefaction pilot plant active full time in the United States. The economics derived early in the decade established the price of transportation fuels from coal at $80 per barrel or higher. However, there have been dramatic improvements in the technology since 1983 that have not been widely appreciated. Recent designs and cost estimates show that a 60 percent decrease in the cost of liquid fuels from coal to an equivalent of $35 per barrel for crude oil. Although this cost is not low enough to justify immediate commercialization, additional improvements have been identified that could make direct liquefaction an attractive way to produce gasoline and other conventional fuels.

  6. Novel bimetallic dispersed catalysts for temperature-programmed coal liquefaction

    SciTech Connect

    Song, Chunshan; Schobert, H.H.

    1993-02-01

    Development of new catalysts is a promising approach to more efficient coal liquefaction. It has been recognized that catalysts are superior to supported catalysts for primary liquefaction of coals, because the control of initial coal dissolution or depolymerization requires intimate contact between the catalyst and coal. This research is a fundamental and exploratory study on catalytic coal liquefaction, with the emphasis on the development of novel bimetallic dispersed catalysts for temperature-programmed liquefaction. The ultimate goal of the present research is to develop novel catalytic hydroliquefaction process using highly active dispersed catalysts. The primary objective of this research is to develop novel bimetallic dispersed catalysts from organometallic molecular that can be used in low precursors concentrations (< 1 %) but exhibit high activity for efficient hydroliquefaction of coals under temperature-programmed conditions. The major technical approaches are, first, to prepare the desired heteronuclear organometallic molecules as catalyst precursors that contain covalently bound, two different metal atoms and sulfur in a single molecule. Such precursors will generate finely dispersed bimetallic catalysts such as Fe-Mo, Co-Mo and Ni-Mo binary sulfides upon thermal decomposition. The second major technical approach is to perform the liquefaction of coals unpregnated with the organometallic precursors under temperature-programmed conditions, where the programmed heat-up serves as a step for both catalyst activation and coal pretreatment or preconversion. Two to three different complexes for each of the Fe-Mo, Co-Mo, and Ni-Mo combinations will be prepared. Initial catalyst screening tests will be conducted using a subbituminous coal and a bituminous coal. Effects of coal rank and solvents will be examined with the selected bimetallic catalysts which showed much higher activity than the dispersed catalysts from conventional precursors.

  7. Coal liquefaction process utilizing coal/CO.sub.2 slurry feedstream

    DOEpatents

    Comolli, Alfred G.; McLean, Joseph B.

    1989-01-01

    A coal hydrogenation and liquefaction process in which particulate coal feed is pressurized to an intermediate pressure of at least 500 psig and slurried with CO.sub.2 liquid to provide a flowable coal/CO.sub.2 slurry feedstream, which is further pressurized to at least 1000 psig and fed into a catalytic reactor. The coal particle size is 50-375 mesh (U.S. Sieve Series) and provides 50-80 W % coal in the coal/CO.sub.2 slurry feedstream. Catalytic reaction conditions are maintained at 650.degree.-850.degree. F. temperature, 1000-4000 psig hydrogen partial pressure and coal feed rate of 10-100 lb coal/hr ft.sup.3 reactor volume to produce hydrocarbon gas and liquid products. The hydrogen and CO.sub.2 are recovered from the reactor effluent gaseous fraction, hydrogen is recycled to the catalytic reactor, and CO.sub.2 is liquefied and recycled to the coal slurrying step. If desired, two catalytic reaction stages close coupled together in series relation can be used. The process advantageously minimizes the recycle and processing of excess hydrocarbon liquid previously needed for slurrying the coal feed to the reactor(s).

  8. Upgrading of coal liquefaction feedstock by selective agglomeration

    SciTech Connect

    Lai, R.; Sinha, K.; Richardson, A.; Killmeyer, R.; Utz, B.; Hickey, R.; Cillo, D.

    1994-03-01

    The technical feasibility study of using selective agglomeration (with coal-derived oil) to upgrade Illinois No. 6 coal for a liquefaction feedstock was completed. Effects of coal particle size, slurry pH, oil-to-coal ratio, and operating temperature on mineral matter reduction, clean coal weight recovery, and clean coal moisture content were studied. The addition of coal-derived naphtha or kerosene as conditioners to increase hydrophobicity and recovery of coal was also investigated. Results showed that approximately 70% of the mineral matter could be removed from this coal at a clean coal weight recovery of over 85% by grinding the coal to a mean volume diameter of about 10 microns and properly selecting of the operation variables.

  9. STUDY OF SOLVENT AND CATALYST INTERACTIONS IN DIRECT COAL LIQUEFACTION

    SciTech Connect

    Michael T. Klein

    1998-10-01

    Major objectives of the present project are to develop a better understanding of the roles of the catalyst and the liquefaction solvent in the coal liquefaction process. An open question concerning the role of the catalyst is whether intimate contact between the catalyst and the coal particles is important or required. To answer this question, it had been planned to coat an active catalyst with a porous silica coating which was found to retain catalyst activity while preventing actual contact between catalyst and coal. Consultation with people in DuPont who coat catalysts for increasing abrasion resistance have indicated that only portions of the catalyst are coated by their process (spray drying) and that sections of uncoated catalyst remain. For that reason, it was decided to suspend the catalyst in a basket separated from the coal in the reactor. The basket walls were to be permeable to the liquefaction solvent but not to the coal particles. Several such baskets were constructed of stainless steel with holes which would not permit passage of coal particles larger than 30 mesh. Liquefactions run with the coal of greater than 30 mesh size gave normal conversion of coal to liquid in the absence of catalyst in the basket, but substantially increased conversion when Ni/Mo on alumina catalyst was in the basket. While this result is interesting and suggestive of some kind of mass transfer of soluble material occurring between the catalyst and the coal, it does not eliminate the possibility of breakdown of the coal particle into particle sizes permeable to the basket. Indeed, a small amount of fine coal has been found inside the basket. To determine whether fine coal from breakdown of the coal particles is responsible for the conversion, a new basket is being prepared with 0.5{micro}m pore size.

  10. Solvent treatment of coal for improved liquefaction

    DOEpatents

    Appell, Herbert R.; Narain, Nand K.; Utz, Bruce R.

    1986-05-06

    Increased liquefaction yield is obtained by pretreating a slurry of solid carbonaceous material and a liquid hydrocarbonaceous solvent at a temperature above 200.degree. C. but below 350.degree. C. for a period of 10 minutes to four hours prior to exposure to liquefaction temperatures.

  11. Advanced coal-liquefaction research. Technical progress report, August 1, 1982-December 31, 1982

    SciTech Connect

    Not Available

    1983-07-01

    This report describes progress on the Advanced Coal-Liquefaction Project by the Gulf Research and Development Company's Merriam Laboratory. It was demonstrated that all oil products from the SRC II Processing of Powhatan No. 3 (Pittsburgh seam), Elkol-Sorensen or Belle Ayr coals boiling above 270/sup 0/C (518/sup 0/F) can be recycled to extinction. There was no loss in liquid yield, no increase in gas make and no significant change in hydrogen requirement. It has also been demonstrated that the net C/sub 5/-270/sup 0/C (518/sup 0/F) product is inactive in the Ames test and presumably poses substantially less threat than the conventional product as a potential carcinogen. The potential impact of coal cleaning and pyrite addition on liquefaction were determined with a high-reactivity Pittsburgh seam coal from the Ireland Mine. The results indicate that deep cleaning (to 6-8 wt % ash) by heavy media separation with add back of pyrite would give a better yield structure than the normal cleaning (to 12 wt % ash) envisioned for liquefaction plants. Screening of feedstocks for liquefaction processes was extended to the low-ash (5 wt % MF basis), subbituminous Elkol-Sorensen coal. Although the low ash content allowed increased recycle of bottoms product, the relatively low reactivity of the organic matrix resulted in a lower oil yield than with subbituminous Belle Ayr coal. A simulation of staged liquefaction was carried out by preparing filtrate in the SRC I mode and then studying the production of gas and distillate at lower temperature (420/sup 0/C, 788/sup 0/F) using a molybdenum emulsion catalyst. Distillate yields were low (29 wt %, based on MF coal) compared to single-stage, high temperature runs. Multiple-pass operations indicated no mechanistic barriers to high distillate yields although reaction rates were unacceptably low at the conditions employed in these preliminary experiments.

  12. Catalyst system and process for benzyl ether fragmentation and coal liquefaction

    DOEpatents

    Zoeller, Joseph Robert

    1998-04-28

    Dibenzyl ether can be readily cleaved to form primarily benzaldehyde and toluene as products, along with minor amounts of bibenzyl and benzyl benzoate, in the presence of a catalyst system comprising a Group 6 metal, preferably molybdenum, a salt, and an organic halide. Although useful synthetically for the cleavage of benzyl ethers, this cleavage also represents a key model reaction for the liquefaction of coal; thus this catalyst system and process should be useful in coal liquefaction with the advantage of operating at significantly lower temperatures and pressures.

  13. Low Severity Coal Liquefaction Promoted by Cyclic Olefins

    SciTech Connect

    Christine W. Curtis

    1998-04-09

    The development of the donor solvent technology for coal liquefaction has drawn a good deal of attention over the last three decades. The search for better hydrogen donors led investigators to a class of compounds known as cyclic olefins. Cyclic olefins are analogues of the conventional hydroaromatic donor species but do not contain aromatic rings. The cyclic olefins are highly reactive compounds which readily release their hydrogen at temperatures of 200 C or higher. Considerable effort has been o expended toward understanding the process of hydrogen donation. Most of this work was conducted in bomb reactors, with product analysis being carried out after the reaction was complete. Efforts directed towards fundamental studies of these reactions in situ are rare. The current work employs a high temperature and high pressure infrared cell to monitor in situ the concentrations of reactants and products during hydrogen release from hydrogen donor compounds.

  14. The Wilsonville Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama

    SciTech Connect

    Not Available

    1990-05-01

    The investigation of various Two-Stage Liquefaction (TSL) process configurations was conducted at the Wilsonville Advanced Coal Liquefaction R D Facility between July 1982 and September 1986. The facility combines three process units. There are the liquefaction unit, either thermal (TLU) or catalytic, for the dissolution of coal, the Critical Solvent Deashing unit (CSD) for the separation of ash and undissolved coal, and a catalytic hydrogenation unit (HTR) for product upgrading and recycle process solvent replenishment. The various TSL process configurations were created by changing the process sequence of these three units and by recycling hydrotreated solvents between the units. This report presents a description of the TSL configurations investigated and an analysis of the operating and performance data from the period of study. Illinois No. 6 Burning Star Mine coal Wyodak Clovis Point Mine coal were processed. Cobalt-molybdenum and disposable iron-oxide catalysts were used to improve coal liquefaction reactions and nickel-molybdenum catalysts were used in the hydrotreater. 28 refs., 31 figs., 13 tabs.

  15. Fine particle clay catalysts for coal liquefaction. Quarterly technical report, May 9, 1991--August 8, 1991

    SciTech Connect

    Olson, E.S.

    1991-12-31

    The efficient production of environmentally acceptable distillate fuels requires catalysts for hydrogenation and cleavage of the coal macromolecules and removal of oxygen, nitrogen, and sulfur heteroatoms. The goal of the proposed research is to develop new catalysts for the direct liquefaction of coal. This type of catalyst consists of fine clay particles that have been treated with reagents which form pillaring structures between the aluminosilicate layers of the clay. The pillars not only hold the layers apart but also constitute the active catalytic sites for hydrogenation of the coal and the solvent used in the liquefaction. The pillaring catalytic sites are composed of pyrrhotite, which has been previously demonstrated to be active for coal liquefaction. The pyrrhotite sites are generated in situ by sulfiding the corresponding oxyiron species. The size of the catalyst will be less than 40 nm in order to promote intimate contact with the coal material. Since the clays and reagents for pillaring and activating the clays are inexpensive, the catalysts can be discarded after use, rather than regenerated by a costly process. The proposed work will evaluate methods for preparing the fine particle iron-pillared clay dispersions and for activating the particles to generate the catalysts. Characterization studies of the pillared clays and activated catalysts will be performed. The effectiveness of the pillared clay dispersion for hydrogenation and coal liquefaction will be determined in several types of testing.

  16. Coal liquefaction and hydrogenation: Processes and equipment. (Latest citations from the US Patent database). Published Search

    SciTech Connect

    Not Available

    1993-07-01

    The bibliography contains citations of selected patents concerning methods, processes, and apparatus for coal liquefaction and hydrogenation. Included are patents for catalytic two-stage, catalytic single-step, fixed-bed, hydrogen-donor, internal heat transfer, and multi-phase processes. Topics also include catalyst production, catalyst recovery, desulfurization, pretreatment of coals, energy recovery processes, solvent product separation, hydrogenating gases, and pollution control. (Contains 250 citations and includes a subject term index and title list.)

  17. Coal liquefaction process streams characterization and evaluation. Volume 2, Participants program final summary evaluation

    SciTech Connect

    Brandes, S.D.; Robbins, G.A.; Winschel, R.A.; Burke, F.P.

    1994-05-01

    This 4.5-year project consisted of routine analytical support to DOE`s direct liquefaction process development effort (the Base Program), and an extensive effort to develop, demonstate, and apply new analytical methods for the characterization of liquefaction process streams (the Participants Program). The objective of the Base Program was to support the on-going DOE direct coal liquefaction process development program. Feed, process, and product samples were used to assess process operations, product quality, and the effects of process variables, and to direct future testing. The primary objective of the Participants Program was to identify and demonstrate analytical methods for use in support of liquefaction process develpment, and in so doing, provide a bridge between process design, development, and operation and analytical chemistry. To achieve this direct coal liquefaction-derived materials. CONSOL made an evaluation of each analytical technique. During the performance of this project, we obtained analyses on samples from numerous process development and research programs and we evaluated a variety of analytical techniques for their usefulness in supporting liquefaction process development. Because of the diverse nature of this program, we provide here an annotated bibliography of the technical reports, publications, and formal presentations that resulted from this program to serve as a comprehensive summary of contract activities.

  18. SURFACE-MODIFIED COALS FOR ENHANCED CATALYST DISPERSION AND LIQUEFACTION

    SciTech Connect

    Dr. Yaw D. Yeboah

    1999-09-01

    This is the final report of the Department of Energy Sponsored project DE-FGF22-95PC95229 entitled, surface modified coals for enhanced catalyst dispersion and liquefaction. The aims of the study were to enhance catalyst loading and dispersion in coal for improved liquefaction by preadsorption of surfactants and catalysts on the coal and to train and educate minority scientists in catalysts and separation science. Illinois No. 6 Coal (DEC-24) was selected for the study. The surfactants investigated included dodecyl dimethyl ethyl ammonium bromide (DDAB), a cationic surfactant, sodium dodecyl sulfate, an anionic surfactant, and Triton x-100, a neutral surfactant. Ammonium molybdate tetrahydrate was used as the molybdenum catalyst precursor. Zeta potential, BET, FTIR, AFM, UV-Vis and luminescence intensity measurements were undertaken to assess the surface properties and the liquefaction activities of the coal. The parent coal had a net negative surface charge over the pH range 2-12. However, in the presence of DDAB the negativity of the surface charge decreased. At higher concentrations of DDAB, a positive surface charge resulted. In contrast to the effect of DDAB, the zeta potential of the coal became more negative than the parent coal in the presence of SDS. Adsorption of Triton reduced the net negative charge density of the coal samples. The measured surface area of the coal surface was about 30 m{sup 2}/g compared to 77m{sup 2}/g after being washed with deionized water. Addition of the surfactants decreased the surface area of the samples. Adsorption of the molybdenum catalyst increased the surface area of the coal sample. The adsorption of molybdenum on the coal was significantly promoted by preadsorption of DDAB and SDS. Molybdenum adsorption showed that, over a wide range of concentrations and pH values, the DDAB treated coal adsorbed a higher amount of molybdenum than the samples treated with SDS. The infrared spectroscopy (FTIR) and the atomic force

  19. Cooperative research in coal liquefaction. Final report, May 1, 1990-- April 30, 1991

    SciTech Connect

    Huffman, G.P.

    1992-02-15

    The Consortium for Fossil Fuel Liquefaction Science (CFFLS) is currently engaged in a three year contract with the US Department of Energy investigating a range of research topics dealing with direct coal liquefaction. This report summarizes the results of this program in its second year, from May 1, 1990 to April 30, 1991. Accomplishments for this period are presented for the following tasks: Iron-based catalysts for coal liquefaction, exploratory research on coal conversion, novel coal liquefaction concepts, and novel catalysts for coal liquefaction.

  20. Solvent tailoring in coal liquefaction. Quarterly report, April-June 1984

    SciTech Connect

    Tarrer, A.R.; Curtis, C.W.; Guin, J.A.; Williams, D.C.

    1984-07-01

    Although the numerous functions of the solvent during liquefaction are not completely understood, the provision for (and the maintenance of) an effective process solvent is necessary for effective coal liquefaction. In this project, the function of the process solvent regarding vapor-liquid equilibrium, hydrogen donation, and catalyst activity has been explored. In previously reported work, a number of donor compounds were evaluated for their relative efficiency in converting coal to cresol solubles. Attempts to correlate the relative efficiency of the various donor compounds were made on the basis of thermodynamic stability and structural features of the molecules. Currently, work is underway with selected donor compounds to determine if the chemical nature of the compound influences the product distribution obtained during coal liquefaction as well as affecting the amount of conversion obtained. The product distribution, which is being used to evaluate the liquefaction products, is based upon extraction of the products into different solvents. The products are divided into oil, pentane soluble material; asphaltenes, pentane insoluble, benzene soluble material; preasphaltenes, benzene insoluble, methylene chloride/methanol soluble material; and insoluble organic matter, methylene chloride/methanol insoluble material. The effectiveness of the hydrogen donor solvent will be measured by the amount of higher quality material (oil and asphaltenes) obtained as well as by the amount of coal converted.

  1. Advanced liquefaction using coal swelling and catalyst dispersion techniques. Quarterly technical progress report No. 7, April 1993--June 1993

    SciTech Connect

    Curtis, C.W.; Chander, S.; Gutterman, C.

    1994-09-01

    The overall objective of this project is to develop a new approach for the direct liquefaction of coal to produce an all-distillate product slate at a sizable cost reduction over current technology. The approach integrates coal selection, pretreatment, coal swelling with catalyst impregnation, liquefaction, product recovery with characterization, alternate bottoms processing, and carrying out a technical assessment including an economic evaluation. The project is being carried out under contract to the United States Department of Energy. All three coals used in this study (Black Thunder, Burning Star bituminous, and Martin Lake lignite) are effectively swelled by a number of solvents. The most effective solvents are those having hetero-functionality. In addition, a synergistic effect has been demonstrated, in which solvent blends are more effective for coal swelling than the pure solvents alone. Therefore, it will be necessary to use only low levels of swelling agents and yet promote the impregnation of catalyst precursors. The rate of the impregnation of catalyst precursors into swollen coal increases greatly as the effectiveness of the solvent to swell the coal increases. This effect is also demonstrated by improved catalyst precursor impregnation with increased contact temperature. Laboratory- and bench-scale liquefaction experimentation is underway using swelled and catalyst impregnated coal samples. Higher coal conversions were observed for the SO{sub 2}-treated coal than the raw coal, regardless of catalyst type. Conversions of swelled coal were highest when Molyvan-L, molybdenum naphthenate, and nickel octoate, respectively, were added to the liquefaction solvent.

  2. Subacute inhalation toxicity of a medium-boiling coal liquefaction product (154-378 degrees C) in the rat [Part III].

    PubMed

    Chu, I; Rinehart, W; Hoffman, G; Villeneuve, D C; Otson, R; Valli, V E

    1989-01-01

    The short-term inhalation toxicity of a medium-boiling coal liquefaction product (CLP) was investigated in the rat. Groups of 5 male and 5 female Sprague-Dawley rats were exposed to CLP aerosols at 25 mg/m3 (low dose) or 100 mg/m3 (high dose) 6 h/d, 5 d/w, for 4 wk. The control group was exposed to filtered air while the positive control received diesel fuel aerosols at 100 mg/m3. Male rats exposed to high-dose CLP aerosols exhibited growth depression and increased hepatic aminopyrine demethylase activity compared to control animals. High-dose females had decreased hemoglobin content and hematocrit values. These biochemical and hematological effects were not observed in animals of either sex treated with the diesel fuel. No other biochemical and hematological changes were observed. Mild histological changes occurred in the liver and thyroid of rats treated with CLP and diesel fuel aerosols. Based on the data presented, inhalation of CLP aerosols resulted in toxicological effects that were similar to those caused by dermal exposure.

  3. Controlled short residence time coal liquefaction process

    DOEpatents

    Anderson, Raymond P.; Schmalzer, David K.; Wright, Charles H.

    1982-05-04

    Normally solid dissolved coal product and a distillate liquid product are produced by continuously passing a feed slurry comprising raw feed coal and a recycle solvent oil and/or slurry together with hydrogen to a preheating-reaction zone (26, alone, or 26 together with 42), the hydrogen pressure in the preheating-reaction zone being at least 1500 psig (105 kg/cm.sup.2), reacting the slurry in the preheating-reaction zone (26, or 26 with 42) at a temperature in the range of between about 455.degree. and about 500.degree. C. to dissolve the coal to form normally liquid coal and normally solid dissolved coal. A total slurry residence time is maintained in the reaction zone ranging from a finite value from about 0 to about 0.2 hour, and reaction effluent is continuously and directly contacted with a quenching fluid (40, 68) to substantially immediately reduce the temperature of the reaction effluent to below 425.degree. C. to substantially inhibit polymerization so that the yield of insoluble organic matter comprises less than 9 weight percent of said feed coal on a moisture-free basis. The reaction is performed under conditions of temperature, hydrogen pressure and residence time such that the quantity of distillate liquid boiling within the range C.sub.5 -455.degree. C. is an amount at least equal to that obtainable by performing the process under the same conditions except for a longer total slurry residence time, e.g., 0.3 hour. Solvent boiling range liquid is separated from the reaction effluent and recycled as process solvent.

  4. Formation of disperse-slurry of coal liquefaction residue

    SciTech Connect

    Corbeels, R.J.; Vasconcellos, S.R.

    1986-03-11

    This patent describes a process for forming a disperse-slurry in aqueous medium of comminuted particles of a hydrophobic coal liquefaction residue containing phenolic components which are conducive to creaming. This process consists of: contacting the hydrophobic H-coal residue, containing phenolic components which are conducive to creaming, with 0.001-0.1 parts per 100 parts of aqueous medium of a cationic surfactant R/sup 1/R/sup 2/R/sup 3/R/sup 4/N+X- wherein R/sup 1/ is a C/sub 12/-C/sub 20/ hydrocarbon group; each of R/sup 2/, R/sup 3/ and R/sup 4/ is a C/sub 1/-C/sub 6/ lower hydrocarbon group or a poly(oxyalkylene) group having 12-25 repeating units; and X is an inert anion whereby the surfactant is adsorbed onto the particles; and comminuting, in the presence of aqueous medium, the hydrophobic coal liquefaction residue, containing phenolic components which are conducive to creaming, in the presence of the surfactant thereby forming a slurry of comminuted hydrophobic coal liquefaction residue in aqueous medium characterized by decreased creaming decreased wall adhesion, and reduced phase separation; and recovering the slurry of comminuted hydrophobic coal liquefaction residue in aqueous medium characterized by decreased creaming, enhanced dispersability, decreased wall adhesion, and reduced phase separation.

  5. Low-rank coal research: Volume 1, Control technology, liquefaction, and gasification: Final report

    SciTech Connect

    Weber, G.F.; Collings, M.E.; Schelkoph, G.L.; Steadman, E.N.; Moretti, C.J.; Henke, K.R.; Rindt, J.R.; Hetland, M.D.; Knudson, C.L.; Willson, W.G.

    1987-04-01

    Volume I contains articles on SO/sub x//NO/sub x/ control, waste management, low-rank direct liquefaction, hydrogen production from low-rank coals, and advanced wastewater treatment. These articles have been entered individually into EDB and ERA. (LTN)

  6. Coal liquefaction process streams characterization and evaluation. Novel analytical techniques for coal liquefaction: Fluorescence microscopy

    SciTech Connect

    Rathbone, R.F.; Hower, J.C.; Derbyshire, F.J.

    1991-10-01

    This study demonstrated the feasibility of using fluorescence and reflectance microscopy techniques for the examination of distillation resid materials derived from direct coal liquefaction. Resid, as defined here, is the 850{degrees}F{sup +} portion of the process stream, and includes soluble organics, insoluble organics and ash. The technique can be used to determine the degree of hydrogenation and the presence of multiple phases occurring within a resid sample. It can also be used to infer resid reactivity. The technique is rapid, requiring less than one hour for sample preparation and examination, and thus has apparent usefulness for process monitoring. Additionally, the technique can distinguish differences in samples produced under various process conditions. It can, therefore, be considered a potentially useful technique for the process developer. Further development and application of this analytical method as a process development tool is justified based on these results.

  7. Low severity coal liquefaction promoted by cyclic olefins. Quarterly report, October 1991--December 1991

    SciTech Connect

    Curtis, C.W.

    1991-12-31

    The objective of this project is to evaluate the efficacy of low severity coal liquefaction in the presence of highly reactive hydrogen donors, cyclic olefins. The work that was performed this quarter involved performing a literature search in which different aspects of low severity coal liquefaction were examined. In addition, two new mater`s graduate students learned the fundamental differences between high severity coal liquefaction and low severity coal liquefaction by examining the literature and reading texts on coal liquefaction. The literature review presented for the first quarter`s work is a compilation of the material which we have found to data involving low severity coal liquefaction. Additional review of low severity liquefaction literature is being conducted this quarter and will be reported in the next quarterly report. In addition, a summary of the work involving the reactivity of cyclic olefins in the absence and presence of coal will be presented next quarter.

  8. Cooperative research in coal liquefaction. Technical progress report, May 1, 1993--April 30, 1994

    SciTech Connect

    Huffman, G.P.

    1994-10-01

    Accomplishments for the past year are presented for the following tasks: coliquefaction of coal with waste materials; catalysts for coal liquefaction to clean transportation fuels; fundamental research in coal liquefaction; and in situ analytical techniques for coal liquefaction and coal liquefaction catalysts some of the highlights are: very promising results have been obtained from the liquefaction of plastics, rubber tires, paper and other wastes, and the coliquefaction of wastes with coal; a number of water soluble coal liquefaction catalysts, iron, cobalt, nickel and molybdenum, have been comparatively tested; mossbauer spectroscopy, XAFS spectroscopy, TEM and XPS have been used to characterize a variety of catalysts and other samples from numerous consortium and DOE liquefaction projects and in situ ESR measurements of the free radical density have been conducted at temperatures from 100 to 600{degrees}C and H{sub 2} pressures up to 600 psi.

  9. Short Contact Time Direct Coal Liquefaction Using a Novel Batch Reactor

    SciTech Connect

    He Huang; Michael T. Klein; William H. Calkins

    1997-01-30

    The primary objective of this research is to optimize the design and operation of the bench scale batch reactor (SCTBR) for studying direct coal liquefaction at short contact times (.01 to 10 minutes or longer). Additional objectives are to study the kinetics of direct coal liquefaction particularly at short reaction times and to investigate the role of organic oxygen components of coal and their reaction pathways during coal liquefaction. Many of those objectives have already been achieved. This quarterly report discusses further kinetic studies of the liquefaction in tetralin of a Montana Lignite, Wyodak-Anderson subbituminous coal, Illinois #6 hv bituminous coal, Pittsburgh #8 hv bituminous coals, and Pocohontas lV bituminous coal at short contact times. All of these coals showed a distinct extraction stage. Further work has also been done to attempt to clarify the role of the liquefaction solvent in the direct liquefaction process.

  10. Preparation and modifications of recoverable particle catalysts for coal liquefaction

    SciTech Connect

    Mochida, Isao; Sakanishi, Kinya; Taniguchi, Hideki; Hasuo, Haru-umi

    1995-12-31

    Highly active catalyst of higher activity is still a key to design the more efficient coal liquefaction process, which will increase the oil yield, minimize its cost, and environmental impact due to catalyst disposal. The authors assumed that the recovery and recycle of the catalyst from the residue are an approach to improve the economy of coal liquefaction and to reduce the solid waste. The organic residue has been recycled with the catalyst and minerals to the primary liquefaction stage as the bottom recycle. Its favorable results have been reported, although the accumulation of the inorganic solid requires a fixed rate of purging the catalyst as well as minerals. The authors have examined Fe{sub 3}Al, strong ferromagnetic particles, as one of the potentially recoverable catalysts, in order to prepare an active catalyst with the recovery function through magnetic separation.

  11. The dual role of oxygen functions in coal pretreatment and liquefaction: Crosslinking and cleavage reactions. First annual report, April 1, 1991--March 31, 1992

    SciTech Connect

    Serio, M.A.; Kroo, E.; Teng, H.; Charpenay, S.; Solomon, P.R.

    1992-08-01

    The overall objective of this project is elucidate and model the dual role of oxygen functions in thermal pretreatment and liquefaction of low rank coals through the application of analytical techniques and theoretical models. The project will be an integrated study of model polymers representative of coal structures, raw coals of primarily low rank, and selectivity modified coals in order to provide specific information relevant to the reactions of real coals. The investigations will include liquefaction experiments in microautoclave reactors along with extensive analysis of intermediate solid, liquid and gaseous products. Attempts will be made to incorporate the results of experiments on the different systems into a liquefaction model.

  12. Steam pretreatment for coal liquefaction. Final report, September 26, 1990--March 18, 1995

    SciTech Connect

    Graff, R.A.; Balogh-Nair, V.; Ivanenko, O.; Brathwaite, C.

    1995-10-16

    The objective of this study is to demonstrate the use of subcritical steam to pretreat coal for slurry liquefaction, allowing liquefaction to be carried out at lower severity and improving product yield and quality. Samples of Illinois No. 6 coal were pretreated in 750 psia steam at 340{degree}C for 15 minutes. These samples, as well as raw coal, were liquefied at high (400{degree}C, 30 min.) and low (385{degree}C, 15 min.) severity conditions under 1500 psia hydrogen with tetralin as the donor solvent. Improved yields were obtained at both conditions. (Improved yields were not obtained at a liquefaction temperature of 350{degree}C as that put the sample into the region of retrogressive reactions). The deleterious effects of slow heating and exposure of the sample to air were demonstrated. Under low severity conditions, steam pretreatment more that doubled the oil yield, increasing it from 12.5 to 29 wt %. Tests were also conducted with aromatic ethers as model compounds. These were exposed to inert gas and steam at pretreatment conditions and in some cases to liquid water at 315{degree}C. {alpha}-Benzylnaphthyl ether and {alpha}- naphthylmethyl phenyl ether show little difference in conversion and product distribution when the thermolysis atmosphere is changed from inert gas to steam. However when these compounds were reacted in the presence of 5 {angstrom} zeolite, the yields of the thermolysis products improved. Zeolite proved effective in suppressing isomerization of the starting materials. These results suggested that zeolites might be beneficial in steam pretreatment of coal and in coal liquefaction. Pretreatment and liquefaction of mixtures of coal and zeolites increases yields of asphaltenes and preasphaltenes.

  13. Novel bimetallic dispersed catalysts for temperature-programmed coal liquefaction. Technical progress report, April--June 1995

    SciTech Connect

    Kirby, S.; Song, Chunshan; Schobert, H.H.

    1995-09-01

    Coal liquefaction involves cleavage of methylene, dimethylene and ether bridges connecting polycyclic aromatic units and the reactions of various oxygen functional groups. Here in this quarterly, we report on our continued effort on hydrodeoxygenation of O-containing polycyclic model compounds using novel organometallic catalyst precursors. Compounds containing oxygen functional groups, especially phenols, are undesirable components of coal-derived liquids. Removal of these compounds from the products of coal liquefaction is required. A beneficial alternative would be the removal of these compounds, or the prevention of their formation, during the liquefaction reaction itself, rather than as a separate processing step. A novel organometallic catalyst precursor containing Co and Mo has been studied as a potential hydrogenation catalyst for coal liquefaction. To ascertain the hydrodeoxygenation activity of this catalyst under liquefaction conditions, model compounds were investigated. Anthrone, 2,6-di-t-butyl-4-methyl-phenol, dinaphthyl ether, and xanthene were reacted in the presence of the Co-Mo catalyst precursor and a precursor containing only Mo over a range of temperatures, providing a comparison of conversions to deoxygenated products. These conversions give an indication of the hydrodeoxygenating abilities of organometallic catalyst precursors within a coal liquefaction system. For example, at 400{degrees}C dinaphthylether was converted 100% (4.5% O-containing products) in the presence of the Co-Mo organometallic precursor, compared to 76.5% conversion (7.4% O-products) in the presence of the Mo catalyst.

  14. Fine particle clay catalysts for coal liquefaction. Final technical report

    SciTech Connect

    Olson, E.S.

    1995-08-01

    In an effort to develop new disposable catalysts for direct coal liquefaction, several types of clay-supported pyrrhotite catalysts were prepared and tested. These included iron-pillared montmorillonite, mixed iron/alumina-pillared montmorillonite, iron-impregnated montmorillonite, and iron oxometallate-impregnated montmorillonite.

  15. Direct liquefaction of plastics and coprocessing of coal with plastics

    SciTech Connect

    Huffman, G.P.; Feng, Z.; Mahajan, V.

    1995-12-31

    The objectives of this work were to optimize reaction conditions for the direct liquefaction of waste plastics and the coprocessing of coal with waste plastics. In previous work, the direct liquefaction of medium and high density polyethylene (PE), polypropylene (PPE), poly(ethylene terephthalate) (PET), and a mixed plastic waste, and the coliquefaction of these plastics with coals of three different ranks was studied. The results established that a solid acid catalyst (HZSM-5 zeolite) was highly active for the liquefaction of the plastics alone, typically giving oil yields of 80-95% and total conversions of 90-100% at temperatures of 430-450 {degrees}C. In the coliquefaction experiments, 50:50 mixtures of plastic and coal were used with a tetralin solvent (tetralin:solid = 3:2). Using approximately 1% of the HZSM-5 catalyst and a nanoscale iron catalyst, oil yields of 50-70% and total conversion of 80-90% were typical. In the current year, further investigations were conducted of the liquefaction of PE, PPE, and a commingled waste plastic obtained from the American Plastics Council (APC), and the coprocessing of PE, PPE and the APC plastic with Black Thunder subbituminous coal. Several different catalysts were used in these studies.

  16. Organic contaminants in direct coal liquefaction--a preliminary assessment.

    PubMed

    Tanita, R; Telesca, D; Walker, J; Berardinelli, S

    1980-11-01

    Area samples taken at two coal liquefaction facilities were analyzed by either gas chromatography or gas chromatography/mass spectrometry to identify the types of organic contaminants to which workers may be exposed. Results indicate that the contaminants consisted primarily of one or two ring low-molecular weight aromatic compounds.

  17. The acute toxicity of coal liquefaction-derived materials.

    PubMed

    McKee, R H; Biles, R W; Kapp, R W; Hinz, J P

    1984-08-01

    The acute toxicity of a series of potential streams from the EDS coal liquefaction process have been assessed in animal bioassays. In general, the materials present minimal acute toxic hazards. However, there was some evidence of ocular and dermal irritation. These results indicate that eye and dermal contact should be minimized, particularly when the process streams contain high concentrations of phenolic materials.

  18. Evaluation of coal liquefaction technologies by Salmonella mutagenesis.

    PubMed

    Warshawsky, D; Schoeny, R; Moore, G

    1982-02-01

    Coal liquefaction materials made by two processes were found to be mutagenic in the Salmonella/microsome assay. Data from this type of in vitro assay can be used in the toxicological assessment of these processes. Such evaluations of the health and environmental impacts of technologies would aid in the development of alternate energy sources.

  19. SLURRY PHASE IRON CATALYSTS FOR INDIRECT COAL LIQUEFACTION

    SciTech Connect

    Abhaya K. Datye

    1998-11-19

    This report describes research conducted to support the DOE program in indirect coal liquefaction. Specifically, they have studied the attrition behavior of iron Fischer-Tropsch catalysts, their interaction with the silica binder and the evolution of iron phases in a synthesis gas conversion process. The results provide significant insight into factors that should be considered in the design of catalysts for converting coal based syngas into liquid fuels.

  20. Control of pyrite addition in coal liquefaction process

    DOEpatents

    Schmid, Bruce K.; Junkin, James E.

    1982-12-21

    Pyrite addition to a coal liquefaction process (22, 26) is controlled (118) in inverse proportion to the calcium content of the feed coal to maximize the C.sub.5 --900.degree. F. (482.degree. C.) liquid yield per unit weight of pyrite added (110). The pyrite addition is controlled in this manner so as to minimize the amount of pyrite used and thus reduce pyrite contribution to the slurry pumping load and disposal problems connected with pyrite produced slag.

  1. Slurry Phase Iron Catalysts for Indirect Coal Liquefaction

    SciTech Connect

    Abhaya K. Datye

    1998-09-10

    This report describes research conducted to support the DOE program in indirect coal liquefaction. Specifically, we have studied the attrition behavior of Iron Fischer-Tropsch catalysts, their interaction with the silica binder and the evolution of iron phases in a synthesis gas conversion process. The results provide significant insight into factors that should be considered in the design of catalysts for the conversion of coal-derived synthesis gas into liquid fuels.

  2. Technology for advanced liquefaction processes: Coal/waste coprocessing studies

    SciTech Connect

    Cugini, A.V.; Rothenberger, K.S.; Ciocco, M.V.

    1995-12-31

    The efforts in this project are directed toward three areas: (1) novel catalyst (supported and unsupported) research and development, (2) study and optimization of major operating parameters (specifically pressure), and (3) coal/waste coprocessing. The novel catalyst research and development activity has involved testing supported catalysts, dispersed catalysts, and use of catalyst testing units to investigate the effects of operating parameters (the second area) with both supported and unsupported catalysts. Several supported catalysts were tested in a simulated first stage coal liquefaction application at 404{degrees}C during this performance period. A Ni-Mo hydrous titanate catalyst on an Amocat support prepared by Sandia National laboratories was tested. Other baseline experiments using AO-60 and Amocat, both Ni-Mo/Al{sub 2}O{sub 3} supported catalysts, were also made. These experiments were short duration (approximately 12 days) and monitored the initial activity of the catalysts. The results of these tests indicate that the Sandia catalyst performed as well as the commercially prepared catalysts. Future tests are planned with other Sandia preparations. The dispersed catalysts tested include sulfated iron oxide, Bayferrox iron oxide (iron oxide from Miles, Inc.), and Bailey iron oxide (micronized iron oxide from Bailey, Inc.). The effects of space velocity, temperature, and solvent-to-coal ratio on coal liquefaction activity with the dispersed catalysts were investigated. A comparison of the coal liquefaction activity of these catalysts relative to iron catalysts tested earlier, including FeOOH-impregnated coal, was made. These studies are discussed.

  3. Wilsonville Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama. Technical progress report, Run 243 with Illinois 6 coal

    SciTech Connect

    Not Available

    1984-02-01

    This report presents the operating results for Run 243 at the Advanced Coal Liquefaction R and D Facility in Wilsonville, Alabama. This run was made in an Integrated Two-Stage Liquefaction (ITSL) mode using Illinois 6 coal from the Burning Star mine. The primary objective was to demonstrate the effect of a dissolver on the ITSL product slate, especially on the net C/sub 1/-C/sub 5/ gas production and hydrogen consumption. Run 243 began on 3 February 1983 and continued through 28 June 1983. During this period, 349.8 tons of coal was fed in 2947 hours of operation. Thirteen special product workup material balances were defined, and the results are presented herein. 29 figures, 19 tables.

  4. Status of coal liquefaction in the United States and related research and development at the Oak Ridge National Laboratory

    SciTech Connect

    Salmon, R.; Cochran, H.D. Jr.; McNeese, L.E.

    1982-10-05

    We divide coal liquefaction processes into four categories: (1) indirect liquefaction, such as Fischer-Tropsch and methanol synthesis, in which coal is fist gasified to produce a synthesis gas which is then recombined to produce liquids; (2) direct liquefaction processes, typified by H-Coal, Exxon Donor Solvent (EDS), and SRC-I and II, in which a slurry of coal and solvent is subjected to high severity liquefaction conditions, either with or without added catalyst; (3) two-stage liquefaction, such as Conoco's CSF process, in which an initial dissolution at mild conditions is followed by a more severe catalytic hydrogenation-hydrocracking step; or the short contact time two-stage liquefaction processes being developed currently by groups which include Chevron, Electric Power Research Institute (EPRI), Department of Energy/Fossil Energy (DOE/FE); and (4) pyrolysis and hydropyrolysis processes, such as COED and Cities Service-Rockewell, in which coal is carbonized to produce liquids, gases, and char. Pilot plant experience with the various processes is reviewed (including equipment problems, corrosion and abrasion, refractory life, heat recovery, coke deposits, reactor kinetics, scale-up problems, health hazards, environmental impacts, upgrading products, economics, etc.). Commercialization possibilities are discussed somewhat pessimistically in the light of reduction of US Oil imports, weakening oil prices, conversion to coal, smaller automobiles, economics and finally, some uncertainty about SFC goals and policies. (LTN)

  5. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction

    SciTech Connect

    Not Available

    1993-01-01

    Improved coal liquefaction was reinvestigated for the current two-stage process on the basis of the associated molecular nature of coal. Since a significant portion of coal molecules are physically associated as pointed in our recent paper, physical dissolution should be considered. The step-wise, high-temperature soaking is a simple and effective method for coal dissolution. Larger dissolution makes liquefaction severity lower. Broad molecular mass distribution in the associated coal was another important factor. The selective reaction of fractions with high molecular weight isolated after the high-temperature soaking makes gas yield lower. Tests using an autoclave by the concept shown in Figure 5 enabled to more oil and 15-20% less gas yields. It is expected that the procedure will result in great cost reduction in coal liquefaction.

  6. Enhancing low severity coal liquefaction reactivity using mild chemical pretreatment. Quarterly technical progress report, December 1991--February 1992

    SciTech Connect

    Shams, K.G.; Miller, R.L.; Baldwin, R.M.

    1992-07-13

    In this paper, we describe results from a study in which mild chemical pretreatment of coal has been used to enhance low severity liquefaction reactivity. We have found that ambient pretreatment of eight Argonne coals using methanol and a trace amount of hydrochloric acid improves THF-soluble conversions 24.5 wt% (maf basis) for Wyodak subbituminous coal and 28.4 wt% for Beulah-Zap lignite with an average increase of 14.9 wt% for liquefaction of the eight coals at 623 K (350{degree}C) reaction temperature and 30 min. reaction time. Similar enhancement results occurred using, hexane or acetone in place of methanol. Pretreatment with methanol and HCI separately indicated that both reagents were necessary to achieve maximum liquefaction improvement. Acid concentration was the most important pretreatment variable studied; liquefaction reactivity increased with increasing acid concentration up to 2 vol%. No appreciable effect on reactivity was observed at higher acid concentrations. Although vapor phase alcohol/HCI mixtures have been shown to partially alkylate bituminous coals, analysis of Wyodak and Illinois {number_sign}6 coal samples indicated that no organic phase alteration occurred during pretreatment; however, over 90 wt% of the calcium was removed from each coal. Calcium is thought to catalyze retrogressive reactions during coal pyrolysis, and thus calcium removal prior to low severity liquefaction minimizes the rate of THF-insoluble product formation.

  7. Conversion of Low-Rank Wyoming Coals into Gasoline by Direct Liquefaction

    SciTech Connect

    Polyakov, Oleg

    2013-12-31

    Under the cooperative agreement program of DOE and funding from Wyoming State’s Clean Coal Task Force, Western Research Institute and Thermosolv LLC studied the direct conversion of Wyoming coals and coal-lignin mixed feeds into liquid fuels in conditions highly relevant to practice. During the Phase I, catalytic direct liquefaction of sub-bituminous Wyoming coals was investigated. The process conditions and catalysts were identified that lead to a significant increase of desirable oil fraction in the products. The Phase II work focused on systematic study of solvothermal depolymerization (STD) and direct liquefaction (DCL) of carbonaceous feedstocks. The effect of the reaction conditions (the nature of solvent, solvent/lignin ratio, temperature, pressure, heating rate, and residence time) on STD was investigated. The effect of a number of various additives (including lignin, model lignin compounds, lignin-derivable chemicals, and inorganic radical initiators), solvents, and catalysts on DCL has been studied. Although a significant progress has been achieved in developing solvothermal depolymerization, the side reactions – formation of considerable amounts of char and gaseous products – as well as other drawbacks do not render aqueous media as the most appropriate choice for commercial implementation of STD for processing coals and lignins. The trends and effects discovered in DCL point at the specific features of liquefaction mechanism that are currently underutilized yet could be exploited to intensify the process. A judicious choice of catalysts, solvents, and additives might enable practical and economically efficient direct conversion of Wyoming coals into liquid fuels.

  8. Advanced direct coal liquefaction concepts. Final report, Volume 2

    SciTech Connect

    Berger, D.J.; Parker, R.J.; Simpson, P.L.

    1994-07-01

    Integration of innovative steps into new advanced processes have the potential to reduce costs for producing liquid fuels. In this program, objective is to develop a new approach to liquefaction that generates an all distillate product slate at a reduced cost of about US$25/barrel of crude oil equivalent. A Counterflow Reactor was developed in cooperation with GfK mbH, Germany. Advantages are low hydrogen recycle rates and low feed preheating requirements. Coal/heavy oil slurry is injected into the top of the reactor while the recycle gas and make up hydrogen is introduced into the bottom; hydrogenation products are withdrawn from the top. PU study resulted in distillable oil yields up to 74 wt % on feed (dry ash free) from coprocessing feed slurries containing 40 wt % Vesta subbituminous coal and 60 wt % Cold Lake heavy vacuum tower bottoms. Technologies developed separately by CED and ARC were combined. A 1-kg/hr integrated continuous flow bench scale unit was constructed at the ARC site in Devon, Alberta, based on modifications to a unit at Nisku, Alberta (the modified unit was used in the preliminary economic evaluation).

  9. Inspection of integrated two-stage liquefaction products by petroleum assay

    SciTech Connect

    Winschel, R.A.; Zhou, P.

    1991-12-31

    A series of standard petroleum inspection tests was performed on the net product and fractions thereof from the direct liquefaction of Pittsburgh seam (Ireland Mine) coal. The product examined was generated during Run 259, period G in the catalytic/catalytic, close-coupled Integrated Two-Stage Liquefaction operating mode at the Advanced Coal Liquefaction Tests Facility in Wilsonville, Alabama. In this paper, the results of these inspection tests are reported and compared with American Society for Testing and Materials (ASTM) specifications for gasoline, jet fuel and diesel fuel. Qualitative refining requirements are inferred from the data.

  10. Inspection of integrated two-stage liquefaction products by petroleum assay

    SciTech Connect

    Winschel, R.A. ); Zhou, P. )

    1991-01-01

    A series of standard petroleum inspection tests was performed on the net product and fractions thereof from the direct liquefaction of Pittsburgh seam (Ireland Mine) coal. The product examined was generated during Run 259, period G in the catalytic/catalytic, close-coupled Integrated Two-Stage Liquefaction operating mode at the Advanced Coal Liquefaction Tests Facility in Wilsonville, Alabama. In this paper, the results of these inspection tests are reported and compared with American Society for Testing and Materials (ASTM) specifications for gasoline, jet fuel and diesel fuel. Qualitative refining requirements are inferred from the data.

  11. Dermal toxicity of a medium-boiling (154-378 degrees C) coal liquefaction product in the rat--Part I.

    PubMed

    Chu, I; Villeneuve, D C; Côte, M; Valli, V E; Otson, R

    1988-01-01

    The subchronic dermal toxicity of a medium-boiling coal liquefaction product (CLP, 154-378 degrees C) was investigated in the rat. CLP was applied to the shaved backs of rats at dose levels of 50, 100, 200, or 400 mg/kg body weight.d, 7 d/wk for a period of 13 wk. Control groups received 0.4 ml/kg of normal saline. Signs of dermal irritation were observed at sites of application in males dosed at 200 and 400 mg/kg body weight and were characterized by thickened, focally necrotic and ulcerative skin. All animals survived the full length of the treatment period. Growth depression was observed in males at all dose levels, but no significant decrease in weight gain was observed in females. An increase in liver/body weight ratios was observed in all treatment groups of both sexes. The organ/body weight ratios for the spleen, heart, kidney, and brain were also increased in the upper dose groups of both sexes. Treatment with CLP caused a dose-dependent decrease in hemoglobin and packed cell volume in both sexes of all dose groups. The number of erythrocytes was decreased and that of neutrophils was increased in some CLP-treated groups of both sexes. There was a mild myeloid hyperplasia with increased myeloid/erythroid ratios in the 200- and 400-mg/kg groups of both sexes. Hepatic microsomal ethoxyresorufin deethylase activity was increased in all treatment groups of females, and in males dosed at 100 mg/kg and higher. In the renal tubules mild treatment-related histological changes occurred, which consisted of eosinophilic inclusions, increased cytoplasmic volume, and pyknosis. These changes were noted in the high-dose groups of both sexes. These data indicate that the medium-boiling CLP could produce systemic toxicity when applied dermally at 50 mg/kg body weight.d.

  12. Role of iron-based catalyst and hydrogen transfer in direct coal liquefaction

    SciTech Connect

    Xian Li; Shuxun Hu; Lijun Jin; Haoquan Hu

    2008-03-15

    The aim of this research is to understand the major function of iron-based catalysts on direct coal liquefaction (DCL). Pyrolysis and direct liquefaction of Shenhua bituminous coal were carried out to investigate the effect of three solvents (wash-oil from coal-tar, cycle-oil from coal liquefaction, and tetralin) in a N{sub 2} or a H{sub 2} atmosphere and with or without catalyst. The hydrogen content in the solvent and liquid product and the H{sub 2} consumption for every run were calculated to understand the hydrogen transfer approach in DCL. The results showed that the iron-based catalyst promotes the coal pyrolysis, and the dominating function of the catalyst in DCL is to promote the formation of activated hydrogen and to accelerate the secondary distribution of H in the reaction system including the gas, liquid, and solid phases. The major transfer approach of the activated hydrogen is from molecular hydrogen to solvent and then from solvent to coal, and the solvent takes on the role of a 'bridge' in the hydrogen transfer approach. 31 refs., 5 figs., 3 tabs.

  13. Coal liquefaction process solvent characterization and evaluation: Technical progress report, January 1, 1986--March 31, 1986

    SciTech Connect

    Winschel, R.A.; Robbins, G.A.; Burke, F.P.

    1986-07-01

    Conoco Coal research Division is characterizing samples of direct coal liquefaction process oils based on a variety of analytical techniques to provide a detailed description of the chemical composition of the oils, to more fully understand the interrelationship of process oil composition and process operations, to aid in plant operation, and to lead to process improvements. The approach taken is to obtain analyses of a large number of well-defined process oils taken during periods of known operating conditions and known process performance. A variety of coal liquefaction process oils were dewaxes by variants of commercial processes in order to improve their quality as donor solvents. Twenty-five oils were analyzed from Hydrocarbon Research Incorporated's (HRI) Catalytic Two-Stage Liquefaction (CTSL) Run 227- 27. Ten microautoclave tests were made to ''calibrate'' the reactivity of our standard coal. Nineteen samples of coal and reaction products of coal and potassium/crown ether, supplied by Purdue University, were analyzed by infrared spectroscopy to derive quantitative and qualitative structural information. 22 refs., 13 figs., 38 tabs.

  14. Rationale for continuing R&D in indirect coal liquefaction

    SciTech Connect

    Gray, D.; Tomlinson, G.

    1995-12-31

    The objective of this analysis is to use the world energy demand/supply model developed at MITRE to examine future liquid fuels supply scenarios both for the world and for the United States. This analysis has determined the probable extent of future oil resource shortages and the likely time frame in which the shortages will occur. The role that coal liquefaction could play in helping to alleviate this liquid fuels shortfall is also examined. The importance of continuing R&D to improve process performance and reduce the costs of coal-derived transportation fuel is quantified in terms of reducing the time when coal liquids will become competitive with petroleum.

  15. Coal liquefaction in an inorganic-organic medium

    DOEpatents

    Vermeulen, Theodore; Grens, II, Edward A.; Holten, Ronald R.

    1982-01-01

    Improved process for liquefaction of coal by contacting pulverized coal in an inorganic-organic medium solvent system containing a ZnCl.sub.2 catalyst, a polar solvent with the structure RX where X is one of the elements O, N, S or P, and R is hydrogen or a lower hydrocarbon radical; the solvent system can contain a hydrogen donor solvent (and must when RX is water) which is immiscible in the ZnCl.sub.2 and is a hydroaromatic hydrocarbon, selected from tetralin, dihydrophenanthrene, dihydroanthracene or a hydrogenated coal derived hydroaromatic hydrocarbon distillate fraction.

  16. Advanced liquefaction using coal swelling and catalyst dispersion techniques. Quarterly technical progress report, April--June 1992

    SciTech Connect

    Curtis, C.W.; Gutterman, C.; Chander, S.

    1992-08-26

    Research in this project centers upon developing a new approach to the direct liquefaction of coal to produce an all-distillate product slate at a sizable cost reduction over current technology. The approach integrates all aspects of the coal liquefaction process including coal selection, pretreatment, coal swelling with catalyst impregnation, coal liquefaction experimentation, product recovery with characterization, alternate bottoms processing, and a technical assessment including an economic evaluation. The project is being carried out under contract to the United States Department of Energy. On May 28, 1992, the Department of Energy authorized starting the experimental aspects of this projects; therefore, experimentation at Amoco started late in this quarterly report period. Research contracts with Auburn University, Pennsylvania State University, and Foster Wheeler Development Corporation were signed during June, 1992, so their work was just getting underway. Their work will be summarized in future quarterly reports. A set of coal samples were sent to Hazen Research for beneficiation. The samples were received and have been analyzed. The literature search covering coal swelling has been up-dated, and preliminary coal swelling experiments were carried out. Further swelling experimentation is underway. An up-date of the literature on the liquefaction of coal using dispersed catalysts is nearing completion; it will be included in the next quarterly report.

  17. Donor solvent coal liquefaction with bottoms recycle at elevated pressure

    DOEpatents

    Bauman, Richard F.; Taunton, John W.; Anderson, George H.; Trachte, Ken L.; Hsia, Steve J.

    1982-01-01

    An improved process for liquefying solid carbonaceous materials wherein increased naphtha yields are achieved by effecting the liquefaction at a pressure within the range from about 1750 to about 2800 psig in the presence of recycled bottoms and a hydrogen-donor solvent containing at least 0.8 wt % donatable hydrogen. The liquefaction is accomplished at a temperature within the range from about 700.degree. to about 950.degree. F. The coal:bottoms ratio in the feed to liquefaction will be within the range from about 1:1 to about 5:1 and the solvent or diluent to total solids ratio will be at least 1.5:1 and preferably within the range from about 1.6:1 to about 3:1. The yield of naphtha boiling range materials increases as the pressure increases but generally reaches a maximum at a pressure within the range from about 2000 to about 2500 psig.

  18. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Technical progress report, August 1992--November 1992

    SciTech Connect

    Song, C.; Huang, L.; Wenzel, K.; Saini, A.K.; Burgess, C.; Hatcher, P.G.; Schobert, H.H.

    1992-12-01

    During this quarterly period progress has been made in the following three subjects related to the effects of low-temperature thermal and catalytic pretreatments on coal structure and reactivity in liquefaction. First, the liquefaction behavior of three bituminous coals with a carbon content ranging from 77% to 85% was evaluated spectroscopically by {sup 13}C NMR and pyrolysis/gas chromatography/mass spectrometry to delineate the structural changes that occur in the coal during liquefaction. Complementary data includes ultimate and proximate analysis, along with optical microscopy for maceral determinations. Even though these are all bituminous coals they exhibit quite different physical and chemical characteristics. The coals vary in rank, ranging from HvC b to HvA b, in petrographic composition, different maceral percentages, and in chemical nature, percent of carbon and of volatiles. It is these variations that govern the products, their distribution, and conversion percentages. Some of the products formed can be traced to a specific maceral group. Second, pyrolysis-GC-MS and FTIR techniques were used to characterize Wyodak coal before and after drying in vacuum and in air and the residues from its thermal and catalytic liquefactions. The analysis of the air-dried coal shows a decrease in the phenolic type structures in the coal network and increase in the carbonyl structures as the oxidative drying proceeds. An enhanced decrease in the carbonyl structure is observed in the liquefaction residues from the raw coal as compared to that of the vacuum dried coal. The analyses of the liquefaction residues of the air-dried coal show an increase in the ether linkages which may have a negative impact on liquefaction. The extent of the solvent adduction also increases during liquefaction with the extent of oxidation of the coal. Finally, the effects of reaction conditions were investigated on conversion of low-rank coals using a Texas subbituminous coal.

  19. Steam pretreatment for coal liquefaction. Fifth quarterly report, 1 October 1991--31 December 1991

    SciTech Connect

    Graff, R.A.; balogh-Nair, V.

    1992-06-18

    Steam pretreatment is the reaction of coal with steam at temperatures well below those usually used for solubilization. The objective of the proposed work is to test the application of steam pretreatment to coal liquefaction. Installation of the stirred autoclave for conventional slurry liquefaction (slow heating) was completed and preliminary testing carried out. Two liquefaction tests with untreated Illinois No. 6 coal gave satisfactory results. An additional pretreatment test of Blind Canyon coal was conducted this quarter which confirms the tentative conclusions previously reached: volatiles yields are increased by the addition of sulfided iron catalyst; it is not possible to ascertain (by the procedure used) whether extraction yield decreases or remains constant. Chromatographic separation and analysis of the products from treated {alpha}-benzylnaphthyl ether has been continued. A transformation of the product over several weeks has been noted. The {sup 1}H nmr spectrum of this product obtained in a glass lined reactor is found to be different from that obtained previously in a stainless steel reactor. The model compound {alpha}-naphthylmethyl phenyl ether has been steam pretreated and the analysis of its liquid product started. Three major components have been identified.

  20. Advanced liquefaction using coal swelling and catalyst dispersion techniques. Volume 1, Final technical report, October 1, 1991--September 30, 1994

    SciTech Connect

    Curtis, C.W.; Gutterman, C.; Chander, S.

    1994-12-31

    The overall objective of this project was to develop a new approach for the direct liquefaction of coal to produce an all-distillate product slate at a sizable cost reduction over current technology. The approach integrated coal selection, pretreatment, coal swelling with catalyst impregnation, liquefaction, product recovery with characterization, alternate bottoms processing, and a technical assessment including an economic evaluation. Heterofunctional solvents were the most effective in swelling coals. Also solvent blends such as isopropanol/water were more effective than pure solvents alone. Impregnating slurry catalysts simultaneously during coal swelling showed that better uptake was achieved with nonswelling solvent and higher impregnation temperature. Some enhancement in initial coal conversion was seen liquefying SO{sub 2}-treated Black Thunder coal with slurry catalysts, and also when hydrogen donor liquefaction solvents were used. Noncatalytic reactions showed no benefit from SO{sub 2} treatment. Coupling coal swelling and SO{sub 2} treatment with slurry catalysts was also not beneficial, although high conversion was seen with continuous operation and long residence time, however, similar high conversion was observed with untreated coal. SO{sub 2} treatment is not economically attractive unless it provides about 17% increase in coal reactivity. In most cases, the best results were obtained when the coal was untreated and the slurry catalyst was added directly into the reactor. Foster Wheeler`s ASCOT process had better average liquid yields than either Wilsonville`s vacuum tower/ROSE combination or delayed coking process. This liquid product also had good quality.

  1. Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction

    SciTech Connect

    Klein, M.T.

    1991-12-30

    The purpose of this work is to investigate the kinetics-assisted design, synthesis and characterization of fme-pardcle, unsupported catalysts for coal liquefaction. The goal is to develop a fundamental understanding of coal catalysis and catalysts that will, in turn, allow for the specification of a novel optimal catalyst for coal liquefaction.

  2. Coal liquefaction. Quarterly report, January-March 1979. [US DOE supported

    SciTech Connect

    1980-01-01

    Progress in DOE-supported coal liquefaction pilot plant projects is reported: company, location, contract, funding, process description, history and progress in the current quarter. Related projects discussed are: coking and gasification of liquefaction plant residues, filtration of coal liquids and refining of coal liquids by hydrogenation. (LTN)

  3. Advanced direct coal liquefaction. Quarterly technical progress report No. 2, December 1983-February 1984

    SciTech Connect

    Paranjape, A.S.

    1984-04-30

    Five Bench-Scale coal liquefaction runs were completed with Wyoming subbituminous coal in a two-stage process scheme. In this process scheme, LDAR, the lighter fraction of ash-free resid, was fed to the catalytic stage prior to its recycle to the thermal stage, whereas DAR, the heavy fraction of the deashed resid, was directly recycled to the thermal stage without any intermediate processing step. The results indicate that increasing coal space rate in the dissolver resulted in lower coal conversion and reduced distillate yield in this process configuration. The coal conversions decreased from 92 wt% to 89 wt% (MAF coal) and the distillate yield was reduced from 50 wt% to less than 40 wt% (MAF coal), as the coal space velocity increased. Attempts to duplicate the yields of Run 32, at comparable process conditions in Runs 37 and 38, were unsuccessful. Several process parameters were investigated but failed to show why the yields of Run 32 could not be duplicated. Valuable process related information was gained as a result of process parameter studies completed during these runs. At comparable process conditions, coal conversions were lower by about 3 to 4 relative percent and were only in the 87 wt% (MAF coal) range. Similarly, the distillate yield was about 40 wt% (MAF coal) which is about 10 wt% lower than observed in Run 32. Although no exact cause for these results could be determined, it appeared that the H/C atomic ratio of the solvent and possibly the flow pattern (plug-flow versus back-mixed) could have affected the coal conversion and quantity of distillate product produced. A significant decrease in coal conversion of 4 to 5 wt% was observed when the disposable catalyst (iron oxide) was removed from the reaction mixture and therefore substantiates the need for a disposable catalyst in the liquefaction of Wyoming subbituminous coal.

  4. Effects of coal rank on the chemical composition and toxicological activity of coal liquefaction materials

    SciTech Connect

    Wright, C.W.; Dauble, D.D.

    1986-05-01

    This report presents data from the chemical analysis and toxicological testing of coal liquefaction materials from the EDS and H-Coal processes operated using different ranks of coal. Samples of recycle solvent from the bottoms recycle mode of the EDS direct coal liquefaction process derived from bituminous, sub-bituminous, and lignite coals were analyzed. In addition, the H-Coal heavy fuel oils derived from bituminous and sub-bituminous coals were analyzed. Chemical methods of analysis included adsoprtion column chromatography, high-resolution gas chromatography, gas chromatography/mass spectrometry, and low-voltage probe-inlet mass spectrometry. The toxicological activity of selected samples was evaluated using the standard microbial mutagenicity assay, an initiation/promotion assay for mouse-skin tumorigenicity, and a static bioassy with Daphnia magna for aquatic toxicity of the water-soluble fractions. 22 refs., 16 figs., 14 tabs.

  5. Microbial recovery of metals from spent coal liquefaction catalysts

    SciTech Connect

    Sperl, P.L.; Sperl, G.T.

    1991-01-01

    This project was initiated on October 1, 1989, for the purpose of recovering metals from spent coal liquefaction catalysts. Two catalyst types are the subject of the contract. The first is a Ni-Mo catalyst supported on alumina (Shell 324) as is used in a pilot scale coal liquefaction facility at Wilsonville, Alabama. A large sample of spent catalyst has been obtained. The second material is an unsupported ammonium molybdate catalyst used in a pilot process by the Department of energy at the Pittsburgh energy Technology Center. The object of the contract is to treat these spent catalysts with microorganisms, especially Thiobacillus ferrooxidans, but also other Thiobacillus sp. and possibly Sulfolobus, to leach and remove the metals (Ni and Mo) from the spent catalysts into a form which can be readily recovered by conventional techniques.

  6. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Technical progress report, December 1992--March 1993

    SciTech Connect

    Song, C.; Saini, A.K.; Wenzel, K.; Huang, L.; Hatcher, P.G.; Schobert, H.H.

    1993-04-01

    This work is a fundamental study of catalytic pretreatments as a potential preconversion step to low-severity liquefaction. The ultimate goal of this work is to provide the basis for the design of an improved liquefaction process and to facilitate our understanding of those processes that occur when coals are initially dissolved. The main objectives of this project are to study the effects of low-temperature pretreatments on coal structure and their impacts on the subsequent liquefaction. The effects of pretreatment temperatures, catalyst type, coal rank and influence of solvent will be examined. We have made significant progress in the following four aspects during this quarterly period: (1) influence of drying and oxidation of coal on the conversion and product distribution in catalytic liquefaction of Wyodak subbituminous coal using a dispersed catalyst; (2) spectroscopic characterization of dried and oxidized Wyodak coal and the insoluble residues from catalytic and thermal liquefaction; (3) the structural alteration of low-rank coal in low-severity liquefaction with the emphasis on the oxygen-containing functional groups; and (4) effects of solvents and catalyst dispersion methods in temperature-programmed and non-programmed liquefaction of three low-rank coals.

  7. Non-catalytic liquefaction of coal with bagasse, a biomass waste

    SciTech Connect

    Rafiqul, I.; Lugang, B.; Yan, Y.; Li, T.

    1999-07-01

    Liquefaction of a Chinese bituminous coal with bagasse, a kind of biomass waste, have been carried out in an autoclave of 300 ml capacity at a temperature range of 350--450 C, reaction time 15--45 min and cool hydrogen pressure 300--700 PSIG (2.04 4.76 MPa). Optimization of the co-liquefaction process was done with respect to oil yield by Factorial Experiment Design Method. Oil yield reached 48% at optimum conditions of temperature: 420 C, cool hydrogen pressure: 500 PSIG and reaction time: 40 min. A polynomial mathematical model, a second order response surface model, has been obtained for correlating the oil yield response factor as well as conversion with the major process variables. The equation derived by the authors holds good in determining the effect of process variables on response factors for any regime conditions in the range of the Planned Experimental Design. Experimental data were also correlated by a kinetic model. The model is based on coal and bagasse, undergoing thermal cracking, is first converted parallel to form preasphaltene and asphaltene and low molecular gaseous products; then consecutively oil is formed from preasphaltene and asphaltene. Activation energies for these three reactions are 32.51 KJ/mol, 75.14 KJ/mol and 44.65 KJ/mol, respectively. These values are lower than that of liquefaction of coal alone. It justifies that the addition of bagasse is effective in enhancing the process of co-liquefaction and giving higher yield of oil than for liquefaction of coal alone. Calculated values from this model fairly agree with the experimental data.

  8. Two-stage, closed coupled catalytic liquefaction of coal. Sixteenth quarterly report, 1 July 1992--30 September 1992

    SciTech Connect

    Comolli, A.G.; Johanson, E.S.; Karolkiewicz, W.F.; Lee, L.K.; Stalzer, R.H.

    1992-12-01

    This quarterly report covers activities of the Two-Stage, Close-Coupled Catalytic Liquefaction of Coal Program during the period of July 1--September 30, 1992, at Hydrocarbon Research, Inc., in Lawrenceville and Princeton, New Jersey. This DOE contract period is from October 1, 1998 to December 31, 1992. The overall purpose of the program is to achieve higher yields of better quality transportation and turbine fuels and to lower the capital and production costs in order to make the products from direct coal liquefaction competitive with other fossil fuel products. The quarterly report covers work on Laboratory testing, Bench Scale Studies and PDU Activities focusing on scale-up of the Catalytic Two-Stage Liquefaction (CTSL) processing of sub-bituminous Black Thunder Coal.

  9. Coal liquefaction process solvent characterization and evaluation: Progress report, 1 April--30 June 1986

    SciTech Connect

    Winschel, R.A.; Robbins, G.A.; Burke, F.P.

    1986-11-01

    Conoco Coal Research Division is characterizing samples of direct coal liquefaction process oils based on a variety of analytical techniques to provide a detailed description of the chemical composition of the oils to more fully understand the interrelationship of process oil composition and process operations, to aid in plant operation, and to lead to process improvements. The approach taken is to obtain analyses of a large number of well-defined process oils taken during periods of known operating conditions and known process performance. A set of thirty-one process oils from the Hydrocarbon Research, Inc. (HRI) Catalytic Two-Stage Liquefaction (CTSL) bench unit was analyzed to provide information on process performance. The Fourier-Transform infrared (FTIR) spectroscopic method for the determination of phenolics in cola liquids was further verified. A set of four tetahydrofuran-soluble products from Purdue Research Foundation's reactions of coal/potassium/crown ether, analyzed by GC/MS and FTIR, were found to consist primarily of paraffins (excluding contaminants). Characterization data (elemental analyses, /sup 1/H-NMR and phenolic concentrations) were obtained on a set of twenty-seven two-stage liquefaction oils. Two activities were begun but not completed. First, analyses were started on oils from Wilsonville Run 250 (close- coupled ITSL). Also, a carbon isotopic method is being examined for utility in determining the relative proportion of coal and petroleum products in coprocessing oils.

  10. Status of the Development of EDS Coal Liquefaction.

    PubMed

    Vick, G K; Epperly, W R

    1982-07-23

    This article traces the evolution and development of a modern coal liquefaction technology, the EDS (Exxon Donor Solvent) process, over a period of 15 years. During this time the technology has been advanced from laboratory experiments to a pilot plant with a coal feed rate of 250 tons per day, and findings from several areas of science and technology have been important. The process is now in the final stage of development to generate the data needed to design a plant of commercial size.

  11. Short Contact Time Direct Coal Liquefaction Using a Novel Batch Reactor

    SciTech Connect

    He Huang; Michael T. Klein; William H. Calkins

    1997-04-03

    The primary objective of this research is to optimize the design and operation of the bench scale batch reactor (SCTBR) for studying direct coal liquefaction at short contact times (.01 to 10 minutes or longer) . An additional objective is to study the kinetics of direct coal liquefaction particularly at short reaction times. Both of these objectives have been nearly achieved, however this work has shown the great importance of the liquefaction solvent characteristics and the solvent-catalyst interaction on the liquefaction process. This has prompted us to do a preliminary investigation of solvents and the solvent-catalyst systems in coal liquefaction. SUMMARY AND CONCLUSIONS 1) Conversion vs time data have been extended to 5 coals of ranks from lignite to low volatile bituminous coal. A broad range of reaction rates have been observed with a maximum in the high volatile bituminous range. 2) A series of direct coal liquefaction runs have been made using a range of nitrogen containing solvents that given high liquefaction conversions of coal. These runs are now being analyzed. 3) The coalification process has been shown by TGA to go through an intermediate stage which may account for the greater reactivity of bituminous coals in the direct coal liquefaction process. 4) It was shown that coal rank can be accurately determined by thermogravimetric analysis

  12. Surface modified coals for enhanced catalyst dispersion and liquefaction

    SciTech Connect

    Dr. Yaw D. Yeboah

    1998-10-29

    The aim of the study is to enhance catalyst loading and dispersion in coal for improved liquefaction by preadsorption of surfactants and catalysts on to the coal. During this reporting period, zeta potential measurements were conducted to assess the surface charge on the raw, pretreated and catalyzed coal samples. The surface area, transmission spectroscopy and luminescence intensity of the raw coal and pretreated coal samples were also determined to assess the quality of the coal surface. Across a broad range of pH values, the raw coal had an overall negative charge. Coal treated with anionic surfactant SDS maintained an overall net negative surface negative charge. The interaction between the coal and cationic surfactant DDAB caused the opposite effect resulting in a more positive coal surface charge. Although one would have expected little or no effect of the neutral surfactant Triton X-100, there appears to be some difference in the results of the raw coal and the coal treated with Triton X-100. The authors believe that the Triton not only binds to the nonpolar sites but also has a strong affinity for the polar sites through electrostatic bonding and interaction between the hydrophobic tails. The addition of molybdenum to coal pretreated with DDAB caused a reduction in the positive charge of the coal surface probably due to possible ionic interaction between the coal surface, the surfactant and the catalyst. The adsorption isotherm of the coal was characteristic of isotherms for porous samples and the surface area of the coal increased from 30 m{sup 2}/g to 77 m{sup 2}/g when washed with deionized water. This suggests coal washing may be one method of increasing the surface area for surfactant adsorption. Although the transmission measurements provided valuable information about the coal it resulted in little information on the amount of adsorbed Triton. However, the maximum solid-liquid ratio for optimum surfactant loading of Triton X-100 was determined via

  13. Two-stage, close coupled catalytic liquefaction of coal. Eleventh quarterly report, 1 April 1991--30 June 1991

    SciTech Connect

    Comolli, A.G.; Johanson, E.S.; Panvelker, S.V.; Popper, G.A.; Stalzer, R.H.

    1991-10-01

    The overall purpose of the program is to achieve higher yields of better quality transportation and turbine fuels and to lower the capital and production costs in order to make the products from direct coal liquefaction competitive with other fossil fuel products.

  14. Two-stage, close coupled catalytic liquefaction of coal. [Catalysts: FeOOH and NiMo

    SciTech Connect

    Comolli, A.G.; Johanson, E.S.; Panvelker, S.V.; Popper, G.A.; Stalzer, R.H.

    1991-10-01

    The overall purpose of the program is to achieve higher yields of better quality transportation and turbine fuels and to lower the capital and production costs in order to make the products from direct coal liquefaction competitive with other fossil fuel products.

  15. Fractionally distilled SRC-I, SRC-II, EDS, H-Coal and ITSL direct coal liquefaction process materials: a comparative summary of chemical analysis and biological testing

    SciTech Connect

    Wright, C.W.; Later, D.W.; Dauble, D.D.; Wilson, B.W.

    1985-07-01

    This document reports and compares the results compiled from chemical analyses and biological testing of coal liquefaction process materials which were fractionally distilled, after production, into various comparable boiling-point range cuts. Comparative analyses were performed on solvent refined coal (SRC)-I, SRC-II, H-Coal, EDS an integrated two-stage liquefaction (ITSL) distillate materials. Mutagenicity and carcinogenicity assays were conducted in conjunction with chromatographic and mass spectrometric analyses to provide detailed, comparative, chemical and biological assessments. Where possible, results obtained from the distillate cuts are compared to those from coal liquefaction materials with limited boiling ranges. Work reported here was conducted by investigators in the Biology and Chemistry Department at the Pacific Northwest Laboratory (PNL), Richland, WA. 38 refs., 16 figs., 27 tabs.

  16. Ion exchange and adsorption on low rank coals for liquefaction

    SciTech Connect

    Vorres, K.S.

    1994-09-01

    The objectives of this program are to study the application of catalysts and the catalysis of liquefaction of low rank coals. Ion exchange and adsorption techniques are being used or modified to incorporate catalytically active metals (Fe, Co, Ni and Mo) in relatively small (100-2000 ppM) quantities into coal samples. Relative oil yields are being determined by PETC and Auburn University workers as collaborators to establish the effectiveness of the catalyst incorporation techniques. It is hoped that these techniques will provide highly active forms of the catalyst in low concentrations to minimize the need for metals recovery. A two step preparation of the coal is used to (1) remove material which both limits oil conversion and prepares for the addition of exchangeable catalyst, and (2) add catalytically active material which enhances the conversion of the coal matter to the oil fraction in the processing.

  17. Coal liquefaction technology. (Latest citations from the NTIS Bibliographic database). Published Search

    SciTech Connect

    1996-09-01

    The bibliography contains citations concerning the technologies and processes for converting coal to liquid chemicals and fuels. Topics include materials characterization of liquefaction processes, catalysis, pyrolysis, depolymerization, coprocessing, and integrated liquefaction. Also discussed are liquid fuel use in automobiles and power generation, low-temperature carbonization technology, multi-stage liquefaction, cost benefit analysis, and commercialization of liquefaction technology. (Contains 50-250 citations and includes a subject term index and title list.) (Copyright NERAC, Inc. 1995)

  18. Process for utilizing mineral-containing residue from coal liquefaction processes

    SciTech Connect

    Leonard, R.E.

    1981-02-10

    A process is described for utilizing mineral-containing residue from coal liquefaction processes to produce a hydraulic cement. The residue is mixed with siliceous and calcareous matereals and compacted. The compacted solids are introduced into a kiln and fired to produce hydraulic cement clinker. The primary fuel for the clinker production is contained in the residue. The clinker is removed from the kiln and ground to produce cement.

  19. Low severity coal liquefaction promoted by cyclic olefins. Quarterly report, January--March 1994

    SciTech Connect

    Curtis, C.W.

    1994-06-01

    Previous research has suggested that using a more effective hydrogen donor solvent in the low severity coal liquefaction reaction improves coal conversion. In order to understand the results of these methods, both independently and combined, a factorial experiment was designed. Pretreating coal with hydrochloric and sulfurous acid solutions in both water and methanol is compared with pretreating coal using only methanol and with no pretreatment. The effects of these pretreatments on coal liquefaction behavior are contrasted with the ammonium acetate pretreatment. Within each of these, individual reactions are performed with the hydroaromatic 1,2,3,4-tetrahydronaphthalene (tetralin, TET) and the cyclic olefin 1,4,5,8-tetrahydronaphthalene (isotetralin, ISO). The final aspect of the factorial experiment is the comparison of Wyodak subbituminous coal (WY) from the Argonne Premium Sample Bank and Black Thunder subbituminous coal (BT) provided by Amoco. Half of the reactions in the matrix have now been completed. In all but one case, Black Thunder-HCl/H{sub 2}O, the ISO proved to be more reactive than TET. After the other four reactions using this combination are complete, the average conversion may be greater with the cyclic olefin. The second part of this paper describes the current and future work with Fourier transform infrared spectroscopy. The objective of this work is to determine the kinetics of reaction of isotetralin at high temperatures and pressures. This quarter combinations of three products typically produced from isotetralin were used in spectral subtraction.

  20. Continuous bench-scale slurry catalyst testing direct coal liquefaction rawhide sub-bituminous coal

    SciTech Connect

    Bauman, R.F.; Coless, L.A.; Davis, S.M.

    1995-12-31

    In 1992, the Department of Energy (DOE) sponsored research to demonstrate a dispersed catalyst system using a combination of molybdenum and iron precursors for direct coal liquefaction. This dispersed catalyst system was successfully demonstrated using Black Thunder sub-bituminous coal at Wilsonville, Alabama by Southern Electric International, Inc. The DOE sponsored research continues at Exxon Research and Development Laboratories (ERDL). A six month continuous bench-scale program using ERDL`s Recycle Coal Liquefaction Unit (RCLU) is planned, three months in 1994 and three months in 1995. The initial conditions in RCLU reflect experience gained from the Wilsonville facility in their Test Run 263. Rawhide sub-bituminous coal which is similar to the Black Thunder coal tested at Wilsonville was used as the feed coal. A slate of five dispersed catalysts for direct coal liquefaction of Rawhide sub-bituminous coal has been tested. Throughout the experiments, the molybdenum addition rate was held constant at 100 wppm while the iron oxide addition rate was varied from 0.25 to 1.0 weight percent (dry coal basis). This report covers the 1994 operations and accomplishments.

  1. Exploratory research on solvent refined coal liquefaction. Quarterly technical progress report, January 1, 1980-March 31, 1980

    SciTech Connect

    Not Available

    1982-01-01

    This report summarizes the progress of the Exploratory Research on Solvent Refined Coal Liquefaction project by The Pittsburg and Midway Coal Mining Co.'s Merriam Laboratory for the period January 1, 1980 through March 31, 1980. A series of experiments was conducted with three western coals to study the relationship between coal properties and liquefaction behavior. All three coals were low in iron (0.2 to 0.4%, dry coal basis) and processing in both the SRC I and SRC II modes does not appear to be feasible at normal conditions without added catalyst. Adding 1 to 2% pyrite to the feed slurry increased oil yields considerably while reducing SRC and IOM yields and improved operability. Product quality was also generally improved by the catalyst. Operability and oil yields were generally found to be better at 450/sup 0/C than at 465/sup 0/C.

  2. Non-catalytic transfer hydrogenation in supercritical CO2 for coal liquefaction

    NASA Astrophysics Data System (ADS)

    Elhussien, Hussien

    This thesis presents the results of the investigation on developing and evaluating a low temperature (<150°C) non - catalytic process using a hydrogen transfer agent (instead of molecu-lar hydrogen) for coal dissolution in supercritical CO2. The main idea behind the thesis was that one hydrogen atom from water and one hydrogen atom from the hydrogen transfer agent (HTA) were used to hydrogenate the coal. The products of coal dissolution were non-polar and polar while the supercritical CO2, which enhanced the rates of hydrogenation and dissolution of the non-polar molecules and removal from the reaction site, was non-polar. The polar modifier (PM) for CO2 was added to the freed to aid in the dissolution and removal of the polar components. The addition of a phase transfer agent (PTA) allowed a seamless transport of the ions and by-product between the aqueous and organic phases. DDAB, used as the PTA, is an effective phase transfer catalyst and showed enhancement to the coal dissolution process. COAL + DH- +H 2O → COAL.H2 + DHO-- This process has a great feature due to the fact that the chemicals were obtained without requir-ing to first convert coal to CO and H2 units as in indirect coal liquefaction. The experiments were conducted in a unique reactor set up that can be connected through two lines. one line to feed the reactor with supercritical CO 2 and the other connected to gas chromatograph. The use of the supercritical CO2 enhanced the solvent option due to the chemical extraction, in addition to the low environmental impact and energy cost. In this thesis the experiment were conducted at five different temperatures from atmos-pheric to 140°C, 3000 - 6000 psi with five component of feed mixture, namely water, HTA, PTA, coal, and PM in semi batch vessels reactor system with a volume of 100 mL. The results show that the chemicals were obtained without requiring to first convert coal to CO and H2 units as in indirect coal liquefaction. The results show that

  3. Coal liquefaction catalyst development. Quarterly progress report No. 3, October 1-December 31, 1979

    SciTech Connect

    Kim, D. K.; Pellet, R. J.; Mahoney, J. A.

    1980-01-01

    Catalytic baseline runs continued with HDS-1442A in order to improve our baseline statistics as well as to monitor batch reactor performance. Testing of several new catalyst formulations was completed. No promising candidates for testing in the continuous aging unit were identified. The new SRC-II slurry oil was evaluated as a hydrogen donor liquefaction solvent. Our data indicates that the SRC-II heavy distillate oil is not as effective a hydrogen donor solvent as the hydrogenated anthracene oil. It is possible that the catalyst plays a key role in the thermal liquefaction reactions by improving the hydrogen donor properties of the slurry oil through in-situ hydrogenation. The differences in liquefaction behavior between Illinois No. 6 and Wyodak coal were determined. A major portion of our effort was concerned with ascertaining the liquefaction behavior of a Western coal such as Wyodak with AMOCAT type catalysts. A two-month program to determine the feasibility of using the Amoco continuous aging unit for SRC-I product upgrading was outlined.

  4. Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama

    SciTech Connect

    Not Available

    1992-09-01

    This report presents the results of Run 262 performed at the Advanced Coal Liquefaction R D Facility in Wilsonville, Alabama. The run started on July 10, 1991 and continued until September 30, 1991, operating in the Close-Coupled Integrated Two-Stage Liquefaction mode processing Black Thunder Mine subbituminous coal (Wyodak-Anderson seam from Wyoming Powder River Basin). A dispersed molybdenum catalyst was evaluated for its performance. The effect of the dispersed catalyst on eliminating solids buildup was also evaluated. Half volume reactors were used with supported Criterion 324 1/16'' catalyst in the second stage at a catalyst replacement rate of 3 lb/ton of MF coal. The hybrid dispersed plus supported catalyst system was tested for the effect of space velocity, second stage temperature, and molybdenum concentration. The supported catalyst was removed from the second stage for one test period to see the performance of slurry reactors. Iron oxide was used as slurry catalyst at a rate of 2 wt % MF coal throughout the run (dimethyl disulfide (DMDS) was used as the sulfiding agent). The close-coupled reactor unit was on-stream for 1271.2 hours for an on-stream factor of 89.8% and the ROSE-SR unit was on-feed for 1101.6 hours for an on-stream factor of 90.3% for the entire run.

  5. Subtask 3.9 - Direct Coal Liquefaction Process Development

    SciTech Connect

    Aulich, Ted; Sharma, Ramesh

    2012-07-01

    The Energy and Environmental Research Center (EERC), in partnership with the U.S. Department of Energy (DOE) and Accelergy Corporation, an advanced fuels developer with technologies exclusively licensed from ExxonMobil, undertook Subtask 3.9 to design, build, and preliminarily operate a bench-scale direct coal liquefaction (DCL) system capable of converting 45 pounds/hour of pulverized, dried coal to a liquid suitable for upgrading to fuels and/or chemicals. Fabrication and installation of the DCL system and an accompanying distillation system for off-line fractionation of raw coal liquids into 1) a naphtha middle distillate stream for upgrading and 2) a recycle stream was completed in May 2012. Shakedown of the system was initiated in July 2012. In addition to completing fabrication of the DCL system, the project also produced a 500-milliliter sample of jet fuel derived in part from direct liquefaction of Illinois No. 6 coal, and submitted the sample to the Air Force Research Laboratory (AFRL) at Wright Patterson Air Force Base, Dayton, Ohio, for evaluation. The sample was confirmed by AFRL to be in compliance with all U.S. Air Force-prescribed alternative aviation fuel initial screening criteria.

  6. Direct use of methane in coal liquefaction

    DOEpatents

    Sundaram, Muthu S.; Steinberg, Meyer

    1987-01-01

    This invention relates to a process for converting solid carbonaceous material, such as coal, to liquid and gaseous hydrocarbons utilizing methane, generally at a residence time of about 20-120 minutes at a temperature of 250.degree.-750.degree. C., preferably 350.degree.-450.degree. C., pressurized up to 6000 psi, and preferably in the 1000-2500 psi range, preferably directly utilizing methane 50-100% by volume in a mix of methane and hydrogen. A hydrogen donor solvent or liquid vehicle such as tetralin, tetrahydroquinoline, piperidine, and pyrolidine may be used in a slurry mix where the solvent feed is 0-100% by weight of the coal or carbonaceous feed. Carbonaceous feed material can either be natural, such as coal, wood, oil shale, petroleum, tar sands, etc., or man-made residual oils, tars, and heavy hydrocarbon residues from other processing systems.

  7. Direct use of methane in coal liquefaction

    DOEpatents

    Sundaram, M.S.; Steinberg, M.

    1985-06-19

    This invention relates to a process for converting solid carbonaceous material, such as coal, to liquid and gaseous hydrocarbons utilizing methane, generally at a residence time of about 20 to 120 minutes at a temperature of 250 to 750/sup 0/C, preferably 350 to 450/sup 0/C, pressurized up to 6000 psi, and preferably in the 1000 to 2500 psi range, preferably directly utilizing methane 50 to 100% by volume in a mix of methane and hydrogen. A hydrogen donor solvent or liquid vehicle such as tetralin, tetrahydroquinoline, piperidine, and pyrolidine may be used in a slurry mix where the solvent feed is 0 to 100% by weight of the coal or carbonaceous feed. Carbonaceous feed material can either be natural, such as coal, wood, oil shale, petroleum, tar sands, etc., or man-made residual oils, tars, and heavy hydrocarbon residues from other processing systems. 1 fig.

  8. Exploratory Research on Novel Coal Liquefaction Concept

    SciTech Connect

    R. A. Winschel; S. D. Brandes

    1997-12-12

    Task 3 experimental tests were concluded this quarter. Second-stage testing of first-stage distilled filtrates and of a Wilsonville resid from Run 263 were completed. The first-stage filtrates were found to have higher reactivity than the Wilsonville material. Task 4 experimental testing was initiated. First-stage microautoclave tests were made at reduced catalyst loading and reduced solvent to coal ratio without negatively affecting coal conversion. Lower severity second-stage catalytic upgrading tests were begun. The single-pass resid conversion obtained in the first completed second-stage test was high (67-69 %).

  9. Cooperative research in coal liquefaction infratechnology and generic technology development: Final report, October 1, 1985 to December 31, 1986

    SciTech Connect

    Sendlein, L.V.A.

    1987-06-29

    During the first year of its research program, the Consortium for Fossil Fuel Liquefaction Science has made significant progress in many areas of coal liquefaction and coal structure research. Research topics for which substantial progress has been made include integrated coal structure and liquefaction studies, investigation of differential liquefaction processes, development and application of sophisticated techniques for structural analysis, computer analysis of multivariate data, biodesulfurization of coal, catalysis studies, co-processing of coal and crude oil, coal dissolution and extraction processes, coal depolymerization, determination of the liquefaction characteristics of many US coals for use in a liquefaction database, and completion of a retrospective technology assessment for direct coal liquefaction. These and related topics are discussed in considerably more detail in the remainder of this report. Individual projects are processed separately for the data base.

  10. Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama. Run 260 with Black Thunder Mine subbituminous coal: Technical progress report

    SciTech Connect

    Not Available

    1992-01-01

    This report presents the results of Run 260 performed at the Advanced Coal Liquefaction R&D Facility in Wilsonville. The run was started on July 17, 1990 and continued until November 14, 1990, operating in the Close-Coupled Integrated Two-Stage Liquefaction mode processing Black Thunder mine subbituminous coal (Wyodak-Anderson seam from Wyoming Powder River Basin). Both thermal/catalytic and catalytic/thermal tests were performed to determine the methods for reducing solids buildup in a subbituminous coal operation, and to improve product yields. A new, smaller interstage separator was tested to reduce solids buildup by increasing the slurry space velocity in the separator. In order to obtain improved coal and resid conversions (compared to Run 258) full-volume thermal reactor and 3/4-volume catalytic reactor were used. Shell 324 catalyst, 1/16 in. cylindrical extrudate, at a replacement rate of 3 lb/ton of MF coal was used in the catalytic stage. Iron oxide was used as slurry catalyst at a rate of 2 wt % MF coal throughout the run. (TNPS was the sulfiding agent.)

  11. Impact of hydrogen partial pressure on coal liquefaction. Final technical report

    SciTech Connect

    Kang, D.; Hoover, D.S.; Schweighardt, F.K.

    1984-06-01

    This program was conducted to determine the effects of hydrogen partial pressure on the SRC-I direct coal liquefaction process and SRC-I Demonstration Plant design. A native solvent was produced in quantity and slurried with Kentucky number 9 Mulford coal in a series of coal liquefaction runs under varying hydrogen gas rates, temperatures, residence times, and hydrogen partial pressures. The results showed that hydrogen partial pressure significantly affected product distribution; the magnitude of the effect was comparable to changes in temperature and residence time. Also, the impact of hydrogen partial pressure was enhanced by increases in both temperature and residence time. Operating at low hydrogen partial pressure did not show any apparent advantage; it reduced coal conversion, reduced oil yield, and had a detrimental effect on the yield distribution of other products. An increase in hydrogen partial pressure had the following effects: increased coal conversion; increased conversion of asphaltenes and preasphaltenes to lighter products; significantly increased the oil yield; increased light gas yields; decreased sulfur content in the SRC; increased hydrogen content of the recycle solvent; and increased hydrogen consumption. This study strongly suggests that further studies should be conducted to optimize the effects of hydrogen partial pressure on the process, both within and, preferably, beyond the constraints of the current basic SRC-I design, considering the major impact of this variable on the process. 10 references, 37 figures, 10 tables.

  12. Process of preparing a donor solvent for coal liquefaction

    SciTech Connect

    Ditman, J.G.; Ditman, R.D.

    1987-05-05

    A process is described for preparing a hydrogen donor solvent having a high concentration of higher molecular weight polycyclic aromatic and heterocyclic compounds suitable for use in coal liquefaction comprising: distilling liquefied coal to separate the coal into a fraction having a boiling point less than about 350/sup 0/F and a residue having a boiling point greater than about 350/sup 0/F; deasphalting the residue from the distillation in a first solvent capable of substantially extracting from the residue a high hydrogen to carbon ratio first oil comprising lower molecular weight compounds and saturated compounds; and deasphalting the residue from the first deasphalting step in a solvent capable of substantially extracting from the residue the donor solvent.

  13. The use of mixed pyrrhotite/pyrite catalysts for co-liquefaction of coal and waste rubber tires

    SciTech Connect

    Dadyburjor, D.B.; Zondlo, J.W.; Sharma, R.K.

    1995-12-31

    The overall objective of this research program is to determine the optimum processing conditions for tire/coal co-liquefaction. The catalysts used will be a ferric-sulfide-based materials, as well as promising catalysts from other consortium laboratories. The intent here is to achieve the maximum coal+tire conversion at the mildest conditions of temperature and pressure. Specific objectives include an investigation of the effects of time, temperature, pressure, catalyst and co-solvent on the conversion and product slate of the co-liquefaction. Accomplishments and conclusions are discussed.

  14. Power recovery system for coal liquefaction process

    DOEpatents

    Horton, Joel R.

    1985-01-01

    Method and apparatus for minimizing energy required to inject reactant such as coal-oil slurry into a reaction vessel, using high pressure effluent from the latter to displace the reactant from a containment vessel into the reaction vessel with assistance of low pressure pump. Effluent is degassed in the containment vessel, and a heel of the degassed effluent is maintained between incoming effluent and reactant in the containment vessel.

  15. Novel bimetallic dispersed catalysts for temperature-programmed coal liquefaction. Final report

    SciTech Connect

    Chunshan Song; Schobert, H.H.; Parfitt, D.P.

    1997-11-01

    Development of new catalysts is a promising approach to more efficient coal liquefaction. It has been recognized that dispersed catalysts are superior to supported catalysts for primary liquefaction of coals, because the control of initial coal dissolution or depolymerization requires intimate contact between the catalyst and coal. This research is a fundamental and exploratory study on catalytic coal liquefaction, with the emphasis on exploring novel bimetallic dispersed catalysts for coal liquefaction and the effectiveness of temperature-programmed liquefaction using dispersed catalysts. The primary objective of this research was to explore novel bimetallic dispersed catalysts from organometallic molecular precursors, that could be used in low concentrations but exhibit relatively high activity for efficient hydroliquefaction of coals under temperature-programmed conditions. We have synthesized and tested various catalyst precursors in liquefaction of subbituminous and bituminous coals and in model compound studies to examine how do the composition and structure of the catalytic precursors affect their effectiveness for coal liquefaction under different reaction conditions, and how do these factors affect their catalytic functions for hydrogenation of polyaromatic hydrocarbons, for cleavage of C-C bonds in polycyclic systems such as 4-(1-naphthylmethyl)bibenzyl, for hydrogenolysis of C-O bond such as that in dinaphthylether, for hydrodeoxygenation of phenolic compounds and other oxygen-containing compounds such as xanthene, and for hydrodesulfurization of polycyclic sulfur compounds such as dibenzothiophene. The novel bimetallic and monometallic precursors synthesized and tested in this project include various Mo- and Fe-based compounds.

  16. Short contact time direct coal liquefaction using a novel batch reactor. Quarterly progress report, January 1--May 15, 1995

    SciTech Connect

    Klein, M.T.; Calkins, W.H.

    1995-05-31

    The objective of this research is to optimize the design and operation of the bench scale batch reactor for coal liquefaction at short contact times (0.01 to 10 minutes or longer). Additional objectives are to study the kinetics of direct coal liquefaction particularly at short reaction times, and to investigate the role of the organic oxygen components of coal and their reaction pathways during liquefaction. Experimental progress is reported for uncatalyzed liquefactions, catalyzed liquefactions, liquefaction in the presence of solvents other than tetralin, and kinetics of gas formation during coal liquefaction. Analytical methods were developed for the determination of the boiling range of coal liquids by thermogravimetric analysis and the determination of phenolic hydroxyl in coal, coal liquids, and coal residues.

  17. Short contact time direct coal liquefaction using a novel batch reactor. Quarterly report, 1996

    SciTech Connect

    Klein, M.T.; Calkins, W.H.; Huang, H.

    1996-05-01

    The objective of this research is to optimize the design and operation of the bench scale batch reactor (SCTBR) for coal liquefaction at short contact times (0.01 to 10 minutes or longer). Additional objectives are to study the kinetics of direct coal liquefaction particularly at short reaction times, and to investigate the role of the organic oxygen components of coal and their reaction pathways during liquefaction. Many of those objectives have already been achieved and others are still in progress. This quarterly report covers further progress toward those objectives. Much of the previous quarterly report was concerned mainly in the retrograde reactions occurring during the liquefaction process. This report is largely devoted to the kinetics and mechanisms of the liquefaction process itself and the influence of the liquefaction solvents.

  18. Effects of the components of coal hydro-liquefaction residue on its rheological characteristics

    SciTech Connect

    Ren, Y.; Jin, S.; Xu, Y.; Wei, A.; Zhang, D.; Gao, J.

    2009-07-01

    Four kinds of typical coal liquefaction residue samples, coming from Shenhua coal liquefaction pilot plant, were used to investigate the effects of components of residue, separation time, and temperature on its rheological characteristics. Coal liquefaction residue is a non-Newtonian pseudoplastic fluid whose apparent viscosity decreases with increasing shear rate. Moreover, the residue has high viscosity at the initial softening temperature, and its viscosity drops greatly with increasing temperature. The oil content in residue has a great effect on the decline of the apparent viscosity of residue. The asphaltene can increase the apparent viscosity at lower temperatures but decrease it at higher temperatures. However, the solid only increases the apparent viscosity as it can be neither softened nor dissolved to become fluid. After simulating the separation condition, it is found that prolonging the separation time and enhancing the separation temperature will increase the apparent viscosity of residue, which is bad for preventing pipes from being blocked. So choosing the right separation time and separation temperature is necessary to actual industrial production.

  19. Microbial liquefaction of peat for the production of synthetic fuels

    SciTech Connect

    Gunasekaran, M.

    1988-01-01

    Objectives of this study were: to evaluate the potential of using various microorganisms to hydrolyse and liquify peat; to determine the optimal conditions for peat hydrolysis and liquefaction; to study the co-metabolizable substances; to separate the compounds present in liquified peat by alumina and silica acid chromatography and capillary gas chromatography; and to identify the compounds in liquified peat by capillary GC-Mass spectrometry. Organisms used in the study include: Coprinus comatus, Coriolus hirsutus, Ganoderma lucidum, Lentinus edodes, Lenzites trabea, Phanerochaete chrysosporium, Pleurotus ostreatus, P. sapidus, Polyporus adjustus, Neurospora sitophila, Rhizophus arrhizus, Bacillus subtilis, Acinetobacter sp. and Alcaligenes sp. The fungi were maintained and cultivated in potato dextrose agar at 30 C. The bacteria were maintained in nutrient agar at 30 C. We have also initiated work on coal solubilization in addition to the studies on peat liquefaction. A relatively new substratum or semi-solid base for culture media called Pluronic F-127, or Polyol (BASF, New Jersey). Objectives of this study were: (1) to study the growth patterns of Candida ML 13 on pluronic as substratum; (2) to determine the rate of microbial coal solubilization on pluronic F-127 amended in different growth media; (3) to separate the mycelial mat of Candida ML 13 from unsolubilized coal particles and solubilized coal products from pluronic F-127; (4) to determine the effects of pH on microbial coal solubilization in pluronic F-127 media; (5) the effect of concentration of pluronic F-127 in media on coal solubilization; and, (6) to study the role of extracellular factors secreted by Candida ML 13 on coal solubilization in pluronic F-127 media. Results are discussed. 4 refs.

  20. Synthesis of model compounds for coal liquefaction research

    SciTech Connect

    Not Available

    1991-11-01

    Coal liquefaction investigations required the availability of model compounds for mechanistic investigations. Towards this end, IITRI was funded to develop an approach for the synthesis of one of the target compound. This study was carried out in several phases as outlined here. Initial synthetic investigations on obtaining 2-tetrolol was carried out using high pressure and temperature reduction with Raney nickel catalyst. The next step consisted in incorporation of a hydroxymethyelene group at the C-3 position. This was successfully carried out utilizing 2-tetrolol, formaldehyde, and calcium oxide. An alternate improved method was developed using 3-carboxyl-2-naphthol. This required less time, gave a cheer product in higher yield. Efforts at the introduction of a chloromethylene group only yielded polymeric material or starting material in spite of protection the phenolic group by various groups. They synthesis of 3, 5-dimethyl-6- bromobenzyl chloride was successfully carried out by performing the Blank reaction of 2, 4-dimethyl bromobenzene. The product was characterized by GC/MS. Purification was not possible, as it was a complex mixture. Efforts at converting it to the acetate followed by separation to was not feasible. Unlike in the case of 2- hydroxyteralol, hydroxymetylation by established procedure yielded only the starting materials. Commercially available 4-methoxy-1- maphthaldehyde was protected as the ethylene acetal. The Wittig reagent 3-chlorobenzyl phosphonium bromide was prepared and condensed with 4-methoxy-1-napthaldehyde successfully and proved that the overall synthetic approach was proceeding in the desired direction. All the necessary intermediates have been synthesized,and we have demonstrated using model compounds, that the synthetic objective can be attained.

  1. Indirect liquefaction of coal. [Coal gasification plus Fischer-Tropsch, methanol or Mobil M-gasoline process

    SciTech Connect

    1980-06-30

    The most important potential environmental problems uniquely associated with indirect liquefaction appear to be related to the protection of occupational personnel from the toxic and carcinogenic properties of process and waste stream constituents, the potential public health risks from process products, by-products and emissions and the management of potentially hazardous solid wastes. The seriousness of these potential problems is related partially to the severity of potential effects (i.e., human mortality and morbidity), but even more to the uncertainty regarding: (1) the probable chemical characteristics and quantities of process and waste streams; and (2) the effectiveness and efficiencies of control technologies not yet tested on a commercial scale. Based upon current information, it is highly improbable that these potential problems will actually be manifested or pose serious constraints to the development of indirect liquefaction technologies, although their potential severity warrants continued research and evaluation. The siting of indirect liquefaction facilities may be significantly affected by existing federal, state and local regulatory requirements. The possibility of future changes in environmental regulations also represents an area of uncertainty that may develop into constraints for the deployment of indirect liquefaction processes. Out of 20 environmental issues identified as likely candidates for future regulatory action, 13 were reported to have the potential to impact significantly the commercialization of coal synfuel technologies. These issues are listed.

  2. Surface Modified Coals for Enhanced Catalyst Dispersion and Liquefaction

    SciTech Connect

    Yaw D. Yeboah

    1998-12-04

    The aim of this study is to enhance catalyst loading and dispersion in coal for improved liquefaction by preadsorption of surfactants and catalysts on to the coal. During this reporting period, the effects of dodecyl dimethyl ethyl ammonium bromide (DDAB) (a cationic surfactant), sodium dodecyl sulfate (SDS) (an anionic surfactant), Triton X-100 (a neutral surfactant), and ferrous sulfate (as a catalyst precursor) on the coal surface charge at various pH values were determined. The results of the zeta potential measurements suggest that ferrous sulfate as catalyst precursor creates a distinctly different condition on the coal surface compared to that of molybdenum as reported in the previous progress reports. The effects of the adsorption of the surfactants also varied distinctly with the type of surfactant. With the adsorption of DDAB, the cationic surfactant, the surface charge was more positive. The opposite effect was observed for the SDS, the anionic surfactant. The coals treated with Triton X-100, the neutral surfactant, also showed an overall negative surface charge density. The adsorption of the catalyst precursor (ferrous sulfate) resulted in a net negative charge on the coal surface.

  3. Advanced coal liquefaction research. Quarterly technical progress report, January 1-March 31, 1983

    SciTech Connect

    Not Available

    1983-12-01

    This report describes progress on the Advanced Coal Liquefaction project by the Gulf Research and Development Company's Merriam Laboratory during the months of January through March 1983. The liquefaction behavior of Illinois No. 6 coal beneficiated in various ways was studied in both single-stage recycle (SRC II) and short contact time (SCT) modes of operation. The distillate yield increased as the iron level in the feed slurry increased in both modes of operation. In the SCT mode, the conversion increased at greater depths of cleaning. In the SRC II mode, the distillate yield and conversion were much higher with deep cleaning and add-back of pyrite than with conventional cleaning. Pyrite addition resulted in a significant increase in short contact time conversion of subbituminous Belle Ayr coal in both high and low quality solvents. Solvent quality itself, however, had little effect on conversion. With Loveridge coal, the hydrocarbon gas yield and conversion decreased as the residence time was reduced in the range of 3 to 8 minutes. The bottoms product was filterable only at residence times of 6 minutes or greater. Addition of a small amount of nickel to a molybdenum emulsion catalyst improved yields slightly with Belle Ayr coal in the SRC II mode. Higher levels of nickel resulted in the same oil yield as with none at all.

  4. Studies of the effect of selected nondonor solvents on coal liquefaction yields

    SciTech Connect

    Jolley, R. L.; Rodgers, B. R.; Benjamin, B. M.; Poutsma, M. L.; Douglas, E. C.; McWhirter, D. A.

    1983-09-01

    The objective of this research program was to evaluate the effectiveness of selected nondonor solvents (i.e., solvents that are not generally considered to have hydrogen available for hydrogenolysis reactions) for the solubilization of coals. Principal criteria for selection of candidate solvents were that the compound should be representative of a major chemical class, should be present in reasonable concentration in coal liquid products, and should have the potential to participate in hydrogen redistribution reactions. Naphthalene, phenanthrene, pyrene, carbazole, phenanthridine, quinoline, 1-naphthol, and diphenyl ether were evaluated to determine their effect on coal liquefaction yields and were compared with phenol and two high-quality process solvents, Wilsonville SRC-I recycle solvent and Lummus ITSL heavy oil solvent. The high conversion efficacy of 1-naphthol may be attributed to its condensation to binaphthol and the consequent availability of hydrogen. The effectiveness of both the nitrogen heterocycles and the polycyclic aromatic hydrocarbon (PAH) compounds may be due to their polycyclic aromatic nature (i.e., possible hydrogen shuttling or transfer agents) and their physical solvent properties. The relative effectiveness for coal conversion of the Lummus ITSL heavy oil solvent as compared with the Wilsonville SRC-I process solvent may be attributed to the much higher concentration of 3-, 4-, and 5-ring PAH and hydroaromatic constituents in Lummus solvent. The chemistry of coal liquefaction and the development of recycle, hydrogen donor, and nondonor solvents are reviewed. The experimental methodology for tubing-bomb tests is outlined, and experimental problem areas are discussed.

  5. Coal liquefaction process streams characterization and evaluation. Quarterly technical progress report, October 1--December 31, 1992

    SciTech Connect

    Brandes, S.D.; Winschel, R.A.; Burke, F.P.; Robbins, G.A.

    1993-10-01

    The Research and Development Department of CONSOL Inc. is conducted a program to characterize process and product streams from direct coal liquefaction process development projects sponsored by the Department of Energy. In this program, CONSOL obtains samples from current process development activities in coal liquefaction and coal-oil coprocessing, and characterizes them using established analytical techniques. In addition, selected samples are characterized by other analytical techniques to evaluate their potential for aiding process development. These analyses and interpretation of the results in relation to process operations are provided by the subcontractor. Major topics reported in this thirteenth quarterly report are the following: (1) Analyses were performed on three coals and eleven process oils from HRI, Inc. process development unit Run 260--03, which was the first process development unit test of Black Thunder Mine subbituminous coal, significant operating problems were encountered, and sample properties are discussed in context to the operational problems; (2) a summary of the status of the Participants Program is given; (3) summaries of the final reports produced by the University of Chicago, the University of Utah, Iowa State University, and the University of Kentucky under the Participants Program, are presented.

  6. Novel bimetallic dispersed catalysts for temperature-programmed coal liquefaction

    SciTech Connect

    Chunshan, Song; Kirby, S.; Schmidt, E.

    1995-12-31

    The objective of this project is to explore bimetallic dispersed catalysts for more efficient coal liquefaction. Coal liquefaction involves cleavage of methylene, dimethylene and ether bridges connecting various aromatic units and the reactions of various oxygen functional groups. This paper describes recent results on (1) hydrodeoxygenation of O-containing polycyclic model compounds using novel organometallic catalyst precursors; and (2) activity and selectivity of dispersed Fe catalysts from organometallic and inorganic precursors for hydrocracking of 4-(1-naphthylmethyl) bibenzyl. The results showed that some iron containing catalysts have higher activity in the sulfur-free form, contrary to conventional wisdom. Adding sulfur to Fe precursors with Cp-ligands decreased the activity of the resulting catalyst. This is in distinct contrast to the cases with iron pentacarbonyl and superfine Fe{sub 2}O{sub 3}, where S addition increased their catalytic activity substantially. A positive correlation between sulfur addition and increased activity can be seen, but a reversed trend between Fe cluster size and hydrocracking conversion could be observed, for carbonyl-type Fe precursors. It is apparent that the activity and selectivity of Fe catalysts for NMBB conversion depends strongly on both the type of ligand environment, the oxidation state and the number of intermetal bonds in the molecular precursor.

  7. Effects of coal beneficiation and solvent quality on short contact time liquefaction of bituminous coal

    SciTech Connect

    Not Available

    1984-07-01

    A series of beneficiated coals (Illinois No. 6) from the Burning Star Mine No. 2 were evaluated in a bench scale continuous coal liquefaction unit. These included run-of-mine (22% ash), coal conventionally cleaned at the mine site preparation plant (11% ash), coal cleaned by oil agglomeration (10% ash), and deep-cleaned coal (3% ash). The oil agglomeration technique was of particular interest as it was known to preferentially leave pyrite in the cleaned coal. In short contact time liquefaction, the primary measure of reactivity is conversion to soluble material. In this study, it was found that conversion to soluble material was not correlated with iron content but rather was related to depth of cleaning. The two highest iron content coals, the run-of-mine and oil-agglomerated, exhibited the lowest conversions. Conversion was maximized with the deep-cleaned coal which had the lowest iron content. The oil-agglomerated and conventionally-cleaned coal were of similar ash content; the conventionally-cleaned coal contained less iron but showed an increased conversion compared to the oil-agglomerated coal. In contract to the conversion results, there was a strong correlation between iron in the feed coal and distillate yield. For two-stage processing, quality of the SRC is also of importance. Conversion of preasphaltenes to more soluble materials was maximized with the high iron coals and was minimized with the deep-cleaned coal. More favorable results were obtained with the Lummus solvent but differences between the two solvents were small. 27 references, 4 figures, 6 tables.

  8. Advanced coal liquefaction research. Technical progress report, January 1, 1983-December 31, 1983

    SciTech Connect

    Not Available

    1984-05-01

    The most significant work this year involved two methods of improving product quality which advanced the SRC II process far beyond that envisioned for the original demonstration plant. With both bituminous and subbituminous feedstocks, all distillate product boiling above 345/sup 0/C (653/sup 0/F) was recycled to extinction without loss of total oil yield or significant increase in hydrogen consumption. In a further refinement, all of the overhead from the high temperature, high pressure separator was passed through a vapor-phase hydrotreater. This resulted in a dramatic improvement in product quality. A proportional blend of distillate product contained less than 1 ppM of nitrogen. Total oil yield was similar to the low quality product produced in the conventional SRC II process. A large number of multiple-stage liquefaction experiments were carried out to better understand each step in the process. These included 3-stage operations; dissolution, hydrogenation and hydrocracking; and several variations of 2-stage processes. Variables investigated were temperature and residence time in each stage and both slurry and fixed-bed catalyst systems. The effect of residence time on conversion in single pass experiments was found to be quite different for the subbituminous Belle Ayr Mine and bituminous Illinois No. 6 coals studied. With bituminous coal, conversion to soluble material was quite high and the limit of conversion was approached in only a few minutes. With a subbituminous coal, however, conversion was much lower and the limit of conversion was approached much more slowly. In other work, the liquefaction of Illinois No. 6 coal beneficiated in various ways was studied in both SRC II and short contact time modes of operation. Additional short contact time experiments explored the effects of solvent quality and catalysts with Belle Ayr coal and the effects of residence time with Loveridge coal. 32 figures, 8 tables.

  9. Catalytic coal liquefaction with treated solvent and SRC recycle

    DOEpatents

    Garg, D.; Givens, E.N.; Schweighardt, F.K.

    1986-12-09

    A process is described for the solvent refining of coal to distillable, pentane soluble products using a dephenolated and denitrogenated recycle solvent and a recycled, pentane-insoluble, solvent-refined coal material, which process provides enhanced oil-make in the conversion of coal. 2 figs.

  10. Catalytic coal liquefaction with treated solvent and SRC recycle

    DOEpatents

    Garg, Diwakar; Givens, Edwin N.; Schweighardt, Frank K.

    1986-01-01

    A process for the solvent refining of coal to distillable, pentane soluble products using a dephenolated and denitrogenated recycle solvent and a recycled, pentane-insoluble, solvent-refined coal material, which process provides enhanced oil-make in the conversion of coal.

  11. Catalytic two-stage coal liquefaction process having improved nitrogen removal

    DOEpatents

    Comolli, Alfred G.

    1991-01-01

    A process for catalytic multi-stage hydrogenation and liquefaction of coal to produce high yields of low-boiling hydrocarbon liquids containing low concentrations of nitogen compounds. First stage catalytic reaction conditions are 700.degree.-800.degree. F. temperature, 1500-3500 psig hydrogen partial pressure, with the space velocity maintained in a critical range of 10-40 lb coal/hr ft.sup.3 catalyst settled volume. The first stage catalyst has 0.3-1.2 cc/gm total pore volume with at least 25% of the pore volume in pores having diameters of 200-2000 Angstroms. Second stage reaction conditions are 760.degree.-870.degree. F. temperature with space velocity exceeding that in the first stage reactor, so as to achieve increased hydrogenation yield of low-boiling hydrocarbon liquid products having at least 75% removal of nitrogen compounds from the coal-derived liquid products.

  12. Direct liquefaction of low-rank coal. Quarterly technical progress report, January 1--March 31, 1995

    SciTech Connect

    Hetland, M.D.

    1995-04-01

    A multistep direct liquefaction process specifically aimed at low-rank coals (LRCs) has been developed at the Energy & Environmental Research Center (EERC). The process consists of a preconversion treatment to prepare the coal for solubilization, solubilization of the coal in the solvent, and polishing using a phenolic solvent or solvent blend to complete solubilization of the remaining material. The product of these three steps can then be upgraded during a traditional hydrogenation step. This project addresses two research questions necessary for the further development and scaleup of this process: (1) determination of the recyclability of the solvent used during solubilization and (2) determination of the minimum severity required for effective hydrotreatment of the liquid product. The project involves two tasks, the first consisting of ten recycle tests and the second consisting of twelve hydrotreatment tests performed at various conditions. Activities performed during this quarter are discussed.

  13. A characterization and evaluation of coal liquefaction process streams. The kinetics of coal liquefaction distillation resid conversion

    SciTech Connect

    Klein, M.T.; Calkins, W.H.; Huang, H.; Wang, S.; Campbell, D.

    1998-03-01

    Under subcontract from CONSOL Inc., the University of Delaware studied the mechanism and kinetics of coal liquefaction resid conversion. The program at Delaware was conducted between August 15, 1994, and April 30, 1997. It consisted of two primary tasks. The first task was to develop an empirical test to measure the reactivity toward hydrocracking of coal-derived distillation resids. The second task was to formulate a computer model to represent the structure of the resids and a kinetic and mechanistic model of resid reactivity based on the structural representations. An introduction and Summary of the project authored by CONSOL and a report of the program findings authored by the University of Delaware researchers are presented here.

  14. Advanced liquefaction using coal swelling and catalyst dispersion techniques. Quarterly technical progress report, January--March 1993

    SciTech Connect

    Curtis, C.W.; Gutterman, C.; Chander, S.

    1993-09-01

    The overall objective of this project is to develop a new approach for the direct liquefaction of coal to produce an all-distillate product slate at a sizable cost reduction over current technology. The approach integrates coal selection, pretreatment, coal swelling with catalyst impregnation, liquefaction, product recovery with characterization, alternate bottoms processing, and carrying out a technical assessment including an economic evaluation. The primary coal of this program, Black Thunder subbituminous coal, can be effectively beneficiated to about 4 wt% ash using aqueous sulfurous acid pretreatment. This treated coal can be further beneficiated to about 2 wt% ash using commercially available procedures. All three coals used in this study (Black Thunder, Burning Star bituminous, and Martin Lake lignite) are effectively swelled by a number of solvents. The most effective solvents are those having hetero-functionality. In addition, a synergistic effect has been demonstrated, in which solvent blends are more effective for coal swelling than the pure solvents alone. Therefore, it will be necessary to use only low levels of swelling agents and yet promote the impregnation of catalyst precursors. The rate of the impregnation of catalyst precursors into swollen coal increases greatly as the effectiveness of the solvent to swell the coal increases.

  15. Combustion of two-stage coal liquefaction residues in a hybrid boiler. Final report. [High ash liquefaction residues

    SciTech Connect

    Patel, R.L.; Griffith, B.F.

    1986-10-01

    A bench- and pilot-scale study has been performed on high ash liquefaction residues (ash concentrates). These residues were prepared beforehand in Wilsonville, Alabama, 6-ton/day test facility, from Illinois No. 6 Burning Star high volatile bituminous and Wyodak (Wyoming-Dakotals) subbituminous coals. A detailed characterization of both residues was conducted using standard ASTM and special in-house techniques. The Drop Tube Furnace System (DTFS) was used to determine the combustion characteristics of both liquefaction residues as well as the combustion kinetics of a closely size-graded Illinois No. 6 residue char. The pilot-scale Fireside Performance Test Facility (FPTF) was used to determine the slagging and fouling characteristics of the Illinois No. 6 liquefaction residue at 2.3 MBtu/hr and temperature and time conditions simulating utility pulverized coal fired boilers. The kinetic information was subsequently used in conjunction with a C-E's proprietary mathematical model to predict the combustion performance of the Illinois No. 6 liquefaction residue in a conceptual hybrid boiler designed for Illinois No. 6 Exxon Donor Solvent (EDS) residue. Liquefaction residue results indicated carbon heat losses ranging up to 2 times those predicted for Illinois No. 6 EDS residue. They, nevertheless, indicated that the liquefaction residue can be successfully burned in a correctly designed and correctly operated hybrid boiler. Pilot-scale FPTF study indicated high to severe lower furnace slagging potential for the Illinois No. 6 liquefaction residue at temperatures above the 2625 to 2650/sup 0/F range. The convection pass fouling potential was low to medium. The fly ash erosion potential was found to be high. Bench-scale results also indicated severe slagging potential and moderate to high fouling potential for the Wyodak liquefaction residue. 25 refs., 32 figs., 22 tabs.

  16. Fine particle clay catalysts for coal liquefaction. Quarterly technical progress report, November 9, 1992--February 8, 1993

    SciTech Connect

    Olson, E.S.

    1995-10-01

    The mixed iron/alumina pillared clay catalysts and clay-supported iron catalysts have been shown in previous reports of this project to significantly improve yields of heptane-soluble products obtained in the liquefaction of both as received and acid-exchanged Wyodak subbituminous coal and Blind Canyon bituminous coal. In this quarter, the soluble product (LSW) obtained from the noncatalytic low-severity liquefaction of Wyodak coal was used as a feed to determine the activity of iron based catalysts for the hydrogenation and depolymerization steps. Comparison data for liquefaction of the soluble LSW with other catalysts were desired, and these data were obtained for a dispersed form of iron sulfide, prepared via iron hydroxyoxide (PETC method). The iron oxyhydroxide catalyst was directly precipitated on LSW product using either water or ethanol as the solvent. An insight into the functioning of the mixed iron/alumina pillared clay in coal liquefaction was investigated by preparing and studying an iron oxoaluminate structure. An investigation of new methods for the production of tetralin soluble iron oxometallate catalysts and the determination of their catalytic activities was continued in this quarter. The hydrogenation activity of iron oxoaluminate was investigated using pyrene and 1-methylnaphthalene as the test compounds, and results were compared with thermal reactions. In order to determine the loss of activity, recovered catalyst was recycled a second time for the hydrotreating of pyrene. Reaction of 1-methylnaphthalene with iron oxoaluminate also gave very high conversion to 1- and 5-methyltetralins and small amount of 2- and 6-methyltetralins. Liquefaction of Wyodak subbituminous and Blind Canyon bituminous coal was investigated using an in situ sulfided soluble iron oxoaluminate catalyst.

  17. Power recovery system for coal liquefaction process

    DOEpatents

    Horton, Joel R.; Eissenberg, David M.

    1985-01-01

    A flow work exchanger for use in feeding a reactant material to a high-pressure reactor vessel comprises an outer shell, an inner shell concentrically disposed within said outer shell, means for conducting said reactant into the lower end of said lower shell and then to said reactor vessel, and means for conducting a hotter product effluent from said reactor vessel into the upper end of said inner shell and out of the annulus between said inner and outer shells.

  18. Power recovery system for coal liquefaction process

    DOEpatents

    Horton, J.R.; Eissenberg, D.M.

    A flow work exchanger for use in feeding a reactant material to a high-pressure reactor vessel comprises an outer shell, an inner shell concentrically disposed within said outer shell, means for conducting said reactant into the lower end of said lower shell and thence to said reactor vessel, and means for conducting a hotter product effluent from said reactor vessel into the upper end of said inner shell and out of the annulus between said inner and outer shells.

  19. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction

    SciTech Connect

    Song, C.; Saini, A.K.; Huang, L.; Wenzel, K.; Hou, L.; Hatcher, P.G.; Schobert, H.H.

    1992-08-01

    Low-temperature catalytic pretreatment is a promising approach to the development of an improved liquefaction process- This work is a fundamental study on effects of pretreatments on coal structure and reactivity in liquefaction. The main objectives of this project are to study the coal structural changes induced by low-temperature catalytic and thermal pretreatments by using spectroscopic techniques; and to clarify the pretreatment-induced changes in reactivity or convertibility of coals in the subsequent liquefaction. This report describes the recent progress of our work. Substantial progress has been made in the spectroscopic characterization of structure and pretreatment-liquefaction reactions of a Montana subbituminous Coal (DECS-9), and thermochemical analysis of three mw and reacted bituminous coals. Temperature programmed liquefaction has been performed on three low-rank coals both in the presence and absence of dispersed molybdenum sulfide catalyst. We also performed a detailed study of the effects of mild thermal pretreatment -- drying in air and in vacuum -- on thermal and catalytic liquefaction of a Wyodak subbituminous coal. Important information on structure and structure transformation during thermal pretreatment and liquefaction reactions of low-rank coals has been derived by applying solid-state CPMAS [sup 13]C NMR and flash pyrolysis-GC-MS (Py-GC-MS) for characterization of the macromolecular network of a Montana subbituminous coal and its residues from temperature-programmed and nonprogrammed liquefaction (TPL and N-PL) at final temperatures ranging from 300 to 425[degree]C in H-donor and non-donor solvents. The results revealed that this coal contains significant quantities of oxygen-bearing structures, corresponding to about 18 O-bound C per 100 C atoms and one O-bound C per every 5 to 6 aromatic C.

  20. Two-stage, close coupled catalytic liquefaction of coal

    SciTech Connect

    Comolli, A.G.; Johanson, E.S.; Panvelker, S.V.; Popper, G.A.; Smith, T.O.

    1990-09-01

    During the first quarter of 1990, work was carried out in the microautoclave, microreactor, and Bench-Scale units. An economics analysis on sub-bituminous coal processing at two space velocities was also completed. Several supported catalysts and a sample of iron oxide were screened in the microautoclave unsulfided and sulfided with DMDS and TNPS. A second shipment of Black Thunder coal from Wilsonville, oil agglomerated cleaned Illinois {number sign}6 coal from Homer City, OTISCA cleaned coal a New Mexico coal were evaluated for relative conversions with and without catalyst. Results of Bench-Scale developments with cleaned, oil agglomerated, Illinois {number sign}6 coal from Homer City(CC-6), Dispersed Catalyst/Supported Catalyst Two-Stage and reversed sequential operation (CC-7), on Black Thunder Coal (CC-7), and preliminary observations on OTISCA cleaned coal are presented. The oil agglomerated cleaned coal gave higher conversion and distillate production than the OTISCA cleaned coal. The Dispersed/Supported Two-Stage operation yielded higher gas production than the reverse sequence but also showed the higher coal conversion. Economic analysis of sub-bituminous coal processing at two space velocities showed a 3% higher return on investment with a 50% increase in space velocity. 13 tabs.

  1. A characterization and evaluation of coal liquefaction process streams. Status assessment

    SciTech Connect

    Brandes, S.D.

    1995-07-01

    A review of the literature dealing with the modeling of fossil-fuel resid conversion to product oils and an updated assessment of the physico-chemical analytical methodology applicable to coal-liquefaction product streams is presented in this document. Analytical methodologies included here are either those which are different than those previously surveyed or are improvements on, or significantly different applications of methods previously surveyed. The literature cited spans the time period from 1991 to the present. The literature was examined from the 1960s through the present. When possible, for each model described, the methodology for deriving the model and the relative quality of the kinetic parameters derived is discussed. Proposed reaction schemes used for constructing coal-conversion models, in many cases, include the conversion of a resid intermediate to light products. These models are, therefore, also of interest, and are included here. Analytical techniques were identified that were shown to be useful for providing physico-chemical information of coal-liquefaction resids. These techniques are nuclear magnetic resonance spectroscopy, mass spectrometry (especially the technique of field ionization mass spectrometry), electron spin resonance spectroscopy coupled to thermogravimetric analysis, and a suite of petroleum inspection tests. It is recommended that these techniques be used in the present contract. 76 refs.

  2. Advanced coal liquefaction. Final project report

    SciTech Connect

    1996-12-02

    Molecular level liquid phase separation was explored using modified microporous ceramic membranes with pore size reduced from 40{Angstrom} via chemical vapor deposition. At room temperature, membranes with pore sizes <30{Angstrom} were sufficient to achieve >97% rejection of naphthyl-bibenzyl-methane (NBBM) in toluene, likely attributed to the hindrance effect of NBBM through the porous avenue of the membrane. The rejection diminished dramatically as the temperature was increased. The permeance of the mixture was substantially lower than that of the solvent resulted from the interference by the solute through the transport avenue. Also, it was found that the rejection increases along with the transmembrane pressure increase, probably attributed to the pore size distribution of the membrane. The smaller pore sizes become accessible to the solvent while rejecting the solute at the higher pressure. In addition to size-based separation, active transport of molecules through an appropriate pore size at 300-400{degrees}C was observed, as a result of interaction with the surface. Decomposition of NBBM took place at 400{degrees}C in a modified membrane packed with the catalyst synthesized using the similar protocol as membranes. The separation property of this membrane at 400{degrees}C was analyzed indirectly based upon the reaction product distribution.

  3. Characteristics of process oils from HTI coal/plastics co-liquefaction runs

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.

    1995-12-31

    The objective of this project is to provide timely analytical support to DOE`s liquefaction development effort. Specific objectives of the work reported here are presented. During a few operating periods of Run POC-2, HTI co-liquefied mixed plastics with coal, and tire rubber with coal. Although steady-state operation was not achieved during these brief tests periods, the results indicated that a liquefaction plant could operate with these waste materials as feedstocks. CONSOL analyzed 65 process stream samples from coal-only and coal/waste portions of the run. Some results obtained from characterization of samples from Run POC-2 coal/plastics operation are presented.

  4. Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry of coal liquids produced during a coal liquefaction process

    SciTech Connect

    Jacqui F. Hamilton; Alistair. C. Lewis; Marcos Millan; Keith D. Bartle; Alan A. Herod; Rafael Kandiyoti

    2007-01-15

    Comprehensive two-dimensional gas chromatography (GC) coupled to time-of-flight mass spectrometry (MS) has been applied to the analysis of coal-derived liquids from the former British Coal Point-of-Ayr coal liquefaction plant. The feed to the hydrocracker and the resulting product were analyzed. The results refer almost exclusively to the plant-derived recycle solvent, known as the liquefaction solvent; the molecular mass range of the GC does not exceed that of the solvent. The method allows for the resolution of the numerous structural isomers of tetralin and methyl indan, one pair of hydrogen-donor (necessary for the dissolution of coal) and isomeric nondonor (that reduce the hydrogen donors) components of the recycle solvent. In addition, the n-alkanes that concentrate in the recycle solvent are easily observed in comparison with the results from one-dimensional GC-MS. 24 refs., 6 figs., 1 tab.

  5. Fine particle clay catalysts for coal liquefaction. Quarterly technical progress report, February 9, 1993--May 8, 1993

    SciTech Connect

    Olson, E.S.

    1995-10-01

    An investigation of new methods for the production and utilization of tetralin-soluble iron oxometallate precursors for coal liquefaction catalysts was continued in this quarter. Further descriptions of the catalytic activities of the sulfided forms were obtained. The hydrogenation activities of catalysts derived from iron oxotitanate and cobalt oxoaluminate were investigated using pyrene as a the test compound, and results were compared with thermal reactions. The hydrogenation activity of iron oxotitanate was superior to other catalysts including iron oxoaluminate. The hydrogenation activity of cobalt oxoaluminate was similar to that of iron oxoaluminate reported in previous quarterly report. The liquefaction of Wyodak subbituminous coal was investigated using in situ sulfided iron oxotitanate catalyst. In order to improve the usefulness of iron oxoaluminate as a liquefaction catalyst, iron oxoaluminate was supported on acid-treated montmorillonite (K-10). Supporting the iron oxoaluminate on an acidic support significantly improved the hydrogenation activity of iron oxoaluminate. The hydrocracking activity was increased by a large factor. Thus the aluminate and titanate structures surrounding the pyrrhotite that forms during sulfidation have a beneficial effect in preventing deactivation of the iron sites, and the presence of the acidic sites in the clay results in effective catalytic synergism between catalyst and support. These clay-supported iron oxometallates are highly promising catalysts for coal liquefaction. Iron oxyhydroxide and triiron supported on acid-treated montmorillonite (K-10) were tested for the liquefaction of ion-exchanged Wyodak (IEW) to minimize effects of the coal mineral matter. Both sulfided catalysts gave very high conversions of coal to THF-soluble and heptane-soluble (oils) products.

  6. Applied research and evaluation of process concepts for liquefaction and gasification of western coals. Final report

    SciTech Connect

    Wiser, W. H.

    1980-09-01

    Fourteen sections, including five subsections, of the final report covering work done between June 1, 1975 to July 31, 1980 on research programs in coal gasification and liquefaction have been entered individually into EDB and ERA. (LTN)

  7. Results of u-bend stress-corrosion-cracking specimen exposures in coal-liquefaction pilot plants

    SciTech Connect

    Baylor, V.B.; Keiser, J.R.; Allen, M.D.; Howell, M.; Newsome, J.F.

    1982-04-01

    Pilot plants with capacities of up to 600 tons/d are currently demonstrating the engineering feasibility of several coal liquefaction processes including Solvent Refined Coal (SRC), Exxon Donor Solvent (EDS), and H-Coal. These plants are the first step toward commercial production of synthetic fuels. Among other factors, development of the technology depends on reliable materials performance. A concern is the application of those austenitic stainless steels necessary for general corrosion resistance, because they are susceptible to stress corrosion cracking. This cracking results from tensile stresses in combination with offensive agents such as polythionic acids, chlorides, and caustics. To screen candidate construction materials for resistance to stress corrosion cracking, we exposed racks of stressed U-bend specimens in welded and as-wrought conditions at four coal liquefaction pilot plants. Results from exposures through June 1980 were described in a previous report for exposures in the SRC plants. This report summarizes the on-site test results from June 1980 through October 1981 for the two SRC pilot plants and the H-Coal and Exxon coal liquefaction pilot plants.

  8. Direct coal liquefaction baseline design and system analysis

    SciTech Connect

    Not Available

    1991-07-01

    The primary objective of the study is to develop a computer model for a base line direct coal liquefaction design based on two stage direct coupled catalytic reactors. This primary objective is to be accomplished by completing the following: a base line design based on previous DOE/PETC results from Wilsonville pilot plant and other engineering evaluations; a cost estimate and economic analysis; a computer model incorporating the above two steps over a wide range of capacities and selected process alternatives; a comprehensive training program for DOE/PETC Staff to understand and use the computer model; a thorough documentation of all underlying assumptions for baseline economics; and a user manual and training material which will facilitate updating of the model in the future.

  9. Direct coal liquefaction baseline design and system analysis

    SciTech Connect

    Not Available

    1991-04-01

    The primary objective of the study is to develop a computer model for a base line direct coal liquefaction design based on two stage direct coupled catalytic reactors. This primary objective is to be accomplished by completing the following: a base line design based on previous DOE/PETC results from Wilsonville pilot plant and other engineering evaluations; a cost estimate and economic analysis; a computer model incorporating the above two steps over a wide range of capacities and selected process alternatives; a comprehensive training program for DOE/PETC Staff to understand and use the computer model; a thorough documentation of all underlying assumptions for baseline economics; and a user manual and training material which will facilitate updating of the model in the future.

  10. Direct coal liquefaction baseline design and system analysis

    SciTech Connect

    Not Available

    1991-01-01

    The primary objective of the study is to develop a computer model for a base line direct coal liquefaction design based on two stage direct coupled catalytic reactors. This primary objective is to be accomplished by completing the following: a base line design based on previous DOE/PETC results from Wilsonville pilot plant and other engineering evaluations; a cost estimate and economic analysis; a computer model incorporating the above two steps over a wide range of capacities and selected process alternatives; a comprehensive training program for DOE/PETC Staff to understand and use the computer model; a thorough documentation of all underlying assumptions for baseline economics; and a user manual and training material which will facilitate updating of the model in the future.

  11. Application of urine mutagenicity to monitor coal liquefaction workers.

    PubMed

    Recio, L; Enoch, H G; Hannan, M A; Hill, R H

    1984-06-01

    The Salmonella/microsomal assay was used to monitor workers' urine for mutagenicity as a potential indicator of human exposure to mutagens/carcinogens. Urine samples from 57 workers at a coal liquefaction pilot plant in Catlettsburg, Kentucky, were assayed for mutagenicity during work periods. Urine samples were collected twice during plant operations and once when the individuals were away from the plant for at least 48 h. In 7 individual smokers (5 operator/maintenance workers and 2 administrative staff workers) there was an indication of enhanced urine mutagenicity during work periods. Urine mutagenicity of nonsmokers from the pilot plant was significantly higher than that of an additional control group of nonsmokers from Lexington, Kentucky. While cigarette smoking was the major factor affecting urine mutagenicity, no significant mutagenicity that could be directly attributed to the pilot plant workers' environment was evident.

  12. A CHARACTERIZATION AND EVALUATION OF COAL LIQUEFACTION PROCESS STREAMS

    SciTech Connect

    G.A. Robbins; S.D. Brandes; D.J. Pazuchanics; D.G. Nichols; R.A. Winschel

    1998-12-01

    This is the Technical Progress Report for the fifteenth quarter of activities under DOE Contract No. DE-AC22-94PC93054. It covers the period January 1 through March 31, 1998. Described in this report are the following activities: (1) CONSOL characterized 41 process stream samples obtained from HTI Run PB-01 (227-90), in which Black Thunder Mine coal, Hondo VTB resid, municipal solid waste (MSW) plastics, and virgin plastics were co-liquefaction feedstocks with all-dispersed Fe and Mo catalysts. (2) A request was made for samples from the Nippon Coal Oil NEDOL pilot plant in Kashima, Japan. (3) Phenols were extracted from two samples of separator overhead oil from HTI Run PB-03 Periods 10A and 10B. The phenols were converted to ethylphenyl ethers, and the ethers were distilled to produce a sample within the diesel fuel boiling range. The ethers were mixed with diesel fuel to make 1%, 5%, 10%, and 20% solutions. The four mixtures and a control sample (0% ether) were tested for diesel fuel properties by Intertek Testing Services, Caleb Brett. (4) Computational studies related to the University of Delaware's resid conversion model were continued on the Hewlett Packard Apollo HP-735 RISC workstation at CONSOL R and D. The Structure Optimization Program and the Structure Once-Through Program were used to generate physicochemical properties and structure models for the 15 coal resid samples which have been under study.

  13. Liquefaction/solubilization of low-rank Turkish coals by white-rot fungus (Phanerochaete chrysosporium)

    SciTech Connect

    Elbeyli, I.Y.; Palantoken, A.; Piskin, S.; Kuzu, H.; Peksel, A.

    2006-08-15

    Microbial coal liquefaction/solubilization of three low-rank Turkish coals (Bursa-Kestelek, Kutahya-Seyitomer and Mugla-Yatagan lignite) was attempted by using a white-rot fungus (Phanerochaete chrysosporium DSM No. 6909); chemical compositions of the products were investigated. The lignite samples were oxidized by nitric acid under moderate conditions and then oxidized samples were placed on the agar medium of Phanerochaete chrysosporium. FTIR spectra of raw lignites, oxidized lignites and liquid products were recorded, and the acetone-soluble fractions of these samples were identified by GC-MS technique. Results show that the fungus affects the nitro and carboxyl/carbonyl groups in oxidized lignite sample, the liquid products obtained by microbial effects are the mixture of water-soluble compounds, and show limited organic solubility.

  14. Assessment of Long-Term Research Needs for Coal-Liquefaction Technologies

    SciTech Connect

    Penner, S.S.

    1980-03-01

    The Fossil Energy Research Working Group (FERWG), at the request of J.M. Deutch (Under Secretary of DOE), E. Frieman (Director, Office of Energy Research) and G. Fumich, Jr. (Assistant Secretary for Fossil Fuels), has studied and reviewed currently funded coal-liquefaction technologies. These studies were performed in order to provide an independent assessment of critical research areas that affect the long-term development of coal-liquefaction technologies. This report summarizes the findings and research recommendations of FERWG.

  15. Type II preliminary pilot-plant evaluation of a coal-liquefaction residue - water slurry using vaccum-tower bottoms from the H-Coal liquefaction process

    SciTech Connect

    Wu, C.M.; Robin, A.M.

    1982-09-01

    About 6.7 tons of vacuum tower bottoms (residue) which were obtained during the liquefaction of Illinois No. 6 coal from the H-Coal liquefaction process pilot plant at Catlettsburg, Kentucky were successfully gasified at Texaco's Montebello Research Laboratory. The single 9.5-hour run with H-Coal liquefaction residue-water slurry was completed at 750 to 760 psig gasifier pressure. The run consisted of two test periods, each at a different gasifier temperature. Over 99.6 percent conversion of carbon in the feed to syngas was achieved yielding 32.9 to 33.7 standard cubic feet of dry syngas per pound of residue charged. The oxygen requirement was about 1.0 pound of oxygen per pound of residue. The dry syngas contained 78.5 to 79.7 (vol.) percent carbon monoxide plus hydrogen.

  16. Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama. Run 261 with Illinois No. 6 Burning Star Mine coal

    SciTech Connect

    Not Available

    1992-09-01

    This report presents the results of Run 261 performed at the Advanced Coal Liquefaction R & D Facility in Wilsonville, Alabama. The run started on January 12, 1991 and continued until May 31, 1991, operating in the Close-Coupled Integrated Two-Stage Liquefaction mode processing Illinois No. 6 seam bituminous coal (from Burning star No. 2 mine). In the first part of Run 261, a new bimodal catalyst, EXP-AO-60, was tested for its performance and attrition characteristics in the catalytic/catalytic mode of the CC-ITSL process. The main objective of this part of the run was to obtain good process performance in the low/high temperature mode of operation along with well-defined distillation product end boiling points. In the second part of Run 261, Criterion (Shell) 324 catalyst was tested. The objective of this test was to evaluate the operational stability and catalyst and process performance while processing the high ash Illinois No. 6 coal. Increasing viscosity and preasphaltenes made it difficult to operate at conditions similar to EXP-AO-60 catalyst operation, especially at lower catalyst replacement rates.

  17. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction

    SciTech Connect

    Not Available

    1993-04-01

    The near equal conversions were obtained even with high coal/liquid ratio (1/3--1/2) for two-step wise high-temperature soaking and the first stage liquefaction. Expected conversions were not observed when vacuum distillation after soaking was used in stead of cyclohexane extraction. This is presumably due to the difficulty with redispersion of vacuum distillated bottoms in the coal liquid, because a batch wise procedure was taken by using glasswares. It is suggested that the proposed procedure in the previous quarter should be tested by a continuous procedure under enough heating conditions to keep low viscosity of the bottoms.

  18. Liquefaction of coal by Polyporus versicolor and Poria monticola. Progress report, 1 January-31 March 1985

    SciTech Connect

    Cohen, M.S.

    1985-01-01

    Both Polyporus versicolor and Poria monticola were obtained from the American Type Culture Collection. Growth of Polyporus was shown to be faster and stronger than that of Poria under all conditions tested and the results reported here are based upon liquefaction of lignite coal by Polyporus. The liquefied coal samples were treated with acetonitrile which gave two fractions, a black precipitate and a light yellow liquid phase supernatant. This supernatant consists of acetonitrile and organic compounds which are soluble in acetonitrile. If the supernatant is drawn off with a Pasteur pipette followed by addition of water to the black precipitate, the precipitate dissolves instantly in the water producing a black liquid. Using these techniques, the products of coal liquefaction have been divided into two phases which are soluble either in acetonitrile or in water. Both fractions have been analyzed by HPLC and compounds have been partially separated. No peaks have been identified. However, two principal peaks of the acetonitrile fraction have been sent to PETC for chemical analysis by GC-MS. 9 figs.

  19. Coal liquefaction and gas conversion: Proceedings. Volume 2

    SciTech Connect

    Not Available

    1993-12-31

    Volume II contains papers presented at the following sessions: Indirect Liquefaction (oxygenated fuels); and Indirect Liquefaction (Fischer-Tropsch technology). Selected papers have been processed separately for inclusion in the Energy Science and Technology Database.

  20. Reactivity of heteroatom-containing organics during liquefaction of subbituminous coal: Quarterly technical progress report, March 15, 1988-June 15, 1988

    SciTech Connect

    Aulich, T.R.; Knudson, C.L.; Hawthorne, S.B.

    1988-01-01

    Deuteration of AO4 liquefaction solvent to an isotopic purity of approximately 99% was accomplished using a teflon-lined Parr bomb reactor. Tubing bomb liquefaction tests were performed using two sets of reaction conditions including coal and AO4, and coal and deuterated AO4. The THF insolubles to be used in testing the stability of the deuterated AO4 under liquefaction conditions were extracted using a Soxhlet apparatus and methylene chloride solvent. A system enabling product slurry distillation directly from the tubing bomb following completion of the liquefaction reaction was designed, constructed, and utilized to recover and quantitate volatile fractions of product slurries. The AO4 solvent was also distilled using the same equipment and procedure. Weighed amounts of eight deuterium-labeled species were added to weighed amounts of both labeled and non-labeled AO4 in preparation for the four remaining tubing bomb tests. 3 figs.

  1. Advanced coal liquefaction research: Technical progress report, January 1, 1987-March 31, 1987

    SciTech Connect

    Gall, W.; McIlvried, H.G. III

    1987-05-01

    This report describes the work performed by Energy International during the first quarter of 1987. Most of this work involved using a larger microautoclave reactor. Studies were made of the effect of the size of the coal charge on conversion and product yield reproducibility using Powhatan No. 6 Mine and Illinois No. 6 coals. Good coal conversion and product yield reproducibility for duplicate runs were obtained after minor modifications were made to the product workup technique. The experimental program using 50/sup 0/F distillate fractions of process solvent obtained from the GR and DC P-99 SRC-II PDU has been completed. Initial results indicate that all six distillates are essentially equal as hydrogen donor solvents. A sample of Wilsonville SRC deashed oil was received and distilled into two distillate fractions: 650 to 850/sup 0/F. A 3 x 3 factorial design of experiments with replicates of the corner and center points (14 runs total) will be made with the 850 to 1005/sup 0/F distillate cut using Illinois No. 6 coal. EI will perform the coal liquefaction runs in its 105 ml microautoclave reactor. 2 refs., 6 figs., 24 tabs.

  2. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction

    SciTech Connect

    Song, C.; Saini, A.; Huang, L.; Wenzel, K.; Hatcher, P.G.; Schobert, H.H.

    1992-01-01

    Low-temperature catalytic pretreatment is a promising approach to the development of an improved liquefaction process. This work is a fundamental study on effects of pretreatments on coal structure and reactivity in liquefaction. The main objectives of this project are to study the coal structural changes induced by low-temperature catalytic and thermal pretreatments by using spectroscopic techniques; and to clarify the pretreatment-induced changes in reactivity or convertibility of coals in the subsequent liquefaction. This report describes the progress of our work during the first quarterly period. Substantial progress has been made in the spectroscopic characterization of fresh and THF-extracted samples of two subbituminous coals and fresh samples of three bituminous coals using cross-polarization magic angle spinning (CPMAS) solid state {sup 13}C NMR and pyrolysis-GC-MS techniques. CPMAS {sup 13}C NMR and pyrolysis-GC-MS provided important information on carbon distribution/functionality and molecular components/structural units, respectively, for these coal samples. Pyrolysis-GC-MS revealed that there are remarkable structural differences in structural units between the subbituminous coals and the bituminous coals. Furthermore, significant progress has been made in the pretreatments and spectroscopic characterization of catalytically and thermally pretreated as well as physically treated Wyodak subbituminous coal, and temperature-staged and temperature-programmed thermal and catalytic liquefaction of a Montana subbituminous coal.

  3. A Characterization and Evaluation of Coal Liquefaction Process Streams

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.

    1997-03-31

    This is the Technical Progress Report for the tenth quarter of activities under DOE Contract No. DE-AC22-94PC93054. It covers the period October 1 through December 31, 1996. Described in this report are the following activities: (1) CONSOL characterized two HTI coal/petroleum coprocessing samples for Ni and V concentrations, as requested by DOE. The results are reported in Appendix 1. (2) CONSOL began work to evaluate the potential for producing alkylphenyl ethers, and specifically ethylphenyl ethers, from coal liquefaction phenols. The work includes a literature review and experimentation. The status of this ongoing work is described in this report. (3) A set of samples was requested from HTI Run ALC-2 (Appendix 2). (4) The University of Delaware is conducting resid reactivity tests and is developing a kinetic mechanistic model of resid reactivity. A summary of Delaware`s progress is appended to this report (Appendix 3). (5) A paper was submitted for presentation at the 213th National Meeting of the American Chemical Society, April 13-17, 1997, in San Francisco, CA, (Appendix 4).

  4. A characterization and evaluation of coal liquefaction process streams. Quarterly technical progress report, April 1--June 30, 1996

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.

    1997-03-01

    The objectives of this project are to support the DOE direct coal liquefaction process development program and to improve the useful application of chemical analyses to direct coal liquefaction process development. Independent analyses by well-established methods are obtained of samples produced in direct coal liquefaction processes under evaluation by DOE. Additionally, new analytical instruments and techniques to examine coal-derived samples are being evaluated. The data obtained form this study are used to guide process development and to develop an improved data base on coal and coal liquids properties. A sample bank, established and maintained for use in this project, is available for use by other researchers. The reactivity of the non-distillable resids toward hydrocracking at liquefaction conditions (i.e., resid reactivity) is being examined. From the literature and experimental data, a kinetic model of resid conversion will be constructed. Such a model will provide insights to improve process performance and the economics of direct coal liquefaction.

  5. Advanced liquefaction using coal swelling and catalyst dispersion techniques. Quarterly technical progress report, October--December 1992

    SciTech Connect

    Curtis, C.W.; Gutterman, C.; Chander, S.

    1992-12-31

    The evaluation of various catalyst pre or pyrene coal conversion continued. Higher coal conversions were observed for the S0{sub 2}-treated coal than the raw coal, regardless of catalyst type. Coal conversions were highest for Molyvan-L, molybdenum naphthenate, and nickel octoate. A technique to measure the effect of coal swelling and catalyst impregnation upon coal liquefaction has been developed, and experimentation is under way. Reactivity tests have been performed using S0{sub 2}-treated and untreated swelled Black Thunder Coal. Thermal reactions with swelled coals yielded much less coal conversion and pyrene conversion than did the swelled coal reactions with Molyvan-L. The study of bottoms processing consists of coupling solvent deasphalting with delayed coking to maximize the production of coal-derived liquids while rejecting solids within the coke drum. The batch deasphalting screening tests have been completed. While n-butane/pentane solvent blends initially appeared best, pentane alone at 380{degree}F provided an oil yield (63.6 wt%) that was desired for subsequent tests. The production of asphalt for the transport tests is underway. The target deasphalted oil yields are 40, 50 and 60 wt% of feed. This would produce asphalt with ash levels ranging from 20 to 30 wt% with which to run the transport tests.

  6. Kinetics assisted design of catalysts for coal liquefaction. Final report

    SciTech Connect

    Klein, M.T.; Foley, H.C.; Calkins, W.H.; Scouten, C.

    1998-02-01

    The thermal and catalytic reactions of 4-(1-naphthylmethyl)bibenzyl (NBBM), a resid and coal model compound, were examined. Catalytic reaction of NBBM was carried out at 400 C under hydrogen with a series of transition metal-based catalytic materials including Fe(CO){sub 4}PPh{sub 3}, Fe(CO){sub 3}(PPh{sub 3}){sub 2}, Fe(CO){sub 2}(PPh{sub 3}){sub 2}CS{sub 2}, Fe(CO){sub 5}, Mo(CO){sub 6}, Mn{sub 2}(CO){sub 10}, Fe{sub 2}O{sub 3} and MoS{sub 2}. Experimental findings and derived mechanistic insights were organized into molecular-level reaction models for NBBM pyrolysis and catalysis. Hydropyrolysis and catalysis reaction families occurring during NBBM hydropyrolysis at 420 C were summarized in the form of reaction matrices which, upon exhaustive application to the components of the reacting system, yielded the mechanistic reaction model. Each reaction family also had an associated linear free energy relationship (LFER) which provided an estimate of the rate constant k{sub i} given a structural property of species i or its reaction. Including the catalytic reaction matrices with those for the pyrolysis model provided a comprehensive NBBM catalytic reaction model and allowed regression of fundamental LFER parameters for the catalytic reaction families. The model also allowed specification of the property of an optimal catalyst. Iron, molybdenum and palladium were predicted to be most effective for model compound consumption. Due to the low costs associated with iron and its disposal, it is a good choice for coal liquefaction catalysis and the challenge remains to synthesize small particles able to access the full surface area of the coal macromolecule.

  7. Cooperative Research Program in Coal-Waste Liquefaction

    SciTech Connect

    Gerald Huffman

    2000-03-31

    The results of a feasibility study for a demonstration plant for the liquefaction of waste plastic and tires and the coprocessing of these waste polymers with coal are presented. The study was conducted by a committee that included nine representatives from the CFFS, six from the U.S. Department of Energy - Federal Energy Technology Center (FETC), and four from Burns and Roe, Inc. The study included: (1) An assessment of current recycling practices, particularly feedstock recycling in Germany; (2) A review of pertinent research, and a survey of feedstock availability for various types of waste polymers; and (3) A conceptual design for a demonstration plant was developed and an economic analysis for various feedstock mixes. The base case for feedstock scenarios was chosen to be 200 tons per day of waste plastic and 100 tons per day of waste tires. For this base case with oil priced at $20 per barrel, the return on investment (ROI) was found to range from 9% to 20%, using tipping fees for waste plastic and tires typical of those existing in the U.S. The most profitable feedstock appeared to waste plastic alone, with a plant processing 300 t/d of plastic yielding ROI's from 13 to 27 %, depending on the tipping fees for waste plastic. Feedstock recycling of tires was highly dependent on the price that could be obtained for recovered carbon. Addition of even relatively small amounts (20 t/d) of coal to waste plastic and/or coal feeds lowered the ROI's substantially. It should also be noted that increasing the size of the plant significantly improved all ROI's. For example, increasing plant size from 300 t/d to1200 t/d approximately doubles the estimated ROI's for a waste plastic feedstock.

  8. Using gas chromatography to characterize a direct coal liquefaction naphtha.

    PubMed

    Omais, Badaoui; Courtiade, Marion; Charon, Nadège; Roullet, Christophe; Ponthus, Jérémie; Thiébaut, Didier

    2012-02-24

    Speciation of oxygenated compounds in direct coal liquefaction naphthas is essential considering their important roles in coal conversion reactions. This study attempts to characterize them as fully as possible using gas chromatographic systems. Firstly, GC-MS was deployed allowing the identification of a few ketones, alcohols, and phenols. This conventional analysis was complemented by the application of GC-GC-FID aiming to overcome the coelutions highlighted when using one-dimensional gas chromatography. Heart-cutting and comprehensive two-dimensional gas chromatography were used and the comprehensive system led to better performances as expected considering the complexity of the matrix. In fact, it allowed the identification of more than a hundred of oxygenated compounds belonging to five chemical families: alcohols, ketones, furans, acids and phenols. Average response factors of each of these families were determined by GC×GC-FID using calibration curves and vary from 1 (hydrocarbons) to 2.50 (carboxylic acids). Thanks to a breakthrough columns set involving a trifluoropropyl stationary phase, alcohols and phenols which represent around 14% of the sample were fully identified. A detailed quantification of these species was carried out for the first time in such matrices using the determined response factors. It was concluded that 90% (w/w) of the alcohols are aromatic (phenols), 5% (w/w) are cyclic and 5% (w/w) are linear. A quantification of hydrocarbon families was also achieved and shows that the matrix is mostly naphthenic (56%, w/w), but also contains aromatics (22%, w/w) and paraffins (8%, w/w). This detailed characterization leads to a better understanding of coal conversion processes and is essential to convert them into synthetic fuels.

  9. A study of microbial enzymes and coal liquefaction: Quarterly report, December 1, 1988--February 28, 1989

    SciTech Connect

    Fennell, P.M.

    1989-01-01

    The overall objective is to study the role of microbes in coal liquefaction. The project will be concerned with the effects of the non-ionic detergent, Renex 690, on the release of active enzyme(s) from the mycelia of fungi and/or bacteria, for the purpose of enzyme(s) purification and characterization. The project will employ the microorganism, Phanerochaete chrysosporium, that has been shown to be responsible for the solubilization of low rank coals. Specific goals are: (1) to study the effects of the non-ionic detergent Renex 690 on the activity of ligninase in submerged agitated culture; (2) to study the effects of Renex 690 on enzyme activity in the presence of veratryl alcohol and other products; and (3) to purify ligninase from P. chrysosporium in the presence of Renex 690 by ion exchange liquid chromatography. 2 figs.

  10. DOE indirect coal liquefaction program -- An overview and the prospects for its early commercial deployment

    SciTech Connect

    Miller, C.L.; Shen, J.; Schmetz, E.; Winslow, J.; Tischer, R.

    1997-12-31

    Coal is the most abundant domestic energy resource in the US. The Fossil Energy organization within the US Department of Energy (DOE) has been supporting a coal liquefaction program to develop improved technologies to convert coal to clean burning and cost-effective liquid fuels and/or premium chemicals to complement the dwindling supply of domestic petroleum crude. The goal of this program is to produce coal liquids that are competitive with crude at $20 to $25 per barrel. Indirect and direct liquefaction routes are the two technologies being pursued under the DOE coal liquefaction program. In indirect liquefaction, the emphasis is on the development of improved liquid phase reactor technology to directly convert ``lean syngas`` (low hydrogen to carbon monoxide ratio synthesis gas) produced from advanced coal gasifiers. Liquid phase reactor is also known as slurry-phase bubble column reactor (SBCR), and the two terms are considered interchangeable in this paper. An earlier overview of the DOE indirect liquefaction program, including the development highlights of the Liquid Phase Methanol technology now under commercial demonstration, can be found elsewhere (Shen et al.1996). This paper will give an updated review of the program and briefly discuss the future program activities. It also will discuss the prospects for the early commercial deployment of this technology via its integration into an Integrated Gasification Combined Cycle (IGCC) facility to coproduce power, fuels, and chemicals.

  11. Type III extended pilot-plant evaluation of molten H-Coal liquefaction residue. Gasification of residual-materials from coal liquefaction

    SciTech Connect

    Wu, C.M.; Robin, A.M.

    1982-12-01

    A Type III extended pilot plant evaluation of molten H-Coal liquefaction residue, which was obtained from the liquefaction of Illinois No. 6 coal at the H-Coal liquefaction process pilot plant at Catlettsburg, Kentucky, was successfully completed at Texaco's Montebello Research Laboratory. Approximately 55 tons of residue were gasified during five runs which were carried out at 750 to 790 psig in the Texaco pilot plant residue gasifier. The steam-to-residue ratio and the gasifier temperature were varied to determine optimum operating conditions. The runs lasted from 3.5 hours to 64 hours, and a total 138 hours of on-stream time was accumulated. This work was authorized by DOE Deliver Order Number 7 under DOE contract EX-76-C-01-2247 and amendment DEAC-01-76ET-10137. It is part of a continuing project to evaluate residual materials from various DOE sponsored coal liquefaction projects to determine their suitability for conversion to hydrogen using one of the Texaco gasification processes.

  12. Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction

    SciTech Connect

    Klein, M.T.

    1991-02-22

    The first task in our proposed study of catalysts for coal liquefaction was to prepare ultrafine dispersed metal sulfide particles by reactive precipitation from solutions of appropriate metal precursors. At this point, equipment to allow us to prepare these air-sensitive materials in an anaerobic environment has been acquired and assembled. Initial experiments aimed at synthesizing iron sulfide particles have been initiated. As part of the investigation of short contact time catalytic coal liquefaction, initial efforts focused on the noncatalytic pyrolysis reactions of coal and a model compound, Dibenzyl ether (DBE). Two different reactor configurations were examined; catalytic experiments are planned for the coming month.

  13. EDS coal liquefaction process development. Phase V. Quarterly technical progress report, July 1-September 30, 1980

    SciTech Connect

    1981-02-01

    This report is the tenth Quarterly Technical Progress Report for US Department of Energy Cooperative Agreement No. DE-FC01-77ET10069 (formerly EF-77-A-01-2893) for Exxon Donor Solvent (EDS) Coal Liquefaction Process Development - Phase V. The Laboratory Process Research and Development studies were conducted at various Exxon Research and Engineering Co. (ER and E) facilities: Research and Development Division at Baytown, Texas; Products Research Division at Linden, New Jersey; and the Exxon Research and Development Laboratories at Baton Rouge, Louisiana. The Engineering Research and Development studies were performed at the Synthetic Fuels Engineering and Exxon Engineering Technology Departments of ER and E at Florham Park, New Jersey. The information dealing with the Management, Detailed Engineering, and Procurement activities related to revamp of the FLEXICOKING Prototype Unit was generated at Exxon Company, USA, Houston, Texas, and Exxon Engineering - Project Management Department of ER and E, Florham Park, New Jersey. The information dealing with operation of the 250 T/D Exxon Coal Liquefaction Pilot Plant (ECLP) was generated at Exxon Company, USA, Houston, Texas.

  14. Heterofunctionality interaction with donor solvent coal liquefaction. Final progress report, August 1982-April 1984

    SciTech Connect

    Cronauer, D.C.

    1984-05-01

    This project was undertaken to understand the role of the coal liquefaction solvent through a study of the interaction between the hydrogen donor solvent characteristics and the heterofunctionality of the solvent. Specifically, hydroxyl- and nitrogen-containing solvents were studied and characterized. A series of coal liquefaction experiments were carried out at 450/sup 0/C in a continuous feed stirred-tank reactor (CSTR) to observe the effect of adding phenolics to anthracene oil (AO) and SRC-II recycle solvents. The addition of phenol to AO at a ratio of 5/65 resulted in a nominal increase in coal conversion to THF solubles, but the amount of asphaltenes more than doubled resulting in a sizable net loss of solvent. The addition of m-cresol to both AO and SRC-II solvents had a positive effect on coal conversion to both THF and pentane solubles (oils). The partial removal of an OH-concentrate from SRC-II solvent was carried out using Amberlyst IRA-904 ion exchange resin. The resin-treated oil was only marginally better than raw SRC-II recycle solvent for coal liquefaction. Hydroaromatics having nitrogen functionality should be good solvents for coal liquefaction considering their effective solvent power, ability to penetrate and swell coal, and their ability to readily transfer hydrogen, particularly in the presence of oxygen functionality. However, these benefits are overshadowed by the strong tendency of the nitrogen-containing species to adduct with themselves and coal-derived materials.

  15. Short residence time coal liquefaction. Topical report, May 1978-July 1982

    SciTech Connect

    Not Available

    1984-02-01

    This report is the second in a series of topical reports describing work conducted for the US Department of Energy at Gulf Oil Corporation's Merriam Coal Liquefaction Laboratory. It reviews research carried out over several years to determine the role of process variables in an SRC I type coal dissolution process. The data reported describe the effects of temperature (440 to 500/sup 0/C), pressure (1000 to 3000 psig) and residence time (1 to 10 minutes) using bituminous coal (Kentucky 9/14, Indiana V, and Pittsburgh seams) in the short residence time solvent refined coal (SRC) process. All of the research was conducted using a continuous bench scale unit. The short residence time SRC process was originally envisioned as a stand-alone process which would produce a low cost solid SRC I type product. With interest shifting toward the production of higher quality products, the short residence time SRC process can now be thought of as a minimum cost first stage of a multi-staged process. 9 references, 16 figures, 23 tables.

  16. Determination of unconverted HDPE in coal/plastics co-liquefaction stream samples

    SciTech Connect

    Robbins, G.A.; Winschel, R.A.; Burke, F.P.

    1996-12-31

    In several coal/plastics liquefaction runs performed by Hydrocarbon Technologies, Inc. (HTI), a substantial amount of incompletely converted high-density polyethylene (HDPE) was present in ash-free recycle resid streams when either the ROSE-SR unit was used in Run POC-2, or the pressure filter unit was used in Runs CMSL-8 and CMSL-9. This indicates that the HDPE is less reactive than coal at the liquefaction conditions used. In these ash-free streams, there is no solid organic or inorganic material arising from the coal, and the incompletely converted HDPE can be recovered by extraction and filtration with tetrahydrofuran (THF) at room temperature. The HDPE (or HDPE-like material, which could also consist of heavy waxes) is THF insoluble. However, in ashy streams, there are both inorganic ({open_quotes}ash{close_quotes}) and organic (unconverted coal) components present from liquefaction of the coal, that interfere with an easy and clean separation of the HDPE from the coal/plastics liquefaction stream sample. Therefore, CONSOL developed an analytical procedure for HDPE in the ashy stream samples based on extraction of HDPE from the sample using hot (150{degrees}C) decalin (decahydronaphthalene), in which the HDPE is soluble. The decalin extraction is both preceded and succeeded by extractions and washes with THF at room temperature, to remove the coal-derived components from the sample.

  17. Characteristics and Thermal Behaviour of Low Rank Malaysian Coals towards Liquefaction Performance via Thermogravimetric Analysis

    NASA Astrophysics Data System (ADS)

    Ishak, M. A. M.; Ismail, K.; Nawawi, W. I.; Jawad, A. H.; Abdullah, M. F.; Kasim, M. N.; Ani, A. Y.

    2016-07-01

    In this study, thermal behaviour of two low-rank Malaysian coals namely Mukah Balingian (MB) and Batu Arang (BA) were obtained under pyrolysis conditions via Thermogravimetric analysis (TGA) at a heating rate of 20°C min-1. The thermal characteristics of the coals were investigated prior to direct liquefaction in order to determine the liquefaction performance, i.e. coal conversion and oil yield. The differential weight loss (DTG) results for both coals showed that there are three main stages evolved which consists of moisture, volatile matter and heavier hydrocarbons that correspond to temperature range of 150, 200-500 and 550-800°C, respectively. Apparently, the DTG curves of BA coal reveals a similar pattern of thermal evolution profile in comparison to that of the MB coal. However, the calculated mean reactivity of BA coal is higher than that of MB, which implied that BA would probably enhance coal conversion and oil yield in comparison to MB coal. Interestingly, results showed that under the same liquefaction conditions (i.e. at 4MPa pressure and 420°C), conversion and oil yield of both coals were well correlated with their reactivity and petrofactor value obtained.

  18. Bimetallic promotion of cooperative hydrogen transfer and heteroatom removal in coal liquefaction

    SciTech Connect

    Eisch, J.J.

    1991-10-01

    The ultimate objective of this research is to uncover new catalytic processes for the liquefaction of coal and for upgrading coal-derived fuels by removing undesirable organosulfur, organonitrogen and organooxygen constituents. Basic to both the liquefaction of coal and the purification of coal liquids is the transfer of hydrogen from such sources as dihydrogen, metal hydrides or partially reduced aromatic hydrocarbons to the extensive aromatic rings in coal itself or to aromatic sulfides, amines or ethers. Accordingly, this study is exploring how such crucial hydrogen-transfer processes might be catalyzed by soluble, low-valent transition metal complexes and/or Lewis acids under moderate conditions of temperature and pressure. By learning the mechanism whereby H{sub 2}, metal hydrides or partially hydrogenated aromatics do transfer hydrogen to model aromatic compounds, with the aid of homogeneous, bimetallic catalysts, we hope to identify new methods for producing superior fuels from coal.

  19. A Characterization and Evaluation of Coal Liquefaction Process Streams. Results of Inspection Tests on Nine Coal-Derived Distillation Cuts in the Jet Fuel Boiling Range

    SciTech Connect

    S. D. Brandes; R. A. Winschel

    1999-12-30

    This report describes the assessment of the physical and chemical properties of the jet fuel (180-300 C) distillation fraction of nine direct coal liquefaction products and compares those properties to the corresponding specifications for aviation turbine fuels. These crude coal liquids were compared with finished fuel specifications specifically to learn what the refining requirements for these crudes will be to make them into finished fuels. The properties of the jet fuel fractions were shown in this work to require extensive hydrotreating to meet Jet A-1 specifications. However, these materials have a number of desirable qualities as feedstocks for the production of high energy-density jet fuels.

  20. EDS coal liquefaction process development: Phase V. Final technical progress report, Volume I

    SciTech Connect

    1984-02-01

    All objectives in the EDS Cooperative Agreement for Phases III-B through V have been achieved for the RCLU pilot plants. EDS operations have been successfully demonstrated in both the once-through and bottoms recycle modes for coals of rank ranging from bituminous to lignitic. An extensive data base detailing the effects of process variable changes on yields, conversions and product qualities for each coal has been established. Continuous bottoms recycle operations demonstrated increased overall conversion and improved product slate flexibility over once-through operations. The hydrodynamics of the liquefaction reactor in RCLU were characterized through tests using radioactive tracers in the gas and slurry phases. RCLU was shown to have longer liquid residence times than ECLP. Support work during ECLP operations contributed to resolving differences between ECLP conversions and product yields and those of the small pilot plants. Solvent hydrogenation studies during Phases IIIB-V of the EDS program focused on long term activity maintenance of the Ni-MO-10 catalyst. Process variable studies for solvents from various coals (bituminous, subbituminous, and lignitic), catalyst screening evaluations, and support of ECLP solvent hydrogenation operations. Product quality studies indicate that highly cyclic EDS naphthas represent unique and outstanding catalytic reforming feedstocks. High volumes of high octane motor gasoline blendstock are produced while liberating a considerable quantity of high purity hydrogen.

  1. Novel nanodispersed coal liquefaction catalysts: Molecular design via microemulsion-based synthesis. Technical progress report, July--September 1993

    SciTech Connect

    Boakye, E.; Vittal, M.; Osseo-Asare, K.

    1993-10-01

    The objective of this project is to pursue the development of highly dispersed and inexpensive catalysts for improved coal solubilization and upgrading of coal liquids. A novel study of the synthesis of liquefaction catalysts of manometer size is being carried out. It is based on the molecular design of inverse micelles (microemulsions). These surfactant-stabilized, metal-bearing microdrops offer unique opportunities for synthesizing very small particles by providing a cage-like effect that limits particle nucleation, growth and agglomeration. The emphasis is on molybdenum- and iron-based catalysts, but the techniques being developed should also be generally applicable. The size of these very small and monodispersed particles will be accurately determined both separately and after in situ and ex situ coal impregnation. The as-prepared nanoparticles as well as the catalyst-impregnated coal matrix are characterized using a battery of techniques, including dynamic light scattering, x-ray diffraction and transmission electron microscopy. Catalytic activity tests are conducted under standardized coal liquefaction conditions. The effects of particle size of these unsupported catalysts on the product yield and distribution during conversion of a bituminous and a subbituminous coal are being determined.

  2. Advanced coal liquefaction research. Quarterly technical progress report, April 1-June 30, 1983

    SciTech Connect

    Not Available

    1984-04-01

    Two methods of improving product quality were examined which advance the SRC II process far beyond that envisioned for the original demonstration plant. All distillate product boiling above 310/sup 0/C (590/sup 0/F) was recycled to extinction without loss of total oil yield or significant increase in hydrogen consumption. This product has substantially reduced potential for genetic damage and is more amenable to upgrading. In a further refinement, all of the overhead from the high temperature, high pressure separator was passed through a vapor-phase hydrotreater. This resulted in a dramatic improvement in product quality. A proportional blend of distillate product contained less than 1 ppM of nitrogen. Total oil yield was similar to the low quality product produced in the conventional SRC II process. Coal liquefaction was carried out in three stages to better understand how the variables affect dissolution, hydrogenation and hydrocracking steps. Short contact time dissolution of Illinois No. 6 coal was conducted with minimal hydrocarbon gas yield and hydrogen consumption and high conversion to toluene and pyridine soluble products. In the hydrogenation step, liquid yield increased as temperature was increased to 412/sup 0/C (774/sup 0/F) from 356/sup 0/C (673/sup 0/F). The hydrogen level in the products went through a maximum in the range of 380 to 400/sup 0/C (716 to 752/sup 0/F), however. Very little distillate was made in the subsequent hydrocracking step at a variety of conditions. 33 figures, 10 tables.

  3. Fuel-blending stocks from the hydrotreatment of a distillate formed by direct coal liquefaction

    SciTech Connect

    Andile B. Mzinyati

    2007-09-15

    The direct liquefaction of coal in the iron-catalyzed Suplex process was evaluated as a technology complementary to Fischer-Tropsch synthesis. A distinguishing feature of the Suplex process, from other direct liquefaction processes, is the use of a combination of light- and heavy-oil fractions as the slurrying solvent. This results in a product slate with a small residue fraction, a distillate/naphtha mass ratio of 6, and a 65.8 mass % yield of liquid fuel product on a dry, ash-free coal basis. The densities of the resulting naphtha (C{sub 5}-200{sup o}C) and distillate (200-400{sup o}C) fractions from the hydroprocessing of the straight-run Suplex distillate fraction were high (0.86 and 1.04 kg/L, respectively). The aromaticity of the distillate fraction was found to be typical of coal liquefaction liquids, at 60-65%, with a Ramsbottom carbon residue content of 0.38 mass %. Hydrotreatment of the distillate fraction under severe conditions (200{sup o}C, 20.3 MPa, and 0.41 g{sub feed} h{sup -1} g{sub catalyst}{sup -1}) with a NiMo/Al{sub 2}O{sub 3} catalyst gave a product with a phenol content of {lt}1 ppm, a nitrogen content {lt}200 ppm, and a sulfur content {lt}25 ppm. The temperature was found to be the main factor affecting diesel fraction selectivity when operating at conditions of WHSV = 0.41 g{sub feed} h{sup -1} g{sub catalyst}{sup -1} and PH{sub 2} = 20.3 MPa, with excessively high temperatures (T {gt} 420{sup o}C) leading to a decrease in diesel selectivity. The fuels produced by the hydroprocessing of the straight-run Suplex distillate fraction have properties that make them desirable as blending components, with the diesel fraction having a cetane number of 48 and a density of 0.90 kg/L. The gasoline fraction was found to have a research octane number (RON) of 66 and (N + 2A) value of 100, making it ideal as a feedstock for catalytic reforming and further blending with Fischer-Tropsch liquids. 44 refs., 9 figs., 12 tabs.

  4. Direct liquefaction of low-rank coal. Final technical report, July 13, 1994--November 30, 1995

    SciTech Connect

    Hetland, M.D.; Rindt, J.R.

    1996-02-01

    A multistep direct liquefaction process specifically aimed at low- rank coals has been developed at the Energy & Environmental Research Center. The process consists of a preconversion treatment to prepare the coal for solubilization, solubilization of the coal in the solvent, and polishing using a phenolic solvent or solvent blend to complete solubilization of the remaining material. The product of these three steps can then be upgraded during a traditional hydrogenation step. This project addresses two research questions necessary for the further development and scaleup of this process: 1) determination of the recyclability of the solvent used during solubilization and 2) determination of the minimum severity required for effective hydrotreatment of the liquid product. The project was performed during two tasks: the first consisting of ten recycle tests and the second consisting of twelve hydrotreatment tests performed at various conditions. This project showed that the solvent could be recycled during the preconversion, solubilization and polishing steps of the multistep process and that lower-severity conditions can be used to successfully hydrotreat the product of the multistep process. The success of this project indicates that additional studies should be performed to evaluate the liquid-phase reactions taking place during batch tests in which the gas flow is continuous (i.e., the gas effects would be negligible). In addition, the entire multistep process (including hydrotreatment) should be evaluated during continuous unit operations. 2 refs., 11 figs., 27 tabs.

  5. Novel bimetallic dispersed catalysts for temperature-programmed coal liquefaction. Technical progress report, October 1995--December 1995

    SciTech Connect

    Song, C.; Cooke, W.S.; Schmidt, E.; Schobert, H.H.

    1996-02-01

    Coal liquefaction involves cleavage of methylene, dimethylene and ether bridges connecting polycyclic aromatic units and the reactions of various oxygen functional groups. Here in this quarterly, we report on the catalytic effects of several molybdenum-, cobalt-, and iron-containing compounds in the reactions of dibenzothiophene (DBT) with hydrogen under conditions related to coal liquefaction. The catalytic effects of several molybdenum-, cobalt-, and iron-containing compounds have been examined in the hydrogenation and hydrodesulfurization reactions of dibenzothiophene (DBT) under conditions related to coal liquefaction. The metal compounds are candidate catalyst precursors for direct coal liquefaction. The reactions were carried out in batch microautoclave reactors at 400{degrees}C for 30 minutes with 6.9 MPa (cold) hydrogen pressure, and tridecane solvent. A metal loading of 0.5 mol% resulted in low conversion and only hydrogenation. Addition of sulfur in 4:1 molar ratio led only to a minor increase in conversion and hydrodesulfurization. The use of a higher boiling solvent (octadecane vs. tridecane) was beneficial in providing increased conversion, hydrodesulfurization, and hydrogenation. An increase in metal compound loading to 36.2 mol% led to a dramatic increase in conversion, hydrodesulfurization, and hydrocracking. Molybdenum hexacarbonyl at 36 mol% loading, with added sulfur at 6:1 ratio and octadecane solvent, gave 100% conversion of dibenzothiophene to other products with 100% hydrodesulfurization. Ammonium tetrathiomolybdate and molybdenum(III) chloride are less active under similar conditions. A cobalt-molybdenum thiocubane complex gave unexpectedly low conversions. Iron and cobalt carbonyls also provided very low conversions, even with added sulfur.

  6. Status of health and environmental research relative to direct coal liquefaction: 1976 to the present

    SciTech Connect

    Gray, R.H.; Cowser, K.E.

    1982-06-01

    This document describes the status of health and environmental research efforts, supported by the US Department of Energy (DOE), to assist in the development of environmentally acceptable coal liquefaction processes. Four major direct coal liquefaction processes are currently in (or have been investigated at) the pilot plant stage of development. Two solvent refined coal processes (SRC-I and -II), H-coal (a catalytic liquefaction process) and Exxon donor solvent (EDS). The Pacific Northwest Laboratory was assigned responsibility for evaluating SRC process materials and prepared comprehensive health and environmental effects research program plans for SRC-I and -II. A similar program plan was prepared for H-coal process materials by the Oak Ridge National Laboratory. A program has been developed for EDS process materials by Exxon Research and Engineering Co. The program includes short-term screening of coal-derived materials for potential health and ecological effects. Longer-term assays are used to evaluate materials considered most representative of potential commercial practice and with greatest potential for human exposure or release to the environment. Effects of process modification, control technologies and changing operational conditions on potential health and ecological effects are also being evaluated. These assessments are being conducted to assist in formulating cost-effective environmental research programs and to estimate health and environmental risks associated with a large-scale coal liquefaction industry. Significant results of DOE's health and environmental research efforts relative to coal liquefaction include the following: chemical characterization, health effects, ecological fate and effects, amelioration and risk assessment.

  7. Coal liquefaction process solvent characterization and evaluation: Technical progress report, January 1--March 31, 1988

    SciTech Connect

    Winschel, R.A.; Robbins, G.A.; Burke, F.P.

    1989-03-01

    Consolidation Coal Research and Development is characterizing samples of direct coal liquefaction process oils based on a variety of analytical techniques to provide a detailed description of the chemical composition of the oils, to more fully understand the interrelationship of process oil composition and process operations, to aid in plant operation, and to lead to process improvements. The approach taken is to obtain analyses of a large number of well-defined process oils taken during periods of known operating conditions and known process performance. A set of two feed coals and 45 oils from Wilsonville Run 254 were analyzed to provide information on the performance of these coals in catalytic/catalytic operation in close-coupled integrated two-stage liquefaction (CC-ITSL) with ash recycle. Oils from Wilsonville Run 254 were dewaxed to evaluate any improvement on donor solvent quality. One oil from Wilsonville Run 254 was distillated both at Consol and at Wilsonville using their respective distillation procedures. The distillation fractions were analyzed. Carbon isotope ratios were determined on the two planned feedstocks for Wilsonville Run 255 (Ohio 6 coal and Martin Lake lignite). Three microautoclave tests were made to access the donor liquefaction reactivity of Elkhorn 3 coal. Sixteen microautoclave tests were made to ''calibrate'' the reactivity of our standard coal. Six microautoclave tests were made with two oils from Wilsonville Run 254 to determine the reproducibility of microautoclave tests as applied to samples containing high concentrations of solids. A series of ten fluid-coker tars, produced by Lummus-Crest, Inc., from coal liquefaction vacuum bottoms, was characterized to evaluate their use as liquefaction recycle oils. 11 refs., 26 tabs.

  8. [A Quick Quantitative Analysis for Group Composition of Coal Liquefaction Oil by Ultraviolet Spectroscopy].

    PubMed

    Fan, Wen-jun; Wu, Mei-xiang; Hao, Jian-shu; Feng, Jie; Li, Wen-ying

    2015-07-01

    Gas chromatography is now the primary analysis method for the coal liquefaction oil. However, a simple and rapid quantification/qualification of the coal liquefaction oil can hardly be realized, because the coal liquefaction oil is in a heterogeneous state with a long boiling range. The aim of this study was to establish a rapid and accurate method for the quantification of phenolic compounds, aromatics and aliphatic hydrocarbons in coal liquefaction oil. A representative composition of coal liquefaction light oil, i.e., the distillate fractions of the boiling point range 180-200 degrees C, was chosen as the investigated object. The characteristic absorption peaks of the samples in the UV spectra (200-400 nm) were examined, using three kinds of solvents, cyclohexane, ethanol, 50 Wt% NaOH/ethanol mixture. Among them, the mixture solvent provided the best performance, where the aromatics interfered minimally with the quantification of phenolic compounds by avoiding the peak overlapping problem. By comparison of the UV absorption standard curves between the standard compounds (phenol, m-cresol, p-cresol and o-cresol) and the phenolic mixtures in coal liquefaction oil, m-cresol was selected for the quantification of phenolic compounds in coal liquefaction oil. The content of phenolic compounds was determined to be 32.14% according to the calibration curve of m-cresol at 290 nm, and this result is largely consistent with that determined by weighing after separation. Based on UV and GC analysis of the dephenolized oil, the standard curve of tetrahydronaphthalene at 266 nm was used for the quantification of aromatic hydrocarbons in coal liquefaction oil. The contents of aromatic and aliphatic hydrocarbons were determined to be 44.91% and 22.95%, respectively. To verify the accuracy of the method, recovery of added standards in the oil samples was determined and found to be 104.3%-110.75% and 84.3%-91.75% for phenolic compounds and aromatics, respectively. These results

  9. [A Quick Quantitative Analysis for Group Composition of Coal Liquefaction Oil by Ultraviolet Spectroscopy].

    PubMed

    Fan, Wen-jun; Wu, Mei-xiang; Hao, Jian-shu; Feng, Jie; Li, Wen-ying

    2015-07-01

    Gas chromatography is now the primary analysis method for the coal liquefaction oil. However, a simple and rapid quantification/qualification of the coal liquefaction oil can hardly be realized, because the coal liquefaction oil is in a heterogeneous state with a long boiling range. The aim of this study was to establish a rapid and accurate method for the quantification of phenolic compounds, aromatics and aliphatic hydrocarbons in coal liquefaction oil. A representative composition of coal liquefaction light oil, i.e., the distillate fractions of the boiling point range 180-200 degrees C, was chosen as the investigated object. The characteristic absorption peaks of the samples in the UV spectra (200-400 nm) were examined, using three kinds of solvents, cyclohexane, ethanol, 50 Wt% NaOH/ethanol mixture. Among them, the mixture solvent provided the best performance, where the aromatics interfered minimally with the quantification of phenolic compounds by avoiding the peak overlapping problem. By comparison of the UV absorption standard curves between the standard compounds (phenol, m-cresol, p-cresol and o-cresol) and the phenolic mixtures in coal liquefaction oil, m-cresol was selected for the quantification of phenolic compounds in coal liquefaction oil. The content of phenolic compounds was determined to be 32.14% according to the calibration curve of m-cresol at 290 nm, and this result is largely consistent with that determined by weighing after separation. Based on UV and GC analysis of the dephenolized oil, the standard curve of tetrahydronaphthalene at 266 nm was used for the quantification of aromatic hydrocarbons in coal liquefaction oil. The contents of aromatic and aliphatic hydrocarbons were determined to be 44.91% and 22.95%, respectively. To verify the accuracy of the method, recovery of added standards in the oil samples was determined and found to be 104.3%-110.75% and 84.3%-91.75% for phenolic compounds and aromatics, respectively. These results

  10. Short contact time direct coal liquefaction using a novel batch reactor. Progress report, January 1, 1994--May 15, 1994

    SciTech Connect

    Klein, M.T.; Calkins, W.H.

    1994-05-31

    The objective for this research is to optimize the design and operation of the bench scale batch reactor (SCTBR) for coal liquefaction at short contact times (0.01 to 10 minutes or longer). This reactor is simple enough and low enough in cost to serve as a suitable replacement for the traditional tubing-bomb reactors for many coal liquefaction and other high-pressure, high-temperature reaction studies. The liquefaction of selected Argonne Premium coals and the role of organic oxygen components of the coal and their reaction pathways at very low conversions are being investigated.

  11. Sequential low-temperature depolymerization and liquefaction of US coal. Final report, January 1, 1987--January 1, 1991

    SciTech Connect

    Shabtai, J.S.; Wiser, W.H.

    1992-05-01

    Based on the above described differences in the reactivity of intercluster linkages, an effective new procedure for low-temperature coal depolymerization-liquefaction was proposed and initially examined in our laboratory and then further developed in the framework of this project. The pre-extraction with THF removes most of the easily extractable material within the coal network, leaving the porous system of the coal more susceptible to catalyst impregnation. During subsequent impregnation, the FeCl{sub 3} catalyst becomes uniformly dispersed in the coal particles as recently demonstrated by electron probe microscopy. The partial depolymerization of the coal during the HT step involves preferential hydrogenolytic cleavage of alkylene (e.g. , methylene), benzyl etheric, cycloalkyl etheric, and some activated thioetheric linkages. The following BCD step completes the coal depolymerization by base-catalyzed hydrolysis (or alcoholysis) of diaryl etheric, aryl cycloalkyl etheric, diaryl thioetheric, and other bridging groups. Depolymerized coal samples obtained by the above sequential HT-BCD treatment consist of mixtures of low molecular weight products, composed primarily of monocluster compounds. In the final step, the depolymerized product undergoes exhaustive heteroatom removal, partial ring hydrogenation, and some C-C hydrogenolysis to yield a light hydrocarbon oil. As demonstrated in the present work this procedure has the advantages of very high overall coal conversion to low molecular weight hydrocarbon oils. It also provides very valuable structural information on the fundamental building units of the coal structure.

  12. Liquefaction of sugarcane bagasse for enzyme production.

    PubMed

    Cunha, F M; Kreke, T; Badino, A C; Farinas, C S; Ximenes, E; Ladisch, M R

    2014-11-01

    The objective of this paper is to report liquefaction of pretreated and sterilized sugarcane bagasse for enhancing endoglucanase production through submerged fermentation by Aspergillus niger. After initial solid state fermentation of steam pretreated bagasse solids by A. niger, fed-batch addition of the substrate to cellulase in buffer over a 12h period, followed by 36h reaction, resulted in a liquid slurry with a viscosity of 0.30±0.07Pas at 30% (w/v) solids. Addition of A. niger for submerged fermentation of sterile liquefied bagasse at 23% w/v solids resulted in an enzyme titer of 2.5IUmL(-1) or about 15× higher productivity than solid-state fermentation of non-liquefied bagasse (final activity of 0.17IUmL(-1)). Bagasse not treated by initial solid-state fermentation but liquefied with enzyme gave 2IUmL(-1). These results show the utility of liquefied bagasse as a culture medium for enzyme production in submerged fermentations.

  13. Short residence time coal liquefaction process including catalytic hydrogenation

    DOEpatents

    Anderson, Raymond P.; Schmalzer, David K.; Wright, Charles H.

    1982-05-18

    Normally solid dissolved coal product and a distillate liquid product are produced by continuously passing a feed slurry comprising raw feed coal and a recycle solvent oil and/or slurry together with hydrogen to a preheating-reaction zone (26, alone, or 26 together with 42), the hydrogen pressure in the preheating-reaction zone being at least 1500 psig (105 kg/cm.sup.2), reacting the slurry in the preheating-reaction zone (26, or 26 with 42) at a temperature in the range of between about 455.degree. and about 500.degree. C. to dissolve the coal to form normally liquid coal and normally solid dissolved coal. A total slurry residence time is maintained in the reaction zone ranging from a finite value from about 0 to about 0.2 hour, and reaction effluent is continuously and directly contacted with a quenching fluid (40, 68) to substantially immediately reduce the temperature of the reaction effluent to below 425.degree. C. to substantially inhibit polymerization so that the yield of insoluble organic matter comprises less than 9 weight percent of said feed coal on a moisture-free basis. The reaction is performed under conditions of temperature, hydrogen pressure and residence time such that the quantity of distillate liquid boiling within the range C.sub.5 -454.degree. C. is an amount at least equal to that obtainable by performing the process under the same condition except for a longer total slurry residence time, e.g., 0.3 hour. Solvent boiling range liquid is separated from the reaction effluent (83) and recycled as process solvent (16). The amount of solvent boiling range liquid is sufficient to provide at least 80 weight percent of that required to maintain the process in overall solvent balance.

  14. Short residence time coal liquefaction process including catalytic hydrogenation

    DOEpatents

    Anderson, R.P.; Schmalzer, D.K.; Wright, C.H.

    1982-05-18

    Normally solid dissolved coal product and a distillate liquid product are produced by continuously passing a feed slurry comprising raw feed coal and a recycle solvent oil and/or slurry together with hydrogen to a preheating-reaction zone, the hydrogen pressure in the preheating-reaction zone being at least 1,500 psig (105 kg/cm[sup 2]), reacting the slurry in the preheating-reaction zone at a temperature in the range of between about 455 and about 500 C to dissolve the coal to form normally liquid coal and normally solid dissolved coal. A total slurry residence time is maintained in the reaction zone ranging from a finite value from about 0 to about 0.2 hour, and reaction effluent is continuously and directly contacted with a quenching fluid to substantially immediately reduce the temperature of the reaction effluent to below 425 C to substantially inhibit polymerization so that the yield of insoluble organic matter comprises less than 9 weight percent of said feed coal on a moisture-free basis. The reaction is performed under conditions of temperature, hydrogen pressure and residence time such that the quantity of distillate liquid boiling within the range C[sub 5]-454 C is an amount at least equal to that obtainable by performing the process under the same condition except for a longer total slurry residence time, e.g., 0.3 hour. Solvent boiling range liquid is separated from the reaction effluent and recycled as process solvent. The amount of solvent boiling range liquid is sufficient to provide at least 80 weight percent of that required to maintain the process in overall solvent balance. 6 figs.

  15. Inspection of integrated two-stage liquefaction products as petroleum refining feedstocks

    SciTech Connect

    Winschel, R.A.; Burke, F.P.; Zhou, P.

    1991-12-31

    Regardless of the specific technology used to produce transportation fuels from coal, the net product of the liquefaction process will have to undergo additional refining to make finished products. Consequently, there is a need to characterize the material that exits the liquefaction plant as net product and enters the refinery as feed. The net product of the Integrated Two-Stage Liquefaction (ITSL) process, as practiced at the 6 ton/day (5.5 tonne/day) Wilsonville, Alabama (USA) plant, is a distillable liquid boiling predominantly below 650{degrees}F (343{degrees}C). Products from ITSL operations at the Wilsonville plant were evaluated through the use of standard petroleum tests on several occasions. However, those evaluations were performed on materials generated much earlier in the ITSL campaign and, thus, may not be representative of products generated from the process as it is currently configured. For this work, net products were obtained for analysis from ITSL operations during fully lined-out material balance operating periods.Samples were taken fro Run 259G, which was operated with Ireland Mine coal (hvAb, Pittsburgh seam, West Virginia, USA) and from Run 260D, which was operated with Black Thunder Mine coal (subbituminous, Powder River Basin, Wyoming, USA). A complete suite of light crude oil assay tests was performed on each sample. These assays included tests on the whole coal liquid, and the separated naphtha (<380{degrees}F/193{degrees}C), jet fuel or kerosene (380{degrees}F/193{degrees}C {times} 510{degrees}F/266{degrees}C), and diesel fuel (>510{degrees}F/266{degrees}C) fractions. The results of the assays were compared against typical petroleum product specifications. The discussion will concentrate on the test results of the bituminous coal product.

  16. Improved Fischer-Tropsch catalysts for indirect coal liquefaction

    SciTech Connect

    Wilson, R.B. Jr.; Tong, G.T.; Chan, Y.W.; Huang, H.W.; McCarty, J.G.

    1989-02-01

    The Fischer-Tropsch synthesis (FTS)reaction is the established technology for the production of liquid fuels from coal by an indirect route using coal-derived syngas (CO + H{sub 2}). Modern FTS catalysts are potassium- and copper-promoted iron preparations. These catalysts exhibit moderate activity with carbon monoxide-rich feedstocks such as the syngas produced by advanced coal gasification processes. However, the relatively large yields of by-product methane and high-molecular-weight hydrocarbon waxes detract from the production of desired liquid products in the C{sub 5}-C{sub 16} range needed for motor and aviation fuel. The goal of this program is to decrease undesirable portions of the FTS hydrocarbon yield by altering the Schultz-Flory polymerization product distribution through design and formulation of improved catalysts. Two approaches were taken: (1) reducing the yield of high-molecular-weight hydrocarbon waxes by using highly dispersed catalysts produced from surface-confined multiatomic clusters on acid supports and (2) suppressing methane production by uniformly pretreating active, selective conventional FTS catalysts with submonolayer levels of sulfur.

  17. Coal liquefaction: A research and development needs assessment: Final report, Volume II

    SciTech Connect

    Schindler, H.D.; Burke, F.P.; Chao, K.C.; Davis, B.H.; Gorbaty, M.L.; Klier, K.; Kruse, C.W.; Larsen, J.W.; Lumpkin, R.E.; McIlwain, M.E.; Wender, I.; Stewart, N.

    1989-03-01

    Volume II of this report on an assessment of research needs for coal liquefaction contains reviews of the five liquefaction technologies---direct, indirect, pyrolysis, coprocessing, and bioconversion. These reviews are not meant to be encyclopedic; several outstanding reviews of liquefaction have appeared in recent years and the reader is referred to these whenever applicable. Instead, these chapters contain reviews of selected topics that serve to support the panel's recommendations or to illustrate recent accomplishments, work in progress, or areas of major research interest. At the beginning of each of these chapters is a brief introduction and a summary of the most important research recommendations brought out during the panel discussions and supported by the material presented in the review. A review of liquefaction developments outside the US is included. 594 refs., 100 figs., 60 tabs.

  18. Coal combustion products

    USGS Publications Warehouse

    Kalyoncu, R.S.; Olson, D.W.

    2001-01-01

    Coal-burning powerplants, which supply more than half of U.S. electricity, also generate coal combustion products, which can be both a resource and a disposal problem. The U.S. Geological Survey collaborates with the American Coal Ash Association in preparing its annual report on coal combustion products. This Fact Sheet answers questions about present and potential uses of coal combustion products.

  19. The permeation by liquefied coal of gloves used in coal liquefaction pilot plants.

    PubMed

    Bennett, R D; Feigley, C E; Oswald, E O; Hill, R H

    1983-06-01

    The protective capabilities of PVC, natural rubber and milled nitrile rubber gloves currently used in coal liquefaction pilot plants were assessed and the effectiveness of a laundering method was evaluated. The breakthrough times and cumulative permeation for exposure to toluene and to liquefied coal were determined by measurement of radiolabeled phenol tracer in the aqueous receiving medium. Breakthrough times, normalized by division by the square of the material thickness, agreed with the findings of other studies. On exposure to liquefied coal, the nitrile laboratory glove resisted breakthrough the longest (between 12 and 24 hours), although it was the thinnest material tested. Breakthrough times for the other gloves ranged from 2.75 to 6.5 hours with the times for the natural rubber glove materials intermediate to the two PVC glove materials tested. However, when normalized for thickness, both PVC materials were more resistant to breakthrough than rubber. It was found that the laundering method did not completely decontaminate samples of PVC glove material pre-exposed to liquefied coal for 24 hours under laboratory conditions.

  20. Liquefaction of bamboo shoot shell for the production of polyols.

    PubMed

    Ye, Liyi; Zhang, Jingmiao; Zhao, Jie; Tu, Song

    2014-02-01

    Bamboo (Dendrocalamus latiflorus Munro) shoot shell (BSS) was liquefied in polyethylene glycol 400 (PEG400) and ethylene glycol (EG) catalyzed by sulfuric acid under atmospheric pressure. The effects of liquefaction conditions such as liquid-solid ratio, temperature, time, catalyst, solvents ratio, and material size on the liquefaction yield of BSS have been investigated. Methods including Elemental analysis, Thermogravimetric analysis, Fourier transform infrared spectroscopy, nuclear magnetic resonance and gas chromatography-mass spectrometry were selected to analyze the characteristics of products in three fractions: an aqueous fraction (AQ), an acetone-soluble fraction (AS) and a residue (RS), respectively. Results showed that the highest liquefaction percentage was 99.79% under the optimal conditions (liquid-solid ratio 6:1; temperature 150°C; reaction time 80min; raw size more than 40 mesh; catalyst mass percentage of solvent 4%; solvent volume ratio 3:1). Polyols could be obtained effectively by the liquefaction of BSS, an agricultural by-product.

  1. Mild coal pretreatment to improve liquefaction reactivity. Final technical report, September 1990--February 1994

    SciTech Connect

    Miller, R.L.; Shams, K.G.

    1994-07-01

    Recent research efforts in direct coal liquefaction are focused on lowering the level of reaction severity, identification and determination of the causes of retrogressive reactions, and improving the economics of the process. Ambient pretreatment of coals using methanol and a trace amount of hydrochloric acid was extensively studied in connection with low severity coal liquefaction. Ambient pretreatment of eight Argonne coals using methanol/HCl improved THF-soluble conversions 24.5 wt % (maf basis) for Wyodak subbituminous coal and 28.4 wt % for Beulah-Zap lignite with an average increase of 14.9 wt % for the eight Argonne coals at 623 K (350{degrees}C) reaction temperature and 30 minutes reaction time. Optimal pretreatment conditions were determined using Wyodak and Illinois No. 6 coals. Acid concentration was the most important pretreatment variable studied; liquefaction reactivity increased with increasing acid concentration up to 2 vol %. The FTIR spectra of treated and untreated Wyodak coal samples demonstrated formation of carboxylic functional groups during pretreatment, a result of divalent (Ca, Mg) cationic bridge destruction. The extent of liquefaction reactivity directly correlated with the amount of calcium removed during pretreatment, and results from calcium ``addback`` experiments supported the observation that calcium adversely affected coal reactivity at low severity reaction conditions. Model compound studies using benzyl phenyl ether demonstrated that calcium cations catalyzed retrogressive reactions, inhibited hydrogenation reactions at low severity reaction conditions, and were more active at higher reaction temperatures. Based on kinetic data, mechanisms for hydrogenation-based inhibition and base-catalyzed retrogressive reactions are proposed. The base-catalyzed retrogressive reactions are shown to occur via a hydrogen abstraction mechanism where hydrogenation inhibition reactions are shown to take place via a surface quenching mechanism.

  2. Catalytic coal liquefaction. Quarterly report, October-December 1982

    SciTech Connect

    Weller, S.W.

    1983-01-01

    The catalysis of hydrogen transfer from tetralin to coal has been investigated in a tubing bomb and in an autoclave, in the absence of added hydrogen gas. On the basis of naphthalene production in tubing bomb experiments, many metals apparently increase hydrogen transfer from tetralin. Blank experiments with powdered catalyst but no coal indicate that only stannous chloride and ammonium heptamolybdate have a large effect. In the case of the molybdenum catalyst, even this effect is suspect, because blank runs with molybdate dispersed on an alumina carrier (itself non-catalytic) result in greatly increased dissociation of tetralin to naphthalene and gaseous hydrogen. Coal acts as a high-area carrier for impregnated catalyst. Thermodynamic considerations of tetralin dissociation are helpful in understanding significant differences between tubing bomb and autoclave results. When the gas:liquid volume ratio is relatively high, as in a tubing bomb, tetralin dissociation will be relatively small and equilibrium hydrogen pressure relatively high. The reverse may be true in an autoclave. Both factors lead to the expectation of higher coal conversion in a tubing bomb, in agreement with experiment.

  3. Direct liquefaction of low-rank coal. Quarterly technical progress report, July 1, 1995--September 30, 1995

    SciTech Connect

    Hetland, M.D.

    1995-11-01

    A multistep direct liquefaction process specifically aimed at low-rank coals (LRCs) has been developed at the Energy & Environmental Research Center (EERC). The process consists of a preconversion treatment to prepare the coal for solubilization, solubilization of the coal in the solvent, and polishing using a phenolic solvent or solvent blend to complete solubilization of the remaining material. The product of these three steps can then be upgraded during a traditional hydrogenation step. This project addresses two research questions necessary for the further development and scaleup of this process: (1) determination of the recyclability of the solvent used during solubilization and (2) determination of the minimum severity required for effective hydrotreatment of the liquid product. The project is being performed as two tasks, the first consisting of ten recycle tests and the second consisting of twelve hydrotreatment tests performed at various conditions. Several activities were performed during this quarter. (1) A paper entitled {open_quotes}Solvent Recyclability in a Multistep Direct Liquefaction Process{close_quotes} was presented at the 1995 Coal Liquefaction and Gas Conversion Contractors{close_quote} Review Conference that was held in Pittsburgh, PA, August 29-31, 1995. (2) The Task 1 solvent recyclability tests were completed. (3) The Task 1 quality assurance/quality control checks were performed. (4) The first seven Task 2 hydrotreatability tests were completed. Analysis of the Task 1 data indicates that (1) the multistep process produces adequate quantities of excess solvent for recycle and (2) the product slates of all of the tests were fairly consistent.

  4. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction. Quarterly report, September 20, 1991--December 31, 1991

    SciTech Connect

    Not Available

    1992-07-01

    The main task of this quarter was to install reactors to conduct preconversion and liquefaction of coal. Coal and coal liquids were collected. The anaerobic chamber (Model 855-AC; Plas Labs, inc.) was procured and set up to store coal samples under an inert gas. Equipment to treat products was assembled, including Soxhlet extraction units, fractionation columns, a distillation column, and a rotary evaporator. Two gas chromatographs for analysis of gases and liquid were adjusted. Two reactor systems were installed for the experimental apparatus. One was Model 4576 high-temperature and high-pressure autoclave (Parr Instrument, 500{degrees}C and 5000 psi) (see Figure 1); the other was a 27 ml of microreactors. The autoclave was obtained from the manufacturer and assembled. The experimental set-up of microreactors are shown in Figure 2.

  5. Role of the mineral components in the catalytic liquefaction of coal

    SciTech Connect

    Zekel', L.A.; Krasnobaeva, N.V.; Pchelina, D.P.; Titova, T.A.; Shpirt, M.Ya.

    1983-01-01

    The paper demonstrates the effect of oxides of Fe, Al, and Si, CaCO/sub 3/ and ash of certain coals on the liquefaction of Irsha-Bordodinsk coal from the Kansk-Achinsk opencast site, in the presence of catalysts such as ammonium paramolybdate and iron sulphate. Iron compounds, together with those of Ni, Zn and V have a positive catalytic effect in contrast to the negative effect attributable to compounds of Al, alkaline compounds, alkaline earth metals and As.

  6. Direct liquefaction of low-rank coal. Quarterly technical progress report, April 1, 1995--June 30, 1995

    SciTech Connect

    Hetland, M.D.

    1995-07-01

    A multistep direct liquefaction process specifically aimed at low-rank coals (LRCs) has been developed at the Energy & Environmental Research Center (EERC). The process consists of a preconversion treatment to prepare the coal for solubilization, solubilization of the coal in the solvent, and polishing using a phenolic solvent or solvent blend to complete solubilization of the remaining material. The product of these three steps can then be upgraded during a traditional hydrogenation step. This project will address two research questions necessary for the further development and scaleup of this process: (1) determination of the recyclability of the solvent used during solubilization and (2) determination of the minimum severity required for effective hydrotreatment of the liquid product. The project will be performed as two tasks, the first consisting of ten recycle tests and the second consisting of twelve hydrotreatment tests performed at various conditions.

  7. Design of generic coal conversion facilities: Indirect coal liquefaction, Fischer-Tropsch synthesis

    SciTech Connect

    Not Available

    1991-10-01

    A comprehensive review of Fischer-Tropsch (F-T) technology, including fixed, fluidized, and bubble column reactors, was undertaken in order to develop an information base before initiating the design of the Fischer-Tropsch indirect liquefaction PDU as a part of the Generic Coal Conversion Facilities to be built at the Pittsburgh Energy Technology Center (PETC). The pilot plant will include a fixed bed and slurry bubble column reactor for the F-T mode of operation. The review encompasses current status of both these technologies, their key variables, catalyst development, future directions, and potential improvement areas. However, more emphasis has been placed on the slurry bubble column reactor since this route is likely to be the preferred technology for commercialization, offering process advantages and, therefore, better economics than fixed and fluidized bed approaches.

  8. Liquefaction of bituminous coals using disposable ore catalysts and hydrogen. Final report, February 7, 1982-July 31, 1982

    SciTech Connect

    Mathur, V.K.

    1982-09-01

    There are a number of problems associated with the production of liquid fuels from coal. The most complex is the use of commercial catalysts which are expensive, with short life, and cannot be recovered or regenerated. The objective of this study was to conduct experiments on coal hydrogenation using low cost mineral ores as disposable catalysts. Coal samples from Blacksville Mine, Pittsburgh Bed were hydrogenated using a number of ores, ore concentrates and industrial waste products as catalysts. Experiments were also conducted using a commercial catalyst (Harshaw Chemicals, 0402T) and no catalyst at all to compare the results. Since iron pyrite has been reported to be a good disposable catalyst, experiments were also conducted using pyrite individually as well as in admixture with other ores or concentrates. The liquefaction was conducted at 425/sup 0/C under 2000 psig (13,790 kPa) hydrogen pressure for a reaction time of 30 minutes using SRC-II heavy distillate as a vehicle oil. The conclusions of this study are as follows: (a) Results of liquefaction using two cycle technique showed that the catalytic activity of iron pyrite could be enhanced by adding materials like limonite, laterite or red mud. Iron pyrite in admixture with limonite ore or molybdenum oxide concentrate gave the best results among all the binary mixtures studied. (b) Iron pyrite with molybdenum oxide concentrate and cobaltic hydroxide cake (metal loading in each case the same as in Harshaw catalyst) gave results which compared favorably with those obtained using the Harshaw catalyst. It is recommended that work on this project should be continued exploring other ores and their mixtures for their catalytic activity for coal liquefaction.

  9. Coal production 1989

    SciTech Connect

    Not Available

    1990-11-29

    Coal Production 1989 provides comprehensive information about US coal production, the number of mines, prices, productivity, employment, reserves, and stocks to a wide audience including Congress, federal and state agencies, the coal industry, and the general public. 7 figs., 43 tabs.

  10. Type II preliminary pilot plant evaluation of a coal liquefaction residue-water slurry using vacuum tower bottoms from the Exxon donor solvent coal liquefaction process

    SciTech Connect

    Colpitts, S.G.; Robin, A.M.

    1982-03-01

    About 16 tons of vacuum tower bottoms (residue) from the Exxon Donor Solvent (EDS) Process from the liquefaction of Illinois No. 6 coal were successfully gasified at Texaco's Montebello Research Laboratory. The EDS residue was ground, slurried with water, and fed at ambient temperatures to the gasifier. The gasifier operated smoothly at 1000 psig for almost 17 hours. It was manually shut down after all of the slurry charge had been gasified. A 99.9 percent conversion of the carbon in the feed to syngas was achieved yielding 36.0 SCF of dry syngas per pound of residue charged. The oxygen requirement was 0.9 pounds of oxygen per pound of residue. The dry syngas contained about 80.8 (vol) percent carbon monoxide plus hydrogen. A comparison of the gasification efficiency of EDS residue-water slurry with the gasification efficiency of molten EDS residue revealed that the molten process was more efficient. The molten system had a greater volume percent carbon monoxide plus hydrogen in the product syngas than the residue-water slurry, 88.0% versus 80.9%, and required less oxygen for gasification, 0.80 versus 0.90 pounds of oxygen per pound of residue.

  11. Low-severity catalytic two-stage liquefaction process: Illinois coal conceptual commercial plant design and economics

    SciTech Connect

    Abrams, L.M.; Comolli, A.G.; Popper, G.A.; Wang, C.; Wilson, G.

    1988-09-01

    Hydrocarbon Research, Inc. (HRI) is conducting a program for the United States Department of Energy (DOE) to evaluate a Catalytic Two-Stage Liquefaction (CTSL) Process. This program which runs through 1987, is a continuation of an earlier DOE sponsored program (1983--1985) at HRI to develop a new technology concept for CTSL. The earlier program included bench-scale testing of improved operating conditions for the CTSL Process on Illinois No. 6 bituminous coal and Wyoming sub-bituminous coal, and engineering screening studies to identify the economic incentive for CTSL over the single-stage H-Coal/reg sign/ Process for Illinois No. 6 coal. In the current program these engineering screening studies are extended to deep-cleaned Illinois coal and use of heavy recycle. The results from this comparison will be used as a guide for future experiments with respect to selection of coal feedstocks and areas for further process optimization. A preliminary design for CTSL of Illinois deep-cleaned coal was developed based on demonstrated bench-scale performance in Run No. 227-47(I-27), and from HRI's design experience on the Breckinridge Project and H-Coal/reg sign/ Process pilot plant operations at Catlettsburg. Complete conceptual commercial plant designs were developed for a grassroots facility using HRI's Process Planning Model. Product costs were calculated and economic sensitivities analyzed. 14 refs., 11 figs., 49 tabs.

  12. "An Economic Process for Coal Liquefaction to Liquid Fuels" SBIR Phase II -- Final Scientific/Technical Report

    SciTech Connect

    Ganguli, Partha Sarathi

    2009-02-19

    The current commercial processes for direct coal liquefaction utilize expensive backmix-flow reactor system and conventional catalysts resulting in incomplete and retrogressive reactions that produce low distillate liquid yield and high gas yield, with high hydrogen consumption. The new process we have developed, which uses a less expensive reactor system and highly active special catalysts, resulted in high distillate liquid yield, low gas yield and low hydrogen consumption. The new reactor system using the special catalyst can be operated smoothly for direct catalytic coal liquefaction. Due to high hydrogenation and hydrocracking activities of the special catalysts, moderate temperatures and high residence time in each stage of the reactor system resulted in high distillate yield in the C{sub 4}-650{degrees}F range with no 650{degrees}F{sup +} product formed except for the remaining unconverted coal residue. The C{sub 4}-650{degrees}F distillate is more valuable than the light petroleum crude. Since there is no 650{degrees}F{sup +} liquid product, simple reforming and hydrotreating of the C{sub 4}-650{degrees}F product will produce the commercial grade light liquid fuels. There is no need for further refinement using catalytic cracking process that is currently used in petroleum refining. The special catalysts prepared and used in the experimental runs had surface area between 40-155 m{sup 2}/gm. The liquid distillate yield in the new process is >20 w% higher than that in the current commercial process. Coal conversion in the experimental runs was moderate, in the range of 88 - 94 w% maf-coal. Though coal conversion can be increased by adjustment in operating conditions, the purpose of limiting coal conversion to moderate amounts in the process was to use the remaining unconverted coal for hydrogen production by steam reforming. Hydrogen consumption was in the range of 4.0 - 6.0 w% maf-coal. A preliminary economic analysis of the new coal liquefaction process was

  13. Coal Production 1992

    SciTech Connect

    Not Available

    1993-10-29

    Coal Production 1992 provides comprehensive information about US coal production, the number of mines, prices, productivity, employment, productive capacity, and recoverable reserves to a wide audience including Congress, Federal and State agencies, the coal industry, and the general public. In 1992, there were 3,439 active coal mining operations made up of all mines, preparation plants, and refuse operations. The data in Table 1 cover the 2,746 mines that produced coal, regardless of the amount of production, except for bituminous refuse mines. Tables 2 through 33 include data from the 2,852 mining operations that produced, processed, or prepared 10 thousand or more short tons of coal during the period, except for bituminous refuse, and includes preparation plants with 5 thousand or more employee hours. These mining operations accounted for over 99 percent of total US coal production and represented 83 percent of all US coal mining operations in 1992.

  14. Surface modified coals for enhanced catalyst dispersion and liquefaction. Semiannual progress report, September 1, 1995--February 29, 1996

    SciTech Connect

    Abotsi, G.M.K.

    1996-10-01

    The aim of this work is to enhance catalyst loading and dispersion in coal for improved liquefaction by preadsorption of surfactants onto coal. The application of surfactants to coal beneficiation and coal-water slurry preparation is well known. However, the effects of surfactants on catalyst loading and dispersion prior to coal liquefaction have not been investigated. The current work is focused on the influence of the cationic surfactant dodecyl dimethyl ethyl ammonium bromide (DDAB) and sodium dodecyl sulfate (SDS, anionic) on the surface properties of a bituminous coal and its molybdenum uptake from solution. The results show that DDAB created positively charged sites on the coal and increased molybdenum loading compared to the original coal. In contrast, SDS rendered the coal surface negative and reduced molybdenum uptake. The results show that efficient loading of molybdenum catalyst onto coal can be achieved by pretreatment of the coal with dodecyl dimethyl ethyl ammonium bromide.

  15. Advanced coal liquefaction research. Quarterly technical progress report, July 1, 1983-September 30, 1983

    SciTech Connect

    1984-04-01

    Work this quarter focused on staged liquefaction. The effect of residence time on conversion in single pass experiments was found to be quite different for the subbituminous Belle Ayr Mine and bituminous Illinois No. 6 coals studied. With bituminous coal, conversion to soluble material is quite high and the limit of conversion is approached in only a few minutes. With a subbituminous coal, however, conversion is much lower and the limit of conversion is approached much more slowly. Short contact time (SCT) dissolution of Belle Ayr coal was studied as a possible first stage in a two-stage process. Conversion, hydrocarbon gas yield and hydrogen consumption were increased as residence time or temperature were increased. Conversion was also significantly increased by partial slurry recycle. Pyrite was found to be the most effective slurry catalyst for increasing conversion, followed by ammonium molybdate emulsion and finally nickel-molybdenum on alumina. Illinois No. 6 coal was liquefied in two stages. Conditions in the first stage dissolution were varied to determine the effect on upgradability in the second stage. An SCT (6 minute) coal dissolution stage is preferred over one at 30 minutes because hydrocarbon gas yield was much lower while overall oil yields for the combined dissolution and upgrading stages were nearly the same. Use of a NiMo/Al/sub 2/O/sub 3/ catalyst in a trickle-bed second stage resulted in a higher oil yield and lower product heteroatom content than use of the same catalyst in the slurry phase. The total oil yield was lower with a pyrite slurry catalyst than with a NiMo/Al/sub 2/O/sub 3/ slurry catalyst. With Belle Ayr coal and added pyrite, there was no change in total oil yield, conversion or product quality brought about by adding an 8-minute first stage at 450/sup 0/C (842/sup 0/F) to a 2-hour second stage operated at 420/sup 0/C (788/sup 0/F). 39 figures, 12 tables.

  16. Ion exchange and absorption techniques to apply catalysts for liquefaction of lower rank coals

    SciTech Connect

    Vorres, K.S.; Cronauer, D.C.; Curtis, C.W.; Brannan, C.J.

    1994-07-01

    Samples of Beulah-zap lignite, Black Thunder and Wyodak subbituminous, and Illinois No. 6 high volatile bituminous coals have been prepared by acid treatment to remove exchangeable cations. Subsequent treatments were made with solutions of catalytic metals including iron or cobalt or nickel to exchange with the acid sites, or with molybdate to adsorb on the surface. Samples were then subjected to liquefaction conditions in microautoclave tubular microreactors and solvent extraction was used to establish total conversion or yields of oils, asphaltenes and preasphaltenes. Results of the liquefaction experiments are compared with the catalyst loadings.

  17. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction

    SciTech Connect

    Song, C.; Saini, A.K.; Hatcher, P.G.; Schobert, H.H.

    1992-05-01

    Low-temperature catalytic pretreatment is a promising approach to the development of an improved liquefaction process. This work is a fundamental study on effects of pretreatments on coal structure and reactivity in liquefaction. The main objectives of this project are to study the coal structural changes induced by low-temperature catalytic and thermal pretreatments by using spectroscopic techniques; and to clarify the pretreatment-induced changes in reactivity or convertibility of coals in the subsequent liquefaction. This report describes the progress of our work during the second quarterly period. Significant progress has been made in the spectroscopic characterization of fresh and THF-extracted samples of Wyodak subbituminous coals, catalytic and thermal low-temperature pretreatments in the absence and presence of hydrogen-donor and non-donor solvents, and the spectroscopic characterization of thermally and catalytically pretreated coals using cross-polarization magic angle spinning (CPMAS) solid-state {sup 13}C NMR, pyrolysis-GC-MS and FT-IR techniques.

  18. Catalytic multi-stage liquefaction of coal at HTI: Bench-scale studies in coal/waste plastics coprocessing

    SciTech Connect

    Pradhan, V.R.; Lee, L.K.; Stalzer, R.H.

    1995-12-31

    The development of Catalytic Multi-Stage Liquefaction (CMSL) at HTI has focused on both bituminous and sub-bituminous coals using laboratory, bench and PDU scale operations. The crude oil equivalent cost of liquid fuels from coal has been curtailed to about $30 per barrel, thus achieving over 30% reduction in the price that was evaluated for the liquefaction technologies demonstrated in the late seventies and early eighties. Contrary to the common belief, the new generation of catalytic multistage coal liquefaction process is environmentally very benign and can produce clean, premium distillates with a very low (<10ppm) heteroatoms content. The HTI Staff has been involved over the years in process development and has made significant improvements in the CMSL processing of coals. A 24 month program (extended to September 30, 1995) to study novel concepts, using a continuous bench scale Catalytic Multi-Stage unit (30kg coal/day), has been initiated since December, 1992. This program consists of ten bench-scale operations supported by Laboratory Studies, Modelling, Process Simulation and Economic Assessments. The Catalytic Multi-Stage Liquefaction is a continuation of the second generation yields using a low/high temperature approach. This paper covers work performed between October 1994- August 1995, especially results obtained from the microautoclave support activities and the bench-scale operations for runs CMSL-08 and CMSL-09, during which, coal and the plastic components for municipal solid wastes (MSW) such as high density polyethylene (HDPE)m, polypropylene (PP), polystyrene (PS), and polythylene terphthlate (PET) were coprocessed.

  19. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. [Quarterly] technical progress report, April--June 1993

    SciTech Connect

    Song, C.; Huang, L.; Saini, A.K.; Schobert, H.H.; Hatcher, P.G.

    1993-07-01

    In this quarter, progress has been made in the following two aspects: (1) effects of drying and mild oxidation on conversion and product distribution during non-catalytic and catalytic liquefaction of a Montana subbituminous coal (DECS-9); and (2) effects of solvent and catalyst on conversion and structural changes of a Texas subbituminous coal (DECS-1). Influence of drying and mild oxidation on catalytic and non-catalytic liquefaction (at 350C for 30 min with 6.9 MPa (cold) H{sub 2} was studied using Wyodak subbituminous coal. For non-catalytic runs, fresh raw coal gave higher conversion and higher oil yield than both the vacuum- and air-dried coals, regardless of the solvent. Compared to the vacuum-dried coal, the coal dried in air in 100C for 2 h gave a better conversion in the presence of either a hydrogen donor tetralin or a non-donor 1-methylnaphthalene (1-MN) solvent. Catalytic runs were performed using in-situ generated molybdenum sulfide catalyst from ammonium tetrathiomolybdate (ATTM) precursor impregnated on either raw coal or predried coal samples. The solvent-free runs using ATTM loaded on the raw coal gave higher conversion and higher oil yield than loading ATTM on vacuum- or air-dried coal. In the presence of either tetralin or 1-MN, however, the runs using ATTM loaded on air-dried coal afford better conversions and oil yields as compared to the runs using vacuum-dried coal. Upon drying coal in air at 150C for 20 h, the conversion significantly decreased to a lower value than that of the vacuum-dried coal in the non-catalytic runs, and the same trend was observed in the runs of the dried coals loaded with ATTM. Physical, chemical, and surface chemical aspects of effects of drying and oxidation and the role of water are also discussed in the report.

  20. Mild coal pretreatment to improve liquefaction reactivity. Quarterly technical progress report, September--November 1991

    SciTech Connect

    Miller, R.L.

    1991-12-31

    This report describes work completed during the fifth quarter of a three year project to study the effects of mild chemical pretreatment on coal dissolution reactivity during low severity liquefaction or coal/oil coprocessing. The overall objective of this research is to elucidate changes in the chemical and physical structure of coal by pretreating with methanol or other simple organic solvent and a trace amount of hydrochloric acid and measure the influence of these changes on coal dissolution reactivity. Work this quarter focused on analytical characterization of untreated and treated Wyodak subbituminous coal and Illinois {number_sign}6 bituminous coal. Mossbauer spectroscopy and x-ray diffraction techniques were used to study the effect of methanol/HCl pretreatment on the composition of each coal`s inorganic phase. Results from these studies indicated that calcite is largely removed during pretreatment, but that other mineral species such as pyrite are unaffected. This finding is significant, since calcite removal appears to directly correlate with low severity liquefaction enhancement. Further work will be performed to study this phenomenon in more detail.

  1. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Final technical report, Volume 1 - effects of solvents, catalysts and temperature conditions on conversion and structural changes of low-rank coals

    SciTech Connect

    Lili Huang; Schobert, H.H.; Chunshan Song

    1998-01-01

    The main objectives of this project were to study the effects of low-temperature pretreatments on coal structure and their impacts on subsequent liquefaction. The effects of pretreatment temperatures, catalyst type, coal rank, and influence of solvent were examined. Specific objectives were to identify the basic changes in coal structure induced by catalytic and thermal pretreatments, and to determine the reactivity of the catalytically and thermally treated coals for liquefaction. In the original project management plan it was indicated that six coals would be used for the study. These were to include two each of bituminous, subbituminous, and lignite rank. For convenience in executing the experimental work, two parallel efforts were conducted. The first involved the two lignites and one subbituminous coal; and the second, the two bituminous coals and the remaining subbituminous coal. This Volume presents the results of the first portion of the work, studies on two lignites and one subbituminous coal. The remaining work accomplished under this project will be described and discussed in Volume 2 of this report. The objective of this portion of the project was to determine and compare the effects of solvents, catalysts and reaction conditions on coal liquefaction. Specifically, the improvements of reaction conversion, product distribution, as well as the structural changes in the coals and coal-derived products were examined. This study targeted at promoting hydrogenation of the coal-derived radicals, generated during thermal cleavage of chemical bonds, by using a good hydrogen donor-solvent and an effective catalyst. Attempts were also made in efforts to match the formation and hydrogenation of the free radicals and thus to prevent retrogressive reaction.

  2. Mild acidic pretreatment to enhance low severity coal liquefaction promoted by cyclic olefins. Quarterly report, July 1995--September 1995

    SciTech Connect

    Curtis, C.W.

    1996-03-01

    Research continued on low severity coal liquefaction. Research using high temperature infrared of cyclic olefins progressed well during this quarter. Several fluorinated solvents were found that provide a high temperature medium for isotetralin and its aromatic and aliphatic analogues.

  3. Coal liquefaction in an inorganic-organic medium. [DOE patent application

    DOEpatents

    Vermeulen, T.; Grens, E.A. II; Holten, R.R.

    Improved process for liquefaction of coal by contacting pulverized coal in an inorganic-organic medium solvent system containing a ZnCl/sub 2/ catalyst, a polar solvent with the structure RX where X is one of the elements O, N, S, or P, and R is hydrogen or a lower hydrocarbon radical; the solvent system can contain a hydrogen donor solvent (and must when RX is water) which is immiscible in the ZnCl/sub 2/ and is a hydroaromatic hydrocarbon selected from tetralin, dihydrophenanthrene, dihydroanthracene or a hydrogenated coal derived hydroaromatic hydrocarbon distillate fraction.

  4. Coal liquefaction process streams characterization and evaluation. Quarterly technical progress report, April 1--June 30, 1992

    SciTech Connect

    Brandes, S.D.; Lancet, M.S.; Robbins, G.A.; Winschel, R.A.; Burke, F.P.

    1992-11-01

    This is the eleventh Quarterly Technical Progress Report under DOE Contract DE-AC22-89PC89883. Major topics reported are: (1) The results of a study designed to determine the effects of the conditions employed at the Wilsonville slurry preheater vessel on coal conversion is described. (2) Stable carbon isotope ratios were determined and used to source the carbon of three product samples from Period 49 of UOP bench-scale coprocessing Run 37. The results from this coprocessing run agree with the general trends observed in other coprocessing runs that we have studied. (3) Microautoclave tests and chemical analyses were performed to ``calibrate`` the reactivity of the standard coal used for determining donor solvent quality of process oils in this contract. (4) Several aspects of Wilsonville Close-Coupled Integrated Two-Stage Liquefaction (CC-ITSL) resid conversion kinetics were investigated; results are presented. Error limits associated with calculations of deactivation rate constants previously reported for Runs 258 and 261 are revised and discussed. A new procedure is described that relates the conversions of 850{degrees}F{sup +} , 1050{degrees}F{sup +}, and 850 {times} 1050{degrees}F material. Resid conversions and kinetic constants previously reported for Run 260 were incorrect; corrected data and discussion are found in Appendix I of this report.

  5. Time phased alternate blending of feed coals for liquefaction

    DOEpatents

    Schweigharett, Frank; Hoover, David S.; Garg, Diwaker

    1985-01-01

    The present invention is directed to a method for reducing process performance excursions during feed coal or process solvent changeover in a coal hydroliquefaction process by blending of feedstocks or solvents over time. ,

  6. Coal liquefaction process using pretreatment with a binary solvent mixture

    DOEpatents

    Miller, Robert N.

    1986-01-01

    An improved process for thermal solvent refining or hydroliquefaction of non-anthracitic coal at elevated temperatures under hydrogen pressure in a hydrogen donor solvent comprises pretreating the coal with a binary mixture of an aromatic hydrocarbon and an aliphatic alcohol at a temperature below 300.degree. C. before the hydroliquefaction step. This treatment generally increases both conversion of coal and yields of oil.

  7. Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction. Technical progress report, October 25, 1990--October 24, 1991: Draft

    SciTech Connect

    Klein, M.T.

    1991-12-30

    The purpose of this work is to investigate the kinetics-assisted design, synthesis and characterization of fme-pardcle, unsupported catalysts for coal liquefaction. The goal is to develop a fundamental understanding of coal catalysis and catalysts that will, in turn, allow for the specification of a novel optimal catalyst for coal liquefaction.

  8. Fine particle clay catalysts for coal liquefaction. Quarterly technical progress report, May 8, 1993--August 8, 1993

    SciTech Connect

    Olson, E.S.

    1995-10-01

    High hydrocracking and liquefaction activity can be achieved with 10 wt.% of sulfided clay-supported iron catalysts. Further tests and demonstrations of this activity were required. Iron hydroxyoxide was generated on acid-treated montmorillonite. The new batch of catalyst exhibited high hydrocracking activity, Three hour tests with the solubilized intermediate from low-severity treatment of Wyodak coal (LSW) gave a high conversion (45%) of the heptane-insoluble LSW intermediate to heptane-soluble products. An investigation of new methods for the production of catalysts from tetralin-soluble iron oxometallates and the determination of their catalytic activities was continued in this quarter. Iron oxotitanate and iron oxoaluminate gave very high conversions of LSW to heptane solubles (61% and 54%, respectively). The high yields of heptane soluble products obtained with these catalysts offers a potential for use in liquefaction stages with solubilized coal, or at least serve as a model for producing active catalysts via mixed metal oxides. Methods for successfully testing dispersed iron catalysts with the low-severity intermediate were also devised. Catalyst recovered from the dispersed iron hydroxyoxide-catalyzed reaction of ion-exchanged Wyodak gave a high conversion (47%) of LSW to heptane solubles.

  9. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction. Quarterly report, October 1, 1992--December 31, 1992

    SciTech Connect

    Not Available

    1993-01-01

    Improved coal liquefaction was reinvestigated for the current two-stage process on the basis of the associated molecular nature of coal. Since a significant portion of coal molecules are physically associated as pointed in our recent paper, physical dissolution should be considered. The step-wise, high-temperature soaking is a simple and effective method for coal dissolution. Larger dissolution makes liquefaction severity lower. Broad molecular mass distribution in the associated coal was another important factor. The selective reaction of fractions with high molecular weight isolated after the high-temperature soaking makes gas yield lower. Tests using an autoclave by the concept shown in Figure 5 enabled to more oil and 15-20% less gas yields. It is expected that the procedure will result in great cost reduction in coal liquefaction.

  10. Urinary 1-hydroxypyrene: a biomarker for polycyclic aromatic hydrocarbon exposure in coal liquefaction workers.

    PubMed

    Quinlan, R; Kowalczyk, G; Gardiner, K; Hale, K; Walton, S; Calvert, I

    1995-04-01

    This study was undertaken to assess the suitability of urinary 1-hydroxypyrene (1-OHPyr) as a biological marker of polycyclic aromatic hydrocarbon (PAH) exposure in coal liquefaction workers. This is believed to be the first evaluation of the method in coal liquefaction workers. Ten workers were selected from a group of 30 workers considered likely to be at risk of contamination from PAHs by virtue of their jobs. Spot urine samples were collected at the start of a work period and at the end of each work shift, with analysis of 1-OHPyr being undertaken by high-performance liquid chromatography linked to a fluorescence detector. Exposure was assessed by the completion of questionnaires. Excretion of 1-OHPyr increased significantly over the working period, and there was a significant increase in 1-OHPyr where start-shift and end-shift samples were taken over one shift. A significant decrease in 1-OHPyr was found during breaks away from work.

  11. Microbial recovery of metals from spent coal liquefaction catalysts. [Thiobacillus denitrificans, Sulfolobus

    SciTech Connect

    Sperl, P.L.; Sperl, G.T.

    1991-01-01

    This project was initiated on October 1, 1989, for the purpose of recovering metals from spent coal liquefaction catalysts. The catalyst is a Ni-Mo catalyst supported on alumina (Shell 324) as is used in a pilot scale coal liquefaction facility at Wilsonville, Alabama. This plant is run and operated by Southern Clean Fuels. A large sample of spent catalyst from this facility has been obtained. The object of the contract is to treat the spent catalysts with microorganisms, especially Thiobacillus ferrooxidans, but also other Thiobacillus sp. and possibly Sulfolobus, and other potentially useful microorganisms to leach and remove the metals (Ni and Mo) form the spent catalysts into a form which can be readily recovered by conventional techniques.

  12. Microbial recovery of metals from spent coal liquefaction catalysts. Quarterly report, October--December 1991

    SciTech Connect

    Sperl, P.L.; Sperl, G.T.

    1991-12-31

    This project was initiated on October 1, 1989, for the purpose of recovering metals from spent coal liquefaction catalysts. The catalyst is a Ni-Mo catalyst supported on alumina (Shell 324) as is used in a pilot scale coal liquefaction facility at Wilsonville, Alabama. This plant is run and operated by Southern Clean Fuels. A large sample of spent catalyst from this facility has been obtained. The object of the contract is to treat the spent catalysts with microorganisms, especially Thiobacillus ferrooxidans, but also other Thiobacillus sp. and possibly Sulfolobus, and other potentially useful microorganisms to leach and remove the metals (Ni and Mo) form the spent catalysts into a form which can be readily recovered by conventional techniques.

  13. Microbial recovery of metals from spent coal liquefaction catalysts. Quarterly report, April--June 1991

    SciTech Connect

    Sperl, P.L.; Sperl, G.T.

    1991-12-31

    This project was initiated on October 1, 1989, for the purpose of recovering metals from spent coal liquefaction catalysts. Two catalyst types are the subject of the contract. The first is a Ni-Mo catalyst supported on alumina (Shell 324) as is used in a pilot scale coal liquefaction facility at Wilsonville, Alabama. A large sample of spent catalyst has been obtained. The second material is an unsupported ammonium molybdate catalyst used in a pilot process by the Department of energy at the Pittsburgh energy Technology Center. The object of the contract is to treat these spent catalysts with microorganisms, especially Thiobacillus ferrooxidans, but also other Thiobacillus sp. and possibly Sulfolobus, to leach and remove the metals (Ni and Mo) from the spent catalysts into a form which can be readily recovered by conventional techniques.

  14. Coal liquefaction process using pretreatment with a binary solvent mixture

    DOEpatents

    Miller, R.N.

    1986-10-14

    An improved process for thermal solvent refining or hydroliquefaction of non-anthracitic coal at elevated temperatures under hydrogen pressure in a hydrogen donor solvent comprises pretreating the coal with a binary mixture of an aromatic hydrocarbon and an aliphatic alcohol at a temperature below 300 C before the hydroliquefaction step. This treatment generally increases both conversion of coal and yields of oil. 1 fig.

  15. A characterization and evaluation of coal liquefaction process streams. Quarterly technical progress report, April 1--June 30, 1995

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1995-09-01

    The objectives of this project are to support the DOE direct coal liquefaction process development program and to improve the useful application of analytical chemistry to direct coal liquefaction process development. Independent analyses by well-established methods will be obtained of samples produced in direct coal liquefaction processes under evaluation by DOE. Additionally, analytical instruments and techniques which are currently underutilized for the purpose of examining coal-derived samples will be evaluated. The data obtained from this study will be used to help guide current process development and to develop an improved data base on coal and coal liquids properties. A sample bank will be established and maintained for use in this project and will be available for use by other researchers. The reactivity of the non-distillable resids toward hydrocracking at liquefaction conditions (i.e., resid reactivity) will be examined. From the literature and data experimentally obtained, a mathematical kinetic model of resid conversion will be constructed. It is anticipated that such a model will provide insights useful for improving process performance and thus the economics of direct coal liquefaction. The paper describes activities carried out this quarter. 11 refs., 21 figs., 17 tabs.

  16. A characterization and evaluation of coal liquefaction process streams. Quarterly technical progress report, January 1, 1996--March 31, 1996

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1996-07-01

    The objectives of this project are to support the DOE direct coal liquefaction process development program and to improve the useful application of analytical chemistry to direct coal liquefaction process development. This project builds on work performed in DOE Contract No. DE-AC22-89PC89883. Independent analyses by well-established methods are obtained of samples produced in direct coal liquefaction processes under evaluation by DOE. Additionally, analytical instruments and techniques which are currently under utilized for the purpose of examining coal-derived samples are being evaluated. The data obtained from this study is used to help guide current process development and to develop an improved data base on coal and coal liquids properties. A sample bank, established and maintained for use in this project, is available for use by other researchers. The reactivity of the non-distillable resids toward hydrocracking at liquefaction conditions (i.e., resid reactivity) is being examined. From the literature and data experimentally obtained, a mathematical kinetic model of resid conversion will be constructed. It is anticipated that such a model will provide insights useful for improving process performance and thus the economics of direct coal liquefaction.

  17. A characterization and evaluation of coal liquefaction process streams. Quarterly technical progress report, January 1, through March 31, 1995

    SciTech Connect

    1995-05-01

    The objectives of this project are to support the DOE direct coal liquefaction process development program and to improve the useful application of analytical chemistry to direct coal liquefaction process development. Independent analyses by well-established methods will be obtained of samples produced in direct coal liquefaction processes under evaluation by DOE. Additionally, analytical instruments and techniques which are currently underutilized for the purpose of examining coal-derived samples will be evaluated. The data obtained from this study will be used to help guide current process development and to develop an improved data base on coal and coal liquids properties. A sample bank will be established and maintained for use in this project and will be available for use by other researchers. The reactivity of the non-distillable resids toward hydrocracking at liquefaction conditions (i.e., resid reactivity) will be examined. From the literature and data experimentally obtained, a mathematical kinetic model of resid conversion will be constructed. It is anticipated that such a model will provide insights useful for improving process performance and thus the economics of direct coal liquefaction. Accomplishments for this quarter are described.

  18. Corrosion studies at the Wilsonville, Alabama, coal liquefaction facility during 1983

    SciTech Connect

    Keiser, J.R.; Olsen, A.R.; Newsome, J.F.; Howell, M.

    1984-10-01

    During 1983, Oak Ridge National Laboratory continued a study of materials performance at the Wilsonville, Alabama, Advanced Coal Liquefaction Research and Development Facility. Materials performance was evaluated by exposure and analysis of corrosion coupons and U-bend specimens, chemical analysis of related process streams, and ultrasonic determination of the thickness of walls of various components. The results of these studies are useful to current plant operators and to designers of future large-scale plants. 18 references, 4 figures, 12 tables.

  19. Dispersed catalysts for co-processing and coal liquefaction

    SciTech Connect

    Bockrath, B.; Parfitt, D.; Miller, R.

    1995-12-31

    The basic goal is to improve dispersed catalysts employed in the production of clean fuels from low value hydrocarbons. The immediate objective is to determine how the properties of the catalysts may be altered to match the demands placed on them by the properties of the feedstock, the qualities of the desired end products, and the economic constraints put upon the process. Several interrelated areas of the application of dispersed catalysts to co-processing and coal conversion are under investigation. The first involves control of the selectivity of MoS{sub 2} catalysts for HDN, HDS, and hydrogenation of aromatics. A second area of research is the development and use of methods to evaluate dispersed catalysts by means of activity and selectivity tests. A micro-flow reactor has been developed for determining intrinsic reactivities using model compounds, and will be used to compare catalysts prepared in different ways. Micro-autoclaves will also be used to develop data in batch experiments at higher partial pressures of hydrogen. The third area under investigation concerns hydrogen spillover reactions between MoS{sub 2} catalysts and carbonaceous supports. Preliminary results obtained by monitoring H{sub 2}/D{sub 2} exchange reactions with a pulse-flow microreactor indicate the presence of spillover between MoS{sub 2} and a graphitic carbon. A more complete study will be made at a later stage of the project. Accomplishments and conclusions are discussed.

  20. The dual role of oxygen functions in coal pretreatment and liquefaction: Crosslinking and cleavage reactions. Fifth quarterly report, April 1, 1992--June 30, 1992

    SciTech Connect

    Serio, M.A.; Kroo, E.; Teng, H.; Charpenay, S.; Solomon, P.R.

    1992-12-01

    Preparation of ion-exchanged (including barium, calcium and potassium) demineralized Zap and Wyodak has been completed. Both vacuum dried and moist samples were prepared, using procedures described previously. The modified samples were subjected to functional group analysis as KBr pellets with FT-IR, and programmed pyrolysis analysis with TG-FTIR. Liquefaction experiments of these samples were also performed and products were analyzed. The data show that both the pyrolytic tar and liquefaction yields decrease with the extent of ion-exchange, i.e., in the order of (demineralized) > (ion-exchanged at pH 8) > (ion-exchanged at pH 12.5). For the pyrolysis of vacuum dried samples, the tar yield was higher for the potassium-exchanged coals than the calcium and barium-exchanged samples, suggesting that bivalent cations tighten the coal structure by cross-linking coal fragments and make it more difficult for tar molecules to escape. The liquefaction results show that the potassium-exchanged samples have higher liquefaction yields (especially asphaltenes) than for the barium- and calcium-exchanged samples. This can probably be attributed to the same reason for the high pyrolytic tar yield, i.e., that bivalent cations can serve as a cross-linking agents to tighten the coal structure. Remoisturization of vacuum dried Zap and Wyodak was done in the attempt to understand if moisture uptake for low rank coals is a reversible process and to see if moisture influences the role of the cations. Preliminary results show that the moisture content can reach that of the raw samples by remoisturization for Zap, but not for Wyodak. Furthermore, the chemical structure of the coal samples seems to have been changed by remoisturization, since different C0{sub 2} evolution behaviors were observed.

  1. Coal liquefaction process streams characterization and evaluation: Application of liquid chromatographic separation methods to THF-soluble portions of integrated two-stage coal liquefaction resids

    SciTech Connect

    Green, J.B.; Pearson, C.D.; Young, L.L.; Green, J.A. )

    1992-05-01

    This study demonstrated the feasibility of using non-aqueous ion exchange liquid chromatography (NIELC) for the examination of the tetrahydrofuran (THF)-soluble distillation resids and THF-soluble whole oils derived from direct coal liquefaction. The technique can be used to separate the material into a number of acid, base, and neutral fractions. Each of the fractions obtained by NIELC was analyzed and then further fractionated by high-performance liquid chromatography (HPLC). The separation and analysis schemes are given in the accompanying report. With this approach, differences can be distinguished among samples obtained from different process streams in the liquefaction plant and among samples obtained at the same sampling location, but produced from different feed coals. HPLC was directly applied to one THF-soluble whole process oil without the NIELC preparation, with limited success. The direct HPLC technique used was directed toward the elution of the acid species into defined classes. The non-retained neutral and basic components of the oil were not analyzable by the direct HPLC method because of solubility limitations. Sample solubility is a major concern in the application of these techniques.

  2. A characterization and evaluation of coal liquefaction process streams. Quarterly technical progress report, July 1, 1996--September 30, 1996

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.

    1997-08-01

    CONSOL completed characterization of 64 samples from five run conditions of HTI Run ALC-1 (227-94), in which raw and cleaned (oil-agglomerated at low pH) Black Thunder Mine subbituminous coal was fed and processed using only dispersed catalysts in the liquefaction reactors. Extraction of THF-soluble resid from the pressure-filter cakes was more complete when agglomerates were fed, leaving only 5% or less THF solubles in the extracted cakes. When raw coal was fed, the extracted cakes contained 9-34% THF solubles. HTI also observed improved filtration during the periods that agglomerates were fed. Improved operability, if verified by additional work, could be an economically significant benefit of coal cleaning by oil agglomeration at low pH. An apparently higher Mo addition rate (see fourth bullet) may have contributed to the benefits of using oil-agglomerated coal. Other stream sample characteristics changed when oil-agglomerated coal was fed in Conditions 2-4, relative to when uncleaned coal was fed in Conditions 1 and 5. The ash content of the 0-6 bottoms samples was lower when oil-agglomerates were fed. The THF-soluble 524{degrees}C+ resid concentration in the feed slurry doubled when agglomerated coal was fed. Three factors may have influenced these characteristics. Higher coal conversion would have produced more resid. More efficient toluene-extraction of the filter cake would have recycled more resid. Removal of distillate as product to offset oil fed as part of the agglomerated coal would preferentially recycle the heaviest components.

  3. Novel bimetallic dispersed catalysts for temperature-programmed coal liquefaction. Technical progress report, October 1994--December 1994

    SciTech Connect

    Schmidt, E.; Kirby, S.; Song, Chunshan

    1995-02-01

    Coal liquefaction involves cleavage of methylene and dimethylene and ether-type bridges connecting polycyclic aromatic units. The selected compounds for model coal liquefaction reactions are 4-(l-naphthylmethyl)bibenzyl (NMBB) and several oxygen-containing compounds. This report mainly describes the synthesis and screening of selected iron and molybdenum compounds as precursors of dispersed catalysts for hydrocracking of NMBB and oxygen-containing compounds. Experiments using NMBB were carried out at 400{degrees}C for 30 min. under 6.9 MPa H{sub 2} pressure. All catalyst precursors converted NMBB predominately into naphthalene and 4-methylbibenzyl. Generally, ferrocene demonstrated very low activity as catalyst. Even sulfur addition did not increase activity. Hydrated iron sulfate FeSO{sub 4} x 7 H{sub 2}O gave similar conversion like ferrocene. In order to clarify the effect of sulfur alone on model compound conversion, NMBB was treated with sulfur in concentrations of 1.2 to 3.4 wt %, corresponding to conditions present in catalytic runs with sulfur. It was found that increasing sulfur concentrations lead to higher NMBB conversion. Furthermore, sulfur had a permanent influence on the reactor walls. It reacted with the transition metals in the steel to form a microscopic black iron sulfide layer on the surface, which could not be removed mechanically. Non catalytic runs after experiments with added sulfur yielded higher conversion than a normal run with a new reactor. The objective of the work on oxygen-compounds is to investigate the utility of highly dispersed catalysts, from organometallic precursors, in the removal of heteroatom functionality from the products of a reaction performed under liquefaction conditions. The bimetallic catalytic precursor CoMo-T2 exhibited a sizable increase in the yield of non-O-containing products, compared to the run using a standard inorganic catalyst precursor (ATTM) or a non-catalytic reaction.

  4. Status and economics of SRC-I coal liquefaction development

    SciTech Connect

    Tao, J.C.; Jones, J.P. III

    1982-11-01

    The results of commercial plant economic analysis indicate that the SRC-I technology is economically viable in the long-term. To achieve commercialization by the mid-1990s, it is necessary to proceed with the design, construction, and operation of the demonstration plant to prove the technical feasibility, economic viability, and environmental acceptability of the SRC-I technology. Today, synthetic fuels development no longer holds the urgency that elevated it to a position of national prominence a few years ago. However, most analysts agree that the underlying circumstances that will determine the U.S. energy future are unchanged. World oil supplies are dwindling, and the largest source of U.S. petroleum supplies remains one of the most politically volatile regions. In fact, the oil glut proclaimed only a few months ago shows signs of evaporating. Already, spot shortages of crucial energy products have been reported-most notably transportation fuels. The U.S. still has within its borders the largest coal reserves in the free world.

  5. The mechanism of hydrogen incorporation in coal liquefaction. Final report

    SciTech Connect

    1995-11-01

    The purpose of the research was to determine the detailed molecular mechanism for the introduction of hydrogen into coal when it is heated in an atmosphere of H{sub 2} in the absence of catalysts and to use this information as a baseline for the study of catalyzed processes. The plan was to study the reaction of model compounds with D{sub 2} in a glass-lined reactor of the authors` design and, by determining the distribution of D atoms in the reaction products, to deduce the reaction mechanism(s). As of the date of this report (Nov. 1995), the authors have, they believe conclusively, demonstrated the mechanism of the thermal process. They have studied several gas-phase reactions and, recently, have extended these to surface-immobilized models. The data are consistent in their support of the proposed sequence. Within the past year, they have begun to look at catalyzed hydrothermolysis and, while the work is at an early stage, they can draw a few significant conclusions, presented in the report.

  6. DIRECT LIQUEFACTION PROOF-OF-CONCEPT PROGRAM

    SciTech Connect

    A.G. Comolli; T.L.K. Lee; J. Hu; G. Popper; M.D. Elwell; J. Miller; D. Parfitt; P. Zhou

    1999-12-30

    This report presents the results of the bench-scale work, Bench Run PB-09, HTI Run Number 227-106, conducted under the DOE Proof-of-Concept Option Program indirect coal liquefaction at Hydrocarbon Technologies Inc. in Lawrenceville, New Jersey. Bench Run PB-09 was conducted using two types of Chinese coal, Shenhua No.2 and Shenhua No.3, and had several goals. One goal was to study the liquefaction performance of Shenhua No.2 and Shenhua No.3 with respect to coal conversion and distillate production. Another goal of Bench Run PB-09 was to study the effect of different GelCatw formulations and loadings. At the same time, the space velocity and the temperature of the fmt reactor, K-1, were varied to optimize the liquefaction of the two Chinese coals. The promoter-modified HTI GelCat{trademark} catalyst was very effective in the direct liquefaction of coal with nearly 92% maf coal conversion with Shenhua No.3 and 93% maf coal conversion with 9 Shenhua No.2. Distillate yields (CQ-524 C)varied from 52-68% maf for Shenhua No.3 coal to 54-63% maf for Shenhua No.2 coal. The primary conclusion from Bench Run PB-09 is that Shenhua No.3 coal is superior to Shenhua No.2 coal in direct liquefaction due to its greater distillate production, although coal conversion is slightly lower and C{sub 1}-C{sub 3} light gas production is higher for Shenhua No.3. The new promoter modified GelCat{trademark} proved successful in converting the two 9 Chinese coals and, under some conditions, producing good distillate yields for a coal-only bench run. Run PB-09 demonstrated significantly better performance of China Shenhua coal using HTI's coal direct liquefaction technology and GelCat{trademark} catalyst than that obtained at China Coal Research Institute (CCRI, coal conversion 88% and distillate yield 61%).

  7. Cooperative research in coal liquefaction. Final report, May 1, 1992--April 30, 1993

    SciTech Connect

    Huffman, G.P.

    1996-03-01

    Research on sulfate and metal (Mo, Sn) promoted Fe{sub 2}O{sub 3} catalysts in the current year focused on optimization of conditions. Parameters varied included temperature, solvent, solvent-to-coal ratio, and the effect of presulfiding versus in situ sulfiding. Oil yields were found to increase approximately proportionately with both temperature and solvent-to-coal ratio. The donor solvent, tetralin, proved to give better total conversion and oil yields than either 1-methylnaphthalene or Wilsonville recycle oil. A significant enhancement of both total liquefaction yields and oil yields from lignites and subbituminous coals has been achieved by incorporating iron into the coal matrix by cation exchange. A study has been conducted on the synthesis of iron, molybdenum, and tungsten catalysts using a laser pyrolysis technique.

  8. Quarterly report: Pumps-status of slurry pumps in coal liquefaction processes. Third quarter - CY 1981

    SciTech Connect

    1996-07-01

    This paper summarizes recent slurry pumps (centrifugal and reciprocal) operating experience in the liquefaction pilot plants. In addition, the activities concerning slurry pumps conducted in supporting research facilities are also noted. The purpose of the summary is to concentrate on the critical component problems common to all the liquefaction plants to avoid duplication of efforts, and to help provide timely solutions to the pump problems. The summary information used in this paper was obtained primarily from the Critical Component and Materials Meetings which are sponsored by the Office of Coal Processing of the Fossil Energy. The Department of Energy. Information from various Technical Reports published by the liquefaction plant personnel are also reviewed based on availability and relevance to topics covered in this report. It is intended that this report will be followed by updates as pertinent information concerning problem pumps becomes available. The following section s of the paper will provide a brief outline of early slurry pump experience as background material followed by a summary of recent slurry pump operating experience at liquefaction pilot plants.

  9. Fundamental Kinetics of Supercritical Coal Liquefaction: Effect of Catalysts and Hydrogen-Donor Solvents

    SciTech Connect

    McCoy, Ben J; Madras, Girodhar; Smith, J M; Kodera, Yoichi

    1997-04-16

    This is the quarterly report on our recent progress toward the overall objective to understand the supercritical fluid extraction of hydrocarbons from coal. Our strategy is to simulate coal as a high molecular-weight polymeric material by studying the degradation of polymers under various conditions. The hypothesis we are testing is that degradation of such macromolecules is applicable to the decomposition (depolymerization) of the coal network. Polymer degradation and coal liquefaction are influenced strongly by the solvent in the reaction. This motivated our investigation of the effect of hydrogen donor solvents on polymer degradation. In particular, we obtained new experimental data to show how a hydrogen donor, 6-hydroxy tetralin, influences the degradation rate of polystyrene. We also developed a detailed radical mechanism for hydrogen donation based on the Rice-Herzfeld chain reaction concept with the elementary steps of initiation, depropagation, hydrogen abstraction, and termination. Expressions for the degradation rate parameters were obtained by applying continuous distribution kinetics to the MWD of the reacting polymer. The theory explains the different influences of the hydrogen donor solvent on the degradation rate coefficients for different polymers. Though developed for the degradation of polymers, the mechanism and the theory are potentially applicable for chain scission and addition reactions among distributions of paraffins, olefins, and radicals of all chain lengths. The concepts can, in principle, be extended to examine the effect of hydrogen donors on coal liquefaction and on the complex mixture of liquefaction compounds. Based on this work, a research paper titled "Effect of Hydrogen Donors on Polymer Degradation", has been submitted for publication. Our research paper entitled, "Molecular weight effect on the dynamics of polystyrene degradation", has been accepted for publication by the journal, Industrial and Engineering Chemistry Research.

  10. Cooperative research in coal liquefaction. Final report, May 1, 1991--April 30, 1992

    SciTech Connect

    Huffman, G.P.

    1996-03-01

    Extensive research continued on catalysts based on novel anion-treated (mainly sulfated) oxides and oxyhydroxides of iron [Fe{sub x}O{sub y}/SO{sub 4}]. In addition, sulfated oxides of tin as well as molybdenum promoted iron oxides were used. Incorporation of small amounts of sulfate, molybdate, or tungstate anions by wet precipitation/impregnation methods was found to increase the surface acidic character of iron oxides; more importantly, it reduced the grain sizes significantly with corresponding increases in specific surface areas. These anion-treated iron and tin oxides were more active for direct coal liquefaction and coal-heavy oil coprocessing than their untreated counterparts. With these catalyst systems, higher conversion levels are obtained as compared to the soluble precursors of iron and molybdenum at the same catalyst metalloading (3500 ppm iron and 50 ppm molybdenum with respect to coal). Sulfated iron oxides and oxyhydroxides were equally active as coal liquefaction catalysts. The sulfate, molybdate, and tungstate anions were found to have similar promotional effects on the properties and activities of iron oxides. One step in the synthesis of anion-treated iron and tin oxides is precipitation as hydroxides using either urea or ammonium hydroxide. The catalysts prepared using urea as a precipitation agent were more reproducible than those using ammonium, hydroxide in terms of activities and properties. These catalysts/catalyst precursors were characterized by several techniques to determine their physical (size and structure related) and chemical (acidity) properties. Sulfated and molybdated iron oxides were found to have grain sizes as small as 10-20 nm. An attempt was made to correlate the physicochemical properties of these catalysts with their activity for coal liquefaction.

  11. Novel nanodispersed coal liquefaction catalysts: Molecular design via microemulsion-based synthesis. Final technical report, October 1990--December 1994

    SciTech Connect

    Osseo-Asare, K.; Boakye, E.; Vittal, M.

    1995-04-01

    This report described the synthesis of Molybdenum Sulfides in microemulsions by acidification of ammonium tetrathiomolybdate. Molybdenum Sulfides have been shown to be potential coal liquefaction catalysts. The importance of particle size, temperature effects, and coal surface chemistry to impregnation are discussed.

  12. Novel bimetallic dispersed catalysts for temperature-programmed coal liquefaction. Technical progress report, October--December 1992

    SciTech Connect

    Song, Chunshan; Schobert, H.H.

    1993-02-01

    Development of new catalysts is a promising approach to more efficient coal liquefaction. It has been recognized that catalysts are superior to supported catalysts for primary liquefaction of coals, because the control of initial coal dissolution or depolymerization requires intimate contact between the catalyst and coal. This research is a fundamental and exploratory study on catalytic coal liquefaction, with the emphasis on the development of novel bimetallic dispersed catalysts for temperature-programmed liquefaction. The ultimate goal of the present research is to develop novel catalytic hydroliquefaction process using highly active dispersed catalysts. The primary objective of this research is to develop novel bimetallic dispersed catalysts from organometallic molecular that can be used in low precursors concentrations (< 1 %) but exhibit high activity for efficient hydroliquefaction of coals under temperature-programmed conditions. The major technical approaches are, first, to prepare the desired heteronuclear organometallic molecules as catalyst precursors that contain covalently bound, two different metal atoms and sulfur in a single molecule. Such precursors will generate finely dispersed bimetallic catalysts such as Fe-Mo, Co-Mo and Ni-Mo binary sulfides upon thermal decomposition. The second major technical approach is to perform the liquefaction of coals unpregnated with the organometallic precursors under temperature-programmed conditions, where the programmed heat-up serves as a step for both catalyst activation and coal pretreatment or preconversion. Two to three different complexes for each of the Fe-Mo, Co-Mo, and Ni-Mo combinations will be prepared. Initial catalyst screening tests will be conducted using a subbituminous coal and a bituminous coal. Effects of coal rank and solvents will be examined with the selected bimetallic catalysts which showed much higher activity than the dispersed catalysts from conventional precursors.

  13. Development of significantly improved catalysts for coal liquefaction and upgrading of coal extracts. Quarterly progress report No. 4, July 1-September 30, 1982

    SciTech Connect

    Sinha, V.T.; Kutzenco, P.D.; Preston, W.J.; Brinen, J.S.; Graham, S.W.; Butensky, M.; Muchnick, T.L.; Hyman, D.

    1982-01-01

    Cold flow ebullation tests to determine the ranges of operability of bead catalysts continued. Data reported show the effects of higher catalyst density, wider particle size distributions, and higher fluid viscosity on ebullation of bead catalysts. A relation for determining limiting diameters in a liquid-solid fluidized bed was developed. Correlation of the three-phase data is being investigated. The CSTR Catalyst Aging Test Unit is described. The system operates under computer control. High pressure hydrogen and coal slurry are fed continuously to a one-liter stirred autoclave. High pressure nitrogen for inerting and flush oil are used in the event of an interlock shutdown. The product is passed to a 3-gallon collection vessel or to a smaller sampling vessel during material balance periods. The gas disentrains from the mixture and is scrubbed. Analytical techniques to be used in the course of the catalyst testing program were evaluated. H-COAL PDU products and SRC-II Heavy distillate were analyzed. Standard deviations for many of the procedures were determined. Specific methods are summarized. Development of surface analytical techniques to study coal liquefaction catalysts focused on used Amocat 1A catalysts from coal run 10 at the H-COAL Pilot Plant. Preliminary results of analysis by ESCA and x-ray microprobe are given.

  14. Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama. Run 262 with Black Thunder subbituminous coal: Technical progress report

    SciTech Connect

    Not Available

    1992-09-01

    This report presents the results of Run 262 performed at the Advanced Coal Liquefaction R&D Facility in Wilsonville, Alabama. The run started on July 10, 1991 and continued until September 30, 1991, operating in the Close-Coupled Integrated Two-Stage Liquefaction mode processing Black Thunder Mine subbituminous coal (Wyodak-Anderson seam from Wyoming Powder River Basin). A dispersed molybdenum catalyst was evaluated for its performance. The effect of the dispersed catalyst on eliminating solids buildup was also evaluated. Half volume reactors were used with supported Criterion 324 1/16`` catalyst in the second stage at a catalyst replacement rate of 3 lb/ton of MF coal. The hybrid dispersed plus supported catalyst system was tested for the effect of space velocity, second stage temperature, and molybdenum concentration. The supported catalyst was removed from the second stage for one test period to see the performance of slurry reactors. Iron oxide was used as slurry catalyst at a rate of 2 wt % MF coal throughout the run (dimethyl disulfide (DMDS) was used as the sulfiding agent). The close-coupled reactor unit was on-stream for 1271.2 hours for an on-stream factor of 89.8% and the ROSE-SR unit was on-feed for 1101.6 hours for an on-stream factor of 90.3% for the entire run.

  15. Chemical and toxicological aspects of coal liquefaction and other complex mixtures.

    PubMed

    Gray, R H

    1984-12-01

    Chemists, biologists, and ecologists at Battelle's Pacific Northwest Laboratories are developing a data base to aid engineers in the safe design of coal liquefaction process options. Objectives of this effort have been to identify and evaluate long-term health and environmental issues, evaluate options to permit environmentally acceptable design, and assess risk to man and the environment from deployment of a large-scale coal liquefaction industry. Chemically complex materials produced by various coal liquefaction processes, and under various stages of process design and operating conditions, have been screened for potential health and environmental effects. Biologically active materials have been fractionated and rescreened. Chemical constituents of biologically active fractions have been identified, and the environmental fate of problematic agents is currently being determined. This approach, linking engineering and life sciences research, is also relevant to the development of other energy technologies and industries that produce chemically complex materials. Results indicate that full-boiling-range coal-derived liquids are generally more active than shale oil and petroleum crudes in biological and ecological test systems. Several biologically active agents have been identified, including primary aromatic amines (PAA), polynuclear aromatic hydrocarbons (PAH), and phenols. Some components of coal-derived materials are taken up by biota and metabolized. Hydrotreating, a refining or upgrading process, reduces PAA, PAH, and phenol content, as well as mutagenicity, carcinogenicity, and toxicity of coal liquids. Selective distillation restricts PAA and PAH content, as well as mutagenicity and carcinogenicity to high-boiling-range coal liquids. Other process conditions (i.e., extraction severity, catalyst age, etc.) and environmental factors influence chemical characteristics and biological activity of coal-derived materials. Eliminating toxic input of coal liquids to

  16. Instrumentation impulse-line plugging in coal-liquefaction-process application. [1/2 in. diam. tubes

    SciTech Connect

    Carr, K.R.

    1983-02-01

    Instrumentation impulse line systems in coal liquefaction process applications were studied for the purpose of seeking methods by which the problem of line plugging can be alleviated or eliminated. The emphasis was on purged systems in which approx. 1/2-in.-diam lines carry a purge fluid at a low flow rate (approx. 2 gph or 5 scfm) to provide a pressure transmitting medium between a process solids-bearing liquid and the measuring instrument. Plugging of impulse lines is a maintenance harassment and can cause periods of degraded measurements accuracy in coal liquefaction as well as other important industries, such as petroleum refining. The approach taken in this work was to compile information on purged instrumentation impulse line systems design and operating experience, to formulate and record recommended practices for coal liquefaction processes, and to define possibilities for alternative systems. Sources of information utilized were the personnel of five operating coal liquefaction facilities, applications engineers for suppliers of pressure measurement and flow control equipment, process control engineers in petroleum refining, and the literature. This report includes a description of the purged impulse lines application and problems, a summary of recommended practives for purged impulse line systems in coal liquefaction processes based on a compilation of operating experiences, and a discussion of possibilities for unpurged impulse lines systems which should be experimentally evlauated in process locations which might yield the greatest potential benefit. Also, the study idnetified a development need for a purge fluid flow rate controller to be used in conventional impulse lines.

  17. Steam pretreatment for coal liquefaction. Fourth quarterly report, 1 July 1991--30 September 1991

    SciTech Connect

    Graff, R.A.; Balogh-Nair, V.

    1992-06-18

    Steam pretreatment is the reaction of coal with steam at temperatures well below those usually used for solubilization. The objective of the proposed work is to test the application of steam pretreatment to coal liquefaction. A 300 ml stirred autoclave for liquefaction tests is being installed. Pretreatment and extraction tests were made with Blind Canyon coal alone, mixed with Illinois No. 6 coal, impregnated with iron, and impregnated with iron and sulfided using phenyl disulfide. Measurements show an increase in volatiles yield and a decrease in extraction yield with catalyst addition. These results are not yet definitive, because both yields may be artificially decreased by insoluble residue from phenyl disulfide. About one ram of purified {alpha}-naphthylmethyl phenyl ether was prepared and an additional 0. 8 gram were synthesized. Steam pretreatment of the model compound {alpha}-benzylnaphthyl ether was repeated with a Pyrex liner for the reactor tube. No differences have yet appeared as a result of using this liner (compared to bare stainless steel), evidence against any catalytic wall effect.

  18. A characterization and evaluation of coal liquefaction process streams. Quarterly technical progress report, July 1--September 30, 1995

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1995-12-01

    The objectives of this project are to support the DOE direct coal liquefaction process development program and to improve the useful application of analytical chemistry to direct coal liquefaction process development. Independent analyses by well-established methods will be obtained of samples produced in direct coal liquefaction processes under evaluation by DOE. Additionally, analytical instruments and techniques which are currently underutilized for the purpose of examining coal-derived samples will be evaluated. The data obtained from this study will be used to help guide current process development and to develop an improved data base on coal and coal liquids properties. A sample bank will be established and maintained for use in this project and will be available for use by other researchers. The reactivity of the non-distillable resids toward hydrocracking at liquefaction conditions (i.e., resid reactivity) will be examined. From the literature and data experimentally obtained, a mathematical kinetic model of resid conversion will be constructed. It is anticipated that such a model will provide insights useful for improving process performance and thus the economics of direct coal liquefaction. Some of the contract activities for this quarter are: We completed many of the analyses on the 81 samples received from HTI bench-scale run CMSL-9, in which coal, coal/mixed plastics, and coal/high density polyethylene were fed; Liquid chromatographic separations of the 15 samples in the University of Delaware sample set were completed; and WRI completed CP/MAS {sup 13}C-NMR analyses on the Delaware sample set.

  19. A characterization and evaluation of coal liquefaction process streams. Quarterly technical progress report, October 1--December 31, 1995

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1996-05-01

    The objectives of this project are to support the DOE direct coal liquefaction process development program and to improve the useful application of analytical chemistry to direct coal liquefaction process development. Independent analyses by well-established methods will be obtained of samples produced in direct coal liquefaction processes under evaluation by DOE. Additionally, analytical instruments and techniques which are currently underutilized for the purpose of examining coal-derived samples will be evaluated. The data obtained from this study will be used to help guide current process development and to develop an improved data base on coal and coal liquids properties. During this reporting period, CONSOL completed analyses of 81 feed and process stream samples from HTI bench Run CMSL-9. HTI liquefaction bench unit Run CMSL-9 (227-87) was operated with all-dispersed catalyst and Black Thunder Mine (Wyodak and Anderson seam) coal, with and without mixed plastics or high density polyethylene (HDPE) as coprocessing feedstocks. The dispersed catalysts used were Molyvan A and HTI`s iron catalyst, a sulfated iron hydroxide. Results are discussed in this report.

  20. Survey study of the efficiency and economics of hydrogen liquefaction

    NASA Technical Reports Server (NTRS)

    1975-01-01

    The production of liquid hydrogen, with coal as the starting material, is reported. The minimum practicable energy and cost for liquefaction of gaseous hydrogen in the 1985-2000 time period is presented to investigate the possible benefits of the integration of coal gasification processes with the liquefaction process.

  1. Advanced liquefaction using coal swelling and catalyst dispersion techniques. Volume 2, appendices. Final technical report, October 1, 1991--September 30, 1994

    SciTech Connect

    Curtis, C.W.; Chander, S.; Gutterman, C.

    1995-04-01

    Liquefaction experiments were undertaken using subbituminous Black Thunder mine coal to observe the effects of aqueous SO{sub 2} coal beneficiation and the introduction of various coal swelling solvents and catalyst precursors. Aqueous SO{sub 2} beneficiation of Black Thunder coal removed alkali metals and alkaline earth metals, increased the sulfur content and increased the catalytic liquefaction conversion to THF solubles compared to untreated Black Thunder coal. The liquefaction solvent had varying effects on coal conversion, depending upon the type of solvent added. The hydrogen donor solvent, dihydroanthracene, was most effective, while a coal-derived Wilsonville solvent promoted more coal conversion than did relatively inert 1-methylnaphthalene. Swelling of coal with hydrogen bonding solvents tetrahydrofuran (THF), isopropanol, and methanol, prior to reaction resulted in increased noncatalytic conversion of both untreated and SO{sub 2} treated Black Thunder coals, while dimethylsulfoxide (DMSO), which was absorbed more into the coal than any other swelling solvent, was detrimental to coal conversion. Swelling of SO{sub 2} treated coal before liquefaction resulted in the highest coal conversions; however, the untreated coal showed the most improvements in catalytic reactions when swelled in either THF, isopropanol, or methanol prior to liquefaction. The aprotic solvent DMSO was detrimental to coal conversion.

  2. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction. Final report, September 20, 1991--September 19, 1993

    SciTech Connect

    Not Available

    1993-09-01

    One of the main goals for competitive coal liquefaction is to decrease gas yields to reduce hydrogen consumption. Complexing this element as methane and ethane decreases process efficiently and is less cost effective. To decrease the gas yield and increase the liquid yield, an effective preconversion process has been explored on the basis of the physically associated molecular nature of coal. Activities have been focused on two issues: (1) maximizing the dissolution of associated coal and (2) defining the different reactivity associated with a wide molecular weight distribution. Two-step soaking at 350{degrees}C and 400{degrees}C in a recycle oil was found to be very effective for coal solubilization. No additional chemicals, catalysts, and hydrogen are required for this preconversion process. High-volatile bituminous coals tested before liquefaction showed 80--90% conversion with 50--55% oil yields. New preconversion steps suggested are as follows: (1) dissolution of coal with two-step high-temperature soaking, (2) separation into oil and heavy fractions of dissolved coal with vacuum distillation, and (3) selective liquefaction of the separated heavy fractions under relatively mild conditions. Laboratory scale tests of the proposed procedure mode using a small autoclave showed a 30% increase in the oil yield with a 15--20% decrease in the gas yield. This batch operation projects a substantial reduction in the ultimate cost of coal liquefaction.

  3. Bimetallic promotion of cooperative hydrogen transfer and heteroatom removal in coal liquefaction. Quarterly summary, June 1, 1991--August 31, 1991

    SciTech Connect

    Eisch, J.J.

    1991-10-01

    The ultimate objective of this research is to uncover new catalytic processes for the liquefaction of coal and for upgrading coal-derived fuels by removing undesirable organosulfur, organonitrogen and organooxygen constituents. Basic to both the liquefaction of coal and the purification of coal liquids is the transfer of hydrogen from such sources as dihydrogen, metal hydrides or partially reduced aromatic hydrocarbons to the extensive aromatic rings in coal itself or to aromatic sulfides, amines or ethers. Accordingly, this study is exploring how such crucial hydrogen-transfer processes might be catalyzed by soluble, low-valent transition metal complexes and/or Lewis acids under moderate conditions of temperature and pressure. By learning the mechanism whereby H{sub 2}, metal hydrides or partially hydrogenated aromatics do transfer hydrogen to model aromatic compounds, with the aid of homogeneous, bimetallic catalysts, we hope to identify new methods for producing superior fuels from coal.

  4. Letdown valve (anti eroded type for slurry use) on 150 t/d coal liquefaction pilot plant

    SciTech Connect

    Kamada, Mitsushi; Kobayashi, Masatoshi; Yoshida, Haruhiko; Yamagiwa, Hisashi

    1999-07-01

    The letdown valve developed by NEDO has been tested on the 150 t/d coal liquefaction pilot plant using the NEDOL process for more than 6,000 hours of on-coal operation. Several factors affecting the damage of the letdown valve that handled a fluid containing coal-derived oil, catalyst and residue including ash have been evaluated. The countermeasure for the damage has been studied to develop an advanced letdown valve to be used demonstration plant.

  5. Process for coal liquefaction by separation of entrained gases from slurry exiting staged dissolvers

    DOEpatents

    Givens, Edwin N.; Ying, David H. S.

    1983-01-01

    There is described an improved liquefaction process by which coal is converted to a low ash and low sulfur carbonaceous material that can be used as a fuel in an environmentally acceptable manner without costly gas scrubbing equipment. In the process, coal is slurried with a solvent, passed through a preheater and at least two dissolvers in series in the presence of hydrogen-rich gases at elevated temperatures and pressures. Solids, including mineral ash and unconverted coal macerals are separated from the condensed dissolver effluent. In accordance with the improved process, fresh hydrogen is fed to each dissolver and the entrained gas from each dissolver is separated from the slurry phase and removed from the reactor system before the condensed phase is passed to the next dissolver in the series. In accordance with another process, the feeds to the dissolvers are such that the top of each downstream dissolver is used as a gas-liquid separator.

  6. Catalytic coal liquefaction. Final technical report, June 1, 1981-May 31, 1984

    SciTech Connect

    Weller, S.W.

    1984-07-01

    Molybdenum catalysts (both supported and unsupported) have been examined in various stages of preparation and use with respect to BET surface area and low temperature oxygen chemisorption. The results are detailed. X-ray diffraction has been used to characterize ammonium molybdate - after calcination, heated in tetralin under nitrogen and after use in an autoclave. Metal salts have been tested for catalytic effects by heating a tetralin-coal mixture (without hydrogen) at a loading of 1% of the coal. Only ammonium heptamolybdate and stannous chloride had a large incremental effect (based on blank runs with tetralin and catalyst without coal). Differences in liquefaction behavior in tubing bombs and in autoclaves are explained by thermodynamic considerations based on the gas to liquid volume in the two cases. (LTN)

  7. Advanced direct coal liquefaction concepts. Quarterly report, April 1, 1993--June 30, 1993

    SciTech Connect

    Berger, D.J.; Parker, R.J.; Simpson, P.L. |

    1993-11-01

    Construction and commissioning of the bench unit for operation of the first stage of the process was completed. Solubilization of Black Thunder coal using carbon monoxide and steam was successfully demonstrated in the counterflow reactor system. The results were comparable with those obtained in the autoclave with the exception that coal solubilization at the same nominal residence times was slightly lower. The bench unit has now been modified for two stage operation. The Wilsonville process derived solvent for Black Thunder coal (V-1074) was found to be essentially as stable as the previous solvent used in the autoclave runs (V-178 + 320) at reactor conditions. This solvent (V-1074) is, therefore, being used in the bench unit tests. Carbon monoxide may be replaced by synthesis gas for the coal solubilization step in the process. However, in autoclave tests, coal conversion was found to be dependent on the amount of carbon monoxide present in the synthesis gas. Coal conversions ranged from 88% for pure carbon monoxide to 67% for a 25:75 carbon monoxide/hydrogen mixture at equivalent conditions. Two stage liquefaction tests were completed in the autoclave using a disposable catalyst (FeS) and hydrogen in the second stage. Increased coal conversion, higher gas and oil and lower asphaltene and preasphaltene yields were observed as expected. However, no hydrogen consumption was observed in the second stage. Other conditions, in particular, alternate catalyst systems will be explored.

  8. Liquefaction of low rank coals with slurry catalysts. Part I. Comparison of coals. [7 low rank coals

    SciTech Connect

    Not Available

    1984-07-01

    One of the most significant achievements over the last several years in development of the SRC-II process was extension of its applicability to include low-rank coals. With addition of moderate amounts of pyrite, operation was trouble-free and oil yields exceeding those obtainable with higher rank feedstocks were obtained. In addition, product sulfur level was lower due to the relatively low sulfur content of the lower rank coals. Total oil yield generally decreased as rank decreased from high volatile C bituminous to lignite. An exception to this was the oil yield from Texas lignite, which was the highest of those from the seven coals evaluated. Oil yields from all of these coals were greater than those generally obtained from higher rank bituminous coals, however. There was no apparent correlation between rank and conversion to pyridine-soluble material. The distillate products fom these coals were similar in composition, but the hydrogen and heteroatom levels were related to those in the feed coal. 2 figures, 6 tables.

  9. Gasification of residual materials from coal liquefaction. Type I evaluation of H-Coal Liquefaction Residue from Illinois No. 6 coal as a feedstock for the Texaco Gasification Processes

    SciTech Connect

    Robin, A.M.

    1981-11-01

    A laboratory evaluation of a 20-pound sample of Vacuum Tower Bottoms from the H-Coal liquefaction pilot plant at Catlettsburg, Kentucky was completed at Texaco's Montebello Research Laboratory. The sample, which was obtained from the liquefaction of Illinois No. 6 coal, was judged to be a suitable feedstock for the Texaco Gasification Processes. It can be charged directly to the gasifier as a molten fluid at a temperature of about 450/sup 0/F or it may be charged at ambient temperature as a water slurry of ground residue. Based on these results, operating conditions and yields were estimated for gasifying 1000 pounds per hour of molten undiluted residue and for gasifying 1600 pounds per hour of solid residue in a water slurry both at a pressure of 1200 psig.

  10. Highly Dispersed Pseudo-Homogeneous and Heterogeneous Catalysts Synthesized via Inverse Micelle Solutions for the Liquefaction of Coal

    SciTech Connect

    Hampden-Smith, M.; Kawola, J.S.; Martino, A.; Sault, A.G.; Yamanaka, S.A.

    1999-01-05

    The mission of this project was to use inverse micelle solutions to synthesize nanometer sized metal particles and test the particles as catalysts in the liquefaction of coal and other related reactions. The initial focus of the project was the synthesis of iron based materials in pseudo-homogeneous form. The frost three chapters discuss the synthesis, characterization, and catalyst testing in coal liquefaction and model coal liquefaction reactions of iron based pseudo-homogeneous materials. Later, we became interested in highly dispersed catalysts for coprocessing of coal and plastic waste. Bifunctional catalysts . to hydrogenate the coal and depolymerize the plastic waste are ideal. We began studying, based on our previously devised synthesis strategies, the synthesis of heterogeneous catalysts with a bifunctional nature. In chapter 4, we discuss the fundamental principles in heterogeneous catalysis synthesis with inverse micelle solutions. In chapter 5, we extend the synthesis of chapter 4 to practical systems and use the materials in catalyst testing. Finally in chapter 6, we return to iron and coal liquefaction now studied with the heterogeneous catalysts.

  11. Liquefaction of low rank coals with slurry catalysts. Part III. Variable effects. [Low rank coal

    SciTech Connect

    Not Available

    1984-07-01

    One of the most significant achievements over the last several years in development of the SRC II process was extension of its applicability to include low-rank coals. With addition of moderate amounts of pyrite, operation was trouble-free and oil yields exceeding those obtainable with higher rank feedstocks were achieved. In addition, product sulfur level was lower due to the relatively low sulfur content of the lower rank coals. The effects of run conditions with low-rank coals and added pyrite are discussed in this report. The ratio of distillate product to hydrocarbon gas produced (or hydrogen consumed) is increased by lowering the reaction temperature over the range of 450/sup 0/C (842/sup 0/F) to 420/sup 0/C (788/sup 0/F). The oil production rate is also decreased, so there is an economic tradeoff between reactor vessel size and hydrogen production requirements. Raising the temperature above 450/sup 0/C (842/sup 0/F) at 1.0 hour residence time is detrimental, resulting in increased gas make, reduced oil yield and less conversion to pyridine-soluble components. Operation and yields at 450/sup 0/C (842/sup 0/F) and 1.0 hour residence time are improved by increasing the pressure to 2250 from 1800 psig. Operation is not possible at 1600 psig. 5 figures, 7 tables.

  12. Coal liquefaction process streams characterization and evaluation. Quarterly technical progress report, January 1--March 31, 1992

    SciTech Connect

    Robbins, G.A.; Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1992-08-01

    This is the tenth Quarterly Technical Progress Report under DOE Contract DE-AC22-89PC89883. Process oils from Wilsonville Run 262 were analyzed to provide information on process performance. Run 262 was operated from July 10 through September 30, 1991, in the thermal/catalytic Close-Coupled Integrated Two-Stage Liquefaction (CC-ITSL) configuration with ash recycle. The feed coal was Black Thunder Mine subbituminous coal. The high/low temperature sequence was used. Each reactor was operated at 50% of the available reactor volume. The interstage separator was in use throughout the run. The second-stage reactor was charged with aged Criterion 324 catalyst (Ni/Mo on 1/16 inch alumina extrudate support). Slurry catalysts and sulfiding agent were fed to the first-stage reactor. Molyvan L is an organometallic compound which contains 8.1% Mo, and is commercially available as an oil-soluble lubricant additive. It was used in Run 262 as a dispersed hydrogenation catalyst precursor, primarily to alleviate deposition problems which plagued past runs with Black Thunder coal. One test was made with little supported catalyst in the second stage. The role of phenolic groups in donor solvent properties was examined. In this study, four samples from direct liquefaction process oils were subjected to O-methylation of the phenolic groups, followed by chemical analysis and solvent quality testing.

  13. Additive effect of waste tire on the hydrogenolysis reaction of coal liquefaction residue

    SciTech Connect

    Motoyuki Sugano; Daigorou Onda; Kiyoshi Mashimo

    2006-12-15

    A numerous amount of waste tire is landfilled or dumped all over the world, which causes environmental problems, such as destruction of natural places and the risk of fires. On the other hand, the coal liquefaction residue (CLR) is produced in 30% yield through the process supporting unit (PSU) of the NEDOL coal liquefaction process. Therefore, the investigation on an effective method for utilization of waste tire and CLR is required. In this study, the simultaneous hydrogenolysis of CLR and pulverized waste tire was carried out by using tetralin. The yields in the simultaneous hydrogenolysis were compared with algebraic sum of the yields of the individual hydrogenolyses of waste tire alone and coal alone. In the simultaneous hydrogenolysis, the synergistic effects to upgrading, such as an increase in the yield of the oil constituent and a decrease in the yield of the asphaltene constituent, occurred because of the stabilization of asphaltenic radicals from CLR with aliphatic radicals from tire. The decrease in asphaltene yield in the simultaneous hydrogenolysis was pronounced with the increase in the tire:CLR ratio because the solvent effects of liquefied tire, such as stabilization of radicals, hydrogen shuttling, and heat transfer, were enhanced. Accordingly, it is estimated that the simultaneous hydrogenolysis of CLR and waste tire is an effective method for processing both materials. 15 refs., 3 figs., 2 tabs.

  14. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Technical progress report, October 1993--December 1993

    SciTech Connect

    Song, C.; Huang, L.; Wenzel, K.A.; Hatcher, P.G.; Schobert, H.H.

    1994-02-01

    In this quarter, progress has been made in the following two aspects: The influences of temperature, dispersed Mo catalyst, and solvent on the liquefaction conversion and composition of products from low-rank coals; and the hydrous pyrolysis of a lignite and spectroscopic characterization of its structural transformation during the hydrous pyrolysis. The analytical work described in this quarter also represents molecular-level characterization of products. The purpose of the first part of the work described in this quarter is to study the influences of temperature, solvent and dispersed Mo catalyst on the liquefaction conversion and chemical composition of the products. Many specialty chemicals, including one- to four-ring aromatics, could potentially be produced by liquefying coal. To achieve this goal, not only a high coal conversion but also a desirable product distribution is necessary. Therefore, it is of great importance to understand the structural changes of the coal during reaction and to investigate the conditions under which the aliphatics or aromatics can be removed from the macromolecular structure of coal. This quarterly report also describes the hydrous pyrolysis of Potapsco lignite and spectroscopic characterization of its structural transformation during the hydrous pyrolysis. This work has some implications both on the structural changes of low-rank coals during pretreatment and on the geochemical reactions during coalification stage. Vitrinite, a major component of most coals, is derived from degraded wood in ancient peat swamps. Organic geochemical studies conducted on a series of coalified wood samples derived mostly from gymnosperms have allowed the development of a chemical reaction series to characterize the major coalification reactions which lignin, the major coal-producing component of wood, undergoes.

  15. Liquefaction of low rank coals with slurry catalysts. Part II. Comparison of catalysts. [Low rank coals

    SciTech Connect

    Not Available

    1984-07-01

    One of the most significant achievements over the last several years in development of the SRC-II process was extension of its applicability to include low rank coals. With addition of moderate amounts of pyrite, operation was trouble free and oil yields exceeding those obtainable with higher rank feedstocks were obtained. In addition, product sulfur level was lower due to the relatively low sulfur content of the lower rank coals. Pyrite was the first catalyst tried and numerous other materials were investigated in an attempt to find a better additive. These included emulsions (Mo, Fe and Ni/Mo), ferric oxide alone and doped with Mo, iron on Al/sub 2/O/sub 3/ and several sources of H/sub 2/S. None were found to be more effective, and on the basis of cost, pyrite is still preferred. Additive levels much lower than those used initially were found to be sufficient for smooth operation. As little as 0.6 wt % FeS/sub 2/, based on MF Belle Ayr coal, provided satisfactory operation, which makes use of low rank coals in the SRC II process even more attractive. 8 figures, 6 tables.

  16. Synthesis of model compounds for coal liquefaction research. Final report, April 15, 1990--April 14, 1991

    SciTech Connect

    Not Available

    1991-11-01

    Coal liquefaction investigations required the availability of model compounds for mechanistic investigations. Towards this end, IITRI was funded to develop an approach for the synthesis of one of the target compound. This study was carried out in several phases as outlined here. Initial synthetic investigations on obtaining 2-tetrolol was carried out using high pressure and temperature reduction with Raney nickel catalyst. The next step consisted in incorporation of a hydroxymethyelene group at the C-3 position. This was successfully carried out utilizing 2-tetrolol, formaldehyde, and calcium oxide. An alternate improved method was developed using 3-carboxyl-2-naphthol. This required less time, gave a cheer product in higher yield. Efforts at the introduction of a chloromethylene group only yielded polymeric material or starting material in spite of protection the phenolic group by various groups. They synthesis of 3, 5-dimethyl-6- bromobenzyl chloride was successfully carried out by performing the Blank reaction of 2, 4-dimethyl bromobenzene. The product was characterized by GC/MS. Purification was not possible, as it was a complex mixture. Efforts at converting it to the acetate followed by separation to was not feasible. Unlike in the case of 2- hydroxyteralol, hydroxymetylation by established procedure yielded only the starting materials. Commercially available 4-methoxy-1- maphthaldehyde was protected as the ethylene acetal. The Wittig reagent 3-chlorobenzyl phosphonium bromide was prepared and condensed with 4-methoxy-1-napthaldehyde successfully and proved that the overall synthetic approach was proceeding in the desired direction. All the necessary intermediates have been synthesized,and we have demonstrated using model compounds, that the synthetic objective can be attained.

  17. Exploratory research on direct coal liquefaction using a high-pressure and high-temperature polarizing microscope

    SciTech Connect

    Wender, I.; Panvelker, S.; Wen, M.

    1988-09-01

    A high-pressure and high-temperature polarizing microscope has been developed. This instrument was used to study (1) liquefaction of Illinois No. 6 and Wyodak coals in the presence of molten-salt and liquid (organometallic) catalysts, (2) behavior of individual coal macerals, and (3) mesophase formation from solvent refined coal and coal asphaltenes. The instrument was found to be particularly suited to study mesophase formation through the use of polarized light and to study materials such as macerals, the basic constituents of coals. The macerals are usually available only in milligram quantities. 4 refs., 9 figs., 2 tabs.

  18. Selective enrichment of phenols from coal liquefaction oil by solid phase extraction method

    SciTech Connect

    Tian, M.; Feng, J.

    2009-07-01

    This study focuses on the solid phase extraction method for the enrichment and separation of phenol from coal liquefaction oil. The phenols' separation efficiency was compared on different solid phase extraction (SPE) cartridges, and the effect of solvents with different polarity and solubility parameter on amino-bonded silica was compared for selection of optimal elution solution. The result showed that amino-bonded silica has the highest selectivity and best extraction capability due to two factors, weak anion exchange adsorption and polar attraction adsorption.

  19. Solvent tailoring in coal liquefaction. Quarterly report, July-September 1983

    SciTech Connect

    Tarrer, A.R.; Curtis, C.W.; Guin, J.A.; Williams, D.C.

    1983-01-01

    A series of twenty-three aromatic compounds were ranked for their donor solvent efficacy for the dissolution of Western Kentucky No. 9/14 coal. The transfer of hydrogen from the solvent to the coal fragments, as measured by coal conversion, was examined at three levels of available hydrogen. The hydrogen donors are ranked according to their ability to convert coal to THF solubles. Aromatic analogs of the donors showed little ability to convert coal to THF solubles. Factors which influence hydrogen donation include the presence of heteroatoms or substituents both internal and external to the aromatic or hydroaromatic rings, the degree of hydrogenation, the aromaticity or nonaromaticity of the hydroaromatics, and the presence of five-membered rings. A relationship between heats of formation and hydrogen donor ability is shown for hydroaromatics within two ring or three ring homologous series. A model hydrogen acceptor, benzophenone, is also used to rank donors. No correlation exists in the ranking of hydrogen donors by the model acceptor used in this work and in other experimental studies and that obtained by conversion of Western Kentucky coal at typical liquefaction conditions. 24 references.

  20. Economics of hydrogen production and liquefaction updated to 1980

    NASA Technical Reports Server (NTRS)

    Baker, C. R.

    1979-01-01

    Revised costs for generating and liquefying hydrogen in mid-1980 are presented. Plant investments were treated as straight-forward escalations resulting from inflation. Operating costs, however, were derived in terms of the unit cost of coal, fuel gas and electrical energy to permit the determination of the influence of these parameters on the cost of liquid hydrogen. Inflationary influence was recognized by requiring a 15% discounted rate of return on investment for Discounted Cash Flow financing analysis, up from 12% previously. Utility financing was revised to require an 11% interest rate on debt. The scope of operation of the hydrogen plant was revised from previous studies to include only the hydrogen generation and liquefaction facilities. On-site fuel gas and power generation, originally a part of the plant complex, was eliminated. Fuel gas and power are now treated as purchased utilities. Costs for on-site generation of fuel gas however, are included.

  1. Synthesis of model compounds for coal liquefaction research

    SciTech Connect

    Asaro, M.F.; Bottaro, J.C.; Hirschon, A.S.

    1991-05-01

    The objective of this project are to develop feasible synthetic routes to produce (1) 4(4{prime}-hydroxy-5{prime},6{prime},7{prime},8{prime}-tetrahydro-1{prime}-naphthylmethyl)-6-methyldibenzothiophene, and (2) a 1-hydroxynaphthalene-dibenzothiophene polymer. These compounds are thought to be representative of sulfur containing molecules in coal. The program is divided into three tasks, the first of which is a project work plan that we have already submitted. Tasks 2 and 3 are as follows: Synthesis of 4(4-hydroxy-5{prime},6{prime},7{prime},8{prime}-tetrahydro-1{prime}-naphthylmethyl)-6-methyldibenzothiophene and synthesis of 1-hydroxynaphthalene-dibenzothiophene polymer linked by methylene bonds. 14 refs.

  2. Coal liquefaction process streams characterization and evaluation: High performance liquid chromatography (HPLC) of coal liquefaction process streams using normal-phase separation with uv diode array detection

    SciTech Connect

    Clifford, D.J.; McKinney, D.E.; Hou, Lei; Hatcher, P.G.

    1994-01-01

    This study demonstrated the considerable potential of using two-dimensional, high performance liquid chromatography (HPLC) with normal-phase separation and ultraviolet (UV) diode array detection for the examination of filtered process liquids and the 850{degrees}F{sup {minus}} distillate materials derived from direct coal liquefaction process streams. A commercially available HPLC column (Hypersil Green PAH-2) provided excellent separation of the complex mixture of polynuclear aromatic hydrocarbons (PAHs) found in coal-derived process streams process. Some characteristics of the samples delineated by separation could be attributed to processing parameters. Mass recovery of the process derived samples was low (5--50 wt %). Penn State believes, however, that, improved recovery can be achieved. High resolution mass spectrometry and gas chromatography/mass spectrometry (GC/MS) also were used in this study to characterize the samples and the HPLC fractions. The GC/MS technique was used to preliminarily examine the GC-elutable portion of the samples. The GC/MS data were compared with the data from the HPLC technique. The use of an ultraviolet detector in the HPLC work precludes detecting the aliphatic portion of the sample. The GC/MS allowed for identification and quantification of that portion of the samples. Further development of the 2-D HPLC analytical method as a process development tool appears justified based on the results of this project.

  3. EDS Coal Liquefaction Process Development. Phase V. Laboratory evaluation of the characteristics of EDS Illinois bottoms

    SciTech Connect

    Lao, T C; Levasseur, A A

    1984-02-01

    This interim report documents work carried out by Combustion Engineering, Inc. under a contract to Exxon Research and Engineering Company to develop a conceptual Hybrid Boiler design fueled by the vacuum distillation residue (vacuum bottoms) derived from Illinois No. 6 coal in the EDS Coal Liquefaction Process. This report was prepared by Combustion Engineering, Inc., and is the first of two reports on the predevelopment phase of the Hybrid Boiler program. This report covers the results of a laboratory investigation to assess the fuel and ash properties of EDS vacuum bottoms. The results of the laboratory testing reported here were used in conjunction with Combustion Engineering's design experience to predict fuel performance and to develop appropriate boiler design parameters. These boiler design parameters were used to prepare the engineering design study reported in EDS Interim Report FE-2893-113, the second of the two reports on the predevelopment phase of the Hybrid Boiler Program. 46 figures, 29 tables.

  4. Microbial recovery of metals from spent coal liquefaction catalysts. Final report

    SciTech Connect

    Sperl, P.L.; Sperl, G.T.

    1995-07-01

    This project was initiated on October 1, 1989, for the purpose of recovering metals from spent coal liquefaction catalysts. Two catalyst types were the subject of the contract. The first was a Ni-No catalyst support on alumina (Shell 324), the catalyst used in a pilot scale coal liquefaction facility at Wilsonville, Alabama. The second material was an unsupported ammonium molybdate catalyst used in a pilot process by the Department of Energy at the Pittsburgh Energy Technology Center. This material was obtained in late February 1990 but has not been pursued since the Mo content of this particular sample was too low for the current studies and the studies at the Pittsburgh Energy Technology Center have been discontinued. The object of the contract was to treat these spent catalysts with microorganisms, especially Thiobacillus ferrooxidans , but also other Thiobacillus spp. and possibly Sulfolobus and other potential microorganisms, to leach and remove the metals (Ni and Mo) from the spent catalysts into a form which could be readily recovered by conventional techniques.

  5. Oxide-supported metal carbonyls: novel catalysts for the liquefaction of coal. Final technical report

    SciTech Connect

    Melson, G.A.

    1985-01-01

    Coal liquefaction, hydrodesulfurization (HDS), and hydrodenitrogenation (HDN) catalysts have been investigated increasingly in recent years because of the need to understand how to develop more selective and stable materials for coal utilization. One catalyst that has been used extensively for HDS and subjected to numerous characterization and model reaction studies is Co-Mo/Al/sub 2/O/sub 3/. In these studies, the catalyst preparation technique has usually involved the incipient-wetness impregnation of ..gamma..-Al/sub 2/O/sub 3/ with ammonium molybdates and cobalt nitrates. Such a technique leads to a variety of surface species, bulk-like and monolayer forms, which have been described and can be controlled by alterations in the preparation techniques and materials. However, certain structural and chemical factors of the catalysts, e.g., Co and Mo reducibility and dispersion or surface speciation at low and high metal concentrations, seem to be independent of such alterations. To investigate whether these factors can be affected by preparation techniques and to develop oxide-supported, metal catalysts having controlled metal dispersions and speciation, a catalyst preparation technique using metal carbonyls with an extraction process to metal-load oxide supports has been developed (J.E. Crawford, G.A. Melson, L.E. Makovsky, F.R. Brown, J. Catal., 83: 454 (1983)). This report discusses the surface and bulk characterization, and presents initial HDS and liquefaction results, for these catalysts. 7 refs., 4 figs., 1 tab.

  6. Catalytic multi-stage liquefaction of coal. Third quarterly report, 1 April 1993--31 June 1993

    SciTech Connect

    Comolli, A.G.; Johanson, E.S.; Lee, L.K.; Pradhan, V.R.; Stalzer, R.H.

    1993-07-01

    This quarterly report covers the activities of Catalytic Multi-Stage Liquefaction of Coal during the Period April 1 -- June 30, 1993, at Hydrocarbon Research, Inc. in Lawrenceville and Princeton, New Jersey. This DOE Contract Period is from December 8, 1992 to December 7, 1994. The overall objective of this program is to produce liquid fuels from coal by direct liquefaction at a cost that is competitive with conventional fuels. Specifically, this continuous bench-scale program contains provisions to examine new ideas in areas such as: Low temperature pretreatments, more effective catalysts, on-line hydrotreating, new coal feedstocks, other hydrogen sources, more concentrated coal feeds and other highly responsive process improvements while assessing the design and economics of the bench-scale results. This quarterly report covers work on Laboratory Scale Studies, Continuous Bench-Scale Operations, Technical Assessment and Project Management.

  7. Advanced liquefaction using coal swelling and catalyst dispersion techniques. Quarterly technical progress report, July--September 1992

    SciTech Connect

    Curtis, C.W.; Gutterman, C.; Chander, S.

    1992-12-31

    The experimental study of coal swelling ratios have been determined with a wide variety of solvents. Only marginal levels of coal swelling were observed for the hydrocarbon solvents, but high levels were found with solvents having heteroatom functionality. Blends were superior to pure solvents. The activity of various catalyst precursors for pyrene hydrogenation and coal conversion was measured. Higher coal conversions were observed for the S0{sub 2}-treated coal than the raw coal, regardless of catalyst type. Coal conversions were highest for Molyvan-L, molybdenum naphthenate, and nickel octoate, respectively. Bottoms processing consists of a combination of the ASCOT process coupling solvent deasphalting with delayed coking. Initial results indicate that a blend of butane and pentane used near the critical temperature of butane is the best solvent blend for producing a yield/temperature relationship of proper sensitivity and yet retaining an asphalt phase of reasonable viscosity. The literature concerning coal swelling, both alone and in combination with coal liquefaction, and the use of dispersed or unsupported catalysts in coal liquefaction has been updated.

  8. Catalytic direct liquefaction of high-sulfur coals and their blends with asphaltite in the absence of a solvent

    SciTech Connect

    Omer Gul; Parvana Gafarova; Arif Hesenov; Harold H. Schobert; Oktay Erbatur

    2007-08-15

    Two high-sulfur Turkish coals (Mengen and Kangal) and an asphaltite (Avgamasya) were liquefied with and without the catalyst precursors ammonium heptamolybdate (AHM) and ammonium tetrathiomolybdate (ATTM) at 300, 350, 400, and 450{sup o}C. Blends of these coals with the asphaltite were also liquefied using ATTM. Effective conversions of both coals into oils and into asphaltene and preasphaltene fractions were achieved with both catalyst precursors, although ATTM was more effective than AHM. Maximum conversion for Mengen coal with ATTM (89.2%) was achieved at 400{sup o}C, although the maximum yield of oils (56.9%) was obtained at 450{sup o}C. Kangal, in the presence of ATTM, gave maximum conversion (87.7%) at 400{sup o}C; the corresponding oil yield (49.6%) was not much less than that obtained at 450{sup o}C (49.9%). Some retrogressive reactions toward the formation of aromatics were observed during liquefaction at 450{sup o}C in the presence of AHM or ATTM with both coals. Also, using these catalyst precursors results in effective hydrogenation of two-ring or higher condensed aromatics and effective hydrogenolysis of the alicyclic part of hydroaromatic structures. On the other hand, these catalyst precursors do not provide effective saturation of monoaromatic rings, although the use of ATTM yielded partial reduction of these compounds. The distribution of main product fractions obtained from these reactions and the detailed analysis of oils obtained are reported. 118 refs., 4 figs., 15 tabs.

  9. Slurry Phase Iron Catalysts for Indirect Coal LIquefaction.

    SciTech Connect

    Datye, A.K.

    1997-08-08

    This report covers the fourth six month period of this three year grant under the University Coal Research program. During this period, we have begun the synthesis of precipitated catalysts using a bench-top spray dryer. The influence of binders on particle strength was also studied using the ultrasonic fragmentation approach to derive particle breaking stress. A similar approach was used to derive particle strength of catalysts obtained from Mr. Robert Gormley at FETC. Over the next six month period, this work will be continued while the catalysts prepared here will be examined by TPR to determine reducibility and the extent of adverse iron-silica interactions. A fundamental study of Fe/silica interactions has been performed using temperature programmed reaction and TEM to provide understanding of how the silica binders influence the activity of Fe catalysts. To understand differences in the reducibility of the iron phase caused by silica, we have set up a temperature programmed reduction facility. TPR in H, as well as in CO was performed of Fe/ SiO, catalysts prepared by impregnation as well as by precipitation. What is unique about these studies is that high resolution TEM was performed on samples removed from the reactor at various stages of reduction. This helps provide direct evidence for the phase changes that are detected by TPR. We have continued the analysis of catalysts received from slurry reactor runs at Texas A&M university (TAMU) and the University of Kentucky Center for Applied Energy Research (CAER) by x-ray diffraction. The purpose of the XRD analysis was to determine the phase composition of catalysts derived from a slurry reaction run using Fe Fischer-Tropsch catalysts. We had previously described how catalyst removed in the hot wax may oxidize to magnetite if the wax is air-exposed. We have now received catalysts from CAER that were removed under a protective inert blanket, and we are in the process of analyzing them, but preliminary work

  10. Biological production of ethanol from coal

    SciTech Connect

    Not Available

    1992-12-01

    Due to the abundant supply of coal in the United States, significant research efforts have occurred over the past 15 years concerning the conversion of coal to liquid fuels. Researchers at the University of Arkansas have concentrated on a biological approach to coal liquefaction, starting with coal-derived synthesis gas as the raw material. Synthesis gas, a mixture of CO, H[sub 2], CO[sub 2], CH[sub 4] and sulfur gases, is first produced using traditional gasification techniques. The CO, CO[sub 2] and H[sub 2] are then converted to ethanol using a bacterial culture of Clostridium 1jungdahlii. Ethanol is the desired product if the resultant product stream is to be used as a liquid fuel. However, under normal operating conditions, the wild strain'' produces acetate in favor of ethanol in conjunction with growth in a 20:1 molar ratio. Research was performed to determine the conditions necessary to maximize not only the ratio of ethanol to acetate, but also to maximize the concentration of ethanol resulting in the product stream.

  11. Short contact time direct coal liquefaction using a novel batch reactor. Quarterly technical progress report, September 15, 1995--January 15, 1996

    SciTech Connect

    Klein, M.T.; Calkins, W.H.; Huang, He

    1996-01-26

    The objective of this research is to optimize the design and operation of the bench scale batch reactor (SCTBR) f or coal liquefaction at short contact times (0.01 to 10 minutes or longer). Additional objectives are to study the kinetics of direct coal liquefaction particularly at short reaction times, and to investigate the role of the organic oxygen components of coal and their reaction pathways during liquefaction. Many of those objectives have already been achieved and others are still in progress. This quarterly report covers further progress toward those objectives.

  12. Low severity coal liquefaction promoted by cyclic olefins. Quarterly report, October 1994--December 1994

    SciTech Connect

    Curtis, C.W.

    1995-05-01

    The research performed during the October to December 1994 quarter centered on two areas. The first area involved the writing of a paper based on research performed on this project concerning the mild acidic pretreatment of low rank coals and their liquefaction behavior in the presence of hydrogen donors with different reactivities. The second area that was worked on during the quarter was the high temperature infrared analysis of cyclic olefins. The work is ongoing and is currently involving a considerable amount of equipment and technique development. Cyclic olefins, such as 1,4,5,8-tetrahydronaphthalene (isotetralin) and 1,4,5,8,9,10-hexahydroanthracene (HHA), are highly reactive hydrogen donor compounds that readily donate their hydrogen to coal and model acceptors when heated. Numerous reactions have been performed using these cyclic olefins with high rank and low rank coals as well as with model acceptors. In each case the cyclic olefins have proven themselves to be active donors. Further evaluation of the reactivity of these donors with pretreated low rank coals and at different temperatures is described more fully in this report.

  13. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Technical progress report, August 1992--July 1992

    SciTech Connect

    Song, C.; Saini, A.K.; Huang, L.; Wenzel, K.; Hou, L.; Hatcher, P.G.; Schobert, H.H.

    1992-08-01

    Low-temperature catalytic pretreatment is a promising approach to the development of an improved liquefaction process- This work is a fundamental study on effects of pretreatments on coal structure and reactivity in liquefaction. The main objectives of this project are to study the coal structural changes induced by low-temperature catalytic and thermal pretreatments by using spectroscopic techniques; and to clarify the pretreatment-induced changes in reactivity or convertibility of coals in the subsequent liquefaction. This report describes the recent progress of our work. Substantial progress has been made in the spectroscopic characterization of structure and pretreatment-liquefaction reactions of a Montana subbituminous Coal (DECS-9), and thermochemical analysis of three mw and reacted bituminous coals. Temperature programmed liquefaction has been performed on three low-rank coals both in the presence and absence of dispersed molybdenum sulfide catalyst. We also performed a detailed study of the effects of mild thermal pretreatment -- drying in air and in vacuum -- on thermal and catalytic liquefaction of a Wyodak subbituminous coal. Important information on structure and structure transformation during thermal pretreatment and liquefaction reactions of low-rank coals has been derived by applying solid-state CPMAS {sup 13}C NMR and flash pyrolysis-GC-MS (Py-GC-MS) for characterization of the macromolecular network of a Montana subbituminous coal and its residues from temperature-programmed and nonprogrammed liquefaction (TPL and N-PL) at final temperatures ranging from 300 to 425{degree}C in H-donor and non-donor solvents. The results revealed that this coal contains significant quantities of oxygen-bearing structures, corresponding to about 18 O-bound C per 100 C atoms and one O-bound C per every 5 to 6 aromatic C.

  14. [FTIR analysis of products derived from wood liquefaction with 1-octanol].

    PubMed

    Zou, Xian-Wu; Yang, Zhi; Qin, Te-Fu

    2009-06-01

    Solvolysis is one of the important processes of biomass liquefaction. To produce superior quality liquid biofuel from biomass under mild conditions, it is essential to exploit novel reactive liquid solvent. Furthermore, the evaluation of liquefaction efficiency is carried out mainly by the means of analysis of the products derived from biomass liquefaction. In the present study, liquefaction of poplar wood powder in acidified 1-octanol was investigated with a stainless steel autoclave. Residue, heavy oil and light oil were separated from the liquefaction products by extraction with acetone and n-hexane successively. FTIR analysis was carried out on these liquefaction compositions to illuminate the liquefaction regularities and mechanisms of cellulose, hemicellulose and lignin of wood. The results showed that liquefaction oils were complex mixture containing hydroxide, carbonyl, methoxyl, aromatic and aether. Liquefactions of cellulose and hemicellulose were easier than that of lignin. Cellulose and hemicellulose were converted to light oil, however, lignin was mainly converted to heavy oil. At 150 degrees C, lignin was depolymerized and degraded into micromolecular aromatic compounds, among which condensation reactions took place when reaction temperature increased.

  15. Part 1. The effect of microwave receptors on the liquefaction of Turkish coals by microwave energy in a hydrogen donor solvent

    SciTech Connect

    Emine Yagmur; Taner Togrul

    2005-12-01

    The effects of microwave receptors to coal (receptor/coal) ratio and the period of heating by microwave energy on the solubilization of Turkish coals (Tuncbilek, Mugla-Yatagan, Beypazari lignites, and Zonguldak bituminous coal) in tetralin have been investigated. V{sub 2}O{sub 5} and TiO{sub 2} were used as microwave receptors. The changes of liquid product yield indicated that it depended significantly on the type and amount of receptor and the type of coal. A significant increase in the lignite conversions to oil fractions was observed by the addition of the V{sub 2}O{sub 5} receptor. The use of TiO{sub 2} receptor decreased the yield of THF soluble coal products. However, both V{sub 2}O{sub 5} and TiO{sub 2} receptors decreased the yield of preasphaltene (PAS) and asphaltene (AS) due to their catalytic effect on the coal liquefaction. 15 refs., 9 figs., 1 tab.

  16. Coal liquefaction process streams characterization and evaluation: Estimation of total phenol concentrations in coal liquefaction resids by {sup 31}P NMR spectroscopy

    SciTech Connect

    Mohan, J.T.; Verkade, J.G.

    1992-11-01

    In this study, Iowa State University researchers used {sub 31}P-tagged reagents to derivatize the labile hydrogen functional groups in the THF-soluble portion of 850{degrees}F{sup +} distillation resid materials and the THF-soluble portion of process oils derived from direct coal liquefaction.{sup 31}P-NMR was used to analyze the derivatized samples. NMR peak assignments can be made by comparison to model compounds similarly derivatized. Species can be quantified by integration of the NMR signals. Different {sup 31}P-NMR tagged reagents can be used to produce different degrees of peak resolution in the NMR spectrum. This, in turn, partially dictates the degree of speciation and/or quantification of species, or classes of compounds, that can be accomplished. Iowa State chose a {sup 31}P-tagged reagent (ClPOCMe{sub 2}CMe{sub 2}O) which was shown previously to be particularly useful in the derivatization of phenols. The derivatized samples all exhibited a small group of peaks attributed to amines and a broad group of peaks in the phenol region. The presence of paramagnetic species in the samples caused the NMR signals to broaden. Electron paramagnetic resonance (EPR) spectra confirmed the presence of paramagnetic organic free radicals in selected samples. Various methods were employed to process the NMR data. The complexity and broadness of the phenol peak, however, made speciation of the phenols impractical.

  17. Coal liquefaction process streams characterization and evaluation: Estimation of total phenol concentrations in coal liquefaction resids by [sup 31]P NMR spectroscopy

    SciTech Connect

    Mohan, J.T.; Verkade, J.G. )

    1992-11-01

    In this study, Iowa State University researchers used [sub 31]P-tagged reagents to derivatize the labile hydrogen functional groups in the THF-soluble portion of 850[degrees]F[sup +] distillation resid materials and the THF-soluble portion of process oils derived from direct coal liquefaction.[sup 31]P-NMR was used to analyze the derivatized samples. NMR peak assignments can be made by comparison to model compounds similarly derivatized. Species can be quantified by integration of the NMR signals. Different [sup 31]P-NMR tagged reagents can be used to produce different degrees of peak resolution in the NMR spectrum. This, in turn, partially dictates the degree of speciation and/or quantification of species, or classes of compounds, that can be accomplished. Iowa State chose a [sup 31]P-tagged reagent (ClPOCMe[sub 2]CMe[sub 2]O) which was shown previously to be particularly useful in the derivatization of phenols. The derivatized samples all exhibited a small group of peaks attributed to amines and a broad group of peaks in the phenol region. The presence of paramagnetic species in the samples caused the NMR signals to broaden. Electron paramagnetic resonance (EPR) spectra confirmed the presence of paramagnetic organic free radicals in selected samples. Various methods were employed to process the NMR data. The complexity and broadness of the phenol peak, however, made speciation of the phenols impractical.

  18. [The mechanisms of hydrogen incorporation in coal liquefaction

    SciTech Connect

    Guthrie, R.

    1993-01-28

    In earlier reports we have describe d our efforts to understand the mechanism of deuterium incorporation during the thermolysis of 1,2-diphenylethane and 2,2,5,5-tetramethyl-3,4-diphenylhexane under D[sub 2] gas in a glass vessel. We have reported that in both of these cases, there is substantial deuterium incorporation. A summary of our conclusions follows: Conclusions previously reported for the 1,2-diphenylethane (DPE) system. 1. Benzyl radicals produced in the thermolysis react mainly with DPE to extract a hydrogen atom and produce undeuterated toluene. 2. The 1,2-diphenylethyl radicals produced are mainly responsible for the reaction with D[sub 2] to give D atoms. 3. D atoms then react with aromatic rings to form adduct radicals which are, at least in part, reconverted to D-substituted aromatics in termination steps. 4.2-Phenylethyl radicals react in a less discriminating manner, 1/3 to 1/2 of the events probably involving direct reaction with D[sub 2]. 5. A reasonable match to major product distribution can be accomplished using a model consisting of the set of ten reactions.

  19. Chemical analysis and mutational assay of distilled oils from the H-coal direct liquefaction process: a status report

    SciTech Connect

    Wilson, B.W.; Later, D.W.; Wright, C.W.; Stewart, D.L.

    1985-01-01

    Samples from the H-Coal process, a catalytic, single-stage, coal liquefaction technology, were chemically characterized and screened for microbial mutagenicity. For these investigations, a blend of light and heavy H-Coal process oils was fractionally distilled into 50/sup 0/F boiling point cuts. The chemical analyses and biological testing results presented in this status report deal primarily with the blended material and the distillate fractions boiling above 650/sup 0/F. Results from the microbial mutagenicity assays indicated that onset of biological activity in the crude materials occurred above 700/sup 0/F. Similar trends have been observed for Solvent Refined Coal (SRC) I, SRC II, Integrated Two-Stage Liquefaction (ITSL) and Exxon EDS process materials. After chemical class fractionation, the primary source of microbial mutagenicity of the crude boiling point cuts was the nitrogen-containing polycyclic aromatic compound (N-PAC) fractions. Amino polycyclic aromatic hydrocarbons (amino-PAH) were present at sufficient concentration levels in the N-PAC fractions to account for the observed mutagenic responses. In general, the chemical composition of the H-Coal materials studied was similar to that of other single-stage liquefaction materials. The degree of alkylation in these materials was determined to be greater than in the SRC and less than in the EDS process distillate cuts. 13 references, 8 figures, 11 tables.

  20. Direct coal liquefaction baseline design and system analysis. Quarterly report, July 1995--September 1992

    SciTech Connect

    1993-01-01

    The primary objective of the study is to develop a computer model for a base line direct coal liquefaction design based on two stage direct coupled catalytic reactors. This primary objective is to be accomplished by completing the following: (1) A base line design based on previous DOE/PETC results from Wilsonville pilot plant and other engineering evaluations; (2) A cost estimate and economic analysis; (3) A computer model incorporating the above two steps over a wide range of capacities and selected process alternatives; (4) A comprehensive training program for DOE/PETC Staff to understand and use the computer model; (5) A thorough documentation of all underlying assumptions for baseline economics, and (6) A user manual and training material which will facilitate updating of the model in the future. With the inclusion of the improved baseline case, the above primary objective is extended to include the impact of higher space velocity through liquefaction reactor. The progress made during any particular quarter is published in a quarterly report following the duration of the quarter. The report consists of the following four sections: (1) Introduction; (2) Summary; (3) Technical Progress Report (By Tasks); and (4) Key Personnel Staffing Report.

  1. Coal liquefaction process streams characterization and evaluation. Quarterly technical progress report, July 1--September 30, 1992

    SciTech Connect

    Brandes, S.D.; Winschel, R.A.; Burke, F.P.

    1992-11-01

    This is the twelfth Quarterly Technical Progress Report under DOE Contract DE-AC22-89PC89883. Major topics reported are: Summaries of the final reports produced by Lehigh University, West Virginia University, and Vander Sande Associates under the Participants Program are presented. Analytical data produced by CONSOL are provided in Appendix I for all samples employed in the Participants Program and issued with the samples to research groups in the Participants Program. A paper was presented at the 1992 US Department of Energy Pittsburgh Energy Technology Center Liquefaction Contractors` Review Conference, held in Pittsburgh September 23--24, 1992, entitled ``The Chemical Nature of Coal Liquid Resids and the Implications for Process Development``. It appears as Appendix 2 in this report.

  2. Direct coal liquefaction baseline design and system analysis. Quarterly report, April--June 1991

    SciTech Connect

    Not Available

    1991-07-01

    The primary objective of the study is to develop a computer model for a base line direct coal liquefaction design based on two stage direct coupled catalytic reactors. This primary objective is to be accomplished by completing the following: a base line design based on previous DOE/PETC results from Wilsonville pilot plant and other engineering evaluations; a cost estimate and economic analysis; a computer model incorporating the above two steps over a wide range of capacities and selected process alternatives; a comprehensive training program for DOE/PETC Staff to understand and use the computer model; a thorough documentation of all underlying assumptions for baseline economics; and a user manual and training material which will facilitate updating of the model in the future.

  3. Direct coal liquefaction baseline design and system analysis. Quarterly report, January--March 1991

    SciTech Connect

    Not Available

    1991-04-01

    The primary objective of the study is to develop a computer model for a base line direct coal liquefaction design based on two stage direct coupled catalytic reactors. This primary objective is to be accomplished by completing the following: a base line design based on previous DOE/PETC results from Wilsonville pilot plant and other engineering evaluations; a cost estimate and economic analysis; a computer model incorporating the above two steps over a wide range of capacities and selected process alternatives; a comprehensive training program for DOE/PETC Staff to understand and use the computer model; a thorough documentation of all underlying assumptions for baseline economics; and a user manual and training material which will facilitate updating of the model in the future.

  4. Direct coal liquefaction baseline design and system analysis. Quarterly report, September--December 1990

    SciTech Connect

    Not Available

    1991-01-01

    The primary objective of the study is to develop a computer model for a base line direct coal liquefaction design based on two stage direct coupled catalytic reactors. This primary objective is to be accomplished by completing the following: a base line design based on previous DOE/PETC results from Wilsonville pilot plant and other engineering evaluations; a cost estimate and economic analysis; a computer model incorporating the above two steps over a wide range of capacities and selected process alternatives; a comprehensive training program for DOE/PETC Staff to understand and use the computer model; a thorough documentation of all underlying assumptions for baseline economics; and a user manual and training material which will facilitate updating of the model in the future.

  5. Analysis of toxicity of leachates from coal liquefaction wastewater treatment sludge

    SciTech Connect

    Dahlberg, M.D.; Ruppel, T.C.

    1985-03-01

    The disposal requirements for wastewater treatment sludge from coal liquefaction plants will be determined by toxicity tests established by the Environmental Protection Agency (EPA) to enforce the Resource Conservation and Recovery Act (RCRA). Concentrations of eight elements in samples from a noncommercial plant were well below the standards used in the EP (extraction procedure) test of the EPA. Toxicity bioassays with Daphnia magna supported the results of the EP tests. Leachates generated according to the American Society for Testing and Materials extraction procedure (ASTM D-3987) were also tested. Concentrations of RCRA elements were frequently below the minimum detectable concentrations, and no differences in toxicity of the EP and ASTM extracts were evident. 17 references, 3 tables.

  6. Bimetallic promotion of cooperative hydrogen transfer and heteroatom removal in coal liquefaction

    SciTech Connect

    Eisch, J.J.

    1992-04-07

    The ultimate objective of this research has been to uncover novel reagents and experimental conditions for heteroatom removal and hydrogen transfer processes, which would be applicable to the liquefaction of coal under low-severity conditions. To this end, one phase of this research has investigated the cleavage of carbon-heteroatom bonds involving sulfur, oxygen, nitrogen and halogen by subvalent transition-metal complexes. A second phase of the study has assessed the capability of the same transition-metal complexes or of organoaluminum Lewis acids to catalyze the cleavage of carbon-hydrogen bonds in aromatics and hence to promote hydrogen shuttling. Finally, a third phase of our work has uncovered a remarkable synergistic effect of combinations of transition metals with organoaluminum Lewis acids on hydrogen shuttling between aromatics and hydroaromatics. (VC)

  7. Fine particle clay catalysts for coal liquefaction. Quarterly technical progress report, May 9, 1992--August 8, 1992

    SciTech Connect

    Olson, E.S.

    1995-10-01

    An investigation of new methods for the production of mixed pillared clay catalysts and clay-supported catalysts and determination of their catalytic activities were continued in this quarter. To demonstrate the reproducibility of the preparative method for high activity iron/alumina-pillared montmorillonite catalysts, a new batch of the catalyst was prepared and tested for hydrocracking activity with bibenzyl. This preparation gave conversion and product distribution similar to that reported previously. The mixed iron/alumina-pillared clay was also prepared using a pillaring solution that was aged for longer period of time. To determine the importance of the type of pillaring support in hydrocracking activity, iron/zirconia-pillared montmorillonite was prepared using the same technique as that for iron/alumina-pillared montmorillonite. The reaction of bibenzyl with the sulfided iron/zirconia-pillared catalyst gave a lower hydrocracking conversion than the iron/alumina-pillared catalyst. Addition of a second catalytic metal to the clay support was attempted to determine if a synergistic effect could improve liquefaction. Ferric nitrate and stannous chloride were added to the clay, but the resulting catalyst was relatively poor for hydrocracking and hydrogenation compared with ferric nitrate supported on the clay. New disposable iron catalysts with high acidity and surface area are desired for coal liquefaction. Synthetic iron aluminosilicates were prepared by methods similar to those used for the nickel-substituted synthetic mica montmorillonite (NiSMM) catalysts, which are very effective for hydrogenation and reforming of hydrocarbons. The iron aluminosilicate catalysts were tested for hydrocracking and hydrogenation of bibenzyl, naphthalene and pyrene. Pyrene hydrogenation was effectively catalyzed by the sulfided synthetic iron catalyst.

  8. Coal liquefaction process wherein jet fuel, diesel fuel and/or ASTM No. 2 fuel oil is recovered

    DOEpatents

    Bauman, Richard F.; Ryan, Daniel F.

    1982-01-01

    An improved process for the liquefaction of coal and similar solid carbonaceous materials wherein a hydrogen donor solvent or diluent derived from the solid carbonaceous material is used to form a slurry of the solid carbonaceous material and wherein the naphthenic components from the solvent or diluent fraction are separated and used as jet fuel components. The extraction increases the relative concentration of hydroaromatic (hydrogen donor) components and as a result reduces the gas yield during liquefaction and decreases hydrogen consumption during said liquefaction. The hydrogenation severity can be controlled to increase the yield of naphthenic components and hence the yield of jet fuel and in a preferred embodiment jet fuel yield is maximized while at the same time maintaining solvent balance.

  9. Coal liquefaction process wherein jet fuel, diesel fuel and/or astm no. 2 fuel oil is recovered

    SciTech Connect

    Bauman, R.F.; Ryan, D.F.

    1982-06-01

    An improved process for the liquefaction of coal and similar solid carbonaceous materials wherein a hydrogen donor solvent or diluent derived from the solid carbonaceous material is used to form a slurry of the solid carbonaceous material and wherein the naphthenic components from the solvent or diluent fraction are separated and used as jet fuel components. The extraction increases the relative concentration of hydroaromatic (hydrogen donor) components and as a result reduces the gas yield during liquefaction and decreases hydrogen consumption during said liquefaction. The hydrogenation severity can be controlled to increase the yield of naphthenic components and hence the yield of jet fuel and in a preferred embodiment jet fuel yield is maximized while at the same time maintaining solvent balance.

  10. Investigation on mechanism of coal liquefaction-hydrocracking of model compounds

    SciTech Connect

    Wu, J.Z.; Gao, J.S.; Hang, Y.Z.; Oelert, H.H.

    1997-12-31

    There is strong evidence for the existence of -O-CH{sub 2}- and -CH{sub 2}-CH{sub 2}-bridge linkages in coal, especially in low rank coals, so there is a close relationship between hydrocracking kinetic of model compounds and coal liquefaction. In a tube autoclave with the volume of 17 ml the hydrocracking experiments of six model compounds are carried out in the presence of tetralin. The results show that the stability order of six model compounds in hydrocracking is as follows: Ph-Ch{sub 2}-Ph > Ph-O-Ph > Ph-Ch{sub 2}-Ch{sub 2}-Ph > Ph-O-CH{sub 2}-Ph > Ph-CH{sub 2}-S-CH{sub 2}-Ph > Ph-CH{sub 2}-S-S-CH{sub 2}-Ph. Introducing 10% (in weight) of benzyl phenyl ether can increase the decomposition ratios of diphenyl methane and diphenyl ether from 4.3% to 12.6% and 18.3% to 31.5% respectively. From the hydrocracking kinetic experiments for both benzyl phenyl ether (BPE) and dibenzyl (DB), the reaction corresponds to first order. The apparent activation (DE) is 83.9 kJ/mol for BPE and 150 kJ/mol for DB in the range of temperature 330--450 C, that is, the same as coal liquefaction. The influence of initial hydrogen pressure on hydrocracking of model compounds is also described in this paper. Under the conditions of the experiments the decomposition ratios (DR) of model compounds increase linearly with the increase of initial hydrogen pressure, e.g., DR is only 34.3% under 3.0 MPa (420 C), but 56.8% can be obtained when the initial hydrogen pressure reaches 8.5 MPa. Moreover, changing the initial pressure can influence not only DR of model compounds but also their hydrocracking mechanisms. Applying Mo-Ni, Y- and 5A-sieves to hydrocracking of model compounds are all effective. For more stable compounds such as dibenzyl methane and diphenyl ether the Y-sieve is better than the Mo-Ni catalyst, but it is just contrary to crack for benzyl phenyl ether.

  11. Short contact time direct coal liquefaction using a novel batch reactor. Progress report, September 27, 1993--December 31, 1993

    SciTech Connect

    Klein, M.T.; Calkins, W.H.

    1994-01-19

    The objective for this research is to optimize the design and operation of the bench scale batch reactor (STBR) for coat liquefaction at short contact times (0.01 to 10 minutes). This reactor is simple and low enough in cost to serve as a suitable replacement for the traditional tubing-bomb reactors for coal liquefaction and other high-pressure, high-temperature reaction studies. The details of the reactor system are shown in Figure 2. The heating bath used is a Techne IFB-52 industrial fluidized sand bath, which maintains a reaction temperature of {plus_minus}2{degrees}C. The 30 cm{sup 3} reactor is capable of containing up to 17 MPa (2500 psi) pressure at temperatures up to 550{degrees}C. The tubing used for preheater and precooler was 1/4in. 316 stainless steel with wall thickness of 0.035in. The lengths of the preheater and precooler are selected based on the particular process being studied. Since a gas (e.g. hydrogen or nitrogen) is bubbled through the reaction mixture under pressure and out through a letdown valve, a small water cooled condenser above the reactor before the let-down valve is added to avoid loss of solvent or other low boiling components. Coal liquefaction runs are made by preparing slurries of coal in reagent grade tetralin. Various ratios of tetralin to coal are used, and in some cases, a catalyst such as Ni/Mo on alumina is added.

  12. Dependence of liquefaction behavior on coal characteristics. Part VI. Relationship of liquefaction behavior of a set of high sulfur coals to chemical structural characteristics. Final technical report, March 1981 to February 1984

    SciTech Connect

    Neill, P. H.; Given, P. H.

    1984-09-01

    The initial aim of this research was to use empirical mathematical relationships to formulate a better understanding of the processes involved in the liquefaction of a set of medium rank high sulfur coals. In all, just over 50 structural parameters and yields of product classes were determined. In order to gain a more complete understanding of the empirical relationships between the various properties, a number of relatively complex statistical procedures and tests were applied to the data, mostly selected from the field of multivariate analysis. These can be broken down into two groups. The first group included grouping techniques such as non-linear mapping, hierarchical and tree clustering, and linear discriminant analyses. These techniques were utilized in determining if more than one statistical population was present in the data set; it was concluded that there was not. The second group of techniques included factor analysis and stepwise multivariate linear regressions. Linear discriminant analyses were able to show that five distinct groups of coals were represented in the data set. However only seven of the properties seemed to follow this trend. The chemical property that appeared to follow the trend most closely was the aromaticity, where a series of five parallel straight lines was observed for a plot of f/sub a/ versus carbon content. The factor patterns for each of the product classes indicated that although each of the individual product classes tended to load on factors defined by specific chemical properties, the yields of the broader product classes, such as total conversion to liquids + gases and conversion to asphaltenes, tended to load largely on factors defined by rank. The variance explained and the communalities tended to be relatively low. Evidently important sources of variance have still to be found.

  13. Production of Advanced Biofuels via Liquefaction - Hydrothermal Liquefaction Reactor Design: April 5, 2013

    SciTech Connect

    Knorr, D.; Lukas, J.; Schoen, P.

    2013-11-01

    This report provides detailed reactor designs and capital costs, and operating cost estimates for the hydrothermal liquefaction reactor system, used for biomass-to-biofuels conversion, under development at Pacific Northwest National Laboratory. Five cases were developed and the costs associated with all cases ranged from $22 MM/year - $47 MM/year.

  14. Kinetic and product composition study on the cellulose liquefaction in polyhydric alcohols.

    PubMed

    Shi, Yan; Li, Jingdan; Wang, Jing; Zhao, Tiantian; Yang, Hongmin; Jiang, Jianchun; Jiang, Xiaoxiang

    2016-08-01

    The liquefaction process of cellulose in polyhydric alcohols (PEG 400 and glycerol) was studied by TG-FTIR. Three stages were observed during the solvolysis process and the main liquefaction stage could be further divided into two zones. The differences of liquefaction behavior of cellulose in the two solvents were compared, and the functional groups of volatiles produced by solvolysis were also evaluated. A step-wise procedure based on iso-conversional and Master-plots methods was used for the kinetic and mechanism analysis of the main liquefaction stage. The calculation results based on the kinetic model were in agreement with the experimental data of the conversion rate. The kinetic parameters and mechanism functions between cellulose liquefaction in PEG400 and in glycerol were quite different, which verified that solvolysis behavior and reaction process were seriously influenced by solvent species. Finally, the detailed types of volatiles and product distribution were measured by Py-GC-MS. PMID:27155797

  15. Kinetic and product composition study on the cellulose liquefaction in polyhydric alcohols.

    PubMed

    Shi, Yan; Li, Jingdan; Wang, Jing; Zhao, Tiantian; Yang, Hongmin; Jiang, Jianchun; Jiang, Xiaoxiang

    2016-08-01

    The liquefaction process of cellulose in polyhydric alcohols (PEG 400 and glycerol) was studied by TG-FTIR. Three stages were observed during the solvolysis process and the main liquefaction stage could be further divided into two zones. The differences of liquefaction behavior of cellulose in the two solvents were compared, and the functional groups of volatiles produced by solvolysis were also evaluated. A step-wise procedure based on iso-conversional and Master-plots methods was used for the kinetic and mechanism analysis of the main liquefaction stage. The calculation results based on the kinetic model were in agreement with the experimental data of the conversion rate. The kinetic parameters and mechanism functions between cellulose liquefaction in PEG400 and in glycerol were quite different, which verified that solvolysis behavior and reaction process were seriously influenced by solvent species. Finally, the detailed types of volatiles and product distribution were measured by Py-GC-MS.

  16. Gasification of residual materials from coal liquefaction: Type-III extended pilot-plant evaluation of a molten Exxon donor solvent (EDS) liquefaction process residue from Illinois No. 6 coal

    SciTech Connect

    Robin, A.M.; Yang, H.L.

    1982-08-01

    A Type III Extended Pilot Plant Evaluation of Exxon EDS Vacuum Residue, which was obtained from the liquefaction of Illinois No. 6 coal at the Exxon Baytown Texas coal liquefaction pilot plant, was successfully completed at Texaco's Montebello Research Laboratory. A total of forty-four tons of EDS residue was gasified during five runs which were carried out at 1200 psig in the Texaco pilot plant residue gasifier. The solvent dilution levels, the steam-to-residue ratio and the oxygen-to-residue ratio were varied to determine optimum operating conditions. A total of 97 hours of on-stream time was accumulated. The longest continuous run was 28 hours. This work was authorized by DOE Delivery Order Number 6 under DOE contract DEAC01-76ET10137. It is part of a continuing project to evaluate residual materials from various DOE sponsored coal liquefaction projects to determine their suitability for conversion to hydrogen in one of the Texaco gasification processes.

  17. Gasification of residual materials from coal liquefaction. Type III extended pilot plant evaluation of a pelletized and ground Kerr McGee mineral ash residue from SRC-I coal liquefaction process

    SciTech Connect

    Wu, C.M.; Robin, A.M.

    1984-02-01

    A Type III extended pilot plant evaluation of pelletized and ground Kerr McGee mineral ash residue, which was obtained from the liquefaction of Illinois No. 6 coal at the SRC-I coal liquefaction process pilot plant at Wilsonville, Alabama, was successfully completed at Texaco's Montebello Research Laboratory (MRL). A total of 60 tons of residue was gasified during three runs which were carried out at 950 psig in the MRL High Pressure Solids Gasification Unit II gasifier. The oxygen-to-residue ratio was varied to determine optimum operating conditions. The runs lasted from 6.9 hours to 56.3 hours and a total of 72.9 hours of on-stream time was accumulated. This work was authorized by DOE Delivery Order Number 9 under DOE contract DEAC-01-76ET-10137. It is part of a continuing project to evaluate residual materials from various DOE sponsored coal liquefaction projects to determine their suitability for conversion to hydrogen using one of the Texaco gasification processes. 5 figures, 5 tables.

  18. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Technical progress report, October 1991--December 1991

    SciTech Connect

    Song, C.; Saini, A.; Huang, L.; Wenzel, K.; Hatcher, P.G.; Schobert, H.H.

    1992-01-01

    Low-temperature catalytic pretreatment is a promising approach to the development of an improved liquefaction process. This work is a fundamental study on effects of pretreatments on coal structure and reactivity in liquefaction. The main objectives of this project are to study the coal structural changes induced by low-temperature catalytic and thermal pretreatments by using spectroscopic techniques; and to clarify the pretreatment-induced changes in reactivity or convertibility of coals in the subsequent liquefaction. This report describes the progress of our work during the first quarterly period. Substantial progress has been made in the spectroscopic characterization of fresh and THF-extracted samples of two subbituminous coals and fresh samples of three bituminous coals using cross-polarization magic angle spinning (CPMAS) solid state {sup 13}C NMR and pyrolysis-GC-MS techniques. CPMAS {sup 13}C NMR and pyrolysis-GC-MS provided important information on carbon distribution/functionality and molecular components/structural units, respectively, for these coal samples. Pyrolysis-GC-MS revealed that there are remarkable structural differences in structural units between the subbituminous coals and the bituminous coals. Furthermore, significant progress has been made in the pretreatments and spectroscopic characterization of catalytically and thermally pretreated as well as physically treated Wyodak subbituminous coal, and temperature-staged and temperature-programmed thermal and catalytic liquefaction of a Montana subbituminous coal.

  19. Microbial recovery of metals from spent coal liquefaction catalysts. Final and quarterly report, July 1994--September 1994

    SciTech Connect

    Sandbeck, K.A.; Cleveland, D.

    1995-08-01

    Research is reported on the recovery of molybdenum and nickel from spent coal liquefaction catalysts. Mo release from spent coal liquefaction catalysts has been shown to be dependent upon many parameters, but release is dominated by microbial growth. The microbial Mo release is a rapid process requiring less than one week for 90% of the releaseable Mo to be solubilized from whole washed (THF) catalyst. It could be expected that the rates would be even greater with crushed catalyst. Efforts were centered on optimizing the parameters that stimulate microbial growth and action and further efforts centered on catalyst pre-treatment prior to microbial bio-leaching. Recent experiments suggest that hydrogen peroxide promises to be an effective pre-treatment wash. Hydrogen peroxide was also found to be an effective and economical agent for metals solubilization per se and could promote solubilization without subjecting the catalyst to microbial growth.

  20. EDS coal liquefaction process development: Phase V. Quarterly technical progress report, January 1-March 31, 1984

    SciTech Connect

    1984-07-01

    This report is the twenty-first Quarterly Technical Progress Report for US Department of Energy Cooperative Agreement No. DE-FC05-77ET10069 for EDS Coal Liquefaction Process Development Phase V. A detailed comparison of RCLU, CLPP, and ECLP yields has been initiated. This study builds off previous yield modeling results, which found that RCLU, CLPP, and ECLP yields were generally consistent given the scatter of the data, although some differences were noted. These pilot unit yield differences have now been quantified, and operating/configurational differences which account for some of them have been identified. Preliminary yield comparison results after correcting for these known process differences between the pilot plants indicate that: RCLU and CLPP yields are generally consistent; ECLP's conversion is about 5 lb/100 lb DAF coal lower than RCLU/CLPP at comparable operating conditions; and work has been initiated to define the EDS slurry preheater feed system design (based on slurry distributor manifold guidelines and coking correlation predictions, which influence furnace pass control issues such as slurry flow measurement). EDS hydrotreated naphtha showed a low level of systemic toxicity to rats exposed to the vapor six hours per day, five days per week for thirteen weeks.

  1. Fundamental studies of coal liquefaction. Quarterly report No. 7, April 1--July 1, 1993

    SciTech Connect

    Ross, D.S.

    1993-07-14

    In our last report we discussed observations in our cell concerning the behavior or Illinois No. 6 coal in tetralin to 460{degrees}C. We noted that there were possibly two distinct types of particles comprising the organic phase, reacting respectively at 420{degrees}--430{degrees}C, and at 450{degrees}--460{degrees}C. Alternatively we could interpret the data as describing a range of reactivity bounded by those temperatures. As evidenced by the contraction of the particles, the reactions were rapid. The particles lost half of their substance within 1 min, and we suggested that the rates were too fast to be accommodated by the commonly held scheme for coal liquefaction involving thermolytic scission of weak, bibenzyl-like bonds. Our analyses were aided by our use of Adobe Photoshop, which allows us to store, digitized versions of our recorded images. The images can then be manipulated at will to provide quantitative data on morphological changes. We noted in our last report that printer limitations prevented us from presenting images with the desirable quality, and we are at present attempting to find access to equipment which will provide satisfactory figures. Accordingly our progress will be described here without any photographs, and we expect to present a more complete account of our work in our next report. The work reported here includes studies of Illinois No. 6 coal with water as the medium, and a control run with argon as medium. Our temperature ramping was like that used last time, 25{degrees}C/min to 250{degrees}C, and then 10{degrees}C/min to 450{degrees}C. The results from the earlier work and the data presented here can therefore be directly compared.

  2. Fine particle clay catalysts for coal liquefaction. Quarterly technical progress report, November 9, 1991--February 8, 1992

    SciTech Connect

    Olson, E.S.

    1995-10-01

    The investigation of methods for the production and testing of iron-pillared clay catalysts was continued in this quarter. The surface area of the mixed alumina/iron pillared clay catalyst decreased to 51 m{sup 2}/g on sulfidation. Thus the stability of the alumina pillars during the sulfidation and thermal treatments prevented the total collapse that occurred in the case of the iron-pillared clays. Previously the mixed alumina/iron pillared clays were tested for hydrocracking activities with bibenzyl. This testing was extended to a determination of activity with a second model compound substrate (pyrene), representative of the polynuclear aromatic systems present in coal. Testing of the mixed alumina/iron-pillared catalysts with 1-methylnaphthalene gave interesting results that demonstrate shape selectivity. The clay-supported iron hydroxyoxide catalysts prepared by impregnation of iron species on acidic clays were further investigated. Sulfidation of these catalysts using the carbon disulfide in situ method gave hydrocracking activities with bibenzyl that were somewhat less than those obtained by presulfidation with H{sub 2}/H{sub 2}S mixtures. Liquefaction of Wyodak subbituminous coal was very successful with the iron impregnated clay catalyst, giving a highly soluble product. High conversions were also obtained with the mixed alumina/iron-pillared clay catalyst, but the yield of oil-solubles was considerably lower. Several new catalysts were synthesized with the idea of decreasing the pillar density and thereby increasing the micropore volume. These catalysts were prepared by first pillaring with an organic ammonium pillaring agent, then introducing a lower number of silica or alumina pillars. Finally the iron component was added either before or after thermal removal of organic pillars.

  3. Advanced direct liquefaction concepts for PETC generic units

    SciTech Connect

    Not Available

    1992-04-01

    In the Advance Coal Liquefaction Concept Proposal (ACLCP) carbon monoxide (CO) and water have been proposed as the primary reagents in the pretreatment process. The main objective of this project is to develop a methodology for pretreating coal under mild conditions based on a combination of existing processes which have shown great promise in liquefaction, extraction and pyrolysis studies. The aim of this pretreatment process is to partially depolymerise the coal, eliminate oxygen and diminish the propensity for retograde reactions during subsequent liquefaction. The desirable outcome of the CO pretreatment step should be: (1) enhanced liquefaction activity and/or selectivity toward products of higher quality due to chemical modification of the coal structure; (2) cleaner downstream products; (3) overall improvement in operability and process economics.

  4. Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction. Technical progress report, October 26, 1990--January 26, 1991: Draft

    SciTech Connect

    Klein, M.T.

    1991-02-22

    The first task in our proposed study of catalysts for coal liquefaction was to prepare ultrafine dispersed metal sulfide particles by reactive precipitation from solutions of appropriate metal precursors. At this point, equipment to allow us to prepare these air-sensitive materials in an anaerobic environment has been acquired and assembled. Initial experiments aimed at synthesizing iron sulfide particles have been initiated. As part of the investigation of short contact time catalytic coal liquefaction, initial efforts focused on the noncatalytic pyrolysis reactions of coal and a model compound, Dibenzyl ether (DBE). Two different reactor configurations were examined; catalytic experiments are planned for the coming month.

  5. Reconfigured, close-coupled reconfigured, and Wyodak coal integrated two-stage coal liquefaction process materials from the Wilsonville facility: Chemical and toxicological evaluation

    SciTech Connect

    Wright, C.W.

    1987-03-01

    This document reports the results of the chemical analysis and toxicological testing of process materials sampled during the operation of the Advanced Coal Liquefaction Research and Development Facility (Wilsonville, AL) in the reconfigured, integrated (RITSL run No. 247), the close-coupled, reconfigured, integrated (CCRITSL run No. 249), and the Wyodak coal integrated (ITSL run No. 246) two-stage liquefaction operating modes. Chemical methods of analysis included proton nuclear magnetic resonance spectroscopy, adsorption column chromatography, high resolution gas chromatography, gas chromatography/mass spectrometry, and low-voltage probe-inlet mass spectrometry. Toxicological evaluation of the process materials included a histidine reversion assay for microbial mutagenicity, an initiation/promotion assay for tumorigenicity in mouse skin, and an aquatic toxicity assay using Daphnia magna. The results of these analyses and tests are compared to the previously reported results derived from the Illinois No. 6 coal ITSL and nonintegrated two-stage liquefaction (NTSL) process materials from the Wilsonville facility. 21 refs., 13 figs., 21 tabs.

  6. Premium carbon products from coal

    SciTech Connect

    Rusinko, F. Jr.; Morrison, J.L.

    2000-07-01

    The face of the US coal industry and its markets are changing. Environmental concerns over global warming and plant emissions are two factors that will continue to gain national attention and consequently will challenge the use of coal in the US within its traditional markets. The decline of coke production in the US has lead to high quality metallurgical-grade coal being used to generate electricity. One could argue this is a waste of a limited valuable resource. The debate over global warming and the generation of greenhouse gases, particularly CO{sub 2}, will undoubtedly negatively impact the use of coal in newly constructed power plants. What is the future of the US coal industry and the industries that benefit from coal? This paper will review the use of coal and coal-derived materials in new, non-fuel markets. It will review a new industrial consortium that has recently been formed to stimulate the use of coal in value-added carbon markets. One of the questions the reader should ask when reading this paper is: Is coal more valuable for its carbon content or its BTU content? Carbon materials such as carbon fibers, carbon-carbon composites, specialty and mechanical graphite, activated carbon, carbon black, and carbon foams may provide new markets for the coal industry. These markets are expanding and some of these markets are in their infancy. These new material applications offer an exciting, but little recognized, opportunity for the expanded use of coal.

  7. Preconversion processing of bituminous coals: New directions to improved direct catalytic coal liquefaction. Quarterly report, January 1, 1993--March 31, 1993

    SciTech Connect

    Not Available

    1993-04-01

    The near equal conversions were obtained even with high coal/liquid ratio (1/3--1/2) for two-step wise high-temperature soaking and the first stage liquefaction. Expected conversions were not observed when vacuum distillation after soaking was used in stead of cyclohexane extraction. This is presumably due to the difficulty with redispersion of vacuum distillated bottoms in the coal liquid, because a batch wise procedure was taken by using glasswares. It is suggested that the proposed procedure in the previous quarter should be tested by a continuous procedure under enough heating conditions to keep low viscosity of the bottoms.

  8. Hydrogeologic investigation of the Advanced Coal Liquefaction Research and Development Facility, Wilsonville, Alabama

    SciTech Connect

    Gardner, F.G.; Kearl, P.M.; Mumby, M.E.; Rogers, S.

    1996-09-01

    This document describes the geology and hydrogeology at the former Advanced Coal Liquefaction Research and Development (ACLR&D) facility in Wilsonville, Alabama. The work was conducted by personnel from the Oak Ridge National Laboratory Grand Junction office (ORNL/GJ) for the U.S. Department of Energy (DOE) Pittsburgh Energy Technology Center (PETC). Characterization information was requested by PETC to provide baseline environmental information for use in evaluating needs and in subsequent decision-making for further actions associated with the closeout of facility operations. The hydrogeologic conceptual model presented in this report provides significant insight regarding the potential for contaminant migration from the ACLR&D facility and may be useful during other characterization work in the region. The ACLR&D facility is no longer operational and has been dismantled. The site was characterized in three phases: the first two phases were an environmental assessment study and a sod sampling study (APCO 1991) and the third phase the hydraulic assessment. Currently, a Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA) remedial investigation (RI) to address the presence of contaminants on the site is underway and will be documented in an RI report. This technical memorandum addresses the hydrogeologic model only.

  9. Investigating comprehensive two-dimensional gas chromatography conditions to optimize the separation of oxygenated compounds in a direct coal liquefaction middle distillate.

    PubMed

    Omais, Badaoui; Courtiade, Marion; Charon, Nadège; Thiébaut, Didier; Quignard, Alain; Hennion, Marie-Claire

    2011-05-27

    Considering the global energetic context, diversifying fuels is of growing importance and many new alternatives are promising. Coal liquefaction products definitely appear among the new generation substitutes. These product's characteristics are very far from fuel specifications as they are mainly composed of naphthenes, aromatics, polycondensed naphthenic and aromatic structures and heteroatomic compounds (nitrogen and oxygen), with a very low paraffin content. Identification and quantification of oxygen-containing species in coal-derived liquids are of considerable importance to understand their behaviors in further processing. However, these species have not been characterized as fully as the predominant hydrocarbon components. Literature shows that these compounds consist mainly in alkylated phenolic and furanic structures. Therefore, comprehensive two-dimensional gas chromatography has been investigated to provide enhanced molecular characterization of these complex samples. Several different configurations involving innovative column configurations were tested. Each of them was optimized by testing different column lengths, modulation periods, and oven conditions. A comparison of the contribution of each column configuration was carried out regarding four main criteria: individual separation of oxygenates, group type separation, resolution, and space occupation. One of them enabled an outstanding separation of paraffins, naphthenes, monoaromatics, diaromatics and targeted O-compounds in a direct coal liquefaction product. It was therefore subjected to further experimentations using a time-of-flight mass spectrometer to validate the identification and unravel more than fifty oxygenated molecular structures. A group-type quantification was also established for four column arrangements and gives the distribution of paraffins, naphthenes and aromatics. It can be concluded from this study that a non-orthogonal arrangement involving a highly polar column in the

  10. Studies in coal liquefaction with application to the SRC and related processes. Quarterly report, November 1981-January 1982

    SciTech Connect

    Tarrer, A.R.; Guin, J.A.; Curtis, C.W.

    1982-01-01

    The concentration of hydroaromatics in a coal liquefaction solvent is regarded as a significant factor in the determination of solvent quality. An analytical method is described based on catalytic solvent dehydrogenation (CSD) for the measurement of transferable hydrogen, including hydroaromatic sources, in a solvent. The dehydrogenation of several model compounds in the presence of Pd/CaCO/sub 3/ was conducted under batch conditions. Hydroaromatics containing six-member rings were found to dehydrogenate effectively. Lesser degrees of dehydrogenation were found for alkyl-substituted aromatics and saturated compounds. CSD was applied to a series of hydrogenated creosote oils plus several light recycle oils. The normalized H/sub 2/ volumes obtained by CSD could be correlated with the coal-dissolution ability of the creosote oils. It was not possible to include the light recycle oils in the same correlation. /sup 13/C-NMR was used to measure the transferable hydrogen of selected hydrogenated creosote oils and light recycle oils. Values of transferable hydrogen determined by /sup 13/C-NMR were generally larger than the corresponding values obtained by CSD. A smooth correlation was found between coal conversion and transferable hydrogen as measured by /sup 13/C-NMR. The light recycle oils could not be fitted to the curve defined by the creosote oils. Minerals indigenous to coal provide an internal but weak source of catalytic activity during liquefaction reactions. A sensitive probe reaction, cyclohexene hydrogenation/isomerization, was used to compare the catalytic activity of several clay minerals, oxides used as catalyst supports, pyrite and liquefaction residue ashes.

  11. Coal liquefaction by base-catalyzed hydrolysis with CO.sub.2 capture

    SciTech Connect

    Xiao, Xin

    2014-03-18

    The one-step hydrolysis of diverse biomaterials including coal, cellulose materials such as lumber and forestry waste, non-food crop waste, lignin, vegetable oils, animal fats and other source materials used for biofuels under mild processing conditions which results in the formation of a liquid fuel product along with the recovery of a high purity CO.sub.2 product is provided.

  12. Liquefaction process

    DOEpatents

    Gorbaty, Martin L.; Stone, John B.; Poddar, Syamal K.

    1982-01-01

    Scale formation during the liquefaction of lower ranking coals and similar carbonaceous materials is significantly reduced and/or prevented by pretreatment with a combination of pretreating agents comprising SO.sub.2 and an oxidizing agent. The pretreatment is believed to convert at least a portion of the scale-forming components and particularly calcium, to the corresponding sulfate prior to liquefaction. The pretreatment may be accomplished with the combination of pretreating agents either simultaneously by using a mixture comprising SO.sub.2 and an oxidizing agent or sequentially by first treating with SO.sub.2 and then with an oxidizing agent.

  13. Catalytic Two-Stage Liquefaction (CTSL) process bench studies with bituminous coal. Final report, [October 1, 1988--December 31, 1992

    SciTech Connect

    Comolli, A.G.; Johanson, E.S.; Karolkiewicz, W.F.; Lee, L.K.; Stalzer, R.H.; Smith, T.O.

    1993-03-01

    Reported herein are the details and results of Laboratory and Bench-Scale experiments using bituminous coal concluded at Hydrocarbon Research, Inc., under DOE contract during the period October 1, 1988 to December 31, 1992. The work described is primarily concerned with the application of coal cleaning methods and solids separation methods to the Catalytic Two-Stage Liquefaction (CTSL) Process. Additionally a predispersed catalyst was evaluated in a thermal/catalytic configuration, and an alternative nickel molybdenum catalyst was evaluated for the CTSL process. Three coals were evaluated in this program: Bituminous Illinois No. 6 Burning Star and Sub-bituminous Wyoming Black Thunder and New Mexico McKinley Mine seams. The results from a total of 16 bench-scale runs are reported and analyzed in detail. The tests involving the Illinois coal are reported herein, and the tests involving the Wyoming and New Mexico coals are described in Topical Report No. 1. On the laboratory scale, microautoclave tests evaluating coal, start-up oils, catalysts, thermal treatment, CO{sub 2} addition and sulfur compound effects are reported in Topical Report No. 3. Other microautoclave tests, such as tests on rejuvenated catalyst, coker liquids, and cleaned coals, are described in the Bench Run sections to which they refer. The microautoclave tests conducted for modelling the CTSL process are described in the CTSL Modelling section of Topical Report No. 3 under this contract.

  14. High conversion of coal to transportation fuels for the future with low HC gas production. Progress report, October 1, 1995--December 31, 1995

    SciTech Connect

    Wiser, W.H.; Oblad, A.G.

    1996-01-01

    Experimental coal liquefaction studies conducted in a batch microreactor in our laboratory have demonstrated potential for high conversions of coal to liquids with low yields of hydrocarbon (HC) gases, hence a small consumption of hydrogen in the primary liquefaction step. Ratios of liquids/HC gases as high as 30/1, at liquid yields as high as 82% of the coal by weight, have been achieved. The principal objective of this work is to examine how nearly we may approach these results in a continuous-flow system, at a size sufficient to evaluate the process concept for production of transportation fuels from coal.

  15. Zinc sulfide liquefaction catalyst

    DOEpatents

    Garg, Diwakar

    1984-01-01

    A process for the liquefaction of carbonaceous material, such as coal, is set forth wherein coal is liquefied in a catalytic solvent refining reaction wherein an activated zinc sulfide catalyst is utilized which is activated by hydrogenation in a coal derived process solvent in the absence of coal.

  16. Characterization of selected Ohio coals to predict their conversion behavior relative to 104 North American Coals. [Factors correlating with liquefaction behavior

    SciTech Connect

    Whitacre, T. P.; Hunt, T. J.; Kneller, W. A.

    1982-02-01

    Twenty-six coal samples from Ohio were collected as washed and seam samples, and lithobodies within the seams. Characterization of these samples included determination of % maceral, % anti R/sub max/, LTA, chlorine content and proximate/ultimate and qualitative mineral analyses. These data were compared to data from a similar project by Yarzab, R.F., et al., 1980 completed at Pennsylvania State University using tetralin as the hydrogen donor solvent. The characteristics of these coals were correlated with liquefaction conversion and other data accrued on 104 North American coals by statistical analyses. Utilizing percent carbon, sulfur, volatile matter, reflectance, vitrinite and total reactive macerals, Q-mode cluster analysis demonstrated that Ohio coals are more similar to the coals of the Interior province than to those of the Appalachian province. Linear multiple regression analysis for the 104 North American coals provided a prediction equation for conversion (R = .96). The predicted conversion values for the samples range from 58.8 to 79.6%, with the Lower Kittanning (No. 5) and the Middle Kittanning (No. 6) coal seams showing the highest predicted percent conversion (respectively, 73.4 and 72.2%). The moderately low FSI values for the No. 5 and No. 6 coals (respectively, 2.5 and 3) and their moderately high alkaline earth content (respectively, 0.69 and 0.74%) suggest that these coals possess the best overall properties for conversion. Stepwise regression has indicated that the most important coal characteristics affecting conversion are, in decreasing order of importance: % volatile matter, % vitrinite and % total sulfur. Conversion processes can be expected to produce higher yields with Ohio coals due to the presence of such mineral catalysts as pyrite and kaolinite. It is believed that the presence of these disposable catalysts increases the marketability of Ohio coals.

  17. Solvent tailoring in coal liquefaction. Quarterly report, May 1982-August 1982. [Comparison of subcritical and supercritical conditions

    SciTech Connect

    Tarrer, A.R.; Guin, J.A.; Curtis, C.W.; Williams, D.C.

    1982-01-01

    The initial objective of this work was to study the phase distribution of donor solvents and solvent mixtures during the liquefaction of coal, to investigate the effects of phase distribution on coal conversion, and to determine the advantages, if any, of operating at subcritical and/or supercritical conditions. Computer simulations were used to predict the phase distribution, for various binary systems, as a function of temperature. The FLASH program was used to theoretically predict phase distribution for various model systems. Due to limitations in the computer program, success was achieved only in a few cases. Even in these cases, the existence of two-phase regions was observed only at temperatures and pressures far below normal liquefaction conditions. An extensive review of the literature was carried out in order to survey methods of experimentally studying vapor-liquid equilibria. Finally, some preliminary laboratory studies were carried out with the use of benzothiophene-dodecane as the model reaction system. It was felt that the study of the effect of reactor configuration on conversion would provide insight into whether phase distribution or mass transfer was the limiting consideration for coal conversion. However, no conclusive results were obtained from these studies.

  18. [Mechanism of hydrogen incorporation in coal liquefaction]. Thirteenth progress report, [July--September 1994

    SciTech Connect

    Guthrie, R.D.

    1994-12-01

    This document is divided into: Thermal reactions of unsaturated compounds with D{sub 2}, silica-catalyzed hydrogenations of alkenes, experiments with surface attached coal models, and experiments with 2,2,5,5-tetramethyl-3,4-diphenylhexane (formation of stilbene and other products).

  19. PRODUCTION OF FOAMS, FIBERS AND PITCHES USING A COAL EXTRACTION PROCESS

    SciTech Connect

    Chong Chen; Elliot B. Kennel; Liviu Magean; Pete G. Stansberry; Alfred H. Stiller; John W. Zondlo

    2004-06-20

    This Department of Energy National Energy Technology Laboratory sponsored project developed processes for converting coal feedstocks to carbon products, including coal-derived pitch, coke foams and fibers based on solvent extraction processes. A key technology is the use of hydrogenation accomplished at elevated temperatures and pressures to obtain a synthetic coal pitch. Hydrogenation, or partial direct liquefaction of coal, is used to modify the properties of raw coal such that a molten synthetic pitch can be obtained. The amount of hydrogen required to produce a synthetic pitch is about an order of magnitude less than the amount required to produce synthetic crude oil. Hence the conditions for synthetic pitch production consume very little hydrogen and can be accomplished at substantially lower pressure. In the molten state, hot filtration or centrifugation can be used to separate dissolved coal chemicals from mineral matter and insolubles (inertinite), resulting in the production of a purified hydrocarbon pitch. Alternatively, if hydrogenation is not used, aromatic hydrocarbon liquids appropriate for use as precursors to carbon products can obtained by dissolving coal in a solvent. As in the case for partial direct liquefaction pitches, undissolved coal is removed via hot filtration or centrifugation. Excess solvent is boiled off and recovered. The resultant solid material, referred to as Solvent Extracted Carbon Ore or SECO, has been used successfully to produce artificial graphite and carbon foam.

  20. SRC-1: coal liquefaction demonstration plant. Project Baseline assessment report supplement

    SciTech Connect

    Not Available

    1984-09-01

    ICRC issued a Revised Baseline for the SRC-I Demonstration Project in order to incorporate the results of these research activities and the changes in the design that had occurred since FY82. The Revised Baseline, prepared by ICRC, provides the necessary information for any future government or commercial decisions relating to the design, construction and operation of an SRC-I-type coal liquefaction facility. No further activities to complete the design of the demonstration plant, or to proceed with construction are planned by DOE. The Project Baseline is an ICRC-documented reference for controlling any future project work and cost. The original Baseline was issued in March 1982; this summary document is available from National Technical Information Service (NTIS) as document number DOE/ORO/030540-T13. The Revised Baseline (dated April 1984) is available as document numbers DOE/OR/03054-T14 and T16. Supporting documentation, in the main concerned with research activities undertaken in support of the design, is also available from NTIS as DOE/OR/03054-T1 through T10 and DOE/OR/03054-1 through 125. The Baseline itself is made up of a documented design configuration, a documented estimate, in First Quarter Fiscal Year 1982 Dollars (1QFY82$), and a detailed schedule of the activities required to complete the project as of 3QFY82. The Baseline design is embodied in the 26 process design packages and other support documentation identified in the Baseline, as well as preliminary engineering flow diagrams prepared for all of the major process areas of the plant. All elements of the Project Baseline were developed within the constraints of the project criteria.