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.

Process for improving soluble coal yield in a coal deashing process

DOEpatents

Rhodes, Donald E.

1980-01-01

Coal liquefaction products are contacted with a deashing solvent and introduced into a first separation zone. The first separation zone is maintained at an elevated temperature and pressure, determined to maximize the recovery of soluble coal products, to cause said coal liquefaction products to separate into a first light phase and a first heavy phase. Under these conditions the heavy phase while still fluid-like in character is substantially non-flowable. Flowability is returned to the fluid-like heavy phase by the introduction of an additional quantity of deashing solvent into the first separation zone at a location below the interface between the first light and heavy phases or into the heavy phase withdrawal conduit during withdrawal of the first heavy phase and prior to any substantial pressure reduction. The first heavy phase then is withdrawn from the first separation zone for additional downstream processing without plugging either the withdrawal conduit or the downstream apparatus. The first light phase comprising the soluble coal products is withdrawn and recovered in an increased yield to provide a more economical coal deashing process.

Deashing macroalgae biomass by pulsed electric field treatment.

PubMed

Robin, Arthur; Sack, Martin; Israel, Alvaro; Frey, Wolfgang; Müller, Georg; Golberg, Alexander

2018-05-01

Among all biomass constituents, the ashes are major hurdles for biomass processing. Ashes currently have low market value and can make a non-negligible fraction of the biomass dry weight significantly impacting its further processing by degrading equipment, lowering process yield, inhibiting reactions and decreasing products qualities. However, most of the current treatments for deashing biomass are of poor efficiency or industrial relevance. This work is the first report on the use of Pulsed Electric Field (PEF) to enhance deashing of biomass from a high ash content green marine macroalga, Ulva sp., using hydraulic pressing. By inducing cell permeabilization of the fresh biomass, PEF was able to enhance the ash extraction from 18.4% (non-treated control) to 37.4% of the total ash content in average, significantly enhancing the extraction of five of the major ash elements (K, Mg, Na, P and S) compared to pressing alone. Copyright © 2018 Elsevier Ltd. All rights reserved.

Investigating the sorption behavior of cadmium from aqueous solution by potassium permanganate-modified biochar: quantify mechanism and evaluate the modification method.

PubMed

Fan, Zixi; Zhang, Qian; Li, Meng; Niu, Dongyuan; Sang, Wenjiao; Verpoort, Francis

2018-03-01

In this work, a KMnO 4 -modified-biochar-based composite material with manganese oxide produced at 600 °C was fabricated to investigate the sorption mechanism of Cd(II) and to comprehensively evaluate the effect of the modification on biochar properties. Cd(II) adsorption mechanisms were mainly controlled by interaction with minerals, complexation with oxygen-containing functional groups, and cation-π interaction. The sorption capacity was significantly reduced after a deash treatment of biochar, almost shrunk by 3 and 3.5 times for pristine biochar (PBC) and modified biochar (MBC). For deashed PBC, oxygen-containing functional groups were the main contributor toward Cd(II) adsorption while interaction with minerals was significantly compromised and became negligible. The sorption capacity was also apparently decreased after the deash treatment of MBC; however, for deashed MBC, interaction with minerals still was the main contributor to the sorption ability, which could be attributed to the mechanism of interaction of Cd(II) with loaded MnO x on biochar. Cation-π interaction in MBC was notably enhanced compared to PBC due to the oxidation of KMnO 4 on biomass. Also, sorption performance by oxygen-containing functional groups was also enhanced. Hence, the modification by KMnO 4 has a significant effect on the Cd(II) sorption performance of biochar.

Fermentation and chemical treatment of pulp and paper mill sludge

DOEpatents

Lee, Yoon Y; Wang, Wei; Kang, Li

2014-12-02

A method of chemically treating partially de-ashed pulp and/or paper mill sludge to obtain products of value comprising taking a sample of primary sludge from a Kraft paper mill process, partially de-ashing the primary sludge by physical means, and further treating the primary sludge to obtain the products of value, including further treating the resulting sludge and using the resulting sludge as a substrate to produce cellulase in an efficient manner using the resulting sludge as the only carbon source and mixtures of inorganic salts as the primary nitrogen source, and including further treating the resulting sludge and using the resulting sludge to produce ethanol.

Deashing of coal liquids with ceramic membrane microfiltration and diafiltration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bishop, B.; Goldsmith, R.

1995-12-31

Removal of mineral matter from liquid hydrocarbons derived from the direct liquefaction of coal is required for product acceptability. Current methods include critical solvent deashing (Rose{sup {reg_sign}} process from Kerr-McGee) and filtration (U.S. Filter leaf filter as used by British Coal). These methods produce ash reject streams containing up to 15% of the liquid hydrocarbon product. Consequently, CeraMem proposed the use of low cost, ceramic crossflow membranes for the filtration of coal liquids bottoms to remove mineral matter and subsequent diafiltration (analogous to cake washing in dead-ended filtration) for the removal of coal liquid from the solids stream. The usemore » of these ceramic crossflow membranes overcomes the limitations of traditional polymeric crossflow membranes by having the ability to operate at elevated temperature and to withstand prolonged exposure to hydrocarbon and solvent media. In addition, CeraMem`s membrane filters are significantly less expensive than competitive ceramic membranes due to their unique construction. With these ceramic membrane filters, it may be possible to reduce the product losses associated with traditional deashing processes at an economically attractive cost. The performance of these ceramic membrane microfilters is discussed.« less

Enhanced Ethanol Production from De-Ashed Paper Sludge by Simultaneous Saccharification and Fermentation and Simultaneous Saccharification and Co-Fermentation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kang, L.; Wang, W.; Pallapolu, V. R.

2011-11-01

A previous study demonstrated that paper sludges with high ash contents can be converted to ethanol by simultaneous saccharification and fermentation (SSF) or simultaneous saccharification and co-fermentation (SSCF). High ash content in the sludge, however, limited solid loading in the bioreactor, causing low product concentration. To overcome this problem, sludges were de-ashed before SSF and SSCF. Low ash content in sludges also increased the ethanol yield to the extent that the enzyme dosage required to achieve 70% yield in the fermentation process was reduced by 30%. High solid loading in SSF and SSCF decreased the ethanol yield. High agitation andmore » de-ashing of the sludges were able to restore the part of the yield loss caused by high solid loading. Substitution of the laboratory fermentation medium (peptone and yeast extract) with corn steep liquor did not bring about any adverse effects in the fermentation. Fed-batch operation of the SSCF and SSF using low-ash content sludges was effective in raising the ethanol concentration, achieving 47.8 g/L and 60.0 g/L, respectively.« less

Coal hydrogenation and deashing in ebullated bed catalytic reactor

DOEpatents

Huibers, Derk T. A.; Johanson, Edwin S.

1983-01-01

An improved process for hydrogenation of coal containing ash with agglomeration and removal of ash from an ebullated bed catalytic reactor to produce deashed hydrocarbon liquid and gas products. In the process, a flowable coal-oil slurry is reacted with hydrogen in an ebullated catalyst bed reaction zone at elevated temperature and pressure conditions. The upward velocity and viscosity of the reactor liquid are controlled so that a substantial portion of the ash released from the coal is agglomerated to form larger particles in the upper portion of the reactor above the catalyst bed, from which the agglomerated ash is separately withdrawn along with adhering reaction zone liquid. The resulting hydrogenated hydrocarbon effluent material product is phase separated to remove vapor fractions, after which any ash remaining in the liquid fraction can be removed to produce substantially ash-free coal-derived liquid products.

Variation in sorption of propiconazole with biochars: The effect of temperature, mineral, molecular structure, and nano-porosity

USDA-ARS?s Scientific Manuscript database

Sorption behavior of propiconazole (PROPI) by plant-residue derived biochars (PLABs) and animal manure-derived biochars (ANIBs) obtained at three heating treatment temperatures (HTTs) at 300, 450 and 600 degrees Celsius (denoted as BCs300, BCs450, and BCs600) and their corresponding de-ashed BCs450 ...

Chemical comminution and deashing of low-rank coals

DOEpatents

Quigley, David R.

1992-01-01

A method of chemically comminuting a low-rank coal while at the same time increasing the heating value of the coal. A strong alkali solution is added to a low-rank coal to solubilize the carbonaceous portion of the coal, leaving behind the noncarbonaceous mineral matter portion. The solubilized coal is precipitated from solution by a multivalent cation, preferably calcium.

Chemical comminution and deashing of low-rank coals

DOEpatents

Quigley, David R.

1992-12-01

A method of chemically comminuting a low-rank coal while at the same time increasing the heating value of the coal. A strong alkali solution is added to a low-rank coal to solubilize the carbonaceous portion of the coal, leaving behind the noncarbonaceous mineral matter portion. The solubilized coal is precipitated from solution by a multivalent cation, preferably calcium.

Process for producing low-sulfur boiler fuel by hydrotreatment of solvent deashed SRC

DOEpatents

Roberts, George W.; Tao, John C.

1985-01-01

In this invention, a process is disclosed characterized by heating a slurry of coal in the presence of a process-derived recycle solvent and passing same to a dissolver zone, separating the resultant gases and liquid/solid products therefrom, vacuum distilling the liquid/solids products, separating the portions of the liquid/solids vacuum distillation effluent into a solid ash, unconverted coal particles and SRC material having a boiling point above 850.degree. F. and subjecting same to a critical solvent deashing step to provide an ash-free SRC product. The lighter liquid products from the vacuum distillation possess a boiling point below 850.degree. F. and are passed through a distillation tower, from which recycled solvent is recovered in addition to light distillate boiling below 400.degree. F. (overhead). The ash-free SRC product in accompanyment with at least a portion of the process derived solvent is passed in combination to a hydrotreating zone containing a hydrogenation catalyst and in the presence of hydrogen is hydroprocessed to produce a desulfurized and denitrogenized low-sulfur, low-ash boiler fuel and a process derived recycle solvent which is recycled to slurry the coal in the beginning of the process before heating.

Operation of the solvent-refined-coal pilot plant, Wilsonville, Alabama. Annual technical report, January-December 1980

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lewis, H.E.

1981-08-01

The plant was in operation for the equivalent of 247 days, an on-stream factor of 67.7%. Kentucky 9 coals from the Lafayette, Dotiki and Fies mines were processed. During 1980, the operating conditions and equipment were adjusted to evaluate potential process improvements. These experiments produced significant results in the following areas: Operating V103 High Pressure Separator in the hot mode; varying T102 Vacuum Column operating temperature; adding light SRC (LSRC), a product of the third stage of the Critical Solvent Deashing (CSD) unit, to the process solvent; investigating the effects of the chlorine content of the feed coal on corrosionmore » in the process vessels; evaluating the effects of adding sodium carbonate on corrosion rates; operating under conditions of low severity; i.e., low reactor temperature and long residence time; and testing an alternate CSD deashing solvent. A series of simulation runs investigating the design operating conditions for a planned 6000 ton per day SRC-I demonstation plant were also completed. Numerous improvements were made in the CSD processing area, and the components for a hydrotreating unit were installed.« less

Enrichment of individual KIR2DL4 sequences from genomic DNA using long-template PCR and allele-specific hybridization to magnetic bead-bound oligonucleotide probes.

PubMed

Roberts, C H; Turino, C; Madrigal, J A; Marsh, S G E

2007-06-01

DNA enrichment by allele-specific hybridization (DEASH) was used as a means to isolate individual alleles of the killer cell immunoglobulin-like receptor (KIR2DL4) gene from heterozygous genomic DNA. Using long-template polymerase chain reaction (LT-PCR), the complete KIR2DL4 gene was amplified from a cell line that had previously been characterized for its KIR gene content by PCR using sequence-specific primers (PCR-SSP). The whole gene amplicons were sequenced and we identified two heterozygous positions in accordance with the predictions of the PCR-SSP. The amplicons were then hybridized to allele-specific, biotinylated oligonucleotide probes and through binding to streptavidin-coated beads, the targeted alleles were enriched. A second PCR amplified only the exonic regions of the enriched allele, and these were then sequenced in full. We show DEASH to be capable of enriching single alleles from a heterozygous PCR product, and through sequencing the enriched DNA, we are able to produce complete coding sequences of the KIR2DL4 alleles in accordance with the typing predicted by PCR-SSP.

Development of clean coal and clean soil technologies using advanced agglomeration technologies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ignasiak, B.; Pawlak, W.; Szymocha, K.

1990-04-01

The specific objectives of the bituminous coal program were to explore and evaluate the application of advanced agglomeration technology for: (1)desulphurization of bituminous coals to sulphur content acceptable within the current EPA SO{sub 2} emission guidelines; (2) deashing of bituminous coals to ash content of less than 10 percent; and (3)increasing the calorific value of bituminous coals to above 13,000 Btu/lb. (VC)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

Prior to 1978, the Wilsonville Advanced Coal Liquefaction facility material balance surrounded only the thermal liquefaction unit and involved analyses of only the slurry stream and individual gas streams. The distillate solvent yield was determined by difference. Subsequently, several modifications and additional process units were introduced to this single unit system. With the inclusion of the deashing unit in 1978 and the catalytic hydrogenation unit in 1981, the process has evolved into a sophisticated two-stage coal liquefaction process and has the potential for various modes of integration. This report presents an elemental balancing procedure and a simplified presentation format thatmore » is sufficiently flexible to meet current and future needs. The development of the elemental balancing technique and the relevant computer programs to handle the calculations have been addressed. This will be useful in modelling individual unit performance as well as determining the impact of each unit on the overall liquefaction system, provided the units are on a steady-state basis. Five different material balance envelopes are defined. Three of these envelopes pertain to the individual units (the thermal liquefaction or TL unit, the Critical Solvent Deashing or CSD unit and the H-Oil Ebullated Bed Hydrotreating or HTR unit). The fourth or single stage material balance envelope combines the TL and CSD units. The fifth envelope is the two-stage configuration combining all three units. 3 references.« less

Constitution of Drop-Tube-Generated Coal Chars from Vitrinite- and Inertinite-Rich South African Coals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Louw, Enette B.; Mitchell, Gareth D.; Wang, Juan

The structural transformations of coal and the resultant char morphologies are strongly dependent on the initial structure and degree of thermoplasticity achieved during coal-to-char transition. These are a function of petrographic composition, rank, particle size, and heating rate and strongly affect combustion behavior. This study compares the devolatilization and subsequent combustion behavior of an inertinite-rich (87.7% dmmf) and a vitrinite-rich (91.8% dmmf) South African coal, wet-screened to a narrow particle size distribution of 200 x 400 mesh. Pyrolysis chars were generated under rapid-heating conditions (104-105 °C/s) in a drop-tube reactor to closely resemble chars generated in pulverized combustion conditions. Themore » inertinite-rich coal took ~ 400 ms to devolatilize in the drop-tube, compared to only ~ 240 ms for the vitrinite-rich sample. The chemical and physical structure (the constitution) of the chars were investigated through a range of chemical, physical, and optical characteristics including the maceral differences, and high ash yields. To evaluate the combustion reactivity non-isothermal burn-out profiles were obtained through thermogravimetrical analyses (TGA) in air. The vitrinite-rich char had on average 20% higher reaction rates than the inertinite-rich char under the various combustion conditions. The char samples were de-ashed with HCl and HF acid which resulted in an increase in combustion reactivity. The maximum reaction rate of the high-ash (36% ash yield) inertinite-rich char increased with 80% after de-ashing. While the vitrinite-rich char with an ash yield of 15%, had a 20% increase in reactivity after de-ashing. The ash acted as a barrier, and the removal of ash most likely increased the access to reactive surface area. The chemical and physical structures of the chars were characterized through a range of different analytical techniques to quantify the factors contributing to reactivity differences. The morphologies of the chars were characterized with SEM and optical microscopy, while quantitative information on the ordered nature of chars was obtained through XRD on de-ashed chars. The inertinite-rich coal experienced limited fluidity during heat-treatment, resulting in slower devolatilization, limited growth in crystallite height (11.8 to 12.6Å), only rounding of particle edges, and producing > 40% of mixed-dense type chars. The vitrinite-char showed more significant structural transformations; producing mostly (80%) extensively swollen crassisphere, tenuisphere, and network-type chars, and XRD showed a large increase in crystallite height (4.3 to 11.7Å). Nitrogen adsorption and small-angle X-ray scattering (SAXS) were utilized to compare the nitrogen surface areas and pore size distributions. Both chars were mostly mesoporous but the inertinite-rich char had double the average pore size, which also resulted in a larger nitrogen surface area since nitrogen can only access surface areas in larger pores. The BET surface area was 3.9 and 2.7 m2/g for the inertinite- and vitrinite-rich chars respectively. SAXS data showed that the vitrinite-rich char had 60% higher frequencies of pores in the micropore range. Helium porosimetry indicated that the inertinite-rich coal and resultant char had higher densities than the vitrinite coal and char; 1.6 and 2.0 g/cm3, compared to 1.3 and 1.9 g/cm3 (dry basis). Non-isothermal TGA burnout profiles showed the inertinite-rich char had a burnout temperature of 680°C, slightly higher than the vitrinite-rich char’s 650 °C. This, along with the peak shape and position in the burnout profiles indicate that the vitrinite-rich char has a higher reactivity. The higher reactivity is due to a combination of factors likely including less organization, grater porosity and access to the reactive site, less ash blocking, and char morphology differences.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

M. Mercedes Maroto-Valer; John M. Andresen; Yinzhi Zhang

This research program focused on the development of fly ash derived sorbents to capture CO{sub 2} from power plant flue gas emissions. The fly ash derived sorbents developed represent an affordable alternative to existing methods using specialized activated carbons and molecular sieves, that tend to be very expensive and hinder the viability of the CO{sub 2} sorption process due to economic constraints. Under Task 1 'Procurement and characterization of a suite of fly ashes', 10 fly ash samples, named FAS-1 to -10, were collected from different combustors with different feedstocks, including bituminous coal, PRB coal and biomass. These samples presentedmore » a wide range of LOI value from 0.66-84.0%, and different burn-off profiles. The samples also spanned a wide range of total specific surface area and pore volume. These variations reflect the difference in the feedstock, types of combustors, collection hopper, and the beneficiation technologies the different fly ashes underwent. Under Task 2 'Preparation of fly ash derived sorbents', the fly ash samples were activated by steam. Nitrogen adsorption isotherms were used to characterize the resultant activated samples. The cost-saving one-step activation process applied was successfully used to increase the surface area and pore volume of all the fly ash samples. The activated samples present very different surface areas and pore volumes due to the range in physical and chemical properties of their precursors. Furthermore, one activated fly ash sample, FAS-4, was loaded with amine-containing chemicals (MEA, DEA, AMP, and MDEA). The impregnation significantly decreased the surface area and pore volume of the parent activated fly ash sample. Under Task 3 'Capture of CO{sub 2} by fly ash derived sorbents', sample FAS-10 and its deashed counterpart before and after impregnation of chemical PEI were used for the CO{sub 2} adsorption at different temperatures. The sample FAS-10 exhibited a CO{sub 2} adsorption capacity of 17.5mg/g at 30 C, and decreases to 10.25mg/g at 75 C, while those for de-ashed counterpart are 43.5mg/g and 22.0 mg/g at 30 C and 75 C, respectively. After loading PEI, the CO{sub 2} adsorption capacity increased to 93.6 mg/g at 75 C for de-ashed sample and 62.1 mg/g at 75 C for raw fly ash sample. The activated fly ash, FAS-4, and its chemical loaded counterparts were tested for CO{sub 2} capture capacity. The activated carbon exhibited a CO{sub 2} adsorption capacity of 40.3mg/g at 30 C that decreased to 18.5mg/g at 70 C and 7.7mg/g at 120 C. The CO{sub 2} adsorption capacity profiles changed significantly after impregnation. For the MEA loaded sample the capacity increased to 68.6mg/g at 30 C. The loading of MDEA and DEA initially decreased the CO{sub 2} adsorption capacity at 30 C compared to the parent sample but increased to 40.6 and 37.1mg/g, respectively, when the temperature increased to 70 C. The loading of AMP decrease the CO{sub 2} adsorption capacity compared to the parent sample under all the studied temperatures. Under Task 4 'Comparison of the CO{sub 2} capture by fly ash derived sorbents with commercial sorbents', the CO{sub 2} adsorption capacities of selected activated fly ash carbons were compared to commercial activated carbons. The CO{sub 2} adsorption capacity of fly ash derived activated carbon, FAS-4, and its chemical loaded counterpart presented CO{sub 2} capture capacities close to 7 wt%, which are comparable to, and even better than, the published values of 3-4%.« less

Bioconversion of paper mill sludge to bioethanol in the presence of accelerants or hydrogen peroxide pretreatment.

PubMed

Gurram, Raghu Nandan; Al-Shannag, Mohammad; Lecher, Nicholas Joshua; Duncan, Shona M; Singsaas, Eric Lawrence; Alkasrawi, Malek

2015-09-01

In this study we investigated the technical feasibility of convert paper mill sludge into fuel ethanol. This involved the removal of mineral fillers by using either chemical pretreatment or mechanical fractionation to determine their effects on cellulose hydrolysis and fermentation to ethanol. In addition, we studied the effect of cationic polyelectrolyte (as accelerant) addition and hydrogen peroxide pretreatment on enzymatic hydrolysis and fermentation. We present results showing that removing the fillers content (ash and calcium carbonate) from the paper mill sludge increases the enzymatic hydrolysis performance dramatically with higher cellulose conversion at faster rates. The addition of accelerant and hydrogen peroxide pretreatment further improved the hydrolysis yields by 16% and 25% (g glucose / g cellulose), respectively with the de-ashed sludge. The fermentation process of produced sugars achieved up to 95% of the maximum theoretical ethanol yield and higher ethanol productivities within 9h of fermentation. Copyright © 2015 Elsevier Ltd. All rights reserved.

Acetone-butanol-ethanol production from Kraft paper mill sludge by simultaneous saccharification and fermentation.

PubMed

Guan, Wenjian; Shi, Suan; Tu, Maobing; Lee, Yoon Y

2016-01-01

Paper mill sludge (PS), a solid waste from pulp and paper industry, was investigated as a feedstock for acetone-butanol-ethanol (ABE) production by simultaneous saccharification and fermentation (SSF). ABE fermentation of paper sludge by Clostridium acetobutylicum required partial removal of ash in PS to enhance its enzymatic digestibility. Enzymatic hydrolysis was found to be a rate-limiting step in the SSF. A total of 16.4-18.0g/L of ABE solvents were produced in the SSF of de-ashed PS with solid loading of 6.3-7.4% and enzyme loading of 10-15FPU/g-glucan, and the final solvent yield reached 0.27g/g sugars. No pretreatment and pH control were needed in ABE fermentation of paper sludge, which makes it an attractive feedstock for butanol production. The results suggested utilization of paper sludge should not only consider the benefits of buffering effect of CaCO3 in fermentation, but also take into account its inhibitory effect on enzymatic hydrolysis. Published by Elsevier Ltd.