Biomimetic 'greener' approach to nanomaterials and their safer application in catalysis and remediation

EPA Science Inventory

Vitamins B1,1a B2, C,1b and tea polyphenols1c which function both as reducing and capping agents, provide extremely simple, one-pot, green synthetic methods to bulk quantities of nanomaterials in water. Shape-controlled synthesis of noble nanostructures via microwave (MW)-assiste...

Microwave-Assisted Synthesis of Phenothiazine and Quinoline Derivatives

PubMed Central

Găină, Luiza; Cristea, Castelia; Moldovan, Claudia; Porumb, Dan; Surducan, Emanoil; Deleanu, Călin; Mahamoud, Abdalah; Barbe, Jacques; Silberg, Ioan A.

2007-01-01

Application of a dynamic microwave power system in the chemical synthesis of some phenothiazine and quinoline derivatives is described. Heterocyclic ring formation, aromatic nucleophilic substitution and heterocyclic aldehydes/ketones condensation reactions were performed on solid support, or under solvent free reaction conditions. The microwave-assisted Duff formylation of phenothiazine was achieved. Comparison of microwave-assisted synthesis with the conventional synthetic methods demonstrates advantages related to shorter reaction times and in some cases better reaction yields.

Microwave Assisted Synthesis of Biorelevant Benzazoles.

PubMed

Seth, Kapileswar; Purohit, Priyank; Chakraborti, Asit K

2017-01-01

The benzazole scaffolds are present in various therapeutic agents and have been recognized as the essential pharmacophore for diverse biological activities. These have generated interest and necessity to develop efficient synthetic methods of these privileged classes of compounds to generate new therapeutic leads for various diseases. The biological activities of the benzazoles and efforts towards their synthesis have been summarized in a few review articles. In view of these, the aim of this review is to provide an account of the developments that have taken place in the synthesis of biorelevant benzazoles under microwave irradiation as the application of microwave heating has long been recognized as a green chemistry tool for speedy generation of synthetic targets. Attention has been focused to those literature reports wherein the use of microwave irradiation is the key step in the formation of the heterocyclic ring system or in functionalization of the benzazole ring system to generate the essential pharmacophoric feature. The convenient and economic way to synthesize these privileged class of heterocycles through the use of microwave irradiation that would be beneficial for the drug discovery scientist to synthesize biologically active benzazoles and provide access to wide range of reactions for the synthesis of benzazoles constitute the theme of this review. Examples have been drawn wherein the use of microwave heating offers distinct advantage in terms of improved product yields and reduction of reaction time as compared to those observed for the synthesis under conventional heating. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

A Review of Microwave-Assisted Reactions for Biodiesel Production

PubMed Central

Nomanbhay, Saifuddin; Ong, Mei Yin

2017-01-01

The conversion of biomass into chemicals and biofuels is an active research area as trends move to replace fossil fuels with renewable resources due to society’s increased concern towards sustainability. In this context, microwave processing has emerged as a tool in organic synthesis and plays an important role in developing a more sustainable world. Integration of processing methods with microwave irradiation has resulted in a great reduction in the time required for many processes, while the reaction efficiencies have been increased markedly. Microwave processing produces a higher yield with a cleaner profile in comparison to other methods. The microwave processing is reported to be a better heating method than the conventional methods due to its unique thermal and non-thermal effects. This paper provides an insight into the theoretical aspects of microwave irradiation practices and highlights the importance of microwave processing. The potential of the microwave technology to accomplish superior outcomes over the conventional methods in biodiesel production is presented. A green process for biodiesel production using a non-catalytic method is still new and very costly because of the supercritical condition requirement. Hence, non-catalytic biodiesel conversion under ambient pressure using microwave technology must be developed, as the energy utilization for microwave-based biodiesel synthesis is reported to be lower and cost-effective. PMID:28952536

A Review of Microwave-Assisted Reactions for Biodiesel Production.

PubMed

Nomanbhay, Saifuddin; Ong, Mei Yin

2017-06-15

The conversion of biomass into chemicals and biofuels is an active research area as trends move to replace fossil fuels with renewable resources due to society's increased concern towards sustainability. In this context, microwave processing has emerged as a tool in organic synthesis and plays an important role in developing a more sustainable world. Integration of processing methods with microwave irradiation has resulted in a great reduction in the time required for many processes, while the reaction efficiencies have been increased markedly. Microwave processing produces a higher yield with a cleaner profile in comparison to other methods. The microwave processing is reported to be a better heating method than the conventional methods due to its unique thermal and non-thermal effects. This paper provides an insight into the theoretical aspects of microwave irradiation practices and highlights the importance of microwave processing. The potential of the microwave technology to accomplish superior outcomes over the conventional methods in biodiesel production is presented. A green process for biodiesel production using a non-catalytic method is still new and very costly because of the supercritical condition requirement. Hence, non-catalytic biodiesel conversion under ambient pressure using microwave technology must be developed, as the energy utilization for microwave-based biodiesel synthesis is reported to be lower and cost-effective.

Comparison of Conventional and Microwave-assisted Synthesis of Benzimidazole Derivative from Citronellal in Kaffir lime oil (Citrus hystrix DC.)

NASA Astrophysics Data System (ADS)

Warsito, W.; Noorhamdani, A. S.; Suratmo; Dwi Sapri, R.; Alkaroma, D.; Azhar, A. Z.

2018-04-01

Simple method has been used for the synthesis of benzimidazole derivative from citronellal in kaffir lime oil under microwave irradiation. These compounds were synthesized also by conventional heating for comparison. In addtion, microwave-assited synthesis was also compared between using to dichloromethane and methanol solvents with variation of reaction time for 30 to 70 minutes and 4 to 12 h for conventional heating. The 2-citronellyl benzimidazole compound synthesized were characterised by FT-IR, GC-MS, 1H and 13C NMR spectroscopy. Comparison between conventional and microwave-assisted synthesis was done by comparing between correlation of reaction time and percentage yield. The time optimum of microwave-assisted and conventional synthesis using dichloromethane solvent respectively at 60 minutes (yield 19.23%) and 8 hours (yield 11.54%). In addition, microwave-assited synthesis increasing 157.81 times compared by conventional heating. While using methanol solvent tends to increase linearly however the percentage of yield only 0.77 times of synthesis using dichloromethane solvent.

Microwave-assisted synthesis of organics and nanomaterials

EPA Science Inventory

Microwave-assisted chemistry techniques and greener reaction media are dramatically reducing chemical waste and reaction times in several organic transformations and material synthesis. This presentation summarizes author’s own experience in developing MW-assisted chemical proces...

Microwave-Assisted Rapid Access to Bio-active Heterocycles: Synthesis of 1,3,4-Oxadiazoles, 1,3,4-Thiadiazoles, 1,3-Dioxanes, Pyrazoles, Hydrazones and 3,4-Dihydropyrimidin-2(1H)-ones under Benign Conditions

EPA Science Inventory

Green chemistry is a rapidly developing new field that provides us a proactive avenue for the sustainable development of future science and technologies.1 It emphasis the use of highly efficient and environmental benign synthetic protocols to deliver bio-active heterocycles, acc...

MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES USING BIODEGRADABLE POLYMER CARBOXYMETHYL CELLULOSE

EPA Science Inventory

Microwave-assisted synthesis of noble nanostructures (Au, Pt, and Pd) using biodegradable polymer carboxymethyl cellulose (CMC) under microwave irradiation (MW) at 100 0C is reported. The reaction occurs within a few minutes, whereas at room temperature the reaction does not pro...

Microwave-assisted one-pot synthesis of water-soluble rare-earth doped fluoride luminescent nanoparticles with tunable colors

PubMed Central

Mi, Cong-Cong; Tian, Zhen-huang; Han, Bao-fu; Mao, Chuan-bin; Xu, Shu-kun

2012-01-01

Polyethyleneimine (PEI) functionalized multicolor luminescent LaF3 nanoparticles were synthesized via a novel microwave-assisted method, which can achieve fast and uniform heating under eco-friendly and energy efficient conditions. The as-prepared nanoparticles possess a pure hexagonal structure with an average size of about 12 nm. When doped with different ions (Tb3+ and Eu3+), the morphology and structure of the nanoparticles were not changed, whereas the optical properties varied with doped ions and their molar ratio, and as a result emission of four different colors (green, yellow, orange and red) were achieved by simply switching the types of doping ions (Eu3+ versus Tb3 +) and the molar ratio of the two doping ions. PMID:22879690

Microwave-Assisted Synthesis of "N"-Phenylsuccinimide

ERIC Educational Resources Information Center

Shell, Thomas A.; Shell, Jennifer R.; Poole, Kathleen A.; Guetzloff, Thomas F.

2011-01-01

A microwave-assisted synthesis of "N"-phenylsuccinimide has been developed for the second-semester organic teaching laboratory. Utilizing this procedure, "N"-phenylsuccinimide can be synthesized in moderate yields (40-60%) by heating a mixture of aniline and succinic anhydride in a domestic microwave oven for four minutes. This technique reduces…

Microwave-assisted synthesis of medicinally relevant indoles.

PubMed

Patil, S A; Patil, R; Miller, D D

2011-01-01

Indoles represent an important structural class in medicinal chemistry with broad spectrum of biological activities. The synthesis of indoles, therefore, has attracted enormous attention from synthetic chemists. Microwave methods for the preparation of indole analogs have been developed to speed up the synthesis, therefore, microwave assisted organic synthesis (MAOS) in controlled conditions is an invaluable technique for medicinal chemistry. In this review, indole forming classical reactions such as Fischer, Madelung, Bischler-Mohlau, Batcho-Leimgruber, Hemetsberger-Knittel, Graebe-Ullmann, Diels-Alder and Wittig type reactions using microwave radiation has been summarized. In addition, metal mediated cyclizations along with solid phase synthesis of indoles have been discussed. © 2011 Bentham Science Publishers Ltd.

Phase Transformation of VO2 Nanoparticles Assisted by Microwave Heating

PubMed Central

Sikong, Lek.

2014-01-01

The microwave assisted synthesis nowadays attracts a great deal of attention. Monoclinic phase VO2 (M) was prepared from NH4VO3 and H2C2O4 · 2H2O by a rapid microwave assisted technique. The synthesis parameters, microwave irradiation time, microwave power, and calcinations temperature were systematically varied and their influences on the structure and morphology were evaluated. The microwave power level has been carried out in range 180–600 W. TEM analysis demonstrated nanosized samples. The structural and morphological properties were measured using XRD, TEM, and thermal analyses. The variations of vanadium phase led to thermochromic properties. PMID:24688438

Microwave-assisted 'greener' synthesis of organics and nanomaterials

EPA Science Inventory

Microwave selective heating techniques in conjunction with greener reaction media are dramatically reducing chemical waste and reaction times in several organic transformations and material synthesis. This presentation summarizes author’s own experience in developing MW-assisted ...

Microwave-Assisted Rapid Enzymatic Synthesis of Nucleic Acids.

PubMed

Hari Das, Rakha; Ahirwar, Rajesh; Kumar, Saroj; Nahar, Pradip

2016-07-02

Herein we report microwave-induced enhancement of the reactions catalyzed by Escherichia coli DNA polymerase I and avian myeloblastosis virus-reverse transcriptase. The reactions induced by microwaves result in a highly selective synthesis of nucleic acids in 10-50 seconds. In contrast, same reactions failed to give desired reaction products when carried out in the same time periods, but without microwave irradiation. Each of the reactions was carried out for different duration of microwave exposure time to find the optimum reaction time. The products produced by the respective enzyme upon microwave irradiation of the reaction mixtures were identical to that produced by the conventional procedures. As the microwave-assisted reactions are rapid, microwave could be a useful alternative to the conventional and time consuming procedures of enzymatic synthesis of nucleic acids.

Microwave-Assisted Synthesis – Catalytic Applications in Aqueous Media

EPA Science Inventory

The development of sustainable methods directed towards the synthesis of molecules is due to the heightened awareness and recognition of alternative eco-friendly and economical protocols that have minimum impact on environment. Among others, microwave (MW)-assisted methodology ha...

"In silico" mechanistic studies as predictive tools in microwave-assisted organic synthesis.

PubMed

Rodriguez, A M; Prieto, P; de la Hoz, A; Díaz-Ortiz, A

2011-04-07

Computational calculations can be used as a predictive tool in Microwave-Assisted Organic Synthesis (MAOS). A DFT study on Intramolecular Diels-Alder reactions (IMDA) indicated that the activation energy of the reaction and the polarity of the stationary points are two fundamental parameters to determine "a priori" if a reaction can be improved by using microwave irradiation.

Sustainable synthesis of chemical entities by microwave heating with nano-catalysis in water

EPA Science Inventory

•Sustainable synthesis of chemical entities by microwave heating with nano-catalysis in water •CRADA’s with the private companies, CEM corporation and VeruTEK Technologies •Green Chemistry principles are accommodated via multi-faceted approach. Learning from nature- using na...

Microwave-assisted solid phase conversion study of Meldrum's acid to ethylenetetracarboxylic dianhydride (C 6O 6)

NASA Astrophysics Data System (ADS)

Taherpour, Avat (Arman)

2010-01-01

Utilization of microwave irradiation provides an effective method for fast synthesizing of some important compounds. Microwave-assisted solid phase is an especial class in chemical synthesis. By the use of MW-irradiation on chemicals, sometimes interesting results can be seen. The synthesis of the interesting molecule ethylenetetracarboxylic dianhydride (C 6O 6) was attempted with a few different methods. In this study, the microwave-assisted solid phase conversion of Meldrum's acid to ethylenetetracarboxylic dianhydride was reported. This conversion was characterized by FT-IR, GC/MS and NMR spectroscopy results.

Ionic liquid assisted microwave synthesis route towards color-tunable luminescence of lanthanide- doped BiPO 4

DOE PAGES

Cybinska, Joanna; Lorbeer, Chantal; Mudring, Anja -Verena

2015-07-08

Ln 3+-doped (Ln=Sm, Eu, Tb, Dy) nanoparticles of BiPO 4 with a particle size below 10 nm were synthesized in a straightforward manner from the appropriate mixture of the respective metal acetates and the task-specific ionic liquids choline or butylammonium dihydrogen-phosphate by conversion in a laboratory microwave (120 °C, 10 min). The ionic liquid acts not only as a solvent and microwave susceptor, but also as the reaction partner and nanoparticle stabilizer. The materials were thoroughly characterized not only with respect to their optical properties but also by PXRD, FT-IR, TEM techniques. Furthermore, depending on the lanthanide, the nanomaterial showsmore » intense luminescence of different colors such as: orange (Sm 3+), red (Eu 3+), green (Tb 3+) or even white (Dy 3+).« less

DEXTROSE-TEMPLATED MICROWAVE-ASSISTED COMBUSTION SYNTHESIS OF SPONGY METAL OXIDES

EPA Science Inventory

Microwave-assisted combustion synthesis of porous nanocrystalline titania and carbon coated titania is reported using dextrose as template and the product was compared with the one obtained using conventional heating furnace. Out of three compositions viz., 1:1, 1:3, and 1:5 (met...

MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES USING BIODEGRADABLE POLYMER CARBOXYMETHYL CELLULOSE

EPA Science Inventory

Microwave-assisted (MW) synthesis of noble metals such as Au, Pt and Pd is reported using biodegradable polymer carboxymethyl cellulose (CMC) at 100°C within few seconds. The possible reduction entails the coupling of polar hydroxyl units in beta-glucopyranose units with micr...

MICROWAVE-ASSISTED SHAPE-CONTROLLED BULK SYNTHESIS OF NOBLE NANOCRYSTALS AND THEIR CATALYTIC PROPERTIES

EPA Science Inventory

Bulk and shape-controlled synthesis of gold (Au) nanostructures with various shapes such as prisms, cubes and hexagons is described that occurs via microwave-assisted spontaneous reduction of noble metal salts using an aqueous solution of α-D-glucose, sucrose and maltose. The exp...

A Student-Centered First-Semester Introductory Organic Laboratory Curriculum Facilitated by Microwave-Assisted Synthesis (MAOS)

ERIC Educational Resources Information Center

Russell, Cianán B.; Mason, Jeremy D.; Bean, Theodore G.; Murphree, S. Shaun

2014-01-01

An instructional laboratory curriculum for a first-semester introductory organic chemistry course has been developed using microwave-assisted organic synthesis (MAOS). Taking advantage of short reaction times, materials were developed to facilitate collaborative experimental design, analysis, and debriefing of results during the normal laboratory…

Microwave assisted total synthesis of a benzothiophene-based new chemical entity (NCE)

EPA Science Inventory

Pharmaceutical scientists are required to generate diverse arrays of complex targets in short span of time, which can now be achieved by microwave-assisted organic synthesis. New chemical entities (NCE) can be built in a fraction of the time using this technique. However, there a...

Microwave-assisted extraction of green coffee oil and quantification of diterpenes by HPLC.

PubMed

Tsukui, A; Santos Júnior, H M; Oigman, S S; de Souza, R O M A; Bizzo, H R; Rezende, C M

2014-12-01

The microwave-assisted extraction (MAE) of 13 different green coffee beans (Coffea arabica L.) was compared to Soxhlet extraction for oil obtention. The full factorial design applied to the microwave-assisted extraction (MAE), related to time and temperature parameters, allowed to develop a powerful fast and smooth methodology (10 min at 45°C) compared to a 4h Soxhlet extraction. The quantification of cafestol and kahweol diterpenes present in the coffee oil was monitored by HPLC/UV and showed satisfactory linearity (R(2)=0.9979), precision (CV 3.7%), recovery (<93%), limit of detection (0.0130 mg/mL), and limit of quantification (0.0406 mg/mL). The space-time yield calculated on the diterpenes content for sample AT1 (Arabica green coffee) showed a six times higher value compared to the traditional Soxhlet method. Copyright © 2014 Elsevier Ltd. All rights reserved.

Green synthesis of noble nanometals (Au, Pt, Pd) using glycerol under microwave irradiation conditions

EPA Science Inventory

A newer application of glycerol in the field of nanomaterials synthesis has been developed from both the economic and environmental points of view. Glycerol can act as a reducing agent for the fabrication of noble nanometals, such as Au, Pt, and Pd, under microwave irradiation. T...

GREENER SYNTHESIS OF HETEROCYCLIC COMPOUNDS USING MICROWAVE IRRADIATION

EPA Science Inventory

An introduction of our interest in the microwave-assisted greener synthesis of a variety of heterocyclic compounds will be presented. It involves microwave (MW) exposure of neat reactants (undiluted) catalyzed by the surfaces of recyclable mineral supports, such as alumina, sili...

Microwave-assisted green synthesis of silver nanostructures.

PubMed

Nadagouda, Mallikarjuna N; Speth, Thomas F; Varma, Rajender S

2011-07-19

Over the past 25 years, microwave (MW) chemistry has moved from a laboratory curiosity to a well-established synthetic technique used in many academic and industrial laboratories around the world. Although the overwhelming number of MW-assisted applications today are still performed on a laboratory (mL) scale, we expect that this enabling technology may be used on a larger, perhaps even production, scale in conjunction with radio frequency or conventional heating. Microwave chemistry is based on two main principles, the dipolar mechanism and the electrical conductor mechanism. The dipolar mechanism occurs when, under a very high frequency electric field, a polar molecule attempts to follow the field in the same alignment. When this happens, the molecules release enough heat to drive the reaction forward. In the second mechanism, the irradiated sample is an electrical conductor and the charge carriers, ions and electrons, move through the material under the influence of the electric field and lead to polarization within the sample. These induced currents and any electrical resistance will heat the sample. This Account summarizes a microwave (MW)-assisted synthetic approach for producing silver nanostructures. MW heating has received considerable attention as a promising new method for the one-pot synthesis of metallic nanostructures in solutions. Researchers have successfully demonstrated the application of this method in the preparation of silver (Ag), gold (Au), platinum (Pt), and gold-palladium (Au-Pd) nanostructures. MW heating conditions allow not only for the preparation of spherical nanoparticles within a few minutes but also for the formation of single crystalline polygonal plates, sheets, rods, wires, tubes, and dendrites. The morphologies and sizes of the nanostructures can be controlled by changing various experimental parameters, such as the concentration of metallic salt precursors, the surfactant polymers, the chain length of the surfactant polymers, the solvents, and the operation reaction temperature. In general, nanostructures with smaller sizes, narrower size distributions, and a higher degree of crystallization have been obtained more consistently via MW heating than by heating with a conventional oil-bath. The use of microwaves to heat samples is a viable avenue for the greener synthesis of nanomaterials and provides several desirable features such as shorter reaction times, reduced energy consumption, and better product yields.

One-step microwave synthesis of photoluminescent carbon nanoparticles from sodium dextran sulfate water solution

NASA Astrophysics Data System (ADS)

Kokorina, Alina A.; Goryacheva, Irina Y.; Sapelkin, Andrei V.; Sukhorukov, Gleb B.

2018-04-01

Photoluminescent (PL) carbon nanoparticles (CNPs) have been synthesized by one-step microwave irradiation from water solution of sodium dextran sulfate (DSS) as the sole carbon source. Microwave (MW) method is very simple and cheap and it provides fast synthesis of CNPs. We have varied synthesis time for obtaining high luminescent CNPs. The synthesized CNPs exhibit excitation-dependent photoluminescent. Final CNPs water solution has a blue- green luminescence. CNPs have low cytotoxicity, good photostability and can be potentially suitable candidates for bioimaging, analysis or analytical tests.

CATALYST-FREE REACTIONS UNDER SOLVENT-FEE CONDITIONS: MICROWAVE-ASSISTED SYNTHESIS OF HETEROCYCLIC HYDRAZONES BELOW THE MELTING POINT OF NEAT REACTANTS: JOURNAL ARTICLE

EPA Science Inventory

NRMRL-CIN-1437 Jeselnik, M., Varma*, R.S., Polanc, S., and Kocevar, M. Catalyst-free Reactions under Solvent-fee Conditions: Microwave-assisted Synthesis of Heterocyclic Hydrazones below the Melting Point of Neat Reactants. Published in: Chemical Communications 18:1716-1717 (200...

Green and microwave synthesis of SrAl2O4 nanoparticles by application of pomegranate juice: study and characterization

NASA Astrophysics Data System (ADS)

Riahi-Madvaar, Ramin; Taher, Mohammad Ali; Fazelirad, Hamid

2017-11-01

In the present paper, a green method was applied for the synthesis of SrAl2O4 nanostructures with the aid of microwave irradiation and pomegranate juice. SrAl2O4 nanocrystals were obtained when the raw materials were irradiated with 720-900 W for 6-10 min and then calcinated at 550 °C for 5 h. Using pomegranate juice as a dispersion and stabilizing agent, SrAl2O4 nanoparticles have been made with better properties in view of morphology and particle size. Also, the effect of some parameters affecting synthesis process such as microwave power and reaction time on the morphology and particle size of product was studied and optimized. X-ray diffraction and field emission-scanning electron microscopy were used to study and characterize the manufactured SrAl2O4 nanoparticles.

MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES

EPA Science Inventory

Microwave-assisted (MW) spontaneous reduction of noble metal salts, silver (Ag), gold (Au), platinum (Pt) and palladium (Pd) is reported using sugar solutions such as -D glucose, sucrose and maltose, etc. to generate nanomaterials. These MW-assisted reactions, conducted in aqueo...

Microwave-Assisted Synthesis of a MK2 Inhibitor by Suzuki-Miyaura Coupling for Study in Werner Syndrome Cells.

PubMed

Bagley, Mark C; Baashen, Mohammed; Chuckowree, Irina; Dwyer, Jessica E; Kipling, David; Davis, Terence

2015-06-03

Microwave-assisted Suzuki-Miyaura cross-coupling reactions have been employed towards the synthesis of three different MAPKAPK2 (MK2) inhibitors to study accelerated aging in Werner syndrome (WS) cells, including the cross-coupling of a 2-chloroquinoline with a 3-pyridinylboronic acid, the coupling of an aryl bromide with an indolylboronic acid and the reaction of a 3-amino-4-bromopyrazole with 4-carbamoylphenylboronic acid. In all of these processes, the Suzuki-Miyaura reaction was fast and relatively efficient using a palladium catalyst under microwave irradiation. The process was incorporated into a rapid 3-step microwave-assisted method for the synthesis of a MK2 inhibitor involving 3-aminopyrazole formation, pyrazole C-4 bromination using N-bromosuccinimide (NBS), and Suzuki-Miyaura cross-coupling of the pyrazolyl bromide with 4-carbamoylphenylboronic acid to give the target 4-arylpyrazole in 35% overall yield, suitable for study in WS cells.

Eco-friendly and green synthesis of BiVO4 nanoparticle using microwave irradiation as photocatalayst for the degradation of Alizarin Red S

NASA Astrophysics Data System (ADS)

Abraham, S. Daniel; David, S. Theodore; Bennie, R. Biju; Joel, C.; Kumar, D. Sanjay

2016-06-01

Bismuth vanadate (BiVO4) nanocrystals have been successfully synthesised using microwave-assisted combustion synthesis (MCS), and characterised using Fourier transform infrared (FT-IR) and Raman spectra, surface area analysis (BET), X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy Dispersive X-ray analysis (EDX), diffused reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The XRD results confirmed the formation of monoclinic bismuth vanadate. The formations of BiO & VO43-vibrations were ascertained from FT-IR data. The morphology of hallow internal structural micro entities were confirmed by SEM. The optical properties were determined by DRS and PL spectra. Hence, the influence of the preparation methods on the structure, morphology and optical activities of bismuth vanadate was investigated systematically. Photocatalytic degradation (PCD) of Alizarin Red S (ARS), an effective disrupting chemical in aqueous medium was investigated using BiVO4 nanoparticles. The kinetics of PCD was found to follow pseudo first-order.

Microwave-assisted one-pot synthesis of new phenanthrene fused-tetrahydrodibenzo-acridinones as potential cytotoxic and apoptosis inducing agents.

PubMed

Kumar, Niggula Praveen; Sharma, Pankaj; Reddy, T Srinivasa; Shankaraiah, Nagula; Bhargava, Suresh K; Kamal, Ahmed

2018-05-10

An expeditious microwave-assisted one-pot synthesis of new cytotoxic phenanthrene fused-tetrahydrodibenzo-acridinones has been successfully accomplished. This protocol offers wide substrate scope, catalyst-free synthesis, atom-economy, simple recrystallization, high yields, and ethanol was used as green solvent. These new compounds were tested for their in vitro cytotoxicity against cervical (HeLa), prostate (PC-3), fibrosarcoma (HT-1080), ovarian (SKOV-3) cancer cells, and were safer to normal (Hek-293T) kidney cell line. All the compounds have displayed significant cytotoxicity profile, among them 8m being the most potent compound with an IC 50 0.24 ± 0.05 μM against SKOV-3 ovarian cancer cells. Flow cytometry analysis revealed that cells were blocked at the G2/M phase of the cell cycle. The effect of 8m on F-actin polymerisation was also studied. Hoechst staining clearly showed the decreased number of viable cells and indicated apoptosis progression. Compound 8m caused the collapse of mitochondrial membrane potential as observed via JC-1 staining and also enhanced the generation of reactive oxygen species. The increase of caspase-3 activation by 3.7 folds supported the strong apoptosis induction. In addition, an in vitro 3D-spheroid progression assay was performed with 8m that significantly suppressed the tumor cells. Copyright © 2018 Elsevier Masson SAS. All rights reserved.

A Microwave-Assisted Reduction of Cyclohexanone Using Solid-State-Supported Sodium Borohydride

ERIC Educational Resources Information Center

White, Lori L.; Kittredge, Kevin W.

2005-01-01

The reduction of carbonyl groups by sodium borohydride though is a well-known reaction in most organic lab texts, a difficulty for an instructor adopting this reaction in a student lab is that it is too long. Using a microwave assisted organic synthesis solves this difficulty and one such reaction, which is the microwave-assisted reduction of…

Microwave-assisted synthesis of highly fluorescent nanoparticles of a melamine-based porous covalent organic framework for trace-level detection of nitroaromatic explosives.

PubMed

Zhang, Wang; Qiu, Ling-Guang; Yuan, Yu-Peng; Xie, An-Jian; Shen, Yu-Hua; Zhu, Jun-Fa

2012-06-30

Covalent organic frameworks (COFs) are a new generation of porous materials constructed from light elements linked by strong covalent bonds. Herein we present rapid preparation of highly fluorescent nanoparticles of a new type of COF, i.e. melamine-based porous polymeric network SNW-1, by a microwave-assisted synthesis route. Although the synthesis of SNW-1 has to be carried out at 180°C for 3d under conventional reflux conditions, SNW-1 nanoparticles could be obtained in 6h by using such a microwave-assisted method. The results obtained have clearly demonstrated that microwave-assisted synthesis is a simple yet highly efficient approach to nanoscale COFs or other porous polymeric materials. Remarkably, the as-synthesized SNW-1 nanoparticles exhibit extremely high sensitivity and selectivity, as well as fast response to nitroaromatic explosives such as 2,4,6-trinitrotoluene (TNT), 2,4,6-trinitrophenylmethylnitramine (Tetryl) and picric acid (PA) without interference by common organic solvents, which is due to the nanoscaled size and unique hierarchical porosity of such fluorescence-based sensing material. Copyright © 2012 Elsevier B.V. All rights reserved.

Microwave-Mediated Synthesis of Lophine: Developing a Mechanism to Explain a Product

ERIC Educational Resources Information Center

Crouch, R. David; Howard, Jessica L.; Zile, Jennifer L.; Barker, Kathryn H.

2006-01-01

The microwave-mediated preparation of lophine (2,4,5-triphenylimidazole) is described. This experiment allows for an introduction to the emerging technology of microwave-assisted organic synthesis while providing an opportunity for students to employ the principles of carbonyl chemistry in devising a mechanism to explain the formation of the…

Organo- and nano-catalyst in greener reaction medium: Microwave-assisted expedient synthesis of fine chemicals

EPA Science Inventory

The use of emerging microwave (MW) -assisted chemistry techniques is dramatically reducing chemical waste and reaction times in several organic syntheses and chemical transformations. A brief account of our experiences in developing MW-assisted organic transformations, which invo...

One-pot green synthesis of carbon quantum dot for biological application

NASA Astrophysics Data System (ADS)

Asghar, Khushnuma; Qasim, Mohd; Das, D.

2017-05-01

A one-pot microwave assisted method for synthesizing carbon quantum dots (CQDs) from honey is presented in this paper. The structural, morphological and optical properties of synthesized CQDs were characterized by XRD, TEM, UV-Vis spectrophotometer, and Raman techniques. The average particle size of CQDs is found to be 2 to 7 nm. The main advantage of this work is the use of inexpensive, less toxic and environmental friendly precursors and synthesis procedure for CQDs. In addition to this, the particle size of prepared CQDs was found to be ultrafine with narrow size distribution. The as-prepared CQDs, with smaller particle size, good stability, good optical properties, water dispersibility and low toxicity, show promising potential for applications in biomedical field.

Green Microwave-Assisted Combustion Synthesis of Zinc Oxide Nanoparticles with Citrullus colocynthis (L.) Schrad: Characterization and Biomedical Applications.

PubMed

Azizi, Susan; Mohamad, Rosfarizan; Mahdavi Shahri, Mahnaz

2017-02-16

In this paper, a green microwave-assisted combustion approach to synthesize ZnO-NPs using zinc nitrate and Citrullus colocynthis (L.) Schrad (fruit, seed and pulp) extracts as bio-fuels is reported. The structure, optical, and colloidal properties of the synthesized ZnO-NP samples were studied. Results illustrate that the morphology and particle size of the ZnO samples are different and depend on the bio-fuel. The XRD results revealed that hexagonal wurtzite ZnO-NPs with mean particle size of 27-85 nm were produced by different bio-fuels. The optical band gap was increased from 3.25 to 3.40 eV with the decreasing of particle size. FTIR results showed some differences in the surface structures of the as-synthesized ZnO-NP samples. This led to differences in the zeta potential, hydrodynamic size, and more significantly, antioxidant activity through scavenging of 1, 1-Diphenyl-2-picrylhydrazyl (DPPH) free radicals. In in vitro cytotoxicity studies on 3T3 cells, a dose dependent toxicity with non-toxic effect of concentration below 0.26 mg/mL was shown for ZnO-NP samples. Furthermore, the as-synthesized ZnO-NPs inhibited the growth of medically significant pathogenic gram-positive ( Bacillus subtilis and Methicillin-resistant Staphylococcus aurous ) and gram-negative ( Peseudomonas aeruginosa and Escherichia coli ) bacteria. This study provides a simple, green and efficient approach to produce ZnO nanoparticles for various applications.

Determining the microwave coupling and operational efficiencies of a microwave plasma assisted chemical vapor deposition reactor under high pressure diamond synthesis operating conditions

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

Nad, Shreya; Department of Physics and Astronomy, Michigan State University, East Lansing, Michigan 48824; Gu, Yajun

2015-07-15

The microwave coupling efficiency of the 2.45 GHz, microwave plasma assisted diamond synthesis process is investigated by experimentally measuring the performance of a specific single mode excited, internally tuned microwave plasma reactor. Plasma reactor coupling efficiencies (η) > 90% are achieved over the entire 100–260 Torr pressure range and 1.5–2.4 kW input power diamond synthesis regime. When operating at a specific experimental operating condition, small additional internal tuning adjustments can be made to achieve η > 98%. When the plasma reactor has low empty cavity losses, i.e., the empty cavity quality factor is >1500, then overall microwave discharge coupling efficienciesmore » (η{sub coup}) of >94% can be achieved. A large, safe, and efficient experimental operating regime is identified. Both substrate hot spots and the formation of microwave plasmoids are eliminated when operating within this regime. This investigation suggests that both the reactor design and the reactor process operation must be considered when attempting to lower diamond synthesis electrical energy costs while still enabling a very versatile and flexible operation performance.« less

Physicochemical characterization of microwave assisted synthesis of silver nanoparticles using Aloe Vera (Aloe barbadensis)

NASA Astrophysics Data System (ADS)

Kuponiyi, Abiola John

Biosynthesis of silver nanoparticles (AgNP) using different biological extracts is gaining recognition for its numerous applications in different disciplines. Although different approaches (physical and chemical) have been used for the synthesis of AgNP, the green chemistry method is most preferable because of its high efficacy, cost effectiveness, and environmental benignity. Aloe Vera (AV) contains chemical compounds (anthraquinones) that are known to possess antibacterial, antivirus and anticancer properties and the extract is a good chemical reduction agent for AgNP. Hence, it was hypothesized that a microwave assisted synthesis will produce highly concentrated, homogeneous, stable and biologically active AgNP. Thus, the main objective of the study was to evaluate the effect of microwave assisted synthesis of AgNP, the effect of pulse laser treatment on size reduction of a microwave synthesized AgNP, and the physicochemical characterization of AgNP synthesized with Aloe Vera water and ethanol extract. The experiment was conducted in two phases. Phase 1 was first conducted to optimize the experimental variables, thus establishing the optimum variables to apply in the second phase. The experiment in Phase 1 was conducted using three-factor factorial experimental design comprised of the following factors: 1) Extraction Solvent, 2) Heating Methods, 3) pH; and their corresponding levels were water and ethanol, conventional and microwave, pH (7, 8, 10 and 12), respectively. All synthesis was conducted at constant temperature of 80°C. Phase II experimental treatments were Laser ablation (0, 5, and 10 min) and Storage time (Week 1, 2 & 3). The Phase I of the results showed that increased AgNP concentrations were significantly (p < 0.05) influenced by synthesis time, hence, (15 min) gave the highest concentration. The solvent type, heating methods and pH had a significant effect (p < 0.05) on the concentration AgNP. Hence, ethanol extract (99.2 ppm), microwave method (77 ppm), and pH 10 (125 ppm) are variables that exhibited the maximum contribution to the formation of AgNP. The phase II ANOVA results indicated that laser treatment has a significant effect (p < 0.01) on the concentration of AgNP during synthesis. The intensity of the absorption peak significantly (p < 0.01) increases with laser exposure time. While 214 ppm was observed at laser exposures time 0 min, 224 and 229 ppm at 5 and 10 min and at the following rates of formation 0.384, 0.408 and 0.4288 min -1 respectively. Particle sizes (hydrodynamic diameter) were approximately 37.84 nm with no laser treatment in contrast (p < 0.01) with laser treated samples at 5 and 10 min at week 1 were 10.1 and 8.72 nm, respectively. However, storability up to the maximum storage period of six weeks of the AgNP solutions does not significantly (p > 0.05) impact the particle size distribution. Hence, the Zeta potential of the particles has values typically ranging between +100 mV to -100 mV, hence indicative of colloidal stability matrix. Furthermore, the Polydispersity indexes of Week 1, 2, & 3 treatments were 0.312, 0.591 and 0.768 respectfully, indicating that the control is monodispersed while treatments week 2 & 3 indicating the laser ablation effect in further reduction of sizes to a different level of aggregation. Microwave synthesis showed significantly (p < 0.05) higher concentration of biological compounds such as aliphatic amines, alkenes (=C-H), alkanes (C-H), alcohol (O-H) and unsaturated esters(C-O).

Sustainable Synthesis of Nanomaterials Using Microwave irradiation

EPA Science Inventory

The presentation summarizes our recent activity in MW-assisted synthesis of nanomaterials under benign conditions. Shape-controlled aqueous synthesis of noble nanostructures via MW-assisted spontaneous reduction of noble metal salts using -D-glucose, sucrose, and maltose will be...

Microwave-Assisted Organic Synthesis in the Organic Teaching Lab: A Simple, Greener Wittig Reaction

ERIC Educational Resources Information Center

Martin, Eric; Kellen-Yuen, Cynthia

2007-01-01

A greener, microwave-assisted Wittig reaction has been developed for the second-semester organic teaching laboratory. Utilizing this microwave technique, a variety of styrene derivatives have been successfully synthesized from aromatic aldehydes in good yields (41-68%). The reaction not only occurs under neat reaction conditions, but also employs…

TiO{sub 2} synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

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

Moura, K.F.; Maul, J.; Albuquerque, A.R.

2014-02-15

In this study, a microwave assisted solvothermal method was used to synthesize TiO{sub 2} with anatase structure. The synthesis was done using Ti (IV) isopropoxide and ethanol without templates or alkalinizing agents. Changes in structural features were observed with increasing time of synthesis and evaluated using periodic quantum chemical calculations. The anatase phase was obtained after only 1 min of reaction besides a small amount of brookite phase. Experimental Raman spectra are in accordance with the theoretical one. Micrometric spheres constituted by nanometric particles were obtained for synthesis from 1 to 30 min, while spheres and sticks were observed aftermore » 60 min. - Graphical abstract: FE-SEM images of anatase obtained with different periods of synthesis associated with the order–disorder degree. Display Omitted - Highlights: • Anatase microspheres were obtained by the microwave assisted hydrothermal method. • Only ethanol and titanium isopropoxide were used as precursors during the synthesis. • Raman spectra and XRD patterns were compared with quantum chemical calculations. • Time of synthesis increased the short-range disorder in one direction and decreased in another.« less

Portable microwave assisted extraction: An original concept for green analytical chemistry.

PubMed

Perino, Sandrine; Petitcolas, Emmanuel; de la Guardia, Miguel; Chemat, Farid

2013-11-08

This paper describes a portable microwave assisted extraction apparatus (PMAE) for extraction of bioactive compounds especially essential oils and aromas directly in a crop or in a forest. The developed procedure, based on the concept of green analytical chemistry, is appropriate to obtain direct in-field information about the level of essential oils in natural samples and to illustrate green chemical lesson and research. The efficiency of this experiment was validated for the extraction of essential oil of rosemary directly in a crop and allows obtaining a quantitative information on the content of essential oil, which was similar to that obtained by conventional methods in the laboratory. Copyright © 2013 Elsevier B.V. All rights reserved.

Microwave-Assisted Synthesis of a MK2 Inhibitor by Suzuki-Miyaura Coupling for Study in Werner Syndrome Cells

PubMed Central

Bagley, Mark C.; Baashen, Mohammed; Chuckowree, Irina; Dwyer, Jessica E.; Kipling, David; Davis, Terence

2015-01-01

Microwave-assisted Suzuki-Miyaura cross-coupling reactions have been employed towards the synthesis of three different MAPKAPK2 (MK2) inhibitors to study accelerated aging in Werner syndrome (WS) cells, including the cross-coupling of a 2-chloroquinoline with a 3-pyridinylboronic acid, the coupling of an aryl bromide with an indolylboronic acid and the reaction of a 3-amino-4-bromopyrazole with 4-carbamoylphenylboronic acid. In all of these processes, the Suzuki-Miyaura reaction was fast and relatively efficient using a palladium catalyst under microwave irradiation. The process was incorporated into a rapid 3-step microwave-assisted method for the synthesis of a MK2 inhibitor involving 3-aminopyrazole formation, pyrazole C-4 bromination using N-bromosuccinimide (NBS), and Suzuki-Miyaura cross-coupling of the pyrazolyl bromide with 4-carbamoylphenylboronic acid to give the target 4-arylpyrazole in 35% overall yield, suitable for study in WS cells. PMID:26046488

Microwave-assisted solid-phase synthesis of highly fluorescent carbon nanoparticles and its application in intracellular pH sensing.

PubMed

Yang, Shenghong; Chen, Xiao; Liu, Shuqin; Wang, Fuxin; Ouyang, Gangfeng

2018-08-15

Fluorescent carbon nanoparticles (FCNPs) have been deeply researched and widely applied in recent years due to their good optics performance, chemical stability and biocompatibility. Herein, a green and rapid microwave-assisted solid-phase synthesis (solvent-free) approach was proposed for the fabrication of highly FCNPs in a very short period of time, 4 min. The as-prepared FCNPs can emit a blue emission with quantum yield of up to 63.2% in water solution and show yellow fluorescence in the solid state. The FCNPs also exhibit special solvent effect that the fluorescence emission can be adjusted by controlling the solvent ratio of ethanol and water. Most importantly, the FCNPs possess a narrow-range pH response. The probe responds linearly and rapidly to minor pH fluctuations within the range of 3.47-5.10 and the correlation coefficient is above 0.99. The proposed FCNPs also exhibit high photostability and reusability. As expected, the cell imaging and intracellular pH monitoring was achieved successfully in living SMMC 7721 hepatoma cells by this probe. The FCNPs is promising as a convenient and general fluorescent pH sensor for bioimaging applications. Copyright © 2018. Published by Elsevier B.V.

Microwave-Assisted Eco-Friendly Synthesis of Organics and Nanomaterials

EPA Science Inventory

This presentation summarizes our recent activity in MW-assisted synthesis, which involves benign alternatives, such as the use of supported reagents, and greener reaction medium in aqueous or solvent-free conditions.1 The greener synthesis of heterocyclic compounds, coupling reac...

Green synthesis of Copper nanoparticle using ionic liquid-based extraction from Polygonum minus and their applications.

PubMed

Ullah, Habib; Wilfred, Cecilia Devi; Shaharun, Maizatul Shima

2018-06-06

The present work reports the extraction of phenolic compounds from Polygonum minus using ionic liquid as extracting solvent. In this work, 1-Butyl-3-methylimidazolium hydrogen sulfate [BMIM][HSO 4 ] was used for the extraction of bioactive compounds. Accordingly, ionic liquids based microwave-assisted extraction treatment for separating of bioactive compounds from polygonum minus was first performed in the present study. The results obtained in this work have high extraction yield in comparison with conventional solvent. UV/Vis results showed that microwave synthesis was fast, well dispersed and nanosized copper nanoparticle (CuNPs) in comparison with conventional synthesis. CuNPs was characterized by X-Rays diffractometer (XRD), Fourier transform infrared (FTIR), dynamic light scattering (DLS), field emission scanning electron microscopy combined with energy dispersive x-rays (FESEM-EDX), and thermogravimetric analysis (TGA). All the instrumental analyses confirmed the particles were nanosized. Furthermore, the antibacterial activity of as-synthesized CuNPs showed effective inhibitory zone against three different bacteria. The photocatalytic degradation of copper nanoparticles was studied using methylene blue (MB) and methyl orange (MO) dyes under UV light and degraded 99.9% within short time 8 and 7 minutes.

Ultrafast synthesis and characterization of carbonated hydroxyapatite nanopowders via sonochemistry-assisted microwave process.

PubMed

Zou, Zhaoyong; Lin, Kaili; Chen, Lei; Chang, Jiang

2012-11-01

Herein, carbonated hydroxyapatite (CHAp) nanopowders were synthesized via sonochemistry-assisted microwave process. The influences of microwave and ultrasonic irradiation on the crystallinity, morphology, yield, Ca/P molar ratio, specific surface area and dispersibility were investigated and compared with the conventional precipitation method. The results showed that sonochemistry-assisted microwave process significantly increased the synthetic efficiency. The well-crystallized nanopowders could be obtained at high yield of 98.8% in ultra-short-period of 5min. In addition, the crystallization process was promoted with the increase of ultrasonic and microwave power and the reaction time during the sonochemistry-assisted microwave process. The sonochemistry assistance also remarkably increased the specific surface area and dispersibility of the as-obtained products. These results suggest that the sonochemistry-assisted microwave process is an effective approach to synthesize CHAp with high efficiency. Copyright © 2012 Elsevier B.V. All rights reserved.

Accessing Stereochemically Rich Sultams via Microwave-Assisted, Continuous Flow Organic Synthesis (MACOS) Scale-out

PubMed Central

Organ, Michael G.; Hanson, Paul R.; Rolfe, Alan; Samarakoon, Thiwanka B.; Ullah, Farman

2011-01-01

The generation of stereochemically-rich benzothiaoxazepine-1,1′-dioxides for enrichment of high-throughput screening collections is reported. Utilizing a microwave-assisted, continuous flow organic synthesis platform (MACOS), scale-out of core benzothiaoxazepine-1,1′-dioxide scaffolds has been achieved on multi-gram scale using an epoxide opening/SNAr cyclization protocol. Diversification of these sultam scaffolds was attained via a microwave-assisted intermolecular SNAr reaction with a variety of amines. Overall, a facile, 2-step protocol generated a collection of benzothiaoxazepine-1,1′-dioxides possessing stereochemical complexity in rapid fashion, where all 8 stereoisomers were accessed from commercially available starting materials. PMID:22116791

Microwave-assisted transformations and synthesis of polymer nanocomposites and nanomaterials

EPA Science Inventory

The use of emerging MW-assisted chemistry techniques in conjunction with greener reaction media is dramatically reducing chemical waste and reaction times in several organic transformations and material synthesis. This account summarizes our own experience in developing MW-assist...

Access to small size distributions of nanoparticles by microwave-assisted synthesis. Formation of Ag nanoparticles in aqueous carboxymethylcellulose solutions in batch and continuous-flow reactors

NASA Astrophysics Data System (ADS)

Horikoshi, Satoshi; Abe, Hideki; Torigoe, Kanjiro; Abe, Masahiko; Serpone, Nick

2010-08-01

This article examines the effect(s) of the 2.45-GHz microwave (MW) radiation in the synthesis of silver nanoparticles in aqueous media by reduction of the diaminesilver(i) complex, [Ag(NH3)2]+, with carboxymethylcellulose (CMC) in both batch-type and continuous-flow reactor systems with a particular emphasis on the characteristics of the microwaves in this process and the size distributions. This microwave thermally-assisted synthesis is compared to a conventional heating (CH) method, both requiring a reaction temperature of 100 °C to produce the nanoparticles, in both cases leading to the formation of silver colloids with different size distributions. Reduction of the diaminesilver(i) precursor complex, [Ag(NH3)2]+, by CMC depended on the solution temperature. Cooling the reactor during the heating process driven with 390-Watt microwaves (MW-390W/Cool protocol) yielded silver nanoparticles with sizes spanning the range 1-2 nm. By contrast, the size distribution of Ag nanoparticles with 170-Watt microwaves (no cooling; MW-170W protocol) was in the range 1.4-3.6 nm (average size ~3 nm). The overall results suggest the potential for a scale-up process in the microwave-assisted synthesis of nanoparticles. Based on the present data, a flow-through microwave reactor system is herein proposed for the continuous production of silver nanoparticles. The novel flow reactor system (flow rate, 600 mL min-1) coupled to 1200-Watt microwave radiation generated silver nanoparticles with a size distribution 0.7-2.8 nm (average size ca. 1.5 nm).

Microwave-Assisted Synthesis of Mesoporous Nano-Hydroxyapatite Using Surfactant Templates

EPA Science Inventory

Mesoporous nano-hydroxyapatite (n-HAP) was expeditiously synthesized using the pseudo sol-gel microwave-assisted protocol (30 min) in the presence of two novel templates, namely sodium lauryl ether sulfate (SLES) and linear alkylbenzenesulfonate (LABS). The cooperative self-assem...

Glutathione promoted expeditious green synthesis of silver nanoparticles in water using microwaves

EPA Science Inventory

Silver nanoparticles with size range 5-10 nm has been synthesized under microwave irradiation conditions using gluathione, an absolutely benign antioxidant that serves as the reducing as well as capping agent in aqueous medium. This rapid protocol yields the nanoparticles within ...

Microwave assisted tandem reactions for the synthesis of 2-hydrazolyl-4-thiazolidinones

PubMed Central

Saiz, Cecilia; Pizzo, Chiara; Manta, Eduardo; Wipf, Peter; Mahler, S. Graciela

2009-01-01

A tandem method for the synthesis of 2-hydrazolyl-4-thiazolidinones (5) from commercially available materials in a 3 component reaction has been developed. The reaction connects aldehydes, thiosemicarbazides and maleic anhydride, effectively assisted by microwave irradiation. The synthesis of a new type of compound, 2-hydrazolyl-5,5-diphenyl-4-thiazolidinone (7), obtained by treatment of thiosemicarbazone with benzil in basic media is also reported. HOMO/LUMO energies, orbital coefficients and charge distribution were used to explain the proposed reaction mechanism. PMID:19756224

Comparative efficacy of microwave, visible light and ultrasound irradiation for green synthesis of dihydropyrimidinones in fruit juice medium

NASA Astrophysics Data System (ADS)

Pramanik, Tanay; Padan, Simarjit Kaur; Gupta, Richa; Bedi, Pooja; Singh, Gurinderpal

2017-07-01

Dihydropyrimidinones (DHPM) were synthesized via multi component condensation reaction employing urea, ethyl acetoacetate and aromatic aldehydes as reactants. Apple, pomegranate, grape juice were used individually as biodegradable, eco friendly, and green reaction medium whereas microwave, visible light and ultrasound irradiation were applied individually as green source of energy for carrying out the aforesaid reactions. It was observed that the reactions under microwave irradiation were taking minimum time to go for completion whereas the reactions under ultrasound and visible light irradiation were taking approximately same time duration to form products. This is the first of its kind study where the three different reaction methodologies based on three different sources of green energies were compared with each other for their effectiveness and efficiency towards multi component condensation reactions.

Silicon carbide passive heating elements in microwave-assisted organic synthesis.

PubMed

Kremsner, Jennifer M; Kappe, C Oliver

2006-06-09

Microwave-assisted organic synthesis in nonpolar solvents is investigated utilizing cylinders of sintered silicon carbide (SiC)--a chemically inert and strongly microwave absorbing material--as passive heating elements (PHEs). These heating inserts absorb microwave energy and subsequently transfer the generated thermal energy via conduction phenomena to the reaction mixture. The use of passive heating elements allows otherwise microwave transparent or poorly absorbing solvents such as hexane, carbon tetrachloride, tetrahydrofuran, dioxane, or toluene to be effectively heated to temperatures far above their boiling points (200-250 degrees C) under sealed vessel microwave conditions. This opens up the possibility to perform microwave synthesis in unpolar solvent environments as demonstrated successfully for several organic transformations, such as Claisen rearrangements, Diels-Alder reactions, Michael additions, N-alkylations, and Dimroth rearrangements. This noninvasive technique is a particularly valuable tool in cases where other options to increase the microwave absorbance of the reaction medium, such as the addition of ionic liquids as heating aids, are not feasible due to an incompatibility of the ionic liquid with a particular substrate. The SiC heating elements are thermally and chemically resistant to 1500 degrees C and compatible with any solvent or reagent.

REVISITING NUCLEOPHILIC SUBSTITUTION REACTIONS: MICROWAVE-ASSISTED SYNTHESIS OF AZIDES, THIOCYANATES AND SULFONES IN AQUEOUS MEDIUM

EPA Science Inventory

A practical, rapid and efficient microwave (MW) promoted synthesis of various azides, thiocyanates and sulfones, is described in aqueous medium. This general and expeditious MW-enhanced nucleophilic substitution approach uses easily accessible starting materials such as halides o...

Microwave-Assisted Chemistry: A Rapid and Sustainable Route to Synthesis of Organics and Nanomaterials

EPA Science Inventory

The use of emerging MW-assisted chemistry techniques in conjunction with benign reaction media is dramatically reducing chemical waste and reaction times in several organic syntheses and chemical transformations. This review summarizes recent developments in MW-assisted synthesis...

Purchase of Microwave Reactors for Implementation of Small-scale Microwave-accelerated Organic Chemistry Laboratory Program in Undergraduate Curriculum and Synthetic Chemistry Research at HU

DTIC Science & Technology

2015-05-16

synthesis of iron magnetic nanoparticles is being investigated (Appendix A; Scheme IV). In the first step, precursor iron(III) chloride nanoparticles...and other methods. Currently, we are developing a two-step scheme for the synthesis of esters that will require distillation and/or column...recognize the link between them. We are developing for the above purpose, the microwave-assisted, two-step synthesis of high boiling point esters. The

Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

PubMed

Ieronymaki, Matthaia; Androutsou, Maria Eleni; Pantelia, Anna; Friligou, Irene; Crisp, Molly; High, Kirsty; Penkman, Kirsty; Gatos, Dimitrios; Tselios, Theodore

2015-09-01

A fast and efficient microwave (MW)-assisted solid-phase peptide synthesis protocol using the 2-chlorotrityl chloride resin and the Fmoc/tBu methodology, has been developed. The established protocol combines the advantages of MW irradiation and the acid labile 2-chlorotrityl chloride resin. The effect of temperature during the MW irradiation, the degree of resin substitution during the coupling of the first amino acids and the rate of racemization for each amino acid were evaluated. The suggested solid phase methodology is applicable for orthogonal peptide synthesis and for the synthesis of cyclic peptides. © 2015 Wiley Periodicals, Inc.

Microwave assisted synthesis of luminescent carbonaceous nanoparticles from silk fibroin for bioimaging.

PubMed

Gao, Hongzhi; Teng, Choon Peng; Huang, Donghong; Xu, Wanqing; Zheng, Chaohui; Chen, Yisong; Liu, Minghuan; Yang, Da-Peng; Lin, Ming; Li, Zibiao; Ye, Enyi

2017-11-01

Bombyx mori silk as a natural protein based biopolymer with high nitrogen content, is abundant and sustainable because of its mass product all over the world per year. In this study, we developed a facile and fast microwave-assisted synthesis of luminescent carbonaceous nanoparticles using Bombyx mori silk fibroin and silk solution as the precursors. As a result, the obtained carbonaceous nanoparticles exhibit a photoluminescence quantum yield of ~20%, high stability, low cytotoxicity, high biocompatibility. Most importantly, we successfully demonstrated bioimaging using these luminescent carbonaceous nanoparticles with excitation dependent luminescence. In addition, the microwave-assisted hydrothermal method can be extended to convert other biomass into functional nanomaterials. Copyright © 2017 Elsevier B.V. All rights reserved.

REVISITING CLASSICAL NUCLEOPHILIC SUBSTITUTIONS IN AQUEOUS MEDIUM: MICROWAVE-ASSISTED SYNTHESIS OF ALKYL AZIDES

EPA Science Inventory

An efficient and clean synthesis of alkyl azides using microwave (MW) radiation is described in aqueous medium by reacting alkyl halides or tosylates with alkali azides. This general and expeditious MW-enhanced approach to nucleophilic substitution reactions is applicable to the ...

Microwave-Assisted Selective Hydrogenation of Furfural to Furfuryl Alcohol Employing a Green and Noble Metal-Free Copper Catalyst.

PubMed

Romano, Pedro N; de Almeida, João M A R; Carvalho, Yuri; Priecel, Peter; Falabella Sousa-Aguiar, Eduardo; Lopez-Sanchez, Jose A

2016-12-20

Green, inexpensive, and robust copper-based heterogeneous catalysts achieve 100 % conversion and 99 % selectivity in the conversion of furfural to furfuryl alcohol when using cyclopentyl-methyl ether as green solvent and microwave reactors at low H 2 pressures and mild temperatures. The utilization of pressurized microwave reactors produces a 3-4 fold increase in conversion and an unexpected enhancement in selectivity as compared to the reaction carried out at the same conditions using conventional autoclave reactors. The enhancement in catalytic rate produced by microwave irradiation is temperature dependent. This work highlights that using microwave irradiation in the catalytic hydrogenation of biomass-derived compounds is a very strong tool for biomass upgrade that offers immense potential in a large number of transformations where it could be a determining factor for commercial exploitation. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microwave-assisted synthesis of cyclodextrin polyurethanes

USDA-ARS?s Scientific Manuscript database

Cyclodextrin (CD) has often been incorporated into polyurethanes in order to facilitate its use in encapsulation or removal of organic species for various applications. In this work a microwave-assisted method has been developed to produce polyurethanes consisting of alpha-, ß-, and gamma-CD and thr...

Parallel and automated library synthesis of 2-long alkyl chain benzoazoles and azole[4,5-b]pyridines under microwave irradiation.

PubMed

Martínez-Palou, Rafael; Zepeda, L Gerardo; Höpfl, Herbert; Montoya, Ascensión; Guzmán-Lucero, Diego J; Guzmán, Javier

2005-01-01

A versatile route to 40-membered library of 2-long alkyl chain substituted benzoazoles (1 and 2) and azole[4,5-b]pyridines (3 and 4) via microwave-assisted combinatorial synthesis was developed. The reactions were carried out in both monomode and multimode microwave oven. With the latter, all reactions were performed in high-throughput experimental settings consisting of an 8 x 5 combinatorial library designed to synthesize 40 compounds. Each step, from the addition of reagents to the recovery of final products, was automated. The microwave-assisted N-long chain alkylation reactions of 2-alkyl-1H-benzimidazole (1) and 2-alkyl-1H-benzimidazole[4,5-b] pyridines (3) were also studied.

Microwave-Assisted Hydantoins Synthesis on Solid Support

ERIC Educational Resources Information Center

Coursindel, Thibault; Martinez, Jean; Parrot, Isabelle

2010-01-01

In this laboratory activity, students are introduced to a three-step synthesis of hydantoin (imidazolidine-2,4-dione), a moiety that is found in many biologically active compounds. Using a microwave oven and solid-support technology, this synthetic experiment is designed for masters-degree candidates working in organic chemistry or upper-level…

Microwave-Assisted Chemistry: Synthetic Applications for Rapid Assembly of Nanomaterials and Organics

EPA Science Inventory

The magic of microwave (MW) heating technique, termed as the Bunsen burner of the 21th Century, has emerged as valuable alternative in synthesis of organics, polymers, inorganics, and nanomaterials. Important innovations in MW-assisted chemistry now enable chemists to prepare cat...

Solid-Phase and Microwave-Assisted Syntheses of 2,5-Diketopiperazines: Small Molecules with Great Potential

PubMed Central

O'Neill, J.C.; Blackwell, H. E.

2008-01-01

Diketopiperazines (DKPs) are a well-known class of heterocycles that have recently emerged as a promising biologically active scaffold. Solid-phase organic synthesis has become an important tool in the combinatorial exploration of these privileged structures, expediting the synthesis and, therefore, the discovery of active compounds. To date, certain DKPs have shown potent activities against a range of diseases and biological phenomena, including bacterial infections, various cancers, asthma, infertility, premature labor, and HIV. Recent applications of solid-phase DKP synthesis, with a particular focus on cyclative cleavage and microwave-assisted reactions, are highlighted herein. PMID:18288948

Microwave-assisted synthesis and anti-YFV activity of 2,3-diaryl-1,3-thiazolidin-4-ones.

PubMed

Sriram, Dharmarajan; Yogeeswari, Perumal; Kumar, T G Ashok

2005-09-01

The purpose of this study was to prepare several 1,3-thaizolidin-4-ones bearing variously substituted diaryl ring at C-2 and N-3 positions and evaluate them for their anti-YFV activity. Several 1,3-thaizolidin-4-ones were prepared by reacting substituted benzaldehyde with equimolar amount of an appropriate substituted aromatic amine in the presence of an excess of mercaptoacetic acid in toluene utilizing microwave irradiation. The synthesized compounds were also evaluated for their inhibitory effects on the replication of YFV in green monkey kidney (Vero) cells (ATCC CCL81), by means of a cytopathic effect reduction assay. The compound DS1 emerged as the most potent anti-YFV agent with EC50 of 6.9 microM and CC50 more than 100 microM making it more potent than ribavirin. 2,3-diaryl-1,3-thiazolidin-4-ones possess anti-YFV potency.

Greener and Expeditious Synthesis of Bioactive Heterocycles using Microwave Irradiation

EPA Science Inventory

The utilization of green chemistry techniques is dramatically reducing chemical waste and reaction times as has recently been proven in several organic syntheses and chemical transformations. To illustrate these advantages in the synthesis of bio-active heterocycles, we have stud...

Morphological evolution of Bi2Se3 nanocrystalline materials synthesized by microwave assisted solvothermal method

NASA Astrophysics Data System (ADS)

Bera, Sumit; Behera, P.; Mishra, A. K.; Krishnan, M.; Patidar, M. M.; Singh, D.; Gangrade, M.; Venkatesh, R.; Deshpande, U. P.; Phase, D. M.; Ganesan, V.

2018-04-01

Structural, morphological and spectroscopic properties of Bi2Se3 nanoparticles synthesized by microwave assisted solvothermal method were investigated systematically. A controlled synthesis of different morphologies by a small variation in synthesis procedure is demonstrated. Powder X-ray diffraction (XRD) confirmed the formation of single phase. Crystallite and particle size reductions were studied with XRD and AFM (Atomic Force Microscopy). Different morphologies such as hexagonal nanoflakes with cross section of around˜6µm, nanoflower and octahedral agglomerated crystals of nearly ˜60 nm size have been observed in scanning electron microscope while varying the microwave assisted synthesis procedures. A significant blue shift observed in diffuse reflectance spectroscopy evidences the energy gap tuning as a result of morphological evolution. The difference in morphology observed in this three fast, facile and scalable synthesis is advantageous for tuning the thermoelectric figure of merit and for probing the surface states of these topological insulators. Low temperature resistivity remains similar for all three variants depicting a 2D character as evidenced by a -lnT term of localization.

Microwave assisted esterification of acidified oil from waste cooking oil by CERP/PES catalytic membrane for biodiesel production.

PubMed

Zhang, Honglei; Ding, Jincheng; Zhao, Zengdian

2012-11-01

The traditional heating and microwave assisted method for biodiesel production using cation ion-exchange resin particles (CERP)/PES catalytic membrane were comparatively studied to achieve economic and effective method for utilization of free fatty acids (FFAs) from waste cooking oil (WCO). The optimal esterification conditions of the two methods were investigated and the experimental results showed that microwave irradiation exhibited a remarkable enhanced effect for esterification compared with that of traditional heating method. The FFAs conversion of microwave assisted esterification reached 97.4% under the optimal conditions of reaction temperature 60°C, methanol/acidified oil mass ratio 2.0:1, catalytic membrane (annealed at 120°C) loading 3g, microwave power 360W and reaction time 90min. The study results showed that it is a fast, easy and green way to produce biodiesel applying microwave irradiation. Copyright © 2012 Elsevier Ltd. All rights reserved.

BULK SYNTHESIS OF SILVER NANORODS IN POLY(ETHYLENE GLYCOL) USING MICROWAVE IRRADIATION

EPA Science Inventory

Microwave-assisted (MW), surfactantless, greener approach to bulk synthesis of silver nanorods employing poly (ethylene glycol) (PEG) is described. An aqueous solution of silver nitrate (AgNO-3,- 0.1 M, 4 mL) and 4 mL of PEG (molecular weight 300) were mixed at room temperature t...

Microwave assisted synthesis of bridgehead alkenes.

PubMed

Cleary, Leah; Yoo, Hoseong; Shea, Kenneth J

2011-04-01

A new, concise method to synthesize triene precursors for the type 2 intramolecular Diels-Alder reaction has been developed. Microwave irradiation of the trienes provides a convenient method for the synthesis of bridgehead alkenes. Higher yields, shorter reaction times, and lower reaction temperatures provide a general and efficient route to this interesting class of molecules.

Microwave Assisted Synthesis of Bridgehead Alkenes

PubMed Central

Cleary, Leah; Yoo, Hoseong; Shea, Kenneth J.

2011-01-01

A new, concise method to synthesize triene precursors for the type 2 intramolecular Diels–Alder reaction has been developed. Microwave irradiation of the trienes provides a convenient method for the synthesis of bridgehead alkenes. Higher yields, shorter reaction times and lower reaction temperatures provide a general and efficient route to this interesting class of molecules. PMID:21384818

Microwave-assisted combustion synthesis of nano iron oxide/iron-coated activated carbon, anthracite, cellulose fiber, and silica, with arsenic adsorption studies

EPA Science Inventory

Combustion synthesis of iron oxide/iron coated carbons such as activated carbon, anthracite, cellulose fiber and silica is described. The reactions were carried out in alumina crucibles using a Panasonic kitchen microwave with inverter technology, and the reaction process was com...

Green Pea and Garlic Puree Model Food Development for Thermal Pasteurization Process Quality Evaluation.

PubMed

Bornhorst, Ellen R; Tang, Juming; Sablani, Shyam S; Barbosa-Cánovas, Gustavo V; Liu, Fang

2017-07-01

Development and selection of model foods is a critical part of microwave thermal process development, simulation validation, and optimization. Previously developed model foods for pasteurization process evaluation utilized Maillard reaction products as the time-temperature integrators, which resulted in similar temperature sensitivity among the models. The aim of this research was to develop additional model foods based on different time-temperature integrators, determine their dielectric properties and color change kinetics, and validate the optimal model food in hot water and microwave-assisted pasteurization processes. Color, quantified using a * value, was selected as the time-temperature indicator for green pea and garlic puree model foods. Results showed 915 MHz microwaves had a greater penetration depth into the green pea model food than the garlic. a * value reaction rates for the green pea model were approximately 4 times slower than in the garlic model food; slower reaction rates were preferred for the application of model food in this study, that is quality evaluation for a target process of 90 °C for 10 min at the cold spot. Pasteurization validation used the green pea model food and results showed that there were quantifiable differences between the color of the unheated control, hot water pasteurization, and microwave-assisted thermal pasteurization system. Both model foods developed in this research could be utilized for quality assessment and optimization of various thermal pasteurization processes. © 2017 Institute of Food Technologists®.

Microwave-assisted synthesis of porous carbon-titania and highly crystalline titania nanostructures.

PubMed

Parker, Alison; Marszewski, Michal; Jaroniec, Mietek

2013-03-01

Porous carbon-titania and highly crystalline titania nanostructured materials were obtained through a microwave-assisted one-pot synthesis. Resorcinol and formaldehyde were used as carbon precursors, triblock copolymer Pluronic F127 as a stabilizing agent, and titanium isopropoxide as a titania precursor. This microwave-assisted one-pot synthesis involved formation of carbon spheres according to the recently modified Stöber method followed by hydrolysis and condensation of titania precursor. This method afforded carbon-titania composite materials containing anatase phase with specific surface areas as high as 390 m(2) g(-1). The pure nanostructured titania, obtained after removal of carbon through calcination of the composite material in air, was shown to be the anatase phase with considerably higher degree of crystallinity and the specific surface area as high as 130 m(2) g(-1). The resulting titania, because of its high surface area, well-developed porosity, and high crystallinity, is of great interest for catalysis, water treatment, lithium batteries, and other energy-related applications.

Synthesis of hexagonal wurtzite Cu{sub 2}ZnSnS{sub 4} prisms by an ultrasound-assisted microwave solvothermal method

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

Long, Fei, E-mail: long.drf@gmail.com; Chi, Shangsen; Institute of Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083

Wurtzite Cu{sub 2}ZnSnS{sub 4} (CZTS) hexagonal prisms were synthesized by a simple ultrasound-microwave solvothermal method. The product was characterized by XRD, FESEM, EDS, TEM, Raman and UV–vis spectrometer. The hexagonal prisms were 0.5–2 μm wide and 5–12 μm long. The PVP played an important role in the formation of the CZTS hexagonal prisms. In addition, the ultrasound-assisted microwave process was helpful for synthesis of wurtzite rather than kesterite phase CZTS. A nucleation–dissolution–recrystallization mechanism was also proposed to explain the growth of the CZTS hexagonal prisms. - Graphical abstract: Wurtzite Cu{sub 2}ZnSnS{sub 4} hexagonal prisms were synthesized by ultrasound-microwave solvothermal method.more » The ultrasound-assisted microwave process and PVP were useful to the growth of CZTS. A nucleation–dissolution–recrystallization growth mechanism was also proposed. - Highlights: • Wurtzite Cu{sub 2}ZnSnS{sub 4} was prepared by ultrasound-assisted microwave solvothermal method. • The wurtzite CZTS hexagonal prisms are demonstrated a band gap of 1.49 eV. • Synergistic effect of ultrasound and microwave is helpful to prepare Wurtzite CZTS. • PVP plays an important role in the formation of the CZTS hexagonal prisms. • Nucleation–dissolution–recrystallization growth mechanism of the CZTS was proposed.« less

Microwave-assisted synthesis of sensitive silver substrate for surface-enhanced Raman scattering spectroscopy

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

Xia Lixin; Wang Haibo; Wang Jian

A sensitive silver substrate for surface-enhanced Raman scattering (SERS) spectroscopy is synthesized under multimode microwave irradiation. The microwave-assisted synthesis of the SERS-active substrate was carried out in a modified domestic microwave oven of 2450 MHz, and the reductive reaction was conducted in a polypropylene container under microwave irradiation with a power of 100 W for 5 min. Formaldehyde was employed as both the reductant and microwave absorber in the reductive process. The effects of different heating methods (microwave dielectric and conventional) on the properties of the SERS-active substrates were investigated. Samples obtained with 5 min of microwave irradiation at amore » power of 100 W have more well-defined edges, corners, and sharper surface features, while the samples synthesized with 1 h of conventional heating at 40 deg. C consist primarily of spheroidal nanoparticles. The SERS peak intensity of the {approx}1593 cm{sup -1} band of 4-mercaptobenzoic acid adsorbed on silver nanoparticles synthesized with 5 min of microwave irradiation at a power of 100 W is about 30 times greater than when it is adsorbed on samples synthesized with 1 h of conventional heating at 40 deg. C. The results of quantum chemical calculations are in good agreement with our experimental data. This method is expected to be utilized for the synthesis of other metal nanostructural materials.« less

TiO2 synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

NASA Astrophysics Data System (ADS)

Moura, K. F.; Maul, J.; Albuquerque, A. R.; Casali, G. P.; Longo, E.; Keyson, D.; Souza, A. G.; Sambrano, J. R.; Santos, I. M. G.

2014-02-01

In this study, a microwave assisted solvothermal method was used to synthesize TiO2 with anatase structure. The synthesis was done using Ti (IV) isopropoxide and ethanol without templates or alkalinizing agents. Changes in structural features were observed with increasing time of synthesis and evaluated using periodic quantum chemical calculations. The anatase phase was obtained after only 1 min of reaction besides a small amount of brookite phase. Experimental Raman spectra are in accordance with the theoretical one. Micrometric spheres constituted by nanometric particles were obtained for synthesis from 1 to 30 min, while spheres and sticks were observed after 60 min.

Heteropoly acid-catalyzed microwave-assisted three-component aza-Diels-Alder cyclizations: diastereoselective synthesis of potential drug candidates for Alzheimer's disease.

PubMed

Borkin, Dmitry; Morzhina, Elena; Datta, Silpi; Rudnitskaya, Aleksandra; Sood, Abha; Török, Marianna; Török, Béla

2011-03-07

A highly diastereoselective microwave-assisted three component synthesis of azabicyclo[2.2.2]octan-5-ones by a silicotungstic acid-catalyzed aza-Diels-Alder cyclization is described. The one-pot process involves the formation of the in situ generated Schiff base and its immediate cyclization with cyclohex-2-enone. The short reaction times, good yields and excellent diastereoselectivity make this annulation a practical and environmentally attractive method for the synthesis of the target compounds. Preliminary assays were carried out to determine the activity of the products in AChE as well as in amyloid β fibrillogenesis inhibition.

A NOVEL HIGH-SPEED METHOD FOR THE GENERATION OF 4-ARYLDIHYDROPYRIMIDINE COMPOUND LIBRARIES USING A MICROWAVE-ASSISTED BIGINELLI CONDENSATION PROTOCOL -

EPA Science Inventory

In this presentation we report the application of microwave assisted chemistry to the parallel synthesis of 4-aryl-3,4-dihydropyrimidin-2(1H)-ones employing a solventless Biginelli multicomponent condensation protocol. The novel method employs neat mixtures of B-ketoesters, aryl ...

Trace detection of tetrahydrocannabinol (THC) with a SERS-based capillary platform prepared by the in situ microwave synthesis of AgNPs.

PubMed

Yüksel, Sezin; Schwenke, Almut M; Soliveri, Guido; Ardizzone, Silvia; Weber, Karina; Cialla-May, Dana; Hoeppener, Stephanie; Schubert, Ulrich S; Popp, Jürgen

2016-10-05

In the present study, an ultra-sensitive and highly reproducible novel SERS-based capillary platform was developed and utilized for the trace detection of tetrahydrocannabinol (THC). The approach combines the advantages of microwave-assisted nanoparticle synthesis, plasmonics and capillary forces. By employing a microwave-assisted preparation method, glass capillaries were reproducibly coated with silver nanoparticles in a batch fabrication process that required a processing time of 3 min without needing to use any pre-surface modifications or add surfactants. The coated capillaries exhibited an excellent SERS activity with a high reproducibility and enabled the detection of low concentrations of target molecules. At the same time, only a small amount of analyte and a short and simple incubation process was required. The developed platform was applied to the spectroscopic characterization of tetrahydrocannabinol (THC) and its identification at concentration levels down to 1 nM. Thus, a highly efficient detection system for practical applications, e.g., in drug monitoring/detection, is introduced, which can be fabricated at low cost by using microwave-assisted batch synthesis techniques. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

PubMed Central

Lovingood, Derek D.; Owens, Jeffrey R.; Seeber, Michael; Kornev, Konstantin G.; Luzinov, Igor

2013-01-01

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan δ solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials' morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by Stöber's methods, which have smooth surfaces. PMID:24379052

Green and Selective Fluorescent Sensor for Detection of Sn (IV) and Mo (VI) Based on Boron and Nitrogen-Co-Doped Carbon Dots.

PubMed

Tabaraki, Reza; Abdi, Omran; Yousefipour, Sedigheh

2017-03-01

A green and simple microwave-assisted method was used to synthesis water-soluble boron and nitrogen-co-doped carbon dots (B-N-CDs). These B-N-CDs were successfully used for the fluorescent determination of Sn 4+ and Mo 6+ ions. This probe had a fast response time at pH = 4 with high sensitivity and selectivity. Linear correlation between F 0 /F and the concentration was seen in the range of 0.2-18 μM and 0.2-25 μM for Sn 4+ and Mo 6+ , respectively. Under optimum condition, the limit of detection (LOD) for Sn 4+ and Mo 6+ were 150 nM and 132 nM, respectively. The performance of the sensor was evaluated by different real samples such as tap, river and mineral water, canned fish sample and tomato samples.

Multicapillary Flow Reactor: Synthesis of 1,2,5-Thiadiazepane 1,1-Dioxide Library Utilizing One-Pot Elimination and Inter-/Intramolecular Double aza-Michael Addition Via Microwave-Assisted, Continuous-Flow Organic Synthesis (MACOS)

PubMed Central

Ullah, Farman; Zang, Qin; Javed, Salim; Zhou, Aihua; Knudtson, Christopher A.; Bi, Danse; Hanson, Paul R.; Organ, Michael G.

2013-01-01

A microwave-assisted, continuous-flow organic synthesis (MACOS) protocol for the synthesis of functionalized 1,2,5-thiadiazepane 1,1-dioxide library, utilizing a one-pot elimination and inter-/intramolecular double aza-Michael addition strategy is reported. The optimized protocol in MACOS was utilized for scale-out and further extended for library production using a multicapillary flow reactor. A 50-member library of 1,2,5-thiadiazepane 1,1-dioxides was prepared on a 100- to 300-mg scale with overall yields between 50 and 80% and over 90 % purity determined by proton nuclear magnetic resonance (1H-NMR) spectroscopy. PMID:24244871

Synthesis of new 2-amino-4H-pyran-3,5-dicarboxylate derivatives using nanocrystalline MIIZr4(PO4)6 ceramics as reusable and robust catalysts under microwave irradiation

NASA Astrophysics Data System (ADS)

Safaei-Ghomi, Javad; Javidan, Abdollah; Ziarati, Abolfazl; Shahbazi-Alavi, Hossein

2015-08-01

In the present paper, we report the successful synthesis of nanocrystalline MIIZr4(PO4)6 ceramics (M: Mn, Ni, Fe, Co). These nano-structures were characterized by X-ray diffraction, scanning electron microscopy, and vibrating sample magnetometer (VSM). Size of nano-structures was in the range of 20-150 nm. Nano-MIIZr4(PO4)6 as an efficient and green catalyst has been used for the preparation of 2-amino-4H-pyran-3,5-dicarboxylate derivatives by the three-component condensation reaction of ethyl cyanoacetate, ethyl acetoacetate, and various aromatic aldehydes under microwave irradiation. Extraordinarily, the best results were obtained using MnZr4(PO4)6 nanocrystallines as an efficient catalyst. This method provides several advantages including easy work-up, excellent yields, short reaction times, using of microwave as green method, recoverability of the catalyst, and little catalyst loading.

Innovative green technique for preparing of flame retardant cotton

USDA-ARS?s Scientific Manuscript database

Due to its environmentally benign character, microwave-assisted or supercritical carbon dioxide high pressure reactors are considered in green chemistry as a substitute for organic solvents in chemical reactions. In this paper, an innovative approach for preparation of flame retardant cotton fabric ...

Plasma-assisted microwave processing of materials

NASA Technical Reports Server (NTRS)

Barmatz, Martin (Inventor); Jackson, Henry (Inventor); Ylin, Tzu-yuan (Inventor)

1998-01-01

A microwave plasma assisted method and system for heating and joining materials. The invention uses a microwave induced plasma to controllably preheat workpiece materials that are poorly microwave absorbing. The plasma preheats the workpiece to a temperature that improves the materials' ability to absorb microwave energy. The plasma is extinguished and microwave energy is able to volumetrically heat the workpiece. Localized heating of good microwave absorbing materials is done by shielding certain parts of the workpiece and igniting the plasma in the areas not shielded. Microwave induced plasma is also used to induce self-propagating high temperature synthesis (SHS) process for the joining of materials. Preferably, a microwave induced plasma preheats the material and then microwave energy ignites the center of the material, thereby causing a high temperature spherical wave front from the center outward.

GREENER AND CONTROLLED SYNTHESIS OF NOBLE NANOSTRUCTURES IN AQUEOUS MEDIA USING MICROWAVE IRRADIATION

EPA Science Inventory

Microwave-assisted spontaneous reduction of gold salts is described using sugar solutions such as alpha-D-glucose, sucrose and maltose, etc. The expeditious reactions are conducted in aqueous media using microwave irradiation wherein the reduction occurs within 30 to 60 seconds ...

MICROWAVE-ACCELERATED CARBON-NITROGEN BOND FORMATION: A GREEN CHEMICAL APPROACH FOR THE SYNTHESIS OF AMINES AND HETEROCYCLES IN AQUEOUS MEDIA

EPA Science Inventory

The concept of "green chemistry" is widely adopted to meet the fundamental scientific challenges of protecting the human health and environment while simultaneously achieving commercial viability. One of the thrust areas for achieving this target is to explore alternative reactio...

Fast microwave-assisted green synthesis of xanthan gum grafted acrylic acid for enhanced methylene blue dye removal from aqueous solution.

PubMed

Makhado, Edwin; Pandey, Sadanand; Nomngongo, Philiswa N; Ramontja, James

2017-11-15

In the present project, graft polymerization was employed to synthesis a novel adsorbent using acrylic acid (AA) and xanthan gum (XG) for cationic methylene dye (MB + ) removal from aqueous solution. The XG was rapidly grafted with acrylic acid (CH 2 =CHCOOH) under microwave heating. Fourier-transform infrared spectroscopy (FTIR), Proton Nuclear magnetic resonance spectroscopy ( 1 H NMR), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Thermal gravimetric analysis (TGA) techniques were used to verify the adsorbent formed under optimized reaction conditions. Optimum reaction conditions [AA (0.4M), APS (0.05M), XG (2gL -1 ), MW power (100%), MW time (80s)] offer maximum %G and %GE of 484 and 78.3, respectively. The removal ratio of adsorbent to MB + reached to 92.8% at 100mgL -1 . Equilibrium and kinetic adsorptions of dyes were better explained by the Langmuir isotherm and pseudo second-order kinetic model respectively. The results demonstrate xanthan gum grafted polyacrylic acid (mw XG-g-PAA) absorbent had the universality for removal of dyes through the chemical adsorption mechanism. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis of carbon-based quantum dots from starch extracts: Optical investigations.

PubMed

Al-Douri, Y; Badi, N; Voon, C H

2018-03-01

Carbon-based quantum dots (C-QDs) were synthesized through microwave-assisted carbonization of an aqueous starch suspension mediated by sulphuric and phosphoric acids. The as-prepared C-QDs showed blue, green and yellow luminescence without the addition of any surface-passivating agent. The C-QDs were further analyzed by UV-vis spectroscopy to measure the optical response of the organic compound. The energy gaps revealed narrow sizing of C-QDs in the semiconductor range. The optical refractive index and dielectric constant were investigated. The C-QDs size distribution was characterized. The results suggested an easy route to the large scale production of C-QDs materials. Copyright © 2017 John Wiley & Sons, Ltd.

A novel route for the synthesis of nanotubes and fullerene-like nanostructures of molybdenum disulfide

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

Panigrahi, Pravas Kumar, E-mail: pravas.iit@gmail.com; Pathak, Amita, E-mail: ami@chem.iitkgp.ernet.in

Graphical abstract: Nanotubes and fullerene-like nanostructures of MoS{sub 2} were synthesized via a microwave-assisted route in solution phase. Highlights: Black-Right-Pointing-Pointer Microwave-assisted route for synthesis of nanotube and fullerene-like nanostructures of MoS{sub 2}. Black-Right-Pointing-Pointer Morphological analysis of the synthesized products. Black-Right-Pointing-Pointer Solvent plays important role in the modification of morphology of MoS{sub 2}. -- Abstract: The paper described the synthesis of nanotubes and fullerene-like nanostructures of MoS{sub 2} through a technically simple, rapid, and energy-efficient microwave-assisted synthesis technique, which involved the use of elemental sulfur dissolved in a mixture of monoethanolamine and hydrazine hydrate as the sulfide source. The microwave inducedmore » reaction between the molybdate with sulfide ions, in the presence of hydrazine hydrate in the reaction medium, resulted in the formation of gray colored powders of amorphous MoS{sub 2}. The as-obtained powders were calcined at 600 Degree-Sign C for 2 h and characterized by different techniques. HRTEM analysis of the calcined samples indicated the formation of fullerene-like MoS{sub 2} structures when the starting solution mixture was irradiated with microwave for a period of 200 s, while on 600 s of irradiation of the same revealed the formation of folded sheets like MoS{sub 2} nanotubes. BET surface areas of the calcined samples have been measured and a plausible reaction mechanism for the formation of nanotubes and fullerene-like nanostructures of MoS{sub 2} has been proposed.« less

Microwave-assisted green synthesis of superparamagnetic nanoparticles using fruit peel extracts: surface engineering, T 2 relaxometry, and photodynamic treatment potential.

PubMed

Bano, Shazia; Nazir, Samina; Nazir, Alia; Munir, Saeeda; Mahmood, Tariq; Afzal, Muhammad; Ansari, Farzana Latif; Mazhar, Kehkashan

2016-01-01

Superparamagnetic iron oxide nanoparticles (SPIONs) have the potential to be used as multimodal imaging and cancer therapy agents due to their excellent magnetism and ability to generate reactive oxygen species when exposed to light. We report the synthesis of highly biocompatible SPIONs through a facile green approach using fruit peel extracts as the biogenic reductant. This green synthesis protocol involves the stabilization of SPIONs through coordination of different phytochemicals. The SPIONs were functionalized with polyethylene glycol (PEG)-6000 and succinic acid and were extensively characterized by X-ray diffraction analysis, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, Rutherford backscattering spectrometry, diffused reflectance spectroscopy, fluorescence emission, Fourier-transform infrared spectroscopy, ultraviolet-visible spectroscopy, and magnetization analysis. The developed SPIONs were found to be stable, almost spherical with a size range of 17-25 nm. They exhibited excellent water dispersibility, colloidal stability, and relatively high R 2 relaxivity (225 mM(-1) s(-1)). Cell viability assay data revealed that PEGylation or carboxylation appears to significantly shield the surface of the particles but does not lead to improved cytocompatibility. A highly significant increase of reactive oxygen species in light-exposed samples was found to play an important role in the photokilling of human cervical epithelial malignant carcinoma (HeLa) cells. The bio-SPIONs developed are highly favorable for various biomedical applications without risking interference from potentially toxic reagents.

Microwave-assisted green synthesis of superparamagnetic nanoparticles using fruit peel extracts: surface engineering, T2 relaxometry, and photodynamic treatment potential

PubMed Central

Bano, Shazia; Nazir, Samina; Nazir, Alia; Munir, Saeeda; Mahmood, Tariq; Afzal, Muhammad; Ansari, Farzana Latif; Mazhar, Kehkashan

2016-01-01

Superparamagnetic iron oxide nanoparticles (SPIONs) have the potential to be used as multimodal imaging and cancer therapy agents due to their excellent magnetism and ability to generate reactive oxygen species when exposed to light. We report the synthesis of highly biocompatible SPIONs through a facile green approach using fruit peel extracts as the biogenic reductant. This green synthesis protocol involves the stabilization of SPIONs through coordination of different phytochemicals. The SPIONs were functionalized with polyethylene glycol (PEG)-6000 and succinic acid and were extensively characterized by X-ray diffraction analysis, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, Rutherford backscattering spectrometry, diffused reflectance spectroscopy, fluorescence emission, Fourier-transform infrared spectroscopy, ultraviolet-visible spectroscopy, and magnetization analysis. The developed SPIONs were found to be stable, almost spherical with a size range of 17–25 nm. They exhibited excellent water dispersibility, colloidal stability, and relatively high R2 relaxivity (225 mM−1 s−1). Cell viability assay data revealed that PEGylation or carboxylation appears to significantly shield the surface of the particles but does not lead to improved cytocompatibility. A highly significant increase of reactive oxygen species in light-exposed samples was found to play an important role in the photokilling of human cervical epithelial malignant carcinoma (HeLa) cells. The bio-SPIONs developed are highly favorable for various biomedical applications without risking interference from potentially toxic reagents. PMID:27570452

Evaluation of the essential oil of Foeniculum vulgare Mill (fennel) fruits extracted by three different extraction methods by GC/MS.

PubMed

Hammouda, Faiza M; Saleh, Mahmoud A; Abdel-Azim, Nahla S; Shams, Khaled A; Ismail, Shams I; Shahat, Abdelaaty A; Saleh, Ibrahim A

2014-01-01

Hydrodistillation (HD) and steam-distillation, or solvent extraction methods of essential oils have some disadvantages like thermal decomposition of extracts, its contamination with solvent or solvent residues and the pollution of residual vegetal material with solvent which can be also an environmental problem. Thus, new green techniques, such as supercritical fluid extraction and microwave assisted techniques, are potential solutions to overcome these disadvantages. The aim of this study was to evaluate the essential oil of Foeniculum vulgare subsp. Piperitum fruits extracted by three different extraction methods viz. Supercritical fluid extraction (SFE) using CO2, microwave-assisted extraction (MAE) and hydro-distillation (HD) using gas chromatography-mass spectrometry (GC/MS). The results revealed that both MAE and SFE enhanced the extraction efficiency of the interested components. MAE gave the highest yield of oil as well as higher percentage of Fenchone (28%), whereas SFE gave the highest percentage of anethol (72%). Microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE) not only enhanced the essential oil extraction but also saved time, reduced the solvents use and produced, ecologically, green technologies.

Synthesis and photophysical characterizations of thermal-stable naphthalene benzimidazoles.

PubMed

Erten-Ela, Sule; Ozcelik, Serdar; Eren, Esin

2011-07-01

Microwave-assisted synthesis, photophysical and electrochemical properties of thermal-stable naphthalene benzimidazoles and naphthalimides are studied in this paper. Microwave-assisted synthesis of naphthalene benzimidazoles provide higher yields than the conventional thermal synthesis. Comparative photophysical properties of naphthalene benzimidazoles and naphthalimides are revealed that conjugation of electron-donating group onto naphthalimide moiety increases fluorescence quantum yields. Fluorophore-solvent interactions are also investigated using Lippert-Mataga equation for naphthalimides and naphthalene benzimidazoles. Thermal stabilities of naphthalene benzimidazoles are better than naphthalimides due to increased aromaticity. The experimental E(LUMO) levels of naphthalene benzimidazoles are found to be between 3.15 and 3.28 eV. Therefore, naphthalene benzimidazole derivatives consisting of anchoring groups are promising materials in organic dye sensitized solar cells. © Springer Science+Business Media, LLC 2011

Microwave-Assisted Synthesis of Boron and Nitrogen co-doped Reduced Graphene Oxide for the Protection of Electromagnetic Radiation in Ku-Band.

PubMed

Umrao, Sima; Gupta, Tejendra K; Kumar, Shiv; Singh, Vijay K; Sultania, Manish K; Jung, Jung Hwan; Oh, Il-Kwon; Srivastava, Anchal

2015-09-09

The electromagnetic interference (EMI) shielding of reduced graphene oxide (MRG), B-doped MRG (B-MRG), N-doped MRG (N-MRG), and B-N co-doped MRG (B-N-MRG) have been studied in the Ku-band frequency range (12.8-18 GHz). We have developed a green, fast, and cost-effective microwave assisted route for synthesis of doped MRG. B-N-MRG shows high electrical conductivity in comparison to MRG, B-MRG and N-MRG, which results better electromagnetic interference (EMI) shielding ability. The co-doping of B and N significantly enhances the electrical conductivity of MRG from 21.4 to 124.4 Sm(-1) because N introduces electrons and B provides holes in the system and may form a nanojunction inside the material. Their temperature-dependent electrical conductivity follows 2D-variable range hopping (2D-VRH) and Efros-Shklovskii-VRH (ES-VRH) conduction model in a low temperature range (T<50 K). The spatial configuration of MRG after doping of B and N enhances the space charge polarization, natural resonance, dielectric polarization, and trapping of EM waves by internal reflection leading to a high EMI shielding of -42 dB (∼99.99% attenuation) compared to undoped MRG (-28 dB) at a critical thickness of 1.2 mm. Results suggest that the B-N-MRG has great potential as a candidate for a new type of EMI shielding material useful in aircraft, defense industries, communication systems, and stealth technology.

Microwave-assisted synthesis of iron oxide nanoparticles in biocompatible organic environment

NASA Astrophysics Data System (ADS)

Aivazoglou, E.; Metaxa, E.; Hristoforou, E.

2018-04-01

The development of magnetite and maghemite particles in uniform nanometer size has triggered the interest of the research community due to their many interesting properties leading to a wide range of applications, such as catalysis, nanomedicine-nanobiology and other engineering applications. In this study, a simple, time-saving and low energy-consuming, microwave-assisted synthesis of iron oxide nanoparticles, is presented. The nanoparticles were prepared by microwave-assisted synthesis using polyethylene glycol (PEG) or PEG and β-cyclodextrin (β-CD)/water solutions of chloride salts of iron in the presence of ammonia solution. The prepared nano-powders were characterized using X-Ray Diffraction (XRD), Transition Electron Microscopy (TEM), Fourier-transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, Vibrating Sample Magnetometer (VSM), X-Ray Photoelectron Spectroscopy (XPS) and Thermal analysis (TG/DSC). The produced nanoparticles are crystallized mostly in the magnetite and maghemite lattice exhibiting very similar shape and size, with indications of partial PEG coating. Heating time, microwave power and presence of PEG, are the key factors shaping the size properties of nanoparticles. The average size of particles ranges from 10.3 to 19.2 nm. The nanoparticles exhibit a faceted morphology, with zero contamination levels. The magnetic measurements indicate that the powders are soft magnetic materials with negligible coercivity and remanence, illustrating super-paramagnetic behavior.

Methane Synthesis from Automotive Paint Sludge via Microwave Assisted Pyrolysis

NASA Astrophysics Data System (ADS)

Rosli, N. L.; Rahman, N. Abd; Kadri, A.

2018-05-01

Methane gas, which has one atom of carbon and four atoms of hydrogen, is a valuable energy resource, which can be used in the energy sector. The purpose of this research work is to identify methane synthesis from Automotive Paint Sludge (APS) using microwave assisted pyrolysis. APS is known as a hazardous waste since it contains various chemicals that categorized as heavy metals and toxic substances. A modified conventional kitchen microwave was used to pyrolise the APS. The microwave was set with the power level of 600 W and 50 minutes radiation time. Through the experiment, pyrogas was collected into tedlar bag and was analysed using Gas Chromatography with Flame Ionization Detector (GC-FID). Results from the GC-FID were shown that the retention time of 3.3583, 3.2733, and 3.2267 min are proved to be methane gas. The results obtained are resembled with the results from the literature. This indicates methane gas was presented in the pyrogas of pyrolysis of APS and there is a possibility of producing methane gas. The research study suggests that it is possible to synthesize methane gas from the APS via microwave assisted pyrolysis, and in the meantime reduce the volume of APS in the landfill.

A concise synthesis of benzimidazoles via the microwave-assisted one-pot batch reaction of amino acids up to a 10-g scale.

PubMed

Peng, Pai; Xiong, Jin-Feng; Mo, Guang-Zhen; Zheng, Jia-Li; Chen, Ren-Hong; Chen, Xiao-Yun; Wang, Zhao-Yang

2014-10-01

An efficient method for the synthesis of aminomethyl benzimidazoles is developed by using a one-pot batch reaction between amino acids and o-phenylenediamines. This reaction proceeds smoothly in an unmodified household microwave oven, even though scale-up is to 10 g. A desirable method for the quick synthesis of benzimidazoles, which are used as a kind of important intermediates in drug synthesis, is provided by the scale-up utilization of amino acid resource.

Microwave-assisted synthesis and micellization behavior of soy-based copoly(2-oxazoline)s.

PubMed

Hoogenboom, Richard; Leenen, Mark A M; Huang, Haiying; Fustin, Charles-André; Gohy, Jean-François; Schubert, Ulrich S

2006-01-01

Polymers based on renewable resources are promising candidates for replacing common organic polymers, and thus, for reducing oil consumption. In this contribution we report the microwave-assisted synthesis of block and statistical copolymers from 2-ethyl-2-oxazoline and 2-"soy alkyl"-2-oxazoline via a cationic ring-opening polymerization mechanism. The synthesized copolymers were characterized by gel permeation chromatography and 1 H-NMR spectroscopy. The micellization of these amphiphilic copolymers was investigated by dynamic light scattering and atomic force microscopy to examine the effect of hydrophobic block length and monomer distribution on the resulting micellar characteristics.

Microwave-assisted chemistry: synthetic applications for rapid assembly of nanomaterials and organics.

PubMed

Gawande, Manoj B; Shelke, Sharad N; Zboril, Radek; Varma, Rajender S

2014-04-15

The magic of microwave (MW) heating technique, termed the Bunsen burner of the 21st century, has emerged as a valuable alternative in the synthesis of organic compounds, polymers, inorganic materials, and nanomaterials. Important innovations in MW-assisted chemistry now enable chemists to prepare catalytic materials or nanomaterials and desired organic molecules, selectively, in almost quantitative yields and with greater precision than using conventional heating. By controlling the specific MW parameters (temperature, pressure, and ramping of temperature) and choice of solvents, researchers can now move into the next generation of advanced nanomaterial design and development. Microwave-assisted chemical reactions are now well-established practices in the laboratory setting although some controversy lingers as to how MW irradiation is able to enhance or influence the outcome of chemical reactions. Much of the discussion has focused on whether the observed effects can, in all instances, be rationalized by purely thermal Arrhenius-based phenomena (thermal microwave effects), that is, the importance of the rapid heating and high bulk reaction temperatures that are achievable using MW dielectric heating in sealed reaction vessels, or whether these observations can be explained by so-called "nonthermal" or "specific microwave" effects. In recent years, innovative and significant advances have occurred in MW hardware development to help delineate MW effects, especially the use of silicon carbide (SiC) reaction vessels and the accurate measurement of temperature using fiber optic (FO) temperature probes. SiC reactors appear to be good alternatives to MW transparent borosilicate glass, because of their high microwave absorptivity, and as such they serve as valuable tools to demystify the claimed magical MW effects. This enables one to evaluate the influence of the electromagnetic field on the specific chemical reactions, under truly identical conventional heating conditions, wherein temperature is measured accurately by fiber optic (FO) probe. This Account describes the current status of MW-assisted synthesis highlighting the introduction of various prototypes of equipment, classes of organic reactions pursued using nanomaterials, and the synthesis of unique and multifunctional nanomaterials; the ensuing nanomaterials possess zero-dimensional to three-dimensional shapes, such as spherical, hexagonal, nanoprisms, star shapes, and nanorods. The synthesis of well-defined nanomaterials and nanocatalysts is an integral part of nanotechnology and catalysis science, because it is imperative to control their size, shape, and compositional engineering for unique deployment in the field of nanocatalysis and organic synthesis. MW-assisted methods have been employed for the convenient and reproducible synthesis of well-defined noble and transition core-shell metallic nanoparticles with tunable shell thicknesses. Some of the distinctive attributes of MW-selective heating in the synthesis and applications of magnetic nanocatalysts in organic synthesis under benign reaction conditions are highlighted. Sustainable nanomaterials and their applications in benign media are an ideal blend for the development of greener methodologies in organic synthesis; MW heating provides superb value to the overall sustainable process development via process intensification including the flow systems.

Nitration of Phenols Using Cu(NO[subscript 3])[subscript 2]: Green Chemistry Laboratory Experiment

ERIC Educational Resources Information Center

Yadav, Urvashi; Mande, Hemant; Ghalsasi, Prasanna

2012-01-01

An easy-to-complete, microwave-assisted, green chemistry, electrophilic nitration method for phenol using Cu(NO[subscript 3])[subscript 2] in acetic acid is discussed. With this experiment, students clearly understand the mechanism underlying the nitration reaction in one laboratory session. (Contains 4 schemes.)

Sustainable Synthesis of Organics and Nanomaterials Using Microwave Irradiation

EPA Science Inventory

MW-assisted synthesis of heterocyclic compounds and nanomaterials under benign conditions is summarized. Shape-controlled aqueous synthesis of noble nanostructures via MW spontaneous reduction of metal salts using -D-glucose, sucrose, and maltose will be presented. A general met...

Alternative energy input: Mechanochemical, microwave and ultrasound-assisted organic synthesis

EPA Science Inventory

Microwave, ultrasound, sunlight and mechanochemical mixing can be used to augment conventional laboratory techniques. By applying these alternative means of activation, a number of chemical transformations have been achieved thereby improving many existing protocols with superi...

One-step solution combustion synthesis of pure Ni nanopowders with enhanced coercivity: The fuel effect

NASA Astrophysics Data System (ADS)

Khort, Alexander; Podbolotov, Kirill; Serrano-García, Raquel; Gun'ko, Yurii K.

2017-09-01

In this paper, we report a new modified one-step combustion synthesis technique for production of Ni metal nanoparticles. The main unique feature of our approach is the use of microwave assisted foam preparation. Also, the effect of different types of fuels (urea, citric acid, glycine and hexamethylenetetramine) on the combustion process and characteristics of resultant solid products were investigated. It is observed that the combination of microwave assisted foam preparation and using of hexamethylenetetramine as a fuel allows producing pure ferromagnetic Ni metal nanoparticles with enhanced coercivity (78 Oe) and high value of saturation magnetization (52 emu/g) by one-step solution combustion synthesis under normal air atmosphere without any post-reduction processing.

Microwave-assisted domino and multicomponent reactions with cyclic acylketenes: expeditious syntheses of oxazinones and oxazindiones.

PubMed

Presset, Marc; Coquerel, Yoann; Rodriguez, Jean

2009-12-17

The microwave-assisted Wolff rearrangement of cyclic 2-diazo-1,3-diketones in the presence of aldehydes and primary amines provides a straightforward access to functionalized bi- and pentacyclic oxazinones following an unprecedented three-component domino reaction. Alternatively, in the presence of acyl azides, an efficient Curtius/Wolff/hetero-Diels-Alder sequence allows the direct synthesis of oxazindiones.

Role of modifier in microwave assisted extraction of oleanolic acid from Gymnema sylvestre: application of green extraction technology for botanicals.

PubMed

Mandal, Vivekananda; Dewanjee, Saikat; Mandal, Subhash C

2009-08-01

This work highlights the development of a green extraction technology for botanicals with the use of microwave energy. Taking into consideration the extensive time involved in conventional extraction methods, coupled with usage of large volumes of organic solvent and energy resources, an ecofriendly green method that can overcome the above problems has been developed. The work compares the effect of sample pretreatment with untreated sample for improved yield of oleanolic acid from Gymnema sylvestre leaves. The pretreated sample with water produced 0.71% w/w oleanolic acid in one extraction cycle with 500 W microwave power, 25 mL methanol and only an 8 min extraction time. On the other hand, a conventional heat reflux extraction for 6 hours could produce only 0.62% w/w oleanolic acid. The detailed mechanism of extraction has been studied through scanning electron micrographs. The environmental impact of the proposed green method has also been evaluated.

Microwave Synthesis and Characterization of Waste Soybean Oil-Based Gemini Imidazolinium Surfactants with Carbonate Linkage

NASA Astrophysics Data System (ADS)

Tripathy, Divya Bajpai; Mishra, Anuradha

Gemini surfactants are presently gaining attention due to their unusual self-assembling characteristics and incomparable interfacial activity. Current research work involves the cost-effective microwave (MW) synthesis of waste soybean oil-based gemini imidazolinium surfactants (GIS) having a carbonate linkage in its spacer moiety. Structural characterizations of the materials have been done using FT-IR, 1H-NMR and 13C-NMR. Using indigenous and natural material as base and MW as energy source for synthesizing the GIS with easily degradable chemical moiety make them to be labeled as green surfactants.

TiO2-coated mesoporous carbon: conventional vs. microwave-annealing process.

PubMed

Coromelci-Pastravanu, Cristina; Ignat, Maria; Popovici, Evelini; Harabagiu, Valeria

2014-08-15

The study of coating mesoporous carbon materials with titanium oxide nanoparticles is now becoming a promising and challenging area of research. To optimize the use of carbon materials in various applications, it is necessary to attach functional groups or other nanostructures to their surface. The combination of the distinctive properties of mesoporous carbon materials and titanium oxide is expected to be applied in field emission displays, nanoelectronic devices, novel catalysts, and polymer or ceramic reinforcement. But, their synthesis is still largely based on conventional techniques, such as wet impregnation followed by chemical reduction of the metal nanoparticle precursors, which takes time and money. The thermal heating based techniques are time consuming and often lack control of particle size and morphology. Hence, since there is a growing interest in microwave technology, an alternative way of power input into chemical reactions through dielectric heating is the use of microwaves. This work is focused on the advantages of microwave-assisted synthesis of TiO2-coated mesoporous carbon over conventional thermal heating method. The reviewed studies showed that the microwave-assisted synthesis of such composites allows processes to be completed within a shorter reaction time allowing the nanoparticles formation with superior properties than that obtained by conventional method. Copyright © 2014 Elsevier B.V. All rights reserved.

Microwave-Assisted Piloty-Robinson Synthesis of 3,4-Disubstituted Pyrroles

PubMed Central

Milgram, Benjamin C.; Eskildsen, Katrine; Richter, Steven M.; Scheidt, W. Robert; Scheidt, Karl A.

2007-01-01

The synthesis of N-acyl 3,4-disubstituted pyrroles can be accomplished directly from hydrazine and an aldehyde via a Piloty-Robinson pyrrole synthesis. The use of microwave radiation for the cyclization and pyrrole formation greatly reduces the time necessary for this process and facilitates moderate to good yields from hydrazine for the corresponding 3,4-disubstituted products (5–12). By simple hydrolysis, the free N–H pyrroles can be accessed after the Piloty-Robinson reaction and then used directly in the synthesis of octaethylporphyrin (H2OEP, 14) and octaethyltetraphenylporphyrin (H2OETPP, 15). PMID:17432915

Microwave assisted combustion synthesis of nanocrystalline CoFe2O4 for LPG sensing

NASA Astrophysics Data System (ADS)

Chaudhari, Prashant; Acharya, S. A.; Darunkar, S. S.; Gaikwad, V. M.

2015-08-01

A microwave-assisted citrate precursor method has been utilized for synthesis of nanocrystalline powders of CoFe2O4. The process takes only a few minutes to obtain as-synthesized CoFe2O4. Structural properties of the synthesized material were investigated by X-ray diffraction; scanning electron microscopy, Thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy. The gas sensing properties of thick film of CoFe2O4 prepared by screen printing towards Liquid Petroleum Gas (LPG) revealed that CoFe2O4 thick films are sensitive and shows maximum sensitivity at 350°C for 2500 ppm of LPG.

Conventional and microwave assisted synthesis of pyrazolone Mannich bases possessing anti-inflammatory, analgesic, ulcerogenic effect and antimicrobial properties.

PubMed

Sivakumar, Kullampalayam Krishnasamy; Rajasekaran, Aiyalu; Senthilkumar, Palaniappan; Wattamwar, Prasad P

2014-07-01

In the present study, an efficient synthesis of some Mannich base of 5-methyl-2-[(2-oxo-2H-chromen-3-yl)carbonyl]-2,4-dihydro-3H-pyrazol-3-one (4a-j) have been described by using conventional and non-conventional (microwave) techniques. Microwave assisted reactions showed that require shorter reaction time and good yield. The newly synthesized compounds were screened for their anti-inflammatory, analgesic activity, antioxidant, and antibacterial effects were compared with standard drug. Among the compounds studied, compound (4f) showing nearly equipotent anti-inflammatory and analgesic activity than the standard drug (indomethacin), along with minimum ulcerogenic index. Compounds (4b and 4i) showing 1.06 times more active than ciprofloxacin against tested Gram-negative bacteria. Copyright © 2014 Elsevier Ltd. All rights reserved.

Green bio-oil extraction for oil crops

NASA Astrophysics Data System (ADS)

Zainab, H.; Nurfatirah, N.; Norfaezah, A.; Othman, H.

2016-06-01

The move towards a green bio-oil extraction technique is highlighted in this paper. The commonly practised organic solvent oil extraction technique could be replaced with a modified microwave extraction. Jatropha seeds (Jatropha curcas) were used to extract bio-oil. Clean samples were heated in an oven at 110 ° C for 24 hours to remove moisture content and ground to obtain particle size smaller than 500μm. Extraction was carried out at different extraction times 15 min, 30 min, 45 min, 60 min and 120 min to determine oil yield. The biooil yield obtained from microwave assisted extraction system at 90 minutes was 36% while that from soxhlet extraction for 6 hours was 42%. Bio-oil extracted using the microwave assisted extraction (MAE) system could enhance yield of bio-oil compared to soxhlet extraction. The MAE extraction system is rapid using only water as solvent which is a nonhazardous, environment-friendly technique compared to soxhlet extraction (SE) method using hexane as solvent. Thus, this is a green technique of bio-oil extraction using only water as extractant. Bio-oil extraction from the pyrolysis of empty fruit bunch (EFB), a biomass waste from oil palm crop, was enhanced using a biocatalyst derived from seashell waste. Oil yield for non-catalytic extraction was 43.8% while addition of seashell based biocatalyst was 44.6%. Oil yield for non-catalytic extraction was 43.8% while with addition of seashell-based biocatalyst was 44.6%. The pH of bio-oil increased from 3.5 to 4.3. The viscosity of bio-oil obtained by catalytic means increased from 20.5 to 37.8 cP. A rapid and environment friendly extraction technique is preferable to enhance bio-oil yield. The microwave assisted approach is a green, rapid and environmental friendly extraction technique for the production of bio-oil bearing crops.

Greener and rapid access to bio-active heterocycles: one-pot solvent-free synthesis of 1,3,4-oxadiazoles and 1,3,4-thiadiazoles

EPA Science Inventory

A novel one-pot solvent free synthesis of 1,3,4-oxadiazoles and 1,3,4-thiadiazoles by condensation of acid hydrazide and triethyl orthoalkanates under microwave irradiations is reported. This green protocol was catalyzed efficiently by solid supported Nafion®NR50 and phosphorus p...

Microwave-Assisted Synthesis of Nanomaterials and Nanocomposites

EPA Science Inventory

The aqueous preparation of nanoparticles using vitamins B1 and B2, and vitamin C which can function both as reducing and capping agents prompted us accomplished the bulk syntheses of Ag and Fe nanorods using polyethylene glycol (PEG) under microwave (MW) irradiation conditions; t...

Microwave assisted synthesis of cyclic carbonates from olefins with sodium bicarbonates as the C1 source.

PubMed

Yang, Xiaoqing; Wu, Jie; Mao, Xianwen; Jamison, Timothy F; Hatton, T Alan

2014-03-25

An effective transformation of alkenes into cyclic carbonates has been achieved using NaHCO3 as the C1 source in acetone-water under microwave heating, with selectivities and yields significantly surpassing those obtained using conventional heating.

DEXTRON TEMPLATED MICROWAVE-ASSISTED SYNTHESIS OF POROUS TITANIUM DIOXIDE

EPA Science Inventory

An alternative route to the preparation and formation of porous titania powders and carbon coated titania using microwave radiation is described. Inexpensive dextrose was chosen as capping agent or template in view of its high water solubility when compared to other sugar templat...

Microwave-Assisted Organic Synthesis Using Benign Reaction Medium and Reagents

EPA Science Inventory

Account of chemical reactions expedited by microwave (MW) exposure of neat reactants for the rapid one-pot assembly of heterocyclic compounds from in situ generated reactive intermediates via enamines or using hypervalent iodine reagents will be described that can be adapted for ...

Response surface methodology applied to the study of the microwave-assisted synthesis of quaternized chitosan.

PubMed

dos Santos, Danilo Martins; Bukzem, Andrea de Lacerda; Campana-Filho, Sérgio Paulo

2016-03-15

A quaternized derivative of chitosan, namely N-(2-hydroxy)-propyl-3-trimethylammonium chitosan chloride (QCh), was synthesized by reacting glycidyltrimethylammonium chloride (GTMAC) and chitosan (Ch) in acid medium under microwave irradiation. Full-factorial 2(3) central composite design and response surface methodology (RSM) were applied to evaluate the effects of molar ratio GTMAC/Ch, reaction time and temperature on the reaction yield, average degree of quaternization (DQ) and intrinsic viscosity ([η]) of QCh. The molar ratio GTMAC/Ch was the most important factor affecting the response variables and RSM results showed that highly substituted QCh (DQ = 71.1%) was produced at high yield (164%) when the reaction was carried out for 30min. at 85°C by using molar ratio GTMAC/Ch 6/1. Results showed that microwave-assisted synthesis is much faster (≤30min.) as compared to conventional reaction procedures (>4h) carried out in similar conditions except for the use of microwave irradiation. Copyright © 2015 Elsevier Ltd. All rights reserved.

A Rapid Microwave-Assisted Thermolysis Route to Highly Crystalline Carbon Nitrides for Efficient Hydrogen Generation.

PubMed

Guo, Yufei; Li, Jing; Yuan, Yupeng; Li, Lu; Zhang, Mingyi; Zhou, Chenyan; Lin, Zhiqun

2016-11-14

Highly crystalline graphitic carbon nitride (g-C 3 N 4 ) with decreased structural imperfections benefits from the suppression of electron-hole recombination, which enhances its hydrogen generation activity. However, producing such g-C 3 N 4 materials by conventional heating in an electric furnace has proven challenging. Herein, we report on the synthesis of high-quality g-C 3 N 4 with reduced structural defects by judiciously combining the implementation of melamine-cyanuric acid (MCA) supramolecular aggregates and microwave-assisted thermolysis. The g-C 3 N 4 material produced after optimizing the microwave reaction time can effectively generate H 2 under visible-light irradiation. The highest H 2 evolution rate achieved was 40.5 μmol h -1 , which is two times higher than that of a g-C 3 N 4 sample prepared by thermal polycondensation of the same supramolecular aggregates in an electric furnace. The microwave-assisted thermolysis strategy is simple, rapid, and robust, thereby providing a promising route for the synthesis of high-efficiency g-C 3 N 4 photocatalysts. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nanosize Fe x O y @SBA-3: A Comparative Study Between Conventional and Microwave Assisted Synthesis.

PubMed

Barik, Sunita; Badamali, Sushanta K; Sahoo, Sagarika; Behera, Nandakishor; Dapurkar, Sudhir E

2018-01-01

The present study is focussed on development of highly dispersed nanosize iron oxide (FexOy) particles within the uniform mesopore channels of SBA-3. Herein we report a comparative study between conventional incipient wetness and microwave assisted synthesis routes adopted to devise nanoparticles. The developed materials are characterised by following X-ray diffraction, high resolution transmission electron microscopy, proton induced X-ray emission, diffuse reflectance UV-visible spectroscopy, thermogravimetry and Fourier transform infrared spectroscopy. Mesoporous siliceous SBA-3 was prepared at room temperature to obtain samples with good crystallinity and ordered pore structure. Pore channels of SBA-3 were used as nanoreactor for developing iron oxide nanoparticles. Iron oxide nanoparticles developed under microwave activation showed uniform distribution within the SBA-3 structure along with retaining the orderness of the pore architecture. On the contrary, iron oxides developed under incipient wetness method followed by conventional heating resulted in agglomeration of nanoparticles along with significant loss in SBA-3 pore structure. Proton induced X-ray emission studies revealed the extremely high purity of the samples and almost thrice higher amount of iron oxide particles are encapsulated within the host by microwave assisted preparation as compared to incipient/conventional heating method.

Synthesis and swelling characteristics of chitosan and CMC grafted sodium acrylate-co-acrylamide using modified nanoclay and examining its efficacy for removal of dyes.

PubMed

Nagarpita, M V; Roy, Pratik; Shruthi, S B; Sailaja, R R N

2017-09-01

Chitosan/carboxy methyl chitosan (CMC) grafted sodium acrylate-co-acrylamide/nanoclay superabsorbent nanocomposites have been synthesized in this study by following conventional and microwave assisted grafting methods. Microwave assisted grafting method showed higher grafting yield with enhanced reaction rate. Effect of nanoclay on water adsorption and swelling behaviour of both the composites in acidic, neutral and alkaline medium has been studied. Results showed enhanced swelling rate and water adsorption of both composites after adding 5% of silane treated nanoclay. Dye adsorption capacity of both the composites has been investigated for crystal violet, napthol green and sunset yellow dyes. It was observed that addition of 5% nanoclay enhanced the dye adsorption in both the composites. Langmuir and Freundlich isotherm models have been used to explain the dye adsorption capabilities. The chitosan and CMC nanocomposites follow both the models with R 2 value more than 0.97. Both the composites showed enhanced dye adsorption with 5% nanoclay. Effect of pH on dye adsorption has also been studied in both the composites. Chitosan nanocomposites showed better performance in dye removal as compared to CMC nanocomposites. Copyright © 2017 Elsevier B.V. All rights reserved.

Microwave-assisted one-pot synthesis of ring-fused aminals under catalyst- and solvent-free conditions

EPA Science Inventory

Heterocyclic compounds hold a special place in drug discovery and variety of techniques such as combinatorial synthesis, parallel synthesis, and automated library production to increase the output of these entities has been developed. Although most of these techniques are rapid a...

A microwave assisted intramolecular-furan-Diels-Alder approach to 4-substituted indoles.

PubMed

Petronijevic, Filip; Timmons, Cody; Cuzzupe, Anthony; Wipf, Peter

2009-01-07

The key steps of a versatile new protocol for the convergent synthesis of 3,4-disubstituted indoles are the addition of an alpha-lithiated alkylaminofuran to a carbonyl compound, a microwave-accelerated intramolecular Diels-Alder cycloaddition and an in situ double aromatization reaction.

AN EFFICIENT AQUEOUS N-HETEROCYCLIZATION OF ANILINE DERIVATIVES: MICROWAVE-ASSISTED SYNTHESIS OF N-ARYL AZACYCLOALKANES

EPA Science Inventory

N-aryl azacycloalkanes, an important class of building blocks in natural product and pharmaceuticals, are synthesized via an efficient and simple eco-friendly protocol that involves double N-alkylation of aniline derivatives. The reaction is accelerated by exposure to microwaves ...

Microwave-assisted water extraction of green tea polyphenols.

PubMed

Nkhili, Ezzohra; Tomao, Valerie; El Hajji, Hakima; El Boustani, Es-Seddik; Chemat, Farid; Dangles, Olivier

2009-01-01

Green tea, a popular drink with beneficial health properties, is a rich source of specific flavanols (polyphenols). There is a special interest in the water extraction of green tea polyphenols since the composition of the corresponding extracts is expected to reflect the one of green tea infusions consumed worldwide. To develop a microwave-assisted water extraction (MWE) of green tea polyphenols. MWE of green tea polyphenols has been investigated as an alternative to water extraction under conventional heating (CWE). The experimental conditions were selected after consideration of both temperature and extraction time. The efficiency and selectivity of the process were determined in terms of extraction time, total phenolic content, chemical composition (HPLC-MS analysis) and antioxidant activity of the extracts. By MWE (80 degrees C, 30 min), the flavanol content of the extract reached 97.46 (+/- 0.08) mg of catechin equivalent/g of green tea extract, vs. only 83.06 (+/- 0.08) by CWE (80 degrees C, 45 min). In particular, the concentration of the most bioactive flavanol EGCG was 77.14 (+/- 0.26) mg of catechin equivalent/g of green tea extract obtained by MWE, vs 64.18 (+/- 0.26) mg/g by CWE. MWE appears more efficient than CWE at both 80 and 100 degrees C, particularly for the extraction of flavanols and hydroxycinnamic acids. Although MWE at 100 degrees C typically affords higher yields in total phenols, MWE at 80 degrees C appears more convenient for the extraction of the green tea-specific and chemically sensitive flavanols.

Ionic liquid-based ultrasonic/microwave-assisted extraction combined with UPLC-MS-MS for the determination of tannins in Galla chinensis.

PubMed

Lu, Chunxia; Wang, Hongxin; Lv, Wenping; Ma, Chaoyang; Lou, Zaixiang; Xie, Jun; Liu, Bo

2012-01-01

Ionic liquid was used as extraction solvents and applied to the extraction of tannins from Galla chinensis in the simultaneous ultrasonic- and microwave-assisted extraction (UMAE) technique. Several parameters of UMAE were optimised, and the results were compared with of the conventional extraction techniques. Under optimal conditions, the content of tannins was 630.2 ± 12.1 mg g⁻¹. Compared with the conventional heat-reflux extraction, maceration extraction, regular ultrasound- and microwave-assisted extraction, the proposed approach exhibited higher efficiency (11.7-22.0% enhanced) and shorter extraction time (from 6 h to 1 min). The tannins were then identified by ultraperformance liquid chromatography tandem mass spectrometry. This study suggests that ionic liquid-based UMAE is an efficient, rapid, simple and green sample preparation technique.

Rapid microwave assisted synthesis of YIn1-xMnxO3 blue pigments: Synthesis, microstructure and optical properties

NASA Astrophysics Data System (ADS)

Zhou, Yuncheng; Jiang, Peng; Kuang, Jianlei; Yang, Xueshan; Cao, Wenbin

2018-07-01

The YIn1-xMnxO3 (0.1 ≤x ≤ 0.5) blue pigment samples are successfully prepared through a sol-gel process followed by microwave assisted sintering process. All the samples are shown single phases in the X-ray diffraction results. In the morphology study from scanning electronic microscope, the samples are composed of loosely connected small particles. The oxidation state of Mn is confirmed to be 3 + from the results of X-ray photonelectronic scan. The optical properties are characterized by UV-Visible spectrum and UV-visible-NIR spectrum. The samples exhibit intense blue color and they show small absorption in infrared region.

Microwave assisted synthesis of amorphous magnesium phosphate nanospheres.

PubMed

Zhou, Huan; Luchini, Timothy J F; Bhaduri, Sarit B

2012-12-01

Magnesium phosphate (MgP) materials have been investigated in recent years for tissue engineering applications, attributed to their biocompatibility and biodegradability. This paper describes a novel microwave assisted approach to produce amorphous magnesium phosphate (AMP) in a nanospherical form from an aqueous solution containing Mg(2+) and HPO(4) (2-)/PO(4) (3-). Some synthesis parameters such as pH, Mg/P ratio, solution composition were studied and the mechanism of AMP precursors was also demonstrated. The as-produced AMP nanospheres were characterized and tested in vitro. The results proved these AMP nanospheres can self-assemble into mature MgP materials and support cell proliferation. It is expected such AMP has potential in biomedical applications.

A microwave assisted intramolecular-furan-Diels–Alder approach to 4-substituted indoles†

PubMed Central

Petronijevic, Filip; Timmons, Cody; Cuzzupe, Anthony; Wipf, Peter

2009-01-01

The key steps of a versatile new protocol for the convergent synthesis of 3,4-disubstituted indoles are the addition of an α-lithiated alkylaminofuran to a carbonyl compound, a microwave-accelerated intramolecular Diels–Alder cycloaddition and an in situ double aromatization reaction. PMID:19082013

Green synthesis and characterization of gold and silver nanoparticles using Mussaenda glabrata leaf extract and their environmental applications to dye degradation.

PubMed

Francis, Sijo; Joseph, Siby; Koshy, Ebey P; Mathew, Beena

2017-07-01

Plant-derived nanomaterials opened a green approach in solving the current environment issues. Present study focused on rapid microwave-assisted synthesis and applications of gold and silver nanoparticles mediated by aqueous leaf extract of Mussaenda glabrata. The synthesized nanoparticles were characterized by UV-vis, FT-IR, powder XRD, energy-dispersive X-ray spectroscopy (EDX), transmission electron (TEM), and atomic force microscopic techniques (AFM). FCC crystal structure of both nanoparticles was confirmed by peaks corresponding to (111), (200), (220), and (311) planes in XRD spectra and bright circular spots in SAED pattern. IC 50 values shown by gold and silver nanoparticles (44.1 ± 0.82 and 57.92 ± 1.33 μg/mL) reflected their high free radical scavenging potential. The synthesized gold and silver nanoparticles revealed their potency to inhibit pathogenic microorganisms Bacillus pumilus, Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, Aspergillus niger, and Penicillium chrysogenum. Anthropogenic pollutants rhodamine B and methyl orange were effectively degraded from aquatic environment and waste water sewages of dye industries using the prepared nanocatalysts. The catalytic capacities of the synthesized nanoparticles were also exploited in the reduction of 4-nitrophenol. Graphical abstract.

Microwave assisted facile hydrothermal synthesis and characterization of zinc oxide flower grown on graphene oxide sheets for enhanced photodegradation of dyes

NASA Astrophysics Data System (ADS)

Kashinath, L.; Namratha, K.; Byrappa, K.

2015-12-01

Microwave assisted hydrothermal process of synthesis of ZnO-GO nanocomposite by using ZnCl2 and NaOH as precursors is being reported first time. In this investigation, a novel route to study on synthesis, interaction, kinetics and mechanism of hybrid zinc oxide-graphene oxide (ZnO-GO) nanocomposite using microwave assisted facile hydrothermal method has been reported. The results shows that the ZnO-GO nanocomposite exhibits an enhancement and acts as stable photo-response degradation performance of Brilliant Yellow under the UV light radiation better than pure GO and ZnO nanoparticles. The microwave exposure played a vital role in the synthesis process, it facilitates with well define crystalline structure, porosity and fine morphology of ZnO/GO nanocomposite. Different molar concentrations of ZnO precursors doped to GO sheets were been synthesized, characterized and their photodegradation performances were investigated. The optical studies by UV-vis and Photo Luminescence shows an increase in band gap of nanocomposite, which added an advantage in photodegradation performance. The in situ flower like ZnO nano particles are were densely decorated and anchored on the surfaces of graphene oxide sheets which aids in the enhancement of the surface area, adsorption, mass transfer of dyes and evolution of oxygen species. The nanocomposite having high surface area and micro/mesoporous in nature. This structure and morphology supports significantly in increasing photo catalytic performance legitimate to the efficient photosensitized electron injection and repressed electron recombination due to electron transfer process with GO as electron collector and transporter dependent on the proportion of GO in ZnO/GO composite.

Microwave Assisted Synthesis of Py-Im Polyamides

PubMed Central

2012-01-01

Microwave synthesis was utilized to rapidly build Py-Im polyamides in high yields and purity using Boc-protection chemistry on Kaiser oxime resin. A representative polyamide targeting the 5′-WGWWCW-3′ (W = A or T) subset of the consensus Androgen and Glucocorticoid Response Elements was synthesized in 56% yield after 20 linear steps and HPLC purification. It was confirmed by Mosher amide derivatization of the polyamide that a chiral α-amino acid does not racemize after several additional coupling steps. PMID:22578091

A 4-(o-chlorophenyl)-2-aminothiazole: Microwave assisted synthesis, spectral, thermal, XRD and biological studies

NASA Astrophysics Data System (ADS)

Rajmane, S. V.; Ubale, V. P.; Lawand, A. S.; Nalawade, A. M.; Karale, N. N.; More, P. G.

2013-11-01

A 4-(o-chlorophenyl)-2-aminothiazole (CPAT) has been synthesized by reacting o-chloroacetophenone, iodine and thiourea under microwave irradiation as a green chemistry approach. The reactions proceed selectively and within a couple of minutes giving high yields of the products. The compound was characterized by elemental, spectral (UV-visible, IR, NMR and GC-MS), XRD and thermal analyses. The TG curve of the compound was analyzed to calculate various kinetic parameters (n, E, Z, ΔS and ΔG) by using Coats-Redfern (C.R.), MacCallum-Tanner (M.T.) and Horowitz-Metzger (H.M.) method. The compound was tested for the evaluation of antibacterial activity against B. subtilis and E. coli and antifungal activity against A. niger and C. albicans. The compound was evaluated for their in vitro nematicidal activity on plant parasitic nematode Meloidogyne javanica and molluscicidal activity on fresh water helminthiasis vector snail Lymnea auricularia. The compound is biologically active in very low concentration. X-ray diffraction study suggests a triclinic crystal system for the compound.

Microwave promoted simple, efficient and regioselective synthesis of trisubstituted imidazo[1,2-a]benzimidazoles on soluble support.

PubMed

Chen, Li-Hsun; Hsiao, Ya-Shan; Yellol, Gorakh S; Sun, Chung-Ming

2011-03-14

An efficient microwave-assisted and soluble polymer-supported synthesis of medicinally important imidazole-fused benzimidazoles has been developed. The protocol involves the rapid condensation of polymer-bound amino benzimidazoles with various α-bromoketones and subsequent in situ intramolecular cyclization under microwave irradiation resulting in a one pot synthesis of imidazole interlacing benzimidazole polymer conjugates. The condensed product was obtained with excellent regioselectivity. The biologically interesting imidazo[1,2-a]benzimidazoles was released from polymer support at ambient temperature. Diversity in the triheterocyclic nucleus was achieved by the different substitutions at its 2, 3, and 9 positions. The new protocol has the advantages of short reaction time, easy workup process, excellent yields, reduced environmental impact, wide substrate scope and convenient procedure.

Agile green process design for the intensified Kolbe-Schmitt synthesis by accompanying (simplified) life cycle assessment.

PubMed

Kressirer, Sabine; Kralisch, Dana; Stark, Annegret; Krtschil, Ulrich; Hessel, Volker

2013-05-21

In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe-Schmitt synthesis starting from resorcinol. Different CO₂ precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO₂, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave irradiation. Furthermore, the consideration of workup procedures was crucial for a holistic view on the environmental burdens.

Green synthesis of gold nanoparticles using extracts of Artocarpus Lakoocha fruit and its leaves, and Eriobotrya Japonica leaves

NASA Astrophysics Data System (ADS)

Sharma, Ankita; Dhiman, Naresh; Singh, Bhanu P.; Gathania, Arvind K.

2014-04-01

Gold nanoparticles (AuNPs) synthesis is demonstrated successfully using fresh young leaves of Artocarpus Lakoocha (A. Lakoocha), fruit pulp of A. Lakoocha and loquat (Eriobotrya Japonica) leaves. We have also compared green synthesis with chemical assisted tri-n-octyl-phosphine (TOP) stabilized gold nanoparticles. Samples were characterized with transmission electron microscopy (TEM), Fourier transform infrared spectroscopy and UV-Visible spectroscopy. TEM images have shown that the average size of the particles is 15.06, 36.8 and 25.08 nm for A. Lakoocha fruits, A. Lakoocha leaves and loquat leaves assisted gold nanoparticles, respectively. Hydrogen tetrachloroaurate is reduced and AuNPs are stabilized by phenols, hydroxyls and carboxyls groups such as terpenoids, flavonoids, tannins etc, present in young leaves and fruit extracts. It was observed that green synthesis using botanical extracts is a cost effective and non- toxic way for nanoparticle preparation.

Development of microwave assisted spectrophotometric method for the determination of glucose

NASA Astrophysics Data System (ADS)

Ali, Asif; Hussain, Zahid; Arain, Muhammad Balal; Shah, Nasrullah; Khan, Khalid Mohammad; Gulab, Hussain; Zada, Amir

2016-01-01

A spectrophotometric method was developed based on the microwave assisted synthesis of Maillard product. Various conditions of the reaction were optimized by varying the relative concentration of the reagents, operating temperature and volume of solutions used in the reaction in the microwave synthesizer. The absorbance of the microwave synthesized Maillard product was measured in the range of 360-740 nm using UV-Visible spectrophotometer. Based on the maximum absorbance, 370 nm was selected as the optimum wave length for further studies. The LOD and LOQ of glucose was found 3.08 μg mL- 1 and 9.33 μg mL- 1 with standard deviation of ± 0.05. The developed method was also applicable to urine sample.

Green synthesis of silver nanoparticles in xylan solution via Tollens reaction and their detection for Hg(2+).

PubMed

Luo, Yuqiong; Shen, Suqin; Luo, Jiwen; Wang, Xiaoying; Sun, Runcang

2015-01-14

This work reported a facile and green method to prepare highly stable and uniformly distributed Ag nanoparticles (AgNPs), in which a biopolymer xylan was used as the stabilizing and reducing agent via the Tollens reaction under microwave irradiation. Different variables were evaluated to optimize the reaction conditions. Complete characterization was performed using UV-Vis, XRD, TEM, size distribution analysis and XPS. The results revealed that AgNPs were well dispersed with diameters of 20-35 nm due to the packing of xylan. The optimal conditions were as follows: microwave irradiation temperature was 60-70 °C, microwave power was 800 W, microwave time was 30 min, the ratio of xylan to AgNO3 was 50 mg: 0.13 mmol, and ammonia concentration was 2%. In addition, the AgNPs were collected via high-speed centrifugal separation, and the supernatant was tested by HPAEC, GPC, FT-IR, and NMR. By comparing the structure of xylan before and after the reaction, the reaction mechanism was discussed. It was noted that the xylan-AgNPs composites showed high selectivity and sensitivity for Hg(2+) detection. The other 15 metal ions used had no obvious effect on the detection of Hg(2+), and the limit of detection (LOD) was 4.6 nM, which is lower than the allowed maximum level of 30 nM for drinking water by WHO. In addition, the xylan-AgNPs composites can be applied for Hg(2+) detection in real water samples. This study provides a novel way for the high-value utilization of a rich biomass resource, and a green method for the synthesis of AgNPs for the selective and sensitive detection of harmful heavy metals.

Microwave-assisted synthesis of transition metal phosphide

DOEpatents

Viswanathan, Tito

2014-12-30

A method of synthesizing transition metal phosphide. In one embodiment, the method has the steps of preparing a transition metal lignosulfonate, mixing the transition metal lignosulfonate with phosphoric acid to form a mixture, and subjecting the mixture to a microwave radiation for a duration of time effective to obtain a transition metal phosphide.

MICROWAVE-ASSISTED SYNTHESIS OF CROSSLINKED POLY(VINYL ALCOHOL) NANOCOMPOSITES COMPRISING SINGLE-WALLED CARBON NANOTUBES, MULTI-WALLED CARBON NANOTUBES AND BUCKMINSTERFULLERENE

EPA Science Inventory

We report a facile method to accomplish cross-linking reaction of poly (vinyl alcohol) (PVA) with single-wall carbon nanotubes (SWNT), multi-wall carbon nanotubes (MWNT), and Buckminsterfullerene (C-60) using microwave (MW) irradiation. Nanocomposites of PVA cross-linked with SW...

MICROWAVE-ASSISTED SHAPE CONTROLLED BULK SYNTHESIS OF AG AND FE NANORODS IN POLY (ETHYLENE GLYCOL) SOLUTIONS

EPA Science Inventory

Bulk syntheses of silver (Ag) and iron (Fe) nanorods using poly (ethylene glycol), PEG, under microwave irradiation (MW) conditions are reported. Favorable conditions to make Ag nanorods were established and can be extended to make Fe nanorods with uniform size and shape. The nan...

Student-Driven Design of Peptide Mimetics: Microwave-Assisted Synthesis of Peptoid Oligomers

ERIC Educational Resources Information Center

Pohl, Nicola L. B.; Kirshenbaum, Kent; Yoo, Barney; Schulz, Nathan; Zea, Corbin J.; Streff, Jennifer M.; Schwarz, Kimberly L.

2011-01-01

An experiment for the undergraduate organic laboratory is described in which peptide mimetic oligomers called "peptoids" are built stepwise on a solid-phase resin. Students employ two modern strategies to facilitate rapid multistep syntheses: solid-phase techniques to obviate the need for intermediate purifications and microwave irradiation to…

PETI-298 Prepared by Microwave Synthesis: Neat Resin and Composite Properties

NASA Technical Reports Server (NTRS)

Smith, Joseph G.; Connell, John W.; Li, Chao-Jun; Wu, Wei; Criss, Jim M., Jr.

2004-01-01

PETI-298 is a high temperature/high performance matrix resin that is processable into composites by resin transfer molding (RTM), resin infusion and vacuum assisted RTM techniques. It is typically synthesized in a polar aprotic solvent from the reaction of an aromatic anhydride and a combination of diamines and endcapped with phenylethynylphthalic anhydride. Microwave synthesis of PETI-298 was investigated as a means to eliminate solvent and decrease reaction time. The monomers were manually mixed and placed in a microwave oven for various times to determine optimum reaction conditions. The synthetic process was subsequently scaled-up to 330g. Three batches were synthesized and combined to give 1 kg of material that was characterized for thermal and rheological properties and compared to PETI-298 prepared by the classic solution based synthetic method. The microwave synthesized PETI-298 was subsequently used to fabricate flat laminates on T650 carbon fabric by RTM. The composite panels were analyzed and mechanical properties determined and compared with those fabricated from PETI-298 prepared by the classic solution method. The microwave synthesis process and characterization of neat resin and carbon fiber reinforced composites fabricated by RTM will be presented. KEY WORDS: Resin Transfer Molding, High Temperature Polymers, Phenylethynyl Terminated Imides, Microwave Synthesis

Synthesis of C-glycosyl-bis-1,2,3-triazole derivatives from 3,4,6-tri-O-acetyl-D-glucal.

PubMed

Shamim, Anwar; Souza, Frederico B; Trossini, Gustavo H G; Gatti, Fernando M; Stefani, Hélio A

2015-08-01

We have developed an efficient, CuI-catalyzed, microwave-assisted method for the synthesis of bis-1,2,3-triazole derivatives starting from a 3,4,6-tri-O-acetyl-D-glucal-derived mesylate. This mesylate was obtained from 3,4,6-tri-O-acetyl-D-glucal through C-glycosidation, deprotection of acetate groups to alcohols, and selective mesylation of the primary alcohol. This mesylate moiety was then converted to an azide through a microwave-assisted method with good yield. The azide, once synthesized, was then treated with different terminal alkynes in the presence of CuI to synthesize various bis-triazoles in high yields and short reaction times.

Pb(core)/ZnO(shell) nanowires obtained by microwave-assisted method

PubMed Central

2011-01-01

In this study, Pb-filled ZnO nanowires [Pb(core)/ZnO(shell)] were synthesized by a simple and novel one-step vapor transport and condensation method by microwave-assisted decomposition of zinc ferrite. The synthesis was performed using a conventional oven at 1000 W and 5 min of treatment. After synthesis, a spongy white cotton-like material was obtained in the condensation zone of the reaction system. HRTEM analysis revealed that product consists of a Pb-(core) with (fcc) cubic structure that preferentially grows in the [111] direction and a hexagonal wurtzite ZnO-(Shell) that grows in the [001] direction. Nanowire length was more than 5 μm and a statistical analysis determined that the shell and core diameters were 21.00 ± 3.00 and 4.00 ± 1.00 nm, respectively. Experimental, structural details, and synthesis mechanism are discussed in this study. PMID:21985637

Microwave assisted green synthesis and characterizations of noble metal nanoparticles and their roles as catalysts in organic reduction reactions and anticancer agent

NASA Astrophysics Data System (ADS)

Francis, Sijo; Koshy, Ebey P.; Mathew, Beena

2018-04-01

Nanomaterials are interesting chemicals that uncover the explorations and expectations of decades. The report suggests environmentally benevolent and easy route for the synthesis of noble metal nanoparticles. Personnel, laboratory and ecological benefits of the synthesized nanoparticles are demonstrated herein. The aqueous extract from the leaves of Litchi chinensis Sonn is performed as the alternative reducing agent. The microwave activated silver and gold nanoparticles have spherical geometries with crystalline essence. X-ray diffraction technique witnessed the face centered cubic lattice for the nano silver and gold particles that preferentially oriented towards the (111) plane. The reduction of nitro anilines is performed to elucidate the heterogeneous catalytic power of the nanoparticles. The nano catalyst is a potential candidate to meet the challenges raised from organic pollutant dye that cause environmental contamination. The chemical stability, low-cost factor and plant based origin of the new nanoparticles are admired. The multitudes of health hazards especially human carcinoma can be effectively inhibited by the silver and gold nanoparticles. The leaf extract, silver and gold nanoparticles showed IC50 values 66.56 ± 0.80, 23.55 ± 0.43 and 20.38 ± 0.41 μg ml‑1 respectively against the human lung adenocarcinoma cell lines A549 determined using the MTT dye conversion assay.

Comparison of heat and mass transfer of different microwave-assisted extraction methods of essential oil from Citrus limon (Lisbon variety) peel.

PubMed

Golmakani, Mohammad-Taghi; Moayyedi, Mahsa

2015-11-01

Dried and fresh peels of Citrus limon were subjected to microwave-assisted hydrodistillation (MAHD) and solvent-free microwave extraction (SFME), respectively. A comparison was made between MAHD and SFME with the conventional hydrodistillation (HD) method in terms of extraction kinetic, chemical composition, and antioxidant activity. Higher yield results from higher extraction rates by microwaves and could be due to a synergy of two transfer phenomena: mass and heat acting in the same way. Gas chromatography/mass spectrometry (GC/MS) analysis did not indicate any noticeable differences between the constituents of essential oils obtained by MAHD and SFME, in comparison with HD. Antioxidant analysis of the extracted essential oils indicated that microwave irradiation did not have adverse effects on the radical scavenging activity of the extracted essential oils. The results of this study suggest that MAHD and SFME can be termed as green technologies because of their less energy requirements per ml of essential oil extraction.

Enabling technologies and green processes in cyclodextrin chemistry.

PubMed

Cravotto, Giancarlo; Caporaso, Marina; Jicsinszky, Laszlo; Martina, Katia

2016-01-01

The design of efficient synthetic green strategies for the selective modification of cyclodextrins (CDs) is still a challenging task. Outstanding results have been achieved in recent years by means of so-called enabling technologies, such as microwaves, ultrasound and ball mills, that have become irreplaceable tools in the synthesis of CD derivatives. Several examples of sonochemical selective modification of native α-, β- and γ-CDs have been reported including heterogeneous phase Pd- and Cu-catalysed hydrogenations and couplings. Microwave irradiation has emerged as the technique of choice for the production of highly substituted CD derivatives, CD grafted materials and polymers. Mechanochemical methods have successfully furnished greener, solvent-free syntheses and efficient complexation, while flow microreactors may well improve the repeatability and optimization of critical synthetic protocols.

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

Ding, Ling; Song, Yu, E-mail: songyu@dlpu.edu.cn; Yang, Wei

Open-framework zinc phosphates were synthesized by microwave-assisted technique, and it was shown that the morphology of as-prepared materials could be easily tailored by changing synthesis temperature, reaction time and pH value. During the synthesis, when the reaction temperature increases from 130 °C to 220 °C, the products transformed from hexagonal prisms to polyhedron along with the disappearance of the hexagonal prisms vertical plane. Simultaneously, both the reaction time and pH value could promote the nucleation and growth of crystal particles. More interestingly, the target products with different morphologies could be obtained by varying the usage of NaOH or NH{sub 3}·H{submore » 2}O at 130 °C during the microwave synthesis process. - Graphical abstract: Zinc phosphates with variable morphologies can be obtained by simply tuning the microwave-heating temperatures. Display Omitted - Highlights: • Synthesis of open-framework Zn{sub 4} (H{sub 3}O) (NH{sub 4}){sub 3}(PO{sub 4}){sub 4} compounds employing microwave technique. • Dependence of morphology on the reaction conditions. • Morphology transformation from hexagonal prisms to polyhedron was observed.« less

Design of guanidinium ionic liquid based microwave-assisted extraction for the efficient extraction of Praeruptorin A from Radix peucedani.

PubMed

Ding, Xueqin; Li, Li; Wang, Yuzhi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

2014-12-01

A series of novel tetramethylguanidinium ionic liquids and hexaalkylguanidinium ionic liquids have been synthesized based on 1,1,3,3-tetramethylguanidine. The structures of the ionic liquids were confirmed by (1)H NMR spectroscopy and mass spectrometry. A green guanidinium ionic liquid based microwave-assisted extraction method has been developed with these guanidinium ionic liquids for the effective extraction of Praeruptorin A from Radix peucedani. After extraction, reversed-phase high-performance liquid chromatography with UV detection was employed for the analysis of Praeruptorin A. Several significant operating parameters were systematically optimized by single-factor and L9 (3(4)) orthogonal array experiments. The amount of Praeruptorin A extracted by [1,1,3,3-tetramethylguanidine]CH2CH(OH)COOH is the highest, reaching 11.05 ± 0.13 mg/g. Guanidinium ionic liquid based microwave-assisted extraction presents unique advantages in Praeruptorin A extraction compared with guanidinium ionic liquid based maceration extraction, guanidinium ionic liquid based heat reflux extraction and guanidinium ionic liquid based ultrasound-assisted extraction. The precision, stability, and repeatability of the process were investigated. The mechanisms of guanidinium ionic liquid based microwave-assisted extraction were researched by scanning electron microscopy and IR spectroscopy. All the results show that guanidinium ionic liquid based microwave-assisted extraction has a huge potential in the extraction of bioactive compounds from complex samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

RISK REDUCTION VIA GREENER SYNTHESIS OF NOBLE METAL NANOSTRUCTURES AND NANOCOMPOSITES

EPA Science Inventory

Aqueous preparation of nanoparticles using vitamins B2 and C which can function both as reducing and capping agents are described. Bulk and shape-controlled synthesis of noble nanostructures via microwave (MW)-assisted spontaneous reduction of noble metal salts using a-D-glucose,...

Eco-friendly Synthesis of Organics and Nanomaterials ...

EPA Pesticide Factsheets

The presentation summarizes our recent activity in chemical synthesis involving benign alternatives, such as the use of supported reagents, and greener reaction medium in aqueous or solvent-free conditions.1 The synthesis of heterocyclic compounds, coupling reactions, and a variety of name reactions2 are the primary beneficiaries as exemplified by the synthesis of N-aryl azacycloalkanes, isoindoles, and dihydropyrazoles, 1,3,4-oxadiazoles, 1,3,4-thiadiazoles, 1,3-dioxanes, pyrazoles, catalyzed by basic water or polystyrene sulfonic acid (PSSA) in conjunction with microwave (MW) irradiation.2 Vitamins B1, B2, C, and tea and wine polyphenols which function both as reducing and capping agents, provide extremely simple, one-pot, green synthetic methods to bulk quantities of nanomaterials in water.3a Shape-controlled synthesis of noble nanostructures via MW-assisted spontaneous reduction of noble metal salts using sugars will be presented.3b A general method has been developed for the cross-linking reaction of poly (vinyl alcohol) (PVA) with metallic systems; bimetallic systems,3c and SWNT, MWNT, and C-60.3d The strategy is extended to the formation of biodegradable carboxymethylcellulose (CMC) composite films with noble nanometals;3e such metal decoration and alignment of carbon nanotubes in CMC is possible using MW approach3f which also enables the shape-controlled bulk synthesis of Ag and Fe nanorods in poly (ethylene glycol).3g MW hydrothermal process delivers m

CATALYST-FREE REACTIONS UNDER SOLVENT-FEE CONDITIONS: MICROWAVE-ASSISTED SYNTHESIS OF HETEROCYCLIC HYDRAZONES BELOW THE MELTING POINT OF NEAT REACTANTS

EPA Science Inventory

The reaction of neat 5- or 8-oxobenzopyran-2(1H)-ones with a variety of aromatic and heteroaromatic hydrazines are remarkable accelerated upon irradiation in a household microwave oven in the absence of any catalyst, solid support or solvent thus providing an environmentally frie...

Simple Microwave-Assisted Synthesis of Amphiphilic Carbon Quantum Dots from A3/B2 Polyamidation Monomer Set.

PubMed

Choi, Yujin; Jo, Seongho; Chae, Ari; Kim, Young Kwang; Park, Jeong Eun; Lim, Donggun; Park, Sung Young; In, Insik

2017-08-23

Highly fluorescent and amphiphilic carbon quantum dots (CQDs) were prepared by microwave-assisted pyrolysis of citric acid and 4,7,10-trioxa-1,13-tridecanediamine (TTDDA), which functioned as an A 3 and B 2 polyamidation type monomer set. Gram quantities of fluorescent CQDs were easily obtained within 5 min of microwave heating using a household microwave oven. Because of the dual role of TTDDA, both as a constituting monomer and as a surface passivation agent, TTDDA-based CQDs showed a high fluorescence quantum yield of 29% and amphiphilic solubility in various polar and nonpolar solvents. These properties enable the wide application of TTDDA-based CQDs as nontoxic bioimaging agents, nanofillers for polymer composites, and down-converting layers for enhancing the efficiency of Si solar cells.

Copper-granule-catalyzed microwave-assisted click synthesis of polyphenol dendrimers.

PubMed

Lee, Choon Young; Held, Rich; Sharma, Ajit; Baral, Rom; Nanah, Cyprien; Dumas, Dan; Jenkins, Shannon; Upadhaya, Samik; Du, Wenjun

2013-11-15

Syringaldehyde- and vanillin-based antioxidant dendrimers were synthesized via microwave-assisted alkyne-azide 1,3-dipolar cycloaddition using copper granules as a catalyst. The use of Cu(I) as a catalyst resulted in copper contaminated dendrimers. To produce copper-free antioxidant dendrimers for biological applications, Cu(I) was substituted with copper granules. Copper granules were ineffective at both room temperature and under reflux conditions (<5% yield). However, they were an excellent catalyst when dendrimer synthesis was performed under microwave irradiation, giving yields up to 94% within 8 h. ICP-mass analysis of the antioxidant dendrimers obtained with this method showed virtually no copper contamination (9 ppm), which was the same as the background level. The synthesized antioxidants, free from copper contamination, demonstrated potent radical scavenging with IC50 values of less than 3 μM in the 2,2-diphenyl-1-picrylhydrazyl (DPPH) assay. In comparison, dendrimers synthesized from Cu(I)-catalyzed click chemistry showed a high level of copper contamination (4800 ppm) and no detectable antioxidant activity.

Microwave-Assisted Synthesis of Goethite Nanoparticles Used for Removal of Cr(VI) from Aqueous Solution

PubMed Central

Kynicky, Jindrich; Adam, Vojtech

2017-01-01

The microwave-assisted synthesis of goethite nanoparticles has been studied. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential thermal analysis (DTA) and Brunauer–Emmett–Teller (BET) method. Goethite rod-like nanoparticles have been successfully synthesized in 10 min of microwave treating at 100 °C. Particle size is in the range from 30 to 60 nm in width and from 200 to 350 nm in length. BET analysis indicated that the surface area of the product is 158.31 m2g−1. The feasibility of Cr(VI) removal fromaqueous solution depends on the pH of the solution and contact time. The maximum adsorptionis reached at pH 4.0 and 540 min of contact time. The adsorption kinetics was analyzedby the pseudo-first- and second-order models and the results reveal that the adsorption process obeys the pseudo-second-order model. The adsorption data were fitted well with the Langmuir adsorption isotherm. PMID:28773142

Microwave assisted synthesis and structure-activity relationship of 4-hydroxy-N'-[1-phenylethylidene]-2H/2-methyl-1,2-benzothiazine-3-carbohydrazide 1,1-dioxides as anti-microbial agents.

PubMed

Ahmad, Naveed; Zia-ur-Rehman, Muhammad; Siddiqui, Hamid Latif; Ullah, Muhammad Fasih; Parvez, Masood

2011-06-01

A series of 4-hydroxy-N'-[1-phenylethylidene]-2H/2-methyl, 1,2-benzothiazine-3-carbohydrazide 1,1-dioxides was synthesized from commercially available sodium saccharin. Base catalyzed ring expansion of methyl (1,1-dioxido-3-oxo-1,2-benzisothiazol-2(3H)-yl)acetate followed by ultrasound mediated hydrazinolysis and subsequent reaction with 1-phenylethanones under the influence of microwaves yielded the title compounds. Besides, microwave assisted synthesis of 1,4-dihydropyrazolo[4,3-c][1,2]benzothiazin-3-ol 5,5-dioxide and 4-methyl-1,4-dihydropyrazolo[4,3-c][1,2]benzothiazin-3-ol 5,5-dioxide is also discussed. Most of the synthesized compounds were found to possess moderate to significant anti-microbial (anti-bacterial and anti-fungal) activities. It is found that compounds with greater lipophilicity (N-methyl analogues) possessed higher anti-bacterial activities. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

Synthesis of unnatural amino acids via microwave-assisted regio-selective one-pot multi-component reactions of sulfamidates

EPA Science Inventory

Synthesis of triazole-based unnatural amino acids, triazole bisaminoacids and β-amino triazole has been described via stereo and regioselective one-pot multi-component reaction of sulfamidates, sodium azide, and alkynes under MW irradiation conditions. The developed method is app...

Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

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

Sciancalepore, Corrado, E-mail: corrado.sciancalepore@unimore.it; Bondioli, Federica; INSTM Consortium, Via G. Giusti 9, 51121 Firenze

2015-02-15

An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals wasmore » followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe{sub 3}O{sub 4} nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis.« less

Effect of deposition parameters on the structural properties of ZnO nanopowders prepared by microwave-assisted hydrothermal synthesis.

PubMed

Caglar, Yasemin; Gorgun, Kamuran; Aksoy, Seval

2015-03-05

ZnO nanopowders were synthesized via microwave-assisted hydrothermal method at different deposition (microwave irradiation) times and pH values. The effects of pH and deposition (microwave irradiation) time on the crystalline structure and orientation of the ZnO nanopowders have been investigated by X-ray diffraction (XRD) study. XRD observations showed that the crystalline quality of ZnO nanopowders increased with increasing pH value. The crystallite size and texture coefficient values of ZnO nanopowders were calculated. The structural quality of ZnO nanopowder was improved by deposition parameters. Field emission scanning electron microscope (FESEM) was used to analyze the surface morphology of the ZnO nanopowders. Microwave irradiation time and pH value showed a significant effect on the surface morphology. Copyright © 2014 Elsevier B.V. All rights reserved.

The microwave-assisted ionic liquid nanocomposite synthesis: platinum nanoparticles on graphene and the application on hydrogenation of styrene

PubMed Central

2013-01-01

The microwave-assisted nanocomposite synthesis of metal nanoparticles on graphene or graphite oxide was introduced in this research. With microwave assistance, the Pt nanoparticles on graphene/graphite oxide were successfully produced in the ionic liquid of 2-hydroxyethanaminium formate [HOCH2CH2NH3][HCO2]. On graphene/graphite oxide, the sizes of Pt nanoparticles were about 5 to 30 nm from transmitted electron microscopy (TEM) results. The crystalline Pt structures were examined by X-ray diffraction (XRD). Since hydrogenation of styrene is one of the important well-known chemical reactions, herein, we demonstrated then the catalytic hydrogenation capability of the Pt nanoparticles on graphene/graphite oxide for the nanocomposite to compare with that of the commercial catalysts (Pt/C and Pd/C, 10 wt.% metal catalysts on activated carbon from Strem chemicals, Inc.). The conversions with the Pt nanoparticles on graphene are >99% from styrene to ethyl benzene at 100°C and under 140 psi H2 atmosphere. However, ethyl cyclohexane could be found as a side product at 100°C and under 1,520 psi H2 atmosphere utilizing the same nanocomposite catalyst. PMID:24103100

Microwave-assisted preparation of carbon nanofiber-functionalized graphite felts as electrodes for polymer-based redox-flow batteries

NASA Astrophysics Data System (ADS)

Schwenke, A. M.; Janoschka, T.; Stolze, C.; Martin, N.; Hoeppener, S.; Schubert, U. S.

2016-12-01

A simple and fast microwave-assisted protocol to functionalize commercially available graphite felts (GFs) with carbon nanofibers (CNFs) for the application as electrode materials in redox-flow batteries (RFB) is demonstrated. As catalyst for the CNF synthesis nickel acetate is applied and ethanol serves as the carbon source. By the in-situ growth of CNFs, the active surface of the electrodes is increased by a factor of 50, which is determined by the electrochemical double layer capacities of the obtained materials. Furthermore, the morphology of the CNF-coating is investigated by scanning electron microscopy. Subsequently, the functionalized electrodes are applied in a polymer-based redox-flow battery (pRFB) using a TEMPO- and a viologen polymer as active materials. Due to the increased surface area as compared to an untreated graphite felt electrode, the current rating is improved by about 45% at 80 mA cm-2 and, furthermore, a decrease in overpotentials is observed. Thus, using this microwave-assisted synthesis approach, CNF-functionalized composite electrodes are prepared with a very simple protocol suitable for real life applications and an improvement of the overall performance of the polymer-based redox-flow battery is demonstrated.

The synthesis of α-aryl-α-aminophosphonates and α-aryl-α-aminophosphine oxides by the microwave-assisted Pudovik reaction

PubMed Central

Tajti, Ádám; Ádám, Anna; Csontos, István; Karaghiosoff, Konstantin; Czugler, Mátyás; Ábrányi-Balogh, Péter

2017-01-01

A family of α-aryl-α-aminophosphonates and α-aryl-α-aminophosphine oxides was synthesized by the microwave-assisted solvent-free addition of dialkyl phosphites and diphenylphosphine oxide, respectively, to imines formed from benzaldehyde derivatives and primary amines. After optimization, the reactivity was mapped, and the fine mechanism was evaluated by DFT calculations. Two α-aminophosphonates were subjected to an X-ray study revealing a racemic dimer formation made through a N–H···O=P intermolecular hydrogen bridges pair. PMID:28179951

Simultaneous phase and morphology controllable synthesis of copper selenide films by microwave-assisted nonaqueous approach

NASA Astrophysics Data System (ADS)

Li, Jing; Fa, Wenjun; Li, Yasi; Zhao, Hongxiao; Gao, Yuanhao; Zheng, Zhi

2013-02-01

Copper selenide films with different phase and morphology were synthesized on copper substrate through controlling reaction solvent by microwave-assisted nonaqueous approach. The films were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The result showed that the pure films could be obtained using cyclohexyl alcohol or benzyl alcohol as solvent. The cubic Cu2-xSe dendrites were synthesized in cyclohexyl alcohol reaction system and hexagonal CuSe flaky crystals were obtained with benzyl alcohol as solvent.

Microwave-assisted rapid synthesis of methyl 2,4,5-trimethoxyphenylpropionate, a metabolite of Cordia alliodora.

PubMed

Sinha, A K; Joshi, B P; Sharma, A; Kumar, J K; Kaul, V K

2003-12-01

Microwave assisted condensation of asaronaldehyde (2) with malonic acid in piperidine-AcOH provides 2,4,5-trimethoxycinnamic acid (3) in 87% yield within 4 min, which upon further reduction with PdCl2- HCOOH-aq. NaOH gives 3-(2,4,5-trimethoxy)phenyl propionic acid (4) in 88% yield within 3 min. Esterification of 4 with MeOH-H+ gives methyl 2,4,5-trimethoxyphenylpropionate (1), a metabolite of Cordia alliodora, in 94% yield within 3 min (overall 69% yield).

Eco-Contribution for the Production of N-Arylnitrones: Solvent-Free and Assisted by Microwaves

PubMed Central

Reyes, Leonor; Corona, Sandra; Arroyo, Gabriel; Delgado, Francisco; Miranda, René

2010-01-01

A simple green approach for the production of benzylideneaniline oxides is offered. This contribution was performed via the condensation of phenylhydroxylamine with several aryl aldehydes, in the absence of both catalyst and solvent, and using microwave irradiation as the activating reaction mode. In addition, good yields of the products were achieved in a short time. It is also worth noting that the work-up procedure is simple and the products do not require further purification. Finally, an interesting comparison without the use of microwave irradiation is also discussed. PMID:20640169

Microwave-assisted synthesis of highly luminescent N- and S-co-doped carbon dots as a ratiometric fluorescent probe for levofloxacin.

PubMed

Li, Huiyu; Xu, Yuan; Ding, Jie; Zhao, Li; Zhou, Tianyu; Ding, Hong; Chen, Yanhua; Ding, Lan

2018-01-10

Uniform N- and S-co-doped carbon dots (NSCDs) with fluorescence quantum yields of up to 64% were synthesized via a one-step microwave-assisted method. Ammonium citrate and L-cysteine act as precursors, and synthesis is completed in 2.5 min using a 750 W microwave oven to give a 62% yield. The NSCDs show bright blue fluorescence (with excitation/emission peaks at 353/426 nm) and have narrow size distribution. On exposure to levofloxacin (LEV), the emission maximum shifts to 499 nm. This effect was used to design ratiometric (2-wavelength) assays for LEV. The fluorometric method (based on measurement of the fluorescence intensity ratio at 499 and 426 nm) has a detection limit of 5.1 μg·L -1 (3σ/k) and a linear range that extends from 0.01 to 70 mg·L -1 . The method was applied to the determination of LEV in three kinds of spiked water samples and has recoveries in the range from 98.6 to 106.8%. The fluorescent probe described here is highly selective and sensitive. Graphical Abstract Highly luminescent N- and S-co-doped carbon dots were synthesized using AC (ammonium citrate) and Cys (L-cysteine) by microwave-assisted method, and were applied to the visual and ratiometric fluorescence determination of LEV (levofloxacin).

Microwave-assisted intramolecular dehydrogenative Diels-Alder reactions for the synthesis of functionalized naphthalenes/solvatochromic dyes.

PubMed

Kocsis, Laura S; Benedetti, Erica; Brummond, Kay M

2013-04-01

Functionalized naphthalenes have applications in a variety of research fields ranging from the synthesis of natural or biologically active molecules to the preparation of new organic dyes. Although numerous strategies have been reported to access naphthalene scaffolds, many procedures still present limitations in terms of incorporating functionality, which in turn narrows the range of available substrates. The development of versatile methods for direct access to substituted naphthalenes is therefore highly desirable. The Diels-Alder (DA) cycloaddition reaction is a powerful and attractive method for the formation of saturated and unsaturated ring systems from readily available starting materials. A new microwave-assisted intramolecular dehydrogenative DA reaction of styrenyl derivatives described herein generates a variety of functionalized cyclopenta[b]naphthalenes that could not be prepared using existing synthetic methods. When compared to conventional heating, microwave irradiation accelerates reaction rates, enhances yields, and limits the formation of undesired byproducts. The utility of this protocol is further demonstrated by the conversion of a DA cycloadduct into a novel solvatochromic fluorescent dye via a Buchwald-Hartwig palladium-catalyzed cross-coupling reaction. Fluorescence spectroscopy, as an informative and sensitive analytical technique, plays a key role in research fields including environmental science, medicine, pharmacology, and cellular biology. Access to a variety of new organic fluorophores provided by the microwave-assisted dehydrogenative DA reaction allows for further advancement in these fields.

Microwave-assisted Intramolecular Dehydrogenative Diels-Alder Reactions for the Synthesis of Functionalized Naphthalenes/Solvatochromic Dyes

PubMed Central

Kocsis, Laura S.; Benedetti, Erica; Brummond, Kay M.

2013-01-01

Functionalized naphthalenes have applications in a variety of research fields ranging from the synthesis of natural or biologically active molecules to the preparation of new organic dyes. Although numerous strategies have been reported to access naphthalene scaffolds, many procedures still present limitations in terms of incorporating functionality, which in turn narrows the range of available substrates. The development of versatile methods for direct access to substituted naphthalenes is therefore highly desirable. The Diels-Alder (DA) cycloaddition reaction is a powerful and attractive method for the formation of saturated and unsaturated ring systems from readily available starting materials. A new microwave-assisted intramolecular dehydrogenative DA reaction of styrenyl derivatives described herein generates a variety of functionalized cyclopenta[b]naphthalenes that could not be prepared using existing synthetic methods. When compared to conventional heating, microwave irradiation accelerates reaction rates, enhances yields, and limits the formation of undesired byproducts. The utility of this protocol is further demonstrated by the conversion of a DA cycloadduct into a novel solvatochromic fluorescent dye via a Buchwald-Hartwig palladium-catalyzed cross-coupling reaction. Fluorescence spectroscopy, as an informative and sensitive analytical technique, plays a key role in research fields including environmental science, medicine, pharmacology, and cellular biology. Access to a variety of new organic fluorophores provided by the microwave-assisted dehydrogenative DA reaction allows for further advancement in these fields. PMID:23609566

Microwave-assisted hydrothermal synthesis of marigold-like ZnIn2S4 microspheres and their visible light photocatalytic activity

NASA Astrophysics Data System (ADS)

Chen, Zhixin; Li, Danzhen; Xiao, Guangcan; He, Yunhui; Xu, Yi-Jun

2012-02-01

Marigold-like ZnIn2S4 microspheres were synthesized by a microwave-assisted hydrothermal method with the temperature ranging from 80 to 195 °C. X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen sorption analysis, UV-visible spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperatures were almost the same. The degradation of methyl orange (MO) under the visible light irradiation has been used as a probe reaction to investigate the photocatalytic activity of as-prepared ZnIn2S4, which shows that the ZnIn2S4 sample synthesized at 195 °C shows the best photocatalytic activity for MO degradation. In addition, the photocatalytic activities of all the samples prepared by the microwave-assisted hydrothermal method are better than those prepared by a normal hydrothermal method, which could be attributed to the formation of more defect sites during the microwave-assisted hydrothermal treatment.

Lactic acid as an invaluable green solvent for ultrasound-assisted scalable synthesis of pyrrole derivatives.

PubMed

Wang, Shi-Fan; Guo, Chao-Lun; Cui, Ke-Ke; Zhu, Yan-Ting; Ding, Jun-Xiong; Zou, Xin-Yue; Li, Yi-Hang

2015-09-01

Lactic acid has been used as a bio-based green solvent to study the ultrasound-assisted scale-up synthesis. We report here, for the first time, on the novel and scalable process for synthesis of pyrrole derivatives in lactic acid solvent under ultrasonic radiation. Eighteen pyrrole derivatives have been synthesized in lactic acid solvent under ultrasonic radiation and characterized by (1)H NMR, IR, ESI MS. The results show, under ultrasonic radiation, lactic acid solvent can overcome the scale-up challenges and exhibited many advantages, such as bio-based origin, shorter reaction time, lower volatility, higher yields, and ease of isolating the products. Copyright © 2015 Elsevier B.V. All rights reserved.

Microwave-Assisted Synthesis of some Novel Azoles and Azolopyrimidines as Antimicrobial Agents.

PubMed

Gomha, Sobhi M; Farghaly, Thoraya A; Mabkhot, Yahia Nasser; Zayed, Mohie E M; Mohamed, Amany M G

2017-02-23

In this study, new derivatives of pyrazole, isoxazole, pyrazolylthiazole, and azolopyrimidine having a thiophene ring were synthesized under microwave irradiation. Their pharmacological activity toward bacteria and fungi inhibition was screened and compared to the references Chloramphenicol and Trimethoprim / sulphamethoxazole . The antimicrobial results of the investigated compounds revealed promising results and some derivatives have activities similar to the references used.

Enabling technologies and green processes in cyclodextrin chemistry

PubMed Central

Caporaso, Marina; Jicsinszky, Laszlo; Martina, Katia

2016-01-01

Summary The design of efficient synthetic green strategies for the selective modification of cyclodextrins (CDs) is still a challenging task. Outstanding results have been achieved in recent years by means of so-called enabling technologies, such as microwaves, ultrasound and ball mills, that have become irreplaceable tools in the synthesis of CD derivatives. Several examples of sonochemical selective modification of native α-, β- and γ-CDs have been reported including heterogeneous phase Pd- and Cu-catalysed hydrogenations and couplings. Microwave irradiation has emerged as the technique of choice for the production of highly substituted CD derivatives, CD grafted materials and polymers. Mechanochemical methods have successfully furnished greener, solvent-free syntheses and efficient complexation, while flow microreactors may well improve the repeatability and optimization of critical synthetic protocols. PMID:26977187

Microwave-assisted Ullmann C-S bond formation: synthesis of the P38alpha MAPK clinical candidate VX-745.

PubMed

Bagley, Mark C; Davis, Terence; Dix, Matthew C; Fusillo, Vincenzo; Pigeaux, Morgane; Rokicki, Michal J; Kipling, David

2009-11-06

Microwave irradiation promotes the rapid and efficient reaction of a thiophenol and aryl or heteroaryl halide using a copper or palladium catalyst and a range of ligands, depending upon substrate. Of particular utility is the use of copper(I) iodide (5 mol %) and trans-cyclohexane-1,2-diol as ligand under basic conditions and microwave irradiation to give the corresponding sulfide in high yield. This method for C-S bond formation is applied in the four-step synthesis of the clinical candidate VX-745 in 38% overall yield. The inhibitory activity of VX-745 against p38alpha MAPK is confirmed in Werner syndrome dermal fibroblasts at 1.0 microM concentration by immunoblot assay.

1,2,3-Triazole-Functionalized Polysulfone Synthesis through Microwave-Assisted Copper-Catalyzed Click Chemistry: A Highly Proton Conducting High Temperature Membrane.

PubMed

Sood, Rakhi; Donnadio, Anna; Giancola, Stefano; Kreisz, Aurélien; Jones, Deborah J; Cavaliere, Sara

2016-07-06

Microwave heating holds all the aces regarding development of effective and environmentally friendly methods to perform chemical transformations. Coupling the benefits of microwave-enhanced chemistry with highly reliable copper-catalyzed azide-alkyne cycloaddition (CuAAC) click chemistry paves the way for a rapid and efficient synthesis procedure to afford high performance thermoplastic materials. We describe herein fast and high yielding synthesis of 1,2,3-triazole-functionalized polysulfone through microwave-assisted CuAAC as well as explore their potential as phosphoric acid doped polymer electrolyte membranes (PEM) for high temperature PEM fuel cells. Polymers with various degrees of substitution of the side-chain functionality of 1,4-substituted 1,2,3-triazole with alkyl and aryl pendant structures are prepared by sequential chloromethylation, azidation, and microwave-assisted CuAAC using a range of alkynes (1-pentyne, 1-nonyne, and phenylacetylene). The completeness of reaction at each step and the purity of the clicked polymers were confirmed by (1)H-(13)C NMR, DOSY-NMR and FTIR-ATR spectroscopies. The thermal and thermochemical properties of the modified polymers were characterized by differential scanning calorimetry and thermogravimetric analysis coupled with mass spectroscopy (TG-MS), respectively. TG-MS analysis demonstrated that the commencement of the thermal degradation takes place with the decomposition of the triazole ring while its substituents have critical influence on the initiation temperature. Polysulfone functionalized with 4-phenyl-1,2,3-triazole demonstrates significantly higher Tg, Td, and elastic modulus than the ones bearing 4-propyl-1,2,3-triazole and 4-heptyl-1,2,3-triazole groups. After doping with phosphoric acid, the functionalized polymers with acid doping level of 5 show promising performance with high proton conductivity in anhydrous conditions (in the range of 27-35 mS/cm) and satisfactorily high elastic modulus (in the range of 332-349 MPa).

Microwave assisted transformation of N,N-diphenylamine as precursors of organic light emitting diodes (OLED)

NASA Astrophysics Data System (ADS)

Jefri, Wahyuningrum, Deana

2015-09-01

In this research, study on the transformation of N,N-diphenylamine (DPA) using iodine (I2) utilizing solid state Microwave Assisted Organic Synthesis (MAOS) method has been carried out. The reaction was performed by variations of three parameters namely the mole of reagents, the amount and type of solid support (alumina/Al2O3), and the reaction conditions. Experimental results showed that neutral-alumina was a better solid support than basic-alumina. The optimum temperature for the reaction was approximately at 125-133 °C with reaction time of 15 minutes and microwave reactor power at 500-600 W. The separation of the yellowish green product solution with preparative Thin Layer Chromatography (TLC) method using n-hexane:ethyl acetate = 4:1 (v/v) as eluent yielded two fractions (I and II) and both fractions can undergo fluorescence under 365 nm UV light. Based on the LC chromatogram with methanol:water = 95:5 (v/v) as eluent and its corresponding mass spectra (ESI+), fraction I contained three compounds, which were tetracarbazole A, triphenylamine, and impurities in the form of plasticizer such as bis(2-ethylhexyl) phthalate. Fraction II also contained three compounds, which were tetracarbazole C, tetraphenylhydrazine, and plasticizer such as bis(2-ethylhexyl) phthalate. Both FT-IR (KBr disks) and NMR (500 MHz, CDCl3) spectra of fraction I and II confirmed the aromatic amine groups in those compounds. The observed fluorescence colors of fraction I and II were violet and violet-blue, respectively. Based on their structures and fluorescence characters, the compounds in fraction I and II have the potential to be used as Organic Light Emitting Diode (OLED) compound precursors.

Microwave assisted transformation of N,N-diphenylamine as precursors of organic light emitting diodes (OLED)

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

Jefri,; Wahyuningrum, Deana, E-mail: deana@chem.itb.ac.id

2015-09-30

In this research, study on the transformation of N,N-diphenylamine (DPA) using iodine (I2) utilizing solid state Microwave Assisted Organic Synthesis (MAOS) method has been carried out. The reaction was performed by variations of three parameters namely the mole of reagents, the amount and type of solid support (alumina/Al2O3), and the reaction conditions. Experimental results showed that neutral-alumina was a better solid support than basic-alumina. The optimum temperature for the reaction was approximately at 125-133 °C with reaction time of 15 minutes and microwave reactor power at 500-600 W. The separation of the yellowish green product solution with preparative Thin Layer Chromatographymore » (TLC) method using n-hexane:ethyl acetate = 4:1 (v/v) as eluent yielded two fractions (I and II) and both fractions can undergo fluorescence under 365 nm UV light. Based on the LC chromatogram with methanol:water = 95:5 (v/v) as eluent and its corresponding mass spectra (ESI+), fraction I contained three compounds, which were tetracarbazole A, triphenylamine, and impurities in the form of plasticizer such as bis(2-ethylhexyl) phthalate. Fraction II also contained three compounds, which were tetracarbazole C, tetraphenylhydrazine, and plasticizer such as bis(2-ethylhexyl) phthalate. Both FT-IR (KBr disks) and NMR (500 MHz, CDCl{sub 3}) spectra of fraction I and II confirmed the aromatic amine groups in those compounds. The observed fluorescence colors of fraction I and II were violet and violet-blue, respectively. Based on their structures and fluorescence characters, the compounds in fraction I and II have the potential to be used as Organic Light Emitting Diode (OLED) compound precursors.« less

Microwave assisted synthesis for A2E and development of LC-ESI-MS method for quantification of ocular bisretinoids in human retina.

PubMed

Kotnala, A; Senthilkumari, S; Halder, N; Kumar, A; Velpandian, T

2018-01-15

To develop a microwave assisted method for the rapid synthesis of A2E and also to develop a method to quantify N-retinylidene-N-retinylethanolamine(A2E), all-trans retinal dimer (ATRD), A2-glycerophospho ethanolamine (A2GPE), dihydropyridine phosphatidyl ethanolamine (A2DHPE) and monofuran A2E (MFA2E) in age matched retina. The development of microwave assisted synthesis of A2E, its purification and characterization for its utility in quantification in human retina. The semi-quantitative method development using LC-ESI-MS, LC-ESI-MS/MS and LC-APCI-MS/MS from pooled macula and peripheral retina for the bisretinoid analysis has been done. Maximum A2E conversion using microwave assisted process took place at 80°C for 45min with a yield of 55.01%. Highly sensitive and specific mass spectrometric method was developed using reverse phase C-18 separation with positive electrospray ionization and positive atmospheric phase chemical ionization of tandom mass spectrometry. A gradient mobile phase separation was achieved using water and methanol with 0.1% TFA. Multiple reaction monitoring acquisition for ESI and APCI was performed at ATRD m/z 551.2/522.2, A2GPE m/z 746.4/729.5, A2DHPEm/z 594.4/576.5, MFA2E m/z 608.2/591.2, A2E m/z 592.4/418.2. Method was validated using LC-ESI-SIM mode to determine selectivity, linearity, sensitivity, precision and accuracy. An attempt towards optimization of the synthetic procedure of A2E was made so as to reduce the lengthy reaction time without compromising the yield. Developed method was capable enough for the detection of low level of bisretinids in retina. Copyright © 2017 Elsevier B.V. All rights reserved.

Microwave-assisted synthesis of Mn{sub 3}O{sub 4} nanoparticles@reduced graphene oxide nanocomposites for high performance supercapacitors

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

She, Xiao; Zhang, Xinmin; Liu, Jingya

2015-10-15

Highlights: • Mn{sub 3}O{sub 4}@rGO nanocomposites were prepared by one-step microwave-assisted method. • The growth of Mn{sub 3}O{sub 4} and the reduction of graphene oxide occurred simultaneously. • Specific capacitance of the nanocomposite is higher than those of rGO and Mn{sub 3}O{sub 4}. • The nanocomposites have good rate capability and cycling stability. - ABSTRACT: One-step microwave-assisted synthetic route for the fabrication of Mn{sub 3}O{sub 4} nanoparticles@reduced graphene oxide (Mn{sub 3}O{sub 4}@rGO) nanocomposites has been demonstrated. The morphological structures of the nanocomposites are characterized by Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction (XRD), thermogravimetric analyses (TGA), and scanningmore » electron microscopy (SEM), respectively. All of the results indicate that the microwave-assisted synthesis results in the growth of Mn{sub 3}O{sub 4} and the reduction of graphene oxide simultaneously in ethylene glycol-water system. The specific capacitance of the as-prepared Mn{sub 3}O{sub 4}@rGO nanocomposite is higher than those of rGO and pure Mn{sub 3}O{sub 4}, which indicates the synergetic interaction between rGO and Mn{sub 3}O{sub 4}. The nanocomposites also have good rate capability and cycling stability in electrochemical experiments. This facile technique may be extended to the large scale and cost effective production of other composites based on graphene and metal oxide for many applications.« less

Innovative phytosynthesized silver nanoarchitectures with enhanced antifungal and antioxidant properties

NASA Astrophysics Data System (ADS)

Ortan, Alina; Fierascu, Irina; Ungureanu, Camelia; Fierascu, Radu Claudiu; Avramescu, Sorin Marius; Dumitrescu, Ovidiu; Dinu-Pirvu, Cristina Elena

2015-12-01

While in the early era of nanotechnology, nanoparticles of noble metals were obtained through expensive methods, using toxic chemical reagents, in the last decade attempts are made to obtain the desired chemical composition, size, morphology, and other properties by eco and green synthesis, using plants. The aim of this paper is to compare two extraction methods (hydroalcoholic extraction and microwave extraction) used to phytosynthesize silver nanoparticles, in terms of nanoparticle (NP) morphology, antioxidant, and antifungal action, using an European native plant, Anthriscus cerefolium (L.) Hoffm. The extracts and the obtained NPs were characterized by modern analytical techniques (GC-MS, UV-Vis, SEM, TEM) and by phytochemical assays (total flavonoids, total terpenoids and total phenolic content). The antifungal activity (evaluated using the Kirby-Bauer method, against Aspergillus niger and Penicillium hirsutum) and the antioxidant activity (determined by the DPPH assay and a chemiluminescence assay) revealed notable differences between the samples, differences due to the extraction procedure followed. Also, preliminary studies regarding the stability and the toxicity of the nanoparticles are presented. By using the microwave-assisted extraction, not only smaller particles (less than 10 nm) were obtained, but also with better antifungal and antioxidant properties than the ones obtained by classical extraction.

Rapid microwave-assisted synthesis of sub-30nm lipid nanoparticles.

PubMed

Dunn, Stuart S; Beckford Vera, Denis R; Benhabbour, S Rahima; Parrott, Matthew C

2017-02-15

Accessing the phase inversion temperature by microwave heating may enable the rapid synthesis of small lipid nanoparticles. Nanoparticle formulations consisted of surfactants Brij 78 and Vitamin E TPGS, and trilaurin, trimyristin, or miglyol 812 as nanoparticle lipid cores. Each formulation was placed in water and heated by microwave irradiation at temperatures ranging from 65°C to 245°C. We observed a phase inversion temperature (PIT) for these formulations based on a dramatic decrease in particle Z-average diameters. Subsequently, nanoparticles were manufactured above and below the PIT and studied for (a) stability toward dilution, (b) stability over time, (c) fabrication as a function of reaction time, and (d) transmittance of lipid nanoparticle dispersions. Lipid-based nanoparticles with distinct sizes down to 20-30nm and low polydispersity could be attained by a simple, one-pot microwave synthesis. This was carried out by accessing the phase inversion temperature using microwave heating. Nanoparticles could be synthesized in just one minute and select compositions demonstrated high stability. The notable stability of these particles may be explained by the combination of van der Waals interactions and steric repulsion. 20-30nm nanoparticles were found to be optically transparent. Published by Elsevier Inc.

Microwave-assisted synthesis of 3-aminobenzo[b]thiophene scaffolds for the preparation of kinase inhibitors.

PubMed

Bagley, Mark C; Dwyer, Jessica E; Molina, Maria D Beltran; Rand, Alexander W; Rand, Hayley L; Tomkinson, Nicholas C O

2015-06-28

Microwave irradiation of 2-halobenzonitriles and methyl thioglycolate in the presence of triethylamine in DMSO at 130 °C provides rapid access to 3-aminobenzo[b]thiophenes in 58-96% yield. This transformation has been applied in the synthesis of the thieno[2,3-b]pyridine core motif of LIMK1 inhibitors, the benzo[4,5]thieno[3,2-e][1,4]diazepin-5(2H)-one scaffold of MK2 inhibitors and a benzo[4,5]thieno[3,2-d]pyrimidin-4-one inhibitor of the PIM kinases.

Microwave-Assisted Synthesis of Red-Light Emitting Au Nanoclusters with the Use of Egg White

ERIC Educational Resources Information Center

Tian, Jinghan; Yan, Lei; Sang, Aohua; Yuan, Hongyan; Zheng, Baozhan; Xiao, Dan

2014-01-01

We developed a simple, cost-effective, and eco-friendly method to synthesize gold nanoclusters (AuNCs) with red fluorescence. The experiment was performed using HAuCl[subscript 4], egg white, Na[subscript 2]CO[subscript 3] (known as soda ash or washing soda), and a microwave oven. In our experiment, fluorescent AuNCs were prepared within a…

Diels-Alder cycloadditions by microwave-assisted, continuous flow organic synthesis (MACOS): the role of metal films in the flow tube.

PubMed

Shore, Gjergji; Organ, Michael G

2008-02-21

Thin Pd films have been deposited on the inside of capillary-sized tubes through which compounds undergoing Diels-Alder reactions have been flowed while being heated with microwave irradiation; dramatic rate accelerations are observed in the presence of the film, which has been shown to play both a heating and catalytic role.

Cd–cysteine precursor nanowire templated microwave-assisted transformation route to CdS nanotubes

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

Liu, Xiao-Lin, E-mail: liu_x_l@sina.cn; Zhu, Ying-Jie; Zhang, Qian

2012-12-15

Graphical abstract: Cadmium sulfide polycrystalline nanotubes have been successfully synthesized by microwave-assisted transformation method using Cd–cysteine precursor nanowires as the source material and template in ethylene glycol at 160 °C or ethanol at 60 °C. Display Omitted Highlights: ► Cd–cysteine precursor nanowires were successfully synthesized in alkaline solution. ► CdS nanotubes were prepared by templated microwave-assisted transformation method. ► CdS nanotubes can well duplicate the size and morphology of precursor nanowires. ► This method has the advantages of the simplicity and low cost. -- Abstract: We report the Cd–cysteine precursor nanowire templated microwave-assisted transformation route to CdS nanotubes. In thismore » method, the Cd–cysteine precursor nanowires are synthesized using CdCl{sub 2}·2.5H{sub 2}O, L-cysteine and ethanolamine in water at room temperature. The Cd–cysteine precursor nanowires are used as the source material and template for the subsequent preparation of CdS nanotubes by a microwave-assisted transformation method using ethylene glycol or ethanol as the solvent. This method has the advantages of the simplicity and low cost, and may be extended to the synthesis of nanotubes of other compounds. The products are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM).« less

GREEN AND CONTROLLED SYNTHESIS OF GOLD AND PLATINUM NANOMATERIALS USING VITAMIN B2: DENSITY-ASSISTED SELF-ASSEMBLY OF NANOSPHERES, WIRES AND RODS

EPA Science Inventory

For the first time, we report density-assisted self-assembly and efficient synthesis of gold (Au) and platinum (Pt) nanospheres, nanowires and nanorods using vitamin B₂ (riboflavin) without employing any special capping or dispersing agent at room temperature; this env...

One-step microwave-assisted synthesis of water-dispersible Fe3O4 magnetic nanoclusters for hyperthermia applications

NASA Astrophysics Data System (ADS)

Sathya, Ayyappan; Kalyani, S.; Ranoo, Surojit; Philip, John

2017-10-01

To realize magnetic hyperthermia as an alternate stand-alone therapeutic procedure for cancer treatment, magnetic nanoparticles with optimal performance, within the biologically safe limits, are to be produced using simple, reproducible and scalable techniques. Herein, we present a simple, one-step approach for synthesis of water-dispersible magnetic nanoclusters (MNCs) of superparamagnetic iron oxide by reducing of Fe2(SO4)3 in sodium acetate (alkali), poly ethylene glycol (capping ligand), and ethylene glycol (solvent and reductant) in a microwave reactor. The average size and saturation magnetization of the MNC's are tuned from 27 to 52 nm and 32 to 58 emu/g by increasing the reaction time from 10 to 600 s. Transmission electron microscopy images reveal that each MNC composed of large number of primary Fe3O4 nanoparticles. The synthesised MNCs show excellent colloidal stability in aqueous phase due to the adsorbed PEG layer. The highest SAR value of 215 ± 10 W/gFe observed in 52 nm size MNC at a frequency of 126 kHz and field of 63 kA/m suggest the potential use of these MNC in hyperthermia applications. This study further opens up the possibilities to develop metal ion-doped MNCs with tunable sizes suitable for various biomedical applications using microwave assisted synthesis.

Microwave-assisted template-free synthesis of butterfly-like CuO through Cu2Cl(OH)3 precursor and the electrochemical sensing property

NASA Astrophysics Data System (ADS)

Xie, Hanjie; Zhu, Lianjie; Zheng, Wenjun; Zhang, Jing; Gao, Fubo; Wang, Yan

2016-11-01

An energy-efficient and environmentally friendly microwave-assisted method was adopted for synthesis of butterfly-like CuO assembled by nanosheets through a Cu2Cl(OH)3 precursor, using no template. Formation mechanism of the butterfly-like CuO was explored and discussed systematically for the first time on the basis of both experimental results and crystal structure transformations in atomic level. The electrochemical sensing properties of the butterfly-like CuO modified electrode to ascorbic acid (AA) were studied for the first time. The results reveal that Cu(OH)2 nanowires were formed once the Cu2+ ions, located in between two CuO4 parallelogram chains of a Cu2Cl(OH)3 precursor, dissolve into the solution as Cu(OH)42- complex ions after ion exchange reactions and simultaneous assemble along a axis. Upon microwave irradiation, the adjacent CuO4 parallelogram chains of the Cu(OH)2 nanowires dehydrate and assemble along c axis, forming CuO nanosheets with (002) as the main exposed facet, which were further assembled to butterfly-like CuO under the action of microwave field, suggesting that microwave field functions like a 'directing agent'. The butterfly-like CuO modified electrode shows good electrochemical sensing properties to AA with a low detecting limit, short response time and wide linear response range.

cis-Apa: a practical linker for the microwave-assisted preparation of cyclic pseudopeptides via RCM cyclative cleavage.

PubMed

Baron, Alice; Verdié, Pascal; Martinez, Jean; Lamaty, Frédéric

2011-02-04

A new linker cis-5-aminopent-3-enoic acid (cis-Apa) was prepared for the synthesis of cyclic pseudopeptides by cyclization-cleavage by using ring-closing methatesis (RCM). We developed a new synthetic pathway for the preparation of the cis-Apa linker that was tested in the cyclization-cleavage process of different RGD peptide sequences. Different macrocyclic peptidomimetics were prepared by using this integrated microwave-assisted method, showing that the readily available cis-Apa amino acid is well adapted as a linker in the cyclization-cleavage process.

Synthesis of Graphite Oxide with Different Surface Oxygen Contents Assisted Microwave Radiation

PubMed Central

Ibarra-Hernández, Adriana

2018-01-01

Graphite oxide is synthesized via oxidation reaction using oxidant compounds that have lattice defects by the incorporation of unlike functional groups. Herein, we report the synthesis of the graphite oxide with diverse surface oxygen content through three (B, C, D) different modified versions of the Hummers method assisted microwave radiation compared with the conventional graphite oxide sample obtained by Hummers method (A). These methods allow not only the production of graphite oxide but also reduced graphene oxide, without undergoing chemical, thermal, or mechanical reduction steps. The values obtained of C/O ratio were ~2, 3.4, and ~8.5 for methodologies C, B, and D, respectively, indicating the presence of graphite oxide and reduced graphene oxide, according to X-ray photoelectron spectroscopy. Raman spectroscopy of method D shows the fewest structural defects compared to the other methodologies. The results obtained suggest that the permanganate ion produces reducing species during graphite oxidation. The generation of these species is attributed to a reversible reaction between the permanganate ion with π electrons, ions, and radicals produced after treatment with microwave radiation. PMID:29438280

Microwave-assisted synthesis of triple-helical, collagen-mimetic lipopeptides

PubMed Central

Banerjee, Jayati; Hanson, Andrea J; Muhonen, Wallace W; Shabb, John B; Mallik, Sanku

2018-01-01

Collagen-mimetic peptides and lipopeptides are widely used as substrates for matrix degrading enzymes, as new biomaterials for tissue engineering, as drug delivery systems and so on. However, the preparation and subsequent purification of these peptides and their fatty-acid conjugates are really challenging. Herein, we report a rapid microwave-assisted, solid-phase synthetic protocol to prepare the fatty-acid conjugated, triple-helical peptides containing the cleavage site for the enzyme matrix metalloproteinase-9 (MMP-9). We employed a PEG-based resin as the solid support and the amino acids were protected with Fmoc- and tert-butyl groups. The amino acids were coupled at 50 °C (25 W of microwave power) for 5 min. The deprotection reactions were carried out at 75 °C (35 W of microwave power) for 3 min. Using this protocol, a peptide containing 23 amino acids was synthesized and then conjugated to stearic acid in 14 h. PMID:20057380

Microwave assisted synthesis and characterization of barium titanate nanoparticles for multi layered ceramic capacitor applications.

PubMed

Thirumalai, Sundararajan; Shanmugavel, Balasivanandha Prabu

2011-01-01

Barium titanate is a common ferroelectric electro-ceramic material having high dielectric constant, with photorefractive effect and piezoelectric properties. In this research work, nano-scale barium titanate powders were synthesized by microwave assisted mechano-chemical route. Suitable precursors were ball milled for 20 hours. TGA studies were performed to study the thermal stability of the powders. The powders were characterized by XRD, SEM and EDX Analysis. Microwave and Conventional heating were performed at 1000 degrees C. The overall heating schedule was reduced by 8 hours in microwave heating thereby reducing the energy and time requirement. The nano-scale, impurity-free and defect-free microstructure was clearly evident from the SEM micrograph and EDX patterns. LCR meter was used to measure the dielectric constant and dielectric loss values at various frequencies. Microwave heated powders showed superior dielectric constant value with low dielectric loss which is highly essential for the fabrication of Multi Layered Ceramic Capacitors.

Ultra-fast microwave-assisted hydrothermal synthesis of long vertically aligned ZnO nanowires for dye-sensitized solar cell application.

PubMed

Mahpeykar, S M; Koohsorkhi, J; Ghafoori-Fard, H

2012-04-27

Long vertically aligned ZnO nanowire arrays were synthesized using an ultra-fast microwave-assisted hydrothermal process. Using this method, we were able to grow ZnO nanowire arrays at an average growth rate as high as 200 nm min(-1) for maximum microwave power level. This method does not suffer from the growth stoppage problem at long growth times that, according to our investigations, a normal microwave-assisted hydrothermal method suffers from. Longitudinal growth of the nanowire arrays was investigated as a function of microwave power level and growth time using cross-sectional FESEM images of the grown arrays. Effect of seed layer on the alignment of nanowires was also studied. X-ray diffraction analysis confirmed c-axis orientation and single-phase wurtzite structure of the nanowires. J-V curves of the fabricated ZnO nanowire-based mercurochrome-sensitized solar cells indicated that the short-circuit current density is increased with increasing the length of the nanowire array. According to the UV-vis spectra of the dyes detached from the cells, these increments were mainly attributed to the enlarged internal surface area and therefore dye loading enhancement in the lengthened nanowire arrays.

On the importance of simultaneous infrared/fiber-optic temperature monitoring in the microwave-assisted synthesis of ionic liquids.

PubMed

Obermayer, David; Kappe, C Oliver

2010-01-07

The temperature profiles obtained from both an external infrared and internal fiber-optic sensor were compared for heating and synthesizing the ionic liquid 1-butyl-3-methylimidazolium bromide (bmimBr) under microwave conditions. Utilizing a single-mode microwave reactor that allows simultaneous infrared/fiber-optic temperature measurements, significant differences between the two methods of temperature monitoring were revealed. Due to the strong microwave absorptivity of ionic liquids and the delay experienced in monitoring temperature on the outer surface of a heavy-walled glass vial, external infrared temperature sensors can not be used to accurately control the temperature in the heating of ionic liquids under microwave conditions. The use of internal fiber-optic probes allows the monitoring and control of the heating behavior in a much better way. In order to prevent the strong exotherm in the synthesis of bmimBr under microwave conditions the use of a reaction vessel made out of silicon carbide is the method of choice. Because of the high thermal conductivity and effusivity of silicon carbide, the heat generated during the ionic liquid formation is efficiently exchanged with the comparatively cool air in the microwave cavity via the silicon carbide ceramic.

A rapid microwave-assisted synthesis of a sodium-cadmium metal-organic framework having improved performance as a CO2 adsorbent for CCS.

PubMed

Palomino Cabello, Carlos; Arean, Carlos Otero; Parra, José B; Ania, Conchi O; Rumori, P; Turnes Palomino, G

2015-06-07

We report on a facile and rapid microwave-assisted method for preparing a sodium-cadmium metal-organic framework (having coordinatively unsaturated sodium ions) that considerably shortens the conventional synthesis time from 5 days to 1 hour. The obtained (Na,Cd)-MOF showed an excellent volumetric CO2 adsorption capacity (5.2 mmol cm(-3) at 298 K and 1 bar) and better CO2 adsorption properties than those shown by the same metal-organic framework when synthesized following a more conventional procedure. Moreover, the newly prepared material was found to display high selectivity for adsorption of carbon dioxide over nitrogen, and good regenerability and stability during repeated CO2 adsorption-desorption cycles, which are the required properties for any adsorbent intended for carbon dioxide capture and sequestration (CSS) from the post-combustion flue gas of fossil fuelled power stations.

Microwave-Assisted Synthesis, Microstructure, and Magnetic Properties of Rare-Earth Cobaltites.

PubMed

Gutiérrez Seijas, Julia; Prado-Gonjal, Jesús; Ávila Brande, David; Terry, Ian; Morán, Emilio; Schmidt, Rainer

2017-01-03

The series of perovskite rare-earth (RE) doped cobaltites (RE)CoO 3 (RE = La-Dy) was prepared by microwave-assisted synthesis. The crystal structure undergoes a change of symmetry depending on the size of the RE cation. LaCoO 3 is rhombohedral, S.G. R3̅c (No. 167), while, for the rest of the RE series (Pr-Dy), the symmetry is orthorhombic, S.G. Pnma (No. 62). The crystal structure obtained by X-ray diffraction was confirmed by high-resolution transmission electron microscopy, which yielded a good match between experimental and simulated images. It is further shown that the well-known magnetism in LaCoO 3 , which involves a thermally induced Co 3+ (d 6 ) low spin to intermediate or high spin state transition, is strongly modified by the RE cation, and a rich variety of magnetic order has been detected across the series.

One-pot microwave assisted stereoselective synthesis of novel dihydro-2'H-spiro[indene-2,1'-pyrrolo-[3,4-c]pyrrole]-tetraones and evaluation of their antimycobacterial activity and inhibition of AChE.

PubMed

Bharkavi, Chelliah; Vivek Kumar, Sundaravel; Ashraf Ali, Mohamed; Osman, Hasnah; Muthusubramanian, Shanmugam; Perumal, Subbu

2017-07-15

An efficient one-pot microwave assisted stereoselective synthesis of novel dihydro-2'H-spiro[indene-2,1'-pyrrolo[3,4-c]pyrrole]-tetraone derivatives through three-component 1,3-dipolar cycloaddition of azomethine ylides generated in situ from ninhydrin and sarcosine with a series of 1-aryl-1H-pyrrole-2,5-diones is described. The synthesised compounds were screened for their antimycobacterial and AChE inhibition activities. Compound 4b (IC 50 1.30µM) has been found to display twelve fold antimycobacterial activity compared to cycloserine and it is thirty seven times more active than pyrimethamine. Compound 4h displays maximum AchE inhibitory activity with IC 50 value of 0.78±0.01µmol/L. Copyright © 2017 Elsevier Ltd. All rights reserved.

Cationic pentaheteroaryls as selective G-quadruplex ligands by solvent-free microwave-assisted synthesis.

PubMed

Petenzi, Michele; Verga, Daniela; Largy, Eric; Hamon, Florian; Doria, Filippo; Teulade-Fichou, Marie-Paule; Guédin, Aurore; Mergny, Jean-Louis; Mella, Mariella; Freccero, Mauro

2012-11-05

We report herein a solvent-free and microwaved-assisted synthesis of several water soluble acyclic pentaheteroaryls containing 1,2,4-oxadiazole moieties (1-7). Their binding interactions with DNA quadruplex structures were thoroughly investigated by FRET melting, fluorescent intercalator displacement assay (G4-FID) and CD spectroscopy. Among the G-quadruplexes considered, attention was focused on telomeric repeats together with the proto-oncogenic c-kit sequences and the c-myc oncogene promoter. Compound 1, and to a lesser extent 2 and 5, preferentially stabilise an antiparallel structure of the telomeric DNA motif, and exhibit an opposite binding behaviour to structurally related polyoxazole (TOxaPy), and do not bind duplex DNA. The efficiency and selectivity of the binding process was remarkably controlled by the structure of the solubilising moieties. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Plant Polyphenol-Assisted Green Synthesis of Hollow CoPt Alloy Nanoparticles for Dual-Modality Imaging Guided Photothermal Therapy.

PubMed

Song, Xiao-Rong; Yu, Shu-Xian; Jin, Gui-Xiao; Wang, Xiaoyong; Chen, Jianzhong; Li, Juan; Liu, Gang; Yang, Huang-Hao

2016-03-01

Theranostic nanomedicines that integrate diagnostic and therapeutic moieties into a single nanoscale platform are playing an increasingly important role in fighting cancer. Here, a facile and green synthetic strategy for hollow CoPt alloy nanoparticles (HCPA-NPs) using plant polyphenols as assisted agents is reported for the first time. This novel strategy enables size-controlled synthesis of HCPA-NPs through the control of the molecular sizes of polyphenols. It is also a versatile strategy for synthesizing other hollow alloy nanoparticles with various metal compositions due to the diverse metal-chelating ability of the polyphenols. Further studies show that HCPA-NPs have good biocompatibility and can be successfully implemented for magnetic resonance and photoacoustic dual-modal imaging guided photothermal therapy. This work brings new insights for the green synthesis of hollow nanoparticles and extends these biocompatible nanoparticles for theranostic applications. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microwave-Assisted Synthesis Cd Metal Hexagonal Nanosheets

NASA Astrophysics Data System (ADS)

Sun, Yidong; She, Houde; Bai, Wencai; Li, Liangshan; Zhou, Hua

2018-07-01

Sodium borohydride (NaBH4) as reducing agent, oleic acid (OA) as surfactant, deionized water as the dispersant, reducing cadmium nitrate (Cd(NO3)2 · 4H2O) can get Cd nanosheets by microwave method. Room temperature photoluminescence (PL) spectrum for Cd nanosheets recorded under xenon light wavelength of 325 nm exhibited obviously emission bands at 331, 379, and 390 nm. By analyzing the results of XRD and TEM, the nanosheets are thought as hexagonal phase and the size is about 20 nm. This synthesis performs in a lower temperature. Moreover our method is quite simple and the cost of the experiment is relatively lower.

Synthesis and characterization of zinc borophosphates with ANA-zeotype framework by the microwave method

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

Song, Yu, E-mail: songyu@dlpu.edu.cn; Ding, Ling; An, Qingda

2013-06-15

Zinc borophosphate (NH{sub 4}){sub 16}[Zn{sub 16}B{sub 8}P{sub 24}O{sub 96}] (denoted as ZnBP-ANA) with ANA-zeotype structure has been synthesized by employing microwave-assisted solvothermal synthesis in the reaction system ZnCl{sub 2}∙6H{sub 2}O-(NH{sub 4}){sub 2}HPO{sub 4}–H{sub 3}BO{sub 3} using ethylene glycol as a co-solvent. The influences of various experimental parameters, such as reaction temperature, solvent ratio, zinc precursors and reactive power, have been systematically investigated. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA), and so on. Small and homogeneous ZnBP-ANA single crystal with regular cube morphology are crystallized by using microwave solvothermal synthesis method withinmore » a shorter time, and its grain size decreases with power. - Graphical abstract: Tailor-made ANA zeolites with varied size can be prepared by simply changing the reaction power. - Highlights: • Zinc borophosphate zeolites with ANA-zeotype structures were prepared by microwave technique. • The size of crystals could be controlled by tuning power. • Synthesis period can be significantly reduced by raising reaction temperature.« less

Green Synthesis of Red-Emitting Carbon Nanodots as a Novel "Turn-on" Nanothermometer in Living Cells.

PubMed

Wang, Chuanxi; Jiang, Kaili; Wu, Qian; Wu, Jiapeng; Zhang, Chi

2016-10-04

Temperature measurements in biology and medical diagnostics, along with sensitive temperature probing of living cells, is of great importance; however, it still faces significant challenges. Herein, a novel "turn-on" carbon-dot-based fluorescent nanothermometry device for spatially resolved temperature measurements in living cells is presented. The carbon nanodots (CNDs) are prepared by a green microwave-assisted method and exhibit red fluorescence (λem =615 nm) with high quantum yields (15 %). Then, an on-off fluorescent probe is prepared for detecting glutathione (GSH) based on aggregation-induced fluorescence quenching. Interestingly, the quenched fluorescence could be recovered by increasing temperature and the CNDs-GSH mixture could behave as an off-on fluorescent probe for temperature. Thus, red-emitting CNDs can be utilized for "turn-on" fluorescent nanothermometry through the fluorescence quenching and recovery processes, respectively. We employ MC3T3-E1 cells as an example model to demonstrate the red-emitting CNDs can function as "non-contact" tools for the accurate measurement of temperature and its gradient inside a living cell. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microwave-assisted synthesis of isosorbide-derived diols for the preparation of thermally stable thermoplastic polyurethane

PubMed Central

Kasmi, Nejib; Roso, Martina; Hammami, Nadia; Majdoub, Mustapha; Boaretti, Carlo; Sgarbossa, Paolo; Vianello, Chiara; Maschio, Giuseppe; Modesti, Michele; Lorenzetti, Alessandra

2017-01-01

Abstract In order to prepare thermally stable isosorbide-derived thermoplastic polyurethane, the synthesis of two new chiral exo–exo configured diols, prepared from isosorbide, and two types of diphenols (bisphenol A and thiodiphenol) was described. The synthesis conditions were optimized under conventional heating and microwave irradiations. To prove their suitability in polymerization, these monomers were successfully polymerized using 4,4′-diphenylmethane diisocyanate (MDI) and hexamethylene diisocyanate (HDI). Both monomers and polymers have been studied by NMR, FT-IR, TGA, DSC; intrinsic viscosity of polymers has also been determined. The results showed the effectiveness of the synthetic strategy proposed; moreover, a dramatic reduction of the reaction time and an important improvement of the monomers yield using microwave irradiation have been demonstrated. The monomers, as well as the polymers, showed excellent thermal stability both in air and nitrogen. It was also shown that the introduction of sulphur in the polyurethane backbone was effective in delaying the onset of degradation as well as the degradation rate. PMID:29491826

Deep Eutectic Solvent-Based Microwave-Assisted Method for Extraction of Hydrophilic and Hydrophobic Components from Radix Salviae miltiorrhizae.

PubMed

Chen, Jue; Liu, Mengjun; Wang, Qi; Du, Huizhi; Zhang, Liwei

2016-10-17

Deep eutectic solvents (DESs) have attracted significant attention as a promising green media. In this work, twenty-five kinds of benign choline chloride-based DESs with microwave-assisted methods were applied to quickly extract active components from Radix Salviae miltiorrhizae . The extraction factors, including temperature, time, power of microwave, and solid/liquid ratio, were investigated systematically by response surface methodology. The hydrophilic and hydrophobic ingredients were extracted simultaneously under the optimized conditions: 20 vol% of water in choline chloride/1,2-propanediol (1:1, molar ratio) as solvent, microwave power of 800 W, temperature at 70 °C, time at 11.11 min, and solid/liquid ratio of 0.007 g·mL -1 . The extraction yield was comparable to, or even better than, conventional methods with organic solvents. The microstructure alteration of samples before and after extraction was also investigated. The method validation was tested as the linearity of analytes ( r ² > 0.9997 over two orders of magnitude), precision (intra-day relative standard deviation (RSD) < 2.49 and inter-day RSD < 2.96), and accuracy (recoveries ranging from 95.04% to 99.93%). The proposed DESs combined with the microwave-assisted method provided a prominent advantage for fast and efficient extraction of active components, and DESs could be extended as solvents to extract and analyze complex environmental and pharmaceutical samples.

An efficient green synthesis of 2-arylbenzothiazole analogues as potent antibacterial and anticancer agents.

PubMed

Chhabra, Mohit; Sinha, Sohini; Banerjee, Swagata; Paira, Priyankar

2016-01-01

We have demonstrated a novel and green approach for the synthesis of 2-substituted benzothiazole analogues. A number of 2-aryl and heteroaryl benzothiazole scaffolds were synthesized using Amberlite IR-120 resin under microwave irradiation. The catalytic role and reusability of the resin was well established here. 2-Substituted benzothiazole analogues (3a-l) were also tested against several bacterial strains (Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Salmonella) and cancer cell lines (MCF-7 and HeLa). The stability of compound 2-phenyl benzothiazole (3a) and 2-pyridin-2-yl-benzothiazole (3k) in GSH (0.01mM dissolved in DMSO) was measured by UV-Vis spectroscopy. Compound 3k also shows remarkable fluorescence in MeOH. Copyright © 2015 Elsevier Ltd. All rights reserved.

A study of thermal properties of sodium titanate nanotubes synthesized by microwave-assisted hydrothermal method

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

Preda, Silviu, E-mail: predas01@yahoo.co.uk; Rutar, Melita; Jožef Stefan International Postgraduate School, Jamova cesta 39, SI-1000 Ljubljana

2015-11-15

Highlights: • The microwave-assisted hydrothermal route was used for titanate nanotubes synthesis. • Conversion to single-phase nanotube morphology completes after 8 h reaction time. • The nanotube morphology is stable up to 600 °C, as determined by in-situ XRD and SEM. • Sodium ions migrate to the surface due to thermal motion and structure condensation. - Abstract: Sodium titanate nanotubes (NaTiNTs) were synthesized by microwave-assisted hydrothermal treatment of commercial TiO{sub 2}, at constant temperature (135 °C) and different irradiation times (15 min, 1, 4, 8 and 16 h). The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electronmore » microscopy, differential scanning calorimetry and specific surface area measurements. The irradiation time turned out to be the key parameter for morphological control of the material. Nanotubes were observed already after 15 min of microwave irradiation. The analyses of the products irradiated for 8 and 16 h confirm the complete transformation of the starting TiO{sub 2} powder to NaTiNTs. The nanotubes are open ended with multi-wall structures, with the average outer diameter of 8 nm and specific surface area up to 210 m{sup 2}/g. The morphology, surface area and crystal structure of the sodium titanate nanotubes synthesized by microwave-assisted hydrothermal method were similar to those obtained by conventional hydrothermal method.« less

Solvothermal synthesis of selenium nano and microspheres deposited on silicon surface by microwave-assisted method

NASA Astrophysics Data System (ADS)

Ahmad, Muthanna

2016-10-01

This work describes a new application of the solvothermal method, based on the microwave heating, for the synthesis of nano and microparticles of selenium. The reaction of selenium with hydrofluoric acid on the silicon surface is induced by microwave irradiation under high pressure and temperature of 60 bar and 160 °C, respectively. This method allows the deposition of spherical-like particles on the in situ etched silicon surface. The size of deposited selenium spheres scales from tens of nanometers up to tens of micrometers. The morphology and composition of the deposited selenium were analyzed by various analytical techniques. The formation dynamic of spherical structure is explained on the base of reduction of selenium species by hydrogen inside gas bubbles which are generated on the silicon surface by the etching process.

Microwave Synthesis of BCNO/SiO2 Nanocomposite Material

NASA Astrophysics Data System (ADS)

Faryuni, I. D.; Ramdhani, F.; Sampurno, J.; Nuryadin, B. W.; Noor, F. A.; Iskandar, F.

2017-07-01

In the present work, we report the preparation of BCNO/SiO2 phosphor synthesized using a microwave-assisted method. This method allows a lower temperature and a shorter reaction time than simple heating (furnace). The phosphors were prepared from precursors containing, boric acid, urea, citric acid and SiO2 nanoparticles. To These precursors, silica nanoparticles were added at various concentrations from 0 to 5 %wt. The emission wavelength produced by the phosphor was varied by varying the fraction mass of the silica that were added to the precursors. The results showed that higher photoluminescence (PL) intensity was produced by the BCNO/SiO2 with 3 %wt silica addition. The novelty of this research is using microwave heating for BCNO/SiO2 synthesis, which is usually conducted using a simple heating method.

Synthesis and characterization of [BMIM]bromide using microwave-assisted organic synthesis method and its application for dissolution of palm empty fruit bunch

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

Arianie, Lucy, E-mail: lucy205@yahoo.com; Wahyuningrum, Deana, E-mail: deana@chem.itb.ac.id; Nurrachman, Zeily, E-mail: deana@chem.itb.ac.id

The decrease of cellulose crystallinity index of palm empty fruit bunch is crucial for the next application of cellulose as raw material for various biofuel and its derivatives. The aim of this research is to decrease the cellulose crystallinity index of palm empty fruit bunch using 1-butyl-3-methylimidazoliumbromide or [BMIM] bromide which has been synthesized using Microwave-Assisted Organic Synthesis (MAOS) method. Conventional reaction method has also been carried out to synthesize [BMIM]bromide for comparison as well. The characterization of synthesized product using FTIR, {sup 1}H-NMR, {sup 13}C-NMR and LC-MS showed that these reactions have been carried out successfully. The results showedmore » that MAOS method is up to 90% faster in producing [BMIM]bromide compare to the conventional method. The application of [BMIM]bromide for dissolution of palm empty fruit bunch showed that cellulose and lignin could be extracted using stirring process for 20 hours. The decrease of cellulose crystallinity index and its morphology changes were identified using FTIR and Scanning Electron Microscope.« less

Synthesis and characterization of [BMIM]bromide using microwave-assisted organic synthesis method and its application for dissolution of palm empty fruit bunch

NASA Astrophysics Data System (ADS)

Arianie, Lucy; Wahyuningrum, Deana; Nurrachman, Zeily; Natalia, Dessy

2014-03-01

The decrease of cellulose crystallinity index of palm empty fruit bunch is crucial for the next application of cellulose as raw material for various biofuel and its derivatives. The aim of this research is to decrease the cellulose crystallinity index of palm empty fruit bunch using 1-butyl-3-methylimidazoliumbromide or [BMIM] bromide which has been synthesized using Microwave-Assisted Organic Synthesis (MAOS) method. Conventional reaction method has also been carried out to synthesize [BMIM]bromide for comparison as well. The characterization of synthesized product using FTIR, 1H-NMR, 13C-NMR and LC-MS showed that these reactions have been carried out successfully. The results showed that MAOS method is up to 90% faster in producing [BMIM]bromide compare to the conventional method. The application of [BMIM]bromide for dissolution of palm empty fruit bunch showed that cellulose and lignin could be extracted using stirring process for 20 hours. The decrease of cellulose crystallinity index and its morphology changes were identified using FTIR and Scanning Electron Microscope.

Rapid tea catechins and caffeine determination by HPLC using microwave-assisted extraction and silica monolithic column.

PubMed

Rahim, A A; Nofrizal, S; Saad, Bahruddin

2014-03-15

A rapid reversed-phase high performance liquid chromatographic method using a monolithic column for the determination of eight catechin monomers and caffeine was developed. Using a mobile phase of water:acetonitrile:methanol (83:6:11) at a flow rate of 1.4 mL min(-1), the catechins and caffeine were isocratically separated in about 7 min. The limits of detection and quantification were in the range of 0.11-0.29 and 0.33-0.87 mg L(-1), respectively. Satisfactory recoveries were obtained (94.2-105.2 ± 1.8%) for all samples when spiked at three concentrations (5, 40 and 70 mg L(-1)). In combination with microwave-assisted extraction (MAE), the method was applied to the determination of the catechins and caffeine in eleven tea samples (6 green, 3 black and 2 oolong teas). Relatively high levels of caffeine were found in black tea, but higher levels of the catechins, especially epigallocatechin gallate (EGCG) were found in green teas. Copyright © 2013 Elsevier Ltd. All rights reserved.

The catalytic oxidation of malachite green by the microwave-Fenton processes.

PubMed

Zheng, Huaili; Zhang, Huiqin; Sun, Xiaonan; Zhang, Peng; Tshukudu, Tiroyaone; Zhu, Guocheng

2010-01-01

Catalytic oxidation of malachite green using the microwave-Fenton process was investigated. 0% of malachite green de-colorization using the microwave process and 23.5% of malachite green de-colorization using the Fenton process were observed within 5 minutes. In contrast 95.4% of malachite green de-colorization using the microwave-Fenton was observed in 5 minutes. During the microwave-Fenton process, the optimum operating conditions for malachite green de-colorization were found to be 3.40 of initial pH, 0.08 mmol/L of Fe2+ concentration and 12.5 mmol/L of H2O2 concentration. Confirmatory tests were carried out under the optimum conditions and the COD removal rate of 82.0% and the de-colorization rate of 99.0% were observed in 5 minutes. The apparent kinetics equation of -dC/dt=0.0337 [malachite green]0.9860[Fe2+)]0.8234[H2O2]0.1663 for malachite green de-colorization was calculated, which implied that malachite green was the dominant factor in determining the removal efficiency of malachite green based on microwave-Fenton process.

Room Temperature Magnetic Behavior In Nanocrystalline Ni-Doped Zro2 By Microwave-Assisted Polyol Synthesis

NASA Astrophysics Data System (ADS)

Parimita Rath, Pragyan; Parhi, Pankaj Kumar; Ranjan Panda, Sirish; Priyadarshini, Barsharani; Ranjan Sahoo, Tapas

2017-08-01

This article, deals with a microwave-assisted polyol method to demonstrate a low temperature route < 250°C, to prepare a high temperature cubic zirconia phase. Powder XRD pattern shows broad diffraction peaks suggesting nanometric size of the particles. Magnetic behavior of 1-5 at% Ni doped samples show a threshold for substitutional induced room temperature ferromagnetism up to 3 at% of Ni. TGA data reveals that Ni-doped ZrO2 polyol precursors decompose exothermically below 300°C. IR data confirms the reduction of Zr(OH)4 precipitates to ZrO2, in agreement with the conclusions drawn from the TGA analysis.

Microwave-assisted synthesis and critical analysis for YBa2Cu3O6+δ nanoparticles

NASA Astrophysics Data System (ADS)

Chhaganlal Gandhi, Ashish; Lin, Jauyn Grace

2018-05-01

A new cost effective scheme of a microwave-assisted sol–gel route followed by a short annealing time is proposed to synthesize YBCO nanoparticles (NPs) of various sizes. The advanced techniques of synchrotron radiation x-ray diffraction (SRXRD) and electron spin resonance (ESR) are used to analyze the size effects on their magnetic/superconducting properties. The major interesting finding is that the size of YBCO NPs could confine the amount of oxygen content and consequently change the superconducting transition temperature (T C ) of YBCO NPs. The ESR result demonstrates a sensitive probe to characterize surface defects in the oxygen-deficient YBCO NPs.

A rapid green strategy for the synthesis of Au "meatball"-like nanoparticles using green tea for SERS applications

NASA Astrophysics Data System (ADS)

Wu, Shichao; Zhou, Xi; Yang, Xiangrui; Hou, Zhenqing; Shi, Yanfeng; Zhong, Lubin; Jiang, Qian; Zhang, Qiqing

2014-09-01

We report a simple and rapid biological approach to synthesize water-soluble and highly roughened "meatball"-like Au nanoparticles using green tea extract under microwave irradiation. The synthesized Au meatball-like nanoparticles possess excellent monodispersity and uniform size (250 nm in diameter). Raman measurements show that these tea-generated meatball-like gold nanostructures with high active surface areas exhibit a high enhancement of surface-enhanced Raman scattering. In addition, the Au meatball-like nanoparticles demonstrate good biocompatibility and remarkable in vitro stability at the biological temperature. Meanwhile, the factors that influence the Au meatball-like nanoparticles morphology are investigated, and the mechanisms behind the nonspherical shape evolution are discussed.

Microwave synthesis of noncentrosymmetric BaTiO3 truncated nanocubes for charge storage applications.

PubMed

Swaminathan, V; Pramana, Stevin S; White, T J; Chen, L; Chukka, Rami; Ramanujan, R V

2010-11-01

Truncated nanocubes of barium titanate (BT) were synthesized using a rapid, facile microwave-assisted hydrothermal route. Stoichiometric composition of pellets of nanocube BT powders was prepared by two-stage microwave process. Characterization by powder XRD, Rietveld refinement, SEM, TEM, and dielectric and polarization measurements was performed. X-ray diffraction revealed a polymorphic transformation from cubic Pm3̅m to tetragonal P4mm after 15 min of microwave irradiation, arising from titanium displacement along the c-axis. Secondary electron images were examined for nanocube BT synthesis and annealed at different timings. Transmission electron microscopy showed a narrow particle size distribution with an average size of 70 ± 9 nm. The remanence and saturation polarization were 15.5 ± 1.6 and 19.3 ± 1.2 μC/cm(2), respectively. A charge storage density of 925 ± 47 nF/cm(2) was obtained; Pt/BT/Pt multilayer ceramic capacitor stack had an average leakage current density of 5.78 ± 0.46 × 10(-8) A/cm(2) at ±2 V. The significance of this study shows an inexpensive and facile processing platform for synthesis of high-k dielectric for charge storage applications.

Solvent-free, microwave-assisted synthesis of thiophene oligomers via Suzuki coupling.

PubMed

Melucci, Manuela; Barbarella, Giovanna; Sotgiu, Giovanna

2002-12-13

The purpose of this study was to obtain a rapid, efficient, and environmentally friendly methodology for the synthesis of highly pure thiophene oligomers. The solvent-free, microwave-assisted coupling of thienyl boronic acids and esters with thienyl bromides, using aluminum oxide as the solid support, allowed us to rapidly check the reaction trends on changing times, temperature, catalyst, and base and easily optimize the experimental conditions to obtain the targeted product in fair amounts. This procedure offers a novel, general, and very rapid route to the preparation of soluble thiophene oligomers. Thus, for example, quaterthiophene was obtained in 6 min by reaction of 2-bromo-2,2'-bithiophene with bis(pinacolato)diboron (isolated yield 65%), whereas quinquethiophene was obtained in 11 min by reaction of dibromoterthiophene with thienylboronic acid (isolated yield 74%). The synthesis of new chiral 2,2'-bithiophenes is reported. The detailed analysis of the byproducts of some reactions allowed us to elucidate a few aspects of reaction mechanisms. While the use of microwaves proved to be very convenient for the coupling between conventional thienyl moieties, the same was not true for the coupling of thienyl rings to thienyl-S,S-dioxide moieties. Indeed, in this case, the targeted product was obtained in low yields because of the competitive, accelerated, Diels-Alder reaction that affords a variety of condensation products.

Synthesis, growth and characterization of ZnO microtubes using a traveling-wave mode microwave system

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

Al-Naser, Qusay A.H.; Zhou, Jian, E-mail: jianzhou@whut.edu.cn; Wang, Han

Highlights: • ZnO microtubes were successfully synthesized within 15 min. • Introducing a design of a traveling-wave mode microwave system. • Growth temperature of ZnO microtubes becomes predominant between 1350 °C and 1400 °C. • ZnO microtube showed a strong ultraviolet and a weak and broad green emission. • ZnO microtube is composed only of ZnO with high crystallinity. - Abstract: Field emission scanning electron microscopy (FESEM) investigation reveals that zinc oxide (ZnO) microtubes have been successfully synthesized via a traveling-wave mode microwave system. These products are hexagonal tubular crystals with an average diameter of 60 μm and 250 μmmore » in length, having a well faceted end and side surfaces. The wall thickness of the ZnO tubes is about 3–5 μm. The influence of reaction temperature on the formation of crystalline ZnO hexagonal tubes is studied. Room temperature photoluminescence (PL) spectra have also been examined to explore the optical property which exhibits strong ultraviolet emission at 377.422 nm and a weak and broad green emission band at 587.548 nm. X-ray diffraction (XRD) and energy dispersive spectrometer (EDS) show that the product is composed only of ZnO with high crystallinity. The presented synthesis method possesses several advantages, which would be significant to the deeper study and wide applications of ZnO tubes in the future.« less

Microwave and continuous flow technologies in drug discovery.

PubMed

Sadler, Sara; Moeller, Alexander R; Jones, Graham B

2012-12-01

Microwave and continuous flow microreactors have become mainstream heating sources in contemporary pharmaceutical company laboratories. Such technologies will continue to benefit from design and engineering improvements, and now play a key role in the drug discovery process. The authors review the applications of flow- and microwave-mediated heating in library, combinatorial, solid-phase, metal-assisted, and protein chemistries. Additionally, the authors provide a description of the combination of microwave and continuous flow platforms, with applications in the preparation of radiopharmaceuticals and in drug candidate development. Literature reviewed is chiefly 2000 - 2012, plus key citations from earlier reports. With the advent of microwave irradiation, reactions that normally took days to complete can now be performed in a matter of minutes. Coupled with the introduction of continuous flow microreactors, pharmaceutical companies have an easy way to improve the greenness and efficiency of many synthetic operations. The combined force of these technologies offers the potential to revolutionize discovery and manufacturing processes.

Microwave-assisted synthesis of N-pyrazole ureas and the p38alpha inhibitor BIRB 796 for study into accelerated cell ageing.

PubMed

Bagley, Mark C; Davis, Terence; Dix, Matthew C; Widdowson, Caroline S; Kipling, David

2006-11-21

Microwave irradiation of substituted hydrazines and beta-ketoesters gives 5-aminopyrazoles in excellent yield, which can be transformed to the corresponding N-carbonyl derivatives by treatment with an isocyanate or chloroformate. Derivatization of 4-nitronaphth-1-ol using predominantly microwave heating methods and reaction with an N-pyrazole carbamate provides a rapid route to the N-pyrazole urea BIRB 796 in high purity, as a potent and selective inhibitor of p38alpha mitogen-activated protein kinase for the study of accelerated ageing in Werner syndrome cells.

Microwave-assisted ignition

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

Bechtold, J.K.; Booty, M.R.; Kriegsmann, G.A.

1996-12-31

In recent years, microwave heating has been proposed as an alternative to ignite materials during the process of self-propagating high-temperature synthesis. The microwave heating and ignition of a combustible material is modeled and analyzed in the small Biot number and large activation energy regimes. Both the temporal and spatial evolution of the temperature within the material are described. The ignition characteristics are determined by a localized equation for the perturbation to the inert temperature, which is shown to exhibit thermal runaway behavior. Analysis of this local equation provides explicit ignition conditions in terms of the physical parameters in the problem.

Integrated Electrochemical Processes for CO 2 Capture and Conversion to Commodity Chemicals

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

Hatton, T. Alan; Jamison, Timothy

2013-09-30

The Massachusetts Institute of Technology (MIT) and Siemens Corporations (SCR) are developing new chemical synthesis processes for commodity chemicals from CO 2. The process is assessed as a novel chemical sequestration technology that utilizes CO 2 from dilute gas streams generated at industrial carbon emitters as a raw material to produce useful commodity chemicals. Work at Massachusetts Institute of Technology (MIT) commenced on October 1st, 2010, and finished on September 30th, 2013. During this period, we have investigated and accomplished five objectives that mainly focused on converting CO 2 into high-value chemicals: 1) Electrochemical assessment of catalytic transformation of COmore » 2 and epoxides to cyclic carbonates; 2) Investigation of organocatalytic routes to convert CO 2 and epoxide to cyclic carbonates; 3) Investigation of CO 2 Capture and conversion using simple olefins under continuous flow; 4) Microwave assisted synthesis of cyclic carbonates from olefins using sodium bicarbonates in a green pathway; 5) Life cycle analyses of integrated chemical sequestration process. In this final report, we will describe the detailed study performed during the three year period and findings and conclusions drawn from our research.« less

Structural, chemical and optical properties of SnO2 NPs obtained by three different synthesis routes

NASA Astrophysics Data System (ADS)

Drzymała, Elżbieta; Gruzeł, Grzegorz; Depciuch, Joanna; Budziak, Andrzej; Kowal, Andrzej; Parlinska-Wojtan, Magdalena

2017-08-01

Polyol (P), chemical precipitation (C) and microwave-assisted (M) syntheses were chosen to produce SnO2 nanoparticles with uniform size and minimum agglomeration. Their structural, chemical and optical properties were investigated using dynamic light scattering (DLS), scanning transmission electron microscopy (STEM), Raman, Fourier Transform Infrared (FTIR) using the Attenuated Total Reflectance (ATR) technique and Ultraviolet-Visible (UV-Vis) spectroscopies. STEM observations showed that the SnO2(P) and SnO2(C) nanoparticles (NPs) are combined into larger agglomerates with heterogeneous thickness, while the microwave-assisted NPs form a uniform thin layer across the TEM grid. The strongest agglomeration of the SnO2(C) NPs, observed by DLS, STEM and UV-Vis is explained by the very moderate amount of water present on the surface of the NPs identified by FTIR spectroscopy. High resolution STEM combined with SAED and X-ray diffraction (XRD) patterns confirmed the crystalline character of the NPs. In the nanoparticles from polyol synthesis, chlorine from the remains of metal precursors during reduction was detected by energy dispersive spectroscopy (EDS), contrary to the NPs obtained by the chemical precipitation and microwave-assisted methods. All three syntheses routes lead to small, 2-10 nm SnO2 NPs, which were the result of the low concentration of Cl ions in the solutions.

Microwave assisted synthesis, characterization and biocidal activities of some new chelates of carbazole derived Schiff bases of cadmium and tin metals

NASA Astrophysics Data System (ADS)

Yadav, Manju; Mishra, Neelima; Sharma, Nutan; Chandra, Sulekh; Kumar, Dinesh

2014-11-01

This study is planned to report the advancement of green microwave approach in the fabrication of a new series of biologically potent (N^X, where X = O/S) donor Schiff bases and their cadmium(II) and tin(II) complexes. The ligands and their metal complexes have been characterized in terms of elemental analysis, molar ionic conductance, magnetic moment and spectral (IR, UV-Vis, NMR (1H, 119Sn), FAB-mass, thermal and XRD) data. The data revealed that the ligands coordinated to the metal center via nitrogen and oxygen/sulfur atoms and form an octahedral arrangement of the ligands around central metal atom. All compounds were evaluated for their in vitro antimicrobial activities against two pathogenic bacteria Bacillus subtilis and Escherichia coli and two fungi Aspergillus niger and Aspergillus flavus by standard disc diffusion method. The discs were stored in an incubator at 37 °C. The compounds were dissolved in DMF at 500 and 1000 ppm concentrations for screening biocidal activity. The compounds were dissolved in DMF to get the 100 and 200 ppm concentration of test solutions for screening fungicidal activity. The inhibition zone around each disc was measured (in mm) after 24 h and 96 h for biocidal and fungicidal activities respectively.

Influence of Polarity and Activation Energy in Microwave–Assisted Organic Synthesis (MAOS)

PubMed Central

Rodríguez, Antonio M; Prieto, Pilar; de la Hoz, Antonio; Díaz-Ortiz, Ángel; Martín, D Raúl; García, José I

2015-01-01

The aim of this work was to determine the parameters that have decisive roles in microwave-assisted reactions and to develop a model, using computational chemistry, to predict a priori the type of reactions that can be improved under microwaves. For this purpose, a computational study was carried out on a variety of reactions, which have been reported to be improved under microwave irradiation. This comprises six types of reactions. The outcomes obtained in this study indicate that the most influential parameters are activation energy, enthalpy, and the polarity of all the species that participate. In addition to this, in most cases, slower reacting systems observe a much greater improvement under microwave irradiation. Furthermore, for these reactions, the presence of a polar component in the reaction (solvent, reagent, susceptor, etc.) is necessary for strong coupling with the electromagnetic radiation. We also quantified that an activation energy of 20–30 kcal mol−1 and a polarity (μ) between 7–20 D of the species involved in the process is required to obtain significant improvements under microwave irradiation. PMID:26246993

Quinazoline derivatives: synthesis and bioactivities

PubMed Central

2013-01-01

Owing to the significant biological activities, quinazoline derivatives have drawn more and more attention in the synthesis and bioactivities research. This review summarizes the recent advances in the synthesis and biological activities investigations of quinazoline derivatives. According to the main method the authors adopted in their research design, those synthetic methods were divided into five main classifications, including Aza-reaction, Microwave-assisted reaction, Metal-mediated reaction, Ultrasound-promoted reaction and Phase-transfer catalysis reaction. The biological activities of the synthesized quinazoline derivatives also are discussed. PMID:23731671

Ultra-Fast Microwave Synthesis of ZnO Nanorods on Cellulose Substrates for UV Sensor Applications

PubMed Central

Pimentel, Ana; Samouco, Ana; Araújo, Andreia; Martins, Rodrigo; Fortunato, Elvira

2017-01-01

In the present work, tracing and Whatman papers were used as substrates to grow zinc oxide (ZnO) nanostructures. Cellulose-based substrates are cost-efficient, highly sensitive and environmentally friendly. ZnO nanostructures with hexagonal structure were synthesized by hydrothermal under microwave irradiation using an ultrafast approach, that is, a fixed synthesis time of 10 min. The effect of synthesis temperature on ZnO nanostructures was investigated from 70 to 130 °C. An Ultra Violet (UV)/Ozone treatment directly to the ZnO seed layer prior to microwave assisted synthesis revealed expressive differences regarding formation of the ZnO nanostructures. Structural characterization of the microwave synthesized materials was carried out by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The optical characterization has also been performed. The time resolved photocurrent of the devices in response to the UV turn on/off was investigated and it has been observed that the ZnO nanorod arrays grown on Whatman paper substrate present a responsivity 3 times superior than the ones grown on tracing paper. By using ZnO nanorods, the surface area-to-volume ratio will increase and will improve the sensor sensibility, making these types of materials good candidates for low cost and disposable UV sensors. The sensors were exposed to bending tests, proving their high stability, flexibility and adaptability to different surfaces. PMID:29140304

Microwave-assisted rapid synthesis of birnessite-type MnO{sub 2} nanoparticles for high performance supercapacitor applications

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

Zhang, Xiong; Miao, Wang; Li, Chen

Highlights: • Birnessite-type MnO{sub 2} nanoparticles were prepared by the microwave-assisted reflux. • The microwave reaction duration was only 5 min. • A specific capacitance of 329 F g{sup −1} was obtained for birnessite-type MnO{sub 2}. - Abstract: Birnessite-type MnO{sub 2} nanoparticles have been successfully synthesized by the microwave-assisted reflux as short as 5 min. The microstructure and morphology of the products were characterized by X-ray diffraction, N{sub 2} adsorption–desorption isotherms, scanning electron microscopy, transmission electron microscopy. The electrochemical properties of the as-prepared MnO{sub 2} as an electrode material for supercapacitor were investigated by cyclic voltammetry and galvanostatic charge-discharge measurementsmore » in 1 M Na{sub 2}SO{sub 4} electrolyte, and a high specific capacitance of 329 F g{sup −1} was achieved at a current density of 0.2 A g{sup −1}. The specific capacitance retention was 92% after 1000 cycles at 2 A g{sup −1}, suggesting that it is a promising electrode material for supercapacitors.« less

MICROWAVES IN GREEN AND SUSTAINABLE CHEMISTRY

EPA Science Inventory

In this chapter, we have outlined roles of microwave chemistry in the establishment of green and sustainable chemistry. Many examples, mostly from the authors' laboratories, have been presented of green microwave processes under solvent-free conditions or with solvents, including...

Green and energy-efficient methods for the production of metallic nanoparticles

PubMed Central

Naghdi, Mitra; Taheran, Mehrdad; Verma, M; Surampalli, R Y; Valero, J R

2015-01-01

Summary In the last decade, researchers paid great attention to the concept of “Green Chemistry”, which aims at development of efficient methods for the synthesis of nanoparticles (NPs) in terms of the least possible impact on human life and environment. Generally, several reagents including precursors, reducing agents, stabilizing agents and solvents are used for the production of NPs and in some cases, energy is needed to reach the optimum temperature for reduction. Therefore, to develop a green approach, researchers had the opportunity to investigate eco-friendly reagents and new energy transfer techniques. In order to substitute the harmful reagents with green ones, researchers worked on different types of saccharides, polyols, carboxylic acids, polyoxometalates and extracts of various plants that can play the role of reducers, stabilizers or solvents. Also, there are some reports on using ultraviolet (UV), gamma and microwave irradiation that are capable of reducing and provide uniform heating. According to the literature, it is possible to use green reagents and novel energy transfer techniques for production of NPs. However, these new synthesis routes should be optimized in terms of performance, cost, product quality (shape and size distribution) and scale-up capability. This paper presents a review on most of the employed green reagents and new energy transfer techniques for the production of metallic NPs. PMID:26734527

Green and energy-efficient methods for the production of metallic nanoparticles.

PubMed

Naghdi, Mitra; Taheran, Mehrdad; Brar, Satinder Kaur; Verma, M; Surampalli, R Y; Valero, J R

2015-01-01

In the last decade, researchers paid great attention to the concept of "Green Chemistry", which aims at development of efficient methods for the synthesis of nanoparticles (NPs) in terms of the least possible impact on human life and environment. Generally, several reagents including precursors, reducing agents, stabilizing agents and solvents are used for the production of NPs and in some cases, energy is needed to reach the optimum temperature for reduction. Therefore, to develop a green approach, researchers had the opportunity to investigate eco-friendly reagents and new energy transfer techniques. In order to substitute the harmful reagents with green ones, researchers worked on different types of saccharides, polyols, carboxylic acids, polyoxometalates and extracts of various plants that can play the role of reducers, stabilizers or solvents. Also, there are some reports on using ultraviolet (UV), gamma and microwave irradiation that are capable of reducing and provide uniform heating. According to the literature, it is possible to use green reagents and novel energy transfer techniques for production of NPs. However, these new synthesis routes should be optimized in terms of performance, cost, product quality (shape and size distribution) and scale-up capability. This paper presents a review on most of the employed green reagents and new energy transfer techniques for the production of metallic NPs.

Combining Sustainable Synthesis of a Versatile Ruthenium Dihydride Complex with Structure Determination Using Group Theory and Spectroscopy

ERIC Educational Resources Information Center

Armstrong, Christopher; Burnham, Jennifer A. J.; Warminski, Edward E.

2017-01-01

A good-yielding two-step synthesis of RuH[subscript 2](CO)(PPh[subscript 3])[subscript 3] using conventional or microwave-assisted reflux techniques is described for use in undergraduate teaching laboratories. RuH[subscript 2](CO)(PPh[subscript 3])[subscript 3] is synthesized from RuCl[subscript 3]·xH[subscript 2]O, PPh[subscript 3], and KOH in…

The effects of fuel type in synthesis of NiFe2O4 nanoparticles by microwave assisted combustion method

NASA Astrophysics Data System (ADS)

Karcıoğlu Karakaş, Zeynep; Boncukçuoğlu, Recep; Karakaş, İbrahim H.

2016-04-01

In this study, it was investigated the effects of the used fuels on structural, morphological and magnetic properties of nanoparticles in nanoparticle synthesis with microwave assisted combustion method with an important method in quick, simple and low cost at synthesis of the nanoparticles. In this aim, glycine, urea and citric acid were used as fuel, respectively. The synthesised nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer-Emmet-Teller surface area (BET), and vibrating sample magnetometry (VSM) techniques. We observed that fuel type is quite effective on magnetic properties and surface properties of the nanoparticles. X-ray difractograms of the obtained nanoparticles were compared with standard powder diffraction cards of NiFe2O4 (JCPDS Card Number 54-0964). The results demonstrated that difractograms are fully compatible with standard reflection peaks. According to the results of the XRD analysis, the highest crystallinity was observed at nanoparticles synthesized with glycine. The results demonstrated that the nanoparticles prepared with urea has the highest surface area. The micrographs of SEM showed that all of the nanoparticles have nano-crystalline behaviour and particles indication cubic shape. VSM analysis demonstrated that the type of fuel used for synthesis is highly effective a parameter on magnetic properties of nanoparticles.

Greener and Sustainable Trends in Synthesis of Organics and ...

EPA Pesticide Factsheets

Trends in greener and sustainable process development during the past 25 years are abridged involving the use of alternate energy inputs (mechanochemistry, ultrasound- or microwave irradiation), photochemistry, and greener reaction media as applied to synthesis of organics and nanomaterials. In the organic synthesis arena, examples comprise assembly of heterocyclic compounds, coupling and a variety of other name reactions catalyzed by basic water or recyclable magnetic nanocatalysts. Generation of nanoparticles benefits from the biomimetic approaches where vitamins, sugars, and plant polyphenols, including agricultural waste residues, can serve as reducing and capping agents. Metal nanocatalysts (Pd, Au, Ag, Ni, Ru, Ce, Cu, etc.) immobilized on biodegradable supports such as cellulose and chitosan, or on recyclable magnetic ferrites via ligands, namely dopamine or glutathione, are receiving special attention. These strategic approaches attempt to address most of the Green Chemistry Principles while producing functional chemicals with utmost level of waste minimization. Feature article for celebration of 25 years of Green Chemistry on invitation from American Chemical Society (ACS) journal, ACS Sustainable Chemistry & Engineering.

Microwave-assisted synthesis and electrochemical evaluation of VO 2 (B) nanostructures

DOE PAGES

Ashton, Thomas E.; Borras, David Hevia; Iadecola, Antonella; ...

2015-12-01

Understanding how intercalation materials change during electrochemical operation is paramount to optimising their behaviour and function and in situ characterisation methods allow us to observe these changes without sample destruction. Here, we first report the improved intercalation properties of bronze phase vanadium dioxide VO2 (B) prepared by a microwave assisted route which exhibits a larger electrochemical capacity (232 mAh g -1) compared to VO 2 (B) prepared by a solvothermal route (197 mAh g -1). These electrochemical differences have also been followed using in situ X-ray absorption spectroscopy allowing us to follow oxidation state changes as they occur during batterymore » operation.« less

Microwave-assisted deuterium exchange: the convenient preparation of isotopically labelled analogues for stable isotope dilution analysis of volatile wine phenols.

PubMed

Crump, Anna M; Sefton, Mark A; Wilkinson, Kerry L

2014-11-01

This study reports the convenient, low cost, one-step synthesis of labelled analogues of six volatile phenols, guaiacol, 4-methylguaiacol, 4-ethylguaiacol, 4-ethylphenol, eugenol and vanillin, using microwave-assisted deuterium exchange, for use as internal standards for stable isotope dilution analysis. The current method improves on previous strategies in that it enables incorporation of deuterium atoms on the aromatic ring, thereby ensuring retention of the isotope label during mass spectrometry fragmentation. When used as standards for SIDA, these labelled volatile phenols will improve the accuracy and reproducibility of quantitative food and beverage analysis. Copyright © 2014 Elsevier Ltd. All rights reserved.

Rapid, Microwave-Assisted Synthesis of Cubic, Three-Dimensional, Highly Porous MOF-205 for Room Temperature CO2 Fixation via Cyclic Carbonate Synthesis.

PubMed

Babu, Robin; Roshan, Roshith; Kathalikkattil, Amal Cherian; Kim, Dong Woo; Park, Dae-Won

2016-12-14

A dual-porous, three-dimensional, metal-organic framework [Zn 4 O(2,6-NDC)(BTB) 4/3 ] (MOF-205, BET = 4200 m 2 /g) has been synthesized using microwave power as an alternative energy source for the first time, and its catalytic activity has been exploited for CO 2 -epoxide coupling reactions to produce five-membered cyclic carbonates under solvent-free conditions. Microwave synthesis was performed at different time intervals to reveal the formation of the crystals. Significant conversion of various epoxides was obtained at room temperature, with excellent selectivity toward the desired five-membered cyclic carbonates. The importance of the dual porosity and the synergistic effect of quaternary ammonium salts on efficiently catalyzed CO 2 conversion were investigated using various experimental and physicochemical characterization techniques, and the results were compared with those of the solvothermally synthesized MOF-205 sample. On the basis of literature and experimental inferences, a rationalized mechanism mediated by the zinc center of MOF-205 for the CO 2 -epoxide cycloaddition reaction has been proposed.

Microwave assisted synthesis and characterization of magnesium substituted calcium phosphate bioceramics.

PubMed

Khan, Nida Iqbal; Ijaz, Kashif; Zahid, Muniza; Khan, Abdul S; Abdul Kadir, Mohammed Rafiq; Hussain, Rafaqat; Anis-Ur-Rehman; Darr, Jawwad A; Ihtesham-Ur-Rehman; Chaudhry, Aqif A

2015-11-01

Hydroxyapatite is used extensively in hard tissue repair due to its biocompatibility and similarity to biological apatite, the mineral component of bone. It differs subtly in composition from biological apatite which contains other ions such as magnesium, zinc, carbonate and silicon (believed to play biological roles). Traditional methods of hydroxyapatite synthesis are time consuming and require strict reaction parameter control. This paper outlines synthesis of magnesium substituted hydroxyapatite using simple microwave irradiation of precipitated suspensions. Microwave irradiation resulted in a drastic decrease in ageing times of amorphous apatitic phases. Time taken to synthesize hydroxyapatite (which remained stable upon heat treatment at 900°C for 1h) reduced twelve folds (to 2h) as compared to traditionally required times. The effects of increasing magnesium concentration in the precursors on particle size, surface area, phase-purity, agglomeration and thermal stability, were observed using scanning electron microscopy, BET surface area analysis, X-ray diffraction and photo acoustic Fourier transform infra-red spectroscopy. Porous agglomerates were obtained after a brief heat-treatment (1h) at 900°C. Copyright © 2015 Elsevier B.V. All rights reserved.

Microwave-Assisted Synthesis of Bio-Active Heterocycles and Fine Chemicals in Aqueous Media

EPA Science Inventory

Human health, especially in the aging population, mostly depends on various medicines, and researchers are combating against emerging diseases by new drug discovery. Heterocyclic compounds hold a special place among pharmaceutically active natural products as well as synthetic co...

MICROWAVE-ASSISTED SYNTHESIS OF NITROGEN AND OXYGEN CONTAINING HETEROCYCLES IN AQUEOUS MEDIUM

EPA Science Inventory

Pharmaceutical scientists are required to generate diverse arrays of complex targets in short periods of time. A primary driver of organic chemistry is, therefore, the development of efficient and environmentally benign synthetic protocols. This can be achieved via the selection ...

MICROWAVE-ASSISTED PREPARATION OF CYCLIC UREAS FROM DIAMINES

EPA Science Inventory

Rajender S. Varma* and Yong-Jin Kim
Cyclic ureas are useful intermediates for a variety of pharmaceuticals and pesticides. One of the attractive approaches for the synthesis of cyclic ureas uses condensation of diamines with urea as a carbonyl source under dynamic evacuation. ...

Microwave-assisted hydrothermal synthesis of marigold-like ZnIn{sub 2}S{sub 4} microspheres and their visible light photocatalytic activity

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

Chen Zhixin, E-mail: czx@fzu.edu.cn; Analysis and Test Center, Fuzhou University, Fuzhou 350002; Li Danzhen

Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a microwave-assisted hydrothermal method with the temperature ranging from 80 to 195 Degree-Sign C. X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen sorption analysis, UV-visible spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperatures were almost the same. The degradation of methyl orange (MO) under the visible light irradiation has been used as a probe reaction to investigate the photocatalytic activity of as-prepared ZnIn{sub 2}S{sub 4}, which shows that the ZnIn{sub 2}S{submore » 4} sample synthesized at 195 Degree-Sign C shows the best photocatalytic activity for MO degradation. In addition, the photocatalytic activities of all the samples prepared by the microwave-assisted hydrothermal method are better than those prepared by a normal hydrothermal method, which could be attributed to the formation of more defect sites during the microwave-assisted hydrothermal treatment. - Graphical abstract: Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a fast microwave-assisted hydrothermal method at 80-195 Degree-Sign C with a very short reaction time of 10 min. The as-prepared ZnIn{sub 2}S{sub 4} sample can be used as visible light photocatalyst for degradation of organic dyes. Highlights: Black-Right-Pointing-Pointer ZnIn{sub 2}S{sub 4} microspheres were synthesized by microwave-assisted hydrothermal method. Black-Right-Pointing-Pointer The crystal structure and optical property of the products were almost the same. Black-Right-Pointing-Pointer Increment of the temperature renders high surface area due to the bubbling effect. Black-Right-Pointing-Pointer The ZnIn{sub 2}S{sub 4} synthesized at 195 Degree-Sign C shows the best visible catalytic activity for MO.« less

Thermal and biological evolution of Fe(III)-Sulfanilamide complexes synthesized by green strategy

NASA Astrophysics Data System (ADS)

Prajapat, Garima; Rathore, Uma; Gupta, Rama; Bhojak, N.

2018-05-01

Sulfonamides belong to a category of sulfadrugs, that are widely used as antibiotic medicines. Their metal complexes, also called Metallodrugs, are known to have diverse pharmacological applications and are significantly used as therapeutic agents for treatment of several human diseases. Fe(III) complexes of two sulfonamides, namely Sulfanilamide and Sulfadiazine have been synthesized by the method of Microwave Assisted Organic Synthesis (MAOS), using acetone as solvent medium. Presence of excellent donor atoms such as N and O, induce these drugs to exhibit a chelating behavior with the metal ion, and to act as bidentate ligands. Both the complexes were found to have four coordinated, tetrahedral geometry with one molecule of water of crystallisation. Thermal decomposition studies were carried out in an inert nitrogen atmosphere by Thermogravimetric (TGA) and Derivative Thermogravimetric (DTA) analysis. Interpretation of thermograms have been done to evaluate various kinetic and thermodynamic parameters, using integral method of Coats and Redfern. The antibacterial activity for both complexes have been screened against E.coli, S. aureus and B. subtilis.

Facile and rapid one-pot microwave-assisted synthesis of Pd-Ni magnetic nanoalloys confined in mesoporous carbons

NASA Astrophysics Data System (ADS)

Martínez de Yuso, Alicia; Le Meins, Jean-Marc; Oumellal, Yassine; Paul-Boncour, Valérie; Zlotea, Claudia; Matei Ghimbeu, Camelia

2016-12-01

An easy and rapid one-pot microwave-assisted soft-template synthesis method for the preparation of Pd-Ni nanoalloys confined in mesoporous carbon is reported. This approach allows the formation of mesoporous carbon and the growth of the particles at the same time, under short microwave irradiation (4 h) compared to the several days spent for the classical approach. In addition, the synthesis steps are diminished and no thermopolymerization step or reduction treatment being required. The influence of the Pd-Ni composition on the particle size and on the carbon characteristics was investigated. Pd-Ni solid solutions in the whole composition range could be obtained, and the metallic composition proved to have an important effect on the nanoparticle size but low influence on carbon textural properties. Small and uniformly distributed nanoparticles were confined in mesoporous carbon with uniform pore size distribution, and dependence between the nanoparticle size and the nanoalloy composition was observed, i.e., increase of the particle size with increasing the Ni content (from 5 to 14 nm). The magnetic properties of the materials showed a strong nanoparticle size and/or composition effect. The blocking temperature of Pd-Ni nanoalloys increases with the increase of Ni amount and therefore of particle size. The magnetization values are smaller than the bulk counterpart particularly for the Ni-rich compositions due to the formed graphitic shells surrounding the particles inducing a dead magnetic layer.

A green approach toward quinoxalines and bis-quinoxalines and their biological evaluation against A431, human skin cancer cell lines.

PubMed

Bandyopadhyay, Debasish; Cruz, Jessica; Morales, Liza D; Arman, Hadi D; Cuate, Erica; Lee, Young S; Banik, Bimal K; Kim, Dae J

2013-08-01

The objective of this study was to develop a practical green procedure to synthesize quinoxalines and bis-quinoxalines and evaluate their inhibitory effects on the viability of A431 human epidermoid carcinoma cells. A series of quinoxaline and bis-quinoxaline derivatives have been designed and synthesized following a microwave-assisted and bismuth nitrate-catalyzed eco-friendly route. A detailed comparison has been made between microwave-induced protocol with the reactions occurred at room temperature. The structure of the compounds have been elucidated by various spectroscopic methods and finally confirmed by x-ray crystallographic analyses. Two quinoxaline derivatives, compounds 6 and 12 have demonstrated inhibitory effects on the viability of A431 human epidermoid carcinoma cells when compared with HaCaT nontumorigenic human keratinocyte cells. Notably, compound 6 inhibits Stat3 phosphorylation/activation in A431 skin cancer cells.

Bimetallic Nanoparticles as Efficient Catalysts: Facile and Green Microwave Synthesis

PubMed Central

Blosi, Magda; Ortelli, Simona; Costa, Anna Luisa; Dondi, Michele; Lolli, Alice; Andreoli, Sara; Benito, Patricia; Albonetti, Stefania

2016-01-01

This work deals with the development of a green and versatile synthesis of stable mono- and bi-metallic colloids by means of microwave heating and exploiting ecofriendly reagents: water as the solvent, glucose as a mild and non-toxic reducer and polyvinylpirrolidone (PVP) as the chelating agent. Particle size-control, total reaction yield and long-term stability of colloids were achieved with this method of preparation. All of the materials were tested as effective catalysts in the reduction of p-nitrophenol in the presence of NaBH4 as the probe reaction. A synergistic positive effect of the bimetallic phase was assessed for Au/Cu and Pd/Au alloy nanoparticles, the latter showing the highest catalytic performance. Moreover, monoand bi-metallic colloids were used to prepare TiO2- and CeO2-supported catalysts for the liquid phase oxidation of 5-hydroxymethylfufural (HMF) to 2,5-furandicarboxylic acid (FDCA). The use of Au/Cu and Au/Pd bimetallic catalysts led to an increase in FDCA selectivity. Finally, preformed Pd/Cu nanoparticles were incorporated into the structure of MCM-41-silica. The resulting Pd/Cu MCM-41 catalysts were tested in the hydrodechlorination of CF3OCFClCF2Cl to CF3OCF=CF2. The effect of Cu on the hydrogenating properties of Pd was demonstrated. PMID:28773672

Green Adeptness in the Synthesis and Stabilization of Copper Nanoparticles: Catalytic, Antibacterial, Cytotoxicity, and Antioxidant Activities

NASA Astrophysics Data System (ADS)

Din, Muhammad Imran; Arshad, Farhan; Hussain, Zaib; Mukhtar, Maria

2017-12-01

Copper nanoparticles (CuNPs) are of great interest due to their extraordinary properties such as high surface-to-volume ratio, high yield strength, ductility, hardness, flexibility, and rigidity. CuNPs show catalytic, antibacterial, antioxidant, and antifungal activities along with cytotoxicity and anticancer properties in many different applications. Many physical and chemical methods have been used to synthesize nanoparticles including laser ablation, microwave-assisted process, sol-gel, co-precipitation, pulsed wire discharge, vacuum vapor deposition, high-energy irradiation, lithography, mechanical milling, photochemical reduction, electrochemistry, electrospray synthesis, hydrothermal reaction, microemulsion, and chemical reduction. Phytosynthesis of nanoparticles has been suggested as a valuable alternative to physical and chemical methods due to low cytotoxicity, economic prospects, environment-friendly, enhanced biocompatibility, and high antioxidant and antimicrobial activities. The review explains characterization techniques, their main role, limitations, and sensitivity used in the preparation of CuNPs. An overview of techniques used in the synthesis of CuNPs, synthesis procedure, reaction parameters which affect the properties of synthesized CuNPs, and a screening analysis which is used to identify phytochemicals in different plants is presented from the recent published literature which has been reviewed and summarized. Hypothetical mechanisms of reduction of the copper ion by quercetin, stabilization of copper nanoparticles by santin, antimicrobial activity, and reduction of 4-nitrophenol with diagrammatic illustrations are given. The main purpose of this review was to summarize the data of plants used for the synthesis of CuNPs and open a new pathway for researchers to investigate those plants which have not been used in the past.

Microwave-assisted synthesis of gold, silver, platinum and palladium nanostructures and their use in electrocatalytic applications.

PubMed

Safavi, Afsaneh; Tohidi, Maryam

2014-09-01

Microwave-assisted ionic liquid method was used for synthesis of various noble metals, such as gold, silver, platinum and palladium nanomaterials. This route does not employ any template agent, surface capping agents or reducing agents. The process is fast, simple and of high yield. Different metal precursors in various ionic liquids media (1-butyl-3-methylimidazolium tetrafluoroborate, octyl pyridinium hexaflurophosphate and 1-octyl-3-methylimidazolium hexaflurophosphate) were applied to produce metal nanomaterials. Silver, platinium and palladium nanoparticles exhibit spherical morphology while nanosheets with high aspect ratio were obtained for gold. These metal nanostructures were incorporated into a carbon ionic liquid electrode to investigate their electrocatalytic properties. It was found that synthesis in different ionic liquids result in different activity. Excellent electrocatalytic effects toward adenine, hydrazine, formaldehyde and ethanol were observed for the modified electrodes with different nanoparticles synthesized in 1-butyl-3-methylimidazolium tetrafluoroborate. The high conductivity, large surface-to-volume ratio and active sites of nanosized metal particles are responsible for their electrocatalytic activity. In contrast, the carbon ionic liquid electrode modified with synthesized metal nanoparticles in octyl pyridinium hexaflurophosphate and 1-octyl-3-methylimidazolium hexaflurophosphate showed negligible activity for detection of these probes.

Microwave assisted synthesis of sheet-like Cu/BiVO{sub 4} and its activities of various photocatalytic conditions

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

Chen, Xi; College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006; Li, Li, E-mail: qqhrll@163.com

2015-09-15

The Cu/BiVO{sub 4} photocatalyst with visible-light responsivity was prepared by the microwave-assisted hydrothermal method. The phase structures, chemical composition and surface physicochemical properties were well-characterized via X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance absorption (UV–vis/DRS), scanning electron microscopy (SEM), and N{sub 2} adsorption–desorption tests. Results indicate that the crystal structure of synthetic composite materials is mainly monoclinic scheelite BiVO{sub 4}, which is not changed with the increasing doping amount of Cu. In addition, the presence of Cu not only enlarges the range of the composite materials under the visible-light response, but also increases the BET value significantly.more » Compared to pure BiVO{sub 4}, 1% Cu/BiVO{sub 4}-160 performs the highest photocatalytic activity to degrade methylene blue under the irradiation of ultraviolet, visible and simulated sunlight. In addition, the capture experiments prove that the main active species was superoxide radicals during photocatalytic reaction. Moreover, the 1% Cu/BiVO{sub 4}-160 composite shows good photocatalytic stability after three times of recycling. - Graphical abstract: A series of BiVO{sub 4} with different amounts of Cu doping were prepared by the microwave-assisted method, moreover, which performed the high photocatalytic activities to degrade methylene blue under multi-mode. - Highlights: • A series of Cu/BiVO{sub 4} with different amounts of Cu doping were prepared by microwave-assisted synthesis. • The morphologies of as-samples were different with the amount of Cu doping increased. • Compared with pure BiVO{sub 4}, as-Cu/BiVO{sub 4} showed stronger absorption in the visible light region obviously. • 1% Cu/BiVO{sub 4}-160 performed the high photocatalytic activities to degrade methylene blue under multi-mode. • OH{sup •} and h{sup +} both play important roles in the photocatalytic reaction.« less

Microwave-assisted rapid photocatalytic degradation of malachite green in TiO2 suspensions: mechanism and pathways.

PubMed

Ju, Yongming; Yang, Shaogui; Ding, Youchao; Sun, Cheng; Zhang, Aiqian; Wang, Lianhong

2008-11-06

Microwave-assisted photocatalytic (MPC) degradation of malachite green (MG) in aqueous TiO2 suspensions was investigated. A 20 mg/L sample of MG was rapidly and completely decomposed in 3 min with the corresponding TOC removal efficiency of about 85%. To gain insight into the degradation mechanism, both GC-MS and LC-ESI-MS/MS techniques were employed to identify the major intermediates of MG degradation, including N-demethylation intermediates [(p-dimethylaminophenyl)(p-methylaminophenyl)phenylmethylium (DM-PM), (p-methylaminophenyl)(p-methylaminophenyl)phenylmethylium (MM-PM), (p-methylaminophenyl)(p-aminophenyl)phenylmethylium (M-PM)]; a decomposition compound of the conjugated structure (4-dimethylaminobenzophenone (DLBP)); products resulting from the adduct reaction of hydroxyl radical; products of benzene removal; and other open-ring intermediates such as phenol, terephthalic acid, adipic acid, benzoic acid, etc. The possible degradation mechanism of MG included five processes: the N-demethylation process, adduct products of the hydroxyl radical, the breakdown of chromophores such as destruction of the conjugated structure intermediate, removal of benzene, and an open-ring reaction. To the best of our knowledge, it is the first time the whole MG photodegradation processes have been reported.

Microwave-Assisted Synthesis of Nano-materials in Aqueous

EPA Science Inventory

Whether it is termed a revolution or simply a continuous evolution, clearly development of new materials and their understanding on smaller and smaller length scale is at the root of progress in many areas of materials science.1 This is true in developing existing bulk materials...

Conversion of agricultural residues to carboxymethylcellulose and carboxymethylcellulose acetate

USDA-ARS?s Scientific Manuscript database

In view of continuing interest in the use of agricultural by-products, we have converted cellulose, wheat straw, barley straw, and rice hull into carboxymethylcellulose (CMC). Microwave-assisted synthesis was found to be a partly effective alternative to the conventional heating process. The CMC thu...

Novel polyurethanes from xylan and TDI: Preparation and characterization

USDA-ARS?s Scientific Manuscript database

In this work a novel polyurethane was developed involving xylan and tolylene-2,4-diisocyanate (TDI). Polymer synthesis was achieved via conventional heat or microwave-assisted reaction in dimethylsulfoxide. Because xylan has multiple OH groups on each polymer chain, the TDI/xylan molar ratio neede...

Microwave (MW) promoted high yield expedient synthesis of steryl ferulates--A class of novel biologically active compounds: A comparative study of their antioxidant activity with that of naturally occurring γ-oryzanol.

PubMed

Begum, Ashma; Borah, Preetismita; Chowdhury, Pritish

2016-03-01

Synthetic steryl ferulates [3-O-(trans-4-feruloyl)-sterols] are currently gaining considerable importance in recent years to be used as nutraceuticals and food additives as well as in pharmaceutical applications substituting γ-oryzanol - a class of naturally occurring steryl ferulates having potent antioxidant and other organoleptic properties. Considering the importance of this class of compounds coupled with green technology associated with microwave energy (MW) in organic synthesis, we report here an expedited and high yield synthesis of steryl ferulates from abundant steroids, viz., cholesterol, cholestanol, stigmasterol, stigmastanol, β-sitosterol, β-campesterol, β-campestanol and ergosterol applying MW energy in the crucial step of esterification process of sterols with trans-4-O-acetylferulic acid to furnish their esterified products, viz., 3-O-(trans-4-O-acetylferuloyl)-sterols for their eventual deprotection to their respective steryl ferulates. We further report an efficient and scalable process of producing acetylferulic acid. Testing of synthesized steryl ferulates against antioxidant assays has also been highlighted. Copyright © 2015 Elsevier Inc. All rights reserved.

Microwave optimization of mucilage extraction from Opuntia ficus indica Cladodes.

PubMed

Felkai-Haddache, Lamia; Dahmoune, Farid; Remini, Hocine; Lefsih, Khalef; Mouni, Lotfi; Madani, Khodir

2016-03-01

In this study, microwave-assisted extraction (MAE) of polysaccharides from Opuntia ficus indica Cladodes were investigated using response surface methodology (RSM). The effects of three extraction factors on the yield of mucilage were examined. The results indicated that the optimum extraction conditions were determined as follows: microwave power X1, 700 W; extraction time X2, 5.15 minand ratio water/raw material X3, 4.83 mL/g at fixed pH 11. Under these optimal extraction conditions, mucilage yield was found to be Y, 25.6%. A comparison between the model results and experimental data gave a high correlation coefficient (R(2)=0.88), adjusted coefficient (Radj=0.83) and low root mean square error (RMSE=2.45) and showed that the two models were able to predict a mucilage yield by green extraction microwave process. Copyright © 2015 Elsevier B.V. All rights reserved.

Microwave assisted scalable synthesis of titanium ferrite nanomaterials

NASA Astrophysics Data System (ADS)

Shukla, Abhishek; Bhardwaj, Abhishek K.; Singh, S. C.; Uttam, K. N.; Gautam, Nisha; Himanshu, A. K.; Shah, Jyoti; Kotnala, R. K.; Gopal, R.

2018-04-01

Titanium ferrite magnetic nanomaterials are synthesized by one-step, one pot, and scalable method assisted by microwave radiation. Effects of titanium content and microwave exposure time on size, shape, morphology, yield, bonding nature, crystalline structure, and magnetic properties of titanium ferrite nanomaterials are studied. As-synthesized nanomaterials are characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), Raman spectroscopy, transmission electron microscopy (TEM), and vibrating sample magnetometer measurements. XRD measurements depict the presence of two phases of titanium ferrite into the same sample, where crystallite size increases from ˜33 nm to 37 nm with the increase in titanium concentration. UV-Vis measurement showed broad spectrum in the spectral range of 250-600 nm which reveals that its characteristic peaks lie between ultraviolet and visible region; ATR-FTIR and Raman measurements predict iron-titanium oxide structures that are consistent with XRD results. The micrographs of TEM and selected area electron diffraction patterns show formation of hexagonal shaped particles with a high degree of crystallinity and presence of multi-phase. Energy dispersive spectroscopy measurements confirm that Ti:Fe compositional mass ratio can be controlled by tuning synthesis conditions. Increase of Ti defects into titanium ferrite lattice, either by increasing titanium precursor or by increasing exposure time, enhances its magnetic properties.

Synthesis of Illudinine from Dimedone.

PubMed

Morrison, Alec E; Hoang, Tung T; Birepinte, Mélodie; Dudley, Gregory B

2017-02-17

A total synthesis of the illudalane sesquiterpene illudinine was realized in eight steps and 14% overall yield from commercially available dimedone. The approach features tandem fragmentation/Knoevenagel-type condensation and microwave-assisted oxidative cycloisomerization to establish the isoquinoline core. Completion of the synthesis involves a recently reported cascade S N Ar/Lossen rearrangement on a densely functionalized aryl bromide and an optimized procedure for O-methylation of 8-hydroxyisoquinolines. The oxidative cycloisomerization proceeds by way of a novel inverse-demand intramolecular dehydro-Diels-Alder cycloaddition, which has a potentially broader appeal for preparing substituted isoquinolines.

The Catalytic Enantioselective Total Synthesis of (+)-Liphagal**

PubMed Central

Day, Joshua J.; McFadden, Ryan M.; Virgil, Scott C.; Kolding, Helene; Alleva, Jennifer L.; Stoltz, Brian M.

2012-01-01

Ring a ding: The first catalytic enantioselective total synthesis of the meroterpenoid natural product (+)-liphagal is disclosed. The approach showcases a variety of technology including enantioselective enolate alkylation, a photochemical alkyne-alkene [2+2] reaction, microwave-assisted metal catalysis, and an intramolecular aryne capture cyclization reaction. Pivotal to the successful completion of the synthesis was a sequence involving ring expansion from a [6-5-4] tricycle to a [6-7] bicyclic core followed by stereoselective hydrogenation of a sterically occluded tri-substituted olefin to establish the trans homodecalin system found in the natural product. PMID:21671325

Microwave assisted synthesis of camellia oleifera shell-derived porous carbon with rich oxygen functionalities and superior supercapacitor performance

NASA Astrophysics Data System (ADS)

Liang, Jiyuan; Qu, Tingting; Kun, Xiang; Zhang, Yu; Chen, Shanyong; Cao, Yuan-Cheng; Xie, Mingjiang; Guo, Xuefeng

2018-04-01

Biomass-derived carbon (BDCs) materials are receiving extensive attention as electrode materials for energy storage because of the considerable economic value offering possibility for practical applications, but the electrochemical capacitance of BDCs are usually relatively low resulted from limited electric double layer capacitance. Herein, an oxygen-rich porous carbon (KMAC) was fabricated through a rapid and convenient microwave assisted carbonization and KOH activation of camellia oleifera shell. The obtained KMAC possesses three-dimensional porous architecture, large surface area (1229 m2/g) and rich oxygen functionalities (C/O ratio of 1.66). As the electrode materials for supercapacitor, KMAC exhibits superior supercapacitive performances as compared to the activated carbon (KAC) derived from direct carbonization/KOH activation method in 2.0 M H2SO4 (315 F/g vs. 202 F/g) and 6.0 M KOH (251 F/g vs. 214 F/g) electrolyte due to the rich oxygen-containing functional groups on the surface of porous carbon resulted from the developed microwave-assisted carbonization/activation approach.

Investigations on structural and optical properties of starch capped ZnS nanoparticles synthesized by microwave irradiation method

NASA Astrophysics Data System (ADS)

Lalithadevi, B.; Mohan Rao, K.; Ramananda, D.

2018-05-01

Following a green synthesis method, zinc sulfide (ZnS) nanoparticles were prepared by chemical co-precipitation technique using starch as capping agent. Microwave irradiation was used as heating source. X-ray diffraction studies indicated that nanopowders obtained were polycrystalline possessing ZnS simple cubic structure. Transmission electron microscopic studies indicated that starch limits the agglomeration by steric stabilization. Interaction between ZnS and starch was confirmed by Fourier transform infrared spectroscopy as well as Raman scattering studies. Quantum size effects were observed in optical absorption studies while quenching of defect states on nanoparticles was improved with increase in starch addition as indicated by photoluminescence spectra.

TANDEM BIS-ALDOL REACTION OF KETONES: A FACILE ONE-POT SYNTHESIS OF 1,3-DIOXANES IN AQUEOUS MEDIUM

EPA Science Inventory

A novel tandem bis-aldol reaction of ketone with paraformaldehyde catalyzed by polystyrenesulfonic acid in aqueous medium delivers 1,3-dioxanes in high yield. This one pot, operationally simple microwave-assisted synthetic protocol proceeds efficiently in water in the absence of ...

Nano-organocatalyst: Magnetically retrievable ferrite-anchored glutathione for microwave-assisted Paal-Knorr reaction, Aza-Michael addition and pyrazole synthesis

EPA Science Inventory

Postsynthetic surface modification of magnetic nanoparticles by glutathione imparts desirable chemical functionality and enables the generation of catalytic sites on the surfaces of ensuing organocatalysts. In this article, we discuss the developments, unique activity and high s...

Electrochemically exfoliated graphene as a novel microwave susceptor: the ultrafast microwave-assisted synthesis of carbon-coated silicon-graphene film as a lithium-ion battery anode.

PubMed

Kim, Jong Min; Ko, Dongjin; Oh, Jiseop; Lee, Jeongyeon; Hwang, Taejin; Jeon, Youngmoo; Hooch Antink, Wytse; Piao, Yuanzhe

2017-10-19

Graphene nanocomposites have attracted much attention in many applications due to their superior properties. However, preparing graphene nanocomposites requires a time-consuming thermal treatment to reduce the graphene or synthesize nanomaterials, in most cases. We present an ultrafast synthesis of a carbon-coated silicon-graphene nanocomposite using a commercial microwave system. Electrochemically exfoliated graphene is used as a novel microwave susceptor to deliver efficient microwave energy conversion. Unlike graphene oxide, it does not require a time-consuming pre-thermal reduction or toxic chemical reduction to absorb microwave radiation efficiently. A carbon-coated silicon nanoparticle-electrochemically exfoliated graphene nanocomposite film was prepared by a few seconds' microwave irradiation. The sp 2 domains of graphene absorb microwave radiation and generate heat to simultaneously reduce the graphene and carbonize the polydopamine carbon precursor. The as-prepared N-doped carbon-coated silicon-graphene film was used as a lithium-ion battery anode. The N-doped carbon coating decreases the contact resistance between silicon nanoparticles and graphene provides a wide range conductive network. Consequently, it exhibited a reversible capacity of 1744 mA h g -1 at a current density of 0.1 A g -1 and 662 mA h g -1 at 1.0 A g -1 after 200 cycles. This method can potentially be a general approach to prepare various graphene nanocomposites in an extremely short time.

Ultrasound-assisted microwave preparation of Ag-doped CdS nanoparticles.

PubMed

Ma, Jun; Tai, Guo'an; Guo, Wanlin

2010-03-01

Ag-doped CdS nanoparticles were synthesized by an ultrasound-assisted microwave synthesis method. The X-ray diffraction patterns reveal a structural evolution from cubic to hexagonal with increasing molar ratios of Ag(+)/Cd(2+) from 0% to 5%. It shows that the Ag-doped hexagonal CdS nanoparticles are polycrystal. The X-ray photoelectron spectroscopy of the CdS nanoparticles doping with 5% Ag(+) shows that the doped Ag in CdS is metallic. Simultaneously, the characteristic Raman peaks of the CdS nanoparticles enhance with increasing Ag(+) concentrations. The photocatalytic activity of different Ag-doped samples show a reasonable change due to different ratios of Ag which doped into CdS. Copyright 2009 Elsevier B.V. All rights reserved.

Rapid synthesis of graft copolymers from natural cellulose fibers.

PubMed

Thakur, Vijay Kumar; Thakur, Manju Kumari; Gupta, Raju Kumar

2013-10-15

Cellulose is the most abundant natural polysaccharide polymer, which is used as such or its derivatives in a number of advanced applications, such as in paper, packaging, biosorption, and biomedical. In present communication, in an effort to develop a proficient way to rapidly synthesize poly(methyl acrylate)-graft-cellulose (PMA-g-cellulose) copolymers, rapid graft copolymerization synthesis was carried out under microwave conditions using ferrous ammonium sulfate-potassium per sulfate (FAS-KPS) as redox initiator. Different reaction parameters such as microwave radiation power, ratio of monomer, solvent and initiator concentrations were optimized to get the highest percentage of grafting. Grafting percentage was found to increase with increase in microwave power up to 70%, and maximum 36.73% grafting was obtained after optimization of all parameters. Fourier transforms infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA/DTA/DTG) analysis were used to confirm the graft copolymerization of poly(methyl acrylate) (PMA) onto the mercerized cellulose. The grafted cellulosic polymers were subsequently subjected to the evaluation of different physico-chemical properties in order to access their application in everyday life, in a direction toward green environment. The grafted copolymers demonstrated increased chemical resistance, and higher thermal stability. Published by Elsevier Ltd.

Eco-friendly microwave-assisted protocol to prepare hyaluronan-fatty acid conjugates and to induce their self-assembly process.

PubMed

Calce, Enrica; Mercurio, Flavia Anna; Leone, Marilisa; Saviano, Michele; De Luca, Stefania

2016-06-05

An environmentally sustainable and energy-efficient synthetic process has been developed to prepare hyaluronan-based nano-sized material. It consists in a microwave-promoted acylation of the hydroxyl function of the polysaccharide with natural fatty acids, performed under solvent-free conditions. The efficient interaction of the solid reagents with the MW radiation accounts for the obtained high yielded products. The self-assembly process of the obtained compounds very fast occurred in an aqueous medium under MW-radiation, thus allowing the development of a green protocol for the nano-particles preparation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microwave-assisted synthesis of C-doped TiO2 and ZnO hybrid nanostructured materials as quantum-dots sensitized solar cells

NASA Astrophysics Data System (ADS)

Rangel-Mendez, Jose R.; Matos, Juan; Cházaro-Ruiz, Luis F.; González-Castillo, Ana C.; Barrios-Yáñez, Guillermo

2018-03-01

The microwave-assisted solvothermal synthesis of C-doped TiO2 and ZnO hybrid materials was performed. Saccharose, titanium isopropoxide and zinc acetate were used as organic and inorganic sources for the synthesis. The influence of temperature and reaction time on the textural and optoelectronic properties of the hybrid materials was verified. Carbon quantum-dots of TiO2 and ZnO nanostructured spheres were obtained in a second pot by controlled calcination steps of the precursor hybrid materials. A carefully characterization by adsorption-desorption N2 isotherms, XRD, XPS, SEM, UV-vis/DR and electro- and photo-electrochemistry properties of the carbon quantum-dots TiO2 and ZnO spheres was performed. The photoelectrochemical activity of TiO2-C and ZnO-C films proved to be dependent on the conditions of synthesis. It was found a red-shift in the energy band gap of the semiconductors with values of 3.02 eV and 3.13 eV for the TiO2-C and ZnO-C, respectively, clearly lower than those on bare semiconductors, which is associated with the C-doping effect. From the photo-electrochemistry characterization of C-doped TiO2 and ZnO films can be concluded that the present materials have potential applications as photoelectrodes for quantum-dots sensitized solar cells.

Microwave-assisted solid-phase peptide synthesis of the 60-110 domain of human pleiotrophin on 2-chlorotrityl resin.

PubMed

Friligou, Irene; Papadimitriou, Evangelia; Gatos, Dimitrios; Matsoukas, John; Tselios, Theodore

2011-05-01

A fast and efficient microwave-assisted solid phase peptide synthesis (MW-SPPS) of a 51mer peptide, the main heparin-binding site (60-110) of human pleiotrophin (hPTN), using 2-chlorotrityl chloride resin (CLTR-Cl) following the 9-fluorenylmethyloxycarbonyl/tert-butyl (Fmoc/tBu) methodology and with the standard N,N'-diisopropylcarbodiimide/1-hydroxybenzotriazole (DIC/HOBt) coupling reagents, is described. An MW-SPPS protocol was for the first time successfully applied to the acid labile CLTR-Cl for the faster synthesis of long peptides (51mer peptide) and with an enhanced purity in comparison to conventional SPPS protocols. The synthesis of such long peptides is not trivial and it is generally achieved by recombinant techniques. The desired linear peptide was obtained in only 30 h of total processing time and in 51% crude yield, in which 60% was the purified product obtained with 99.4% purity. The synthesized peptide was purified by reversed phase high performance liquid chromatography (RP-HPLC) and identified by electrospray ionization mass spectrometry (ESI-MS). Then, the regioselective formation of the two disulfide bridges of hPTN 60-110 was successfully achieved by a two-step procedure, involving an oxidative folding step in dimethylsulfoxide (DMSO) to form the Cys(77)-Cys(109) bond, followed by iodine oxidation to form the Cys(67)-Cys(99) bond.

Simultaneous extraction, identification and quantification of phenolic compounds in Eclipta prostrata using microwave-assisted extraction combined with HPLC-DAD-ESI-MS/MS.

PubMed

Fang, Xinsheng; Wang, Jianhua; Hao, Jifu; Li, Xueke; Guo, Ning

2015-12-01

A simple and rapid method was developed using microwave-assisted extraction (MAE) combined with HPLC-DAD-ESI-MS/MS for the simultaneous extraction, identification, and quantification of phenolic compounds in Eclipta prostrata, a common herb and vegetable in China. The optimized parameters of MAE were: employing 50% ethanol as solvent, microwave power 400 W, temperature 70 °C, ratio of liquid/solid 30 mL/g and extraction time 2 min. Compared to conventional extraction methods, the optimized MAE can avoid the degradation of the phenolic compounds and simultaneously obtained the highest yields of all components faster with less consumption of solvent and energy. Six phenolic acids, six flavonoid glycosides and one coumarin were firstly identified. The phenolic compounds were quantified by HPLC-DAD with good linearity, precision, and accuracy. The extract obtained by MAE showed significant antioxidant activity. The proposed method provides a valuable and green analytical methodology for the investigation of phenolic components in natural plants. Copyright © 2015 Elsevier Ltd. All rights reserved.

A green surfactant-assisted synthesis of hierarchical TS-1 zeolites with excellent catalytic properties for oxidative desulfurization.

PubMed

Du, Shuting; Li, Fen; Sun, Qiming; Wang, Ning; Jia, Mingjun; Yu, Jihong

2016-02-25

Hierarchical TS-1 zeolites with uniform intracrystalline mesopores have been successfully synthesized through the hydrothermal method by using the green and cheap surfactant Triton X-100 as the mesoporous template. The resultant materials exhibit remarkably enhanced catalytic activity in oxidative desulfurization reactions compared to the conventional TS-1 zeolite.

Microwave assisted synthesis, characterization and biocidal activities of some new chelates of carbazole derived Schiff bases of cadmium and tin metals.

PubMed

Yadav, Manju; Mishra, Neelima; Sharma, Nutan; Chandra, Sulekh; Kumar, Dinesh

2014-11-11

This study is planned to report the advancement of green microwave approach in the fabrication of a new series of biologically potent (N^X, where X=O/S) donor Schiff bases and their cadmium(II) and tin(II) complexes. The ligands and their metal complexes have been characterized in terms of elemental analysis, molar ionic conductance, magnetic moment and spectral (IR, UV-Vis, NMR ((1)H, (119)Sn), FAB-mass, thermal and XRD) data. The data revealed that the ligands coordinated to the metal center via nitrogen and oxygen/sulfur atoms and form an octahedral arrangement of the ligands around central metal atom. All compounds were evaluated for their in vitro antimicrobial activities against two pathogenic bacteria Bacillus subtilis and Escherichia coli and two fungi Aspergillus niger and Aspergillus flavus by standard disc diffusion method. The discs were stored in an incubator at 37°C. The compounds were dissolved in DMF at 500 and 1000 ppm concentrations for screening biocidal activity. The compounds were dissolved in DMF to get the 100 and 200 ppm concentration of test solutions for screening fungicidal activity. The inhibition zone around each disc was measured (in mm) after 24 h and 96 h for biocidal and fungicidal activities respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Novel benzothiophene 1,1-dioxide deoxygenation path for the microwave-assisted synthesis of substituted benzothiophene-fused pyrrole derivatives.

PubMed

Karakuş, Hamza; Dürüst, Yaşar

2017-02-01

The reaction of C-(4-substituted-phenyl)-N-(benzoyl)-N-methylglycines with benzo[b]thiophene 1,1-dioxide unexpectedly gave benzothiophene-fused pyrrole derivatives in toluene under microwave irradiation via a cycloaddition and metal-free Pummerer-type sulfone deoxygenation path. In order to obtain the desired sulfone derivatives, the sulfide group underwent oxidation with m-CPBA to afford sulfones. The structures of all the new products were elucidated by spectroscopic/physical methods and, in two cases, by X-ray diffraction.

Furfural Synthesis from d-Xylose in the Presence of Sodium Chloride: Microwave versus Conventional Heating.

PubMed

Xiouras, Christos; Radacsi, Norbert; Sturm, Guido; Stefanidis, Georgios D

2016-08-23

We investigate the existence of specific/nonthermal microwave effects for the dehydration reaction of xylose to furfural in the presence of NaCl. Such effects are reported for sugars dehydration reactions in several literature reports. To this end, we adopted three approaches that compare microwave-assisted experiments with a) conventional heating experiments from the literature; b) simulated conventional heating experiments using microwave-irradiated silicon carbide (SiC) vials; and at c) different power levels but the same temperature by using forced cooling. No significant differences in the reaction kinetics are observed using any of these methods. However, microwave heating still proves advantageous as it requires 30 % less forward power compared to conventional heating (SiC vial) to achieve the same furfural yield at a laboratory scale. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of Structurally Diverse 2,3-Fused Indoles via Microwave-Assisted AgSbF6-Catalysed Intramolecular Difunctionalization of o-Alkynylanilines

PubMed Central

Huang, Yuanqiong; Yang, Yan; Song, Hongjian; Liu, Yuxiu; Wang, Qingmin

2015-01-01

2,3-Fused indoles are found in numerous natural products and drug molecules. Although several elegant methods for the synthesis of this structural motif have been reported, long reaction times and harsh conditions are sometimes required, and the yields tend to be low. Herein, we report a microwave method for straightforward access to various types of 2,3-fused indoles via AgSbF6-catalysed intramolecular difunctionalization of o-alkynylanilines. AgSbF6 played a role in both the hydroamination step and the imine-formation step. This method, which exhibited excellent chemoselectivity (no ring-fused 1,2-dihydroquinolines were formed), was used for formal syntheses of the natural products conolidine and ervaticine and the antihistamine drug latrepirdine. PMID:26310858

Green synthesis of Si-incorporated hydroxyapatite using sodium metasilicate as silicon precursor and in vitro antibiotic release studies.

PubMed

Abinaya Sindu, P; Kolanthai, Elayaraja; Suganthi, R V; Thanigai Arul, K; Manikandan, E; Catalani, Luiz H; Narayana Kalkura, S

2017-10-01

The aim of the current study is to synthesize nanosized silicon incorporated HAp (Si-HAP) using sodium metasilicate as the silicon source. The sol-gel derived samples were further subjected to microwave irradiation. Incorporation of Si into HAp did not alter the HAp phase, as confirmed by the X-ray diffraction analysis (XRD). Moreover, variation in the lattice parameters of the Si-incorporated HAp indicates that Si is substituted into the HAp lattice. The decrease in the intensity of the peaks attributed to hydroxyl groups, which appeared in the FTIR and Raman spectra of Si-HAp, further confirms the Si substitution in HAp lattices. The silicon incorporation enhanced the nanorods length by 70%, when compared to that of pure HAp. Microwave irradiation improved the crystallinity of Si-HAp when compared to as-synthesized Si-HAp samples. As-synthesized Si-incorporated HAp sample showed an intense blue emission under UV excitation. Microwave irradiation reduced the intensity of blue emission and exhibited red shift due to the reduction of defects in the Si-HAp crystal. The morphological change from rod to spherical and ribbon-like forms was observed with an increase in silicon content. Further, Si-HAp exhibited better bioactivity and low dissolution rate. Initially there was a burst release of amoxicillin from all the samples, subsequently it followed a sustained release. The microwave-irradiated HAp showed extended period of sustained release than that of as-synthesized HAp and Si-HAp. Similarly, the microwave-irradiated Si-incorporated samples exhibited prolonged drug release, as compared to that of the as-synthesized samples. Hence, Si-HAp is rapidly synthesized by a simple and cost effective method without inducing any additional phases, as compared to the conventional sintering process. This study provides a new insight into the rapid green synthesis of Si-HAp. Si-HAp could emerge as a promising material for the bone tissue replacement and as a drug delivery system. Copyright © 2017 Elsevier B.V. All rights reserved.

Microwave Enhancement of Autocatalytic Growth of Nanometals.

PubMed

Ashley, Bridgett; Vakil, Parth N; Lynch, Brian B; Dyer, Christopher M; Tracy, Joseph B; Owens, Jeffery; Strouse, Geoffrey F

2017-10-24

The desire for designing efficient synthetic methods that lead to industrially important nanomaterials has led a desire to more fully understand the mechanism of growth and how modern synthetic techniques can be employed. Microwave (MW) synthesis is one such technique that has attracted attention as a green, sustainable method. The reports of enhancement of formation rates and improved quality for MW driven reactions are intriguing, but the lack of understanding of the reaction mechanism and how coupling to the MW field leads to these observations is concerning. In this manuscript, the growth of a metal nanoparticles (NPs) in a microwave cavity is spectroscopically analyzed and compared with the classical autocatalytic method of NP growth to elucidate the underpinnings for the observed enhanced growth behavior for metal NPs prepared in a MW field. The study illustrates that microwave synthesis of nickel and gold NPs below saturation conditions follows the Finke-Watzky mechanism of nucleation and growth. The enhancement of the reaction arises from the size-dependent increase in MW absorption cross section for the metal NPs. For Ni, the presence of oxides is considered via theoretical computations and compared to dielectric measurements of isolated nickel NPs. The study definitively shows that MW growth can be modeled by an autocatalytic mechanism that directly leads to the observed enhanced rates and improved quality widely reported in the nanomaterial community when MW irradiation is employed.

Microwave-Assisted γ-Valerolactone Production for Biomass Lignin Extraction: A Cascade Protocol.

PubMed

Tabasso, Silvia; Grillo, Giorgio; Carnaroglio, Diego; Calcio Gaudino, Emanuela; Cravotto, Giancarlo

2016-03-26

The general need to slow the depletion of fossil resources and reduce carbon footprints has led to tremendous effort being invested in creating "greener" industrial processes and developing alternative means to produce fuels and synthesize platform chemicals. This work aims to design a microwave-assisted cascade process for a full biomass valorisation cycle. GVL (γ-valerolactone), a renewable green solvent, has been used in aqueous acidic solution to achieve complete biomass lignin extraction. After lignin precipitation, the levulinic acid (LA)-rich organic fraction was hydrogenated, which regenerated the starting solvent for further biomass delignification. This process does not requires a purification step because GVL plays the dual role of solvent and product, while the reagent (LA) is a product of biomass delignification. In summary, this bio-refinery approach to lignin extraction is a cascade protocol in which the solvent loss is integrated into the conversion cycle, leading to simplified methods for biomass valorisation.

Rapid, facile microwave-assisted synthesis of xanthan gum grafted polyaniline for chemical sensor.

PubMed

Pandey, Sadanand; Ramontja, James

2016-08-01

Grafting method, through microwave radiation procedure is extremely productive in terms of time consumption, cost effectiveness and environmental friendliness. In this study, conductive and thermally stable composite (mwXG-g-PANi) was synthesized by grafting of aniline (ANi) on to xanthan gum (XG) using catalytic weight of initiator, ammonium peroxydisulfate in the process of microwave irradiation in an aqueous medium. The synthesis of mwXG-g-PANi were confirm by FTIR, XRD, TGA, and SEM. The influence of altering the microwave power, exposure time of microwave, concentration of monomer and the amount of initiator of graft polymerization were studied over the grafting parameters, for example, grafting percentage (%G) and grafting efficiency (%E). The maximum %G and %E achieved was 172 and 74.13 respectively. The outcome demonstrates that the microwave irradiation strategy can increase the reaction rate by 72 times over the conventional method. Electrical conductivity of XG and mwXG-g-PANi composite film was performed. The fabricated grafted sample film were then examined for the chemical sensor. The mwXG-g-PANi, effectively integrated and handled, are NH3 sensitive and exhibit a rapid sensing in presence of NH3 vapor. Chemiresistive NH3 sensors with superior room temperature sensing performance were produced with sensor response of 905 at 1ppb and 90% recovery within few second. Copyright © 2016 Elsevier B.V. All rights reserved.

Microwave-assisted synthesis of HKUST-1 and functionalized HKUST-1-@H3PW12O40: selective adsorption of heavy metal ions in water analyzed with synchrotron radiation.

PubMed

Zou, Fang; Yu, Runhan; Li, Rongguan; Li, Wei

2013-08-26

A simple, rapid and efficient synthesis of the metal-organic framework (MOF) HKUST-1 [Cu3(1,3,5-benzene-tri-carboxilic-acid)2] by microwave irradiation is described, which afforded a homogeneous and highly selective material. The unusually short time to complete the synthesis by microwave irradiation is mainly attributable to rapid nucleation rather than to crystal growth rate. Using this method, HKUST-1-MW (MW=microwave) could be prepared within 20 min, whereas by hydrothermal synthesis, involving conventional heating, the preparation time is 8 h. Work efficiency was improved by the good performance of the obtained HKUST-1-MW which exhibited good selective adsorption of heavy metal ions, as well as a remarkably high adsorption affinity and adsorption capacity, but no adsorption of Hg(2+) under the same experimental conditions. Of particular importance is the preservation of the structure after metal-ion adsorption, which remained virtually intact, with only a few changes in X-ray diffraction intensity and a moderate decline in surface area. Synthesis of the polyoxometalate-containing HKUST-1-MW@H3PW12O40 afforded a MOF with enhanced stability in water, due to the introduced Keggin-type phosphotungstate, which systematically occluded in the cavities constituting the walls between the mesopores. Different Cu/W ratios were investigated according to the extrusion rate of cooper ions concentration, without significant structural changes after adsorption. The MOFs obtained feature particle sizes between 10-20 μm and their structures were determined using synchrotron-based X-ray diffraction. The results of this study can be considered important for potentially wider future applications of MOFs, especially to attend environmental issues. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis of Pd-N-heterocyclic carbene Pd-catalyst and its application in MW-assisted Heck and Suzuki reaction

EPA Science Inventory

The first Pd-N-heterocyclic carbene (NHC) complex in the form of organic silica is prepared using sol-gel method and its application in Heck and Suzuki reactions are demonstrated. These C-C coupling reactions proceeded efficiently under the influence of microwave irradiation, wit...

Fly-ash:H2SO4 catalyzed solvent free efficient synthesis of some aryl chalcones under microwave irradiation

NASA Astrophysics Data System (ADS)

Thirunarayanan, G.; Mayavel, P.; Thirumurthy, K.

2012-06-01

Some 2E aryl chalcones have been synthesized using greener catalyst Fly-ash:H2SO4 assisted solvent free environmentally benign Crossed-Aldol reaction. The yields of chalcones are more than 90%. The synthesized chalcones are characterized by their physical constants and spectral data.

MICROWAVE-ASSISTED CHEMISTRY: SYNTHESIS OF AMINES AND HETEROCYCLES VIA CARBON-NITROGEN BOND FORMATION IN AQUEOUS MEDIA

EPA Science Inventory

Improved C-N bond formation under MW influence is demonstrated by a) solventless three-component coupling reaction to generate propargyl amines that uses only Cu (I); b) aqueous N-alkylation of amines by alkyl halides that proceeds expeditiously in the presence of NaOH to deliver...

A microwave-assisted solution combustion synthesis to produce europium-doped calcium phosphate nanowhiskers for bioimaging applications.

PubMed

Wagner, Darcy E; Eisenmann, Kathryn M; Nestor-Kalinoski, Andrea L; Bhaduri, Sarit B

2013-09-01

Biocompatible nanoparticles possessing fluorescent properties offer attractive possibilities for multifunctional bioimaging and/or drug and gene delivery applications. Many of the limitations with current imaging systems center on the properties of the optical probes in relation to equipment technical capabilities. Here we introduce a novel high aspect ratio and highly crystalline europium-doped calcium phosphate nanowhisker produced using a simple microwave-assisted solution combustion synthesis method for use as a multifunctional bioimaging probe. X-ray diffraction confirmed the material phase as europium-doped hydroxyapatite. Fluorescence emission and excitation spectra and their corresponding peaks were identified using spectrofluorimetry and validated with fluorescence, confocal and multiphoton microscopy. The nanowhiskers were found to exhibit red and far red wavelength fluorescence under ultraviolet excitation with an optimal peak emission of 696 nm achieved with a 350 nm excitation. Relatively narrow emission bands were observed, which may permit their use in multicolor imaging applications. Confocal and multiphoton microscopy confirmed that the nanoparticles provide sufficient intensity to be utilized in imaging applications. Copyright © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Green and Sustainable Separation of Natural Products from Agro-Industrial Waste: Challenges, Potentialities, and Perspectives on Emerging Approaches.

PubMed

Zuin, Vânia G; Ramin, Luize Z

2018-01-17

New generations of biorefinery combine innovative biomass waste resources from different origins, chemical extraction and/or synthesis of biomaterials, biofuels, and bioenergy via green and sustainable processes. From the very beginning, identifying and evaluating all potentially high value-added chemicals that could be removed from available renewable feedstocks requires robust, efficient, selective, reproducible, and benign analytical approaches. With this in mind, green and sustainable separation of natural products from agro-industrial waste is clearly attractive considering both socio-environmental and economic aspects. In this paper, the concepts of green and sustainable separation of natural products will be discussed, highlighting the main studies conducted on this topic over the last 10 years. The principal analytical techniques (such as solvent, microwave, ultrasound, and supercritical treatments), by-products (e.g., citrus, coffee, corn, and sugarcane waste) and target compounds (polyphenols, proteins, essential oils, etc.) will be presented, including the emerging green and sustainable separation approaches towards bioeconomy and circular economy contexts.

Microwave-assisted solvothermal synthesis of hierarchical TiO2 microspheres for efficient electro-field-assisted-photocatalytic removal of tributyltin in tannery wastewater.

PubMed

Zhao, Yang; Huang, Zhiding; Chang, Wenkai; Wei, Chao; Feng, Xugen; Ma, Lin; Qi, Xiaoxia; Li, Zenghe

2017-07-01

Organotin compounds have been widely used in recent decades, however, the residential tributyltin (TBT) in environment has potential harmful effects on human health due to the disruption of endocrine system even at trace level. Herein, this work reports on an effective electro-field-assisted-photocatalytic technique for removal of TBT by applying an electric field to photocatalysis of as-prepared hierarchical TiO 2 microspheres. The synthesis of catalytic materials is based on a self-assembly process induced by microwave-assisted solvothermal reaction. Hierarchical TiO 2 microspheres consisting of nanowires can be obtained in short time with this facile method and possess high surface area and superior optical properties. As the catalyst, it was found that the reaction rate constant of electro-field-assisted-photocatalytic removal (0.0488 min -1 ) of TBT exhibited almost a 9 fold improvement as compared to that of photocatalysis (0.0052 min -1 ). The proposed mechanism of electro-field-assisted-photocatalytic removal of TBT was verified by using 117 Sn-enriched TBT spike solution as an isotopic tracer. In addition, varying impacts from some key reaction conditions, such as voltage of potential, pH value and the presence of Cr and formaldehyde were also discussed. The overall satisfactory TBT removal performance of the proposed electro-field-assisted-photocatalysis procedure with hierarchical TiO 2 microspheres, which was validated using actual tannery wastewater samples from three different kinds of tanning procedures. These attributes suggest that this electro-field-assisted-photocatalysis may have broad applications for the treatment of tannery wastewater. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microwave-assisted synthesis of NiS2 nanostructures for supercapacitors and cocatalytic enhancing photocatalytic H2 production.

PubMed

Pang, Huan; Wei, Chengzhen; Li, Xuexue; Li, Guochang; Ma, Yahui; Li, Sujuan; Chen, Jing; Zhang, Jiangshan

2014-01-06

Uniform NiS2 nanocubes are successfully synthesized with a microwave-assisted method. Interestingly, NiS2 nanocubes, nanospheres and nanoparticles are obtained by controlling microwave reaction time. NiS2 nanomaterials are primarily applied to supercapacitors and cocatalytic enhancing photocatalytic H2 production. Different morphologies of NiS2 nanostructures show different electrochemical and cocatalytic enhancing H2 production activities. Benefited novel nanostructures, NiS2 nanocube electrodes show a large specific capacitance (695 F g(-1) at 1.25 A g(-1)) and excellent cycling performance (the retention 93.4% of initial specific capacitance after 3000 cycles). More importantly, NiS2 nanospheres show highly cocatalytic enhancing photocatalytic for H2 evolution, in which the photocatalytic H2 production is up to 3400 μmol during 12 hours under irradiation of visible light (λ>420 nm) with an average H2 production rate of 283 μmol h(-1).

Microwave-assisted synthesis of NiS2 nanostructures for supercapacitors and cocatalytic enhancing photocatalytic H2 production

NASA Astrophysics Data System (ADS)

Pang, Huan; Wei, Chengzhen; Li, Xuexue; Li, Guochang; Ma, Yahui; Li, Sujuan; Chen, Jing; Zhang, Jiangshan

2014-01-01

Uniform NiS2 nanocubes are successfully synthesized with a microwave-assisted method. Interestingly, NiS2 nanocubes, nanospheres and nanoparticles are obtained by controlling microwave reaction time. NiS2 nanomaterials are primarily applied to supercapacitors and cocatalytic enhancing photocatalytic H2 production. Different morphologies of NiS2 nanostructures show different electrochemical and cocatalytic enhancing H2 production activities. Benefited novel nanostructures, NiS2 nanocube electrodes show a large specific capacitance (695 F g-1 at 1.25 A g-1) and excellent cycling performance (the retention 93.4% of initial specific capacitance after 3000 cycles). More importantly, NiS2 nanospheres show highly cocatalytic enhancing photocatalytic for H2 evolution, in which the photocatalytic H2 production is up to 3400 μmol during 12 hours under irradiation of visible light (λ>420 nm) with an average H2 production rate of 283 μmol h-1.

α-Fe2O3 nanosheet-assembled hierarchical hollow mesoporous microspheres: Microwave-assisted solvothermal synthesis and application in photocatalysis.

PubMed

Sun, Tuan-Wei; Zhu, Ying-Jie; Qi, Chao; Ding, Guan-Jun; Chen, Feng; Wu, Jin

2016-02-01

α-Fe2O3 nanosheet-assembled hierarchical hollow mesoporous microspheres (HHMSs) were prepared by thermal transformation of nanosheet-assembled hierarchical hollow mesoporous microspheres of a precursor. The precursor was rapidly synthesized using FeCl3·6H2O as the iron source, ethanolamine (EA) as the alkali source, and ethylene glycol (EG) as the solvent by the microwave-assisted solvothermal method. The samples were characterized by X-ray powder diffraction (XRD), thermogravimetric (TG) analysis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption-desorption isotherm. The effects of the microwave solvothermal temperature and EA amount on the morphology of the precursor were investigated. The as-prepared α-Fe2O3 HHMSs exhibit a good photocatalytic activity for the degradation of salicylic acid, and are promising for the application in wastewater treatment. Copyright © 2015 Elsevier Inc. All rights reserved.

Microwave-assisted synthesis of NiS2 nanostructures for supercapacitors and cocatalytic enhancing photocatalytic H2 production

PubMed Central

Pang, Huan; Wei, Chengzhen; Li, Xuexue; Li, Guochang; Ma, Yahui; Li, Sujuan; Chen, Jing; Zhang, Jiangshan

2014-01-01

Uniform NiS2 nanocubes are successfully synthesized with a microwave-assisted method. Interestingly, NiS2 nanocubes, nanospheres and nanoparticles are obtained by controlling microwave reaction time. NiS2 nanomaterials are primarily applied to supercapacitors and cocatalytic enhancing photocatalytic H2 production. Different morphologies of NiS2 nanostructures show different electrochemical and cocatalytic enhancing H2 production activities. Benefited novel nanostructures, NiS2 nanocube electrodes show a large specific capacitance (695 F g−1 at 1.25 A g−1) and excellent cycling performance (the retention 93.4% of initial specific capacitance after 3000 cycles). More importantly, NiS2 nanospheres show highly cocatalytic enhancing photocatalytic for H2 evolution, in which the photocatalytic H2 production is up to 3400 μmol during 12 hours under irradiation of visible light (λ>420 nm) with an average H2 production rate of 283 μmol h−1. PMID:24389929

Microwave: An Important and Efficient Tool for the Synthesis of Biological Potent Organic Compounds.

PubMed

Kumari, Kamlesh; Vishvakarma, Vijay K; Singh, Prashant; Patel, Rajan; Chandra, Ramesh

2017-01-01

Green Chemistry is an interdisciplinary science or it can also be explained as a branch of chemistry. It is generally described as the chemistry to aim to synthesize chemical compounds to trim down the utilization of harmful chemicals proposed by the Environmental Protection Agency (EPA). Recently, the plan of academicians, researchers, industrialists is to generate greener and more efficient methodologies to carry out various organic syntheses. In the present scenario, green chemistry utilizes the raw materials economically, minimizes the waste and prevents the uses of harmful or hazardous chemicals to make the organic reactions simple and efficient. Microwave technique is a new, simple and efficient technology which opens new prospects to the chemists to carry out various organic and inorganic reactions, which are difficult via conventional methodology. It is used to decrease the duration of time to carry various organic transformation along with maximum yield, minimum by-products, minimum energy utilization, less manpower etc. e.g. various famous organic reactions have been carried out by various research groups like Aldol condensation, Knoevenagel condensation, Beckmann rearrangement, Vilsmeier reaction, Perkin reaction, Benzil-Benzilic acid rearrangement, Fischer cyclization, Mannich reaction, Claisen-Schmidt condensation, etc. Further, reduction, oxidation, coupling, condensation reaction were also performed using microwave technology. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Synthesis of phthalide-fused indoline by microwave irradiation and preliminary binding study with metal cations

NASA Astrophysics Data System (ADS)

Ling, Sheryn Wong Shue; Latip, Jalifah; Hassan, Nurul Izzaty; Hasbullah, Siti Aishah

2018-04-01

An efficient and green method of synthesizing phthalide-fused indoline, 3-[(1,3,3-trimethylindolin-2-ylidene)methyl]isobenzofuran-1(3H)-one (3) has been developed by the coupling reaction of 1,3,3-trimethyl-2-methyleneindoline, 1 and phthalaldehydic acid, 2 under solvent-free domestic microwave irradiation. The compound was produced with an excellent yield (98 %) and at a shorter reaction time (5 min) as compared to the conventional method. Compound 3 was fully characterized by analytical and spectral methods. Preliminary binding study of 3 towards different types of metal cations was done by "naked eye" colorimetric detection and UV-vis spectrophotometer. Compound 3 exhibits good selectivity and sensitivity for Sn2+ compared to other metal cations.

One-pot microwave assisted synthesis under green chemistry conditions, antioxidant screening, and cytotoxicity assessments of benzimidazole Schiff bases and pyrimido[1,2-a]benzimidazol-3(4H)-ones.

PubMed

Neochoritis, Constantinos G; Zarganes-Tzitzikas, Tryfon; Tsoleridis, Constantinos A; Stephanidou-Stephanatou, Julia; Kontogiorgis, Christos A; Hadjipavlou-Litina, Dimitra J; Choli-Papadopoulou, Theodora

2011-01-01

The synthesis of a number of benzimidazole Schiff bases 3 and 3-oxo-pyrimido[1,2-a]benzimidazoles 4 in excellent yields by a one-step sequence from the reaction of 2-aminobenzimidazole under green chemistry conditions is described. Structural assignments of the new compounds as well as complete assignment of (1)H and (13)C NMR signals have been unambiguously achieved based on the analysis of their (1)H and (13)C NMR (1D and 2D), IR, MS and elemental analysis data. To the synthesized Schiff bases the E-configuration was assigned on the basis of comparison of experimental and calculated (DFT) (13)C NMR chemical shifts. Compounds 3 and 4 were evaluated as inhibitors of lipoxygenase (LOX) and of lipid peroxidation (LPO). All the tested derivatives showed inhibition of lipid peroxidation, whereas most of them were found to have higher activation than the reference compound trolox; The Schiff bases 3e, 3h, and 3i, and the pyrimidobenzimidazoles 4a, 4e and 4f were found to be the most potent. The most potent LOX inhibitor within the subset of Schiff bases was found compound 3i, followed by 3f, whereas compounds 4a and 4g were found the most potent of the 3-oxo-pyrimido[1,2-a]benzimidazole group. Moreover, some cytotoxicity assessments were undertaken, whereupon it was found that Schiff base 3i and pyrimidobenzimidazoles 4e and 4f did not exhibit cytotoxicity at similar concentrations resembling thus the inhibitory activity of lipid peroxidation. The most cytotoxic Schiff base and pyrimidobenzimidazole were found to be 3d and 4c, respectively. Copyright © 2010 Elsevier Masson SAS. All rights reserved.

Green synthesis of chondroitin sulfate-capped silver nanoparticles: characterization and surface modification.

PubMed

Cheng, Kuang-ming; Hung, Yao-wen; Chen, Cheng-cheung; Liu, Cheng-che; Young, Jenn-jong

2014-09-22

A one-step route for the green synthesis of highly stable and nanosized silver metal particles with narrow distribution is reported. In this environmentally friendly synthetic method, silver nitrate was used as silver precursor and biocompatible chondroitin sulfate (ChS) was used as both reducing agent and stabilizing agent. The reaction was carried out in a stirring aqueous medium at the room temperature without any assisted by microwave, autoclave, laser irradiation, γ-ray irradiation or UV irradiation. The transparent colorless solution was converted to the characteristics light red then deep red-brown color as the reaction proceeds, indicating the formation of silver nanoparticles (Ag NPs). The Ag NPs were characterized by UV-visible spectroscopy (UV-vis), photon correlation spectroscopy, laser Doppler anemometry, transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FT-IR). The results demonstrated that the obtained metallic nanoparticles were Ag NPs capped with ChS. In this report, dynamic light scattering (DLS) was used as a routinely analytical tool for measuring size and distribution in a liquid environment. The effects of the reaction time, reaction temperature, concentration and the weight ratio of ChS/Ag+ on the particle size and zeta potential were investigated. The TEM image clearly shows the morphology of the well-dispersed ChS-capped Ag NPs are spherical in shape, and the average size (<20 nm) is much smaller than the Z-average value (76.7 nm) measured by DLS. Meanwhile, the ChS-capped Ag NPs coated with N-[(2-hydroxy-3-trimethylammonium) propyl] chitosan chloride (HTCC) were prepared by an ionic gelation method and the surface charge of Ag NPs was switched from negative to positive. Copyright © 2014 Elsevier Ltd. All rights reserved.

Low temperature synthesis and characterization of Na–M–(O)–F phases with M=Ti, V

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

Nava-Avendaño, Jessica; Ayllón, José A.; Frontera, Carlos

2015-03-15

Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} was prepared by the microwave assisted method, and presents a chiolite related structure with cell parameters a=10.5016(5), b=10.4025(5), and c=10.2911(5) Å and Cmca (no. 64) space group. From solvothermal synthesis at 100 °C the cryolite Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} was prepared, which crystallizes in the monoclinic system with a=5.5403(2), b=5.6804(2), c=7.9523(2) Å, β=90.032(7)° cell parameters and P2{sub 1}/n (no. 14) space group. Under similar synthesis conditions but with higher HF concentration the chiolite-type phase Na{sub 5−δ}V{sub 3}F{sub 14} was achieved, which exhibits a=10.5482(2), b=10.4887(1) and c=10.3243(1) Å cell parameters and Cmc2{sub 1} (no. 36) spacemore » group. A single crystal also having the chiolite structure was synthesized at 200 °C which exhibits tetragonal symmetry (a=7.380(3) and c=10.381(11) Å and space group P4{sub 2}2{sub 1}2 (no. 94)). Bond valence sum indicates that it contains V{sup 4+} and therefore can be formulated as Na{sub 5}V{sub 3}O{sub 3}F{sub 11}. - Graphical abstract: Na{sub 5}M{sub 3}(O,F){sub 14} with M=Ti and V having chiolite structure and Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} cryolite were prepared by means of microwave-assisted and solvothermal synthesis. - Highlights: • Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} chiolite was prepared by a microwave assisted method and characterized. • Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} and Na{sub 5−δ}V{sub 3}F{sub 14} were prepared by solvothermal synthesis. • The compounds were structurally characterized by diffraction techniques. • O/F distribution was estimated by applying Pauling’s second rule.« less

On being green: can flow chemistry help?

PubMed

Ley, Steven V

2012-08-01

The principles of Green Chemistry are important but challenging drivers for most modern synthesis programs. To meet these challenges new flow chemistry tools are proving to be very effective by providing improved heat/mass transfer opportunities, lower solvent usage, less waste generation, hazardous compound containment, and the possibility of a 24/7 working regime. This machine-assisted approach can be used to effect repetitive or routine scale-up steps or when combined with reagent and scavenger cartridges, to achieve multi-step synthesis of complex natural products and pharmaceutical agents. Copyright © 2012 The Japan Chemical Journal Forum and Wiley Periodicals, Inc.

Synthesis, characterization, and properties of low-dimensional nanostructured materials

NASA Astrophysics Data System (ADS)

Hu, Xianluo

2007-05-01

Nanometer scale structures represent an exciting and rapidly expanding area of research. Studies on new physical/chemical properties and applications of nanomaterials and nanostructures are possible only when nanostructured materials are made available with desired size, morphology, crystal and microstructure, and composition. Thus, controlled synthesis of nanomaterials is the essential aspect of nanotechnology. This thesis describes the development of simple and versatile solution-based approaches to synthesize low-dimensional nanostructures. The first major goal of this research is to design and fabricate morphology-controlled alpha-Fe 2O3 nanoarchitectures in aqueous solution through a programmed microwave-assisted hydrothermal route, taking advantage of microwave irradiation and hydrothermal effects. Free-standing alpha-Fe2O3 nanorings are prepared by hydrolysis of FeCl3 in the presence of phosphate ions. The as-formed architecture of alpha-Fe2O 3 nanorings is an exciting new member in the family of iron oxide nanostructures. Our preliminary results demonstrate that sensors made of the alpha-Fe 2O3 nanorings exhibit high sensitivity not only for bio-sensing of hydrogen peroxide in a physiological solution but also for gas-sensing of alcohol vapor at room temperature. Moreover, monodisperse alpha-Fe 2O3 nanocrystals with continuous aspect-ratio tuning and fine shape control are achieved by controlling the experimental conditions. The as-formed alpha-Fe2O3 exhibits shape-dependent infrared optical properties. The growth process of colloidal alpha-Fe 2O3 crystals in the presence of phosphate ions is discussed. In addition, through an efficient microwave-assisted hydrothermal process, self-assembled hierarchical alpha-Fe2O3 nanoarchitectures are synthesized on a large scale. The second major goal of this research is to develop convenient microwave-hydrothermal approaches for the fabrication of carbon-based nanocomposites: (1) A one-pot solution-phase route, namely microwave-assisted hydrothermal reduction/carbonization (MAHRC), is developed to prepare coaxial Ag/amorphous-carbon (a-C) nanocables. The as-grown Ag/C nanocables can self-assemble in an end-to-end fashion. (2) A novel Se/C nanocomposite with core-shell structures is prepared. The new material consists of a trigonal-Se (t-Se) core and an amorphous-C (a-C) shell. The Se/C composite can be converted to hollow carbon capsules by thermal treatment. (3) A Fe 3O4/C nanocomposite is synthesized by a green wet-chemical approach. The product possesses porous microstructures and exhibits superparamagnetic behavior. The third major goal of this research is develop facile solution-based methods for preparing carbonaceous nano test tubes, thin films of metal iodides, and spherical selenium spheres: (1) Carbonaceous nano test tubes are fabricated by a facile "decoring" route using a core-sheath Te carbon nanocomposite as the precursor. The as-formed carbonaceous material looks like a "test tube" with an average diameter of about 120 nm and lengths up to 5 mum. (2) Tetrahedral-shaped CuI crystals were formed on a variety of copper substrates (e.g. grids, flat/porous foils, and macro-/nano- wires) via an interfacial reaction between a copper substrate and iodine in water at room temperature. This preparation approach can also be used to grow PbI2 and AgI nano- and micro-crystals with different morphologies on corresponding substrates. (3) Colloidal trigonal selenium (t-Se) microspheres are synthesized through a mild hydrothermal reduction reaction, using glucose as a reducing regent and water as an environmentally friendly solvent. Importantly, the resulting t-Se microspheres inherit functional groups from the starting materials and possess hydrophilic and biocompatible surfaces.

Tailoring surface and photocatalytic properties of ZnO and nitrogen-doped ZnO nanostructures using microwave-assisted facile hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rangel, R.; Cedeño, V.; Ramos-Corona, A.; Gutiérrez, R.; Alvarado-Gil, J. J.; Ares, O.; Bartolo-Pérez, P.; Quintana, P.

2017-08-01

Microwave hydrothermal synthesis, using an experimental 23 factorial design, was used to produce tunable ZnO nano- and microstructures, and their potential as photocatalysts was explored. Photocatalytic reactions were conducted in a microreactor batch system under UV and visible light irradiation, while monitoring methylene blue degradation, as a model system. The variables considered in the microwave reactor to produce ZnO nano- or microstructures, were time, NaOH concentration and synthesis temperature. It was found that, specific surface area and volume/surface area ratio were affected as a consequence of the synthesis conditions. In the second stage, the samples were plasma treated in a nitrogen atmosphere, with the purpose of introducing nitrogen into the ZnO crystalline structure. The central idea is to induce changes in the material structure as well as in its optical absorption, to make the plasma-treated material useful as photocatalyst in the visible region of the electromagnetic spectrum. Pristine ZnO and nitrogen-doped ZnO compounds were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), specific surface area (BET), XPS, and UV-Vis diffuse reflectance spectroscopy. The results show that the methodology presented in this work is effective in tailoring the specific surface area of the ZnO compounds and incorporation of nitrogen into their structure, factors which in turn, affect its photocatalytic behavior.

ADVANCES IN GREEN CHEMISTRY: CHEMICAL SYNTHESES USING MICROWAVE IRRADIATION, ISBN 81-901238-5-8

EPA Science Inventory

16. Abstract Advances in Green Chemistry: Chemical Syntheses Using Microwave Irradiation
Microwave-accelerated chemical syntheses in solvents as well as under solvent-free conditions have witnessed an explosive growth. The technique has found widespread application predomi...

Effect of blanching treatments on antioxidant activity of frozen green capsicum (Capsicum annuum L. var bell pepper) using radical scavenging activity (DPPH) assay

NASA Astrophysics Data System (ADS)

Azizzuddin, Norafida; Abdullah, Aminah

2016-11-01

Blanching treatments are needed to deactivate enzymes in frozen vegetables. Antioxidant activity using DPPH radical scavenging activity assay were evaluated in steaming, boiling water, and microwave blanching at different temperature, time and microwave power level on frozen green capsicum. Green capsicum was chosen for frozen treatment compared to other capsicum with different maturity index because of the firm texture. The objective of this study was to compare the antioxidant activity of frozen green capsicum between conventional and Oxi Count Kit® assay for DPPH radical scavenging activity. Results showed frozen green capsicum blanched using microwave at high level/90 seconds (sample J) contained higher level of DPPH in both conventional method and Oxi Count Kit® compared to other treatments. However, there were no significant differences between sample J and fresh sample (sample A). Overall, the sequences from highest to lowest in blanching treatments for both DPPH conventional method, and DPPH Oxi Count Kit® were J (microwave high level/90 seconds) > A (Fresh) > H (Microwave Medium Level/120 seconds) > D (Boiling Water 80°C/150 seconds) > K (Microwave High Level/120 seconds) > I (Microwave Medium Level/150 seconds) > F (Microwave Low Level/150 seconds)> B (Steam 100°C/150 seconds) > E (Boiling Water 100°C /120 seconds) > G (Microwave Low Level /180 seconds)> C (Steam 100°C/180 seconds). Almost all frozen green capsicum samples showed no significant differences for comparison between test using DPPH conventional method and Oxi Count Kit®. Frozen storage for 0, and 3rd months showed no significant differences which indicate no changes on antioxidant activity during frozen storage at -18°C.

Ultrasound and microwave assisted synthesis of isoindolo-1,2-diazine: a comparative study.

PubMed

Bejan, Vasilichia; Mantu, Dorina; Mangalagiu, Ionel I

2012-09-01

A comparative study, ultrasound (US) versus microwave (MW) versus conventional thermal heating (TH), for synthesis of isoindolo-1,2-diazine is described. The reaction pathway is fast, efficient and straight applicable, involving a Huisgen [3+2] dipolar cycloaddition of cycloimmonium ylides to 1,4-naphthoquinone. A feasible reaction mechanism for the obtaining of the fully aromatized tetra- and penta- cyclic isoindolo-1,2-diazine is presented. Under US irradiation the yields are much higher (sometimes substantially, by almost double), the reaction time decreases substantially, the reaction conditions are milder. The use of a generator with a higher nominal power induces higher yields and short reaction times. Overall the use of US it proved to be more efficient than MW or TH. A feasible explication for US efficiency is presented. Copyright © 2012 Elsevier B.V. All rights reserved.

An efficient microwave assisted synthesis of novel class of Rhodanine derivatives as potential HIV-1 and JSP-1 inhibitors.

PubMed

Kamila, Sukanta; Ankati, Haribabu; Biehl, Edward R

2011-08-24

(Z)-5-(2-(1H-Indol-3-yl)-2-oxoethylidene)-3-phenyl-2-thioxothiazolidin-4-one (7a-q) derivatives have been synthesized by the condensation reaction of 3-phenyl-2-thioxothiazolidin-4-ones (3a-h) with suitably substituted 2-(1H-indol-3-yl)-2-oxoacetaldehyde (6a-d) under microwave condition. The thioxothiazolidine-4-ones were prepared from corresponding aromatic amines (1a-e) and di-(carboxymethyl)-trithiocarbonyl (2). The aldehydes (6a-h) were synthesized from the corresponding acidchlorides (5a-d) using HSnBu(3).

An efficient microwave assisted synthesis of novel class of Rhodanine derivatives as potential HIV-1 and JSP-1 inhibitors

PubMed Central

Kamila, Sukanta; Ankati, Haribabu; Biehl, Edward R.

2011-01-01

(Z)-5-(2-(1H-Indol-3-yl)-2-oxoethylidene)-3-phenyl-2-thioxothiazolidin-4-one (7a-q) derivatives have been synthesized by the condensation reaction of 3-phenyl-2-thioxothiazolidin-4-ones (3a-h) with suitably substituted 2-(1H-indol-3-yl)-2-oxoacetaldehyde (6a-d) under microwave condition. The thioxothiazolidine-4-ones were prepared from corresponding aromatic amines (1a-e) and di-(carboxymethyl)-trithiocarbonyl (2). The aldehydes (6a-h) were synthesized from the corresponding acidchlorides (5a-d) using HSnBu3. PMID:21804651

Microwave-assisted synthesis of 5-aminopyrazol-4-yl ketones and the p38(MAPK) inhibitor RO3201195 for study in Werner syndrome cells.

PubMed

Bagley, Mark C; Davis, Terence; Dix, Matthew C; Murziani, Paola G S; Rokicki, Michal J; Kipling, David

2008-07-01

5-Aminopyrazol-4-yl ketones are prepared rapidly and efficiently using microwave dielectric heating from beta-ketonitriles by treatment with N,N'-diphenylformamidine followed by heterocyclocondensation by irradiation with a hydrazine. The inhibitory activity of RO3201195 prepared by this methodology was confirmed in hTERT-immortalized HCA2 and WS dermal fibroblasts at 200nM concentration, both by ELISA and immunoblot assay, and displays excellent kinase selectivity for p38alpha MAPK over the related stress-activated kinase JNK.

Microwave-Assisted Synthesis and Physicochemical Characterization of Tetrafuranylporphyrin-Grafted Reduced-Graphene Oxide.

PubMed

Bosca, Federica; Orio, Laura; Tagliapietra, Silvia; Corazzari, Ingrid; Turci, Francesco; Martina, Katia; Pastero, Linda; Cravotto, Giancarlo; Barge, Alessandro

2016-01-26

This work describes the design of a modified porphyrin that bears four furan rings linked by 1,2-bis-(2-aminoethoxy)ethane spacers. This unit is a well-suited scaffold for a Diels-Alder reaction with commercial reduced-graphene oxide, which is also described in this paper. A new hybrid material is obtained, thanks to efficient grafting under microwave irradiation, and fully characterized in terms of structure (UV, TGA, Raman) and morphology (HR-TEM and AFM). Potential applications in photo- and sonodynamic therapy are envisaged. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microwave-assisted synthesis of carbon nanotubes from tannin, lignin, and derivatives

DOEpatents

Viswanathan, Tito

2014-06-17

A method of synthesizing carbon nanotubes. In one embodiment, the method includes the steps of: (a) dissolving a first amount of a first transition-metal salt and a second amount of a second transition-metal salt in water to form a solution; (b) adding a third amount of tannin to the solution to form a mixture; (c) heating the mixture to a first temperature for a first duration of time to form a sample; and (d) subjecting the sample to a microwave radiation for a second duration of time effective to produce a plurality of carbon nanotubes.

Green synthesis, structure and fluorescence spectra of new azacyanine dyes

NASA Astrophysics Data System (ADS)

Enchev, Venelin; Gadjev, Nikolai; Angelov, Ivan; Minkovska, Stela; Kurutos, Atanas; Markova, Nadezhda; Deligeorgiev, Todor

2017-11-01

A series of symmetric and unsymmetric monomethine azacyanine dyes (monomethine azacyanine and merocyanine sulfobetaines) were synthesized with moderate to high yields via a novel method using microwave irradiation. The compounds are derived from a condensation reaction between 2-thiomethylbenzotiazolium salts and 2-imino-3-methylbenzothiazolines proceeded under microwave irradiation. The synthetic approach involves the use of green solvent and absence of basic reagent. TD-DFT calculations were performed to simulate absorption and fluorescent spectra of synthesized dyes. Absorption maxima, λmax, of the studied dyes were found in the range 364-394 nm. Molar absorbtivities were evaluated in between 40300 and 59200 mol-1 dm3 cm-1. Fluorescence maxima, λfl, were registered around 418-448 nm upon excitation at 350 nm. A slight displacements of theoretically estimated absorption maxima according to experimental ones is observed. The differences are most probably due to the fact that the DFT calculations were carried out without taking into account the solvent effect. In addition, the merocyanine sulfobetaines also fluorescence in blue optical range (420-480 nm) at excitation in red range (630-650 nm).

Electrochemiluminescence energy transfer-promoted ultrasensitive immunoassay using near-infrared-emitting CdSeTe/CdS/ZnS quantum dots and gold nanorods

PubMed Central

Li, Lingling; Chen, Ying; Lu, Qian; Ji, Jing; Shen, Yuanyuan; Xu, Mi; Fei, Rong; Yang, Guohai; Zhang, Kui; Zhang, Jian-Rong; Zhu, Jun-Jie

2013-01-01

The marriage of energy transfer with electrochemiluminescence has produced a new technology named electrochemiluminescence energy transfer (ECL-ET), which can realize effective and sensitive detection of biomolecules. To obtain optimal ECL-ET efficiency, perfect energy overlapped donor/acceptor pair is of great importance. Herein, we present a sensitive ECL-ET based immunosensor for the detection of tumor markers, using energy tunable CdSeTe/CdS/ZnS double shell quantum dots (QDs) and gold nanorods (GNRs) as the donor and acceptor, respectively. Firstly a facile microwave-assisted strategy for the synthesis of green- to near-infrared-emitting CdSeTe/CdS/ZnS QDs with time- and component-tunable photoluminescence was proposed. And, on the basis of the adjustable optical properties of both CdSeTe/CdS/ZnS QDs and GNRs, excellent overlap between donor emission and acceptor absorption can be obtained to ensure effective ECL-ET quenching, thus improving the sensing sensitivity. This method represents a novel approach for versatile detection of biomolecules at low concentrations. PMID:23524874

Nickel–cobalt layered double hydroxide ultrathin nanoflakes decorated on graphene sheets with a 3D nanonetwork structure as supercapacitive materials

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

Yan, Tao; Li, Ruiyi; Li, Zaijun, E-mail: zaijunli@263.net

2014-03-01

Graphical abstract: The microwave heating reflux approach was developed for the fabrication of nickel–cobalt layered double hydroxide ultrathin nanoflakes decorated on graphene sheets, in which ammonia and ethanol were used as the precipitator and medium for the synthesis. The obtained composite shows a 3D flowerclusters morphology with nanonetwork structure and largely enhanced supercapacitive performance. - Highlights: • The paper reported the microwave synthesis of nickel–cobalt layered double hydroxide/graphene composite. • The novel synthesis method is rapid, green, efficient and can be well used to the mass production. • The as-synthesized composite offers a 3D flowerclusters morphology with nanonetwork structure. •more » The composite offers excellent supercapacitive performance. • This study provides a promising route to design and synthesis of advanced graphene-based materials with the superiorities of time-saving and cost-effective characteristics. - Abstract: The study reported a novel microwave heating reflux method for the fabrication of nickel–cobalt layered double hydroxide ultrathin nanoflakes decorated on graphene sheets (GS/NiCo-LDH). Ammonia and ethanol were employed as precipitant and reaction medium for the synthesis, respectively. The resulting GS/NiCo-LDH offers a 3D flowerclusters morphology with nanonetwork structure. Due to the greatly enhanced rate of electron transfer and mass transport, the GS/NiCo-LDH electrode exhibits excellent supercapacitive performances. The maximum specific capacitance was found to be 1980.7 F g{sup −1} at the current density of 1 A g{sup −1}. The specific capacitance can remain 1274.7 F g{sup −1} at the current density of 15 A g{sup −1} and it has an increase of about 2.9% after 1500 cycles. Moreover, the study also provides a promising approach for the design and synthesis of metallic double hydroxides/graphene hybrid materials with time-saving and cost-effective characteristics, which can be potentially applied in the energy storage/conversion devices.« less

Urchin-like CdS/ZrO2 nanocomposite prepared by microwave-assisted hydrothermal combined with ion-exchange and its multimode photocatalytic activity

NASA Astrophysics Data System (ADS)

Li, Li; Wang, Lili; Zhang, Wenzhi; Zhang, Xiuli; Chen, Xi; Dong, Xue

2014-12-01

A series of urchin-like CdS/ZrO2 nanocomposites with different mole ratios of Cd/Zr were prepared by a two-step method combining the microwave-assisted hydrothermal and ion exchange methods. The products were characterized by X-ray diffraction, ultraviolet-visible diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, and N2 adsorption-desorption measurements. The results of the study revealed that the CdS/ZrO2 nanocomposites had mixed phases of tetragonal ZrO2 and hexagonal CdS. Moreover, the samples prepared by the microwave-assisted hydrothermal method possessed the urchin-like structure with a surface composed of protrude-like nanoparticles in large quantities. The absorption in the visible region changed slightly with increasing mole ratio of Cd/Zr. Moreover, compared to the nanocomposites prepared by the conventional heating, the nanocomposites prepared by the microwave-assisted hydrothermal synthesis showed significantly different Brunauer-Emmett-Teller values, and the urchin-like CdS/ZrO2 structures were obtained. The photocatalytic degradation of methyl orange under ultraviolet (UV) light irradiation indicated that the photocatalytic activity of the CdS/ZrO2 nanocomposite with CdS/ZrO2 molar ratio of 30 % was higher than those of CdS, ZrO2, and other different ratios of CdS/ZrO2 nanocomposites. Moreover, under UV light, visible light, and microwave-assisted multimode photocatalytic degradation, the urchin-like CdS/ZrO2 nanocomposites significantly affected the photodegradation of various dyes. To understand the possible reaction mechanism of the photocatalysis by the CdS/ZrO2 nanocomposites, a series of controlled experiments were performed, and the stability and reusability of the CdS/ZrO2 nanocomposites were further investigated by the photocatalytic reaction.

Bio-refinery of orange peels waste: a new concept based on integrated green and solvent free extraction processes using ultrasound and microwave techniques to obtain essential oil, polyphenols and pectin.

PubMed

Boukroufa, Meryem; Boutekedjiret, Chahrazed; Petigny, Loïc; Rakotomanomana, Njara; Chemat, Farid

2015-05-01

In this study, extraction of essential oil, polyphenols and pectin from orange peel has been optimized using microwave and ultrasound technology without adding any solvent but only "in situ" water which was recycled and used as solvent. The essential oil extraction performed by Microwave Hydrodiffusion and Gravity (MHG) was optimized and compared to steam distillation extraction (SD). No significant changes in yield were noticed: 4.22 ± 0.03% and 4.16 ± 0.05% for MHG and SD, respectively. After extraction of essential oil, residual water of plant obtained after MHG extraction was used as solvent for polyphenols and pectin extraction from MHG residues. Polyphenols extraction was performed by ultrasound-assisted extraction (UAE) and conventional extraction (CE). Response surface methodology (RSM) using central composite designs (CCD) approach was launched to investigate the influence of process variables on the ultrasound-assisted extraction (UAE). The statistical analysis revealed that the optimized conditions of ultrasound power and temperature were 0.956 W/cm(2) and 59.83°C giving a polyphenol yield of 50.02 mgGA/100 g dm. Compared with the conventional extraction (CE), the UAE gave an increase of 30% in TPC yield. Pectin was extracted by conventional and microwave assisted extraction. This technique gives a maximal yield of 24.2% for microwave power of 500 W in only 3 min whereas conventional extraction gives 18.32% in 120 min. Combination of microwave, ultrasound and the recycled "in situ" water of citrus peels allow us to obtain high added values compounds in shorter time and managed to make a closed loop using only natural resources provided by the plant which makes the whole process intensified in term of time and energy saving, cleanliness and reduced waste water. Copyright © 2014 Elsevier B.V. All rights reserved.

Microwave assisted synthesis of porous ZnO/SnS heterojunction and its application in visible light degradation of ciprofloxacin

NASA Astrophysics Data System (ADS)

Makama, A. B.; Salmiaton, A.; Saion, E. B.; Choong, T. S. Y.; Abdullah, N.

2016-07-01

Porous ZnO/SnS heterojunctions were successfully synthesized via microwave-assisted heating of aqueous solutions containing different amounts of SnS precursors (SnCl2 and Na2S) in the presence of fixed amount of ZnCO3 nanoparticles. The experimental results revealed that the heterojunctions exhibited much higher visible light-driven photocatalytic activity for the degradation of the ciprofloxacin than pure SnS nanocrystals. The photocatalytic degradation efficiency (1-Ct/C0) of the pollutant for the most active heterogeneous nanostructure is about four times more efficient than pure SnS. The enhanced photocatalytic efficiency is ascribed to the synergic effect of high photon absorption and reduction in the recombination of electrons and holes because of efficient separation and electron transfer from the SnS to ZnO nanoparticles.

Microwave-assisted synthesis of cyclodextrin polyurethanes.

PubMed

Biswas, Atanu; Appell, Michael; Liu, Zengshe; Cheng, H N

2015-11-20

Cyclodextrin (CD) has often been incorporated into polyurethanes in order to facilitate its use in encapsulation or removal of organic species for various applications. In this work a microwave-assisted method has been developed to produce polyurethanes consisting of α-, β-, and γ-CD and three common diisocyanates. As compared to conventional heating, this new synthetic method saves energy, significantly reduces reaction time, and gets similar or improved yield. The reaction products have been fully characterized with (13)C, (1)H, and two-dimensional NMR spectroscopy. With suitable stoichiometry of starting CD and diisocyanate, the resulting CD polyurethane is organic-soluble and water-insoluble and is shown to remove Nile red dye and phenol from water. Possible applications include the removal of undesirable materials from process streams, toxic compounds from the environment, and encapsulation of color or fragrance molecules. Published by Elsevier Ltd.

Microwave-assisted synthesis of Pt/CNT nanocomposite electrocatalysts for PEM fuel cells.

PubMed

Zhang, Weimin; Chen, Jun; Swiegers, Gerhard F; Ma, Zi-Feng; Wallace, Gordon G

2010-02-01

Microwave-assisted heating of functionalized, single-wall carbon nanotubes (FCNTs) in ethylene glycol solution containing H(2)PtCl(6), led to the reductive deposition of Pt nanoparticles (2.5-4 nm) over the FCNTs, yielding an active catalyst for proton-exchange membrane fuel cells (PEMFCs). In single-cell testing, the Pt/FCNT composites displayed a catalytic performance that was superior to Pt nanoparticles supported by raw (unfunctionalized) CNTs (RCNTs) or by carbon black (C), prepared under identical conditions. The supporting single-wall carbon nanotubes (SWNTs), functionalized with carboxyl groups, were studied by thermogravimetric analysis (TGA), cyclic voltammetry (CV), and Raman spectroscopy. The loading level, morphology, and crystallinity of the Pt/SWNT catalysts were determined using TGA, SEM, and XRD. The electrochemically active catalytic surface area of the Pt/FCNT catalysts was 72.9 m(2)/g-Pt.

Removal of caffeine from green tea by microwave-enhanced vacuum ice water extraction.

PubMed

Lou, Zaixiang; Er, Chaojuan; Li, Jing; Wang, Hongxin; Zhu, Song; Sun, Juntao

2012-02-24

In order to selectively remove caffeine from green tea, a microwave-enhanced vacuum ice water extraction (MVIE) method was proposed. The effects of MVIE variables including extraction time, microwave power, and solvent to solid radio on the removal yield of caffeine and the loss of total phenolics (TP) from green tea were investigated. The optimized conditions were as follows: solvent (mL) to solid (g) ratio was 10:1, microwave extraction time was 6 min, microwave power was 350 W and 2.5 h of vacuum ice water extraction. The removal yield of caffeine by MVIE was 87.6%, which was significantly higher than that by hot water extraction, indicating a significant improvement of removal efficiency. Moreover, the loss of TP of green tea in the proposed method was much lower than that in the hot water extraction. After decaffeination by MVIE, the removal yield of TP tea was 36.2%, and the content of TP in green tea was still higher than 170 mg g(-1). Therefore, the proposed microwave-enhanced vacuum ice water extraction was selective, more efficient for the removal of caffeine. The main phenolic compounds of green tea were also determined, and the results indicated that the contents of several catechins were almost not changed in MVIE. This study suggests that MVIE is a new and good alternative for the removal of caffeine from green tea, with a great potential for industrial application. Copyright © 2011 Elsevier B.V. All rights reserved.

MW-assisted synthesis of SVO for ICD primary batteries

NASA Astrophysics Data System (ADS)

Beninati, Sabina; Fantuzzi, Matteo; Mastragostino, Marina; Soavi, Francesca

An Ag 2V 4O 11 (SVO) cathode material prepared by microwave (MW)-assisted solid-state synthesis (MW-SVO) was developed for lithium primary batteries for implantable cardioverter/defibrillators (ICDs). This paper presents the results of physical-chemical and electrochemical characterizations of MW-SVO as well as those of SVO prepared by conventional thermal route (T-SVO). A specific effect of MWs which accelerates the synthesis reaction and contributes to yield a material of different morphology and degree of crystallinity compared with those of T-SVO was observed. The results of pulsed electrochemical tests carried out at 37 °C in operative conditions of ICDs on Li/MW-SVO batteries with cathode mass loading sized for practical use are also reported. These tests demonstrated that MW-SVO can be used for high performing lithium primary battery delivering in few seconds the specific energy values required by ICD application.

Synthesis, characterization and oxidation of metallic cobalt (Co) thin film into semiconducting cobalt oxide (Co3O4)thin film using microwave plasma CVD

NASA Astrophysics Data System (ADS)

Rahman Ansari, Akhalakur; Hussain, Shahir; Imran, Mohd; Abdel-wahab, M. Sh; Alshahrie, Ahmed

2018-06-01

The pure cobalt thin film was deposited on the glass substrate by using DC magnetron sputtering and then exposed to microwave assist oxygen plasma generated in microwave plasma CVD. The oxidation process of Co thin film into Co3O4 thin films with different microwave power and temperature were studied. The influences of microwave power, temperature and irradiation time were investigated on the morphology and particle size of oxide thin films. The crystal structure, chemical conformation, morphologies and optical properties of oxidized Co thin films (Co3O4) were studied by using x-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Raman Spectroscopy and UV–vis Spectroscopy. The data of these films showed complete oxidation pure metallic cobalt (Co) into cobalt oxide (Co3O4). The optical properties were studied for calculating the direct band gaps which ranges from 1.35 to 1.8 eV.

A low cost technique for synthesis of gold nanoparticles using microwave heating and its application in signal amplification for detecting Escherichia Coli O157:H7 bacteria

NASA Astrophysics Data System (ADS)

Thanh Ngo, Vo Ke; Giang Nguyen, Dang; Phat Huynh, Trong; Lam, Quang Vinh

2016-09-01

In the present work a low cost technique for preparation of gold nanoparticles (AuNPs) using microwave heating was developed. The effect of different elements (precursor reagents, irradiation time, and microwave radiation power) on the final morphology of AuNPs obtained through the microwave assisted technique has been investigated. The characterization of the samples has been carried out by transmission electron microscopy, UV-vis absorption spectroscopy, Fourier transform infrared spectroscopy, and powder x-ray diffraction. The results showed that to some extent the above-mentioned characterizations influenced the size of synthetized nanoparticles and application of microwave heating has many advantages such as low cost, rapid preparation and highly uniform particles. As an application in quartz crystal microbalance (QCM) immunosensor, AuNPs are conjugated with the Escherichia coli (E.coli) O157:H7 antibodies for signal amplification to detect E.coli O157:H7 bacteria residual in QCM system.

Green Extraction of Natural Antioxidants from the Sterculia nobilis Fruit Waste and Analysis of Phenolic Profile.

PubMed

Zhang, Jiao-Jiao; Li, Ya; Lin, Sheng-Jun; Li, Hua-Bin

2018-05-02

The waste of Sterculia nobilis fruit was massively produced during food processing, which contains lots of natural antioxidants. In this study, antioxidants in the Sterculia nobilis fruit waste were extracted using the green microwave-assisted extraction (MAE) technique. The effects of five independent variables (ethanol concentration, solvent/material ratio, extraction time, temperature, and microwave power) on extraction efficiency were explored, and three major factors (ethanol concentration, extraction time, and temperature) showing great influences were chosen to study their interactions by response surface methodology. The optimal conditions were as follows: 40.96% ethanol concentration, 30 mL/g solvent/material ratio, 37.37 min extraction time at 66.76 °C, and 700 W microwave power. The Trolox equivalent antioxidant capacity value obtained in optimal conditions was in agreement with the predicted value. Besides, MAE improved the extraction efficiency compared with maceration and Soxhlet extraction methods. Additionally, the phenolic profile in the extract was analyzed by UPLC-MS/MS, and eight kinds of phenolic compounds were identified and quantified, including epicatechin, protocatechuic acid, ferulic acid, gallic acid, p -coumaric acid, caffeic acid, quercetin, and p -hydroxycinnamic acid. This study could contribute to the value-added utilization of the waste from Sterculia nobilis fruit, and the extract could be developed as food additive or functional food.

A New Route to Azafluoranthene Natural Products via Direct Arylation

PubMed Central

Ponnala, Shashikanth; Harding, Wayne W.

2013-01-01

Microwave-assisted direct arylation was successfully employed in the synthesis of azafluoranthene alkaloids for the first time. Direct arylation reactions on a diverse set of phenyltetrahydroisoquinolines produces the indeno[1,2,3-ij]isoquinoline nucleus en route to a high yielding azafluoranthene synthesis. The method was used as a key step in the efficient preparation of the natural products rufescine and triclisine. As demonstrated herein, this synthetic approach should be generally applicable to the preparation of natural and un-natural azafluoranthene alkaloids as well as “azafluoranthene-like” isoquinoline alkaloids. PMID:23503080

Microwave-assisted rapid synthesis and characterization of CaF₂ particles-filled cellulose nanocomposites in ionic liquid.

PubMed

Deng, Fu; Fu, Lian-Hua; Ma, Ming-Guo

2015-05-05

In this article, we try to compound cellulose/alkali earth metal fluorides (MF2, M=Ca, Mg, Sr, Ba) nanocomposites via microwave-assisted ionic liquid method, wherein cellulose/CaF2 and cellulose/MgF2 were successfully synthesized through this method while cellulose/SrF2 and cellulose/BaF2 could not be synthesized. We focused on the synthesis of cellulose/CaF2 and investigated the influences of the different time and different temperature for the synthesis of cellulose/CaF2 nanocomposites. The influence of different heating methods such as oil-bath heating method was also studied. Ionic liquid ([Bmim][BF4]) was used for dissolving microcrystalline cellulose and providing the source of fluoride ionic and the alkali earth metal nitrate (Ca(NO3)2, Mg(NO3)2, Sr(NO3)2, and Ba(NO3)2) was used as the reaction initiator. They were investigated by X-ray powder diffraction (XRD), Fourier transform infrared spectrometry (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TG), derivative thermogravimetric (DTG), and energy-dispersive X-ray spectra (EDS). The different heating modes have influence on the morphology and property. The different temperature and heating time also have a certain influence on the morphology and crystallinity of calcium fluoride. Copyright © 2014 Elsevier Ltd. All rights reserved.

Microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid for the determination of sulfonamides in environmental water samples.

PubMed

Song, Ying; Wu, Lijie; Lu, Chunmei; Li, Na; Hu, Mingzhu; Wang, Ziming

2014-12-01

An easy, quick, and green method, microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid, was first developed and applied to the extraction of sulfonamides in environmental water samples. 1-Ethy-3-methylimidazolium hexafluorophosphate, which is a solid-state ionic liquid at room temperature, was used as extraction solvent in the present method. After microwave irradiation for 90 s, the solid-state ionic liquid was melted into liquid phase and used to finish the extraction of the analytes. The ionic liquid and sample matrix can be separated by freezing and centrifuging. Several experimental parameters, including amount of extraction solvent, microwave power and irradiation time, pH of sample solution, and ionic strength, were investigated and optimized. Under the optimum experimental conditions, good linearity was observed in the range of 2.00-400.00 μg/L with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for sulfathiazole, sulfachlorpyridazine, sulfamethoxazole, and sulfaphenazole were 0.39, 0.33, 0.62, and 0.85 μg/L, respectively. When the present method was applied to the analysis of environmental water samples, the recoveries of the analytes ranged from 75.09 to 115.78% and relative standard deviations were lower than 11.89%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Eco-friendly microwave-assisted green and rapid synthesis of well-stabilized gold and core-shell silver-gold nanoparticles.

PubMed

El-Naggar, Mehrez E; Shaheen, Tharwat I; Fouda, Moustafa M G; Hebeish, Ali A

2016-01-20

Herein, we present a new approach for the synthesis of gold nanoparticles (AuNPs) individually and as bimetallic core-shell nanoparticles (AgNPs-AuNPs). The novelty of the approach is further maximized by using curdlan (CRD) biopolymer to perform the dual role of reducing and capping agents and microwave-aided technology for affecting the said nanoparticles with varying concentrations in addition to those affected by precursor concentrations. Thus, for preparation of AuNPs, curdlan was solubilized in alkali solution followed by an addition of tetrachloroauric acid (HAuCl4). The curdlan solution containing HAuCl4 was then subjected to microwave radiation for up to 10 min. The optimum conditions obtained with the synthesis of AuNPs were employed for preparation of core-shell silver-gold nanoparticles by replacing definite portion of HAuCl4 with an equivalent portion of silver nitrate (AgNO3). The portion of AgNO3 was added initially and allowed to be reduced by virtue of the dual role of curdlan under microwave radiation. The corresponding portion of HAuCl4 was then added and allowed to complete the reaction. Characterization of AuNPs and AgNPs-AuNPs core-shell were made using UV-vis spectra, TEM, FTIR, XRD, zeta potential, and AFM analysis. Accordingly, strong peaks of the colloidal particles show surface plasmon resonance (SPR) at maximum wavelength of 540 nm, proving the formation of well-stabilized gold nanoparticles. TEM investigations reveal that the major size of AuNPs formed at different Au(+3)concentration lie below 20 nm with narrow size distribution. Whilst, the SPR bands of AgNPs-AuNPs core-shell differ than those obtained from original AgNPs (420 nm) and AuNPs (540 nm). Such shifting due to SPR of Au nanoshell deposited onto AgNPs core was significantly affected by the variation of bimetallic ratios applied. TEM micrographs show variation in contrast between dark silver core and the lighter gold shell. Increasing the ratio of silver ions leads to significant decrease in zeta potential of the formed bimetallic core-shell. FT-IR discloses the interaction between CRD and metal nanoparticles, which could be the question of reducing and stabilizing metal and bimetallic nanoparticles. XRD patterns assume insufficient difference for the AuNPs and AgNPs-AuNPs core-shell samples due to close lattice constants of Ag and Au. Based on AFM, AuNPs and AgNPs-AuNPs core-shell exhibited good monodispersity with spherical particles possessing different sizes in the studied samples. The average sizes of both metal and bimetallic core-shell were found to be 52 and 45 nm, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

Rapid Polyol-Assisted Microwave Synthesis of Nanocrystalline LiFePO4/C Cathode for Lithium-Ion Batteries.

PubMed

Paul, Baboo Joseph; Gim, Jihyeon; Baek, Sora; Kang, Jungwon; Song, Jinju; Kim, Sungjin; Kim, Jaekook

2015-08-01

Nanocrystalline LiFePO4/C has been synthesized under a very short period of time (90 sec) using a polyol-assisted microwave heating synthesis technique. The X-ray diffraction (XRD) data indicates that the rapidly synthesized materials correspond to phase pure olivine. Post-annealing of the as-prepared sample at 600 °C in argon atmosphere yields highly crystalline LiFePO4/C. The morphology of the samples studied using scanning electron microscopy (SEM) reveals the presence of secondary particles formed from aggregation of primary particles in the range of 30-50 nm. Transmission electron microscopy (TEM) images reveal a thin carbon layer coating on the surface of the primary particle. The charge/discharge studies indicate that the as-prepared and annealed LiFePO4/C samples delivered initial discharge capacities of 126 and 160 mA h g-1, respectively, with good capacity retentions at 0.05 mA cm-2 current densities. The post-annealing process indeed improves the crystallinity of the LiFePO4 nanocrystals, which enhances the electrode performance of LiFePO4/C.

Microwave-assisted synthesis of novel purine nucleosides as selective cholinesterase inhibitors.

PubMed

Schwarz, S; Csuk, R; Rauter, A P

2014-04-21

Alzheimer's disease (AD), the most common form of senile dementia, is characterized by high butyrylcholinesterase (BChE) levels in the brain in later AD stages, for which no treatment is available. Pursuing our studies on selective BChE inhibitors, that may contribute to understand the role of this enzyme in disease progression, we present now microwave-assisted synthesis and anticholinesterase activity of a new nucleoside series embodying 6-chloropurine or 2-acetamido-6-chloropurine linked to D-glucosyl, D-galactosyl and D-mannosyl residues. It was designed to assess the contribution of sugar stereochemistry, purine structure and linkage to the sugar for cholinesterase inhibition efficiency and selectivity. Compounds were subjected to Ellman's assay and their inhibition constants determined. The α-anomers were the most active compounds, while selectivity for BChE or acetylcholinesterase (AChE) inhibition could be tuned by the purine base, by the glycosyl moiety and by N(7)-ligation. Some of the nucleosides were far more potent than the drug galantamine, and the most promising competitive and selective BChE inhibitor, the N(7)-linked 2-acetamido-α-D-mannosylpurine, showed a Ki of 50 nM and a selectivity factor of 340 fold for BChE over AChE.

Synthesis and Characterization of Doped ZnO Nanomaterials: Potential Application in Third Generation Solar Cells

NASA Astrophysics Data System (ADS)

Adcock Smith, Echo D.

ZnO nanomaterials are being incorporated into next-generation solar cell designs including dye-sensitized solar cells, multijunction solar cells, and quantum dot sensitized solar cells. ZnO nanorod (NR) arrays and nanoparticles (NP) used in these devices are typically fabricated using chemical vapor deposition and/or high-temperature reaction conditions. These methods are costly, require high energy, pressure or excessive time, but produce repeatable, defined growth that is capable of easily incorporating metal dopants. Less expensive methods of fabrication such as chemical bath deposition (CBD) eliminate the costly steps but can suffer from undefined growth, excessive waste and have a difficult time incorporating dopants into ZnO materials without additives or increased pH. This dissertation presents a novel method of growing cobalt and vanadium doped ZnO nanomaterials through microwave synthesis. The cobalt growth was compared to standard CBD and found to be faster, less wasteful, reproducible and better at incorporating cobalt ions into the ZnO lattice than typical oven CBD method. The vanadium doped ZnO microwave synthesis procedure was found to produce nanorods, nanorod arrays, and nanoparticles simultaneously. Neither the cobalt nor the vanadium growth required pH changes, catalysts or additives to assist in doping and therefore use less materials than traditional CBD. This research is important because it offers a simple, quick way to grow ZnO nanostructures and is the first to report on growing both cobalt and vanadium doped zinc oxide nanorod arrays using microwave synthesis. This synthesis method presented is a viable candidate for replacing conventional growth synthesis which will result in lowering the cost and time of production of photovoltaics while helping drive forward the development of next-generation solar cells.

Synthesis of alkyl- and aryl-amino-substituted anthraquinone derivatives by microwave-assisted copper(0)-catalyzed Ullmann coupling reactions.

PubMed

Baqi, Younis; Müller, Christa E

2010-05-01

This protocol describes the efficient, generally applicable Ullmann coupling reaction of bromaminic acid with alkyl- or aryl-amines in phosphate buffer under microwave irradiation using elemental copper as a catalyst. The reaction leads to a number of biologically active compounds. As a prototypical example, the synthesis of a new, potent antagonist of human platelet P2Y(12) receptors, which has potential as an antithrombotic drug, is described in detail. The optimized protocol includes a description of an appropriate reaction setup, thin layer chromatography for monitoring the reaction and a procedure for the isolation, purification and characterization of the anticipated product. The reaction is performed without the use of a glove box and there is no requirement for an inert atmosphere. The reaction typically proceeds within 2-30 min, the protocol, including workup, generally takes 1-3 h to complete.

Microwave assisted growth of nanorods vanadium dioxide VO2 (R): structural and electrical properties

NASA Astrophysics Data System (ADS)

Derkaoui, I.; Khenfouch, M.; Mothudi, B. M.; Moloi, S. J.; Zorkani, I.; Jorio, A.; Maaza, M.

2018-03-01

Nanostructured metal oxides have attracted a lot of attention recently owning to their unique structural advantages and demonstrated promising chemical and physical properties for various applications. In this study, we report the structural and electrical properties of vanadium dioxide VO2 (R) prepared via a single reaction microwave (SRC) synthesis. Our results are revealing that the components of VO2 (R) films have a rod-like shape with a uniform size distribution. The nanorods with very smooth and flat surfaces have a typical length of up to 2μm and a width of about several nanometers. The structural investigations reveal the high crystallinity of VO2 (R) ensuring good electrical contact and showing a high conductivity as a function of temperature. This synthesis method provides a new simple route to fabricate one-dimensional nanostructured metal oxides which is suitable for a large field of applications especially for smart windows.

Antifreeze glycopeptide analogues: microwave-enhanced synthesis and functional studies.

PubMed

Heggemann, Carolin; Budke, Carsten; Schomburg, Benjamin; Majer, Zsuzsa; Wissbrock, Marco; Koop, Thomas; Sewald, Norbert

2010-01-01

Antifreeze glycoproteins enable life at temperatures below the freezing point of physiological solutions. They usually consist of the repetitive tripeptide unit (-Ala-Ala-Thr-) with the disaccharide alpha-D-galactosyl-(1-3)-beta-N-acetyl-D-galactosamine attached to each hydroxyl group of threonine. Monoglycosylated analogues have been synthesized from the corresponding monoglycosylated threonine building block by microwave-assisted solid phase peptide synthesis. This method allows the preparation of analogues containing sequence variations which are not accessible by other synthetic methods. As antifreeze glycoproteins consist of numerous isoforms they are difficult to obtain in pure form from natural sources. The synthetic peptides have been structurally analyzed by CD and NMR spectroscopy in proton exchange experiments revealing a structure as flexible as reported for the native peptides. Microphysical recrystallization tests show an ice structuring influence and ice growth inhibition depending on the concentration, chain length and sequence of the peptides.

Effect of microwave-assisted sintering on dielectric properties of CaCu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Rani, Suman; Ahlawat, Neetu; Punia, R.; Kundu, R. S.; Ahlawat, N.

2016-05-01

In this present work, CaCu3Ti4O12 (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It was observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.

Microwave-assisted extraction for Hibiscus sabdariffa bioactive compounds.

PubMed

Pimentel-Moral, Sandra; Borrás-Linares, Isabel; Lozano-Sánchez, Jesús; Arráez-Román, David; Martínez-Férez, Antonio; Segura-Carretero, Antonio

2018-07-15

H. sabdariffa has demonstrated positive results against chronic diseases due to the presence of phytochemicals, mainly phenolic compounds. The extraction process of bioactive compounds increases the efficient collection of extracts with high bioactivity. Microwave-Assisted Extraction (MAE) constituted a "green technology" widely employed for plant matrix. In this work, the impact of temperature (50-150 °C), composition of extraction solvent (15-75% EtOH) and extraction time (5-20 min) on the extraction yield and individual compounds concentrations were evaluated. Furthermore, the characterization of 16 extracts obtained was performed by HPLC-ESI-TOF-MS. The results showed that 164 °C, 12.5 min, 45% ethanol was the best extraction condition, although glycoside flavonoids were degraded. Besides that, the optimal conditions for extraction yield were 164 °C, 60% ethanol and 22 min. Thus, temperature and solvent concentration have demonstrated to be potential factors in MAE for obtaining bioactive compounds from H. sabdariffa. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis of BiFeO{sub 3} thin films on single-terminated Nb : SrTiO{sub 3} (111) substrates by intermittent microwave assisted hydrothermal method

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

Velasco-Davalos, Ivan; Ambriz-Vargas, Fabian; Kolhatkar, Gitanjali

We report on a simple and fast procedure to create arrays of atomically flat terraces on single crystal SrTiO{sub 3} (111) substrates and the deposition of ferroelectric BiFeO{sub 3} thin films on such single-terminated surfaces. A microwave-assisted hydrothermal method in deionized water and ammonia solution selectively removes either (SrO{sub 3}){sup 4−} or Ti{sup 4+} layers to ensure the same chemical termination on all terraces. Measured step heights of 0.225 nm (d{sub 111}) and uniform contrast in the phase image of the terraces confirm the single termination in pure and Nb doped SrTiO{sub 3} single crystal substrates. Multiferroic BiFeO{sub 3} thinmore » films were then deposited by the same microwave assisted hydrothermal process on Nb : SrTiO{sub 3} (111) substrates. Bi(NO{sub 3}){sub 3} and Fe(NO{sub 3}){sub 3} along with KOH served as the precursors solution. Ferroelectric behavior of the BiFeO{sub 3} films on Nb : SrTiO{sub 3} (100) substrates was verified by piezoresponse force microscopy.« less

PLE in the analysis of plant compounds. Part I. The application of PLE for HPLC analysis of caffeine in green tea leaves.

PubMed

Dawidowicz, Andrzej L; Wianowska, Dorota

2005-04-29

A broad spectrum of sample preparation methods is currently used for the isolation of pharmacologically active compounds from plant and herbal materials. The paper compares the effectiveness of infusion, microwave assisted solvent extraction (MASE), matrix solid-phase dispersion (MSPD) and pressurised liquid extraction (PLE) as sample preparation methods for the isolation of caffeine from green tea leaves. The effect of PLE variables, such as extraction temperature, pressure and time, on the yield of caffeine from the investigated matrix is discussed. The obtained results revealed that PLE, in comparison with other sample preparation methods applied, has significantly lower efficacy for caffeine isolation from green tea leaves. The evaluation of PLE conditions leads to the conclusion that elevated pressure applied in the PLE process is the factor hindering the extraction.

Green procedure with a green solvent for fats and oils' determination. Microwave-integrated Soxhlet using limonene followed by microwave Clevenger distillation.

PubMed

Virot, Matthieu; Tomao, Valérie; Ginies, Christian; Visinoni, Franco; Chemat, Farid

2008-07-04

Here is described a green and original alternative procedure for fats and oils' determination in oleaginous seeds. Extractions were carried out using a by-product of the citrus industry as extraction solvent, namely d-limonene, instead of hazardous petroleum solvents such as n-hexane. The described method is achieved in two steps using microwave energy: at first, extractions are attained using microwave-integrated Soxhlet, followed by the elimination of the solvent from the medium using a microwave Clevenger distillation in the second step. Oils extracted from olive seeds were compared with both conventional Soxhlet and microwave-integrated Soxhlet extraction procedures performed with n-hexane in terms of qualitative and quantitative determination. No significant difference was obtained between each extract allowing us to conclude that the proposed method is effective and valuable.

ARTICLES: Microwave Assisted Synthesis of a New Triplet Iridium(III) Pyrazine Complex

NASA Astrophysics Data System (ADS)

Wu, Qiu-hua; Wang, Chuan-hong; Song, Xi-ming; Zhang, Guo-lin

2010-06-01

A new cyclometalated iridium(III) complex Ir(DPP)3 (DPP = 2,3-diphenylpyrazine) was prepared by reaction of DPP with iridium trichloride hydrate under microwave irradiation. The structure of the complex was confirmed by elemental analysis, 1H NMR, and mass spectroscopy. The UV-Vis absorption and photoluminescent properties of the complex were investigated. The complex shows strong 1MLCT (singlet metal to ligand charge-transfer) and 3MLCT (triplet metal to ligand charge-transfer) absorption at 382 and 504 nm, respectively. The complex also shows strong photoluminescence at 573 nm at room temperature. These results suggest the complex to be a promising phosphorescent material.

Nonlinear optical behavior of two tetrathiafulvalene derivatives in the picosecond regime

NASA Astrophysics Data System (ADS)

Marcovicz, Crislaine; Ferreira, Rudson C.; Santos, Arthur B. S.; Reyna, Albert S.; de Araújo, Cid B.; Malvestiti, Ivani; Falcão, Eduardo H. L.

2018-06-01

We report the microwave-assisted synthesis of two symmetrical tetrathiafulvalene (TTF) derivatives via trialkyl phosphite-promoted coupling of a DMIT precursor. The microwave irradiation led to an increase in the reaction yield and significantly reduced the reaction time, affording the 2,3,6,7-tetrakis(2‧-methylacetatethio)tetrathiafulvalene (4) in 74% isolated yield. Hydrolysis of 4 yielded the tetraacid 5 in excellent yield. The nonlinear optical properties of both TTF compounds at 532 nm were studied by using the Z-scan technique in the picosecond regime exhibiting large third-order refractive index and saturated nonlinear absorption with promising applications in optical limiting devices.

Microwave assisted synthesis of bis and tris(ω-bromoacetophenones): versatile precursors for novel bis(imidazo[1,2-a]pyridines), bis(imidazo[1,2-a]pyrimidines) and their tris-analogs

PubMed Central

2013-01-01

Background α-Bromination of the side chain of aromatic ketones using NBS in the presence of p-toluenesulfonic acid (p-TsOH) in acetonitrile is very common. However, regioselective bromination of bis and tris(ω-bromoacetophenones) with NBS in the presence of p-TsOH in acetonitrile under microwave irradiation is quite novel. The bis- and tris(ω-bromoacetophenones) are used in synthesis of bis and tris(heterocycles). bis(heterocycles) have received a great deal of attention, because many biologically active natural and synthetic products have molecular symmetry. The use of the pressurized microwave irradiation is very advantageous to many syntheses and provide a large rate enhancement. Results Bis and tris(ω-bromoacetophenones) were obtained as single monobrominated derivatives in a shorter time than the conventional conditions. The results clearly demonstrate the better reactivity and selectivity of NBS/p-TsOH/CH3CN as a brominating mixture under microwave conditions. The reaction of bis and tris(ω-bromoacetophenone) with 2-aminopyridine and 2-aminopyrimidine proceeded smoothly in a mixture of anhydrous ethanol and DMF under reflux or using 300 W/105°C/ 20 min microwave irradiation conditions to afford the corresponding bis(imidazo[1,2-a]pyridine), bis(imidazo[1,2-a]pyrimidine) and tris(imidazo[1,2-a]pyridine) derivatives in moderate to excellent yields. The carbonyl analogue of the targeted bis(imidazopyridines) could be synthesized by the reaction of N,N-dimethyl-N'-(pyridin-2-yl)formimidamide with bis(ω-bromoacetophenone) in refluxing ethanol. The structures of the newly synthesized compounds were confirmed by their spectral data as well as their elemental analyses. Conclusion In conclusion, selective α-bromination of bis- and tris(acetophenones) has been accomplished efficiently utilizing NBS/p-TsOH/CH3CN under microwave irradiation. In addition, a facile synthesis of novel series of bis- and tris(imidazopyridine) and bis(imidazopyrimidine) derivatives. PMID:23782550

Enhanced low-temperature lithium storage performance of multilayer graphene made through an improved ionic liquid-assisted synthesis

NASA Astrophysics Data System (ADS)

Raccichini, Rinaldo; Varzi, Alberto; Chakravadhanula, Venkata Sai Kiran; Kübel, Christian; Balducci, Andrea; Passerini, Stefano

2015-05-01

The electrochemical properties of graphene are strongly depending on its synthesis. Between the different methods proposed so far, liquid phase exfoliation turns out to be a promising method for the production of graphene. Unfortunately, the low yield of this technique, in term of solid material obtained, still limit its use to small scale applications. In this article we propose a low cost and environmentally friendly method for producing multilayer crystalline graphene with high yield. Such innovative approach, involving an improved ionic liquid assisted, microwave exfoliation of expanded graphite, allows the production of graphene with advanced lithium ion storage performance, for the first time, at low temperatures (<0 °C), as low as -30 °C, with respect to commercially available graphite.

Microwave-synthesized freestanding iron-carbon nanotubes on polyester composites of woven Kevlar fibre and silver nanoparticle-decorated graphene

NASA Astrophysics Data System (ADS)

Hazarika, Ankita; Deka, Biplab K.; Kim, Doyoung; Kong, Kyungil; Park, Young-Bin; Park, Hyung Wook

2017-01-01

We synthesized Ag nanoparticle-decorated multilayered graphene nanosheets (Ag-graphene) from graphite nanoplatelets and silver nitrate through 90-100 s of microwave exposure, without the use of any mineral acids or harsh reducing agents. Fe nanoparticle-decorated carbon nanotubes (Fe-CNTs) were grown on polypyrrole (PPy) deposited on woven Kevlar fibre (WKF), using ferrocene as a catalyst, under microwave irradiation. Fe-CNTs grown on WKF and Ag-graphene dispersed in polyester resin (PES) were combined to fabricate Ag-graphene/Fe-CNT/PPy-coated WKF/PES composites by vacuum-assisted resin transfer moulding. The combined effect of Fe-CNTs and Ag-graphene in the resulting composites resulted in a remarkable enhancement of tensile properties (a 192.56% increase in strength and 100.64% increase in modulus) as well as impact resistance (a 116.33% increase). The electrical conductivity significantly increased for Ag-graphene/Fe-CNT/PPy-coated WKF/PES composites. The effectiveness of electromagnetic interference shielding, which relies strongly on the Ag-graphene content in the composites, was 25 times higher in Ag-graphene/Fe-CNT/PPy-coated WKF/PES than in neat WKF/PES composites. The current work offers a novel route for fabricating highly promising, cost effective WKF/PES composites through microwave-assisted synthesis of Fe-CNTs and Ag-graphene.

Microwave-synthesized freestanding iron-carbon nanotubes on polyester composites of woven Kevlar fibre and silver nanoparticle-decorated graphene.

PubMed

Hazarika, Ankita; Deka, Biplab K; Kim, DoYoung; Kong, Kyungil; Park, Young-Bin; Park, Hyung Wook

2017-01-11

We synthesized Ag nanoparticle-decorated multilayered graphene nanosheets (Ag-graphene) from graphite nanoplatelets and silver nitrate through 90-100 s of microwave exposure, without the use of any mineral acids or harsh reducing agents. Fe nanoparticle-decorated carbon nanotubes (Fe-CNTs) were grown on polypyrrole (PPy) deposited on woven Kevlar fibre (WKF), using ferrocene as a catalyst, under microwave irradiation. Fe-CNTs grown on WKF and Ag-graphene dispersed in polyester resin (PES) were combined to fabricate Ag-graphene/Fe-CNT/PPy-coated WKF/PES composites by vacuum-assisted resin transfer moulding. The combined effect of Fe-CNTs and Ag-graphene in the resulting composites resulted in a remarkable enhancement of tensile properties (a 192.56% increase in strength and 100.64% increase in modulus) as well as impact resistance (a 116.33% increase). The electrical conductivity significantly increased for Ag-graphene/Fe-CNT/PPy-coated WKF/PES composites. The effectiveness of electromagnetic interference shielding, which relies strongly on the Ag-graphene content in the composites, was 25 times higher in Ag-graphene/Fe-CNT/PPy-coated WKF/PES than in neat WKF/PES composites. The current work offers a novel route for fabricating highly promising, cost effective WKF/PES composites through microwave-assisted synthesis of Fe-CNTs and Ag-graphene.

Microwave-assisted in situ synthesis of reduced graphene oxide-BiVO4 composite photocatalysts and their enhanced photocatalytic performance for the degradation of ciprofloxacin.

PubMed

Yan, Yan; Sun, Shaofang; Song, Yang; Yan, Xu; Guan, Weisheng; Liu, Xinlin; Shi, Weidong

2013-04-15

To improve the photodegradation efficiency for ciprofloxacin (CIP), a new-type microwave-assisted in situ growth method is developed for the preparation of reduced graphene oxide (RGO) -BiVO4 composite photocatalysts. The as-produced RGO-BiVO4 composite photocatalysts show extremely high enhancement of CIP degradation ratio over the pure BiVO4 photocatalyst under visible light. Specially, the 2 wt% RGO-BiVO4 composite photocatalyst exhibits the highest CIP degradation ratio (68.2%) in 60 min, which is over 3 times than that (22.7%) of the pure BiVO4 particles. The enhancement of photocatalytic activities of RGO-BiVO4 photocatalysts can be attributed to the effective separation of electron-hole pairs rather than the improvement of light absorption. Copyright © 2013 Elsevier B.V. All rights reserved.

Microwave Assisted-Method for the Synthesis of Perylene Ester Imides as a Gateway towards Unsymmetrical Perylene Bisimides.

PubMed

Gupta, Ravindra Kumar; Achalkumar, Ammathnadu Sudhakar

2018-05-18

A high yielding microwave-assisted synthetic method to obtain unsymmetrical perylene diester monoimide (PEI), by treating the perylene tetrester (PTE) with requisite amine is reported. Perylene-based molecules are widely used in the construction of self-assembled supramolecular structures because of their propensity to aggregate under various conditions. In comparison to perylene bisimides (PBIs), PEIs are less studied in organic electronics/self-assembly due to the synthetic difficulty and low yields in their preparation. PEIs are less electron deficient and have an unsymmetric structure in comparison to PBIs. Further, the PEIs got higher solubility than PBIs. The present method is applicable with a wide range of substrates like aliphatic, aromatic, benzyl amines, PTEs and bay-annulated PTEs. This method provides a tuning handle for the optical/electronic properties of perylene derivatives and also provides an easy access to unsymmetrical PBIs from the PEIs.

Microwave-assisted synthesis and characterization of nickel ferrite nanoparticles

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

Carpenter, Gopal; Sen, Ravindra; Gupta, Nitish, E-mail: nitish.nidhi75@gmail.com

2015-08-28

Nickel ferrite nanoparticles (NiFe{sub 2}O{sub 4}) were successfully prepared by microwave-assisted combustion method (MWAC) using citric Electron acid as a chelating agent. NiFe{sub 2}O{sub 4} nanoparticles were characterized by X-ray diffraction (XRD) pattern, Scanning Microscopy (SEM), Fourier transform infrared (FTIR) and UV-Visible techniques. XRD analysis revealed that NiFe{sub 2}O{sub 4} nanoparticles have spinel cubic structure with the average crystalline size of 26.38 nm. SEM analysis revealed random and porous structural morphology of particles and FTIR showed absorption bands related to octahedral and tetrahedral sites, in the range 400–600cm{sup −1} which strongly favor the formation of NiFe{sub 2}O{sub 4} nanoparticles. The opticalmore » band gap is determined by UV Visible method and found to be 5.4 eV.« less

Polymerization of tellurophene derivatives via microwave-assisted palladium-catalyzed ipso-arylative polymerization**

PubMed Central

Park, Young S.; Wu, Qin; Nam, Chang-Yong; Grubbs, Robert B.

2014-01-01

We report the synthesis of a tellurophene-containing low bandgap polymer, PDPPTe2T, via microwave-assisted palladium-catalyzed ipso-arylative polymerization of 2,5-bis[(α-hydroxy-α,α-diphenyl)methyl]tellurophene with a diketopyrrolopyrrole (DPP) monomer. Compared with the corresponding thiophene analog, PDPPTe2T absorbs light of longer wavelengths and has a smaller bandgap. Bulk heterojunction solar cells prepared from PDPPTe2T and PC71BM show PCE values of up to 4.4%. External quantum efficiency measurements show that PDPPTe2T produces photocurrent at wavelengths up to 1 μm. DFT calculations suggest that the atomic substitution from sulfur to tellurium increases electronic coupling to decrease the length of the carbon-carbon bonds between the tellurophene and thiophene rings, which results in the red-shift in absorption upon substitution of tellurium for sulfur. PMID:25145499

Rapid and Facile Microwave-Assisted Surface Chemistry for Functionalized Microarray Slides

PubMed Central

Lee, Jeong Heon; Hyun, Hoon; Cross, Conor J.; Henary, Maged; Nasr, Khaled A.; Oketokoun, Rafiou; Choi, Hak Soo; Frangioni, John V.

2011-01-01

We describe a rapid and facile method for surface functionalization and ligand patterning of glass slides based on microwave-assisted synthesis and a microarraying robot. Our optimized reaction enables surface modification 42-times faster than conventional techniques and includes a carboxylated self-assembled monolayer, polyethylene glycol linkers of varying length, and stable amide bonds to small molecule, peptide, or protein ligands to be screened for binding to living cells. We also describe customized slide racks that permit functionalization of 100 slides at a time to produce a cost-efficient, highly reproducible batch process. Ligand spots can be positioned on the glass slides precisely using a microarraying robot, and spot size adjusted for any desired application. Using this system, we demonstrate live cell binding to a variety of ligands and optimize PEG linker length. Taken together, the technology we describe should enable high-throughput screening of disease-specific ligands that bind to living cells. PMID:23467787

One-pot microwave assisted synthesis and structural elucidation of novel ethyl 3-substituted-7-methylindolizine-1-carboxylates with larvicidal activity against Anopheles arabiensis

NASA Astrophysics Data System (ADS)

Chandrashekharappa, Sandeep; Venugopala, Katharigatta N.; Nayak, Susanta K.; Gleiser, Raquel M.; García, Daniel A.; Kumalo, Hezekiel M.; Kulkarni, Rashmi S.; Mahomoodally, Fawzi M.; Venugopala, Rashmi; Mohan, Mahendra K.; Odhav, Bharti

2018-03-01

In the present investigation a series of novel ethyl 3-substituted-7-methylindolizine-1-carboxylates was achieved by microwave assisted one-pot method. The purity of the compounds was ascertained by HPLC and structural elucidation of the title compounds was achieved by FT-IR, NMR (1H and 13C), LC-MS and elemental analysis. One randomly selected compound from the series was further studied by single crystal X-ray method for intra and intermolecular interactions. Larvicidal properties of the characterized compounds were evaluated against Anopheles arabiensis and it was found that indolizine pharmacophore influences larvicidal activity as we can see larvicidal activity for all the analogues. The synthesized analogues (2j, 2m and 2f) were the most potent compounds based on the functional groups on the indolizine pharmacophore for larvicidal assay.

Design and assembly of new non-viral RNAi delivery agents by microwave-assisted quaternization (MAQ) of tertiary amines

PubMed Central

Ghosh, Animesh; Mukherjee, Koushik; Jiang, Xinpeng; Zhou, Ying; McCarroll, Joshua; Qu, James; Swain, Pamela M.; Baigude, Huricha; Rana, Tariq M.

2010-01-01

RNA interference (RNAi), a gene-silencing phenomenon whereby double-stranded RNA (dsRNA) triggers the sequence-specific degradation of homologous mRNA. RNAi has been quickly and widely applied to discover gene functions and holds great potential to provide a new class of therapeutic agents. However, new chemistry and delivery approaches are greatly needed to silence disease-causing genes without toxic effects. We reasoned that conjugation of the cholesterol moiety to cationic lipids would enhance RNAi efficiencies and lower the toxic effects of lipid-mediated RNAi delivery. Here, we report the first design and synthesis of new cholesterol-conjugated cationic lipids for RNAi delivery using microwave-assisted quaternization (MAQ) of tertiary amines. This strategy can be employed to develop new classes of non-viral gene delivery agents under safe and fast reaction conditions. PMID:20722369

Chemo-selective high yield microwave assisted reaction turns cellulose to green chemicals.

PubMed

Hassanzadeh, Salman; Aminlashgari, Nina; Hakkarainen, Minna

2014-11-04

Exceptionally high cellulose liquefaction yields, up to 87% as calculated from the amount of solid residue, were obtained under mild conditions by utilizing the synergistic effect of microwave radiation and acid catalysis. The effect of processing conditions on degradation products was fingerprinted by rapid laser desorption ionization-mass spectrometry (LDI-MS) method. The reaction was chemo-tunable, enabling production of glucose (Glc) or levulinic acid (LeA) at significantly high selectivity and yields, the relative molar yields being up to 50 and 69%, respectively. A turning point from pure depolymerization to glucose to further degradation to levulinic acid and formic acid was observed at approximately 50% liquefaction or above 140 °C. This was accompanied by the formation of small amounts of solid spherical carbonized residues. The reaction was monitored by multiple analytical techniques. The high yields were connected to the ability of the process to break the strong secondary interactions in cellulose. The developed method has great potential for future production of green platform chemicals. Copyright © 2014 Elsevier Ltd. All rights reserved.

Microwave Assisted Enzymatic Kinetic Resolution of (±)-1-Phenyl-2-propyn-1-ol in Nonaqueous Media

PubMed Central

Devendran, Saravanan; Yadav, Ganapati D.

2014-01-01

Kinetic resolution of 1-phenyl-2-propyn-1-ol, an important chiral synthon, was studied through trans-esterification with acyl acetate to investigate synergism between microwave irradiation and enzyme catalysis. Lipases from different microbial origins were employed for the kinetic resolution of (R/S)-1-phenyl-2-propyn-1-ol, among which Candida antarctica lipase B, immobilized on acrylic resin (Novozym 435), was found to be the best catalyst in n-hexane as solvent. Vinyl acetate was the most effective among different acyl esters studied. The effect of various parameters was studied in a systematic manner. Definite synergism between microwave and enzyme was observed. The initial rate was improved around 1.28 times under microwave irradiation than conventional heating. Under optimum conditions, maximum conversion (48.78%) and high enantiomeric excess (93.25%) were obtained in 2 h. From modeling studies, it is concluded that the reaction follows the Ping-Pong bi-bi mechanism with dead end alcohol inhibition. Kinetic parameters were obtained by using nonlinear regression. This process is green, clean, and easily scalable as compared to the chemical process. PMID:24707487

Intensification of marrubiin concentration by optimization of microwave-assisted (low CO2 yielding) extraction process for Marrubium vulgare using central composite design and antioxidant evaluation.

PubMed

Mittal, Vineet; Nanda, Arun

2017-12-01

Marrubium vulgare Linn (Lamiaceae) was generally extracted by conventional methods with low yield of marrubiin; these processes were not considered environment friendly. This study extracts the whole plant of M. vulgare by microwave assisted extraction (MAE) and optimizes the effect of various extraction parameters on the marrubiin yield by using Central Composite Design (CCD). The selected medicinal plant was extracted using ethanol: water (1:1) as solvent by MAE. The plant material was also extracted using a Soxhlet and the various extracts were analyzed by HPTLC to quantify the marrubiin concentration. The optimized conditions for the microwave-assisted extraction of selected medicinal plant was microwave power of 539 W, irradiation time of 373 s and solvent to drug ratio, 32 mL per g of the drug. The marrubiin concentration in MAE almost doubled relative to the traditional method (0.69 ± 0.08 to 1.35 ± 0.04%). The IC 50 for DPPH was reduced to 66.28 ± 0.6 μg/mL as compared to conventional extract (84.14 ± 0.7 μg/mL). The scanning electron micrographs of the treated and untreated drug samples further support the results. The CCD can be successfully applied to optimize the extraction parameters (MAE) for M. vulgare. Moreover, in terms of environmental impact, the MAE technique could be assumed as a 'Green approach' because the MAE approach for extraction of plant released only 92.3 g of CO 2 as compared to 3207.6 g CO 2 using the Soxhlet method of extraction.

A new method for microwave assisted ethanolic extraction of Mentha rotundifolia bioactive terpenoids.

PubMed

García-Sarrió, María Jesús; Sanz, María Luz; Sanz, Jesús; González-Coloma, Azucena; Cristina Soria, Ana

2018-04-14

A new microwave-assisted extraction (MAE) method using ethanol as solvent has been optimized by means of a Box-Behnken experimental design for the enhanced extraction of bioactive terpenoids from Mentha rotundifolia leaves; 100°C, 5 min, 1.125 g dry sample: 10 mL solvent and a single extraction cycle were selected as optimal conditions. Improved performance of MAE method in terms of extraction yield and/or reproducibility over conventional solid-liquid extraction and ultrasound assisted extraction was also previously assessed. A comprehensive characterization of MAE extracts was carried out by GC-MS. A total of 46 compounds, mostly terpenoids, were identified; piperitenone oxide and piperitenone were the major compounds determined. Several neophytadiene isomers were also detected for the first time in MAE extracts. Different procedures (solid-phase extraction and activated charcoal (AC) treatment) were also evaluated for clean-up of MAE extracts, with AC providing the highest enrichment in bioactive terpenoids. Finally, the MAE method here developed is shown as a green, fast, efficient and reproducible liquid extraction methodology to obtain M. rotundifolia bioactive extracts for further application, among others, as food preservatives. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microwave-assisted direct synthesis of butene from high-selectivity methane

NASA Astrophysics Data System (ADS)

Lu, Yi-heng; Li, Kang; Lu, Yu-wei

2017-12-01

Methane was directly converted to butene liquid fuel by microwave-induced non-oxidative catalytic dehydrogenation under 0.1-0.2 MPa. The results show that, under microwave heating in a two-stage fixed-bed reactor, in which nickel powder and NiOx-MoOy/SiO2 are used as the catalyst, the methane-hydrogen mixture is used as the raw material, with no acetylene detected. The methane conversion is more than 73.2%, and the selectivity of methane to butene is 99.0%. Increasing the hydrogen/methane feed volume ratio increases methane conversion and selectivity. Gas chromatography/electron impact ionization/mass spectrometry chromatographic analysis showed that the liquid fuel produced by methane dehydrogenation oligomerization contained 89.44% of butene, and the rest was acetic acid, ethanol, butenol and butyric acid, and the content was 1.0-3.0 wt%.

Docking studies on a new human immunodeficiency virus integrase-Mg-DNA complex: phenyl ring exploration and synthesis of 1H-benzylindole derivatives through fluorine substitutions.

PubMed

Ferro, Stefania; De Luca, Laura; Barreca, Maria Letizia; Iraci, Nunzio; De Grazia, Sara; Christ, Frauke; Witvrouw, Myriam; Debyser, Zeger; Chimirri, Alba

2009-01-22

A new model of HIV-1 integrase-Mg-DNA complex that is useful for docking experiments has been built. It was used to study the binding mode of integrase strand transfer inhibitor 1 (CHI-1043) and other fluorine analogues. Molecular modeling results prompted us to synthesize the designed derivatives which showed potent enzymatic inhibition at nanomolar concentration, high antiviral activity, and low toxicity. Microwave assisted organic synthesis (MAOS) was employed in several steps of the synthetic pathway, thus reducing reaction times and improving yields.

Synthesis of stereodefined piperidines from aziridines and their transformation into conformationally constrained amino acids, amino alcohols and 2,7-diazabicyclo[3.3.1]nonanes.

PubMed

Vervisch, Karel; D'hooghe, Matthias; Törnroos, Karl W; De Kimpe, Norbert

2010-11-19

2-(2-Cyano-2-phenylethyl)aziridines were converted into novel cis- and trans-2-chloromethyl-4-phenylpiperidine-4-carbonitriles via alkylation with 1-bromo-2-chloroethane followed by microwave-assisted 6-exo-tet cyclization and regiospecific ring opening. The latter piperidines were used as eligible substrates for the synthesis of stereodefined 2-chloromethyl-, 2-hydroxymethyl-, and 2-carboxymethyl-4-phenylpiperidine-4-carboxylic acids, 2-hydroxymethyl-4-phenylpiperidine-4-carbonitriles, 3-hydroxy-5-phenylazepane-5-carbonitriles, and 5-phenyl-2,7-diazabicyclo[3.3.1]nonanes.

Facile green synthesis of silver doped fluor-hydroxyapatite/β-cyclodextrin nanocomposite in the dual acting fluorine-containing ionic liquid medium for bone substitute applications

NASA Astrophysics Data System (ADS)

Jegatheeswaran, S.; Selvam, S.; Sri Ramkumar, V.; Sundrarajan, M.

2016-05-01

A novel green route has approached for the synthesis of silver doped fluor-hydroxyapatite/β-cyclodextrin composite by the assistance of fluorine-based ionic liquid. The selected [BMIM]BF4 ionic liquid for this work plays a dual role as fluoride source and templating agent. It helps to improve the crystalline structures and the shape of the composites. The crystallinity, surface morphology, topographical studies of the synthesized composite were validated. The XRD results of the composite show typical Ag reflection peaks at 38.1°, 44.2° and 63.4°. The ionic liquid assisted composite displayed the hexagonal shaped HA particles, which are surrounded by spherical nano-Ag particles and these particles are uniformly dispersed in the β-cyclodextrin matrix in both horizontal and cross sections from surface morphology observations. The Ionic liquid assisted silver doped fluor-hydroxyapatite/β-cyclodextrin composite exhibited very good antibacterial activities against Escherichia coli, Salmonella typhi, Klebsiella pneumonia and Serratia liquefaciens pathogens. The antibacterial proficiencies were established using Confocal Laser Scanning Microscopic developed biofilms images and bacterial growth curve analysis. The cytotoxicity results of the ionic liquid assisted composite analyzed by cell proliferation in vitro studies using human osteosarcoma cell line (MG-63) and this study has shown excellent biocompatibility.

Microwave Assisted Grafting of Gums and Extraction of Natural Materials.

PubMed

Singh, Inderbir; Rani, Priya; Kumar, Pradeep

2017-01-01

Microwave assisted modification of polymers has become an established technique for modifying the functionality of polymers. Microwave irradiation reduces reaction time as well as the use of toxic solvents with enhanced sensitivity and yields of quality products. In this review article instrumentation and basic principles of microwave activation have been discussed. Microwave assisted grafting of natural gums, characterization of grafted polymers and their toxicological parameters have also been listed. Pharmaceutical applications viz. drug release retardant, mucoahesion and tablet superdisintegrant potential of microwave assisted gums has also been discussed. An overview of microwave assisted extraction of plant based natural materials has also been presented. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Microwave-Assisted Synthesis of High Dielectric Constant CaCu3Ti4O12 from Sol-Gel Precursor

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Cao, Peng; Huang, Saifang; Zhang, Weijun; Huang, Zhaohui; Gao, Wei

2015-07-01

CaCu3Ti4O12 (CCTO) powders derived from sol-gel precursors were calcined and sintered via microwave radiation. The obtained CCTO powders were compared with that obtained via a conventional heating method. For microwave heating, 89.1 wt.% CCTO was achieved from the sol-gel precursor, after only 17 min at 950°C. In contrast, the conventional calcination method required 3 h to generate 87.6 wt.% CCTO content at 1100°C. In addition, the CCTO powders prepared through 17 min of microwave calcination exhibited a small particle size distribution of D50 = 3.826 μm. It was found that a lengthy hold time of 1 h by microwave sintering is required to obtain a high dielectric constant (3.14 × 103 at 102 Hz) and a reasonably low dielectric loss (0.161) in the sintered CCTO ceramic. Based upon the distinct microstructures, the dielectric responses of the CCTO samples sintered by different methods are attributed to space charge polarization and internal barrier layer capacitor mechanism.

Study on disinfestation of pulses using microwave technique.

PubMed

Singh, Ranjeet; Singh, K K; Kotwaliwale, N

2012-08-01

Mortality of the pulse beetle (Callosobruchus chinensis L.) exposed, continuously, to microwave radiation (2450 MHz) was evaluated as a function of exposure time and percent power level, at adult stages. The microwave exposure time to attain 100% insect mortality at 100 %, 80%, 60%, 40%, and 20% power levels for Chickpea, Pigeon Pea and Green Gram was optimized. Effect of optimized microwave exposure time on viability, germination, cooking and milling characteristics of Chickpea, Pigeon Pea and Green Gram was also evaluated. Adult stage study was characterized by a distinct dose-exposure curve. The mortality curve was following third degree polynomial equation. The seed viability and germination of Chickpea, Pigeon Pea and Green Gram was affected by microwave exposure time and power level. It was observed that as the power level is decreasing the germination and viability of all the pulses are increasing. The effect on cooking and milling characteristics are not affected by microwave exposure time and power level. The insects in the mobile state were observed to move towards the surface from inside the nutrient medium during microwave exposure. They also curled up and in some cases aggregation was observed.

Green extraction of grape skin phenolics by using deep eutectic solvents.

PubMed

Cvjetko Bubalo, Marina; Ćurko, Natka; Tomašević, Marina; Kovačević Ganić, Karin; Radojčić Redovniković, Ivana

2016-06-01

Conventional extraction techniques for plant phenolics are usually associated with high organic solvent consumption and long extraction times. In order to establish an environmentally friendly extraction method for grape skin phenolics, deep eutectic solvents (DES) as a green alternative to conventional solvents coupled with highly efficient microwave-assisted and ultrasound-assisted extraction methods (MAE and UAE, respectively) have been considered. Initially, screening of five different DES for proposed extraction was performed and choline chloride-based DES containing oxalic acid as a hydrogen bond donor with 25% of water was selected as the most promising one, resulting in more effective extraction of grape skin phenolic compounds compared to conventional solvents. Additionally, in our study, UAE proved to be the best extraction method with extraction efficiency superior to both MAE and conventional extraction method. The knowledge acquired in this study will contribute to further DES implementation in extraction of biologically active compounds from various plant sources. Copyright © 2016 Elsevier Ltd. All rights reserved.

In Vitro bile acid binding of kale, mustard greens, broccoli, cabbage and green bell pepper improves with microwave cooking

USDA-ARS?s Scientific Manuscript database

Bile acid binding potential of foods and food fractions has been related to lowering the risk of heart disease and that of cancer. Sautéing or steam cooking has been observed to significantly improve bile acid binding of green/leafy vegetables. It was hypothesized that microwave cooking could impr...

Study on the synthesis and physicochemical properties of starch acetate with low substitution under microwave assistance.

PubMed

Lin, Derong; Zhou, Wei; Zhao, Jingjing; Lan, Weijie; Chen, Rongming; Li, Yutong; Xing, Baoshan; Li, Zhuohao; Xiao, Mengshi; Wu, Zhijun; Li, Xindan; Chen, Rongna; Zhang, Xingwen; Chen, Hong; Zhang, Qing; Qin, Wen; Li, Suqing

2017-10-01

In this study, synthesis and physicochemical properties of starch acetate with low substitution under microwave were studied. A three-level-three-factorial Central Composite Design using Response Surface Methodology (RSM) was employed to optimize the reaction conditions. The optimal parameters are as follows: amount of acetic anhydride of 12%, radiation time of 11min, and microwave power of 100W. These optimal conditions predicted by RSM were confirmed that the degree of substitution (DS) of acetate starch is 0.0691mg/g and the physical and chemical properties of natural corn starch (NCS) and corn starch acetate (ACS) were further studied.The transparency, water separation, water absorption, expansion force, and solubility of ACS low substitution are better than NCS, while the NCS's hydrolysis percentage is higher than ACS, which indicate that the modified corn starch has better performance than native corn starch. The surface morphology of the corn starch acetate was examined by scanning electron microscope (SEM), which showed that it had a smooth surface and a spherical and polygonal shape. However, samples' shape is irregular. Crystal structure was observed by X-ray diffraction, and the ACS can determine the level of microwave technology that can destroy the extent of the crystal and amorphous regions. Fourier transform infrared (FTIR) spectroscopy shows that around 1750cm -1 carbonyl signal determines acetylation bonding successfully. Copyright © 2017 Elsevier B.V. All rights reserved.

Microwave Assisted Synthesis of 1-[5-(Substituted Aryl)-1H-Pyrazol-3-yl]-3,5-Diphenyl-1H-1,2,4-Triazole as Antinociceptive and Antimicrobial Agents

PubMed Central

Khanage, Shantaram Gajanan; Mohite, Popat Baban; Pandhare, Ramdas Bhanudas; Raju, S. Appala

2014-01-01

Purpose: An efficient technique has been developed for microwave assisted synthesis of 1-[5-(substituted aryl)-1H-pyrazol-3-yl]-3,5-diphenyl-1H-1,2,4-triazole as antinociceptive and antimicrobial agents. Methods: The desired compounds (S1-S10) were synthesized by the microwave irradiation via cyclization of formerly synthesized chalcones of 3,5-diphenyl-1H-1,2,4-triazole and hydrazine hydrate in mild acidic condition. All newly synthesized compounds were subjected to study their antinociceptive and antimicrobial activity. The analgesic potential of compounds was tested by acetic acid induced writhing response and hot plate method. The MIC values for antimicrobial activity were premeditated by liquid broth method. Results: The compounds S1, S2, S4, S6 and S10 were found to be excellent peripherally acting analgesic agents when tested on mice by acetic acid induced writhing method and compounds S3, S6 and S1 at dose level of 100 mg/kg were exhibited superior centrally acting antinociceptive activity when tested by Eddy’s hot plate method. In antimicrobial activity compound S10 found to be broad spectrum antibacterial agent at MIC value of 15.62 µg/ml and compound S6 was exhibited antifungal potential at 15.62 µg/mL on both fungal strains. Conclusion: Some novel pyrazoles clubbed with 1,2,4-triazole derivatives were synthesized and evaluated as possible antimicrobial, centrally and peripherally acting analgesics. PMID:24511473

Solution-phase microwave assisted parallel synthesis, biological evaluation and in silico docking studies of 2-chlorobenzoyl thioureas derivatives

NASA Astrophysics Data System (ADS)

Khan, Muhammad Riaz; Zaib, Sumera; Rauf, Muhammad Khawar; Ebihara, Masahiro; Badshah, Amin; Zahid, Muhammad; Nadeem, Muhammad Arif; Iqbal, Jamshed

2018-07-01

An efficient and facile microwave-assisted solution phase parallel synthesis for a 38-member library of N-aroyl-N‧-aryl thioureas was accomplished successfully. These analogues (1-38) were synthesized under identical set of conditions. It has been observed that the reaction time was drastically reduced from 8 to 12 h for conventional methods to only 10-15 mins. Products obtained were more than 98% pure, as characterized by elemental analysis along with FT-IR and 1H, 13C NMR. The solid-phase structural analysis was accomplished by single crystal XRD analysis. The urease inhibitory potential of synthetic compounds was tested and compounds were found to inhibit urease in moderate to significant manner. Compound 17 was the most potent inhibitor of urease having an IC50 value of 0.17 ± 0.1 μM. To check the cytotoxic profile of the derivatives, lungs cancer cell lines were used. Cytotoxicity analysis revealed remarkable toxicity of the compounds against tested lungs carcinoma and compounds showed variation in inhibition activity due to the substituents attached. The molecular docking studies were carried out to identify the possible binding modes of potent inhibitors in the active site of enzyme. The results suggested that the compounds can be further investigated and used against different cancers.

Microwave frequency effect in the formation of Au nanocolloids in polar and non-polar solvents

NASA Astrophysics Data System (ADS)

Horikoshi, Satoshi; Abe, Hideki; Sumi, Takuya; Torigoe, Kanjiro; Sakai, Hideki; Serpone, Nick; Abe, Masahiko

2011-04-01

Given earlier observations that microwave frequencies can have a substantial effect on the photoactivity of a well-known photocatalyst (TiO2), in the synthesis of 3,6-diphenyl-4-n-butylpyridazine through a Diels-Alder process, and in the one-pot solvent-free synthesis of a room-temperature ionic liquid, we proceeded to examine the frequency effects of the 5.8 and 2.45 GHz microwave (MW) radiation in the synthesis of gold nanoparticles in non-polar media, such as oleylamine, which have a low dielectric constant (ε'), and we further examine differences in shape and size under otherwise identical temperature conditions when the synthesis of the gold nanoparticles was carried out in an ethylene glycol polar medium in the presence of polyvinylpyrrolidone. Whereas a change in microwave frequency from 2.45 to 5.8 GHz at equal microwave power levels led to the synthesis of gold nanoparticles in the non-polar media, a change in the microwave frequency had no effect on the size and shape of the gold nanoparticles synthesized in polar media for identical microwave power levels.

Microwave frequency effect in the formation of Au nanocolloids in polar and non-polar solvents.

PubMed

Horikoshi, Satoshi; Abe, Hideki; Sumi, Takuya; Torigoe, Kanjiro; Sakai, Hideki; Serpone, Nick; Abe, Masahiko

2011-04-01

Given earlier observations that microwave frequencies can have a substantial effect on the photoactivity of a well-known photocatalyst (TiO(2)), in the synthesis of 3,6-diphenyl-4-n-butylpyridazine through a Diels-Alder process, and in the one-pot solvent-free synthesis of a room-temperature ionic liquid, we proceeded to examine the frequency effects of the 5.8 and 2.45 GHz microwave (MW) radiation in the synthesis of gold nanoparticles in non-polar media, such as oleylamine, which have a low dielectric constant (ε'), and we further examine differences in shape and size under otherwise identical temperature conditions when the synthesis of the gold nanoparticles was carried out in an ethylene glycol polar medium in the presence of polyvinylpyrrolidone. Whereas a change in microwave frequency from 2.45 to 5.8 GHz at equal microwave power levels led to the synthesis of gold nanoparticles in the non-polar media, a change in the microwave frequency had no effect on the size and shape of the gold nanoparticles synthesized in polar media for identical microwave power levels.

Phosphorous and nitrogen dual heteroatom doped mesoporous carbon synthesized via microwave method for supercapacitor application

NASA Astrophysics Data System (ADS)

Nasini, Udaya B.; Bairi, Venu Gopal; Ramasahayam, Sunil Kumar; Bourdo, Shawn E.; Viswanathan, Tito; Shaikh, Ali U.

2014-03-01

Phosphorus (P) and nitrogen (N) dual heteroatom doped mesoporous carbon (PNDC) synthesized by microwave assisted carbonization of tannin cross-linked to melamine in the presence of polyphosphoric acid was evaluated electrochemically for supercapacitor application. Controlling the N content by varying the amount of tannin to melamine in the carbonization process produced varying nitrogen, phosphorus and oxygen functionalities along with different physical properties. Electrochemical characterization studies revealed that N content is responsible for pseudocapacitance and high surface area plays a vital role in improving the capacitative behavior by enhanced electric double layer formation. In 1.0 M H2SO4 and 6.0 M KOH, PNDC-2 showed a high specific capacitance of 271 F g-1 and 236 F g-1, respectively. XPS results demonstrate the presence of pyridinic-N, quaternary-N as well as quinone type oxygen functionalities, which accounts for redox reactions and likely play an important role in the transportation of electrons during the charge/discharge process. Thus, the microwave assisted synthesis of doped carbon can provide a novel method of synthesizing materials useful for the fabrication of cheap and high performance supercapacitors.

Effect of microwave-assisted sintering on dielectric properties of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramic

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

Rani, Suman, E-mail: sumanranigju@gmail.com; Ahlawat, Neetu; Punia, R.

2016-05-23

In this present work, CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It wasmore » observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.« less

Rapid microwave assisted synthesis of graphene nanosheets/polyethyleneimine/gold nanoparticle composite and its application to the selective electrochemical determination of dopamine.

PubMed

Ponnusamy, Vinoth Kumar; Mani, Veerappan; Chen, Shen-Ming; Huang, Wan-Tran; Jen, Jen-Fon

2014-03-01

In this study, a simple and fast microwave assisted chemical reduction method for the preparation of graphene nanosheet/polyethyleneimine/gold nanoparticle (GNS/PEI/AuNP) composite was developed. PEI, a cationic polymer, was used both as a non-covalent functionalizing agent for the graphene oxide nanosheets (GONSs) through electrostatic interactions in the aqueous medium and also as a stabilizing agent for the formation of AuNPs on PEI wrapped GNSs. This preparation method involves a simple mixing step followed by a simultaneous microwave assisted chemical reduction of the GONSs and gold ions. The prepared composite exhibits the dispersion of high density AuNPs which were densely decorated on the large surface area of the PEI wrapped GNS. X-ray photoelectron spectroscopy, powder X-ray diffraction, high-resolution transmission electron microscopy, field-emission scanning electron microscopy with energy dispersive X-ray spectroscopy, and thermo-gravimetric analysis, were used to characterize the properties of the resultant composite. The prepared GNS/PEI/AuNP composite film exhibited excellent electrocatalytical activity towards the selective determination of dopamine in the presence of ascorbic acid, which showed potential application in electrochemical sensors. The applicability of the presented sensor was also demonstrated for the determination of dopamine in human urine samples. © 2013 Elsevier B.V. All rights reserved.

Rapid syntheses of a metal-organic framework material Cu3(BTC)2(H2O)3 under microwave: a quantitative analysis of accelerated syntheses.

PubMed

Khan, Nazmul Abedin; Haque, Enamul; Jhung, Sung Hwa

2010-03-20

A typical MOF material, Cu-BTC has been synthesized with microwave and conventional electric heating in various conditions to elucidate, for the first time, the quantitative acceleration in the synthesis of a MOF by microwaves. The acceleration by microwaves is mainly due to rapid nucleation rather than rapid crystal growth, even though both stages are accelerated. The acceleration in the nucleation stage by microwaves is due to the very large pre-exponential factor (about 1.4 x 10(10) times that of conventional synthesis) in the Arrhenius plot. However, the activation energy for the nucleation in the case of microwave synthesis is higher than the activation energy of conventional synthesis. The large acceleration in the nucleation, compared with that in the crystal growth, is observed once again by the syntheses in two-steps (changing heating methods from microwave into conventional heating or from conventional heating into microwave heating just after the nucleation is completed). The crystal size of Cu-BTC obtained by microwave-nucleation is generally smaller than the Cu-BTC made by conventional-nucleation, probably due to rapid nucleation and the small size of nuclei with microwave-nucleation.

Microwave Hydrothermal Synthesis of Reduced Graphene Oxide: Effects of Microwave Power and Irradiation Time

NASA Astrophysics Data System (ADS)

Agusu, La; Ode Ahmad, La; Anggara, Desna; Alimin; Mitsudo, Seitaro; Fujii, Yutaka; Kikuchi, Hiromitsu

2018-04-01

Reduced graphene oxide has been synthesihzed by one-pot microwave assisted hydrothermal method. Effects of microwave power and irradiation time to its crystal structure and electrical conductivity were investigated. Here, graphene oxide, firstly, were synthesized by modified hummers method and subsequently mixed with Zn as a reducing agent. Then it was transferred to modified domestic microwave oven (800 watts) with glass distiller equipment for completely reduction process. Three different power levels (240, 400, 630 watts) and two cases of irradiation times (20 and 40 minutes) were treated. XRD study shows that irradiation time variation is more effective than the variation of power level. Power level of 270 watts and for 40 minutes microwave irradiation are enough for producing estimated bilayer rGO with graphene interlayer of ~0.4 nm. Bilayer graphene and water molecule (~0.3 nm) may vibrate the same manner and perhaps they are accepting the same temperature. Graphene seems to be re-arranged in unspecified way among the thermal pressure, temperature gradient and/or water surface tension between graphene and water induced by microwave, in order to achieve thermal equilibrium through out the system The electrical conductivity rGO/PVA (60/40 %w) paper are ranging from 15.6 to 43.4 mS/cm.

"In situ" extraction of essential oils by use of Dean-Stark glassware and a Vigreux column inside a microwave oven: a procedure for teaching green analytical chemistry.

PubMed

Chemat, Farid; Perino-Issartier, Sandrine; Petitcolas, Emmanuel; Fernandez, Xavier

2012-08-01

One of the principal objectives of sustainable and green processing development remains the dissemination and teaching of green chemistry in colleges, high schools, and academic laboratories. This paper describes simple glassware that illustrates the phenomenon of extraction in a conventional microwave oven as energy source and a process for green analytical chemistry. Simple glassware comprising a Dean-Stark apparatus (for extraction of aromatic plant material and recovery of essential oils and distilled water) and a Vigreux column (as an air-cooled condenser inside the microwave oven) was designed as an in-situ extraction vessel inside a microwave oven. The efficiency of this experiment was validated for extraction of essential oils from 30 g fresh orange peel, a by-product in the production of orange juice. Every laboratory throughout the world can use this equipment. The microwave power is 100 W and the irradiation time 15 min. The method is performed at atmospheric pressure without added solvent or water and furnishes essential oils similar to those obtained by conventional hydro or steam distillation. By use of GC-MS, 22 compounds in orange peel were separated and identified; the main compounds were limonene (72.1%), β-pinene (8.4%), and γ-terpinene (6.9%). This procedure is appropriate for the teaching laboratory, does not require any special microwave equipment, and enables the students to learn the skills of extraction, and chromatographic and spectroscopic analysis. They are also exposed to a dramatic visual example of rapid, sustainable, and green extraction of an essential oil, and are introduced to successful sustainable and green analytical chemistry.

The Green Synthesis and Evaluation of Silver Nanoparticles and Zinc Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Gebear-Eigzabher, Bellsabel

Nanoparticle (NP) research has received exceptional attention as the field of study that contributes to transforming the world of materials science. When implementing NPs in consumer and industrial products, their unique properties improve technologies to the extent of significant game-changing breakthroughs. Conversely, the increased production of NPs, their use, their disposal or inadvertent release in the environment drove the need for processes and policies that ensures consumer and environmental safety. Mitigation of any harmful effects that NPs could potentially have combines methods of safe preparation, safe handling and safe disposal as well as containment of any inadvertent release. Our focus is in safe preparation of nanomaterials and we report green and energy efficient synthesis methods for metal NPs and metal oxide NPs of two popular materials: silver (Ag) and zinc oxide (ZnO). The thesis explained: 1) The impact of NPs in nowadays' world; 2) Synthesis methods that were designed to include environmentally-friendly staring materials and energy-saving fabrication processes, with emphasis on maintaining NPs final size and morphology when compared with existing methods; and 3) Nanoparticles characterization and data collection which allowed us to determine and/or validate their properties. Nanoparticles were studied using transmission electron microscope (TEM), X-Ray powder diffraction (XRD), low-voltage (5 keV) transmission electron microscopy (LV EM 5), Fourier-Transform Infrared Spectroscopy (FT-IR), and Ultraviolet-Visible (UV-Vis) spectroscopy. We developed an aqueous-based preparation of zinc oxide nanoparticles (ZnO NPs) using microwave-assisted chemistry to render a well-controlled particle size distribution within each set of reaction conditions in the range of 15 nm to 75 nm. We developed a scalable silver nanoparticles synthesis by chemical reduction methods. The NPs could be used in consumer products. The measurement tools for consumer products were also used on in-house synthesized Ag NPs. Commercially available silver nanoparticles have been compared with the in-house synthesized ones and characterized by Photothermal Lens (PTL) Spectroscopy. In respect to particle size and morphology, the Ag NPs synthesized by chemical reduction methods are similar to Ag nanoparticle solution available in the market. However, the synthesized nanoparticles are high in concentration and do not show signs of aggregation or agglomeration. It was concluded that our Ag NPs are superior to the commercially available ones by exhibiting large concentrations in ultra-stable dispersions.

State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

PubMed

Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

2016-01-28

Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Microwave-synthesized freestanding iron-carbon nanotubes on polyester composites of woven Kevlar fibre and silver nanoparticle-decorated graphene

PubMed Central

Hazarika, Ankita; Deka, Biplab K.; Kim, DoYoung; Kong, Kyungil; Park, Young-Bin; Park, Hyung Wook

2017-01-01

We synthesized Ag nanoparticle-decorated multilayered graphene nanosheets (Ag-graphene) from graphite nanoplatelets and silver nitrate through 90–100 s of microwave exposure, without the use of any mineral acids or harsh reducing agents. Fe nanoparticle-decorated carbon nanotubes (Fe-CNTs) were grown on polypyrrole (PPy) deposited on woven Kevlar fibre (WKF), using ferrocene as a catalyst, under microwave irradiation. Fe-CNTs grown on WKF and Ag-graphene dispersed in polyester resin (PES) were combined to fabricate Ag-graphene/Fe-CNT/PPy-coated WKF/PES composites by vacuum-assisted resin transfer moulding. The combined effect of Fe-CNTs and Ag-graphene in the resulting composites resulted in a remarkable enhancement of tensile properties (a 192.56% increase in strength and 100.64% increase in modulus) as well as impact resistance (a 116.33% increase). The electrical conductivity significantly increased for Ag-graphene/Fe-CNT/PPy-coated WKF/PES composites. The effectiveness of electromagnetic interference shielding, which relies strongly on the Ag-graphene content in the composites, was 25 times higher in Ag-graphene/Fe-CNT/PPy-coated WKF/PES than in neat WKF/PES composites. The current work offers a novel route for fabricating highly promising, cost effective WKF/PES composites through microwave-assisted synthesis of Fe-CNTs and Ag-graphene. PMID:28074877

Dimers of coumarin-1,2,3-triazole hybrids bearing alkyl spacer: Design, microwave-assisted synthesis, molecular docking and evaluation as antimycobacterial and antimicrobial agents

NASA Astrophysics Data System (ADS)

Ashok, Dongamanti; Gundu, Srinivas; Aamate, Vikas Kumar; Devulapally, Mohan Gandhi; Bathini, Raju; Manga, Vijjulatha

2018-04-01

The present study demonstrated the synthesis of new series of coumarin-1,2,3-triazole hybrids under microwave irradiation method. Several dimers of coumarin based 1,2,3-triazole derivatives were synthesized and their antimycobacterial and antimicrobial activities were investigated. The antimycobacterial activity screening results revealed that compounds 6i and 6j were the most active against Mycobacterium tuberculosis H37Rv strain. The active compounds were further evaluated for cytotoxicity with HEK cell lines and exhibited less % of inhibition. The same synthetic hybrids were evaluated for their antimicrobial activity against various bacterial strains and fungal strains and compounds 6e, 6h, 6i and 6j were found to be the most promising antimicrobial potent molecules. Furthermore, the active compounds against Mycobacterium tuberculosis were evaluated for their molecular docking studies against pantothenate synthetase (PS) enzyme of MTB and the docking results are in well agreement with the antitubercular evaluation results.

Design, microwave-mediated synthesis and biological evaluation of novel 4-aryl(alkyl)amino-3-nitroquinoline and 2,4-diaryl(dialkyl)amino-3-nitroquinolines as anticancer agents.

PubMed

Chauhan, Monika; Rana, Anil; Alex, Jimi Marin; Negi, Arvind; Singh, Sandeep; Kumar, Raj

2015-02-01

Design, microwave-assisted synthesis of novel 4-aryl (alkyl)amino-3-nitroquinoline (1a-1l) and 2,4-diaryl (dialkyl)amino-3-nitroquinolines (2a-2k and 3a) via regioselective and complete nucleophilic substitution of 2,4-dichloro-3-nitroquinoline, respectively in water are presented. The newly synthesized compounds were evaluated for the first time for antiproliferative activity against EGFR overexpressing human lung (A-549 and H-460) and colon (HCT-116-wild type and HCT-116-p53 null) cancer cell lines. Some notions about structure-activity relationships (SAR) are presented. Compounds 2e, 2f, 2j and 3a overall exhibited excellent anticancer activity comparable to erlotinib which was used as a positive control. Molecular modeling studies disclosed the recognition pattern of the compounds and also supported the observed SAR. Copyright © 2014 Elsevier Inc. All rights reserved.

A microwave assisted one-pot route synthesis of bimetallic PtPd alloy cubic nanocomposites and their catalytic reduction for 4-nitrophenol

NASA Astrophysics Data System (ADS)

Zhang, Jian; Gan, Wei; Fu, Xucheng; Hao, Hequn

2017-10-01

We herein report a simple, rapid, and eco-friendly chemical route to the one-pot synthesis of bimetallic PtPd alloy cubic nanocomposites under microwave irradiation. During this process, water was employed as an environmentally benign solvent, while dimethylformamide served as a mild reducing agent, and polyvinylpyrrolidone was used as both a dispersant and a stabilizer. The structure, morphology, and composition of the resulting alloy nanocomposites were examined by x-ray diffraction, transmission electron microscopy, and energy dispersive x-ray spectroscopy. A detailed study was then carried out into the catalytic activity of the PtPd nanocomposites with a Pt:Pd molar ratio of 50:50 in the reduction of 4-nitrophenol (4-NP) by sodium borohydride as a model reaction. Compared with pristine Pt and Pd monometallic nanoparticles (PtNPs and PdNPs), the bimetallic PtPd alloy nanocomposites exhibited enhanced catalytic activities and were readily recyclable in the reduction of 4-NP due to synergistic effects.

Microwave-assisted synthesis of 3,6-di(pyridin-2-yl)pyridazines: unexpected ketone and aldehyde cycloadditions.

PubMed

Hoogenboom, Richard; Moore, Brian C; Schubert, Ulrich S

2006-06-23

3,6-Di(pyridin-2-yl)pyridazines are an interesting class of compounds because of their metal-coordinating ability resulting in the self-assembly into [2x2] gridlike metal complexes with copper(I) or silver(I) ions. These and other substituted pyridazines can be prepared by the inverse-electron-demand Diels-Alder reactions between acetylenes and 1,2,4,5-tetrazines. In this contribution, the effect of (superheated) microwave conditions on these generally slow cycloadditions is described. The cycloaddition of acetylenes to 3,6-di(pyridin-2-yl)-1,2,4,5-tetrazine could be accelerated from several days reflux in toluene or N,N-dimethylformamide to several hours in dichloromethane at 150 degrees C. In addition, the unexpected cycloaddition of the enol tautomers of various ketones and aldehydes to 3,6-di(pyridin-2-yl)-1,2,4,5-tetrazine is described in detail providing an alternative route for the synthesis of (substituted) pyridazines.

Fast and Simple Microwave Synthesis of TiO2/Au Nanoparticles for Gas-Phase Photocatalytic Hydrogen Generation.

PubMed

May-Masnou, Anna; Soler, Lluís; Torras, Miquel; Salles, Pol; Llorca, Jordi; Roig, Anna

2018-01-01

The fabrication of small anatase titanium dioxide (TiO 2 ) nanoparticles (NPs) attached to larger anisotropic gold (Au) morphologies by a very fast and simple two-step microwave-assisted synthesis is presented. The TiO 2 /Au NPs are synthesized using polyvinylpyrrolidone (PVP) as reducing, capping and stabilizing agent through a polyol approach. To optimize the contact between the titania and the gold and facilitate electron transfer, the PVP is removed by calcination at mild temperatures. The nanocatalysts activity is then evaluated in the photocatalytic production of hydrogen from water/ethanol mixtures in gas-phase at ambient temperature. A maximum value of 5.3 mmol·[Formula: see text]h -1 (7.4 mmol·[Formula: see text]h -1 ) of hydrogen is recorded for the system with larger gold particles at an optimum calcination temperature of 450°C. Herein we demonstrate that TiO 2 -based photocatalysts with high Au loading and large Au particle size (≈50 nm) NPs have photocatalytic activity.

Microwave-assisted direct synthesis of butene from high-selectivity methane

PubMed Central

Li, Kang; Lu, Yu-wei

2017-01-01

Methane was directly converted to butene liquid fuel by microwave-induced non-oxidative catalytic dehydrogenation under 0.1–0.2 MPa. The results show that, under microwave heating in a two-stage fixed-bed reactor, in which nickel powder and NiOx–MoOy/SiO2 are used as the catalyst, the methane–hydrogen mixture is used as the raw material, with no acetylene detected. The methane conversion is more than 73.2%, and the selectivity of methane to butene is 99.0%. Increasing the hydrogen/methane feed volume ratio increases methane conversion and selectivity. Gas chromatography/electron impact ionization/mass spectrometry chromatographic analysis showed that the liquid fuel produced by methane dehydrogenation oligomerization contained 89.44% of butene, and the rest was acetic acid, ethanol, butenol and butyric acid, and the content was 1.0–3.0 wt%. PMID:29308261

Microwave hydrothermal synthesis and upconversion properties of Yb3+/Er3+ doped YVO4 nanoparticles

NASA Astrophysics Data System (ADS)

Kshetri, Yuwaraj K.; Regmi, Chhabilal; Kim, Hak-Soo; Wohn Lee, Soo; Kim, Tae-Ho

2018-05-01

Yb3+ and Er3+ doped YVO4 (Yb3+/Er3+:YVO4) nanoparticles with highly efficient near-infrared to visible upconversion properties have been synthesized by microwave hydrothermal process. Uniform-sized Yb3+/Er3+:YVO4 nanoparticles were synthesized within 1 h at 140 °C which is relatively faster than the conventional hydrothermal process. Under 980 nm laser excitation, strong green and less strong red emissions are observed which are attributed to 2H11/2, 4S3/2 to 4I15/2 and 4F9/2 to 4I15/2 transitions of Er3+ respectively. The emission intensity is found to depend strongly on the concentration of Yb3+. The quadratic dependence of upconversion intensity on the excitation power indicates that the upconversion process is governed by two-photon absorption process.

Microwave hydrothermal synthesis and upconversion properties of Yb3+/Er3+ doped YVO4 nanoparticles.

PubMed

Kshetri, Yuwaraj K; Regmi, Chhabilal; Kim, Hak-Soo; Lee, Soo Wohn; Kim, Tae-Ho

2018-05-18

Yb 3+ and Er 3+ doped YVO 4 (Yb 3+ /Er 3+ :YVO 4 ) nanoparticles with highly efficient near-infrared to visible upconversion properties have been synthesized by microwave hydrothermal process. Uniform-sized Yb 3+ /Er 3+ :YVO 4 nanoparticles were synthesized within 1 h at 140 °C which is relatively faster than the conventional hydrothermal process. Under 980 nm laser excitation, strong green and less strong red emissions are observed which are attributed to 2 H 11/2 , 4 S 3/2 to 4 I 15/2 and 4 F 9/2 to 4 I 15/2 transitions of Er 3+ respectively. The emission intensity is found to depend strongly on the concentration of Yb 3+ . The quadratic dependence of upconversion intensity on the excitation power indicates that the upconversion process is governed by two-photon absorption process.

Recent progress in the synthesis of metal–organic frameworks

DOE PAGES

Sun, Yujia; Zhou, Hong -Cai

2015-09-25

Metal–organic frameworks (MOFs) have attracted considerable attention for various applications due to their tunable structure, porosity and functionality. In general, MOFs have been synthesized from isolated metal ions and organic linkers under hydrothermal or solvothermal conditions via one-spot reactions. The emerging precursor approach and kinetically tuned dimensional augmentation strategy add more diversity to this field. In addition, to speed up the crystallization process and create uniform crystals with reduced size, many alternative synthesis routes have been explored. Recent advances in microwave-assisted synthesis and electrochemical synthesis are presented in this review. In recent years, post-synthetic approaches have been shown to bemore » powerful tools to synthesize MOFs with modified functionality, which cannot be attained via de novo synthesis. In this study, some current accomplishments of post-synthetic modification (PSM) based on covalent transformations and coordinative interactions as well as post-synthetic exchange (PSE) in robust MOFs are provided.« less

Improved solvent-free microwave extraction of essential oil from dried Cuminum cyminum L. and Zanthoxylum bungeanum Maxim.

PubMed

Wang, Ziming; Ding, Lan; Li, Tiechun; Zhou, Xin; Wang, Lu; Zhang, Hanqi; Liu, Li; Li, Ying; Liu, Zhihong; Wang, Hongju; Zeng, Hong; He, Hui

2006-01-13

Solvent-free microwave extraction (SFME) is a recently developed green technique which is performed in atmospheric conditions without adding any solvent or water. SFME has already been applied to extraction of essential oil from fresh plant materials or dried materials prior moistened. The essential oil is evaporated by the in situ water in the plant materials. In this paper, it was observed that an improved SFME, in which a kind of microwave absorption solid medium, such as carbonyl iron powders (CIP), was added and mixed with the sample, can be applied to extraction of essential oil from the dried plant materials without any pretreatment. Because the microwave absorption capacity of CIP is much better than that of water, the extraction time while using the improved SFME is no more than 30 min using a microwave power of 85 W. Compared to the conventional SFME, the advantages of improved SFME were to speed up the extraction rate and need no pretreatment. Improved SFME has been compared with conventional SFME, microwave-assisted hydrodistillation (MAHD) and conventional hydrodistillation (HD) for the extraction of essential oil from dried Cuminum cyminum L. and Zanthoxylum bungeanum Maxim. By using GC-MS system the compositions of essential oil extracted by applying four kinds of extraction methods were identified. There was no obvious difference in the quality of essential oils obtained by the four kinds of extraction methods.

Mechanochemical Ring-Opening Polymerization of Lactide: Liquid-Assisted Grinding for the Green Synthesis of Poly(lactic acid) with High Molecular Weight.

PubMed

Ohn, Nuri; Shin, Jihoon; Kim, Sung Sik; Kim, Jeung Gon

2017-09-22

Mechanochemical polymerization of lactide is carried out by using ball milling. Mechanical energy from collisions between the balls and the vessel efficiently promotes an organic-base-mediated metal- and solvent-free solid-state polymerization. Investigation of the parameters of the ball-milling synthesis revealed that the degree of lactide ring-opening polymerization could be modulated by the ball-milling time, vibration frequency, mass of the ball media, and liquid-assisted grinding. Liquid-assisted grinding was found to be an especially important factor for achieving a high degree of mechanochemical polymerization. Although polymer-chain scission from the strong collision energy prevented mechanical-force-driven high-molecular-weight polymer synthesis, the addition of only a small amount of liquid enabled sufficient energy dissipation and poly(lactic acid) was thereby obtained with a molecular weight of over 1×10 5  g mol -1 . © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of Precursors on the Synthesis of CuO Nanoparticles Under Microwave for Photocatalytic Activity Towards Methylene Blue and Rhodamine B Dyes.

PubMed

Sanjini, N S; Winston, B; Velmathi, S

2017-01-01

Copper oxide nanoparticles have been successfully synthesized by microwave assisted precipitation method. Different precursors like copper chloride, copper nitrate and copper sulphate were used for synthesis of CuO nanoparticles with different shape, size and catalytic activity. Sodium hydroxide acts as a capping agent and ethanol as solvent for the synthesis. The XRD study was conducted to confirm the single phase monoclinic structure of as-synthesized and annealed CuO nano particles. The morphology of the as-synthesized and annealed CuO samples was analyzed by high resolution field emission scanning electron microscope. Fourier transform infrared spectroscopy was done for all the synthesized CuO nanoparticles for functional group characterization. The wide band gap and photocatalytic activity were studied by UV-Visible spectroscopy. The photocatalytic degradation of Methylene blue (MB) and Rhodamine B (RhB) dyes in aqueous solution were investigated under UV light (254 nm). In all the cases annealed samples showed good catalytic activity compared to as-synthesized CuO nanoparticles. The CuO nanoparticles from CuCl2 precursor act as excellent photocatalyst for both MB and RhB compared to CuNO₃ and CuSO₄.

A Thermal Dehydrogenative Diels–Alder Reaction of Styrenes for the Concise Synthesis of Functionalized Naphthalenes

PubMed Central

Kocsis, Laura S.; Benedetti, Erica

2012-01-01

Functionalized naphthalenes are valuable building blocks in many important areas. A microwave-assisted, intramolecular dehydrogenative Diels-Alder reaction of styrenyl derivatives to provide cyclopenta[b]naphthalene substructures not previously accessible using existing synthetic methods is described. The synthetic utility of these uniquely functionalized naphthalenes was demonstrated by a single-step conversion of one of these cycloadducts to a fluorophore bearing a structural resemblance to Prodan. PMID:22913473

A thermal dehydrogenative Diels-Alder reaction of styrenes for the concise synthesis of functionalized naphthalenes.

PubMed

Kocsis, Laura S; Benedetti, Erica; Brummond, Kay M

2012-09-07

Functionalized naphthalenes are valuable building blocks in many important areas. A microwave-assisted, intramolecular dehydrogenative Diels-Alder reaction of styrenyl derivatives to provide cyclopenta[b]naphthalene substructures not previously accessible using existing synthetic methods is described. The synthetic utility of these uniquely functionalized naphthalenes was demonstrated by a single-step conversion of one of these cycloadducts to a fluorophore bearing a structural resemblance to Prodan.

Convenient approaches to synthesis of furanoid sugar-aza-crown ethers from C-ribosyl azido aldehyde via a reductive amination/amidation.

PubMed

Hsieh, Yu-Chi; Chir, Jiun-Ly; Zou, Wei; Wu, Hsiu-Han; Wu, An-Tai

2009-05-26

A short and highly efficient route to the alpha-anomer of a furanoid sugar-aza-crown ether was developed by a one-pot reductive amination of an alpha-anomer C-ribosyl azido aldehyde. In addition, the beta-anomer furanoid sugar-aza-crown ether was synthesized from a linear disaccharide precursor via amidation and then followed by microwave-assisted amide reduction.

Expeditious microwave-assisted synthesis of 5-alkoxyoxazoles from α-triflyloxy esters and nitriles.

PubMed

Jouanno, Laurie-Anne; Sabot, Cyrille; Renard, Pierre-Yves

2012-10-05

A rapid and general access to diversely substituted 5-alkoxyoxazoles 2 (i.e., R(1), R(2) = alkyl, phenyl) from easily accessible α-triflyloxy/hydroxy esters 1 and nitriles with good yields (41-76%) is reported. The versatility of the cyclization is shown for a range of substrates with high selectivity toward triflates over mesylates and proved to be compatible with sensitive functional groups. As an illustration of this transformation, the first synthesis of the recently isolated hydroxypyridine methyl multijuguinate 4 was achieved in four steps through a hetero Diels-Alder reaction of the 5-alkoxyoxazole and acrylic acid, followed by a protodecarboxylation reaction.

MICROWAVES IN ORGANIC SYNTHESIS

EPA Science Inventory

The effect of microwaves, a non-ionizing radiation, on organic reactions is described both in polar solvents and under solvent-free conditions. The special applications are highlighted in the context of solventless organic synthesis which involve microwave (MW) exposure of neat r...

CHEMICAL SYNTHESIS & TRANSFORMATIONS USING MICROWAVES

EPA Science Inventory

A historical account of the utility of microwaves in a variety of chemical synthesis applications will be presented, including a solvent-free strategy that involves microwave (MW) exposure of neat reactants (undiluted) catalyzed by the surfaces of recyclable mineral supports such...

4-Substituted thieno[2,3-d]pyrimidines as potent antibacterial agents: Rational design, microwave-assisted synthesis, biological evaluation and molecular docking studies.

PubMed

Gill, Rupinder K; Singh, Harpreet; Raj, Tilak; Sharma, Anuradha; Singh, Gagandeep; Bariwal, Jitender

2017-12-01

In an attempt to discover a new class of antibacterial agents with improved efficacy and to overcome the drug-resistant problems, some novel 4-substituted thieno[2,3-d]pyrimidines have been synthesized via microwave-assisted methodology and evaluated for their in vitro antibacterial activity against various pathogenic bacterial strains. Compounds 12b and 13c showed the promising inhibitory potencies against Staphylococcus aureus, Bacillus subtilis, Pseudomonas aeruginosa and Escherichia coli with MICs ranging from 2 to 10 μg/ml. Compound 13c was also found to be highly potent against methicillin-resistant S. aureus (MRSA) with MIC value of 4 μg/ml. Docking simulation studies have been performed to unravel the mode of action and association study indicate the binding of potent compounds with DHPS enzyme. In silico ADME studies suggest the drug-like characteristics of the potent compounds. © 2017 John Wiley & Sons A/S.

Microwave-Assisted Synthesis of NiCo2O4 Double-Shelled Hollow Spheres for High-Performance Sodium Ion Batteries

NASA Astrophysics Data System (ADS)

Zhang, Xiong; Zhou, Yanping; Luo, Bin; Zhu, Huacheng; Chu, Wei; Huang, Kama

2018-03-01

The ternary transitional metal oxide NiCo2O4 is a promising anode material for sodium ion batteries due to its high theoretical capacity and superior electrical conductivity. However, its sodium storage capability is severely limited by the sluggish sodiation/desodiation reaction kinetics. Herein, NiCo2O4 double-shelled hollow spheres were synthesized via a microwave-assisted, fast solvothermal synthetic procedure in a mixture of isopropanol and glycerol, followed by annealing. Isopropanol played a vital role in the precipitation of nickel and cobalt, and the shrinkage of the glycerol quasi-emulsion under heat treatment was responsible for the formation of the double-shelled nanostructure. The as-synthesized product was tested as an anode material in a sodium ion battery, was found to exhibit a high reversible specific capacity of 511 mAh g-1 at 100 mA g-1, and deliver high capacity retention after 100 cycles. [Figure not available: see fulltext.

Microwave-Assisted Synthesis of Highly-Crumpled, Few-Layered Graphene and Nitrogen-Doped Graphene for Use as High-Performance Electrodes in Capacitive Deionization

NASA Astrophysics Data System (ADS)

Amiri, Ahmad; Ahmadi, Goodarz; Shanbedi, Mehdi; Savari, Maryam; Kazi, S. N.; Chew, B. T.

2015-12-01

Capacitive deionization (CDI) is a promising procedure for removing various charged ionic species from brackish water. The performance of graphene-based material in capacitive deionization is lower than the expectation of the industry, so highly-crumpled, few-layered graphene (HCG) and highly-crumpled nitrogen-doped graphene (HCNDG) with high surface area have been introduced as promising candidates for CDI electrodes. Thus, HCG and HCNDG were prepared by exfoliation of graphite in the presence of liquid-phase, microwave-assisted methods. An industrially-scalable, cost-effective, and simple approach was employed to synthesize HCG and HCNDG, resulting in few-layered graphene and nitrogen-doped graphene with large specific surface area. Then, HCG and HCNDG were utilized for manufacturing a new class of carbon nanostructure-based electrodes for use in large-scale CDI equipment. The electrosorption results indicated that both the HCG and HCNDG have fairly large specific surface areas, indicating their huge potential for capacitive deionization applications.

Evaluation of hemocompatibility and in vitro immersion on microwave-assisted hydroxyapatite-alumina nanocomposites.

PubMed

Radha, G; Balakumar, S; Venkatesan, Balaji; Vellaichamy, Elangovan

2015-05-01

This study reports the microwave-assisted synthesis and characterization of nHAp (nano-hydroxyapatite)-alumina composites. The crystalline phase and interaction of alumina with nHAp was analyzed using X-ray diffraction (XRD) and Raman microscopy analysis, respectively. High resolution transmission electron microscopy (HRTEM) micrographs exhibit morphological changes of nHAp composites with increasing alumina concentrations. Microhardness studies reveal the enhanced mechanical strength of nHAp10 and nHAp20 nanocomposites than pure nHAp. In vitro bioactivity of the nanocomposites was studied by immersing samples in simulated body fluid (Hank's solution) for 21 days. The surface of biomineralized samples were analyzed using field emission scanning electron microscopy (FESEM) and energy dispersive X-ray spectroscopy (EDX). Hemolytic assay revealed acceptable compatibility for varying concentrations of all the samples. Cell proliferation assay was systematically investigated for 1 day and 3 days on Saos-2 osteoblast-like cell lines and it was found that nHAp nanocomposites improved the proliferation. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis of ZnMn₂O₄ Nanoparticles by a Microwave-Assisted Colloidal Method and their Evaluation as a Gas Sensor of Propane and Carbon Monoxide.

PubMed

Morán-Lázaro, Juan Pablo; Guillen-López, Erwin Said; López-Urias, Florentino; Muñoz-Sandoval, Emilio; Blanco-Alonso, Oscar; Guillén-Bonilla, Héctor; Guillén-Bonilla, Alex; Rodríguez-Betancourtt, Verónica María; Sanchez-Tizapa, Marciano; Olvera-Amador, María de la Luz

2018-02-27

Spinel-type ZnMn₂O₄ nanoparticles were synthesized via a simple and inexpensive microwave-assisted colloidal route. Structural studies by X-ray diffraction showed that a spinel crystal phase of ZnMn₂O₄ was obtained at a calcination temperature of 500 °C, which was confirmed by Raman and UV-vis characterizations. Spinel-type ZnMn₂O₄ nanoparticles with a size of 41 nm were identified by transmission electron microscopy. Pellet-type sensors were fabricated using ZnMn₂O₄ nanoparticles as sensing material. Sensing measurements were performed by exposing the sensor to different concentrations of propane or carbon monoxide at temperatures in the range from 100 to 300 °C. Measurements performed at an operating temperature of 300 °C revealed a good response to 500 ppm of propane and 300 ppm of carbon monoxide. Hence, ZnMn₂O₄ nanoparticles possess a promising potential in the gas sensors field.

Opioid receptor probes derived from cycloaddition of the hallucinogen natural product salvinorin A.

PubMed

Lozama, Anthony; Cunningham, Christopher W; Caspers, Michael J; Douglas, Justin T; Dersch, Christina M; Rothman, Richard B; Prisinzano, Thomas E

2011-04-25

As part of our continuing efforts toward more fully understanding the structure-activity relationships of the neoclerodane diterpene salvinorin A, we report the synthesis and biological characterization of unique cycloadducts through [4+2] Diels-Alder cycloaddition. Microwave-assisted methods were developed and successfully employed, aiding in functionalizing the chemically sensitive salvinorin A scaffold. This demonstrates the first reported results for both cycloaddition of the furan ring and functionalization via microwave-assisted methodology of the salvinorin A skeleton. The cycloadducts yielded herein introduce electron-withdrawing substituents and bulky aromatic groups into the C-12 position. Kappa opioid (KOP) receptor space was explored through aromatization of the bent oxanorbornadiene system possessed by the cycloadducts to a planar phenyl ring system. Although dimethyl- and diethylcarboxylate analogues 5 and 6 retain some affinity and selectivity for KOP receptors and are full agonists, their aromatized counterparts 13 and 14 have reduced affinity for KOP receptors. The methods developed herein signify a novel approach toward rapidly probing the structure-activity relationships of furan-containing natural products.

Green and efficient sample preparation method for the determination of catalyst residues in margarine by ICP-MS.

PubMed

Hartwig, Carla Andrade; Pereira, Rodrigo Mendes; Novo, Diogo La Rosa; Oliveira, Dirce Taina Teixeira; Mesko, Marcia Foster

2017-11-01

Responding to the need for green and efficient methods to determine catalyst residues with suitable precision and accuracy in samples with high fat content, the present work evaluates a microwave-assisted ultraviolet digestion (MW-UV) system for margarines and subsequent determination of Ni, Pd and Pt using inductively coupled plasma mass spectrometry (ICP-MS). It was possible to digest up to 500mg of margarine using only 10mL of 4molL -1 HNO 3 with a digestion efficiency higher than 98%. This allowed the determination of catalyst residues using the ICP-MS and free of interferences. For this purpose, the following experimental parameters were evaluated: concentration of digestion solution, sample mass and microwave irradiation program. The residual carbon content was used as a parameter to evaluate the efficiency of digestion and to select the most suitable experimental conditions. The accuracy evaluation was performed by recovery tests using a standard solution and certified reference material, and recoveries ranging from 94% to 99% were obtained for all analytes. The limits of detection for Ni, Pd and Pt using the proposed method were 35.6, 0.264 and 0.302ngg -1 , respectively. When compared to microwave-assisted digestion (MW-AD) in closed vessels using concentrated HNO 3 (used as a reference method for sample digestion), the proposed MW-UV could be considered an excellent alternative for the digestion of margarine, as this method requires only a diluted nitric acid solution for efficient digestion. In addition, MW-UV provides appropriate solutions for further ICP-MS determination with suitable precision (relative standard deviation < 7%) and accuracy for all evaluated analytes. The proposed method was applied to margarines from different brands produced in Brazil, and the concentration of catalyst residues was in agreement with the current legislation or recommendations. Copyright © 2017 Elsevier B.V. All rights reserved.

Plant mediated green synthesis: modified approaches.

PubMed

Das, Ratul Kumar; Brar, Satinder Kaur

2013-11-07

Plant mediated green synthesis of different metallic nanoparticles has emerged as one of the options for implementation of green chemistry principles, and successfully made an important contribution towards green nanotechnology. However, beyond the synthesis and application aspects, the science of green synthesis has carried some wrong perceptions in an unforeseen fashion. In this review, some of the key issues related to the green synthesis of metallic nanoparticles employing plants as reducing/capping agents have been addressed. Random selection of plants and its overall impact on the different aspects of green synthesis have been discussed. Emphasis is given to the setting of some standard selection criteria to be adopted for selecting a plant for use in green synthesis. How selection of a plant can positively or negatively influence both procedure and products of a green synthesis process is the prime concern of this article. In addition to selection, the key issue of biocompatibility associated with green synthesized metallic nanoparticles has been considered. Both selection of plant and biocompatibility were reconsidered for their minute details in terms of synthesis, analysis and data interpretation in the green synthesis approach. The key factors capable of fine tuning the core meaning of "green" in the synthesis of any metallic nanoparticles were taken into consideration. This article is an effort towards keeping the core meaning of green synthesis.

Effects of feedstock characteristics on microwave-assisted pyrolysis - A review.

PubMed

Zhang, Yaning; Chen, Paul; Liu, Shiyu; Peng, Peng; Min, Min; Cheng, Yanling; Anderson, Erik; Zhou, Nan; Fan, Liangliang; Liu, Chenghui; Chen, Guo; Liu, Yuhuan; Lei, Hanwu; Li, Bingxi; Ruan, Roger

2017-04-01

Microwave-assisted pyrolysis is an important approach to obtain bio-oil from biomass. Similar to conventional electrical heating pyrolysis, microwave-assisted pyrolysis is significantly affected by feedstock characteristics. However, microwave heating has its unique features which strongly depend on the physical and chemical properties of biomass feedstock. In this review, the relationships among heating, bio-oil yield, and feedstock particle size, moisture content, inorganics, and organics in microwave-assisted pyrolysis are discussed and compared with those in conventional electrical heating pyrolysis. The quantitative analysis of data reported in the literature showed a strong contrast between the conventional processes and microwave based processes. Microwave-assisted pyrolysis is a relatively new process with limited research compared with conventional electrical heating pyrolysis. The lack of understanding of some observed results warrant more and in-depth fundamental research. Copyright © 2017 Elsevier Ltd. All rights reserved.

Rapid synthesis of flower shaped Cu{sub 2}ZnSnS{sub 4} nanoparticles by microwave irradiation for solar cell application

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

Ansari, Mohd Zubair, E-mail: mhd.zubair1@gmail.com; Khare, Neeraj

Single phase Cu{sub 2}ZnSnS{sub 4} (CZTS) nanoparticles have been synthesized by the microwave-assisted solution method in a one step process. Structural, morphological and optical characterizations of the CZTS nanoparticles have been carried out. X-ray diffraction confirms the single phase formation of CZTS nanoparticles with kesterite structure. SEM confirms the homogenous distribution of CZTS nanoparticles flower like assemblies. High resolution TEM image confirms the good crystallinity of the CZTS nanoparticles with the average grain size ~20 nm. The CZTS nanoparticles have strong optical absorption in the visible region with direct band gap as ~1.6 eV which is optimal for photovoltaic application.

Ultrasonic-assisted preparation of nano eggshell powder: a novel catalyst in green and high efficient synthesis of 2-aminochromenes.

PubMed

Mosaddegh, Elaheh

2013-11-01

The nano eggshell powder (NESP) has been prepared by ultrasound irradiation and used as a novel and biodegradable catalyst with high catalytic activity and reusability in green synthesis of 2-aminochromenes via condensation of α- or β-phathol, malononitrile and aromatic aldehydes at 120 °C under solvent-free conditions. The reaction proceeds to completion within 10-35 min in 91-98% yield. Nano eggshell catalyst was characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and X-ray fluorescence, thermal gravimetric, surface area and elemental analyses. In addition, the catalytic activity and chemical structure of nano-sized eggshell were compared with pure CaCO3. Copyright © 2013 Elsevier B.V. All rights reserved.

Rapid microwave-assisted synthesis of polydextrose and identification of structure and function.

PubMed

Wang, Haisong; Shi, Yonghui; Le, Guowei

2014-11-26

Microwave irradiation is a rapid and efficient method to synthesize oligomers and can be employed in polysaccharides production. As an artificial polysaccharide, polydextrose is known for its solid performance in food processing and its additional health benefits. This study was aimed at producing polydextrose by microwave irradiation using glucose and sorbitol as substrates; water and phosphoric acid as initiator and catalyst. The actual maximum yield was 99%. Synthetic polydextrose were purified by ethanol elution and Sepherdex G-25 column chromatography. Its purity was demonstrated by the high-performance gel-permeation chromatography as a single symmetrical sharp peak, additionally the average molecular weight was calculated to be 2.131 kDa. FT-IR spectra showed that the synthesized polydextrose has the structural feature similar to Polydextrose-Litesse(®). In vitro fermentation revealed that polydextrose possesses the biological function similar to Polydextrose-Litesse(®) in increasing the concentration of short chain fatty acid and decreasing pH. This research demonstrated the feasibility of a rapid and efficient microwave mediated method to synthesize polydextrose and potentially other value added carbohydrate polymers. Copyright © 2014 Elsevier Ltd. All rights reserved.

Green engineered biomolecule-capped silver and copper nanohybrids using Prosopis cineraria leaf extract: Enhanced antibacterial activity against microbial pathogens of public health relevance and cytotoxicity on human breast cancer cells (MCF-7).

PubMed

Jinu, U; Gomathi, M; Saiqa, I; Geetha, N; Benelli, G; Venkatachalam, P

2017-04-01

This research focused on green engineering and characterization of silver (PcAgNPs) and copper nanoparticles (PcCuNPs) using Prosopis cineraria (Pc) leaf extract prepared by using microwave irradiation. We studied their enhanced antimicrobial activity on human pathogens as well as cytotoxicity on breast cancer cells (MCF-7). Biofabricated silver and copper nanoparticles exhibited UV-Visible absorbance peaks at 420 nm and 575 nm, confirming the bioreduction and stabilization of nanoparticles. Nanoparticles were characterized by FTIR, XRD, FESEM, and EDX analysis. FTIR results indicated the presence of alcohols, alkanes, aromatics, phenols, ethers, benzene, amines and amides that were possibly involved in the reduction and capping of silver and copper ions. XRD analysis was performed to confirm the crystalline nature of the silver and copper nanoparticles. FESEM analysis suggested that the nanoparticles were hexagonal or spherical in shape with size ranging from 20 to 44.49 nm and 18.9-32.09 nm for AgNPs and CuNPs, respectively. EDX analysis confirmed the presence of silver and copper elemental signals in the nanoparticles. The bioengineered silver and copper nanohybrids showed enhanced antimicrobial activity against Gram-positive and Gram-negative MDR human pathogens. MTT assay results indicated that CuNPs show potential cytotoxic effect followed by AgNPs against MCF-7 cancer cell line. IC 50 were 65.27 μg/ml, 37.02 μg/ml and 197.3 μg/ml for PcAgNPs, PcCuNPs and P. cineraria leaf extracts, respectively, treated MCF-7 cells. The present investigation highlighted an effective protocol for microwave-assisted synthesis of biomolecule-loaded silver and copper nanoparticles with enhanced antibacterial and anticancer activity. Results strongly suggested that bioengineered AgNPs and CuNPs could be used as potential tools against microbial pathogens and cancer cells. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microwave sintering of boron carbide

DOEpatents

Blake, R.D.; Katz, J.D.; Petrovic, J.J.; Sheinberg, H.

1988-06-10

A method for forming boron carbide into a particular shape and densifying the green boron carbide shape. Boron carbide in powder form is pressed into a green shape and then sintered, using a microwave oven, to obtain a dense boron carbide body. Densities of greater than 95% of theoretical density have been obtained. 1 tab.

Microwave-assisted hydrothermal synthesis of Ag₂(W(1-x)Mox)O₄ heterostructures: Nucleation of Ag, morphology, and photoluminescence properties.

PubMed

Silva, M D P; Gonçalves, R F; Nogueira, I C; Longo, V M; Mondoni, L; Moron, M G; Santana, Y V; Longo, E

2016-01-15

Ag2W(1-x)MoxO4 (x=0.0 and 0.50) powders were synthesized by the co-precipitation (drop-by-drop) method and processed using a microwave-assisted hydrothermal method. We report the real-time in situ formation and growth of Ag filaments on the Ag2W(1-x)MoxO4 crystals using an accelerated electron beam under high vacuum. Various techniques were used to evaluate the influence of the network-former substitution on the structural and optical properties, including photoluminescence (PL) emission, of these materials. X-ray diffraction results confirmed the phases obtained by the synthesis methods. Raman spectroscopy revealed significant changes in local order-disorder as a function of the network-former substitution. Field-emission scanning electron microscopy was used to determine the shape as well as dimensions of the Ag2W(1-x)MoxO4 heterostructures. The PL spectra showed that the PL-emission intensities of Ag2W(1-x)MoxO4 were greater than those of pure Ag2WO4, probably because of the increase of intermediary energy levels within the band gap of the Ag2W(1-x)MoxO4 heterostructures, as evidenced by the decrease in the band-gap values measured by ultraviolet-visible spectroscopy. Copyright © 2015 Elsevier B.V. All rights reserved.

One pot light assisted green synthesis, storage and antimicrobial activity of dextran stabilized silver nanoparticles.

PubMed

Hussain, Muhammad Ajaz; Shah, Abdullah; Jantan, Ibrahim; Tahir, Muhammad Nawaz; Shah, Muhammad Raza; Ahmed, Riaz; Bukhari, Syed Nasir Abbas

2014-12-03

Green synthesis of nanomaterials finds the edge over chemical methods due to its environmental compatibility. Herein, we report green synthesis of silver nanoparticles (Ag NPs) mediated with dextran. Dextran was used as a stabilizer and capping agent to synthesize Ag NPs using silver nitrate (AgNO3) under diffused sunlight conditions. UV-vis spectra of as synthesized Ag nanoparticles showed characteristic surface plasmon band in the range from ~405-452 nm. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) studies showed spherical Ag NPs in the size regime of ~50-70 nm. Face centered cubic lattice of Ag NPs was confirmed by powder X-ray diffraction (PXRD). FT-IR spectroscopy confirmed that dextran not only acts as reducing agent but also functionalizes the surfaces of Ag NPs to make very stable dispersions. Moreover, on drying, the solution of dextran stabilized Ag NPs resulted in the formation of thin films which were found stable over months with no change in the plasmon band of pristine Ag NPs. The antimicrobial assay of the as synthesized Ag NPs showed remarkable activity. Being significantly active against microbes, the Ag NPs can be explored for antimicrobial medical devices.

Supercritical Carbon Dioxide and Microwave-Assisted Extraction of Functional Lipophilic Compounds from Arthrospira platensis

PubMed Central

Esquivel-Hernández, Diego A.; López, Víctor H.; Rodríguez-Rodríguez, José; Alemán-Nava, Gibrán S.; Cuéllar-Bermúdez, Sara P.; Rostro-Alanis, Magdalena; Parra-Saldívar, Roberto

2016-01-01

Arthrospira platensis biomass was used in order to obtain functional lipophilic compounds through green extraction technologies such as supercritical carbon dioxide fluid extraction (SFE) and microwave-assisted extraction (MAE). The temperature (T) factor was evaluated for MAE, while for SFE, pressure (P), temperature (T), and co-solvent (ethanol) (CS) were evaluated. The maximum extraction yield of the obtained oleoresin was (4.07% ± 0.14%) and (4.27% ± 0.10%) for SFE and MAE, respectively. Extracts were characterized by gas chromatography mass spectrometry (GC-MS) and gas chromatography flame ionization detector (GC-FID). The maximum contents of functional lipophilic compounds in the SFE and MAE extracts were: for carotenoids 283 ± 0.10 μg/g and 629 ± 0.13 μg/g, respectively; for tocopherols 5.01 ± 0.05 μg/g and 2.46 ± 0.09 μg/g, respectively; and for fatty acids 34.76 ± 0.08 mg/g and 15.88 ± 0.06 mg/g, respectively. In conclusion, the SFE process at P 450 bar, T 60 °C and CS 53.33% of CO2 produced the highest yield of tocopherols, carotenoids and fatty acids. The MAE process at 400 W and 50 °C gives the best extracts in terms of tocopherols and carotenoids. For yield and fatty acids, the MAE process at 400 W and 70 °C produced the highest values. Both SFE and MAE showed to be suitable green extraction technologies for obtaining functional lipophilic compounds from Arthrospira platensis. PMID:27164081

Supercritical Carbon Dioxide and Microwave-Assisted Extraction of Functional Lipophilic Compounds from Arthrospira platensis.

PubMed

Esquivel-Hernández, Diego A; López, Víctor H; Rodríguez-Rodríguez, José; Alemán-Nava, Gibrán S; Cuéllar-Bermúdez, Sara P; Rostro-Alanis, Magdalena; Parra-Saldívar, Roberto

2016-05-05

Arthrospira platensis biomass was used in order to obtain functional lipophilic compounds through green extraction technologies such as supercritical carbon dioxide fluid extraction (SFE) and microwave-assisted extraction (MAE). The temperature (T) factor was evaluated for MAE, while for SFE, pressure (P), temperature (T), and co-solvent (ethanol) (CS) were evaluated. The maximum extraction yield of the obtained oleoresin was (4.07% ± 0.14%) and (4.27% ± 0.10%) for SFE and MAE, respectively. Extracts were characterized by gas chromatography mass spectrometry (GC-MS) and gas chromatography flame ionization detector (GC-FID). The maximum contents of functional lipophilic compounds in the SFE and MAE extracts were: for carotenoids 283 ± 0.10 μg/g and 629 ± 0.13 μg/g, respectively; for tocopherols 5.01 ± 0.05 μg/g and 2.46 ± 0.09 μg/g, respectively; and for fatty acids 34.76 ± 0.08 mg/g and 15.88 ± 0.06 mg/g, respectively. In conclusion, the SFE process at P 450 bar, T 60 °C and CS 53.33% of CO₂ produced the highest yield of tocopherols, carotenoids and fatty acids. The MAE process at 400 W and 50 °C gives the best extracts in terms of tocopherols and carotenoids. For yield and fatty acids, the MAE process at 400 W and 70 °C produced the highest values. Both SFE and MAE showed to be suitable green extraction technologies for obtaining functional lipophilic compounds from Arthrospira platensis.

Alternative oil extraction methods from Echium plantagineum L. seeds using advanced techniques and green solvents.

PubMed

Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

2018-04-01

The edible oil processing industry involves large losses of organic solvent into the atmosphere and long extraction times. In this work, fast and environmentally friendly alternatives for the production of echium oil using green solvents are proposed. Advanced extraction techniques such as Pressurized Liquid Extraction (PLE), Microwave Assisted Extraction (MAE) and Ultrasound Assisted Extraction (UAE) were evaluated to efficiently extract omega-3 rich oil from Echium plantagineum seeds. Extractions were performed with ethyl acetate, ethanol, water and ethanol:water to develop a hexane-free processing method. Optimal PLE conditions with ethanol at 150 °C during 10 min produced a very similar oil yield (31.2%) to Soxhlet using hexane for 8 h (31.3%). UAE optimized method with ethanol at mild conditions (55 °C) produced a high oil yield (29.1%). Consequently, advanced extraction techniques showed good lipid yields and furthermore, the produced echium oil had the same omega-3 fatty acid composition than traditionally extracted oil. Copyright © 2017 Elsevier Ltd. All rights reserved.

Ultrafast microwave-assisted synthesis of nitrogen-doped carbons as electrocatalysts for oxygen reduction reaction.

PubMed

Xu, Jingjing; Zhang, Ruifang; Lu, Shiyao; Liu, Huan; Li, Zhaoyang; Zhang, Xinyu; Ding, Shujiang

2018-07-27

A facile and ultrafast microwave-assisted thermolysis approach has been adopted to synthesize hierarchical nitrogen-doped carbon within a very short time. The precursor PANI@carbon felt composite was pyrolyzed in microwave oven for different time (10, 20, 30, 40, 50 s) and denoted as NC-X (X = 10, 20, 30, 40, 50). As for NC-30, nitrogen-doping content is obtained up to 3.62 at% with striking enrichment of pyridinic N as high as 45% of the total nitrogen content. Raman analysis indicates the extent graphitization level for the resultant NC-30 and the relative intensity I D /I G was 1.26. High nitrogen-doping content and graphitization level provide effective active sites and efficient electron transfer channel. The resultant NC-30 exhibits pronounced ORR activity with an onset potential of 0.94 V (versus RHE), half-wave potential of 0.80 V and diffusion limiting current density of -5.23 mA cm -2 , comparable to those of the commercial Pt/C. It also shows enhanced stability with current retention of 98.3% over 7.5 h as well as superior tolerance against methanol. The simple preparation and excellent ORR performance of NC-30 suggest its promising practical application.

One-step microwave-assisted colloidal synthesis of hybrid silver oxide/silver nanoparticles: characterization and catalytic study

NASA Astrophysics Data System (ADS)

Prakoso, S. P.; Taufik, A.; Saleh, R.

2017-04-01

This study reports the characterization and catalytic activities of silver-oxide/silver nanoparticles (Ag2O/Ag NPs) synthesized by microwave-assisted colloidal method in the presence of anionic sodium dodecyl sulfate (SDS) surfactant. To promote different contents of silver in silver oxide, the volume ratio (VR) of ethylene glycol (EG) was varied (VR: 10% to 14%) in relation to the total volume of distilled water solvent. The plasmonic resonance of Ag2O/Ag NPs could be detected around a wavelength of 350 nm, and it is suggested that Ag2O/Ag NPs were successfully formed in the colloid solution following exposure to microwaves. Additionally, the growth rate for each crystal phase within Ag2O and Ag was influenced by an increase of EG as revealed by x-ray diffraction patterns. The morphology, average diameter, and uniformity of Ag2O/Ag NPs were studied simultaneously by transmission electron microscopy. Infrared absorption measurement of Ag2O/Ag NPs confirmed the existence of SDS surfactant as a protective agent. Based on the characterization data, Ag2O/Ag NPs synthesized using this technique exhibited good properties, with high-yield production of NPs. The photocatalytic experiments demonstrate the key role of the crystal phase of Ag2O/Ag NPs in photocatalytic efficiency.

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

Murgia, Fabrizio; Antitomaso, Philippe; Stievano, Lorenzo

The ternary Chevrel phase Cu{sub 2}Mo{sub 6}S{sub 8} was successfully synthetized using a simple and cost-effective solid-state microwave-assisted reaction. While solid-state routes require days of high-temperature treatment under inert atmosphere, highly pure and crystalline Cu{sub 2}Mo{sub 6}S{sub 8} could be obtained in only 400 s from this precursor, the Chevrel binary phase Mo{sub 6}S{sub 8} was then obtained by copper removal through acidic leaching, and was evaluated as a positive electrode material for Mg-battery. The electrochemical performance in half-cell configuration shows reversible capacity exceeding 80 mAh/g, which is comparable to previous works carried out with materials synthesized by conventional high-temperaturemore » solid-state routes. - Graphical abstract: Ultrafast micro-wave synthesis of Chevrel phase Cu{sub 2}Mo{sub 6}S{sub 8} towards Mo{sub 6}S{sub 8} as positive electrode of Mg-battery. - Highlights: • Chevrel phase Cu{sub 2}Mo{sub 6}S{sub 8} is synthesized by fast microwave-assisted solid-state reaction. • Highly-pure and well-crystalline Cu{sub 2}Mo{sub 6}S{sub 8} is obtained. • Mo{sub 6}S{sub 8} obtained from leaching is tested as a positive electrode for Mg batteries.« less

Cu2ZnSnS4 Nanoparticles Synthesized by a Novel Diethylenetriamine-Assisted Hydrothermal Method

NASA Astrophysics Data System (ADS)

Liang, Feng; Gao, Juan; Zou, Changwei; Shao, Lexi

2018-05-01

A diethylenetriamine (DETA)-assisted hydrothermal method was explored for the synthesis of kesterite Cu2ZnSnS4 (CZTS) nanoparticles. As complexing agent, DETA was employed to dissolve sulfur and to form complex with metal ions. By introducing DETA to the system, pure CZTS nanoparticles with bandgap of 1.54 eV could be successfully obtained and the agglomeration of samples could be restrained by increasing the concentration of DETA. From the discussion about the experimental results, the formation mechanism of CZTS nanoparticles was proposed. As the reagents used in this experiment is low-toxic and inexpensive, this method was considered as an effective and green route for the synthesis of CZTS nanoparticles.

Understanding the infrared to visible upconversion luminescence properties of Er{sup 3+}/Yb{sup 3+} co-doped BaMoO{sub 4} nanocrystals

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

Adhikari, Rajesh; Choi, Jinhyuk; Narro-García, R.

2014-08-15

In this paper we report the infrared to visible upconversion luminescence properties of Er{sup 3+}/Yb{sup 3+} co-doped BaMoO{sub 4} nanocrystals synthesized via microwave assisted sol–gel processing route. Structural, morphological and upconversion luminescence properties were investigated by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), UV–vis diffuse reflectance spectroscopy (UV–vis DRS) and Upconversion Photoluminescence spectra analysis. Results revealed that the oval shaped BaMoO{sub 4} nanocrystals ranging in size from 40 to 60 nm having tetragonal scheelite crystal structure were obtained by sol–gel route. The infrared to visible upconversion luminescence has been investigated in Er{sup 3+}/Yb{sup 3+} co-doped in BaMoO{sub 4}with different Yb{supmore » 3+} concentrations. Intense green upconversion emissions around 528, 550 nm, and red emission at 657 nm corresponding to the {sup 2}H{sub 11/2}, {sup 4}S{sub 3/2}, and {sup 4}F{sub 9/2} transitions, respectively to the {sup 4}I{sub 15/2} ground state were observed when excited by CW laser radiation at 980 nm. The green emissions were greatly enhanced after the addition of sensitizer (Yb{sup 3+} ions). The effect of Yb{sup 3+} on the upconversion luminescence intensity was analyzed and explained in terms of the energy transfer process based. The reported work establishes the understanding of molybdates as an alternative host material for upconversion luminescence. - Graphical abstract: Infrared to visible upconversion luminescence of Er{sup 3+}/Yb{sup 3+} co-doped BaMoO{sub 4} nanocrystals. - Highlights: • Nanocrystals were synthesized by microwave assisted sol–gel processing route. • Strong green emissions were observed in Er{sup 3+}/Yb{sup 3+} co-doped BaMoO{sub 4} nanocrystals. • Provides an insight on Upconversion luminescence properties of oxides host materials.« less

Synthesis of Silver Nanoparticles from Microbial Source-A Green Synthesis Approach, and Evaluation of its Antimicrobial Activity against Escherichia coli

NASA Astrophysics Data System (ADS)

Behera, S. S.; Jha, S.; Arakha, M.; Panigrahi, T. K.

2012-03-01

TRACT Nanoparticles synthesis by biological methods using various microorganisms, plants, and plant extracts and enzymes have attracted a great attention as these are cost effective, nontoxic, eco-friendly and an alternative to physical and chemical methods. In this research, Silver nanoparticles (Ag-NPs) were synthesized from AgNO3 solution by green synthesis process with the assistance of microbial source only. The detailed characterization of the Ag NPs were carried out using UV-visible spectroscopy, Scanning electron microscopy (SEM), Energy dispersive X-ray Spectroscopy (EDS), Dynamic light scattering (DLS) analysis, and their antimicrobial evaluation was done against Escherichia coli. The UV-visible spectroscopy analysis showed the surface plasmon resonance property of nanoparticles. The DLS analysis showed the particle distribution of synthesized silver nanoparticles in solution, and SEM analysis showed the morphology of nanoparticles. The elemental composition of synthesized sample was confirmed by EDS analysis. Antibacterial assay of synthesized Ag NP was carried out in solid (Nutrient Agar) growth medium against E.coli. The presence of zone of inhibition clearly indicated the antibacterial activity of silver nanoparticles.

Proton-conducting beta"-alumina via microwave-assisted synthesis and mechanism of enhanced corrosion prevention of a zinc rich coating with electronic control

NASA Astrophysics Data System (ADS)

Kirby, Brent William

Proton Conducting beta-alumina via Microwave Assisted Synthesis. The microwave assisted synthesis of proton conducting Mg- and Li-stabilized NH4+/H3O+ beta-alumina from a solution based gel precursor is reported. beta-alumina is a ceramic fast ion conductor containing two-dimensional sheets of mobile cations. Na +-beta-alumina is the most stable at the sintering temperatures (1740°C) reached in a modified microwave oven, and can be ion exchanged to the K+ form and then to the NH4+/H 3O+ form. beta-phase impurity is found to be 20% for Mg-stabilized material and 30-40% for Li-stabilized material. The composition of the proton conducting form produced here is deficient in NH4 + as compared to the target composition (NH4)1.00 (H3O)0.67Mg0.67Al10.33O 17. Average grain conductivity for Li-stabilized material at 150°C is 6.6x10-3 +/- 1.6x10-3 S/cm with 0.29 +/- 0.05 eV activation energy, in agreement with single crystal studies in the literature. Grain boundary conductivity is found to be higher in the Li-stabilized material. A hydrogen bond energy hypothesis is presented to explain these differences. Li-stabilized NH4+/H3O + beta-alumina is demonstrated as a fuel cell electrolyte, producing 28 muA/cm2 of electrical current at 0.5 V. Mechanism of Enhanced Corrosion Prevention of a Zinc Rich Coating with Electronic Control. A corrosion inhibition system consisting of high weight-loading zinc rich coating applied to steel panels is examined. An electronic control unit (ECU) consisting of a battery and a large capacitor in series with the panel is shown to improve corrosion protection upon immersion in 3% NaCl solution. Weekly solution changes to avoid zinc saturation in solution system were necessary to see well differentiated results. The corrosion product, hydrozincite [Zn5(CO3) 2(OH)6] is observed to deposit within the pores of the coating and on the surface as a barrier layer. Simonkolleite [Zn5(OH) 8Cl2·H2O] is found to form in place of the original zinc particles. The barrier layer is denser and more adherent with the ECU in place. A mechanism is proposed in which the characteristic time constant of the ECU is roughly matched to the time scale of ionic motion within the coating. The capacitive nature of the ECU retards the motion of ions, and affects the formation of denser corrosion products.

Effect of Microwave Vacuum Drying on the Drying Characteristics, Color, Microstructure, and Antioxidant Activity of Green Coffee Beans.

PubMed

Dong, Wenjiang; Cheng, Ke; Hu, Rongsuo; Chu, Zhong; Zhao, Jianping; Long, Yuzhou

2018-05-11

The aim of this study is to investigate the effect of microwave vacuum drying (MVD) on the drying characteristics and quality attributes of green coffee beans. We specifically focused on the effective moisture diffusion coefficient ( D eff ), surface temperature, glass transition temperature ( T g ), water state, and microstructure. The kinetics of color changes during drying, total phenolic content (TPC), and antioxidant activity (DPPH, FRAP, and ABTS) were also characterized. Microwave power during MVD affected the porosity of coffee beans, their color, TPC, and antioxidant activity. The Allometric 1 model was the most suitable for simulating surface temperature rise kinetics. Thermal processing of green coffee beans resulted in increased b* , L* , Δ E , and TPC values, and greater antioxidant capacity. These findings may provide a theoretical reference for the technical improvement, mechanisms of flavor compound formation, and quality control of dried green coffee beans.

Solution-Phase Synthesis of a Tricyclic Pyrrole-2-Carboxamide Discovery Library Applying a Stetter-Paal-Knorr Reaction Sequence

PubMed Central

Iyer, Pravin S.; Fodor, Matthew D.; Coleman, Claire M.; Twining, Leslie A.; Mitasev, Branko

2012-01-01

The solution phase synthesis of a discovery library of 178 tricyclic pyrrole-2-carboxamides was accomplished in nine steps and seven purifications starting with three benzoyl protected amino acid methyl esters. Further diversity was introduced by two glyoxaldehydes and forty-one primary amines. The combination of Pauson-Khand, Stetter and microwave assisted Paal Knorr reactions was applied as a key sequence. The discovery library was designed with the help of QikProp 2.1 and physicochemical data are presented for all pyrroles. Library members were synthesized and purified in parallel and analyzed by LC-MS. Selected compounds were fully characterized. PMID:16677007

Rapid synthesis of N, S co-doped carbon dots and their application for Fe3+ ion detection

NASA Astrophysics Data System (ADS)

Zhang, Jian; Wang, Junbin; Fu, Jinping; Fu, Xucheng; Gan, Wei; Hao, Hequn

2018-02-01

In this study, nitrogen and sulfur co-doped carbon dots (NSCDs) were fabricated by microwave-assisted one-pot synthesis using vitamin C and thiourea as precursors. The as-prepared NSCDs demonstrated excellent properties, including aqueous dispensability, strong fluorescence emission, excellent environmental stability, high selectivity, and sensitivity toward Fe3+ ions. The NSCD-based material can be used as a "turn off" fluorescent probe for detecting Fe3+ ions at a low detection limit (4.2 nM). In addition, the "turn off" and "turn on" of NSCD fluorescent probe could be modulated by adding Fe3+ and EDTA, indicating weak interaction between the Fe3+ ions and NSCDs.

Synthesis and measurement of ultrafast waveforms from five discrete optical harmonics.

PubMed

Chan, Han-Sung; Hsieh, Zhi-Ming; Liang, Wei-Hong; Kung, A H; Lee, Chao-Kuei; Lai, Chien-Jen; Pan, Ru-Pin; Peng, Lung-Han

2011-03-04

Achieving the control of light fields in a manner similar in sophistication to the control of electromagnetic fields in the microwave and radiofrequency regimes has been a major challenge in optical physics research. We manipulated the phase and amplitude of five discrete harmonics spanning the blue to mid-infrared frequencies to produce instantaneous optical fields in the shape of square, sawtooth, and subcycle sine and cosine pulses at a repetition rate of 125 terahertz. Furthermore, we developed an all-optical shaper-assisted linear cross-correlation technique to retrieve these fields and thereby verified their shapes and confirmed the critical role of carrier-envelope phase in Fourier synthesis of optical waveforms.

Bio-based products via microwave-assisted maleation of tung oil

USDA-ARS?s Scientific Manuscript database

A simple “green” and convenient chemical modification of tung oil for maleinized tung oil (TOMA) was developed via microwave-assisted one-step maleation. The mechanism of this microwave-assisted maleation was investigated by nuclear magnetic resonance (NMR) and gel permeation chromatography (GPC). T...

Effect of Microwave Radiation Power on the Size of Aggregates of ZnO NPs Prepared Using Microwave Solvothermal Synthesis

PubMed Central

Chudoba, Tadeusz; Gierlotka, Stanisław; Lojkowski, Witold

2018-01-01

This paper reports the possibility of changing the size of zinc oxide nanoparticles (ZnO NPs) aggregates through a change of synthesis parameters. The effect of the changed power of microwave heating on the properties of ZnO NPs obtained by the microwave solvothermal synthesis from zinc acetate dissolved in ethylene glycol was tested for the first time. It was found that the size of ZnO aggregates ranged from 60 to 120 nm depending on the power of microwave radiation used in the synthesis of ZnO NPs. The increase in the microwave radiation power resulted in the reduction of the total synthesis time with simultaneous preservation of the constant size and shape of single ZnO NPs, which were synthesized at a pressure of 4 bar. All the obtained ZnO NPs samples were composed of homogeneous spherical particles that were single crystals with an average size of 27 ± 3 nm with a developed specific surface area of 40 m2/g and the skeleton density of 5.18 ± 0.03 g/cm3. A model of a mechanism explaining the correlation between the size of aggregates and the power of microwaves was proposed. This method of controlling the average size of ZnO NPs aggregates is presented for the first time and similar investigations are not found in the literature. PMID:29783651

Fast and simple microwave synthesis of TiO2/Au nanoparticles for gas-phase photocatalytic hydrogen generation

NASA Astrophysics Data System (ADS)

May-Masnou, Anna; Soler, Lluís; Torras, Miquel; Salles, Pol; Llorca, Jordi; Roig, Anna

2018-04-01

The fabrication of small anatase titanium dioxide (TiO2) nanoparticles (NPs) attached to larger anisotropic gold (Au) morphologies by a very fast and simple two-step microwave-assisted synthesis is presented. The TiO2/Au NPs are synthesized using polyvinylpyrrolidone (PVP) as reducing, capping and stabilizing agent through a polyol approach. To optimize the contact between the titania and the gold and facilitate electron transfer, the PVP is removed by calcination at mild temperatures. The nanocatalysts activity is then evaluated in the photocatalytic production of hydrogen from water/ethanol mixtures in gas-phase at ambient temperature. A maximum value of 5.3 mmol·gcat-1·h-1 (7.4 mmol·gTiO2-1·h-1) of hydrogen is recorded for the system with larger gold particles at an optimum calcination temperature of 450 °C. Herein we demonstrate that TiO2-based photocatalysts with high Au loading and large Au particle size (≈ 50 nm) NPs have photocatalytic activity.

Microwave Synthesis, Characterization, and Photoluminescence Properties of Nanocrystalline Zirconia

PubMed Central

Singh, A. K.; Nakate, Umesh T.

2014-01-01

We report synthesis of ZrO2 nanoparticles (NPs) using microwave assisted chemical method at 80°C temperature. Synthesized ZrO2 NPs were calcinated at 400°C under air atmosphere and characterized using FTIR, XRD, SEM, TEM, BET, and EDS for their formation, structure, morphology, size, and elemental composition. XRD results revealed the formation of mixed phase monoclinic and tetragonal ZrO2 phases having crystallite size of the order 8.8 nm from most intense XRD peak as obtained using Scherrer formula. Electron microscope analysis shows that the NPs were less than 10 nm and highly uniform in size having spherical morphology. BET surface area of ZrO2 NPs was found to be 65.85 m2/g with corresponding particle size of 16 nm. The band gap of synthesized NPs was found to be 2.49 eV and PL spectra of ZrO2 synthesized NPs showed strong peak at 414 nm, which corresponds to near band edge emission (UV emission) and a relatively weak peak at 475 and 562 nm. PMID:24578628

Optimization of the recovery of high-value compounds from pitaya fruit by-products using microwave-assisted extraction.

PubMed

Ferreres, Federico; Grosso, Clara; Gil-Izquierdo, Angel; Valentão, Patrícia; Mota, Ana T; Andrade, Paula B

2017-09-01

A green microwave-assisted extraction of high value-added compounds from exotic fruits' peels was optimized by Box-Behnken design using 3 factors: solid/solvent ratio, X 1 , temperature, X 2 , and extraction time, X 3 . By using Derringer's desirability function, optimum extraction yields are obtained with X 1 =1/149.95g/mL, X 2 =72.27°C and X 3 =39.39min (white-fleshed red pitaya) and X 1 =1/148.96g/mL, X 2 =72.56°C and X 3 =5.02min (yellow pitaya) and a maximum betacyanin content is achieved with X 1 =1/150g/mL, X 2 =49.33°C and X 3 =5min. None of the factors influenced the extraction of phenolic compounds. Eighteen cinnamoyl derivatives, 17 flavonoid derivatives and 4 betacyanins were identified by HPLC-DAD-ESI/MS n , 23 and 15 new compounds being described in yellow and white-fleshed red pitayas, respectively. These results indicate that it is possible to reuse these by-products to recover compounds for food and pharmaceutical industries. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis of SnO2 and Ag Nanoparticles from Electronic Wastes with the Assistance of Ultrasound and Microwaves

NASA Astrophysics Data System (ADS)

Cerchier, Pietrogiovanni; Dabalà, Manuele; Brunelli, Katya

2017-09-01

In this work, SnO2 and Ag nanoparticles were produced with a raw material nitric acid solution, which came from the leaching of printed circuit boards. First, a precursor of tin oxide was precipitated from the nitric acid solution by three different techniques: (I) conventional heating, (II) microwave irradiation, and (III) ultrasound treatment. Second, this precursor was transformed into tin oxide nanoparticles by heat treatment in a furnace. Third, hydrochloric acid was added to the nitric acid solution to induce the precipitation of silver chloride. Fourth, silver chloride was reduced to metallic silver nanoparticles in an ammonia solution using glucose syrup as both the reducing agent and the capping agent. The reduction reaction was carried out through (I) conventional heating, (II) microwave irradiation, and (III) ultrasound treatment. The nanoparticles were characterized by scanning electron microscope (SEM), x-ray diffractometer (XRD), infrared (IR)-spectroscopy, transmission electron microscope (TEM), ultraviolet (UV)-spectroscopy, and laser diffraction particle size analyzer.

Microwave assisted synthesis and anti-lipase activity of some new fluorine-containing benzimidazoles.

PubMed

Menteşe, E; Yilmaz, F; Ülker, S; Kahveci, B

2015-01-01

In this study, a new series of fluorine containing benzimidazoles (4a-l) and bisbenzimidazoles (6a-c, 8) were synthesized by the reaction of o-phenylenediamines with iminoester hydrochlorides (3a-l, 7) in methanol under microwave irradiation. The structures of these newly synthesized compounds were identified by IR, (1)H-NMR, (13)C-NMR, mass spectroscopy and elemental analysis data. The synthesized compounds were screened for their pancreatic lipase activities. Our results indicate that the compounds 6a, 6b and 6c can serve as an anti-lipase agent. The compounds 6b and 6c inhibited pancreatic lipase activity by 84.03% and 97.49% at a concentration of 3 µg/mL, respectively. © Georg Thieme Verlag KG Stuttgart · New York.

Microwave assisted synthesis of biarlys by Csbnd C coupling reactions with a new chitosan supported Pd(II) catalyst

NASA Astrophysics Data System (ADS)

Baran, Talat; Menteş, Ayfer

2016-10-01

In this study a new type chitosan-based support has been produced for Pd(II) catalyst and its catalytic performance in Suzuki Csbnd C reactions has been studied under microwave irradiation without using any solvent. The chemical identification of the catalyst was performed using TG/DTG, FTIR, UV-Vis ICP-OES, SEM/EDAX, 13C NMR, molar conductivity, XRD and magnetic moment techniques. The performance of this new Pd(II) catalyst was studied in Suzuki Csbnd C reactions. The Pd(II) catalyst exhibited a good catalytic performance in very short time (4 min) by giving high TONs and TOFs with low amount of the catalyst (0.015 mol%). The catalyst also had reusability and did not lose its activity until six runs.

Microwave-assisted synthesis and structure-activity relationships of neuroactive pyrazolo[3,4-b]pyrrolo[3,4-d]pyridine derivatives.

PubMed

Nascimento-Júnior, Nailton M; Mendes, Thaiana C F; Leal, Daniella M; Corrêa, Claudia Maria N; Sudo, Roberto T; Zapata-Sudo, Gisele; Barreiro, Eliezer J; Fraga, Carlos A M

2010-01-01

We described herein the optimization of the synthetic methodology exploited to obtain the pyrazolo[3,4-b]pyrrolo[3,4-d]pyridine sedative prototype 1a and novel analogues designed by successive molecular simplifications. By applying microwave irradiation during the hetero Diels-Alder key-step to obtain the heterotricyclic scaffold, under solvent-free conditions, we were able to obtain the desired compounds in drastically shorter times and better yields. Additionally, in vivo evaluation of the sedative effects of these heterocyclic derivatives showed that 1a and the novel structurally-related analogue 1e were the most efficient compounds to impair the locomotor activity in mice at the dose of 10micromol/kg. Copyright 2009 Elsevier Ltd. All rights reserved.

Microwave-assisted acid pretreatment of alkali lignin: Effect on characteristics and pyrolysis behavior.

PubMed

Duan, Dengle; Ruan, Roger; Wang, Yunpu; Liu, Yuhuan; Dai, Leilei; Zhao, Yunfeng; Zhou, Yue; Wu, Qiuhao

2018-03-01

This study performed microwave-assisted acid pretreatment on pure lignin. The effects of microwave temperature, microwave time, and hydrochloric acid concentration on characteristics and pyrolysis behavior of lignin were examined. Results of ultimate analysis revealed better properties of all pretreated samples than those of raw lignin. Fourier transform infrared spectroscopy analysis showed breakage of βO4 bond and aliphatic side chain, decrease in OH groups, and formation of CO groups in pretreatment. Microwave temperature exerted more significant influence on lignin structure. Thermal stability of treated lignin was improved and insensitive to short microwave time and acid concentration under mild conditions. Resulting from improved alkyl-phenols and decreased alkoxy-phenols, microwave-assisted acid pretreatment of lignin yielded bio-oil with excellent quality. Total yield of phenols in pyrolysis vapors (200 °C) improved to 14.15%, whereas that of guaiacols decreased to 22.36%. This study shows that microwave-assisted acid pretreatment is a promising technology for lignin conversion. Copyright © 2017 Elsevier Ltd. All rights reserved.

The effect of RO3201195 and a pyrazolyl ketone P38 MAPK inhibitor library on the proliferation of Werner syndrome cells.

PubMed

Bagley, Mark C; Dwyer, Jessica E; Baashen, Mohammed; Dix, Matthew C; Murziani, Paola G S; Rokicki, Michal J; Kipling, David; Davis, Terence

2016-01-21

Microwave-assisted synthesis of the pyrazolyl ketone p38 MAPK inhibitor RO3201195 in 7 steps and 15% overall yield, and the comparison of its effect upon the proliferation of Werner Syndrome cells with a library of pyrazolyl ketones, strengthens the evidence that p38 MAPK inhibition plays a critical role in modulating premature cellular senescence in this progeroid syndrome and the reversal of accelerated ageing observed in vitro on treatment with SB203580.

Simple and efficient sustainable semi-synthesis of oleacein [2-(3,4-hydroxyphenyl) ethyl (3S,4E)-4-formyl-3-(2-oxoethyl)hex-4-enoate] as potential additive for edible oils.

PubMed

Costanzo, Paola; Bonacci, Sonia; Cariati, Luca; Nardi, Monica; Oliverio, Manuela; Procopio, Antonio

2018-04-15

A simple and very environmental friendly microwave assisted method to produce oleacein in good yield starting from the easily available oleuropein is here presented. The methodology is proposed to produce the appropriate amount of hydroxytyrosol derivatives to enrich a commercial oil for an oil which provides beneficial effects on the human health. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microwave-Assisted Organocatalytic Intramolecular Knoevenagel/Hetero Diels-Alder Reaction with O-(Arylpropynyloxy)-Salicylaldehydes: Synthesis of Polycyclic Embelin Derivatives.

PubMed

Martín-Acosta, Pedro; Feresin, Gabriela; Tapia, Alejandro; Estévez-Braun, Ana

2016-10-21

A highly efficient and regioselective approach to new polycyclic embelin derivatives through a domino Knoevenagel condensation/intramolecular hetero Diels-Alder reaction using O-(arylpropynyloxy)-salicylaldehydes in the presence of ethylenediamine diacetate (EDDA) is reported. This organocatalyzed protocol is compatible toward a wide range of aryl-substituted alkynyl ethers with electron-donating and electron-withdrawing groups. When other active methylene compounds were subjected to this domino reaction the corresponding adducts were obtained in high yield.

Microwave-assisted one-step synthesis of white light-emitting carbon dot suspensions

NASA Astrophysics Data System (ADS)

Vanessa, Hinterberger; Wenshuo, Wang; Cornelia, Damm; Simon, Wawra; Martin, Thoma; Wolfgang, Peukert

2018-06-01

In this contribution, we demonstrate that an aqueous solution with adjustable fluorescent color, including white light emission, can be achieved by a rapid one-step microwave synthesis method resulting in a mixture of blue-emitting carbon dots (CDs) and the yellow-emitting 2,3-diaminophenazine (DAP). Aqueous mixtures of o-phenylene-diamine (oPD) and citric acid (CA) are used as precursors. The resulting product structures are analyzed by FT-IR and NMR spectroscopy and the size of the resulting CDs is determined by atomic force microscopy to be 1.1 ± 0.3 nm. The synthesized solution exhibits two fluorescence emission peaks at 430 and 560 nm, which were found to originate from the CDs and DAP, respectively. The intensity ratio of both fluorescence peaks depends on pH, which is driven by the protonation state of DAP. In consequence, the fluorescence emission color of the CD solution can be tuned precisely and reproducibly from blue to white to yellow by careful control of the pH. Finally, at a pH level of 5.4, at which there is equal blue and yellow emission intensity, a white light emitting solution can be successfully produced in a very fast and simple synthesis procedure.

Microwave-assisted Synthesis of Benzimidazole Derivatives from Citronellal in Kaffir Lime (Citrus hystrix DC.) Oil

NASA Astrophysics Data System (ADS)

Sapri Ramadhan, Dwi; Warsito; Dhiaul Iftitah, Elvina

2018-01-01

Benzimidazoles are an important group of heterocyclic aromatic organic compound in the field of medicinal chemistry. It plays a very important role in pharmacological activity such as, analgesic, antiinflammatory, antibacterial, anti ungal, anti iral, antithelmenthic, anti convulsant, antihypertensive, and antiulcer. The synthesis of benzimidazole derivative under microwave irradiation of citronellal as raw material which is extracted from Citrus hystrix DC. (kaffir lime) leaves. The reaction using methanol and dichloromethane as solvent with variation of reaction time at 30, 40, 50, 60, and 70 minutes and mole ratio of citronellal to 1,2-phenylenediamine, 1:1, 1:1.5, and 1:2, respectively. Synthesis products was characterized by FT-IR and GC-MS. The optimum reaction time was obtained at 60 minutes in the present of dichloromethane and 1:2 mole ratio of citronellal to 1,2-phenylenediamine. The yield of the product is 42.19%. Structure of the synthesized compound were assigned on spectrum bands for C=N str at 1661 cm-1, C-N str at 1271 cm-1, C=C str of benzene ring at 1622 and 1456 cm-1 and C=C str of alkene at 1379 cm-1. GC-MS analysis showed single peak with retention time of 15.339 minute and m/z 242.

Cook/chill foodservice system with a microwave oven: aerobic plate counts from beef loaf, potatoes and frozen green beans.

PubMed

Dahl, C A; Matthews, M E; Marth, E H

1980-06-01

The purpose was to evaluate microbiological quality and end temperature (ET) of portioned food after heating in a microwave oven as used in a hospital cook/chill foodservice system. Beef loaf (15 kg), potatoes (6 kg), and green beans (5 kg) were prepared in a laboratory. After initial cooking to 60 degrees C, and storage (7 degrees C for 24 h), beef loaf (100 g) was microwave heated: 20, 50, 80 or 110 s. Potatoes were reconstituted, stored (7 degrees C for 24 h), portioned (100 g/portion), and microwave-heated: 25, 45, 65 or 84 s. Beans were thawed (7 degrees C for 24 h), portioned (100 g/portion), and microwave-heated: 20, 50, 80 or 110 s. Aerobic plate counts (APC) for foods were obtained throughout product flow. Wide ranges of Et and of APC in foods indicates that research is needed, for greater control of microwave-heating through advanced microwave engineering and food technology, to produce food with constant microbiological quality.

Microwave-Irradiation-Assisted HVAC Filtration for Inactivation of Viral Aerosols (Postprint)

DTIC Science & Technology

2012-02-01

Baggiani, A. and Senesi, S. (2004). Effect of Microwave Radiation on Bacillus subtilis Spores . J. Appl. Microbiol. 97: 1220–1227. Damit, B., Lee, C.N...AFRL-RX-TY-TP-2012-0020 MICROWAVE-IRRADIATION-ASSISTED HVAC FILTRATION FOR INACTIVATION OF VIRAL AEROSOLS POSTPRINT Myung-Heui Woo and...12-APR-2011 -- 11-DEC-2011 Microwave Irradiation-Assisted HVAC Filtration for Inactivation of Viral Aerosols (POSTPRINT) FA8650-06-C-5913 0602102F

Central composite rotatable design for investigation of microwave-assisted extraction of ginger (Zingiber officinale)

NASA Astrophysics Data System (ADS)

Fadzilah, R. Hanum; Sobhana, B. Arianto; Mahfud, M.

2015-12-01

Microwave-assisted extraction technique was employed to extract essential oil from ginger. The optimal condition for microwave assisted extraction of ginger were determined by resposnse surface methodology. A central composite rotatable design was applied to evaluate the effects of three independent variables. The variables is were microwave power 400 - 800W as X1, feed solvent ratio of 0.33 -0.467 as X2 and feed size 1 cm, 0.25 cm and less than 0.2 cm as X3. The correlation analysis of mathematical modelling indicated that quadratic polynomial could be employed to optimize microwave assisted extraction of ginger. The optimal conditions to obtain highest yield of essential oil were : microwave power 597,163 W : feed solvent ratio and size of feed less than 0.2 cm.

Microwave-assisted solvothermal synthesis of flower-like Ag/AgBr/BiOBr microspheres and their high efficient photocatalytic degradation for p-nitrophenol

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

Li, Tingting, E-mail: tingtingli1983@hotmail.com; State Key Laboratory of Chemo/Biosensing and Chemometrics, Hunan University, Changsha 410082; Department of Environment and Chemical Engineering, Key Laboratory of Jiangxi Province for Ecological Diagnosis, Remediation and Pollution Control, Nanchang Hangkong University, Nanchang 330063

Flower-like Ag/AgBr/BiOBr microspheres were successfully fabricated by the approach of microwave-assisted solvothermal and in situ photo-assisted reduction. A reactive ionic liquid 1-hexadecyl-3-methylimidazolium bromide ([C{sub 16}mim]Br) was employed as Br source in the presence of surfactant polyvinylpyrrolidone (PVP). The photocatalytic activity of Ag/AgBr/BiOBr towards the decomposition of p-nitrophenol under visible light irradiation was evaluated. The results indicated that Ag/AgBr/BiOBr showed enhanced photocatalytic activity towards p-nitrophenol, comparing with P25, BiOBr and Ag/AgBr. More than 96% of p-nitrophenol was decomposed in 3.5 h under visible-light irradation. The excellent photocatalytic activity of flower-like Ag/AgBr/BiOBr microspheres can be attributed to the large specific surface area,more » strong visible-light absorption, suitable energy band structure and surface plasmon resonance effect of Ag nanoparticles. The possible photocatalytic mechanism was proposed based on the active species test and band gap structure analysis. - Graphical abstract: The photocatalytic reaction mechanisms of the as-prepared Ag/AgBr/BiOBr. Display Omitted - Highlights: • Successful synthesis of flower-like Ag/AgBr/BiOBr microspheres. • The Ag/AgBr/BiOBr showed much higher photocatalytic activity towards p-nitrophenol as compared to BiOBr and Ag/AgBr. • The reasons for the excellent photocatalytic activity are the large specific surface area, strong visible-light absorption and surface plasmon resonance effect of Ag nanoparticles. • The O{sub 2}·{sup −}, Br{sup 0} and photogenerated h{sup +} play key roles in the photocatalytic degradation process.« less

Microwave-assisted synthesis and humidity sensing of nanostructured {alpha}-Fe{sub 2}O{sub 3}

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

Deshmukh, Rupali G.; Badadhe, Satish S.; Mulla, Imtiaz S.

2009-05-06

Nanocrystalline {alpha}-Fe{sub 2}O{sub 3} has been prepared on a large-scale by a facile microwave-assisted hydrothermal route from a solution of Fe(NO{sub 3}){sub 3}.9H{sub 2}O and pentaerythritol. A systematic study of the morphology, crystallinity and oxidation state of Fe using different characterization techniques, such as transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy was performed. It reveals that nanostructured {alpha}-Fe{sub 2}O{sub 3} comprises bundles of nanorods with a rhombohedral crystalline structure. The individual nanorod has 8-10 nm diameter and {approx}50 nm length. The as-prepared nanostructured {alpha}-Fe{sub 2}O{sub 3} (sensor) gives selective response towards humidity. The sensor shows high sensitivity, fastmore » linear response to change in the humidity with almost 100% reproducibility. The sensor works at room temperature and rejuvenates without heat treatment. The as-prepared nanostructured {alpha}-Fe{sub 2}O{sub 3} appears to be a promising humidity sensing material with the potential for commercialization.« less

The synthesis of Cu/Fe/Fe3O4 catalyst through the aqueous solution ball milling method assisted by high-frequency electromagnetic field

NASA Astrophysics Data System (ADS)

Yingzhe, Zhang; Yuxing, He; Qingdong, Qin; Fuchun, Wang; Wankun, Wang; Yongmei, Luo

2018-06-01

In this paper, nano-magnetic Cu/Fe/Fe3O4 catalyst was prepared by a new aqueous solution ball milling method assisted by high-frequency electromagnetic field at room temperature. The products were characterized by means of X-ray diffraction (XRD), high-resolution transmission electron microscope (HRTEM), selected area electron diffraction (SAED), and vibrating sample magnetometer (VSM). Microwave induced catalytic degradation of methylene blue (MB) was carried out in the presence of Cu/Fe/Fe3O4. The concentration of methylene blue was determined by UV-Vis spectrophotometry. The solid catalyst showed high catalytic activity of degrade MB and considerable saturation magnetization, lower remanence and coercivity. It indicate that the catalyst can be effectively separated for reuse by simply applying an external magnetic field and it can greatly promote their potential industrial application to eliminate organic pollutants from waste-water. Finally, we found that it is the non-thermal effect of microwave that activated the catalytic activity of Cu/Fe/Fe3O4 to degrade MB.

Rapid microwave-assisted synthesis of highly luminescent nitrogen-doped carbon dots for white light-emitting diodes

NASA Astrophysics Data System (ADS)

Wang, Yaling; Zheng, Jingxia; Wang, Junli; Yang, Yongzhen; Liu, Xuguang

2017-11-01

Highly luminescent nitrogen-doped carbon dots (N-CDs) were synthesized rapidly by one-step microwave-assisted hydrothermal method using citric acid as carbon source and ethylenediamine as dopant. The influences of reaction temperature, reaction time and raw material ratio on the fluorescence performance of N-CDs were investigated. Then N-CDs with the highest quantum yield were selected as fluorescent materials for fabricating white light-emitting diodes (LEDs). Highly luminescent N-CDs with the quantum yield of 75.96% and blue-to-red spectral composition of 51.48% were obtained at the conditions of 180 °C, 8 min and the molar ratio of citric acid to ethylenediamine 2:1. As-prepared highly luminescent N-CDs have an average size of 6.06 nm, possess extensive oxygen- and nitrogen-containing functional groups on their surface, and exhibit strong absorption in ultraviolet region. White LEDs based on the highly luminescent N-CDs emit warm white light with color coordinates of (0.42, 0.40) and correlated color temperature of 3416 K.

Conventional and microwave-assisted synthesis of new indole-tethered benzimidazole-based 1,2,3-triazoles and evaluation of their antimycobacterial, antioxidant and antimicrobial activities.

PubMed

Ashok, Dongamanti; Gundu, Srinivas; Aamate, Vikas Kumar; Devulapally, Mohan Gandhi

2018-04-18

A new series of triheterocycles containing indole-benzimidazole-based 1,2,3-triazole hybrids have been synthesized in good yields via a microwave-assisted click reaction. All the compounds were characterized by IR, [Formula: see text] NMR, [Formula: see text] NMR and mass spectroscopy and were evaluated for their in vitro antitubercular activity against the Mycobacterium tuberculosis H37Rv strain. Compounds 4b, 4h and 4i displayed highly potent antitubercular activity with MIC 3.125-6.25 [Formula: see text]. The antioxidant potential was evaluated using 2,2-diphenyl-1-picryl hydrazine and [Formula: see text] radical scavenging activity, and compounds 4e,4f and 4g showed excellent radical scavenging activity with [Formula: see text] values in the range of 08.50-10.05 [Formula: see text]. Furthermore, the compounds were evaluated for antimicrobial activity against numerous bacterial and fungal strains, and compounds 4b, 4c and 4h were found to be the most promising potential antimicrobial molecules with MIC 3.125-6.25 [Formula: see text].

Opioid Receptor Probes Derived from Cycloaddition of the Hallucinogen Natural Product Salvinorin A†

PubMed Central

Lozama, Anthony; Cunningham, Christopher W.; Caspers, Michael J.; Douglas, Justin T.; Dersch, Christina M.; Rothman, Richard B.; Prisinzano, Thomas E.

2011-01-01

As part of our continuing efforts toward more fully understanding the structure-activity relationships of the neoclerodane diterpene salvinorin A, we report the synthesis and biological characterization of unique cycloadducts through [4+2] Diels-Alder cycloaddition. Microwave-assisted methods were developed and successfully employed, aiding in functionalizing the chemically sensitive salvinorin A scaffold. This demonstrates the first reported results for both cycloaddition of the furan ring and functionalization via microwave-assisted methodology of the salvinorin A skeleton. The cycloadducts yielded herein introduce electron-withdrawing substituents and bulky aromatic groups into the C-12 position. Kappa opioid (KOP) receptor space was explored through aromatization of the bent oxanorbornadiene system possessed by the cycloadducts to a planar phenyl ring system. Although dimethyl- and diethylcarboxylate analogues 5 and 6 retain some affinity and selectivity for KOP receptors and are full agonists, their aromatized counterparts 13 and 14 have reduced affinity for KOP receptors. The methods developed herein signify a novel approach toward rapidly probing the structure-activity relationships of furan containing natural products. PMID:21338114

Microwave-Enhanced Organic Syntheses for the Undergraduate Laboratory: Diels-Alder Cycloaddition, Wittig Reaction, and Williamson Ether Synthesis

ERIC Educational Resources Information Center

Baar, Marsha R.; Falcone, Danielle; Gordon, Christopher

2010-01-01

Microwave heating enhanced the rate of three reactions typically performed in our undergraduate organic chemistry laboratory: a Diels-Alder cycloaddition, a Wittig salt formation, and a Williamson ether synthesis. Ninety-minute refluxes were shortened to 10 min using a laboratory-grade microwave oven. In addition, yields improved for the Wittig…

Gold Nanoparticle Microwave Synthesis

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

Krantz, Kelsie E.; Christian, Jonathan H.; Coopersmith, Kaitlin

At the nanometer scale, numerous compounds display different properties than those found in bulk material that can prove useful in areas such as medicinal chemistry. Gold nanoparticles, for example, display promise in newly developed hyperthermia therapies for cancer treatment. Currently, gold nanoparticle synthesis is performed via the hot injection technique which has large variability in final particle size and a longer reaction time. One underdeveloped area by which these particles could be produced is through microwave synthesis. To initiate heating, microwaves agitate polar molecules creating a vibration that gives off the heat energy needed. Previous studies have used microwaves formore » gold nanoparticle synthesis; however, polar solvents were used that partially absorbed incident microwaves, leading to partial thermal heating of the sample rather than taking full advantage of the microwave to solely heat the gold nanoparticle precursors in a non-polar solution. Through this project, microwaves were utilized as the sole heat source, and non-polar solvents were used to explore the effects of microwave heating only as pertains to the precursor material. Our findings show that the use of non-polar solvents allows for more rapid heating as compared to polar solvents, and a reduction in reaction time from 10 minutes to 1 minute; this maximizes the efficiency of the reaction, and allows for reproducibility in the size/shape of the fabricated nanoparticles.« less

Fe-containing nanoparticles used as effective catalysts of lignin reforming to syngas and hydrogen assisted by microwave irradiation

NASA Astrophysics Data System (ADS)

Tsodikov, M. V.; Ellert, O. G.; Nikolaev, S. A.; Arapova, O. V.; Bukhtenko, O. V.; Maksimov, Yu. V.; Kirdyankin, D. I.; Vasil'kov, A. Yu.

2018-03-01

Active iron-containing nanosized components have been formed on the lignin surface. The metal was deposited on the lignin from an ethanol solution of Fe(acac)3 and from a colloid solution of iron metal particles obtained beforehand by metal vapor synthesis. These active components are able to absorb microwave radiation and are suitable for microwave-assisted high-rate dehydrogenation and dry reforming of lignin without addition of a carbon adsorbent, as a supplementary radiation absorbing material, to the feedstock. The dependence of the solid lignin heating dynamics on the concentration of supported iron particles was investigated. The threshold Fe concentration equal to 0.5 wt.%, providing the highest rate of sample heating up to the reforming and plasma generation temperature was identified. The microstructure and magnetic properties of iron-containing nanoparticles supported on lignin were studied before and after the reforming. The Fe3O4 nanoparticles and also core-shell Fe3O4@γ-Fe-C nanostructures are formed during the reforming of lignin samples. The catalytic performance of iron-based nanoparticles toward the lignin conversion is manifested as increasing selectivity to hydrogen and syngas, which reaches 94% at the Fe concentration of 2 wt.%. It was found that with microwave irradiation under argon, hydrogen predominates in the gas. In the CO2 atmosphere, dry reforming takes place to give syngas with the CO/H2 ratio of 0.9. In both cases, the degree of hydrogen recovery from lignin reaches 90-94%. [Figure not available: see fulltext.

Microwave-assisted synthesis of palladium nanoparticles intercalated nitrogen doped reduced graphene oxide and their electrocatalytic activity for direct-ethanol fuel cells.

PubMed

Kumar, Rajesh; da Silva, Everson T S G; Singh, Rajesh K; Savu, Raluca; Alaferdov, Andrei V; Fonseca, Leandro C; Carossi, Lory C; Singh, Arvind; Khandka, Sarita; Kar, Kamal K; Alves, Oswaldo L; Kubota, Lauro T; Moshkalev, Stanislav A

2018-04-01

Palladium nanoparticles decorated reduced graphene oxide (Pd-rGO) and palladium nanoparticles intercalated inside nitrogen doped reduced graphene oxide (Pd-NrGO) hybrids have been synthesized by applying a very simple, fast and economic route using microwave-assisted in-situ reduction and exfoliation method. The Pd-NrGO hybrids materials show good activity as catalyst for ethanol electro oxidation for direct ethanol fuel cells (DEFCs) as compared to Pd-rGO hybrids. The enhanced direct ethanol fuel cell can serve as alternative to fossil fuels because it is renewable and environmentally-friendly with a high energy conversion efficiency and low pollutant emission. As proof of concept, the electrocatalytic activity of Pd-NrGO hybrid material was accessed by cyclic voltammetry in presence of ethanol to evaluate its applicability in direct-ethanol fuel cells (DEFCs). The Pd-NrGO catalyst presented higher electro active surface area (∼6.3 m 2  g -1 ) for ethanol electro-oxidation when compared to Pd-rGO hybrids (∼3.7 m 2  g -1 ). Despite the smaller catalytic activity of Pd-NrGO, which was attributed to the lower exfoliation rate of this material in relation to the Pd-rGO, Pd-NrGO showed to be very promising and its catalytic activity can be further improved by tuning the synthesis parameters to increase the exfoliation rate. Copyright © 2018 Elsevier Inc. All rights reserved.

Microwave-assisted synthesis of graphene modified CuO nanoparticles for voltammetric enzyme-free sensing of glucose at biological pH values.

PubMed

Foroughi, Faranak; Rahsepar, Mansour; Hadianfard, Mohammad Jafar; Kim, Hasuck

2017-12-18

The effect of graphene nanosheets on the glucose sensing performance of CuO powders was investigated. CuO and graphene-modified CuO nanoparticles (NPs) were fabricated by microwave-assisted synthesis and characterized by X-ray diffraction, transmission electron microscopy and X-ray photoelectron spectroscopy. The material was placed on a glassy carbon electrode (GCE) which then was characterized by cyclic voltammetry and chronoamperometry with respect to the capability of sensing glucose both at pH 13 and pH 7.4. The results revealed that the modified GCE has a fast and selective linear response to glucose at pH 13 that covers the 0.21 μM to 12 mM concentration range, with a 0.21 μM low detection limit. The presence of graphene nanosheets results in an improved sensitivity which is to 700 μA mM -1  cm -2 . In solution of pH 7.4, the respective data are a linear analytical range from 5 to 14 mM; a 5 μM LOD and a sensitivity of 37.63 μA mM -1  cm -2 at working potential of -0.05 V (vs. Ag/AgCl) and scan rate of 50 mV s -1 . Ascorbic acid, dopamine, uric acid, sucrose, maltose and fructose do not interfere. Graphical abstract ᅟ.

Recent developments on ultrasound-assisted one-pot multicomponent synthesis of biologically relevant heterocycles.

PubMed

Banerjee, Bubun

2017-03-01

Heterocycles are the backbone of organic compounds. Specially, N- &O-containing heterocycles represent privileged structural subunits well distributed in naturally occurring compounds with immense biological activities. Multicomponent reactions (MCRs) are becoming valuable tool for synthesizing structurally diverse molecular entities. On the other hand, the last decade has seen a tremendous outburst in modifying chemical processes to make them sustainable for the betterment of our environment. The application of ultrasound in organic synthesis is fulfilling some of the goals of 'green and sustainable chemistry' as it has some advantages over the traditional thermal methods in terms of reaction rates, yields, purity of the products, product selectivity, etc. Therefore the synthesis of biologically relevant heterocycles using one-pot multi-component technique coupled with the application of ultrasound is one of the thrusting areas in the 21st Century among the organic chemists. The present review deals with the "up to date" developments on ultrasound assisted one-pot multi-component synthesis of biologically relevant heterocycles reported so far. Copyright © 2016 Elsevier B.V. All rights reserved.

Recent Advances in the Synthesis and Stabilization of Nickel and Nickel Oxide Nanoparticles: A Green Adeptness

PubMed Central

Rani, Aneela

2016-01-01

Green protocols for the synthesis of nanoparticles have been attracting a lot of attention because they are eco-friendly, rapid, and cost-effective. Nickel and nickel oxide nanoparticles have been synthesized by green routes and characterized for impact of green chemistry on the properties and biological effects of nanoparticles in the last five years. Green synthesis, properties, and applications of nickel and nickel oxide nanoparticles have been reported in the literature. This review summarizes the synthesis of nickel and nickel oxide nanoparticles using different biological systems. This review also provides comparative overview of influence of chemical synthesis and green synthesis on structural properties of nickel and nickel oxide nanoparticles and their biological behavior. It concludes that green methods for synthesis of nickel and nickel oxide nanoparticles are better than chemical synthetic methods. PMID:27413375

Solid state green synthesis and catalytic activity of CuO nanorods in thermal decomposition of potassium periodate

NASA Astrophysics Data System (ADS)

Patel, Vinay Kumar; Bhattacharya, Shantanu

2017-09-01

The present study reports a facile solid state green synthesis process using the leaf extracts of Hibiscus rosa-sinensis to synthesize CuO nanorods with average diameters of 15-20 nm and lengths up to 100 nm. The as-synthesized CuO nanorods were characterized by x-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and selected area electron diffraction. The formation mechanism of CuO nanorods has been explained by involving the individual role of amide I (amino groups) and carboxylate groups under excess hydroxyl ions released from NaOH. The catalytic activity of CuO nanorods in thermal decomposition of potassium periodate microparticles (µ-KIO4) microparticles was studied by thermo gravimetric analysis measurement. The original size (~100 µm) of commercially procured potassium periodate was reduced to microscale length scale to about one-tenth by PEG200 assisted emulsion process. The CuO nanorods prepared by solid state green route were found to catalyze the thermal decomposition of µ-KIO4 with a reduction of 18 °C in the final thermal decomposition temperature of potassium periodate.

Study on Suitable Light Conditions and Efficient Lipid Extraction Technologies for Biodiesel Production Based on Microalgae

NASA Astrophysics Data System (ADS)

Wang, Yao; Zhang, Qingtao; Sun, Yuan; Yang, Chengjia

2018-01-01

As a new generation biodiesel feedstock, microalgae have most potential to replace fossil fuel. However, the limited scale and high cost are two bottleneck problems. Efficient microwave-assisted lipid extraction technologies and suitable light conditions for Chlorella Sorokiniana need further study for lowering the cost. In this study, three photoperiod groups(24L:0D, 12L:12D, 0L:24D), three illumination intensity groups (1800 lux, 3600 lux, 5400 lux)and four light spectrum groups (Red, green, blue, and white) were used to culture Chlorella Sorokiniana to investigate those effects on algae growth rate and biomass accumulation. The suitable microwave treatment was also studied to achieve an optimizing quantum fracturing technology. 400 w, 750 w and 1000 w microwave power were set and 60 °C, 75 °C, 90 °C microwave conditions were investigated. The results showed that Chlorella Sorokiniana under 24L:0D photoperiod with 5400 lux white light can achieve better growth rate. The 90 °C / 1000w microwave treatment was identified as the most simple, easy, and effective way for lipid extraction from Chlorella Sorokiniana. As the raw material of biodiesel production, C18:1, C18:2 and C18:3 have accounted for important components of fatty acid in Chlorella Sorokiniana. Therefore, Chlorella Sorokiniana is a good raw material for the production of good quality biodiesel under suitable and efficient technologies.

Production of xylooligosaccharide from wheat bran by microwave assisted enzymatic hydrolysis.

PubMed

Wang, Tseng-Hsing; Lu, Shin

2013-06-01

The effective production of xylooligosaccharides (XOS) from wheat bran was investigated. Wheat bran contains rich hemicellulose which can be hydrolyzed by enzyme; the XOS were obtained by microwave assisted enzymatic hydrolysis. To improve the productivity of XOS, repeated microwave assisted enzymatic hydrolysis and activated carbon adsorption method was chosen to eliminate macromolecules in the XOS. On the basis of experimental data, an industrial XOS production process consisting of pretreatment, repeated microwave assisted enzymatic treatment and purification was designed. Using the designed process, 3.2g dry of purified XOS was produced from 50 g dry wheat bran powder. Copyright © 2012 Elsevier Ltd. All rights reserved.

Continuous microwave flow synthesis of mesoporous hydroxyapatite.

PubMed

Akram, Muhammad; Alshemary, Ammar Z; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O; Hussain, Rafaqat

2015-11-01

We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution. Copyright © 2015 Elsevier B.V. All rights reserved.

Microwave Assisted Synthesis, Physicochemical, Photophysical, Single Crystal X-ray and DFT Studies of Novel Push-Pull Chromophores.

PubMed

Khan, Salman A; Asiri, Abdullah M; Basisi, Hadi Mussa; Arshad, Muhammad Nadeem; Sharma, Kamlesh

2015-11-01

Two push-pull chromophores were synthesized by knoevenagel condensation under microwave irradiation. The structure of synthesized chromophores were established by spectroscopic (FT-IR, (1)H NMR, (13)C NMR, EI-MS) and elemental analysis. Structure of the chromophores was further conformed by X-ray crystallographic. UV-Vis and fluorescence spectroscopy measurements provided that chromophores were good absorbent and fluorescent properties. Fluorescence polarity studies demonstrated that chromophores were sensitive to the polarity of the microenvironment provided by different solvents. Physicochemical parameters, including singlet absorption, extinction coefficient, stokes shift, oscillator strength, dipole moment and flurescence quantum yield were investigated in order to explore the analytical potential of the synthesized chromophores. In addition, the total energy, frontier molecular orbitals, hardness, electron affinity, ionization energy, electrostatic potential map were also studied computationally by using density functional theoretical method.

An Efficient, Eco-friendly and Sustainable One-Pot Synthesis of 3,4-Dihydropyrimidin-2(1H)-ones Directly from Alcohols Catalyzed by Heteropolyanion-Based Ionic Liquids.

PubMed

Fu, Renzhong; Yang, Yang; Ma, Xudong; Sun, Yu; Li, Jin; Gao, Hang; Hu, Huaxing; Zeng, Xiaojun; Yi, Jun

2017-09-11

Efficient, eco-friendly and sustainable access to 3,4-dihydropyrimidin-2(1 H )-ones directly from alcohols under microwave and solvent-free conditions has been reported. The practical protocol involves heteropolyanion-based catalyzed oxidation of alcohols to aldehydes with NaNO₃ as the oxidant followed by cyclocondensation with dicarbonyl compounds and urea or thiourea in a two-step, one-pot manner. Compatibility with different functional groups, good to excellent yields and reusable catalysts are the main highlights. The utilization of alcohols instead of aldehydes is a valid and green alternative to the classical Biginelli reaction.

Synthesis and Spectral Evaluation of Some Unsymmetrical Mesoporphyrinic Complexes

PubMed Central

Boscencu, Rica; Oliveira, Anabela Sousa; Ferreira, Diana P.; Ferreira, Luís Filipe Vieira

2012-01-01

Synthesis and spectral evaluation of new zinc and copper unsymmetrical mesoporphyrinic complexes are reported. Zn(II)-5-(4-acetoxy-3-methoxyphenyl)-10,15,20- tris-(4-carboxymethylphenyl)porphyrin, Zn(II)-5-[(3,4-methylenedioxy)phenyl]-10,15,20- tris-(4-carboxymethylphenyl)porphyrin, Cu(II)-5-(4-acetoxy-3-methoxyphenyl)-10,15,20- tris-(4-carboxymethylphenyl)porphyrin and Cu(II)-5-[(3,4-methylenedioxy)phenyl]-10,15,20- tris-(4-carboxymethylphenyl)porphyrin were synthesized using microwave-assisted synthesis. The complexes were characterized by elemental analysis, FT-IR, UV-Vis, EPR and NMR spectroscopy, which fully confirmed their structure. The spectral absorption properties of the porphyrinic complexes were studied in solvents with different polarities. Fluorescence emission and singlet oxygen formation quantum yields were evaluated for the compounds under study, revealing high yields for the zinc derivatives. The copper complexes are not emissive and only display residual capacity for singlet oxygen formation. PMID:22942693

Advances in nanosized zeolites

NASA Astrophysics Data System (ADS)

Mintova, Svetlana; Gilson, Jean-Pierre; Valtchev, Valentin

2013-07-01

This review highlights recent developments in the synthesis of nanosized zeolites. The strategies available for their preparation (organic-template assisted, organic-template free, and alternative procedures) are discussed. Major breakthroughs achieved by the so-called zeolite crystal engineering and encompass items such as mastering and using the physicochemical properties of the precursor synthesis gel/suspension, optimizing the use of silicon and aluminium precursor sources, the rational use of organic templates and structure-directing inorganic cations, and careful adjustment of synthesis conditions (temperature, pressure, time, heating processes from conventional to microwave and sonication) are addressed. An on-going broad and deep fundamental understanding of the crystallization process, explaining the influence of all variables of this complex set of reactions, underpins an even more rational design of nanosized zeolites with exceptional properties. Finally, the advantages and limitations of these methods are addressed with particular attention to their industrial prospects and utilization in existing and advanced applications.

New microwave-integrated Soxhlet extraction. An advantageous tool for the extraction of lipids from food products.

PubMed

Virot, Matthieu; Tomao, Valérie; Colnagui, Giulio; Visinoni, Franco; Chemat, Farid

2007-12-07

A new process of Soxhlet extraction assisted by microwave was designed and developed. The process is performed in four steps, which ensures complete, rapid and accurate extraction of the samples. A second-order central composite design (CCD) has been used to investigate the performance of the new device. The results provided by analysis of variance and Pareto chart, indicated that the extraction time was the most important factor followed by the leaching time. The response surface methodology allowed us to determine optimal conditions for olive oil extraction: 13 min of extraction time, 17 min of leaching time, and 720 W of irradiation power. The proposed process is suitable for lipids determination from food. Microwave-integrated Soxhlet (MIS) extraction has been compared with a conventional technique, Soxhlet extraction, for the extraction of oil from olives (Aglandau, Vaucluse, France). The oils extracted by MIS for 32 min were quantitatively (yield) and qualitatively (fatty acid composition) similar to those obtained by conventional Soxhlet extraction for 8 h. MIS is a green technology and appears as a good alternative for the extraction of fat and oils from food products.

Optimization and stabilization of gold nanoparticles by using herbal plant extract with microwave heating

NASA Astrophysics Data System (ADS)

Yasmin, Akbar; Ramesh, Kumaraswamy; Rajeshkumar, Shanmugam

2014-04-01

In this study, we have synthesized the gold nanoparticles by using Hibiscus rosa-sinensis, a medicinal plant. The gold nanoparticles were synthesized rapidly by the involvement of microwave heating. By changing of plant extract concentration, gold solution concentration, microwave heating time and power of microwave heating the optimized condition was identified. The surface Plasmon resonance found at 520 nm confirmed the gold nanoparticles synthesis. The spherical sized nanoparticles in the size range of 16-30 nm were confirmed by Transmission Electron Microscope (TEM). The stability of the nanoparticles is very well proved in the invitro stability tests. The biochemical like alkaloids and flavonoids play a vital role in the nanoparticles synthesis was identified using the Fourier Transform Infrared Spectroscopy (FTIR). Combining the phytochemical and microwave heating, the rapid synthesis of gold nanoparticles is the novel process for the medically applicable gold nanoparticles production.

Ball Milling Assisted Solvent and Catalyst Free Synthesis of Benzimidazoles and Their Derivatives.

PubMed

El-Sayed, Taghreed H; Aboelnaga, Asmaa; Hagar, Mohamed

2016-08-24

Benzoic acid and o-phenylenediamine efficiently reacted under the green solvent-free Ball Milling method. Several reaction parameters were investigated such as rotation frequency; milling balls weight and milling time. The optimum reaction condition was milling with 56.6 g weight of balls at 20 Hz frequency for one hour milling time. The study was extended for synthesis of a series of benzimidazol-2-one or benzimidazol-2-thione using different aldehydes; carboxylic acids; urea; thiourea or ammonium thiocyanate with o-phenylenediamine. Moreover; the alkylation of benzimidazolone or benzimidazolthione using ethyl chloroacetate was also studied.

Recent advances in nanoscale-metal assisted biochar derived from waste biomass used for heavy metals removal.

PubMed

Ho, Shih-Hsin; Zhu, Shishu; Chang, Jo-Shu

2017-12-01

Pollution of heavy metals (HMs) is a detrimental treat to human health and need to be cleaned up in a proper way. Biochar (BC), a low-cost and "green" adsorbent, has attracted significant attention due to its considerable HMs removal capacity. In particular, nano-metals have recently been used to assist BC in improving its reactivity, surface texture and magnetism. Synthesis methods and metal precursors greatly influence the properties and structures of the nanocomposites, thereby affecting their HMs removal performance. This review presents advances in synthesis methods, formation mechanisms and surface characteristics of BC nanocomposites, along with the discussions on HMs removal mechanisms and the effects of environmental factors on HMs removal efficiency. Performance of using BC nanocomposites to remediate real HMs-containing wastewater and issues associated with its process scale-up are also discussed. This review aims to provide useful information to facilitate the development of HMs removal by nanoscale-metal assisted BC. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microwave-Assisted Synthesis of Silver Vanadium Phosphorus Oxide, Ag 2VO 2PO 4 : Crystallite Size Control and Impact on Electrochemistry

DOE PAGES

Huang, Jianping; Marschilok, Amy C.; Takeuchi, Esther S.; ...

2016-03-07

We study silver vanadium phosphorus oxide, Ag 2VO 2PO 4, that is a promising cathode material for Li batteries due in part to its large capacity and high current capability. Herein, a new synthesis of Ag 2VO 2PO 4 based on microwave heating is presented, where the reaction time is reduced by approximately 100× relative to other reported methods, and the crystallite size is controlled via synthesis temperature, showing a linear correlation of crystallite size with temperature. Notably, under galvanostatic reduction, the Ag 2VO 2PO 4 sample with the smallest crystallite size delivers the highest capacity and shows the highestmore » loaded voltage. Further, pulse discharge tests show a significant resistance decrease during the initial discharge coincident with the formation of Ag metal. Thus, the magnitude of the resistance decrease observed during pulse tests depends on the Ag 2VO 2PO 4 crystallite size, with the largest resistance decrease observed for the smallest crystallite size. Additional electrochemical measurements indicate a quasi-reversible redox reaction involving Li + insertion/deinsertion, with capacity fade due to structural changes associated with the discharge/charge process. In summary, this work demonstrates a faster synthetic approach for bimetallic polyanionic materials which also provides the opportunity for tuning of electrochemical properties through control of material physical properties such as crystallite size.« less

Microwave-Assisted Ignition for Improved Internal Combustion Engine Efficiency

NASA Astrophysics Data System (ADS)

DeFilippo, Anthony Cesar

The ever-present need for reducing greenhouse gas emissions associated with transportation motivates this investigation of a novel ignition technology for internal combustion engine applications. Advanced engines can achieve higher efficiencies and reduced emissions by operating in regimes with diluted fuel-air mixtures and higher compression ratios, but the range of stable engine operation is constrained by combustion initiation and flame propagation when dilution levels are high. An advanced ignition technology that reliably extends the operating range of internal combustion engines will aid practical implementation of the next generation of high-efficiency engines. This dissertation contributes to next-generation ignition technology advancement by experimentally analyzing a prototype technology as well as developing a numerical model for the chemical processes governing microwave-assisted ignition. The microwave-assisted spark plug under development by Imagineering, Inc. of Japan has previously been shown to expand the stable operating range of gasoline-fueled engines through plasma-assisted combustion, but the factors limiting its operation were not well characterized. The present experimental study has two main goals. The first goal is to investigate the capability of the microwave-assisted spark plug towards expanding the stable operating range of wet-ethanol-fueled engines. The stability range is investigated by examining the coefficient of variation of indicated mean effective pressure as a metric for instability, and indicated specific ethanol consumption as a metric for efficiency. The second goal is to examine the factors affecting the extent to which microwaves enhance ignition processes. The factors impacting microwave enhancement of ignition processes are individually examined, using flame development behavior as a key metric in determining microwave effectiveness. Further development of practical combustion applications implementing microwave-assisted spark technology will benefit from predictive models which include the plasma processes governing the observed combustion enhancement. This dissertation documents the development of a chemical kinetic mechanism for the plasma-assisted combustion processes relevant to microwave-assisted spark ignition. The mechanism includes an existing mechanism for gas-phase methane oxidation, supplemented with electron impact reactions, cation and anion chemical reactions, and reactions involving vibrationally-excited and electronically-excited species. Calculations using the presently-developed numerical model explain experimentally-observed trends, highlighting the relative importance of pressure, temperature, and mixture composition in determining the effectiveness of microwave-assisted ignition enhancement.

Closed vessel miniaturized microwave assisted chelating extraction for determination of trace metals in plant materials

NASA Astrophysics Data System (ADS)

Czarnecki, Sezin; Duering, Rolf-Alexander

2013-04-01

In recent years, the use of closed vessel microwave assisted extraction (MAE) for plant samples has shown increasing research interest which will probably substitute conventional procedures in the future due to their general disadvantages including consumption of time and solvents. The objective of this study was to demonstrate an innovative miniaturized closed vessel microwave assisted extraction (µMAE) method under the use of EDTA (µMAE-EDTA) to determine metal contents (Cd, Co, Cu, Mn, Ni, Pb, Zn) in plant samples (Lolio-Cynosuretum) by inductively coupled plasma-optical emission spectrometry (ICP-OES). Validation of the method was done by comparison of the results with another miniaturized closed vessel microwave HNO3 method (µMAE-H) and with two other macro scale MAE procedures (MAE-H and MAE-EDTA) which were applied by using a mixture of nitric acid (HNO3) and hydrogen peroxide (H2O2) (MAE-H) and EDTA (MAE-EDTA), respectively. The already established MAE-H method is taken into consideration as a reference validation MAE method for plant material. A conventional plant extraction (CE) method, based on dry ashing and dissolving of the plant material in HNO3, was used as a confidence comparative method. Certified plant reference materials (CRMs) were used for comparison of recovery rates from different extraction protocols. This allowed the validation of the applicability of the µMAE-EDTA procedure. For 36 real plant samples with triplicates each, µMAE-EDTA showed the same extraction yields as the MAE-H in the determination of Cd, Co, Cu, Mn, Ni, Pb, and Zn contents in plant samples. Analytical parameters in µMAE-EDTA should be further investigated and adapted for other metals of interest. By the reduction and elimination of the use of hazardous chemicals in environmental analysis and thus allowing a better understanding of metal distribution and accumulation process in plants and also the metal transfer from soil to plants and into the food chain, µMAE-EDTA is seen as a promising technique for achieving green chemistry goals.

DIRECT SYNTHESIS OF TERTIARY AMINES IN WATER USING MICROWAVES

EPA Science Inventory

A direct synthesis of tertiary amines is presented that proceeds expeditiously via N-alkylation of amines using alkyl halides in alkaline aqueous medium. This environmentally benign reaction is accelerated upon exposure to microwave irradiation resulting in shortened reaction tim...

Optimization of enzymes-microwave-ultrasound assisted extraction of Lentinus edodes polysaccharides and determination of its antioxidant activity.

PubMed

Yin, Chaomin; Fan, Xiuzhi; Fan, Zhe; Shi, Defang; Gao, Hong

2018-05-01

Enzymes-microwave-ultrasound assisted extraction (EMUE) method had been used to extract Lentinus edodes polysaccharides (LEPs). The enzymatic temperature, enzymatic pH, microwave power and microwave time were optimized by response surface methodology. The yields, properties and antioxidant activities of LEPs from EMUE and other extraction methods including hot-water extraction, enzymes-assisted extraction, microwave-assisted extraction and ultrasound-assisted extraction were evaluated. The results showed that the highest LEPs yield of 9.38% was achieved with enzymatic temperature of 48°C, enzymatic pH of 5.0, microwave power of 440W and microwave time of 10min, which correlated well with the predicted value of 9.79%. Additionally, LEPs from different extraction methods possessed typical absorption peak of polysaccharides, which meant different extraction methods had no significant effects on type of glycosidic bonds and sugar ring of LEPs. However, SEM images of LEPs from different extraction methods were significantly different. Moreover, the different LEPs all showed antioxidant activities, but LEPs from EMUE showed the highest reducing power when compared to other LEPs. The results indicated LEPs from EMUE can be used as natural antioxidant component in the pharmaceutical and functional food industries. Copyright © 2018 Elsevier B.V. All rights reserved.

Microwave-Assisted Size Control of Colloidal Nickel Nanocrystals for Colloidal Nanocrystals-Based Non-volatile Memory Devices

NASA Astrophysics Data System (ADS)

Yadav, Manoj; Velampati, Ravi Shankar R.; Mandal, D.; Sharma, Rohit

2018-03-01

Colloidal synthesis and size control of nickel (Ni) nanocrystals (NCs) below 10 nm are reported using a microwave synthesis method. The synthesised colloidal NCs have been characterized using x-ray diffraction, transmission electron microscopy (TEM) and dynamic light scattering (DLS). XRD analysis highlights the face centred cubic crystal structure of synthesised NCs. The size of NCs observed using TEM and DLS have a distribution between 2.6 nm and 10 nm. Furthermore, atomic force microscopy analysis of spin-coated NCs over a silicon dioxide surface has been carried out to identify an optimum spin condition that can be used for the fabrication of a metal oxide semiconductor (MOS) non-volatile memory (NVM) capacitor. Subsequently, the fabrication of a MOS NVM capacitor is reported to demonstrate the potential application of colloidal synthesized Ni NCs in NVM devices. We also report the capacitance-voltage (C-V) and capacitance-time (C-t) response of the fabricated MOS NVM capacitor. The C-V and C-t characteristics depict a large flat band voltage shift (V FB) and high retention time, respectively, which indicate that colloidal Ni NCs are excellent candidates for applications in next-generation NVM devices.