• Title/Summary/Keyword: Microwave synthesis

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Clean and Efficient Synthesis of Furfural From Xylose by Microwave-Assisted Biphasic System using Bio-Based Heterogeneous Acid Catalysts

  • Vo, Anh Thi Hoang;Lee, Hong-shik;Kim, Sangyong;Cho, Jin Ku
    • Clean Technology
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    • v.22 no.4
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    • pp.250-257
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    • 2016
  • As an attempt to replacing petroleum-based chemicals with bio-based ones, synthesis of furfural from biomass-derived xylose attracts much attention in recent days. Conventionally, furfural from xylose has been produced via the utilization of highly corrosive, toxic, and environmentally unfriendly mineral acids such as sulfuric acid or hydrochloric acid. In this study, microwave-assisted biphasic reaction process in the presence of novel bio-based heterogeneous acid catalysts was developed for the eco-benign and effective synthesis of furfural from xylose. The microwave was irradiated for reaction acceleration and a biphasic system consisting of $H_2O$ : MIBK (1 : 2) was designed for continuous extraction of furfural into the organic phase in order to reduce the undesired side products formed by decomposition/condensation/oligomerization in the acidic aqueous phase. Moreover, sulfonated amorphous carbonaceous materials were prepared from wood powder, the most abundant lignocellulosic biomass. The prepared catalysts were characterized by FT-IR, XPS, BET, elemental analysis and they were used as bio-based heterogeneous acid catalysts for the dehydration of xylose into furfural more effectively. For further optimization, the effect of temperature, reaction time, water/organic solvent ratio, and substrate/catalyst ratio on the xylose conversion and furfural yield were investigated and 100% conversion of xylose and 74% yield of furfural was achieved within 5 h at $180^{\circ}C$. The bio-based heterogeneous acid catalysts could be used three times without any significant loss of activity. This greener protocol provides highly selective conversion of xylose to furfural as well as facile isolation of product and bio-based heterogeneous acid catalysts can alternate the environmentally-burdened mineral acids.

Recent Progress on Metal-Organic Framework Membranes for Gas Separations: Conventional Synthesis vs. Microwave-Assisted Synthesis (기체분리용 금속유기구조체 분리막의 최근 연구 동향 및 성과)

  • Ramu, Gokulakrishnan;Jeong, Hae-Kwon
    • Membrane Journal
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    • v.27 no.1
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    • pp.1-42
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    • 2017
  • Metal-organic frameworks (MOFs) are nanoporous materials that consist of organic and inorganic moieties, with well-defined crystalline lattices and pore structures. With a judicious choice of organic linkers present in the MOFs with different sizes and chemical groups, MOFs exhibit a wide variety of pore sizes and chemical/physical properties. This makes MOFs extremely attractive as novel membrane materials for gas separation applications. However, the synthesis of high-quality MOF thin films and membranes is quite challenging due to difficulties in controlling the heterogeneous nucleation/growth and achieving strong attachment of films on porous supports. Microwave-based synthesis technology has made tremendous progress in the last two decades and has been utilized to overcome some of these challenges associated with MOF membrane fabrication. The advantages of microwaves as opposed to conventional synthesis techniques for MOFs include shorter synthesis times, ability to achieve unique and complex structures and crystal size reductions. Here, we review the recent progress on the synthesis of MOF thin films and membranes with an emphasis on how microwaves have been utilized in the synthesis, improved properties achieved and gas separation performance of these films and membranes.

Syntheses of FAPO-5 Molecular Sieves with Microwave Irradiation and Their Characterization (마이크로파 가열에 의한 FAPO-5 분자체의 합성 및 특성 분석)

  • Jang, Jong-San;Lee, Jin-Ho;Jeong, Seong-Hwa;Hwang, Jin-Su
    • Journal of the Korean Chemical Society
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    • v.50 no.1
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    • pp.53-59
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    • 2006
  • .FAPO-5 molecular sieves were synthesized starting from the same reactant gel at 170 oC using microwave irradiation technique and conventional hydrothermal reaction. The FAPO-5 molecular sieves were characterized by several techniques such as SEM, FTIR, UV/Vis, and ESR. Moreover, the oxidation of styrene over FAPO-5s was carried out, and compared to check the oxidation and epoxidation ability of the two FAPO-5s. FAPO-5 can be obtained easily by microwave irradiation within 15 min at 170oC, whereas FAPO-5 synthesis is completed in 6 h by conventional electric heating, confirming the acceleration about 20 times by microwave technique. There are no appreciable differences between two FAPO-5s in surface area and coordination state of iron. The FAPO-5 synthesized by microwave irradiation shows higher epoxide selectivity in the styrene epoxidation, which may be explained by the higher hydrophobicity of the catalyst.

Microwave-Assisted and Conventional Synthesis of Benzothieno [3,2-e] [1,3,4] triazolo[4,3-c]pyrimidines: A Comparative Study

  • Gaonkar, Santhosh L.;Ahn, Chuljin;Princia, Princia;Shetty, Nitinkumar S.
    • Journal of the Korean Chemical Society
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    • v.58 no.4
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    • pp.388-392
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    • 2014
  • Benzothieno[2,3-d]pyrimidines (2,3,4) and benzothieno[3,2-e][1,3,4]triazolo[4,3-c] pyrimidines (5a-c) were synthesized from the precursor 2-amino-7-oxo-4,5,6,7-tetrahydro-1-benzothiophene-3-carbonitrile 1 by employing the conventional method as well as the microwave irradiation technique. The precursor 2-amino-3-cyanothiophene analogue 1 was synthesized by employing the well-known Gewald reaction. In the present work it has been found that the microwave supported syntheses are more efficient than the conventional classical heating methods. The structures of all the compounds were ascertained by spectral and analytical data.

Heat treatment effect on synthesis of mesoporous silica (Mesoporous Silica의 제조에 열처리가 끼치는 영향)

  • Park, Kyu-Sung;Kim, Duk-Su;Kim, Il-Doo;Kim, Ho-Gi
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.07b
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    • pp.1113-1115
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    • 2002
  • Mesoporous silica, MCM-41, was synthesized by sol-gel method. The organic structure-directing agent must be removed to make the desired proes. To achieve this, alternative calcination method using microwave oven was adapted to this removal stage. Microwave calcination was shown to provide a novel, rapid and inexpensive method of praparing nanoporous material. It was studied how the porous structure, surface area and pore size distribution were changes under microwave calcination.

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Microwave Hydrothermal Sythesis of PbTiO$_3$ and PMN Ceramic Powders (마이크로파 수열법에 의한 PbTiO$_3$ PMN 세라믹분말의 합성)

  • Bai, Kang
    • Journal of the Korean Ceramic Society
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    • v.35 no.5
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    • pp.465-471
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    • 1998
  • Lead titanate(PT) and lead magnesium niobate(PMN) ceramic powders were prepared by microwave hy-drothermal method using teflon bomb. Raw materials were Pb(NO3)2 and TiO2 for lead titanate and Pb(NO3)2 Nb2O5 and Mg(NO)3.6H2O for PMN with NaOH as mineralizer in both cases. in lead titanate synthsis rate of microwave hydrothermal method was faster three times than one f conventional hydrothermal methods In lead magnesium niobate synthsis the mixture of perovskite and pyrochlore phases was obtained by single step technique and the PMN was not obtained by double step technique due to low temperature limitation of teflon bomb.

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