• Title/Summary/Keyword: Heterogeneous Reaction

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Preparation, Characterization and First Application of Aerosil Silica Supported Acidic Ionic Liquid as a Reusable Heterogeneous Catalyst for the Synthesis of 2,3-Dihydroquinazolin-4(1H)-ones

  • Yassaghi, Ghazaleh;Davoodnia, Abolghasem;Allameh, Sadegh;Zare-Bidaki, Atefeh;Tavakoli-Hoseini, Niloofar
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2724-2730
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    • 2012
  • A new heterogeneous acidic catalyst was successfully prepared by impregnation of silica (Aerosil 300) by an acidic ionic liquid, named 1-(4-sulfonic acid)butylpyridinium hydrogen sulfate [$PYC_4SO_3H$][$HSO_4$], and characterized using FT-IR spectroscopy, the $N_2$ adsorption/desorption analysis (BET), thermal analysis (TG/DTG), and X-ray diffraction (XRD) techniques. The amount of loaded acidic ionic liquid on Aerosil 300 support was determined by acid-base titration. This new solid acidic supported heterogeneous catalyst exhibits excellent activity in the synthesis of 2-aryl-2,3-dihydroquinazolin-4(1H)-ones by cyclocondensation reaction of 2-aminobenzamide with aromatic aldehydes under solvent-free conditions and the desired products were obtained in very short reaction times with high yields. This catalyst has the advantages of an easy catalyst separation from the reaction medium and lower problems of corrosion. Recycling of the catalyst and avoidance of using harmful organic solvent are other advantages of this simple procedure.

Experimental Study for the Identification of the Nascent Product of OH Heterogeneous Reaction with NaCl using Chemical Ionization Mass Spectrometry

  • Park, Jong-Ho;Ivanov, Andrey V.;Molina, Mario J.
    • Mass Spectrometry Letters
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    • v.3 no.4
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    • pp.108-111
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    • 2012
  • An experimental study on the nascent product of the OH heterogeneous reaction with NaCl was performed under dry and wet conditions using a bead-filled flow tube system coupled to a high-pressure chemical ionization mass spectrometer. The ozone concentration in the flow tube for the atomic hydrogen removal was varied in order to control the conversion reaction of molecular chlorine into HCl for the identification of the nascent product. The mass spectrometric observation was that the $O_3$ introduction reduced the concentration HCl, while it increased the concentration of $Cl_2$ and ClO. Based on the experimental results, we suggest that the nascent product of the titled reaction is gaseous $Cl_2$, which is followed by fast conversion into HCl in presence of H. No significant difference in the concentration profile between under dry and wet (RH = 2%) conditions was observed.

Montmorillonite K-10 Clay as an Efficient Reusable Heterogeneous Catalyst for the Solvent-Free Microwave Mediated Synthesis of 5-Substituted 1H-Tetrazoles

  • Marvi, Omid;Alizadeh, Abdolhamid;Zarrabi, Saeid
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.4001-4004
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    • 2011
  • Various 5-substituted 1H-tetrazole derivatives were synthesized in a simple and environmentally benign method from the reaction of aryl and benzyl nitriles with sodium azide in solvent-free media using montmorillonite K-10 clay as solid recyclable heterogeneous acidic catalyst and microwave irradiation in good yields and short reaction times.

Montmorillonite KSF Clay as Novel and Recyclable Heterogeneous Catalyst for the Microwave Mediated Synthesis of Indan-1,3-Diones

  • Marvi, Omid;Giahi, Masoud
    • Bulletin of the Korean Chemical Society
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    • v.30 no.12
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    • pp.2918-2920
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    • 2009
  • Various indan-1,3-dione derivatives were synthesized from the reaction of different phthalic anhydrides with diethylmalonate using montmorillonite KSF clay as a recyclable heterogeneous acidic catalyst and microwave irradiation in good yields and short reaction times.

Heterogeneous Suzuki Cross-Coupling Reaction Catalyzed by Magnetically Recyclable Nanocatalyst

  • Choi, Kwang-Hyun;Shokouhimehr, Mohammadreza;Sung, Yung-Eun
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1477-1480
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    • 2013
  • The Suzuki cross-coupling reactions proceeded in excellent yields when it was catalyzed by magnetically recyclable nanocatalyst. This nanocatalyst provided very high catalytic activity with low loading level (1 mol %), because the palladium nanoparticles were so small in size (~2 nm) and located on the surface of the nanocomposite. It was also easily recovered from the reaction mixture using a magnet and reused for six consecutive cycles.

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.

Production of Methyl Ester from Coconut Oil using Microwave: Kinetic of Transesterification Reaction using Heterogeneous CaO Catalyst

  • Mahfud, Mahfud;Suryanto, Andi;Qadariyah, Lailatul;Suprapto, Suprapto;Kusuma, Heri Septya
    • Korean Chemical Engineering Research
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    • v.56 no.2
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    • pp.275-280
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    • 2018
  • Methyl ester derived from coconut oil is very interesting to study since it contains free-fatty acid with chemical structure of medium carbon chain ($C_{12}-C_{14}$), so the methyl ester obtained from its part can be a biodiesel and another partially into biokerosene. The use of heterogeneous catalysts in the production of methyl ester requires severe conditions (high pressure and high temperature), while at low temperature and atmospheric conditions, yield of methyl ester is relatively very low. By using microwave irradiation trans-esterification reaction with heterogeneous catalysts, it is expected to be much faster and can give higher yields. Therefore, we studied the production of methyl ester from coconut oil using CaO catalyst assisted by microwave. Our aim was to find a kinetic model of methyl ester production through a transesterification process from coconut oil assisted by microwave using heterogeneous CaO catalyst. The experimental apparatus consisted of a batch reactor placed in a microwave oven equipped with a condenser, stirrer and temperature controllers. Batch process was conducted at atmospheric pressure with a variation of CaO catalyst concentration (0.5; 1.0; 1.5; 2.0, 2.5%) and microwave power (100, 264 and 400 W). In general, the production process of methyl esters by heterogeneous catalyst will obtain three layers, wherein the first layer is the product of methyl ester, the second layer is glycerol and the third layer is the catalyst. The experimental results show that the yield of methyl ester increases along with the increase of microwave power, catalyst concentration and reaction time. Kinetic model of methyl ester production can be represented by the following equation: $-r_{TG}=1.7{\cdot}10^6{_e}{\frac{-43.86}{RT}}C_{TG}$.

Synthesis of Palladium Nanoparticles Encapsulated in Phosphine Ligand-Grafted Mesoporous Silicas and Their Application to Suzuki Cross-Coupling Reaction (팔라듐 나노입자가 담지된 메조포러스 실리카의 제조와 이를 이용한 Suzuki Cross-Coupling 반응의 적용연구)

  • Kim, Sang-Wook;Joo, Jin
    • Clean Technology
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    • v.17 no.1
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    • pp.13-18
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    • 2011
  • Phosphine ligand-grafted mesoporous silica materials with large pores were prepared for the ligand-modified heterogeneous Pd nanocatalysts. New heterogeneous catalytic system was developed using palladium nanoparticles encapsulated in phosphine ligand-grafted mesoporous silica. The catalyst showed good catalytic activities for Suzuki cross-coupling using bromobenzene derivatives due to excellent phosphine ligand effects. Catalytic results showed nanoparticie catalysts can be recycled twice with decreased yields.

Heterogeneous Ignition of $H_2/O_2/CO_2$ Mixture Over Platinum Catalyst (수소/산소/이산화탄소 혼합기의 백금촉매반응특성 : 비균일 반응의 점화 온도)

  • Nam, Chang-Ho;Shin, Hyun-Dong
    • 한국연소학회:학술대회논문집
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    • 2001.11a
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    • pp.90-96
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    • 2001
  • Catalytic ignition of $H_2/O_2/CO_2$ mixtures over platinum catalyst is experimentally investigated by using microcalorimetry. For comparison, $N_2$ and Ar is also used as diluent gas. The gas mixture flows toward platinum foil heated by electric current at atmosphere pressure and ambient temperature. The ignition temperature range 350-445K according to the fuel ratio, dilution ratio and diluent gas. It increases as the fuel ratio and dilution ratio increase. $H_2/O_2$ mixture with $CO_2$ ignites at higher temperature than with other diluents by 30-50K. Several experimental evidences show the inhibition effects of $CO_2$ in $H_2-O_2$ heterogeneous reaction is considerable

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