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Synthesis of isoamyl salicylate using a novel mesoporous titania superacid as a catalyst
Tingshun Jiang,Qian Zhao,Jinyu Chu,Hengbo Yin 한국화학공학회 2008 Korean Journal of Chemical Engineering Vol.25 No.5
Mesoporous titania was prepared by hydrothermal method and mesoporous titania solid superacid catalyst was prepared by wet impregnation method. The structure and property of the as-prepared catalysts were characterized by means of XRD, FT-IR and N2 physical adsorption. Isoamyl salicylate was synthesized by using concentrated sulfuric acid and solid superacid as catalyst, respectively. The effects of the molar ratio of raw material, the amount of catalyst, reaction time and reaction temperature on the yield of the product were systematically investigated. The results show that mesoporous titania solid superacid is a good catalyst for synthesizing isoamyl salicylate. The optimum conditions of isoamyl salicylate synthesized by using mesoporous titania solid superacid are the following: the molar ratio of salicylic acid to isoamyl alcohol is 1 : 4, the quantity of catalyst is 1.6 g, the reaction time is 5 h, the reaction temperature is 130 oC and the yield can reach 94.6%.
許廷順(Xu Tingshun),朴炳仙(Park Byung-seon) 중국어문학연구회 2009 중국어문학논집 Vol.0 No.54
본 연구는 선봉 소설 발전 전후의 당대 소설 언어 변화의 양상을 재정리하기 위한 시도의 일환이다. 전통적인 선봉 소설 언어 혁명이란 표현법에 대한 의문을 제기하였다. 선봉 소설 전기의 언어 혁신은 효과가 있다고 생각했지만 선봉 서설의 경우 실패라고 해도 과언이 아니다. 선봉 소설에 있어서 언어 실험의 실질은 언어 폭동이다. 본문은 “신 시기에 소설 언어 변천의 주요한 힘”, “문학 언어 의식의 각성”, “새로운 문법의 탐색”, “문학 언어의 환경성”, “문학 언어의 문화 내포 의미”, “언어에서 추구한 다원성과 단독성” 등 6대 주제를 중심으로 논술하였다. 선봉 소설의 창작과 연구에서 존재하는 오류에 대한 초보적인 반성도 시도하였다.
Qian Zhao,Tingshun Jiang,Changsheng Li,Hengbo Yin 한국공업화학회 2011 Journal of Industrial and Engineering Chemistry Vol.17 No.2
Ni-loading MCM-41 mesoporous molecular sieve (Ni/MCM-41) and Ni-substituted MCM-41 mesoporous molecular sieve (Ni-MCM-41) were synthesized by wet impregnation method and hydrothermal method, respectively. Their mesoporous structures were evaluated by X-ray diffraction (XRD) and N2physical adsorption technique. Chemical vapor deposition (CVD) was employed to catalytically synthesize carbon nanotubes (CNTs) using Ni-MCM-41 or Ni/MCM-41 as catalyst via pyrolysis of ethanol at atmospheric pressure and 700 8C. The resulting carbon nanotubes were characterized by means of transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM)and Raman spectroscopy, respectively. The results show that the multi-wall carbon nanotubes (MWCNTs) were successfully obtained at 700 8C utilizing NiMCM-41 (or Ni/MCM-41) as a catalytic template by the pyrolysis of ethanol. MWCNTs obtained over Ni-MCM-41 catalyst have uniform diameter and high quality. On the other hand, the technique has great advantages such as low cost and easy operation for the preparation of carbon nanotubes.
Oxidation of cyclopentene catalyzed by tungsten-substituted molybdophosphoric acids
Jinjuan Xue,Haixia Li,Dongzhi Zhang,Tingshun Jiang,Longbao Yu,Yutang Shen,Hengbo Yin 한국화학공학회 2009 Korean Journal of Chemical Engineering Vol.26 No.3
A series of Keggin type tungsten-substituted molybdophosphoric acids (H3PMo12−nWnO40·XH2O) were synthesized and characterized by ICP-AES, FT-IR, TG-DSC, and XRD. The tungsten substitution extent significantly affected their catalytic activity in the oxidation of cyclopentene and the selectivity of the resultant products. The tungsten-substituted molybdophosphoric acids with tungsten substitution numbers in a range of 3-6.8 exhibited high catalytic activity in the oxidation of cyclopentene. After reaction for 8 h, the conversion of cyclopentene was up to 97%; the oxidation products mainly consisted of glutaraldehyde, cis-1,2-cyclopentanediol and trans-1,2-cyclopentanediol with the yields of ca. 23%, 27%, and 45%, respectively.
Qian Zhao,Qian Wang,Yajing Tang,Tingshun Jiang,Chang-sheng Li,Hengbo Yin 한국화학공학회 2010 Korean Journal of Chemical Engineering Vol.27 No.4
Ce-incorporated MCM-41 mesoporous molecular sieves (CeMCM-41) were synthesized by microwave irradiation method from sodium silicate and ammonium cerium (IV) nitrate precursors and using cetyltrimethyl ammonium bromide (CTAB) as template. The resulting samples were characterized by means of XRD, TEM, FT-IR, UV-Vis,XPS and N2 physical adsorption, respectively. The effect of the Si/Ce molar ratio on the textural properties of CeMCM-41 was investigated. The results reveal that the CeMCM-41 was successfully synthesized. The resultant mesoporous materials have specific surface areas in the range of 602-1,216 m2/g and pore sizes in the range of ca. 2.6-2.9 nm. The structural properties are related to the amount of cerium incorporation. The surface area and pore volume of the resulting CeMCM-41 were gradually reduced as the cerium content in the sample increased, and the mesoporous ordering diminished.
Dongzhi Zhang,Chen Ge,Jinjuan Xue,Tingshun Jiang,Longbao Yu,Yutang Shen,Hengbo Yin 한국공업화학회 2009 Journal of Industrial and Engineering Chemistry Vol.15 No.4
A series of Cu–Zn–Zr catalysts were prepared by a coprecipitation method and characterized by X-ray diffraction, X-ray photoelectron spectroscopy, temperature programmed reduction, and N2 adsorption. The catalytic activity of the Cu–Zn–Zr catalyst in the hydrogenation of maleic anhydride using ethanol as a solvent was studied at 220–280℃ and 1 MPa. Maleic anhydride was mainly hydrogenated to gbutyrolactone and tetrahydrofuran while ethanol dehydrogenated to ethyl acetate. After reduction, CuO species present in the calcined Cu–Zn–Zr catalysts were converted to metallic copper (Cu0). The presence of ZrO2 favored the deep hydrogenation of g-butyrolactone to tetrahydrofuranwhile the presence of ZnO was beneficial to the formation of the intermediate product g-butyrolactone. The molar ratios of the hydrogen produced in ethanol dehydrogenation to the hydrogen consumed in maleic anhydride hydrogenation increased with the increase of the reaction temperature.
Aili Wang,Yiqian Jiang,Weiguang Chen,Yanjun Liu,Yutang Shen,Tingshun Jiang,Zhanao Wu,Hengbo Yin 한국공업화학회 2012 Journal of Industrial and Engineering Chemistry Vol.18 No.1
Methyltrichlorosilane and low-boiling residue from the synthesis of methylchlorosilanes via the direct reaction of silicon and methyl chloride were effectively converted to high-valued dimethyldichlorosilane catalyzed by 1-butyl-3-methylimidazolium chloroaluminate, [BMIM]Cl-nAlCl3, ionic liquid catalysts. The yield of dimethyldichlorosilane reached 69.1% when the redistribution reaction between methyltrichlorosilane and low-boiling residue was catalyzed by [BMIM]Cl-6AlCl3 at a reaction temperature of 150 8C for 300 min. The conversion of methyltrichlorosilane was 87.8%. And the conversions of tetramethylsilane, methylhydrodichlorosilane, and dimethylhydrochlorosilane present in low-boiling residue were ca. 100%, respectively. The ionic liquids could be recycled efficiently. This research provided an eco-friendly and economical route for the treatment of methyltrichlorosilane and low-boiling residue, which were the by-products in the direct synthesis of methylchlorosilanes. The possible reaction route was also discussed.
Oxidation of cyclopentene catalyzed by phosphotungstic quaternary ammonium salt catalysts
Jinjuan Xue,Aili Wang,Jingbo Wang,Dongzhi Zhang,Weiguang Chen,Longbao Yu,Tingshun Jiang,Hengbo Yin 한국공업화학회 2010 Journal of Industrial and Engineering Chemistry Vol.16 No.2
A series of phosphotungstic quaternary ammonium salts, Q3 (PW12O40) and Q3(PW4O16) [Q = (C5H5)N+(C16H33), (C16H33)N+(CH3)3, (C4H9)4N+, and (CH3)4N+], were used as the catalysts in oxidation of cyclopentene. The catalysts [(C5H5)N(C16H33)]3(PW4O16) and [(C16H33)N(CH3)3]3(PW4O16) showed high catalytic activity in the selective oxidation of cyclopentene while using H2O2 (50%) as an oxidant and 2-propanol as a solvent. The oxidation products mainly consisted of glutaraldehyde, cis-1,2-cyclopentanediol and trans-1,2-cyclopentanediol. The above-mentioned two catalysts were dissolved completely in the reaction medium during the catalysis process and precipitated themselves from the reaction system after reaction, showing the characteristics of reaction-controlled phase-transfer catalysis. The types of quaternary ammonium cations and the phosphotungstic anions in phosphotungstic quaternary ammonium salts affected catalytic activity.
Gas phase dehydration of glycerol catalyzed by rutile TiO_2-supported heteropolyacids
Lingqin Shen,Aili Wang,Hengbo Yin,Yonghai Feng,Longbao Yu,Tingshun Jiang,Yutang Shen,Zhanao Wu,박은덕 한국공업화학회 2011 Journal of Industrial and Engineering Chemistry Vol.17 No.3
Gas phase dehydration of glycerol catalyzed by the rutile TiO2-supported heteropolyacids was investigated. The TiO_2-supported heteropolyacid catalysts were prepared by the incipient wetness impregnation method using silicotungstic, phosphotungstic, and phosphomolybdic acids as active compounds. The as-prepared catalysts were characterized by X-ray diffraction, infrared spectroscopy,temperature programmed desorption of ammonia, and surface area measurement. The heteropolyacids supported by rutile TiO_2 were crystallites. The catalytic activity of the catalysts in the gas phase dehydration of glycerol was significantly affected by the type and loading of heteropolyacids. TiO_2-supported silicotungstic acid (20 wt.%) catalyst showed the highest catalytic activity with an acrolein selectivity of 80 mol% at a conversion of glycerol of 99% and a reaction temperature of 280 8C under ambient pressure. The possible reaction route in the gas phase dehydration of glycerol catalyzed by the TiO_2-supported heteropolyacid catalysts was also discussed briefly.
Acylation of salicylamide to 5-acetylsalicylamide using ionic liquids as dual catalyst and solvent
Weiguang Chen,Yunsheng Zhang,Zhangzhun Lu,Aili Wang,Yutang Shen,Tingshun Jiang,Longbao Yu,Hengbo Yin 한국공업화학회 2010 Journal of Industrial and Engineering Chemistry Vol.16 No.5
The Lewis acidic ionic liquids, 1-butyl-3-methylimidazolium chloroaluminate ([BMIM]Cl-nAlCl3) and Nbutylpyridinium chloroaluminate ([BPy]Cl-nAlCl3), were used as both catalyst and solvent in Friedel–Crafts acylation of salicylamide with acetyl chloride to 5-acetylsalicylamide. The Lewis acidic ionic liquids, substituting for the conventional carcinogenic nitrobenzene solvent and anhydrous AlCl3catalyst, showed excellent catalytic activity in the acylation of salicylamide to 5-acetylsalicylamide. When [BMIM]Cl-2AlCl3 was used as the catalyst, the yield of 5-acetylsalicylamide reached 81.3%. When [BPy]-2AlCl3 was used as the catalyst, the maximum yield of 5-acetylsalicylamide was 89.2%. The content of AlCl3 and the structure of the cations in the ionic liquids had synergistic effect on the acylation reaction. 2010 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.