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机构地区:[1]山东科技大学化学与环境工程学院,山东青岛266510 [2]山东大学化学与化工学院,山东济南250100
出 处:《化学工业与工程》2011年第6期6-9,16,共5页Chemical Industry and Engineering
基 金:山东省科技厅项目(Y2007B20)
摘 要:以氯乙酸与异丙醇为原料,采用结晶硫酸高铈/硫酸氢钾复合催化剂,催化合成氯乙酸异丙酯。研究了不同助催化剂、催化剂配比和用量对其合成反应的影响,优化了醇酸比、催化剂用量、反应时间等反应条件,并且考察了复合催化剂的重复使用性。结果表明,以结晶硫酸高铈/硫酸氢钾为复合催化剂的效果最好,其最适宜反应条件为:n(醇)/n(酸)为1.35,m(硫酸高铈)/m(硫酸氢钾)为2,n(硫酸高铈)/n(氯乙酸)为0.011,反应时间3 h,酯化率可达92.1%。Isopropyl chloroacetate was synthesized from chloroacetic acid and isopropyl alcohol with Ce(SO4)2·4H2O/KHSO4 as a composite catalyst.Effects of different co-catalysts and the ratio and amount of catalysts on the reaction were considered.The molar ratio of isopropyl alcohol to chloroacetic acid,the reaction time and the amount of catalysts were optimized,and the repeatability of the composite catalyst was checked.The experimental results show that better catalytic efficiency can be obtained by the composite catalyst of Ce(SO4)2·4H2O/KHSO4.The optimized synthesis conditions were determined.The molar ratio of isopropyl alcohol to chloroacetic acid is 1.35∶1,m(Ce(SO4)2·4H2O)/m(KHSO4) is 2,the amount of catalyst is 1.1%(molar percentage),the reaction time is 3 h,in which the yield is 92.1%.
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