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机构地区:[1]湘南学院化学与生命科学系,湖南郴州423000 [2]吉首大学化学化工学院,湖南吉首416000 [3]中国科技大学合肥微尺度物质科学国家实验室,安徽合肥230026
出 处:《日用化学工业》2008年第5期313-315,共3页China Surfactant Detergent & Cosmetics
基 金:湖南省教育厅优秀青年科研基金资助项目(06B089)
摘 要:研究了以壳聚糖硫酸盐为非均相催化剂,丙二酸与乙醇为原料酯化合成丙二酸二乙酯的新工艺,用正交试验确定了反应的较佳工艺条件为:丙二酸的加入量为0.1 mol时,醇酸摩尔比为3.0∶1.0,催化剂用量为反应物总质量的2.0%,带水剂苯15 mL,回流反应时间2.0 h,酯化率可达97%以上。结果表明,该催化剂用于合成丙二酸二乙酯具有良好的催化活性和重复使用性。Diethyl malonate was synthesized by esterification with malonic acid and ethanol as reactants and chitosan sulfate as the heterogeneous catalyst. Through orthogonal designed experiments, the optimal reaction conditions were obtained as follows : amount of malonic acid, 0.1 mol ; mole ratio of ethanol to malonic acid, 3.0 to 1.0; dosage of catalyst, 2.0% of the total mass of the reactants; benzene used as water - stripping agent at dosage of 15 mL; reaction time under reflux boiling, 2. 0 h. Under these Conditions, yield of diethyl malonate achieves higher than 97%. The results showed that chitosan sulfate has excellently catalytic activity and could be used repeatedly.
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