摘要
以溴化2-丁基-3～甲基咪唑盐和磷钨酸为原料制备的具有Keggin结构的1-丁基-3-甲基咪唑磷钨酸盐[（Bmlm）3PW12O40·3H2O3催化合成乙酸乙酯，考察了1-丁基-3-甲基咪唑磷钨酸盐的催化活性以及带水剂、催化剂用量、酸醇摩尔比、反应时间对乙酸乙酯合成收率的影响．实验结果表明，具有Keggin结构的1-丁基-3-甲基咪唑磷钨酸盐[（Bmlm）3PW12O40·3H2O3呈现出较高的催化活性和较好的重复使用性能。优化的合成乙酸乙酯的工艺条件为：酸醇摩尔比为3：1，1-丁基-3-甲基咪唑磷钨酸盐催化剂用量为3g（以每摩尔乙醇计），带水剂甲苯的用量为4.0mL（以每摩尔乙醇计），回流反应时间为5。5h．在此所选择的条件下，合成乙酸乙酯的收率达99．68％～99.91％．
The catalytic synthesis of ethyl acetate by 1-buthyl-3-methylidazolium dodecatungstophosphate [（Bmlm）3PW12O40·3H2O3] preserved the primary Keggin structure which was prepared from 1-Buthyl- 3-methylidazolium bromide and 12-phosphotungstic acid were studied. The effects of water-taken agent, the amount of 1-Buthyl-3-methylidazolium dodecatungstophosphate catalyst, molar ratio of acid and alcohol, and reaction time on synthesis yield of ethyl acetate had been investigated. The experimental results showed that 1-buthyl-3-methylidazolium dodecatungstophosphate with the primary Keggin structure exhibited very high catalytic activity and reusability. The optimum reaction conditions for sysnthesis of ethyl acetate are as followed： molar ratio of acid and alcolhol = 3 ： 1, amount of 1-Buthyl- 3-methylidazolium dodecatungstophosphate catalyst： 3. 0 g on the basis of 1.0 mole alcohol amount, toluene as water-taken agent 4.0 mL on the basis of 1.0 mole alcohol amount, refluxing reaction time 5.5 h. Under the selected reaction conditions, the yield of ethyl acetate were 99.68%-99.91%.
出处
《浙江工业大学学报》
CAS
2008年第5期534-538,共5页
Journal of Zhejiang University of Technology
