微波协同离子液体催化合成增塑剂柠檬酸三丁酯的工艺研究  

Study on Microwave-Assisted Catalytic Synthesis Technology ofPlasticizer TriCutyl Citrote by Ionic Liquid

作　　者：黄飞[1] 戴璐 汪婧 吴琳 张浩冉 朱长安 张愉快 HUANG Fei;DAI Lu;WANG Jing;WU Lin;ZHANG Haoran;ZHU Chang’an;ZHANG Yukuai(School of Chemistry and Chemical Engineering,Huangshan University,Huangshan 245041,China;Engineering Training Center,School of Mechanical and Electrical Engineering,Huangshan University,Huangshan 245041,China)

机构地区：[1]黄山学院化学化工学院,安徽黄山245041 [2]黄山学院机电工程学院工程训练中心,安徽黄山245041

出　　处：《四川轻化工大学学报（自然科学版）》2020年第5期1-6,共6页Journal of Sichuan University of Science & Engineering(Natural Science Edition)

基　　金：安徽省高校自然科学研究项目(KJHS2016B06,KJHS2017B02);国家级大学生创新创业训练计划项目(201810375021);安徽省大学生创新创业训练计划项目(S201910375034)。

摘　　要：针对绿色可降解增塑剂柠檬酸三丁酯合成方法中存在设备腐蚀严重、环境污染大、反应时间长、产率不高等问题,制备了绿色高效离子液体[HSO3-pmim]^+[HSO4]^-催化剂,采用微波协同离子液体催化柠檬酸和正丁醇合成了增塑剂柠檬酸三丁酯。通过单因素实验和正交试验对催化剂种类、催化剂用量、柠檬酸与正丁醇物质的量比、微波功率、微波时间和反应温度进行探究,对比了各实验因素对合成柠檬酸三丁酯产率的影响。经过实验优化,当催化剂[HSO3-pmim]^+[HSO4]^-用量为2.0 g,柠檬酸和丁醇物质的量比为1∶5,微波功率为600 W,微波时间为30 min,反应温度为130℃时,柠檬酸三丁酯产率可达98.8%。该催化剂经过8次循环使用,柠檬酸三丁酯的产率仍可达到91%以上,具有较好的催化活性和稳定性。In order to solve the problems of severe equipment corrosion,high environmental pollution,long reaction time and low yield in the synthesis process of green degradable plasticizer tri-n-butyl citrate.Ionic liquid[HSO3-pmim]^+[HSO4]^-is prepared and used catalytic synthesize plasticizer tri-n-butyl citrate from citric acid and n-butyl alcohol by microwave irradiation.The effects of various experimental factors on the yield of tri-n-butyl citrate are explored through single factor experiment and orthogonal experiment by comparing different the kinds and dosages of catalysts,the molar ratio of citric acid and n-butyl alcohol,microwave power,microwave time and reaction temperature.The experiment optimization show that[HSO3-pmim]^+[HSO4]^-dosage is 2.0 g,the molar ratio of citric acid and n-butyl alcohol is 1∶5,microwave power is 600 W,microwave time is 30 min,and reaction temperature 130℃,the tri-n-butyl citrate yield is up to 98.8%.The ionic liquid[HSO 3-pmim]+[HSO 4]-could be reused eight times without considerable loss of activity and still has a conversion rate of 91%above,it exhibited excellent stability and catalytic activity.

关 键 词：柠檬酸 正丁醇 柠檬酸三丁酯 离子液体[HSO3-pmim]^+[HSO4]^- 微波辐射 

分 类 号：O623.65[理学—有机化学]