微波协同离子液体催化合成柠檬酸三丁酯工艺及其性能  

Microwave-Assisted Catalytic Synthesis Technology of Tributyl Citrate by Ionic Liquid and Its Properties

作　　者：黄飞 戴璐 王溪溪 张浩冉 吴琳 余锐[2] 魏先文[2] Huang Fei;Dai Lu;Wang Xixi;Zhang Haoran;Wu Lin;Yu Rui;Wei Xianwen(College of Chemistry and Chemical Engineering,Collaborative Innovation Center for Fine Chemicals and Materials,Huangshan University,Huangshan 245041,China;College of Chemistry and Materials Science,The Key Laboratory of Functional Molecular Solids,Ministry of Education,Anhui Normal University,Wuhu 241000,China)

机构地区：[1]黄山学院化学化工学院,精细化工与材料协同创新中心,安徽黄山245041 [2]安徽师范大学化学与材料科学学院,功能性分子固体材料教育部重点实验室,安徽芜湖241000

出　　处：《工程塑料应用》2020年第11期129-135,共7页Engineering Plastics Application

基　　金：国家自然科学基金项目(21771003,21271006);安徽省高校自然科学研究项目(KJHS2017B02);国家级大学生创新创业训练计划项目(201810375018,201810375021);安徽省大学生创新创业训练计划项目(S201910375034)。

摘　　要：制备了七种绿色高效离子液体催化剂,采用微波协同离子液体催化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。经过实验优化筛选,实验结果表明:以离子液体[HSO3-pMIM]HSO4为催化剂,其用量为柠檬酸质量的3.5%,柠檬酸和丁醇物质的量比为1:4,微波功率为450 W,微波时间为5 min,反应温度为120℃时,柠檬酸三丁酯产率可达99.3%。该催化剂经过10次循环使用,柠檬酸三丁酯的产率仍可达到97%以上,具有较好的催化活性和稳定性。增塑性能测试表明,柠檬酸三丁酯的拉伸强度、压缩强度、弯曲强度和拉伸剪切强度等均优于邻苯二甲酸二丁酯,可以很好的替代邻苯二甲酸酯类增塑剂。Seven kinds of green efficiently ionic liquid were prepared and used catalytic synthesize plasticizer tributyl citrate by microwave irradiation.The effects of various experimental factors on the yield of tributyl citrate were 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 ionic liquid[HSO3-pMIM]HSO4 as catalyst and it amount was 3.5% based on the mass of citric acid,the molar ratio of citric acid and n-butyl alcohol was 1∶4,microwave power was 450 W,microwave time was 5 min,and reaction temperature 120℃,the tributyl citrate yield was up to 99.3%.The ionic liquid[HSO3-pMIM]HSO4 could be reused ten times without considerable loss of activity and still had a conversion rate of 97% above.It exhibite excellent stability and catalytic activity.Plasticizing performance tests show that tributyl citrate in tensile strength,compression strength,bending strength,and tensile shear strength are superior to dibutyl phthalate.So tributyl citrate would take better replacement of phthalate esters.

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]