乙酰柠檬酸三丁酯合成工艺的改进
Improvement of Synthesis Conditions of Acetyl tri-n-Butyl Citrate
李攀 1王建设 1赵建宏 1王留成 1宋成盈 1徐海升1
作者信息
- 1. 郑州大学化工与能源学院,河南郑州,450001
- 折叠
摘要
以质量分数为40%的甲基磺酸和质最分数均为30%的对甲苯磺酸和氨基磺酸分别组成的混合物为催化剂,采用柠檬酸和正丁醇酯反应后得到的柠檬酸三丁酯(TBC)直接合成乙酰柠檬酸三丁酯(ATBC),考察了酯化温度及脱醇工艺条件对TBC质量的影响.结果表明:在正丁醇与柠檬酸物质的量比为4.5:1,酯化温度130℃,酯化时间5.0 h和催化剂用量为柠檬酸质量的1.5%条件下合成的TBC,在脱醇温度125℃及脱醇时间20 min的条件下,无须精制处理可直接用于乙酰化合成ATBC,在乙酸酐与TBC物质的量比为1.4:1,反应温度为80℃,反应时间1.5 h的条件下,乙酰柠檬酸三丁酯的收率和纯度均达99%以上.
Abstract
The influence of esterification temperature and distillation conditions on the quality of tri-?-butyl citrate(TBC) synthesized from citric acid and 1-butanol, and acetyl tri-M-butyl citrate(ATBC) synthesized from TBC and acetic anhydride over the catalyst composing of mass fraction 40% of methanesulfonic acid, mass fraction 30% of paratoluenesulfonic acid and mass fraction 30% of sulfamic acid were investigated. The results showed that the TBC prepared under the conditions of molar ratio of 1-butanol and citric acid 4.5:1, esterification temperature 130 ℃, esterification time 5.0 h and mass ratio of catalyst to citric acid 1.5% could be used to directly prepare ATBC after being distillated for 20 min at 125 ℃, and the yield and purity of ATBC were above 99% under the conditions of molar ratio of acetic anhydride to TBC 1.4:1, reaction temperature 80 ℃ and reaction time 1.5 h.
关键词
柠檬酸三丁酯/乙酰柠檬酸三丁酯/甲基磺酸/对甲苯磺酸/氨基磺酸Key words
tri-n-butyl citrate/acetyl tri-n-butyl citrate/methanesulfonic acid/para-toluenesulfonic acid/sulfamic acid引用本文复制引用
基金项目
河南省科技攻关项目(07210227002)
出版年
2011
NETL
NSTL
维普
万方数据