乙酰柠檬酸三丁酯的催化合成

Catalytic Synthesis of Acetyl Tri-n-Butyl Citrate

目前常用的邻苯二甲酸酯类增塑剂可能诱发致癌,国内外都在寻找能够替代的无毒增塑剂,柠檬酸酯类增塑剂是安全的替代增塑剂之一。今以柠檬酸三丁酯和乙酸酐为原料,研究了硫酸氢钠、大孔强酸性阳离子交换树脂催化合成乙酰柠檬酸三丁酯的过程,考察了原料摩尔配比、催化剂用量、反应时间、反应温度对乙酰柠檬酸三丁酯收率的影响。在适宜条件下,两种催化剂催化合成乙酰柠檬酸三丁酯的收率可分别达到99.5%和99.8%。精制后,乙酰柠檬酸三丁酯的含量经气相色谱分析大于99%。催化剂重复使用情况的考察表明:硫酸氢钠有较好的重复使用性;使用后经无水乙醇洗涤并干燥过的大孔强酸性阳离子交换树脂也具有很好的重复使用性。

The phthalate used as plasticizer may induce cancer, and the citrate is one of its non-toxic substitutes. Aeetyl tri-n-butyl citrate （ATBC） was synthesized by using tri-n-butyl citrate and acetic anhydride as reactants, sodium bisulfate or the maeroporous strongly acidic cation exchange resin as catalyst. The effects of molar ratio of reactants, dosage of catalyst, reaction time and temperature on the yield of ATBC were investigated. Under the proper reaction conditions, the yield of ATBC catalyzed by sodium bisulfate may reach 99.5%, and that by the macroporous strongly acidic cation exchange resign may achieve 99.8%. According to the analysis of GC, after refining the purity of ATBC synthesized is higher than 99%. It is found that the sodium bisulfate has good reusability, and the macroporous strongly acidic cation exchange resin has excellent reusability too if it is washed by alcohol and dried before its reuse.