乙酰柠檬酸三丁酯合成工艺的改进

Improved Synthetic Process of Acetyl Tributyl Citrate

以柠檬酸、正丁醇和乙酸酐为原料，对甲苯磺酸为催化剂，通过酯化、脱醇、乙酰化、脱乙酸和乙酸酐、中和、水洗等步骤制备了乙酰柠檬酸三丁酯。和文献报道的工艺相比，节省了催化剂用量，减少了近一半的废水量。当反应物摩尔比n（柠檬酸）：n（正丁醇）：n（乙酸酐）：n（对甲苯磺酸）=1：4．3：1．10：0．041，酯化反应温度为130-140℃，酯化时间为4h，乙酰化反应温度为50℃，乙酰化反应时间为1h时，产品的产率为97．5％，酯含量为99．21％，酸值为0．14mgKOH／g，色度小于50（Pt—Co），符合产品质量要求。

Acetyl tributyl citrate was synthesized by used citric acid, n-butanol and acetic anhydride as reactants, p-toluenesulfonie acid as catalyst, through esterification, alcohol removal, aeetylation, acetic acid and acetic anhydride removal, neutralization and water washing. Compared with one reported in the literature, the volume of wastewater dropped to about half of it and catalyst saved also. When the mole ratio of reactants are n（citric aeid）：n（n-butanol）：n（aeetic anhydride）：n（p-toluenesulfonie acid） = 1：4.3：1.10：0.041, the esterifica- tion reaction for 4h at 130-140℃, the acetylation reaction for 1 h at 50℃, the product yield is 97.5%, the ester content is 99.21%, acid value is 0.14 mg KOH/g and the colourity is less than 50（Pt-Co）, which meet the requirements of the product quality.