合成并表征了酸功能化离子液体,用于催化合成柠檬酸三丁酯(TBC).通过考察各种离子液体的催化活性及重复使用性能,选定酸功能化离子液体[HSO3-pmim]HSO4为催化合成TBC的催化剂.研究了催化剂用量、醇酸摩尔比、反应时间等因素对酯化反应的影响,得到其较佳工艺条件为:催化剂用量为反应物总质量的8.0%,醇酸摩尔比为5.5∶1,反应温度110-150℃,反应时间3h.此条件下,酯化率达到99.0%.分离出的离子液体未经任何处理重复使用8次后,酯化率仍为95.2%.
Acidic functionalized ionic liquids were synthesized and characterized. Tributyl citrate (TBC) was synthesized using acidic functionalized ionic liquids as catalysts. According to the study of catalytic activity and the reusability of various ionic liquids, [ HSO3-pmim] HSO4 was chosen to synthesize TBC as the catalyst. The effects of the reaction conditions on the reaction results, such as the amount of catalyst, molar ratio of acid and alcohol, reaction time, were examined and the optimal conditions were obtained. The optimal conditions were as follows: w (catalyst): w (reactants) =8.0%, n (1-butyl alcohol): n (citric acid) =5.5: 1, 110 -150 ℃, 3 h. Under the optimal reaction conditions, the conversion could be 99. 0%. Separated from the products, [ HSO3-pmim ] HSO4 could be reused 8 times without any disposal and the conversion could reach 95.2%.