SO3H-功能化酸性离子液体催化合成己二酸二丁酯

Esterification of Adipic Acid and 1-butanol Catalyzed by SO3H- Functionalized Ionic Liquid without Removal of Water

摘要:

以1, 3-丙烷磺内酯和1, 4-丁烷磺内酯为主要原料，采用两步法合成了八种SO3H-功能化酸性离子液体，考察比较无带水剂条件下不同酸性离子液体的酸性及其对合成己二酸二丁酯的催化活性，并将离子液体酸性强弱与酸催化活性进行关联，同时对反应温度、原料配比、反应时间、催化剂用量等反应工艺条件进行优化。结果表明，优选N-（3-磺酸基）丙基咪唑硫酸氢盐离子液体为催化剂，在反应温度110 ℃、n(1-butanol): n(adipic acid)=6:1、m(cat): m(adipic acid)=1.5 %、反应时间3 h的优化反应条件下，己二酸二丁酯收率最高可达90 %。

Abstract:

Several SO3H-functionalized acidic ionic liquids were synthesized by two-step method, using 1, 3-propane sultone and 1, 4-Butanesultone as raw materials, respectively. Esterification of 1-butanol with adipic acid was carried out by using these different Br謓sted acidic ionic liquids as catalysts without removal of water. The relationship between the Br謓sted acidity-catalytic activity and the relative acidity were studied. Moreover, the reaction conditions of reaction temperature, molar ratio of reactants, reaction time and ionic liquid amount were optimized. The results indicated that, [MimN(CH2)4SO3H][HSO4] acidic ionic liquid was the best catalyst, and under the optimized reaction conditions of 110 ℃, n(1-butanol): n(adipic acid)=6:1, m(cat): m(adipic acid)=1.5 %, 3 h, the yield of dibutyl adipate was 90 %.