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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8种SO3H-功能化酸性离子液体,考察有/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,添加带水剂环己烷,在反应温度110℃、n(1-butanol)∶n(adipic acid)=6∶1、m(cat.)/m(adipic acid)=0.015、反应时间3 h、w(cyclohexane)=15%(基于反应体系总质量,下同)的优化反应条件下,己二酸二丁酯收率为98%。
Using 1,3-propane sultone and 1,4-butane sultone as the main raw materials, eight kinds of SO3H-functionalized acidic ionic liquids were synthesized by a two-step method. The effects of different acidic The acidity of ionic liquid and its catalytic activity for the synthesis of dibutyl adipate were studied. The acid strength and acid catalytic activity of ionic liquid were correlated with each other. The reaction temperature, the ratio of raw materials, the reaction time and the amount of catalyst were optimized. The results showed that N- (3-sulfonic acid) propylimidazolium bisulfate ionic liquid was used as catalyst, cyclohexane with water-entraining agent was added, and the reaction temperature was 110 ℃, n (1-butanol) = 6: 1, adipic acid = 0.015, reaction time 3 h, cyclohexane = 15% (based on the total mass of the reaction system, the same below) The yield of dibutyl ester was 98%.