硫酸钾催化环氧氯丙烷与三乙胺的反应研究

Study on Reaction of Triethylamine with Epichlorohydrin with K_2SO_4 Catalyst

首次将硫酸钾作为催化剂,引入到环氧丙基三乙基氯化铵中间体的合成反应中。与无催化剂体系相比,催化下的反应速率大幅度提高,反应时间显著缩短。以环氧氯丙烷的转化率和产物中环氧基保留率的乘积作为中间体性能的评价指标,通过正交实验优化出最佳条件:甲醇水溶液为溶剂,反应温度50℃、n(硫酸钾)∶n(环氧氯丙烷)=0.010、n(三乙胺)∶n(环氧氯丙烷)=1.0、反应时间为1.5 h。该条件下,环氧氯丙烷的转化率可达92.02%,产物中环氧基保留率达到70.67%。可见硫酸钾用于催化环氧丙基三乙基氯化铵的合成反应是适宜的。

Epoxypropyl triethyl ammonium chloride intermediate was synthesized by the reaction of triethylamine with epichlorohydrin in aqueous methanol using K2SO4 as catalyst. Compared with literature results, the reaction velocity ascended dramatically and the reaction time decreased greatly. Based on the product of epichlorohydrin conversion and epoxy group retention ratio, the optimized reaction conditions were obtained as follows： aqueous methanol as solvent; reaction temperature and time, 50 ℃ and 1.5 h; n （K2SO4） ： n （epichlorohydrin） = 0.010; n （triethylamine） ： n （epichlorohydrin） = 1.0. The epichlorohydrin conversion and epoxy group retention ratio could reach 92.02% and 70.67 % respectively. K2SO4 was a good catalyst for the reaction.