氯化丁基吡啶/AlCl_3离子液体催化体系中富马酸二甲酯合成过程优化

Optimization of synthesis process of dimethyl fumarate using environmentally friendly catalyst 1-butyl pyridium chloride/AlCl_3 ionic liquid

在氯化丁基吡啶与AlCl3 组成的离子液体催化体系中 ,顺丁烯二酸酐与甲醇反应 ,生成富马酸二甲酯 .采用单纯型优化方法对催化剂用量 ,反应时间、反应原料摩尔比进行了优化 .实验结果表明氯化丁基吡啶与AlCl3 组成的离子液体具有异构化和酯化两种催化作用 .在优化条件下m(催化剂 )∶m(顺丁烯二酸酐 ) =0 .0 7∶1 ;n(甲醇 )∶n(顺丁烯二酸酐 ) =1 .1∶1 ,反应时间 3h,反应温度 65℃ ,富马酸二甲酯的收率达到 92 % .

Dimethyl fumarate is synthesized from maleic anhydride and methanol by isomerization and esterification reaction used 1 butyl pyridium chloride/AlCl3 ionic liquid as environmentally friendly catalysts.The reaction time,reaction temperature,amount of catalyst and material molar ratio are optimized by simplex search method for the design of experiments.The experiment results indicate that 1 butyl pyridium chloride/AlCl 3 ionic liquid catalyst can be regarded as two kinds of catalysis for isomerization of maleic anhydride and esterification of fumarate acid.Under the optimum conditions,methanol:maleic anhydride=1.1∶1 (mol ratio),catalyst:maleic anhydride=0.07(mass ratio),temperature is 35?℃ and reaction time is 3?h,the yield of dimethyl fumarate can reach 92%,and the purity of product is over 99.4% .