酸性离子液体[N4H4（CH2）6]·4HSO4催化合成氯乙酸乙酯  

Synthesis of Ethyl Chloroacetate Catalyzed by Acidic Ionic Liquid [N4H4（CH2）6]·4HSO4

作　　者：贾鹏飞[1] 王娟[1] 常永芳[1] 张伟亮 杨孟鑫 张星辰[1] JIA Peng-fei1 , WANG Juan1 , CHANG Yong-fang1 , ZHANG Wei-liang2, YANG Meng-xin1 ,ZHANG Xing-chen1(1. School of Chemical Engineering, Shijiazhuang University, Shijiazhuang 050035, Hebei, China; 2. North China Pharmaceutical HuaSheng Co. , Ltd. , Shijiazhuang 052160, Hebei , Chin)

机构地区：[1]石家庄学院化工学院,河北石家庄050035 [2]华北制药集团华胜有限公司,河北石家庄052160

出　　处：《精细化工》2018年第4期608-611,共4页Fine Chemicals

基　　金：石家庄学院自然科学基金(16YB003);石家庄市科技型中小企业创新基金(17SCX05007)~~

摘　　要：以六次甲基四胺和浓硫酸为原料,制备了酸性离子液体[N4H4（CH2）6]·4HSO4,并将其作为催化剂应用到氯乙酸乙酯的合成中,对酯化反应涉及的工艺参数进行了优化,采用1HNMR对产物进行了表征。结果表明：当n（氯乙酸）∶n（乙醇）=1∶1.8、离子液体质量为氯乙酸质量的30%、反应温度100℃、反应时间3.5 h时,氯乙酸乙酯收率最高,为93.27%。催化剂重复使用6次,氯乙酸乙酯收率为90.16%。An acidic ionic liquid [N4H4（CH2）6]·4HSO4 was prepared by using hexamethylenetetramine and concentrated sulfuric acid as raw materials. It was then used as the catalyst for the synthesis of ethyl chloroacetate,and the technological parameters involved in esterification reation were optimized. The structures of the catalyst and title compound were confirmed by1 HNMR.The results showed that the optimal conditions for the synthesis of ethyl chloroacetate were obtained.When the molar ratio of chloroacetic acid to ethanol was 1∶1. 8,the amount of ionic liquid was 30% of the mass of chloroacetic acid,the reaction temperature was 100 ℃,the reaction time was 3. 5 h,the yield of ethyl chloroacetate reached 93. 27%. Even after the acidic ionic liquid was reused for six runs of reaction,the yield of ethyl chloroacetate was still up to 90. 16%.

关 键 词：氯乙酸乙酯 酸性离子液体 酯化 催化技术 

分 类 号：X131.2[环境科学与工程—环境科学]