SiO2固化SO3H-功能化离子液体催化合成油酸甲酯  

Synthesis of Methyl Oleate Using a Silica-immobilized SO3H-functionalized Ionic Liquid as an Efficient Catalyst

作　　者：赵亚东[1] 郜蕾 高健[1] 郭孟星 任珂[1] 孙晓波[1] 

机构地区：[1]郑州大学化工与能源学院,河南郑州450001 [2]郑州大学国际学院,河南郑州450052

出　　处：《精细化工》2018年第1期81-86,180,共7页Fine Chemicals

基　　金：河南省高等学校重点科研项目(15A530013,15B530004)~~

摘　　要：以1,3-丙烷磺内酯和巯基改性纳米二氧化硅球为原料,采用化学键合接枝法获得固化SO3H-功能化离子液体的酸催化材料（SiO2-IL）。采用NMR、FTIR和热分析方法对SiO2-IL的结构和热稳定性进行了表征。考察了SiO2-IL在油酸与甲醇酯化反应中的催化活性,分析了影响其催化性能的关键因素及原因。结果表明,该离子液体自身所具有的酸性以及固化过程中化学键合接枝程度均对其催化性能有所影响。对反应工艺条件进行了优化。结果表明,在反应温度60℃、n（甲醇）∶n（油酸）=12∶1、m（SiO2-IL）∶m（油酸）=0.09∶1.00、反应时间5 h条件下,油酸甲酯收率最高为94%,催化材料经重复使用5次后,油酸甲酯收率仍可达74%。A silica-immobilized SO3H-functionalized ionic liquid （SiO2-IL） was successfully synthesized via chemical bonding grafting method using 1,3-propane suhone and thiohydroxy modified nano-silica as raw materials. The structure and thermal stability of SiO2-IL were characterized by NMR, F-FIR and TGA. The catalytic activity of SiO2-IL was evaluated for esterification of methanol with oleie acid, and the reason and some key factors affecting the catalytic performance were discussed. The results showed that the acidity of S03 H-functionalized ionic liquid and the stability of chemical bonding grafting could affect the catalytic performance of SiOz-IL. Moreover, the effects of reaction temperature, reaction time, molar ratio of reactants and the catalyst amount on the yield of methyl oleate were investigated. The results showed that under the optimal reaction conditions identi？ ed （ temperature 60 ℃ methanol to oleic acid molar ratio 12：1 ,reaction time 5 h,mass ratio of SiO2-ILto oleic acid 0. 09： 1.00） the methyl oleate yield of 94% was obtained. After Si02-IL was reused for five times,the yield of methyl oleate could still reach 74%.

关 键 词：1 3-丙烷磺内酯 改性纳米二氧化硅球 离子液体 化学键合接枝 油酸甲酯 催化与分离提纯技术 

分 类 号：O643[理学—物理化学]