固体酸催化合成马来酸二丁酯  

Synthesis of dibutylmaleate catalyzed by solid acid

作　　者：闫鹏[1] 郭海福[1] 陈志胜[1] 王赵志[1] 吴燕妮[1] 

机构地区：[1]肇庆学院化学化工学院,广东肇庆526061

出　　处：《化学研究与应用》2011年第5期539-543,共5页Chemical Research and Application

基　　金：肇庆市科技计划项目(2009G013);肇庆学院青年项目(0924)资助

摘　　要：制备了固体酸催化剂Zr(SO4)2/SiO2,并用于合成马来酸二丁酯,考察了Zr(SO4)2负载量、焙烧温度、焙烧时间等催化剂制备条件对催化活性的影响。采用FTIR、XRD、TG等方法对催化剂进行了表征分析。通过正交实验设计优化了固体酸Zr(SO4)2/SiO2催化合成马来酸二丁酯的工艺条件。实验结果表明,Zr(SO4)2/SiO2是合成马来酸二丁酯的良好催化剂,适宜的催化剂制备条件为:硫酸锆负载量57%,焙烧温度400℃,焙烧时间2 h。适宜的催化合成反应条件为:酐醇物质的量比为1∶2.5,催化剂用量为马来酸酐质量的6%,带水剂甲苯8 mL,反应时间2.0 h。在此条件下马来酸二丁酯的酯化率为98.5%。Solid acid catalyst Zr（SO4）2/SiO2 were prepared and applied to synthsize dibutylmaleate.Effects of mass fraction of Zr（SO4）2） in the catalyst,calcination temperature,and calcination time on the catalytic activity were investigated.The catalysts were characterized by FTIR,XRD and TG methods.Process for catalytic synthesis of dibutylmaleate were optimized by orthogonal experiment design.The results showed that solid acid catalyst Zr（SO4）2/SiO2 exhibited high catalytic activity for the synthesis of dibutylmaleate.The appropriate conditions of catalysts preparation were as follows：loading amount of Zr（SO4）2（based on total mass of catalyst）was 57%,calcination temperature of catalyst was 400 ℃,calcination time was 2 h.Under suitable esterification conditions： mole ratio of maleic anhydride to n-butanol was 1∶2.5,mass fraction of Zr（SO4）2/SiO2 in maleic anhydride was 6.0%,water-carrying agent toluene was 8 mL,reaction time was 2 h,the esterification rate was 98.5%.

关 键 词：马来酸二丁酯 固体酸催化剂 硫酸锆 二氧化硅 

分 类 号：O623.624[理学—有机化学]