固体酸催化合成1,6-己二醇二丙烯酸酯工艺条件的优化

摘要

以1,6-己二醇和丙烯酸为原料,采用自制的固体超强酸SO42-/TiO2-SnO2为催化剂,考察了工艺过程各参数(酸醇比、催化剂用量、反应时间和反应温度)对加氢脱氧效果的影响.在单因素实验的基础上,采用正交试验,对催化合成1,6-己二醇二丙烯酸酯(HDDA)工艺条件进行了优化,并对合成产物进行了GC/MS、核磁、FT-IR表征以及物化性质进行了检测.最佳的酯化反应条件为:酸醇摩尔比3.5∶1,催化剂加入量质量分数为5％,反应时间4h,反应温度130℃,在此条件下,HDDA的平均收率可达91.8％,产品纯度很高且与精细标准品理化性质基本一致.%1,6-hexanediol and acrylic acid as raw material,and solid superacid SO42-/TiO2-SnO2 as catalyst,the catalytic synthesis of HDDA process conditions were optimized,based on the single factor experiment and adopting orthogonal test method.The synthetic product was characterized by GC/MS,NMR,FT-IR,and the physicochemical properties were also tested.The optimal conditions of esterification reaction are acid alcohol mole ratio of 3.5 ∶ 1,the amount of catalyst 5％,reaction time 4 h,and reaction temperature 130 ℃.Under these conditions,the average yield of HDDA is up to 91.8 ％,the product purity is very high,and the physicochemical properties are basically the same as fine standards.