催化合成3-甲基-3-丁烯-1-醇醋酸酯及其水解过程研究  

Catalyzed synthesis of 3-methylbut-3-en-1-ol acetate and its hydrolysis

作　　者：周哲[1] 刘清[1] 费兆阳[1,2] 陈献[1] 汤吉海[1] 崔咪芬[1] 乔旭[1,2] 

机构地区：[1]南京工业大学化学化工学院,江苏南京210009 [2]南京工业大学材料化学工程国家重点实验室,江苏南京210009

出　　处：《化学工程》2014年第1期55-59,共5页Chemical Engineering(China)

基　　金：国家自然科学基金资助项目(21276126);江苏省基础研究计划(自然科学基金)项目(BK2010083)

摘　　要：采用酯化水解两步法高效合成3-甲基-3-丁烯-1-醇(MBOH)。首先采用硅烷嫁接法制备了MCM-48嫁接SnCl2催化剂,应用于多聚甲醛、异丁烯和醋酸缩合酯化制备3-甲基-3-丁烯-1-醇醋酸酯(MB-AC),然后MB-AC碱性水解制备MBOH,并对缩合酯化和水解反应进行工艺条件考察。结果表明,最佳缩合酯化反应条件为:2.4 g催化剂,16 g多聚甲醛,120 g异丁烯,128 g醋酸,反应温度140℃,反应时间6 h。在此条件下,MB-AC的收率为55.5%,MBOH的收率为13.8%。进一步将缩合酯化反应产物碱性水解,最佳水解条件为:水解温度50℃,进料速度为60 mL/h,碱溶液质量分数为20%。在此条件下,水解收率为94.5%。酯化水解两步法制备MBOH的总收率达到65.5%。Anchoring of tin dichloride on quaternary ammonium chloride functionalized MCM-48 as a new catalyst was used to catalyze the condensation reaction of paraformaldehyde, isobutene and acetic acid to produce 3- methylbut-3-en-l-ol acetate. By using the innovative esterification-hydrolysis two-step method, 3-methylbut-3-en-1- ol was synthesized effectively. The process conditions of esterification reaction and hydrolysis reaction were investigated. The result shows that under the optimal esterification reaction condition of 2.4 g catalyst, 16 g paraformaldehyde, 120 g isobutene, 128 g acetic acid, reaction temperature 140 ℃, reaction time 6 h, the yields of 3-methylbut-3-en-l-ol acetate and 3-methylbut-3-en-l-ol are 55.5% and 13.8%. The yield of hydrolysis is 94.5% under the optimal reaction condition of reaction temperature 50 ℃, mass fraction of alkali solution 20%, feed rate of alkali solution 20 mL/h. The final yield of MOH prepared by esterification-hydrolysis two-step method reaches to 65.5%

关 键 词：锡嫁接 MCM-48 3-甲基-3-丁烯-1-醇 3-甲基-3-丁烯-1-醇醋酸酯 

分 类 号：O643.32[理学—物理化学]