AlCl3/SBA-15催化尼泊金丁酯的合成  

Synthesis of Butylparaben Catalyzed by AlCl3/SBA-15

作　　者：刘心韵 李琳琳 付海 龚维 陈卓 尹晓刚 Liu Xinyun;Li Linlin;Fu Hai;Gong Wei;Chen Zhuo;Yin Xiaooang(School of Chemistry and Materials Science,Guizhou Normal University,Guizhou Key Laboratory of Functional Materials Chemistry,Guiyang 550001,China;School of Pharmaceutical Sciences,Guizhou Medical University,Guiyang 550025)

机构地区：[1]贵州师范大学化学与材料科学学院,贵州省功能材料化学重点实验室,贵阳550001 [2]贵州医科大学药学院,贵阳550025

出　　处：《化学工业与工程》2019年第6期30-36,共7页Chemical Industry and Engineering

基　　金：贵州医科大学博士启动基金项目(JY[2018]29)

摘　　要：以介孔分子筛SBA-15为载体制备了5种SBA-15负载Lewis酸催化剂,并探讨了其对酯化反应合成尼泊金丁酯产率的影响。采用傅里叶变换红外光谱(FT-IR)、热重分析(TG)、N2吸附-脱附曲线和比表面积测试(BET)等多种手段对催化剂进行结构表征,发现Lewis酸成功负载在SBA-15上。通过单因素实验筛选了催化剂种类、催化剂用量、n(醇)/n(酸)、反应时间和反应温度对酯化收率的影响。确定最适宜反应条件为:反应温度135℃,反应时间3 h,n(AlCl3/SBA-15)/n(对羟基苯甲酸)为8%,n(AlCl3/SBA-15)∶n(TsOH)为2∶1,n(醇)/n(酸)为3∶1,该条件下酯化率可达96.8%。Five kinds of SBA-15 supported Lewis acid catalysts were prepared with mesoporous molecular sieve SBA-15 as the supporter. The structure of the catalyst was characterized by Fourier transform infrared spectroscopy(FT-IR), thermogravimetric analysis(TG), N2 adsorption-desorption curve and specific surface area test(BET). It was found that Lewis acid was successfully loaded onto SBA-15. The effects of catalyst containing different Lewis acids, catalyst loading, molar ratio of starting materials, reaction time and reaction temperature on the yields of the esterification reaction to prepare butylparaben were investigated. The optimal reaction conditions are identified as the following: the molar ratio of AlCl3/SBA-15 is 2∶1, the molar ratio of alcohol to acid is 3∶1, the molar ratio of AlCl3/SBA-15 to p-hydroxybenzoic acid is 2∶1. Under these reaction conditions at 135 ℃ for 3 h, the yield of butylparaben was up to 96.8%.

关 键 词：介孔分子筛SBA-15 LEWIS酸 尼泊金丁酯 

分 类 号：TQ245.2[化学工程—有机化工]