AlCl<sub>3</sub>/SBA-15催化尼泊金丁酯的合成

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%。

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	刘心韵
	李琳琳
	付海
	龚维
	陈卓
	尹晓刚

关键词：介孔分子筛SBA-15； Lewis酸；尼泊金丁酯

Abstract： 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%.

Keywords： mesoporous molecular sieve SBA-15； Lewis acid； butylparaben

Received 2018-12-08;

Fund:贵州医科大学博士启动基金项目（JY[2018]29）。

Corresponding Authors: 尹晓刚,E-mail:21200155@qq.com。 Email: 21200155@qq.com

About author: 刘心韵(1990-),女,博士,主要研究方向为有机合成。

引用本文:

刘心韵, 李琳琳, 付海, 龚维, 陈卓, 尹晓刚.AlCl₃/SBA-15催化尼泊金丁酯的合成[J]. 化学工业与工程, 2019,36(6): 30-36

Liu Xinyun, Li Linlin, Fu Hai, Gong Wei, Chen Zhuo, Yin Xiaogang.Synthesis of Butylparaben Catalyzed by AlCl₃/SBA-15[J]. Chemcial Industry and Engineering, 2019,36(6): 30-36

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