改性固体酸SO_4^(2-)/ZrO_2催化合成没食子酸甲酯的研究  

Study on synthesis of methyl gallate catalyzed by modified solid superacid SO_4^(2-)/ZrO_2

作　　者：赵培瑞[1] 李娜[2] 陈茜文[1] 王广要[1] 

机构地区：[1]中南林业科技大学,湖南长沙410004 [2]长沙商贸旅游职业技术学院,湖南长沙410004

出　　处：《中南林业科技大学学报》2017年第6期114-118,共5页Journal of Central South University of Forestry & Technology

基　　金：湖南省教育厅科研一般项目(15C1407);湖南省科学技术厅科技计划重点项目(2014WK2027)

摘　　要：以低温陈化方法制备改性SO_4^(2-)/ZrO_2型固体超强酸为催化剂合成没食子酸甲酯,考察了不同反应条件对没食子酸甲酯纯度与收率的影响,利用正交设计原理优化合成条件,实验结果表明:催化剂的制备条件为陈化温度:-10℃、浸渍H^+浓度:1.0 mol/L;合成条件为催化剂用量:7.5 g;反应时间:5 h,酸醇摩尔比约为1∶20,不采用带水剂;产品经液相色谱、红外和熔点检测分析,没食子酸甲酯的平均收率达88.80%,纯度达≥99%,符合没食子酸甲酯的质量标准。Based on the low temperature aging method to prepare modified SO42-/ZrO2 solid Superacid as catalyst for synthesis of gallic acid methyl ester. The effects of different reaction conditions on the purity and yield of methyl gallate were investigated. The orthogonal design was used to optimize the prepare and synthesis conditions. The results show that the optimum reaction conditions for nthesis of methyl gallate by modified SO42-/ZRO2 solid superacid were as follows： aging temperature： 10 ℃ , impregnation H＋ concentration： 1.0 mol/L, andthe optimum reaction conditions forsynthesis conditions： catalyst dosage： 7.5 g; reaction time： 5 h; molar ratio of acid to alcohol 1：20. The product was analyzed by liquid chromatography, infrared and melting point analysis. The average yieldand purityof methyl gallate was 88.80% and 99%, respectively, which was in accordance with the quality standard of methyl gallate.

关 键 词：没食子酸甲酯 固体超强酸 正交实验 催化合成 

分 类 号：S713[农业科学—林学] TQ245.24[化学工程—有机化工]