硅胶固载硫酸镓催化合成己酸戊酯.docVIP

硅胶固载硫酸镓催化合成己酸戊酯摘要：目的研究硅胶固载硫酸镓在合成己酸戊酯工艺中的催化性能。方法考察硅胶固载硫酸镓用量、醇酸物质的量比、反应时间、带水剂用量及催化剂重复使用次数等因素对收率的影响。结果硅胶固载硫酸镓具有催化活性高，易分离回收，操作简单，后处理方便，重复使用性良好等优点。最佳反应条件下收率为94.0 %。结论硅胶固载硫酸镓是合成己酸戊酯的良好催化剂。 关键词：乙酸戊酯；硅胶固载硫酸镓；催化；合成 中图分类号：O623.624文献标识码：A文章编号：1672-979X(2008)09-0049-02 Synthesis of Amyl Hexanoate Catalyzed by Gallium Sulfate Supported on Silica Gel YANG Geng-xu1, YANG Wei-bing2 (1. Chemistry and Chemical Engineering, College of Henan University, Kaifeng 475004, China; 2. Henan School of Medicine and Pharmacy, Kaifeng 475001, China) Abstract：Objective To study the catalytic activity of gallium sulfate supported on silica gel in the synthesis of amyl hexanoate. Methods Amyl hexanoate was synthesized from hexanoic acid and n-pentanol by using gallium sulfate supported on silica gel as the catalyst. The effects of amount of gallium sulfate supported on silica gel, molar ratio of alcohol to acid, reaction time, amount of carrying water agent and repeated times of the catalyst on the yield were investigated. Results The gallium sulfate supported on silica gel had high catalytic activity and could be isolated and recovered easily, used repeatedly. The operation was simple and the post-processing could be done conveniently. Under the best conditions, the yield of amyl hexanoate could reach 94.0 %. Conclusion Gallium sulfate supported on silica gel is an excellent catalyst in the synthesis of amyl hexanoate. Key words：amyl hexanoate; gallium sulfate supported on silica gel; catalysis; synthesis 己酸戊酯为无色液体，呈香蕉和菠萝香气，是我国允许使用的食用香料，由己酸和戊醇在苯溶液中用对甲苯磺酸催化酯化而成[1]。己酸戊酯有多种植物的香味成分存在[2-4]，它与环境的友好合成有益于开发多种香精之间的调配。笔者以自制的硅胶固载硫酸镓为催化剂合成己酸戊酯，结果表明此催化剂催化活性高，易分离回收，操作简单，后处理方便，不需加带水剂，还具有良好的重复使用性。在最佳反应条件下己酸戊酯收率达94.0 %。 1实验部分 1.1仪器与试剂 KDM型磁力搅拌电热套和SHB-Ⅲ型循环水式多用真空泵（郑州长城科工贸公司），WZS-1型阿贝折光仪（上海光学仪器厂），Avatar360FT-IR型红外光谱仪（美国Nicolet公司）。 硫酸镓（Ga2(SO4)3?18H2O）为工业品，柱层层析硅胶，其余试剂为分析纯。 1.2催化剂Ga2(SO4)318H2O/硅胶的制备 1.2.1硅胶的预处理将100 g硅胶放在洗净的表面皿上，置入烘箱于150 ℃活化 2 h待用。 1.2.2催化剂的制备称取30 g硫酸镓置于5