纳米稀土复合固体超强酸SO_4^(2-)/ZrO_2-2% Nd_2O_3催化合成对羟基苯甲酸正丁酯  

Synthesis of n-butyl p-hydroxybenzoate catalyzed by nanometer rare earth composite solid superacid SO_4^(2-)/ZrO_2-2% Nd_2O_3

作　　者：冯纪南[1] 邓斌[1] 杨佳[1] 黄海英[2] 

机构地区：[1]湘南学院化学与生命科学系,湖南郴州423000 [2]湘南学院外语系,湖南郴州423000

出　　处：《食品工业科技》2014年第3期253-257,共5页Science and Technology of Food Industry

基　　金：湖南省自然科学基金项目(12JJ3019);湖南省科技厅计划项目(2010GK3123);湖南省教育厅重点科研基金项目(10A113);湖南省重点建设学科资金资助项目

摘　　要：采用共沉淀法制备稀土复合固体超强酸SO2-4/ZrO2-2%Nd2O3催化剂,电镜分析表明,该催化剂颗粒为纳米级。将其用于对羟基苯甲酸和正丁醇的酯化反应中,考察了影响合成反应的诸多因素。结果显示,催化合成对羟基苯甲酸正丁酯的优化工艺条件为:采用过量的正丁醇作共沸带水剂,回流反应时间为3.0h,催化剂用量为对羟基苯甲酸质量的3.5%,正丁醇与对羟基苯甲酸的物质的量比为3.0∶1.0,在此条件下酯化率可达97.5%。产品经熔点测定、元素分析、液相色谱和红外光谱表征为高纯度的对羟基苯甲酸正丁酯。自制催化剂具有良好的催化活性,并可多次重复再生使用。Rare earth composite solid superacid SO4^2-/ZrO2-2%Nd2O3 was prepared by coprecipitation method. The measure result of TEM indicated that catalyst particle was nanoparticle. It was used as catalyst in the esterification reaction between p-hydroxy-benzoic acid and n-butanol.The main influential factors of reaction were investigated.The results showed that the optimum reaction conditions for preparing n-butyl p-hydroxybenzoate were as follows. Excess of n- butanol acted as azeotropic water stripping agents, reaction time by refluxing was 3.Oh,the mass ratio of catalyst to p-hydroxy-benzoic acid was 3.5%, and the molar ratio of n-butanol and p-hydroxy benzoic acid was 3.0：1.0.Under these condition,the yield of the product reached 97.5%.Meanwhile,the products were characterized by melting point determination,elemental analysis, HPLC and IR spectrum.The results demonstrated that as-synthesized products were n-butyl p-hydroxybenzoate with high purity. Furthermore, the self-synthetical catalyst exhibited high catalytic activity, could be recycled and used for many times.

关 键 词：纳米稀土复合固体超强酸 SO4^2- ZrO2-2%Nd2O3 酯化反应 对羟基苯甲酸正丁酯 

分 类 号：TS202.3[轻工技术与工程—食品科学]