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.
出处
《食品工业科技》
CAS
CSCD
北大核心
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
