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中国精品科技期刊2020
冯纪南, 邓斌, 杨佳, 黄海英. 纳米稀土复合固体超强酸SO42-/ZrO2-2% Nd2O3催化合成对羟基苯甲酸正丁酯[J]. 食品工业科技, 2014, (03): 253-257. DOI: 10.13386/j.issn1002-0306.2014.03.019
引用本文: 冯纪南, 邓斌, 杨佳, 黄海英. 纳米稀土复合固体超强酸SO42-/ZrO2-2% Nd2O3催化合成对羟基苯甲酸正丁酯[J]. 食品工业科技, 2014, (03): 253-257. DOI: 10.13386/j.issn1002-0306.2014.03.019
FENG Ji-nan, DENG Bin, YANG Jia, HUANG Hai-ying. Synthesis of n-butyl p-hydroxybenzoate catalyzed by nanometer rare earth composite solid superacid SO42-/ZrO2-2% Nd2O3[J]. Science and Technology of Food Industry, 2014, (03): 253-257. DOI: 10.13386/j.issn1002-0306.2014.03.019
Citation: FENG Ji-nan, DENG Bin, YANG Jia, HUANG Hai-ying. Synthesis of n-butyl p-hydroxybenzoate catalyzed by nanometer rare earth composite solid superacid SO42-/ZrO2-2% Nd2O3[J]. Science and Technology of Food Industry, 2014, (03): 253-257. DOI: 10.13386/j.issn1002-0306.2014.03.019

纳米稀土复合固体超强酸SO42-/ZrO2-2% Nd2O3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 SO42-/ZrO2-2% Nd2O3

  • 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。 

     

    Abstract: Rare earth composite solid superacid SO2- 4 /ZrO 2-2% Nd 2 O 3 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 3.0h, 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.

     

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