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硅藻土负载Dawson结构磷钨酸催化合成对羟基苯甲酸正丁酯

Synthesis of Butyl p-Hydroxybenzoate over Diatomite Supported Phosphotungstic Acid with Dawson Structure

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【作者】 曹小华任杰柳闽生占昌朝严平

【Author】 Cao Xiaohua1,2,Ren Jie1,Liu Minsheng3,Zhan Changchao1,2,Yan Ping2(1.College of Chemical Engineering and Materials Science,Zhejiang University of Technology,Hangzhou Zhejiang 310014,China;2.School of Chemical and Environmental Engineering,Jiujiang University,Jiujiang Jiangxi 332005,China;3.College of Bio-Chemical and Environmental Engineering,Nanjing Xiaozhuang University,Nanjing Jiangsu 211171,China)

【机构】 浙江工业大学化学工程与材料学院九江学院化学与环境工程学院南京晓庄学院生物化工与环境工程学院

【摘要】 以硅藻土为载体,采用浸渍法制备了H6P2W18O62/硅藻土催化剂,并采用FTIR,EDS,XRD,SEM等手段对催化剂进行了表征;以对羟基苯甲酸正丁酯的合成反应为探针,考察了H6P2W18O62/硅藻土催化剂的性能;通过单因次和正交实验研究了H6P2W18O62负载量、催化剂用量、正丁醇与对羟基苯甲酸的摩尔比(醇酸比)、反应时间和反应温度对酯化反应的影响。确定了优化工艺条件为:H6P2W18O62负载量为40%(基于硅藻土的质量)、催化剂用量0.5 g(占反应体系总质量的2.8%)、醇酸比3、反应时间3.0 h、反应温度125℃。在此条件下,对羟基苯甲酸正丁酯的平均收率可达90.8%;催化重复使用5次,对羟基苯甲酸正丁酯收率仍可达65.6%。

【Abstract】 Diatomite supported phosphotungstic acids with Dawson structure were prepared by an impregnation method and used as catalysts for the synthesis of butyl p-hydroxybenzoate by the esterification of p-hydroxy benzoic acid with n-butyl alcohol.The effects of the catalyst preparation and reaction conditions on the esterification were investigated through orthogonal experiments.The yield of butyl p-hydroxybenzoate could reach 90.8% under the optimum conditions of phosphotungstic acid loading on the diatomite support 40%(based on the diatomite mass),mass ratio of the catalyst to the total reactants 2.8%,molar ratio of n-butyl alcohol to p-hydroxy benzoic acid 3,reaction time 3.0 h and reaction temperature 125 ℃.The catalyst could be reused for 5 times and the yield of butyl p-hydroxybenzoate was still kept at 65.6%.

【基金】 国家自然科学基金项目(21161009);江西省自然科学基金项目(20122BAB213001,20114BAB213002);江西省教育厅科技资助项目(GJJ10626,GJJ11613)
  • 【文献出处】 石油化工 ,Petrochemical Technology , 编辑部邮箱 ,2013年02期
  • 【分类号】O643.32
  • 【被引频次】20
  • 【下载频次】337
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