毛志红,王洁,李贵贤,王小瑞,王成君.硅烷化凹凸棒负载H5PV2Mo10O40催化合成苯甲醛乙二醇缩醛[J].分子催化,2011,(5):393-399
硅烷化凹凸棒负载H5PV2Mo10O40催化合成苯甲醛乙二醇缩醛
Synthesis of Benzaldehyde cylic ethylic acetal by the H5PMo10V2O40 Immobilized on Silylated Palygorskite
投稿时间:2011-09-28  修订日期:2011-10-09
DOI:
中文关键词:  杂多酸 硅烷化凹凸棒石 缩醛 催化
英文关键词:heteropoly acid  silanized palygorskite  acetal  catalysis
基金项目:
作者单位E-mail
毛志红 兰州理工大学石油化工学院 magnate1993@163.com 
王洁 兰州理工大学 magnate1993@163.com 
李贵贤* 兰州理工大学 lgxgd@lut.cn 
王小瑞 兰州理工大学 270762693@qq.com 
王成君 兰州理工大学 573728404@qq.com 
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中文摘要:
      以酸活化的凹凸棒石Pa为原料,用3-氨丙基三乙氧基硅烷(APTES)嫁接的方法制备了3-氨丙基三乙氧基硅烷(3-aminopropyl-triethoxysilane, APTES)硅烷化凹凸棒石(PaAPTES)负载的Keggin型杂多酸催化剂(H5PMo10V2O40/PaAPTES),并用红外光谱分析、X射线衍射、Brunauer– Emmett–Teller (BET)比表面积测定对催化剂进行了表征。以苯甲醛与乙二醇的缩合为探针反应,详细探讨了影响缩醛反应的各种因素,得出苯甲醛与乙二醇缩醛反应的最佳条件:在115 ℃反应120 min、乙二醇:苯甲醛=1.75:1、催化剂H5PMo10V2O40/PaAPTES的用量0.1g、带水剂环己烷8 mL,苯甲醛的转化率达到95.49%、苯甲醛环乙二缩醛的选择性99.22%。硅烷化凹凸棒固载的催化剂H5PMo10V2O40/PaAPTES便于从反应体系中分离重复利用多次。
英文摘要:
      The surface of acid-activated palygorskite (Pa) was modified by grafting 3-aminopropyl-triethoxysilane (the silylated Pa denoted PaAPTES) for immobileizetion of molybdovanadophosphoric heteropoly acids (H5PMo10V2O40,). The samples were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Brunauer–Emmett– Teller (BET) specific area measurement.The catalytic activity was tested for the acetal of benzaldehyde with ethylene glycol, under the optimal conditions, i.e., 115 ℃ as reaction temperature, ethylene glycol:acetophenone=1.75:1 and 0.1 g of H5PMo10V2O40/PaAPTES catalyst, 8 mL of cyclohexane as the water-carrying agents, 95.49% conversion of benzaldehyde and 99.22% selectivity for benzaldehyde cylic ethylic acetal were achieved within 120min. The recycling tests show that the catalyst can be easily separated from the reaction system.
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