Keggin型多元杂多酸催化合成苯乙酮环乙二缩酮  

Synthesis of Acetophenone cylic ethylic ketal by the Keggin Type Multicomponent heteropoly acids

作　　者：李贵贤[1] 赵军龙[1,2] 余华[1] 滕志君[1] 宋维维[1] 

机构地区：[1]兰州理工大学石油化工学院,甘肃兰州730050 [2]甘肃银光聚银化工有限公司,甘肃白银730900

出　　处：《分子催化》2010年第2期129-135,共7页Journal of Molecular Catalysis(China)

基　　金：甘肃省教育厅科研基金项目(2005GJ0281)

摘　　要：合成了一系列具有Keggin结构的P-V-Mo-W四元杂多酸H3+xPVxMoyW12-x-yO40.nH2O(其中,x=1,2和3),采用傅里叶变换红外光谱和X射线衍射等方法表征了杂多酸的结构;以磷钒钼钨杂多酸为催化剂合成苯乙酮环乙二缩酮.考察了催化剂的种类、醇酮摩尔比、带水剂的种类和反应条件(催化剂用量、带水剂用量、反应温度、反应时间)对苯乙酮乙二醇缩酮反应的影响.在优化条件下,即苯乙酮0.1 mol、乙二醇0.14 mol、催化剂H6PV3MoW8O400.4 mmol、在110℃反应6 h、带水剂环己烷15 mL,苯乙酮的转化率达到84.1%、苯乙酮环乙二缩酮的选择性达到99.4%.A series of multicomponent heteropoly acids H3 ＋x PVx Moy W12x.y O40 ·nH2O with Keggin structure were synthesized and proved by FT-IR and X-ray spectroscopies. Aeetophenone cylic ethylic ketal was efficiently synthesized over catalysts H3＋xPVxMOyW12-x-yO40. Effects of the type of catalyst, the kind of water-carrying agents, the amount of catalyst and the water-carrying agents, the molar ratio of ethylene glycol to acetophenone, reaction temperature and time were investigated. Under the optimal conditions, i. e. , with 0.1 mol of acetophenone, 0.14 mol of ethylene glycol and 0.4 mmol of H6PV3MoW8O40catalyst, reaction temperature 110℃, 15 mL cyclohexane as the water-carrying agents, 84.1% conversion of acetophenone and 99.4% selectivity for acetophenone cylic ethylic ketal were achieved within 6 h. P-V-

关 键 词：磷钒钼钨杂多酸 环己烷 缩酮 苯乙酮 苯乙酮环乙二缩酮 

分 类 号：O643.3[理学—物理化学]