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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 PV-Mo-W quaternary heteropolyacids H3 + xPVxMoyW12-x-yO40.nH2O with Keggin structure (x = 1, 2 and 3) were synthesized and characterized by Fourier transform infrared spectroscopy and X-ray diffraction And other methods to characterize the structure of the heteropolyacid; Phosphorovanadomolybdotungstic heteropolyacid as a catalyst for the synthesis of acetophenone cyclic ethane ketal. Investigated the type of catalyst, alcohol-ketone molar ratio, the kind of water-carrying agent and the reaction conditions ( Catalyst dosage, the amount of water-carrying agent, reaction temperature, reaction time) on acetophenone ethylene ketal reaction under the optimal conditions, namely acetophenone 0.1 mol, ethylene glycol 0.14 mol, catalyst H6PV3MoW8O400.4 mmol , The reaction was carried out at 110 ℃ for 6 h, cyclohexane 15 mL, the conversion of acetophenone reached 84.1%, the selectivity of acetophenone ring ethylene ketal reached 99.4%.