二氧化硅负载磷钨酸催化合成环己酮1,2-丙二醇缩酮  

Synthesis of cyclohexanone 1,2-propanediol ketal with H_3PW_(12)O_(40)/SiO_2 as catalyst

作　　者：徐明波[1] 刘晓[1] 王娟[1] 喻莉[1] 杨水金[1] 

机构地区：[1]湖北师范学院化学与环境工程学院污染物分析与资源化技术湖北省重点实验室,湖北黄石435002

出　　处：《日用化学工业》2012年第6期440-442,451,共4页China Surfactant Detergent & Cosmetics

基　　金：湖北省教育厅中青年科研基金资助项目(Q20112507)

摘　　要：采用溶胶-凝胶法制备了二氧化硅负载磷钨酸(H3PW12O40/SiO2),以红外光谱和X射线衍射谱对其进行了表征;并以其为催化剂,环己酮和1,2-丙二醇为原料合成了环己酮1,2-丙二醇缩酮。研究了酮醇摩尔比、催化剂用量、反应时间等因素对产物收率的影响,探讨了H3PW12O40/SiO2对缩酮反应的催化活性。实验结果表明:在固定环己酮用量为0.2 mol,n(环己酮)∶n(1,2-丙二醇)=1∶1.3,催化剂的用量占反应物总质量的1.3%,环己烷用量为6 mL,反应时间为45 min的条件下,产品收率可达88.1%。H3PW12O40/SiO2 catalyst was prepared by solgel method. The catalyst was characterized by infra red spectrum and X -ray diffraction pattern. By using this catalyst, eyclohexanone 1,2 -propanediol ketal was synthesized with cyclohexanone and 1,2 -propanediol as starting materials. Factors that influencing the synthesis, such as molar ratio of the starting materials, dosage of the catalyst and reaction time et al on the yield of the product were examined and the catalytic activity of the H3PW12O40/SiO2 catalyst was investigated. Experimental results showed that on the basis of 0. 2 mol of cyclohexanone, when molar ratio of cyclohexanone to 1,2 -propanediol is 1： 1.3, dosage of the catalyst is 1.3 % of total mass of the starting materials, volume of cyclohexane as water stripping agent is 6 mL, and the reaction time is 45 min, yield of the product achieves 88.1%.

关 键 词：香料 环己酮1  2-丙二醇缩酮 催化合成 

分 类 号：TQ234.21[化学工程—有机化工]