二氧化钛负载磷钨钼酸催化合成环己酮乙二醇缩酮

Catalytic Synthesis of Cyclohexanone Ethylene Ketal with H_3PW_6Mo_6O_(40)/TiO_2

首次采用回流法制备了二氧化钛负载磷钨钼杂多酸催化剂H3PW6Mo6O40/TiO2,该催化剂的适宜制备条件为:原料质量比m(TiO2)∶m(H3PW6Mo6O40)=1∶2.0,水用量30mL,回流反应时间2.0h,活化温度150℃。以H3PW6Mo6O40/TiO2为催化剂,对以环己酮与乙二醇为原料合成环己酮乙二醇缩酮的反应条件进行了研究,较系统地研究了酮醇物质的量比、催化剂用量、反应时间对收率的影响。实验结果表明,在n(环己酮)∶n(乙二醇)=1.0∶1.5、催化剂用量占反应物料总质量的0.8%、反应时间1.0h的条件下,环己酮乙二醇缩酮的收率为86.3%。

A new environmental friendly catalyst, Mo6O40/TiO2 was prepared. The optimum conditions are found. That is, mass ratio of m（TiO2）：m（H3PW6Mo6O40） is 1：2.0, volume of water is 30 mL, the reflux reaction time is 2 h,and activated temperature is 150℃. H3PW6Mo6O40TiO2 was used as the catalyst in the synthesis of cyclohexanone ethylene ketal. The effects of varying the n（cyclohexanone）：n （glycol） ratio, catalyst dosage and reaction time on the yield were investigated. The optimal conditions were found to be： n （cyclohexanone）：n （glycol）=1：1.5; mass fraction of catalyst to reactants, 0.8%; reaction time, 1.0 h and dried cyclohexane, 8 mL. Under these conditions, the yield of cyclo- hexanone ethylene ketal was 86.3%.