二氧化钛负载磷钨钼杂多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

采用浸渍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TiO2和H3PW6Mo6O40的质量均为1.0 g,水的用量30 mL,浸渍时间12 h,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,在环己酮与乙二醇的摩尔比为1.0∶1.5、催化剂用量占反应物料总质量的1.0%、反应时间0.75 h的条件下,环己酮乙二醇缩酮的收率为87.7%。

A new environmentally friendly catalyst, H3PW6Mo6O40/TiO2 has been prepared. The optimum conditions have been found to be： masses of TiO2 and H3PW6Mo6O40 of 1.0 g, volume of water 30 mL, a soaking time of 12 h, and activation temperature of 150 ℃. H3PW6Mo6O40/TiO2 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, 1.0 % ; reaction time, 0.75 h and dried cyclohexane, 8 mL. Under these conditions, the yield of cyclohexanone ethylene ketal was 87.7 %.