H_3PW_6Mo_6O_(40)/TiO_2-WO_3催化合成环己酮乙二醇缩酮

Synthesis of cyclohexanone ethylene ketal using H_3PW_6Mo_6O_(40)/TiO_2-WO_3 as catalyst

以二氧化硅负载磷钨钼酸H3PW6Mo6O40/TiO2-WO3为催化剂,环己酮和乙二醇为原料合成环己酮乙二醇缩酮.探讨H3PW6Mo6O40/TiO2-WO3对环己酮乙二醇缩酮反应的催化活性,较系统地研究了酮醇物质的量比、催化剂用量、带水剂用量、反应时间等因素对产物收率的影响.实验表明:H3PW6Mo6O40/TiO2-WO3是合成环己酮乙二醇缩酮的良好催化剂,在n(环己酮)∶n(乙二醇)=1∶1.4,催化剂用量占反应物料总质量的1.0%,带水剂环己烷的用量为6 mL,反应时间60 min的最佳条件下,环己酮乙二醇缩酮的收率可达84.5%.

A new environmental friendly catalyst, H3PW6Mo6O40/TiO2-WO3 was prepared with the impregnation method, and characterized by FT-IR and XRD.Cyclohexanone ethylene ketal was synthesized from cyclohexanone and glycol using H3PW6Mo6O40/TiO2-WO3 as the catalyst.The influence factors on the yield of cyclohexanone ethylene ketal were also discussed.The optimum conditions were indentified： molar ratio of cyclohexanone and glycol is 1∶1.4, mass fraction of catalyst to reactants is 1.0%, cyclohexane dosage is 6 mL and reaction time is 60 minutes.The yield of cyclohexanone ethylene ketal can reach 84.5%under the optimum conditions.