H_3PW_(12)O_(40)/SiO_2催化合成环己酮乙二醇缩酮

Synthesis of Cyclohexanone Ethylene Ketal Using H_3PW_(12)O_(40)/SiO_2 as Catalyst

采用溶胶-凝胶法制备了二氧化硅负载磷钨酸H3PW12O40/SiO2催化剂,并通过FTIR、XRD对其进行了表征。以环己酮和乙二醇为原料,合成了环己酮乙二醇缩酮,探讨了H3PW12O40/SiO2对缩酮反应的催化活性,考察了酮醇摩尔比、催化剂用量、带水剂用量、反应时间对产物收率的影响。结果表明,在n(环己酮)∶n(乙二醇)=1∶1.3,催化剂用量占反应物料总质量的1.2%,带水剂环己烷用量3 mL,反应时间45 min的最佳条件下,环己酮乙二醇缩酮收率可达89.7%。

A new environmental friendly catalyst,H3PW12O40/SiO2 was prepared by the sol-gel method, and characterized by means of FTIR and XRD. Cyclohexanone ethylene ketal was synthesized from cyclohexanone and ethylene glycol using H3PW12O40/SiO2 as catalyst. The influence factors on the yield of cyclohexanone ethylene ketal were also discussed. The optimum conditions were indentified ： molar ratio of cyclohexanone to ethylene glycol is 1 ： 1.3, mass fraction of catalyst to reactants is 1.2 %, cyclohexane dosage is 3 mL and reaction time is 45 min. The yield of cyclohexanone ethylene ketal can reach 89.7% under the optimum conditions.