H3PW12O40/SiO2催化合成环己酮乙二醇缩酮

Synthesis of Cyclohexanone Ethylene Ketal Using H3PW12O40/SiO2 as Catalyst

摘要:

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FT-IR、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，考察了酮醇物质的量比、催化剂用量、带水剂用量、反应时间对产物收率的影响。研究结果表明，H3PW12O40/SiO2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∶1.3，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%。

Abstract:

A new environmental friendly catalyst, H3PW12O40/SiO2 was prepared with the sol-gel method, and characterized by FT-IR and XRD. Cyclohexanone ethylene ketal was synthesized from cyclohexanone and ethylene glycol using H3PW12O40/SiO2 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 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 minutes. The yield of cyclohexanone ethylene ketal can reach 89.7% under the optimum conditions.