SO_4^(2-)/ZrO_2-TiO_2固体酸催化合成环己酮乙二醇缩酮  

Synthesis of cyclohexanon ethylene ketal catalyzed by SO_4^(2-)/ZrO_2-TiO_2 solid acid

作　　者：王敏[1] 张恒[1] 李言信[1] 赵斌[1] 

机构地区：[1]曲阜师范大学化学与化工学院,山东曲阜273165

出　　处：《工业催化》2010年第1期62-65,共4页Industrial Catalysis

基　　金：山东省自然科学基金资助(Z2008B12)

摘　　要：采用共沉淀法制备了SO24-/ZrO2-TiO2固体酸催化剂,以环己酮和乙二醇为原料合成环己酮乙二醇缩酮为探针反应考察了Ti与Zr物质的量比、陈化时间和浸渍时间等对催化剂活性的影响。同时研究了不同带水剂、原料配比、反应时间和催化剂用量等因素对反应收率的影响。结果表明,Ti与Zr物质的量比为1∶1、陈化180 min和浸渍20 min的条件下制得催化剂活性最高。最佳反应条件为:酮与醇物质的量比1∶1.2,环己酮用量0.2 mol时催化剂1.2 g,带水剂环己烷15 mL,反应70 min后,环己酮乙二醇缩酮的收率达93.1%。催化剂重复使用7次,收率保持在85%以上。Cyclohexanon ethylene ketal was synthesized from cyclohexanon and ethylene using SO4^2-/ ZrO2-TiO2 solid acid as the catalyst. Effects of Ti/Zr mole ratio, aging time, impregnation time on its catalytic behaviors and effects of water-carrying agent, feed proportion, reaction time and catalyst dosage on yield of the product were investigated. Optimum condition for preparation of the catalyst was obtained as follows ： Ti/Zr mole ratio of 1 ： 1, aging time of 180 min, impregnation time of 20 min. Optimum reac- tion condition was obtained as follows： cyclohexanon to ethylene molar ratio 1： 1.2, 1.2 g catalyst, 15 mL cyclohexane for 0.2 mol cyclohexanon. Cyclohexanon ethylene ketal yield of 93.1% was attained after reaction for 70 min. The catalyst could be repeatedly used for 7 cycles with product yield of over 85%.

关 键 词：有机合成化学 固体酸催化剂 环己酮乙二醇缩酮 共沉淀法 

分 类 号：O643.36[理学—物理化学] O623.59[理学—化学]