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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。
The SO24- / ZrO2-TiO2 solid acid catalyst was prepared by coprecipitation method. The cyclohexanone and ethylene glycol were used as raw materials to synthesize cyclohexanone ethylene glycol ketal as probe reaction. The molar ratio of Ti to Zr, The time and the impregnation time on the catalyst activity. At the same time, the effects of different water-carrying agents, raw material ratio, reaction time and the amount of catalyst on the reaction yield were studied. The results show that the Ti / Zr ratio is 1: 1, the aging time is 180 min and the impregnation time is 20 min. The optimum reaction conditions were as follows: the molar ratio of ketone to alcohol was 1: 1.2, the amount of cyclohexanone was 0.2 mol, the amount of catalyst was 1.2 g, and the amount of cyclohexane was 15 mL. After 70 min of reaction, cyclohexanone ethylene ketal The yield of 93.1%. The catalyst was reused seven times and the yield remained above 85%.