硅胶固定吗啉功能化离子液体催化合成苯乙酮环乙二缩酮

Catalytic synthesis of acetophenone cycloethylene ketal by the morpholine functionalized acidic lionic liquid on silica gel

以硅胶为固定化载体,硫酸为功能性质子酸,以吗啉和1,3-丙烷磺内酯为起始物料,制备合成出了硅胶负载型吗啉酸性离子液体催化剂。以苯乙酮和乙二醇反应生成苯乙酮环乙二缩酮作为表征反应,通过对硅胶负载吗啉酸性离子液体催化剂用量、苯乙酮和乙二醇的投料比、缩羰基化反应时间、带水剂环己烷用量和催化剂重复使用性能等进行考察。结果表明,在苯乙酮和乙二醇物质的量1∶1.2,催化剂用量为苯乙酮质量的5%,带水剂环己烷用量为200 mL和反应时间4 h的最优工艺条件下,催化剂重复使用5次催化活性未见明显衰退,产物收率75%以上。并且催化剂具有易分离,操作简单,产品质量好的特点。

The morpholine functionalized acidic lionic liquid was designed and synthesized from morpholine,1,3-propane sulfolactone and sulfuric acid as protonic acid fixed on silica gel.With reaction of acetophenone and glycol to form acetophenone cycloethylene ketal as characterization reaction,influences of dosage of the morpholine functionalized acidic lionic liquid on silica gel catalyst,ratio of acetophenone to glycol,the carbonylation reaction time,the usage of water carrying cyclohexane agent,the recycle of catalyst were discussed,the best reaction conditions was found.The results showed when molar ratio of acetophenone to glycol was 1∶1.2,the amount of catalyst was 5%of the mass of acetophenone,the dosage of cyclohexane was 200 mL,and the reaction time was 4 h,the catalyst was reused for 5 times without obvious degradation of catalytic activity,and yield of the product was more than 75%under this optimal conditions.This method takes the advantages of simple operation,mild reaction conditions,high purity and yield of the product.