摘要
制备了一种以苯并噻唑为阳离子和硫酸氢根为阴离子的新型磺酸官能化酸性离子液体[(CH2)3SO3HBth][HSO4],并用于催化环己酮与乙二醇的缩酮化反应。通过考察原料配比、反应时间、催化剂用量、带水剂用量和催化剂重复使用次数等因素对反应的影响,确定1,4-二氧螺环[4,5]癸烷合成工艺最佳条件为:环已酮用量0.01 mol,乙二醇用量0.02 mol,催化剂用量为环已酮物质的量的5%,带水剂环已烷用量10 mL,回流反应时间3 h。在此条件下,1,4-二氧螺环[4,5]癸烷收率97.30%,催化剂具有良好的稳定性,循环使用5次后,催化活性没有明显下降。
A novel sulfonic acid-functionalized ionic liquid [ （CH2 ）3SO3-HBth] [ HSO44] was prepared with benzothiazole as the cation and hydrogen sulfate as the anion, and was used for catalyzing the ketalization of cyclohexane with glycol. The effects of reaction time, mole ratio of reactants, the dosage of the water carrying agent and the catalyst, and the repeated use of the catalyst were investigated. The results showed that 1,4-dioxaspiro[4,51 decane yield of over 97.30% was attained under the optimal reaction condition as follows： cyclohexanone amount 0.01 mol, glycol amount 0.02 mol, catalyst dosage 5% of cyclohexane mol,the amount of water carrying agent cyclohexane 10 mL, reaction time 3 h. The catalyst possessed good stability, and its activity did not decrease obviously after repeated use for five times.
出处
《工业催化》
CAS
2013年第5期54-57,共4页
Industrial Catalysis
