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在微波辐射下,以硅钨酸为催化剂、环己烷为带水剂,合成了环己酮乙二醇缩酮。考察了催化剂的用量、反应时间、酮醇物质的量之比、带水剂的用量及微波功率等诸多因素对产品收率的影响。实验表明,在环己酮用量为0.2mol、n(环己酮)∶n(乙二醇)=1.0∶1.35、催化剂用量为反应物料总质量的2.7%、以15mL环己烷为带水剂、微波功率为500W和反应时间为30 min等优化条件下,环己酮乙二醇缩酮的收率可达71.8%。
Under microwave irradiation, cyclohexanone ethylene glycol ketal was synthesized by using silicotungstic acid as a catalyst and cyclohexane as a water-carrying agent. The influences of the amount of catalyst, reaction time, the ratio of ketone to alcohol, the amount of water-carrying agent and microwave power on the product yield were investigated. The experiments show that when the amount of cyclohexanone is 0.2mol, n (cyclohexanone): n (ethylene glycol) = 1.0:1.35, the amount of catalyst is 2.7% of the total mass of the reaction mass, 15mL of cyclohexane , Microwave power of 500W and reaction time of 30 min under the optimal conditions, cyclohexanone ethylene ketal yield of 71.8%.