微波辐射草酸催化合成环己酮乙二醇缩酮

微波辐射下,以草酸为催化剂、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、反应温度、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0.2 mol、n（环己酮）∶n（乙二醇）为1.0∶1.5、催化剂用量为反应物料总质量的2.2%、以20 mL环己烷为带水剂、微波功率为400 W、反应温度130℃和反应时间为25 min等优化条件下,环己酮乙二醇缩酮的收率可达67.7%。

Synthesis of Cyclohexanone Ethy Lene Ketal with Oxalic Acid as Catalyst under Microwave Irradiation

Cyclohexanone ethy lene ketal was synthesized under microwave irradiation with using oxalic acid as catalyst and hexam ethy lene as water carrying agent.The effects of molar ratio of cyclohexanone to glycol,microwave irradiation power,microwave irradiation time,reaction temperature,catalyst dosage and water-carrying agent amount,etc on the yield were discussed.The results showed that under the conditions of cyclohexanone was 0.2 mol,the molar ratio of n（cyclohexanone）∶n（glycol） was 1∶1.5,them icrowave irradiation power was 400 W,the mass ratio of the catalyst used was 2.2 % of the reactant mass,the water-carrying agent（cyclohexane） was 20 mL,the reaction temperature was 130 ℃ and the microwave irradiation time was 25 min,the yield of cyclohexanone ethy lene ketal could reach 67.7 %.