H_6P_2W_9Mo_9O_(62)/SiO_2催化合成环己酮乙二醇缩酮

Synthesis of Cyclohexanone Ethylene Ketal Catalyzed by H_6P_2W_9Mo_9O_(62)/SiO_2

使用溶胶凝胶法合成H_6P_2W_9Mo_9O_(62)/SiO_2,利用X射线衍射仪(XRD)、红外拉曼光谱仪(FT-IR)、差热分析仪(TG)及扫描电镜(SEM)分析H_6P_2W_9Mo_9O_(62)/SiO_2的热稳定性、结构和形貌。以环己酮和乙二醇为反应原料,H_6P_2W_9Mo_9O_(62)/SiO_2为催化剂,合成环己酮乙二醇缩酮,采用正交试验法,探讨了醇酮物质的量比、催化剂加量、反应时间、环己烷加量对合成缩酮的影响。结果表明,当n(环己酮)∶n(乙二醇)=1∶1.3、催化剂质量为反应物总质量的0.8%、带水剂加量8 mL、反应时间45 min时,环己酮乙二醇缩酮收率可达80.4%。

H6P2W9Mo9062/SiO2 was synthesized in a sol -gel process, and the thermal stability, structure and morphology of H6P2W9Mo9062/SiO2 were analyzed with X -ray diffractometer （XRD） , FTIR Raman spectrometer , differential thermal analyzer （TG） and scanning electron microscope （SEM）. Cyclohexanone ethylene ketal was synthesized with eyclohexanone and ethylene glycol as the reaction materials and H6P2WgMo9062/SiO2 as the catalyst, and the effects of the molar ratio of alcohol ketone, the catalyst amount, the reaction time, and the cyelohexane amount on the synthesis of ketal were studied. According to the results, the yield of cyclohexanone ethylene ketal can reach 80. 4% at the following conditions, i.e. n （cyclohexanone） ： n （ ethylene glycol） = 1 ： 1.3, the catalyst amount accounts for 0. 8 % of total reactants, and the reaction time is 45 min.