微波辐射稀土复合固体超强酸SO4^2-／ZrO2／Gd^3＋催化合成环己酮乙二醇缩酮

以环己酮和乙二醇为原料,稀土复合固体超强酸SO_4~(2-)/ZrO_2/Gd~(3 )为催化剂,在微波辐射和无溶剂下,合成环己酮乙二醇缩酮。探讨了酮醇物质的量比、催化剂用量、微波功率和辐射时间对产品收率的影响。结果表明,环己酮乙二醇缩酮的最佳合成条件为:n(环己酮):n(乙二醇)=1:3.0,催化剂用量为反应物总质量的1.50%,微波功率为425W,辐射时间为10min。在此条件下,缩酮收率可达90.4%,说明稀土复合固体超强酸SO_4~(2-)/ZrO_2/Gd~(3 )是一种合成环己酮乙二醇缩酮的优良催化剂。

Synthesis of cyclohexanone glycol ketal catalyzed by rare earth composite solid superacid SO42-/ZrO2/Gd3+ under microwave radiation

Cyclohexanone glycol ketal was synthesized using cyclohexanone and glycol as reactants and rare earth composite solid superacid SO_4~(2-)/ZrO_2/Gd~(3 )as catalysts without solvent under microwave irradiation.The effects of reactant molar ratio,amount of catalyst,microwave irradiation power,micro- wave irradiation time on the yield of cyclohexanone glycol ketal were studied.The optimal conditions were as follows:n(cyclohexanone):n(glycol)= 1:3.0,mass ratio of catalyst to reactant 1.50 %,mi- crowave irradiation power 425 W and radiation time 10 min.Under these conditions,the yield of cyclo- hexanone glycol ketal could be reach 90.4%,indicating that rare earth composite solid superacid SO_4~(2-)/ZrO_2/Gd~(3 )is a good catalyst for the synthesis of cyclohexanone glycol ketal.