纳米固体超强酸SO_4^(2-)/Fe_2O_3催化合成环己酮1,2-丙二醇缩酮

Synthesis of cyclohexanone 1,2-propanediolketal catalyzed by nanosolid superacid SO_4^(2-)/Fe_2O_3

以纳米固体超强酸SO_4^(2-)/Fe_2O_3为催化剂,催化环己酮和1,2-丙二醇的缩合反应,合成了环己酮1,2-丙二醇缩酮。研究焙烧温度、反应时间、酮醇物质的量比、带水剂用量和催化剂用量等对反应的影响。较适宜的反应条件为:环己酮200 mmol,酮醇物质的量比为1:1.1,催化剂用量为200 mg(占反应物总质量的2.9%),甲苯30 mL,温度(120～130)℃,反应2.5 h,环己酮1,2-丙二醇缩酮收率达97.4%,纯度>98%。

Cyclohexanone 1,2-propanedioketal was synthesized via esterifieation of cyclohexanone and 1,2-propanediol using SO4^2-/Fe2O3 nanosolid superacid as the catalyst. Influence of catalyst calcination temperature, reaction time, mole ratio of reactants, the dosage of water-carrying agent and the catalyst was investigated. The results showed that cyclohexanone 1,2-propanedioketal yield of 97.4% and its purity of over 98% were obtained under the optimum condition as follows： cyclohexanone amount 200 mmol, n （cyelohexanone）：n （1,2-propanediol） = 1： 1.1, catalyst dosage 200 mg （2.9% of the total mass of the reactants） ,toluene 30 mL,reaction temperature （120 -130） ℃ ,reaction time 2.5 h.