Fe 2(SO4)3/SiO2 催化合成环己酮1,2-丙二醇缩酮

采用溶胶-胶凝法和浸渍法制备了二氧化硅负载的硫酸铁Fe₂(SO₄)₃/SiO₂]固体酸催化剂,以环己 酮和1,2-丙二醇为原料,在无溶剂条件下合成了环己酮1,2-丙二醇缩酮。考察了Fe₂(SO₄)₃/SiO₂ 固体酸催化剂 的焙烧温度、Fe₂(SO₄)₃ 在SiO₂ 上的负载量、醇酮物质的量比、催化剂质量和反应时间等因素对产品收率的影响。 实验结果表明,Fe₂(SO₄)₃/SiO₂ 固体酸是合成环己酮1,2-丙二醇缩酮的理想催化剂,较适宜的反应条件为:催化 剂的焙烧温度300℃、Fe₂(SO₄)₃ 在SiO₂ 上的负载量20%、环己酮与1,2-丙二醇的物质的量比1∶1、催化剂质量 分数5%和反应时间70min。在此条件下,环己酮1,2-丙二醇缩酮收率达到98.21%。Fe₂(SO₄)₃/SiO₂催化剂具 有良好的稳定性,重复使用5次后环己酮1,2-丙二醇缩酮的收率为88.90%。

Synthesis of Cyclohexanon 1,2-Propanediol Ketal Over Fe2(SO4)3/SiO2 Catalyst

Cyclohexanone 1,2-propanediol ketal was synthesized by using cyclohexanone 1,2-propylene glycol as starting materials and silica-supported ferric sulfateFe_2(SO_4)_3/SiO_2]solid acid as a catalyst under solvent-less conditions.The catalyst was prepared by sol-gel and impregnation methods.Efects of factors on yield of product,such as calcination temperature of Fe_2(SO_4)_3/SiO_2 solid acid catalyst,the mass fration of Fe_2(SO_4)_3,molar ratio of the reactant,reaction time, mass fraction of catalyst and its stability,were investigated in detail.The results show that the Fe_2(SO_4)_3/SiO_2 has high catalytic activities.The optimal reaction conditions are:calcination temperatures of Fe_2(SO_4)_3/SiO_2 solid acid catalyst 300℃, the mass fration of Fe_2(SO_4)_3 in SiO_2 20%,molar ratio of cyclohexanone to 1,2-propanediol 1:1,the mass fraction of catalyst 5%and the reaction time 70 min.Under the above conditions the yield of cyclohexanone 1,2-propanediol ketal is 98.21%.Fe_2(SO_4)_3/SiO_2 catalyst is excellent in stability and reusability,and yield of cyclohexanone 1,2- propanediol ketal keeps at 88.90%after being used for 5 times.