Journal of Liaoning Petrochemical University

Journal of Liaoning Petrochemical University ›› 2010, Vol. 30 ›› Issue (1): 37-40.DOI: 10.3696/j.issn.1672-6952.2010.01.011

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

REN Li-guo1, ZHANG Xiao-li1, YU Ji-wei2   

  1.  
    1.School of Chemistry and Materials Science,Liaoning Shihua University, Fushun Liaoning 113001,P.R.China; 
    2.Catalysts Factory of Fushun Petrochemical Company,Fushun Liaoning 113001,P.R.China
  • Received:2009-09-15 Published:2010-03-25 Online:2017-07-05

Fe 2(SO4)3/SiO2 催化合成环己酮1,2-丙二醇缩酮

任立国1,张晓丽1,余济伟2   

  1. 1.辽宁石油化工大学化学与材料科学学院,辽宁抚顺113001;2.抚顺石化公司催化剂厂,辽宁抚顺113001
  • 作者简介:任立国(1963-),男,山东郓城县,教授,硕士。

Abstract: Cyclohexanone 1,2-propanediol ketal was synthesized by using cyclohexanone 1,2-propylene glycol as starting materials and silica-supported ferric sulfate \[Fe2(SO4)3/SiO2\] 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 Fe2(SO4)3/SiO2 solid acid catalyst, the mass fration of Fe2(SO4)3, molar ratio of the reactant,reaction time,mass fraction of catalyst and its stability,were investigated in detail. The results show that the Fe2(SO4)3/SiO2 has high catalytic activities. The optimal reaction conditions are: calcination temperatures of Fe2(SO4)3/SiO2 solid acid catalyst 300 ℃, the mass fration of Fe2(SO4)3 in SiO2 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%. Fe2(SO4)3/SiO2 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

Key words: Sol-gel ,  , Ferric sulfate ,  Solid acid ,   Ketalization ,  Cyclohexanone 1,2-propanediol ketal

摘要: 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%。

关键词: 溶胶-胶凝,  , 硫酸铁 ,  , 固体酸 , 缩酮化反应 , 环己酮1, 2-丙二醇缩酮

Cite this article

REN Li-guo, ZHANG Xiao-li, YU Ji-wei. Synthesis of Cyclohexanon 1,2-Propanediol  Ketal Over Fe2(SO4)3/SiO2 Catalyst[J]. Journal of Liaoning Petrochemical University, 2010, 30(1): 37-40.

任立国,张晓丽,余济伟. Fe 2(SO4)3/SiO2 催化合成环己酮1,2-丙二醇缩酮[J]. 辽宁石油化工大学学报, 2010, 30(1): 37-40.