Catalytic Synthesis of Cyclohexanone 1 , 2 -Propanediol Ketal With Zr(SO4)2 /γ-Al2O3  Solid Acid

Journal of Liaoning Petrochemical University ›› 2007, Vol. 27 ›› Issue (2): 32-34.

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Catalytic Synthesis of Cyclohexanone 1 , 2 -Propanediol Ketal With Zr(SO₄)₂ /γ-Al₂O₃ Solid Acid

School of Petrochemical Engineerin , Liaoning University o f Petroleum & Chemical Technology ,Fushun Liaoning 113001 , P .R .China

Received:2006-09-18 Published:2007-06-20 Online:2017-07-05

Zr(SO₄)₂ /γ-Al₂O₃ 固体酸催化合成环己酮1 ,2 -丙二醇缩酮

高文艺, 任立国^＊

辽宁石油化工大学石油化工学院, 辽宁抚顺113001

作者简介:高文艺(1967 -), 男, 河南新郑市, 高级实验师。

Abstract

Abstract:

　Cyclohexanone 1, 2-propanediolketal was synthesized from cyclohexanone and 1, 2-propanediol with Zr(SO₄)₂ /γ-Al₂O₃ so lid acid catalyst prepared by impregnation -calcination processes.The effects of calcination temperature of catalyst ,mass fraction of catalyst , mole ratio of reactants , amount of entrainer , refluxing time were investigated.The optimal conditions are as follows :catalyst calcination temperature is 550 ℃, the mass fraction of Zr(SO₄)₂ is 20 %, the weight mass fraction of catalyst is 0.5 %, the mole ratio of cyclohexanone and 1, 2 -propanediol is 1 ∶1 .5 , toluenevolume is 15 m L, refluxing time is 3h .Under this condition, higher yield(90 .5 %)of the product with good purity(99 .6 %)can be obtained .

Key words: Solid acid, , Condensation reaction, , Cyclohexanone 1, 2 -propanediol ketal

摘要： 　通过直接浸渍-焙烧等方法, 制备了Zr(SO4)2/γ-Al2O3 催化剂, 以环己酮和1 , 2 -丙二醇为原料合成了环己酮1, 2-丙二醇缩酮。考察了催化剂的焙烧温度、催化剂的质量分数、原料摩尔比、带水剂体积、回流时间对反应的影响。最佳反应条件为:焙烧温度为550 ℃, Zr(SO4)2 的质量分数为20 .0%, 催化剂的质量分数为5 .0%,环己酮与1, 2-丙二醇的摩尔比为1∶1 .5 , 甲苯的体积为15 m L, 回流时间为3 h 。环己酮1 , 2 -丙二醇缩酮的收率可达98 .7 %, 纯度达到99 .6%。

关键词: 固体酸, 　缩合反应, 　环己酮1, 2-丙二醇缩酮

GAO Wen -y i,REN Li -g uo. Catalytic Synthesis of Cyclohexanone 1 , 2 -Propanediol Ketal With Zr(SO₄)₂ /γ-Al₂O₃ Solid Acid[J]. Journal of Liaoning Petrochemical University, 2007, 27(2): 32-34.

高文艺, 任立国. Zr(SO₄)₂ /γ-Al₂O₃ 固体酸催化合成环己酮1 ,2 -丙二醇缩酮[J]. 辽宁石油化工大学学报, 2007, 27(2): 32-34.

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Catalytic Synthesis of Cyclohexanone 1 , 2 -Propanediol Ketal With Zr(SO₄)₂ /γ-Al₂O₃ Solid Acid

Zr(SO₄)₂ /γ-Al₂O₃ 固体酸催化合成环己酮1 ,2 -丙二醇缩酮

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