碳基固体酸催化合成环己酮甘油缩酮的研究

doi:10.3696/j.issn.1006-396X.2011.02.009

石油化工高等学校学报 ›› 2011, Vol. 24 ›› Issue (2): 35-39.DOI: 10.3696/j.issn.1006-396X.2011.02.009

碳基固体酸催化合成环己酮甘油缩酮的研究

高文艺,张晓丽,任立国

辽宁石油化工大学化学与材料科学学院,辽宁抚顺113001

收稿日期:2010-12-16 修回日期:2011-03-04 出版日期:2011-04-25 发布日期:2011-04-25
作者简介:高文艺(1967 -), 男, 河南新郑市, 高级实验师, 硕士
基金资助:
辽宁省教育厅资助项目(05L299)

Synthesis of Cyclohexanone Glyceryl Ketal Using Carbon-Based Solid Acid as Catalyst

School of Chemistry & Materials Science, Liaoning Shihua University, Fushun Liaoning 113001,P.R.China

Received:2010-12-16 Revised:2011-03-04 Published:2011-04-25 Online:2011-04-25

摘要/Abstract

摘要： 　利用膨化淀粉与对甲基苯磺酸的部分炭化过程制备碳基固体酸催化剂, 用XRD、红外光谱、元素分析和热分析进行了表征, 研究了碳基固体酸催化剂在环己酮甘油缩酮合成中的催化性能, 考察甘油与环己酮物质的量比、催化剂用量和反应时间等因素的影响。XRD 分析和酸碱电位滴定结果表明, 膨化淀粉和对甲基苯磺酸混合物的部分炭化生成含有高密度-SO3H 基团的芳香碳薄层组成的无定形碳。在n(甘油)/ n(环己酮)= 1.2 、催化剂的质量分数为10 %、环己烷15 mL(占液体反应物总量的10%)和回流反应时间为120 min 的条件下, 环己酮甘油缩酮的收率可达到99 .2 %。催化剂重复使用8 次后, 活性下降很小。

关键词: 碳基固体酸 , 缩合 , 环己酮 , 甘油 , 缩酮

Abstract: Amorphous carbon material prepared from expanded starch and p-toluene sulfonic acid had been examined as a novel strong solid acid catalyst. The catalytic performances were studied on condensation of cyclohexanone with glycerol and characterized by XRD, IR,elementary analysis and TGA.The effects of molar ratio of glycerol with cyclohexanone, catalyst concentration and reaction time were discussed. The results of XRD and acid-base titration indicate the incompletely carbonization of the mixtures of expanded starch and p-toluene sulfonic acid results in amorphous carbon consisting of small polycyclic aromatic carbon sheets with high density of -SO3H groups. When the condensation reaction was carried out with n(glycerol)/n(cyclohexanone)1.2, mass fraction of catalyst 10%, cyclohexane 15 mL（Accounts for 10% of the total amount of liquid reactant ） and refluxe time of 120 min，the maximum yield of ketals is 99.2％. There was very little change in the catalytic activity of the regenerated catalyst，even after eight cycles. 

Key words:

Carbon-based solid acid, , Condensation, , Cyclohexanone, , Glycerol, , Ketal

高文艺,张晓丽,任立国. 碳基固体酸催化合成环己酮甘油缩酮的研究[J]. 石油化工高等学校学报, 2011, 24(2): 35-39.

GAO Wen-yi, ZHANG Xiao-li, REN Li-guo. Synthesis of Cyclohexanone Glyceryl Ketal Using Carbon-Based Solid Acid as Catalyst[J]. Journal of Petrochemical Universities, 2011, 24(2): 35-39.

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碳基固体酸催化合成环己酮甘油缩酮的研究

Synthesis of Cyclohexanone Glyceryl Ketal Using Carbon-Based Solid Acid as Catalyst

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