Synthesis of ε-Caprolactone by Oxidation of Cyclohexanone with Monoperoxysuccinic Acid
Synthesis of ε-Caprolactone by Oxidation of Cyclohexanone with Monoperoxysuccinic Acid作者机构:School of Chemical Engineering Wuhan University of Technology Wuhan 430070 China
出 版 物:《Chinese Journal of Chemical Engineering》 (中国化学工程学报(英文版))
年 卷 期:2013年第21卷第12期
页 面:1404-1409页
核心收录:
学科分类:0710[理学-生物学] 0830[工学-环境科学与工程(可授工学、理学、农学学位)] 081702[工学-化学工艺] 08[工学] 0817[工学-化学工程与技术] 0805[工学-材料科学与工程(可授工学、理学学位)] 0703[理学-化学]
基 金:supported by Henan Coal Chemical Industry Group Co. Jiangsu Qiangquan Chemical Reagent Co.
主 题:ε-己内酯 过氧化氢 环己酮 合成 琥珀酸酐 PSA 无催化剂 异构系统
摘 要:In the absence of catalyst,70%hydrogen peroxide was used to oxidize succinic anhydride to solid monoperoxysuccinic acid(PSA).Then PSA was applied to synthesis ofε-caprolactone(ε-CL)by oxidation of cyclohexanone in the heterogeneous system.In order to achieve material recycle,solid precipitated in the process of synthesizingε-CL was dehydrated via reactive distillation followed by recrystallization to prepare succinic anhydride,which was characterized by IR(infrared spectra)and1HNMR(1H nuclear magnetic resonance).Effects of molar ratio of PSA to cyclohexanone,acetic acid dosage,reaction temperature,reaction time on conversion of cyclohexanone,yield and selectivity ofε-CL were investigated respectively.The results indicated that conversion of cyclohexanone,yield and selectivity ofε-CL were upto 98.1%,97.5%and 99.4%respectively under the optimal conditions.In addition,in the process of synthesizing succinic anhydride,the optimal yield of succinic anhydride reached 67.4%.