环己酮肟溶剂重排制备己内酰胺工艺研究  

Preparation of caprolactam by solvent rearrangement of cyclohexanone oxime

作　　者：张晓辉 詹夏 ZHANG Xiaohui;ZHAN Xia(Caprolactam Division of SINOPEC Hunan Petrochemical Co.,Ltd.,Yueyang 414000)

机构地区：[1]中石化湖南石油化工有限公司己内酰胺部,湖南岳阳414000

出　　处：《合成纤维工业》2024年第3期52-55,共4页China Synthetic Fiber Industry

基　　金：中石化股份有限公司研究项目(219005-3)。

摘　　要：将环己酮肟溶解在惰性溶剂中,以发烟硫酸为催化剂催化环己酮肟贝克曼重排反应制备己内酰胺,考察了反应溶剂、溶剂加入量、酸肟比(发烟硫酸/环己酮肟摩尔比)、重排反应时间和反应温度对环己酮肟转化率和己内酰胺选择性的影响。结果表明:采用环己烷为溶剂,在反应时间1 h、溶剂中环己酮肟质量分数15%、酸肟比1.05、重排反应温度80℃的工艺条件下制备己内酰胺,环己酮肟转化率为100%,己内酰胺选择性达到99.2%;与传统己内酰胺生产工艺相比,溶剂重排工艺的反应温度低、能耗低、硫铵副产少。Cyclohexanone oxime was dissolved in an inert solvent and catalyzed by fuming sulfuric acid to prepare caprolactam through Beckmann rearrangement reaction.The effects of reaction solvents,solvent addition,acid oxime ratio(fuming sulfuric acid-to-cyclohexanone oxime mole ratio),rearrangement reaction time and temperature on the conversion rate of cyclohexanone oxime and selectivity of caprolactam were investigated.The results showed that the conversion rate of cyclohexanone oxime was 100%and the selectivity of caprolactam reached 99.2%when caprolactam was prepared using cyclohexane as the solvent under the process conditions of reaction time of 1 h,a mass fraction of cyclohexanone oxime in the solvent of 15%,a molar ratio of fuming sulfuric acid to cyclohexanone oxime of 1.05 and a rearrangement reaction temperature of 80℃;and the solvent rearrangement process had the advantages of lower reaction temperature,lower energy consumption and fewer by-products of ammonium sulfate compared to traditional caprolactam production processes.

关 键 词：环己酮肟 贝克曼重排 溶剂 环己烷 己内酰胺 

分 类 号：TQ340.42[化学工程—化纤工业]