Chinese Journal of Chemical Engineering ›› 2012, Vol. 20 ›› Issue (5): 889-894.

• 催化、动力学与反应器 • 上一篇    下一篇

三相体系中TS-1分子筛催化环己酮氨肟化制环己酮肟

刘国清1,2; 吴剑2; 罗和安2   

  1. 1 School of Chemistry and Chemical Engineering, Hunan University of Science and Technology, Xiangtan 411201, China 2 School of Chemical Engineering, Xiangtan University, Xiangtan 411105, China
  • 收稿日期:2011-06-09 修回日期:2011-12-15 出版日期:2012-10-28 发布日期:2011-12-15

Ammoximation of cyclohexanone to cyclohexanone oxime catalyzed by titanium silicalite-1 zeolite in three-phase system

LIU Guoqing1,2; WU Jian2; LUO He’an2   

  1. 1 School of Chemistry and Chemical Engineering, Hunan University of Science and Technology, Xiangtan 411201, China 2 School of Chemical Engineering, Xiangtan University, Xiangtan 411105, China
  • Received:2011-06-09 Revised:2011-12-15 Online:2012-10-28 Published:2011-12-15

摘要： An innovative green process of producing ε-caprolactam was proposed by integrating ammoximation and Beckmann rearrangement effectively. As a first part of the new process, TS-1 molecular sieve-catalyzed synthesis of cyclohexanone oxime from cyclohexanone, ammonia and hydrogen peroxide was carried out in a batch plant. Cyclohexane was used as the solvent in the three-phase reaction system. The influences of essential process pa-rameters on ammoximation were investigated. Under the reaction conditions as catalyst content of 2.5% (by mass); H2O2/yclohexanone molar ratio of 1.10; NH3/cyclohexanone molar ratio of 2.20; reaction temperature of 343 K; reaction time of 5 h, high conversion of cyclohexanone and selectivity to oxime (both>99%) were obtained. Thus, the three-phase ammoximation process showed equal catalytic activity as TS-1 but much more convenient and sim-pler for the separation of catalyst in comparison to the industrial two-phase system with t-butanol used as solvent.

关键词: ammoximation, molecular sieve TS-1, cyclohexanone oxime, cyclohexane, three-phase system

Abstract: An innovative green process of producing ε-caprolactam was proposed by integrating ammoximation and Beckmann rearrangement effectively. As a first part of the new process, TS-1 molecular sieve-catalyzed synthesis of cyclohexanone oxime from cyclohexanone, ammonia and hydrogen peroxide was carried out in a batch plant. Cyclohexane was used as the solvent in the three-phase reaction system. The influences of essential process pa-rameters on ammoximation were investigated. Under the reaction conditions as catalyst content of 2.5% (by mass); H2O2/yclohexanone molar ratio of 1.10; NH3/cyclohexanone molar ratio of 2.20; reaction temperature of 343 K; reaction time of 5 h, high conversion of cyclohexanone and selectivity to oxime (both>99%) were obtained. Thus, the three-phase ammoximation process showed equal catalytic activity as TS-1 but much more convenient and sim-pler for the separation of catalyst in comparison to the industrial two-phase system with t-butanol used as solvent.

Key words: ammoximation, molecular sieve TS-1, cyclohexanone oxime, cyclohexane, three-phase system

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