Citation: ZHUO Zuoxi, LIN Longfei, DENG Xiujuan, WANG Yuning, LIU Yueming. Fixed-bed process of liquid-phase ammoximation of cyclohexanone over titanosilicates[J]. Chinese Journal of Catalysis, ;2013, 34(3): 604-611. doi: 10.3724/SP.J.1088.2013.20939 shu

Fixed-bed process of liquid-phase ammoximation of cyclohexanone over titanosilicates

1.
Shanghai Key Laboratory of Green Chemistry and Chemical Processes, Department of Chemistry, EastChinaNormalUniversity, Shanghai 200062, China

Corresponding author: LIU Yueming,
Received Date: 30 September 2012
Available Online: 30 October 2012
Fund Project: 国家自然科学基金(20973064) (20973064) 国家科技支撑计划(2012BAE05B02) (2012BAE05B02) 上海市科委基础研究重点项目(12JC14030600) (12JC14030600) 上海市重点学科建设项目基金(B409). (B409)

Liquid-phase ammoximation of cyclohexanone to the corresponding oxime was conducted in a fixed-bed reactor over titanium silicalite (TS-1), which was proved to be a feasible and universal process. The primary rules of ammoximation were explored in the fixed-bed reactor system.The initial results indicated that the utilization of H₂O₂ was enhanced obviously through this mode, which is attributed to successful hydroxylamine generation and smooth contact with ketones. Further investigations of H₂O₂ reaction behavior showed that the proper weight hourly space velocity of H₂O₂ and the concentrations of ammonia and ketone both play a key role in highly efficient utilization of H₂O₂. The cyclohexanone and H₂O₂ conversion, cyclohexanone-oxime selectivity, and H₂O₂ efficiency reached 18.7%, 94.7%, 99.5%, and 98.7%, respectively, under the optimum reaction conditions of temperature of 333 K, ammonia concentration higher than 2%, cyclohexanone/H₂O₂ molar ratio of 5, and WHSV (H₂O₂)of 0.083h^-¹ with 85% t-BuOH as solvent.
- cyclohexanone,
- ammoximation,
- titanium silicalite,
- fixed bed,
- hydrogen peroxide
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