Reactors, Kinetics, and Catalysis

Beckmann rearrangement in a microstructured chemical system for the preparation of ε-caprolactam

  1. J. S. Zhang,
  2. K. Wang,
  3. Y. C. Lu,
  4. G. S. Luo*

Article first published online: 22 APR 2011

DOI: 10.1002/aic.12612

Issue

AIChE Journal

AIChE Journal

Volume 58, Issue 3, pages 925–931, March 2012

Additional Information

How to Cite

Zhang, J. S., Wang, K., Lu, Y. C. and Luo, G. S. (2012), Beckmann rearrangement in a microstructured chemical system for the preparation of ε-caprolactam. AIChE J., 58: 925–931. doi: 10.1002/aic.12612

Author Information

  1. The State Key Laboratory of Chemical Engineering, Dept. of Chemical Engineering, Tsinghua University, Beijing 100084, China

*The State Key Laboratory of Chemical Engineering, Dept. of Chemical Engineering, Tsinghua University, Beijing 100084, China

Publication History

  1. Issue published online: 6 FEB 2012
  2. Article first published online: 22 APR 2011
  3. Accepted manuscript online: 17 MAR 2011 12:32PM EST
  4. Manuscript Revised: 21 FEB 2011
  5. Manuscript Received: 23 NOV 2010

Funded by

  • National Natural Science Foundation of China. Grant Numbers: 20876084, 21036002
  • National Basic Research Program of China. Grant Number: 2007CB714302

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Keywords:

  • Beckmann rearrangement;
  • ϵ-caprolactam;
  • conversion;
  • selectivity;
  • microstructured chemical system

Abstract

A microstructured chemical system, constructed with a microsieve dispersion mixer, a delay loop and a microhydrolyzer is designed to carry out the Beckmann rearrangement of cyclohexanone oxime to ϵ-caprolactam. The system is operated with oleum as the dispersed phase, and cyclohexanone oxime n-octane solution as the continuous phase. The mixing performance, conversion of cyclohexanone oxime and selectivity to ϵ-caprolactam are investigated and the results show that the reaction can be very well controlled due to the formation of microdroplets ranging from 10–25 μm. Under optimized conditions, the reaction can be accomplished with a residence time less than 40 s, and the selectivity higher than 99%. A two-stage technology of low-temperature to induce reaction, and high-temperature to enhance reaction is developed, and the corresponding molar ratio of oleum to cyclohexanone oxime can be reduced to 0.8, which is much lower than the industrial value of 1.2. © 2011 American Institute of Chemical Engineers AIChE J, 2012

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