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Beckmann rearrangement of cyclohexanone oxime to ε-caprolactam in microreactors

Authors

  • K. T. Zuidhof,

    1. Dept. of Chemical Engineering and Chemistry, Laboratory of Chemical Reactor Engineering, Eindhoven University of Technology, 5600 MB Eindhoven, The Netherlands
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  • M. H. J. M. de Croon,

    1. Dept. of Chemical Engineering and Chemistry, Laboratory of Chemical Reactor Engineering, Eindhoven University of Technology, 5600 MB Eindhoven, The Netherlands
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  • J. C. Schouten

    Corresponding author
    1. Dept. of Chemical Engineering and Chemistry, Laboratory of Chemical Reactor Engineering, Eindhoven University of Technology, 5600 MB Eindhoven, The Netherlands
    • Dept. of Chemical Engineering and Chemistry, Laboratory of Chemical Reactor Engineering, Eindhoven University of Technology, 5600 MB Eindhoven, The Netherlands
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Abstract

Selectivities are presented of the Beckmann rearrangement of cyclohexanone oxime to ε-caprolactam with oleum for various conditions in three microreactors, viz., Y-junction, interdigital, and split and recombine mixers, followed by a 50-cm long microchannel of 250 μm internal diameter. Cyclohexanone oxime is dissolved in cyclooctane, which is inert for oleum. The selectivity is measured in the temperature range of 80–132°C. The concentration range of caprolactam in the reaction mixture is 31–41 wt %, in oleum. The total volumetric flow rate is 0.4 ml/min, whereas the flow rate ratio of ε-caprolactam/oleum over cyclohexanone oxime/cyclooctane ranges from 0.3 to 3. The selectivities measured with the three microreactors are: 70–99+%, 93–99+%, and 95–99+%, respectively. High ε-caprolactam concentration (41 wt %), high temperature (110–132°C), and a ratio of free H2SO4 to SO3 of unity have a negative effect on the selectivity. © 2009 American Institute of Chemical Engineers AIChE J, 2010

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