Beckmann rearrangement of cyclohexanone oxime dissolved in cyclooctane with oleum to ¿-caprolactam was demonstrated in a microreactor setup with internal recirculation operated in continuous mode. The core of the setup comprised a 316 stainless-steel micromixer consisting of 17 split-and-recombine units connected to a delay loop, a 316 stainless-steel microchannel reactor with an internal diameter of 0.250¿mm and a length of 0.50¿m. At 100¿°C, the conversion of cyclohexanone oxime was complete and the selectivity towards ¿-caprolactam was approximately 99¿%. The solvent cyclooctane reduces the observed purity of the produced oleum/¿-caprolactam. This reduction in purity might be a severe hurdle for usage of a solvent on the industrial scale in the Beckmann rearrangement of cyclohexanone oxime in oleum to ¿-caprolactam.
Zuidhof, K. T., Croon, de, M. H. J. M., Schouten, J. C., & Tinge, J. T. (2013). Beckmann rearrangement of cyclohexanone oxime in microreactor setup with internal recirculation. Chemical Engineering & Technology, 36(8), 1387-1394. https://doi.org/10.1002/ceat.201300088