Catalyst preparation for vapor phase Beckmann rearrangement via deboronation/desilication of B-ZSM-5

Masahiko Matsukata, Kohsuke Nakagawa, Yasushi Sekine, Eiichi Kikuchi

Research output: Chapter in Book/Report/Conference proceedingConference contribution

Abstract

Vapor phase Beckmann rearrangement of cyclohexanone oxime to ε-caprolactam is an outstanding achievement of green chemistry. Nest silanols in the vicinity of the external surface of silicalite-1 has been proposed as active sites. In this study, B-ZSM-5(Si/B ratio = 25) was synthesized and the product was agglomerates of nanocrystals. As-made B-ZSM-5 was calcined in air and deboronated by treatment with HCl aq. at 353 K for 3 h. Further, the deboronated sample was desilicated with a mixture of ammonia nitrate and ammonia to develop effective diffusion pathways in the catalyst particles. FT-IR study confirmed the formation of abundant nest silanols. The vapor phase Backmann reaggrangement was performed in a plug flow reactor with a fixed bed of catalyst at WHSV = 8 h-1 and 653 K. The initial catalytic activity was greatly improved by the treatment performed in this study: The pseudo-first-order reaction constant for the parent B-ZSM-5 was 1.8×10-3 s-1, but that for the deboronated/desilicated ZSM-5 was 0.13 s-1.

Original languageEnglish
Title of host publicationAmerican Chemical Society - 235th National Meeting, Abstracts of Scientific Papers
Publication statusPublished - 2008 Dec 1
Event235th National Meeting of the American Chemical Society, ACS 2008 - New Orleans, LA, United States
Duration: 2008 Apr 62008 Apr 10

Publication series

NameACS National Meeting Book of Abstracts
ISSN (Print)0065-7727

Conference

Conference235th National Meeting of the American Chemical Society, ACS 2008
CountryUnited States
CityNew Orleans, LA
Period08/4/608/4/10

ASJC Scopus subject areas

  • Chemistry(all)
  • Chemical Engineering(all)

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    Matsukata, M., Nakagawa, K., Sekine, Y., & Kikuchi, E. (2008). Catalyst preparation for vapor phase Beckmann rearrangement via deboronation/desilication of B-ZSM-5. In American Chemical Society - 235th National Meeting, Abstracts of Scientific Papers (ACS National Meeting Book of Abstracts).