Preparation method of microspherical molecular sieve catalyst and method for gas phase beckmann rearrangement of cyclohexanone oxime

By utilizing waste cyclohexanone oxime gas-phase Beckmann rearrangement catalyst to prepare highly crystalline fine-particle ZSM-5 type all-silica-1 molecular sieve catalyst, the problems of high preparation cost and environmentally unfriendly waste catalyst treatment were solved. This achieved efficient cyclohexanone oxime conversion and caprolactam selectivity, and promoted the recycling of catalyst.

CN122164472APending Publication Date: 2026-06-09BEIJING RISUN TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
BEIJING RISUN TECH CO LTD
Filing Date
2024-12-09
Publication Date
2026-06-09

AI Technical Summary

Technical Problem

The preparation cost of existing all-silica-1 molecular sieve catalysts is high, there is a lack of effective recycling of spent catalysts, and the treatment of deactivated catalysts is not conducive to environmental protection.

Method used

Using waste cyclohexanone oxime gas-phase Beckmann rearrangement catalyst as the silicon source, the catalyst was processed by carbonization, pulping and grinding, and mixing with KOH, organic template agent and alcohol to form a colloidal mixture. The mixture was then crystallized and spray-molded, and post-processed with an alkaline buffer solution containing magnesium salt and bromide salt to prepare ZSM-5 type all-silica-1 molecular sieve catalyst with high crystallinity and fine particles.

Benefits of technology

It significantly reduced the cost of silicon sources, improved the conversion rate of cyclohexanone oxime and the selectivity of caprolactam, achieved effective recycling of catalysts, and reduced environmental pollution.

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Abstract

This invention relates to the field of catalyst technology, and discloses a method for preparing a microsphere molecular sieve catalyst and a method for the gas-phase Beckmann rearrangement reaction of cyclohexanone oxime, comprising: (1) carbonizing a waste cyclohexanone oxime gas-phase Beckmann rearrangement catalyst; (2) mixing the obtained product with water and slurrying it until the particle diameter in the slurry is less than 20 μm; (3) mixing the slurry, KOH, an organic template agent, and an alcohol; (4) crystallizing the colloidal mixture, and optionally concentrating the crystallization mother liquor to obtain a molecular sieve slurry; (5) mixing the molecular sieve slurry with a binder and slurrying it, spray-forming the molecular sieve-binder slurry, and then calcining it; (6) contacting the product obtained from calcination in step (5) with an alkaline buffer solution containing ammonium salt, ammonia, magnesium salt, and bromide salt, and then drying it. The catalyst obtained by this preparation method has a high cyclohexanone oxime conversion rate and caprolactam selectivity in a fluidized bed reaction system.
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