Method for improving Beckmann rearrangement reaction catalyzing performance of shaped MFI molecular sieve

A Beckmann rearrangement and reaction performance technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. The method is simple and the effect of improving the activity

Active Publication Date: 2019-02-01
ZHENGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to overcome the shortcoming that the mole sieve molding catalyst containing MFI structure in the prior art causes catalyst activity and stability to decline due to the addition of a silicon binder, and to provide a molding MFI catalyst that improves its use in the gas phase of cyclohexanone oxime. Improved Catalytic Performance and Stability in the Preparation of Caprolactam by Beckmann Rearrangement

Method used

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  • Method for improving Beckmann rearrangement reaction catalyzing performance of shaped MFI molecular sieve

Examples

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Embodiment 1

[0029] The extruded catalyst sample obtained in Comparative Example 1 was mixed with 25 wt% TPAOH solution at a mass ratio of 1:10, and crystallized at 170°C for 24 hours. After separation and washing, the solid was dried at 60°C and calcined at 450°C for 6 hours to prepare a gas-phase Beckmann rearrangement catalyst for caprolactam production.

Embodiment 2

[0031] The extruded catalyst sample obtained in Comparative Example 1 was mixed with 25 wt% TPAOH solution at a mass ratio of 1:10, and crystallized at 170°C for 48 hours. After separation and washing, the solid was dried at 60°C and calcined at 450°C for 6 hours to prepare a gas-phase Beckmann rearrangement catalyst for caprolactam production.

Embodiment 3

[0033] Examples 1, 2 and Comparative Examples 1, 2 Catalyst rearrangement reaction performance.

[0034] The gas-phase Beckmann rearrangement reaction of cyclohexanone oxime was carried out in a stainless steel fixed-bed reactor with an inner diameter of 6 mm. Crush the strip-shaped catalyst into 40-60mm size particles. Take 0.2000g of catalyst and load it into the reactor, and fill the top and bottom of the catalyst bed with 1.000g of 40-60 mesh quartz sand, and support it with quartz wool. In carrier gas N 2 With a flow rate of 20mL / min, the temperature was raised to 400°C at 13.3°C / min and kept for 1h, then the reaction temperature was lowered to 370°C, and the raw material was an ethanol solution (30wt%) of cyclohexanone oxime through a fixed bed by using an HPLC pressure pump. Reaction, the mass space velocity of cyclohexanone oxime is 8h -1 . Samples were collected every 2 hours using a gas-liquid separator cooled by an ice-water mixture, and each sample was taken fo...

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Abstract

The invention discloses a method for improving the activity, selectivity and stability of a shaped MFI catalyst applied to a vapor phase Beckmann rearrangement reaction of cyclohexanone-oxime, specifically comprising the following steps: using an extrusion-molded catalyst containing an MFI molecular sieve, silica sol, sesbania cannabina powder and the like to be contacted with an aqueous alkalinesolution containing tetrapropyl cations, carrying out solid-liquid separation, and drying and roasting to prepare a modified catalyst. In comparison with unmodified catalysts, the modified catalyst prepared by the above method has the following advantage: activity, selectivity and stability of the modified catalyst are significantly improved.

Description

technical field [0001] The invention relates to a method for improving the activity, selectivity and stability of a shaped MFI catalyst applied to the gas phase Beckmann rearrangement reaction of cyclohexanone oxime. Background technique [0002] Caprolactam (ε-Caprolactam, CPL for short) is an important organic chemical monomer for the synthesis of polyamide 6. At present, concentrated sulfuric acid or fuming sulfuric acid is mainly used in industry to prepare cyclohexanone oxime liquid-phase rearrangement reaction. The process technology is relatively mature, the conversion rate of cyclohexanone oxime and the selectivity of caprolactam are high, and the product quality is also stable, but the biggest disadvantage of this process is the use of highly corrosive concentrated sulfuric acid or oleum, which causes serious environmental protection problems ; In addition, the process will produce 0.64t of ammonium sulfate low-efficiency fertilizer for every 1t of cyclohexanone ox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40C07D223/10C07D201/04
CPCC07D201/04C07D223/10B01J29/40
Inventor 王向宇魏会娟张帆郭路阳温贻强
Owner ZHENGZHOU UNIV
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