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Method for forming article made from cracked zeolite

A technology for shaped products and zeolite, applied in chemical recycling, grain processing, etc., can solve the problems of reduced crystallinity, unsatisfactory fragmentation, and inability to obtain zeolite, and achieve the effect of inhibiting the reduction of crystallinity and effectively fragmenting

Active Publication Date: 2012-03-21
SUMITOMO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when zeolite shaped articles are disintegrated by these physical methods, crystallinity may decrease, disintegration may be unsatisfactory, and zeolites suitable for reshaping are sometimes not available

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0023] Examples of the present invention are shown below, but the present invention is not limited to these examples. In Examples, the measurement of the average particle diameter and X-ray diffraction intensity of the catalyst or crystal was performed by the following methods.

[0024] [average particle diameter]

[0025] Using a particle size distribution measuring device ("MICROTRACHR Model 9320-X100" manufactured by Nikkiso Co., Ltd.), the diameter of 50% by volume (volume median straight value) is measured, and this is called the average particle diameter.

[0026] [X-ray diffraction intensity]

[0027] It was measured using an X-ray diffraction apparatus ["RINT-2100V" manufactured by Rigaku Corporation] using a copper Kα-beam as a light source.

reference example 1

[0028] Reference example 1 (gas-phase Beckmann rearrangement reaction)

[0029] A zeolite shaped article (secondary particle) having an average particle diameter of 60 μm was used as a catalyst, and this zeolite shaped article was spherically shaped from a zeolite (primary particle) having an average particle diameter of 0.2 μm, said zeolite (primary particle) being Composed of crystalline silica with MFI structure. In a fluidized bed reactor in which the catalyst was fluidized, the reaction was carried out at 380° C. for 3 months by feeding vaporized cyclohexanone oxime, methanol and nitrogen, and withdrawing reaction product gas. During the reaction, the space velocity WHSV [feed rate (g / h) for catalyst weight (g)] of cyclohexanone oxime is 2h -1 , and the feed ratio of cyclohexanone oxime / methanol / nitrogen is 1kg / 1.8kg / 0.3m 3 . In addition, during the reaction, part of the catalyst was withdrawn from the reactor, introduced into a calciner, calcined at 500°C under air fl...

Embodiment 1

[0032] 300 g of the used catalyst obtained in Reference Example 1 was put into a beaker, and 700 g of a 6% by weight aqueous solution of tetra-n-propylammonium hydroxide (the concentration of tetra-n-propylammonium was 5.5% by weight; pH =13), and then the mixture was stirred at 110°C for 6 hours. Water was added to the obtained slurry to prepare a 5% by weight slurry, and the average particle diameter was measured to be 0.2 μm.

[0033] Further, the slurry was filtered, and the filtered crystal residue was dried, and then fired at 530° C. for 1 hour under a nitrogen flow, and 1 hour at a temperature of 530° C. under an air flow, to obtain powdery white crystals. When the X-ray diffraction intensity of this powdery white crystal was measured, it was determined to be an MFI structure, and the peak intensity at 2θ=23° was 126% relative to the same peak intensity of the used catalyst obtained in Reference Example 1.

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PUM

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Abstract

The invention provides a method for disintegrating a zeolite molded product containing the step of mixing the zeolite molded product with a basic aqueous solution containing at least 2 wt.% of a quaternary ammonium salt.

Description

technical field [0001] The present invention relates to a method for fragmenting shaped zeolite articles, such as zeolite shaped articles used as catalysts for Beckmann rearrangement reactions. Background technique [0002] As one of the production methods of ε-caprolactam, a generally known method is a method involving Beckmann rearrangement reaction of cyclohexanone oxime in the gas phase in the presence of a solid catalyst (for example, refer to EP0380364). As catalysts, zeolites such as crystalline silica and crystalline metallosilicates can be used, and are generally used in the form of pellets or fine particles (for example, refer to EP0576295). Usually, as time elapses, the catalyst weakens its activity due to the precipitation of carbonaceous substances, thermal degradation, etc., therefore, various regeneration methods have been proposed, such as calcination, chemical treatment, etc. (for example, refer to EP0388070, Japanese Patent Application Publication No. 2003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B02C19/00
CPCY02P20/584
Inventor 星野正大北村胜杉田启介
Owner SUMITOMO CHEM CO LTD
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