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Separation process of molecular sieve catalyst in ketone oxamidinating reaction system

A technology of oximation reaction and separation method, which is applied in the field of separation of molecular sieve catalysts, can solve the problems of molecular sieve loss, parking accidents, easy clogging, etc., and achieve the effect of less solid content, continuous separation and good separation effect

Inactive Publication Date: 2003-07-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The molding of molecular sieves and the use of binders in the molding process not only cause the loss of molecular sieves, but also affect the pore volume and specific surface area of ​​catalysts;
[0006] (2) Install a 5 μm porous plate directly in the reactor to intercept the molecular sieve catalyst. Although the separation is relatively simple, such a small hole is very easy to block without backflushing, and this situation also poses a high demand for stirring. Poor stirring can easily cause parking accidents; and the reactor has a built-in separation element, which is extremely inconvenient to maintain and replace;

Method used

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  • Separation process of molecular sieve catalyst in ketone oxamidinating reaction system

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Embodiment 1

[0018] Maintaining the ammonia concentration in the there-necked flask 4 is 1.8% by weight, the concentration of tert-butanol solvent is 40.2% by weight, the temperature of the reaction material is 80°C, the temperature of the material in the settler 7 is 65°C, the linear velocity of the material is 1.8 cm / min, and the material is settling. The residence time in vessel 7 was 12 minutes. The concentration of the titanium silicon molecular sieve measured from feed liquid collecting bottle 8 is 2ppm.

Embodiment 2

[0020] Maintaining the ammonia concentration in the there-necked flask 4 is 3.0% by weight, the ethanol solvent concentration is 40.2% by weight, the temperature of the reaction material is 80°C, the temperature of the material in the settler 7 is 75°C, and the linear velocity of the material is 3.0 cm / min. The medium residence time was 12 minutes. The concentration of the titanium silicon molecular sieve measured from feed liquid collection bottle 8 is 9ppm.

Embodiment 3

[0022] Maintaining the ammonia concentration in the there-necked flask 4 is 5.0% by weight, the concentration of isopropanol solvent is 35.2% by weight, the temperature of the reaction material is 80°C, the temperature of the material in the settler 7 is 80°C, the linear velocity of the material is 1.0 cm / min, and the material is settling The residence time in vessel 7 was 12 minutes. The concentration of the titanium silicon molecular sieve measured from feed liquid collection bottle 8 is 6ppm.

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Abstract

In the ketone oxamidinating reaction system with water mutually soluble low-carbon alcohol of 30-50 wt% concentration and excessive ammonia water content, the material including titania-silica molecular sieve is deposited at 60-85 deg.c in deposition rate of 0.5-3 cm / min for at least 10 min. The present invention can realize the continuous separation of titania-silica molecular sieve from reaction liquid and is suitable for cyclohexanone oxamidinating reaction system with titania-silica molecular sieve catalyst of 0.1-0.3 micron size.

Description

technical field [0001] The present invention relates to a method for separating molecular sieve catalysts, and more particularly relates to a method for separating molecular sieve catalysts in a ketoammoxime reaction system. Background technique [0002] Cyclohexanone oxime is a key intermediate for the synthesis of caprolactam and an important chemical raw material, mainly used as a raw material for the preparation of nylon 6 monomer for fiber nylon 6 and engineering plastics. [0003] The preparation of cyclohexanone oxime is disclosed in documents such as EP0384390, EP0311983 and EP0496385. EniChem Company first disclosed the method of ammoximation of cyclohexanone to generate cyclohexanone oxime, which is the next step to generate cyclohexanone oxime in the presence of cyclohexanone, ammonia and hydrogen peroxide in the presence of tert-butanol or toluene solvent and titanium silicon molecular sieve catalyst . The method has the characteristics of mild reaction conditi...

Claims

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Application Information

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IPC IPC(8): B01J29/06B01J29/90C07C249/04
CPCY02P20/584
Inventor 李永祥吴巍闵恩泽孙斌张树忠
Owner CHINA PETROLEUM & CHEM CORP
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