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Method for reducing inactivation of hydroxylamine inorganic liquid

An inorganic and hydroxylamine technology, applied in organic chemistry, oxime preparation, etc., can solve the problems of decreased activity and selectivity of hydroxylamine catalyst, poor extraction effect, and reduced production load of the device, achieving remarkable treatment effect, improved production effect, and simple method Effect

Active Publication Date: 2012-11-14
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the toluene-cyclohexanone oxime produced by the ammoximation unit is rich in impurities, the toluene recovered therefrom is used as an extraction agent to extract organic impurities in the ammoximation inorganic liquid, and the extraction effect is poor, which reduces the activity and selectivity of the inorganic liquid. A sharp drop, and eventually lead to a sharp drop in the activity and selectivity of the hydroxylamine catalyst, which seriously affects the production of the device and reduces the production load of the device
[0004] At present, the tolylcyclohexanone oxime system of the ammoximation unit and the tolcyclohexanone oxime system of the ammoximation unit operate in series, which in turn affects the activity of the hydroxylamine inorganic liquid. At present, there are no relevant patent technical documents for reference.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0021] Add 500-1000kg of 4μm-6μm activated carbon to the spent catalyst filter, the pressure of the spent catalyst filter is 0.1MPa, and the temperature is 40°C to form an activated carbon filter cake, and establish an absorption tower feed tank→pump→waste catalyst filter→absorption tower The hydroxylamine inorganic liquid circulation purification process in the feeding tank, after 7 days of filtration, the activity and selectivity of the hydroxylamine inorganic liquid were analyzed, the results are as follows:

[0022] Hydroxylamine inorganic liquid index active(%) Selectivity (%) Unfiltered 14.67 79.52 After 7 days of filtration 15.62 76.24

example 2

[0024] Add 500-1000kg of 4μm-6μm activated carbon to the spent catalyst filter, the pressure of the spent catalyst filter is 0.2Mpa, and the temperature is 50°C to form an activated carbon filter cake, and build an absorption tower feed tank→pump→waste catalyst filter→absorption tower The hydroxylamine inorganic liquid circulation purification process in the feeding tank, after 7 days of filtration, the activity and selectivity of the hydroxylamine inorganic liquid were analyzed, the results are as follows:

[0025] Hydroxylamine inorganic liquid index active(%) Selectivity (%) Unfiltered 14.67 79.52 After 7 days of filtration 16.15 77.39

[0026] Hydroxylamine in the hydroxylamine inorganic liquid decomposes slightly and decomposes into NO X and N 2 O, the temperature and pressure increased slightly.

example 3

[0028] Add 500-1000kg of 4μm-6μm activated carbon to the waste catalyst filter, configure the activated carbon filter cake, and use the adsorption and purification characteristics of activated carbon to establish the absorption tower feed tank→pump→waste catalyst filter→absorption tower feed tank hydroxylamine inorganic liquid circulation In the purification process, the pressure of the spent catalyst filter is 0.15MPa, the temperature is 45°C, the state of the filter cake is stable, and the cycle state is stable. During this period, the activity and selectivity of the hydroxylamine inorganic liquid are analyzed in different time periods, and the results are as follows:

[0029] Hydroxylamine inorganic liquid index active(%) Selectivity (%) Unfiltered 14.67 79.52 After 7 days of filtration 17.60 75.73 After 25 days of filtration 21.25 82.64

[0030] After 25 days of filtration, the activity and selectivity of the hydroxylamine inorganic liq...

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Abstract

The invention relates to a method for reducing the inactivation of the hydroxylamine inorganic liquid. When the impurity-rich toluene-cyclohexanone oxime solution enters the hydroxylamine inorganic liquid system of a hydroxylamine oximation device, the inactivation of hydroxylamine inorganic liquid is reduced, thus the circulating purification process of the hydroxylamine inorganic liquid by an absorption tower feeding tank, a pump, a filter and the absorption tower feeding tank is set. The filter filled with the activated carbon as the adsorbent is used for filtering and purifying the hydroxylamine inorganic liquid continuously. By absorbing and purifying the hydroxylamine inorganic liquid in the absorption tower feeding tank by using the activated carbon, the production capacity of the device is restored to 90% from 70% after being polluted, the influence of the polluted toluene to the inactivation of the hydroxylamine inorganic liquid is reduced, and the activity and selectivity of the hydroxylamine catalyst are guaranteed effectively.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a method for reducing the deactivation of hydroxylamine inorganic liquid, in particular to a method for reducing the deactivation of hydroxylamine inorganic liquid during the preparation of cyclohexanone oxime by azoxyl oximation. Background technique [0002] Caprolactam is an important organic chemical raw material, which is mainly used to make polyamide-6 fiber, and can also be used to make polycaprolactam engineering plastics. Caprolactam is produced by Beckmann rearrangement of cyclohexanone oxime. At present, the main preparation methods of cyclohexanone oxime include hydroxamine oximation and ammonia oximation. [0003] The hydroxaminization unit is the core part of the cyclohexanone oxime prepared by the hydroxaminization method. The main task is to produce the intermediate product of caprolactam - cyclohexanone oxime, and its main raw materials are hydrogen,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/44C07C249/08C07C249/04
Inventor 徐纲留辉毛伟刘卫东
Owner CHINA PETROLEUM & CHEM CORP