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Online discharged material cleaning device and method for deactivated catalysts in cyclohexanone oximation reaction

A technology for oximation reaction and cleaning device, which is applied in the directions of physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems that catalyst treatment is not described and affects the efficient, stable and long-term operation of the ammoximation process, etc. Achieve the effect of ensuring long-term stable operation and ensuring the response effect

Inactive Publication Date: 2016-03-23
HUBEI SANNING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shutdown of the reactor consumes a lot of manpower and material resources, which also affects the efficient and stable long-term operation of the ammoximation process
[0004] Utility models CN201596496U, CN201988375U etc. have reported on the ammoximation reactor for the production of cyclohexanone oxime, but there is no description for the treatment of the catalyst in the production process

Method used

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  • Online discharged material cleaning device and method for deactivated catalysts in cyclohexanone oximation reaction
  • Online discharged material cleaning device and method for deactivated catalysts in cyclohexanone oximation reaction

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Embodiment 1

[0024] Such as figure 1 As shown, a catalyst online discharge cleaning device for cyclohexanone oximation reaction, the bottom of the catalyst discharge tank 1 is connected to the delivery pump 2 through the feed pipeline, and the top of the catalyst discharge tank 1 is connected to the circulating cooler 3 through the feed pipeline Connection, the feeding pipeline of the delivery pump 2 is connected with the lower part of the filter 4 after the feeding pipeline of the circulating cooler 3 is merged, the bottom of the filter 4 is connected with the settling tank 5 through the feeding pipeline, and the upper part of the filter 4 is connected with the settling tank through the feeding pipeline. The clear liquid tank 6 is connected, and the desalinated water recoil pipeline 13 is also arranged on the feed pipeline, and the bottom of the clear liquid tank 6 is connected with the clear liquid delivery pump 7 through the feed pipe and then sent to the oximation reaction kettle.

[0...

Embodiment 2

[0029] The implementation process of the process of the present invention is as follows: the turbid catalyst liquid discharged from the oximation reaction kettle is returned to the catalyst discharge tank, and after being cooled by the transfer pump, it is transported to the filter for cleaning and filtration. The filtration and cleaning steps are divided into three steps: alcohol washing, water washing, and concentration, which are:

[0030] 1. Alcohol washing: introduce tert-butanol into the catalyst filter, and control the flow rate to 0.5-3m 3 / h, after 1-3h, analyze the content of cyclohexanone oxime in the filtered clear liquid <0.05%, and the alcohol washing is qualified;

[0031] 2. Water washing: introduce the desalted water into the catalyst filter, and control the flow rate to 1-5m 3 / h, after 1-3h, analyze the content of tert-butanol in the filtered clear liquid <0.05%, and the water washing is qualified;

[0032] 3. Concentration: N 2 Introduce into catalyst fi...

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Abstract

The invention provides an online discharged material cleaning device for deactivated catalysts in a cyclohexanone oximation reaction. The bottom of a catalyst discharging tank is connected with a delivery pump through a delivery pipeline, the top of the catalyst discharging tank is connected with a recirculation cooler through a delivery pipeline, the delivery pipeline of the delivery pump and the delivery pipeline of the recirculation cooler are converged and then connected with the lower portion of a filter, the bottom of the filter is connected with a settling tank through a delivery pipeline, the upper portion of the filter is connected with a cleaning tank through a delivery pipeline, and the bottom of the cleaning tank is connected with a clear liquid delivery pump through a delivery pipeline and then connected to an oximation reaction kettle. A cleaning method includes: returning turbid catalyst liquid discharged from the oximation reaction kettle into the catalyst discharging tank, performing self-circulation cooling through the delivery pump, delivering to the filter to realize cleaning and filtering, and directly pressing catalyst slurry fluid into the settling tank after filtering and cleaning to realize standing, settling and separating. The reaction material containing catalysts discharged from the reaction kettle can be cleaned by means of alcohol washing, water washing and condensing, material recovery is realized, and contents of organics in the discharged catalysts are lower than 500PPM.

Description

technical field [0001] The invention relates to an online discharging and cleaning device for a cyclohexanone oximation reaction catalyst, which belongs to the field of chemical technology and equipment. Background technique [0002] Cyclohexanone oxime is an important intermediate in the production of caprolactam, which is produced by the oximation reaction of hydroxylamine and cyclohexanone. At present, the main production method of cyclohexanone oxime is to use hydrogen peroxide, ammonia and cyclohexanone to react to generate cyclohexanone oxime in the presence of titanium silicon molecular sieve catalyst and tert-butanol solvent. Remove the molecular sieve catalyst to obtain the reaction clear liquid, and then obtain high-purity cyclohexanone oxime through a series of rectification and extraction processes. [0003] Judging from the current operating conditions of domestic ammonia oximation units, due to the deactivation and loss of catalysts due to certain carbon depos...

Claims

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Application Information

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IPC IPC(8): B01J29/90B01J38/52B01D29/33B01D29/52C07C249/04C07C251/44
CPCY02P20/584
Inventor 李万清周学军李军游华彬车小军万军陈超
Owner HUBEI SANNING CHEM
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