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Method for detecting industrial ammoximation reaction liquid of caprolactam

An ammoximation reaction and caprolactam technology, applied in the chemical industry, can solve the problems of interfering with the determination of impurities in the reaction solution, inability to accurately detect the composition of the reaction solution, and poor reproducibility of test results.

Inactive Publication Date: 2020-10-20
山东方明化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the impurities in the ammoximation reaction solution are polar organic impurities. The industry uses weak polarity chromatographic columns. This type of chromatographic column cannot achieve effective separation of impurities in the reaction solution and cannot accurately detect the composition of the reaction solution.
In addition, the composition of the reaction impurities in the reaction solution is complex, the molecular weight and boiling point range of impurities are widely distributed, and the single gradient temperature chromatographic detection cannot realize the effective separation and content determination of the impurities in the reaction solution
In addition, tert-butanol, the reaction medium in industrial production, will be recycled, resulting in the continuous accumulation of reaction impurities in the reaction solution, interfering with the determination of the true content of impurities in the reaction solution, and it is impossible to accurately know the effectiveness of the raw material cyclohexanone in the ammoximation reaction solution. Conversion status (hereinafter referred to as effective conversion rate)
In addition, due to the participation of hydrogen peroxide and ammonia in the ammoximation reaction, the reaction solution is alkaline and contains more water, which makes the peaks of impurities detected by chromatography fluctuate easily, and the reproducibility of the detection results is poor.

Method used

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  • Method for detecting industrial ammoximation reaction liquid of caprolactam
  • Method for detecting industrial ammoximation reaction liquid of caprolactam
  • Method for detecting industrial ammoximation reaction liquid of caprolactam

Examples

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Effect test

Embodiment 1

[0031] A chromatograph equipped with HP-INNOWAX 60m*0.32mm*0.25μm chromatographic column was used for detection and analysis. First use the pretreatment method to process the chromatographic empty run (no sample injection), and immediately use the gradient temperature rise scheme to detect the ammoximation reaction solution and circulating tert-butanol respectively. The chromatographic detection conditions are: inlet temperature 260°C, split ratio 30:1, sample volume 0.5μL; detector temperature 280°C, detector hydrogen flow rate 30ml / min, detector air flow rate 300ml / min; column carrier gas flow rate 1ml / min. In this example, the chromatographic conditions of the pretreatment method are adopted. The initial temperature is 40° C., kept for 1 min, and then raised to 200° C. at a rate of 20° C. / min, and kept for 1 min. This example adopts N=2 gradient heating scheme, the initial temperature is 40°C, keep for 15min, raise the temperature to 110°C at 10°C / min, keep for 10min, rais...

Embodiment 2

[0038] The chromatograph equipped with HP-INNOWAX 60m*0.32mm*0.5μm chromatographic column is used for detection and analysis. First use the pretreatment method to process the chromatographic empty run (no sample injection), and immediately use the gradient temperature rise scheme to detect the ammoximation reaction solution and circulating tert-butanol respectively. The chromatographic detection conditions are: inlet temperature 260°C, split ratio 30:1, sample volume 0.5μL; detector temperature 280°C, detector hydrogen flow rate 30ml / min, detector air flow rate 300ml / min; column carrier gas flow rate 1ml / min. In this embodiment, the chromatographic conditions of the pretreatment method are adopted. The initial temperature is 35° C., kept for 2 minutes, then raised to 200° C. at a rate of 15° C. / min, and kept for 2 minutes. This example adopts N=3 gradient heating scheme, the initial temperature is 35°C, keep for 10min, raise the temperature to 110°C at 10°C / min, keep for 10mi...

Embodiment 3

[0045]The chromatograph equipped with HP-INNOWAX 60m*0.25mm*0.5μm chromatographic column is used for detection and analysis. First use the pretreatment method to process the chromatographic empty run (no sample injection), and immediately use the gradient temperature rise scheme to detect the ammoximation reaction solution and circulating tert-butanol respectively. The chromatographic detection conditions are: inlet temperature 300°C, split ratio 50:1, sample volume 1μL; detector temperature 300°C, detector hydrogen flow rate 40ml / min, detector air flow rate 400ml / min; column carrier gas flow rate 2ml / min. In this example, the chromatographic conditions of the pretreatment method are adopted. The initial temperature is 30° C., kept for 1 min, and then raised to 220° C. at a rate of 20° C. / min, and kept for 1 min. This example adopts N=3 gradient heating scheme, the initial temperature is 30°C, keep it for 10min, raise the temperature to 90°C at 8°C / min, keep it for 12min, ra...

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Abstract

The invention provides a method for detecting industrial ammoximation reaction liquid of caprolactam. The method comprises the following steps of: carrying out idle running pretreatment on a chromatographic instrument provided with a strong-polarity chromatographic column, and respectively detecting ammoximation reaction liquid and circulating tert-butyl alcohol by using a gradient heating scheme.The method provided by the invention can realize effective separation of various impurities in the ammoximation reaction liquid, can eliminate interference of circulating impurities in the medium tert-butyl alcohol, can realize accurate content detection of the reaction impurities, can accurately determine the effective conversion rate of ammoximation reaction, can accurately evaluate the ammoximation reaction effect, and has good detection result reproducibility.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for detecting a caprolactam industrial ammoximation reaction liquid. Background technique [0002] Caprolactam is an important material in today's organic chemical production. Industrial caprolactam can be used to produce nylon fibers, engineering plastics and synthetic drugs. The cyclohexanone ammoximation method is a process for producing caprolactam, and its main process is that cyclohexanone is reacted with ammonia and hydrogen peroxide in a medium of tert-butanol to generate cyclohexanone oxime; cyclohexanone oxime Beckmann rearrangement to caprolactam. [0003] The ammoximation reaction is an important reaction in the caprolactam process, and the component detection of the liquid material after the ammoximation reaction (hereinafter referred to as the reaction solution) becomes an important basis for evaluating the reaction effect. Most of the impurit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/60G01N30/30G01N30/16G01N30/68
CPCG01N30/02G01N30/60G01N30/30G01N30/16G01N30/68G01N2030/3076G01N2030/3046
Inventor 张彦峰孙利敏任成韵赵兰鸽姚奎于进玉刘毅石峰
Owner 山东方明化工股份有限公司
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