Gas chromatography detection method in caprolactam production process

A technology of gas chromatography and caprolactam, which is applied in the field of gas chromatography detection in the production process of caprolactam, can solve the problems of poor separation and analysis effect, and achieve the effect of improving separation effect and detection ability

Active Publication Date: 2020-08-11
沧州旭阳化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the separation and analysis of ketones, oximes, alcohols, alkanes, amides and other substances that need to be separated during the production of caprolactam are poor.

Method used

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  • Gas chromatography detection method in caprolactam production process
  • Gas chromatography detection method in caprolactam production process
  • Gas chromatography detection method in caprolactam production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] No. 1 quality control point in the production process of caprolactam, that is, at image 3 At the end of the shown step 1), the sample in the caprolactam production process is detected, which is composed of several types of tert-butanol, toluene, cyclohexanone, cyclohexanol, benzene, cyclohexanone oxime, and caprolactam.

[0055] Injection vaporization temperature: 300°C; temperature program: start at 30°C at 5°C / min to 200°C for 10 minutes; carrier gas flow rate: 2mL / min, column liquid film: Carbowax; column length: 60m; inner diameter: 0.52 mm; film thickness: 0.5 μm. The resulting chromatogram is figure 1 shown.

Embodiment 2

[0057] No. 1 quality control point in the production process of caprolactam, that is, at image 3 At the end of the shown step 1), the sample in the caprolactam production process is detected, which is composed of several types of tert-butanol, toluene, cyclohexanone, cyclohexanol, benzene, cyclohexanone oxime, and caprolactam.

[0058] Injection vaporization temperature: 300°C; temperature program: start at 30°C at 5°C / min to 200°C for 10 minutes; carrier gas flow rate: 2mL / min, column liquid film: DB-FFAP; column length: 60m; inner diameter : 0.52mm; film thickness: 0.5μm.

Embodiment 3

[0060] No. 1 quality control point in the production process of caprolactam, that is, at image 3 At the end of the shown step 1), the sample in the caprolactam production process is detected, which is composed of several types of tert-butanol, toluene, cyclohexanone, cyclohexanol, benzene, cyclohexanone oxime, and caprolactam.

[0061] Injection vaporization temperature: 300°C; temperature program: start at 30°C at 5°C / min to 200°C for 10 minutes; carrier gas flow rate: 2mL / min, column liquid film: CP Wax 58CB; column length: 30m; inner diameter : 0.52mm; film thickness: 0.5μm.

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Abstract

The invention relates to a gas chromatography detection method in a caprolactam production process. The method uses gas chromatography to detect an intermediate product at a quality control point in caprolactam production, and the gas chromatography uses a strongly polar chromatographic column stationary liquid selected from at least one of bonded polyethylene glycol and cross-linked polyethyleneglycol. According to the gas chromatography detection method in the caprolactam production process, the separation effect is high, and the impurity detection capacity is good. The impurity analysis capability of each control point in the caprolactam production process is improved, and caprolactam production enterprises can be better guided to carry out lean production control.

Description

technical field [0001] The disclosure relates to a detection method in the production process of caprolactam, specifically, the disclosure relates to a gas chromatography detection method in the production process of caprolactam, and a control method in the production process of caprolactam. Background technique [0002] Caprolactam is a white leaflet-shaped crystal with a mint flavor, soluble in water, petroleum hydrocarbons, cyclohexene, benzene, toluene, ethanol, ether, tetrahydrofurfural, dimethylformamide and chlorinated hydrocarbons, and is an important Organic intermediates used in the production of nylon-6 are mainly used in the production of high-performance fibers and composite materials, and are widely used in textiles, automobiles, electronics, machinery and other fields. [0003] At present, the domestic production of caprolactam mainly adopts the ammoximation reaction of cyclohexanone, hydrogen peroxide and ammonia water under the catalysis of titanium silicon ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88C07D223/10C07C201/06
CPCG01N30/88C07D223/10C07C201/06G01N2030/8886G01N2030/885Y02P20/52
Inventor 石峰张志军潘九海霍增辉刘毅冯书平姚奎孙吉全
Owner 沧州旭阳化工有限公司
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