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Diazotization preparation method of chloroarylamine

A technology of chlorinated arylamine and diazotization, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid nitrile, etc., to achieve the effect of improving environmental protection performance

Inactive Publication Date: 2016-12-28
浙江龙盛染料化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, conventional disperse dyes have great hidden dangers in projects such as tri / tetra / pentachlorophenol, chlorinated benzene, and chlorinated toluene

Method used

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  • Diazotization preparation method of chloroarylamine
  • Diazotization preparation method of chloroarylamine
  • Diazotization preparation method of chloroarylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Diazotization reaction: Add 65% sulfuric acid 33.2g (0.22mol) into the diazonium reaction vessel, cool down to 10°C-15°C, and control the temperature at 10°C-15°C, slowly add 15.5% nitrosyl Sulfuric acid 84.4g (0.103mol), after adding, control the temperature at 20°C to 25°C, slowly add 20.9g (0.1mol) of 99% 2,6-dichloro-4-nitroaniline, and Insulate and react at ℃ for 6-8 hours, and check the end point (take a small amount of diazonium solution and dilute it with ice water, if the solution is clear, it means that the reaction has reached the end point). After the reaction is completed, the prepared 2,6-dichloro-4-nitroaniline diazonium solution is added to 250g of ice water for dilution. After adding the diazo solution, control the temperature below 5°C and keep stirring for 4-6 minutes, then filter to remove impurities. Filtrate to be coupled reaction;

[0018] (2) Coupling reaction: Add 34.16g (0.1mol) of N-cyanoethyl-N-acetoxyethylaniline with a content of 68% i...

Embodiment 2

[0020] (1) Diazotization reaction: Add 40g (0.4mol) of 98% sulfuric acid into the diazonium reaction vessel, cool down to 10°C-15°C, and control the temperature at 10°C-15°C, slowly add 40% nitrosyl sulfuric acid 32.4g (0.102mol), after adding, control the temperature at 20°C to 25°C, slowly add 21.8g (0.1mol) of 95% 2,6-dichloro-4-nitroaniline, and Insulate the reaction for 6-8 hours, and check the end point (take a small amount of diazonium solution and dilute it with ice water, and the clear solution indicates that the reaction has reached the end point). After the reaction is completed, the prepared 2,6-dichloro-4-nitroaniline diazonium solution is added to 300g of ice water for dilution. After adding the diazo solution, control the temperature below 0°C and keep stirring for 4-6 minutes, filter to remove impurities, and filter Liquid to be coupled reaction;

[0021] (2) Coupling reaction: Add 27.3 g (0.1 mol) of 73% N,N-dicyanoethylaniline to 400 g of water, add the filt...

Embodiment 3～16

[0023] According to the preparation method of Example 1, the difference is that the diazo component and coupling component A in the following Table 1 are used in equimolar amounts to prepare conventional disperse dyes.

[0024] Table 1

[0025]

[0026]

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PUM

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Abstract

The invention discloses a diazotization preparation method of chloroarylamine. The method is conducted according to the following steps that metered sulfuric acid is slowly added into a diazotization reaction vessel, stirring is started, then nitrosyl sulfuric acid is slowly added, the temperature is lowered and controlled to be at minus 10 DEG C to 35 DEG C, chloroarylamine is slowly added, and after addition is completed, a diazotization reaction is conducted by keeping the above-mentioned temperature range till the reaction reaches a final point to obtain chloroarylamine diazotization liquid; the chloroarylamine diazotization liquid is slowly added into ice-water mixed liquid or low-temperature water at the temperature below 0 DEG C to be diluted, and after addition is completed, stirring under heat preservation is controlled to be conducted at the temperature below 5 DEG C; filtration is conducted for impurity removal in 3 hours, and filtrate serves as diazotization liquid for use. After conventional disperse dye obtained by coupling the diazotization liquid acquired through the method is used for normal dyeing, all environment protection detection indexes, particularly the chlorinated phenol content, the chlorobenzene content and the chlorinated methylbenzene content, of a textile fabric meet the limitation requirements of the Oeko-Tex Standard 100, and then the more stringent biological environment protection requirements of medium-grade and high-grade fabrics are met.

Description

(1) Technical field [0001] The invention relates to a diazotization preparation method of a dye intermediate, in particular to a diazotization preparation method of chlorinated arylamine. (2) Background technology [0002] Chlorinated arylamines such as 2,6-dichloro-4-nitroaniline are important dye intermediates, mainly used in the production of disperse dyes such as disperse yellow brown 3GL, disperse yellow brown 2RFL, disperse brown 3R, disperse orange S-4RL , Disperse Blue S-BBL, Disperse Yellow Brown SE-4BR, Disperse Yellow Brown H-2RL and other dyes. As conventional disperse dyes, due to their own structure and raw material problems, they can only be free of prohibited aromatic amines, carcinogenic dyes, allergenic dyes and other directly prohibited disperse dyes. In the past, we thought that those that could meet these requirements could be used as environmentally friendly dyes. Nowadays, people are more and more aware of environmental protection, and the dyes used a...

Claims

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Application Information

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IPC IPC(8): C07C245/20C07C255/24C07C253/30
Inventor 祝培明金鑫伟张友珍郭塬智彭光耀张桂香蒋应海李世华
Owner 浙江龙盛染料化工有限公司
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