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Preparation method for 2-[N-(2-cyanoethyl)-4-[(2,6-dichloro-4-nitrobenzophenone)azo]anilino]ethyl acetate

A technology based on p-nitroaniline and cyanoethyl, which is applied in the field of preparation of Disperse Orange 30, can solve the problems of low strength, hindering product development, and the light and darkness of Disperse Orange 30, and achieves bright color, high purity and high yield. Effect

Active Publication Date: 2012-08-01
苏州市罗森助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the disperse orange 30 color light produced by this method is dark, and the intensity is low. The disadvantage is that the product contains polychlorinated benzidine, which hinders the product from entering the international market.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] According to the preparation method of Disperse Orange 30 of the present embodiment, comprises the steps:

[0018] (1) Refining of 2,6-dichloro-p-nitroaniline: Add 500 grams of water, 10 grams of water-soluble solvent ethylene glycol monomethyl ether, and 1 gram of dispersant MF into a 1000ml beaker equipped with a stirring device, fully Stir well. Then add 300 grams of commercially available industrial grade 2,6-dichloro-p-nitroaniline, stir well and raise the temperature to 80°C, filter while hot, drain, then wash with hot water at 80°C for 2 to 3 times, filter The cake is refined 2,6-dichloro-p-nitroaniline with a chromatographic content of more than 99.8wt%, and the polychlorinated benzidine content is less than 5ppm. The filter cake is dried to obtain 195 grams.

[0019] (2) Diazotization reaction: Take 195 grams of the above-mentioned refined 2,6-dichloro-p-nitroaniline, add 300 grams of 98% sulfuric acid, cool down to 0~5°C, and then dropwise add nitrosyl ...

Embodiment 2

[0022] According to the preparation method of Disperse Orange 30 of the present embodiment, comprises the steps:

[0023] (1) Refining of 2,6-dichloro-p-nitroaniline: Add 500 grams of water, 10 grams of water-soluble solvent ethylene glycol monomethyl ether, and 1 gram of dispersant MF into a 1000ml beaker equipped with a stirring device, fully Stir well. Then add 300 grams of commercially available 2,6-dichloro-p-nitroaniline, stir well and raise the temperature to 80°C, filter while hot, drain, and then wash with 80°C hot water for 2 to 3 times, the filter cake is The chromatographic content of refined 2,6-dichloro-p-nitroaniline is more than 99.8wt%, and the content of polychlorinated benzidine in it is less than 5ppm. The filter cake is dried to obtain 195 grams.

[0024] (2) Diazotization reaction: Take 195 grams of the above-mentioned refined 2,6-dichloro-p-nitroaniline, add 300 grams of 98% sulfuric acid, cool down to 0~5°C, and then dropwise add nitrosyl sulfuri...

Embodiment 3

[0027] According to the preparation method of Disperse Orange 30 of the present embodiment, comprises the steps:

[0028] (1) Refining of 2,6-dichloro-p-nitroaniline: Add 500 grams of water, 10 grams of water-soluble solvent ethylene glycol monomethyl ether, and 1 gram of dispersant MF into a 1000ml beaker equipped with a stirring device, fully Stir well. Then add 300 grams of commercially available 2,6-dichloro-p-nitroaniline, stir well and raise the temperature to 80°C, filter while hot, drain, and then wash with 80°C hot water for 2 to 3 times, the filter cake is The refined 2,6-dichloro-p-nitroaniline has a chromatographic content of more than 99.8 wt%, and the filter cake is dried to obtain 195 grams.

[0029] (2) Diazotization reaction: Take 195 grams of the above-mentioned refined 2,6-dichloro-p-nitroaniline, add 300 grams of 98% sulfuric acid, cool down to 0~5°C, and then dropwise add nitrosyl sulfuric acid to make heavy The nitriding reaction yields a solution...

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Abstract

The invention relates to a preparation method for disperse orange 30. The preparation method comprises the following steps of: (1) undergoing a diazotization reaction: undergoing a diazotization reaction on 2,6-dichloroparanitroaniline and nitrosyl sulfuric acid in a sulfuric acid medium to obtain a diazonium product solution; and (2) undergoing a coupling reaction: undergoing a coupling reactionon the diazonium product solution obtained in the step (1) and N-cyanoethyl-N-acetoxyethyl to generate disperse orange 30. Particularly, the chromatograph content of 2,6-dichloro paranitroaniline serving as a raw material used in the step (1) is over 99.8 percent by weight, the content of polychlorinated biphenyl amine is lower than 5 ppm, and the diazotization reaction is undergone at the temperature of 0-5 DEG C in the step (1). A product prepared with the method does not contain any international forbidden byproduct, i.e., polychlorinated biphenyl amine, and a basis is laid for the development of the international market; and moreover, the product prepared with method has high yield, high purity and gorgeous chromatic light.

Description

technical field [0001] The invention relates to a preparation method of Disperse Orange 30. Background technique [0002] Disperse Orange 30, the chemical name is 2-[N-(2-cyanoethyl)-4-[(2,6-dichloro-4-nitrophenyl)azo]anilino]ethyl acetate, the structural formula is as follows : [0003] [0004] Disperse orange is the main color of high-temperature disperse dyes. It has excellent light and sublimation fastness, and is mainly used for dyeing polyester-cotton and polyester-viscose blended fabrics and direct printing of cotton-polyester blended fabrics. At present, the main production method of Disperse Orange 30 is to use industrial-grade 2,6-dichloro-p-nitroaniline as raw material, add nitrosyl sulfuric acid dropwise in sulfuric acid medium to carry out diazotization reaction, and then combine with coupling component N- Cyanoethyl - N-acetoxy ethyl coupling and prepared. Since the current domestic industrial grade 2.6-di-chloro-p-nitroaniline content is about 95%, and...

Claims

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Application Information

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IPC IPC(8): C09B29/08
Inventor 李根荣徐新连
Owner 苏州市罗森助剂有限公司
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