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A kind of preparation method of azo disperse dye with ester group

A technology of disperse dyes and ester-based azo, which is applied in the direction of azo dyes, monoazo dyes, organic dyes, etc., can solve the problems of filter cake purity decrease, color and light deterioration, and affect product quality, so as to reduce the content of organic matter , improve the yield and quality, and reduce the content of organic pollutants

Active Publication Date: 2017-09-22
ZHEJIANG DIBANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In azo disperse dyes, disperse dyes containing ester groups are an important member of disperse dyes. In the traditional process, after the coupling reaction is completed, the temperature is directly raised for crystallization, and disperse dyes containing ester groups are prone to hydrolysis under high temperature and strong acid. Phenomenon, affecting product quality, filter cake purity decline, shade deterioration

Method used

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  • A kind of preparation method of azo disperse dye with ester group
  • A kind of preparation method of azo disperse dye with ester group
  • A kind of preparation method of azo disperse dye with ester group

Examples

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Effect test

Embodiment 1

[0039] Put in 98% sulfuric acid (mass percentage concentration, the same below) 2000kg, 28% (mass percentage concentration, solvent is sulfuric acid, the same below) nitrosyl sulfuric acid 2370kg in the diazonium kettle, turn on the chilled brine, stir and cool, and slowly add 900kg of o-chloro-p-nitroaniline, after the addition, keep it under 5℃, keep it warm until the reaction is complete, and set aside;

[0040] Add 30,000 kg of ice water to the coupling kettle, add 10 kg flatly, 30 kg of urea, and then add the above diazonium liquid for dilution, control the temperature at 0 ~ 5 ℃, and slowly add 1710 kg of N, N-diacetoxyethyl- M-Acetaminoaniline, after keeping the temperature until the end point is qualified, start to add ammonia solution (mass percentage concentration is 15%), adjust the pH value of the system to 5.0~6.0, then heat to 60~65℃, stir and turn crystal for 1 hour, wait for the dye After crystal conversion, it is filtered by a filter press and washed with water u...

Embodiment 2

[0043] Put 1000kg of 98% sulfuric acid and 3150kg of 28% nitrosyl sulfuric acid in the diazotizer successively, turn on the chilled brine and stir to cool down, slowly add 900kg of p-nitroaniline, after the addition, keep the temperature below 5°C, keep it warm until the reaction is complete, and set aside;

[0044] Add 15000kg bottom water to the coupling kettle, add 25kg flat and 735kg N,N-diacetoxyethyl-m-acetamidoaniline, after beating for 2 hours, dig out crushed ice to cool down and then add the above diazonium liquid, add 0~ Incubate at 5°C for 6 hours. After the end point is qualified, start to add ammonia solution (18% by mass) to adjust the pH value of the system to 6.0-7.0, then heat to 65-70°C, stir for 1 hour and wait for the dye to turn. After entering the filter press and washing with water to neutrality, 74 Scarlet Disperse Dye filter cake is obtained. The mother liquor water is collected and used for the preparation of ammonium sulfate. The structure of the dye co...

Embodiment 3

[0047] Put 600kg of 98% sulfuric acid and 200kg of 85% phosphoric acid into the diazonium kettle, turn on the stirring, put in 200kg of 2-amino-3,5-dinitrothiophene, 4 hours after beating, turn on the frozen brine, cool to 0℃, start Add 520kg 28% nitrous acid and sulfuric acid dropwise, after the addition, keep the temperature below 5°C, keep it warm until the reaction is complete, and set aside;

[0048] Add 6000kg of bottom water and 800kg of 98% sulfuric acid to the coupling kettle, then add 10kg of AEO-9 emulsifier and 300kg of N,N-diacetoxyethyl aniline, beating for 20 minutes, and after ice cooling, add the above diazonium liquid, add After the temperature is kept at 0~5℃ for 3 hours, after the end point of the test is qualified, start to add aqueous ammonia solution (10% by mass) to adjust the pH value of the system to 5.5~6.5, then heat to 55~60℃, stir and turn crystal for 1 hour. After the dye is transformed into crystals, it is filtered by a filter press and washed with...

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Abstract

The invention discloses a preparation method of an azo disperse dye with an ester group, which comprises: performing a coupling reaction between a diazonium salt and a coupling component; after the coupling reaction is completed, adding a base to the obtained azo compound material system to adjust the The pH value is 5-7, and then the temperature is raised to transform the crystal, and the dye filter cake is obtained after the post-treatment. The invention adjusts the pH value of the system to 5-7 after the coupling reaction is completed and before the crystal transformation operation, so as to avoid the hydrolysis of the ester group in the dye product, improve the yield of the dye product, and reduce the content of organic matter in the waste water , thereby reducing the difficulty of wastewater post-treatment.

Description

Technical field [0001] The invention belongs to the technical field of preparation of disperse dyes, and specifically relates to a preparation method of azo disperse dyes with ester groups. Background technique [0002] Disperse dyes are a kind of special materials used in the dyeing of polyester fibers. In terms of their chemical structure, they mainly include azo, anthraquinone, nitrodiphenylamine, methine and non-azo heterocycles, etc. Among them, most are azo and anthraquinones. Azo dyes occupy an extremely important position in disperse dyes. Among the disperse dyes that have been industrially produced, dyes with azo structure account for 50% and the output accounts for more than 70%. , Its dye chromatogram covers a wide area, has good application performance, simple production process and low cost. [0003] As we all know, the production method of azo-type disperse dyes mainly includes three processes: 1. Diazotization, that is, diazotization reaction between diazonium compo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B29/085C09B29/09
Inventor 徐万福傅伟松陈华祥徐斌丁亚刚
Owner ZHEJIANG DIBANG CHEM
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