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Preparation method of ester group-containing azo disperse dye

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

Active Publication Date: 2016-03-30
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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  • Preparation method of ester group-containing azo disperse dye
  • Preparation method of ester group-containing azo disperse dye
  • Preparation method of ester group-containing azo disperse dye

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Put 2000kg of 98% sulfuric acid (mass percentage concentration, the same below) and 28% (mass percentage concentration, the solvent is sulfuric acid, the same below) nitrosyl sulfuric acid 2370kg in sequence in the diazo kettle, turn on the frozen brine to stir and cool down, and slowly put in 900kg of o-chloro-p-nitroaniline, after adding, keep warm at below 5°C until the reaction is complete, and set aside;

[0040]Add 30000kg of ice water to the coupling kettle, add 10kg evenly, and 30kg of urea, then add the above-mentioned diazo solution for dilution, control the temperature at 0-5°C, and slowly add 1710kg of N, N-diacetoxyethyl- Acetaminoaniline, keep warm 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 up to 60-65 ° C, stir for 1 hour, and wait for the dye to turn After the crystal enters the filter press and presses and washes to neutrality, the filter...

Embodiment 2

[0043] Put 1000kg of 98% sulfuric acid and 3150kg of 28% nitrosylsulfuric acid into the diazo kettle in turn, turn on the frozen brine to stir and cool down, slowly put in 900kg of p-nitroaniline, after adding, keep it warm until the reaction is complete under 5°C, and set aside;

[0044] Add 15,000kg of bottom water to the coupling kettle, add 25kg of Pingpingjia and 735kg of N, N-diacetoxyethyl-m-acetaniline, after beating for 2 hours, dig out crushed ice to cool down, then add the above-mentioned diazonium solution, and add 0 to 5 Incubate at ℃ for 6 hours, after the detection end point is qualified, start to add ammonia solution (mass percentage concentration is 18%) to adjust the pH value of the system to 6.0-7.0, then raise the temperature to 65-70 ℃, stir for 1 hour and wait for the dye to crystallize before proceeding Filter press filter, wash to neutrality, obtain 74 scarlet disperse dyes filter cake, mother liquor water is used for the preparation of ammonium sulfate ...

Embodiment 3

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

[0048] Add 6000kg of bottom water, 800kg of 98% sulfuric acid to the coupling kettle, then add 10kg of AEO-9 emulsifier and 300kg of N, N-diacetoxyethylaniline, beat for 20min, throw ice to cool down, add the above-mentioned diazo solution, add After the temperature is kept at 0-5°C for 3 hours, after the detection end point is qualified, start to add aqueous ammonia solution (10% by mass percentage) to adjust the pH value of the system to 5.5-6.5, then heat up to 55-60°C, stir and crystallize for 1 hour. After the dye is crystallized, enter the filter press and wash to neutrality to ...

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Abstract

The invention discloses a preparation method of an ester group-containing azo disperse dye. The method comprises the following steps: carrying out a coupling reaction on a diazo salt and a coupling component, adding an alkali to the above obtained azo compound material system after the coupling reaction is completed in order to adjust the pH value of the system to 5-7, carrying out heating crystal transformation, and post-processing to obtain a dye filter cake. The pH value of the system is adjusted to 5-7 after the coupling reaction and before the crystal transformation, so hydrolysis of ester groups in the dye product is avoided, the yield of the dye product is improved, and the content of organic matters in wastewater is reduced, thereby the wastewater post-treatment difficulty is reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of disperse dyes, in particular to a preparation method of an azo disperse dye with an ester group. Background technique [0002] Disperse dyes are a kind of special materials used in polyester fiber dyeing. In terms of their chemical structures, they mainly include azos, anthraquinones, nitrodiphenylamines, methines and non-azoheterocyclics. Among them, azo and anthraquinones are the majority, and azo dyes occupy an extremely important position in disperse dyes. Among the disperse dyes that have been industrially produced, the dye varieties with azo structure account for 50%, and the output accounts for more than 70%. , the dye has a wide chromatographic coverage, 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, the diazotization reaction b...

Claims

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Application Information

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Patent Type & Authority Applications(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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