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Azo type disperse dye composition synthesis method

A technology for disperse dyes and synthesis methods, which is applied in the field of synthesis process of azo-type disperse dye compositions, can solve problems such as unsatisfactory light fastness of single-color varieties, achieve reduction of production costs and sewage discharge, high and low temperature dispersion The effect of stable stability and mild crystal conversion process

Active Publication Date: 2014-04-09
ZHEJIANG JIHUA GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem that 2,4-dinitroaniline easily causes the light fastness of its single-color varieties to be generally not ideal, the present invention proposes a synthetic method of an azo-type disperse dye composition, which not only solves the problem of light fastness The problem of high temperature, and the process of crystal transformation is mild, the high and low temperature dispersion stability and color light of the dye are relatively stable

Method used

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  • Azo type disperse dye composition synthesis method
  • Azo type disperse dye composition synthesis method
  • Azo type disperse dye composition synthesis method

Examples

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Effect test

Embodiment 1

[0032] According to the product being a mixture of disperse violet, the mol ratio of the coupling component N ethyl-N-cyanoethyl m-aminoacetanilide to N-allyl N-cyanoethyl o-methoxy m-acetanilide is reversed to be 3 :2.

[0033]Diazotize 0.2mol of 2,4-dinitroaniline by conventional methods to obtain 0.2mol of the diazo component of 2,4-dinitroaniline, and dilute it into 600g of ice water at about 0°C to synthesize the diazo component Liquid separation; add emulsifier OP-10 and dispersant sulfamic acid 1g each, then weigh 0.132mol of N-ethyl-N-cyanoethyl m-aminoacetanilide, and dissolve it in 10% dilute sulfuric acid solution below 10°C In the range of 0-10°C, add it dropwise to the above-mentioned diluted diazo component liquid to start the coupling reaction, keep it for 0.5-1 hour to obtain the reaction product, and then weigh N-allyl-N-cyanoethyl 0.088 mol of o-methoxy m-acetamidoaniline, dissolved in 10% dilute sulfuric acid, and then added dropwise to the above reaction p...

Embodiment 2

[0034] According to the product being a mixture of disperse violet, the molar ratio of the coupling component N-cyanoethyl-N-benzyl-m-acetanilide to N,N-diallyl-o-methoxy-m-acetanilide is 59: 41.

[0035] 0.2mol of 2,4-dinitroaniline is diazotized by conventional methods to obtain 0.2mol of the diazo component of 2,4-dinitroaniline. In a 2000ml beaker, add 200ml of 10% dilute sulfuric acid and cool down to below 10°C , add 0.118mol N-cyanoethyl-N-benzyl-m-acetanilide and 0.082mol N,N-diallyl-o-methoxy-m-acetanilide under stirring to dissolve, add ice 400g after complete dissolution, and add disperse Add 1g of sulfamic acid and emulsifier OP-10, then add the above diazo component solution dropwise into the dissolved mixed azo component liquid, control the temperature at 0-10°C, keep it until the diazo component Disappearance is the end point. After the end point is reached, the temperature is raised to 40° C. for 1 hour, and filtered to obtain a mixture of disperse violet dyes...

Embodiment 3

[0037] According to the product being a mixture of disperse violet, the molar ratio of the coupling component N,N-diethyl-m-acetanilide to N-allyl-N-cyanoethyl o-methoxy-m-acetanilide is 3: 2.

[0038] 0.2mol2,4-dinitroaniline is diazotized by conventional methods to obtain 0.2mol of the diazo component of 2,4-dinitroaniline, which is divided into two parts of 50% and 50% by weight, and N,N- Dissolve 0.114mol of diethyl-m-aminoacetanilide in 10% sulfuric acid solution below 10°C, pour it into a 2000ml beaker after fully dissolving, add 400g of ice, and add dropwise to the above-mentioned portion at -5~5°C In the nitrogen component, obtain the reaction product, keep it for 1 hour, then dissolve 0.076mol of N-allyl-N-cyanoethyl-o-methoxym-acetaniline with 10% dilute sulfuric acid, dissolve completely, and pour it into the above-mentioned To the reaction product, add a small amount of ice and adjust the temperature of the coupling liquid to about 0°C, add another part of the dia...

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Abstract

The present invention relates to the technical field of disperse dyes, and provides an azo type disperse dye composition synthesis method so as to solve the problem of not ideal light fastness of the single color variety due to 2,4-dinitroaniline. The synthesis method comprises that: a diazo component 2,4-dinitroaniline of various components in the desired mixture concurrently reacts in the same diazotization device, various coupling components of the mixed dye are coupled in the same coupling device through a plurality of coupling manners according to the ratio requirement with the diazo during coupling, the obtained coupling solution can be subjected to a temperature increase crystal transformation treatment before entering a filter if necessary so as to make the crystal form of the obtained dye be stable, and pressure filtration is performed to directly obtain the dye mixture with the required ratio. According to the present invention, the light fastness problem is solved, the crystal transformation process is mild, and the high temperature dispersion stability, the low temperature dispersion stability and the chromatic light of the dye are stable.

Description

technical field [0001] The invention relates to the technical field of disperse dyes, in particular to a synthesis process of an azo-type disperse dye composition. Background technique [0002] The dyes synthesized by 2,4-dinitroaniline generally have the characteristics of bright red and strong color, but due to its structural defects, the light fastness of its monochromatic varieties is generally not ideal. - Introducing electron-withdrawing groups at the position to enhance the light fastness of this dye, but the cost is greatly increased, and it is not suitable for the requirements of production enterprises from an economic point of view. [0003] Chinese patent CN103113758A discloses several purple dyes with 2,4-dinitroaniline as the diazo component structure. This invention discloses a mixture of disperse dyes using compounding technology to successfully solve this problem. However, this invention is usually coupled under low temperature conditions, and after a harsh ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/22C09B67/42C09B29/085C09B29/26D06P1/18D06P3/54
Inventor 孙岩峰陈美芬汪雪松简卫
Owner ZHEJIANG JIHUA GROUP
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