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A kind of clean preparation method of weak basic arylamine azo disperse dye

An aromatic amine azo, disperse dye technology, applied in the direction of azo dyes, monoazo dyes, organic dyes, etc., can solve the problems of difficult post-processing, waste of resources, etc., to achieve environmental protection, saving washing water, energy saving significant effect

Active Publication Date: 2017-12-05
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And when the disperse dye is coupled, since the coupling component is a hydrophobic tertiary amine derivative, it is insoluble in water and needs to be dissolved with an acid. For example, when the coupling component is N,N-dicyanoethylaniline, 50% concentrated Sulfuric acid is used to dissolve it, and after the coupling is completed, a large amount of water is added to dilute the dye, and the dye is obtained by filtration. At the same time, a large amount of sulfuric acid-containing wastewater is generated, which wastes a lot of resources and brings great difficulties to post-treatment.

Method used

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  • A kind of clean preparation method of weak basic arylamine azo disperse dye
  • A kind of clean preparation method of weak basic arylamine azo disperse dye
  • A kind of clean preparation method of weak basic arylamine azo disperse dye

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preparation example Construction

[0035] A cleaning preparation method for weakly basic arylamine azo disperse dyes, comprising the steps of:

[0036] (1) Add the weakly basic arylamine diazonium double salt solid into the coupling component dispersion, and react at 25-50°C for 0.1-5 hours;

[0037] (2) After the reaction is completed, the reaction solution is filtered, and the filter cake is collected and dried to obtain a weakly basic arylamine azo disperse dye.

[0038] Wherein, the weakly basic arylamine diazonium double salt solid has a structure of general formula (I):

[0039]

[0040] In formula (I):

[0041] R 1 -CN, -NO 2 , -Cl, -Br or -I;

[0042] R 2 -H, -CN, -NO 2 , -Cl, -Br or -I;

[0043] x - 1,5-naphthalene disulfonic acid, fluoroboric acid, 2,7-naphthalene disulfonic acid, 2,6-naphthalene disulfonic acid, 1,6-naphthalene disulfonic acid, 1,3,6-naphthalene trisulfonic acid , 1,3,5-naphthalene trisulfonic acid, 1,3-benzenedisulfonic acid, 1,4-benzenedisulfonic acid, 2,6-anthracene di...

Embodiment 1

[0048] Put 200g N,N-dicyanoethylaniline, 1000g water, 2g sodium methylenebismethyl naphthalene sulfonate (MF), 600g quartz sand with a particle diameter of 2mm into a vertical sand mill, and turn it at a speed of 500 rpm / Sand milling under the condition of 2.5 hours for 2.5 hours, measure the particle size distribution of the obtained dispersion liquid, and the average particle size is 7-8 μm. After filtration, the coupling component dispersion liquid was obtained, and the mass percentage of N,N-dicyanoethylaniline was 16.6%.

[0049] Take 119.9g of the above-mentioned coupling dispersion liquid and add it to 100ml of water, stir at room temperature, add 50.6g of 1,5-dinaphthalenesulfonic acid diazonium double salt of 2,6-dichloro-4-nitroaniline within half an hour In the coupling solution, react at 30 degrees centigrade for 2 hours, check with the diazonium ring to confirm the disappearance of the diazonium salt, filter, wash with distilled water until neutral, and obtain 41...

Embodiment 2

[0053] Put 200g of N,N-dicyanoethylaniline, 1200g of water, 800g of quartz sand with a particle size of 2mm, and 2g of MF into a vertical sand mill, and grind at a speed of 100 for 5 hours. Its particle size distribution has an average particle size of 7-8 μm. After filtration, the coupling component dispersion liquid was obtained, and the mass percentage of N,N-dicyanoethylaniline was 16.6%. Take 119.9g of the above coupling component dispersion and add it to 200g of water, stir at room temperature, add 47.1g of 1,5-dinaphthalenesulfonic acid diazonium double salt of 2-chloro-4-nitroaniline within half an hour to the coupling solution, reacted at 35 degrees centigrade for 3 h, checked with the diazonium ring to confirm that the diazonium salt disappeared, filtered, washed with distilled water until neutral, and obtained 38 g of the following structure (compound 2#) disperse dye, yield 98.9%.

[0054]

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Abstract

The present invention provides a clean preparation method for weakly alkaline arylamine azo disperse dye. The method is characterized in that when a weakly alkaline arylamine diazonium double salt solid is coupled with a coupling component, the coupling component is pretreated to obtain a fine particle dispersion to be coupled with the weakly alkaline arylamine diazonium double salt; and the generated disperse dye is precipitated from the coupling system and is filtered and dried, thereby obtaining the weakly alkaline arylamine azo disperse dye. According to the preparation method provided by the present invention, by using a stable double salt structure of a diazonium salt, during the coupling, the process of adding acid for dissolution can be omitted; the coupling is performed at the normal temperature, and extra cooling is not required; and the method has a broad application prospect.

Description

technical field [0001] The invention relates to a preparation method of weakly basic arylamine azo disperse dyes, in particular to a clean preparation method of weakly basic arylamine azo disperse dyes. Background technique [0002] Disperse dyes are non-ionic dyes with simple structure, low water solubility and strong hydrophobicity. They are mainly used for dyeing and printing of synthetic fibers and their blended fabrics. In the process of commercialization, it is sanded together with a dispersant, and it is dyed in a highly dispersed state during dyeing, with excellent color fastness to washing. [0003] In disperse dyes, azo-type disperse dyes account for more than 60% of disperse dyes due to their relatively simple synthesis and complete chromatograms, while azo disperse dyes with weakly basic aromatic amines as diazo components have strong electron-withdrawing groups The introduction of the dye makes the dye red-shift to the maximum absorption wavelength, and obtains...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B29/085
CPCC09B29/0825
Inventor 唐炳涛邱金晶具本植张淑芬
Owner DALIAN UNIV OF TECH
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