Black and active dye

A reactive dye and black technology, which is applied to the composition and synthesis process of deep black reactive dyes, can solve the problems of not reaching the degree of deep black, large difference in fiber affinity, color pattern, etc.

Inactive Publication Date: 2006-02-08
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the output of reactive black obtained by the above-mentioned dyes has reached 10,000 tons, this blended dye has the following serious disadvantages: (1) the blackness is still not ideal, and cannot reach the level of deep black; (2) the two are water soluble There is a large difference in directness and directness to cellulose fibers, and the compatibility of dyeing performance is poor: the

Method used

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  • Black and active dye
  • Black and active dye
  • Black and active dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Synthesis of sodium hydroxymethanesulfonate:

[0065]

[0066] Dissolve 104g of sodium bisulfite (1mol) in 150ml of water in a 500ml three-necked flask, add 88g of 36% formaldehyde solution (1.05mol) dropwise at 35°C, and stir the reaction below 50°C for 3-5 hours. Dehydrate 100ml under reduced pressure at 60-70°C to obtain a concentrated solution. Cool the concentrated solution, add a certain amount of crystallization solvent, stand at 0-5°C for 5 hours to crystallize, filter, wash the filter cake with 30ml of absolute ethanol, and dry to obtain 125g of sodium hydroxymethanesulfonate as a white solid.

Embodiment 2

[0068] Synthesis of sulfomethylated J acids:

[0069]

[0070] Disperse 23.9g of J acid in 200ml of water in a 500ml three-necked bottle, and use 20% Na 2 CO 3 Adjust the pH of the solution to 6-7, add 15g of sodium hydroxymethanesulfonate, and react for 3-6h below 50°C to obtain a sulfomethylated J acid solution, wherein the content of sulfomethylated J acid in the organic matter is ≥95% ( HPLC).

Embodiment 3

[0072] Synthesis of red dye 201:

[0073] Mix 56.2g of para-ester and 13g of sulfuric acid, add 350g of ice-water mixture, beat for 30min, add 47g of 30% NaNO dropwise at 0-5°C 2 Solution, NaNO during dropwise addition and reaction 2 excess. After the dropwise addition, continue to stir the reaction for 2h, the excess NaNO 2 Destroy it with sulfamic acid to obtain the para-ester diazonium salt.

[0074] Add the para-ester diazonium salt to the sulfomethylated J acid solution of Example 2, control the pH ≤ 2 at 0-5°C, and perform the coupling reaction for 3 hours, then adjust the pH to 5-6, and perform the coupling reaction for 3 hours. Concentrate the resulting dye solution, fry it to dryness, and pulverize it to obtain 125 g of dye powder.

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Abstract

The invention provides a black composite reactive dye having three primary color constituents comprising, green disazo dye employing ethylene sulfone series arylamine or aniline derivative as diazo component and H acid as coupling component, one ore more red disazo dyes employing sulfoalkyl J acid or carboxymethyl J acid derivatives as coupling components, one ore more yellow bisazo or polyazo dyes employing sulfochlorinated 3,5-diaminobenzoic acid or sulfoalkyl derivatives as coupling components. The dye can be applied to intermittent and continuous dyeing for cellulose fiber, protein fiber, poly nylon and their fiber mixed fabrics.

Description

technical field [0001] The invention relates to the composition and synthesis process of a multi-component dark black reactive dye. Its characteristic is that the coloring speed of each component of the dye is similar to that of the fiber, and the dyed fiber has good blackness, level dyeing and good fastness. The dye is suitable for exhaust dyeing, pad-steaming, pad-baking and pad-stacking and jet dyeing of cellulose fibers, protein fibers and polyamide fibers. Background technique [0002] Black dye is the most widely used and most productive color in dyes. Among them, C.I. Reactive Black 5 is the most productive reactive dye in the world. But as a black dye, its blackness is not enough. In 1988, South Korea used the principle of complementary color to improve the blackness of the dyed fiber by adding the following orange components, which doubled the output of reactive black. At the same time, it has become the pioneer to improve the quality of active black through dye...

Claims

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Application Information

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IPC IPC(8): C09B67/24
Inventor 吴祖望冯柏成王专林莉
Owner DALIAN UNIV OF TECH
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