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Crosslinking modification method of azo-disperse dye

A technology of disperse dyes and cross-linking modification, applied in the preparation of azo dyes, azo dyes, dyeing methods, etc. problem, to achieve the effect of improving heat-resistant migration, increasing molecular weight, and improving affinity

Active Publication Date: 2014-07-30
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its large molecular weight, it is difficult to permeate and diffuse in the fiber during dyeing, and it is difficult to obtain commercial disperse dyes with good dispersion stability, which affects its further application in the field of fiber dyeing.

Method used

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  • Crosslinking modification method of azo-disperse dye
  • Crosslinking modification method of azo-disperse dye
  • Crosslinking modification method of azo-disperse dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Disperse Red 13 and diphenylmethane-4.4' diisocyanate (MDI) crosslinked

[0044] Reactant Molecular Formula:

[0045]

[0046] Product 1 Molecular Formula

[0047] Synthesis:

[0048] Weigh 2.0 grams of Disperse Red 13 parent dye purified by recrystallization and vacuum drying, add in a 1000ml three-necked flask equipped with a reflux device (connected to a calcium chloride drying tube), add 600ml of toluene through dehydration, and start magnetic stirring , to dissolve the dye, add 10ml of stannous octoate, and gradually heat up to 85°C. Accurately weigh 0.7155 g of diphenylmethane-4.4' diisocyanate (MDI), dilute and dissolve with 40 ml of toluene solvent, slowly drop it into the reactor within 120 min, continue the heat preservation reaction for 2 h, stop heating, cool to room temperature, the product Precipitated, and obtained 1.31 g of the product by filtration, with a yield of 48.24%.

[0049] Molecular Characterization:

[0050] (1) 1 H NMR (400MHz, DMSO):...

Embodiment 2

[0064] Disperse Red 13 and Hexamethylene Diisocyanate (HDI) Crosslinked

[0065] Reactant Molecular Formula:

[0066]

[0067] Product 2 Molecular Structural Formula

[0068] Synthesis:

[0069] Weigh 2.0 grams of Disperse Red 13 parent dye purified by recrystallization and vacuum drying, add in a 1000ml three-necked flask equipped with a reflux device (connected to a calcium chloride drying tube), add 600ml of toluene through dehydration, and start magnetic stirring , to dissolve the dye, add 10ml of stannous octoate, and gradually heat up to 85°C. Accurately weigh 0.4879 g of hexamethylene diisocyanate (HDI), dilute and dissolve it with 40 ml of toluene solvent, slowly drop it into the reactor within 120 min, continue the heat preservation reaction for 2 h, stop heating, cool to room temperature, the product precipitates, and the Filtration afforded 0.7972 g of product, a 32.04% yield.

[0070] Molecular Characterization:

[0071] (1) 1 H NMR (400MHz, DMSO): 1.13(t...

Embodiment 3

[0085] Disperse Orange 3 and diphenylmethane-4.4' diisocyanate (MDI) crosslinking

[0086] Product Molecular Structural Formula:

[0087]

[0088] Product 3 Molecular Structural Formula

[0089] Synthesis:

[0090] Weigh 2.0 grams of Disperse Orange 3 parent dye purified by recrystallization and vacuum drying, add it to a 1000ml three-necked flask equipped with a reflux device (connected to a calcium chloride drying tube), add 600ml of toluene through dehydration, and start magnetic stirring , to dissolve the dye, add 10ml of stannous octoate, and gradually heat up to 85°C. Accurately weigh 0.8879 g of diphenylmethane-4.4' diisocyanate (MDI), dilute and dissolve it with 40 ml of toluene solvent, slowly drop it into the reactor within 120 min, continue the heat preservation reaction for 2 h, stop heating, cool to room temperature, the product Precipitated, obtained 2.3718 g of product by filtration, and the yield was 82.13%.

[0091] Molecular Characterization:

[0092...

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Abstract

The invention relates to a crosslinking modification method of azo-disperse dye. The method comprises the steps of: adding a proper amount of disperse dye parent which is subjected to purification and vacuum drying into a flask equipped with a reflux device, adding an organic solvent which is subjected to dehydration treatment as a reaction solvent, stirring to dissolve the disperse dye parent, adding an organic tin type catalyst, gradually heating to 80-95 DEG C, precisely weighing a crosslinking agent, dissolving and diluting with a proper amount of reaction solvent, slowly dropping into a reactor within 60-90min, performing heat preservation reaction for 2-4h, stopping heating and cooling to room temperature; performing purification and separation through adding the reaction solvent and filtering to obtain a product. With the method, the phenomenon that the color fastness is poor because dye molecules of the current novel hydrophobic fiber disperse dye are easy to migrate in dyeing is improved, and washing fastness and resistance to dry heat of disperse dye obtained by crosslinking modification in spandex dyeing are greatly improved.

Description

technical field [0001] The invention relates to a crosslinking modification method of azo disperse dyes. Background technique [0002] Disperse dyes were first used in the dyeing of acetate fibers, and developed rapidly with the development of polyester fibers (polyester) since the 1950s. Now the world's disperse dyes are the most important and main category in the dye industry. The total domestic production of disperse dyes is about 400,000 tons per year, accounting for 75% of the world's total production. Has strong market competitiveness. [0003] Due to the relatively tight molecular structure of polyester, disperse dyes are generally required to have the characteristics of relatively simple molecular structure and small volume. According to the molecular weight of disperse dyes, it can be divided into three types of disperse dyes: low energy type (small molecular weight), medium energy type and high energy type (larger molecular weight). So far, there are many kinds ...

Claims

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Application Information

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IPC IPC(8): C09B43/26C09B43/155D06P1/18D06P3/26
Inventor 钱红飞
Owner SHAOXING UNIVERSITY
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