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A kind of reactive yellow dye with high washing fastness and preparation method thereof

A technology for yellow dyes and wash fastness, applied in the direction of reactive dyes, azo dyes, organic dyes, etc., can solve the problems of dye compatibility inconsistency, washing fastness can not meet the real life and environmental protection, etc., to achieve various fastness Excellent degree, bright color, high lifting effect

Active Publication Date: 2017-10-27
TAIXING JINYUN DYESTUFF
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Due to the large differences in the structure of the above-mentioned compounded dyes, the compatibility of the dyes is likely to be inconsistent, and the washing fastness cannot meet the needs of real life and environmental protection.

Method used

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  • A kind of reactive yellow dye with high washing fastness and preparation method thereof
  • A kind of reactive yellow dye with high washing fastness and preparation method thereof
  • A kind of reactive yellow dye with high washing fastness and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 1. Condensation reaction for intermediate preparation

[0061] Add 16.2g of acetanilide to 13.8g of chlorosulfonic acid and control the temperature at 20-30°C. After the addition, slowly raise the temperature to 40-65°C and react for 2 hours, add 28.3g of thionyl chloride dropwise for 2 hours, cool down to 25°C and add The precipitate was diluted with ice water and filtered to obtain 63.1 g (40%) of wet product p-acetaminobenzenesulfonyl chloride.

[0062] Two, thioether synthesis

[0063] Add 14.1g of 2-chloroethylamine hydrochloride to 9.4g of mercaptoethanol solution under stirring, adjust pH=4.8 with sodium bicarbonate at the same time, react at 55°C for 4 hours to generate 13.8g of β-hydroxyethyl sulfide ethylamine . After reaching the end point, cool down to 0°C, slowly add 63.1g (40%) of the wet product p-Acetaminobenzenesulfonyl chloride, adjust the pH to 3.8 with baking soda after the addition, control the temperature at 0-2°C for 4 hours, let stand and separ...

Embodiment 2

[0081] 1. Condensation reaction for intermediate preparation

[0082] Add 15.8g of acetanilide to 135g of chlorosulfonic acid and control the temperature at 20-30°C. After the addition, slowly raise the temperature to 40-65°C for 2 hours, add 28.1g of thionyl chloride dropwise for 2 hours, cool down to 25°C and add ice Diluted with water and filtered to obtain 61.4g (40%) of p-acetaminobenzenesulfonyl chloride.

[0083] Two, thioether synthesis

[0084] Add 13.8g of 2-chloroethylamine hydrochloride to 9.1g of mercaptoethanol solution under stirring, adjust pH=4.8 with sodium bicarbonate at the same time, react at 52°C for 4 hours to generate 13.5g of β-hydroxyethyl sulfide ethylamine . After the end point is reached, cool down to 0°C, slowly add 61.4g (40%) of the wet product p-Acetaminobenzenesulfonyl chloride, adjust the pH to 3.5 with baking soda after the addition, control the temperature at 0-2°C for 4 hours, let stand and separate Separate and wash twice to obtain 31....

example 1

[0103] Compared with reactive yellow M-3RE, the synthetic reactive yellow dye of example 1 has the following characteristics:

[0104] Table 1

[0105]

[0106] During the test of the performance indicators in Table 1, the following standards were used:

[0107] GB / T2374-2007 General Conditions for Determination of Dye Dyeing

[0108] GB / T2381-2013 Dyes and dye intermediates - Determination of insoluble content

[0109] GB / T2386-2006 Determination of moisture in dyes and dye intermediates

[0110] GB / T2387-2013 Reactive dyes - Determination of shade and intensity

[0111] GB / T2389-2006 Reactive dyes - Determination of the relative content of hydrolyzed dyes and standard samples

[0112] GB / T2390-2013 Determination of pH value of dyes

[0113] GB / T2391-2006 Reactive dyes - Determination of color fixation rate

[0114] GB / T3671.1-1996 Determination method of solubility and solution stability of water-soluble dyes

[0115] GB3899.1-2007 Nomenclature of Dyestuff Products f...

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Abstract

The invention discloses a reactive yellow dye with high washing fastness and a preparation method thereof. m-phenylenediamine is acylated with sodium cyanate under acidic conditions to generate m-ureamidoaniline, which is combined with 3,6,8-trisulfone The diazonium salt of acid-2-naphthylamine is coupled to obtain a chromogen, and the chromogen and cyanuric chloride are condensed once, and then reacted with acetanilide, chlorosulfonic acid, and thionyl chloride to generate p-acetamidobenzenesulfonyl chloride, and The sulfide generated by the reaction of 2-chloroethylamine hydrochloride and mercaptoethanol is condensed to obtain thioether, and the 2-[2-(4-aminobenzenesulfonamido) ethyl sulfone obtained by re-oxidizing and esterifying the sulfide Base] hydroxyethyl sulfate intermediate for secondary condensation, filter, collect the filtrate, and directly spray dry to obtain a semi-finished product. The reactive yellow dye of the present invention has high directness, good compatibility, high lifting power, high color fixation rate, and excellent fastness; it is suitable for dyeing, printing and printing of cellulose fiber, protein fiber, viscose fiber and polyamide fiber. Pad dyeing, the washing fastness is higher than the 0.5‑1 level of general varieties.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a reactive yellow dye with high washing fastness and a preparation method thereof. Reactive yellow dye has the characteristics of bright color, high solubility, high directness, good compatibility, high lifting power, high color fixing rate, and excellent fastness. The dye is suitable for dyeing, printing and padding of cellulose fiber, protein fiber, viscose fiber and polyamide fiber, and its washing fastness is 0.5-1 higher than that of general varieties. Background technique [0002] The amount of yellow reactive dyes is lower than that of black and red. The main products are C.I reactive yellow 145 (reactive yellow M-3RE), C.I reactive yellow 176 (reactive yellow 3RS), C.I reactive yellow 160 (reactive yellow B-4GLN ), Reactive Yellow S-3R, etc. Although these kinds of yellow varieties can be dyed on cellulose fibers to obtain shades of different vividness, C.I Reacti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B62/51
Inventor 赵卫国苏金奇鞠苏华王国民张卫平
Owner TAIXING JINYUN DYESTUFF