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Method of preparing yellow active dyestuff

A reactive dye and yellow technology, which is applied in the field of preparation of yellow reactive dyes, can solve the problems of low color yield, large consumption of raw materials, dust pollution, etc., and achieve the effects of good reproducibility, improved solubility and high reactivity

Inactive Publication Date: 2008-07-09
TIANJIN DEK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The consumption of raw materials in this process is large, the color yield is low, and the method of post-blending will cause dust pollution to the environment

Method used

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  • Method of preparing yellow active dyestuff
  • Method of preparing yellow active dyestuff
  • Method of preparing yellow active dyestuff

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preparation example Construction

[0025] As shown in Figure 2, the preparation process of the yellow reactive dye of the present invention, a preparation method of the yellow reactive dye, comprises the following steps in turn:

[0026] a. Condensation reaction: prepare an aqueous solution of sodium 2,4-diaminobenzenesulfonate with a pH of 6 to 6.5 with a mass percentage concentration of 10-11%, add 2,3-dibromopropionyl chloride dropwise at a low temperature, stir, and react pH=6~6.5, until the reaction is complete;

[0027] b. Diazotization reaction: add the hydrochloric acid solution to step a, adjust the volume with water to make the mass percentage concentration of the solution 7%, ensure that the Congo red test paper is blue after dipping, and the KI test paper is slightly dipped after dipping. Under the blue condition, add sodium nitrite solution dropwise until the reaction is complete;

[0028] c. Coupling reaction: eliminate the excess nitrous acid in step b with sulfamic acid, add water to adjust the...

Embodiment 1

[0041] 1. Ingredients list:

[0042] raw material name

molecular weight

Molecular ratio

100% dosage (Kg)

Feeding amount (kmol)

Sodium 2,4-diaminobenzenesulfonate

2,3-Dibromopropionyl chloride

Sodium nitrite

hydrochloric acid

1-(2,5-dichloro-4-sulfonic acid)benzene

yl-3-methyl-5-pyrazolone

210

250.5

69

36.5

323

1

1.05

0.816

2

0.8

288.75

361.66

77.42

100.38

355.3

1.375

1.375

1.375

1.375

1.375

[0043] 2, the yellow reactive dye preparation process of the present invention operates as follows:

[0044] a. Dissolution of sodium 2,4-diaminobenzenesulfonate

[0045] Put 2400 liters of bottom water into the reaction tank, add 288.75 kg of sodium 2,4-diaminobenzenesulfonate, heat up to 22°C, stir to dissolve, and make the material completely dissolved and clarified. Adjust pH=...

Embodiment 2

[0077] a. Dissolution of sodium 2,4-diaminobenzenesulfonate

[0078] Put 2400 liters of bottom water into the reaction tank, add 288.75 kg of sodium 2,4-diaminobenzenesulfonate, heat up to 22°C, stir to dissolve, and make the material completely dissolved and clarified. Adjust pH=6~6.5 with dilute hydrochloric acid. The volume is 2625 liters, and the mass percentage concentration of the solution is 11%.

[0079] b. Condensation reaction

[0080] Directly use ice and jacketed circulating cold water to adjust the temperature of solution a to 0 to 5 °C, adjust the mass percentage concentration of the solution to 10%, add 2,3-dibromopropionyl chloride within 1.5 to 2 hours, and use sodium bicarbonate at the same time. The pH was maintained at 6-6.5, and the reaction was stirred for 2 hours. Reaction temperature 0~5 ℃, reaction pH=6~

[0081] 6.5. Finally, the end point was detected by TLC aluminum-based silica gel thin layer plate.

[0082] c, diazotization reaction

[0083...

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Abstract

The invention discloses a process for preparing a yellow reactive dye, which comprises utilizing 2, 4-diamino benzensulfonate, 2, 3-dibromo propionyl chlorine, hydrochloric acid, sodium nitrite, 1-(2,5- dichloro-4- sulfonic acid) phenyl group-3 -methyl-5-pyrazolone and caustic soda to be main raw material, and condensing, diazotizing, coupling, handling alkali, adding auxiliary agent, improving dye strength, adjusting color cast, adjusting intensity, dying and packing. The invention adopts front color matching, color yield percentage is high, and the cost of raw material which is needed is lowered, compared with the original technique, the invention reduces the discharging of waste water, and the dissolvability of dye is improved to a new level.

Description

technical field [0001] The present invention relates to a preparation method of reactive dyes, in particular to the preparation method of yellow reactive dyes. Background technique [0002] Reactive dyes have the remarkable characteristics of bright color, excellent application performance, convenient use and strong applicability. In the 21st century, due to environmental and ecological constraints and economic factors, the requirements for the production, preparation, coloring rate, color fixing rate and dyeing wastewater of reactive dyes are getting higher and higher. A kind of existing yellow reactive dye, its molecular structure formula is as follows: [0003] [0004] The dye industry also calls it yellow 4G. As shown in Figure 1, at present, reactive yellow 4G dyes for wool use 2,4-diaminobenzenesulfonic acid and 2,3-dibromopropionyl chloride to condense in the preparation process, and then go through refining, diazotization, coupling, alkali, etc. Processing, sa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B62/008
Inventor 张兴华苏长湘郭建荣
Owner TIANJIN DEK CHEM
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