Preparation method of crimson reactive dye

A reactive dye and deep red technology, applied in reactive dyes, dyeing methods, organic dyes, etc., can solve the problems of low product content, high energy consumption, environmental pollution, etc., and achieve high color fixation rate, low energy consumption, and low raw material consumption Effect

Active Publication Date: 2013-09-18
中国中化股份有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of preparation method of reactive dye carmine as shown above, to overcome the problems of low product content, high energy consumption and environmental pollution existing in the existing preparation method

Method used

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  • Preparation method of crimson reactive dye
  • Preparation method of crimson reactive dye
  • Preparation method of crimson reactive dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] a) One condensation

[0027] Weigh 1.88 parts of cyanuric chloride, add 18 parts of water and crushed ice, and beat at 0-5°C for 45 minutes. At the same time, weigh 3.41 parts of H acid in 15 parts of water, adjust the pH to 6-6.5 with sodium carbonate, and dissolve it completely. After the beating is finished, drop the above-mentioned H acid solution into the cyanuric chloride suspension within 1 hour. After the dropwise addition, adjust the pH value of the reaction to 2.0-2.5 with sodium carbonate, and react for 2 hours until there is no free H acid, which is the end point.

[0028]

[0029] b) Secondary condensation

[0030] Weigh 3.03 parts of N-ethyl meta-ester and add it to the above-mentioned primary condensation reaction solution, and at the same time raise the temperature to 30-34°C, adjust the pH value to 3-3.5 with sodium carbonate, keep this temperature and pH value for about 4 hours, and perform HPLC The detection of the disappearance of the N-ethyl m...

Embodiment 2

[0039] Repeat the material ratio and process conditions in the operation process of each step in Example 1, the difference is in the secondary condensation of step (b) in Example 1, the reaction temperature is 26~30 ° C, and the pH value is 4~4.5; ( c) After diazotization, adjust the pH of the diazonium salt to 6.5 to 7; (d) during the coupling, adjust the temperature of the dicondensate solution to 15°C, pH = 7 to 7.5, and the pH of the coupling reaction to 8 to 8.5, and finally obtain 15 Part reactive dye crimson.

Embodiment 3

[0041]Repeat the material ratio and process conditions in the operation process of each step in Example 1, the difference is in the secondary condensation of step (b) in Example 1, the reaction pH value is 4~4.5; (c) in the diazotization, Adjust the pH of the diazonium salt at 10-15°C to 6.5-7; (d) in coupling, adjust the temperature of the dicondensate solution to 20°C, pH=7-7.5, and finally obtain 15 parts of reactive dye deep red.

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Abstract

The invention provides a method for preparing a crimson reactive dye with a structure represented by a following formula, wherein M is selected from Na, K, or Li. The method comprises the steps that: (1) an N-ethyl meta-ester solid is added into a primary condensation solution formed by condensation of cyanuric chloride and H acid, and secondary condensation is carried out; the pH of an obtained secondary condensate solution is regulated to neutral or near neutral before a coupling reaction; (2) 2-naphthylamine-1-sulfonic acid is subjected to reverse-method diazotization; the pH of obtained diazonium salt is regulated to neutral or near neutral; (3) the diazonium salt is added into the secondary condensate in one time, and the coupling reaction is carried out under a neutral or weakly alkaline condition, such that a target dye liquid is obtained; and the liquid is directly dried, such that a solid product is obtained. The method provided by the invention has the advantages of low cost, low energy consumption, and no pollution. Various application performance indicators of the prepared product reach or exceed those of products of companies abroad.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a research on a preparation method of reactive dyes, in particular to a preparation method of reactive dye deep red. Background technique [0002] Reactive dyes have the characteristics of bright color, excellent application performance and convenient use. However, restricted by the ecological environment and economic factors, the requirements for the production cost and application performance of reactive dyes are getting higher and higher. Japanese patent JP7179784 discloses a reactive dye dark red, the structural formula is as follows: [0003] [0004] Most of the prior art is to introduce the application report on cotton after the dye structure and other dyes are blended, and its preparation method is only published in "Journal of Dalian University of Technology" in July, 2000. Chlorotriazine / vinyl sulfone dual reactive dye performance research" mentioned in the literature. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B62/51D06P1/38D06P3/14
Inventor 尚庆梅徐飒英
Owner 中国中化股份有限公司
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