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Preparation method of disperse scarlet

A scarlet and dispersing technology, applied in the field of preparation of disperse scarlet, can solve the problems of increasing production cost, generation of three wastes, dust generation, etc., and achieve the effect of reducing waste water discharge, reducing side reactions, and reducing consumption

Active Publication Date: 2010-10-13
JIANGSU YUANZHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defect of this method is that: this method will increase the production cost, and there will be a large amount of three wastes; the cost of purchasing 5,6-dichloro-2-aminobenzothiazole is high, and the The production of thiazole requires a large amount of sulfuric acid, and a large amount of liquid caustic soda must be added for neutralization when the product is precipitated, and a large amount of sulfuric acid-containing wastewater will be produced, which contains a large amount of COD; 5,6-dichloro-2-aminobenzothiazole A large amount of steam is required during drying, and waste gas will be generated, and dust will be generated during crushing

Method used

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  • Preparation method of disperse scarlet

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Example 1. A preparation method for dispersing scarlet, the steps are as follows:

[0031] (1) Preparation of thiourea: Pour appropriate amount of tap water into the reaction kettle, put in 3,4-dichloroaniline after heating up to 60°C, and stir to fully dissolve the material after throwing in, and the dissolution temperature is 60°C; Add hydrochloric acid to the kettle dropwise, immediately after dropping, add ammonium thiocyanate aqueous solution, and immediately add the remaining hydrochloric acid; then raise the temperature to 80°C and keep warm for reaction, and cool and crystallize after the reaction; discharge and filter to obtain thiourea and mother liquor water 1, thiourea is washed with water to neutrality, and dried to obtain thiourea; the weight ratio of the 3,4-dichloroaniline, hydrochloric acid, and ammonium thiocyanate is 1: 0.5: 0.4; the hydrochloric acid added dropwise for the first time is hydrochloric acid 3 / 4 of the total weight;

[0032] (2) Closed...

Embodiment 2

[0035] Example 2. A preparation method for dispersing scarlet, the steps are as follows:

[0036](1) The preparation of thiourea: pour into the reaction kettle the mixed liquor that an amount of mother liquor water I and tap water mix; Drop into 3,4-dichloroaniline after being warmed up to 90 ℃, throw and stir and make material fully dissolve, The dissolution temperature is 90°C; then add hydrochloric acid dropwise to the reaction kettle for the first time, and immediately put in ammonium thiocyanate aqueous solution after dropping, and immediately add the remaining hydrochloric acid; then raise the temperature to 100°C, keep warm for reaction, and cool to crystallize after the reaction; Blowing and filtering to obtain thiourea and mother liquor water I, washing thiourea with water to neutrality, and drying to obtain thiourea; the weight ratio of the 3,4-dichloroaniline, hydrochloric acid, and ammonium thiocyanate is 1: 1.0 : 0.7; The hydrochloric acid that drops for the firs...

Embodiment 3

[0040] Example 3. A preparation method for dispersing scarlet, the steps are as follows:

[0041] (1) The preparation of thiourea: pour into the reaction kettle the mixed liquor that an amount of mother liquor water I and tap water are mixed; Drop into 3,4-dichloroaniline after being warmed up to 75 ℃, throw and stir and make material fully dissolve, The dissolution temperature is 75°C; then add hydrochloric acid dropwise to the reaction kettle for the first time, immediately put in ammonium thiocyanate aqueous solution after dropping, and immediately add the remaining hydrochloric acid; then raise the temperature to 90°C, keep warm for reaction, and cool to crystallize after the reaction; Blowing and filtering to obtain thiourea and mother liquor water I, washing thiourea with water to neutrality, drying to obtain thiourea; the weight ratio of the 3,4-dichloroaniline, hydrochloric acid, ammonium thiocyanate is 1: 0.75 : 0.55; the hydrochloric acid that drops for the first ti...

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Abstract

The invention relates to a preparation method of disperse scarlet, which is characterized by comprising the steps such as preparation of thiourea, closing ring, diazotization, coupling and the like, wherein the thiourea is prepared by adopting 3, 4-dichloroaniline, hydrochloric acid and ammonium thiocyanate for reaction; a closed ring is prepared by adding sulfuric acid, the thiourea and bromine in a reaction kettle; diazotization means that secondary heavy nitrogen is adopted for reaction to prepare secondary heavy nitrogen material; coupling means that emulsifying agent OP-10, N-ethyl-N-cyanoethyl phenylamine, sulfamic acid, defoaming agent tributyl phosphate and the secondary heavy nitrogen material are adopted for reaction until the coupling reaction finish that the N-ethyl-N-cyanoethyl phenylamine is excessive; and finally the finished product of the disperse scarlet can be obtained by press filtering, washing and drying. The preparation method is more reasonable in technique, and the mother solution can be recovered, so that the product yield is effectively improved, the production cost is reduced, and the discharge of the waste water (COD) is decreased.

Description

technical field [0001] The invention relates to a preparation method of a dye, in particular to a preparation method of disperse scarlet. Background technique [0002] The preparation method of disperse scarlet GS in the prior art is: adopt 5,6-dichloro-2-aminobenzothiazole to dissolve in sulfuric acid, add dropwise acetic acid or phosphoric acid, adjust acidity, then dropwise add nitrosyl sulfuric acid, carry out heavy Nitriding, and then react with N-ethyl-N-cyanoethylaniline dissolved in dilute sulfuric acid to generate disperse scarlet GS. The defect of this method is that: this method will increase the production cost, and there will be a large amount of three wastes; the cost of purchasing 5,6-dichloro-2-aminobenzothiazole is high, and the The production of thiazole requires a large amount of sulfuric acid, and a large amount of liquid caustic soda must be added for neutralization when the product is precipitated, and a large amount of sulfuric acid-containing wastewa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/09C09B29/045
Inventor 王海民程燕明张毅
Owner JIANGSU YUANZHENG CHEM
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