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A kind of preparation method of sulfur dye

A technology of sulfur dyes and sulfide bases, applied in sulfur dyes, chemical instruments and methods, dyeing methods, etc., can solve the problems of general blackness of cloth samples and poor decolorization effect.

Active Publication Date: 2022-02-18
SHANXI LINFEN DYE CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the traditional yellow-green photosulfur black dye produced from 2,4-dinitrochlorobenzene produced by chlorobenzene has a green light value of CIEDa -0.2~-0.5 and a yellow light value of -0.2~-0.5, which are relatively large and easy to dye. In the process, there are common problems such as average blackness of the cloth sample and poor decolorization effect after dyeing.

Method used

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  • A kind of preparation method of sulfur dye
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  • A kind of preparation method of sulfur dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment A1

[0027] Add 100g of o-nitrochlorobenzene into a 1000ml Erlenmeyer flask, heat it to a temperature of about 55°C in the observed pot, start stirring, and start to add 180g of mixed acid dropwise. The whole dropping process was controlled at 47±2°C. Add dropwise for about 1h and keep warm for 15 minutes. After the heat preservation is completed, it takes 1 hour to raise the temperature to about 100°C and keep the temperature for 3 hours. After the completion of the reaction, let stand for 40min and separate. The obtained product 2,4-dinitrochlorobenzene (DNCB) was 198g, with a purity of 90.23%, isomers of 9.77%, and a crystallization point of 44.8°C.

Embodiment A2

[0029] Add 100g of o-nitrochlorobenzene into a 1000ml Erlenmeyer flask, heat it to a temperature of about 55°C in the observed pot, start stirring, and start to add 180g of mixed acid dropwise. The whole dropping process was controlled at 47±2°C. Add dropwise for about 1h and keep warm for 15 minutes. After the heat preservation is completed, it takes 2 hours to raise the temperature to about 100°C and keep the temperature for 3 hours. After the completion of the reaction, let stand for 40min and separate. The obtained product DNCB was 190g, with a purity of 91.25%, an isomer of 8.75%, and a crystallization point of 44.1°C.

Embodiment A3

[0031] Add 100g of o-nitrochlorobenzene into a 1000ml Erlenmeyer flask, heat it to a temperature of about 55°C in the observed pot, start stirring, and start to add 180g of mixed acid dropwise. The whole dropping process was controlled at 47±2°C. Add dropwise for about 1h and keep warm for 15 minutes. After the heat preservation is completed, it takes 2.5 hours to raise the temperature to about 100°C and keep the temperature for 3 hours. After the completion of the reaction, let stand for 40min and separate. The obtained product DNCB was 195g, with a purity of 90.23%, an isomer of 9.77%, and a crystallization point of 44.9°C.

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Abstract

The invention discloses a preparation method of sulfur dye, comprising (1), preparation of sodium polysulfide; (2), hydrolysis; (3), vulcanization; (4), oxidation; (5), beating; (6) ,dry. The preparation process for producing sulfur black dyes from dinitrogen produced by o-nitrochlorobenzene and the sulfur black products produced have green light values ​​of ‑0.01~‑0.26 and yellow light values ​​of ‑0.03~‑0.25. Compared with similar yellow-green light sulfur black dyes, the blackness of the sulfur black dyes on cotton fabrics is greatly improved, and the yellow-green light sulfur black dyes produced by the invention have better decolorization effect after dyeing.

Description

technical field [0001] The invention relates to the field of fine chemical sulfur dyes, in particular to a preparation method of sulfur dyes. Background technique [0002] Sulfur black is a black phosphorus flake solid, mainly used for dyeing cotton textiles. Sulfur black is made by boiling 2,4-dinitrophenol and sodium polysulfide in aqueous solution. The production process is: (1), sodium sulfide and sulfur react to produce sodium polysulfide; (2), 2,4- Dinitrochlorinated benzene reacts with sodium hydroxide to produce 2,4-dinitrophenol sodium; (3), 2,4-dinitrophenol sodium reacts with sodium polysulfide to produce sulfur black dye through vulcanization and oxidation reactions; ( 4) Mixing pulp with sodium sulfide and drying to obtain the finished product. Among them, in the production process of 2,4-dinitrochlorobenzene, it is mainly obtained through the following steps: (1), the preparation of mixed acid; (2), the preparation of chlorobenzene; (3), the chlorobenzene Dr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B49/02D06P1/30D06P3/60
CPCC09B49/02D06P1/30D06P3/6025
Inventor 柳岩马晓刚刘志文郭冬冬吕艳军史焕周
Owner SHANXI LINFEN DYE CHEM GROUP CORP
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