Preparation technology of black sulfide dye and its product

A technology for sulfur black and dyes, which is applied in the direction of azo dyes, organic dyes, nitro/nitroso dyes, etc. It can solve the problems of uneven water content of dyes, reduce dye yield, pollute the environment, etc., and achieve good fluidity , Superior application performance and large specific surface area

Active Publication Date: 2006-06-14
浙江长征化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] According to the prior art, the present invention uses a drum dryer to make the water content of the dried dye uneven, which easily causes color difference in dyeing, and some materials will be taken away from the top of the drum with the evaporated water, which reduce...

Method used

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  • Preparation technology of black sulfide dye and its product
  • Preparation technology of black sulfide dye and its product
  • Preparation technology of black sulfide dye and its product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] a. Preparation of sodium polysulfide: add 150 parts of water to a 500ml three-neck flask, heat up to 80°C, add 150 parts of 60% sodium sulfide, stir until all of it dissolves, add 105 parts of sulfur, after adding, keep warm at 98°C for reaction 2 hours to spare.

[0038] b. Hydrolysis: Add 100 parts of water and 150 parts of 2,4-nitrochlorobenzene into a 500ml three-neck flask, add dropwise 210 parts of 30% caustic soda solution at 70°C, keep the reaction at 100°C for 1 hour, and set aside.

[0039] c. Vulcanization: Add the prepared hydrolyzed material and sodium polysulfide solution in a 1000ml autoclave, react at 100°C for 1 hour, then seal the pot cover, heat up to 140°C, react at 120°C for 7 hours, and control the reaction pressure at 0.1Mpa, after the reaction is completed, exhaust, and the discharged hydrogen sulfide gas is recovered into sodium sulfide with 30% caustic soda.

[0040] d. Oxidation and filtration: Put the vulcanized material into a 2000ml beaker...

Embodiment 2

[0044] a. Preparation of sodium polysulfide: add 150 parts of water to a 500ml three-neck flask, heat up to 85°C, add 150 parts of 60% sodium sulfide, stir until all of it dissolves, add 105 parts of sulfur, after adding, keep warm at 99°C for reaction 2 hours to spare.

[0045] b. Hydrolysis: Add 100 parts of water and 150 parts of 2,4-nitrochlorobenzene into a 500ml three-neck flask, add dropwise 210 parts of 30% caustic soda solution at 80°C, keep the reaction at 102°C for 1 hour, and set aside.

[0046] c. Vulcanization: Add the prepared hydrolyzed material and sodium polysulfide solution in a 1000ml autoclave, react at 100°C for 1 hour, then seal the pot cover, heat up to 140°C, react at 130°C for 7 hours, and control the reaction pressure at 0.12Mp, after the reaction is completed, exhaust, and the discharged hydrogen sulfide gas is recovered into sodium sulfide with 30% caustic soda.

[0047] d. Oxidation and filtration: Put the vulcanized material into a 2000ml beaker...

Embodiment 3

[0051] a. Preparation of sodium polysulfide: add 150 parts of water to a 500ml three-necked flask, raise the temperature to 90°C, add 150 parts of 60% sodium sulfide, stir until completely dissolved, add 105 parts of sulfur, after adding, keep warm at 100°C for reaction 2 hours to spare.

[0052] b. Hydrolysis: Add 100 parts of water and 150 parts of 2,4-nitrochlorobenzene into a 500ml three-neck flask, add dropwise 210 parts of 30% caustic soda solution at 90°C, keep the reaction at 105°C for 1 hour, and set aside.

[0053] c. Vulcanization: Add the prepared hydrolyzed material and sodium polysulfide solution in a 1000ml autoclave, react at 100°C for 1 hour, then seal the pot cover, heat up to 140°C, react at 140°C for 7 hours, and control the reaction pressure at 0.13Mp, after the reaction is completed, exhaust, and the discharged hydrogen sulfide gas is recovered into sodium sulfide with 30% caustic soda.

[0054] d. Oxidation and filtration: Put the vulcanized material in...

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Abstract

The present invention relates to a preparation process of sulfide dyes and its product. It particular, it relates to a preparation process of sulfur black dyes by adopting spray-drying process and its prepared sulfur black product. Said sulfur black product is characterized by that its grain diameter is 150-200 micrometers, specific surface area is 300-360 sq.cm/g, it has the good wettability, flowability and dissolvability.

Description

technical field [0001] The invention relates to a preparation process of sulfur dye and its products, in particular to a preparation process of spray-dried sulfur black dye and the prepared sulfur black product. Background technique [0002] Sulfur black dye is a dye that interacts with certain organic aromatic compounds and sulfur or sodium polysulfide. Due to its relatively simple raw materials and production process, low cost, and good washing and light fastness, the demand for sulfur dyes The amount is very large, among which black and blue dyes are used in the largest amount in the dyeing of cotton products, and they are the varieties with the largest output in the dye industry. Sulfur black is made of 2,4-dinitrophenol and sodium polysulfide in aqueous solution. It is boiled, and its production process is as follows: [0003] (1) Sodium sulfide and sulfur react to form sodium polysulfide. [0004] (2) 2,4-dinitrochlorobenzene is hydrolyzed by sodium hydroxide to gene...

Claims

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Application Information

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IPC IPC(8): C09B51/00
Inventor 阮加根赵国生阮国涛
Owner 浙江长征化工有限公司
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