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A kind of preparation method of acid black 172

A technology of acid black and sulfonic acid, applied in chemical instruments and methods, complex metal compounds of azo dyes, organic dyes, etc., can solve the problems of side reactions and impurities, large waste liquid discharge, serious environmental pollution, etc. Achieve the effect of reducing energy consumption, reducing waste water, and reducing side reactions

Active Publication Date: 2019-09-20
JIANGSU SHENGJI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned production method can obtain Acid Black 172, there are still the following problems: after the reaction of the product is complete, steps such as salting out are required; the product yield is low, and there are many side reactions and impurities; the production cost is high and the production efficiency is low , a large amount of waste liquid discharge, serious environmental pollution, and high treatment costs; among them, a large amount of salty dye wastewater is produced in the salting out step, and the separated dye filter cake needs to be dried, crushed and other processes

Method used

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  • A kind of preparation method of acid black 172
  • A kind of preparation method of acid black 172
  • A kind of preparation method of acid black 172

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1), diazotization:

[0040] Add 4800kg of water, 480kg of soda ash, 480kg of ammonium bicarbonate, 24kg of dispersant NNO, 48kg of zinc chloride into the coupling pot, stir for 10 minutes, keep the temperature at 12-17°C, and quickly add 4800kg of 6-nitro-1-diazo-2 -Naphthol-4-sulfonic acid, keep the temperature at 15-22°C, and control the pH=2.0±0.2. React for 30 minutes, then keep warm at 18-25°C for 30-60 minutes, add 4000-5000kg of water to dilute, and stir for 10-30 minutes. Obtain diazo solution.

[0041] (2), coupling:

[0042] Add 2400kg of 2-naphthol dry powder into the diazo solution in the coupling pot, and after stirring evenly, start to add 30% liquid caustic soda dropwise, the temperature will rise naturally, the temperature will be controlled at less than 50°C, and the pH value will be controlled at 9-11. The time for dripping liquid caustic soda is 30-60 minutes. After the dropwise addition of liquid caustic soda is completed, keep the temperature f...

Embodiment 2

[0048] (1), diazotization:

[0049] Add 4800kg of water, 960kg of soda ash, 960kg of ammonium bicarbonate, 24kg of dispersant NNO, 48kg of zinc chloride into the coupling pot, stir for 10 minutes, keep the temperature at 12-17°C, and quickly add 4800kg of 6-nitro-1-diazo-2 -Naphthol-4-sulfonic acid, keep the temperature at 15-22°C, and control the pH=2.0±0.2. React for 30 minutes, then keep warm at 18-25°C for 30-60 minutes, add 4000-5000kg of water to dilute, and stir for 10-30 minutes. Obtain diazo solution.

[0050] (2), coupling:

[0051] Add 2448kg of 2-naphthol dry powder into the diazo liquid in the coupling pot, and after stirring evenly, start to add 30% liquid caustic soda dropwise, the temperature will rise naturally, the temperature will be controlled at less than 50°C, and the pH value will be controlled at 9-11. The time for dripping liquid caustic soda is 30-60 minutes. After the dropwise addition of liquid caustic soda is completed, keep the temperature for...

Embodiment 3

[0057] (1), diazotization:

[0058] Add 4800kg of water, 480kg of soda ash, 700kg of ammonium bicarbonate, 24kg of dispersant NNO, 48kg of zinc chloride into the coupling pot, stir for 10 minutes, keep the temperature at 12-17°C, and quickly add 4800kg of 6-nitro-1-diazo-2 -Naphthol-4-sulfonic acid, keep the temperature at 15-22°C, and control the pH=2.0±0.2. React for 30 minutes, then keep warm at 18-25°C for 30-60 minutes, add 4000-5000kg of water to dilute, and stir for 10-30 minutes. Obtain diazo solution.

[0059] (2), coupling:

[0060] Add 2420kg of 2-naphthol dry powder into the diazo solution in the coupling pot. After stirring well, start to add 30% liquid caustic soda dropwise, and the temperature will rise naturally. The time for adding liquid caustic soda is 30-60 minutes. After the dropwise addition of liquid caustic soda is completed, keep the temperature for 30 to 60 minutes and control the temperature at less than 50°C. Obtain the coupling solution.

[0...

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Abstract

The invention relates to a preparation method of acid black 172. The method comprises the following steps: (1) diazotizing 6-nitro-1-diazo-2-naphthol-4-sulfonic acid by using zinc chloride as a catalyst to obtain a diazo solution; (2) directly adding 2-naphthol into the diazo solution, regulating the pH value with sodium hydroxide, and carrying out coupling to obtain a coupling solution; (3) carrying out chromization on chromic sulfate and acetic acid to obtain a chromizing solution; and (4) adding the chromizing solution into the coupling solution, carrying out complexation, adding salicylic acid to remove chromium to obtain an acid black 172 slurry, and directly carrying out spray drying to obtain the acid black 172 dry powder. The method has the advantages of simple production technique, high production efficiency and fewer side reactions and impurities. The product has the advantages of high quality and no heavy metal chromium, and can be directly subjected to spray drying without salting-out, so the production cost is low.

Description

technical field [0001] The invention belongs to the field of metal complex azo dyes, in particular to a production method of acid black 172. Background technique [0002] Acid Black 172 is an acid dye named according to the International Dyestuff Code. Its trade name is Neutral Black S-RL. It is used in the printing and dyeing of wool, silk, leather, nylon and nylon-cotton blended fabrics. It has high dyeing fastness to wool and polyamide fibers, and the dyeing operation is simple and the application fields are very wide. [0003] The main reaction to produce Acid Black 172 is as follows: [0004] Mainly put 6-nitro-1,2-diazooxynaphthalene-4-sulfonic acid into the dissolving tank, dissolve it with 30% liquid alkali, put the dissolved liquid into the coupling reaction tank, and stir Under certain conditions, pour the 2-naphthol solution dissolved with liquid caustic soda into the coupling reaction tank for reaction. After the coupling reaction is completed, adjust the react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B45/34C09B45/01
Inventor 方标蒋志平代龙龙刘辉
Owner JIANGSU SHENGJI CHEM