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Preparation method of disperse blue

A technology of dispersing blue and dispersing agent, which is applied in chemical instruments and methods, azo dyes, organic dyes, etc. It can solve the problems of low concentration of coupling components, less chance of collision, decomposition of diazonium salt, etc., and achieve improved operational safety , Prevent the decomposition of diazonium salts and reduce the concentration of sulfuric acid

Inactive Publication Date: 2018-12-04
JIANGSU ZHIJIANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the domestically prepared disperse blue 183:1 has a lot of diazonium salt decomposition, many dye impurities, and the shade is not bright enough, and the color of the spelled B56 is dark.
Disperse blue 183:1 shade is not bright enough for the following two reasons: one is the use of diazo in 98% concentrated sulfuric acid medium for synthesis, and the diazo in concentrated sulfuric acid medium will encounter a problem in the coupling, that is, concentrated acid diazo When the salt is added to the ice water containing the coupling components, the concentrated acid will violently exothermic when it meets the water, which will cause the decomposition of the surrounding diazonium salt that will not react in time, resulting in a yellow decomposition product of the finished dye. The second is to add diazonium during coupling The bottom water is 20 times the weight of the component, the concentration of the coupling component is low, and the chance of collision with the diazonium salt is less, resulting in more decomposition of the diazonium salt

Method used

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  • Preparation method of disperse blue
  • Preparation method of disperse blue
  • Preparation method of disperse blue

Examples

Experimental program
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Effect test

Embodiment 1

[0018] A preparation method of disperse blue, comprising the following steps:

[0019] S1: Add 600kg of 75% sulfuric acid and 1224kg of 40% nitrosylsulfuric acid to the reaction kettle, open the jacket cold brine to control the temperature at -5~0℃, slowly add 2-cyano-4-nitro-6- Bromoaniline 915kg, after adding and keeping warm for 5 hours, the diazonium salt was obtained for use, and the reaction formula was:

[0020]

[0021] S2: In the coupling kettle, add 5 kg of sulfamic acid, 5 kg of auxiliary agent OP-10 (nonylphenol polyoxyethylene ether), 1197 kg of 65% coupling components (3-N, N-diethylaminoacetanilide), With 7000kg of crushed ice, start to add the diazonium salt obtained in S1 dropwise under stirring. The dropwise addition time is 2 hours. After the drop is completed, add ice to keep the temperature at -1°C, and fully react for 2 hours. The reaction formula is:

[0022]

[0023] S3: After fully reacting, use steam to raise the temperature to 80°C and keep it...

Embodiment 2

[0025] A preparation method of disperse blue, comprising the following steps:

[0026] S1: Add 562.5kg of 80% sulfuric acid and 1224kg of 40% nitrosylsulfuric acid to the reaction kettle, open the jacket cold brine to control the temperature at -5~0℃, slowly add 2-cyano-4-nitro-6 -Bromoaniline 915kg, after adding the insulation reaction for 5h, get the diazonium salt for use;

[0027] S2: In the coupling kettle, add sulfamic acid 5kg, auxiliary agent SL808 (fatty acid oxyethylene ether) 5kg, 65% coupling component (3-N, N-diethylaminoacetanilide) 1197kg, crushed ice 7000kg, stir Start to add the diazonium salt obtained in S1 dropwise for 2 hours. After dropping, add ice to keep the temperature at -3°C. After fully reacting for 2 hours, use steam to raise the temperature to 80°C. After keeping it for 1 hour, pump the material into the pressure The filter was washed with hot water at 50°C to obtain a filter cake of 1653kg, HPLC 95%.

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Abstract

The invention provides a preparation method of disperse blue, and belongs to the technical field of dye preparation. According to the preparation method, 2-cyano-4-nitro-6-bromo aniline, a sulfuric acid solution, and nitrosyl sulfuric acid are mixed to carry out diazotization to obtain diazo salt, the mass percentage of the sulfuric acid solution is 72 to 85%; ice is added into the diazo salt to control the temperature, then sulfamic acid, a coupling component and a dispersant are added to carry out coupling reactions, and the temperature of coupling reactions is controlled in a range of -10 to 15 DEG C. The provided preparation method has the advantages of simple technology, easy operation, stable yield, and high safety, and the prepared disperse blue dye has a bright color.

Description

technical field [0001] The invention belongs to the technical field of dye preparation, and in particular relates to a preparation method of disperse blue. Background technique [0002] Disperse Blue 183:1 is a kind of dye with a relatively large amount, which can be used for single color or color matching, and is the main component of color matching B56. At present, the domestically prepared disperse blue 183:1 has a lot of decomposition of diazonium salts, a lot of dye impurities, and the shade is not bright enough, and the color of B56 spelled out is dark. Disperse blue 183:1 shade is not bright enough for the following two reasons: one is the use of diazo in 98% concentrated sulfuric acid medium for synthesis, and the diazo in concentrated sulfuric acid medium will encounter a problem in the coupling, that is, concentrated acid diazo When the salt is added to the ice water containing the coupling components, the concentrated acid will violently exothermic when it meets ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/01C09B29/08
CPCC09B29/0007C09B29/0838
Inventor 陈勤伟
Owner JIANGSU ZHIJIANG CHEM