Preparation method for disperse violet 26

A technology of disperse violet and diamino, applied in amino-hydroxyanthraquinone dyes and other directions, can solve the problem of high production cost, and achieve the effects of reducing the generation of by-products, shortening the reaction time, and reducing production costs

Active Publication Date: 2012-08-01
苏州市罗森助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With this process, the highest yield of Disperse Violet 26 c...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of Disperse Violet 26 according to this embodiment includes the following steps in sequence:

[0015] (1) Put 300kg of 1,4-diamino-2,3-dichloroanthraquinone, 300kg of potassium carbonate, 1200kg of phenol and 600kg of cyclohexanone into a 3000-liter condensation kettle in turn, and then slowly raise the temperature, during the heating process , The moisture in the raw materials and the water produced by the reaction are quickly taken out of the reaction system by cyclohexanone. When the temperature rises to 190°C and keeps it for 4 hours, the end of the measurement is reached.

[0016] (2) Segregation: After the end of the condensation is reached, cool the material to 160°C, slowly add 100kg 30wt% of liquid caustic soda, when the temperature is reduced to 120°C, start to drip heating water, stir for 1 hour after the addition, and then at 80°C Discharge, filter, wash to neutrality, and drain to obtain 488 kg of cake with a solid content of 75%, 366 k...

Embodiment 2

[0018] The preparation method of Disperse Violet 26 according to this embodiment includes the following steps in sequence:

[0019] (1) Put 300kg of 1,4-diamino-2,3-dichloroanthraquinone, 300kg of potassium carbonate, 1200kg of phenol and 600kg of chlorobenzene in a 3000-liter condensation kettle, and then slowly raise the temperature. During the heating process, The moisture in the raw materials and the water produced by the reaction are quickly taken out of the reaction system by chlorobenzene. When the temperature rises to 190°C, the end point is reached after keeping it for 5 hours.

[0020] (2) Segregation: After the end of the condensation is reached, cool the material to 160°C, slowly add 100kg 30wt% of liquid caustic soda, when the temperature is reduced to 120°C, start to drip heating water, stir for 1 hour after the addition, and then at 80°C Discharge, filter, wash to neutrality, and drain to obtain 460 kg of cake with 75% solid content, 345 kg of dried cake, disperse...

Embodiment 3

[0022] The preparation method of Disperse Violet 26 according to this embodiment includes the following steps in sequence:

[0023] (1) Put 300kg of 1,4-diamino-2,3-dichloroanthraquinone, 300kg of potassium carbonate, 1200kg of phenol, 300kg of cyclohexanone and 300kg of chlorobenzene into a 2000 liter condensation kettle, and then slowly raise the temperature. During the heating process, the water in the raw materials and the water produced by the reaction are quickly taken out of the reaction system by the solvent. When the temperature rises to 190°C, the end point is reached after keeping it for 5 hours.

[0024] (2) Segregation: After the end of the condensation is reached, cool the material to 160°C, slowly add 100kg 30wt% of liquid caustic soda, when the temperature is reduced to 120°C, start to drip heating water, stir for 1 hour after the addition, and then at 80°C Discharging, filtering, washing until neutral, and draining to obtain 481kg of cake with 75% solid content,...

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PUM

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Abstract

The invention relates to a preparation method for disperse violet 26. In the method, 1,4-diamino-2,3-dichloroanthraquinone and phenol undergo a condensation reaction in the presence of an acid-binding agent, so that 1,4-diamino-2,3-diphenyl oxide anthraquinone is generated; particularly, the condensation reaction is undergone in a water-insoluble inertial organic solvent of which the boiling point is 120-175 DEG C; the feeding weight ratio of the inertial organic solvent to phenol to 1,4-diamino-2,3-diphenyl oxide anthraquinone to the acid-binding agent is (1.5-2.5):(3-5):(0.9-1.1):1; and in the process of the condensation reaction, and water in a system is brought out by using the inertial organic solvent. In the preparation method, water (mainly water generated through a condensation reaction) in the system is brought out quickly by using a solvent, forward proceeding of the reaction is facilitated, the reaction time is greatly shortened, and the generation of a byproduct is reduced, so that the product has high yield and high purity, and the production cost is lowered.

Description

technical field [0001] The invention relates to a preparation method of disperse violet 26. Background technique [0002] The scientific name of Disperse Violet 26 is 1,4-diamino-2,3-diphenoxyanthraquinone, which is a reddish-brown powder, soluble in ethanol, colorless in concentrated sulfuric acid, yellowish red after dilution, and the maximum absorption wavelength is 545nm. Disperse Violet can be used for dyeing of various fabrics, plastics and polyesters. [0003] The existing production method of Disperse Violet 26 is to use 1,4-bis-amino 2,3-dichloroanthracene as a raw material, in the presence of an acid-binding agent potassium carbonate, to condense with phenol to remove two molecules of hydrogen chloride, wherein the condensation The reaction temperature is about 190°C, and the reaction time is about 7 hours. After the reaction reaches the end point, liquid caustic soda is added at 140°C. Water was added dropwise at 120°C for isolation, then filtered and washed to...

Claims

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Application Information

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IPC IPC(8): C09B1/54
Inventor 李根荣徐新连
Owner 苏州市罗森助剂有限公司
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