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Preparation method for disperse violet 26

A technology for dispersing violet and diamino, applied in the direction of amino-hydroxyanthraquinone dyes, etc., can solve the problem of high production cost, achieve the effects of reducing the generation of by-products, high purity, and high yield

Active Publication Date: 2013-07-03
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 can only reach about 75%, and the production cost is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] According to the preparation method of Disperse Violet 26 of the present embodiment, comprise the following steps successively:

[0015] (1) Put 300kg of 1,4-diamino-2,3-dichloroanthraquinone, 300kg of potassium carbonate, 1200kg of phenol and 600kg of cyclohexanone in sequence in a 3000-liter condensation kettle, and then slowly raise the temperature. , the water 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 is kept for 4 hours, the end point is measured.

[0016] (2) Segregation: After the end point of condensation is reached, cool the material to 160°C, slowly add 100kg of 30wt% liquid caustic soda, when the temperature drops to 120°C, start to drop heating water, stir for 1 hour after adding, and then cool at 80°C Blowing, filtering, washing until neutral, and drying to obtain 488 kg of filter cake with a solid content of 75%, 366 kg in dry form...

Embodiment 2

[0018] According to the preparation method of Disperse Violet 26 of the present embodiment, comprise the following steps successively:

[0019] (1) Put 300kg of 1,4-diamino-2,3-dichloroanthraquinone, 300kg of potassium carbonate, 1200kg of phenol and 600kg of chlorobenzene in sequence 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 and is kept for 5 hours, the end point is measured and it has been reached.

[0020] (2) Segregation: After the end point of condensation is reached, cool the material to 160°C, slowly add 100kg of 30wt% liquid caustic soda, when the temperature drops to 120°C, start to drop heating water, stir for 1 hour after adding, and then cool at 80°C Blowing, suction filtering, washing to neutrality, drying to obtain 460kg of fil...

Embodiment 3

[0022] According to the preparation method of Disperse Violet 26 of the present embodiment, comprise the following steps successively:

[0023] (1) Put 300kg of 1,4-diamino-2,3-dichloroanthraquinone, 300kg of potassium carbonate, 1,200kg of phenol, 300kg of cyclohexanone and 300kg of chlorobenzene into a 2000-liter condensation tank in sequence, and then slowly raise the temperature. During the temperature rise process, the moisture 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 and is kept for 5 hours, the end point has been reached.

[0024] (2) Segregation: After the end point of condensation is reached, cool the material to 160°C, slowly add 100kg of 30wt% liquid caustic soda, when the temperature drops to 120°C, start to drop heating water, stir for 1 hour after adding, and then cool at 80°C Blowing, pumping, washing to neutrality, and drying to obtain 481 k...

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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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Patent Type & Authority Patents(China)
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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