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Tech. of separating purifying 3,3-dichlorobenzidine hydrochloride

A dichlorobenzidine hydrochloride and process technology, which is applied in the direction of amino compound purification/separation, organic chemistry, etc., can solve the problem of high loss of 3,3'-dichlorobenzidine hydrochloride, difficulty in crystallization and cooling, and product cost. Advanced problems, to achieve the effect of reducing the amount of wastewater treatment, low cost, and improving production capacity

Inactive Publication Date: 2007-12-12
CHANGZHOU JIASEN CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This separation and refining process has defects such as high product cost, serious pollution, difficult crystallization and cooling, large amount of waste water, and more losses of 3,3'-dichlorobenzidine hydrochloride.

Method used

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  • Tech. of separating purifying 3,3-dichlorobenzidine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A process for separating and refining 3,3'-dichlorobenzidine hydrochloride, the process steps are as follows:

[0026] (1). Washing and dissolving and oil-water separation, add 3,3'-dichlorobenzidine hydrochloride, hydrochloric acid, water and toluene mixture into the washing and dissolving tank, feed a certain amount of hot water at 90°C and stir thoroughly, Partially dissolve 3,3'-dichlorobenzidine hydrochloride, at a temperature of 80°C to 95°C, then stand and separate, the separated water layer is pumped into the decolorization kettle, and continue to pour into the remaining oil layer under stirring conditions Add hot water at 90°C to the oil, then let it stand for separation, pump the separated water layer into the decolorization kettle, and recover the toluene from the remaining oil layer by heating up distillation.

[0027] (2). Evaporate to remove acid and remove impurities and decolorize. In the decolorization kettle, heat up and stir. Under reduced pressure, t...

Embodiment 2

[0031] A process for separating and refining 3,3'-dichlorobenzidine hydrochloride, the process steps are as follows:

[0032] (1). Washing and dissolving and oil-water separation, add 3,3'-dichlorobenzidine hydrochloride, hydrochloric acid, water and toluene mixture materials into the washing and dissolving kettle, pass a certain amount of 90°C dilute The hydrochloric acid intermediate tank is prepared with dilute hydrochloric acid solution, and fully stirred to dissolve part of the 3,3'-dichlorobenzidine hydrochloride, at a temperature of 80°C to 95°C, then stand and separate, and the separated water layer is pumped Put it into the decolorization kettle, continue to add 90°C dilute hydrochloric acid solution to the remaining oil layer, then let it stand for separation, pump the separated water layer into the decolorization kettle, and recover the toluene from the remaining oil layer by heating up distillation.

[0033] (2). Evaporate to remove acid and remove impurities and d...

Embodiment 3

[0037] A process for separating and refining 3,3'-dichlorobenzidine hydrochloride, the process steps are as follows:

[0038] (1). Washing and dissolving and oil-water separation, add 3,3'-dichlorobenzidine hydrochloride, hydrochloric acid, water and toluene mixture materials into the washing and dissolving kettle, and pass a certain amount of 90°C diluted in Example 2 The hydrochloric acid intermediate tank is prepared with dilute hydrochloric acid solution, and fully stirred to dissolve part of the 3,3'-dichlorobenzidine hydrochloride, at a temperature of 80°C to 95°C, then stand and separate, and the separated water layer is pumped Put it into the decolorization kettle, continue to add 90°C dilute hydrochloric acid solution to the remaining oil layer, then let it stand for separation, pump the separated water layer into the decolorization kettle, and recover the toluene from the remaining oil layer by heating up distillation.

[0039](2). Evaporate to remove acid and remove...

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Abstract

A process for separating and refining 3,3'-dichlorobiphenyl amine hydrochloride includes such steps as mixing 3,3'-dichlorobiphenyl amine hydrochloride with hydrochloric acid, water and arylhydrocarbon for washing and dissolving, oil-water separation, evaporating for removing hydrochloric acid, decoloring, removing impurities, filtering, cooling while crystallizing to educe out 3,3'-dichlorobiphenylamine hydrochloride, filtering, and treating filtered cake.

Description

technical field [0001] The present invention relates to a crystallization separation and refining process, in particular to a process for separating and refining 3,3'-dichlorobenzidine hydrochloride, hydrochloric acid, water and aromatic hydrocarbon mixture materials , belonging to the field of fine chemical technology. Background technique [0002] 3,3'-dichlorobenzidine (DCB) hydrochloride (C 12 h 10 Cl 2 N 2 2HCl), slightly soluble in water, soluble in alcohol, easy to oxidize, relatively stable in dilute hydrochloric acid solution, is an important pigment and dye intermediate, and benzidine yellow and urkangjian produced by this intermediate Fast red and azo dyes are better in acid resistance than those produced with benzidine, fast and green in color. The series of organic pigments made with it as the main body account for about 27% of the total organic pigments. In addition, it can also prepare direct dyes with excellent performance. At present, 3,3'-dichlorobenz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/56C07C209/82
Inventor 许文林段玉辉刘学谦
Owner CHANGZHOU JIASEN CHEM
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