Method for preparing 3,3'-dichlorobenzidine hydrochloride by hydrochloric acid translocation

A technology of dichlorobenzidine hydrochloride and dichlorohydrin azobenzene is applied in 3 fields, and can solve the problems of inaccurate process parameters, insufficient utilization of raw materials, and low yield of finished products.

Inactive Publication Date: 2010-02-10
夏恩将
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, sometimes in the transposition reaction, there are problems of unreasonable process steps and inaccurate process parameters, resulting in low yield of finished products, high cost, and raw materials cannot be fully utilized

Method used

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Examples

Experimental program
Comparison scheme
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Embodiment Construction

[0010] Below in conjunction with embodiment the present invention is described in detail:

[0011] Add 200 g of o-nitrochlorobenzene, 90 ml of xylene, 166 ml of 30% sodium hydroxide solution, and 5 g of pt / c 5% wet product in a stainless steel autoclave. Seal it well, first replace it with nitrogen three times, and then replace it with hydrogen three times. The pressure is controlled at 1.5Mpa, the temperature is controlled at 50-90°C, react for 10 hours to generate hydroazobenzene, filter, separate the catalyst and repeat the application, the filtrate is separated, and the oil phase is 2,2'-dichlorohydroazobenzene According to liquid chromatography analysis, the molar ratio of 2,2'-dichlorohydroazobenzene is 95%.

[0012] Mix 820g of 31% hydrochloric acid and 170ml of water to form a 25% starting acid, then add 2,2'-dichlorohydroazobenzene and keep it warm at 0-40°C for 6 hours to obtain 3,3'-dichlorobenzidine salt Crude salt (purity 95%). Filtrate, the filtrate is layered...

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PUM

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Abstract

The invention discloses a method for preparing 3,3'-dichlorobenzidine hydrochloride by hydrochloric acid translocation. The method comprises the following steps: catalytically hydrogenating ortho-nitrochlorobenzene by hydrogen in the presence of catalysts, such as organic solvents, rare metal and the like to prepare 2,2'-dichlorohydrazobenzene; performing a translocation and rearrangement reactionin hydrochloric acid to finally prepare the 3,3'-dichlorobenzidine hydrochloride with yield reaching over 90 percent. The method has reasonable process route; and the finished product prepared by adopting the method has higher yield and purity, and has larger industrial prospect.

Description

technical field [0001] The present invention relates to a kind of preparation method of 3,3'-dichlorobenzidine hydrochloride. Background technique [0002] 3,3'-dichlorobenzidine hydrochloride is an important pigment and dye intermediate, it is slightly soluble in water, soluble in alcohol, easy to oxidize, currently preparing 3,3'-dichlorobenzidine hydrochloride Most of the salts are formed by transposition reaction of 2,2'-dichlorohydroazobenzene through sulfuric acid or hydrochloric acid. But sometimes in the transposition reaction, there are problems of unreasonable process steps and inaccurate process parameters, resulting in low yield of finished products, high cost, and raw materials cannot be fully utilized. Contents of the invention [0003] In order to solve the above problems, the invention provides a method utilizing hydrochloric acid transposition to prepare 3,3'-dichlorobenzidine hydrochloride, and the technical scheme it takes is: [0004] 3,3'-dichloroben...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/42
Inventor 夏恩将夏恩胜岳岩夏念丰
Owner 夏恩将
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