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Method for synthesizing 3,3'-dichlorobenzidine hydrochloride through hydrochloric acid translocation

A technology of dichlorobenzidine hydrochloride and dichlorohydrin azobenzene is applied in the chemical field, and can solve the problems of slow reaction, viscous material, large mass transfer resistance, etc., and achieves easy operation, reduced viscosity, and improved reaction system. Effect

Active Publication Date: 2022-04-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of the shortcomings of the existing hydrochloric acid transposition synthesis process of 3,3'-dichlorobenzidine hydrochloride, by adding additives in the transposition reaction, the material viscosity and mass transfer resistance in the hydrochloric acid transposition reaction can be solved Large, slow reaction and other shortcomings, no need to use a special reactor, drop hydrochloric acid can be carried out at room temperature, no need to pre-cool the raw materials

Method used

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  • Method for synthesizing 3,3'-dichlorobenzidine hydrochloride through hydrochloric acid translocation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 200 g of 2,2'-dichlorohydroazobenzene and 180 g of toluene into the stirred reaction equipment, start stirring, and add 1.2 g of emulsifier TX-4 and 0.3 g of sodium dodecylsulfonate after completely dissolving , and then slowly add 380 g of 31% hydrochloric acid dropwise, and drop it in 2 h. After the dropwise addition, the temperature was raised to 40-50°C for the transposition reaction. After about 4 hours, the content of 2,2'-dichlorohydroazobenzene in the solution was detected to be less than 0.5%, and the transposition reaction was completed. The total operation time was 6 hours. The transposition solution was dissolved in water, and the lower aqueous phase was separated, decolorized and filtered to obtain the finished product of 3,3'-dichlorobenzidine hydrochloride with a yield of 89.5%.

[0021] Note: In Example 1, the mass ratio of 2,2'-dichlorohydroazobenzene to toluene is 1:0.9, and the additives added are sodium dodecylsulfonate and emulsifier TX-4, and t...

Embodiment 2

[0023] Add 200 g of 2,2'-dichlorohydroazobenzene and 200 g of toluene into the stirred reaction equipment, start stirring, and add 1 g of emulsifier TX-7 and 0.2 g of dodecylbenzenesulfonic acid after completely dissolving Sodium, then slowly add 400 g of 31% hydrochloric acid dropwise, and drop it over 1.5 h. After the dropwise addition, the temperature was raised to 40-50°C for the transposition reaction. After about 4 hours, the content of 2,2'-dichlorohydroazobenzene in the solution was detected to be less than 0.5%, and the transposition reaction was completed. The total operation time was 5.5 hours. The transposition solution was dissolved in water, the lower aqueous phase was separated, decolorized and filtered to obtain the finished product of 3,3'-dichlorobenzidine hydrochloride with a yield of 88.7%.

[0024] Note: In Example 2, the mass ratio of 2,2'-dichlorohydroazobenzene to toluene is 1:1, and the additives added are sodium dodecylbenzenesulfonate and emulsifier ...

Embodiment 3

[0026] Add 200 g of 2,2'-dichlorohydroazobenzene and 220 g of toluene into the stirred reaction equipment, start stirring, add 1.6 g of emulsifier TX-9 after completely dissolving, then slowly add 420 g of TX-9 with a concentration of 31 % hydrochloric acid, drop over 2.5 h. After the dropwise addition, the temperature was raised to 40-50°C for transposition reaction. After about 3.5 hours, the content of 2,2'-dichlorohydroazobenzene in the solution was detected to be less than 0.5%, and the transposition reaction was completed. The total operation time was 6 hours. The transposition solution was dissolved in water, the lower aqueous phase was separated, decolorized and filtered to obtain the finished product of 3,3'-dichlorobenzidine hydrochloride with a yield of 89.7%.

[0027] Note: In Example 3, the mass ratio of 2,2'-dichlorohydroazobenzene to toluene is 1:1.1, the additive added is emulsifier TX-9, and the auxiliary agent and 2,2'-dichlorohydroazo The mass ratio of benz...

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Abstract

A method for synthesizing 3,3'-dichlorobenzidine hydrochloride through hydrochloric acid transposition, comprising the following steps: (1) dissolving: adding 2,2'-dichlorohydroazobenzene into toluene to completely dissolve; ( 2) Transposition reaction: Add additives to the above solution, and slowly add 31% hydrochloric acid with the same mass as the solution at room temperature. After the dropwise addition, the temperature was raised to carry out the transposition reaction. After a period of reaction, detect the content of 2,2'-dichlorohydroazobenzene in the solution, and stop the transposition reaction when the detection result is less than 0.5%; (3) Post-treatment: dissolve the transposition solution in water, After separating the lower aqueous phase, decolorize and filter to obtain the finished product of 3,3'-dichlorobenzidine hydrochloride. The invention is easy to operate and easier to implement, so it has better application prospects.

Description

technical field [0001] The invention relates to a method for synthesizing 3,3'-dichlorobenzidine hydrochloride through transposition of hydrochloric acid, which belongs to the technical field of chemical industry. Background technique [0002] 3,3'-Dichlorobenzidine, referred to as DCB, is an important intermediate in the production of dichlorobenzidine-based organic pigments. The output of a series of organic pigments based on it accounts for about 25% of the total organic pigments. It is widely used in Production of ink, paint, rubber, plastic and other coloring and pigment printing slurry pigment dyeing slurry. Its commodity generally exists in the form of hydrochloride, and its structural formula is: [0003] [0004] At present, there are two kinds of transposition processes of 3,3'-dichlorobenzidine hydrochloride: sulfuric acid transposition and hydrochloric acid transposition. Among them, the advantages of sulfuric acid translocation are fast reaction, static str...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/54C07C209/86C07C211/52
CPCC07C209/54C07C209/86C07C211/52
Inventor 史乐萌付春黄伟韦志强郁铭高留冕
Owner CHINA PETROLEUM & CHEM CORP
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