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Preparation method of 3,3',4,4'-tetraaminobiphenyl

A technology of tetraaminobiphenyl and amino, which is applied in the field of compound synthesis, can solve problems such as low yield, long route, and large amount of three wastes, and achieve the effects of short steps, reduced energy consumption, and reduced production volume

Pending Publication Date: 2021-06-08
INSIGHT FINECHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these synthetic routes have disadvantages such as long route, low yield, and large amount of three wastes.

Method used

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  • Preparation method of 3,3',4,4'-tetraaminobiphenyl

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preparation example Construction

[0036] A preparation method of 3,3',4,4'-tetraaminobiphenyl provided in the embodiment of the present invention comprises the following steps:

[0037] Step S1: In the presence of the first catalyst and the second catalyst, the dichlorobiphenyl diamine is subjected to an amino substitution reaction with an ammoniating reagent to obtain a crude product of 3,3',4,4'-tetraaminobiphenyl, wherein , the first catalyst is a mixture of specified amino acid and cuprous salt, and the second catalyst is a phase transfer catalyst.

[0038] In step S1, dichlorobiphenyldiamine (also known as 3,3'-dichlorobiphenyl-4,4'-diamine) undergoes an amino substitution reaction with an ammoniating reagent, and the reaction equation is shown in the following formula:

[0039]

[0040] NH in the above formula 3 Provided by ammoniating reagents.

[0041] Step S2: post-processing the crude 3,3',4,4'-tetraaminobiphenyl product to obtain a purified 3,3',4,4'-tetraaminobiphenyl product.

[0042] The pr...

Embodiment 1

[0062] Adding 173.0g (equivalent to 0.53mol) of dichlorobenzidine diamine and 500g of concentration successively in the beating still with ice water cooling is the ammoniacal liquor of 25%, and after beating, it is transferred into 0.4g cuprous chloride, 5.2 In the autoclave of 5.0g proline and 5.2g tetrabutyl ammonium chloride, replace the air in the autoclave with nitrogen four times, then use 248g concentration to wash the beating autoclave after being 25% ammoniacal liquor and change over to the autoclave together. The temperature of the system is controlled to not exceed 10° C. during the whole process of beating, transferring, replacing and washing.

[0063] Turn on the stirring of the autoclave and continue to feed 170g of ammonia into the autoclave. The autoclave was closed and the temperature was raised. After about 1.5 hours, the temperature of the reaction system in the autoclave was raised to 170° C., and the pressure was 2.7 MPa, and the reaction was kept at this...

Embodiment 2

[0067] Add 173.0g (equivalent to 0.53mol) dichlorobenzidine diamine and 500g concentration of ammonia water of 25% successively in the beating still that cools down with ice water, change into 0.2g cuprous chloride, 6.9g cuprous chloride in advance after beating In the autoclave of histidine and 6.9g tetrabutylammonium chloride, the air in the autoclave was replaced with nitrogen four times, and then the beating autoclave was washed with 248g concentration of 25% ammonia water and transferred to the autoclave. The temperature of the system is controlled to not exceed 10° C. during the whole process of beating, transferring, replacing and washing.

[0068] Turn on the stirring of the autoclave and continue to feed 170g of ammonia into the autoclave. The autoclave was closed and the temperature was raised. After about 1.5 hours, the temperature of the reaction system in the autoclave was raised to 170° C., and the pressure was 2.7 MPa, and the reaction was kept at this temperat...

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Abstract

The invention discloses a preparation method of 3,3',4,4'-tetraaminobiphenyl The method comprises the following steps: in the presence of a first catalyst and a second catalyst, carrying out an amino substitution reaction on dichlorobiphenyl diamine and an ammoniation reagent to obtain a crude 3,3',4,4'-tetraaminobiphenyl product; and carrying out post-treatment on the crude 3,3',4,4'-tetraaminobiphenyl product to obtain a purified 3,3',4,4'-tetraaminobiphenyl product, wherein the first catalyst is a mixture of specified amino acid and cuprous salt, and the second catalyst is a phase transfer catalyst. Specific amino acid and the phase transfer catalyst are innovatively introduced to assist a small amount of cuprous salt in forming a new combined catalyst, so the smooth proceeding of the amino substitution reaction can be efficiently promoted, and reaction yield and product purity are improved. The usage of cuprous salt in the catalyst is obviously reduced, so the post-treatment pressure of high-concentration heavy metal salt wastewater is effectively reduced. Reaction temperature and reaction pressure are milder, so energy consumption is reduced, the safety of a process flow is improved, and the method is more suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a preparation method of 3,3',4,4'-tetraaminobiphenyl. Background technique [0002] 3,3',4,4'-tetraaminobenzidine (3,3-Diamonobenzidine, DAB) is a high-grade polymer material monomer, which is mainly used to synthesize heat-resistant polymer resin and synthetic fiber. Polymer products synthesized with DAB as a monomer have properties such as ultra-high heat resistance, flame retardancy, dimensional thermal stability, chemical resistance at high temperature and comfortable wearing. Therefore, the research and development of DAB products, especially the DAB The research and development of synthetic methods is receiving widespread attention from related industries at home and abroad. [0003] The preparation method of DAB in the prior art mainly comprises following several synthetic routes: [0004] (1) Starting from o-nitroaniline, the raw material of singl...

Claims

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Application Information

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IPC IPC(8): C07C209/10C07C211/50
CPCC07C209/10C07C211/50
Inventor 凌云黄碧波王坤陈立柱殷巍
Owner INSIGHT FINECHEM
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