Method for continuously synthesizing 4-aminodiphenylamine

A technology of aminodiphenylamine and nitrodiphenylamine, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., can solve the problems of low conversion rate of raw materials and low yield of products, and achieve inhibition of initial activity, Effect of low acid content and improved stability

Active Publication Date: 2013-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention relates to a method for continuous synthesis of 4-aminodiphenylamine, which mainly solves the problems of low raw material conversion rate and low product yield in the existing 4-nitrodiphenylamine intermittent hydrogenation process

Method used

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  • Method for continuously synthesizing 4-aminodiphenylamine
  • Method for continuously synthesizing 4-aminodiphenylamine
  • Method for continuously synthesizing 4-aminodiphenylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Weigh Ni / Al 2 o 3 30 milliliters of the catalyst were reduced for 16 hours at a temperature of 450° C. and a hydrogen flow rate of 1500 mL / min. At a hydrogen pressure of 3.5MPa, an inlet temperature of 150°C, and a total space velocity of the raw material liquid phase of 8 h -1 , Under the condition of hydrogen / oil volume ratio of 200:1, feed the raw material for experiment. The weight concentration of aniline in the raw material liquid is 65%, the concentration range of 4-nitrodiphenylamine is 5%-15%, and the concentration range of 4-aminodiphenylamine is 20-30%. The hydrogenation results are shown in Table 1 (the reaction time is 96 hours).

[0021] Table 1

[0022]

Embodiment 2

[0024] The same operation steps as in Example 1 are used to carry out reduction treatment on the catalyst. Under the conditions of hydrogen pressure of 3.5MPa, inlet temperature of 150°C, and hydrogen / oil volume ratio of 300:1, raw materials were fed for testing. The mass concentration of aniline in the raw material liquid is 65%, the concentration range of 4-nitrodiphenylamine is 10%, and the concentration range of 4-aminodiphenylamine is 25%. Liquid phase total space velocity range 6-16 h -1 , hydrogenation results are shown in Table 2 (reaction time is 96 hours).

[0025]

Embodiment 3

[0027] The same operation steps as in Example 1 are used to carry out reduction treatment on the catalyst. The inlet temperature is set to 150°C, and the total space velocity of the raw material liquid phase is 8 h -1 , Hydrogen / oil volume ratio 200:1. The system pressure range is 2.0-4.0 MPa. The weight concentration of aniline in the raw material liquid is 65%, the concentration range of 4-nitrodiphenylamine is 10%, and the concentration range of 4-aminodiphenylamine is 25%. The hydrogenation results are shown in Table 3 (the reaction time is 96 hours).

[0028]

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Abstract

The present invention relates to a method for synthesizing 4-aminodiphenylamine, wherein problems of low raw material conversion rate and low product yield of the existing 4-nitrodiphenylamine batch hydrogenation process are mainly solved with the present invention. The technical scheme is that: a Ni base catalyst is adopted, the raw material adopts aniline as a solvent, 4-nitrodiphenylamine weight content in the reaction solution is 5-20%, 4-aminodiphenylamine weight content is 20-30%, and 4-nitrodiphenylamine is continuously synthesized at a reaction temperature of 100-250 DEG C under a reaction pressure of 2.0-4.0 MPa at the total liquid phase space velocity of 6.0-16.0 h<-1> according to a hydrogen / 4-nitrodiphenylamine volume ratio of 200-600:1. With the present invention, the problems in the prior art are well solved, and the method can be used for industrial production of continuous 4-nitrodiphenylamine synthesis.

Description

technical field [0001] The invention relates to a method for continuous synthesis of 4-aminodiphenylamine. Background technique [0002] The important intermediate of p-phenylenediamine antioxidants is 4-aminodiphenylamine. 4-Aminodiphenylamine, also known as p-aminodiphenylamine and RT-Base, is mainly used in the production of p-phenylenediamine rubber antioxidants 4010NA, 4020, 688, etc., and can also be used in rubber additives, dyes, textiles, printing and pharmaceutical industries Wait. According to incomplete statistics, the amount of 4010NA and 4020 in developed countries currently accounts for more than 70% of the total amount of antioxidants used. In 2007, the global output of 4-aminodiphenylamine was 260,000 tons. It is estimated that the world 4-aminodiphenylamine market capacity will reach 320,000 and 428,000 tons in 2010 and 2015, so its synthesis process has become the focus of research and development by domestic and foreign companies. In the world, Japanes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/50C07C209/36
Inventor 刘仲能孙云飞江兴华李则俊王燕波
Owner CHINA PETROLEUM & CHEM CORP
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