Method for continuous hydrogenation preparation of 4-amino diphenylamine

A continuous technology of aminodiphenylamine, applied in the field of preparation of 4-aminodiphenylamine, which can solve the problems of many side reactions, three wastes pollution, and reduced reactor life

Active Publication Date: 2004-01-28
JIANGSU SINORGCHEM TECH CO LTD
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AI Technical Summary

Problems solved by technology

In order to obtain 4-aminodiphenylamine, different reducing agents can be used to reduce 4-nitrodiphenylamine and 4-nitrosodiphenylamine or/and their compositions, such as iron (Fe) powder, alkali sulfide reduction, but these A common problem in the method is that the reaction conditions are harsh, the yield is low, there are many side reactions, and there are a lot of "three wastes" pollution; in addition, the traditional batch hydrogenation process, because each step of the reactor must undergo pressure test, replacement, reaction and recovery The initial state and other processes, such repeated cumbersome operations, not only have high labor intensity and short catalyst life,

Method used

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  • Method for continuous hydrogenation preparation of 4-amino diphenylamine

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Embodiment 1

[0021] First check the airtightness of the device. It is required that the leakage rate of the system should be less than 5% after the nitrogen pressure test. Then make preparations before feeding, lay the bottom material, replace the nitrogen with hydrogen, pressurize to 1.3MPa, and start the cycler to maintain The flow rate of circulating hydrogen is 6 meters 3 (standard square) / hour, hydrogen enters the hydrogenation reactor in the form of bubbling through the circulator, to increase the gas-liquid mass transfer effect during the reaction, the flow rate of the condensation liquid after the reaction of nitrobenzene and aniline is 200 kg / hour , the flow rate of methyl alcohol is 60 kilograms / hour (weight %), after mixing 4-nitrosodiphenylamine content 15.1 (weight %), 4-nitrosodiphenylamine content 2.5 (weight %) enters the first-stage hydrogenation reactor, reacts The device is equipped with a magnetic seal stirring, cooling and heating system, and at the same time, a compos...

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Abstract

The present invention discloses a method for preparing 4-aminodiphenylamine by continuously hydronating condensate obtained from the reaction by using nitrobenzol and phenylamine as raw material and adopting compound powdered catalyst. i,e, adopts a catalyst and hydrogen gas circulation and solvent circulation combined new process to make the hydrogenation reaction be implemented under the condition of high-concentration, low-temp. and low pressure. The invented catalytic hydrogenation conversion rate can be up to 100%, and its selectivity is greater than 99%, and it is suitable for industrial production of 4-aminophenylamine.

Description

technical field [0001] The invention relates to a preparation method of 4-aminodiphenylamine, in particular to the preparation of 4-aminodiphenylamine by selecting a composite powder catalyst and a process flow and continuously hydrogenating a condensation liquid with nitrobenzene and aniline as raw materials. Background technique [0002] Using nitrobenzene and aniline as raw materials, 4-nitrodiphenylamine and 4-nitrosodiphenylamine or / and their salt condensation liquid can be prepared in the presence of a catalyst. In order to obtain 4-aminodiphenylamine, different reducing agents can be used to reduce 4-nitrodiphenylamine and 4-nitrosodiphenylamine or / and their compositions, such as iron (Fe) powder, alkali sulfide reduction, but these A common problem in the method is that the reaction conditions are harsh, the yield is low, there are many side reactions, and there are a lot of "three wastes" pollution; in addition, the traditional batch hydrogenation process, because e...

Claims

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Application Information

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IPC IPC(8): B01J23/755C07C209/36C07C209/60C07C211/55
Inventor 王农跃
Owner JIANGSU SINORGCHEM TECH CO LTD
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