Preparation method of 4-aminodiphenylamine

A technology of aminodiphenylamine and nitrodiphenylamine, which is applied in the field of preparation of 4-aminodiphenylamine and can solve the problems of low catalyst recycling rate, low product purity or production capacity, equipment corrosion and the like

Inactive Publication Date: 2018-06-15
YANTAI ANOKY FINE CHEM CO LTD +4
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved by the present invention is that the existing 4-aminodiphenylamine preparation method has harsh reaction conditions, serious equipment corrosion, many wastes, serious environmental pollution or low catalyst recycling rate, continuous production, and low product purity or production capacity. etc. defects, and provide a kind of preparation method of 4-aminodiphenylamine

Method used

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  • Preparation method of 4-aminodiphenylamine

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Effect test

Embodiment 1

[0092] A preparation method of 4-aminodiphenylamine, using 4-nitrodiphenylamine as raw material, adopting ReneyNi catalyst, carrying out continuous catalytic hydrogenation reaction in a reactor, after the catalyst is separated and recovered, the reducing solution is desolvated and purified to obtain The target product 4-aminodiphenylamine.

[0093] Specific steps include:

[0094](1) Put 5000kg of methanol and 1250kg of 4-nitrodiphenylamine into the chemical material tank, follow-up feeding is carried out according to the ratio, stir evenly, pump them into the first-stage hydrogenation reactor, add ReneyNi catalyst 125kg, the particle size of the catalyst The diameter is 10nm, pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 90-100°C, and pump 4-nitrodiphenylamine into the primary hydrogenation tank at a flow rate of 6000L / h The raw material solution, into the H 2...

Embodiment 2

[0098] (1) Put 5000kg of methanol and 1250kg of 4-nitrodiphenylamine into the chemical tank, follow up the feeding according to the ratio, stir evenly, pump them into the first-stage hydrogenation reactor, add 125kg of ReneyNi catalyst, the particle size of the catalyst 500μm; pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 80-90°C, and pump 4-nitrodiphenylamine into the first-stage hydrogenation tank at a flow rate of 5000L / h Raw material liquid, pass into H 2 , the hydrogen pressure in the control system is 3.0MPa, and 2.5kg of ReneyNi catalyst is added to the primary hydrogenation reactor every 3 hours. After the material in the primary hydrogenation reactor gradually increases, it flows into the secondary reactor through the overflow port. In the hydrogenation kettle, the material stays in the hydrogenation kettle for about 2-3 hours. After the reaction is qual...

Embodiment 3

[0102] (1) 12500kg of methanol and 1250kg of 4-nitrodiphenylamine are put into the chemical material tank, and the subsequent feeding is stirred evenly according to the ratio. The diameter is 10nm; pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 90-100°C, and pump 4-nitrodiphenylamine into the first-stage hydrogenation tank at a flow rate of 6000L / h The raw material solution, into the H 2 , the hydrogen pressure in the control system is 3.0MPa, and 2.5kg of ReneyNi catalyst is added to the primary hydrogenation reactor every 3 hours. After the material in the primary hydrogenation reactor gradually increases, it flows into the secondary reactor through the overflow port. In the hydrogenation kettle, the material stays in the hydrogenation kettle for about 2-3 hours. After the reaction is qualified (4-nitrodiphenylamine residue ≤ 0.2%), the secondary hydrogenation k...

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Abstract

The invention discloses a preparation method of 4-aminodiphenylamine. 4-nitrodiphenylamine is subjected to continuous catalytic hydrogenation, then settlement and membrane filtration to obtain 4-aminodiphenylamine. The method has the advantages of simple operation, high safety and continuous production, can achieve effects of high production efficiency, high product quality, low labor intensity, environmental friendliness and high utilization rate of catalyst, and is beneficial to industrialization.

Description

technical field [0001] The present invention relates to the preparation method of 4-aminodiphenylamine. Background technique [0002] 4-Aminodiphenylamine is an important fine chemical intermediate, mainly used in the pharmaceutical and dye industries, and can be used to prepare the intermediate of ice dye black salt K and the intermediate of medicine, insecticide and antioxidant. At present, the methods for producing 4-aminodiphenylamine include 4-nitrodiphenylamine iron powder reduction, sodium sulfide reduction method, hydrogenation reduction method, etc., special powder reduction and sodium sulfide reduction, there are many three wastes, serious environmental pollution and cannot be continuously produced , The problem of low production capacity. Therefore, how to provide a method for preparing 4-aminodiphenylamine with high production efficiency, high product quality, low labor intensity and environmental friendliness is still an urgent technical problem to be solved by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C211/54
CPCC07C209/36C07C211/54Y02P20/584
Inventor 刘云龙曲美君戴杰张永明杨勇
Owner YANTAI ANOKY FINE CHEM CO LTD
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