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Catalytic hydrogenation method of 4-nitrodiphenylamine and 4-nitrosodiphenylamine

A technology of nitroso diphenylamine and nitroso diphenylamine is applied in the field of catalytic hydrogenation of 4-nitroso diphenylamine and 4-nitroso diphenylamine condensation solution, and can solve problems such as environmental pollution and human health damage, To achieve the effect of reducing production costs, saving energy consumption and improving economic benefits

Pending Publication Date: 2021-02-09
SINOPEC NANJING RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Trimethylamine waste gas will cause serious pollution to the environment, and will also cause great damage to human health

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Under the catalysis of tetramethylammonium hydroxide, 200g of condensed liquid containing 4-nitrodiphenylamine and 4-nitrosodiphenylamine with a water content of 4.9% obtained from the condensation reaction of raw materials with aniline and nitrobenzene was added to the reaction In the kettle, add 1.0 g of the skeleton nickel catalyst, 0.2 g of ethylene glycol, and 70.0 g of methanol with a water content of 10% into the reactor. After the reactor is sealed and tested for leaks, replace the air in the reactor with nitrogen, and then replace it with hydrogen. The number of replacements is 4 times, the replacement pressure is 0.25MPa, the stirring is started, the temperature is raised to 70°C, the hydrogen pressure is controlled at 2.0MPa, the hydrogenation temperature and hydrogenation pressure are maintained, the reaction time is 120min, and the hydrogenation reducing solution is analyzed by liquid chromatography, 4 - The conversion rate of nitrodiphenylamine and 4-nitros...

Embodiment 2

[0035] Under the catalysis of tetramethylammonium hydroxide, 200g of condensed liquid containing 4-nitrodiphenylamine and 4-nitrosodiphenylamine with a water content of 10.1% obtained from the condensation reaction of raw materials with aniline and nitrobenzene was added to the reaction In the kettle, add 7.0 g of the skeleton nickel catalyst, 2.4 g of glycerol, and 120.0 g of methyl alcohol with a water content of 30% in the reactor. After the reactor is sealed and leak tested, the air in the reactor is replaced with nitrogen, and then replaced with hydrogen. The number of replacements is 3 times, the replacement pressure is 0.28MPa, the stirring is started, the temperature is raised to 75°C, the hydrogen pressure is controlled at 1.4MPa, the hydrogenation temperature and pressure are maintained, the reaction time is 150min, and the hydrogenation reducing solution is analyzed by liquid chromatography, 4 - The conversion rate of nitrodiphenylamine and 4-nitrosodiphenylamine is ...

Embodiment 3

[0039]Under the catalysis of tetramethylammonium hydroxide, 200g of condensation liquid containing 4-nitrodiphenylamine and 4-nitrosodiphenylamine with a water content of 6.0% obtained from the condensation reaction of raw materials with aniline and nitrobenzene was added to the reaction In the still, add 1.6g of skeleton nickel catalyst, 1.0g of pentaerythritol, and 80.0g of methanol with a water content of 40% into the reaction kettle. After the reaction kettle is sealed and tested for leaks, replace the air in the reaction kettle with nitrogen, and then replace it with hydrogen. 5 times, the displacement pressure is 0.15MPa, start stirring, raise the temperature to 65°C, control the hydrogen pressure to 2.0MPa, maintain the hydrogenation temperature and hydrogenation pressure, and the reaction time is 118min. The hydrogenation reducing solution is analyzed by liquid chromatography. The conversion rate of phenyl-diphenylamine and 4-nitroso-diphenylamine is 99.9%, and the yiel...

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Abstract

The invention relates to the technical field of catalytic hydrogenation, and discloses a catalytic hydrogenation method of 4-nitrodiphenylamine and 4-nitrosodiphenylamine. The method comprises the following steps: by taking aniline and nitrobenzene as raw materials, taking a condensation solution containing 4-nitrodiphenylamine and 4-nitrosodiphenylamine obtained by condensation reaction as a hydrotreating object, adding a hydrogenation reaction aid, a hydrogenation reaction solvent and a skeleton nickel catalyst, controlling the hydrogenation temperature to be 58-80 DEG C and the hydrogen pressure to be 1.0-3.0 MPa, observing that the hydrogenation reaction does not absorb hydrogen any more, cooling, and stopping the reaction. The method can reduce the influence of the water content in the condensation liquid and the solvent on the catalytic hydrogenation reduction of the 4-nitrodiphenylamine and 4-nitrosodiphenylamine condensation liquid, solves the problem of normal hydrogenation reaction of the skeleton nickel catalyst in a water-containing system, reduces the energy consumption, saves the production cost, and has wide application prospects.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a catalytic hydrogenation method for condensation liquid of 4-nitrodiphenylamine and 4-nitrosodiphenylamine. Background technique [0002] 4-Nitrodiphenylamine and 4-nitrosodiphenylamine are raw materials for the preparation of 4-aminodiphenylamine, and 4-aminodiphenylamine (p-aminodiphenylamine, also known as RT base) is an important fine chemical intermediate , Widely used in rubber additives, dyes, textile and pharmaceutical industries, etc., mainly used in rubber antioxidant 4010NA, 6PPD, etc. [0003] The process of preparing RT base (4-aminodiphenylamine) by nitrobenzene method takes nitrobenzene and aniline as raw materials, and carries out continuous condensation with tetramethylammonium hydroxide as a condensation catalyst to obtain a compound containing 4-nitrodiphenylamine and 4- The condensation liquid of nitrosodiphenylamine, adding a solvent to t...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C209/38C07C211/55
CPCC07C209/36C07C209/38C07C211/55Y02P20/584
Inventor 吴其建王晓宁陈永平刘卓
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD
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