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Method for reparing p-aminodiphenylamine through solid base method

A technology of solid base and solid base catalyst, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of trimethylamine gas, which is difficult to recover from tetramethylammonium hydroxide, and achieve environmentally friendly, The effect of reducing energy consumption and material consumption and simplifying the production process

Inactive Publication Date: 2019-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The invention provides a method for preparing RT base by solid alkali method, which solves the problems of difficulty in recovering organic base tetramethylammonium hydroxide and decomposition of trimethylamine gas that produces foul smell in the current production process of RT base by nitrobenzene method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of solid base catalyst: styrene-divinylbenzene copolymer with macroporous structure has quaternary ammonium [-N + (CH 3 ) 3 ], 10.0 g of anion exchange resin, placed in 20.0 g of 2.5% chloroplatinic acid solution, added 10.0 g of 35% formaldehyde solution, stirred evenly, and left to stand for 24 hr. Filter and soak the filter cake with 20.0 g of 10% sodium hydroxide solution for 24 hours. Wash with deionized water until the pH value of the washed water does not exceed 9.

[0019] Condensation: add the compound prepared by the above method to a mixed solution of 50.0 g of aniline and 10.0 g of nitrobenzene, control the temperature at 90°C, continue the reaction for 5 hours, add 5.0 g of water, and separate the solid and liquid to obtain 61.5 g of the liquid phase. The content of each component in the liquid phase was analyzed, and it was calculated that the conversion rate of nitrobenzene was 96.3%, the selectivity of 4-nitrodiphenylamine was 15.9%, the s...

Embodiment 2

[0021] Preparation of solid base catalyst: styrene-divinylbenzene copolymer with macroporous structure has quaternary ammonium [-N + (CH 3 ) 3 ], 10.0 g of anion exchange resin, placed in 20.0 g of 5.0% chloroplatinic acid solution, added 20.0 g of 35% formaldehyde solution, stirred evenly, and stood for 24 hr. Filter and soak the filter cake with 20.0 g of 10% sodium hydroxide solution for 24 hours. Wash with deionized water until the pH value of the washed water does not exceed 9.

[0022] Condensation: Add the solid base catalyst prepared by the above method to a mixed solution of 50.0g aniline and 10.0g nitrobenzene, control the temperature at 90°C, continue the reaction for 5hrs, add 5.0g of water, and separate the solid and liquid to obtain 61.5g of the liquid phase . The content of each component in the liquid phase was analyzed, and it was calculated that the conversion rate of nitrobenzene was 96.9%, the selectivity of 4-nitrodiphenylamine was 16.1%, the selectivi...

Embodiment 3

[0024] Preparation of solid base catalyst: styrene-divinylbenzene copolymer with macroporous structure has quaternary ammonium [-N + (CH 3 ) 3 ], 10.0 g of anion exchange resin, placed in 20.0 g of 5.0% chloroplatinic acid solution, added 20.0 g of 35% formaldehyde solution, stirred evenly, and stood for 24 hr. Filter and soak the filter cake with 20.0 g of 10% sodium hydroxide solution for 24 hours. Wash with deionized water until the pH value of the washed water does not exceed 9.

[0025] Condensation: Add the solid base catalyst prepared by the above method into a mixed solution of 50.0g aniline and 10.0g nitrobenzene, control the temperature at 60°C, continue the reaction for 5hrs, add 5.0g of water, and separate the solid and liquid to obtain 62.7g of the liquid phase . The content of each component in the liquid phase was analyzed, and it was calculated that the conversion rate of nitrobenzene was 90.3%, the selectivity of 4-nitrodiphenylamine was 16.4%, the selecti...

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Abstract

According to the invention, condensation is carried out at a temperature of 60-100 DEG C by using a platinum-loaded macroporous polystyrene strong base resin as a condensation catalyst and using aniline and nitrobenzene as raw materials to prepare 4-(nitroso)nitrodiphenylamine, and hydrogenation reduction is carried out on the obtained condensation liquid so as to prepare p-aminodiphenylamine; andwith the application of the method in preparation of p-aminodiphenylamine, the complex recovery processes such as liquid alkali concentration, desalination and the like are not needed so as to simplify the production process and reduce the energy consumption and the material consumption, tetramethylammonium hydroxide easily decomposed to generate trimethylamine is not adopted so as to achieve environmental protection, the conversion rate of nitrobenzene is greater than or equal to 95%, and the selectivity of 4-(nitroso)nitrodiphenylamine is greater than or equal to 93%.

Description

technical field [0001] The invention belongs to the field of fine chemical industry and relates to the preparation of RT base, an intermediate of rubber antioxidant. Background technique [0002] RT base (p-aminodiphenylamine) is widely used in the fields of rubber additives, dyes, textiles, printing and pharmaceutical industries, and is mainly used in the production of rubber antioxidants 4010NA and 6PPD. Foreign RT base manufacturers use diphenylamine method and nitrobenzene method to produce RT base. [0003] The process route of synthesizing p-aminodiphenylamine with diphenylamine abroad is very mature, and many enterprises adopt this route for production, such as Compton-Uniroyal Company, Sumitomo Chemical, Ouchi Xinxing, Russia Nitrogen Consortium, etc., this process It has the disadvantages of long process flow and difficult treatment of a large amount of waste water. [0004] Compared with the diphenylamine method, the nitrobenzene method has higher yield and less ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/55C07C209/36C07C209/38
CPCC07C209/36C07C209/38
Inventor 陈永平王晓宁吴其建刘卓陈永乐
Owner CHINA PETROLEUM & CHEM CORP
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