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A technology for aminodiphenylamine and aniline, which is applied in the field of preparing 4-aminodiphenylamine, and can solve the problems of prolonging operation steps, increasing production costs, and high catalyst preparation costs
Inactive Publication Date: 2005-06-22
CHINA PETROLEUM & CHEM CORP +2
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Problems solved by technology
[0016] The technical problem to be solved by this invention is that in the literature about nitrobenzene method to prepare 4-aminodiphenylamine in the past, there are catalyzers that need precious metals, so that the catalyst preparation cost is high; the main impurity azobenzene oxide / azobenzene and / or hydroazobenzene needs to be recovered separately, prolonging the operation steps, increasing the production cost, or only using the shortcomings of pure raw materials, providing a new method for preparing 4-aminodiphenylamine
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Embodiment 1
[0029]50 grams of 40% (weight) tetramethylammonium hydroxide aqueous solution is warming up to 55 ℃ under-0.090MPa , at -0.096MPa and warming up to 55 ° C, concentrated to a 40% (weight) solution], then add 135 grams of aniline, at -0.090 MPa, warming up to 75 ° C, aniline and water azeotropic distillation dehydration, to water When the / tetramethylammonium hydroxide mol ratio is 5: 1, add the nitrobenzene of 28 grams in 3 hours, continue to stir and maintain 8 hours, obtain coupling product; Wherein the organic matter weight percentage is composed of: aniline 48.9%, 4- Nitrosodiphenylamine 30.1%, 4-nitrodiphenylamine 7.0%, phenazine 0.35%, azobenzene 7.6%, tetramethylammonium hydroxide 6.5%.
[0030] A hydrogenation reduction reaction takes place in an autoclave, and 4 grams of modified skeleton nickel catalyst (dry basis), 45 grams of aniline, and 20 grams of water are added to the coupling product. Under stirring, when the reaction temperature is 70° C., the hydrogen pressu...
Embodiment 2～5
[0034] According to each operation step and condition of embodiment 1, just change the composition of catalyst, its reaction result is listed in table 1.
Embodiment 6
[0039] According to each operation step and condition of embodiment 2, just change the condition of hydrogenation reduction reaction: add aniline 60 grams in autoclave, reaction temperature is 50 ℃, hydrogen pressure rises to 6.0MPa, hydrogenation time is 5 hours. After the reaction, there is no azobenzene, hydroazobenzene and other by-products in the product. The conversion rate of 4-nitrodiphenylamine and 4-nitrosodiphenylamine is 100%, and the yield of 4-aminodiphenylamine is 96.7%. After using the catalyst for 20 times, the reaction result is: no azobenzene, hydroazo Benzene and other by-products. The conversion rate of 4-nitrodiphenylamine and 4-nitrosodiphenylamine is 100%, and the yield of 4-aminodiphenylamine is 96.6%.
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Abstract
The invention relates to a method for preparing 4-aminodiphenylamine by a nitrobenzene method. It mainly solves the need to use precious metals in the catalyst in the past technology, which makes the catalyst preparation cost high; the main impurities produced in the process, azobenzene oxide / azobenzene and / or hydroazobenzene need to be recovered separately or only pure raw materials can be used question. In the present invention, condensation reaction occurs with aniline and nitrobenzene in the presence of water and alkali, and then the condensation liquid containing strong alkali or strong organic base is reacted with water and alkali in the presence of skeleton nickel, especially modified skeleton nickel catalyst. Aromatic amine is used as a solvent, and the technical scheme of hydrogenation reduction reaction to generate 4-aminodiphenylamine solves this problem well, and realizes nitro, nitroso, azo or / and oxidized diphenylamine in one step through hydrogenation reduction reaction. The reduction of nitrogen compounds can be used in the industrial production of 4-aminodiphenylamine.
Description
technical field [0001] The invention relates to a method for preparing 4-aminodiphenylamine, in particular to a method for preparing 4-aminodiphenylamine by a nitrobenzene method. Background technique [0002] 4-aminodiphenylamine (4-aminodiphenylamine), also known as p-aminodiphenylamine, N-phenyl-p-phenylenediamine or RT base, is mainly used in the production of p-phenylenediamine rubber antioxidants 4010NA, 4020, 4010 and 688, etc. . In addition, it can also be used in the synthesis of blue salt VRT for dyes, textiles, printing and pharmaceutical industries. [0003] There are more than ten kinds of production methods for 4-aminodiphenylamine, and the currently industrialized methods mainly include aniline method, formanilide method, diphenylamine method and nitrobenzene method. These several methods all first synthesize 4-nitrodiphenylamine or 4-nitrosodiphenylamine, and then reduce to obtain 4-aminodiphenylamine. [0004] The aniline me...
Claims
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