Preparation process of 4-amino diphenylamine
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
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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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