Process for preparing 4-amino diphenylamine

A technology of aminodiphenylamine and aniline, which is applied in the preparation of amino compounds from amines, the preparation of amino compounds by condensation/addition reactions, organic chemistry, etc., which can solve the problems of prolonging the reaction time, increasing energy consumption, difficulty in separation, and difficulty in reaction control

Active Publication Date: 2006-01-18
JIANGSU SINORGCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are some common disadvantages in these methods: one is that the selected catalyst is expensive, and the application to industrial scale production will cause the production cost to be too high, and there is no advantage compared with the current production process
In this patent, it is necessary to have a solvent and control the content of the proton material in the solution. The introduction of the solvent brings increased energy consumption and difficulty in separation. Controlling the proton material brings difficulty to the...

Method used

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  • Process for preparing 4-amino diphenylamine
  • Process for preparing 4-amino diphenylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Preparation of composite base catalyst:

[0077] In a 1000 ml three-necked flask equipped with a condenser and a stirrer, add 227.5 grams of 20% (by weight) tetramethylammonium hydroxide aqueous solution (0.50 moles), 10 grams of sodium hydroxide (0.25 moles), 346 grams of 30% tetramethylammonium carbonate aqueous solution (0.5 mol), stirred evenly at 72-77 ℃, promptly made composite base catalyst, concentration 27.3% (weight).

Embodiment 2

[0079] Preparation of composite powder catalyst:

[0080] Take 46 grams of nickel powder, 51 grams of aluminum powder, and 3 grams of iron powder, mix them evenly, and melt them into an alloy in an induction furnace. The molten alloy is sprayed on the high-speed rotating copper drum through the nozzle by the pressure of the gas, and it is rapidly quenched. (The cooling rate can reach 10 5 -10 6 K / S). The cooled alloy is rolled into powder by a ball mill, and sieved to obtain 99.7 grams of 40-300 mesh powder. In a three-necked flask equipped with a thermometer and a stirrer with a capacity of 500 milliliters, 375 grams of a concentration of 20% (weight) of NaOH aqueous solution was added slowly, and the powder prepared above was slowly added, stirred at 60° C. for 4 hours, and then The solid was washed with deionized water until neutral to obtain a composite powder catalyst.

Embodiment 3

[0082] A. Condensation

[0083] Open the composite base catalyst, aniline and nitrobenzene transfer pump simultaneously under vacuum, adjust the flow rate to 150 kg / hour of aniline, 30 kg / hour of nitrobenzene, and 200 kg / hour of composite base catalyst, the above components Nitrobenzene, aniline and composite base catalysts are continuously fed into the falling film reactor for heating to carry out condensation reaction; the condensation liquid in the falling film reactor is discharged from the lower part into the primary reactor to continue the condensation reaction; part one The condensate at the bottom of the first-stage reactor is returned to the falling film reactor through the circulation pump to form a partial circulation system. The heat medium of the falling film reactor is alcohol vapor at 78-90°C. Control the reaction temperature to 75°C, the pressure to 0.008MPa (absolute pressure), and the flow rate of the circulating fluid to be 1 meter 3 / Hour. The material f...

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Abstract

The present invention discloses production process of 4-amino diphenylamine with nitrobenzene and phenylamine as materials. For the condensation and hydrogenation, corresponding composite alkali catalyst and composite powdered catalyst are adopted separately. The production process includes the successive steps of condensation, separation I, hydrogenation, separation II and refining, and may be completed continuously. The composite alkali catalyst is separated and reused before the hydrogenation step, and this avoids the heat decomposition of the composite alkali catalyst and increases the catalyst selecting range. The production process has 4-amino diphenylamine yield industrial scale over 95 % and 4-amino diphenylamine purity over 99 wt%.

Description

technical field [0001] The present invention relates to the method for preparing 4-aminodiphenylamine, specifically, relate to using nitrobenzene and aniline as raw materials, using composite base catalyst as condensation catalyst, using conventional hydrogenation catalyst or composite powder catalyst as hydrogenation reaction catalyst, in Including condensation, hydrogenation, separation recovery and recycling of composite base catalyst and, if necessary, separation recovery and recycling of optionally at least partially regenerated composite powder catalyst, separation recovery and recycling of aniline and optional separation recovery and recycling of hydrogenation A method for continuously preparing 4-aminodiphenylamine in five processes of solvent and refining. Background technique [0002] 4-Aminodiphenylamine is an important antioxidant and stabilizer intermediate, and an important chemical product in the rubber industry and polymer industry. According to the differen...

Claims

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Application Information

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IPC IPC(8): C07C211/55C07C209/60C07C209/68
Inventor 王农跃余瑞标茅晓晖冯晓根程千文
Owner JIANGSU SINORGCHEM TECH CO LTD
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