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Method for preparing 4-amino diphenylamine

A technology for aminodiphenylamine and aniline, applied in the field of preparing 4-aminodiphenylamine, can solve the problems of unfavorable continuous production, expensive catalyst, low product purity, etc., avoid the problem of heat-sensitive decomposition, reduce the technical difficulty of industrialization, and increase the choice range effect

Inactive Publication Date: 2004-01-28
JIANGSU SINORGCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Above-mentioned various methods are to prepare 4-aminodiphenylamine with hydrogen hydrogenation as the mixture of above raw materials in the presence of catalyzer, but all there is some common shortcoming: the one, the selected catalyzer is expensive, and application industrial scale production can cause production The cost is too high and there is no advantage compared with the current production process
For example, the tetraalkylammonium hydroxide used in the condensation reaction and the noble metal palladium (Pd), platinum (Pt), rhodium (Rh) used in the hydrogenation reaction, etc., have few sources of raw materials and are extremely expensive.
Second, the operation is relatively cumbersome, which is not conducive to continuous production, so the production scale is limited
Third, the product purity is not high

Method used

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  • Method for preparing 4-amino diphenylamine

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Experimental program
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Effect test

Embodiment 1

[0039] At the same time, turn on the composite catalyst, aniline and nitrobenzene delivery pumps, adjust the flow rate to 150 kg / hour for aniline, 30 kg / hour for nitrobenzene, and 100 kg / hour for the composite alkali catalyst, and continuously enter the forced heat exchanger for forced heat exchange. The heat medium of the heat exchanger is alcohol vapor, and the condensed liquid in the heat exchanger is forced to enter the first-stage reactor from the top to continue dehydration and reaction, and then open the bottom valve of the first-stage reactor and the condensation circulation pump to adjust the outlet of the condensation circulation pump The valve makes the material return to the forced heat exchanger to form a partial circulation system, so that the material is continuously circulated, dehydrated and reacted. Control the reaction temperature to 75°C, the pressure (absolute pressure) to 0.008MPa, and control the circulating fluid flow rate to 2 meters 3 / Hour. As the r...

Embodiment 2

[0045] In the 500 milliliter three-neck flask that is furnished with condenser and stirrer, add 230 grams of water, add tetramethylammonium hydroxide 91 grams (containing pure tetramethylammonium hydroxide 50%, 0.50 moles, all the other are water ), 20 grams (0.5 moles) of sodium hydroxide, 55 grams (0.5 moles) of tetramethylammonium chloride, control mixing temperature 73-77 (℃), stir well, make compound type alkali catalyst, concentration 30.4 (weight % ).

Embodiment 3

[0047] Get 46 grams of nickel powder, 51 grams of aluminum powder, and 3 grams of copper powder, melt in an induction furnace, discharge, cool, and roll into powder, process, sieve, and keep the mesh number at 40-300 mesh. In a 500 ml three-necked flask, a thermometer and a stirrer are installed, and 375 grams of 20% sodium hydroxide aqueous solution is charged, and the metal alloy powder is slowly added, and the reaction temperature is kept at 60° C., and the reaction time is 4 hours, and then washed with water The catalyst is neutralized to obtain a metal powder catalyst.

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Abstract

The present invention discloses a method for producing 4-aminodiphenylamine by using nitrobenzol and phenylamine, and is characterized by that the compound alkali catalyst and compound powdered catalyst which are correspondent to the condensation and hydrogenation reaction are respectively selected and used, and successively undergone the circular process including the procedures of condensation,separating compound alkali catalyst, hydrogenation, separating and hydrogenating solvent, compound powdered catalyst and phenylamine and refining, and its preparation process can be continuously implemented. Said two catalysts are high in catalytic activity, and the content of 4-aminodiphenylamine in the product can be up to 99 wt%, and its industrial production yield rate is greater than 92%.

Description

technical field [0001] The invention relates to a method for preparing 4-aminodiphenylamine, in particular to a method for continuously preparing 4-aminodiphenylamine by using nitrobenzene and aniline as raw materials, adopting two kinds of composite catalysts and a cyclic operation process flow. Background technique [0002] 4-aminodiphenylamine is an intermediate product of important antioxidants and stabilizers, and is an important chemical product in the rubber industry and polymer industry. According to the difference of raw materials used, at present, the method of producing 4-aminodiphenylamine has, (1 ) the aniline method, using p-nitrochlorobenzene and aniline as raw materials, reacting under the action of a catalyst to generate 4-nitrodiphenylamine, and then reducing it to 4-aminodiphenylamine with a sulfurized alkali. (2) formanilide method, take formic acid and aniline as raw materials to condense formanilide, then react with p-nitrochlorobenzene in the presence ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/70B01J23/755C07C209/36C07C209/60C07C211/55
Inventor 王农跃
Owner JIANGSU SINORGCHEM TECH CO LTD
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