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Method for preparing 4-aminodiphenylamine

A technology of aminodiphenylamine and aniline, applied in the field of preparation of 4-aminodiphenylamine, can solve the problems of expensive catalyst, limited production scale, low product purity, etc., achieve high conversion rate and selectivity, reduce pollution, and make the preparation process continuous Effect

Inactive Publication Date: 2003-12-10
JIANGSU SINORGCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods are to prepare 4-aminodiphenylamine with the mixture of the above raw materials by hydrogen hydrogenation in the presence of catalyzers, but there are some common shortcomings: the one, the selected catalyst is expensive, and the application of industrial scale production will cause the production cost to be too high , 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 cumbersome, which is not conducive to continuous production, and the production scale is limited
Third, the product purity is not high

Method used

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  • Method for preparing 4-aminodiphenylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Turn on the composite catalyst, aniline and nitrobenzene delivery pump at the same time, adjust the flow to 150 kg / h of aniline, 30 kg / h of nitrobenzene, and 100 kg / h of compound alkali catalyst, and continuously enter the forced heat exchanger for forced exchange. The heat medium of the heat exchanger is alcohol vapor, and the condensation liquid in the heat exchanger is forced to be pumped into the first-stage reactor from the top of the heat exchanger 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 returns the material to the forced heat exchanger to form a local circulation system, so that the material is continuously circulated, dehydrated and reacted. Control the reaction temperature at 75℃, the pressure (absolute pressure) at 0.008MPa, and control the circulating fluid flow at 2 meters 3 / hour. With the continuous e...

Embodiment 2

[0045] In a 500 ml three-necked flask equipped with a condenser and a stirrer, add 230 grams of water, add 91 grams of tetramethylammonium hydroxide (50%, 0.50 mol, the rest is water) and 20 grams of sodium hydroxide in an out of order (0.5 mol), 52 grams (0.25 mol) of tetramethyl ammonium carbonate, control the mixing temperature to 72-77 (°C), and stir evenly to obtain a composite alkali catalyst with a concentration of 29.9 (wt%).

Embodiment 3

[0047] Take 46 grams of nickel powder, 51 grams of aluminum powder, and 3 grams of copper powder, melt them in an induction furnace, discharging and cooling, and crush them into powder form, process, sieving, and keep the mesh number between 40-300 meshes. A 500 ml three-necked flask is equipped with a thermometer and a stirrer. 375 g of a 20% NaOH aqueous solution is charged. The powder is slowly added. The reaction temperature is maintained at 60°C and the reaction time is 4 hours. Then the catalyst is washed with water to Neutral, that is, a composite powder catalyst is obtained.

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Abstract

The method for producing 4-aminodiphenylamine by using nitrobenzene and phenylamine as raw material uses composite alkaline catalyst and composite powder catalyst and adopts a circulating technological process formed from five procedures of condensation, hydrogenation, separating and recovering the above-mentioned catalysts, separating and recovering hydrogenation solvent and refining to implement the method. The technological process is suitable for industrial production.

Description

Technical field [0001] The invention relates to a method for preparing 4-aminodiphenylamine, in particular to a method for continuously preparing 4-aminodiphenylamine using nitrobenzene and aniline as raw materials, using two composite catalysts and a cyclic operation process. Background technique [0002] 4-aminodiphenylamine is an important intermediate product of antioxidants and stabilizers. It is an important chemical product in the rubber industry and polymer industry. According to the different raw materials used, the current methods for producing 4-aminodiphenylamine include, (1 ) The aniline method uses p-nitrochlorobenzene and aniline as raw materials, reacts under the action of a catalyst to generate 4-nitrodiphenylamine, which is then reduced to 4-aminodiphenylamine with alkali sulfide. (2) Formanilide method, using formic acid and aniline as raw materials to react to form formanilide, and then react with p-nitrochlorobenzene in the presence of an acid binding agent t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C209/36C07C209/60C07C211/55
Inventor 冯晓根
Owner JIANGSU SINORGCHEM TECH CO LTD
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