Producing procedure of 3,4'-diamino diphenyl ether

A technology of diaminodiphenyl ether and m-aminophenol, applied in 3 fields, can solve problems such as unsatisfactory results and difficult product separation, and achieve the effects of easy separation, prolonging reaction time, and reducing reaction temperature

Active Publication Date: 2006-08-16
SHANGHAI PLASTICS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Prior art Japanese Patent Laying-Open 6-219999, open date August 9th, 1994, with sodium hydroxide as condensation agent, sodium hydroxide: m-aminophenol: the mol ratio of p-nitrochlorobenzene equals 1.7: 1: 1.1 , the condensation reaction temperature is 130-140°C, the reaction time is 3 hours, and the yield of the product 3-amino-4-nitrodiphenyl ether is 71.0%. There is a certain amount of unreacted substances in the reaction product, which leads to difficulty in product separation. The result is obviously not ideal and needs to be improved and improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Preparation of 3-amino-4'-nitrodiphenyl ether

[0016] Put 9.8g (0.234mol, content ≥ 96%) NaOH, 80g toluene and 21.8g (0.2mol) m-aminophenol into a 250ml three-necked flask, heat and stir. The temperature of the reactants is generally controlled above 120°C and not more than 130°C. The amount of water separated by reflux is about 2ml, and the time required is about 3.5 hours. Then add 70gDMF and 31.5g (0.2mol) p-nitrochlorobenzene, continue to heat, stir, and steam the toluene. After the toluene is evaporated, control the reaction temperature not to exceed 150°C, and continue heating and stirring. 2 hours after the addition of p-nitrochlorobenzene, the reaction is over, let it cool naturally, and when the temperature drops below 100°C, filter the reaction solution with suction, filter out inorganic salts such as NaCl, and directly use it for catalytic hydrogenation reaction; or The reaction solution was added to 200ml of cold water with stirring. After the addit...

Embodiment 2

[0020] In the manufacturing process of 3-amino-4'-nitrodiphenyl ether, except that the addition of condensing agent NaoH is 54.2g (1.35 moles), other formulas and operating steps are the same as in Example 1, and the result is that the crude yield is 92%. (weight), other is the same as embodiment 1.

[0021] In the process of hydrogenation reduction of 3-amino-4'-nitrodiphenyl ether to produce 3,4'-diaminodiphenyl ether, except that the hydrogenation temperature is 92°C and the hydrogenation pressure is 0.6Mpa, other conditions are the same as in Example 1. Same, the result is the same as Example 1 except that the yield is 66% (weight).

Embodiment 3

[0023] In the manufacturing process of 3-amino-4'-nitrodiphenyl ether, except that the addition of condensing agent NaoH is 60g (1.50 moles), other formulas and operating steps are the same as in Example 1, and the result is that the crude yield is 92.5%. Outside, other is the same as embodiment 1.

[0024]In the process of hydrogenation and reduction of 3-amino-4'-nitrodiphenyl ether to produce 3,4'-diaminodiphenyl ether, except that the hydrogenation temperature is 98°C and the hydrogenation pressure is 0.3Mpa, the others are the same as the examples 1, the result is the same as Example 1 except that the yield is 66.2%.

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Abstract

A process for preparing 3,4'-diaminodiphenyl ether or 3-amino-4'-notrodiphenyl ether includes such steps as reacting between meta-aminophenol or meta-nitrophenol and sodium hydroxide in toluene solvent to obtain phenol sodium, and reacting on p-nitrochlorobenzene at 110-130 deg.c for 3-4 hr.

Description

technical field [0001] The present invention relates to the manufacture method of 3,4'-diaminodiphenyl ether (3,4'-oxydianiline, be called for short 3,4'-ODA), more specifically relate to by m-nitrophenol or m-aminophenol and Condensation reaction of p-nitrochlorobenzene to obtain 3,4'-dinitrodiphenyl ether or 3-amino-4'-nitrodiphenyl ether, and prepare 3,4'-diaminodiphenyl ether through hydrogenation or reduction of iron powder Phenyl ether method. Background technique [0002] 3,4'-Diaminodiphenyl ether is the raw material of aromatic polyamide for fiber. It is also an important raw material for the preparation of fusible polyimide, which is widely used as heat-resistant resin moldings and electrical insulating films. It is also an important raw material for medicine and agriculture. In recent years, in order to expand the use of polyimide, the research on polyimide isomerization is booming, so 3,4'-diaminodiphenyl ether and 4,4'-diaminodiphenyl ether have become a synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/90C07C213/02C07C213/00
Inventor 张龙庆邱维波
Owner SHANGHAI PLASTICS RES INST CO LTD
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