Process for preparing 4,4'-diamino diphenyl ether

The technology of diaminodiphenyl ether and dinitrodiphenyl ether is applied in the field of fine chemical industry, and can solve the problems of high price, high corrosiveness and high cost of hydrazine hydrate, and achieve easy industrial popularization and application, good quality and low production cost. Effect

Inactive Publication Date: 2006-09-06
CHANGZHOU SUNLIGHT PHARMA
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Problems solved by technology

However, hydrazine hydrate is more expensive, the c

Method used

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  • Process for preparing 4,4'-diamino diphenyl ether

Examples

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Embodiment 1

[0029] Put 4Kg of 4,4'-dinitrodiphenyl ether, 200g of skeletal nickel catalyst, 25L of methanol and 5L of dimethylformamide into the 50L high-pressure reactor with stirring device, and pass it into the interlayer of the high-pressure reactor. The steam is heated to raise the temperature, and the high-pressure reactor is first replaced with nitrogen three times, and then replaced with hydrogen three times, and the catalytic hydrogenation reduction reaction is carried out under the conditions of 95-105°C and 0.5Mpa. After the hydrogenation reaction is completed, filter while hot to separate the skeleton nickel catalyst, wash and recycle. The separated filtrate was cooled with ice-water mixture at 0°C, and 2.81Kg of crude 4,4'-diaminodiphenyl ether was precipitated, with a melting point of 190.1-190.6°C, a purity of 99.5% (HPLC), and a molar yield of 91.4 %. The mixed solvent after separating out the product can also be recycled. Crude 4,4'-diaminodiphenyl ether was recrystalli...

Embodiment 2

[0031] Other conditions are the same as in Example 1, except that the mixed solvent is composed of 20L methanol and 10L dimethylformamide. 2.78Kg of crude 4,4'-diaminodiphenyl ether was obtained, with a melting point of 190.0-190.5°C, a purity of 99.5% (HPLC), and a molar yield of 90.4%. Crude 4,4'-diaminodiphenyl ether was recrystallized from ethylene glycol monoethyl ether to obtain 2.63Kg of white crystals of polymer grade 4,4'-diaminodiphenyl ether, with a melting point of 191.0-191.5°C and a purity of 99.7% (HPLC).

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Abstract

The invention relates to a method for preparation of 4, 4í»-diaminodiphenyl oxide, which belongs to the sphere of the fine chemical technology. The 4, 4í»-dinitrodiphenyl oxide performs the reaction of catalysis, hydrogenization and reduction in the alcoholic solvent with the help of the catalyst and the crude 4, 4í»-diaminodiphenyl oxide is gained after the crystallization action. The product of 4, 4í»-diaminodiphenyl oxide is obtained by recrystallization purification of the said crude 4, 4í»-diaminodiphenyl oxide. It is characterized in that it adopts the technique of catalysis, hydrogenization and reduction, optimizes the manufacturing process, is of low cost, slight pollution to the environment, good product quality, high yield rate, strong marketable competitive power, so it is easier for industrial extension application than the traditional reduction with iron powder-hydrochloric acid.

Description

Technical field [0001] The invention relates to a preparation method of 4,4'-diaminodiphenyl ether, which belongs to the technical field of fine chemicals. Background technique [0002] 4,4'-Diaminodiphenyl ether is a high value-added fine chemical product. It is one of the important raw materials of new special engineering plastics polyimide, polyetherimide, polyesterimide, polyamideimide, polymaleimide, polyaramide and other high temperature resistant resins. It is also the raw material for the synthesis of 3,3',4,4'-tetraaminodiphenyl ether, which is used to prepare a series of new heat-resistant aromatic heterocyclic polymer materials such as polybenzimidazole, polyphenylquinoline, polyimidazole The main monomer of pyrolone. It can also be used as a raw material and crosslinking agent for synthetic polymer materials such as high-performance heat-resistant epoxy resin and polyurethane. At the same time, it is also used to replace the carcinogenic benzidine to produce a...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C217/90
Inventor 胡国宜薛建伟丁志伟储秋生闵雪峰
Owner CHANGZHOU SUNLIGHT PHARMA
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