Method for preparing 4,4'-diaminodiphenyl ether

A technology of diaminodiphenyl ether and dinitrodiphenyl ether, applied in the field of preparation 4, can solve the problems of high price, strong corrosion and high cost of hydrazine hydrate, and achieve easy industrial promotion and application, good quality and low production cost Effect

Inactive Publication Date: 2006-07-26
CHANGZHOU SUNLIGHT PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, hydrazine hydrate is more expensive, the cost is higher, and it is highly corrosive and toxic

Method used

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  • Method for preparing 4,4'-diaminodiphenyl ether
  • Method for preparing 4,4'-diaminodiphenyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Into the autoclave of 50L band stirrer, drop into 4Kg 4,4'-dinitrodiphenyl ether, 20g Pd content is the mixed solvent that the Pd / c catalyst of 3%, 25L methyl alcohol and 5L dimethylformamide form, Steam is passed into the interlayer of the high-pressure reactor to heat up the temperature. The high-pressure reactor is first replaced with nitrogen three times, and then replaced with hydrogen three times respectively, and the catalytic hydrogenation reduction reaction is carried out under the conditions of 95-100°C and 0.4Mpa. After the hydrogenation reaction is completed, filter while it is hot to separate the Pd / C catalyst, and then recycle the separated Pd / C catalyst after cleaning and activation. The crude 4,4'-diaminodiphenyl ether is 2.78Kg, the melting point is 190.0~190.4℃, the molar yield is 90.4%, the mixed solvent can also be recycled, and the crude 4,4'-diaminodiphenyl ether is vacuum sublimated 2.77 kg of white crystals of polymer grade 4,4'-diaminodiphenyl e...

Embodiment 2

[0026] Other conditions are the same as in Example 1, except that the Pd / c catalyst adopts a Pd / c catalyst with a Pd content of 5%. 2.83Kg of crude 4,4'-diaminodiphenyl ether was obtained, with a melting point of 190.1-190.5°C and a molar yield of 91.8%. The crude 4,4'-diaminodiphenyl ether was sublimated under reduced pressure to obtain 2.80 kg of white crystals of polymerization-grade crude 4,4'-diaminodiphenyl ether, with a melting point of 191.0-191.5°C and a molar yield of 91.0%.

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Abstract

The invention relates to a preparation method for 4, 4'-diamino diphenyl ether, which comprises: taking catalytic hydrogenation reduction reaction to the 4, 4'-dinitro diphenyl ether in alcohol solvent; crystallizing to obtain the coarse product; reducing pressure to sublimate and refine the coarse product for final product. This invention has well product quality and no pollution with low cost, and more fit to spread than the traditional ferrous powder-chlorhydric acid reduction method.

Description

Technical field [0001] The invention relates to a method for preparing 4,4'-diaminodiphenyl ether, which belongs to the technical field of fine chemicals. Background technique [0002] 4,4'-Diaminodiphenyl ether is a fine organic product with high added value. 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 produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C217/90
Inventor 胡国宜薛建伟丁志伟储秋生闵雪峰
Owner CHANGZHOU SUNLIGHT PHARMA
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