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Process for preparing 4,4-diaminodiphenyl ether

A technology of diaminodiphenyl ether and dinitrodiphenyl ether, which is applied in the field of preparation of 4,4'-diaminodiphenyl ether, can solve the problem of affecting the completeness of the reaction, the purity of the product, and the pollution of the working environment and the atmospheric environment , affecting product quality and yield and other issues, to achieve the effect of improving product purity, high reactivity, and improving product quality and yield

Inactive Publication Date: 2004-09-01
郑效农
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) High production cost
On the one hand, the reaction solvent is butanol solution, since 4,4'-dinitrodiphenyl ether is insoluble in water, only a single butanol solution can be used
On the other hand, the iron powder is gray cast iron powder, the price is high, and the reactivity of gray cast iron powder is poor, the dosage is large, and the reaction time is long
[0005] (2) Big environmental pollution
After the reduction reaction is completed, filter (called hot filter) and crystallization treatment at a relatively high temperature of 70-105 °C, the butanol solvent volatilizes seriously, which not only wastes raw materials, increases production costs, but also pollutes the working environment and the atmospheric environment
[0006] (3) Poor product quality and low yield
Imperfect reaction control affects the thoroughness of the reaction and the purity of the product, affecting the quality and yield of the product

Method used

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  • Process for preparing 4,4-diaminodiphenyl ether

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 2000 ml Erlenmeyer flask, add 800 ml of n-butanol, 400 ml of deionized water, 12 grams of OP-10 surfactant, 11.4 grams of ammonium chloride, 24 grams of 4,4'-dinitrodiphenyl ether, Heat up to 80 degrees. There is a small amount of reflux in the condenser under rapid stirring. At this time, slowly add 48 grams of iron powder of the steel ball grinding slurry that has been pretreated, and control the reaction temperature between 90 and 105 °C with the speed of adding iron powder, and then add 4 in batches. , 4'-dinitrodiphenyl ether and iron powder, the total intake of 4,4'-dinitrodiphenyl ether is 72 grams, and iron powder 120~144 grams. After the reaction reached the end point, 13 grams of sodium bisulfite was added to continue the reaction for 30 minutes. Add 30% ammonia water dropwise until the pH value of the solution is 8-9. After cooling to room temperature 20-25°C, filter to obtain filter cake, wash the filter cake with water for flotation treatment, separa...

Embodiment 2

[0032] 600 milliliters of n-butanol, 600 milliliters of water, other with embodiment 1, get thick 4,4'-diaminodiphenyl ether 47.5 grams, the weight yield of 4,4'-dinitrodiphenyl ether is 66% , melting point 182°C, chromatographic purity 94%.

Embodiment 3

[0034] Surfactant is changed into Tween-80 20 grams, other is with embodiment 1.

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Abstract

A process for preparing 4,4'-diaminodiphenylether includes reduction reaction between 4,4'-dinitrodiphenylether and iron powder in the mixed solution of butanol, water and oil-water amphiprotic surfactant, crystallizing to obtain coarse product, refining by acid and alkali, and vacuudm sublimation. Its advantages are high output rate and quality of product and low pollution.

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 an important polymer for the manufacture of heat-resistant resins and electrical insulation materials, and has important uses in the coating and adhesive industries. 4. 4'-Diaminodiphenyl ether has excellent properties such as high voltage resistance at high temperature, strong radiation, corrosion resistance, and easy processing. It is widely used in aerospace, electromechanical, computer, transportation, transformers, special cables and other industrial fields. With the development of science and technology, the application range and demand of 4,4'-diaminodiphenyl ether will continue to increase. [0003] At present, the preparation and production of 4,4'-diaminodiphenyl ether adopts the reduction method of 4,4'-dinitrodiphenyl ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/90
Inventor 郑效农
Owner 郑效农