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Method for preparing 4,4-di(2,4-diamino phenoxy) diphenylmethane

A technology of diaminophenoxy and dinitrophenoxy, applied in 4 fields, can solve the problems such as no patents, literature reports and the like in the preparation method, and achieve the effects of convenient source of raw materials, less three wastes, and obvious energy saving and consumption reduction

Inactive Publication Date: 2008-08-27
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 4,4'-bis(2,4-diaminophenoxy)diphenylmethane is an important aromatic polyvalent primary amine, but its preparation method has no patents or literature reports

Method used

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  • Method for preparing 4,4-di(2,4-diamino phenoxy) diphenylmethane
  • Method for preparing 4,4-di(2,4-diamino phenoxy) diphenylmethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 53.2 grams (0.1 mole) of 4,4'-bis(2,4-dinitrophenoxy)diphenylmethane, 0.5 gram of palladium mass percentage is 15% palladium / carbon, 800 milliliters of ethanol and 1600 ml of ethylene glycol are added In the reaction flask, stir, heat up to 60° C., and start to add dropwise a hydrazine hydrate solution with a mass concentration of 60% (the molecular weight of hydrazine hydrate is 50.06), totaling 250.0 grams (solution weight). After the dropwise addition of hydrazine hydrate was completed, the stirring reaction was continued for 5 hours at a temperature range of 80°C to 90°C, cooled slightly, filtered while hot, cooling the mother liquor, adding pure water, the crystallized product was precipitated, filtered, and vacuum-dried to obtain 38.9 grams of 4 , 4'-bis(2,4-diaminophenoxy)diphenylmethane crystals with a purity of 99.8%, according to the actual obtained 4,4'-bis(2,4-diaminophenoxy)diphenylmethane The amount and the theoretical amount (41.2 g), the calculated yield...

Embodiment 2

[0029] 53.2 grams (0.1 moles) of 4,4'-bis(2,4-dinitrophenoxy)diphenylmethane, 10.0 grams of palladium mass percentage is 1% palladium / carbon, 100ml ethylene glycol and 2000ml ethanol are added to the reaction In the bottle, stir, heat up to 60° C., start to add dropwise a mass concentration of 85% hydrazine hydrate solution, a total of 294.1 grams (solution weight). After the dropwise addition of hydrazine hydrate was completed, the stirring reaction was continued within the temperature range of 80°C to 90°C for 3.5 hours, cooled slightly, filtered while hot, cooled mother liquor, added pure water, precipitated crystalline product, filtered, and vacuum-dried to obtain 37.6 grams of 4 , 4'-bis(2,4-diaminophenoxy)diphenylmethane crystals with a purity of 99.7%, according to the actual obtained 4,4'-bis(2,4-diaminophenoxy)diphenylmethane The amount and the theoretical amount (41.2 grams), the calculated yield of 4,4'-bis(2,4-diaminophenoxy)diphenylmethane was 91.2%.

Embodiment 3

[0031] 53.2 grams (0.1 moles) of 4,4'-bis(2,4-dinitrophenoxy)diphenylmethane, 5.0 grams of palladium mass percent palladium / carbon 200 milliliters of ethanol and 1000 milliliters of 2-methoxy Add base ethanol in the reaction flask, stir, heat up to 60° C., and start to add dropwise a hydrazine hydrate solution with a mass concentration of 80%, totaling 260.0 grams (solution weight). After the dropwise addition of hydrazine hydrate is completed, continue stirring and reacting for 1 hour at a temperature range of 80°C to 90°C, cool slightly, filter while hot, cool the mother liquor, add pure water, precipitate a crystalline product, filter, and vacuum dry to obtain 32.2 grams of 4 , 4'-bis(2,4-diaminophenoxy)diphenylmethane crystals with a purity of 99.4%, according to the actual obtained 4,4'-bis(2,4-diaminophenoxy)diphenylmethane The amount and the theoretical amount (41.2 grams), the calculated yield of 4,4'-bis(2,4-diaminophenoxy)diphenylmethane was 78.2%.

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Abstract

The invention relates to a preparation method of 4, 4'-bis (2, 4-diamino phenoxy) diphenylmethane, which comprises reacting 4, 4'-bis (2, 4-dinitro phenoxy) diphenylmethane in a system of palladium / charcoal, hydrazine hydrate solution and saturated fatty alcohol, at 80-90DEG C for 1-5h, filtering immediately, cooling the mother liquor, adding pure water, precipitating crystal product, filtering, drying in vacuum and obtaining 4, 4'-bis (2, 4-diamino phenoxy) diphenylmethane crystal. The invention has simple operation, eliminated following refining and extraction, low time consumption, high product yield and high purity (at least 99%), which is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic polyvalent primary amines, in particular to a preparation method of 4,4'-bis(2,4-diaminophenoxy)diphenylmethane. Background technique [0002] Aromatic heterocyclic polymers have excellent thermal stability, nuclear radiation resistance, flame retardancy, organic solvent resistance, and excellent high and low temperature mechanical properties and electrical properties. High-performance fields have been widely used. [0003] With the development of high-performance, lightweight, thin, and refined information electronic products, higher requirements are put forward for the insulating materials of flexible copper clad laminates (FCCL), such as high heat resistance, high strength, and low dielectric constant. and low dielectric loss etc. Therefore, polyimide materials are favored in the field of FCCL. [0004] 4,4'-bis(2,4-diaminophenoxy)diphenylmethane is one of the important raw materials f...

Claims

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Application Information

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IPC IPC(8): C07C217/90C07C213/02C07C213/00
Inventor 虞鑫海
Owner DONGHUA UNIV
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