Process for producing 2,2-bis[2,4-diaminophenyloxy)phenyl]hexafluoropropane

A technology of diaminophenoxy and dinitrophenoxy, which is applied in two fields, can solve the problems of no patents and literature reports in the preparation method, and achieve the effects of convenient source of raw materials, less waste, and high yield

Inactive Publication Date: 2008-08-20
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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

Method used

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  • Process for producing 2,2-bis[2,4-diaminophenyloxy)phenyl]hexafluoropropane
  • Process for producing 2,2-bis[2,4-diaminophenyloxy)phenyl]hexafluoropropane

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 66.8 grams (0.1 mole) of 2,2-bis[4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane, 0.7 gram of palladium with a mass percentage of 15% palladium / carbon, 500 milliliters of ethanol Add 500ml ethylene glycol in the reaction flask, stir, heat up to 60°C, start to add dropwise a mass concentration of 60% hydrazine hydrate solution (hydrazine hydrate molecular weight is 50.06), a total of 250.0 grams (solution weight). After the dropwise addition of hydrazine hydrate is completed, continue to stir and react for 1 hour at a temperature range of 70°C to 85°C, then cool slightly, filter while hot, cool the mother liquor, add pure water, precipitate a crystalline product, filter, and vacuum-dry to obtain 52.1 grams of 2 , 2-bis[4-(2,4-diaminophenoxy)phenyl]hexafluoropropane crystal, the purity is 99.6%, according to the actual obtained 2,2-bis[4-(2,4-diamino The amount of phenoxy) phenyl] hexafluoropropane and the theoretical amount (54.8 grams), calculate the yield of 2,2-bis[4-(...

Embodiment 2

[0029] 66.8 grams (0.1 moles) of 2,2-bis[4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane, 8.8 grams of palladium mass percent 1% palladium / carbon and 4420ml of ethanol were 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 85%, totaling 294.1 grams (solution weight). After the addition of hydrazine hydrate was completed, the stirring reaction was continued for 5 hours at a temperature range of 70°C to 85°C, cooled slightly, filtered while hot, cooling the mother liquor, adding pure water, and crystallized product was precipitated, filtered, and vacuum-dried to obtain 49.4 grams of 2 , 2-bis[4-(2,4-diaminophenoxy)phenyl]hexafluoropropane crystal, the purity is 99.2%, according to the actual obtained 2,2-bis[4-(2,4-diamino The amount of phenoxy) phenyl] hexafluoropropane and the theoretical amount (54.8 grams), calculate the yield of 2,2-bis[4-(2,4-diaminophenoxy)phenyl]hexafluoropropane was ...

Embodiment 3

[0031] With 66.8 grams (0.1 mole) 2,2-bis[4-(2,4-dinitrophenoxy) phenyl]hexafluoropropane, 4.0 grams of palladium mass percent is 5% palladium / carbon and 1000ml 2- Add methoxyethanol in the reaction flask, stir, heat up to 60° C., start to add dropwise hydrazine hydrate solution with a mass concentration of 80%, totaling 260.0 g (solution weight). After the dropwise addition of hydrazine hydrate is completed, continue stirring and reacting for 4 hours at a temperature range of 70°C to 85°C, cool slightly, filter while hot, cool the mother liquor, add pure water, precipitate crystallized product, filter, and vacuum dry to obtain 50.0 g of 2 , 2-bis[4-(2,4-diaminophenoxy)phenyl]hexafluoropropane crystal, the purity is 99.1%, according to the actual obtained 2,2-bis[4-(2,4-diamino The amount of phenoxy) phenyl] hexafluoropropane and the theoretical amount (54.8 grams), calculate the yield of 2,2-bis[4-(2,4-diaminophenoxy)phenyl]hexafluoropropane was 91.3%.

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Abstract

The invention relates to a preparation method of 2,2-double(4-(2,4-diamino phenoxy)phenyl)hexafluoropropane, comprising the steps as following, after being put into the solvent system of the solution of palladium or carbon hydrazine hydrate and saturated fatty alcohol for reaction for 1 to 5 hours with the temperature of 70 to 85 DEG C, the 2,2-double(4-(2,4-dinitro phenoxy)phenyl)hexafluoropropane is filtered when being hot, mother liquor is cooled off, pure water is dripped in, crystal products are precipitated, filtered, and dried in vacuum, and crystals of the 2,2-double(4-(2,4-diamino phenoxy) phenyl) hexafluoropropane are gained. The method has the simple operation, needs no subsequent refining and purifying technique, takes little time, has the products with the high yield and the purity of more than 99 percent, and 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 2,2-bis[4-(2,4-diaminophenoxy)phenyl]hexafluoropropane. 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] 2,2-bis[4-(2,4-diaminophenoxy)phenyl]hexafluoropropane is one of the imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/90C07C213/02C07C213/00
Inventor 虞鑫海
Owner DONGHUA UNIV
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