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Process for producing 2,2-bis[3-amido-4-(4-aminophenoxy)phenyl] hexafluoropropane

A technology of aminophenoxy and hexafluoropropane, applied in 2 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, high yield and few chemical raw materials

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

AI Technical Summary

Problems solved by technology

[0005] 2,2-bis[3-amino-4-(4-aminophenoxy)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[3-amido-4-(4-aminophenoxy)phenyl] hexafluoropropane
  • Process for producing 2,2-bis[3-amido-4-(4-aminophenoxy)phenyl] hexafluoropropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 60.8 grams (0.1 moles) of 2,2-) two [3-amino-4-(4-nitrophenoxy) phenyl] hexafluoropropane, 0.7 gram of palladium mass percent is 15% palladium / carbon, 250 Milliliters of ethanol and 670ml ethylene glycol were added in the reaction flask, stirred, heated up to 60° C., and began to add dropwise a mass concentration of 60% hydrazine hydrate solution (hydrazine hydrate molecular weight was 50.06), a total of 208.3 grams (solution weight). After the dropwise addition of hydrazine hydrate is completed, continue to stir and react at a temperature range of 70°C to 85°C for 1 hour, cool slightly, filter while hot, cool the mother liquor, add an appropriate amount of pure water dropwise, precipitate a crystalline product, filter, and dry in vacuum to obtain 51.1 Gram of 2,2-bis[3-amino-4-(4-aminophenoxy)phenyl]hexafluoropropane crystal, the purity is 99.6%, according to the actual obtained 2,2-bis[3-amino-4- The amount of (4-aminophenoxy)phenyl]hexafluoropropane and the theoretic...

Embodiment 2

[0029] With 60.8 grams (0.1 mole) 2,2-bis[3-amino-4-(4-nitrophenoxy group) phenyl] hexafluoropropane, 12.1 grams of palladium mass percentages are 1% palladium / carbon and 6000ml ethanol Add it into 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 47.1 grams (solution weight). After the addition of hydrazine hydrate is completed, continue to stir and react for 5 hours at a temperature range of 70°C to 85°C, cool slightly, filter while it is hot, cool the mother liquor, add an appropriate amount of pure water dropwise, precipitate a crystalline product, filter, and vacuum dry to obtain 36.8 Gram of 2,2-bis[3-amino-4-(4-aminophenoxy)phenyl]hexafluoropropane crystal, the purity is 99.0%, according to the actual obtained 2,2-bis[3-amino-4- The amount of (4-aminophenoxy)phenyl]hexafluoropropane and the theoretical amount (54.8 grams) were calculated to give 2,2-bis[3-amino-4-(4-aminophenoxy...

Embodiment 3

[0031] 60.8 grams (0.1 moles) of 2,2-bis[3-amino-4-(4-nitrophenoxy group) phenyl] hexafluoropropane, 4.0 grams of palladium mass percentage is 5% palladium / carbon and 1500ml 2 -Add methoxyethanol into 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 130.0 g (solution weight). After the dropwise addition of hydrazine hydrate is completed, continue to stir and react for 4 hours at a temperature range of 70°C to 85°C, cool slightly, filter while hot, cool the mother liquor, add an appropriate amount of pure water dropwise, precipitate a crystalline product, filter, and vacuum dry to obtain 51.3 Gram of 2,2-bis[3-amino-4-(4-aminophenoxy)phenyl]hexafluoropropane crystal, the purity is 99.7%, according to the actual obtained 2,2-bis[3-amino-4- The amount of (4-aminophenoxy)phenyl]hexafluoropropane and the theoretical amount (54.8 grams) were calculated to give 2,2-bis[3-amino-4-(4-aminophen...

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Abstract

The invention relates to a preparation method of 2,2-double(3-amino-4-(4-amino phenoxy)phenyl)hexafluoropropane, comprising the steps as following, after being put into a 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(3-amino-4-(4-nitro 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(3-amino-4-(4-amino phenoxy)phenyl)hexafluoropropane are gained. The preparation 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[3-amino-4-(4-aminophenoxy)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[3-amino-4-(4-aminophenoxy)phenyl]hexafluoropropane is one of...

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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