Method for preparing fluorine-contained multi-function epoxy resin

An epoxy resin, multi-functional technology, applied in the field of preparation of fluorine-containing multi-functional epoxy resin, to achieve the effects of environmental friendliness, good product quality, and easy recovery of solvents

Inactive Publication Date: 2007-08-29
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Preparation of N,N,N',N',O,O'-hexaglycidyl-2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3- Hexafluoropropane (HGBAHPFP) has not been reported publicly

Method used

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  • Method for preparing fluorine-contained multi-function epoxy resin
  • Method for preparing fluorine-contained multi-function epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 36.6 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane (BAHPFP), 55.5 grams (0.6 moles) of cyclo Add oxychloropropane (ECH), 1.8 ml of water and 18 ml of methyl isobutyl ketone (MIBK) into the reaction flask, stir and react at 40°C for 1 hour, heat up, react at 60°C for 1 hour, and then increase the reaction temperature Temperature, react at 80°C for 7 hours, and react at 90°C for 0.5 hours, cool the reaction solution to below 70°C, and add a 50% trimethyl (2-chloroethyl) ammonium chloride phase transfer catalyst aqueous solution at one time 6.0 g, stir quickly, add dropwise 80 g (0.8 moles) of 40% aqueous sodium hydroxide solution, after dropping within 1 hour, react at 50°C for 2 hours, heat up to 80°C and continue the reaction for 2 hours, add 100 ml of water and 150 milliliters of methyl isobutyl ketone (MIBK), after stirring evenly, leave standstill, liquid separation, remove water phase, stay and get organic phase mother liquor, w...

Embodiment 2

[0029] 36.6 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane (BAHPFP), 185.0 grams (2.0 moles) of cyclo Add oxychloropropane (ECH), 3.6 ml of water and 18 ml of methyl isobutyl ketone (MIBK) into the reaction flask, stir and react at 40°C for 1 hour, heat up, react at 60°C for 5 hours, and then increase the reaction temperature temperature, after reacting for 2 hours at 90°C, cool the reaction solution to below 70°C, add 6.0 grams of trimethyl (2-chloroethyl) ammonium chloride phase transfer catalyst aqueous solution with a concentration of 50%, stir rapidly, and drop Add 100 grams (1.0 moles) of 40% sodium hydroxide aqueous solution, after dripping within 1 hour, react at 50°C for 2 hours, heat up to 80°C for 1 hour, continue to react at 90°C for 1 hour, add 100 ml of water and 150 milliliters of methyl isobutyl ketone (MIBK), after stirring evenly, leave standstill, liquid separation, remove water phase, stay and get organic phase mother li...

Embodiment 3

[0031]36.6 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane (BAHPFP), 185.0 grams (2.0 moles) of cyclo Add oxychloropropane (ECH), 3.6 ml of water and 18 ml of toluene into the reaction flask, stir and react at 40°C for 1 hour, heat up, react at 60°C for 4 hours, then increase the reaction temperature, and react at 90°C for 1 hour Afterwards, cooling reaction solution to below 70 ℃, one-time addition concentration is 6.0 grams of trimethyl (2-chloroethyl) ammonium bromide phase-transfer catalyst aqueous solution of 50%, stir rapidly, drip 120 grams (1.2 mole) 40 % concentration of sodium hydroxide aqueous solution, after dripping within 1 hour, react at 50°C for 2 hours, heat up to 80°C for 1 hour, continue to react at 90°C for 1 hour, add 100 ml of water and 300 ml of toluene, and stir evenly , stand still, separate liquid, remove water phase, retain organic phase mother liquid, wash with water, stand still, separate liquid, organic mother l...

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Abstract

The invention discloses a manufacture method for multi-functional epoxy resin containing fluorine that includes the following steps: 2, 2-double (3- amino group-4 - hydroxy benzenes)-1, 1, 1, 3, 3, 3-BAHPFP and ECH reacting for 3-12 hours at 40-90 degree centigrade in water and organic solvent; cooling to 70 degree centigrade, adding PTC solution and alkali material solution, reacting for 2-10 hours at 40-70 degree centigrade, heating to 1-5 hours at 80-90 degree centigrade, adding wate and organic solvent, whisking and laying to gain organic layer, washing, separating to gain N, N, N', N', 0, 0'- hexa-glycidyl group- 2, 2- double (3- amino group-4- hydroxy benzenes)- 1, 1, 1, 3, 3, 3-HGBAHPFP. The invention has the advantages of easy to operate, good quality, high yield, little waste, etc.

Description

technical field [0001] The invention belongs to the field of organic chemical epoxy resin preparation, in particular to a preparation method of fluorine-containing multifunctional epoxy resin. Background technique [0002] Multifunctional epoxy resin is an important raw material for the preparation of high temperature resistant adhesives, fiber reinforced prepregs, packaging materials for electronic components, high temperature resistant electrical insulating paints and coatings. [0003] The molecular structure of multifunctional epoxy resin contains multiple epoxy groups, which can chemically react with various active groups such as amino, hydroxyl, and carboxyl groups. Therefore, it can co-exist with compounds or polymers containing the above active groups. Polymerization to cure and crosslink. [0004] Multi-functional epoxy resin, such as CIBA-GEIGY's MY720, has the following molecular structure: [0005] [0006] Its resin system with aromatic diamine curing agent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/20
Inventor 虞鑫海徐永芬赵炯心
Owner DONGHUA UNIV
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