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Synthesis method for low-viscosity high-temperature-resistant modified epoxy resin

An epoxy resin and a synthesis method technology, applied in the field of polymer materials and composite materials, can solve the problems of low reaction rate, reduced catalyst activity, low catalytic efficiency, etc., and achieve the effects of low viscosity and cost reduction.

Active Publication Date: 2013-10-09
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent CN102666635A has the following disadvantages: First, the polymer-supported basic catalyst is chemically bonded to the insoluble polymer through a trivalent organic phosphorus compound and / or amine compound, or the monomer is polymerized after the basic catalyst is introduced into the monomer , and then obtained by three-dimensional cross-linking with cross-linking monomers such as divinylbenzene, so the reaction rate is lower than that of directly adding catalyst in the reaction system, and the catalytic efficiency is low; the second is to inject air into the reaction system during the reaction process Keep the oxygen concentration in the reaction system and the gas phase on the reaction system to prevent resin gelation. At the same time, due to the oxidation of the catalyst, the catalyst activity is reduced, and the reaction rate is further reduced; the third is that no polymerization inhibitor is added to the resin reaction system, which affects its performance. Resin stability during reaction and storage

Method used

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  • Synthesis method for low-viscosity high-temperature-resistant modified epoxy resin
  • Synthesis method for low-viscosity high-temperature-resistant modified epoxy resin
  • Synthesis method for low-viscosity high-temperature-resistant modified epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 200g of 4,4'-diaminodiphenylmethane epoxy resin into a 500ml three-necked flask equipped with a thermometer, stirrer, nitrogen inlet tube and condenser, gradually heat and stir; when the temperature rises to 80°C, start to add acrylic acid dropwise 49g, and add 2g of tetramethylammonium chloride, 1g of chromium triacetylacetonate, 1g of methyl hydroquinone, and 1g of p-hydroxyanisole, control the reaction temperature between 80 and 120°C, and measure the acid concentration every hour value until the acid value drops below 15mgKOH / g as the end of the reaction. Cool the reaction product, add 67g of trimethylolpropane triacrylate, control the temperature below 60-80°C and stir evenly to obtain a high-temperature-resistant modified epoxy resin.

Embodiment 2

[0028] Put 200g of 4,4'-diaminodiphenylmethane epoxy resin into a 500ml three-necked flask equipped with a thermometer, stirrer, nitrogen inlet tube and condenser, gradually heat and stir; when the temperature rises to 80°C, start to add acrylic acid dropwise 74g, and added benzyltriethylammonium chloride 2g, chromium salicylate 1g, hydroquinone 1g, 1-oxygen-2,2,6,6-tetramethylpiperidin-4-alcohol (TEMPOL ) 1g, control the reaction temperature between 80-120°C, measure the acid value every hour, until the acid value drops below 15mgKOH / g as the end point of the reaction. Cool the reaction product, add 126g of diallyl phthalate, control the temperature below 60-80°C and stir evenly to obtain a high-temperature-resistant modified epoxy resin.

Embodiment 3

[0030] Put 200g of p-aminophenol epoxy resin into a 500ml three-necked flask equipped with a thermometer, stirrer, nitrogen inlet tube and condenser, gradually heat and stir; when the temperature rises to 80°C, start to drop 44g of methacrylic acid, and add benzyl Trimethylammonium chloride 2g, chromium triacetylacetonate 2g, trimethylhydroquinone 1g, 1-oxyl-2,2,6,6-tetramethylpiperidin-4-ol (TEMPOL) 1g, control The reaction temperature is between 80°C and 120°C, and the acid value is measured every hour until the acid value drops below 15mgKOH / g, which is the end point of the reaction. Cool the reaction product, add 42g of triallyl isocyanurate, control the temperature below 60-80°C and stir evenly to obtain a high-temperature-resistant modified epoxy resin.

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Abstract

The invention relates to a synthesis method for low-viscosity high-temperature-resistant modified high-performance epoxy resin. The method comprises the following steps: (1) adding multifunctional epoxy resin into a three-neck flask provided with a thermometer, a stirrer, a nitrogen lead-in pipe and a condenser and gradually heating and stirring; (2) when the temperature is raised to 80 DEG C, dropwise adding unsaturated monocarboxylic acid, adding a catalyst and a polymerization inhibitor, controlling the reaction temperature to be 80-120 DEG C and performing a partial polymerization reaction; (3) measuring the acid value every one hour and reaching a reaction endpoint until the acid value is reduced to 15 mgKOH / g; and (4) cooling a reaction product and adding a cross-linking agent, and controlling the temperature to be 60-80 DEG C and uniformly stirring to obtain the low-viscosity high-temperature-resistant modified epoxy resin. Compared with the multifunctional epoxy resin system, the modified epoxy resin system has the advantages of low viscosity, high activity, high temperature resistance, low cost and the like, is suitable for a resin transfer molding process and is mainly used as matrix resin of an advanced composite material.

Description

technical field [0001] The invention relates to a synthesis method of a low-viscosity high-temperature-resistant modified high-performance epoxy resin, which belongs to the field of polymer materials and composite materials. Background technique [0002] Epoxy resin has good comprehensive mechanical properties, low shrinkage, good stability, and excellent electrical insulation properties. It is used as a matrix resin for coatings, adhesives, and composite materials, and electronic packaging materials, etc. and other fields have been widely used. [0003] After curing, multifunctional epoxy resin has high crosslinking density, large internal stress, high brittleness, low temperature resistance, poor impact toughness, and poor fatigue resistance, which limit epoxy resin as a structural material and the main matrix resin for advanced composite materials. Applications in high-end fields such as aerospace, power electronics, transportation, and adhesives. [0004] Generally, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/16C08G59/17
Inventor 钱建华刘坐镇郭卫红黄锐
Owner EAST CHINA UNIV OF SCI & TECH
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