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Preparation of aliphatic alcohol polyether type aqueous amine epoxy hardener

A technology of epoxy curing agent and fatty alcohol polyether, which is applied in the field of epoxy resin curing agent, can solve the problems of complex preparation method and inability to obtain zero VOC, and achieve the effect of simple preparation method, good flexibility and pollution reduction

Inactive Publication Date: 2011-05-11
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the shortcomings of complex preparation methods of epoxy-amine water-based epoxy curing agents in the prior art and the inability to obtain zero VOC, the invention provides a method for preparing fatty alcohol polyether-type water-based amine epoxy curing agents. It has the advantages of zero VOC, simple preparation process, good curing performance and easy dilution with water

Method used

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  • Preparation of aliphatic alcohol polyether type aqueous amine epoxy hardener
  • Preparation of aliphatic alcohol polyether type aqueous amine epoxy hardener
  • Preparation of aliphatic alcohol polyether type aqueous amine epoxy hardener

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The first step, the preparation of maleic acid monoester

[0034]In a 500ml three-neck flask equipped with a heating mantle, a stirring device, and a thermometer, add 1mol of fatty alcohol polyoxyethylene ether (AEO-4), 1.05mol of maleic anhydride and 0.5% of maleic anhydride quality p-toluenesulfonate The acid is used as a catalyst, and then nitrogen gas is passed through, the temperature is raised to 80°C, and the reaction is stirred at a speed of 300 rpm until the esterification rate > 99%, and maleic acid monoester is obtained.

[0035] The second step, the preparation of monoepoxy maleic acid diester

[0036] In a 500ml three-neck flask equipped with a heating mantle, a stirring device, and a thermometer, add 1.02mol ethylene glycol diglycidyl ether, and the total mass of ethylene glycol diglycidyl ether is 3‰ triethylbenzyl ammonium chloride as a catalyst, usually Nitrogen, after raising the temperature to 120°C, slowly add 1 mol of maleic acid monoester dropwise...

Embodiment 2

[0041] The first step, the preparation of phthalic acid monoester

[0042] In a 500ml three-necked flask equipped with a heating mantle, a stirring device, and a thermometer, add 1 mol of fatty alcohol polyoxyethylene ether (AEO-5), 1.05 mol of phthalic anhydride and 3% sulfuric acid of phthalic anhydride mass as a catalyst , then feed nitrogen, heat up to 90°C, and stir the reaction at a speed of 300 rpm until the esterification rate > 99%, to obtain phthalic acid monoester;

[0043] The second step, the preparation of single epoxy phthalate diester

[0044] In a 500ml three-neck flask equipped with a heating mantle, a stirring device, and a thermometer, add 1.05mol ethylene glycol diglycidyl ether, and 3% triethylamine of the total mass of the epoxy resin as a catalyst, nitrogen gas, and heat up to 100°C Afterwards, slowly add 1 mol of phthalic acid monoester dropwise, and stir at 300 rpm until the acid value is less than 2 to obtain monoepoxy phthalic acid diester.

[004...

Embodiment 3

[0049] The first step, the preparation of methyl tetrahydrophthalic acid monoester

[0050] In a 500ml three-necked flask equipped with a heating mantle, a stirring device, and a thermometer, add 1 mol of fatty alcohol polyoxyethylene ether (AEO-6), 1.05 mol of methyltetrahydrophthalic anhydride and methyltetrahydrophthalic anhydride Sulfuric acid with an acid anhydride mass of 2% is used as a catalyst, then nitrogen is introduced, the temperature is raised to 100° C., and the reaction is stirred at a speed of 300 rpm until the esterification rate > 99%, and methyl tetrahydrophthalic acid monoester is obtained.

[0051] The second step, the preparation of methyl tetrahydrophthalate diester

[0052] In a 500ml three-neck flask equipped with a heating mantle, a stirring device, and a thermometer, add 1.06mol ethylene glycol diglycidyl ether, and 4‰ benzyltrimethylammonium chloride of the total mass of the epoxy resin as a catalyst, pass nitrogen, and heat up After reaching 90°C...

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Abstract

The invention discloses a preparation method for an aliphatic alcohol polyether type water-based amine epoxy hardener. The method comprises the following steps of: 1, carrying out the etherification reaction of acid anhydride and an aliphatic alcohol polyethenoxy ether under the catalysis of an acidic catalyst in the nitrogen atmosphere at a temperature of between 70 and 140 DEG C to obtain an acid anhydride monoester; 2, stirring and reacting an epoxy resin and the acid anhydride monoester under the catalysis of the catalyst till an acid number is less than 2 to obtain a single-epoxy acid anhydride diester; 3, stirring and reacting the single-epoxy acid anhydride diester and polybasic amine under the existence of a solvent at a temperature of between 50 and 120 DEG C till an epoxy value is less than 0.002, and then applying a negative pressure to distill off the solvent and excess polybasic amine to obtain the aliphatic alcohol polyether type water-based amine epoxy hardener. A polyether chain segment is introduced into the hardener molecule to improve the hydrophobicity and flexibility of the hardener. Simultaneously, the introduction of the epoxy resin improves the compatibility of the hardener with the epoxy resin. The aliphatic alcohol polyether type water-based amine epoxy hardener has the advantages of zero VOC, simple preparation process, excellent solidification performance and easy dilution by water.

Description

technical field [0001] The invention belongs to the field of epoxy resin curing agents, and in particular relates to a preparation method of fatty alcohol polyether type water-based amine epoxy curing agents. Background technique [0002] Epoxy resin coatings have excellent physical and chemical properties and are widely used in machinery, electrical, electronic, aviation, aerospace, chemical, transportation, construction and other fields. However, because most of the traditional epoxy resin coatings are solvent-based systems, a large amount of organic solvents will be volatilized during production and construction, which seriously endangers the health of production and construction personnel. On the basis of retaining the excellent adhesion, thermal stability, chemical resistance, insulation and other characteristics of the traditional solvent-based epoxy system, the water-based epoxy coating system uses water as the dispersion medium and contains no or only a small amount ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C08L63/00
Inventor 夏建陵李梅黄坤丁海洋
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY