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Phenolic aldehyde modified polyether amine type epoxy resin curing agent and preparation method thereof

An epoxy resin curing and phenolic modification technology, which is applied in the field of epoxy resin preparation, can solve the problems of unsatisfactory high temperature performance and achieve excellent bonding performance and mechanical properties, low volatility, and moderate curing speed.

Pending Publication Date: 2020-04-17
WUXI ACRYL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its cured epoxy resin is not very ideal in terms of high temperature performance, and the Mannich modified product introduces phenolic hydroxyl and amine active hydrogen, which strengthens the reactivity and improves the amine and epoxy groups. Excellent curing speed, and the phenolic skeleton structure can further increase the heat distortion temperature and improve the heat resistance and corrosion resistance of the cured resin itself

Method used

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  • Phenolic aldehyde modified polyether amine type epoxy resin curing agent and preparation method thereof
  • Phenolic aldehyde modified polyether amine type epoxy resin curing agent and preparation method thereof
  • Phenolic aldehyde modified polyether amine type epoxy resin curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) In a 500mL three-necked flask equipped with a stirrer, reflux condenser, thermometer and dripping device, according to n (amine): n (aldehyde): n (phenol) = 0.75mol: 0.75mol: 0.25mol, add 111.0g of polyetheramine EDR-148 and 23.5g of phenol were stirred while raising the temperature, and the stirring speed was 100-200 rpm.

[0023] (2) When the temperature rose to 75-85° C., 75.1 g of 30% formaldehyde solution was added dropwise at a rate of 1 drop / second, and the reaction was refluxed at 95-105° C. for 4 hours.

[0024] (3) Then the reaction kettle is connected to a vacuum distillation device, vacuum dehydration is carried out, and the distillation is stopped until the liquid phase temperature is 120° C. to obtain the product.

[0025] Performance test: The obtained modified amine curing agent is used in conjunction with bisphenol A epoxy resin (E-51) to form an adhesive, and its bonding performance is studied by measuring the shear strength and peel strength. The...

Embodiment 2

[0029] (1) In a 500mL three-necked flask equipped with a stirrer, reflux condenser, thermometer and dripping device, according to n (amine): n (aldehyde): n (phenol) = 0.75mol: 0.75mol: 0.25mol, add 132.0g of polyetheramine EDR-176 and 23.5g of phenol were stirred while raising the temperature, and the stirring speed was 100-200 rpm.

[0030] (2) When the temperature rose to 75-85° C., 75.1 g of 30% formaldehyde solution was added dropwise at a rate of 1 drop / second, and the reaction was refluxed at 95-105° C. for 4 hours.

[0031] (3) Then the reaction kettle is connected to a vacuum distillation device, vacuum dehydration is carried out, and the distillation is stopped until the liquid phase temperature is 120° C. to obtain the product.

[0032] Performance test: The modified amine curing agent obtained above was used in conjunction with bisphenol A epoxy resin (E-51) to form an adhesive, and its bonding performance was studied by measuring the shear strength and peel streng...

Embodiment 3

[0036] (1) In a 500mL three-necked flask equipped with a stirrer, reflux condenser, thermometer and dripping device, according to n (amine): n (aldehyde): n (phenol) = 0.75mol: 0.75mol: 0.25mol, add 144.0g of polyetheramine EDR-192 and 23.5g of phenol were stirred while raising the temperature, and the stirring speed was 100-200 rpm.

[0037] (2) When the temperature rose to 75-85° C., 75.1 g of 30% formaldehyde solution was added dropwise at a rate of 1 drop / second, and the reaction was refluxed at 95-105° C. for 4 hours.

[0038] (3) Then the reaction kettle is connected to a vacuum distillation device, vacuum dehydration is carried out, and the distillation is stopped until the liquid phase temperature is 120° C. to obtain the product.

[0039] Performance test: The modified amine curing agent obtained above was used in conjunction with bisphenol A epoxy resin (E-51) to form an adhesive, and its bonding performance was studied by measuring the shear strength and peel streng...

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Abstract

The invention relates to a phenolic aldehyde modified polyether amine type epoxy resin curing agent and a preparation method thereof, and belongs to the technical field of epoxy resin preparation. Thepreparation method comprises the steps: adding polyether amine and phenols into a reaction kettle, and stirring while heating; gradually dropwise adding an aldehyde aqueous solution when the temperature rises to a certain degree, and carrying out reflux reaction after dropwise adding is finished; and then carrying out vacuum dehydration, connecting the reaction kettle to a vacuum distillation device for distillation, and distilling to obtain the polyether amine type epoxy resin curing agent. The prepared phenolic aldehyde modified polyether amine is used as an epoxy resin curing agent, and anepoxy resin adhesive system obtained by compounding has excellent bonding performance and mechanical properties. In the aspect of mechanism, phenolic hydroxyl and amine active hydrogen are introducedinto the modifier, so that the reaction activity is enhanced to a great extent, the curing speed of amino and epoxy groups is increased, and the heat resistance and the corrosion resistance are improved.

Description

technical field [0001] The invention relates to a phenolic modified polyetheramine type epoxy resin curing agent and a preparation method thereof, belonging to the technical field of epoxy resin preparation. Background technique [0002] With the rapid development of science and technology, as a new type of chemical material, epoxy resin adhesives are playing an increasingly important role in different fields. Epoxy resin has the advantages of high bonding strength, low shrinkage, easy to obtain raw materials, simple synthesis process, wide service temperature, wide application range, stable size, strong creep resistance, chemical resistance, excellent electrical insulation, etc. It has been widely used in aerospace, civil engineering, electronic appliances, automobile machinery, light industry and other fields. [0003] Curing agents are indispensable and important components for epoxy resin adhesives. Because the uncured epoxy resin is a thermoplastic oligomer, it will n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/36C08G59/62
CPCC08G8/36C08G59/62
Inventor 张松林朱鹏飞潘萍张文泉
Owner WUXI ACRYL TECH
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