Phenolic aldehyde modified amine curing agent and preparation method thereof

A phenolic modified amine and curing agent technology, applied in the direction of adhesives, adhesive types, epoxy resin glue, etc., can solve the problems of high brittleness of cured products, poor curing effect, high toxicity, etc., achieve low curing temperature, The cured product has good performance and is easy to operate

Inactive Publication Date: 2013-05-22
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyamine curing agent occupies a large proportion in the curing system of epoxy resin, but the unmodified polyamine curing agent itself has some disadvantages, such as high toxicity, volatile, and easy absorption of CO during operation. 2 , The cured product is brittle, and the curing effect is not good in the environment with water, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a constant temperature water bath at about 40°C, add 33g of nonylphenol, 14.1g of phenol, and 16.2g of m-cresol into a 250ml three-necked flask equipped with a stirrer and a condenser, mix them, keep warm at about 40°C, and add hexyl 31.3g of diamine, 39.5g of triethylenetetramine, stirred at constant temperature for 5 minutes, started to heat up, and added paraformaldehyde (13.5g in total), added in batches for several times (when the temperature rose from 40°C to 50°C, added more 40% of the total mass of paraformaldehyde, add 30% of the total amount of paraformaldehyde when the temperature rises from 50°C to 60°C, add 20% of the total amount of paraformaldehyde when the temperature rises from 50°C to 70°C, and add 20% of the total amount of paraformaldehyde when the temperature rises from 50°C to 80°C Add 10% of the total amount of paraformaldehyde), heat up to 80°C, and keep warm for 2 hours. Cool to room temperature to obtain a light yellow viscous liquid with an...

Embodiment 2

[0021] In a constant temperature oil-water bath at around 40°C, add 44g of nonylphenol, 18.8g of phenol, and 10.8g of m-cresol to a 250ml three-necked flask equipped with a stirrer and a condenser, keep the temperature at about 40°C, and add hexyl 55.7g of diamine, 46.7g of triethylenetetramine, stirred at constant temperature for 5 minutes, began to heat up, and added paraformaldehyde (15g in total), added in batches for several times (when the temperature rose from 40°C to 50°C, add paraformaldehyde 40% of the total mass of formaldehyde, add 25% of the total amount of paraformaldehyde when the temperature rises from 50°C to 60°C, add 25% of the total amount of paraformaldehyde when the temperature rises from 50°C to 70°C, add 10% of the total amount of paraformaldehyde), after heating up to 80°C, keep it warm for 2.5 hours. Cool to room temperature to obtain a light yellow viscous liquid with an amine value of 485mgKOH / g and a viscosity of 360mPa. s. E-44 epoxy resin is us...

Embodiment 3

[0023] Add 19.3g of nonylphenol, 16.5g of phenol, and 9.5g of m-cresol to a 250ml three-neck flask equipped with a stirrer and a condenser in a constant temperature oil-water bath at about 40°C. Hexamethylenediamine 30.9g, triethylenetetramine 77.9g, stirred at constant temperature for 5 minutes, started to heat up, and added paraformaldehyde (a total of 15g), added in batches for many times (when the temperature rose from 40°C to 50°C, add more 45% of the total mass of paraformaldehyde, add 30% of the total amount of paraformaldehyde when the temperature rises from 50°C to 60°C, add 15% of the total amount of paraformaldehyde when the temperature rises from 50°C to 70°C, and add 15% of the total amount of paraformaldehyde when the temperature rises from 50°C to 80°C Add 10% of the total amount of paraformaldehyde), heat up to 80°C, and keep warm for 3 hours. Cool to room temperature to obtain a light yellow viscous liquid, the amine value is 480mg KOH / g, and the viscosity is ...

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Abstract

The invention discloses a phenolic aldehyde modified amine curing agent which is prepared by polycondensing mixed phenol, polyformaldehyde and mixed amine through Mannich reaction. The preparation method comprises the following steps: adding phenol, nonylphenol and m-cresol at 35-45 DEG C, and evenly mixing; sequentially adding hexamethylene diamine and triethylene tetramine, and adding polyformaldehyde for reaction in batches in the process of gradually heating to 70-80 DEG C; and after the addition of the polyformaldehyde is finished, further reacting at 70-80 DEG C to obtain the product after the reaction is finished. The curing agent can be directly cured in water, has certain toughness and is favorable in curing effect; an epoxy resin cured by the curing agent has high dry shear bonding strength and in-water cured shear bonding strength; and the preparation method of the curing agent is simple to operate and mild in reaction conditions, and industrial production can be realized.

Description

technical field [0001] The invention relates to a phenolic modified amine curing agent and a preparation method thereof, belonging to the technical field of curing agents. Background technique [0002] Epoxy resin adhesives have the advantages of high adhesion, small curing shrinkage, and good corrosion resistance. Therefore, they have been widely used in the fields of building bridges, electronic appliances, restoration of cultural relics, waterproof plugging, and underwater engineering. The curing system of epoxy resin mainly includes polyamine and acid anhydride. Polyamine curing agent occupies a large proportion in the curing system of epoxy resin, but the unmodified polyamine curing agent itself has some disadvantages, such as high toxicity, volatile, and easy absorption of CO during operation. 2 , The cured product is brittle, and the curing effect is not good in the environment with water. The quality of the curing agent determines the curing performance of the epox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/073C08G59/62C09J163/02
Inventor 谢建军丁出曾念姚庆鑫刘军霞
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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