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Dimeric fatty acid-diglycidol ester modified amine hardener, preparation method and application

A technology of diglycidyl ester and dimer fatty acid, which is applied in the field of dimer fatty acid diglycidyl ester modified amine curing agent and its preparation, can solve the problems of poor toughening effect and insufficient impact resistance, and achieve stable operation and responsive The effect of short time and short alkali addition time

Inactive Publication Date: 2018-01-12
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the purposes of the present invention is to provide a dimer fatty acid diglycidyl ester modified amine curing agent in order to solve the above-mentioned technical problems of insufficient impact resistance and poor toughening effect

Method used

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  • Dimeric fatty acid-diglycidol ester modified amine hardener, preparation method and application
  • Dimeric fatty acid-diglycidol ester modified amine hardener, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A dimer fatty acid diglycidyl ester modified amine curing agent is prepared by a method comprising the following steps:

[0044] (1), esterification reaction

[0045] First add 112.00g of dimer fatty acid and 92.52g of epichlorohydrin into a four-neck flask equipped with stirring, nitrogen protection, thermometer and condenser, heat to 50°C and stir evenly, then add 2.24g of catalyst, stir for 10min and heat up to 100°C The esterification reaction was carried out at ℃ for 2.0h, and the obtained reaction solution 1 was the chlorohydrin ester intermediate;

[0046] The amount of the above-mentioned dimerized fatty acid and epichlorohydrin is calculated by molar ratio, dimerized fatty acid: epichlorohydrin is 1:5;

[0047] The catalyst is a quaternary phosphine salt, and the quaternary phosphine salt is tetrabutylphosphine chloride;

[0048] The consumption of catalyst is 2% of dimer fatty acid quality;

[0049] It has been determined that the acid value of the chlorohy...

Embodiment 2

[0070] A dimer fatty acid diglycidyl ester modified amine curing agent is prepared by a method comprising the following steps:

[0071] (1), esterification reaction

[0072] First, add 112.00g of dimer fatty acid and 129.53g of epichlorohydrin into a four-necked flask equipped with stirring, nitrogen protection, thermometer and condenser, heat to 50°C and stir evenly, then add 4.48g of catalyst, stir for 10 minutes and heat up to 80°C The esterification reaction was carried out at ℃ for 3.0 hours, and the obtained reaction solution 1 was the chlorohydrin ester intermediate;

[0073] The amount of the above-mentioned dimerized fatty acid and epichlorohydrin is calculated by molar ratio, dimerized fatty acid: epichlorohydrin is 1:7;

[0074] Described catalyst is tertiary amine, and described tertiary amine is triethylamine;

[0075] The consumption of catalyzer is 4% of dimer fatty acid quality;

[0076] It has been determined that the acid value of the chlorohydrin ester in...

Embodiment 3

[0092] A dimer fatty acid diglycidyl ester modified amine curing agent is prepared by a method comprising the following steps:

[0093] (1), esterification reaction

[0094] First add 112.00g of dimer fatty acid and 166.54g of epichlorohydrin into a four-necked flask equipped with stirring, nitrogen protection, thermometer and condenser, heat to 50°C and stir evenly, then add 1.12g of catalyst, stir for 10 minutes and heat up to 110°C °C for 1.5 hours of esterification reaction, the resulting reaction solution 1 is the chlorohydrin ester intermediate;

[0095] The amount of the above-mentioned dimerized fatty acid and epichlorohydrin is calculated by molar ratio, dimerized fatty acid: epichlorohydrin is 1:9;

[0096] The catalyst is a quaternary phosphonium salt, and the quaternary phosphonium salt is tetrabutylphosphine bromide;

[0097] The consumption of catalyst is 1% of dimerized fatty acid quality;

[0098] It has been determined that the acid value of the chlorohydri...

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Abstract

The invention discloses a dimeric fatty acid-diglycidol ester modified amine hardener, a preparation method and an application. The preparation method comprises the steps: firstly, subjecting dimericfatty acid and epichlorohydrin to an esterification reaction for 1.5 to 3.0 hours in the presence of a catalyst while controlling a temperature to 80 DEG C to 110 DEG C, so as to obtain a chlorohydrinester intermediate; then, subjecting the chlorohydrin ester intermediate and a sodium hydroxide aqueous solution with the mass percent concentration of 20% to 50% for 2 to 5 hours at the temperatureof 40 DEG C to 85 DEG C, so as to obtain a dimeric fatty acid-diglycidol ester; and finally, subjecting the dimeric fatty acid-diglycidol ester and diethylenetriamine to an amination reaction for 1 to4 hours at the temperature of 60 DEG C to 75 DEG C, thereby obtaining the dimeric fatty acid-diglycidol ester modified amine hardener. The obtained dimeric fatty acid-diglycidol ester modified aminehardener has a relatively high amine number and has excellent toughening performance to the hardening of epoxy resin. The preparation process is simple, and the operation is convenient, so that the preparation method is applicable to large-scale industrial production.

Description

technical field [0001] The invention relates to a dimer fatty acid diglycidyl ester modified amine curing agent and a preparation method thereof, in particular to a dimer fatty acid diglycidyl ester modified amine curing agent and a preparation method for curing epoxy resins. Background technique [0002] Epoxy resin has many unique and excellent properties. It has a wide range of uses and develops very rapidly. It has been widely used in the manufacturing fields of coatings, electrical insulation materials, adhesives, and composite materials. It plays an irreplaceable role in many industrial fields. effect. [0003] Epoxy resin itself cannot be used alone, and it needs to be added with a curing agent to be useful. However, the high cross-linking density and large internal stress of epoxy resin cured products lead to its disadvantages such as low toughness, high brittleness, poor fatigue resistance and impact resistance, which to a certain extent limit the compounding of ep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/26C07C69/608C07D301/26C07D303/16C07C213/04C07C219/10C08G59/50
Inventor 吴蓁童伟何辛高晟弢杨志星周心怡赵亮
Owner SHANGHAI INST OF TECH
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