Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Super-toughened glycidol ester modified amine hardener and preparation method thereof

A technology of glycidyl ester and curing agent, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc. Effects of toughness and impact strength, low chlorine content, high epoxy value

Active Publication Date: 2017-11-28
SHANGHAI RESIN FACTORY
View PDF0 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there are epoxy resin curing agents with toughening effect on the market, such as glycidyl ether modified amine curing agent 593, polyether amine D230, etc., but the former 593 curing agent will show insufficient toughness, moisture absorption and other properties and bonding strength Poor, severe heat release, external force or thermal shock and easy to crack, etc. The thermal oxidation stability of the polyether in the latter polyetheramine is not good, and the polyether is easy to break the chain under the action of oxidation, forming low-molecular carbonyl and carbonyl compound
[0007] So far, there is no glycidyl ester modified amine curing agent for conventional epoxy resin curing such as E51 on the market, and there is no glycidyl ester modified amine curing agent with toughening effect

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Super-toughened glycidol ester modified amine hardener and preparation method thereof
  • Super-toughened glycidol ester modified amine hardener and preparation method thereof
  • Super-toughened glycidol ester modified amine hardener and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Heat 112.80g (0.40mol) oleic acid and 110.02g (1.19mol) epichlorohydrin to 50°C in a reactor with stirring, nitrogen protection, and condenser, and add 2.26g of catalyst tetrabutyl chloride Phosphine was reacted at 100°C for 2 hours to obtain the chlorohydrin ester intermediate, and the acid value of the chlorohydrin ester intermediate was measured to be 0.47 mgNaOH / g;

[0041] (2) Cool down to 85°C, add dropwise 112.00g of NaOH solution with a weight concentration of 20% (calculated as NaOH, 0.56mol), drop it for 2.1h, and then react at 85°C for 2h;

[0042] (3) After the cyclization is completed, add 225.60 g of toluene to extract 3 times, each time the amount is 1 / 3 of the total mass of toluene, combine the extracts of each batch, and then wash and neutralize the extracts at room temperature, Wash until the aqueous phase pH=7. Oil and water are separated, and the oil phase is gradually heated from room temperature to 140°C to remove under reduced pressure when t...

Embodiment 2

[0048] (1) Heat 112.80g (0.40mol) of oleic acid and 185.04g (2.00mol) of epichlorohydrin in a reactor with stirring, nitrogen protection, and condenser to 50°C and stir evenly, then add 4.51g of triethylamine After stirring for 10 minutes, the temperature was raised to 80° C., and the temperature was kept at 80° C. for 3 hours to obtain the chlorohydrin ester intermediate. The acid value of the chlorohydrin ester intermediate was measured to be 0.53 mgNaOH / g.

[0049](2) The temperature was lowered to 55° C., and 106.67 g (calculated as NaOH, 0.80 mol) of NaOH solution with a weight concentration of 30% was added dropwise to make it drop within 2.0 hours. After the dropwise addition, the constant temperature reaction was continued at 55° C. for 4 h.

[0050] (3) After the cyclization is completed, add 225.60 g of toluene to extract 3 times, each time the amount is 1 / 3 of the total mass of toluene, combine the extracts of each batch, and then wash and neutralize the extracts at...

Embodiment 3

[0054] (1) Heat 112.80g (0.40mol) of oleic acid and 259.06g (2.80mol) of epichlorohydrin in a reactor with stirring, nitrogen protection, and condenser to 50°C and stir evenly, then add 1.13g of tetrabutyl Phosphine bromide, after stirring for 10 minutes, the temperature was raised to 110 °C, and the temperature was kept at 110 °C for 1.5 hours to obtain the chlorohydrin ester intermediate, and the acid value of the chlorohydrin ester intermediate was measured to be 0.37 mgNaOH / g;

[0055] (2) Cool down to 70°C, add 44.00 g of 40% NaOH solution (calculated as NaOH, 0.44 mol) dropwise, and drop it within 0.8 h. After the dropwise addition, the constant temperature reaction was continued at 70° C. for 3 h;

[0056] (3) After the cyclization is completed, add 225.60 g of toluene to extract 3 times, each time the amount is 1 / 3 of the total mass of toluene, combine the extracts of each batch, and then wash and neutralize the extracts at room temperature, Wash until the aqueous pha...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Amine valueaaaaaaaaaa
Impact strengthaaaaaaaaaa
Amine valueaaaaaaaaaa
Login to View More

Abstract

The invention discloses a super-toughened glycidol ester modified amine hardener and a preparation method thereof. The preparation method comprises the following steps: (1) subjecting oleic acid and epoxy chloropropane to a reaction in the presence of a catalyst, so as to obtain a chlorohydrine intermediate; (2) adding a sodium hydroxide solution into the chlorohydrine intermediate obtained in the step (1), and carrying out a cyclization reaction; (3) then, collecting glycidyl oleate from a reaction product; (4) adding the obtained glycidyl oleate into isophorondiamine, carrying out a reaction, and then, carrying out depressurization to remove excessive isophorondiamine, thereby obtaining the glycidyl oleate modified isophorondiamine hardener. The hardener has the characteristics of large epoxy number, low chlorinity, low viscosity and the like, and the toughness and impact strength of epoxy resin cured products are greatly improved.

Description

technical field [0001] The invention relates to an amine curing agent for epoxy resin and a preparation method thereof. Background technique [0002] Epoxy resin has outstanding adhesive properties, excellent mechanical properties, good heat resistance, high stability, and has excellent properties such as good processability and small shrinkage after curing. It is widely used in coating materials, adhesives, etc. Adhesives, foam materials, fiber reinforced composite materials and other fields. [0003] Since the pure epoxy resin prepolymer has almost no use value, it can only show excellent use value by adding a curing agent for curing reaction. [0004] However, the cured epoxy resin cured by the curing agent currently used has defects such as high crosslinking density, large internal stress, brittleness, and poor impact resistance, which make the application of epoxy resin in some specific high-tech fields subject to varying degrees. limit. Therefore, toughening epoxy r...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C213/04C07C219/08C07D301/26C07D303/16C08G59/50
CPCC07C67/26C07C213/04C07C219/08C07D301/26C07D303/16C08G59/504C07C69/58
Inventor 高晟弢童伟姚慧敏毛小其吴蓁
Owner SHANGHAI RESIN FACTORY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com