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Glycidyl amine type polyfunctional epoxy resin and preparation method thereof

A glycidylamine type, epoxy resin technology, applied in organic chemistry and other directions, can solve the problems affecting the final performance, dimensional stability, high temperature effect of products, etc., and achieve the effects of low cost, easy availability, and low environmental pollution hazards.

Inactive Publication Date: 2015-03-11
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The commonly used glycidyl amine epoxy resin usually has a high moisture absorption rate, which affects the dimensional stability and high temperature resistance of the product, thus affecting the final performance of the product

Method used

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  • Glycidyl amine type polyfunctional epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 11.4 grams (0.1 moles) of methylcyclopentadiamine, 27.8 grams (0.3 moles) of epichlorohydrin, 11.4 grams of water and 11.4 milliliters of ethanol into a three-necked flask, stir and react at 30°C for 4 hours, then increase the reaction temperature , reacted at 75°C for 2 hours, then increased the reaction temperature, and reacted at 85°C for 1 hour (it is beneficial to increase the conversion rate by adopting staged heating), cooling the reaction solution to 60°C, and adding 26.7 grams (0.2 moles) of 30% Concentrated sodium hydroxide aqueous solution, after dripping within 2 hours, continue to react at 80°C for 5 hours, cool down to 35°C, add 900 ml of toluene, stir to dissolve, filter to remove sodium chloride, wash the mother liquor with water, stand still, and separate liquids. Remove the aqueous phase and leave the organic phase mother liquor. The mother liquor is devolatilized in vacuum, and the volatile matter is collected for reuse in the next cycle; the resi...

Embodiment 2

[0032] Add 11.4 grams (0.1 moles) of methylcyclopentadiamine, 92.5 grams (1.0 moles) of epichlorohydrin, 1.14 grams of water and 11 milliliters of ethanol into a three-necked flask, stir and react at 30°C for 3 hours, then increase the reaction temperature , reacted at 75°C for 3 hours, then increased the reaction temperature, and reacted at 85°C for 10 minutes, cooled the reaction solution to 60°C, added dropwise 93.3 grams (0.7 moles) of 30% sodium hydroxide aqueous solution, dropwise within 2 hours After completion, the reaction was continued at 80° C. for 3 hours. Cool down to 35°C, let stand, separate liquid, remove sodium chloride solid and water, and obtain epichlorohydrin layer and resin layer. Reclaim epichlorohydrin for next recycling; put the resin layer into a three-necked flask, add 900 milliliters of toluene to the resin, stir and dissolve, wash the mother liquor with water, let stand, separate liquids, remove the water phase, and leave the organic phase mother l...

Embodiment 3

[0034] Except adding 92.5 grams (1.0 moles) of epichlorohydrin and 66.7 grams of 30% aqueous sodium hydroxide solution, other process steps, material quantities and reaction parameters are the same as in Example 2. As a result, N, N, N' , N'-tetraglycidylmethylcyclopentanediamine was obtained, and the yield was 82%, the epoxy value was 0.592, and the volatile matter was 0.86% according to the amount of methylcyclopentanediamine and the amount of product. .

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Abstract

The invention relates to a glycidyl amine type polyfunctional epoxy resin and a preparation method of the glycidyl amine type polyfunctional epoxy resin. The glycidyl amine type polyfunctional epoxy resin has the structural formula as shown in formula I. The preparation method comprises the following steps of: 1) putting methyl cyclic pentamethylene diamine and epoxy chloropropane into a solvent, and reacting; and 2) dropwise adding an alkali metal hydroxide water solution, carrying out a desalting closed-loop reaction, extracting by an extracting agent, washing by water, skimming, and carrying out vacuum devolatilization to prepare the amber and sticky N, N, N' N'-tetraglycidyl methyl cyclic pentamethylene diamine. The glycidyl amine type polyfunctional epoxy resin and the preparation method thereof disclosed by the invention have the beneficial effects that 1) the production technology is simple, the product performance is high, and the yield is high; 2) the generation of harmful substance in the process of experiment is avoided, and work environment is better; 3) the product yield is high up to 70%; 4) the excessive epoxy chloropropane is easy to recycle; and 5) the solvent in a reaction system is easy to recycle, and can be recycled, thus being less in three wastes, and small in environment pollution hazard.

Description

technical field [0001] The invention relates to a glycidylamine type multifunctional epoxy resin and a preparation method thereof. Background technique [0002] Glycidylamine epoxy resin is an important part of the preparation of coatings, adhesives and composite materials, but the traditional glycidylamine epoxy resin is usually difficult to meet the performance requirements of some products, such as heat resistance, hardness, elasticity, etc. etc. Therefore, other functional groups are introduced into the glycidylamine epoxy resin to improve its performance, and a glycidylamine-type multifunctional epoxy resin is prepared. [0003] Glycidylamine-type multifunctional epoxy resin is a commonly used resin matrix for high-performance composite materials. Strong, excellent mechanical properties and corrosion resistance, it can be used in high temperature resistant adhesives, fiber reinforced prepregs, packaging materials for electronic components, high temperature resistant el...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/36C07D301/27
Inventor 樊庆春李文胡芽吴田段菲红刘生鹏张良均
Owner WUHAN INSTITUTE OF TECHNOLOGY