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Vegetable oil-based flexible amine curing agent, preparation method thereof and vegetable oil-based tough epoxy resin

A technology of tough epoxy resin and oil-based flexible amine, which is applied in the preparation of cyanide reaction, chemical instruments and methods, and the preparation of organic compounds. It can solve the hidden dangers of solvent residues, increase energy consumption, and affect material properties, etc. problems, to eliminate hidden dangers of solvent residues, reduce equipment requirements, and improve flexibility

Active Publication Date: 2020-10-02
杭州至华新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the synthesis process, ethyl acetate or acetone or methyl ethyl ketone or cyclohexane or n-hexane are needed as solvents for diluting epoxidized soybean oil, and after the curing agent is synthesized, the operation of recovering the solvent under reduced pressure cannot eliminate the hidden danger of some solvent residues , which in turn affects the properties of the material mixed with the resin
At the same time, decompression operation reduces equipment safety and increases energy consumption

Method used

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  • Vegetable oil-based flexible amine curing agent, preparation method thereof and vegetable oil-based tough epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The vegetable oil-based tough epoxy resin provided in this embodiment is prepared through the following steps:

[0035] (1) Preparation of vegetable oil-based flexible amine curing agent

[0036] A. Add 150g of cardanol and 60.1g of ethylenediamine into a four-necked flask with mechanical stirring, and heat it to 80°C under nitrogen protection. After 2 hours of reaction, slowly add 30g of formaldehyde in batches, and react at 120°C for 4 After 1 hour, the moisture and unreacted ethylenediamine were removed under vacuum to obtain intermediate 1.

[0037] B, 180g of intermediate 1 is added in the normal pressure reactor, the temperature is raised to 100°C, then the mixed solution of 1.22g of triphenylphosphine (accelerator) and 63.0g of epoxidized soybean oil is added dropwise, The reaction time was 8 hours at 100°C, the temperature was lowered, and the material was discharged to obtain a vegetable oil-based flexible amine curing agent 1. The measured active hydrogen eq...

Embodiment 2

[0041] The vegetable oil-based tough epoxy resin provided in this embodiment is prepared through the following steps:

[0042] (1) Preparation of vegetable oil-based flexible amine curing agent

[0043] A. Add 150g of cardanol and 103.2g of diethylenetriamine into a four-necked flask with mechanical stirring, and heat to 80°C under nitrogen protection. After 2 hours of reaction, slowly add 30g of formaldehyde in batches and react at 120°C After 4 hours, the moisture and unreacted diethylenetriamine were removed under vacuum to obtain intermediate 2.

[0044] B. Add 180g of intermediate 2 into the normal pressure reactor, heat up to 100°C, and then drop the mixed solution of 1.33g of N,N-dimethylbenzylamine (accelerator) and 84.0g of epoxidized soybean oil Add in the way of adding, react at 100°C for 8 hours, cool down and discharge. The measured active hydrogen equivalent was 130.6.

[0045] (2) Preparation of epoxy resin

[0046] Take 177.4g vegetable oil-based flexible a...

Embodiment 3

[0048] The vegetable oil-based tough epoxy resin provided in this embodiment is prepared through the following steps:

[0049] (1) Preparation of vegetable oil-based flexible amine curing agent

[0050] A. Add 150g of cardanol and 146.2g of triethylenetetramine into a four-necked flask with mechanical stirring, and heat it to 80°C under nitrogen protection. After 2 hours of reaction, slowly add 30g of formaldehyde in batches and react at 120°C After 4 hours, the moisture and unreacted triethylenetetramine were removed under vacuum to obtain intermediate 3.

[0051] B. Add 180g of intermediate 3 into the normal pressure reactor, heat up to 120°C, and then drop the mixture of 1.36g of N,N-dimethylbenzylamine (accelerator) and 90.9g of epoxidized soybean oil Add in the way of adding, react at 100°C for 8 hours, cool down and discharge. The measured active hydrogen equivalent was 124.8.

[0052] (2) Preparation of epoxy resin

[0053] Take 172.2g vegetable oil-based flexible ami...

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Abstract

The invention provides a vegetable oil-based flexible amine curing agent based on epoxidized soybean oil and cardanol, a preparation method of the vegetable oil-based flexible amine curing agent and vegetable oil-based tough epoxy resin. The curing agent is prepared by reacting a compound shown in s formula I with epoxidized soybean oil in the presence of an accelerant, wherein the structural formula of the compound shown in the formula I is shown in the specification. The epoxy resin curing agent is subjected to molecular structure design, and a flexible long-chain macromolecular soybean oilchain segment and a flexible cardanol chain segment are introduced into the molecular structure, so that the toughened and modified vegetable oil-based flexible amine curing agent is obtained, the flexible chain segment of epoxy resin molecules is increased, the toughening purpose is achieved, and the flexibility of epoxy resin is improved. Epoxidized soybean oil is derived from soybean oil, cardanol is derived from cashew nut shell oil, and the epoxidized soybean oil and the cardanol are renewable raw materials.

Description

technical field [0001] The invention belongs to the technical field of epoxy curing agent preparation, and in particular relates to a vegetable oil-based flexible amine curing agent, a preparation method thereof, and a vegetable oil-based tough epoxy resin. Background technique [0002] Traditional epoxy resin is brittle and its application in the fields of plastic bonding and electronic potting is limited. Through the toughening design of the molecular structure of epoxy resin, the application range of epoxy resin can be expanded. [0003] At present, there are mainly two ways to toughen epoxy resin: matrix resin toughening and flexible curing agent: [0004] The toughening of the matrix resin mainly increases the toughness of the overall material by introducing tough molecular chains to form a phase-separated structure. [0005] Using a flexible curing agent introduces long chains and ether bonds to improve the toughness of the cured product. At the same time, the curing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/08C07C229/26C08G59/50
CPCC07C227/08C07C213/02C08G59/504C07C229/26C07C215/50
Inventor 林宇腾施小妹吴金彪
Owner 杭州至华新材料科技有限公司
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