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Preparation method of reversible covalent cross-linked reprocessable epoxy resin containing thioester bonds

An epoxy resin and covalent cross-linking technology, which is applied in organic chemistry, plastic recycling, recycling technology, etc., can solve the problems of unreported thioester bonds, etc., and achieve excellent reprocessing performance, wide source of raw materials, and excellent mechanical properties Effect

Active Publication Date: 2020-02-18
西安智聚复合材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, the introduction of thioester bonds into epoxy resins as a dynamic covalent bond has not been reported.

Method used

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  • Preparation method of reversible covalent cross-linked reprocessable epoxy resin containing thioester bonds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Into a round bottom flask equipped with magnetic stirring was put 5 g of succinic anhydride, followed by 45 ml of anhydrous acetonitrile and 5 ml of anhydrous pyridine. Stir at room temperature to form a homogeneous solution. Then 5.3 g of 3-mercaptopropionic acid and 0.35 g of 4-dimethylaminopyridine were added. The reaction was stirred overnight. The reaction solution was concentrated, adjusted to pH=1, extracted with ethyl acetate, and the organic layer was collected and concentrated to obtain a white dicarboxylic acid epoxy curing agent.

[0025] Take 5g of epoxy curing agent and 8.25g of bisphenol A diglycidyl ether, heat the epoxy curing agent with a heat gun to melt and mix evenly, heat in a vacuum oven at 100°C for 8 hours, and cool naturally to room temperature to obtain the available Reprocessed epoxy resin.

Embodiment 2

[0027] Into a round bottom flask equipped with magnetic stirring was put 5 g of succinic anhydride, followed by 45 ml of anhydrous acetonitrile and 5 ml of anhydrous pyridine. Stir at room temperature to form a homogeneous solution. Then 4.6 g of thioglycolic acid and 0.35 g of 4-dimethylaminopyridine were added. The reaction was stirred overnight. Concentrate the reaction solution, adjust the pH to 1, extract with ethyl acetate, collect the organic layer, and concentrate to obtain a dibasic carboxylic acid epoxy curing agent.

[0028] Take 5g of epoxy curing agent and 8.86g of bisphenol A diglycidyl ether, heat the epoxy curing agent with a heat gun to melt and mix evenly, heat in a vacuum oven at 120°C for 6 hours, and cool naturally to room temperature to obtain the available Reprocessed epoxy resin.

Embodiment 3

[0030] Into a round bottom flask equipped with a magnetic stirrer was charged 5 g of phthalic anhydride, followed by 45 ml of anhydrous acetonitrile and 5 ml of anhydrous pyridine. Stir at room temperature to form a homogeneous solution. Then 3.58 g of 3-mercaptopropionic acid and 0.35 g of 4-dimethylaminopyridine were added. The reaction was stirred overnight. Concentrate the reaction solution, adjust the pH to 1, extract with ethyl acetate, collect the organic layer, and concentrate to obtain a dibasic carboxylic acid epoxy curing agent.

[0031] Take 5g of epoxy curing agent and 3.96g of trimethylolpropane triglycidyl ether, heat with a heat gun to melt the epoxy curing agent and mix evenly, heat in a vacuum oven at 100°C for 10 hours, and cool naturally to room temperature. A reworkable epoxy resin is obtained.

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PUM

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Abstract

The invention relates to a preparation method of reversible covalent cross-linked reprocessable epoxy resin containing thioester bonds. The preparation method comprises the following steps: firstly, synthesizing an epoxy curing agent containing a reversible covalent bond-thioester bond by utilizing acid anhydride and mercaptocarboxylic acid, then mixing the epoxy curing agent with an epoxy monomer, and curing epoxy at a specific temperature to obtain the epoxy resin capable of being reprocessed for multiple times. The epoxy curing agent is simple to synthesize, easy to operate and wide in rawmaterial source. And the synthesized epoxy curing agent can be used for various epoxy monomers. Because the dynamic covalent bond thioester bond can be subjected to dynamic exchange reaction, the cured epoxy resin not only has excellent mechanical properties, but also has excellent reprocessing properties.

Description

technical field [0001] The invention belongs to the preparation technology of epoxy resin-based macromolecular materials, and relates to a preparation method of a reversible covalently cross-linked epoxy resin containing thioester bonds. Background technique [0002] Epoxy resin has the properties of light weight, high strength, corrosion resistance and easy processing, and has become an irreplaceable important material in the national economy, national defense construction and scientific and technological development. Through the functional design of epoxy resin, it is endowed with properties such as heat insulation, conductivity, and wave absorption, and it is widely used in military, aerospace and other fields. However, traditional epoxy resins are thermosetting resins with high crosslinking density. Once the epoxy monomer is cured and formed, it cannot be processed and used again, especially after the material is destroyed, it cannot be recycled and processed, and the fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/42C08G59/24C08G59/32C07C327/06C07C327/16
CPCC08G59/423C08G59/32C08G59/245C07C327/06C07C327/16Y02W30/62
Inventor 张秋禹杨裕民李春梅薛颖陈志聪
Owner 西安智聚复合材料科技有限公司
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