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Synthesis of imidazole latent epoxy curing accelerator having toughening effect and application of accelerator in epoxy modification

A curing accelerator and epoxy modification technology, which is applied in the field of imidazole latent curing accelerators, can solve problems such as the lack of research on macromolecular imidazole latent curing accelerators, and achieve mass production and industrial applications. Good compatibility, the effect of low addition amount

Active Publication Date: 2017-02-22
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Reactive passivation is generally achieved through the reaction of small molecules with the active hydrogen of the imidazole ring, and there is still no research on latent curing accelerators for macromolecular imidazoles.

Method used

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  • Synthesis of imidazole latent epoxy curing accelerator having toughening effect and application of accelerator in epoxy modification
  • Synthesis of imidazole latent epoxy curing accelerator having toughening effect and application of accelerator in epoxy modification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step 1: Weigh 5.227g of methacryloyl chloride, dissolve it in 50mL of tetrahydrofuran (THF), and add it dropwise to 2-methylimidazole (4.105g) and triethylamine (6.07 g) in 100mL THF solution, stirred, and the above-mentioned process was carried out in a 250mL three-necked flask. After the dropwise addition, the stirring was continued at room temperature for 24-48 hours, and the reaction ended. The ammonium salt generated during the reaction is removed by suction filtration of the system, and the solvent is removed by rotary evaporation to obtain a free radical comonomer with an imidazole ring.

[0021] The second step: Weigh 3.380g of the monomer containing imidazole ring and double bond synthesized in the first step, as well as HEA2.907g, EHA7.370g, LA2.422g, add them to a 100mL round bottom flask, and add 50mL of ethyl acetate was reacted at 85°C for 24h. After the end, the product was added dropwise to a precipitant to precipitate, and a white solid was obtained, ...

Embodiment 2

[0024] Step 1: Step 1: Weigh 6.320g of methacryloyl chloride, dissolve it in 50mL of tetrahydrofuran (THF), and add it dropwise to 2-methylimidazole (4.105g) and three Ethylamine (6.07g) in 100mL THF solution, stirred, and the above process was carried out in a 250mL three-necked flask. After the dropwise addition, the stirring was continued at room temperature for 24-48 hours, and the reaction ended. The ammonium salt generated during the reaction is removed by suction filtration of the system, and the solvent is removed by rotary evaporation to obtain a free radical comonomer with an imidazole ring.

[0025] Step 2: Weigh 3.380g of the monomer containing imidazole ring and double bond synthesized in the first step, as well as 2.907g of HEA, 7.370g of EHA, and 2.422g of LA, and add them to a 100mL round bottom flask, and add 50mL of ethyl acetate was reacted at 85°C for 24h. After the end, the product was added dropwise to a precipitant to precipitate, and a white solid was...

Embodiment 3

[0028] The first step: Weigh 2-methylimidazole (4.105g) and triethylamine (6.07g), dissolve in 100mL tetrahydrofuran (THF), and add methacryloyl chloride ( 5.227g) in 50mL THF solution, stirred, and the above process was carried out in a 250mL three-necked flask. After the dropwise addition, the stirring was continued at room temperature for 24-48 hours, and the reaction ended. The ammonium salt generated during the reaction is removed by suction filtration of the system, and the solvent is removed by rotary evaporation to obtain a free radical comonomer with an imidazole ring.

[0029] Step 2: Weigh 3.380g of the monomer containing imidazole ring and double bond synthesized in the first step, as well as 2.907g of HEA, 7.370g of EHA, and 2.422g of LA, and add them to a 100mL round bottom flask, and add 50mL of ethyl acetate was reacted at 85°C for 24h. After the end, the product was added dropwise to a precipitant to precipitate, and a white solid was obtained, which was dri...

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Abstract

The invention discloses an acrylate copolymer synthetized through simple free radical polymerization, containing an imidazole ring side group and applied to a latent epoxy curing accelerator to simultaneously toughen epoxy resin. Firstly, imidazole is grafted to a macromolecular chain, the catalytic activity of an imidazole ring can be reduced through a steric effect to achieve the latency purpose; secondly, an acrylate molecular chain participates in formation of an epoxy curing network, microphase separation is formed in an epoxy matrix, and the mechanical property of the epoxy resin is improved. The prepared imidazole latent epoxy curing accelerator having a toughening effect can improve the curing temperature of an imidazole catalyzed DGEBA / MHHPA curing system to about 180 DEG C and has good storage stability at room temperature.

Description

technical field [0001] The invention relates to the field of imidazole-type latent curing accelerators for epoxy resins, in particular to the purpose of reducing imidazole curing activity through macromolecular steric hindrance to achieve latent properties at normal temperature. Background technique [0002] As the resin matrix of adhesives, coatings and composite materials, epoxy resin is widely used in construction, machinery, electronics, aerospace and other fields. In order to optimize the mechanical processing properties of the resin, many studies have been carried out on one of the resin components - the curing agent. The study of latent curing accelerators for epoxy resins has become a hot topic in the research of curing agents for epoxy resins at home and abroad in recent years. The so-called latent curing accelerator means that it has a certain storage stability at room temperature after being blended with epoxy resin and high-temperature curing agent, and can prom...

Claims

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Application Information

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IPC IPC(8): C08F220/18C08F220/28C08F220/60C08G59/68
CPCC08F220/18C08G59/686C08F220/281C08F220/60C08F220/1812
Inventor 刘晓亚赵芳巧费小马魏玮罗静朱叶
Owner JIANGNAN UNIV
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