Heat-resistant alicyclic epoxy resin cured product and preparation method thereof

An epoxy resin curing and alicyclic technology, which is applied in the field of alicyclic epoxy resin, can solve the problems of unsatisfactory optical properties of cured products, inability to fully meet the requirements of high light transmittance, and difficulty in meeting the requirements of high heat resistance.

Active Publication Date: 2018-05-08
JIANGSU TETRA NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The glass transition temperature (Tg for short) of the cured product ranges from 160 to 190°C, which is lower than most aromatic structure glycidyl ether epoxy resins and far lower than cyanic acid The relatively low glass transition temperature of other thermosetting resins such as ester resin (190-290°C) and maleimide (300-350°C) makes it difficult for the current alicyclic epoxy resin to meet the requirements of modern microelectronic packaging technology. High heat resistance requirements for packaging materials;
[0006] (2) The optical performance of the cured product is not ideal, because in some application fields that require high optical performance (such as photoresist, UV-LED packaging materials, etc.), it cannot fully meet the requirements of high light transmittance

Method used

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  • Heat-resistant alicyclic epoxy resin cured product and preparation method thereof
  • Heat-resistant alicyclic epoxy resin cured product and preparation method thereof
  • Heat-resistant alicyclic epoxy resin cured product and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A kind of preparation method of 3,4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl carboxylate, comprises the steps:

[0038] (1) Add 100g of 3-cyclohexene-1-carboxylic acid-3-cyclohexene-1-methyl ester, 200g of toluene, 106g of acetic anhydride and 32g of sodium acetate into a 1000ml three-necked flask, and cool to 10°C while stirring;

[0039] (2) Then start to drop 145g of 35% hydrogen peroxide, control the rate of addition to keep the temperature of the reaction system not exceeding 20°C-25°C, react for 4-8 hours, GC detects 3,4-epoxycyclohexylmethyl3,4 -Epoxy cyclohexyl carboxylate content is greater than 92% and then stops the reaction to obtain a reaction product;

[0040] (3) Slowly add 260 g of commercially available 30% NaOH solution to the reaction product to adjust the pH to 9-12, stir for 30 minutes and leave to separate the phases, and separate the upper organic phase;

[0041] (4) add 50g 10% sodium sulfite aqueous solution to the organic phase that step (3)...

Embodiment 2

[0046] A kind of preparation method of 3,4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl carboxylate, comprises the steps:

[0047] (1) Add 100g of 3-cyclohexene-1-carboxylic acid-3-cyclohexene-1-methyl ester, 300g of toluene, 130g of acetic anhydride and 45g of sodium acetate into a 1000ml three-necked flask, and cool to 6°C while stirring;

[0048] (2) Then start to drop 176g of 35% hydrogen peroxide, control the rate of addition to keep the temperature of the reaction system not exceeding 20°C-25°C, react for 4-8 hours, GC detects 3,4-epoxycyclohexylmethyl3,4 -Epoxy cyclohexyl carboxylate content is greater than 92% and then stops the reaction to obtain a reaction product;

[0049] (3) Slowly add 320 g of commercially available 30% NaOH solution to the reaction product to adjust the pH to 9-12, stir for 30 minutes and leave to separate the phases, and separate the upper organic phase;

[0050] (4) add 60g 10% sodium sulfite aqueous solution to the organic phase that step (3) ob...

Embodiment 3

[0055] A kind of preparation method of 3,4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl carboxylate, comprises the steps:

[0056] (1) Add 100g of 3-cyclohexene-1-carboxylic acid-3-cyclohexene-1-methyl ester, 250g of toluene, 120g of acetic anhydride and 40g of sodium acetate into a 1000ml three-necked flask, and cool to 15°C while stirring;

[0057] (2) Then start to drop 160g of 35% hydrogen peroxide, control the rate of addition to keep the temperature of the reaction system not exceeding 20°C-25°C, react for 4-8 hours, GC detects 3,4-epoxycyclohexylmethyl3,4 -Epoxy cyclohexyl carboxylate content is greater than 92% and then stops the reaction to obtain a reaction product;

[0058] (3) Slowly add 335 g of commercially available 30% NaOH solution to the reaction product to adjust the pH to 9-12, stir for 30 minutes and leave to separate phases, and separate the upper organic phase;

[0059] (4) add 55g 10% sodium sulfite aqueous solution to the organic phase that step (3) obt...

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Abstract

The invention relates to a heat-resistant alicyclic epoxy resin cured product. The cured product comprises the following raw materials in parts by weight: 80-100 parts of 3,4-epoxycyclohexylmethyl 3,4-epoxycyclohexanecarboxylate, 5-20 parts of 4-vinyl-1-cyclohexene dioxide, 1-3 parts of ethylene glycol, 99-135 parts of hexahydrophthalic anhydride and 1 part of an accelerator. The invention also relates to a preparation method of the heat-resistant alicyclic epoxy resin cured product. According to the heat-resistant alicyclic epoxy resin cured product provided by the invention, the light transmittance and glass transition temperature (Tg) are obviously improved, and the properties such as volume resistance, arc resistance and the like are superior to the properties of prior alicyclic epoxyresin cured products.

Description

technical field [0001] The invention relates to the field of alicyclic epoxy resins, in particular to a heat-resistant cured alicyclic epoxy resin and a preparation method thereof. Background technique [0002] Cycloaliphatic epoxy resins and their cured products have excellent comprehensive properties such as processability, thermal stability, electrical insulation, and ultraviolet radiation resistance, and have been widely used in important industrial fields such as aerospace, microelectronic packaging, and motor insulation. In response to the increasing performance and functional requirements of modern industry for polymer materials, the synthesis and performance research of alicyclic epoxy resins has been very active in recent years. [0003] Different from glycidyl ether type epoxy resin, alicyclic epoxy resin is obtained by the epoxidation reaction of unsaturated alicyclic compounds through organic peroxyacid, so the content of free chlorine or metal ions is very low, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/62C08G59/42C08G59/24C08G59/22
CPCC08G59/226C08G59/24C08G59/4284C08G59/62
Inventor 韩建伟常杨军贾泉吴宏亮
Owner JIANGSU TETRA NEW MATERIAL TECH
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