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High-toughness flame-retardant medium-and-low-temperature cured epoxy resin system and preparation method thereof

A technology for curing epoxy resin and epoxy resin, applied in the field of advanced polymer material science, can solve problems such as difficulty in ensuring particle dispersion, achieve excellent flame retardant efficiency, improve flame retardant performance, and good compatibility.

Active Publication Date: 2019-12-31
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with such nanoparticles toughened, there is no physical interaction or chemical bonding with the resin matrix, and it is difficult to ensure the dispersion of the particles in the resin matrix, which has a certain impact on the processing and mechanical properties.

Method used

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  • High-toughness flame-retardant medium-and-low-temperature cured epoxy resin system and preparation method thereof
  • High-toughness flame-retardant medium-and-low-temperature cured epoxy resin system and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Add γ-aminopropyltriethoxysilane, triethyl phosphate and N-methyldiethanolamine into a three-necked flask at a molar ratio of 1:1:4.375, and stir in an oil bath under the protection of nitrogen to control the reaction The temperature is between 80-150 DEG C, and the reaction is carried out for 10-12 hours until no distillate is produced to obtain the product hyperbranched polysilicon phosphate.

[0033] Mix 12 parts of bisphenol A epoxy resin and 48 parts of tetraglycidylamine epoxy resin, add 3 parts of hyperbranched polysilicon phosphate, and stir at room temperature for 10-15 minutes to prepare a resin prepolymer. Then, add 60 parts of acid anhydride curing agent into the above-mentioned prepolymer, stir for 5-10 minutes, pour into the preheated mold, vacuumize to remove air bubbles in a vacuum oven at 60-80°C, and put Blast drying oven for staged heating and curing, the curing process is 90~120°C / 2~4h+140~160°C / 2~3h, cooling, after demoulding, and then post-treatment...

Embodiment 2

[0035] Add γ-aminopropyltriethoxysilane, triethyl phosphate and N-methyldiethanolamine into a three-necked flask at a molar ratio of 1:1:4.375, and stir in an oil bath under the protection of nitrogen to control the reaction The temperature is between 80-150 DEG C, and the reaction is carried out for 10-12 hours until no distillate is produced to obtain the product hyperbranched polysilicon phosphate.

[0036] Mix 12 parts of bisphenol A epoxy resin and 48 parts of tetraglycidylamine epoxy resin, add 5 parts of hyperbranched polysilicon phosphate, and stir at room temperature for 10-15 minutes to prepare a resin prepolymer. Then, add 60 parts of acid anhydride curing agent into the above-mentioned prepolymer, stir for 5-10 minutes, pour into the preheated mold, vacuumize to remove air bubbles in a vacuum oven at 60-80°C, and put Blast drying oven for staged heating and curing, the curing process is 90~120°C / 2~4h+140~160°C / 2~3h, cooling, after demoulding, and then post-treatmen...

Embodiment 3

[0038] Add γ-aminopropyltriethoxysilane, triethyl phosphate and N-methyldiethanolamine into a three-necked flask at a molar ratio of 1:1:4.375, and stir in an oil bath under the protection of nitrogen to control the reaction The temperature is between 80-150 DEG C, and the reaction is carried out for 10-12 hours until no distillate is produced to obtain the product hyperbranched polysilicon phosphate.

[0039] Mix 20 parts of bisphenol A epoxy resin and 40 parts of tetraglycidylamine epoxy resin, add 3 parts of hyperbranched polysilicon phosphate, and stir at room temperature for 10-15 minutes to prepare a resin prepolymer. Then, add 60 parts of acid anhydride curing agent into the above-mentioned prepolymer, stir for 5-10 minutes, pour into the preheated mold, vacuumize to remove air bubbles in a vacuum oven at 60-80°C, and put Blast drying oven for staged heating and curing, the curing process is 90~120°C / 2~4h+140~160°C / 2~3h, cooling, after demoulding, and then post-treatmen...

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Abstract

The invention relates to a high-toughness flame-retardant medium-and-low-temperature cured epoxy resin system and a preparation method thereof. The high-toughness flame-retardant medium-and-low-temperature cured epoxy resin system is composed of silicon-phosphorus-nitrogen containing hyperbranched polysilicophosphate, bisphenol A type epoxy resin, tetraglycidyl amine type epoxy resin and an anhydride curing agent. The silicon-phosphorus-nitrogen synergistic flame retardant with the hyperbranched structure contains various flame retardant elements at the same time, the active terminal primary amine group of the silicon-phosphorus-nitrogen synergistic flame retardant can directly participate in a curing crosslinking reaction of epoxy resin and has good compatibility with a resin matrix, andmeanwhile, an Si-O-Si flexible chain segment is introduced into the epoxy resin, so that the toughness of the resin system is effectively improved. A tertiary amine functional group in the hyperbranched polysilicophosphate plays a role in promoting resin curing, can promote the reaction between an anhydride curing agent and epoxy resin, has a certain catalytic effect on curing, and can complete acuring reaction at a relatively low temperature. The system has a wide application prospect in the aspects of flame retardance of coatings, textiles, furniture, buildings and thermosetting resins.

Description

technical field [0001] The invention belongs to the scientific and technical field of advanced polymer materials, and relates to a high-toughness flame-retardant type medium-low temperature curing epoxy resin system and a preparation method. Background technique [0002] As a commonly used thermosetting resin, epoxy resin has the advantages of excellent mechanical properties, low curing shrinkage, excellent processing performance, and low cost. It is widely used in aerospace, electronic telecommunications, transportation and construction and other fields. However, the flame retardant performance of epoxy resin is extremely poor, and it will continue to burn after a fire and generate a large amount of smoke, so its application often needs to be treated after flame retardant treatment. At the same time, a large number of epoxy groups in the epoxy resin make the cured product have a high crosslinking density, which shows the disadvantages of easy stress cracking, poor impact re...

Claims

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Application Information

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IPC IPC(8): C08G59/58C08G59/50C08G83/00
CPCC08G59/58C08G59/504C08G83/005
Inventor 颜红侠张渊博郭留龙李林刘锐
Owner NORTHWESTERN POLYTECHNICAL UNIV
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