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Siliceous modified high-temperature-resistant cyanate resin, and preparation method and application thereof

A technology of cyanate ester resin and high temperature resistance, which is applied in the field of its preparation and silicon-containing modified high temperature resistant cyanate ester resin, which can solve the problems of lower glass transition temperature, lower mechanical and electrical properties, and insufficient toughness, and achieve excellent The effect of high temperature resistance and good cost advantage

Active Publication Date: 2015-12-30
SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although cyanate resin has high heat resistance, it is difficult to be directly applied to the pultrusion process due to its insufficient toughness due to its own structural limitations, so its modification has become an inevitable trend. The traditional modification method adopts external toughening Agent or resin compounding, but this method will bring about a decrease in the glass transition temperature and a decrease in some mechanical and electrical properties

Method used

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  • Siliceous modified high-temperature-resistant cyanate resin, and preparation method and application thereof
  • Siliceous modified high-temperature-resistant cyanate resin, and preparation method and application thereof
  • Siliceous modified high-temperature-resistant cyanate resin, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0032] (a) Add 400g of n-butanol and 20g of tetramethylammonium hydroxide aqueous solution (mass fraction is 10%) in the 1000mL there-necked flask with thermometer and condenser tube, after stirring and mixing evenly, add dropwise 20g of hydroxyl-terminated A mixed solution of polydimethylsiloxane, 120g γ-(2,3-glycidyloxy) propyltrimethoxysilane and 80g ethanol, the drop rate is controlled within 3 hours, the reaction temperature is controlled at 10°C, hydrolysis and polycondensation 6h, after the reaction is completed, use a rotary evaporator to evaporate the solvent and small molecules remaining in the system to obtain a transparent viscous liquid that can flow at room temperature for use, which is epoxy-containing silsesquioxane (G- POSS).

[0033] (b) Pour 30g of the above-mentioned viscous liquid (G-POSS) and 270g of bisphenol A cyanate resin into a 500mL three-necked bottle and stir evenly, prepolymerize at 80-90°C for 2 hours, and cool the modified resin to Stand-by at...

Embodiment 2

[0037] (a) Add 400g of n-butanol and 20g of tetramethylammonium hydroxide aqueous solution (mass fraction is 10%) in the 1000mL there-necked flask with thermometer and condenser tube, after stirring and mixing evenly, add dropwise 20g of hydroxyl-terminated A mixed solution of polydimethylsiloxane, 120g γ-(2,3-glycidyloxy) propyltrimethoxysilane and 80g ethanol, the drop rate is controlled within 3 hours, the reaction temperature is controlled at 10°C, hydrolysis and polycondensation 6h, after the reaction is completed, use a rotary evaporator to evaporate the solvent and small molecules remaining in the system to obtain a transparent viscous liquid that can flow at room temperature for use, which is the final product epoxy-containing silsesquioxane ( G-POSS).

[0038] (b) Pour 30g of the above-mentioned viscous liquid (G-POSS) and 270g of bisphenol F type cyanate resin into a 500mL three-necked bottle and stir evenly, prepolymerize at 80-90°C for 2 hours, and cool the modifie...

Embodiment 3

[0042] (a) Add 400g of n-butanol and 16g of tetramethylammonium hydroxide aqueous solution (mass fraction is 10%) in the 1000mL there-necked flask with thermometer and condenser tube, after stirring and mixing evenly, add dropwise 26g of hydroxyl-terminated A mixed solution of polydimethylsiloxane, 127g γ-(2,3-glycidoxy) propyltrimethoxysilane and 90g ethanol, the drop rate is controlled at 3.5h, the reaction temperature is controlled at 10°C, and the hydrolysis Polycondensation for 5 hours, after the reaction is completed, use a rotary evaporator to evaporate the solvent and small molecules remaining in the system, and obtain a transparent viscous liquid that can flow at room temperature for use, which is the final product of epoxy-containing silsesquioxane (G-POSS).

[0043] (b) Pour 30g of the above viscous liquid (G-POSS) and 270g of bisphenol F type cyanate resin into a 500mL three-necked bottle and stir evenly, prepolymerize at 80-90°C for 2h, and cool the modified resin...

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Abstract

The invention relates to a siliceous modified high-temperature-resistant cyanate resin, and a preparation method and application thereof. The preparation method comprises the following steps: adding a hydroxy silicone oil-silane coupling agent-organic solvent mixed solution into a tetramethylammonium hydroxide water solution-polar solvent mixed solution, carrying out hydrolytic polycondensation at 5-40 DEG C for 4-8 hours, and distilling to obtain epoxy-containing silsesquioxane; prepolymerizing the epoxy-containing silsesquioxane and a cyanate resin at 50-100 DEG C for 1-8 hours to obtain a modified cyanate resin; and uniformly mixing the modified cyanate resin and modified acid anhydride to obtain the siliceous modified high-temperature-resistant cyanate resin. The intrinsic toughening mode is utilized to improve the brittleness of the cyanate resin without sacrificing the heat resistance of the cyanate resin; and thus, the prepared high-temperature-resistant resin composition for pultrusion, of which Tg is 240-270 DEG C, has the advantages of excellent high temperature resistance and favorable cost.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a silicon-containing modified high-temperature-resistant cyanate resin, its preparation method and application. Background technique [0002] Inside the carbon fiber composite core wire is a uniform solidified core layer composed of carbon fiber and resin, and this material has very high requirements on the curing speed, glass transition temperature and toughness of the resin. [0003] The resins commonly used today are epoxy resin systems. The general-purpose epoxy resin system has the disadvantage of low heat resistance. Although some resins have good heat resistance, the glass transition temperature Tg of the cured product is generally not higher than 180°C, and the interface performance is poor. Poor strength and toughness. Although high heat resistance can be obtained by modifying general-purpose epoxy resin, it is difficult to apply to large-scale pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06
CPCC08G77/14C08L83/06C08G73/065C08G81/024C08G59/3281C08G73/0644C08G77/452C08G81/025C08K3/04
Inventor 吴斌张春琪夏智峰夏媛娇单升升井丰喜屈永明
Owner SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL CO LTD
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