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Preparation method of graphene oxide grafted POSS (polyhedral oligomeric silsesquioxane) modified epoxy resin

An epoxy resin and graphene technology, applied in the field of graphene oxide, can solve the problems of limited application and development, low upper limit temperature, poor fracture toughness and impact resistance, etc., and achieves an increase in the initial temperature of thermal decomposition and improvement in tensile strength. , the effect of increased bending strength

Active Publication Date: 2012-05-09
福州乐道知识产权运营有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cured product of epoxy resin has poor fracture toughness and impact resistance, especially when used as a structural material, the upper limit temperature is low, which largely limits its application and development in high-tech fields such as aviation and aerospace.

Method used

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  • Preparation method of graphene oxide grafted POSS (polyhedral oligomeric silsesquioxane) modified epoxy resin
  • Preparation method of graphene oxide grafted POSS (polyhedral oligomeric silsesquioxane) modified epoxy resin
  • Preparation method of graphene oxide grafted POSS (polyhedral oligomeric silsesquioxane) modified epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) take flake graphite as raw material, adopt Hummers oxidation method to prepare graphite oxide, add 0.5g graphite oxide in 250ml there-necked flask, add 200ml distilled water, disperse 30min under ultrasonic environment, form the graphene oxide mixed solution of uniform dispersion, then Add 5ml of γ-aminohexahedral silsesquioxane (POSS) and 1.0g of NaOH, and adjust the pH value to 7, continue ultrasonic dispersion at 90°C for 3 hours, cool to room temperature after the reaction, add a large amount of water to precipitate, and depressurize Suction filtration, the product was washed 3 times with absolute ethanol to obtain graphene oxide / POSS black powder;

[0019] (2) Take 0.26g of graphene oxide / POSS prepared in step (1) and add it to 26g of epoxy resin E-51 matrix, depressurize and pump, then add 7.8g of 4,4'-diaminodiphenyl sulfone (DDS) Curing agent, mixed and dissolved, poured into a steel mold coated with silicon ester, and cured at 120°C / 2 hours + 160°C / 2 hours ...

Embodiment 2

[0022] (1) take flake graphite as raw material, adopt Hummers oxidation method to prepare graphite oxide, add 0.5g graphite oxide in 250ml there-necked flask, add 200ml distilled water, disperse 30min under ultrasonic environment, form the graphene oxide mixed solution of uniform dispersion, then Add 5ml of γ-aminohexahedral silsesquioxane (POSS) and 1.0g of NaOH, and adjust the pH value to 7, continue ultrasonic dispersion at 90°C for 3 hours, cool to room temperature after the reaction, add a large amount of water to precipitate, reduce Pressure suction filtration, the product was washed 3 times with absolute ethanol to obtain graphene oxide / POSS black powder;

[0023] (2) Take 0.78g of graphene oxide / POSS prepared in step (1) and add it to 26g of epoxy resin E-51 matrix, depressurize and pump, then add 7.8g of 4,4'-diaminodiphenyl sulfone (DDS) Curing agent, mixed and dissolved, poured into a steel mold coated with silicon ester, and cured at 120°C / 2 hours + 160°C / 2 hours +...

Embodiment 3

[0026] (1) take flake graphite as raw material, adopt Hummers oxidation method to prepare graphite oxide, add 0.5g graphite oxide in 250ml there-necked flask, add 200ml distilled water, disperse 30min under ultrasonic environment, form the graphene oxide mixed solution of uniform dispersion, then Add 5ml of γ-aminohexahedral silsesquioxane (POSS) and 1.0g of NaOH, and adjust the pH value to 7, continue ultrasonic dispersion at 90°C for 3 hours, cool to room temperature after the reaction, add a large amount of water to precipitate, reduce Pressure suction filtration, the product was washed 3 times with absolute ethanol to obtain graphene oxide / POSS black powder;

[0027] (2) Take 1.30g of graphene oxide / POSS prepared in step (1) and add it to 26g of epoxy resin E-51 matrix, vacuum pump, then add 7.8g of 4,4'-diaminodiphenyl sulfone (DDS) Curing agent, mixed and dissolved, poured into a steel mold coated with silicon ester, and cured at 120°C / 2 hours + 160°C / 2 hours + 180°C / 2 h...

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Abstract

The invention discloses a preparation method of graphene oxide grafted POSS (polyhedral oligomeric silsesquioxane) modified epoxy resin. The preparation method comprises the following steps of: taking crystalline flake graphite as a raw material, preparing graphite oxide through adopting a Hummers oxidation method, further adding the graphite oxide into distilled water, forming a uniformly-dispersed graphene oxide mixed solution under an ultrasonic environment, further adding POSS and a strong catalyst, performing full reaction, then filtering, washing and drying to get black powder; and further uniformly dispersing graphene oxide / POSS in an epoxy resin matrix, cross-linking and bonding under the action of a curing agent to get a composite material, molding by casting, cooling and demolding. According to the preparation method disclosed by the invention, the POSS is successfully grafted on a graphene oxide sheet layer, and advantages of the graphene oxide structure and the POSS structure are complemented, so that the preparation method has the advantages of low cost and easy obtaining of the raw material, easy operation, simple process, good reproducibility and obvious toughening modification effect against the epoxy resin.

Description

technical field [0001] The invention relates to the technical field of graphene oxide, in particular to a method for preparing a synergistically modified epoxy resin composite material based on graphene oxide grafted gamma-aminohexahedral silsesquioxane (POSS). Background technique [0002] Since the discovery of graphene in 2004, the preparation and modified compounds of graphene have become a research hotspot. Graphene is a new carbon material in which carbon atoms are tightly packed into a single-layer two-dimensional honeycomb lattice structure. The thickness of this graphene crystal film is only 0.335nm, which is only 1 / 100,000th that of hair. The material with the highest strength in the world is the basic unit for constructing other dimensional carbonaceous materials (such as zero-dimensional fullerene, one-dimensional carbon nanotubes, and three-dimensional graphite). It has good solubility in medium, which is conducive to its uniform dispersion and molding processi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K5/549
Inventor 刘括陆绍荣罗崇禧郭栋李善荣
Owner 福州乐道知识产权运营有限公司
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