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Preparation method of functionalized graphene oxide/epoxy resin nanocomposite

A nano-composite material and epoxy resin technology, applied in the field of polymer-based nano-composite materials, can solve the problems of less hydroxyl content, less organosilane molecules, and the influence of mechanical properties of composite materials without mentioning preparation and characterization, etc., to achieve improved Effect of mechanical and thermal properties

Inactive Publication Date: 2014-03-12
HANGZHOU NORMAL UNIVERSITY
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  • Application Information

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Problems solved by technology

[0005] Chinese patent CN 102153877 A discloses a graphene composite material and its preparation method. The invention uses organosilane to modify graphene, and prepares a graphene polymer nanocomposite material, although the dispersion of graphene after modification has been improved, but due to the low content of hydroxyl groups on the surface of graphene itself, there are relatively few organosilane molecules grafted on the surface of graphene, and the gap between graphene sheet and polymer matrix The interface can't be improved very well either
[0007] Bortz et al. directly added graphene oxide to epoxy resin to prepare composite materials, and the results showed that the mechanical properties of the resin matrix were significantly improved; Surface treatment not mentioned [Macromolecules 2012;45(1):238-245]
[0008] Wang Zhou et al. used silane coupling agent KH560 and sodium dodecyl sulfate SDS to modify graphene oxide, and prepared SDS functionalized graphene oxide / epoxy Composite materials, but there is no mention of KH560 modified graphene oxide to prepare epoxy resin composite materials and the impact on the mechanical properties of composite materials [Preparation and Characterization of Epoxy Resin / Graphene Oxide Nanocomposites, Master Thesis, Beijing University of Chemical Technology, 2010]

Method used

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  • Preparation method of functionalized graphene oxide/epoxy resin nanocomposite
  • Preparation method of functionalized graphene oxide/epoxy resin nanocomposite
  • Preparation method of functionalized graphene oxide/epoxy resin nanocomposite

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Effect test

Embodiment 1

[0042] (1) Using graphite as raw material, the prepared GO was prepared by the Hummer method, and then 500mg GO was first dispersed in toluene, ultrasonicated for 1h to obtain a graphene oxide suspension, and under the protection of nitrogen, mechanically prepared at a temperature of 70°C Under stirring, 2.4g of silane coupling agent KH560 was added dropwise to the suspension, and the reaction time was 5h. After the reaction, the black solid powder f-GO was obtained after suction filtration, washing, and drying in a vacuum oven.

[0043] (2) 0.18 g of graphene oxide (f-GO) modified by silane coupling agent in step (1) was ultrasonically treated for 30 min and dispersed in acetone, then 93.7 g of bisphenol A epoxy resin was added, planetary ball mill (250 rpm) for 6 hours to obtain the masterbatch, remove the organic solvent under vacuum (0.1MPa), and then add 86.1g of curing agent (the mass ratio of methyl hexahydrophthalic anhydride to N,N-dimethylbenzylamine is 100:1 mixture...

Embodiment 2

[0053] (1) Using graphite as raw material, the prepared GO was prepared by the Hummer method, and then 500 mg GO was first dispersed in toluene, ultrasonicated for 1 h to obtain a graphene oxide suspension, and mechanically stirred at a temperature of 70 ° C under the protection of nitrogen Next, 2.4g of silane coupling agent KH560 was added dropwise to the suspension, and the reaction time was 5h. After the reaction, the black solid powder f-GO was obtained after suction filtration, washing, and drying in a vacuum oven.

[0054] (2) 0.1625 g of silane coupling agent-modified graphene oxide (f-GO) prepared in step (1) was ultrasonically treated for 30 min. and then dispersed in acetone, then 33.79 g of bisphenol A epoxy resin was added, and the planet After ball milling (250 rpm) for 6 hours, the masterbatch was obtained. Under vacuum conditions (0.5MPa), the organic solvent was removed, and then 31.05g of curing agent were added and mixed, and cured at high temperature (120°C ...

Embodiment 3

[0060] (1) Using graphite as raw material, the prepared GO was prepared by the Hummer method, and then 500mg GO was first dispersed in toluene, ultrasonicated for 1h to obtain a graphene oxide suspension, and under the protection of nitrogen, mechanically prepared at a temperature of 70°C Under stirring, add 7.5g of methyl (γ-glycidoxy)diethoxysilane dropwise to the suspension, the reaction time is 5h, after the reaction is completed, filter with suction, wash, and dry in a vacuum oven to obtain Black solid powder f-GO.

[0061](2) 0.325 g of silane coupling agent-modified graphene oxide (f-GO) prepared in step (1) was ultrasonically treated for 30 min. and dispersed in acetone, then 33.70 g of bisphenol A epoxy resin was added, and the planet After ball milling (250 rpm) for 6 hours, the masterbatch was obtained. Under vacuum conditions (0.3MPa), the organic solvent was removed, and then 30.97g of curing agent was added and mixed, and cured at high temperature (120°C for 1h, ...

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Abstract

The invention relates to the technical field of polymer-based nanocomposites, and provides a preparation method of a functionalized graphene oxide / epoxy resin nanocomposite in order to effectively solve the problems of dispersion and interface of graphene in epoxy resin. The method comprises the steps of performing ultrasonic treatment on the silane coupling agent modified graphene oxide (f-GO) for 20-40 minutes, and dispersing in an organic solvent; adding epoxy resin, and mixing to obtain master batch; removing the organic solvent under a vacuum condition; adding a curing agent and mixing; performing high-temperature curing to obtain the functionalized graphene oxide / epoxy resin nanocomposite. The graphene oxide / epoxy resin nanocomposite prepared by the method provided by the invention can effectively improve the mechanical and thermal properties of epoxy resin, including strength, rigidity, toughness and thermal stability.

Description

technical field [0001] The invention relates to the technical field of polymer-based nanocomposite materials, and more specifically relates to a surface chemical modification of graphene oxide and a preparation method of graphene / polymer nanocomposite materials. Background technique [0002] Graphene is a carbonaceous material in which carbon atoms are closely packed into a single-layer two-dimensional honeycomb lattice structure. It is a crystal with a thickness of only one atom. Since Geim first discovered graphene in 2004, graphene has become Focus in the nanomaterials community. It can be curled into zero-dimensional fullerenes, one-dimensional carbon nanotubes, or stacked into three-dimensional graphite. Graphene is thus the building block from which other carbon allotropes are constructed. Due to the special structure and excellent properties of graphene, such as high Young's modulus and fracture strength (up to 1100GPa and 125GPa, respectively), excellent thermal co...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08L63/02C08L63/04C08K9/06C08K3/04C08G59/42C08G59/50
Inventor 汤龙程万艳君赵丽裴勇兵陈利民吴连斌蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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