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Preparation method of three-dimensional cross-linked graphene foam structure reinforced resin composite material

A technology of resin composite materials and graphene foam, which is applied in the field of preparation of three-dimensional cross-linked graphene foam structure reinforced resin composite materials, can solve the problems of uneven distribution, affecting the performance of composite materials, low effective content of graphene, etc., and achieve performance Excellent, the effect of overcoming self-agglomeration

Inactive Publication Date: 2014-11-19
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation method of graphene / resin composites is mainly the solution mechanical blending method, but when using this method to prepare graphene composites, it is difficult to completely and uniformly disperse the two-dimensional graphene sheets in polymers such as resins. The olefin sheets usually re-agglomerate in the polymer matrix, resulting in an uneven distribution state, which makes the effective content of graphene in the composite material lower than the expected value, thus affecting the properties of the graphene-reinforced resin-based composite material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The graphite oxide aqueous solution was sonicated for 3 hours to prepare 400ml of graphene oxide aqueous solution with a concentration of 1.0mg / ml, and 2g of polyamide-amine was added dropwise, and flocculation quickly appeared, and obvious stratification appeared after standing. After the excess solvent was removed by high-speed centrifugation, the flocs were placed in a mold, pre-frozen at -10°C for 12 hours, and vacuum freeze-dried at -50°C for 24 hours to obtain a porous graphene oxide and polyamide-amine mixture. And heat reaction at 150°C for 12 hours, that is, a porous three-dimensional cross-linked graphene foam structure is formed in the mold, and this structure remains in its original state after ultrasonic dispersion in deionized water for 2 hours.

[0015] Mix epoxy resin, curing agent and accelerator at a mass ratio of 100:70:1, and keep the temperature at 60°C for 30 minutes to reduce the viscosity of the resin and increase its fluidity. Seal the mold so t...

Embodiment 2

[0017] Prepare 50 ml of 2% acetic acid / water mixture, add 0.2 g of chitosan, and stir at 40° C. for 4 h to obtain a transparent chitosan solution. The graphite oxide aqueous solution was ultrasonically treated for 3 hours to prepare 200 ml of graphene oxide aqueous solution with a concentration of 2.0 mg / ml, which was added dropwise to the prepared chitosan solution, and flocculation rapidly occurred. After removing excess solvent by high-speed centrifugation, the flocs were placed in a mold, pre-frozen at -10°C for 12 hours, and vacuum freeze-dried at -50°C for 24 hours to obtain a mixture of porous graphene oxide and chitosan. And heating and reacting at 100° C. for 12 hours, that is, a porous three-dimensional cross-linked graphene foam structure is formed in the mold.

[0018] Seal the mold so that the prepared three-dimensional cross-linked graphene foam structure is in a completely sealed environment, and use a vacuum pump to suck the mold to inhale the thermosetting phe...

Embodiment 3

[0020] The graphite oxide aqueous solution was ultrasonically treated for 4 hours to prepare 100ml of a graphene oxide aqueous solution with a concentration of 4.0mg / mL, and 2g of triethylenetetramine was added dropwise. Flocculation quickly occurred, and obvious stratification appeared after standing. After removing excess solvent by high-speed centrifugation, the flocs were placed in a mold, pre-frozen at -10°C for 12 hours, and vacuum freeze-dried at -50°C for 24 hours to obtain a mixture of porous graphene oxide and triethylenetetramine. And heat reaction at 150°C for 12 hours, that is, a porous three-dimensional cross-linked graphene foam structure is formed in the mold, and this structure remains in its original state after ultrasonic dispersion in deionized water for 2 hours.

[0021] Seal the mold, evacuate the mold and press the resin tank, pour silicone resin into the mold, and then heat it from room temperature to 200°C for 2 hours to cure and form, and obtain a sili...

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Abstract

The invention relates to the field of nano composite material preparation and in particular relates to a preparation method of a three-dimensional cross-linked graphene foam structure reinforced resin composite material. The preparation method comprises the following steps: (1) adding a multiamino compound, forming a flocculate of graphene oxide and the amino compound in a graphene oxide solution, centrifuging, performing freeze-drying and heating for reaction to prepare a three-dimensional cross-linked graphene foam structure; (2) filling the three-dimensional cross-linked graphene foam structure with resin by methods of vacuum pressure or negative pressure flow forming and the like, defoaming, and curing to prepare the three-dimensional cross-linked graphene foam structure reinforced resin composite material. According to the preparation method, the assembled and formed three-dimensional cross-linked graphene foam structure is filled with the resin, so that serious agglomeration phenomenon occurring in a graphene and resin mixing process is effectively avoided and the obtained three-dimensional cross-linked graphene foam structure reinforced resin composite material is excellent in performance.

Description

technical field [0001] The invention relates to a preparation method of a three-dimensional crosslinked graphene foam structure reinforced resin composite material, belonging to the field of nanocomposite material preparation. Background technique [0002] Graphene is a two-dimensional honeycomb crystal structure formed by densely packed carbon atoms, and is the basic structural unit for constructing other dimensional carbon materials (zero-dimensional fullerene, one-dimensional carbon nanotubes, and three-dimensional graphite). The unique crystal structure of graphene endows it with excellent mechanical and electrical properties, and is considered as an ideal reinforcement material for composite materials. Its two-dimensional sheet-like appearance and large specific surface area can produce richer and closer contact with the matrix material, and it has better reinforcement performance than one-dimensional carbon nanotubes. [0003] At present, the preparation method of gra...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08L61/06C08L83/04C08K9/04C08K7/24C08K3/04
Inventor 徐志伟倪亚吴凡陈磊田旭滕堃玥买巍匡丽赟
Owner TIANJIN POLYTECHNIC UNIV
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