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Graphene-surface-grafted free radical polymer composite material, and preparation method and use thereof

A graphene surface, composite material technology, applied in electrical components, electrochemical generators, circuits, etc., can solve the problems of limited performance improvement of secondary batteries, unsuitable for mass production, difficult to control graft content, etc. The preparation method is simple and easy, excellent dispersibility, and high repeatability.

Active Publication Date: 2019-06-14
SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved by the present invention is to overcome the difficulty in controlling the grafting content in the method for grafting the PTMA secondary battery cathode material on the surface of graphene sheet covalently bonded in the prior art, the performance improvement range of the secondary battery is limited, and It is not suitable for defects such as mass production, but provides a graphene surface grafted free radical polymer composite material and its preparation method and use

Method used

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  • Graphene-surface-grafted free radical polymer composite material, and preparation method and use thereof
  • Graphene-surface-grafted free radical polymer composite material, and preparation method and use thereof
  • Graphene-surface-grafted free radical polymer composite material, and preparation method and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0068] Example 1: Synthesis of graphene oxide grafted poly(2,2,6,6-tetramethylpiperidine-4-methacrylate) (GO-g-PTMPM) composite:

[0069] Add 100mg of graphene oxide and 50mL of N-methylpyrrolidone into a 100mL reaction bottle, add 2.25g of TMPM after ultrasonic dispersion, and after bubbling with nitrogen for 30min, add 32.8mg of azobisisobutyronitrile and react at 65°C 48 hours. After the reaction was finished, GO-g-PTMPM with a graft content of 45.4% was obtained by suction filtration, washing and drying.

[0070] FT-IR (cm -1 ):3400(νO-H), 2960(νC-H), 2930(νC-H), 1725(νC=O).

[0071] This example further proves that the graft content of PTMPM grafted on the surface of the graphene oxide sheet can be adjusted by controlling the time of the polymerization reaction.

[0072] attached figure 2 The thermogravimetric curves of GO-g-PTMPM composites obtained by polymerization at 65°C for 3-48h respectively, it can be seen from the figure that as the polymerization reaction t...

Embodiment 2

[0077] Example 2: Synthesis of graphene oxide grafted poly(2,2,6,6-tetramethylpiperidine-4-methacrylate) (GO-g-PTMPM) composite:

[0078] In the reaction bottle of 100mL, add 100mg graphene oxide and 50mL N-methylpyrrolidone, add 2.25g TMPM (molecular weight is 225) after ultrasonic dispersion, pass into nitrogen bubble after 30min, add 16.4mg azobisisobutyronitrile ( The molecular weight is 164), reacted at 65°C for 48 hours. After the reaction was finished, GO-g-PTMPM with a graft content of 30.2% was obtained by suction filtration, washing and drying.

[0079]This example further proves that the graft content of PTMPM grafted on the surface of the graphene oxide sheet can be adjusted by controlling the amount of the initiator.

[0080] Table 2 The graft content of GO-g-PTMPM composites obtained with different initiator dosages

[0081] Monomer to Initiator Molar Ratio

[0082] attached image 3 It is the thermogravimetric curve of the GO-g-PTMPM composite mater...

Embodiment 3

[0083] Example 3: Synthesis of graphene oxide grafted poly(2,2,6,6-tetramethylpiperidine-1-oxyl radical-4-methacrylate) (GO-g-PTMA):

[0084] In the reaction bottle of 250mL, add 100mg GO-g-PTMPM (being specifically the GO-g-PTMPM that graft content is 45.4% among the embodiment 1) and 100mL methyl alcohol, add 30mg disodium edetate and 20mg of sodium tungstate dihydrate, then slowly add 4mL of 30% hydrogen peroxide (density about 1.1). After stirring and reacting for 48h, GO-g-PTMA was obtained by suction filtration, washing and drying.

[0085] FT-IR (cm -1 ):3400(νO-H), 2960(νC-H), 2930(νC-H), 1725(νC=O), 1363(νN-O).

[0086] attached figure 1 The AFM and height distribution diagram of GO on the left, and the AFM and height distribution diagram of GO-g-PTMA on the right, it can be seen that the average thickness of GO sheets is 1.0nm, while the average thickness of GO-g-PTMA is 9nm.

[0087] attached Figure 6 For the electron paramagnetic resonance (ESR) curve of the ...

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Abstract

The invention discloses a graphene-surface-grafted free radical polymer composite material, and a preparation method and a use thereof. The preparation method comprises the following steps: 1) uniformly dispersing graphene in a solvent, uniformly mixing the obtained solution with 2,2,6,6-tetramethyl-4-piperidinyl methacrylate monomer, deoxidizing the obtained solution, uniformly mixing the solution with an initiator, carrying out a reaction for 1-72 h, and carrying out filtration and separation to obtain an intermediate, wherein a mass ratio of the graphene to the monomer to the initiator is 1:(11.25-90):(0.08-0.64), and the graphene is graphene oxide and / or reduced graphene oxide; and 2) uniformly mixing the intermediate, disodium edetate, sodium tungstate and hydrogen peroxide in a solvent, stirring and reacting the obtained mixture, and carrying out filtration and separation to obtain the composite material. The method is simplified, is suitable for mass production, and allows the grafting content of covalent bonds on surface of a graphene sheet to be easily controlled; and when the composite material is applied to cathodes of lithium ion batteries, the obtained secondary batteries have high performances.

Description

technical field [0001] The invention relates to the technical field of organic cathode materials for secondary batteries, in particular to a graphene surface-grafted radical polymer composite material, a preparation method and an application. Background technique [0002] Lithium-ion battery is a secondary battery with excellent characteristics such as high energy density, high open circuit voltage, no memory effect, and long cycle life. It is widely used in consumer electronics, energy storage, and power batteries. The cathode material of lithium-ion batteries is an inorganic compound containing lithium. Lithium-ion batteries used in the 3C industry now mainly use lithium cobalt oxide, lithium manganate or lithium iron phosphate as cathode materials. Although these electrode materials have excellent performance, there are still problems such as low theoretical energy density, non-renewable resources, higher and higher prices, high energy consumption in the manufacturing pro...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F220/36C08F8/06H01M4/36H01M4/583H01M4/62H01M4/60H01M10/0525
CPCY02E60/10
Inventor 黄晓宇李永军刘鹏举张森
Owner SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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