Preparation method of modified graphene

A graphene and modification technology, applied in the field of graphene, can solve the problems of limited number of active reaction sites, insufficient number of branched chains, and inability to achieve graphene sheet monolayer dispersion.

Active Publication Date: 2019-05-10
浙江中科应化科技有限公司
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Problems solved by technology

[0005] Although existing technologies can effectively improve the dispersion of graphene materials in solutions or polymer matrix resins, it is still difficult to achieve complete exfoliation and dispersion of graphene monolayers. The main reason is that graphite oxide synthesized by the Hummers method in a strong acid environment The number of active groups on the surface of graphene and active reaction sites for subsequent chemical modification is limited, which leads to insufficient number of branched chains generated, and the induced steric hindrance effect cannot achieve monolayer dispersion of graphene sheets.

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[0050] The invention provides a method for preparing modified graphene, comprising: S1) dispersing graphene oxide in tetrahydrofuran to obtain a graphene oxide colloidal solution; S2) mixing the graphene oxide colloidal solution with an acid anhydride compound, Irradiating to obtain modified graphene oxide; the acid anhydride compound includes a diformic anhydride structure or isatoic anhydride structure; S3) after hydrolyzing the modified graphene oxide, carboxyl-modified graphene is obtained.

[0051]The present invention has no special limitation on the sources of all raw materials, which can be commercially available or self-made. Wherein, the graphene oxide is preferably graphene oxide obtained by Hummers method oxidation, more preferably graphene oxide obtained by Hummers graphite oxide or graphene-based materials.

[0052] Disperse graphene oxide in tetrahydrofuran to obtain a graphene oxide colloidal solution; the dispersion method in the present invention is preferabl...

Embodiment 1

[0110] First, the graphite or graphene material is oxidized by the Hummers method to obtain graphene oxide. 0.2 g of graphene oxide was ultrasonically dispersed in 100 ml of tetrahydrofuran solution for 15 minutes, and a graphene oxide colloidal solution was obtained after ultrasonic dispersion.

[0111] Then add 0.4 g of maleic anhydride to the graphene oxide colloidal solution, and ultrasonically disperse for 15 minutes. The graphene oxide / maleic anhydride / THF mixture was irradiated in a Co-60 source with a radiation dose of 40 kGy and a dose rate of 25 Gy / min. The modified graphene oxide is obtained after the insoluble matter in the mixed solution after irradiation is suction-filtered, washed to neutrality and dried.

[0112] Weigh 0.2 g of modified graphene oxide, soak in 1 mmol / L KOH aqueous solution and 1 mmol / L hydrochloric acid solution for 5 minutes and 10 minutes respectively for hydrolysis. After the product was suction-filtered and washed with deionized water to ...

Embodiment 2

[0118] First, the graphite or graphene material is oxidized by the Hummers method to obtain graphene oxide. 0.2 g of graphene oxide was ultrasonically dispersed in 100 ml of tetrahydrofuran solution for 15 minutes, and a graphene oxide colloidal solution was obtained after ultrasonic dispersion.

[0119] Then add 0.4 g of maleic anhydride to the graphene oxide colloidal solution, and ultrasonically disperse for 15 minutes. The graphene oxide / maleic anhydride / THF mixture was irradiated in a Co-60 source with a radiation dose of 40 kGy and a dose rate of 25 Gy / min. The modified graphene oxide is obtained after the insoluble matter in the mixed solution after irradiation is suction-filtered, washed to neutrality and dried.

[0120] Weigh 0.2 g of modified graphene oxide, soak in 1 mmol / L KOH aqueous solution and 1 mmol / L hydrochloric acid solution for 5 minutes and 10 minutes respectively for hydrolysis. After the product was suction-filtered and washed with deionized water to ...

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Abstract

The invention provides a preparation method of modified graphene. The preparation method of the modified graphene comprises the following steps: S1) dispersing graphene oxide in tetrahydrofuran to obtain a graphene oxide colloidal solution; S2) mixing the graphene oxide colloidal solution with an anhydride compound, and irradiating the mixture to obtain modified graphene oxide, wherein the anhydride compound comprises a dicarboxylic anhydride structure or an isatoic anhydride structure; and S3) hydrolyzing the modified graphene oxide to obtain carboxyl modified graphene. Compared with the prior art, the preparation method of the modified graphene has the advantages that a chemical modification method and an irradiation modification method are combined and are synergistic, the graphene oxide is grafted by the anhydride compound, and active carboxyl reaction sites with larger density can be formed on the surface of graphene after hydrolysis.

Description

technical field [0001] The invention belongs to the technical field of graphene, in particular to a preparation method of modified graphene. Background technique [0002] Since the graphene material came out in 2004, it has quickly aroused widespread interest in academia and industrial applications. As a special carbon material with a single-layer structure, graphene has a large specific surface area and excellent thermal conductivity, electrical conductivity, strength, toughness and other properties. However, in practical applications, whether it is used independently or combined with other materials, one of the key problems faced by graphene is dispersion. Due to the strong π-π interaction between graphene sheets, graphene sheets are extremely prone to irreversible agglomeration. [0003] At present, the Hummers method is used to first prepare single-layer graphene oxide through strong acid oxidation and ultrasonic mechanical exfoliation, and then chemical reduction is t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/194C01B32/184
Inventor 邓鹏飏柳美华尹园郑春柏魏巍张依帆
Owner 浙江中科应化科技有限公司
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