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Preparation method of noble metal-graphene nanometer composite

A technology of nanocomposites and noble metals, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, chemical/physical processes, etc., to achieve excellent electrocatalytic redox and good dispersion effects

Inactive Publication Date: 2010-08-11
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Sonoelectrochemistry has been successfully used in the preparation of nanomaterials, but the preparation of metal-graphene nanocomposites by this method or similar methods has not been reported in the literature so far.

Method used

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Embodiment 1

[0024] Embodiment 1. can be in the preparation of the PDDA functionalized graphene of stable dispersion in aqueous phase

[0025] According to the method of Hummers, powdered graphite is oxidized to obtain graphene oxide, which is then dispersed in water to form a brownish-yellow solution, and the unstripped graphene oxide is removed by centrifugation after peeling and dispersing under ultrasound for 2 hours. Add PDDA (volume ratio: 200:1) to the mixture, stir for 30min, add hydrazine hydrate (volume ratio to graphene oxide aqueous solution: 200:1), and react at 90°C for 24 hours to obtain polydiallyl dimethyl chloride The graphene aqueous solution functionalized with ammonium chloride was centrifuged and concentrated for later use.

Embodiment 2

[0026] Embodiment 2. The preparation of the PVP functionalized graphene that can be stably dispersed in aqueous phase

[0027] Change the "polydiallyldimethylammonium chloride" in Example 1 to "polyvinylpyrrolidone", and the other preparation conditions are the same as in Example 1 to obtain a product similar to Example 1.

Embodiment 3

[0028] Embodiment 3. The preparation of palladium-graphene nanocomposite

[0029] Palladium-graphene nanocomposites were prepared by sonoelectrochemical method. First, 2 mL of H 2 PdCl 4 (56.5mmol / L) and 2mL of KNO 3 solution (1mol / L) was added to 60mL of polydiallyldimethylammonium chloride (7.5g·L -1 ) aqueous solution; add 2 mL of 0.5 mg / mL PDDA-dispersed graphene aqueous solution, and then adjust the pH value of the solution to 6.5 with 0.1 mol / L NaOH or HCl. Fully stir and disperse, the current pulse time is 0.5s, the current off time is 0.5s, the ultrasonic pulse time is 0.3s, and the current density is 25mA cm -2 , under the condition of ultrasonic intensity 20W, react for 1h. The obtained dark brown solution was centrifuged, washed several times with ultrapure water, concentrated by centrifugation and then used for later use. The morphology and structural characterization of the product can be seen in figure 1 a, c shown.

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Abstract

The invention provides a preparation method of a noble metal-graphene nanometer composite, which comprises the steps of: oxidizing powdered graphite to prepare graphene oxide by oxidizing potassium permanganate; dispersing the graphene oxide in water; ultrasonically stripping a dispersed graphene oxide piece which is formed in water solution; reducing the graphene oxide piece with hydrazine hydrate under the existence of surface active agent to obtain graphene water solution which can be stably dispersed in water phase; centrifugally concentrating the graphene water solution; adding noble metal prodromic salt and electrolyte salt into surface active agent-containing water solution; adding water phase-dispersed graphene in proportion; adjusting PH value; reacting by means of ultrasonic electrochemistry under the density of the constant current and the intensity of ultrasound; centrifugally separating with high speed; and washing with ultrapure water to prepare the noble metal-graphene nanometer composite. The method has the advantages of convenience, speediness and controllability, etc. The prepared graphene nanometer composite has good dispersibility in water, can be stably existed for a long term, and has good electro-catalysis redox characteristic to organic matter.

Description

technical field [0001] The invention relates to a preparation method of a metal-graphene nanocomposite. Background technique [0002] Nanomaterials refer to materials that have at least one dimension in the three-dimensional space in the nanoscale range (1-100nm) or are composed of them as basic structural units. Nanomaterials have unique and excellent optical, electrical, thermal and mechanical properties, showing attractive application prospects, such as the excellent catalytic performance of nano-noble metals. Graphene is a carbon nanomaterial in which carbon atoms are tightly packed into a single-layer two-dimensional honeycomb lattice structure, which has excellent crystallinity and electrical properties (see: Geima K, Novoselooks. The rise of graphene, Nature Materials, 2007 , 6, 183-191.). The theoretical research on graphene has a history of more than 60 years, but it was not until 2004 that two-dimensional graphene crystals that can exist stably were synthesized (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/42B01J37/34H01M4/92
CPCY02E60/50
Inventor 朱俊杰石建军
Owner NANJING UNIV
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