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Method for preparing graphene and polyoxometalate composite through electrochemical reduction

A technology of multi-metal oxygen clusters and composite materials, applied in chemical instruments and methods, graphene, inorganic chemistry, etc.

Inactive Publication Date: 2012-10-24
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the chemical reduction method involves the volatile toxic reagent hydrazine hydrate, and the photochemical method is only suitable for small-scale preparations, so it is necessary to develop an environmentally friendly method that can prepare graphene-polymetallic oxygen cluster composites in large quantities. of

Method used

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  • Method for preparing graphene and polyoxometalate composite through electrochemical reduction
  • Method for preparing graphene and polyoxometalate composite through electrochemical reduction
  • Method for preparing graphene and polyoxometalate composite through electrochemical reduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Weigh 2g NaNO 3 And 2g graphite in a 1L beaker, add 96mL concentrated sulfuric acid (mass fraction 98%) under stirring in an ice water bath (300rpm), and stir for 10min; slowly add 12g KMnO with a small medicine spoon 4 Add to it and stir for 1.5h in an ice-water bath; then heat to 35℃ and stir for 2h; slowly add 80mL of water with a dropper for about 30min, then directly pour 200mL of water (600rpm), and then add 10mL of H 2 O 2 (Mass fraction 30%), stir for 10min; finally add about 10mL of H 2 O 2 , Until all the manganese compounds in the solution are converted into colorless compounds; centrifuge at 12000rpm for 15min, dialyze to pH 5-6; dilute with water to 1000mL, sonicate for 10min, and centrifuge at 5000rpm for 10min to remove unstripped carbon particles; Centrifuge at 12000 rpm for 1 hour to collect the flocculent viscous material. The collection still contains a lot of water. Add about 200 mL of ethanol, centrifuge, collect the precipitate, and dry it in a vacuum ...

Embodiment 2

[0048] Example 2: Preparation of a mixture of graphene oxide and 12-tungstosilicic acid

[0049] Weigh 100 mg of the graphene oxide prepared in Example 1 and place it in a 250 mL two-neck round bottom flask, add 90 mL of water, and stir with ultrasonic (100W) (300 rpm) for 1 h. The graphene oxide is completely dispersed to obtain an aqueous graphene oxide suspension; Dissolve 2.88 g of 12-tungstosilicic acid in 10 mL of water, add dropwise to the graphene oxide aqueous suspension under the combined action of ultrasound and stirring; after the dropwise addition, continue to ultrasonically stir for 1 hour; add ice to cool the entire process. In the mixed solution, the concentration of graphene oxide is 1 mg / mL and the concentration of 12-tungstosilicic acid is 10 mM.

Embodiment 3

[0050] Example 3: Preparation of a mixture of graphene oxide and 12-tungstosilicic acid

[0051] Weigh 100 mg of the graphene oxide prepared in Example 1 and place it in a 250 mL two-neck round bottom flask, add 90 mL of water, and stir with ultrasonic (100W) (300 rpm) for 1 h. The graphene oxide is completely dispersed to obtain an aqueous graphene oxide suspension; Dissolve 5.76 g of 12-tungstosilicic acid in 10 mL of water, add dropwise to the graphene oxide aqueous suspension under the combined action of ultrasound and stirring; after the addition, continue to stir with ultrasound for 1 hour; add ice to cool the entire process. In the mixed solution, the concentration of graphene oxide is 1 mg / mL, and the concentration of 12-tungstosilicic acid is 20 mM.

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Abstract

The invention relates to a method for reduction of graphene oxide by using a polyoxometalate as an electro-catalyst and for preparation of a graphene and polyoxometalate composite. The prepared composite is a powder material with a porous structure and has potential application values in the aspects like catalysis and electrode materials for a lithium ion battery and an electrochemical capacitor. The method comprises a first step of preparation of graphene oxide, a second step of preparation of mixed liquor of graphene oxide and the polyoxometalate, a third step of electrochemical reduction of graphene oxide by the polyoxometalate, a fourth step of separation of the graphene and polyoxometalate composite, etc. According to the invention, electrons are transferred from a working electrode to the polyoxometalate at first, so the polyoxometalate obtains the electrons and is reduced into a heteropoly blue; then the electrons are transferred from the heteropoly blue to graphene oxide, so graphene oxide is reduced and the heteropoly blue loses the electrons and turns into initial polyoxometalate. During the process of reduction, the polyoxometalate can spontaneously adhere onto the surface of produced graphene so as to form the graphene and polyoxometalate composite.

Description

Technical field [0001] The invention belongs to the field of chemicals and materials, and specifically relates to a method for reducing graphene oxide using polymetallic oxygen clusters as electrocatalysts and preparing graphene and polymetallic oxygen cluster composite materials. The obtained materials are used in catalysis, lithium ion batteries and electrochemistry. The electrode material of the capacitor has potential application value. Background technique [0002] Graphene is a new type of two-dimensional nano-carbon material, which is made of sp 2 The hybrid carbon atoms are arranged in a hexagon to form a single-layer atomic crystal with a periodic honeycomb structure, with a thickness of only 0.35nm, which is the thinnest known two-dimensional material (AKGeim, KSNovoselov, Nat. Mater., 2007, 6, 183). The special single atomic layer structure of graphene gives it many excellent properties. For example, graphene is currently the strongest material in the world (Young's m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B33/20C01B25/26C01B32/184
Inventor 王珊李昊龙吴立新
Owner JILIN UNIV
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