Method for catalytic reduction of graphene oxide

A technology of graphene and stone oxide, applied in the field of catalytic reduction of graphene oxide, which can solve the problems of poor compatibility, limited use, and influence on the physical and chemical properties of graphene, and achieve the effect of mild reaction conditions and reduced defects

Inactive Publication Date: 2015-05-27
JIANGSU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Prior to the present invention, previous work mainly used hydrazine hydrate and its derivatives as reducing agents to reduce graphene oxide, but hydrazine hydrate and its derivatives are highly toxic and volatile, and cannot be used on a large scale , and the reduced graphene will be doped with many nitrogen atoms, which will affect the physical and chemical properties of graphene
There is also research on the use of hydrogen iodide/acetic acid mixed system to reduce graphene oxide, but hydrogen iodide is extremely corrosive, which limits the use of this method
Sodium borohydride (NaBH 4 ), ascorbic acid (VC), etc. are used as

Method used

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  • Method for catalytic reduction of graphene oxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of graphene oxide aqueous solution:

[0024] Dissolve 1 mg of graphene oxide into 20 mL of water, disperse and dissolve with 50W ultrasonic to obtain 0.05 mg / mL graphene oxide aqueous solution;

[0025] (2) Add CoCl 2 Solution:

[0026] 2mL of 10 -2 mol / L CoCl 2 The solution is added into the graphene oxide aqueous solution to form a flocculent suspension.

[0027] (3) Add NH 3 BH 3 :

[0028] Add 1 mL of 50 mg / mL NH 3 BH 3 , a black precipitate was obtained, and the size of the metal particles was 2-5nm.

[0029] (4) washing and purifying graphene:

[0030] The black precipitate in step 3 was centrifuged, washed three times with 1 mL of 10% hydrochloric acid, and three times with deionized water, and freeze-dried to obtain reduced graphene oxide powder with a reduction efficiency of 42%.

Embodiment 2

[0032] (1) Preparation of graphene oxide aqueous solution:

[0033] Dissolve 1mg of graphene oxide into 1mL of water, disperse and dissolve with 50W ultrasonic to obtain 1mg / mL graphene oxide aqueous solution;

[0034] (2) Add NiCl 4 Solution:

[0035] 10mL of 10 -4 mol / L NiCl 4 The solution is added into the graphene oxide aqueous solution to form a flocculent suspension.

[0036] (3) Add NH 3 BH 3 :

[0037] Add 2 mL of 25 mg / mL NH 3 BH 3 , a black precipitate was obtained, and the size of the metal particles was 2-5nm.

[0038] (4) washing and purifying graphene:

[0039] The black precipitate in step 3 was centrifuged, washed 3 times with 2 mL of 5% hydrochloric acid, and then 3 times with deionized water, and freeze-dried to obtain reduced graphene oxide powder with a reduction efficiency of 45%.

Embodiment 3

[0041] (1) Preparation of graphene oxide aqueous solution:

[0042] Dissolve 1mg of graphene oxide into 5mL of water, disperse and dissolve with 50W ultrasonic to obtain 0.2mg / mL graphene oxide aqueous solution;

[0043] (2) Add Co(NO 3 ) 2 Solution:

[0044] 5mL of 10 -2 mol / L Co(NO 3 ) 2 The solution is added into the graphene oxide aqueous solution to form a flocculent suspension.

[0045] (3) Add NH 3 BH 3 :

[0046] Add 5 mL of 10 mg / mL NH 3 BH 3 , a black precipitate was obtained, and the size of the metal particles was 2-5nm.

[0047] (4) washing and purifying graphene:

[0048] The black precipitate in step 3 was centrifuged, washed 3 times with 5 mL of 2% hydrochloric acid, and then 3 times with deionized water, and freeze-dried to obtain reduced graphene oxide powder with a reduction efficiency of 50%.

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Abstract

The invention provides a method for catalytic reduction of graphene oxide. The method comprises the following steps: firstly, adding a metal salt solution into a graphene oxide water solution based on a salting-out effect of the graphene oxide to form a cotton-like suspended substance; adding NH3BH3 and catalyzing hydrolysis of the NH3BH3 by utilizing reduced metal particles at room temperature so as to release nascent hydrogen atoms with high reducibility on the surface of the graphene oxide; reducing the graphene oxide by utilizing the hydrogen atoms; and finally removing the metal particles by means of acid washing to obtain graphene. The method disclosed by the invention is used for reducing the graphene oxide without using compounds such as hydrazine hydrate, derivatives of the hydrazine hydrate, hydrogen iodide and the like with high toxicity, high volatility and high corrosivity as a reducing agent and has the characteristics of being environment-friendly and safe; compared with a metal powder/hydrochloric acid reduction system, the method is relatively high in reduction efficiency; meanwhile, the method can be implemented at room temperature, the reaction condition is mild and generation of defects of the graphene during reduction is reduced.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for catalytically reducing graphene oxide. Background technique [0002] Graphene has excellent electrical conductivity, extremely high strength and good light transmission, and its appearance is expected to trigger a revolution in semiconductors and other fields. At present, there are many methods for preparing graphene, including mechanical separation method, chemical redox method, epitaxial growth method, chemical vapor deposition (CVD) and so on. The chemical redox method is to oxidize and exfoliate natural flake graphite in an aqueous solution to obtain graphene oxide, and then add a reducing agent to remove the oxidation functional group of graphene oxide to obtain reduced graphene oxide (graphene). Compared with several other methods, the chemical redox method has the advantages of simple process and low cost. [0003] Graphene oxide can be synt...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 卓其奇张一萍堵晴川晏超
Owner JIANGSU UNIV OF SCI & TECH
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