Method for preparing graphene by reducing graphene oxide by utilizing reducing agent

A graphene and reducing agent technology, applied in graphene, nano-carbon and other directions, can solve the problems of long reaction time, complex process, high toxicity, etc., and achieve the effects of reducing preparation cost, rapid reaction process and mild reaction conditions

Inactive Publication Date: 2012-11-28
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the problems of complex process, long reaction time and high toxicity in the existing method for preparing graphene by reducing graphene oxide with reducing agent, and provide a method for preparing graphene by reducing graphene oxide with reducing agent

Method used

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  • Method for preparing graphene by reducing graphene oxide by utilizing reducing agent
  • Method for preparing graphene by reducing graphene oxide by utilizing reducing agent
  • Method for preparing graphene by reducing graphene oxide by utilizing reducing agent

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specific Embodiment approach 1

[0007] Specific embodiment 1: This embodiment is a method for preparing graphene by reducing graphene oxide with a reducing agent, which is specifically completed according to the following steps: 1. Ultrasonic dispersion: adding deionized water to graphene oxide at a frequency of 80KHz~100KHz ultrasonic wave assisted by ultrasonic dispersion for 20min~40min, then a uniform graphene oxide aqueous dispersion solution with a concentration of 4mg / L~8mg / L will be obtained; 2. Reduction: uniform oxidation with a concentration of 4mg / L~8mg / L Add sodium tellurium hydride aqueous solution to the graphene aqueous dispersion solution, and stir for 1h~3h at room temperature and stirring speed of 200r / min~250r / min, and then separate by suction filtration. The solid obtained is washed with sodium borohydride aqueous solution for 2~8 After washing with deionized water for 1 to 5 times, and then separating by suction filtration, the washed solid is obtained, and then the washed solid is dried ...

specific Embodiment approach 2

[0011] Specific embodiment two: this embodiment is different from specific embodiment one in that: the graphene oxide described in step one is prepared according to the following steps: add 98% sulfuric acid and mass fraction to 500 mesh natural flake graphite Phosphoric acid with a fraction of 83%~98%, add potassium permanganate, react at room temperature for 1.5h~2.5h, then react in a water bath at a temperature of 35℃ for 20h~28h, then add deionized water and mass fraction It is 27.5%~35% hydrogen peroxide, and then centrifuged at a centrifugal speed of 3000r / min~5000r / min. The lower solid obtained is first washed with 3% hydrochloric acid once, and then washed with deionized water by repeated centrifugation. The obtained supernatant is neutral, and graphene oxide is obtained after washing; the volume ratio of the mass of the 500 mesh natural flake graphite to 98% sulfuric acid is (0.02g~0.03g): 1mL; The volume ratio of the mass of 500 mesh natural flake graphite to the phos...

specific Embodiment approach 3

[0012] Specific embodiment three: this embodiment is different from specific embodiment one or two in that the sodium tellurium hydride aqueous solution described in step two is prepared according to the following steps: adding tellurium powder and sodium borohydride into deionized water, Then in an ice-salt bath and a stirring speed of 150r / min~250r / min, the reaction was stirred for 8h~12h to obtain the sodium tellurium hydride aqueous solution; the mass ratio of the tellurium powder to the sodium borohydride was (1.5~1.6): 1; The mass ratio of the deionized water to sodium borohydride is (18.5-19):1. Others are the same as the first or second embodiment.

[0013] The following tests are used to verify the effect of the present invention:

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Abstract

The invention relates to a method for preparing graphene by reducing graphene oxide by utilizing a reducing agent, relating to a preparation method of graphene. The invention aims at solving problems of complex process, long reaction time and high toxicity in the traditional method for preparing the graphene by reducing the graphene oxide by utilizing the reducing agent. The method comprises the following steps of: 1, dispersing the graphene oxide in deionized water through ultrasonic dispersion to obtain a uniform graphene oxide dispersion aqueous solution; and 2, adding a sodium hydride aqueous solution to carry out reduction, separating, washing, drying and grinding to obtain graphene powder. The method disclosed by the invention has the advantages that 1, high toxicity by using hydrazine hydrate and p-phenylenediamine as catalysts is prevented; 2, reduction conditions are simple, a reaction process is quick, reaction conditions are gentle, no special requirements on devices exist, the preparation cost is reduced, and the preparation period is shortened; and 3, the quality of graphene is high. The invention is mainly applied to preparing the graphene.

Description

Technical field [0001] The invention relates to a method for preparing graphene. Background technique [0002] So far, the main methods of preparing graphene include mechanical peeling method, heating SiC method, epitaxial growth method, organic synthesis method, CVD method, graphite oxide reduction method, etc. Among them, the redox method oxidizes graphite into graphite oxide, and then obtains a single-layer graphene oxide solution under ultrasonic conditions, and then reduces it with a reducing agent to obtain graphene, which has become an effective way to prepare graphene. With its low cost and high yield, it is the best way for industrialized mass production of graphene in the future. Therefore, seeking a mild and efficient reducing agent is the key to realizing mass production of graphene. Currently commonly used reducing agents are hydrazine hydrate, sodium borohydride and p-phenylenediammonium. The above reducing agent takes a long time (> 18 hours) The reaction can...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184
Inventor 孙立国汪成韩春华刘抱张艳红
Owner HEILONGJIANG UNIV
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