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Method for rapidly preparing monolayer graphene oxide through one-pot method

A graphene and single-layer technology, applied in the field of nanomaterials, can solve problems such as poor product quality, and achieve the effects of easy operation, less raw material consumption, and short preparation time

Active Publication Date: 2015-02-18
ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The one-step method has high production efficiency and less energy consumption of raw materials, but the product quality is not as good as the two-step method

Method used

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  • Method for rapidly preparing monolayer graphene oxide through one-pot method
  • Method for rapidly preparing monolayer graphene oxide through one-pot method
  • Method for rapidly preparing monolayer graphene oxide through one-pot method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Graphite with a particle size of 0.5 μm and concentrated sulfuric acid was stirred, mixed and infiltrated at room temperature for 5 minutes, potassium persulfate and phosphorus pentoxide were added, and the temperature of the mixture was slowly raised to 30°C and continued to stir for 10 hours. Then the reaction solution was lowered to 20°C, a certain amount of concentrated sulfuric acid was added and potassium permanganate was added slowly, the reaction was carried out at 20°C for 0.5h, and the temperature was raised to 50°C to continue the reaction for 2h. After the reaction is completed, slowly pour the resulting product into iced deionized water for dilution. After stabilization, add hydrogen peroxide and let it stand for a period of time. The precipitate is washed repeatedly with 1mol / L dilute hydrochloric acid and deionized water, and centrifuged to obtain a single-layer oxidation solution. Graphene, which is dispersed into a low-to-high multi-gradient graphene oxi...

Embodiment 2

[0025] Graphite with a particle size of 40 μm and concentrated sulfuric acid was stirred, mixed and infiltrated at room temperature for 0.5 h, potassium persulfate and phosphorus pentoxide were added, the temperature of the mixture was slowly raised to 80° C., and stirring was continued for 2 h. Then the reaction solution was lowered to 28°C, a certain amount of concentrated sulfuric acid was added and potassium permanganate was added slowly, the reaction was carried out at 37°C for 1.5h, and the temperature was raised to 50°C to continue the reaction for 3.5h. After the reaction is completed, slowly pour the resulting product into iced deionized water for dilution. After stabilization, add hydrogen peroxide and let it stand for a period of time. The precipitate is washed repeatedly with 1mol / L dilute hydrochloric acid and deionized water, and centrifuged to obtain a single-layer oxidation solution. Graphene, which is dispersed into a low-to-high multi-gradient graphene oxide s...

Embodiment 3

[0028] Graphite with a particle size of 100 μm and concentrated nitric acid was stirred, mixed and infiltrated at room temperature for 0.5 h, potassium permanganate and potassium phosphate were added, the temperature of the mixture was slowly raised to 50° C., and stirring was continued for 4 h. Then the reaction solution was lowered to 25°C, a certain amount of concentrated nitric acid was added and potassium ferrate was added slowly, the reaction was carried out at 30°C for 2h, and the temperature was raised to 50°C to continue the reaction for 4h. After the reaction is completed, slowly pour the resulting product into iced deionized water for dilution. After stabilization, add hydrogen peroxide and let it stand for a period of time. The precipitate is washed repeatedly with 1mol / L dilute hydrochloric acid and deionized water, and centrifuged to obtain a single-layer oxidation solution. Graphene, which is dispersed into a low-to-high multi-gradient graphene oxide solution wit...

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Abstract

The invention discloses a method for rapidly preparing monolayer graphene oxide through a one-pot method. The method comprises the following steps: stirring, mixing and infiltrating graphite and concentrated acid or the mixed acid of the graphite and concentrated acid for 5 min to 1h at 20-50 DEG C, adding a strong oxidant and an intercalator for intercalating, slowly heating a mixed solution to 30-100 DEG C, and consistently stirring for 1-10 h; cooling a reaction solution to 20-37 DEG C, supplementing a certain amount of the concentrated acid or the mixed acid of the graphite and concentrated acid, slowly adding the strong oxidant, reacting for 0.5-3 h at 20-37 DEG C, heating to the temperature which is 10 DEG C lower than a safe temperature, further reacting for 2-8 h for oxidizing and stripping a graphite sheet layer, after completion of reaction, slowly pouring an obtained product into icy deionized water for diluting, adding hydrogen peroxide after the icy deionized water is stable, performing standing, cleaning precipitate with 1mol / L of dilute hydrochloric acid and deionized water repeatedly, and centrifuging to obtain the monolayer graphene oxide. The method is simple and controllable in preparation process and short in time consumption and low in energy consumption; by the one-pot method, the grapheme can be rapidly and directly converted to the monolayer graphene oxide.

Description

technical field [0001] The invention relates to the field of nanomaterials, in particular to a method for rapidly preparing single-layer graphene oxide in one pot. Background technique [0002] In 2004, the research group of Professor A.K. Geim of the University of Manchester successfully prepared graphene by mechanical exfoliation, overturning the theory that the perfect two-dimensional crystal structure cannot exist stably at non-absolute zero temperature. Then graphene's excellent mechanical properties, electrical properties, thermal properties, and optical properties were discovered one after another. Graphene has a large theoretical specific surface area, coupled with the excellent performance of the monolithic structure, carbon-based materials with graphene as the source material have been greatly developed and applied. [0003] The preparation of graphene by oxidation-reduction method is considered to be the most important method to realize the industrial produc...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 高超彭蠡郑耀臣许震魏杨扬刘峥
Owner ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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