Separation method of graphene oxide different in sizes in graphene oxide preparation process

A separation method and graphene technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of mixed sizes, no distribution rules, and reduced application value of graphene products, and achieve simple methods and equipment. Low requirements, beneficial to industrialized production

Active Publication Date: 2014-08-20
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is a common shortcoming in various existing redox methods for preparing graphene, that is, even if the same process flow and the same process conditions are use

Method used

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  • Separation method of graphene oxide different in sizes in graphene oxide preparation process
  • Separation method of graphene oxide different in sizes in graphene oxide preparation process
  • Separation method of graphene oxide different in sizes in graphene oxide preparation process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] In the first step, graphite oxide is prepared by the improved Hummers method in the redox method:

[0060] Take by weighing 1g flake graphite and 0.5g sodium nitrate and place in a 250mL round-bottomed flask, measure 23mL of concentrated sulfuric acid with a weight percent concentration of 98% and add it to the round-bottomed flask, add a magnet, place the round-bottomed flask in In an ice-water bath, stir for 30 minutes, weigh 3g of potassium permanganate and add it to the reactor, and continue stirring for 1 hour. After the reaction is completed, transfer the reactor to a water bath at 35°C, continue stirring for 30 minutes, and measure 50 mL of Distilled water was added to the round bottom flask, then the round bottom flask was transferred to an oil bath at 98°C, stirring was continued for 15 min, and 140 mL of distilled water and 30% H 2 o 2 10 mL, after the reaction system finally turns bright yellow, centrifuge, then wash with 500 mL of hydrochloric acid with a m...

Embodiment 2

[0072] In the first step, graphite oxide is prepared by the improved Hummers method in the redox method:

[0073] With embodiment 1;

[0074] The second step is the preparation of graphene oxide with mixed size and no regular distribution:

[0075] Weigh 0.1g of the graphite oxide product prepared in the first step and place it in a 250mL flask, add 150mL of ethanol, place the flask in a 120Hz ultrasonic cleaner for 1h, remove the solvent, and the obtained precipitate is cGO, which is optically microscope photo as Image 6 As shown, it is an unseparated graphene oxide precipitate with mixed sizes and no regular distribution;

[0076] The third step is the separation of graphene oxide of different sizes:

[0077] (1) The dispersion liquid formed by adding the Graphene Oxide Precipitation with mixed size and no regularity of distribution in the size obtained in the second step and adding 150mL solvent is left standing in the flask for 3h;

[0078] (2) by slowly pouring out t...

Embodiment 3

[0085] In the first step, graphite oxide is prepared by the improved Hummers method in the redox method:

[0086] With embodiment 1;

[0087] The second step is the preparation of graphene oxide with mixed size and no regular distribution:

[0088] Weigh 0.1g of the graphite oxide product prepared in the first step and place it in a 250mL flask, add 150mL of a mixture of ethanol, methanol and isopropanol in any volume ratio, and place the flask in a 120Hz ultrasonic cleaner for 1h , remove the solvent, the obtained precipitate is cGO, its optical microscope picture is as follows Figure 11 As shown, it is an unseparated graphene oxide precipitate with mixed size and no regular distribution;

[0089] The third step is the separation of graphene oxide of different sizes:

[0090] (1) The dispersion liquid formed by adding the Graphene Oxide Precipitation with mixed size and no regularity of distribution in the size obtained in the second step and adding 150mL solvent is left ...

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Abstract

The invention provides a separation method of graphene oxide different in sizes in a graphene oxide preparation process, and relates to graphene oxide preparation. According to the separation method, graphene oxide prepared by using an oxidation reduction method is separated according to difference of dispersibility of the graphene oxide different in sizes in a solvent so as to obtain the following graphene oxide different in sizes: precipitates B-COSs1 which are graphene oxide products, the sizes of which are greater than 25 micrometers, precipitates GOSs2 which are graphene oxide products, the sizes of which are greater than 15 micrometers and are less than or equal to 25 micrometers, precipitates GOSs3 which are graphene oxide products, the sizes of which are greater than 5 micrometers and less than or equal to 15 micrometers, and precipitates F-COSs4 which are graphene oxide products, the sizes of which are less than or equal to 5 micrometers. The separation method can be used for overcoming the defects that the graphene oxide products which are prepared by using the conventional various oxidation reduction methods and different in sizes are completely mixed and irregular in distribution.

Description

technical field [0001] The technical solution of the present invention relates to the preparation of graphene oxide, specifically a method for separating graphene oxide of different sizes in the preparation of graphene oxide. Background technique [0002] Graphene is a transparent material with a single atomic layer and a two-dimensional network structure developed in the past ten years. It has good electrical conductivity, thermal conductivity, light transmission, and better mechanical strength than other existing materials. It is prefabricated The best material for ladders. Since the first graphene sheet was obtained experimentally in 2004, its applications in biology, medicine, optoelectronic materials, semiconductors and conductors have been unprecedentedly developed. Due to the excellent properties of graphene, it is predicted that the 21st century The most important new materials. At present, the methods for preparing graphene include mechanical exfoliation, vapor de...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/198
Inventor 章文军邹雪锋李焕荣候静菊赵金风刘树亭冯宝龙
Owner HEBEI UNIV OF TECH
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