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Method for preparing large-flake-diameter graphene oxide from natural flaky graphite

A flake graphite and graphene technology, applied in the field of preparing large-diameter graphene oxide from natural flake graphite, can solve problems such as the influence of the flake diameter, the destruction of the crystal structure, the fracture of carbon-carbon bonds, etc., and achieve a large flake diameter and a wide range of uses. Effect

Active Publication Date: 2015-04-29
SOUTHWEAT UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, during the ultrasonic dispersion process, high-energy ultrasonic waves will cause huge damage to the crystal structure of graphene oxide, resulting in the breakage of its carbon-carbon bonds. Even large-diameter graphite oxide is difficult to prepare by ultrasonic exfoliation. Graphene oxide, and the prepared graphene oxide will also contain more structural defects, so the quality, performance and use of the prepared graphene oxide will be affected by more structural defects and smaller sheet diameters
[0007] So far, there is no public report on the successful preparation of large flakes of graphene oxide by oxidation and exfoliation of large flakes of graphite.

Method used

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  • Method for preparing large-flake-diameter graphene oxide from natural flaky graphite
  • Method for preparing large-flake-diameter graphene oxide from natural flaky graphite
  • Method for preparing large-flake-diameter graphene oxide from natural flaky graphite

Examples

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Effect test

example 1

[0034] The method for preparing large-diameter graphene oxide with natural flake graphite comprises steps as follows:

[0035] 1) preparation of graphite oxide suspension; choosing carbon content is 99.5%, and particle size is 200 purpose natural flaky graphite as raw material, adopts improved Hummers method to prepare graphite oxide, promptly according to flaky graphite: the ratio of concentrated sulfuric acid=1Kg: 25L , slowly add natural flake graphite into an acid-resistant reactor filled with concentrated sulfuric acid, fully stir for 30 minutes under ice bath conditions; Potassium acid potassium was slowly added to the above reactor, and stirred for 5 hours at 35°C; finally, 10% hydrogen peroxide and deionized water were slowly added to the reactor in turn, so that the temperature in the reactor was controlled at 60-100°C until There is no longer gas generation in the reactor and the temperature is constant. After adding an appropriate amount of 5% dilute hydrochloric ac...

example 2

[0039] The basic steps of this example are the same as Example 1, the difference lies in:

[0040] Step 1) process graphite oxide suspension; select carbon content as 99.9%, and the natural flake graphite of particle size is 150 objects as raw material, adopts improved Hummers method to prepare graphite oxide, then adds deionized water to obtain graphite oxide solid content is 1 % graphite oxide suspension;

[0041] Step 2) mixing the graphite oxide suspension with deionized water at a volume ratio of 1:50, using a high-speed dispersing homogenizer to stir for 10 min at a speed of 8000 rpm to obtain a large-diameter graphite oxide dispersion mother liquor; and then using Centrifugation removes impurities in the large-diameter graphite oxide dispersion mother liquor to obtain a concentration of 0.2g L -1 Graphene oxide dispersion.

[0042] Such as image 3 Shown, is the 0.2g L that example 2 prepares -1 The photo of the graphene oxide dispersion state, the graphene oxide disp...

example 3

[0044] The basic steps of this example are the same as Example 1, the difference lies in:

[0045] Step 1) processing graphite oxide suspension; choosing carbon content is 98%, and particle size is 100 purpose natural scaly graphites as raw material, adopts improved Hummers method to prepare graphite oxide, then adds deionized water to obtain graphite oxide solid content is 5 % graphite oxide suspension;

[0046] Step 2) The graphite oxide suspension and deionized water are mixed according to the volume ratio of 1:2, and the high-speed dispersing homogenizer is used to stir for 5 minutes at a speed of 10,000 rpm to obtain a large-diameter graphene oxide dispersion mother liquor ; Remove impurities in the large-diameter graphene oxide dispersion mother liquor through flotation, and prepare a concentration of 2g L -1 Graphene oxide dispersion.

[0047] Such as Figure 5 Shown, is the 2g L that example 3 prepares -1 The photo of the state of the graphene oxide dispersion, the...

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Abstract

The invention discloses a method for preparing large-flake-diameter graphene oxide from natural flaky graphite. The method comprises the following steps: 1) preparing graphite oxide from natural flaky graphite with the carbon content of 95-99.9%, and adding deionized water to obtain a graphite oxide suspension; 2) adding deionized water into the graphite oxide suspension, and stripping with a high-speed dispersing and homogenizing machine to obtain a large-flake-diameter graphene oxide dispersed mother solution; and removing impurities in the large-flake-diameter graphene oxide dispersed mother solution by a gravity impurity removal process to obtain the large-flake-diameter graphene oxide. The natural flaky graphite is used as the raw material to prepare the graphite oxide; the high-speed dispersing and homogenizing engine is adopted to strip and disperse the graphite oxide, thereby preventing the high-energy ultrasonic waves from destroying the graphene oxide crystal structure in the stripping and dispersion process; and the prepared large-flake-diameter graphene oxide has the advantages of high purity, large flake diameter and wide application range. The method has the advantages of short technical process and high product quality, and is beneficial to popularization and application.

Description

technical field [0001] The invention relates to a method for preparing large-diameter graphene oxide from natural flake graphite, and belongs to the field of preparation and application of novel carbon nanomaterials, functionalized graphene materials and composite materials. Background technique [0002] To prepare graphene oxide from natural graphite raw materials, it is necessary to first prepare graphite oxide by oxidation treatment on natural graphite raw materials, and then exfoliate graphite oxide to obtain graphene oxide. [0003] In the process of oxidizing natural graphite raw materials to obtain graphite oxide, oxygen-containing functional groups such as carboxyl, hydroxyl and epoxy groups are inserted into the original graphite structure layer. The oxidation treatment method used is usually the Hummers method, etc., that is, the graphite raw material is placed in a concentrated sulfuric acid and nitrate system, and the KMnO 4 As an oxidizing agent, react in a low...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 孙红娟鲜海洋彭同江汪建德
Owner SOUTHWEAT UNIV OF SCI & TECH
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