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Preparation method of graphene oxide

A graphene and graphite powder technology, applied in the field of graphene oxide preparation, can solve the problems of low oxidation degree of graphene oxide, increased difficulty in waste liquid treatment, high equipment cost, etc. Good spacing and dispersion

Inactive Publication Date: 2021-05-28
GUANGDONG MORION NANOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The commonly used method to prepare graphene oxide by chemical method is the Hummers method. The principle is to first treat graphene with strong acid to transform it into a graphite interlayer compound, and then add a strong oxidant for deep exfoliation, and adjust the oxidation degree of the product by controlling the reaction time , which is measured by the atomic ratio of C and O; although it is widely used, the oxidation degree of graphene oxide prepared by this process is not high, and the use of excessive KMnO4 increases the difficulty of subsequent waste liquid treatment, so people continue to try Improving the Hummers method, such as the ultrasonic-assisted Hummers method, although this method is convenient and quick, the equipment is expensive and difficult to maintain, which is not conducive to industrialization

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  • Preparation method of graphene oxide

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Effect test

Embodiment 1

[0048] A preparation method of graphene oxide, comprising the steps of:

[0049] Step 1, low-temperature reaction: Mix concentrated sulfuric acid and phosphoric acid with a mass ratio of 5:1 to prepare the mixed acid and pre-cool it to keep its temperature at 0-2°C;

[0050] In this step, its mass fraction of the concentrated sulfuric acid used is 90%, and its mass fraction of concentrated phosphoric acid is 85%;

[0051] Step 2, oxidation reaction: take a certain amount of mixed acid prepared in step 1 and place it in a jacketed reaction kettle, add natural flake graphite powder with a mesh number of 100 meshes according to the mass ratio under an ice-water bath, fully stir and disperse and press Potassium permanganate was added proportionally, fully stirred and reacted for 0.5 hours;

[0052]In this step, the mass ratio of graphite powder, mixed acid, potassium permanganate is 1:40:3;

[0053] Step 3, medium temperature reaction: switch the water in the jacket of the react...

Embodiment 2

[0062] Embodiment 2: a kind of preparation method of graphene oxide comprises the steps:

[0063] Step 1, low-temperature reaction: mix concentrated sulfuric acid and phosphoric acid with a mass ratio of 15:1 to prepare the mixed acid and pre-cool it to keep its temperature at 8-10°C;

[0064] In this step, its mass fraction of the concentrated sulfuric acid used is 98%, and its mass fraction of concentrated phosphoric acid is 95%;

[0065] Step 2, oxidation reaction: take a certain amount of mixed acid prepared in step 1 and place it in a jacketed reactor, add natural flake graphite powder with a mesh number of 5000 meshes according to the mass ratio under the ice-water bath, fully stir and disperse and press Potassium permanganate was added proportionally, fully stirred and reacted for 5 hours;

[0066] In this step, the mass ratio of graphite powder, mixed acid, potassium permanganate is 1:70:5;

[0067] Step 3, medium temperature reaction: switch the water in the jacket ...

Embodiment 3

[0077] A preparation method of graphene oxide, comprising the steps of:

[0078] Step 1, low-temperature reaction: Mix concentrated sulfuric acid and phosphoric acid with a mass ratio of 5:1 to prepare the mixed acid and pre-cool it to keep its temperature at 0-2°C;

[0079] In this step, its mass fraction of the concentrated sulfuric acid used is 90%, and its mass fraction of the concentrated phosphoric acid is 85~95%;

[0080] Step 2, oxidation reaction: take a certain amount of mixed acid prepared in step 1 and place it in a jacketed reactor, add natural flake graphite powder with a mesh number of 325 mesh under an ice-water bath according to the mass ratio, fully stir and disperse and press Potassium permanganate was added proportionally, fully stirred and reacted for 0.8 hours;

[0081] In this step, the mass ratio of graphite powder, mixed acid, potassium permanganate is 1:40:3;

[0082] Step 3, medium temperature reaction: switch the water in the jacket of the reactio...

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Abstract

The invention relates to the technical field of graphene manufacturing, in particular to a preparation method of graphene oxide. The preparation method comprises the following steps: 1, mixing concentrated sulfuric acid and phosphoric acid in a mass ratio of 5: 1 to obtain mixed acid; 2, taking a certain amount of mixed acid, adding natural crystalline flake graphite powder with the mesh number of 100-5000, stirring and dispersing, and then adding potassium permanganate; 3, continuously stirring and reacting the materials in warm water at 20-60 DEG C; 4, maintaining the temperature of the mixture at 85-99 DEG C, and then adding hydrogen peroxide under a stirring condition to remove residual potassium permanganate; 5, separating the solution prepared in the step 4 by using a centrifugal machine; 6, adding a certain amount of deionized water into the precipitate obtained in the step 5, stirring and dispersing, and introducing into a homogenizer for uninterruptedly and circularly stripping; 7, separating the material obtained in the step 6 by using the centrifugal machine, and washing once by using hydrochloric acid and deionized water respectively; 8, separating the washed solids by using the centrifugal machine; the raw materials are cheap and easy to obtain, operation is safe, dispersity is good, and industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of graphene manufacture, in particular to a preparation method of graphene oxide. Background technique [0002] The commonly used method to prepare graphene oxide by chemical method is the Hummers method. The principle is to first treat graphene with strong acid to transform it into a graphite interlayer compound, and then add a strong oxidant for deep exfoliation, and adjust the oxidation degree of the product by controlling the reaction time , which is measured by the atomic ratio of C and O; although it is widely used, the oxidation degree of graphene oxide prepared by this process is not high, and the use of excessive KMnO4 increases the difficulty of subsequent waste liquid treatment, so people continue to try Improving the Hummers method, such as the ultrasonic-assisted Hummers method, although the method is convenient and quick, the equipment is expensive and difficult to maintain, which is not conduc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198
CPCC01B32/198C01P2004/03C01B2204/32
Inventor 蔡金明郭伟华吕鉴罗琳赵蓝蔚
Owner GUANGDONG MORION NANOTECHNOLOGY CO LTD
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