CN108264036A - A kind of preparation method of fluorine graphene oxide - Google Patents
A kind of preparation method of fluorine graphene oxide Download PDFInfo
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- CN108264036A CN108264036A CN201810272295.6A CN201810272295A CN108264036A CN 108264036 A CN108264036 A CN 108264036A CN 201810272295 A CN201810272295 A CN 201810272295A CN 108264036 A CN108264036 A CN 108264036A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention belongs to fluorine technical field of preparation of graphene oxide, and in particular to a kind of preparation method of fluorine graphene oxide, the method are using graphite oxide as raw material, and the fluorine graphene oxide can be prepared using hydro-thermal method；The fluorine graphene oxide is single layer structure or is multilayered structure (such as 2 100 layers)；The short preparation period of the method, reaction is mild, is easy to control, and yield is high, suitable for large-scale industrial production.
Description
Technical field
The invention belongs to fluorine technical field of preparation of graphene oxide, and in particular to a kind of preparation side of fluorine graphene oxide
Method.
Background technology
The researchers such as University of Manchester Geim in 2004 peel a small amount of graphene from graphite and study its performance, send out
Now it is with special characteristic electron and excellent mechanics, electricity, optics, calorifics and magnetic performance, so as to start graphite
The upsurge of alkene application study.Graphene has excellent conduction, heat conduction and mechanical property, it can be compound as high-strength conducting is prepared
The preferable Nano filling of material, while can also mix and then be polymerized to form compound with the polymer monomer disperseed in the solution
Material system can assign composite material different functionality, show excellent mechanics and electric property, excellent processability
Energy.However, since graphene surface lacks active group, itself easily reunites again, dispersed poor in the polymer, it is difficult to directly
It is connected between polymer interface and forms stronger interaction, can not realize enhancing effect of the graphene in polymer composites
Fruit.Therefore, it is necessary to necessary modification is carried out to graphene, and it is then compound with polymer progress again, reach and put forward high performance purpose.
China Patent Publication No. be CN107652868A in disclose a kind of preparation method of fluorine graphene oxide, be by
Graphite powder, the concentrated sulfuric acid and concentrated phosphoric acid mixing；Graphene oxide is prepared using potassium permanganate and hydrogen peroxide Strong oxdiative method；Again will
It prepares fluorine graphene oxide with dicyclohexylcarbodiimide, fluorochemical monomer ultrasonic mixing；Although this method can be prepared
Fluorine graphene oxide, but its long preparation period, reaction raw materials are dangerous high, and low yield is not suitable for large-scale industry metaplasia
The demand of production.
Invention content
In order to improve the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of fluorine graphene oxide,
The method is the short preparation period using graphite oxide as raw material, and reaction is mild, is easy to control, and yield is high, suitable for extensive
Industrialized production.
The present invention provides following technical solution：
A kind of preparation method of fluorine graphene oxide, the method are using graphite oxide as raw material, using hydro-thermal method, are prepared
Obtain the fluorine graphene oxide.
According to the present invention, the preparation method includes the following steps：
Graphite oxide, oxidant and hydrofluoric acid are mixed, hydro-thermal reaction is carried out, the fluorine graphene oxide is prepared.
According to the present invention, the mass percentage that the graphite oxide accounts for mixed solution is 2-15wt%；The oxidant
The mass percentage for accounting for mixed solution is 3-30wt%；The mass percentage that the hydrofluoric acid accounts for mixed solution is 3-
25wt%；Surplus is water.
Preferably, the mass percentage that the graphite oxide accounts for mixed solution is 5-10wt%；The oxidant accounts for mixed
The mass percentage for closing solution is 5-25wt%；The mass percentage that the hydrofluoric acid accounts for mixed solution is 5-20wt%；
Surplus is water.
According to the present invention, there is no particular limitation for the selection of the graphite oxide, can know for those skilled in the art
Any graphite oxide of dawn；
According to the present invention, there is no particular limitation for the selection of the oxidant, can know for those skilled in the art
Any oxidant；Preferably, the oxidant is selected from strong oxidizer, such as selected from hydrogen peroxide, potassium permanganate etc.；Further preferably
Ground, the oxidant are selected from the hydrogen peroxide solution of a concentration of 15-30wt%；The hydrogen peroxide can be directly added into this when in use
The hydrogen peroxide solution of concentration range, after can also being diluted add in debita spissitudo hydrogen peroxide solution, but need to meet it is above-mentioned fixed
Mass percentage in the mixed solution of justice.
According to the present invention, there is no particular limitation for the selection of the hydrofluoric acid, can know for those skilled in the art
Any hydrofluoric acid；Preferably, a concentration of 30-40wt% of the hydrofluoric acid.The hydrofluoric acid when in use can be direct
The hydrofluoric acid of this concentration range is added in, the hydrofluoric acid solution of debita spissitudo is added in after can also being diluted, but need to be met above-mentioned
Mass percentage in the mixed solution of definition.
By being used cooperatively for hydrofluoric acid and oxidant, the fluorination to graphite oxide can be realized under hydrothermal reaction condition
Effect, and then the fluorine graphene oxide is prepared.
According to the present invention, the hydro-thermal reaction carries out preferably in the hydrothermal reaction kettle with polytetrafluoroethyllining lining, instead
It should preferably be carried out under closed environment；
Preferably, the temperature of the hydro-thermal reaction is 130-180 DEG C, and preferably 150-160 DEG C；The hydro-thermal reaction
Time is 4-12 hours；Preferably 6-8 hours again.
According to the present invention, the method further includes following post-processing step：By the above-mentioned fluorine graphene oxide being prepared
Ultrasound is carried out, is then filtered, washed, dries.
According to the present invention, the ultrasound, to be filtered, washed, dry be conventional treatment that those skilled in the art know
Method, it is preferable that the time of the ultrasound is 30min-3h；The supersound process can further realize the interlayer to product
Stripping.
Preferably, it is described to be filtered into centrifugal filtration.
Beneficial effects of the present invention：
The present invention provides a kind of preparation method of fluorine graphene oxide, the method is the profit using graphite oxide as raw material
The fluorine graphene oxide can be prepared with hydro-thermal method；The fluorine graphene oxide is single layer structure or is multilayered structure
(such as 2-100 layers)；The short preparation period of the method, reaction is mild, is easy to control, and yield is high, suitable for heavy industrialization
Production.
Description of the drawings
Fig. 1 is the SEM figures of fluorine graphene oxide prepared by embodiment 1.
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.Furthermore, it is to be understood that after content disclosed in this invention has been read, ability
Field technique personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the protection that the present invention is limited
Within the scope of.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material etc., are commercially available unless otherwise specified.
Embodiment 1
The preparation of fluorine graphene oxide
By following the configuration of metering mixed solution：
The graphite oxide of 10g, the hydrogen peroxide (the hydrogen peroxide 40g for selecting a concentration of 30wt%) of 12g, 15g hydrofluoric acid
(the hydrofluoric acid 50g for selecting a concentration of 30wt%).
Said components are added in the hydrothermal reaction kettle with polytetrafluoroethyllining lining after mixing, under closed environment,
Heat preservation 6 hours is carried out at 150 DEG C, after being cooled to room temperature, after reaction solution ultrasonic disperse 1 hour, carries out high speed centrifugation, mistake
Filter, freeze-drying, obtain fluorine graphene oxide.
Fig. 1 is the SEM of fluorine graphene oxide prepared by embodiment 1.
Embodiment 2
The preparation of fluorine graphene oxide
By following the configuration of metering mixed solution：
The graphite oxide of 5g, the hydrogen peroxide (the hydrogen peroxide 60g for selecting a concentration of 15wt%) of 9g, 10g hydrofluoric acid (i.e.
Select the hydrofluoric acid 25g of a concentration of 40wt%), 10g water.
Said components are added in the hydrothermal reaction kettle with polytetrafluoroethyllining lining after mixing, under closed environment,
Heat preservation 8 hours is carried out at 160 DEG C, after being cooled to room temperature, after reaction solution ultrasonic disperse 0.5 hour, carries out high speed centrifugation, mistake
Filter, freeze-drying, obtain fluorine graphene oxide.
Embodiment 3
The preparation of fluorine graphene oxide
By following the configuration of metering mixed solution：
The graphite oxide of 12g, the hydrogen peroxide (the hydrogen peroxide 50g for selecting a concentration of 30wt%) of 15g, 15.2g hydrogen fluorine
Sour (the hydrofluoric acid 38g for selecting a concentration of 40wt%).
Said components are added in the hydrothermal reaction kettle with polytetrafluoroethyllining lining after mixing, under closed environment,
Heat preservation 8 hours is carried out at 180 DEG C, after being cooled to room temperature, after reaction solution ultrasonic disperse 0.5 hour, carries out high speed centrifugation, mistake
Filter, freeze-drying, obtain fluorine graphene oxide.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to the above embodiments.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the present invention
Within the scope of shield.
Claims (9)
1. a kind of preparation method of fluorine graphene oxide, which is characterized in that the method is using graphite oxide as raw material, utilizes water
The fluorine graphene oxide is prepared in hot method.
2. preparation method according to claim 1, which is characterized in that the preparation method includes the following steps：It will oxidation
Graphite, oxidant and hydrofluoric acid mixing, carry out hydro-thermal reaction, the fluorine graphene oxide are prepared.
3. preparation method according to claim 1 or 2, which is characterized in that the graphite oxide accounts for the quality of mixed solution
Percentage composition is 2-15wt%；The mass percentage that the oxidant accounts for mixed solution is 3-30wt%；The hydrofluoric acid accounts for
The mass percentage of mixed solution is 3-25wt%；Surplus is water.
4. preparation method according to claim 3, which is characterized in that the graphite oxide accounts for the quality percentage of mixed solution
Content is 5-10wt%；The mass percentage that the oxidant accounts for mixed solution is 5-25wt%；The hydrofluoric acid accounts for mixing
The mass percentage of solution is 5-20wt%；Surplus is water.
5. according to claim 1-4 any one of them preparation methods, which is characterized in that the oxidant is selected from strong oxidizer,
Such as selected from hydrogen peroxide, potassium permanganate etc.；Preferably, the oxidant is selected from the hydrogen peroxide solution of a concentration of 15-30wt%.
6. according to claim 1-5 any one of them preparation methods, which is characterized in that a concentration of 30- of the hydrofluoric acid
40wt%.
7. according to claim 1-6 any one of them preparation methods, which is characterized in that the temperature of the hydro-thermal reaction is 130-
180 DEG C, and preferably 150-160 DEG C；The time of the hydro-thermal reaction is 4-12 hours；Preferably 6-8 hours again.
8. according to claim 1-7 any one of them preparation methods, which is characterized in that the method further includes following post processing
Step：The above-mentioned fluorine graphene oxide being prepared is subjected to ultrasound, is then filtered, washed, dries.
9. according to claim 1-8 any one of them preparation methods, which is characterized in that the time of the ultrasound is 30min-
3h。
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| CN201810272295.6A CN108264036A (en) | 2018-03-29 | 2018-03-29 | A kind of preparation method of fluorine graphene oxide |
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| CN201810272295.6A CN108264036A (en) | 2018-03-29 | 2018-03-29 | A kind of preparation method of fluorine graphene oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111686766A (en) * | 2019-03-11 | 2020-09-22 | 中国科学院福建物质结构研究所 | Metal-fluorine doped carbon composite material, preparation method thereof and application thereof in electrocatalytic nitrogen fixation |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288069A (en) * | 2013-05-10 | 2013-09-11 | 西北工业大学 | Method for preparing fluorinated graphene through microwave hydrothermal method |
| CN105417528A (en) * | 2015-12-09 | 2016-03-23 | 天津大学 | Preparation methods for fluorinated graphene hydrogel material and electrodes thereof |
| CN105967175A (en) * | 2016-05-16 | 2016-09-28 | 河南工业大学 | Preparation method of water-soluble fluorinated graphene |
| CN107200317A (en) * | 2017-04-14 | 2017-09-26 | 北京航空航天大学 | A kind of method that loose structure graphene is prepared based on laser |
-
2018
- 2018-03-29 CN CN201810272295.6A patent/CN108264036A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288069A (en) * | 2013-05-10 | 2013-09-11 | 西北工业大学 | Method for preparing fluorinated graphene through microwave hydrothermal method |
| CN105417528A (en) * | 2015-12-09 | 2016-03-23 | 天津大学 | Preparation methods for fluorinated graphene hydrogel material and electrodes thereof |
| CN105967175A (en) * | 2016-05-16 | 2016-09-28 | 河南工业大学 | Preparation method of water-soluble fluorinated graphene |
| CN107200317A (en) * | 2017-04-14 | 2017-09-26 | 北京航空航天大学 | A kind of method that loose structure graphene is prepared based on laser |
Non-Patent Citations (1)
| Title |
|---|
| XUMING YANG ET AL.: "Acid induced fluorinated graphene oxide", 《RSC ADVANCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111686766A (en) * | 2019-03-11 | 2020-09-22 | 中国科学院福建物质结构研究所 | Metal-fluorine doped carbon composite material, preparation method thereof and application thereof in electrocatalytic nitrogen fixation |
| CN111686766B (en) * | 2019-03-11 | 2021-09-21 | 中国科学院福建物质结构研究所 | Metal-fluorine doped carbon composite material, preparation method thereof and application thereof in electrocatalytic nitrogen fixation |
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Application publication date: 20180710 |