CN106829937B - A kind of preparation method of graphene - Google Patents
A kind of preparation method of graphene Download PDFInfo
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- CN106829937B CN106829937B CN201710029067.1A CN201710029067A CN106829937B CN 106829937 B CN106829937 B CN 106829937B CN 201710029067 A CN201710029067 A CN 201710029067A CN 106829937 B CN106829937 B CN 106829937B
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Abstract
A kind of preparation method of graphene, it tentatively weakens graphite layers Van der Waals force in such a way that laser cracking is handled, then the remover of graphite layers can be plugged into come in conjunction with the graphite of thin layer by molecule, play the release effect to graphite, pass through air bubble expansion again, the mode of explosion, graphite layers binding force is weakened again, to disconnect the connection of graphite between layers, it can be obtained by graphite in this way, graphene and removing agent composition, after remover is removed finally by isolated mode, graphene is extracted from the mixture of graphite and graphene by way of extraction again, just complete the preparation of graphene, simple process, preparation efficiency is high, graphene purity is high, it is environmentally friendly in its preparation process, pollution is not generated.
Description
[technical field]
The invention belongs to carbon material technical fields, are specifically related to a kind of preparation method of graphene.
[background technique]
Graphene due to its unique structure and photoelectric property become carbon material, nanotechnology, Condensed Matter Physics and
The research hotspot in the fields such as functional material.Graphene is strongest as presently found most thin, maximum intensity, electrical and thermal conductivity performance
A kind of novel nano-material, graphene are referred to as " dark fund ", are " kings of new material ", theoretical specific surface area is up to 2630m2/
G can be used for effect transistor, electrode material, composite material, liquid crystal display material, sensor etc..But in the mistake using graphene
The main problem encountered in journey is can not to carry out mass production to it at present.
Currently, the preparation method of graphene is mainly two kinds, a kind of method is mechanical stripping method, and this method is to utilize
Friction and relative motion between object and graphene, the method for obtaining graphene layer material, but this method obtains stone
The efficiency and purity of black alkene are all extremely low, as a result very unsatisfactory；Second method is oxidation-reduction method, and this method is by using sulphur
The oxidants such as the chemical reagent such as acid, nitric acid and potassium permanganate, hydrogen peroxide aoxidize natural graphite, between increasing between graphite linings
Away from, be inserted into oxide between layers in graphite, be made graphite oxide, then reactant is washed, and to clean after
Solid carries out low temperature drying, graphite oxide powder is made, then by the methods of physics removing, high-temperature expansion to graphite oxide powder
It is removed, graphene oxide is made, graphene oxide is restored finally by chemical method, obtains graphene.This method behaviour
Make simple, yield height, but product quality is lower, the graphene prepared easily occurs to reunite and be difficult to disperse, due to existing
Van der Waals interaction, the graphene with high-specific surface area are intended to form irreversible agglomeration, or even accumulation is formed again
Graphite is largely produced to affect graphene, is equally limited its application.In addition, the chemistry redox method is used
Reducing agent it is toxic, certain pollution is caused to environment.
Therefore, we are dedicated to finding that a kind of high production efficiency, product quality be high, graphene purity is high, and are preparing
The free of contamination method for preparing graphene in the process.
[summary of the invention]
For above-mentioned technical problem in the prior art, the present invention provides a kind of simple processes, preparation efficiency height, graphite
The preparation method of the graphene of alkene purity is high, environmental protection, does not generate pollution in preparation process.
In order to solve above-mentioned technical problem, the present invention is adopted the following technical solutions:
A kind of preparation method of graphene, comprises the following steps that
S1: graphite initial material is subjected to Screening Treatment, obtains graphite raw material；
S2: under protective gas atmosphere, laser cracking processing is carried out to graphite raw material；
S3: remover is added to cracking treated in graphite raw material, 30min ~ 1h is sufficiently stirred, makes remover
Solvent molecule is intercalation into the interlayer of graphite, obtains graphite-remover mixed solution；The remover is surfactant,
Binding force is greater than graphite layers Van der Waals force；
S4: it is inflated in graphite-remover mixed solution using bubble generator, so that being stained with the stripping of thin layer graphite
It is filled from agent hydrophobic side by gas height, generates bubble, anxious huge series increases volume；
S5: igniting bubble using bubble destructor, weakens graphite layers again using the impact force that bubble explodes and combines
Power, while the binding force between thin layer graphite and remover is also weakened, obtain graphite, graphene and removing agent composition；
S6: graphite, graphene and the removing agent composition that previous step is obtained carry out centrifugal dehydration treatment, are dried
After sintering processes, remover is removed, the mixture of graphite and graphene is obtained；
S7: the mixture of graphite and graphene is extracted by extraction, obtains graphene mixed solution and graphite
Mixed solution；
S8: after obtained graphene mixed solution is carried out separating treatment and is dried, graphene is obtained.
It in a kind of above-mentioned improvement project of the preparation method of graphene, further include having step S9: will be in step S7
The graphite mixed liquor arrived carries out high temperature drying processing, obtains graphite.
In to a kind of above-mentioned improvement project of the preparation method of graphene, the sintering processes in step S6 are protective atmosphere
Under sintering processes.
In to a kind of above-mentioned improvement project of the preparation method of graphene, the separating treatment in step S8 is electrolysis point
From.
In to a kind of above-mentioned improvement project of the preparation method of graphene, the drying process in step S8 is freeze-drying
Processing.
In to a kind of above-mentioned improvement project of the preparation method of graphene, the Screening Treatment in step S1 was 10000
Mesh choosing.
In to a kind of above-mentioned improvement project of the preparation method of graphene, the bubble destructor is ultrasonic wave dress
It sets.
Compared with prior art, the beneficial effects of the present invention are: it tentatively weakens stone in such a way that laser cracking is handled
Then Van der Waals force between layer of ink can be plugged into the remover of graphite layers by molecule in conjunction with the graphite of thin layer, to play pair
The release effect of graphite, then by way of air bubble expansion, explosion, graphite layers binding force is weakened, again to disconnect graphite linings
Contacting between layer can be obtained by graphite, graphene and removing agent composition in this way, will shell finally by isolated mode
Graphene is extracted from the mixture of graphite and graphene after agent removal, then by way of extraction, is just completed
The preparation of graphene, simple process, preparation efficiency are high, graphene is with high purity, and environmental protection, does not generate pollution in preparation process.
The present invention is described in further detail With reference to embodiment:
[specific embodiment]
A kind of preparation method of graphene, comprises the following steps that
S1: graphite initial material is subjected to Screening Treatment, obtains graphite raw material；
S2: under protective gas atmosphere, laser cracking processing is carried out to graphite raw material, first passes through cracking in this step
The Van der Waals force of processing reduction graphite layers, and widen the spacing of graphite layers；
S3: remover is added to cracking treated in graphite raw material, 30min ~ 1h is sufficiently stirred, makes remover
Solvent molecule is intercalation into the interlayer of graphite, obtains graphite-remover mixed solution；The remover is surfactant,
Binding force is greater than graphite layers Van der Waals force, after graphite and remover are sufficiently mixed, since only lamellate graphite could be weak
In combination in conjunction with the hydrophobic side of remover, the hydrophobic side of such remover will adsorb a small amount of, thin layer graphite；
S4: it is inflated in graphite-remover mixed solution using bubble generator, so that being stained with the stripping of thin layer graphite
It is filled from agent hydrophobic side by gas height, generates bubble, anxious huge series increases volume, after inflation, is adsorbed with a small amount of, thin layer stone
The remover hydrophobic side of ink will gradually widen its spacing with water-wet side；
S5: bubble is ignited using bubble destructor, the bubble destructor is ultrasonic unit, quick-fried using bubble
Fried impact force weakens graphite layers binding force again, to disconnect the connection of graphite between layers, while also weakening thin layer stone
Binding force between ink and remover, according to maximum energy criterion, the not pairs of P orbital electron cloud of graphite layers has an opportunity to be combined into
Annular pi bond generates part graphene, can be obtained by graphite, graphene and removing agent composition in this way；
S6: graphite, graphene and the removing agent composition that previous step is obtained carry out centrifugal dehydration treatment, for removing
Remover, and after removing remover, then be dried and sintering processes, it then can be obtained by graphite and graphene
Mixture；
S7: the mixture of graphite and graphene is extracted by extraction, obtains graphene mixed solution and graphite
Mixed solution；
S8: after obtained graphene mixed solution is carried out separating treatment and is dried, graphene is obtained.
S9: graphite mixed liquor obtained in step S7 is subjected to high temperature drying processing, obtains graphite, the stone that can will be obtained
Ink backs within to be screened in step S1.
In specific operation, the separating treatment in step S8 is electrolytic separation, and the drying process in step S8 is that freezing is dry
Dry processing, the Screening Treatment in step S1 were the choosing of 10000 meshes.
Protective atmosphere recited above is nitrogen.
Remover recited above is the organic matter of C, H, O composition.
It is aobvious for those skilled in the art by the disclosure although the present invention is described in detail referring to above example
And be clear to, and in the case where not departing from the principle of the present invention and scope that the claim limits, it can be right
The present invention makes a variety of changes or modifies.Therefore, the detailed description of the embodiment of the present disclosure is only used to explain, rather than is used to limit
The present invention, but it is defined by the subject-matter of the claims the range of protection.
Claims (7)
1. a kind of preparation method of graphene, which is characterized in that comprise the following steps that
S1: graphite initial material is subjected to Screening Treatment, obtains graphite raw material；
S2: under protective gas atmosphere, laser cracking processing is carried out to graphite raw material；
S3: remover is added to cracking treated in graphite raw material, 30min~1h is sufficiently stirred, makes the molecule of remover
It is intercalation into the interlayer of graphite, obtains graphite-remover mixed solution；The remover is surfactant, and binding force is big
In graphite layers Van der Waals force；
S4: it is inflated in graphite-remover mixed solution using bubble generator, so that being stained with the remover of thin layer graphite
Hydrophobic side is filled by gas height, generates bubble；
S5: igniting bubble using bubble destructor, weakens graphite layers binding force again using the impact force that bubble explodes, together
When also weaken binding force between thin layer graphite and remover, obtain graphite, graphene and removing agent composition；
S6: graphite, graphene and the removing agent composition that previous step is obtained carry out centrifugal dehydration treatment, drying process and burning
After knot processing, remover is removed, the mixture of graphite and graphene is obtained；
S7: the mixture of graphite and graphene is extracted by extraction, obtains graphene mixed solution and graphite mixing
Solution；
S8: after obtained graphene mixed solution is carried out separating treatment and is dried, graphene is obtained.
2. the preparation method of graphene according to claim 1, which is characterized in that further include having step S9: by step S7
Obtained in graphite mixed liquor carry out high temperature drying processing, obtain graphite.
3. the preparation method of graphene according to claim 1, which is characterized in that the sintering processes in step S6 are protection
Sintering processes under atmosphere.
4. the preparation method of graphene according to claim 1, which is characterized in that the separating treatment in step S8 is electrolysis
Separation.
5. the preparation method of graphene according to claim 1, which is characterized in that the drying process in step S8 is freezing
It is dried.
6. the preparation method of graphene according to claim 1, which is characterized in that the Screening Treatment in step S1 was
The choosing of 10000 meshes.
7. the preparation method of graphene according to claim 1, which is characterized in that the bubble destructor is ultrasound
Wave apparatus.
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| CN107117606A (en) * | 2017-06-20 | 2017-09-01 | 成都新柯力化工科技有限公司 | A kind of method that graphene is prepared based on laser ultrasonic stripping |
| CN109665518A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of preparation method of highly conductive graphene |
| CN107539979B (en) * | 2017-10-23 | 2019-02-19 | 南京旭羽睿材料科技有限公司 | A kind of graphene extraction separation method |
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| CN103723712A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of single-layer graphene dimethylformamide solution |
| CN103738949A (en) * | 2013-11-22 | 2014-04-23 | 盐城纳新天地新材料科技有限公司 | Preparation method for single-layer graphene isopropanol solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103723712A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of single-layer graphene dimethylformamide solution |
| CN103738949A (en) * | 2013-11-22 | 2014-04-23 | 盐城纳新天地新材料科技有限公司 | Preparation method for single-layer graphene isopropanol solution |
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