CN106744883A - The preparation method of Graphene - Google Patents
The preparation method of Graphene Download PDFInfo
- Publication number
- CN106744883A CN106744883A CN201710006070.1A CN201710006070A CN106744883A CN 106744883 A CN106744883 A CN 106744883A CN 201710006070 A CN201710006070 A CN 201710006070A CN 106744883 A CN106744883 A CN 106744883A
- Authority
- CN
- China
- Prior art keywords
- graphite
- graphene
- preparation
- remover
- treatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
Abstract
The preparation method of the Graphene that the present invention is provided, it tentatively weakens graphite layers Van der Waals force by way of the cracking of illumination light wave is processed, then the remover that graphite layers are can be plugged into by molecule is combined come the graphite with thin layer, play the release effect to graphite, pass through air bubble expansion again, the mode of blast, graphite layers adhesion is weakened again, to disconnect graphite contact between layers, so can be obtained by graphite, Graphene and stripping agent composition, after finally by separate mode, remover is removed, Graphene is extracted in the mixture by way of extraction from graphite with Graphene again, just complete the preparation of Graphene, process is simple, preparation efficiency is high, Graphene purity is high, environmental protection in its preparation process, pollution is not produced.
Description
【Technical field】
The invention belongs to carbon material technical field, the preparation method of Graphene is specifically related to.
【Background technology】
Graphene becomes carbon material, nanometer technology, Condensed Matter Physics and function due to its unique structure and photoelectric property
The study hotspot in the fields such as material.Graphene is used as the most strong one kind of the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that
Novel nano-material, Graphene is referred to as " dark fund ", is " king of new material ", and its theoretical specific surface area is up to 2630m2/g, can
For effect transistor, electrode material, composite, liquid crystal display material, sensor etc..But in the process using Graphene
In the main problem that runs into be that it cannot largely be produced at present.
At present, the preparation method of Graphene is mainly two kinds, and a kind of method is mechanical stripping method, and the 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 undesirable；Second method is oxidation-reduction method, and the method is by using sulphur
The oxidant such as the chemical reagent such as acid, nitric acid and potassium permanganate, hydrogen peroxide aoxidizes native graphite, between increasing between graphite linings
Away from, insert oxide between layers in graphite, be obtained graphite oxide, then reactant is washed, and to clean after
Solid carries out low temperature drying, and graphite oxide powder is obtained, then by methods such as physics stripping, high-temperature expansions to graphite oxide powder
Peeled off, graphene oxide is obtained, reduced graphene oxide finally by chemical method, obtained Graphene.This method behaviour
Make simple, yield is high, but product quality is relatively low, the Graphene for preparing easily occurs to reunite and be difficult to disperse, due to existing
Van der Waals interaction, the Graphene with high-specific surface area is intended to form irreversible caking, or even piles up formation again
Graphite, it is same to limit its application so as to have impact on the substantial amounts of production of Graphene.In addition, the chemistry redox method institute
The reducing agent of use is toxic, and certain pollution is caused to environment.
Therefore, we are devoted to finding that a kind of production efficiency is high, product quality is high, Graphene purity is high, and are preparing
During the free of contamination method for preparing Graphene.
【The content of the invention】
For above-mentioned technical problem of the prior art, the invention provides a kind of process is simple, preparation efficiency be high, Graphene is pure
The preparation method of degree Graphene high, environmental protection, pollution is not produced in its preparation process.
In order to solve above-mentioned technical problem, the present invention uses following technical proposals：
The preparation method of Graphene, including have the following steps：
S1：Material at the beginning of graphite is carried out into Screening Treatment, graphite raw material is obtained；
S2：Under protective gas atmosphere, illumination light wave cracking treatment is carried out to graphite raw material；
S3：Remover is added in the graphite raw material after cracking treatment, 30min ~ 1h is sufficiently stirred for, makes the solvent of remover
Molecule intercalation obtains graphite-remover mixed solution to the interlayer of graphite；Described remover is surfactant, its combination
Power is more than graphite layers Van der Waals force；
S4：Using bubble generator toward inflation in graphite-remover mixed solution so that be stained with the remover of thin layer graphite
Hydrophobic side is highly filled by gas, produces bubble, anxious huge series increase volume；
S5：Bubble is ignited using bubble destructor, the impulsive force exploded using bubble weakens graphite layers adhesion again, together
When also weaken adhesion between thin layer graphite and remover, obtain graphite, Graphene and peel off agent composition；
S6：Graphite, Graphene and the stripping agent composition that previous step is obtained carry out centrifugal dehydration treatment, dried process and burning
After knot treatment, remover is removed, obtain the mixture of graphite and Graphene；
S7：Graphite is extracted with the mixture of Graphene by extraction, Graphene mixed solution and graphite mixing is obtained
Solution；
S8：After the Graphene mixed solution that will be obtained carries out separating treatment and dried process, Graphene is obtained.
In the improvement project of the preparation method to above-mentioned Graphene, step S9 is also included：By what is obtained in step S7
Graphite mixed liquor carries out high temperature drying treatment, obtains graphite.
In the improvement project of the preparation method to above-mentioned Graphene, in the illumination light wave cracking treatment of step S2, ripple
A length of 1.2um.
In the improvement project of the preparation method to above-mentioned Graphene, the sintering processes in step S6 are under protective atmosphere
Sintering processes.
In the improvement project of the preparation method to above-mentioned Graphene, the separating treatment in step S8 is electrolytic separation.
In the improvement project of the preparation method to above-mentioned Graphene, the dried process in step S8 is at freeze-drying
Reason.
In the improvement project of the preparation method to above-mentioned Graphene, the Screening Treatment in step S1 was 10000 mesh sieves
Choosing.
In the improvement project of the preparation method to above-mentioned Graphene, described bubble destructor is ultrasonic unit.
Compared with prior art, the beneficial effects of the invention are as follows：It is by way of the cracking of illumination light wave is processed come preliminary
Reduction graphite layers Van der Waals force, the remover of graphite layers is then can be plugged into by molecule and is combined come the graphite with thin layer,
The release effect to graphite is played, then by way of air bubble expansion, blast, graphite layers adhesion is weakened again, to disconnect
Graphite contact between layers, so can be obtained by graphite, Graphene and peels off agent composition, finally by separate side
After formula removes remover, then Graphene is extracted in mixture from graphite with Graphene by way of extraction, just
The preparation of Graphene is completed, process is simple, preparation efficiency are high, Graphene purity is high, environmental protection, does not produce dirt in its preparation process
Dye.
With reference to specific embodiment, the present invention is described in further detail：
【Specific embodiment】
The preparation method of Graphene, including have the following steps：
S1：Material at the beginning of graphite is carried out into Screening Treatment, graphite raw material is obtained；
S2：Under protective gas atmosphere, illumination light wave cracking treatment is carried out to graphite raw material, illumination is first passed through in this step
The Van der Waals force of light wave cracking treatment reduction graphite layers, and widen the spacing of graphite layers；
S3：Remover is added in the graphite raw material after cracking treatment, 30min ~ 1h is sufficiently stirred for, makes the solvent of remover
Molecule intercalation obtains graphite-remover mixed solution to the interlayer of graphite；Described remover is surfactant, its combination
Power is more than graphite layers Van der Waals force, after graphite and remover are sufficiently mixed, because only lamellate graphite could weak binding
Ground is combined with the hydrophobic side of remover, the hydrophobic side of such remover will adsorb on a small quantity, the graphite of thin layer；
S4：Using bubble generator toward inflation in graphite-remover mixed solution so that be stained with the remover of thin layer graphite
Hydrophobic side is highly filled by gas, produces bubble, and anxious huge series increase volume after inflation, is adsorbed with a small amount of, thin layer graphite
Remover hydrophobic side will gradually widen its spacing with water-wet side；
S5：Bubble is ignited using bubble destructor, described bubble destructor is ultrasonic unit, is exploded using bubble
Impulsive force weakens graphite layers adhesion again, to disconnect graphite contact between layers, while also reduction thin layer graphite with
Adhesion between remover, according to maximum energy criterion, the not paired P orbital electron cloud of graphite layers have an opportunity combine circularize
π keys, produce part Graphene, so can be obtained by graphite, Graphene and peel off agent composition；
S6：Graphite, Graphene and the stripping agent composition that previous step is obtained carry out centrifugal dehydration treatment, are peeled off for removing
Agent, and after remover is removed, then treatment and sintering processes are dried, then can be obtained by graphite mixed with Graphene
Compound；
S7：Graphite is extracted with the mixture of Graphene by extraction, Graphene mixed solution and graphite mixing is obtained
Solution；
S8：After the Graphene mixed solution that will be obtained carries out separating treatment and dried process, Graphene is obtained.
S9：The graphite mixed liquor that will be obtained in step S7 carries out high temperature drying treatment, obtains graphite, the stone that will can be obtained
Ink is screened in backing within step S1.
In specific operation, in the illumination light wave cracking treatment of step S2, wavelength is 1.2um, the sintering in step S6
The sintering processes under protective atmosphere are processed as, the separating treatment in step S8 is electrolytic separation, the dried process in step S8 is
Freeze-drying process, the Screening Treatment in step S1 was the choosing of 10000 mesh sieves.
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 with reference to above example
And be clear to, and in the case of the principle of the invention and scope for not departing from described claim restriction, can be right
The present invention makes a variety of changes or changes.Therefore, the detailed description of the embodiment of the present disclosure is only used for explaining, rather than for limiting
The present invention, but it is defined by the subject-matter of the claims the scope of protection.
Claims (8)
1. a kind of preparation method of Graphene, it is characterised in that including having the following steps：
S1：Material at the beginning of graphite is carried out into Screening Treatment, graphite raw material is obtained；
S2：Under protective gas atmosphere, illumination light wave cracking treatment is carried out to graphite raw material；
S3：Remover is added in the graphite raw material after cracking treatment, 30min ~ 1h is sufficiently stirred for, makes the solvent of remover
Molecule intercalation obtains graphite-remover mixed solution to the interlayer of graphite；Described remover is surfactant, its combination
Power is more than graphite layers Van der Waals force；
S4：Using bubble generator toward inflation in graphite-remover mixed solution so that be stained with the remover of thin layer graphite
Hydrophobic side is highly filled by gas, produces bubble, anxious huge series increase volume；
S5：Bubble is ignited using bubble destructor, the impulsive force exploded using bubble weakens graphite layers adhesion again, together
When also weaken adhesion between thin layer graphite and remover, obtain graphite, Graphene and peel off agent composition；
S6：Graphite, Graphene and the stripping agent composition that previous step is obtained carry out centrifugal dehydration treatment, dried process and burning
After knot treatment, remover is removed, obtain the mixture of graphite and Graphene；
S7：Graphite is extracted with the mixture of Graphene by extraction, Graphene mixed solution and graphite mixing is obtained
Solution；
S8：After the Graphene mixed solution that will be obtained carries out separating treatment and dried process, Graphene is obtained.
2. the preparation method of Graphene according to claim 1, it is characterised in that also include step S9：By step S7
In the graphite mixed liquor that obtains carry out high temperature drying treatment, obtain graphite.
3. the preparation method of Graphene according to claim 1, it is characterised in that at the illumination light wave cracking of step S2
In reason, wavelength is 1.2um.
4. the preparation method of Graphene according to claim 1, it is characterised in that the sintering processes in step S6 are protection
Sintering processes under atmosphere.
5. the preparation method of Graphene according to claim 1, it is characterised in that the separating treatment in step S8 is electrolysis
Separate.
6. the preparation method of Graphene according to claim 1, it is characterised in that the dried process in step S8 is freezing
Dried process.
7. the preparation method of Graphene according to claim 1, it is characterised in that the Screening Treatment in step S1 was
10000 mesh sieves are selected.
8. the preparation method of Graphene according to claim 1, it is characterised in that described bubble destructor is ultrasound
Wave apparatus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710006070.1A CN106744883B (en) | 2017-01-05 | 2017-01-05 | The preparation method of graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710006070.1A CN106744883B (en) | 2017-01-05 | 2017-01-05 | The preparation method of graphene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106744883A true CN106744883A (en) | 2017-05-31 |
| CN106744883B CN106744883B (en) | 2019-03-22 |
Family
ID=58949524
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710006070.1A Active CN106744883B (en) | 2017-01-05 | 2017-01-05 | The preparation method of graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106744883B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589815A (en) * | 2019-09-11 | 2019-12-20 | 北京航空航天大学 | Preparation method of graphene conductive paste |
| CN111422857A (en) * | 2020-01-14 | 2020-07-17 | 昂星新型碳材料常州有限公司 | Graphene nano-bubble material, preparation method and application thereof, adsorbent, catalyst, optical material and energy storage material |
| WO2021098165A1 (en) * | 2019-11-20 | 2021-05-27 | 厦门大学 | Graphene oxide material, halogenated graphene material, preparation methods therefor, and electrolysis system |
| CN113308172A (en) * | 2021-06-08 | 2021-08-27 | 南京工程学院 | Preparation and use method of composite anticorrosive paint for cable-stayed bridge inhaul cable |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973544A (en) * | 2010-10-29 | 2011-02-16 | 中国科学院上海微***与信息技术研究所 | Method for preparing aqueous solution of single-layer grapheme oxide |
| CN103466612A (en) * | 2013-10-08 | 2013-12-25 | 东南大学 | Method for preparing native grapheme by means of frequency mixing ultrasound |
| CN104803380A (en) * | 2015-05-12 | 2015-07-29 | 中国科学院上海微***与信息技术研究所 | Preparation method of graphene |
| WO2016046529A1 (en) * | 2014-09-22 | 2016-03-31 | Bae Systems Plc | Graphene manufacture |
-
2017
- 2017-01-05 CN CN201710006070.1A patent/CN106744883B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973544A (en) * | 2010-10-29 | 2011-02-16 | 中国科学院上海微***与信息技术研究所 | Method for preparing aqueous solution of single-layer grapheme oxide |
| CN103466612A (en) * | 2013-10-08 | 2013-12-25 | 东南大学 | Method for preparing native grapheme by means of frequency mixing ultrasound |
| WO2016046529A1 (en) * | 2014-09-22 | 2016-03-31 | Bae Systems Plc | Graphene manufacture |
| CN104803380A (en) * | 2015-05-12 | 2015-07-29 | 中国科学院上海微***与信息技术研究所 | Preparation method of graphene |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589815A (en) * | 2019-09-11 | 2019-12-20 | 北京航空航天大学 | Preparation method of graphene conductive paste |
| CN110589815B (en) * | 2019-09-11 | 2021-08-10 | 北京航空航天大学 | Preparation method of graphene conductive paste |
| WO2021098165A1 (en) * | 2019-11-20 | 2021-05-27 | 厦门大学 | Graphene oxide material, halogenated graphene material, preparation methods therefor, and electrolysis system |
| US11905605B2 (en) | 2019-11-20 | 2024-02-20 | Xiamen University | Graphene oxide material, halogenated graphene material, preparation methods therefor, and electrolysis system |
| CN111422857A (en) * | 2020-01-14 | 2020-07-17 | 昂星新型碳材料常州有限公司 | Graphene nano-bubble material, preparation method and application thereof, adsorbent, catalyst, optical material and energy storage material |
| CN113308172A (en) * | 2021-06-08 | 2021-08-27 | 南京工程学院 | Preparation and use method of composite anticorrosive paint for cable-stayed bridge inhaul cable |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106744883B (en) | 2019-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111799464B (en) | MXene/graphene composite nanosheet, preparation method and application thereof, electrode plate and application thereof | |
| CN105253878B (en) | A kind of method that expanded graphite or graphene are directly prepared under normal temperature and pressure | |
| CN106744883A (en) | The preparation method of Graphene | |
| CN104803380B (en) | Preparation method of graphene | |
| CN101710632B (en) | Method for recovering and restoring anode material graphite of waste lithium ion battery | |
| CN102502612B (en) | Method for preparing grapheme through oxidation reduction | |
| WO2015106437A1 (en) | Large-scale preparation method for graphene quantum dots | |
| US20180339906A1 (en) | Preparation method for large-size graphene oxide or graphene | |
| US10472243B2 (en) | Industrial method for preparing large-sized graphene | |
| CN106882796B (en) | Preparation method of three-dimensional graphene structure/high-quality graphene | |
| CN103382026A (en) | Low-cost mass preparation method of high-quality graphene | |
| CN103910354A (en) | Method for preparing graphene through large-scale aqueous phase | |
| CN102320598A (en) | Preparation method of graphene | |
| CN106829937A (en) | A kind of preparation method of Graphene | |
| CN106744884A (en) | A kind of Graphene and preparation method thereof | |
| CN106629689A (en) | High-efficiency catalysis macroscopic quantity preparation method for graphene oxide or compound thereof reduced and peeled based on microwaves | |
| CN102910624A (en) | Preparation method of high-yield graphene without defects | |
| CN102583338A (en) | High-quality graphene powder and preparation method thereof | |
| CN105197918A (en) | High-quality graphene and quick preparation method thereof | |
| CN105016330A (en) | Graphene preparation method | |
| CN110203913A (en) | A method of preparing graphene | |
| CN103130214A (en) | Method of preparing graphene through chemical reduction method | |
| CN106744885B (en) | A kind of device being used to prepare graphene | |
| CN104261394B (en) | The preparation method of Graphene | |
| CN106517170A (en) | Method for preparing graphene through redox assisted by high-speed shearing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |