CN105417529B - A kind of simple production method of high-quality graphene material - Google Patents
A kind of simple production method of high-quality graphene material Download PDFInfo
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/06—Graphene nanoribbons
- C01B2204/065—Graphene nanoribbons characterized by their width or by their aspect ratio
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
A kind of simple production method of high-quality graphene material, belongs to technical field of graphene.It is comprised the following steps that：1）Graphite, water and compounding substances are added in container and carry out shear agitation, the surface tension of the real time measure mixed solution, and by the mixed solution add graphite, water and or mixture, the surface tension of mixed solution is made to maintain in the range of 30~60mN/m always；2）By step 1）To get to graphene product after obtained graphene dispersing solution removal solvent.Present invention firstly provides the surface tension for monitoring mixed solution in real time in shear agitation method, so as to accordingly regulate and control the addition of various raw materials, it is greatly improved graphene preparation efficiency, it can effectively generate and stablize the dispersion liquid of a large amount of high-quality graphenes, the number of plies that be averaged of graphene obtained by preferred embodiment can be less than 5 layers.
Description
Technical field
The invention belongs to technical field of graphene, and in particular to a kind of simple production method of high-quality graphene material.
Background technology
Graphene is a kind of special two-dimensional material arranged according to hexagon by carbon atom and be connected with each other, because of its tool
There is the features such as high conductivity, high mechanical properties, extra specific surface area that can be used to prepare high speed processor, highly sensitive sensing
The various news device such as device, touch display screen, superbattery and high performance solar batteries, in electronics, space flight military project, new energy etc.
Various fields have significant application value.
Realize the large-scale industrial production and practical application of graphene, the preparation method of graphene need at least expire
Three key factors of foot：High quality, high-volume, low cost, although there are many on graphene preparation method both at home and abroad at present
Report, but from the point of view of the actual demands such as high quality, inexpensive volume production, most of graphene preparation methods reported all have each
The defects of kind various kinds.For example, vapour deposition process can meet the requirement of large-scale production high-quality graphene, but have into simultaneously
The defects of this is very high, complex process；Micromechanics stripping method, should by obtaining single-layer or multi-layer graphene directly from raw material stripping
Although method operation is relatively easy, graphene quality obtained is relatively high, has time-consuming, low yield, product size not
The shortcomings of easy to control, is unsuitable for scale of mass production；Oxidizing process is the current most common method for preparing graphene, by using nothing
Machine strong protonic acid（Such as concentrated sulfuric acid, fuming nitric aicd）And strong oxidizer（Such as potassium permanganate）Original graphite is pre-processed, is increased
Graphite layers away from, and further be ultrasonically treated obtain the water or organic solvent solution of graphene；The relatively easy volume production of this method,
Technique is relatively easy, but the physical property of the graphene obtained due to the effect of the substances such as strong oxidizer be subject to it is larger broken
Bad, various performances are greatly reduced；In recent years, people are it is further proposed that oxidation-reduction method uses strong reductant, such as hydrazine reducing agent
Carry out reduction treatment graphene oxide, graphene product performance obtained is made to have larger improvement, but used in this kind of method strong also
The substances such as former agent but there are problems that the shortcomings of corrosivity is strong, toxicity is big, Environmental costs are high and；Coleman et al. (J. Am. Chem. Soc. 2009, 131, 3611-3620) and by being ultrasonically treated stone in the solution of neopelex and water
The graphene of better performances, but the very low (0.002~0.05g/ of obtained graphene dispersing solution concentration has been made in the method for ink
L), it is unfavorable for scale of mass production；In addition, there is also many new graphene preparation methods, but usually can all be related to as prepared
Complex process, a series of problems, such as of high cost, environmental hazard is big etc., high quality, high-volume, inexpensive three weights can be met simultaneously
The graphene preparation method for wanting factor is seldom.
Thus, in order to further meet the actual demand of graphene commercial application, seek it is a kind of it is simple for process, be produced into
This is low, and will not cause higher Environmental costs simultaneously and the simple mass production method tool of graphene comprehensive physical performance is greatly lowered
It is significant.
The content of the invention
In view of the problems of the existing technology, it is an object of the invention to design to provide a kind of high-quality graphene material
The technical solution of simple production method.
The simple production method of a kind of high-quality graphene material, it is characterised in that comprise the following steps that：
1）Graphite, water and compounding substances are added in container and carry out shear agitation, the surface of the real time measure mixed solution
Tension, and by the mixed solution add graphite, water and or mixture, always maintain the surface tension of mixed solution
In the range of 30~60mN/m；
2）By step 1）To get to graphene product after obtained graphene dispersing solution removal solvent.
The simple production method of a kind of high-quality graphene material, it is characterised in that the compounding substances are poly-
Ethylene glycol, polyvinyl alcohol, alkylbenzenesulfonate, alkyl benzene sulphonate salt derivative, napadisilate, naphthalenedisulfonic acid salt derivative,
Anthraquinone disulfonic acid salt, anthraquinone disulfonic acid salt derivative, alkyl diphenyl ether disulfonate, alkyl diphenyl ether disulfonate derivative,
Alkylnaphthalene sulfonate, alkyl naphthalene sulfonic acid salt derivative, Alkyl dinaphthyl ether sulfonate, Alkyl dinaphthyl ether sulfonate derivative, kermes
Red, acid red, temptation one kind red, in quinoline yellow or arbitrary several mixture.
The simple production method of a kind of high-quality graphene material, it is characterised in that the graphite is natural stone
Black, highly directional thermal cracking graphite, expanded graphite, one kind in crystallite Delanium or arbitrary several mixture.
The simple production method of a kind of high-quality graphene material, it is characterised in that the solvent method that removes has
Body is the one or more in centrifugation, suction filtration, heating, drying, freeze-drying, spray drying.
A kind of simple production method of high-quality graphene material, it is characterised in that unstripped residue in raw material
Graphite continues cycling through utilization as raw material.
Compared with prior art, the invention has the advantages that：
1）Present invention firstly provides the surface tension for monitoring mixed solution in real time in shear agitation method, so as to accordingly adjust
The addition of various raw materials is controlled, is greatly improved graphene preparation efficiency, can effectively generate and stablizes a large amount of high quality
The dispersion liquid of graphene, the number of plies that be averaged of graphene obtained by preferred embodiment can be less than 5 layers.
2）Due to being not limited to concrete numerical value using the additive amount of preparation method of the present invention, various raw materials, make to obtain
The graphene dispersing solution concentration obtained is very high, and up to more than 5g/L, preferred embodiment concentration is up to more than 10g/L.The concentration system is so far
In modern document report, the rare high concentration of graphene is prepared using same mixture matter.
3）Graphene product prepared by the present invention can have porous structure and lateral dimension is very big, excellent up to 20 μm or more
Scheme is selected up to 60 μm or more, so far rare document report.
4）It is higher or can be right that the costs such as strong oxidizer, special intercalated material, strong reductant be directed to use in the present invention
Environment generate seriously endanger chemical raw material, because without as conventional oxidation method seriously destruction graphene-structured performance, from
And the graphene that can produce this method possesses higher physical property, the graphene electrical conductivity order of magnitude obtained by preferred embodiment is
104~105S/m。
5）Most of raw materials involved in the present invention are common chemical raw material, lower cost and environmental hazard
It is small, and the method for the present invention is very simple, without the technological process of complicated multi-step, is very suitable for large-scale industry metaplasia
Production.
6）The preparation method of graphene in the present invention can meet large-scale industrial production and practical application simultaneously
Three required key factors：High quality, high-volume, low cost, can possess while show low cost, high concentration, low layer number,
Graphene preparation method rare report so far of so excellent comprehensive characteristics such as high conductance, large scale.
7）Compared to conventional ultrasound preparation method, the shear agitation preparation method employed in the present invention has essence area
Not：The additive amount of various raw materials is not limited to concrete numerical value, and being continuously added for each raw material can improve mixed solution viscosity,
This can directly result in the decline of ultrasonic efficiency, and completely contradict with this, and the raising of solution viscosity can directly improve shearing and stir
Mix the preparation efficiency for obtaining graphene.
8) due to method using the present invention, remaining unstripped graphite raw material, needs not move through complicated place after preparation
Reason, can proceed with and recycle, obtain graphene solution, the production efficiency that greatly reduces that increased production cost.
Description of the drawings
Fig. 1 is the communication apparatus system example schematic employed in the present invention.
Fig. 2 is the Raman spectrum of graphene produced by the present invention.
Fig. 3 is the atomic force microscopy diagram of graphene produced by the present invention.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1：
By expanded graphite, native graphite, cetyl diphenyl ether sodium disulfonate, polyethylene glycol, quinoline yellow, cetyl benzene
Sodium sulfonate be added to the water with high-speed shearing emulsion machine with 3500rpm rotating speeds stirring 6 it is small when obtain graphene dispersing solution, root in the process
The surface tension factually measured adjusts or adds various raw materials at random so that surface tension maintains 35~43mN/m scopes
It is interior, upper strata high-quality graphene dispersion liquid, the graphene dispersion are then obtained after 30 minutes with 3000rpm rotating speeds centrifugal treating again
Liquid concentration be 6.2g/L, gained dispersion liquid is through centrifuging, filter, heating, drying, freeze-drying or spray drying after, obtain graphene
Product.The graphene product carries out Raman spectrum test and understands that obtained graphene is averaged the number of plies as 3 layers, as shown in Figure 2；Through original
Sub- force microscope observation learns graphene lateral dimension up to 40 μm or more, as shown in Figure 3；Graphene electrical conductivity can be obtained after tested
The order of magnitude is 105s/m。
The communication apparatus that can be used in the embodiment 1 as described in Figure 1 carries out surface tension test, which includes
The reaction vessel 1 and measure container 2 that pipeline connects, have been equipped with emulsification pretreatment machine 3, in container 2 is measured in reaction vessel 1
Carry out the measurement of solution surface tension.
Embodiment 2：
By highly directional native graphite, thermal cracking graphite, anthraquinone disulphonate, cetyl benzenesulfonic acid sodium, carmine addition
In water with high-speed shearing emulsion machine with 4000rpm rotating speeds stirring 8 it is small when obtain graphene dispersing solution, in the process according to surveying
Surface tension adjusts or adds various raw materials at random so that surface tension is maintained in the range of 45~49mN/m, then again with
2000rpm rotating speeds centrifugal treating obtains upper strata high-quality graphene dispersion liquid after forty minutes, which is
5.4g/L, gained dispersion liquid obtain graphene product after suction filtration.Understand that obtained graphene is averaged the number of plies as 4 layers after tested,
For lateral dimension up to 20 μm or more, the electrical conductivity order of magnitude is 104s/m。
Embodiment 3：
By expanded graphite, native graphite, crystallite Delanium, neopelex, polyvinyl alcohol, polyethylene glycol,
Naphthalene disulfonate be added to the water with high-speed shearing emulsion machine with 4200rpm rotating speeds stirring 7 it is small when obtain graphene dispersing solution, process
It is middle to adjust according to the surface tension surveyed or add various raw materials at random so that surface tension maintains 33~42mN/m models
In enclosing, upper strata high-quality graphene dispersion liquid, the graphene point are then obtained after 30 minutes with 3000rpm rotating speeds centrifugal treating again
Dispersion liquid concentration be 7.1g/L, gained dispersion liquid is through centrifuging, filter, heating, drying, freeze-drying or spray drying after, obtain graphite
Alkene product.Understand that the obtained graphene number of plies that be averaged is 4 layers after tested, lateral dimension is up to 30 μm or more, the electrical conductivity order of magnitude
For 105s/m。
Embodiment 4：
By expanded graphite, native graphite, quinoline yellow, acid red 27, carmine, double disodium 4-dodecyl-2,4 '-oxydibenzenesulfonates,
Anthraquinone disulphonate be added to the water with high-speed shearing emulsion machine with 3800rpm rotating speeds stirring 8 it is small when obtain graphene dispersing solution, mistake
It adjusts according to the surface tension surveyed in journey or adds various raw materials at random so that surface tension maintains 40~46mN/m
In the range of, upper strata high-quality graphene dispersion liquid, the graphene are then obtained after 35 minutes with 2500rpm rotating speeds centrifugal treating again
Dispersion liquid concentration is 5.1g/L, and gained dispersion liquid obtains graphene product after suction filtration.Understand that obtained graphene is put down after tested
The equal number of plies is 5 layers, and for lateral dimension up to 25 μm or more, the electrical conductivity order of magnitude is 104s/m。
Embodiment 5：
By native graphite, expanded graphite, red, the octadecyl benzenesulfonic acid sodium of temptation, dodecyl naphthalene diether sodium disulfonate, poly-
Ethylene glycol be added to the water with high-speed shearing emulsion machine with 4500rpm rotating speeds stirring 7 it is small when obtain graphene dispersing solution, root in the process
The surface tension factually measured adjusts or adds various raw materials at random so that surface tension maintains 32~40mN/m scopes
It is interior, upper strata high-quality graphene dispersion liquid, the graphene dispersion are then obtained after 30 minutes with 3100rpm rotating speeds centrifugal treating again
Liquid concentration be 6.6g/L, gained dispersion liquid is through centrifuging, filter, heating, drying, freeze-drying or spray drying after, obtain graphene
Product.Understand that the obtained graphene number of plies that be averaged is 3 layers after tested, lateral dimension is up to 35 μm or more, the electrical conductivity order of magnitude
105s/m。
Embodiment 6：
By expanded graphite, native graphite, polyethylene glycol, naphthalene disulfonate, quinoline yellow, famille rose, dodecyl diphenyl oxide
Sodium disulfonate be added to the water with high-speed shearing emulsion machine with 3500rpm rotating speeds stirring 8 it is small when obtain graphene dispersing solution, in the process
It adjusts according to the surface tension surveyed or adds various raw materials at random so that surface tension maintains 39~48mN/m scopes
It is interior, upper strata high-quality graphene dispersion liquid, the graphene dispersion are then obtained after 30 minutes with 3000rpm rotating speeds centrifugal treating again
Liquid concentration is 5.5g/L, and gained dispersion liquid obtains graphene product after suction filtration.Obtained graphene average layer is understood after tested
Number is 3 layers, and for lateral dimension up to 45 μm or more, the electrical conductivity order of magnitude is 105s/m。
Embodiment 7：
By expanded graphite, native graphite, neopelex, red, the dodecyl benzene sulfonic acid triethanolamine of temptation, quinoline
Quinoline Huang be added to the water with high-speed shearing emulsion machine with 3650rpm rotating speeds stirring 8 it is small when obtain graphene dispersing solution, basis in the process
The surface tension surveyed adjusts or adds various raw materials at random so that and surface tension is maintained in the range of 34~44mN/m,
Then upper strata high-quality graphene dispersion liquid, the graphene dispersing solution are obtained after 30 minutes with 3000rpm rotating speeds centrifugal treating again
Concentration is 8.2g/L, and gained dispersion liquid obtains graphene product after suction filtration.Understand that obtained graphene is averaged the number of plies after tested
For 4 layers, for lateral dimension up to 20 μm or more, the electrical conductivity order of magnitude is 105s/m。
Embodiment 8：
By native graphite, expanded graphite, polyvinyl alcohol, anthraquinone disulphonate, acid red 27, two sulphur of hexadecyl diphenyloxide
Sour sodium, dodecyl naphthalene disulfonate be added to the water with high-speed shearing emulsion machine with 4800rpm rotating speeds stirring 8 it is small when obtain graphite
Alkene dispersion liquid adjusts according to the surface tension surveyed in the process or adds various raw materials at random so that surface tension maintains
In the range of 31~40mN/m, upper strata high-quality graphene point is then obtained after 45 minutes with 2600rpm rotating speeds centrifugal treating again
Dispersion liquid, the graphene dispersing solution concentration are 6.1g/L, and gained dispersion liquid obtains graphene product after suction filtration.It understands after tested
Obtained graphene is averaged the number of plies as 4 layers, and for lateral dimension up to 36 μm or more, the electrical conductivity order of magnitude is 104s/m。
Embodiment 9：
By native graphite, expanded graphite, polyethylene glycol, polyvinyl alcohol, dodecyl benzene sulfonic acid triethanolamine, quinoline yellow,
Dodecyl dinaphthyl ether sodium disulfonate, anthraquinone disulphonate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, which are added to the water, uses high speed shear
Mulser with 3700rpm rotating speeds stirring 8 it is small when obtain graphene dispersing solution, adjusted in the process according to the surface tension surveyed
Or various raw materials are added at random so that surface tension is maintained in the range of 38~49mN/m, is then centrifuged again with 2800rpm rotating speeds
Processing 35 minutes after obtain upper strata high-quality graphene dispersion liquid, the graphene dispersing solution concentration be 6.4g/L, gained dispersion liquid
After suction filtration, graphene product is obtained.Understand that obtained graphene is averaged the number of plies as 3 layers after tested, lateral dimension is up to 60 μm
More than, the electrical conductivity order of magnitude is 104s/m。
Embodiment 10：
By native graphite, expanded graphite, double disodium 4-dodecyl-2,4 '-oxydibenzenesulfonates, acid red 27, famille rose, cetyl
Benzene sulfonic acid sodium salt, naphthalene disulfonate be added to the water with high-speed shearing emulsion machine with 4800rpm rotating speeds stirring 10 it is small when obtain graphene
Dispersion liquid adjusts according to the surface tension surveyed in the process or adds various raw materials at random so that surface tension maintains
In the range of 45~55mN/m, upper strata high-quality graphene is then obtained after 38 minutes with 2700rpm rotating speeds centrifugal treating again and is disperseed
Liquid, the graphene dispersing solution concentration are 5.1g/L, and gained dispersion liquid obtains graphene product after suction filtration.Institute is understood after tested
Graphene is made and is averaged the number of plies as 4 layers, lateral dimension is 21 μm or more, and the electrical conductivity order of magnitude is 104s/m。
Claims (4)
1. a kind of simple production method of high-quality graphene material, it is characterised in that comprise the following steps that：
1）Graphite, water and compounding substances are added in container and carry out shear agitation, the surface tension of the real time measure mixed solution,
And by added in the mixed solution graphite, water and or mixture, the surface tension for making mixed solution always maintains 30~
In the range of 60mN/m；The compounding substances are napadisilate, naphthalenedisulfonic acid salt derivative, anthraquinone disulfonic acid salt, anthraquinone two
Arbitrary several mixture in sulfonate derivatives, famille rose, acid red, the red, quinoline yellow of temptation；
2）By step 1）To get to graphene product after obtained graphene dispersing solution removal solvent.
A kind of 2. simple production method of high-quality graphene material as described in claim 1, it is characterised in that the stone
Ink is native graphite, highly directional thermal cracking graphite, expanded graphite, one kind in crystallite Delanium or arbitrary several mixing
Object.
3. a kind of simple production method of high-quality graphene material as described in claim 1, it is characterised in that described removes
Solvent method is specially the one or more in centrifugation, suction filtration, heating, drying, freeze-drying, spray drying.
4. a kind of simple production method of high-quality graphene material as described in claim 1, it is characterised in that in raw material not
The remaining graphite of stripping continues cycling through utilization as raw material.
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| CN113490641A (en) * | 2019-02-28 | 2021-10-08 | 积水化学工业株式会社 | Flaked graphite and method for producing same |
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| Scalable production of large quantities of defect-free few-layer graphene by shear exfoliation in liquids;Keith R. Paton et al;《Nature Materials》;20140420;第13卷;第625页左栏第1段、supplementary information 第S4节放大实验和第S6节中试实验 * |
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Address after: Room 19, No. 101-44, No. 1399, good road, front street, Cang Qian street, Yuhang District, Hangzhou, Zhejiang Applicant after: Hangzhou Wan pestle Mstar Technology Ltd Address before: 311321 No. 26, Changhua Road, Changhua Road, Ling'an City, Hangzhou, Zhejiang Province, No. 26, No. 1, 101 Applicant before: LIN'AN WANCHU MATERIAL TECHNOLOGY CO., LTD. |
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Effective date of registration: 20191204 Address after: 200050 No. 390, Anhua Road, Shanghai, Changning District Patentee after: Ruan Wei Address before: Room 19, No. 101-44, No. 1399, good road, front street, Cang Qian street, Yuhang District, Hangzhou, Zhejiang Patentee before: Hangzhou Wan pestle Mstar Technology Ltd |
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