CN109095462A - A kind of graphene and its preparation method and application - Google Patents
A kind of graphene and its preparation method and application Download PDFInfo
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- CN109095462A CN109095462A CN201810835291.4A CN201810835291A CN109095462A CN 109095462 A CN109095462 A CN 109095462A CN 201810835291 A CN201810835291 A CN 201810835291A CN 109095462 A CN109095462 A CN 109095462A
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Abstract
The present invention provides a kind of preparation methods of graphene, comprising the following steps: graphite microchip is dispersed in medium system, obtains dispersion liquid；Obtained dispersion liquid is uniformly mixed using mixing apparatus, obtained mixture is subjected to physics removing later, obtains graphene semifinished product；Obtained graphene semifinished product is importing directly into high pressure microfluidizer by circulating pump, is removed again, graphene slurry is obtained；Obtained graphene slurry is subjected to physics sedimentation or centrifugal screening classification, obtains different grades, stable graphene slurry；The graphene slurry of acquisition is diluted, is washed repeatedly, is dry, obtains graphene powder.The present invention also provides the graphene prepared by the above method and its applications.The present invention is assisted using pre- intercalation, and the method for multistage removing prepares graphene product, can greatly improve production efficiency and product quality, and it is pollution-free, product cost is controllable.
Description
Technical field
The invention belongs to technical field of nano material, it is related to a kind of graphene and its preparation method and application.
Background technique
Since being found (Novoselov, K.S.et.Science, 2004.306,666669.) from graphene in 2004,
The performances such as its excellent mechanics, conduction, thermally conductive, attracting all over the world more and more team carry out its theoretical and application and grind
Study carefully.Department of national governments, research institution and colleges and universities also launch respectively various incentive policies, encourage grinding in terms of grapheme material
Hair.But graphene price is higher, performance is unstable, lack corresponding test and applies standard, becomes and limits its extensive use
Stumbling-block.Therefore, exploitation can continuous production, environmental protection, cost controllable high-quality graphene and preparation process become current
Can one of research hotspot of field of graphene and graphene realize industrial scale applications, realize what traditional product updated
One of key.
There are two types of different approaches for the preparation method of graphene: Top-down approach and Bottom-up approach.Top-down
It include mechanical stripping method, liquid phase stripping method, supercritical CO in approach2Stripping method and chemistry redox stripping method；Bottom-up
It again include chemical vapour deposition technique (CVD), SiC epitaxial growth method, macromolecular self-assembly method in approach.
In many preparation methods, liquid phase removing, supercritical CO2Removing and oxidation-reduction method are to be easiest to realize industry
The preparation method that metaplasia produces.
Liquid phase stripping method is shearing and the release effect using High shear device or ultrasonic wave, under the conditions of liquid suspension
Prepared by graphene to graphite or expanded graphite.The stripping process of such technique mainly passes through shearing and ultrasonication is realized, dispersion
Medium and dispersing agent play peptizaiton, place graphene microchip reunion or return and fold, which does not chemically react, graphene crystal
Structure will not be destroyed, but yield is not high, be usually no more than 5%, and the piece diameter of graphene product is smaller.
Supercritical CO2The graphene sheet layer of the physical methods such as removing preparation mostly at 1-20 layers, single layer rate 10% hereinafter, and
And be easy back to fold, it needs twice dispersing or removing more, needs additionally to add dispersing agent；Advantage is that microstructural flaws are few, electric, warm
Performance is good, at low cost.
The graphene of oxidation-reduction method preparation can control lamella within 3 layers, and be not easy back to fold, and be more readily dispersed in
Dispersion, but there are microdefects it is more, electric, hot property is bad, at high cost, production process is seriously polluted the disadvantages of.
To sum up, existing graphene and preparation method thereof has some limitations, with Large scale processes production and stone
Black alkene high quality demand development is not inconsistent.
Summary of the invention
In view of this, it is a primary object of the present invention to provide a kind of graphene and its preparation method and application, it is intended to solve
Certainly need that a large amount of poisonous and hazardous chemical reagent or production efficiency are low, high-cost ask in conventional graphite alkene preparation process
Topic, with achieve the purpose that can continuous production, environmental protection, cost is controllable, can match with application end cost needs.
In order to reach above-mentioned purpose, the present invention provides a kind of preparation methods of graphene comprising following steps:
1) it prepares dispersion liquid: graphite microchip being dispersed in medium system, dispersion liquid is obtained；
Preferably, medium system described in step 1) can according to need it is optionally following first,
A) water system decentralized medium
Dispersing agent used in the aqueous dispersion medium is selected from pure water, polyethylene glycol, phenolic resin, ethyl acetate, third
Diol block polyethers, phenols, Arabic gum, polyvinylpyrrolidone, epoxy resin, fatty alcohol, polyoxyethylene ether, carboxymethyl
Cellulose, polyoxypropylene/ethylene copolymer, alkyl phenol, benzoyl peroxide, sulfonated polyaniline, neopelex, gallbladder
One of sour sodium, cetyl trimethylammonium bromide, sodium lignin sulfonate, sodium polymethacrylate or multiple combinations.
Preferably, the dispersing agent is selected from polyvinylpyrrolidone, fatty alcohol, ethylene oxide, sodium taurocholate, sulfonated polyaniline
One of or multiple combinations.
B) organic solvent type decentralized medium
Organic solvent used in the organic solvent type decentralized medium is selected from N-Methyl pyrrolidone, 1- crassitude
Ketone, acetamide, N- methyl propanamide, N-METHYLFORMAMIDE, N, dinethylformamide, tetrahydrofuran, ethyl alcohol, pyridine, I
One of primary glue, polyoxyethylene ether, polyethylene glycol, n-dodecyl-β-D-maltoside solution or multiple combinations.
Preferably, the organic solvent is selected from N-Methyl pyrrolidone, 1- methyl pyrrolidone, acetamide, N- methyl-prop
One of amide, N-METHYLFORMAMIDE, N, dinethylformamide, tetrahydrofuran or multiple combinations.
Preferably, in step 1), the surface of the medium system can be between 25-50mN/m.
Preferably, in step 1), the weight percent of the graphite microchip and dispersion liquid is 0.1:100-50:100.
It is highly preferred that the weight percent of the graphite microchip and dispersion liquid is 1:100-20:100 in step 1).
2) level-one is removed: the dispersion liquid that step 1) is obtained is uniformly mixed using mixing apparatus, the mixing that will be obtained later
Object carries out physics removing (second level removing), obtains graphene semifinished product (level-one removing product).
Preferably, in step 2), the mixing apparatus is in emulsifying device, mechanical stirring equipment, shearing dispersing apparatus
One or more combination.
Preferably, in step 2), physics removing equipment used is selected from high shear dispersion machine, milling apparatus, ultrasound
Equipment, the equipment may be equipped with circulating cooling system.
Preferably, in step 2), the operating condition of the high shear dispersion machine are as follows: shear velocity 40000-400000/s,
Revolving speed >=8000RPM, 0-60 DEG C of shear temperature.
It is highly preferred that in step 3), the operating condition of the high shear dispersion machine are as follows: shear velocity 200000-400000/
S, revolving speed 10000-30000RPM, 0-40 DEG C of shear temperature.
3) second level is removed: the graphene semifinished product that step 2) obtains being importing directly into high pressure microjet by circulating pump and is set
It in standby, is removed again (second level removing), obtains graphene slurry.
Preferably, in step 3), the circulating pump can be selected from one of jerk pump, plunger pump, screw pump, pressure pump
Or multiple combinations.
Preferably, in step 3), the high pressure microfluidizer can be selected from high pressure homogenizer, superhigh-voltage homogenizing machine, height
Press one of mulser or multiple combinations.
4) sieving and grading: the graphene slurry in step 3) is subjected to physics sedimentation or centrifugal screening is classified, obtains difference
Grade, stable graphene slurry.
Preferably, in step 4), the physics is settled into, by step 3) graphene slurry import precipitation apparatus in into
Row natural subsidence, then layering export；Or centrifugal screening classification is carried out, then layering export.
Preferably, in step 4), the precipitation apparatus is selected from one or more combinations of subsider, settling tank, centrifuge.
Preferably, in step 4), the precipitation apparatus is centrifuge.
Preferably, in step 4), the revolving speed of the centrifuge is 2000-8000 revs/min, and centrifugation time is 5-30 points
Clock.
Preferably, in step 4), centrifugal screening classification screening installation used is selected from vibrating screen, mesh screen, filter screen
One of or multiple combinations.
Preferably, before step 1), further include the steps that pre- intercalation, specifically: raw material is placed in high pressure reactor
It is interior, be filled with reaction medium, until 5-20MPa (preferably 7-15MPa), be warming up to 30-100 DEG C (preferably 40-70 DEG C) and with
The revolving speed of 100-3000RPM (preferably 500-2000RPM) stirs, 1-20min (preferably 1-5min) interior quick pressure releasing to 0
(first expand graphite flake edge interlamellar spacing with oxidants such as acid, then increasing temperature and pressure, makes intercalator enter interlayer, further expands
Intercalation is completed in big interlamellar spacing, then pressure release), obtain prestripping graphite microchip (slurry or powder).
Preferably, the high pressure reactor is autoclave, and the pressure-resistant upper limit is 10-20MPa.
Preferably, the reaction medium is selected from hydrochloric acid, sulfuric acid, nitric acid, acetic acid, oxalic acid, carbon dioxide, ethyl alcohol, N- methyl
One of pyrrolidones, N-METHYLFORMAMIDE, pyrene, pyrene formic acid, pyrene butyric acid, pyrene amine, pyrene sodium sulfonate or multiple combinations.
Preferably, the raw material be selected from flaky graphite, crystalline flake graphite, graphite powder, expanded graphite, can the swollen artificial stone of graphite
One of ink or multiple combinations.
Preferably, after step 4), include the steps that washing, drying, specifically: the graphene for obtaining step 4)
Slurry is diluted, washs repeatedly, is dry, obtains graphene powder.
It is highly preferred that the washing, dry step specifically: the graphene slurry for obtaining step 4) uses deionization
Water dilutes 2-3 times (preferably 2 times), and centrifugation to supernatant liquor substantially transparent washs 2-3 times (preferably 2 times), and removes upper layer
Obtained base pastes are dried clear liquid, to obtain graphene powder.
Preferably, the washing is selected from filtering and washing or centrifuge washing, and its purpose is to remove the dispersing agent in slurry.
Preferably, the mode of the drying is selected from one or more of freeze-drying, spray drying, revolving drying group
It closes, its purpose is to remove the decentralized medium in slurry.
In addition, invention further provides the graphenes being prepared by the above method.
In addition, the present invention also provides above-mentioned graphenes to be used to prepare electrically conductive ink, heat radiation coating, anticorrosive paint or compound
Application in material.
Compared with existing graphene preparation technology, the innovation of the invention consists in that with (pre-) intercalation stripping technology, height
Shearing lift-off technology, microjet lift-off technology and classification of sedimentation technology obtain the graphene product of high quality.
Firstly, (pre-) intercalation stripping technology is with weak acid or supercritical CO2Fluid is supplementary means, realizes graphite intercalation, is expanded
Big graphite layers away from.Then, disperse in the liquid phase, add dispersing agent, and graphite is removed using high shear lift-off technology,
It is preliminary to obtain graphene crude product.Finally, further removing using microjet lift-off technology to graphene crude product, graphite is prevented
Alkene microplate returns folded, the final graphene product for obtaining high quality.
Compared to preparation method traditional before, the present invention is mutually cooperateed with, is complementary to one another by preparation process, both can be single
It solely uses, preparation meets the inexpensive grapheme material of low-end applications；It can also be combined, the efficient high-quality graphene for preparing produces
Product.And be only under conditions of finely tuning preparation process, meet differential, the seriation demand of different application field product.
Such as above-mentioned technical proposal, it is provided by the invention can the controllable graphene preparation method of continuous production, environmental protection, cost,
At least have it is following the utility model has the advantages that
1, graphene preparation method provided by the invention uses pre- intercalation auxiliary multi-stage stripping technology, greatly improved
Charge stripping efficiency and product quality, compared with existing stripping technology, the present invention can obtain 100% charge stripping efficiency, wherein 1-
10 layers of graphene reaches 20% or more up to 80% or more, 1-3 layers of high-quality graphene.
2, graphene preparation method provided by the invention, use multistage stripping technology be applied alone or associated with method, according to
Practical application request obtains the graphene product for meeting cost requirement.
3, graphene preparation method provided by the invention, graphene slurry obtained is not easy to reunite, more stable, favorably
In the long-term preservation and transport of graphene.Contain dispersing agent in graphene slurry, dispersing agent herein is preferably polyvinyl pyrrole
Alkanone, fatty alcohol, ethylene oxide, sodium taurocholate, sulfonated polyaniline.In slurry, the compound of macromolecule or ionic is filled in stone
Between black alkene lamella, separation layer and support are formed, it is suppressed that the reunion of graphene.Therefore, macromolecule or ionic of the present invention
The addition for closing object so that the modified graphene slurry being prepared is more stable, be more conducive to graphene long-term preservation and
Transport.
4, graphene preparation method provided by the invention can fast and efficiently obtain the different numbers of plies point by classification
The graphene slurry of cloth.
5, graphene preparation method provided by the invention uses various kinds of equipment mature in the market, simple and convenient, more holds
Easily realize continuous industrialized production.
6, preparation method provided by the invention, preparation process free from admixture generates, it is therefore not necessary to the graphite being prepared
Alkene slurry carries out purification processes, further simplifies preparation process, and be conducive to the protection of environment.
7, preparation method provided by the invention, environmentally protective, cost is controllable, can continuous operations using physical method.
Detailed description of the invention
Fig. 1 is the process flow chart of graphene production of the invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of graphene film obtained in the embodiment of the present invention 1.
Specific embodiment
Present invention is further described in detail with Figure of description combined with specific embodiments below, but not as to this hair
Bright restriction.In the following description, what different " embodiment " or " embodiment " referred to is not necessarily the same embodiment.In addition,
Special characteristic, structure or feature in one or more embodiments can be combined by any suitable form.
Following a variety of materials or reagent are unless stated otherwise commercially available.
Embodiment 1
As shown in Figure 1, present embodiments providing a kind of preparation method of graphene comprising following steps:
Step 1, flaky graphite and pyrene amine are put into autoclave with weight ratio 1:1, are filled with carbon dioxide gas,
9MPa is boosted to, is heated up 32 DEG C, 1000 turns/min of revolving speed reacts 30 minutes, deflation pressure release, residue is collected, to obtain pre- stripping
From graphite microchip；
Step 2, pure water (deionized water) is added in graphite microchip step 1 obtained, prepares dispersion liquid, and graphite microchip with
The weight ratio of water is 5:95, is uniformly mixed using mechanical stirring equipment, and (shear velocity restriction is imported in high shear dispersion machine
3000-21000RPM, preferably 6000-16000RPM), it is set as 25 DEG C, 10000 turns/min of revolving speed, recycles 1 hour, carries out
Physics removing；
Step 3, slurry obtained in step 2 is importing directly into high-pressure emulsification machine by circulating pump, is set as temperature
25 DEG C, pressure 2MPa, recycle 0.5h；
Step 4, slurry obtained in step 3 is centrifuged, 5000 revs/min, is centrifuged 10 minutes, remove bottom
Precipitating, takes upper layer dispersion liquid；
Step 5, the dispersion liquid obtained in step 4 is added to spray drying device by circulating pump, 120 DEG C spraying dry
It is dry, solvent is removed, solid powder is collected, obtains graphene powder sample.
Above-mentioned graphene powder sample is scanned Electronic Speculum and projection Electronic Speculum test, concrete outcome is shown in Fig. 2.It is tied by test
Fruit it is found that preparation graphene powder sample lamella the thickness with a thickness of 1-10 carbon atomic layer, graphene sample transverse direction ruler
Very little i.e. piece diameter is larger, and the atom number of plies is less, has the perfection of lattice and high conductivity of high-quality graphene, and graphene yield is
The 85wt% for the flaky graphite weight being added, and bottom sediment can also repeat 2-5 step in step 4, to improve
Yield.
The graphene powder prepared using above-mentioned operation, can be used for electrically conductive ink, heat radiation coating, anticorrosive paint, composite wood
The fields such as material.
Embodiment 2
Present embodiments provide a kind of preparation method of graphene aqueous slurry comprising following steps:
Step 1, prestripping: flaky graphite and pyrene amine weight ratio 1:1 are put into autoclave, carbon dioxide is filled with
Gas boosts to 9MPa, heats up 32 DEG C, and 1000 turns/min of revolving speed reacts 30 minutes, deflation pressure release, residue is collected, to obtain
Prestripping graphite microchip；
Step 2, the removing of pre-dispersed and level-one: pure water is added in the graphite microchip that step 1 is obtained, and prepares dispersion liquid, and stone
The weight ratio of black microplate and water is 5:95, is uniformly mixed using mechanical stirring equipment, and (shear velocity in high shear dispersion machine is imported
Limit 3000-21000RPM, preferably 6000-16000RPM), it is set as 25 DEG C, 10000 turns/min of revolving speed, recycles 1 hour, with
Carry out physics removing；
Step 3, second level is removed: slurry obtained in step 2 is importing directly into high-pressure emulsification machine by circulating pump, if
It is set to 25 DEG C of temperature, pressure 2MPa, recycles 0.5h；
Step 4, sieving and grading and drying: slurry obtained in step 3 is centrifuged, and 5000 revs/min, from
The heart 10 minutes, bottom sediment is removed, upper layer dispersion liquid is taken, obtains graphene aqueous slurry.
The graphene aqueous slurry prepared using above-mentioned operation has slight reunion, and the graphite reunited in standing 3 months or more
Alkene piece is stirred energetically or ultrasonic power, and the graphene film of reunion is disconnected from each other.
The graphene aqueous slurry prepared using above-mentioned operation, can be used for electrically conductive ink, graphene/resin composite materials.
Embodiment 3
Present embodiments provide a kind of preparation method of graphene aqueous slurry comprising following steps:
Step 1, prestripping: flaky graphite is put into autoclave, is filled with carbon dioxide gas, is boosted to
9MPa heats up 32 DEG C, and 1000 turns/min of revolving speed reacts 30 minutes, deflation pressure release, collects residue, micro- to obtain prestripping graphite
Piece；
Step 2, the removing of pre-dispersed and level-one: NMP (N-Methyl pyrrolidone) is added in the graphite microchip that step 1 is obtained,
Dispersion liquid is prepared, and graphite microchip and the weight ratio of water are 5:95, are uniformly mixed using mechanical stirring equipment, and high shear point is imported
It dissipates in machine, is set as 25 DEG C, 10000 turns/min of revolving speed, recycle 1 hour, to carry out physics removing；
Step 3, second level is removed: slurry obtained in step 2 is importing directly into high-pressure emulsification machine by circulating pump, if
It is set to 25 DEG C of temperature, pressure 2MPa, recycles 0.5h；
Step 4, sieving and grading: slurry obtained in step 3 is centrifuged, and 5000 revs/min, is centrifuged 10 points
Clock removes bottom sediment, takes upper layer dispersion liquid, obtain graphene aqueous slurry.
The graphene aqueous slurry prepared using above-mentioned operation has slight reunion, but the graphite reunited in standing 3 months or more
After alkene piece is agitated or ultrasound, the graphene film of reunion can be disconnected from each other.
The graphene NMP phase slurry prepared using above-mentioned operation, can be used for lithium battery conductive agent, graphene/resin compounded
Material Field.
Embodiment 4
Present embodiments provide a kind of preparation method of graphene comprising following steps:
Step 1, pre-dispersed: after flaky graphite and fatty alcohol are mixed with weight ratio 2:1, by 5wt%, (front is mixed
The weight ratio of object and water is 95:5) it is added in pure water, under normal temperature condition, 1000 turns/min stirs 30min；
Step 2, level-one is removed: the product that step 1 is obtained imports in high shear dispersion machine, is set as 25 DEG C, revolving speed
It 10000 turns/min, recycles 1 hour；
Step 3, second level is removed: slurry obtained in step 2 is importing directly into high-pressure emulsification machine by circulating pump, if
It is set to 25 DEG C of temperature, pressure 2MPa, recycles 0.5h；
Step 4, sieving and grading: slurry obtained in step 3 is centrifuged, and 5000 revs/min, is centrifuged 10 points
Clock removes bottom sediment, takes upper layer dispersion liquid；
Step 5, dry: the dispersion liquid obtained in step 4 is added to spray drying device, 120 DEG C of sprays by circulating pump
Mist is dry, removes solvent, collects solid powder, obtains graphene powder sample.
The graphene powder prepared using above-mentioned operation, can be used for electrically conductive ink, heat radiation coating, anticorrosive paint, composite wood
The fields such as material.
In the above-described embodiments, it all emphasizes particularly on different fields to the description of each embodiment, there is no the portion being described in detail in some embodiment
Point, reference can be made to the related descriptions of other embodiments.
It is understood that the correlated characteristic in above-mentioned apparatus can be referred to mutually.In addition, in above-described embodiment " the
One ", " second " etc. is and not represent the superiority and inferiority of each embodiment for distinguishing each embodiment.
In the instructions provided here, numerous specific details are set forth.It is to be appreciated, however, that implementation of the invention
Example can be practiced without these specific details.In some instances, well known structure and skill is not been shown in detail
Art, so as not to obscure the understanding of this specification.
Technical characteristic in the claims in the present invention and/or specification can be combined, and a combination thereof mode is not limited to weigh
The combination obtained in benefit requirement by adduction relationship.It is combined by the technical characteristic in claim and/or specification
The technical solution and protection scope of the present invention arrived.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by those familiar with the art, all answers
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be with the scope of protection of the claims
It is quasi-.
Claims (10)
1. a kind of preparation method of graphene, which comprises the following steps:
1) it prepares dispersion liquid: graphite microchip being dispersed in medium system, dispersion liquid is obtained；
2) level-one remove: the dispersion liquid that step 1) is obtained using mixing apparatus be uniformly mixed, later by obtained mixture into
The removing of row physics, obtains graphene semifinished product；
3) second level is removed: the graphene semifinished product that step 2) obtains is importing directly into high pressure microfluidizer by circulating pump
In, it is removed again, obtains graphene slurry；
4) sieving and grading: carrying out physics sedimentation or centrifugal screening for the graphene slurry in step 3) and be classified, obtain different grades,
Stable graphene slurry.
2. preparation method according to claim 1, which is characterized in that in step 1), the medium system is appointed as needed
Choosing it is following first,
A) water system decentralized medium
Dispersing agent used in the water system decentralized medium is selected from pure water, polyethylene glycol, phenolic resin, ethyl acetate, propylene glycol
Block polyether, phenols, Arabic gum, polyvinylpyrrolidone, epoxy resin, fatty alcohol, polyoxyethylene ether, carboxymethyl cellulose
Element, polyoxypropylene/ethylene copolymer, alkyl phenol, benzoyl peroxide, sulfonated polyaniline, neopelex, cholic acid
One of sodium, cetyl trimethylammonium bromide, sodium lignin sulfonate, sodium polymethacrylate or multiple combinations；
Preferably, the dispersing agent is in polyvinylpyrrolidone, fatty alcohol, ethylene oxide, sodium taurocholate, sulfonated polyaniline
One or more combinations；
B) organic solvent type decentralized medium
Organic solvent used in the organic solvent type decentralized medium be selected from N-Methyl pyrrolidone, 1- methyl pyrrolidone,
Acetamide, N- methyl propanamide, N-METHYLFORMAMIDE, N, dinethylformamide, tetrahydrofuran, ethyl alcohol, pyridine, Arab
One of glue, polyoxyethylene ether, polyethylene glycol, n-dodecyl-β-D-maltoside solution or multiple combinations；
Preferably, the organic solvent be selected from N-Methyl pyrrolidone, 1- methyl pyrrolidone, acetamide, N- methyl propanamide,
One of N-METHYLFORMAMIDE, N, dinethylformamide, tetrahydrofuran or multiple combinations.
3. preparation method according to claim 1, which is characterized in that
In step 1), the surface of the medium system can be between 25-50mN/m；The graphite microchip and the weight of dispersion liquid hundred
Divide than being 0.1:100-50:100, it is preferable that the weight percent of the graphite microchip and dispersion liquid is 1:100-20:100；
In step 2), the mixing apparatus is selected from one or more of emulsifying device, mechanical stirring equipment, shearing dispersing apparatus
Combination；Physics removing equipment used is selected from high shear dispersion machine, milling apparatus, ultrasonic device；The high shear dispersion
The operating condition of machine are as follows: shear velocity 40000-400000/s, revolving speed >=8000RPM, 0-60 DEG C of shear temperature；Preferably, institute
State the operating condition of high shear dispersion machine are as follows: shear velocity 200000-400000/s, revolving speed 10000-30000RPM, shearing temperature
0-40 DEG C of degree.
4. preparation method according to claim 1, which is characterized in that
In step 3), the circulating pump is selected from one of jerk pump, plunger pump, screw pump, pressure pump or multiple combinations；It is described
High pressure microfluidizer can be selected from one of high pressure homogenizer, superhigh-voltage homogenizing machine, high-pressure emulsification machine or multiple combinations；
In step 4), the physics is settled into, and the graphene slurry in step 3) is carried out physics sedimentation or centrifugal screening is classified,
It imports in precipitation apparatus, carries out sedimentation layering；Later by sedimentation layering export；The precipitation apparatus be selected from subsider, settling tank,
One or more combinations of centrifuge；Centrifugal screening classification screening installation used is in vibrating screen, mesh screen, filter screen
One or more combinations；The washing is selected from filtering and washing or centrifuge washing；The mode of the drying is selected from freeze-drying, spray
One or more of mist is dry, revolving is dry combination.
5. preparation method according to claim 1, which is characterized in that before step 1), further include the steps that pre- intercalation,
Specifically: raw material is placed in high pressure reactor, reaction medium is filled with, boost to 5-20MPa, be warming up to 30-100 DEG C and with
The revolving speed of 100-3000RPM stirs, and quick pressure releasing obtains prestripping graphite microchip to 0 in 1-20min.
6. preparation method according to claim 5, which is characterized in that the high pressure reactor is autoclave,
The pressure-resistant upper limit is 10-20MPa；The reaction medium is selected from hydrochloric acid, sulfuric acid, nitric acid, acetic acid, oxalic acid, carbon dioxide, ethyl alcohol, N-
One of methyl pyrrolidone, N-METHYLFORMAMIDE, pyrene, pyrene formic acid, pyrene butyric acid, pyrene amine, pyrene sodium sulfonate or multiple combinations；Institute
State raw material be selected from flaky graphite, crystalline flake graphite, graphite powder, expanded graphite, can one of swollen graphite electrographite or a variety of
Combination.
7. preparation method according to claim 1, which is characterized in that further include washing, dry step after step 4)
Suddenly, specifically: the graphene slurry that step 4) obtains is diluted, is washed repeatedly, is dry, obtains graphene powder.
8. preparation method according to claim 7, which is characterized in that the washing, dry step specifically: by step
4) the graphene slurry obtained dilutes 2-3 times using deionized water, and centrifugation to supernatant liquor substantially transparent is washed 2-3 times, and removed
Supernatant liquor is removed, obtained base pastes are dried, to obtain graphene powder.
9. a kind of graphene that method according to claim 1-8 is prepared.
10. a kind of graphene according to claim 9 is being used to prepare electrically conductive ink, heat radiation coating, anticorrosive paint or is answering
Application in condensation material.
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735308A (en) * | 2018-12-29 | 2019-05-10 | 厦门十一维科技有限公司 | Adjustable uncured graphene composite material of thermal conductivity and the preparation method and application thereof |
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| CN114927694A (en) * | 2022-06-06 | 2022-08-19 | 浙江华荣电池股份有限公司 | Alkaline dry battery and preparation method thereof |
| CN115924897A (en) * | 2023-02-20 | 2023-04-07 | 江苏希诚新材料科技有限公司 | Device and method for centrifugally stripping single-layer/few-layer graphene dispersion liquid |
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| CN109735308A (en) * | 2018-12-29 | 2019-05-10 | 厦门十一维科技有限公司 | Adjustable uncured graphene composite material of thermal conductivity and the preparation method and application thereof |
| CN110042284A (en) * | 2019-05-08 | 2019-07-23 | 东南大学 | A kind of preparation method of high-strength aluminum alloy |
| CN110386597A (en) * | 2019-09-02 | 2019-10-29 | 石墨烯科技有限公司 | Large-scale production thin graphene equipment and large-scale production thin graphene method |
| CN110386597B (en) * | 2019-09-02 | 2022-09-23 | 石墨烯科技有限公司 | Equipment and method for large-scale production of thin-layer graphene |
| CN111040863A (en) * | 2019-12-12 | 2020-04-21 | 贵安新区瑞诚生物工程有限公司 | Preparation method of graphene lubricating oil, graphene lubricating oil and application |
| CN112978723A (en) * | 2019-12-17 | 2021-06-18 | 山东海科创新研究院有限公司 | Small-size graphene powder and preparation method and application thereof |
| CN113061370A (en) * | 2020-01-02 | 2021-07-02 | 中国科学院福建物质结构研究所 | Graphene ink and preparation method and application thereof |
| CN111117369A (en) * | 2020-02-05 | 2020-05-08 | 广州特种承压设备检测研究院 | Polyaniline functionalized graphene conductive ink and preparation method thereof |
| CN111232982A (en) * | 2020-03-18 | 2020-06-05 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional Ti3C2TXMethod for peeling nanosheet |
| CN111628172A (en) * | 2020-05-12 | 2020-09-04 | 山东领军科技集团有限公司 | Production process of graphene-based battery conductive agent |
| CN111732094A (en) * | 2020-07-07 | 2020-10-02 | 北京石墨烯研究院 | Method for preparing graphene through ultrasonic-assisted supercritical liquid phase stripping |
| CN112210039B (en) * | 2020-10-12 | 2022-08-19 | 中国石油大学(华东) | Preparation method of dispersant for oil-displacing graphene |
| CN112210039A (en) * | 2020-10-12 | 2021-01-12 | 中国石油大学(华东) | Preparation method of dispersant for oil-displacing graphene |
| CN112694083A (en) * | 2021-02-01 | 2021-04-23 | 天津艾克凯胜石墨烯科技有限公司 | Method for continuously producing graphene quantum dot slurry on large scale |
| CN112694083B (en) * | 2021-02-01 | 2022-10-21 | 天津艾克凯胜石墨烯科技有限公司 | Method for continuously producing graphene quantum dot slurry on large scale |
| CN112707390A (en) * | 2021-02-23 | 2021-04-27 | 刘仁武 | Graphene powder preparation method and preparation equipment |
| CN113479869A (en) * | 2021-06-30 | 2021-10-08 | 杭州烯鲸新材料科技有限公司 | Method for grading and screening particle size of graphene |
| CN114212781A (en) * | 2021-12-23 | 2022-03-22 | 江苏杉元科技有限公司 | Low-foam high-conductivity graphene aqueous slurry and preparation method thereof |
| CN114751401A (en) * | 2022-03-14 | 2022-07-15 | 重庆石墨烯研究院有限公司 | Graphite allyl acid resin oily dispersion liquid and preparation method thereof |
| CN114751401B (en) * | 2022-03-14 | 2024-04-19 | 重庆石墨烯研究院有限公司 | Graphene acrylic resin oily dispersion liquid and preparation method thereof |
| CN114735686A (en) * | 2022-04-29 | 2022-07-12 | 湖州市吴兴区核源金属新材研究院 | Preparation method of graphene aqueous solution and graphene nanosheet |
| CN114735686B (en) * | 2022-04-29 | 2024-05-03 | 湖州市吴兴区核源金属新材研究院 | Preparation methods of graphene aqueous solution and graphene nanosheets |
| CN114927694A (en) * | 2022-06-06 | 2022-08-19 | 浙江华荣电池股份有限公司 | Alkaline dry battery and preparation method thereof |
| CN115924897A (en) * | 2023-02-20 | 2023-04-07 | 江苏希诚新材料科技有限公司 | Device and method for centrifugally stripping single-layer/few-layer graphene dispersion liquid |
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