CN107973292A - A kind of devices and methods therefor for producing graphene - Google Patents
A kind of devices and methods therefor for producing graphene Download PDFInfo
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- CN107973292A CN107973292A CN201610931781.5A CN201610931781A CN107973292A CN 107973292 A CN107973292 A CN 107973292A CN 201610931781 A CN201610931781 A CN 201610931781A CN 107973292 A CN107973292 A CN 107973292A
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Abstract
A kind of device for producing graphene, it is to be handled the mixed solution that a graphite is mixed with a solvent for one, the device includes a seal cavity, one presser unit, one high pressure nozzle and a heating unit, the seal cavity houses the mixed solution, the presser unit provides a pressure to the seal cavity to carry out a pressure stroke to the mixed solution, and a Part I of the solvent is set to penetrate into an interlayer spacings of the graphite, the mixed solution for completing the pressure stroke is discharged and a Part II of the solvent is penetrated into the interlayer spacings of the graphite by the high pressure nozzle from the seal cavity, the heating unit carries out the mixed solution discharged from the seal cavity one heating stroke, make those solvent evaporations in the infiltration graphite and produce an outward thrust and form a graphene.
Description
Technical field
The present invention is to be related to a kind of devices and methods therefor for producing graphene, the device of espespecially a kind of quick production graphene
And its method.
Background technology
Graphene (Graphene) is nano material most thin and most hard at present, in general, the acquirement side of graphene
The carbon-coating of graphite can be carried out tearing layer open and obtained by formula by a variety of isolation technics.
As TaiWan, China patent of invention discloses No. 201522214, a kind of preparation method of nano-graphene piece is proposed, wrap
Contain：One intercalation oxidation step, is that the mixture of a graphite material and an at least intercalator and an at least oxidant is carried out intercalation
Oxidation reaction, and form a graphite oxide；One hot strip step, which is taken out, and by the graphite oxide
A heat source is contacted, the graphite oxide is decomposed into multiple nano-graphite chip architectures by expansion or stripping；One mechanical stripping walks
Suddenly, such nano-graphite chip architecture is suspended in a liquid, and a mechanical shear stress is imposed to the liquid, make such nano-graphite
The lateral dimension and reduced down in thickness of chip architecture, and peeling off becomes multiple nano-graphene pieces, and such nano-graphene piece is with being somebody's turn to do
Liquid forms a nano-graphene piece suspension；One drying steps, nano-graphene piece suspension drying is separated and received and paid out
Rice graphene film；And reduction and a heat treatment step, it is to be positioned over nano-graphene piece to be passed through a reducing atmosphere, and by temperature
Degree is increased in the environment of a heat treatment temperature, to reduce the oxygen content of such nano-graphene piece, and reduces lattice defect.
Or such as TaiWan, China patent of invention bulletin I 522314, propose a kind of scale volume production graphene and graphene
The manufacturing equipment of oxide, it includes：First electrode, it is the electrode tip holder comprising graphite starting material, and second electrode, it is bag
The electrode tip holder of graphitiferous original material, a metal or the mixture comprising graphite and metal, and an electrolytic cell, wherein filling electricity
Liquid is solved, sets the first electrode and the second electrode to be connected in the electrolyte and with a power supply unit, wherein the power supply supplies
Device is answered to provide the first bias and the second bias, and a filtering and the module of separation product, for collecting graphene and graphene oxygen
Compound product.
Among the above prior art, TaiWan, China patent of invention discloses No. 201522214 institute in a manner of redox
The graphene-structured of acquisition is usually imperfect, that is, the structural failure of part during disassembling, will so cause graphene conductive
Property or poor heat conduction.TaiWan, China patent of invention bulletin I 522314 electrolytically carries out the process that graphene is disassembled
In, since action pane is small, when further to control the number of plies for tearing graphene after layer open fewer, the electric current that is turned on also it is opposite more
It is small, the electrolysis of graphene is torn the shortcomings that interval velocity substantially reduces and causes speed of production slower open.
The content of the invention
It is a primary object of the present invention to propose a kind of devices and methods therefor for producing graphene, to solve existing graphene
Preparation method destructible graphene-structured and bad speed of production the problem of.
In order to achieve the above object, the present invention provides a kind of device for producing graphene, it is to be directed to one by a graphite and a solvent
The mixed solution mixed is handled, which adds comprising a seal cavity, a presser unit, a high pressure nozzle and one
Hot cell, the seal cavity house the mixed solution, which connects with the seal cavity, there is provided a pressure to the sealing
Cavity makes a Part I of the solvent penetrate between an interlayer of the graphite to carry out a pressure stroke to the mixed solution
Gap, the high pressure nozzle are connected with the seal cavity, the mixed solution of the pressure stroke will be completed from seal cavity discharge and
A Part II of the solvent is set to penetrate into the interlayer spacings of the graphite, which connects with the high pressure nozzle, to certainly should
The mixed solution of seal cavity discharge carries out a heating stroke, make those solvent evaporations in the infiltration graphite and produce one to
Extrapolability and form a graphene.
Wherein, which has one between 100MPa to the pressure between 600MPa.
Wherein, which has a heating-up temperature between 60 DEG C to 300 DEG C.
Wherein, which has an aperture between 50 μm to 2000 μm.
Wherein, further include a collector unit connected with the heating unit and one be arranged at the collector unit and the heating
Separative element between unit.
Wherein, which includes a quartz ampoule passed through for the graphene and one around the copper outside the quartz ampoule
Pipe.
In order to achieve the above object, the present invention separately provides a kind of method for producing graphene, comprise the steps of：
One graphite is mixed with a solvent and forms a mixed solution, and the mixed solution is injected into a seal cavity；
The presser unit that a pressure to the seal cavity are provided by one carries out a pressure stroke to the mixed solution, so that
One Part I of the solvent in the mixed solution penetrates into an interlayer spacings of the graphite；
The mixed solution for completing the pressure stroke is discharged from the seal cavity to make the solvent by a high pressure nozzle
A Part II penetrate into the interlayer spacings of the graphite；And
One heating stroke carries out the mixed solution discharged from the high pressure nozzle by a heating unit, makes the infiltration stone
Those solvent evaporations in ink and produce an outward thrust and form a graphene.
Wherein, which has one between 100MPa to the pressure between 600MPa.
Wherein, which has a heating-up temperature between 60 DEG C to 300 DEG C.
Wherein, which has an aperture between 50 μm to 2000 μm.
As known from the above, the present invention is compared to the accessible effect of the prior art, and the present invention utilizes the presser unit
Pressure release after first pressurizeing to the mixed solution respectively with the high pressure nozzle, so that more solvents penetrate into the layer of the graphite in batches
Between gap, recycle the heating unit to carry out the heating stroke to the mixed solution, so as to penetrate into those solvents in the graphite
Vaporize and produce the outward thrust and form the graphene, therefore this case can obtain the graphene of structural integrity and produce graphene
Speed and yield are significantly increased.
Brief description of the drawings
Fig. 1 is the schematic device that graphene is produced in one embodiment of the invention.
Fig. 2, is the step flow chart that graphene is produced in one embodiment of the invention.
Wherein, reference numeral：
Seal cavity 10
Presser unit 20
High pressure nozzle 30
Heating unit 40
Material storage tube 50
First control valve 60
Second control valve 70
Separative element 80
Collector unit 90
Embodiment
It is related to detailed description of the invention and technology contents, now just coordinates schema to be described as follows：
It please arrange in pairs or groups as shown in fig.1, the schematic device of the production graphene for one embodiment of the invention, the present invention are one
Kind produce the device of graphene, handled for a mixed solution, the mixed solution mixed with a solvent by a graphite and
Into the device includes a seal cavity 10, a presser unit 20, a high pressure nozzle 30 and a heating unit 40, the annular seal space
Body 10 is used to house the mixed solution, which connects with the seal cavity 10, and provides a pressure to the annular seal space
Body 10 makes a Part I of the solvent penetrate into an interlayer spacings of the graphite to carry out a pressure stroke to the mixed solution,
In an embodiment, the pressure stroke which is provided has one between 100MPa to the pressure between 600MPa
Power；In a preferred embodiment, which has one between 200MPa to the pressure between 400MPa.
The high pressure nozzle 30 is connected with the seal cavity 10, will complete the mixed solution of the pressure stroke from the annular seal space
Body 10 discharges and a Part II of the solvent is penetrated into the interlayer spacings of the graphite, in this present embodiment, the high pressure nozzle
30 have an aperture between 50 μm to 2000 μm, and the wherein material of the high pressure nozzle 30 can be diamond, hexagonal boron nitride
Monocrystalline, single-crystal silicon carbide, sapphire single-crystal.
The heating unit 40 is connected with the high pressure nozzle 30, and one is carried out to the mixed solution discharged from the high pressure nozzle 30
Stroke is heated, makes those solvent evaporations in the infiltration graphite and produces an outward thrust and the graphite is disassembled into a graphite
The Fan Dewaerli of alkene, the wherein outward thrust much larger than the interlayer spacings of the graphite.In this present embodiment, the heating unit
40 include a quartz ampoule 41 and a copper pipe 42, and the quartz ampoule 41 is for the graphene by, the copper pipe 42 around the quartz ampoule
41 peripheries and be connected with a high frequency heater, the high frequency heater and the copper pipe 42 utilize alternating electromagnetism sensing heating original
Reason makes the heating stroke have a heating-up temperature between 60 DEG C to 300 DEG C, the wherein heating rate in the quartz ampoule 41
Between 10 DEG C/sec to 30 DEG C/sec, the above heating unit 40 only lift the quartz ampoule 41 arrange in pairs or groups the copper pipe 42 exemplified by, only
The heating unit of the heating-up temperature can be provided, be not limited.
In the present invention, the device of the production graphene further includes a material storage tube 50, the control of one first control valve 60, one second
Valve 70, a separative element 80 and a collector unit 90 processed, the material storage tube 50 are connected with the seal cavity 10, mixed for storing this
Solution is closed, which is arranged between the material storage tube 50 and the seal cavity 10, for controlling by the material storage tube 50
The flow of the mixed solution in the seal cavity 10 is flowed into, which is arranged at the seal cavity 10 and the high pressure spray
Between mouth 30, the flow of the mixed solution in the high pressure nozzle 30, the collector unit are flowed into by the seal cavity 10 for controlling
90 connect with the heating unit 40 and are used to collect the graphene, such as electrostatic trap, which is arranged at the receipts
Collect between unit 90 and the heating unit 40, such as cyclone separator, the separative element 80 can be directed to from 40 row of the heating unit
The graphene that goes out is separated according to different-thickness, the collector unit 90 then will after separation thickness be less than 3 nanometers (<10 layers)
The graphene is collected.In an embodiment, the seal cavity 10, the presser unit 20, the high pressure nozzle 30, the heating unit
40th, the material storage tube 50, first control valve 60, second control valve 70, the separative element 80 and the collector unit 90 be by
One conducting pipeline is connected.
It please arrange in pairs or groups as shown in fig.2, the step flow chart of the production graphene for one embodiment of the invention, the present invention are one
The method that kind produces graphene, comprises the steps of：
Step S1：First a graphite is mixed with a solvent and forms a mixed solution, and it is close that the mixed solution is injected this
Cavity 10 is sealed, in this present embodiment, which can be 1-methyl-2-pyrrolidinone (N-Methyl-2-pyrrolidone, abbreviation
NMP), tetrahydrofuran (Tetrahydrofuran, abbreviation THF), toluene (Toluene), ethyl acetate (Ethyl acetate),
Isopropanol (Isopropanol), ethanol (Ethanol), acetone (Acetone), butanone (Methyl Ethyl Ketone, abbreviation
MEK), chloroform (Chloroform), 2- butylamines (2Amino-butane) or pure water respectively with dodecyl benzene sulfonic acid
Sodium (Sodium Dodecyl Benzene Sulfonate, abbreviation SDBS), polystyrenesulfonate (poly styrene
Sulfonate), abbreviation PSS), NONIN HS 240 (Polyoxyenthylene octyl phenyl ether) adds
Add.
Step S2：A pressure is provided by the presser unit 20 to the seal cavity 10 to carry out one to the mixed solution to add
Stroke is pressed, in an embodiment, which has one between 100MPa to the pressure between 600MPa, preferably implements in one
In example, which has one between 200MPa to the pressure between 400MPa, due to the increase of pressure, makes the mixed solution
In a Part I of the solvent penetrate into interlayer spacings of the graphite.
Step S3：After the pressure reaches a setting pressure, second control valve 70 is opened and by the high pressure nozzle 30
The mixed solution for completing the pressure stroke is discharged from the seal cavity 10, wherein the high pressure nozzle have one between 50 μm extremely
Aperture between 2000 μm, due to therefore swollen from the graphite instantaneous loss of pressure in the mixed solution that the seal cavity 10 is discharged
It is swollen, and a Part II of the solvent is penetrated into the interlayer spacings of the graphite, this step should to penetrate into more solvents
Interlayer spacings.
Step S4：The mixed solution from the high pressure nozzle 30 discharge while, it is molten to the mixing by the heating unit 40
Liquid carries out a heating stroke, makes those solvent evaporations in the infiltration graphite and produces an outward thrust and disassemble into the graphite
The Fan Dewaerli of one graphene, the wherein outward thrust much larger than the interlayer spacings of the graphite.In this present embodiment, should add
Hot stroke has a heating-up temperature between 60 DEG C to 300 DEG C.
In conclusion devices and methods therefor of the present invention for production graphene, due to the present invention using the presser unit and
Pressure release after the high pressure nozzle respectively first pressurizes the mixed solution, so that more solvents penetrate into the interlayer of the graphite in batches
Gap, recycles the heating unit to carry out the heating stroke to the mixed solution, so as to penetrate into those solvent vapour in the graphite
Change and produce the outward thrust and form the graphene, therefore this case can obtain the graphene of structural integrity and produce the speed of graphene
Degree and yield are significantly increased.
Certainly, the present invention can also have other various embodiments, ripe in the case of without departing substantially from spirit of the invention and its essence
Various corresponding changes and deformation, but these corresponding changes and deformation can be made according to the present invention by knowing those skilled in the art
The protection domain of the claims in the present invention should all be belonged to.
Claims (10)
1. a kind of device for producing graphene, is at a mixed solution for mixing a graphite with a solvent
Reason, it is characterised in that the device includes：
One houses the seal cavity of the mixed solution；
One presser unit connected with the seal cavity a, there is provided pressure to the seal cavity is added with carrying out one to the mixed solution
Stroke is pressed, and a Part I of the solvent is penetrated into an interlayer spacings of the graphite；
One high pressure nozzle connected with the seal cavity, the mixed solution for completing the pressure stroke is discharged from the seal cavity
And a Part II of the solvent is set to penetrate into the interlayer spacings of the graphite；And
One heating unit connected with the high pressure nozzle, carries out a heating to the mixed solution discharged from the seal cavity and goes
Journey, makes those solvent evaporations in the infiltration graphite and produces an outward thrust and form a graphene.
2. it is according to claim 1 production graphene device, it is characterised in that the pressure stroke have one between
100MPa is to the pressure between 600MPa.
3. the device of production graphene according to claim 1, it is characterised in that the heating stroke has one between 60 DEG C
Heating-up temperature between 300 DEG C.
4. the device of production graphene according to claim 1, it is characterised in that the high pressure nozzle has one between 50 μm
Aperture between 2000 μm.
5. the device of production graphene according to claim 1, it is characterised in that further include one and connected with the heating unit
Collector unit and one be arranged at separative element between the collector unit and the heating unit.
6. the device of production graphene according to claim 1, it is characterised in that the heating unit includes one and supplies the graphite
Quartz ampoule that alkene passes through and one is around the copper pipe outside the quartz ampoule.
A kind of 7. method for producing graphene, it is characterised in that comprise the steps of：
One graphite is mixed with a solvent and forms a mixed solution, and the mixed solution is injected into a seal cavity；
The presser unit that a pressure to the seal cavity are provided by one carries out a pressure stroke to the mixed solution, so that this is mixed
The Part I for closing the solvent in solution penetrates into an interlayer spacings of the graphite；
The mixed solution for completing the pressure stroke is discharged from the seal cavity to make the one of the solvent by a high pressure nozzle
Part II penetrates into the interlayer spacings of the graphite；And
One heating stroke carries out the mixed solution discharged from the high pressure nozzle by a heating unit, makes in the infiltration graphite
Those solvent evaporations and produce an outward thrust and form a graphene.
8. it is according to claim 7 production graphene method, it is characterised in that the pressure stroke have one between
100MPa is to the pressure between 600MPa.
9. the method for production graphene according to claim 7, it is characterised in that the heating stroke has one between 60 DEG C
Heating-up temperature between 300 DEG C.
10. the method for production graphene according to claim 7, it is characterised in that the high pressure nozzle has one between 50 μ
Aperture between m to 2000 μm.
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| WO2014163127A1 (en) * | 2013-04-05 | 2014-10-09 | 積水化学工業株式会社 | Method for manufacturing flaked graphite and flaked graphite liquid dispersion, as well as flaked graphite, flaked graphite liquid dispersion, and flaked graphite/resin composite material |
| CN105776193A (en) * | 2016-02-29 | 2016-07-20 | 成都新柯力化工科技有限公司 | Method for preparing graphene nanoplatelets with pulsed high pressure water jet mill |
| CN105819437A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for large-scale clean graphene preparation |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103723707A (en) * | 2012-10-16 | 2014-04-16 | 铼钻科技股份有限公司 | Graphene sheet preparation method and graphene sheet prepared by same |
| WO2014163127A1 (en) * | 2013-04-05 | 2014-10-09 | 積水化学工業株式会社 | Method for manufacturing flaked graphite and flaked graphite liquid dispersion, as well as flaked graphite, flaked graphite liquid dispersion, and flaked graphite/resin composite material |
| CN103418159A (en) * | 2013-05-09 | 2013-12-04 | 青岛科技大学 | New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid |
| CN105776193A (en) * | 2016-02-29 | 2016-07-20 | 成都新柯力化工科技有限公司 | Method for preparing graphene nanoplatelets with pulsed high pressure water jet mill |
| CN105819437A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for large-scale clean graphene preparation |
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