CN106927456A - A kind of use mechanical stripping method prepares the process units and method of Graphene - Google Patents
A kind of use mechanical stripping method prepares the process units and method of Graphene Download PDFInfo
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Abstract
The present invention relates to process units and method that a kind of use mechanical stripping method prepares Graphene, it is characterised in that the described method comprises the following steps：Step one, by purity more than 98%, during particle diameter puts into High-Pressure Water breaker for the graphite raw material of 2 μm ~ 1cm, start high-pressure pump, pressure is adjusted, by the graphite flakes mixed liquor filtering drying in collecting tank；After step 2, filtering drying, graphite flakes, dispersant and solvent are added in graphite expansion heater, dispersed suspension is obtained by ultrasonic vibration；Step 3, will be heated after suspension enter in high-shear device and sheared；Step 4, graphene suspension is delivered to filter cake is obtained in centrifuge；, with appropriate distillation water washing 3 times, filter cake is transferred in freeze drier, freeze-drying 3h, that is, obtain graphene product for step 5, the filter cake for obtaining step 4.
Description
Technical field
The present invention relates to the process units and preparation method of a kind of two-dimensional nano new material, and in particular to one kind is using machinery
Stripping method prepares the process units and preparation method of Graphene.
Background technology
Graphene is substantially mono-layer graphite, it is also contemplated that Graphene is the CNT after launching.Graphene film
(graphene sheets) provide many outstanding performances, people studying its nanoelectronics, nano-complex,
Purposes in battery, ultracapacitor, hydrogen storage and biologic applications.The use of the major limitation of graphene film is at present cannot
It is largely produced.Similar to CNT and many other nano materials, synthesizing and processing a large amount of graphene films
During, crucial challenge is aggtegation.Unless it is completely separate from one another, otherwise due to there is Van der Waals interaction, have
The graphene film for having high-specific surface area is intended to form irreversible caking (agglomerates), or even piles up formation again
Graphite.In the work for by chemical conversion or thermal expansion/also original large-scale production Graphene all before this,
Run into this problem.Prevent aggtegation especially important for graphene film because their most special performances only with
Single piece is relevant.It is attached on the graphene film by by other molecules or polymer, aggtegation can be reduced.So
And, for majority application, it is undesirable to there is external stabilizer.New strategy is needed largely to produce relatively pure graphite
Alkene piece, and make its holding individually separated.
The graphite being made up of flat graphene film stacking is relatively inexpensive, and it can greatly be measured by natural origin and synthesis source
Arrive.For generating graphene film, this common carbon material is to be easiest to utilize and source the most cheap.The machine of graphite
Originally tool cutting causes the discovery of graphene film, and currently used for the experimental research of most Graphenes.However, this side
The current production capacity of method is low to cause it to be not suitable for large-scale use, is only applied in an experiment.
A large amount of productions of high-quality graphene are to realize the wide variety of premise of Graphene, also always Graphene research
One focus.Conventional graphene preparation method has four kinds at present：Supercritical methanol technology, epitaxial growth method, chemical vapour deposition technique and
Graphite oxide reducing process.Supercritical methanol technology yield is too low, is only applicable to laboratory small-scale test；Epitaxial growth method sets for production
Standby, condition is required to higher, is not suitable for production requirement at this stage；Chemical vapour deposition technique is difficult to obtain uniform individual layer stone
Black alkene, and complex process；The reduced graphene that graphite oxide reducing process is obtained often has too many defect, for Graphene
Electrical properties are fatal influences.
The content of the invention
It is an object of the invention to overcome above-mentioned deficiency, there is provided a kind of use mechanical stripping method prepares the production dress of Graphene
Put and method, can obtain large area, do not have defective Graphene on the basis of graphite flake layer natural structure is not destroyed, make
The regulation that the graphene product for obtaining passes through technological parameter, it is ensured that its preferable mode of appearance, whole production process uses physics
Method, environmental protection, process is simple.
The object of the present invention is achieved like this：A kind of use mechanical stripping method prepares the process units of Graphene, including
Charging tank, giant, high-pressure pump and collecting tank, the bottom of the charging tank are connected with collecting tank, logical in the collecting tank
Cross support to fix, the giant is arranged in the connectivity part of charging tank and collecting tank, muzzle is located inside charging tank, angle
It is 15 °, hydraulic pressure is 200kpa, the giant is connected with high-pressure pump, is fed intake in the muzzle opposite face of the giant
Top tank structure is provided with clipper on face, and the bottom of the charging tank is provided with recoil water pipe, and the recoil water pipe is by recoil
Water pump is connected with water tank, and the bottom of the charging tank is provided with agitator；
The graphite expansion heater includes heating furnace, and charging aperture and thermometer, lower section are provided with above the heating furnace
Discharging opening is provided with, the lower outer of the heating furnace is provided with chuck, Heating medium is provided with the chuck with heat
Matchmaker exports, and heating agent uses deep fat or steam, in the agitating paddle that is internally provided with of the heating furnace, the agitating paddle and heating furnace roof
The stirring motor in portion is connected, and multiple Vltrasonic devices is evenly distributed with the internal side wall of the heating furnace, by Vltrasonic device
Act on graphite mixed liquor and obtain dispersed suspension；
The high-shear device includes reactor and motor, and the motor is installed on the bottom of reactor, in the defeated of the motor
Go out on end and be connected with clipper, charging aperture, pressure gauge and thermometer are provided with the top of the reactor, in the reactor
Internal face on be provided with shearing groove, helically formula rises arrangement to shearing groove, is provided with the middle and lower part of the reactor
Discharging opening, chuck is provided with the periphery of the reactor, and Heating medium and outlet, the reactor are provided with the chuck
Discharging opening be connected with the charging aperture of storage tank, the discharging opening of the storage tank is connected with the charging aperture of centrifuge, the centrifugation
The discharging opening of machine is connected with the charging aperture of freeze drier, and agitation blade is nested with the periphery of the clipper, described
Agitation blade includes fixed seat and reach blade, and the fixed seat is nested and is fixed on the periphery of clipper, described to stretch
The one end for going out formula blade is connected with fixed seat, and the direction of rotation of incline direction and clipper is conversely, the reach blade
The other end is connected with tip blades, and the tip blades are vertical setting with reach blade.
Preferably, the shearing groove is combined by tetrahedron or tooth form or both and constituted.
Preferably, the tetrahedron of the shearing groove or the corner angle of tooth form are 10 ° ~ 160 °, and length is 1cm-
1000cm, thickness is 0.5cm ~ 3cm.
The method for preparing Graphene using above-mentioned process units is as follows：
Step one, by purity more than 98%, particle diameter is put into High-Pressure Water breaker for 1 μm ~ 2cm graphite flakes raw materials,
Start high-pressure pump, adjust pressure 1.5atm, the High-Pressure Water sprayed by giant clashes into graphite flakes, then by graphite squama
Piece mixed liquor is expelled in collecting tank, by the graphite flakes mixed liquor filtering drying in collecting tank；
After step 2, filtering drying, graphite flakes, dispersant and solvent are added in graphite expansion heater, by super
Acoustic vibration obtains dispersed suspension, and it is 80 ~ 150 DEG C that suspension is heated into temperature, supersonic frequency 20KHz ~ 40KHz,
Summation watt rating is 5w/L ~ 100w/L, and the mass concentration of 2 ~ 5h of duration, wherein graphite flakes is 1% ~ 25%；
Step 3, will be heated after suspension enter in high-shear device, add hydrochloric acid, increase clipper rotating speed is 2000-
7500 rpm/min, it is 80 DEG C ~ 150 DEG C to keep reactor temperature, after stirring 2h-10h, adds sodium acid carbonate, is stopped after 1 ~ 10h
Only react, upper strata suspension is expelled in storage tank by discharging opening, stand 2 ~ 24h；
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 1000-6000 rpm/
Min, 10min ~ 2h, take supernatant liquor, and vacuum filter obtains filter cake；
Step 5, the filter cake for obtaining step 4 are with appropriate distillation water washing 3 times, and filter cake is transferred in freeze drier, cold
Dry 3h is freezed, that is, obtains graphene product；
The solvent includes water, acetonitrile, n-butanol, ethanol, acetone, N, N-dimethylformamide, in 1-METHYLPYRROLIDONE
One or more mixture, dispersant includes cetyl trimethylammonium bromide, lauryl sodium sulfate, DBSA
Sodium, sodium taurocholate, polyvinyl alcohol, one or more in polyvinylpyrrolidone of compounding.
Compared with prior art, the invention has the advantages that：
1st, during the present invention holds on to Graphene stripping preparation process, most important shear action leads to excessive speeds, shears groove
The mode such as setting, give full play to shearing between material and material at high speed with " collision " of groove, realize stone
The successful stripping of black alkene, further, since producing Graphene using the method that physics is peeled off, prime cost is graphite, labour cost, water
The electricity charge and administration fee, graphite raw material are cheap, and by further optimum management, production cost has high advantage.
2nd, the present invention is good using Graphene quality obtained in mechanical stripping method, and graphite passes through the mutual shear action of itself,
The micro powder granule on surface can be removed.By follow-up centrifugation, dry obtained Graphene distribution is homogeneous, and edge is rounded.
3rd, the present invention does not use noxious material, and production process is simply controllable, and environmental pollution is small.New Two Dimensional material Graphene
Successful preparation can produce huge economic and social benefit, to environment do not exist any destruction.
4th, the Graphene of present invention production provides important raw material for composite, photoelectric field field, due to
Surface smooths, and yardstick is homogeneous, neat in edge, applies " the Si great Te of performance Graphene that can be maximum in fields such as Material claddings
Property ".The lamellar structure of Graphene is preferably saved, during use, interfacial interaction is strong, can play the material of maximum
Mechanical property.
Brief description of the drawings
Fig. 1 is the structural representation of mesohigh current breaker of the present invention.
Fig. 2 is the structural representation of graphite expansion heater in the present invention.
Fig. 3 is the structural representation of high-shear device in the present invention.
Fig. 4 is the structural representation of clipper in high-shear device of the present invention.
Wherein：
Charging tank 1
Giant 2
High-pressure pump 3
Collecting tank 4
Support 5
Clipper 6
Recoil water pipe 7
Recoil water pump 8
Water tank 9
Agitator 10
Heating furnace 101
Charging aperture 102
Thermometer 103
Discharging opening 104
Chuck 105
Hot coal import 106
Heating agent outlet 107
Agitating paddle 108
Stirring motor 109
Vltrasonic device 110
Reactor 201
Motor 202
Clipper 203
Agitation blade 2031
Fixed seat 2032
Reach blade 2033
Tip blades 2034
Charging aperture 204
Pressure gauge 205
Thermometer 206
Shearing groove 207
Discharging opening 208
Storage tank 209
Centrifuge 2010
Freeze drier 2011.
Specific embodiment
Referring to Fig. 1-Fig. 4, the present invention relates to process units and method that a kind of use mechanical stripping method prepares Graphene：
Embodiment one,
Step one, referring to Fig. 1, by purity more than 98%, particle diameter is that 100 μm of graphite flakes raw material is put into High-Pressure Water and broken
In crushing device, start high-pressure pump, adjust pressure 200kpa, the High-Pressure Water sprayed by giant clashes into graphite flakes, breaks
The Van der Waals force of bad its interlayer, makes graphite flakes peeling-off, and then graphite flakes mixed liquor is expelled in collecting tank, will receive
Graphite flakes mixed liquor filtering drying in collection tank；
Step 2, referring to Fig. 2, through filtering drying after, 50kg graphite flakes and 1kg sodium taurocholate dispersants are added to graphite expansion
In heater, 350kg distilled water is being added, with the ultrasound that frequency is 40KHz, density power 30w/L vibration 2h obtain uniform
Scattered suspension, then toward deep fat or steam is passed through in chuck, makes to be heated to temperature for 80 DEG C, and the duration is 5h, plus
Stirring motor is opened in thermal process, by agitating paddle so that suspension is uniformly heated, because temperature raises graphite flakes layer
Van der Waals force between layer reduces, and is easy to shearing below；
Step 3, referring to Fig. 3, will be heated after suspension enter in high-shear device, hydrochloric acid 3.5kg is added, after stirring 2h
Add saleratus, sodium carbonate and hydrochloric acid enter into the interlayer reaction of graphite flakes, the carbon dioxide of generation is by graphite squama
The layer of piece is opened with layer top, and increase clipper rotating speed is 5000 rpm/min, due to rotating speed higher, the shearing between material itself
And the interaction of groove is sheared with inwall so that graphite is successively peeled off, and keeps steady temperature, rotating speed, is stopped after 5h anti-
Should, upper strata suspension is expelled in storage tank by discharging opening, stand 24h；
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 1000-6000 rpm/
Min, centrifugal action 10min, by centrifugation, multi-layer graphene is deposited in bottom to the graphite being not peeled off, and takes supernatant liquor,
Vacuum filter；
, with appropriate absolute ethanol washing 3 times, filter cake is transferred in freeze drier for step 5, the filter cake for obtaining step 4,
Freeze-drying 3h, that is, obtain graphene product.
Embodiment two,
Step one, by purity more than 98%, particle diameter is during 150 μm of graphite flakes raw material puts into High-Pressure Water breaker,
Start high-pressure pump, adjust pressure 200kpa, the High-Pressure Water sprayed by giant clashes into graphite flakes, destroys its interlayer
Van der Waals force, makes graphite flakes peeling-off, and then graphite flakes mixed liquor is expelled in collecting tank, by the stone in collecting tank
Black scale mixed liquor filtering drying；
Step 2, through filtering drying after, by 20kg graphite flakes and 1kg polyvinyl alcohol dispersants be added to graphite expansion heating dress
In putting, 400kg distilled water is added, with the ultrasound that frequency is 20KHz, density power 5w/L vibration 2h obtain dispersed
Suspension, then toward deep fat or steam is passed through in chuck, makes to be heated to temperature for 100 DEG C, and the duration is 2h, heating process
Middle opening stirring motor, by agitating paddle so that suspension is uniformly heated, due to temperature raise graphite flakes layer with layer it
Between Van der Waals force reduce, be easy to shearing below；
Step 3, will be heated after suspension, after filtration washing, enter in high-shear device, add hydrochloric acid 3.5kg, stirring
2 saleratus, sodium carbonate and hydrochloric acid are added to enter into the interlayer reaction of graphite flakes after 2h, sodium carbonate and hydrochloric acid enter into graphite
The interlayer reaction of scale, the carbon dioxide of generation opens the layer of graphite flakes with layer top, and increase clipper rotating speed is 3500
Rpm/min, due to rotating speed higher, shearing between material itself and shears the interaction of groove with inwall so that stone
Ink is successively peeled off.Steady temperature, rotating speed are kept, reaction is stopped after 8h, upper strata suspension is expelled to by storing by discharging opening
In tank, 15 h are stood；
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 2000-5000 rpm/
Min, centrifugal action 1h, by centrifugation, multi-layer graphene is deposited in bottom to the graphite being not peeled off, and takes supernatant liquor, very
Sky filtering；
, with appropriate absolute ethanol washing 3 times, filter cake is transferred in freeze drier for step 5, the filter cake for obtaining step 4,
Freeze-drying 3h, that is, obtain graphene product.
Embodiment three,
Step one, by purity more than 98%, particle diameter is during 250 μm of graphite flakes raw material puts into High-Pressure Water breaker,
Start high-pressure pump, adjust pressure 1.5atm, the High-Pressure Water sprayed by giant clashes into graphite flakes, destroys its interlayer
Van der Waals force, makes graphite flakes peeling-off, and then graphite flakes mixed liquor is expelled in collecting tank, by the stone in collecting tank
Black scale mixed liquor filtering drying；
Step 2, through filter drying after, 30kg graphite flakes and 1kg lauryl sodium sulfate dispersants are added to graphite expansion and added
In thermal, add in 500kg 1-METHYLPYRROLIDONEs, be 28KHz with frequency, summation watt rating is the ultrasonic vibration of 25w/L
3h, obtains dispersed suspension, then toward deep fat or steam is passed through in chuck, makes to be heated to temperature for 120 DEG C, continues
Time is 3h, and stirring motor is opened in heating process, by agitating paddle so that suspension is uniformly heated, because temperature is raised
Graphite flakes Van der Waals force between layers reduces, and is easy to shearing below；
Step 3, will be heated after suspension enter in high-shear device, put into bicarbonate after adding hydrochloric acid 3.5kg immersion 6h
Potassium 2kg, stirs 5h, and sodium acid carbonate and hydrochloric acid enter into the interlayer reaction of graphite flakes, and the carbon dioxide of generation is by graphite
The layer of scale is opened with layer top, and increase clipper rotating speed is 7500 rpm/min, due to rotating speed higher, cutting between material itself
Cut and sheared with inwall the interaction of groove so that graphite is successively peeled off.Steady temperature, rotating speed are kept, is stopped after 7h
, be expelled to upper strata suspension in storage tank by discharging opening by reaction, stands 12 h；
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 1000-6000 rpm/
Min, centrifugal action 2h, by centrifugation, multi-layer graphene is deposited in bottom to the graphite being not peeled off, and takes supernatant liquor, very
Sky filtering, the filter cake for obtaining；
, with appropriate absolute ethanol washing 3 times, filter cake is transferred in freeze drier for step 5, the filter cake for obtaining step 4,
Freeze-drying 3h, that is, obtain graphene product.
Claims (6)
1. a kind of use mechanical stripping method prepares the process units of Graphene, it is characterised in that it includes charging tank（1）, water under high pressure
Rifle（2）, high-pressure pump（3）And collecting tank（4）, the charging tank（1）Bottom and collecting tank（4）It is connected, in the collecting tank
（4）By support（5）It is fixed, the giant（2）Installed in charging tank（1）With collecting tank（4）Connectivity part in, muzzle position
In charging tank（1）Inside, the giant（2）With high-pressure pump（3）It is connected, in the giant（2）Muzzle opposite face
Charging tank（1）Clipper is provided with internal face（6）, in the charging tank（1）Bottom be provided with recoil water pipe（7）, institute
State recoil water pipe（7）By the water pump that recoils（8）With water tank（9）It is connected, in the charging tank（1）Bottom be provided with agitator
（10）；
The graphite expansion heater includes heating furnace（101）, in the heating furnace（101）Top is provided with charging aperture
（102）And thermometer（103）, lower section is provided with discharging opening（104）, in the heating furnace（101）Lower outer be provided with folder
Set（105）, in the chuck（105）On be provided with Heating medium（106）Exported with heating agent（107）, in the heating furnace（101）
Be internally provided with agitating paddle（108）, the agitating paddle（108）With heating furnace（101）The stirring motor at top（109）It is connected,
In the heating furnace（101）Internal side wall on be evenly distributed with multiple Vltrasonic devices（110）；
The high-shear device includes reactor（201）And motor（202）, the motor（202）It is installed on reactor（201）'s
Bottom, in the motor（202）Output end on be connected with clipper（203）, in the reactor（201）Top be provided with
Charging aperture（204）, pressure gauge（205）And thermometer（206）, in the reactor（201）Internal face on be provided with shearing ditch
Groove（207）, the shearing groove（207）Helically formula rises arrangement, in the reactor（201）Middle and lower part be provided with discharging
Mouthful（208）, the reactor（201）Discharging opening and storage tank（209）Charging aperture be connected, the storage tank（209）Go out
Material mouth and centrifuge（210）Charging aperture be connected, the centrifuge（210）Discharging opening and freeze drier（211）Charging
Mouth is connected.
2. a kind of use mechanical stripping method according to claim 1 prepares the process units of Graphene, it is characterised in that
The clipper（203）Periphery be nested with agitation blade（2031）, the agitation blade（2031）Including fixation
Seat（2032）With reach blade（2033）, the fixed seat（2032）Nesting is simultaneously fixed on clipper（203）Periphery, it is described
Reach blade（2033）One end and fixed seat（2032）It is connected, incline direction and clipper（203）Direction of rotation phase
Instead, the reach blade（2033）The other end be connected with tip blades（2034）, the tip blades（2034）With stretch out
Formula blade（2033）It is vertical setting.
3. a kind of use mechanical stripping method according to claim 1 prepares the process units of Graphene, it is characterised in that institute
State shearing groove（207）Combined by tetrahedron or tooth form or both and constituted.
4. a kind of use mechanical stripping method according to claim 1 prepares the process units of Graphene, it is characterised in that institute
State shearing groove（207）Tetrahedron or tooth form corner angle be 10 ° ~ 160 °, length is 1cm-1000cm, and thickness is
0.5cm~3cm。
5. a kind of use mechanical stripping method as claimed in claim 1 prepares the application method of the process units of Graphene, and it is special
Levy and be：The described method comprises the following steps：
Step one, by purity more than 98%, during particle diameter puts into High-Pressure Water breaker for the graphite raw material of 2 μm ~ 1cm, open
Dynamic high-pressure pump, the High-Pressure Water sprayed by giant clashes into graphite flakes, and graphite flakes mixed liquor then is expelled into receipts
In collection tank, by the graphite flakes mixed liquor filtering drying in collecting tank；
After step 2, filtering drying, graphite flakes, dispersant and solvent are added in graphite expansion heater, by super
Acoustic vibration obtains dispersed suspension, and it is 80 ~ 150 DEG C, wherein 2 ~ 5h of duration, graphite that suspension is heated into temperature
The mass concentration of scale is 1% ~ 25%；
Step 3, will be heated after suspension enter in high-shear device, while add saleratus and hydrochloric acid, increase shearing
Device rotating speed is 7500 rpm/min, and it is 80 DEG C ~ 150 DEG C to keep reactor temperature, reaction is stopped after 5 ~ 10h, by discharging opening
Upper strata suspension is expelled in storage tank, 12 ~ 24h is stood；
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 1000-6000 rpm/
Min, 10min ~ 2h, take supernatant liquor, and vacuum filter obtains filter cake；
Step 5, the filter cake for obtaining step 4 are with appropriate distillation water washing 3 times, and filter cake is transferred in freeze drier, cold
Dry 3h is freezed, that is, obtains graphene product.
6. a kind of use mechanical stripping method according to claim 5 prepares the preparation method of the process units of Graphene, its
Be characterised by solvent include water, petroleum ether, DMF, 1-METHYLPYRROLIDONE, acetone, ether, ethyl acetate,
One or more mixture of toluene, dispersant includes cetyl trimethylammonium bromide, lauryl sodium sulfate, dodecyl
Benzene sulfonic acid sodium salt, sodium taurocholate, polyvinyl alcohol, one or more in polyvinylpyrrolidone of compounding.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587572A (en) * | 2018-05-14 | 2018-09-28 | 长沙理工大学 | It is a kind of using ultra-thin graphite slice as the composite phase-change heat-storage material of amorphous matrix and preparation method |
| CN109835889A (en) * | 2019-04-16 | 2019-06-04 | 江苏碳谷二维世界科技有限公司 | A kind of the mechanical stripping device and graphene preparation method of graphene |
| CN115608273A (en) * | 2022-09-19 | 2023-01-17 | 昆明云天墨睿科技有限公司 | Graphene oxide production device and production method |
| CN115818630A (en) * | 2022-11-21 | 2023-03-21 | 中国铝业股份有限公司 | Graphene stripping device and graphene production system |
-
2017
- 2017-04-05 CN CN201710216895.6A patent/CN106927456A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587572A (en) * | 2018-05-14 | 2018-09-28 | 长沙理工大学 | It is a kind of using ultra-thin graphite slice as the composite phase-change heat-storage material of amorphous matrix and preparation method |
| CN109835889A (en) * | 2019-04-16 | 2019-06-04 | 江苏碳谷二维世界科技有限公司 | A kind of the mechanical stripping device and graphene preparation method of graphene |
| CN115608273A (en) * | 2022-09-19 | 2023-01-17 | 昆明云天墨睿科技有限公司 | Graphene oxide production device and production method |
| CN115608273B (en) * | 2022-09-19 | 2023-07-28 | 昆明云天墨睿科技有限公司 | Graphene oxide production device and production method |
| CN115818630A (en) * | 2022-11-21 | 2023-03-21 | 中国铝业股份有限公司 | Graphene stripping device and graphene production system |
| CN115818630B (en) * | 2022-11-21 | 2023-08-15 | 中国铝业股份有限公司 | Graphene stripping device and graphene production system |
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