CN104609413B - A kind of tonne of class mechanical stripping device producing Graphene and production method thereof - Google Patents
A kind of tonne of class mechanical stripping device producing Graphene and production method thereof Download PDFInfo
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Abstract
The invention discloses a kind of tonne of class mechanical stripping device producing Graphene and production method thereof, it is characterised in that: device is in series by one or more levels peel-off device;Peel-off device includes material bin, rotor, sub-material storehouse etc., matches with the lower section of material bin in the lower section of its rotor, and when making rotor rotate, the outer surface of rotor and the inner surface of material bin form Relative friction at mated position;During use, graphite raw material is in the position coordinated by the shear action of frictional force, and in graphite, the Van der Waals force of each graphite layers is disintegrated, so that graphite is stripped thinning acquisition Graphene, enters sub-material storehouse.The class mechanical stripping device that the present invention tonne produces Graphene is simple to operate, and gained Graphene crystal structure is perfect, specific surface area big, conduct electricity very well, and can realize the mass production of Graphene.
Description
Technical field
The present invention relates to mass production facilities and the production method of Graphene.
Background technology
Graphene (Graphene), also known as mono-layer graphite, be a kind of by carbon atom with sp2Hybrid orbital composition hexangle type is Nidus Vespae
The flat film of lattice, is the two-dimension nano materials of only one of which carbon atom thickness.Being found that while only about 10 years of Graphene,
But the research and development tide of the another ripple of ripple have swept the globe has been caused.Graphene be a kind of by carbon atom tightly packed two
Dimension crystal, has the features such as magical electric transmission, conduction, heat conduction and machinery.The physics of Univ Manchester UK in 2004
Scholar An Deliehaimu and Constantine's Nuo Woxiao love, successfully separated Graphene at laboratory from graphite, it was demonstrated that
Therefore Graphene can win Nobel Prize in physics in 2010 with individualism, thus started Graphene prepare, modified and should
Global research boom.Graphene is used for ultracapacitor, transparency electrode, lithium ion battery, sensor, functional paint
With the application prospect of the aspects such as polymer nanocomposites, open the New Times of grapheme material.
As there being scholar to be sayed, 19th century were the epoch of ironware, and 20th century were the epoch of silicon, and 21 century is the epoch of carbon.Carbon
It is one of most common element of distributed in nature, is to constitute the most important element of all life body on the earth.The characteristic of material with carbon element is several
Contain the character of all substances on the earth.Advanced material with carbon element has new structure and excellent physical and chemical performance, is to future
Development has new material that is great and that determine meaning.
New material industry, as one of the emphasis of emerging strategic industries, is also foundation stone and the guide of following Hi-tech Industry Development,
It it is China's important foundation of becoming world manufacturing industry power.Graphene as advanced material with carbon element, it be current find
The material of high-quality.It has following characteristics: the thinnest, 0.35nm, is referred to as the material that the world now is the thinnest;Specific surface area is maximum,
2620m2/g;The hardest, rigidity is better than diamond, is the material that mankind's known strength is the highest, hard 100 times than iron and steel;Tension,
Can elastic stretching 20%;Thermal conductivity is the highest, 5300W/m.k;High mobility 200,000cm2/v.s(300k);High light transmittance,
Light transmittance is 97.7%/monolayer;High current carrying capacity: high 6 orders of magnitude of current density ratio copper;The most peculiar, Graphene is two
Dimension quantum material, linear band dispersion, carrier effective mass is zero, can observe quantum hall effect under greenhouse;
Also there is room temperature ballistic transport characteristic.
Graphene has the most wide application prospect, although the present or potential stage, commonly used does not the most beat with industrialization
Beginning face, but from the perspective of scientific forecasting, have become as very important major fields.Such as, its alternative reconciliation
The drawbacks such as the most traditional lithium cell charging speed is slow, power reservoir capacity is poor, the life-span is short, pollution, it is possible to resolve the key of Development of Electric Vehicles
A difficult problem, makes New-energy electric vehicle flourish.Future new era supercomputer can be manufactured for another example with substituted for silicon;Substitute
Transparent conductive film, is applied to the electronics industry such as touch screen, Flexible Displays, solaode;Apply also for sea
Water desalination, degradation plastic, heat dissipation film, corrosion-inhibiting coating, biomaterial, composite, panel computer, wrist-watch calendar, shifting
Mobile phone, photodetector, graphene paper, Graphene cloth and space flight military project, ultralight flak jackets, ultra-thin and ultra-light aircraft, super
Thin folding cell phone, the sky elevator etc. even having imagination.The demand that Graphene is created, it is most likely that start one and have swept the globe
Subversiveness new technique new industrial revolution.From the point of view of global development trend, it is great that no one is ready that forfeiture Graphene development brings
Opportunity.
The mode preparing the current comparative maturity of Graphene has Physical and chemical method, and wherein the Typical Representative of Physical is to glue with adhesive tape
The mode of patch obtains from graphite crystal, and this method can take the very perfect Graphene crystal of structure, is relatively specific for exploitation
Electronic device or physical study, it is impossible to volume production.Volume production relies primarily on chemical method, a kind of for generating filmy graphite alkene " certainly
Lower and on " method, be namely assembled into by approach such as chemical gaseous phase deposition, epitaxial growth or organic synthesiss from little molecule or carbon atom
Graphene film.This method scale is relatively easily done greatly, and the crystal structure of obtained Graphene is relatively complete, is more suitable for doing touch
Screen or the transparent conductive film of solaode, and it is difficult to apply to the preparation of powder body Graphene.Another way be exactly " from upper and
Under " method, the most also it is chemical stripping method, it is simply that utilize intercalator that the Van der Waals force of the three-dimensional each interlayer of graphite crystal is disintegrated, make
Graphite is disassembled out layer by layer, shell into which floor graphene product of monolayer or minority.The process route of current each producer and intercalation used
Agent is differentiated.Some salt intercalation then liquid phases are peeled off, and Graphene oxygen content prepared by this method is low, conducts electricity very well,
But extent of exfoliation is more relatively low, specific surface area is the biggest;Then some initial oxidation intercalations are peeled off, and this method extent of exfoliation is high,
Specific surface area is big, but the Graphene defect made is the most, and oxygen content is big, constrains the process of industrialization of Graphene.
Summary of the invention
The present invention is for avoiding the weak point existing for above-mentioned prior art, it is provided that a kind of tonne of class machinery stripping producing Graphene
From device and production method thereof, to pollution-free, zero-emission, the mass production high-specific surface area of low energy consumption, nothing can be realized
Defect Graphene.
The present invention solves that technical problem adopts the following technical scheme that
The present invention tonne produces the class mechanical stripping device of Graphene, and its feature is: described device is set by one or more levels stripping
Standby in series;
The structure of described peel-off device is: the upper end of a material bin is provided with two charging apertures, and lower end is provided with discharging opening, described
Below discharging opening, connection and sub-material storehouse, be provided with filter screen in described sub-material storehouse, and described sub-material storehouse is divided into coarse fodder by described filter screen
Storehouse and fines storehouse, after in material bin, material is entered sub-material storehouse by discharging opening, through strainer filtering, can enter thin by the material of filter screen
Feed bin, does not enters coarse fodder storehouse by the material of filter screen;A rotor it is provided with in described material bin;The lower section of described rotor and institute
Matching in the lower section stating material bin, when making described rotor rotate, the outer surface of rotor and the inner surface of material bin are in mated position
Place forms Relative friction;
The coarse fodder storehouse of peel-off devices at different levels is provided by another charging aperture of pipeline communication and the first order peel-off device taking out pump;On
The fines storehouse of one-level peel-off device is provided by the charging aperture of pipeline communication and the next stage peel-off device taking out pump, and afterbody is shelled
The pipeline communication taking out pump and finished product receptacle it is provided by from the fines storehouse of equipment;
The outer surface of described rotor and the inner surface of material bin are made up of identical material high hardness material at mated position, described
High hardness material is the material that hardness is more than graphite.
Preferably, described hardness is marble, granite, diamond, essence steel, carbon steel, Gao Meng more than the material of graphite
Steel, tungsten carbide or rustless steel.
The outer surface of described rotor and the inner surface of material bin are plane or the Alveolus type being provided with multiple teeth groove at mated position
Flour milling.
In described fines storehouse, the lower section that is positioned at described filter screen be provided with filter screen brush;
The pipeline that the fines storehouse of afterbody peel-off device connects with finished product receptacle is provided with drying equipment.
Utilizing the production method of tonne production Graphene of above-mentioned class mechanical stripping device, its feature is:
Start the rotor of peel-off device at different levels and take out pump;
Rotate rotor, make the outer surface of rotor and the inner surface of material bin form frictional force at mated position;
It is mixed and stirred for graphite and liquid adjuvants uniformly, then joining the material bin of first order peel-off device from charging aperture,
Graphite in the position that rotor matches with material bin by the shear action of frictional force, the Van der Waals force of each graphite layers in graphite
Disintegrate, so that graphite is stripped thinning acquisition Graphene, enter sub-material storehouse from feed opening, sieve through filter screen, pass through filter screen
Material (include meeting filter screen mesh number unstripped graphite raw material and peel off the Graphene obtained) enter next stage peel-off device,
Again peel off thinning, peel off obtained finished product Graphene layer by layer through multistage peel-off device and enter finished product receptacle;Strippings at different levels
Equipment is not returned the material bin continuation stripping of first order peel-off device by the material of filter screen.
Wherein said liquid adjuvants is deionized water, ethanol, N-Methyl pyrrolidone, N,N-dimethylformamide, Benzyl Benzoate
One or more mixing in ester.
The quality of described graphite is 0.01~150:100g/ml with the volume ratio of described liquid adjuvants.
The present invention utilizes the Relative friction of class mechanical stripping device rotor and material bin, makes graphite raw material be peeled off layer by layer, thus
Obtaining Graphene, the outer surface of rotor and the inner surface of material bin are made up of more than the material of graphite hardness at mated position,
To reduce the abrasion of device.
Compared with the prior art, the present invention has the beneficial effect that:
1, the class mechanical stripping device of the present invention tonne production Graphene is simple to operate, and gained Graphene crystal structure is perfect, compare table
Area is big, conduct electricity very well, and can realize the mass production of Graphene.
2, the Graphene extent of exfoliation that prepared by the present invention is the most adjustable, can adjust gained graphite according to splitting time with peeling off number of times
The number of plies of alkene;
3, Graphene prepared by the present invention is almost without defect, and oxygen content is extremely low;
4, the present invention prepares any exogenous impurity particle that do not induces one in the middle of the method for Graphene, maintains Graphene to the full extent
Purity, has substantially accomplished zero destruction to Graphene, it is achieved that zero damage, no pollution, zero-emission, low energy consumption, high yield, is
The inevitable choice of Graphene volume production from now on;
5, the method for the Graphene of present invention synthesis is simple, reliable and stable, produces line and replicates simple, it is possible to fast responding market
Demand.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention tonne produces the class mechanical stripping device of Graphene;
Fig. 2 is the signal that the present invention tonne produces in the class mechanical stripping device of Graphene at material bin and rotor mated position
Figure;
Fig. 3 is that the graphene dispersion of the embodiment of the present invention 1 preparation is to the microscope figure on silicon oxide;
Fig. 4 is the TEM figure of the Graphene of the embodiment of the present invention 1 preparation;
Fig. 5 is the purity table of the Graphene of the embodiment of the present invention 1 preparation;
Fig. 6 is the photo of the embodiment of the present invention 2 marble mill;
Fig. 7 is that the graphene dispersion of the embodiment of the present invention 2 preparation is to the microscope figure on silicon oxide;
Fig. 8 is the TEM figure of the Graphene of the embodiment of the present invention 2 preparation;
Fig. 9 is the purity table of the Graphene of the embodiment of the present invention 3 preparation;
Label in figure: 1a charging aperture;1b discharging opening;2 material bins;3 rotors;4a coarse fodder storehouse;4b fines storehouse;5 filters
Net;6 filter screen brushes;7 take out pump;8 finished product receptacles.
Detailed description of the invention
Embodiment 1
As it is shown in figure 1, the class mechanical stripping device that the present embodiment tonne produces Graphene is in series by three grades of peel-off devices;
The structure of peel-off device is: the upper end of a material bin 2 is provided with two charging aperture 1a, and lower end is provided with discharging opening 1b, goes out
Material mouth 1b below connection with sub-material storehouse, in sub-material storehouse, be provided with filter screen 5, filter screen 5 sub-material storehouse is divided into coarse fodder storehouse 4a and
Fines storehouse 4b, after in material bin 2, material is entered sub-material storehouse by discharging opening 1b, filters through filter screen 5, can be by the thing of filter screen 5
Material enters fines storehouse 4b, does not enters coarse fodder storehouse 4a by the material of filter screen 5;A rotor 3 it is provided with in material bin 2;Rotor
Match with the lower section of material bin 2 in the lower section of 3, when making rotor 3 rotate, and the outer surface of rotor 3 and the inner surface of material bin 2
Relative friction is formed at mated position;
The coarse fodder storehouse 4a of peel-off devices at different levels is provided by another charging aperture of pipeline communication and the first order peel-off device taking out pump 7
1a;The fines storehouse of upper level peel-off device is provided by the charging aperture 1a of pipeline communication and the next stage peel-off device taking out pump 7,
The fines storehouse of afterbody peel-off device is provided by the pipeline communication taking out pump 7 and finished product receptacle 8;
The outer surface of rotor 3 and the inner surface of material bin 2 are made up of identical material high hardness material at mated position, high hard
Degree material is the material that hardness is more than graphite.The present embodiment selects marble material.In being embodied as, rotor matches with material bin
The size of the position closed arbitrarily can adjust according to the needs of yield.
As in figure 2 it is shown, the inner surface of the outer surface of described rotor (3) and material bin (2) at mated position be plane or
It is provided with the Alveolus type flour milling of multiple teeth groove.The version being set to Alveolus type flour milling is a kind of structure being similar to mill, phase
Than the frictional force that can add greater trochanter and material bin in plane, it is easier to the multi-layer graphene of composition graphite is disassembled out layer by layer, with
Obtain more Graphene.
In being embodied as, in described fines storehouse 4b, the lower section that is positioned at filter screen 5 be provided with filter screen brush 6, in order to cleaning filter screen
5。
In use, various sizes of powdery graphite alkene sheet can be obtained by selecting the graphite raw material of different meshes, it is possible to
With by selecting the filter screen of different meshes to obtain the Graphene of required mesh number.
Additionally, can be peeled off by graphite raw material by the stripping of every one-level peel-off device is single or multiple lift Graphene, then pass through
The filtration of filter screen, the Graphene meeting mesh number demand is mingled with unstripped graphite raw material entrance next stage peel-off device, multilamellar stone
Ink alkene may be stripped as single-layer graphene in next stage peel-off device, and graphite raw material continues to be stripped into Graphene, through too much
The stripping layer by layer of level peel-off device can peel off into single-layer graphene by as much as possible for graphite raw material.
In being embodied as, because raw material is the mixing of graphite and liquid adjuvants, therefore obtain in finished product receptacle is Graphene
Dispersion liquid, can arrange dry as required on the pipeline that the fines storehouse of afterbody peel-off device connects with finished product receptacle
Equipment, is dried the graphene dispersing solution obtained after peel-off devices at different levels are peeled off by drying equipment, removes liquid adjuvants,
Dry graphene powder is collected in finished product receptacle.
It is as follows that the class mechanical stripping device utilizing the present embodiment produces tonne method producing Graphene:
Start the rotor of peel-off device at different levels and take out pump;
Rotate rotor, make the outer surface of rotor and the inner surface of material bin form frictional force at mated position;
1000g blocky graphite and 1000mL deionized water are mixed and stirred for uniformly, join first order stripping from charging aperture and set
In standby material bin, graphite in the position that rotor matches with material bin by the shear action of frictional force, each layer stone in graphite
Van der Waals force between ink alkene is disintegrated, so that graphite is peeled off thinning acquisition Graphene layer by layer, enters sub-material storehouse from feed opening,
Sieve through filter screen, meet the Graphene of filter screen mesh number and be mingled with and meet the graphite raw material of filter screen mesh number and enter first order peel-off device
Fines storehouse, enters second level peel-off device under pumping, again peels off thinning, the most again through third level peel-off device,
The finished product graphene dispersing solution obtained in the fines storehouse of third level peel-off device enters finished product receptacle;In peel-off devices at different levels not
The material bin being returned first order peel-off device by the material of filter screen continues to peel off.
Graphene dispersing solution is dried and removes ionized water, then dry Graphene is carried out specific surface area test, it is known that
The specific surface area of the Graphene that the present embodiment is obtained can reach 200~300m2/g。
Graphene is configured to the alcoholic solution of 0.01mg/mL, is dispersed in silicon oxide substrate, examines under a microscope pattern,
As shown in Figure 3, it can be seen that the present embodiment gained graphene film footpath is in 1~10 μm, and is all monolayer.
The graphene dispersion of the present embodiment is on TEM copper mesh TEM test, as shown in Figure 4, it will also be seen that gained
Graphene is single layer structure.
Doing purity analysis with dried dry powder Graphene, analysis result is as shown in Figure 5, it is known that Graphene content 99.7% with
On.
Meanwhile, by analyzing test, the electrical conductivity of the present embodiment gained Graphene is more than 30000S/m.
According to the demand of yield Yu solution concentration, can be realized by the ratio of regulation rotor speed and initial auxiliary agent and Graphene,
This device can realize the graphite conversion ratio to Graphene more than 90%, can complete the Graphene production of 100 kilograms per hour.
Embodiment 2
When the class mechanical stripping device of the present invention only has one-level peel-off device to constitute, mill structure can be reduced to, will material
Storehouse 2 and rotor 3 are equivalent to the two panels circle marble mill of marble stone grinder, and the contact surface of two fan mills arranges well-regulated ditch
Groove, as shown in Figure 6.During use, 500g crystalline flake graphite is joined a diameter of 1m marble stone grinder two panels circular millstone it
Between, rotate counterclockwise mill, while add ethanol from mill top, the most well-regulated groove in the inside of the upper lower fan of stone grinder,
And deep outside, centre is shallow, certain gap is also left in centre.The rotation ground along with upper prochlorite, graphite is first between two panels mill
Enter according to the skewed slot passage carved in the gap of mid portion, progress in the groove of rule afterwards, graphite in the process
The Van der Waals force of interlayer is disintegrated by frictional shearing, and graphite is peeled off into monolayer or multi-layer graphene, rotating grinding board 30 points layer by layer
Clock, just obtains the Graphene alcoholic solution of solid content 500g.
Take a small amount of alcoholic solution drop in respectively on oxidized silicon chip and TEM copper mesh observe, it is thus achieved that optical microphotograph picture as it is shown in fig. 7,
Gained graphene film footpath is more than 100 μm, and with the presence of monolayer and few layer, TEM characterizes as shown in Figure 8, demonstrates gained Graphene
There is monolayer and few Rotating fields.Testing by analysis, the specific surface area of gained Graphene is at 45m2About/g, electrical conductivity is more than
10000S/m。
Compared with the class mechanical stripping device being made up of three grades of peel-off devices used with embodiment 1, the ratio of the present embodiment gained Graphene
Surface area is little, electrical conductivity is little, and the most all monolayers of gained Graphene.
Embodiment 3
As a comparison, the present embodiment uses chemical method to prepare graphene powder, specific as follows: add 5mL in the flask of 250mL
Oleum, ice bath stirring is lower adds 2g graphite powder and 1g NaNO3Mixture, add 6g Gao Meng after stirring in three times
Acid potassium, period temperature not can exceed that 20 DEG C.Continue stirring to temperature and rise to 35 DEG C, within continuously stirred 30 minutes, add deionized water,
Being stirred for 20 minutes making solution uniform, add 5mL hydrogen peroxide, now solution is gradually in glassy yellow, and filtered while hot, by gained
Product cleans until solution is neutrality with 5% hydrochloric acid and deionized water successively, the product after cleaning put in vacuum drying oven
It is dried at 60 DEG C, it is thus achieved that graphite oxide.Take 100mg graphite oxide to be dispersed in 100mL water and obtain brown color suspension, will
Liquid is placed on ultrasonic disperse 1h in ultrasonic cleaner and obtains stable dispersions.Move it in flask heating in water bath subsequently to 80 DEG C,
Dropping 2mL hydrazine hydrate, filters after reaction 24h, and products therefrom methanol and deionized water respectively rinse 6 times, at vacuum drying oven
Middle with 60 DEG C be dried, obtain Graphene.
The a small amount of Graphene taking the present embodiment does specific surface area test, it is known that the specific surface area of the present embodiment gained Graphene is
550~650m2/g.Take a small amount of Graphene and do purity analysis, as shown in Figure 9, it can be seen that wherein sulfur content reaches about 5%,
Carbon content is about 94%, and electrical conductivity is about 850S/m.Therefore, although the Graphene prepared in this way has relatively
Big specific surface area, but purity is low, and electrical conductivity is low, and employs extremely toxic substance hydrazine hydrate etc., pollutes environment.
Claims (5)
1. one kind of tonne of class mechanical stripping device producing Graphene, it is characterised in that: described device is set by one or more levels stripping
Standby in series;
The structure of described peel-off device is: the upper end of a material bin (2) is provided with two charging apertures (1a), and lower end is provided with out
Material mouth (1b), the connection of described discharging opening (1b) lower section and sub-material storehouse, be provided with filter screen (5), described filter in described sub-material storehouse
Described sub-material storehouse is divided into coarse fodder storehouse (4a) and fines storehouse (4b) by net (5), and material bin (2) interior material is by discharging opening (1b)
After entering sub-material storehouse, filtering through filter screen (5), the material that can pass through filter screen (5) enters fines storehouse (4b), not by filter screen (5)
Material enter coarse fodder storehouse (4a);A rotor (3) it is provided with in described material bin (2);The lower section of described rotor (3) with
Match in the lower section of described material bin (2), when making described rotor (3) rotate, and the outer surface of rotor (3) and material bin (2)
Inner surface at mated position, form Relative friction;
The coarse fodder storehouse (4a) of peel-off devices at different levels is provided by taking out another of the pipeline communication of pump (7) and first order peel-off device
Charging aperture (1a);The fines storehouse (4b) of upper level peel-off device is provided by the pipeline communication taking out pump (7) and shells with next stage
From the charging aperture (1a) of equipment, the fines storehouse (4b) of afterbody peel-off device is provided by taking out the pipeline communication of pump (7)
With finished product receptacle (8);
The inner surface of the outer surface of described rotor (3) and material bin (2) at mated position by identical material high hardness material
Constituting, described high hardness material is the material that hardness is more than graphite;Described hardness is marble, granite more than the material of graphite
Stone, diamond, carbon steel, potassium steel, tungsten carbide or rustless steel;
The outer surface of described rotor (3) is plane at mated position with the inner surface of material bin (2) or is provided with multiple tooth
The Alveolus type flour milling of groove.
Class mechanical stripping device the most according to claim 1, it is characterised in that: in described fines storehouse (4b), it is positioned at
The lower section of described filter screen (5) is provided with filter screen brush (6);
The pipeline that the fines storehouse of afterbody peel-off device connects with finished product receptacle (8) is provided with drying equipment.
3. the class mechanical stripping device tonne that a kind utilizes described in claim 1 produces the production method of Graphene, it is characterised in that:
Start the rotor of peel-off device at different levels and take out pump;
Rotate rotor, make the outer surface of rotor and the inner surface of material bin form frictional force at mated position;
It is mixed and stirred for graphite and liquid adjuvants uniformly, then joining the material bin of first order peel-off device from charging aperture,
Graphite in the position that rotor matches with material bin by the shear action of frictional force, the Van der Waals force of each graphite layers in graphite
Disintegrate, so that graphite is stripped thinning acquisition Graphene, enter sub-material storehouse from feed opening, sieve through filter screen, pass through filter screen
Material enter next stage peel-off device, again peel off thinning, peel off obtained finished product graphite layer by layer through multistage peel-off device
Alkene enters finished product receptacle;Peel-off devices at different levels are not returned the material bin continuation stripping of first order peel-off device by the material of filter screen
From.
Method the most according to claim 3, it is characterised in that: described liquid adjuvants is deionized water, ethanol, N-methyl
Ketopyrrolidine, N,N-dimethylformamide mix with one or more in benzyl benzoate.
Method the most according to claim 3, it is characterised in that: the quality of described graphite and the volume ratio of described liquid adjuvants
It is 0.01~150:100g/mL.
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