CN106587031A - Device for continuously preparing graphene and method for producing graphene - Google Patents
Device for continuously preparing graphene and method for producing graphene Download PDFInfo
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- CN106587031A CN106587031A CN201610939741.5A CN201610939741A CN106587031A CN 106587031 A CN106587031 A CN 106587031A CN 201610939741 A CN201610939741 A CN 201610939741A CN 106587031 A CN106587031 A CN 106587031A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention belongs to the technical field of graphene and particularly relates to a device for continuously preparing graphene and a method for producing graphene. The device comprises a raw material grinding tank, a grinding medium storage bin, a stirring tank, a continuous grinding mechanism, a material storage tank, a centrifugal filtering device and a drying device. A blade type stirring mill is arranged in the raw material grinding tank. The continuous grinding mechanism comprises a high-pressure pump, the grinding bin, a flow guide ring, a dispersion impeller and a transmission shaft. The flow guide ring is located in the middle of the grinding bin and fixedly connected with the transmission shaft, the dispersion impeller is located between the flow guide ring and the bottom of the grinding bin, and the transmission shaft passes through the center of the dispersion impeller. The probability that graphene is smashed is reduced through continuous stripping step by step, structural defects of graphene are reduced, and meanwhile the situation that structural defects are caused again to stripped graphene due to re-grinding is avoided. The invention further discloses the method for producing graphene by means of the device for continuously preparing graphene from the slurry.
Description
Technical field
The invention belongs to technical field of graphene, more particularly to a kind of device for continuously preparing Graphene and Graphene are produced
Method.
Background technology
Graphene is with sp by carbon atom2The two-dimensional material of the cellular hexaplanar structure that hydridization is formed.Graphene stone
Black alkene has good electricity-optics performance, mechanical property, heat-conductive characteristic and high charge carrier mobility, together
When also have stronger mechanical strength and pliability, before the aspects such as electronics, magnetics, optics, biology have a wide range of applications
Scape.Due to having potential application prospect in various fields, therefore the basis of Graphene has become various countries' science with applied research
The focus of family's research.
Since Graphene finds, the preparation of Graphene is always the focus of people's research.The preparation method of Graphene
Including mechanical stripping method, graphite oxide reducing process, epitaxial growth method, chemical vapour deposition technique etc..Oxidation-reduction method is at present should
With more method, but the method can introduce a large amount of defects in preparation process, can not repair completely in reduction, have a strong impact on
The performances such as the electricity of Graphene；Epitaxial growth method and chemical vapour deposition technique can obtain the Graphene list of high-quality bulk
Piece, but both approaches preparation condition is harsh, and yield is not high, and substrate is had high demands, and transfer has greatly difficulty, is prepared into
This is very high.By contrast, mechanical stripping is more easy to obtain the Graphene of low cost.The method of mechanical stripping is entered from the surface of graphite flake
Row is successively peeled off and obtains graphene film, can prepare the Graphene closest to perfect condition, is that one kind can be prepared with low cost
The simple method of high-quality graphene.At present the conventional method of mechanical stripping method includes adhesive tape method, ultrasonic method, polishing
Deng wherein polishing is divided into conventional grinding, ball milling, stirring ball-milling etc..
Conventional grinding stripping means is primarily referred to as grinding graphite in mortar formula beveller, the friction produced by pressure
Power is sheared to graphite, and pestle body can make Graphene produce fault of construction to the pressure that graphite applies, or even can make stone after stripping
Black alkene is crushed so that have " burr " obtained product edge more, and crystalline size is little, and easily causes pestle body to graphite applying pressure
Power is uneven, and then easily produces overground, the quality of impact Graphene.Ball milling is referred in ball mill by abrading-ball to graphite composite powder
Grinding, overcomes the pressurized inequality of conventional powder grinding, locally applies the big shortcoming of pressure, but the abrading-ball meeting in mechanical milling process
Impact being provided to powder body and shearing two kinds of active force, abrading-ball not only againsts the inwall of ball grinder and applies shearing work to graphite
With, and abrading-ball can back and forth clash into the inwall of ball grinder, and the Graphene to peeling off produces huge impulsive force；Come from abrading-ball
This impulsive force can also make Graphene produce fault of construction, the size of Graphene after reducing peeling off so that obtained product edge
There is " burr " more, and crystalline size is little.Stirring ball-milling is a kind of mechanical mill mode of stirring in combination with spheroidal graphite, and agitator is in chamber
Abrading-ball collision friction is driven in vivo, and powder body is ground；The percussion of its abrading-ball is gentle compared with ball milling method, but due to mill
The presence of ball, still makes Graphene produce fault of construction, graphite after reducing peeling off the Graphene generation impulsive force peeled off unavoidably
The size of alkene so that obtained product edge produces " burr ", and reduce crystalline size.
In sum, current mechanical milling method such as ball-milling method mainly uses grinding to graphite applying pressure, using solid
Rubbing action between body abrasive media and graphite makes graphite peel off into Graphene, but this impulsive force easily causes the crystalline substance of Graphene
Lattice defect, reduces the crystalline size of graphene product, and the crunch of simultaneous grinding medium can cause graphite Rotating fields to become more
Plus closely peeling effect can be caused on the contrary to reduce, cause milling time length, with high costs；If reducing impulsive force on the contrary, rub
Wipe power little, part powder body shearing force deficiency can be caused, it is difficult to which shearing is peeled off, therefore the technological parameter of equipment is difficult to debugging to most preferably
Working condition, affects large-scale industrialized production.
The content of the invention
Graphene size that the present invention is obtained for current Graphene mechanical stripping equipment is little, defect is more, charge stripping efficiency is low
Problem, propose a kind of device for continuously preparing Graphene and Graphene production method, its object is to be related to it is a kind of be adapted to it is big
Technical scale, can continuous high-efficient produce high-quality graphene device.It is a further object of the present invention to provide a kind of continuous
The method that metaplasia produces high-quality graphene.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of device for continuously preparing Graphene, it is characterised in that including raw mill tank（1）, abrasive media warehouse（2）, stirring
Groove（3）, continuously grinding mechanism（4）, storage tank（5）, centrifugal filter device（6）And drying device（7）；Wherein described raw mill
Tank（1）Inside it is provided with blade stirrer mill（11）；Raw mill tank and abrasive media warehouse bottom are respectively provided with discharging opening（12）、
（21）, agitator tank（3）Enterprising material mouth is set（31）With lower charging aperture（32）, the discharging opening of raw mill tank（12）And abrasive media
The discharging opening of warehouse（21）Respectively with agitator tank（3）Enterprising material mouth be connected, in order to transferring raw material and grinding in stock tank
Medium；Continuously grinding mechanism（4）Including high-pressure pump（41）, grinding storehouse（42）, guide ring（43）, dispersion impeller（44）And power transmission shaft
（45）；The grinding storehouse（42）Bottom is provided with charging aperture（421）, middle part be provided with discharging opening（422）, the high-pressure pump（41）Respectively
With agitator tank（3）Lower charging aperture（32）, grinding storehouse（42）Charging aperture（421）It is connected, grinds storehouse（42）Discharging opening（422）
With storage tank（5）；The guide ring（43）Positioned at grinding storehouse（42）Middle part and and power transmission shaft（45）It is fixedly connected, the dispersion leaf
Wheel（44）Positioned at the guide ring（43）With the grinding storehouse（42）Bottom between, the power transmission shaft（45）By the dispersion
Impeller（44）Center；The storage tank（5）With centrifugal filter device（6）One end be connected, drying device（7）With centrifugal filtration
Device（6）The other end be connected.
Blade stirrer mill described above（11）It is interior arrange at least two mill be situated between, it is described mill be situated between a diameter of 0.1～
10mm, described abrasive media can be the various shapes such as spherical, bar-shaped, and preferably spherical, material is preferably quartz sand, glass
Pearl, ceramic bead, the mixture of zirconium pearl.Graphite raw material is tentatively ground by blade stirrer mill, improves follow-up graphite
Grinding charge stripping efficiency.
High-pressure pump described above（41）Including at least one pair of plunger（411）, each plunger is arranged at a pump chamber（412）
Interior, the liquid material in two pump chambers of correspondence is passed through baffling road by every a pair of plungers（413）Nozzle（414）Spray simultaneously to grinding
Mill storehouse.Graphite dispersion slurry is sucked by high-pressure pump, baffling road is enabled flow through by plunger motion, make the stone for flowing up and down
Black dispersed slurry becomes left and right flowing, makes graphite mix homogeneously and reaches the purpose of preliminary crushing, and Jing is arranged on folding runner exit
The nozzle of pairing make the graphite slurry of preliminary crushing clash, shearing effect in flow at high speed, shock when spraying at a high speed
Graphite laminated is made under void effect triple role when effect, moment crunch drop, the secondary stripping of graphite is reached.
Guide ring described above（43）Periphery is provided with two spiral helicine blades, and spiral helicine blade can be carried for slurry
For spiral helicine movement locus upwards, when slurry is thrown off guide ring, its direction of motion can be thrown to guide ring
Side or other any directions, contribute to increasing the severity of the collision frequency of slurry and collision, such that it is able to improve grinding effect
Rate, reduces circular grinding number of times.
Described dispersion impeller（44）Including two leaf dishes be arrangeding in parallel（441）, the leaf dish is provided with plurality of passages
（442）, each two leaf dish is by the support column that multiple cross sections are circular or ellipse（443）It is fixed, dispersion impeller（44）Center
It is provided with through hole（444）.
To realize above-mentioned second purpose, what the present invention was achieved through the following technical solutions：
A kind of usage right requires continuously to prepare the method that Graphene device produces Graphene, its feature described in any one of 1-5
It is that specific production method is as follows：
（1）Graphite raw material is put in raw mill tank, is roughly ground graphite raw material using medium milling；
（2）Corase grind graphite raw material in raw mill tank is entered in agitator tank by the enterprising material mouth of agitator tank, is subsequently adding
Abrasive media in abrasive media warehouse, water is injected from lower charging aperture, and the mixing speed for arranging agitator tank is 100 ~ 800rpm,
Obtain graphite dispersion slurry；
（3）Start continuously grinding mechanism, by high-pressure pump by step（2）In graphite dispersion slurry spray into grinding storehouse, dispersion
Under the running up of impeller, dispersed slurry carries out shearing grinding from the medial wall that the bottom in grinding storehouse rushes at grinding storehouse, while not
Shearing the graphite of stripping completely can separate with the Graphene that peel off, not shear completely the graphite of stripping because action of gravity by by
Power transmission shaft drives the guide ring of rotation randomly to fall on the different passages of dispersion impeller, rotates through the high speed of dispersion impeller,
Again the graphite to not shearing stripping completely is circulated shearing, and the wherein jet fluid speed of high-pressure pump is 100 ~ 150m/s,
The rotating speed of dispersion impeller is 1000 ~ 5000rpm, and milling time is 1 ~ 10min；
（4）By step（3）The grinding product for obtaining is expelled in storage tank from the discharging opening in grinding storehouse, stands 12 ~ 24h；
（5）By step（4）The graphene suspension in storage tank after standing is delivered in centrifugal filter device, arranges centrifugation
Rotating speed is 5000 ~ 10000 rpm, 10 ~ 30min of centrifugation time, takes the supernatant, and filter is filtrated to get in vacuum apparatus
Cake；
（6）By step（5）The filter cake for obtaining is cleaned 2 ~ 3 times respectively with ethanol, water, and 2 ~ 4h is dried in vacuum drying oven, is obtained final product
Graphene product.
Above-mentioned steps（1）Described in abrasive media be a diameter of 0.1～10mm quartz sands, bead, ceramic bead, zirconium
At least two mixture in pearl.
Above-mentioned steps（2）Described in abrasive media by weight percentage by as follows into being grouped into：Amphiphilic polymers 30 ~
45%th, nano modification brucite 25 ~ 30%, micro-expanding agent 10 ~ 15%, binding agent 5～15%, cyclodextrin 5 ~ 10%, carbamide 5 ~ 10%.
The characteristics of projecting compared with prior art and beneficial effect are：
1st, a kind of device for continuously preparing Graphene of the present invention, to graphite raw material continuously grinding stripping is carried out, and is first to utilize
Blade stirrer mill is roughly ground to graphite, and by high-pressure pump instantaneous pressure drop, highly pressurised liquid shearing, high-speed impact work are produced
With comprehensive functions such as the, higher-order of oscillation and cavitation erosions, make graphite produce crystal face horizontal displacement and sliding motion between layers, reach stone
The secondary stripping of ink；By cooperating for guide ring and dispersion impeller, make not shear completely the graphite of stripping with having peeled off
Graphene is separated, and the graphite that stripping is not sheared completely falls dispersion impeller by guide ring, is rotated through the high speed of dispersion impeller,
Again the graphite to not shearing stripping completely is circulated shearing, and graphite is completely exfoliated.Peel off by the way that substep is continuous, reduce
Graphite or the pulverized probability of Graphene, reduce the fault of construction of Graphene, while preventing the Graphene peeled off because grinding again
Mill causes fault of construction.
2nd, it is 1 ~ 10 layer by the Graphene number of plies obtained in Graphene process units mechanical stripping of the present invention, fault of construction
Few, edge is rounded, and dispersive property is excellent, and production efficiency is high, and specific productivity reaches 40 ~ 60%.
3rd, stripping is carried out to graphite using Graphene process units of the present invention and prepares Graphene, due to using mechanical stripping
Method produces Graphene, cheap, with great cost advantage, and is capable of achieving the commercial production of scale；Preparation process
Strong acid and strong base or other noxious substances are not used, additive is few, without the need for using substantial amounts of organic solvent so that prepare Graphene more
For environmental protection, process is simple.
Description of the drawings
Fig. 1 is the structural representation of Graphene process units of the present invention；
Fig. 2 is the high-pressure pump structure schematic diagram of the continuously grinding mechanism in the embodiment of the present invention 1；
Fig. 3 is the structural representation of the dispersion impeller of the continuously grinding mechanism in the embodiment of the present invention 1；
In figure：1st, raw mill tank；2nd, abrasive media warehouse；3rd, agitator tank；4th, continuously grinding mechanism；5th, storage tank；6th, it is centrifuged
Defecator；7th, drying device；11st, blade stirrer mill；12nd, raw mill tank discharging opening；21st, abrasive media warehouse discharging
Mouthful；The enterprising material mouth of 31 agitator tanks；32nd, charging aperture under agitator tank；41st, high-pressure pump；42nd, storehouse is ground；43rd, guide ring；44th, leaf is disperseed
Wheel；45th, power transmission shaft；411st, plunger；412nd, pump chamber；413rd, baffling road；414th, nozzle；421st, storehouse charging aperture is ground；422nd, grind
Bin discharge port external；441st, leaf dish；442nd, passage；443rd, support column；444th, through hole.
Specific embodiment
The present invention is explained in detail below in conjunction with specific embodiment, is not restricted to the present invention.Without departing from
In the case of said method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change
Enter, should be included within the scope of the present invention.
Embodiment 1
The present embodiment provides the device that a kind of slurry continuously grinding prepares Graphene.
A kind of device for continuously preparing Graphene, as shown in figure 1, including raw mill tank successively（1）, abrasive media warehouse
（2）, agitator tank（3）, continuously grinding mechanism（4）, storage tank（5）, centrifugal filter device（6）And drying device（7）.Raw mill
Tank（1）Inside it is provided with blade stirrer mill（11）, for roughly grinding to graphite raw material；Abrasive media warehouse（2）For storing
Abrasive media；Raw mill tank and abrasive media warehouse bottom are respectively provided with discharging opening（12）、（21）；Agitator tank（3）For preparing
Graphite slurry, agitator tank（3）Enterprising material mouth is set（31）With lower charging aperture（32）, the discharging opening of raw mill tank（12）And grinding
The discharging opening of medium warehouse（21）Respectively with agitator tank（3）Enterprising material mouth be connected, in order to transferring raw material in stock tank and
Abrasive media.Continuously grinding mechanism（4）For peeling off to the shearing of graphite slurry continuous process, storage tank（5）For collect and it is quiet
Put continuous shear stress and peel off the Graphene slurry for obtaining, storage tank（5）With centrifugal filter device（6）One end be connected, drying device
（7）With centrifugal filter device（6）The other end be connected.Centrifugal filter device（6）For by storage tank（5）Interior upper strata suspension enters
Row centrifugation, filtration, washing, drying device（7）Graphene after filtering for vacuum drying.
Continuously grinding mechanism（4）Including high-pressure pump（41）, grinding storehouse（42）, guide ring（43）, dispersion impeller（44）And biography
Moving axis（45）.Grinding storehouse（42）Bottom is provided with charging aperture（421）, middle part be provided with discharging opening（422）, high-pressure pump（41）Respectively with stir
Mix groove（3）Lower charging aperture（32）, grinding storehouse（42）Charging aperture（421）It is connected, grinds storehouse（42）Discharging opening（422）With storage
Batch can（5）；Guide ring（43）Positioned at grinding storehouse（42）Middle part and and power transmission shaft（45）It is fixedly connected, dispersion impeller（44）Positioned at leading
Stream ring（43）With grinding storehouse（42）Bottom between, power transmission shaft（45）By the dispersion impeller（44）Center.Guide ring
（43）Periphery is provided with two spiral helicine blades, and spiral helicine blade can provide spiral helicine motion rail upwards for slurry
Mark, when slurry is thrown off guide ring, its direction of motion can be thrown to guide ring top or other any directions, contribute to
Increase the collision frequency of slurry and the severity of collision, such that it is able to improve grinding efficiency, reduce circular grinding number of times.
As shown in Fig. 2 high-pressure pump（41）Including a pair of plungers（411）, each plunger is arranged at a pump chamber（412）It is interior,
Liquid material in two pump chambers of correspondence is passed through baffling road by every a pair of plungers（413）Nozzle（414）Spray simultaneously to grinding storehouse.
As shown in figure 3, dispersion impeller（44）Including two leaf dishes be arrangeding in parallel（441）, the leaf dish be provided with 4 lead to
Road（442）, two leaf dishes are oval support column by 4 cross sections（443）It is fixed, dispersion impeller（44）Center is provided with through hole
（444）.
Embodiment 2
The present embodiment provides a kind of production method of Graphene, and it is to be carried out using the preparation facilitiess of the Graphene of embodiment 1
The method of production, the method is comprised the following steps：
（1）Graphite raw material is put in raw mill tank, the quartz sand and ceramic bead of a diameter of 2mm is added, is ground using medium
Mill is roughly ground graphite raw material；
（2）Corase grind graphite raw material in raw mill tank is entered in agitator tank by the enterprising material mouth of agitator tank, is subsequently adding
Abrasive media in abrasive media warehouse, water is injected from lower charging aperture, and the mixing speed for arranging agitator tank is 500rpm, is obtained
Graphite dispersion slurry；Wherein described abrasive media is by weight percentage by as follows into being grouped into：Amphiphilic polymers 40%, nanometer
Modified hydrotalcite 30%, micro-expanding agent 10%, binding agent 5%, cyclodextrin 10%, carbamide 5%.
（3）Start continuously grinding mechanism, by high-pressure pump by step（2）In graphite dispersion slurry spray into grinding storehouse,
Under the running up of dispersion impeller, dispersed slurry carries out shearing grinding from the medial wall that the bottom in grinding storehouse rushes at grinding storehouse, together
When do not shear the graphite of stripping completely and can separate with the Graphene that peel off, the graphite of stripping is not sheared completely because action of gravity is logical
Cross and drive the guide ring of rotation randomly to fall on the different passages of dispersion impeller by power transmission shaft, revolve through the high speed of dispersion impeller
Turn, again the graphite to not shearing stripping completely is circulated shearing, and the wherein jet fluid speed of high-pressure pump is 100m/s, point
The rotating speed of scattered impeller is 5000rpm, and milling time is 1min；
（4）By step（3）The grinding product for obtaining is expelled in storage tank from the discharging opening in grinding storehouse, stands 24h；
（5）By step（4）The graphene suspension in storage tank after standing is delivered in centrifugal filter device, arranges centrifugation
Rotating speed is 10000 rpm, centrifugation time 30min, takes the supernatant, and filter cake is filtrated to get in vacuum apparatus；
（6）By step（5）The filter cake for obtaining is cleaned 2 ~ 3 times respectively with ethanol, water, and 4h is dried in vacuum drying oven, obtains final product stone
Black alkene product.
The graphite ene product of gained is characterized using atomic force ultramicroscope, learns that graphite ene product is less than 10
The Graphene of layer accounts for 92%, thus, the graphite ene product of embodiment 2 has the advantages that high-quality, high yield.
Embodiment 3
The present embodiment provides a kind of production method of Graphene, and it is to be carried out using the preparation facilitiess of the Graphene of embodiment 1
The method of production, the method is comprised the following steps：
（1）Graphite raw material is put in raw mill tank, ceramic bead and the zirconium pearl of a diameter of 5mm is added, using medium milling
Graphite raw material is roughly ground；
（2）Corase grind graphite raw material in raw mill tank is entered in agitator tank by the enterprising material mouth of agitator tank, is subsequently adding
Abrasive media in abrasive media warehouse, water is injected from lower charging aperture, and the mixing speed for arranging agitator tank is 800rpm, is obtained
Graphite dispersion slurry；Wherein described abrasive media is by weight percentage by as follows into being grouped into：Amphiphilic polymers 30%, nanometer
Modified hydrotalcite 30%, micro-expanding agent 10%, binding agent 10%, cyclodextrin 10%, carbamide 10%.
（3）Start continuously grinding mechanism, by high-pressure pump by step（2）In graphite dispersion slurry spray into grinding storehouse,
Under the running up of dispersion impeller, dispersed slurry carries out shearing grinding from the medial wall that the bottom in grinding storehouse rushes at grinding storehouse, together
When do not shear the graphite of stripping completely and can separate with the Graphene that peel off, the graphite of stripping is not sheared completely because action of gravity is logical
Cross and drive the guide ring of rotation randomly to fall on the different passages of dispersion impeller by power transmission shaft, revolve through the high speed of dispersion impeller
Turn, again the graphite to not shearing stripping completely is circulated shearing, and the wherein jet fluid speed of high-pressure pump is 150m/s, point
The rotating speed of scattered impeller is 3000rpm, and milling time is 5min；
（4）By step（3）The grinding product for obtaining is expelled in storage tank from the discharging opening in grinding storehouse, stands 12h；
（5）By step（4）The graphene suspension in storage tank after standing is delivered in centrifugal filter device, arranges centrifugation
Rotating speed is 5000 rpm, centrifugation time 20min, takes the supernatant, and filter cake is filtrated to get in vacuum apparatus；
（6）By step（5）The filter cake for obtaining is cleaned 2 ~ 3 times respectively with ethanol, water, and 2h is dried in vacuum drying oven, obtains final product stone
Black alkene product.
The graphite ene product of gained is characterized using atomic force ultramicroscope, learns that graphite ene product is less than 10
The Graphene of layer accounts for 95%, thus, the graphite ene product of embodiment 3 has the advantages that high-quality, high yield.
Claims (8)
1. a kind of device for continuously preparing Graphene, it is characterised in that including raw mill tank（1）, abrasive media warehouse（2）, stir
Mix groove（3）, continuously grinding mechanism（4）, storage tank（5）, centrifugal filter device（6）And drying device（7）；Wherein described raw material grinds
Grinding jar（1）Inside it is provided with blade stirrer mill（11）；Raw mill tank and abrasive media warehouse bottom are respectively provided with discharging opening（12）、
（21）, agitator tank（3）Enterprising material mouth is set（31）With lower charging aperture（32）, the discharging opening of raw mill tank（12）And abrasive media
The discharging opening of warehouse（21）Respectively with agitator tank（3）Enterprising material mouth（31）Be connected, in order to transferring raw material in stock tank and
Abrasive media；Continuously grinding mechanism（4）Including high-pressure pump（41）, grinding storehouse（42）, guide ring（43）, dispersion impeller（44）And biography
Moving axis（45）；The grinding storehouse（42）Bottom is provided with charging aperture（421）, middle part be provided with discharging opening（422）, the high-pressure pump（41）
Respectively with agitator tank（3）Lower charging aperture（32）, grinding storehouse（42）Charging aperture（421）It is connected, grinds storehouse（42）Discharging opening
（422）With storage tank（5）；The guide ring（43）Positioned at grinding storehouse（42）Middle part and and power transmission shaft（45）It is fixedly connected, it is described
Dispersion impeller（44）Positioned at the guide ring（43）With the grinding storehouse（42）Bottom between, the power transmission shaft（45）By institute
State dispersion impeller（44）Center；The storage tank（5）With centrifugal filter device（6）One end be connected, drying device（7）With from
Heart defecator（6）The other end be connected.
2. a kind of device for continuously preparing Graphene according to claim 1, it is characterised in that described vane type is stirred
Mix mill（11）Interior at least two mills that arrange are situated between, a diameter of 0.1～10mm that the mill is situated between.
3. a kind of device for continuously preparing Graphene according to claim 1, it is characterised in that described high-pressure pump
（41）Including at least one pair of plunger（411）, each plunger is arranged at a pump chamber（412）Interior, every a pair of plungers will two pumps of correspondence
The liquid material of intracavity passes through baffling road（413）Nozzle（414）Spray simultaneously to grinding storehouse.
4. a kind of device for continuously preparing Graphene according to claim 1, it is characterised in that described guide ring（43）
Periphery is provided with two spiral helicine blades.
5. a kind of device for continuously preparing Graphene according to claim 1, it is characterised in that described dispersion impeller
（44）Including two leaf dishes be arrangeding in parallel（441）, the leaf dish is provided with plurality of passages（442）, each two leaf dish is by multiple
Cross section is the support column of circular or ellipse（443）It is fixed, dispersion impeller（44）Center is provided with through hole（444）.
6. a kind of usage right requires continuously to prepare the method that Graphene device produces Graphene described in any one of 1-5, and it is special
Levy is that specific production method is as follows：
（1）Graphite raw material is put in raw mill tank, is roughly ground graphite raw material using medium milling；
（2）Corase grind graphite raw material in raw mill tank is entered in agitator tank by the enterprising material mouth of agitator tank, is subsequently adding
Abrasive media in abrasive media warehouse, water is injected from lower charging aperture, and the mixing speed for arranging agitator tank is 100 ~ 800rpm,
Obtain graphite dispersion slurry；
（3）Start continuously grinding mechanism, by high-pressure pump by step（2）In graphite dispersion slurry spray into grinding storehouse, dispersion
Under the running up of impeller, dispersed slurry carries out shearing grinding from the medial wall that the bottom in grinding storehouse rushes at grinding storehouse, while not
Shearing the graphite of stripping completely can separate with the Graphene that peel off, not shear completely the graphite of stripping because action of gravity by by
Power transmission shaft drives the guide ring of rotation randomly to fall on the different passages of dispersion impeller, rotates through the high speed of dispersion impeller,
Again the graphite to not shearing stripping completely is circulated shearing, and the wherein jet fluid speed of high-pressure pump is 100 ~ 150m/s,
The rotating speed of dispersion impeller is 1000 ~ 5000rpm, and milling time is 1 ~ 10min；
（4）By step（3）The grinding product for obtaining is expelled in storage tank from the discharging opening in grinding storehouse, stands 12 ~ 24h；
（5）By step（4）The graphene suspension in storage tank after standing is delivered in centrifugal filter device, arranges centrifugation
Rotating speed is 5000 ~ 10000 rpm, 10 ~ 30min of centrifugation time, takes the supernatant, and filter is filtrated to get in vacuum apparatus
Cake；
（6）By step（5）The filter cake for obtaining is cleaned 2 ~ 3 times respectively with ethanol, water, and 2 ~ 4h is dried in vacuum drying oven, is obtained final product
Graphene product.
7. according to claim 6 a kind of using the method that Graphene device produces Graphene is continuously prepared, its feature exists
In step（1）Described in abrasive media be in a diameter of 0.1～10mm quartz sands, bead, ceramic bead, zirconium pearl at least
Two kinds of mixture.
8. according to claim 6 a kind of using the method that Graphene device produces Graphene is continuously prepared, its feature exists
In step（2）Described in abrasive media by weight percentage by as follows into being grouped into：Amphiphilic polymers 30 ~ 45%, nanometer change
Property brucite 25 ~ 30%, micro-expanding agent 10 ~ 15%, binding agent 5～15%, cyclodextrin 5 ~ 10%, carbamide 5 ~ 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610939741.5A CN106587031B (en) | 2016-11-02 | 2016-11-02 | A kind of device and graphene production method continuously preparing graphene |
Applications Claiming Priority (1)
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| CN107311166A (en) * | 2017-05-18 | 2017-11-03 | 北京化工大学 | A kind of preparation method and its usage of thin layer carbon |
| CN107601480A (en) * | 2017-10-20 | 2018-01-19 | 南通富莱克流体装备有限公司 | Graphene production equipment |
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| CN109019566A (en) * | 2018-09-05 | 2018-12-18 | 七台河宝泰隆石墨烯新材料有限公司 | A kind of graphene continuously can control production technology |
| CN109179383A (en) * | 2018-01-17 | 2019-01-11 | 中原大学 | Graphene structure, method for preparing graphene and lithium ion battery electrode |
| CN112960669A (en) * | 2021-02-01 | 2021-06-15 | 兰州大学 | Preparation device and preparation method of biomedical graphene dispersion liquid |
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| CN112960669B (en) * | 2021-02-01 | 2022-08-30 | 兰州大学 | Preparation device and preparation method of biomedical graphene dispersion liquid |
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