CN106587031B - A kind of device and graphene production method continuously preparing graphene - Google Patents
A kind of device and graphene production method continuously preparing graphene Download PDFInfo
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- CN106587031B CN106587031B CN201610939741.5A CN201610939741A CN106587031B CN 106587031 B CN106587031 B CN 106587031B CN 201610939741 A CN201610939741 A CN 201610939741A CN 106587031 B CN106587031 B CN 106587031B
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- C01B2204/00—Structure or properties of graphene
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Abstract
The invention belongs to technical field of graphene, in particular to a kind of device and graphene production method for continuously preparing graphene.The device includes raw material grinding pot, abrasive media warehouse, stirred tank, continuously grinding mechanism, storage tank, centrifugal filter device and drying device；Wherein blade stirrer is equipped in the raw material grinding pot to grind；Continuously grinding mechanism includes high-pressure pump, grinding storehouse, guide ring, dispersion impeller and transmission shaft；The guide ring is located in the middle part of grinding storehouse and is fixedly connected with transmission shaft, and the dispersion impeller is located between the guide ring and the bottom in the grinding storehouse, the center that the transmission shaft passes through the dispersion impeller.The present invention reduces the pulverized probability of graphene, reduces the fault of construction of graphene, while preventing the graphene removed because regrinding leads to fault of construction by the continuous removing of substep.The invention also discloses the methods for using the slurry continuously grinding to prepare graphene device production graphene.
Description
Technical field
The invention belongs to technical field of graphene, in particular to a kind of device for continuously preparing graphene and graphene production
Method.
Background technique
Graphene is by carbon atom with sp2The two-dimensional material for the honeycomb 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 there are also stronger mechanical strength and flexibility, electronics, magnetics, optics, in terms of have a wide range of applications before
Scape.Due to having potential application prospect in various fields, basis and the application study of graphene have become various countries' science
The hot spot of family's research.
Since graphene discovery, the preparation of graphene always is the hot spot of research.The preparation method of graphene
Including mechanical stripping method, graphite oxide reduction method, epitaxial growth method, chemical vapour deposition technique etc..Oxidation-reduction method is to answer at present
With more method, but this method can introduce a large amount of defects during the preparation process, cannot repair, seriously affect completely in reduction
The performances such as the electricity of graphene；The graphene list of epitaxial growth method and the available high-quality bulk of chemical vapour deposition technique
Piece, but both methods preparation condition is harsh, yield is not high, and high to substrate requirement, transfer has greatly difficulty, is prepared into
This is very high.In contrast, mechanical stripping is easier to obtain the graphene of low cost.The method of mechanical stripping from the surface of graphite flake into
Successively removing obtains graphene film to row, can prepare the graphene closest to perfect condition, be that a kind of can be prepared with low cost
The simple and easy method of high-quality graphene.The common method of mechanical stripping method includes tape method, ultrasonic method, polishing at present
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 generated by pressure
Power shears graphite, and pestle body can make graphene generate fault of construction the pressure that graphite applies, or even can make stone after removing
Black alkene crushes, so that product edge obtained has " burr " more, and crystalline size is small, and be easy to cause pestle body to apply graphite and press
Power is uneven, and then is easy to produce overground, influences the quality of graphene.Ball milling refers in the ball mill by abrading-ball to graphite composite powder
Grinding overcomes the conventional powder grinding uneven, part that is pressurized and applies the big disadvantage of pressure, but the abrading-ball meeting in mechanical milling process
Impact is provided to powder and shears two kinds of active force, and the inner wall that abrading-ball not only againsts ball grinder applies shearing to graphite and makees
With, and abrading-ball can hit the inner wall of ball grinder back and forth, generate huge impact force to the graphene of removing；From abrading-ball
This impact force can also make graphene generate fault of construction, the size of graphene after removing be reduced, so that product edge obtained
There is " burr ", and crystalline size is small more.Stirring ball-milling is a kind of mechanical mill mode for stirring and combining with spheroidal graphite, and blender is in chamber
Abrading-ball collision friction is driven in vivo, and powder is ground；The percussion of its abrading-ball is mild compared with ball milling method, but due to mill
The presence of ball still generates impact force to the graphene of removing unavoidably, and graphene is made to generate fault of construction, reduces graphite after removing
The size of alkene so that product edge obtained generates " burr ", and reduces crystalline size.
In conclusion current mechanical milling method such as ball-milling method mainly applies pressure to graphite using grinding, using admittedly
Rubbing action between body abrasive media and graphite makes graphite removing at graphene, but this impact force easily causes the crystalline substance of graphene
Lattice defect reduces the crystalline size of graphene product, and the crunch of simultaneous grinding medium, which will lead to graphite linings structure, to be become more
Stepping up the close peeling effect that will lead to instead reduces, and causes milling time long, with high costs；Instead if reducing impact force, rub
It is small to wipe power, it is insufficient to will lead to part powder shearing force, it is difficult to shearing removing, therefore the technological parameter of equipment be difficult to debug it is best
Working condition influences large-scale industrialized production.
Summary of the invention
The graphene size that the present invention is obtained for current graphene mechanical stripping equipment is small, defect is more, charge stripping efficiency is low
The problem of, propose a kind of device and graphene production method for continuously preparing graphene, its object is to be related to a kind of be suitble to greatly
Technical scale, can continuous high-efficient production high-quality graphene device.It is a further object of the present invention to provide a kind of continuous
The method of metaplasia production high-quality graphene.
To achieve the above object, the present invention adopts the following technical scheme:
It is a kind of continuously to prepare the device of graphene, it is characterised in that including raw material grinding pot (1), abrasive media warehouse (2),
Stirred tank (3), continuously grinding mechanism (4), storage tank (5), centrifugal filter device (6) and drying device (7)；The wherein raw material
Blade stirrer mill (11) is equipped in grinding pot (1)；Raw material grinding pot and abrasive media warehouse bottom be respectively provided with discharge port (12),
(21), enterprising material mouth (31) and lower feed inlet (32), the discharge port (12) and abrasive media of raw material grinding pot is arranged in stirred tank (3)
The discharge port (21) of warehouse is connected with the enterprising material mouth of stirred tank (3) respectively, in order to transferring raw material and grinding in stock tank
Medium；Continuously grinding mechanism (4) includes high-pressure pump (41), grinding storehouse (42), guide ring (43), dispersion impeller (44) and transmission shaft
(45)；The grinding storehouse (42) lower part is equipped with feed inlet (421), middle part is equipped with discharge port (422), and the high-pressure pump (41) is respectively
It is connected with the feed inlet (421) of the lower feed inlet (32) of stirred tank (3), grinding storehouse (42), grinds the discharge port (422) of storehouse (42)
With storage tank (5)；The guide ring (43) is located in the middle part of grinding storehouse (42) and is fixedly connected with transmission shaft (45), the dispersion leaf
Wheel (44) is located between the guide ring (43) and the bottom of grinding storehouse (42), and the transmission shaft (45) passes through the dispersion
The center of impeller (44)；The storage tank (5) is connected with one end of centrifugal filter device (6), drying device (7) and centrifugal filtration
The other end of device (6) is connected.
At least two mill of setting is situated between in blade stirrer mill (11) described above, and the diameter that the mill is situated between is 0.1~
10mm, the abrasive media can be the various shapes such as spherical, rodlike, and preferably spherical, material is preferably quartz sand, glass
Pearl, ceramic bead, zirconium pearl mixture.Graphite raw material is tentatively ground by blade stirrer mill, improves subsequent graphite
Grind charge stripping efficiency.
High-pressure pump (41) described above includes at least a pair of of plunger (411), each plunger is set to a pump chamber (412)
Interior, every a pair of plunger sprays the liquid material in corresponding two pump chambers simultaneously to grinding by the nozzle (414) of baffling road (413)
Grind storehouse.Graphite dispersion slurry is sucked by high-pressure pump, baffling road is enabled flow through by plunger motion, makes the stone flowed up and down
Black dispersed slurry becomes left and right flowing, is uniformly mixed graphite and achievees the purpose that tentatively to crush, is mounted on folding runner exit
The nozzle of pairing so that the graphite slurry tentatively crushed is clashed, shearing effect in flow at high speed, shock when high speed is sprayed
Make graphite laminated under void effect triple role when effect, moment crunch drop, reaches the secondary removing of graphite.
Guide ring (43) periphery described above is equipped with two spiral helicine blades, and spiral helicine blade can mention for slurry
For upward spiral helicine motion profile, when slurry is thrown off guide ring, the direction of motion can be and be thrown to guide ring
Square or any other direction helps to increase the collision frequency of slurry and the severity of collision, so as to improve grinding effect
Rate reduces circular grinding number.
The dispersion impeller (44) includes two leaf dishes (441) disposed in parallel, and the leaf dish is equipped with plurality of passages
(442), the support column (443) that every two leaf dish is round or oval by multiple cross sections is fixed, dispersion impeller (44) center
Equipped with through-hole (444).
To realize above-mentioned second purpose, what the present invention was achieved through the following technical solutions:
A method of graphene device production graphene continuously being prepared using claim 1-5 is described in any item,
It is characterized in that specific production method is as follows:
(1) graphite raw material is put into raw material grinding pot, is roughly ground graphite raw material using medium milling；
(2) the corase grinding graphite raw material in raw material grinding pot is entered in stirred tank by the enterprising material mouth of stirred tank, then
The abrasive media in abrasive media warehouse is added, water inject from lower feed inlet, be arranged the mixing speed of stirred tank for 100 ~
800rpm obtains graphite dispersion slurry；
(3) start continuously grinding mechanism, the graphite dispersion slurry in step (2) is sprayed by grinding storehouse by high-pressure pump,
Under the running at high speed of dispersion impeller, dispersed slurry carries out shearing grinding from the inner sidewall that the bottom in grinding storehouse rushes at grinding storehouse, together
When do not shear completely removing graphite can with remove graphene separation, completely shearing removing graphite lead to due to gravity
It crosses and is randomly fallen on the different channels of dispersion impeller by the guide ring of transmission shaft driving rotation, the high speed rotation by dispersion impeller
Turn, circulation shear is carried out to the graphite of not shearing removing completely again, wherein the injection fluid velocity of high-pressure pump is 100 ~ 150m/
S, the revolving speed of dispersion impeller are 1000 ~ 5000rpm, and milling time is 1 ~ 10min；
(4) grinding product that step (3) obtains is expelled in storage tank from the discharge port in grinding storehouse, standing 12 ~ for 24 hours；
(5) graphene suspension in storage tank after standing step (4) is delivered in centrifugal filter device, is arranged
Centrifugal rotational speed is 5000 ~ 10000 rpm, and 10 ~ 30min of centrifugation time takes supernatant liquor, is obtained by filtration in vacuum apparatus
Filter cake；
(6) filter cake that step (5) obtains is cleaned 2 ~ 3 times with ethyl alcohol, water respectively, dries 2 ~ 4h in a vacuum drying oven,
Up to graphene product.
Abrasive media described in above-mentioned steps (1) is that diameter is 0.1~10mm quartz sand, bead, ceramic bead, zirconium
At least two mixtures in pearl.
Abrasive media described in above-mentioned steps (2) is by weight percentage by as follows at being grouped as: amphiphilic polymers 30 ~
45%, nano modification hydrotalcite 25 ~ 30%, micro-expanding agent 10 ~ 15%, binder 5~15%, cyclodextrin 5 ~ 10%, urea 5 ~ 10%.
Prominent feature and beneficial effect are compared with prior art:
1, a kind of device for continuously preparing graphene of the present invention carries out continuously grinding removing to graphite raw material, is first
Graphite is roughly ground using blade stirrer mill, instantaneous pressure drop, highly pressurised liquid shearing, high-speed impact are generated by high-pressure pump
The comprehensive functions such as effect, the higher-order of oscillation and cavitation erosion, make graphite generate crystal face horizontal displacement and sliding motion between layers, reach
The secondary removing of graphite；By the mutual cooperation of guide ring and dispersion impeller, make the graphite for not shearing removing completely is same to remove
Graphene separation, the graphite of shearing removing completely falls on dispersion impeller by guide ring, and high speed by dispersion impeller is revolved
Turn, circulation shear is carried out to the graphite of not shearing removing completely again, graphite is completely exfoliated.Pass through the continuous removing of substep, drop
Low graphite or the pulverized probability of graphene, reduce the fault of construction of graphene, while preventing the graphene removed because again
Secondary grinding leads to fault of construction.
2, graphene number of plies made from graphene process units mechanical stripping is 1 ~ 10 layer through the invention, fault of construction
Few, edge is rounded, and dispersion performance is excellent, and high production efficiency, specific productivity reaches 40 ~ 60%.
3, removing 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, has great cost advantage, and can realize the industrial production of scale；Preparation process
Without using strong acid and strong base or other noxious materials, additive is few, without a large amount of organic solvent, so that preparing graphene more
For environmentally protective, simple process.
Detailed description of the invention
Fig. 1 is the structural schematic diagram 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 schematic diagram of the dispersion impeller of the continuously grinding mechanism in the embodiment of the present invention 1；
In figure: 1, raw material grinding pot；2, abrasive media warehouse；3, stirred tank；4, continuously grinding mechanism；5, storage tank；6,
Centrifugal filter device；7, drying device；11, blade stirrer is ground；12, raw material grinding pot discharge port；21, abrasive media warehouse goes out
Material mouth；The enterprising material mouth of 31 stirred tanks；32, feed inlet under stirred tank；41, high-pressure pump；42, storehouse is ground；43, guide ring；44, disperse
Impeller；45, transmission shaft；411, plunger；412, pump chamber；413, baffling road；414, nozzle；421, storehouse feed inlet is ground；422, it grinds
Grind bin discharge port external；441, leaf dish；442, channel；443, support column；444, through-hole.
Specific embodiment
The present invention is explained in detail below in conjunction with specific embodiment, is not restricted to the present invention.It is not departing from
In the case where above method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change
Into should all be included in the protection scope of the present invention.
Embodiment 1
The present embodiment provides the devices that a kind of slurry continuously grinding prepares graphene.
A kind of device continuously preparing graphene, as shown in Figure 1, successively including raw material grinding pot (1), abrasive media warehouse
(2), stirred tank (3), continuously grinding mechanism (4), storage tank (5), centrifugal filter device (6) and drying device (7).Raw material grinding
Blade stirrer mill (11) is equipped in tank (1), for roughly grinding to graphite raw material；Abrasive media warehouse (2) is for storing
Abrasive media；Raw material grinding pot and abrasive media warehouse bottom are respectively provided with discharge port (12), (21)；Stirred tank (3) is for preparing
Enterprising material mouth (31) and lower feed inlet (32), the discharge port (12) of raw material grinding pot and grinding is arranged in graphite slurry, stirred tank (3)
The discharge port (21) of medium warehouse is connected with the enterprising material mouth of stirred tank (3) respectively, in order to transferring raw material in stock tank and
Abrasive media.Continuously grinding mechanism (4) be used for graphite slurry continuous process shear remove, storage tank (5) for collect and it is quiet
The graphene slurry that continuous shear stress is removed is set, storage tank (5) is connected with one end of centrifugal filter device (6), drying device
(7) it is connected with the other end of centrifugal filter device (6).Centrifugal filter device (6) be used for by the interior upper layer suspension of storage tank (5) into
Row centrifuge separation is filtered, washed, and drying device (7) is for being dried in vacuo filtered graphene.
Continuously grinding mechanism (4) includes high-pressure pump (41), grinding storehouse (42), guide ring (43), dispersion impeller (44) and passes
Moving axis (45).Grind storehouse (42) lower part be equipped with feed inlet (421), middle part be equipped with discharge port (422), high-pressure pump (41) respectively with stir
The lower feed inlet (32) for mixing slot (3), the feed inlet (421) for grinding storehouse (42) are connected, and grind discharge port (422) and the storage of storehouse (42)
Batch can (5)；Guide ring (43) is located in the middle part of grinding storehouse (42) and is fixedly connected with transmission shaft (45), and dispersion impeller (44), which is located at, to be led
It flows between ring (43) and the bottom for grinding storehouse (42), the center that transmission shaft (45) passes through the dispersion impeller (44).Guide ring
(43) periphery is equipped with two spiral helicine blades, and spiral helicine blade can provide upward spiral helicine movement rail for slurry
Mark, when slurry is thrown off guide ring, the direction of motion, which can be, is thrown to guide ring top or any other direction, is facilitated
Increase the collision frequency of slurry and the severity of collision, so as to improve grinding efficiency, reduces circular grinding number.
As shown in Fig. 2, high-pressure pump (41) includes a pair of of plunger (411), each plunger is set in a pump chamber (412),
Every a pair of plunger sprays the liquid material in corresponding two pump chambers simultaneously to grinding storehouse by the nozzle (414) of baffling road (413).
As shown in figure 3, dispersion impeller (44) includes two leaf dishes (441) disposed in parallel, the leaf dish is equipped with 4 and leads to
Road (442), two leaf dishes are fixed by the support column (443) that 4 cross sections are ellipse, and dispersion impeller (44) center is equipped with through-hole
(444).
Embodiment 2
The present embodiment provides a kind of production methods of graphene, for using the preparation facilities of the graphene of embodiment 1
The method produced, method includes the following steps:
(1) graphite raw material is put into raw material grinding pot, the quartz sand and ceramic bead that diameter is 2mm is added, utilizes Jie
Graphite raw material is roughly ground in matter grinding；
(2) the corase grinding graphite raw material in raw material grinding pot is entered in stirred tank by the enterprising material mouth of stirred tank, then
The abrasive media in abrasive media warehouse is added, water is injected from lower feed inlet, the mixing speed that stirred tank is arranged is 500rpm,
Obtain graphite dispersion slurry；Wherein the abrasive media is by weight percentage by as follows at being grouped as: amphiphilic polymers 40%,
Nano modification hydrotalcite 30%, micro-expanding agent 10%, binder 5%, cyclodextrin 10%, urea 5%.
(3) start continuously grinding mechanism, the graphite dispersion slurry in step (2) is sprayed by grinding storehouse by high-pressure pump,
Under the running at high speed of dispersion impeller, dispersed slurry carries out shearing grinding from the inner sidewall that the bottom in grinding storehouse rushes at grinding storehouse, together
When do not shear completely removing graphite can with remove graphene separation, completely shearing removing graphite lead to due to gravity
It crosses and is randomly fallen on the different channels of dispersion impeller by the guide ring of transmission shaft driving rotation, the high speed rotation by dispersion impeller
Turn, circulation shear is carried out to the graphite of not shearing removing completely again, wherein the injection fluid velocity of high-pressure pump is 100m/s, point
The revolving speed for dissipating impeller is 5000rpm, milling time 1min；
(4) grinding product that step (3) obtains is expelled in storage tank from the discharge port in grinding storehouse, is stood for 24 hours；
(5) graphene suspension in storage tank after standing step (4) is delivered in centrifugal filter device, is arranged
Centrifugal rotational speed is 10000 rpm, and centrifugation time 30min takes supernatant liquor, filter cake is obtained by filtration in vacuum apparatus；
(6) filter cake that step (5) obtains is cleaned 2 ~ 3 times with ethyl alcohol, water respectively, dries 4h in a vacuum drying oven, i.e.,
Obtain graphene product.
Resulting graphite ene product is characterized using atomic force electron microscope, learns graphite ene product 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 methods of graphene, for using the preparation facilities of the graphene of embodiment 1
The method produced, method includes the following steps:
(1) graphite raw material is put into raw material grinding pot, the ceramic bead and zirconium pearl that diameter is 5mm is added, utilizes medium
Graphite raw material is roughly ground in grinding；
(2) the corase grinding graphite raw material in raw material grinding pot is entered in stirred tank by the enterprising material mouth of stirred tank, then
The abrasive media in abrasive media warehouse is added, water is injected from lower feed inlet, the mixing speed that stirred tank is arranged is 800rpm,
Obtain graphite dispersion slurry；Wherein the abrasive media is by weight percentage by as follows at being grouped as: amphiphilic polymers 30%,
Nano modification hydrotalcite 30%, micro-expanding agent 10%, binder 10%, cyclodextrin 10%, urea 10%.
(3) start continuously grinding mechanism, the graphite dispersion slurry in step (2) is sprayed by grinding storehouse by high-pressure pump,
Under the running at high speed of dispersion impeller, dispersed slurry carries out shearing grinding from the inner sidewall that the bottom in grinding storehouse rushes at grinding storehouse, together
When do not shear completely removing graphite can with remove graphene separation, completely shearing removing graphite lead to due to gravity
It crosses and is randomly fallen on the different channels of dispersion impeller by the guide ring of transmission shaft driving rotation, the high speed rotation by dispersion impeller
Turn, circulation shear is carried out to the graphite of not shearing removing completely again, wherein the injection fluid velocity of high-pressure pump is 150m/s, point
The revolving speed for dissipating impeller is 3000rpm, milling time 5min；
(4) grinding product that step (3) obtains is expelled in storage tank from the discharge port in grinding storehouse, stands 12h；
(5) graphene suspension in storage tank after standing step (4) is delivered in centrifugal filter device, is arranged
Centrifugal rotational speed is 5000 rpm, and centrifugation time 20min takes supernatant liquor, filter cake is obtained by filtration in vacuum apparatus；
(6) filter cake that step (5) obtains is cleaned 2 ~ 3 times with ethyl alcohol, water respectively, dries 2h in a vacuum drying oven, i.e.,
Obtain graphene product.
Resulting graphite ene product is characterized using atomic force electron microscope, learns graphite ene product 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 (4)
1. a kind of device for continuously preparing graphene, it is characterised in that including raw material grinding pot (1), abrasive media warehouse (2), stir
Mix slot (3), continuously grinding mechanism (4), storage tank (5), centrifugal filter device (6) and drying device (7)；Wherein the raw material is ground
Blade stirrer mill (11) is equipped in grinding jar (1)；Raw material grinding pot and abrasive media warehouse bottom be respectively provided with discharge port (12),
(21), enterprising material mouth (31) and lower feed inlet (32), the discharge port (12) and abrasive media of raw material grinding pot is arranged in stirred tank (3)
The discharge port (21) of warehouse is connected with the enterprising material mouth (31) of stirred tank (3) respectively, in order to transferring raw material in stock tank and
Abrasive media；Continuously grinding mechanism (4) includes high-pressure pump (41), grinding storehouse (42), guide ring (43), dispersion impeller (44) and passes
Moving axis (45)；The grinding storehouse (42) lower part is equipped with feed inlet (421), middle part is equipped with discharge port (422), the high-pressure pump (41)
It is connected respectively with the feed inlet (421) of the lower feed inlet (32) of stirred tank (3), grinding storehouse (42), grinds the discharge port of storehouse (42)
(422) with storage tank (5)；The guide ring (43) is located in the middle part of grinding storehouse (42) and is fixedly connected with transmission shaft (45), described
Dispersion impeller (44) is located between the guide ring (43) and the bottom of grinding storehouse (42), and the transmission shaft (45) passes through institute
State the center of dispersion impeller (44)；The storage tank (5) is connected with one end of centrifugal filter device (6), drying device (7) with from
The other end of heart filter device (6) is connected；
The high-pressure pump (41) includes at least a pair of of plunger (411), each plunger is set in a pump chamber (412), each
Plunger is sprayed the liquid material in corresponding two pump chambers simultaneously to grinding storehouse by the nozzle (414) of baffling road (413)；Institute
Guide ring (43) periphery stated is equipped with two spiral helicine blades；The dispersion impeller (44) includes two leaves disposed in parallel
Disk (441), the leaf dish are equipped with plurality of passages (442), the branch that every two leaf dish is round or oval by multiple cross sections
Dagger (443) is fixed, and dispersion impeller (44) center is equipped with through-hole (444)；
It is as follows using the production method for continuously preparing graphene device:
(1) graphite raw material is put into raw material grinding pot, is roughly ground graphite raw material using medium milling；
(2) the corase grinding graphite raw material in raw material grinding pot is entered in stirred tank by the enterprising material mouth of stirred tank, is then added
Abrasive media in abrasive media warehouse injects water from lower feed inlet, and the mixing speed that stirred tank is arranged is 100 ~ 800rpm,
Obtain graphite dispersion slurry；
(3) start continuously grinding mechanism, the graphite dispersion slurry in step (2) is sprayed by grinding storehouse by high-pressure pump, is being dispersed
Under the running at high speed of impeller, dispersed slurry carries out shearing grinding from the inner sidewall that the bottom in grinding storehouse rushes at grinding storehouse, while not
Completely shearing removing graphite can with remove graphene separation, completely shearing removing graphite due to gravity by by
The guide ring of transmission shaft driving rotation is randomly fallen on the different channels of dispersion impeller, by the high speed rotation of dispersion impeller,
Circulation shear is carried out to the graphite of not shearing removing completely again, wherein the injection fluid velocity of high-pressure pump is 100 ~ 150m/s,
The revolving speed of dispersion impeller is 1000 ~ 5000rpm, and milling time is 1 ~ 10min；
(4) grinding product that step (3) obtains is expelled in storage tank from the discharge port in grinding storehouse, standing 12 ~ for 24 hours；
(5) graphene suspension in storage tank after standing step (4) is delivered in centrifugal filter device, and setting centrifugation turns
Speed is 5000 ~ 10000rpm, and 10 ~ 30min of centrifugation time takes supernatant liquor, filter cake is obtained by filtration in vacuum apparatus；
(6) filter cake that step (5) obtains is cleaned 2 ~ 3 times with ethyl alcohol, water respectively, dry in a vacuum drying oven 2 ~ 4h to get
Graphene product.
2. a kind of device for continuously preparing graphene according to claim 1, it is characterised in that the blade stirrer
It grinds at least two mill of setting in (11) to be situated between, the diameter that the mill is situated between is 0.1~10mm.
3. a kind of device for continuously preparing graphene according to claim 1, it is characterised in that as described in step (1) to grind
Grinding media is that diameter is 0.1~10mm quartz sand, bead, ceramic bead, at least two mixtures in zirconium pearl.
4. a kind of device for continuously preparing graphene according to claim 1, it is characterised in that step is ground described in (2)
Grinding media is by weight percentage by as follows at being grouped as: amphiphilic polymers 30 ~ 45%, nano modification hydrotalcite 25 ~ 30%, micro- swollen
Swollen dose 10 ~ 15%, binder 5~15%, cyclodextrin 5 ~ 10%, urea 5 ~ 10%.
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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 |
| CN107311162B (en) * | 2017-06-30 | 2019-10-22 | 上海地霸电子科技有限公司 | A kind of continuous production graphene device |
| CN107601480B (en) * | 2017-10-20 | 2023-07-25 | 南通富莱克流体装备有限公司 | Graphene production equipment |
| TWI692441B (en) * | 2018-01-17 | 2020-05-01 | 中原大學 | Graphene structure, method of producing graphene and electrode of lithium-ion made of the same |
| CN108394891A (en) * | 2018-06-05 | 2018-08-14 | 陆挚译 | A kind of graphene preparation system |
| 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 |
| 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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| CN101230205B (en) * | 2008-01-07 | 2010-06-02 | 徐州开达精细化工有限公司 | Super-fine smashing method for reduction dye |
| CN203494580U (en) * | 2013-08-30 | 2014-03-26 | 无锡新光粉体科技有限公司 | Medium stirring type wet method grinding and dispersing device |
| CN104722367B (en) * | 2013-12-20 | 2017-07-07 | 无锡新光粉体科技有限公司 | A kind of medium stirred type wet grinding dispersal device |
| CN104445158B (en) * | 2014-10-23 | 2016-05-04 | 江阴碳谷科技有限公司 | Graphene stripping off device, Graphene production system and the method for producing Graphene |
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| CN105540575A (en) * | 2016-01-28 | 2016-05-04 | 成都新柯力化工科技有限公司 | Method for preparing graphene by using high-pressure homogenizer delamination |
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