CN109502576A - The sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed and preparation method - Google Patents
The sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed and preparation method Download PDFInfo
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- CN109502576A CN109502576A CN201910013426.3A CN201910013426A CN109502576A CN 109502576 A CN109502576 A CN 109502576A CN 201910013426 A CN201910013426 A CN 201910013426A CN 109502576 A CN109502576 A CN 109502576A
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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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
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The present invention relates to a kind of sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed and preparation methods, it realizes the dustlessization pretreatment of raw material by powder suction-type pre-mixing apparatus;Using the stripping off device of sealed helical flow Field Design, fluid power (laminar flow, the turbulent flow, hole) effect generated using ultrahigh speed rotation, the material moved in stripping off device by helical flow field is acted on, so that the Van der Waals force between destroying graphite flake layer, realizes the removing of graphene nanometer sheet;Again by sedimentation device and centrifugal separation device, the graphene nanometer sheet of different-thickness and size is obtained.The relevant technologies and device breach the technical bottleneck in current graphene high quality and low cost preparation field.Low pollution can be achieved, high quality, more specifications, customize production, there is technical advantage outstanding and vitality.
Description
Technical field
The present invention relates to a kind of grapheme material technology of preparing and device, specifically a kind of sealed helical flow field of ultrahigh speed
Graphene nanometer sheet preparation facilities and preparation method.
Background technique
Graphene is a kind of new carbon, is to be currently known a kind of most thin material, the thickness of only one carbon atom;
With up to 2630m2The theoretical specific surface area of/g;Excellent mechanical strength, such as the up to stretch modulus of 1TPa and 130GPa
Breaking strength is the presently found material with highest mechanical strength;Fabulous electric conductivity, conductivity are up to 106S/m,
It is the optimal material of electric conductivity found so far;Excellent heating conduction, thermal conductivity are up to 5000W/mK, and so far
The highest material of thermal conductivity until the present.In addition, it is nearly transparent, 2.3% light is only absorbed, and there is electron energy band, physics/change
It learns property and is easy to the features such as regulating and controlling.Although current graphene Related product industry size and industrial output value are smaller than escheat, make
For the international forward position new material that a kind of technology content is very high, application potential is very wide, to semiconductor industry, photovoltaic industry, storage
The traditional fields such as energy technology, aerospace, military project, display of new generation and emerging field will generate revolutionary influence, graphene
Industry upsurge is flourishing, and research and development of products enters the rapid expanding phase, and associated product category is also increasingly various.
Although graphene preparation method has mechanical stripping method, epitaxial growth method, chemical vapour deposition technique (CVD method), chemistry
Oxidation-reduction method, organic synthesis method, ultrasonic dispersion, carbon nanotube patterning method, solvent-thermal method, plasma enhanced process, flame method,
All multi-methods such as arc discharge method, but green non-pollution, high-quality, industrialization production ability are strong, and customizable, more specifications are raw
The technology of preparing of production is still urgently broken through.
Summary of the invention
In order to solve the technical problems in background technology, it is fixed to provide a kind of low pollution, high quality, more specifications by the present invention
The sealed helical flow field graphene nanometer sheet preparation facilities of the ultrahigh speed of inhibition and generation industrialization production and preparation method.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed, device by batching kettle, solvent feed pipe,
Graphite pulvis feed pipe, the pre-dispersed machine of suction-type, the sealed helical flow field dispersion machine of ultrahigh speed, sedimentation kettle, vertical separating machine and
Finished product kettle composition;
Mixed material is sent into wherein by the sealed helical flow field dispersion machine of ultrahigh speed by batching kettle, is connected on batching kettle
Solvent feed pipe and graphite pulvis feed pipe, the pre-dispersed machine of suction-type that wherein graphite powder passes through connection graphite pulvis feed pipe
It is entered back into batching kettle after dispersion;
Graphene nanometer sheet mix products after removing dispersion are passed through sedimentation by the sealed helical flow field dispersion machine of ultrahigh speed
Carry out natural subsidence in kettle, sedimentation kettle separates graphene nanometer sheet and liquid using vertical separating machine, vertical separating machine with
Finished product kettle is connected, and separating obtained graphene nanometer sheet is passed through in finished product kettle;
Wherein, the sealed helical flow field dispersion machine of the ultrahigh speed includes equipment base, and equipment base inner is equipped with superelevation
Chamber is removed in the sealed helical flow field of speed, and the sealed helical flow field removing chamber of ultrahigh speed is driven by high speed gear, institute
The feed inlet for stating the sealed helical flow field removing chamber of ultrahigh speed is connected with charging pumping plant, the sealed helical flow field stripping of ultrahigh speed
Discharge port from chamber is connected with discharging pumping plant, in addition, the sealed helical flow field removing chamber outer layer of ultrahigh speed has cooling system to be formed
Pressure cooling layer, internal layer has surface to have the high speed rotor of through-hole and shelled by high speed rotor and the sealed helical flow field of ultrahigh speed
From the aquashear layer formed between chamber.
The preparation method of the sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed:
The method refers to the removing chamber that material is passed through to the sealed helical flow field dispersion machine of ultrahigh speed, when material is by removing
When feed inlet enters below chamber, top discharge port flows out, high speed rotor ultrahigh speed will be formed material from bottom to top when rotating
Helical flow field, and the aquashear layer formed between rotor and removing chamber, and then material shape stratified flow is imitated respectively in shear layer
Should under shearing and stretching, turbulence effect under pressure wave deformation, the temporary impact wave that is formed of the bubble breaking under void effect,
The Van der Waals force of graphite between layers is destroyed, realizes the physics removing of graphite between layers.Unstripped material passes through high speed
Rotor through-hole constantly enters shear layer and is removed.The heat that stripping process generates is led by the cooling layer outside removing chamber
Out.
The material is to carry out mixing in batching kettle by graphite powder and solvent to form, wherein graphite powder expects pipe passes through
It is entered back into batching kettle after inhaling the pre-dispersed machine dispersion of powder, solvent is passed through in batching kettle by solvent pipe.
The graphene material for completing dispersion is passed through in sedimentation kettle and settles by the sealed helical flow field dispersion machine of ultrahigh speed,
Graphene material after sedimentation, which is passed through again in vertical separating machine, carries out separating dry space from moist space, final graphene be passed through in finished product kettle complete it is whole
A ingredient, dispersion and the process of collection.
The high speed rotor ultrahigh speed rotation refers to the linear velocity for realizing that rotor 60 arrives 200m/s.
The method can respectively by adjusting in graphite pulvis feed pipe graphite pulvis specification (- 10000 mesh of 10 mesh),
The linear velocity (60m/s -200m/s) of the sealed helical flow field dispersion machine of ultrahigh speed, the sedimentation time (0.1h -100h) for settling kettle,
The revolving speed (200rpm -20000rpm) of vertical separating machine and time (0.5min -60min), to obtain different-thickness and size
Graphene nanometer sheet product.
Beneficial effects of the present invention:
The sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed and preparation method have developed a set of unique, steady
Fixed, complete graphene slurry scale manufacturing technique process and technical equipment, it using mechanical stripping method come to graphene into
Row dispersion, dispersion process material consumption energy consumption is lower, and pollution-free, the ultrahigh speed sealing in the sealed helical flow field dispersion machine of ultrahigh speed
Formula helical flow field removes chamber and uses sealed helical flow Field Design, and the rotor of intermediate high speed rotor layer is not less than the linear speed of 60m/s
Degree, the fluid power effect generated using high speed rotation are destroyed the Van der Waals force of graphite between layers, realize graphite between layers
Physics removing;Again by sedimentation device and centrifugal separation device, the graphene nanometer sheet of different-thickness and size is obtained.It is related
Technology and device breach the technical bottleneck in current graphene high quality and low cost preparation field.Low pollution, high-quality can be achieved
Amount, customizes production at more specifications, has technical advantage outstanding and vitality.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the structural schematic diagram of the sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed of the present invention.
Fig. 2 is that the knot of chamber is removed in the sealed helical flow field of ultrahigh speed in the sealed helical flow field dispersion machine of ultrahigh speed in Fig. 1
Structure schematic diagram.
Fig. 3 is the appearance schematic diagram of Fig. 2 high speed rotor layer.
Fig. 4 is the enlarged drawing of Fig. 3 high speed rotor layer.
Fig. 5 is that the layer of chamber is removed in the sealed helical flow field of ultrahigh speed in the sealed helical flow field dispersion machine of ultrahigh speed in Fig. 2
Shape structural schematic diagram.
The enlarged drawing of the through hole between Fig. 5 high speed rotor layer and aquashear layer Fig. 6.
Fig. 7 is entire preparation system locating for the sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed of the present invention
In schematic diagram.
Fig. 8 is the scanning electron microscope phenogram for the product that embodiment 1 is obtained using preparation facilities of the present invention.
Fig. 9 is the scanning electron microscope phenogram for the product that embodiment 2 is obtained using preparation facilities of the present invention.
Figure 10 is the scanning electron microscope phenogram for the product that embodiment 3 is obtained using preparation facilities of the present invention.
In figure: batching kettle 1, graphite powder expects pipe 3, inhales the pre-dispersed machine 4 of powder, the sealed helical flow field of ultrahigh speed point at solvent pipe 2
It dissipates the sealed helical flow field removing chamber 5.2 of machine 5, equipment base 5.1, ultrahigh speed, force cooling layer 5.2.1, high speed rotor layer
5.2.2, aquashear layer 5.2.3, high speed gear 5.3, charging pumping plant 5.4, discharging pumping plant 5.5, cooling system 5.6, sedimentation
Kettle 6, vertical separating machine 7, finished product kettle 8.
Specific embodiment
Below in conjunction with attached drawing, the present invention is described in further detail.
Referring to Fig. 1 to Figure 10, the present invention relates to a kind of sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed
And preparation method, it includes the sealed helical flow field dispersion machine 5 of ultrahigh speed, the sealed helical flow field dispersion machine 5 of ultrahigh speed
It is equipped with the sealed helical flow field of ultrahigh speed including equipment base 5.1, inside equipment base 5.1 and removes chamber 5.2, the ultrahigh speed is close
Envelope formula helical flow field removing chamber 5.2 is driven by high speed gear 5.3, so that high-speed rotation is carried out, 5.3 energy of high speed gear
Enough drive realizes that rotor 20 arrives 200m/s using the sealed helical flow field removing chamber 5.2 of ultrahigh speed of sealed helical flow Field Design
Linear velocity, to reach ultrahigh speed, the feed inlet and charging pumping plant of the sealed helical flow field removing chamber 5.2 of ultrahigh speed
5.4 are connected, and the discharge port of the sealed helical flow field removing chamber 5.2 of ultrahigh speed is connected with discharging pumping plant 5.5, and ultrahigh speed
Be additionally provided with cooling system 5.6 between the discharge port and discharging pumping plant 5.5 of sealed helical flow field removing chamber 5.2, for point
Material after dissipating carries out cooling down.
Furthermore the sealed helical flow field removing chamber 5.2 of ultrahigh speed has three-decker, respectively pressure cooling layer from outside to inside
5.2.1, high speed rotor layer 5.2.2 and aquashear layer 5.2.3, wherein the aquashear layer 5.2.3 of innermost layer is equivalent to one
The feed inlet of the blade of annular, the sealed helical flow field removing chamber 5.2 of ultrahigh speed is connected to cooling layer 5.2.1 is forced, ultrahigh speed
The discharge port and aquashear layer 5.2.3 intermediate connection of sealed helical flow field removing chamber 5.2, and high speed rotor layer 5.2.2
Through-hole is offered on wall between aquashear layer 5.2.3, the through-hole is for allowing the solution of containing graphene to pass through, to material
It sheared, elongated, stirred.
The sealed helical flow field removing chamber of ultrahigh speed uses sealed helical flow Field Design, the rotor of intermediate high speed rotor layer
Linear velocity not less than 60m/s, material are constantly passed through the aquashear layer of ultrahigh speed sealed helical flow field removing chamber, and from
It is pierced by through-hole between aquashear layer and high speed rotor layer, when by the through-hole, utilizes the fluid power of high speed rotation generation
Laminar flow effect: (laminar flow, turbulent flow, hole) effect causes the shearing and elongation of material;Turbulence effect: under the action of pressure wave
Cause the arbitrary deformation of material;Void effect: bubble moment is broken, generates shock wave, to generate vigorous agitation, destroys graphite
About 2eV/nm between layers2Van der Waals force, realize graphite between layers physics removing, the stone being finally stripped out
Black alkene is adhered on the shell of the pressure cooling layer of ultrahigh speed sealed helical flow field removing chamber, is cooled down, thus facilitate by
It is stripped down.It uses green non-pollution simultaneously and recyclable solvent, is regulated and controled by special ratios, it is steady to obtain graphene
Surely surface tension (40~the 50mJm dispersed-2), the final high efficiency dispersion for realizing graphene, material consumption and energy consumption are lower, and
It is pollution-free.
Mixed material is sent into wherein, on batching kettle 1 by the sealed helical flow field dispersion machine 5 of ultrahigh speed by batching kettle 1
It is connected with solvent pipe 2 and graphite powder expects pipe 3, wherein graphite powder expects pipe 3 is by entering back into batching kettle 1 after inhaling the pre-dispersed dispersion of machine 4 of powder
In, the graphene nanometer sheet mix products after removing dispersion are passed through in sedimentation kettle 6 by the sealed helical flow field dispersion machine 5 of ultrahigh speed
Carry out natural subsidence, sedimentation kettle 6 separates graphene nanometer sheet and liquid using vertical separating machine 7, vertical separating machine 7 and at
Product kettle 8 is connected, and separating obtained graphene nanometer sheet is passed through in finished product kettle 8.
By adjusting the graphite pulvis specification (- 10000 mesh of 10 mesh) in graphite pulvis feed pipe 3, the sealed spiral shell of ultrahigh speed
The linear velocity (20m/s -200m/s) of line flow field dispersion machine 5, the sedimentation time (0.1h -100h) for settling kettle 6, vertical separating machine 7
Revolving speed (200rpm -20000rpm) and time (0.5min -60min), to obtain the graphene nano of different-thickness and size
Piece product.
The side of graphene nanometer sheet is prepared according to the sealed helical flow field graphene nanometer sheet preparation facilities of the ultrahigh speed
Method, working principle are as follows:
Graphene raw material and solvent are each led into graphite powder expects pipe and solvent pipe, graphite powder expects pipe is divided in advance by inhaling powder
Entered back into batching kettle 1 after dissipating machine dispersion, solvent is passed directly into batching kettle 1 by solvent pipe, batching kettle 1 to graphene material and
Solvent carries out mixing, and mixed material is passed through in the sealed helical flow field dispersion machine of ultrahigh speed, and material is sealed from ultrahigh speed
The feed inlet of helical flow field removing chamber, which enters, to be forced to be cooled down in cooling layer, and subsequent high speed rotor layer is generated using high speed rotation
Fluid power, the through-hole that material opens up on the wall between high speed rotor layer and aquashear layer is passed through in aquashear layer, object
When material high speed rotation passes through through-hole, cause the shearing and elongation of material, and cause the random of material under the action of pressure wave
Deformation, bubble moment is broken, generates shock wave and disperses to generate vigorous agitation to material, the sealed helical of ultrahigh speed
The graphene material for completing dispersion is passed through in sedimentation kettle and settles by flow field dispersion machine, and the graphene material after sedimentation is passed through again
Separating dry space from moist space is carried out in vertical separating machine, final graphene, which is passed through in finished product kettle, completes entire ingredient, dispersion and the process of collection.
Using above-mentioned preparation facilities and preparation method, following specific embodiments can be used:
Embodiment 1
The crystalline flake graphite of 1000g, 10 mesh is passed through by graphite pulvis feed pipe 3 and the pre-dispersed machine 4 of suction-type by matching
Material kettle 1, while the water of 1000ml also enters batching kettle 1 by solvent feed pipe 2, material futher stirs dispersion in batching kettle 1
Uniformly;
The sealed helical flow field dispersion machine 5 of ultrahigh speed is opened, after so that the ultrahigh speed rotor linear velocity in it is reached 60m/s,
Material will have been stirred evenly in batching kettle 1, and removing chamber, removing 10min are entered by the lower section feed inlet of dispersion machine 5;
After the completion of material removing, material is entered into the natural standing sedimentation of sedimentation kettle 6 by the discharge port above removing chamber
The material for completing sedimentation is transferred to the centrifuge separation that vertical separating machine 7 carries out 200rpm, 60min by 0.1h;
After the completion of centrifugation, supernatant is recycled, will centrifugation products therefrom be transferred to finished product kettle 8 stored, packed for standby use.
The graphene nano sheet product that products therefrom is 5 μm or so of piece diameter size, is specifically shown in its scanning electron microscope
Characterization result Fig. 8.
Embodiment 2
5000 mesh, solvent is selected to be changed to N methyl pyrrolidone, ultrahigh speed rotor by water the crystalline flake graphite in embodiment 1
Linear velocity reaches 100m/s, splitting time 1h, natural standing sedimentation 50h, the centrifuge separation for carrying out 10000rpm, 30min;Its
It is same as Example 1.
The graphene nano sheet product that products therefrom is 3 μm or so of piece diameter size, is specifically shown in its scanning electron microscope
Characterization result Fig. 9.
Embodiment 3
Crystalline flake graphite in embodiment 1 selected to 10000 mesh, solvent by water are changed to acetone, ultrahigh speed rotor linear velocity reaches
To 200m/s, splitting time 2h, natural standing sedimentation 100h, the centrifuge separation for carrying out 20000rpm, 0.5min;It is other with it is real
It is identical to apply example 1.
The graphene nano sheet product that products therefrom is 1 μm or so of piece diameter size, is specifically shown in its scanning electron microscope
Characterization result Figure 10.
Above-mentioned desirable embodiment according to the present invention is enlightenment, and through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention'.This invention it is technical
Range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (5)
1. a kind of sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed, it is characterised in that: described device is by ingredient
Kettle (1), solvent feed pipe (2), graphite pulvis feed pipe (3), the pre-dispersed machine of suction-type (4), the sealed helical flow field of ultrahigh speed
Dispersion machine (5), sedimentation kettle (6), vertical separating machine (7) and finished product kettle (8) composition;
Mixed material is sent into wherein by the sealed helical flow field dispersion machine (5) of ultrahigh speed by batching kettle (1), batching kettle (1)
On be connected with solvent feed pipe (2) and graphite pulvis feed pipe (3), wherein graphite powder by connection graphite pulvis feed pipe (3)
The pre-dispersed machine of suction-type (4) dispersion after enter back into batching kettle (1);
Graphene nanometer sheet mix products after removing dispersion are passed through sedimentation kettle by the sealed helical flow field dispersion machine (5) of ultrahigh speed
(6) natural subsidence is carried out in, sedimentation kettle (6) separates graphene nanometer sheet and liquid using vertical separating machine (7), and vertical point
Disembark (7) be connected with finished product kettle (8), separating obtained graphene nanometer sheet is passed through in finished product kettle (8);
Wherein, the sealed helical flow field dispersion machine (5) of the ultrahigh speed includes equipment base (5.1), and equipment base (5.1) is internal
Equipped with sealed helical flow field removing chamber (5.2) of ultrahigh speed, sealed helical flow field removing chamber (5.2) of ultrahigh speed passes through height
Fast transmission case (5.3) drives, the feed inlet and charging pumping plant of sealed helical flow field removing chamber (5.2) of ultrahigh speed
(5.4) it is connected, the discharge port of sealed helical flow field removing chamber (5.2) of ultrahigh speed is connected with discharging pumping plant (5.5), this
Outside, the pressure cooling layer (5.2.1) that sealed helical flow field removing chamber (5.2) outer layer of ultrahigh speed has cooling system to be formed, internal layer
There is surface to have the high speed rotor (5.2.2) of through-hole and removed by high speed rotor (5.2.2) and the sealed helical flow field of ultrahigh speed
The aquashear layer (5.2.3) formed between chamber (5.2).
2. the preparation method of the sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed according to claim 1,
It is characterized by: the method refers to the removing chamber that material is passed through to the sealed helical flow field dispersion machine of ultrahigh speed, when material by
When removing feed inlet entrance below chamber, the outflow of top discharge port, high speed rotor ultrahigh speed will be to material from bottom to top when rotating
The aquashear layer for forming helical flow field, and being formed between rotor and removing chamber, and then in shear layer respectively to material forming layer
Flow the pressure wave deformation under the shearing and stretching, turbulence effect under effect, the instantaneous punching that the bubble breaking under void effect is formed
Wave is hit, the Van der Waals force of graphite between layers is destroyed, realizes the physics removing of graphite between layers.Unstripped material passes through
High speed rotor through-hole constantly enters shear layer and is removed, and the heat that stripping process generates passes through the cooling layer conduction outside removing chamber
The graphene material for completing dispersion is passed through in sedimentation kettle and settles, sinks by export, the sealed helical flow field dispersion machine of ultrahigh speed
Graphene material after drop, which is passed through again in vertical separating machine, carries out separating dry space from moist space, and final graphene is passed through in finished product kettle and completes entirely
Ingredient, dispersion and the process of collection.
3. the preparation method of the sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed according to claim 2,
It is characterized by: the material is to carry out mixing in batching kettle by graphite powder and solvent to form, wherein graphite powder expects pipe is logical
It is entered back into batching kettle after crossing the pre-dispersed machine dispersion of suction powder, solvent is passed through in batching kettle by solvent pipe.
4. the preparation method of the sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed according to claim 2,
It is characterized by: the high speed rotor ultrahigh speed rotation refers to the linear velocity for realizing that rotor 60 arrives 200m/s.
5. the preparation method of the sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed according to claim 2,
It is characterized by: the method can be respectively by adjusting graphite pulvis specification (10 mesh-in graphite pulvis feed pipe (3)
10000 mesh), the linear velocity (60m/s -200m/s) of the sealed helical flow field dispersion machine (5) of ultrahigh speed, the sedimentation for settling kettle (6)
Time (0.1h -100h), vertical separating machine (7) revolving speed (200rpm -20000rpm) and time (0.5min -60min), to obtain
Obtain the graphene nanometer sheet product of different-thickness and size.
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