KR101807373B1 - Graphene crushing and centrifugation apparatus - Google Patents
Graphene crushing and centrifugation apparatus Download PDFInfo
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- KR101807373B1 KR101807373B1 KR1020150189803A KR20150189803A KR101807373B1 KR 101807373 B1 KR101807373 B1 KR 101807373B1 KR 1020150189803 A KR1020150189803 A KR 1020150189803A KR 20150189803 A KR20150189803 A KR 20150189803A KR 101807373 B1 KR101807373 B1 KR 101807373B1
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1806—Stationary reactors having moving elements inside resulting in a turbulent flow of the reactants, such as in centrifugal-type reactors, or having a high Reynolds-number
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Abstract
The present invention relates to a graphene separation centrifugal separator, and more particularly, to a graphene separation centrifugal separator which comprises: a graphite particle agitator supplied with a graphite mixture liquid from a graphite agitator; A graphite feed port through which the graphite mixture liquid is fed from the graphite particle agitator; a graphene outlet through which a graphene mixture liquid in which graphite mixed with the graphite mixture liquid is pulverized into fine particles of a reference size is discharged; A centrifugal casing having a high pressure jet port for discharging the mixed graphite particle mixture; A graphite supply pipe connected to the graphite supply port and supplying the graphite mixture into the centrifuge casing; A rotation driving part inserted into the centrifuge casing and having a driving shaft for rotating the centrifuge casing at a high speed; A warming portion coupled to an outer periphery of the driving shaft and rotating together with the driving shaft to separate graphite mixed in the graphite mixed solution flowing through the graphite supply pipe; An impact peeling plate disposed in the high pressure jet port and causing the graphite particles discharged at a high speed through the high pressure jet port to collide and peel off; A graphite particle flow space in which the mixture of graphite particles discharged from the high pressure discharge port flows and a graphene flow space discharged from the graphen discharge port are formed so as to be separated from each other, A housing having a graphene discharge hole for discharging the graphene of the flow space to the outside; And a recirculation pipe extending from the lower portion of the housing to communicate with the graphite particle flow space and re-supplying the graphite particle mixture to the graphite particle agitator.
Description
BACKGROUND OF THE
Graphene is a material in which the carbon atoms of graphite, which is a natural three dimensional carbon isotope in nature, are arranged in a form having a hexagonal planar structure in the form of a two dimensional sheet. The carbon atom of graphene forms a sp 2 bond and forms a flat sheet of single atom thickness.
Graphene has very good electrical conductivity and thermal conductivity, and the physical properties such as quantum transparency and high specific surface area according to its excellent mechanical strength, flexibility, stretchability and thickness are explained by the unique bonding structure of the atoms present therein . Three out of four outermost electrons constituting graphene form a sp 2 hybrid orbital to form a sigma bond, and one of the remaining electrons forms a pi bond with surrounding carbon atoms to form a hexagonal two-dimensional structure. Therefore, graphene has a different band structure from other carbon isotopes, and exhibits excellent electric conductivity because of its absence of band gap. However, it has a semi-metallic material whose electron density is zero at the Fermi level. It is possible.
As a result, it can be applied to a wide variety of electric and electronic fields such as next-generation materials, capacitors, electromagnetic shielding materials, sensors, and displays that can replace silicon electronic and electrical materials, as well as automotive, energy, aerospace, architecture, medicine, and steel There are many studies to utilize this in various fields.
Examples of the method for producing such graphene include a method of peeling a graphene layer from a graphite sheet using an adhesive tape (a Scotch-tape method or a Peel off method), a chemical vapor deposition method, a silicon carbide substrate (SiC) (Epitaxial growth method), a method of peeling graphite using heat (thermalexfoliation), a chemical oxidation and reduction method and the like have been studied.
Among them, the chemical redox method is advantageous in that various functional groups can be easily introduced into the sheet, but it is difficult to mass-produce it and it is not economical. In this method, strong acid and deoxidation reaction Hydrazine and the like. Most of these reducing agents have a high risk of corrosivity, explosiveness, and toxicity to human body, and the generated graphene may contain impurities and the like.
In addition, this method requires filtration and redispersion of the order of 6 to 7 to wash off strong acid and reducing agent present on the graphene surface. In the filtration and redispersion process, the surface of the graphene is polarized so that the graphene is peeled off again and returns to the graphite. Thus, there is a disadvantage that most of the characteristics of the graphene are lost.
Accordingly, there is a new need for a method for manufacturing graphene which is more economical, more efficient, and less dangerous, while having excellent physical properties such as electrical conductivity.
Disclosure of the Invention An object of the present invention is to solve the above-mentioned problems, and it is an object of the present invention to provide a method of separating graphite from a graphite mixture dispersed in water or various media repeatedly and separating graphene grains of less than nano- And a centrifugal separator.
The above objects and various advantages of the present invention will become more apparent from the preferred embodiments of the present invention by those skilled in the art.
The object of the present invention can be achieved by a graphene separation centrifugal apparatus. The graphene separation centrifugal separator of the present invention comprises: a graphite particle agitator supplied with a graphite mixture liquid from a graphite agitator; A graphite feed port through which the graphite mixture liquid is fed from the graphite particle agitator; a graphene outlet through which a graphene mixture liquid in which graphite mixed with the graphite mixture liquid is pulverized into fine particles of a reference size is discharged; A centrifugal casing having a high pressure discharge port through which the mixed graphite particle mixture liquid is discharged; A graphite supply pipe connected to the graphite supply port and supplying the graphite mixture into the centrifuge casing; A rotation driving part inserted into the centrifuge casing and having a driving shaft for rotating the centrifuge casing at a high speed; A warming portion coupled to the outer periphery of the driving shaft and rotating together with the driving shaft to peel off the graphite mixed in the graphite mixed solution flowing through the graphite supply pipe; An impact peeling plate disposed in the high pressure jet port and causing the graphite particles discharged at a high speed through the high pressure jet port to collide and peel off; A graphite particle flow space in which the mixture of graphite particles discharged from the high pressure discharge port flows and a graphene flow space in which the graphene mixture discharged from the graphen discharge port flows are formed in the centrifugal casing rotatably inside A housing having a graphene discharge hole for discharging the graphene mixed solution in the graphene flow space to the outside; And a recirculation pipe extending from the lower portion of the housing to communicate with the graphite particle flow space and re-supplying the graphite particle mixture to the graphite particle agitator.
According to an embodiment of the present invention, the graphene smaller than the reference size is moved to the graphen outlet by the influence of the drag due to the rotational force generated by the driving of the rotation driving portion, and the graphite particles larger than the reference size are centrifugal force or piston And can be discharged to the high-pressure discharge port by the reciprocating movement pressure.
According to one embodiment, the graphite supply port is formed through one side of the centrifugal casing, and the graphen discharge port is formed in a ring shape along the outer peripheral surface of the other side of the centrifugal casing facing the graphite supply port And the high-pressure jet port may be formed on a side surface of the centrifugal casing.
According to one embodiment, the warm-up section includes a rotor coupled to the drive shaft, and a plurality of rotary plates coupled to the rotor at regular intervals in the radial direction. The inner wall surface of the centrifugal casing protrudes from the plate surface And a movement stopping protrusion for forming a graphene flow gap corresponding to the reference size between the lower end edge of the rotating plate and the lower end edge of the rotating plate.
According to one embodiment, the impact peeling plate is formed of a cemented carbide, and may be disposed at an angle to the ejecting direction of the graphite particles of the high-pressure jet port at an angle.
The graphene separation centrifugal separator according to the present invention separates the graphite mixture mixed with the graphite by rotating in the centrifugal casing and peeling the graphene mixture once again with a strong impact on the collision separation plate formed in the high- do. Then, graphene peeled to a size smaller than the reference size can be centrifuged and discharged to the outside.
That is, peeling of graphite and separation of graphene can be performed in one apparatus.
In addition, the graphene separation centrifugal separator according to the present invention can infinitely increase the injection speed at which the graphite particles are injected into the high-pressure ejection port beyond supersonic speed, and the structure is simple.
In addition, only a very small amount of interfacial activator for holding graphite particles and a very small amount of agent for adjusting pH are put into operation, so that graphene peeled off due to washing and filtration due to the use of strong acid and reducing agent, It is possible to prevent the problem from being discarded. As a result, there is an advantage that the separated graphene is not polarized and the purity is high.
1 is a perspective view showing an external configuration of a graphene separation centrifugal separator according to the present invention,
FIG. 2 is an exploded perspective view showing the structure of the warm section of the graphene separation centrifugal separator according to the present invention,
3 is a cross-sectional view showing a cross-sectional configuration of a graphene separation centrifugal separator according to the present invention,
4 is a perspective view showing the construction of a warm section of the graphene separation centrifugal separator according to the present invention,
FIG. 5 is a view showing the construction of a recycling tube of a graphene separation centrifugal separator according to the present invention. FIG.
FIG. 6 and FIG. 7 are photographs showing results of experiments on light mixed with graphene separated from the graphene separation centrifuge according to the present invention.
For a better understanding of the present invention, a preferred embodiment of the present invention will be described with reference to the accompanying drawings. The embodiments of the present invention may be modified into various forms, and the scope of the present invention should not be construed as being limited to the embodiments described in detail below. The present embodiments are provided to enable those skilled in the art to more fully understand the present invention. Therefore, the shapes and the like of the elements in the drawings can be exaggeratedly expressed to emphasize a clearer description. It should be noted that in the drawings, the same members are denoted by the same reference numerals. Detailed descriptions of well-known functions and constructions which may be unnecessarily obscured by the gist of the present invention are omitted.
FIG. 1 is a perspective view showing an external configuration of a graphene separation
As shown in the drawing, the graphen peeling
Accordingly, compared with the conventional method of manufacturing a graphene, it is economical, efficient, and low-risk, so that graphene with good quality can be manufactured.
The graphene separation
The graphene separation
The graphite mixed liquid (A) used throughout this specification refers to a mixed liquid in which a large-sized graphite mass initially supplied to the
The
The graphite supply port 111a is formed through the supply surface 111 and the
The graphene mixture liquid C discharged from the
On the other hand, the inner wall surface of the
The high-
The high-
A
Meanwhile, a
Accordingly, the graphite particle mixture liquid B and the graphene mixture liquid C flowing in the
The
Between the
On the other hand, the
The
The
That is, the
The
At the outer periphery of the
The
The classifying principle in which the
The
Here, the
The centrifugal force F =? 2 VP, the pressure-dependent velocity V =
The graphene grains smaller than the reference size can be peeled off from the graphite particles by controlling the injection speed of the graphite particles mixed with water and the dispersant mixed with theThe
The pair of
The
Since the graphite particle mixture liquid B and the graphene mixture liquid C in the
The
One end of the housing
The inner wall surface of the housing
The
Although not shown in the drawing, a plurality of packing members may be disposed on the inner wall surface of the housing
The operation of the graphene
The
The operator supplies power to the driving
The graphite particle mixture liquid B containing the graphite particles primarily separated by the centrifugal force caused by the rotation of the
The graphite particle mixture liquid B moved along the
In this process, the graphene mixture liquid C mixed with the graphene peeled at a reference size, that is, the nano-size or smaller, is subjected to a drag force to move the moving space between the
On the other hand, the graphite particle mixture liquid B mixed with the non-peeled graphite particles is ejected again to the high-
6 and 7 are photographs showing the results of testing the size of graphene mixed in the graphene mixed solution separated in the graphene separation centrifugal separator according to the present invention. FIG. 6 is a photograph of a graphene mixed solution in which 10 mg of graphene is mixed with 1 ml of water, and FIG. 7 is a photograph of a graphene mixed solution containing 5 mg of graphene mixed with 1 ml of water.
6 and 7 show that graphene is mixed with water and has a clear color. The graphenes of FIGS. 6 and 7 were manufactured under the conditions of a centrifuge at 4,000 rpm and a centrifugal radius of 10 cm. FIG. 6 shows a concentration of 5 mg / ml and FIG. 7 shows a concentration of 10 mg / ml.
In the case of non-nanoparticles like graphene, it precipitates on the bottom of the transparent container after a certain period of time. However, graphene retains its mixed state without precipitation even after a long period of light weight. Particularly, since graphene is peeled off as one layer, the graphite combined with two or more layers has a clear and transparent shape as opposed to a black one.
When laser light is irradiated from the outside of the transparent container, a clear red line appears inside the transparent container. In the case of water that has not been mixed with anything, no change is observed even when irradiated with laser light from the outside. When graphene is mixed in water, graphene scatters light and a red line appears as shown in Figures 6 and 7.
Meanwhile, the graphene separation centrifugal separator according to the present invention moves the graphite particles to the high pressure ejection port at a high pressure by the centrifugal force, and collides with the collision crushing plate. However, as the case may be, the graphite particles may be moved to the high-pressure jet port by the driving pressure of the reciprocating piston to collide with the impact crushing plate.
As described above, in the graphene separation centrifugal separator according to the present invention, the graphite is rotated and peeled in the centrifugal casing, and peeled off again with a strong impact on the collisional separation plate of the recirculation pipe to separate graphene , And graphene peeled below the reference size can be centrifuged and discharged to the outside.
In addition, the graphene separation centrifugal separator according to the present invention can infinitely increase the injection speed at which the graphite particles are injected into the high-pressure ejection port beyond supersonic speed, and the structure is simple.
In addition, since only a very small amount of graphene tablet for holding graphite particles for driving and a very small amount of preparation for adjusting pH are injected, there is a high purity of separated graphene.
The embodiments of the graphene separation centrifugal separator of the present invention described above are merely illustrative and those skilled in the art will appreciate that various modifications and equivalent embodiments are possible without departing from the scope of the present invention. . Therefore, it is to be understood that the present invention is not limited to the above-described embodiments. Accordingly, the true scope of the present invention should be determined by the technical idea of the appended claims. It is also to be understood that the invention includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
10: Graphite stirring tank 20: Mixing stirring tank
100: Grape separation centrifuge device 110: Centrifugal casing
111: supply surface 111a: graphite supply port
113:
114: Movement stopper projection 115: Grain outlet
117: high pressure jet port 117a: guide surface
118:
118b: second outlet pipe 120: graphite feed pipe
121: casing coupling bearing 123: bearing coupling member
130: rotation driving part 131:
133: shaft fixing member 140:
141:
141b: Spindle coupling ring 143: Spindle
143a: spindle edge 150: recirculation tube
150a: Once 150b:
151:
161: housing
161b: bearing
161d: fastening
161f: partition
161h: Graphene flow space 162: Exposure tube connection hole
163: coupling flange 165: recirculating tube coupling tube
167: Graphene Exhaust Balls
A: Graphite
B: graphite particles
C: Graphene
Claims (5)
A graphene discharge port through which a graphite supply port to which a graphite mixture liquid is supplied from the graphite particle agitating vessel and a graphene mixture fluid in which graphene peeled off from the graphite mixture liquid is discharged is discharged; A centrifugal casing having a high pressure discharge port through which the mixed graphite particle mixture liquid is discharged;
A graphite supply pipe connected to the graphite supply port and supplying the graphite mixture into the centrifuge casing;
A rotation driving part inserted into the centrifuge casing and having a driving shaft for rotating the centrifuge casing at a high speed;
A warming portion coupled to an outer periphery of the driving shaft and rotating together with the driving shaft to separate the graphene from the graphite mixed liquid fed through the graphite feeding pipe and the graphite mixed mixture fed again through the recirculating pipe;
A collision peeling plate disposed in the high pressure jet port and causing the graphite particles contained in the graphite particle mixture discharged through the high pressure jet port to collide with each other to cause graphene to peel off;
A graphite particle flow space in which the mixture of graphite particles discharged from the high pressure discharge port flows and a graphene flow space in which the graphene mixture discharged from the graphen discharge port flows are formed in the centrifugal casing rotatably inside A housing having a graphene discharge hole for discharging the graphene mixed solution in the graphene flow space to the outside;
And a recirculation tube extending from the lower portion of the housing so as to communicate with the graphite particle flow space and re-supplying the graphite particle mixture to the graphite particle agitator.
The graphene having a size smaller than the reference size is moved to the graphen outlet due to the influence of the drag due to the rotational force generated by the driving of the rotation driving unit, and the graphite particles having a size larger than the reference size are moved by centrifugal force or reciprocating pressure of the piston And discharged to the high-pressure spouting port.
Wherein the graphite supply port is formed through one side of the centrifugal casing,
Wherein the graphene discharge port is formed in a ring shape along an outer circumferential surface of a depressed other side surface of the centrifugal casing in a direction opposite to the graphite supply port,
And the high-pressure jet port is formed on a side surface of the centrifugal casing.
The warm-
A rotor coupled to the drive shaft; and a plurality of rotating plates coupled to the rotor at regular intervals in the radial direction,
Wherein the inner wall surface of the centrifugal casing is provided with a movement blocking protrusion protruding from the plate surface and forming a gap between the lower end edge of the rotating plate and the graphene flow gap corresponding to the reference size. .
The impact peeling plate is formed of a cemented carbide,
Wherein the graphen peeling centrifugal separator is disposed at an angle to the ejecting direction of the graphite particles of the high-pressure ejection port at an angle.
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CN108557807A (en) * | 2018-06-05 | 2018-09-21 | 李训祺 | A kind of graphene preparation facilities |
CN109019581A (en) * | 2018-07-13 | 2018-12-18 | 北京欧美中科学技术研究院 | A kind of commercial scale plant for purification of graphite oxide alkene solution |
KR102038502B1 (en) | 2019-03-07 | 2019-10-30 | 김용식 | Method of manufacturing mask sheet |
KR102353798B1 (en) | 2020-03-04 | 2022-01-20 | (주)투디엠 | Apparatus for exfoliation of 2-dimensional material |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003238135A (en) | 2002-02-19 | 2003-08-27 | Mitsui Mining Co Ltd | Method for manufacturing spheroidal graphite particle |
KR101103672B1 (en) | 2011-05-18 | 2012-01-11 | 성균관대학교산학협력단 | Apparatus for continuous synthesis and purification of graphene oxide with centrifugal separation type for mass production, and method of synthesis and purification of graphene oxide using the same |
KR101378734B1 (en) | 2013-01-22 | 2014-04-04 | 주식회사 제이오 | Apparatus and method for exfoliating graphite using high temperature and high pressure medium |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003238135A (en) | 2002-02-19 | 2003-08-27 | Mitsui Mining Co Ltd | Method for manufacturing spheroidal graphite particle |
KR101103672B1 (en) | 2011-05-18 | 2012-01-11 | 성균관대학교산학협력단 | Apparatus for continuous synthesis and purification of graphene oxide with centrifugal separation type for mass production, and method of synthesis and purification of graphene oxide using the same |
KR101378734B1 (en) | 2013-01-22 | 2014-04-04 | 주식회사 제이오 | Apparatus and method for exfoliating graphite using high temperature and high pressure medium |
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