KR101807373B1 - Graphene crushing and centrifugation apparatus - Google Patents

Graphene crushing and centrifugation apparatus Download PDF

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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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graphite
graphene
mixture
casing
discharged
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KR20170079352A (en
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한철주
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한철주
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/19Preparation by exfoliation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1806Stationary 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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  • Chemical Kinetics & Catalysis (AREA)
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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

{GRAPHENE CRUSHING AND CENTRIFUGATION APPARATUS}

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a graphene separation centrifugal apparatus, and more particularly to a graphene separation centrifugal apparatus capable of separating graphite into nano-sized graphene and centrifuging graphene.

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.

Korean Patent Laid-Open No. 10-2014-0092310 "Copper foil for manufacturing graphene, a method for producing the same, and a method for producing graphene" Korean Patent Publication No. 10-2014-0083671 "Graphene, a composition for producing graphene and a method for producing graphene using the same,

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 centrifugal separator 100 according to the present invention. FIG. 2 is an exploded perspective view of the graphene separation centrifugal separator 100, Sectional configuration of the centrifuge casing 110. As shown in Fig.

As shown in the drawing, the graphen peeling centrifugal separator 100 according to the present invention, when the graphite mixed liquid A containing large particles of graphite is introduced into the centrifugal casing 100, The graphene mixed solution C mixed with graphene is centrifuged and discharged to the outside. That is, peeling of graphite and centrifugal separation of graphene are simultaneously performed.

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 centrifugal separator 100 according to the present invention includes a graphite stirring vessel 10 for stirring graphite with water and a dispersing agent and a centrifugal separator 110 for receiving a graphite mixture liquid A from the graphite stirring vessel 10, And a graphen storage tank 30 in which the graphene C separated from the graphene separation centrifugal separator 100 is accommodated.

The graphene separation centrifugal separator 100 includes a centrifugal separator 110 for separating the graphite mixture A from the centrifugal separator 110 after the graphite mixture A is supplied, A rotation driving unit 130 for applying a driving force to rotate the centrifugal casing 110 at a high speed, a warm section 140 for rotating the centrifugal casing 110 and separating graphite, A housing 160 and 160a enclosing the outside of the casing 110 and containing the graphite particle mixture liquid B and the graphene mixture liquid C discharged from the centrifugal casing 110 to be separated from each other, And a recycle tube 150 for supplying the particle mixture liquid (B) again to the mixing and stirring tank (20).

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 graphite stirring tank 10 is mixed with water and a dispersant as shown in FIG. 1, (B) refers to a mixed liquid in which graphite grains larger than a reference size are mixed with grains which have been introduced into the centrifuge casing 110 through the graphite supply pipe 120 and contacted with the warm section 140 one time or more and separated, The mixed solution (C) refers to a mixed solution obtained by mixing graphene separated to a size smaller than the reference size.

The centrifugal casing 110 is rotated by the rotation driving unit 130 and provides a space where graphite contained in the graphite mixed solution A is peeled and centrifuged with graphite particles and graphene. The centrifuge casing 110 is formed in a conical shape in which the supply surface 111 and the discharge surface 113a are formed on both sides. The centrifugal casing 110 is provided so as to be gradually wider in diameter from the supply surface 111 and has a diameter gradually narrowed to the discharge surface 113a with respect to the high-pressure discharge port 117. [

The graphite supply port 111a is formed through the supply surface 111 and the discharge surface 113a is formed to be recessed from the discharge end 113 to a predetermined depth. A graphene mixture liquid C mixed with graphene having a reference size, that is, a nano size or smaller size is formed between the discharge surface 113a and the discharge end 113, Are formed in a ring shape.

The graphene mixture liquid C discharged from the graphene discharge port 115 is guided along the discharge end 113 and then transferred to the graphene storage tank 30 through the graphene discharge hole 167 of the housing 160 .

On the other hand, the inner wall surface of the centrifugal casing 110 extending from the high-pressure spout 117 to the graphen outlet 115 is provided with a slanting protrusion 114 protruding at a predetermined height. The movement stopper projection 114 forms a flow space d for moving the graphene mixture liquid C to the graphen outlet 115 between the edge 143a of the rotating plate 143 and the enlarged portion 143a as shown in FIG. do. The flow space d is formed as a fine gap as the size of the graphene mixed with the graphene mixture liquid C to prevent the graphite particles larger than the reference size from passing therethrough.

The high-pressure spout 117 is formed to protrude radially outward from the side surface of the centrifuge casing 110 by a predetermined length. The high-pressure discharge port 117 serves as a passage for guiding the graphite particle mixture liquid B to collide with the collision-crush plate 151 at a high pressure by the centrifugal force generated when the cold section 140 rotates.

The high-pressure spout 117 has a smoothly rounded guiding curved surface 117a on the inner wall surface connected to the centrifuge casing 110. [ Whereby the graphite particle mixture liquid B can be easily moved to the high-pressure discharge port 117 along the guide curved surface 117a.

A discharge nozzle 118 is integrally formed on the upper portion of the high-pressure spout 117. The discharge nozzle 118 is formed to have a diameter significantly smaller than the diameter of the high-pressure discharge port 117 as shown in FIG. 3 so that the graphite particles mixed in the graphite particle mixture liquid B are discharged at a higher speed V1 151). The discharge nozzle 118 is provided with a first discharge pipe 118a connected to the high pressure discharge port 117 and a second discharge pipe 118b connected to the first discharge pipe 118a. The diameter r2 of the second discharge pipe 118b is formed to be smaller than the diameter r1 of the first discharge pipe 118a so that the discharge velocity V1 of the graphite particles gradually increases to hit the impact peeling plate 151. As a result, the effect of collision between the impact peeling plate 151 and the graphite particles becomes larger, so that it is possible to peel the particles up to the size of nano unit.

Meanwhile, a partition plate 119 is formed at a position adjacent to the discharge nozzle 118 along the circumferential direction of the centrifuge casing 110 so as to extend a certain area. The partition plates 119 are inserted into the partition plate insertion grooves 161f of the housings 160 and 160a as shown in Figs. 2 and 3 so that the inside of the housings 160 and 160a is filled with the graphite particle flow space 161g and the graphene flow And a space 161h.

Accordingly, the graphite particle mixture liquid B and the graphene mixture liquid C flowing in the housings 160 and 160a can be accommodated without being mixed with each other.

The graphite supply pipe 120 is inserted into the graphite supply port 111a of the centrifugal casing 110 to supply the graphite mixture liquid A and the graphite particle mixture liquid B into the centrifugal casing 110. The graphite supply pipe 120 receives the graphite mixture A from the mixing and stirring tank 20 and the graphite particle mixture B from the recycle pipe 150.

Between the graphite supply pipe 120 and the smoking supply port 111a is provided a casing coupling bearing 121 for supporting the graphite supply pipe 120 between the rotating centrifugal casing 110. The casing engaging bearing 121 is fixed to the centrifuge casing 110 by a bearing engaging member 123. When the centrifugal casing 110 rotates by the rotation driving unit 130, the casing engaging bearing 121 rotates together with the centrifugal casing 110, and the graphite supply pipe 120, which is provided inside the casing engaging bearing 121, It is not rotated and remains fixed.

On the other hand, the graphite supply pipe 120 is connected to the other end 150b of the recycle pipe 150. The graphite supply pipe 120 is connected to the centrifugal casing 110 together with the graphite mixed liquid A mixed with the large graphite and the graphite particle mixture B mixed with the graphite particles moved through the recirculating pipe 150, .

The rotation driving unit 130 provides a driving force for rotating the centrifuge casing 110. The rotation driving unit 130 includes a driving shaft 131 inserted into the centrifuge casing 110, a shaft fixing member 133 integrally fixing the driving shaft 131 to the centrifugal casing 110, (Not shown). The drive motor 135 is provided outside the centrifuge casing 110 and the housings 160 and 160a and the drive shaft 131 is coupled to the drive motor 135. [

The hot section 140 is connected to the driving shaft 131 and rotates and is connected to the centrifugal casing 110 rotating with the non-rotating graphite mixture liquid A and the graphite particle mixture liquid B flowing through the graphite feed pipe 120 The speed difference is buffered.

That is, the hot section 140 is formed by the speed difference between the non-rotating graphite mixture liquid A and the graphite particle mixture liquid B flowing through the graphite supply pipe 120 and the rotating centrifugal casing 110, The incomplete flow generated in the centrifugal separator 110 affects the centrifugal liquid surface to prevent deterioration of the graphene separation effect.

The hot section 140 includes a rotor 141 concentrically coupled to the drive shaft 131 and a plurality of rotary plates 143 coupled to the rotor 141. 4 is a perspective view showing a configuration of the warm section 140. As shown in FIG. The rotor 141 is coupled to the outside of the drive shaft 131 as shown in FIG. At this time, a coupling member (not shown) such as a pin is inserted into the rotor 141 and the drive shaft 131 so as to penetrate the rotor 141 and the rotor 141 together with the drive shaft 131.

At the outer periphery of the rotor 141, a rotation plate coupling ring 141b is formed along the circumferential direction. A plurality of rotation plate coupling rings 141b are provided on the upper and lower sides along the axial direction of the rotor 141.

The rotation plate 143 is provided in a plate shape formed of a cemented carbide material. The rotation plate 143 is provided with a ring insertion groove 143b which is fixedly coupled to the rotor 141 by interference fit with the rotation plate coupling ring 141b on one side. When the rotor 141 rotates, the rotating plate 143 also rotates to complement the incomplete flow of the graphite mixed liquid A and the graphite particle mixed liquid B introduced into the centrifugal casing 110. 3, the interval between the rotation plate edge 143a and the movement stopping protrusion 114 is narrowed to ensure stable rotation of the liquid surface while ensuring simultaneous rotation of the centrifugation liquid surface.

The classifying principle in which the rotation driving part 130 and the warm part 140 separate graphite particles and graphene mixed in the graphene mixture liquid C and the graphite particle mixture liquid B is obtained by the Stokes' And the particles are dispersed by the centrifugal force and the drag force generated by the centrifugal force. When the point at which the centrifugal force and the drag are equal is defined as the cut size, the cut size has a probability of being a coarse fraction and a differential fraction of 50:50, and the graphen influenced by the centrifugal force is deflected into the coarse fraction to form graphen discharge And the graphite particles affected by the drag force are deflected as differential powders and discharged to the high-pressure discharge port 117. [

The impact peeling plate 151 passes through the discharge nozzle 118 in the centrifugal casing 110 and collides with the graphite mixed liquid A and the graphite particle mixed liquid B in which the velocity is increased to collapse into small particles.

Here, the impact separation plate 151 is disposed at an angle to the direction in which the graphite mixture liquid A and the graphite particle mixture liquid B are discharged from the discharge nozzle 118 at a predetermined angle. The angle of the impact peeling plate 151 may be in the range of 10 ° to 80 °.

The centrifugal force F =? 2 VP, the pressure-dependent velocity V =

Figure 112017078447002-pat00001
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 the impact peeling plate 151 to 100 m / s or more.

The recirculation pipe 150 is connected to the recirculation pipe coupling pipe 165 of the lower housing 160a to re-supply the graphite particle mixture liquid B to the mixing and stirring tank 20. One end of the recirculation pipe 150 is fixed to the recirculation pipe coupling pipe 165, and the other end is fixed to the mixing agitating tank 20.

The pair of housings 160 and 160a cover the centrifugal casing 110, which rotates when the centrifugal casing 110 is wound around the centrifugal casing 110 at the upper and lower portions thereof, (B) and the graphene mixture (C) are separated and accommodated.

The housings 160 and 160a include a housing main body 161 enclosing the outside of the centrifugal casing 110, a coupling flange 163 coupling the pair of housings 160 and 160a to each other, And a graphene outer discharge hole 167 for discharging the graphene mixture liquid C discharged to the graphen discharge outlet 115 to the outside .

Since the graphite particle mixture liquid B and the graphene mixture liquid C in the housings 160 and 160a are accommodated in the lower housing 160a by weight, the circulation pipe coupling pipe 165 and the graphene outer discharge holes 167 Is provided only in the lower housing 160a.

The housing body 161 receives the centrifuge casing 110 therein so that the centrifuge casing 110 can rotate inside. The housing main body 161 is provided in a pair of left and right sides, and the engaging flanges 163 are disposed in contact with each other, and then fixed by a fastening member 164 such as a bolt.

One end of the housing main body 161 is provided with a supply pipe insertion groove 161a into which the graphite supply pipe 120 is inserted and a bearing insertion groove 161b formed in the supply pipe insertion groove 161a so as to be stepped and into which the casing coupling bearing 121 is inserted, . The other end of the housing main body 161 is formed with a drive shaft insertion groove 161c into which the drive shaft 131 is inserted and a fastening member insertion groove 161d in a stepped manner.

The inner wall surface of the housing main body 161 is provided with a partition plate insertion groove 161f into which the partition plate 119 is inserted and a plurality of partition walls which protrude from both sides of the partition plate insertion groove 161f to seal around the partition plate 119 The engaging jaw 161e is protruded. The graphite particle flow space 161g and the graphene flow space 161h are independently formed with the partition plate 119 therebetween and the graphene mixture liquid C and the graphite particle mixture liquid B are not mixed with each other.

The graphene discharge hole 167 is connected to the graphen tank 30 and discharges the graphene mixed liquid C discharged through the graphen discharge outlet 115 to the outside. The graphene outer discharge hole 167 is formed adjacent to the discharge surface 113a.

Although not shown in the drawing, a plurality of packing members may be disposed on the inner wall surface of the housing main body 161 to prevent leakage of the graphite mixed liquid, the graphite mixed liquid, and the graphene mixed liquid.

The operation of the graphene separation centrifuge apparatus 100 according to the present invention having such a configuration will be described with reference to FIGS. 1 to 5. FIG.

The drive shaft 131 is connected to the drive motor 135 for driving the grape-removing centrifuge device 100. The outer surface of the centrifuge casing 110 is surrounded by a pair of housings 160 and 160a. At this time, the recycle pipe 150 is connected to the recycle pipe coupling pipe 165 and the mixing / stirring tank 20.

The operator supplies power to the driving motor 135 and then supplies the graphite mixed liquid A of the mixing agitation tank 20 to the graphite supply pipe 120. At this time, the graphite mixture liquid (A) is supplied from the graphite mixing tank (10). When the graphite mixture liquid A is injected into the centrifugal casing 110, the rotating rotor 141 and the warm section 140 and the graphite of the graphite mixture liquid A collide with each other and are primarily separated.

The graphite particle mixture liquid B containing the graphite particles primarily separated by the centrifugal force caused by the rotation of the rotor 141 and the warm section 140 is discharged to the high pressure discharge port 117 at a high speed. 5, the graphite particle mixture liquid B transferred to the discharge nozzle 118 through the high-pressure discharge port 117 is discharged at a higher speed due to the difference in diameters of the first discharge pipe 118a and the second discharge pipe 118b And collides against the collision peeling plate 151 in an accelerated state. The graphite particles are broken into smaller particles by the impact of collision and are accommodated in the graphite particle flow space 161g of the housings 160 and 160a. Then, it is moved to the mixing agitating tank 20 along the recycle pipe 150.

The graphite particle mixture liquid B moved along the recycle pipe 150 is stirred together with the graphite mixture liquid A supplied from the graphite stirring tank 10 in the mixing and stirring tank 20 and then mixed again with the centrifugal casing 110, And the graphite and the graphite particles collide with the rotating plate 143 so that the peeling progresses and the graphene separation process is performed.

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 edge 141a of the rotating plate 143 and the moving stopper protrusion 114 d and then discharged to the graphen outlet 115. [ The graphene mixture liquid C discharged to the graphen outlet 115 is moved to the graphene flow space 161h of the housing 160 and 160a and is discharged to the graphen reservoir 30 through the graphene discharge hole 167. [ Respectively.

On the other hand, the graphite particle mixture liquid B mixed with the non-peeled graphite particles is ejected again to the high-pressure ejection port 117 by the centrifugal force and then strikes against the impact peeling plate 151 and is peeled off again. To the centrifugal casing 110 while repeating the circulation path to separate the graphenes separated to the reference size or less.

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: discharge end 113a: discharge face
114: Movement stopper projection 115: Grain outlet
117: high pressure jet port 117a: guide surface
118: exhaust nozzle 118a: first exhaust pipe
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: rotor 141a: drive shaft insertion hole
141b: Spindle coupling ring 143: Spindle
143a: spindle edge 150: recirculation tube
150a: Once 150b:
151: impact peeling plate 160, 160a: housing
161: housing main body 161a: supply tube insertion groove
161b: bearing insertion groove 161c: drive shaft insertion groove
161d: fastening member insertion groove 161e:
161f: partition plate insertion groove 161g: graphite particle flow space
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 graphite particle agitator supplied with a graphite mixture liquid from a graphite agitator;
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 method according to claim 1,
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.
3. The method of claim 2,
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 method of claim 3,
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. .
5. The method of claim 4,
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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