KR100910382B1 - Production device of carbon nano-tube using fluidized bed of dispersing catalysts - Google Patents

Abstract

The present invention relates to a carbon nanotube synthesis apparatus, and more particularly, to a carbon nanotube synthesis apparatus for improving the yield when synthesizing carbon nanotubes in a fluidized bed by dispersing a catalyst.

Carbon nanotube synthesis apparatus according to an embodiment of the present invention is a reaction gas supply unit for supplying a reaction gas, a reaction chamber for reacting the reaction gas and the catalyst to synthesize the carbon nanotubes, a plurality of reaction gas passes in the reaction chamber And a rotating unit for rotating the spray plate having holes and dispersing the catalyst remaining on the spray plate.

Carbon Nanotubes, Catalyst Dispersion, Fluidized Beds

Description

Production device of carbon nano-tube using fluidized bed of dispersing catalysts

The present invention relates to a carbon nanotube synthesis apparatus, and more particularly, to a carbon nanotube synthesis apparatus for improving the yield when synthesizing carbon nanotubes in a fluidized bed by dispersing a catalyst.

Carbon nanotubes form a hexagonal honeycomb pattern by combining one carbon atom with three other carbon atoms around it. Carbon nanotubes have excellent electrical, thermal, and mechanical properties compared to conventional devices, and can be applied to various industrial fields such as field emission devices, electrochemical and energy storage, ultra-fine mechatronic systems, and organic and inorganic composite materials.

As a method of synthesizing such carbon nanotubes, a laser ablation method is performed by vaporizing a specimen made of a mixture of metal and graphite powder using a laser, and arc discharge by applying voltage to two carbon rods having different diameters. Arc discharge method to synthesize carbon dioxide, chemical vapor deposition (CVD) to grow carbon nanotubes by heat or plasma by injecting gaseous raw gas into the reactor, and hydrocarbon in liquid or gas phase Pyrolysis of hydrocarbon is supplied to a reaction tube heated with a transition metal to decompose hydrocarbons to produce carbon nanotubes in a gaseous state.

Recently, various attempts have been made to synthesize carbon nanotubes in large quantities. Among them, a chemical vapor deposition method for injecting a gaseous reaction gas into a reactor and receiving energy from heat or a plasma is thermally decomposed, and a thermally decomposed radical and a catalyst are combined to synthesize a large amount of carbon nanotubes.

However, the chemical vapor deposition method is limited to the exposed portion of the bonding area of the catalyst and the reaction gas by applying a catalyst to the substrate thin film of the transition metal to combine with the reaction gas. Therefore, when the catalyst is stacked on the substrate, the upper catalyst has a contact surface for bonding with the reaction gas, but the lower catalyst has little contact surface for bonding with the reaction gas, thereby inhibiting the synthesis of carbon nanotubes.

In addition, due to the high temperature of the reactor, agglomeration or solidification of the catalyst may occur. This is an obstacle in synthesizing the carbon nanotubes in a large amount, and there is a need for a method of increasing the area or time for the catalyst to contact the reaction gas while preventing it.

Therefore, in synthesizing carbon nanotubes using a catalyst, a method for efficiently contacting the catalyst with a reaction gas in a reactor is needed.

The present invention has been made in view of the above problems, and an object of the present invention is to provide a carbon nanotube synthesis apparatus that promotes a reaction with a reaction gas by dispersing a catalyst and improves the yield at the time of synthesizing carbon nanotubes.

In addition, an object of the present invention is to provide a carbon nanotube synthesizing apparatus capable of efficiently synthesizing carbon nanotubes by reducing the accumulation of powdered catalyst in the bottom of the reaction chamber or the like and scattering them into the reaction chamber.

The objects of the present invention are not limited to the above-mentioned objects, and other objects that are not mentioned will be clearly understood by those skilled in the art from the following description.

Carbon nanotube synthesis apparatus according to an embodiment of the present invention to achieve the above object is a reaction gas supply for supplying a reaction gas; A reaction chamber in which the reaction gas reacts with the catalyst to synthesize carbon nanotubes; An injection plate having a plurality of holes through which reaction gas passes in the reaction chamber; And a rotating unit rotating the spray plate to disperse the catalyst remaining on the spray plate.

Specific details of other embodiments are included in the detailed description and the drawings. Advantages and features of the present invention and methods for achieving them will be apparent with reference to the embodiments described below in detail with the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but can be implemented in various different forms, only the embodiments are to make the disclosure of the present invention complete, the general knowledge in the art to which the present invention belongs It is provided to fully inform the person having the scope of the invention, which is defined only by the scope of the claims. Like reference numerals refer to like elements throughout.

According to the present invention, the yield can be improved in the synthesis of carbon nanotubes by increasing the contact area between the catalyst and the reaction gas.

The catalyst can be efficiently used in the synthesis of carbon nanotubes by reducing the agglomeration of the catalyst or the hardening of the catalyst on the bottom.

The effects of the present invention are not limited to the above-mentioned effects, and other effects not mentioned will be clearly understood by those skilled in the art from the description of the claims.

Preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

1 shows a perspective view of a carbon nanotube synthesis device according to an embodiment of the present invention, Figure 2 shows a cross-sectional view of the carbon nanotube synthesis device according to an embodiment of the present invention. Figure 3 is a perspective view showing a jet plate and a rotating part in the carbon nanotube synthesis apparatus according to an embodiment of the present invention.

1 and 2, the carbon nanotube synthesis apparatus according to an embodiment of the present invention is the reaction gas supply unit 100, the reaction chamber 200, the injection plate 300, the rotating unit 400, the heating unit ( 500 and the catalyst supply unit 600.

The reaction chamber 200 provides a space in which carbon nanotubes are synthesized by the fluidized bed. The reaction chamber 200 is made of a heat resistant material such as quartz or graphite. In the reaction chamber 200, the reaction gas supplied by the reaction gas supply unit 100 forms a fluidized bed in the reaction chamber 200 to actively generate a reaction with the catalyst. The reaction gas is decomposed into radicals while flowing in the reaction chamber 200, and the decomposed radicals react with the catalyst to synthesize carbon nanotubes.

The reaction chamber 200 may include a gas exhaust 250 to remove the reaction gas in the reaction chamber 200 after the synthesis of the carbon nanotubes is completed. The gas exhaust unit 250 may further include a gas removal unit 260 for converting the gas exhausted for safety into a safe compound by a reaction.

The reaction gas supply unit 100 supplies the reaction gas into the reaction chamber 200. The reaction gas supply unit 100 may be used in one or a combination of acetylene, ethylene, methane, benzene, xylene, carbon monoxide, carbon dioxide. The reaction gas supply unit 100 may include a plurality of gas tanks 120 to supply a plurality of reaction gases.

The reaction gas supply unit 100 may include a supply line 110, a gas tank 120, a valve 125, and a nozzle unit 130 to supply the reaction gas. The gas tank 120 serves to store the reaction gas, and a plurality of gas tanks 120 may be used when a plurality of reaction gases are used for the synthesis of carbon nanotubes. Supply line 110 provides a path for the reaction gas to pass through the gas tank. The nozzle unit 130 is an inlet for the reaction gas to enter the reaction chamber. The nozzle unit 130 may have a tubular shape or a flare shape to allow the reaction gas to spread into the reaction chamber 200. The valve 125 may control the access of the reaction gas from the gas tank 120 to open and close the passage of the supply line.

The reaction gas supply unit 100 may supply an inert gas such as argon or nitrogen after the synthesis of the carbon nanotubes as well as the supply of the reaction gas is completed.

The injection plate 300 includes a plurality of holes 310 and is mounted in the reaction chamber. The injection plate 300 serves to uniformly spread the reaction gas supplied by the reaction gas supply unit 100 into the reaction chamber 200. In addition, the injection plate 300 may temporarily hold the catalyst sprayed on the injection plate. The reaction gas attracts the catalyst remaining on the injection plate while passing through the hole 310 of the injection plate 300 to achieve a flow inside the reaction chamber. The jet plate 300 may rotate by the action of the rotating unit 400. The injection plate 300 may be formed of a magnetic material such as iron, or a portion thereof, or may be rotated by a magnetic force of the rotating unit 400 by attaching a magnet to the edge of the injection plate 300.

The jet plate 300 may further include a support part 325 for supporting the jet plate in the reaction chamber 200 and a slide part 315 for guiding rotation of the jet plate 300. Therefore, the spray plate 300 may be rotated by a small force that rotates the spray plate 300 from the outside while being seated in the reaction chamber 200.

The rotating unit 400 serves to rotate the jet plate. The rotating unit 400 rotates the spray plate 300 having the plurality of holes 310 to disperse the catalyst on the spray plate 300. As the catalyst is scattered, a part of the catalyst may enter the plurality of holes, and the catalyst entering the hole may move along the fluidized bed in the reaction chamber by the reaction gas passing through the hole. On the other hand, the component for rotating the rotating unit 400 may be implemented by various means. As an example, the rotating unit 400 may be rotated by an element that connects the belt 400 or a chain and provides a driving force such as a motor. As another example, the rotary part 400 may be inscribed with a sawtooth-shaped pattern on the rotary part 400 disposed surrounding the outer surface of the reaction chamber 200, and the rotary part 400 may be rotated by an element providing a tooth and a driving force to engage the tooth. .

The rotating unit 400 may rotate the spray plate by applying a magnetic force to the spray plate 300. As an example, referring to FIG. 3, a magnet 410 in which an N pole and an S pole cross each other may be disposed on an outer surface of the reaction chamber. Therefore, by rotating the rotating unit 400 is attached to the magnet pole 410 cross the N pole and the S pole on the outer surface of the reaction chamber it is possible to rotate the injection plate 300 located therein. In this case, the injection plate 300 may also include magnets 320 of the S pole and the N pole corresponding to the N pole and the S pole located on the outer surface of the reaction chamber 200.

As another example, the spray plate 300 may be rotated by an electromagnet. The electromagnet may be applied to the outer surface of the reaction chamber to rotate the jet plate 300. The spray plate 300 may be rotated by disposing a permanent magnet near the outer surface of the spray plate 300 and sequentially changing the poles of the electromagnets on the outer surface of the reaction chamber.

The heating unit 500 heats the reaction chamber 200 to a process temperature at which the process is performed. The heating unit 500 may heat the reaction chamber by the heating wire 510 or the induction coil as a whole while surrounding the reaction chamber 200. The heating unit 500 may include a heat insulation wall surrounding the outer wall of the reaction chamber 200 and a heating wire 510 or an induction coil inside the heat insulation wall. When the carbon nanotubes are synthesized, they may be heated to a range of approximately 500 to 1100 degrees Celsius.

The catalyst supply unit 600 serves to supply a catalyst for the synthesis of carbon nanotubes in the reaction chamber 200. The catalyst supply unit 600 may include a storage unit 610 and a supply pipe 620. The supply pipe 620 provides a passage through which the catalyst in powder form passes, and sprays the catalyst supplied from the storage 610 onto the jet plate. The storage unit 610 may include a pinwheel 615 having a jar shape having a pointed bottom or agitating the catalyst in the center of the storage unit 610 so that the powdered catalyst does not have an empty space. Alternatively, the storage unit may be shaken by a vibrator (not shown) in case the catalyst of the storage unit 610 does not slip on the wall.

Referring to the operation of the carbon nanotube synthesis apparatus according to an embodiment of the present invention configured as described above are as follows.

First, the reaction chamber 200 is heated by the heating unit 500. The heating unit 500 is heated to a process temperature of 500 ~ 1100 ° C range. When the internal temperature of the reaction chamber 200 reaches the required process temperature, the reaction gas is supplied to the reaction chamber 200. The catalyst is supplied to the injection plate 300 by the catalyst supply unit 600 together with the supply of the reaction gas. Therefore, the reaction gas forms a fluidized bed in the reaction chamber 200 while passing through the hole 310 of the injection plate 300. The reaction gas may draw a catalyst on the injection plate 300 while passing through the hole 310 of the injection plate 300 to drift with the catalyst to form a fluidized bed. The reaction gas may be thermally decomposed by high temperature heat inside the reaction chamber 200 to be decomposed into radicals. The decomposed radicals react with the catalyst to synthesize carbon nanotubes.

Figure 4a shows the catalyst accumulated on the injection plate when the injection plate does not rotate, Figure 4b shows the catalyst accumulated on the injection plate when the injection plate rotates in the carbon nanotube synthesis apparatus according to an embodiment of the present invention .

When the reaction gas is supplied to form a fluidized bed in the reaction chamber 200, the rotating unit 400 rotates the injection plate 300. The spray plate 300 rotates to induce movement of the catalyst remaining on the spray plate 300.

Referring to FIG. 4A, when the spray plate 300 does not rotate, the catalyst may be continuously stacked on the spray plate, and the stacked catalyst may harden the catalyst in the reaction chamber 200 due to hardening. . However, the catalyst may be moved to the wall surface of the reaction chamber 200 by centrifugal force by rotating the injection plate 300 as shown in FIG. 4B. The catalyst may move to the hole of the injection plate while moving out, and the catalyst moved to the hole 310 of the injection plate 300 forms a flow by the reaction gas passing through the hole. As such, by rotating the jet plate by the rotating unit 400, the catalyst remains in the jet plate, thereby reducing the phenomenon that the catalyst is hardened or the catalyst is accumulated. The catalyst forms a fluidized bed with the reaction gas, thereby widening the contact surface between the catalyst and the reaction gas, thereby synthesizing the carbon nanotubes in large quantities.

5 is a perspective view of a carbon nanotube synthesis apparatus according to another embodiment of the present invention.

Referring to FIG. 5, the carbon nanotube synthesis apparatus according to another embodiment of the present invention may include a reaction gas supply unit 100, a reaction chamber 200, an injection plate 300, a rotating unit 400, a heating unit 500, The catalyst supply unit 600 and the locking unit 350 may be included.

In the carbon nanotube synthesis apparatus, the reaction gas supply unit 100, the reaction chamber 200, the injection plate 300, the rotating unit 400, the heating unit 500, and the catalyst supply unit 600 have been described in detail, and thus will be omitted. The locking unit 350 will be described in detail.

The catching part 350 serves to sweep the catalyst remaining on the injection plate 300. The catching part 350 may be fixed or move relative to the rotation of the jet plate 300. For example, when the catching part 350 is fixed to the inner wall of the reaction chamber 200 and positioned near the upper surface of the spraying plate 300, the retaining portion 350 catches the remaining catalyst when the spraying plate 300 rotates. ) Can be moved.

The catching part 350 may include a rod-shaped body portion having a length about the radius of the jetting plate, or may include a broom-type brush on the rod-shaped body portion. The catching part 350 may be fixed to one or more reaction chambers 200. Alternatively, the locking portion 350 has a hole having a predetermined diameter in the center of the injection plate 300, is penetrated through the hole is fixed and fixed to the rotation of the injection plate 300 is fixed to the catalyst It can be caught and moved.

Referring to the operation of the carbon nanotube synthesis device according to another embodiment of the present invention configured as described above are as follows.

Figure 6 shows the action of the locking portion in the carbon nanotube synthesis apparatus according to another embodiment of the present invention. Actions by other components except for the locking portion 350 are the same as described above, and thus will be omitted, and the operation of the locking portion 350 will be described later.

Referring to FIG. 6, the locking portion 350 is fixed on the spray plate 300, and the distance between the spray plate 300 and the locking portion 350 may be adjusted as short as possible. Therefore, when the spray plate 300 is rotated by the rotating unit 400, the catalyst remaining on the spray plate 300 is caught by the catching part 350. Therefore, the catalysts caught by the locking part 350 may be pushed out and moved to the plurality of holes 310 provided in the injection plate 300 while being pushed out. The catalysts that are pushed out are scattered into the reaction chamber 200 while forming a fluidized bed by the reaction gas passing through the hole 310, and thus the contact surface between the catalyst and the reaction gas is relatively widened, and thus the yield of carbon nanotubes is increased. Can increase.

Although embodiments of the present invention have been described above with reference to the accompanying drawings, those skilled in the art to which the present invention pertains have various permutations, modifications, and modifications without departing from the spirit or essential features of the present invention. It is to be understood that modifications may be made and other embodiments may be embodied. Therefore, it should be understood that the embodiments described above are exemplary in all respects and not restrictive.

1 is a perspective view of a carbon nanotube synthesis apparatus according to an embodiment of the present invention.

2 is a cross-sectional view of a carbon nanotube synthesis apparatus according to an embodiment of the present invention.

Figure 3 is a perspective view showing a jet plate and a rotating part in the carbon nanotube synthesis apparatus according to an embodiment of the present invention.

4A is a view showing catalysts stacked on a spray plate when the spray plate does not rotate.

Figure 4b is a view showing a catalyst stacked on the injection plate when the injection plate rotates in the carbon nanotube synthesis apparatus according to an embodiment of the present invention.

5 is a perspective view of a carbon nanotube synthesis apparatus according to another embodiment of the present invention.

6 is a view showing the action of the locking portion in the carbon nanotube synthesis apparatus according to another embodiment of the present invention.

* Description of the main parts of the drawings *

100: reaction gas supply unit 200: reaction chamber

300: injection plate 400: rotating part

500: heating unit 600: catalyst supply unit

Claims (7)

A reaction gas supply unit supplying a reaction gas; A reaction chamber for synthesizing carbon nanotubes by reacting the reaction gas with a catalyst; An injection plate having a plurality of holes through which the reaction gas passes in the reaction chamber; A rotating unit which rotates the spray plate to disperse the catalyst remaining on the spray plate; And And a locking portion for moving the catalyst remaining on the jet plate when the jet plate is rotated. The method of claim 1, Magnets are installed near the outer peripheral surface of the jet plate, The rotating unit rotates the jet plate by a magnetic force applied outside the reaction chamber, carbon nanotube synthesis apparatus. delete delete The method of claim 1, wherein the locking portion A body part fixed to the reaction chamber; And Located on one surface of the body portion comprising a plurality of brushes for sweeping out the catalyst, carbon nanotube synthesis apparatus. The method of claim 1, Carbon nanotube synthesizing apparatus further comprises a heating unit for heating the reaction chamber. The method of claim 1, Carbon nanotube synthesis apparatus further comprises a catalyst supply for supplying a catalyst.

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