KR20140103669A - Apparatus for producing carbon nanostructures with horizontal obstructing plates - Google Patents

Abstract

The present invention provides an apparatus for manufacturing a carbon nanostructure, comprising: a main body of a reactor having a reaction space formed therein; rising flow inhibiting members that are horizontal obstructing plates for separating the reaction space into upper and lower parts, are attached to an edge member and the inside of the edge member, and have a plurality of ventholes formed thereon; a catalyst supply pipe for supplying a catalyst into the main body from the bottom part of the main body of the reactor; a reactive gas supply pipe connected to the lower part of the reactor to supply reactive gas, which includes a carbon source, reducing gas and inert gas, into the reactor; and a product discharge pipe for discharging a generated carbon nanostructure and mixed gas. The apparatus for manufacturing a carbon nanostructure generates a carbon nanostructure by making the catalyst, the carbon source and the reactive gas react while flowing in the reaction space.

Description

TECHNICAL FIELD [0001] The present invention relates to a carbon nanostructure manufacturing apparatus having a horizontal baffle plate,

The present invention relates to a carbon nanostructure manufacturing apparatus, and more particularly, to a fluidized bed reactor for manufacturing carbon nanotubes or fibers.

Fluidized bed reactors are reactor devices that can be used to perform a variety of multiphase chemical reactions. In a fluidized bed reactor, a fluid (gas or liquid) reacts with a solid material in a particulate state, typically the solid material is a catalyst having the shape of a small sphere and the fluid is flowed at a rate sufficient to float the solid material So that the solid material behaves like a fluid.

On the other hand, carbon nanostructures (CNS) refer to nano-sized carbon structures having various shapes such as nanotubes, nanofibers, fullerenes, nanocons, nanohorns, and nano-rods and have various excellent properties It is highly utilized in various technical fields. Carbon nanotubes (CNTs), which are typical carbon nanostructures, are formed by bonding three neighboring carbon atoms to each other in a hexagonal honeycomb structure to form a carbon plane, and the carbon plane is cylindrically shaped to have a tube shape. Carbon nanotubes have a characteristic of being a conductor or a semiconductor depending on the structure, that is, the diameter of the tube, and can be widely applied in various technical fields, and thus, they are popular as new materials. For example, the carbon nanotubes can be applied to an electrode of an electrochemical storage device such as a secondary cell, a fuel cell or a supercapacity, an electromagnetic wave shielding, a field emission display, or a gas sensor.

For example, carbon nanotubes can be produced by arc discharge, laser evaporation, and chemical vapor deposition. In the chemical vapor deposition method among the above-mentioned manufacturing methods, carbon nanotubes are produced by dispersing and reacting metal catalyst particles and a hydrocarbon-based raw material gas in a reactor at a high temperature. That is, the metal catalyst reacts with the raw material gas to grow carbon nanotubes while floating in the fluidized bed reactor by the raw material gas.

Korean Patent Registration No. 10-1082831 discloses a carbon nanotube synthesizing apparatus including a plurality of dispersion plates that vertically divide the interior of a vertical reaction chamber and uniformly disperse the source gas supplied from the upper side into the chamber . Since the catalyst and the source gas are supplied from the upper side of the vertical reactor, the apparatus is provided with a catalyst dropping hole in a plurality of dispersion plates in order to prevent the channeling effect of the free-falling catalyst. Particularly, the plurality of dispersing plates of the above patent discloses a method of growing the carbon nanotubes by increasing the contact time with the gas while the catalyst is staying for a predetermined time on a dispersing plate in the form of a porous plate, .

However, in the case of a fluidized bed reactor in which a catalyst and a source gas are supplied from the bottom of the reactor, a fluidized bed is formed in the reaction bed filled with the bed material and the catalyst. The gas injected to the lower part of the dispersion plate and discharged to the upper part moves to the upper part of the reaction area in the form of bubbles, and the phenomenon occurs that the bubbles are combined and gassed and then exploded at the upper part of the reaction area. The explosive force of the bubbles causes the solid particles surrounding the mixed gas to rise excessively to the top. For example, in a fluidized bed reactor for producing a carbon nanostructure, a bubble explosion in the reaction region excessively raises the catalyst and the powder of the carbon nanostructure to the upper portion of the reactor main body. As a result, the contact between the raw gas and the catalyst is smooth And the solid particles are caused to flow out of the reactor, thereby reducing the yield of the product.

SUMMARY OF THE INVENTION The present invention has been made in order to solve the above-mentioned problems, and it is an object of the present invention to improve the yield of the carbon nanostructure manufacturing process and smoothly operate the fluidized bed reactor.

It is another object of the present invention to provide a fluidized bed reactor for producing carbon nanostructures having a horizontal baffle enabling efficient contact between a raw material gas and a catalyst.

In order to achieve the above object, according to the present invention, there is provided a reactor comprising: a reactor body having a reaction space formed therein;

A horizontal flow interrupting plate for vertically separating the reaction space, comprising: a frame member; and an upward flow suppressing member attached to the inside of the frame member and having a plurality of through holes formed therein;

A catalyst supply pipe for supplying a catalyst from the bottom of the reactor main body to the inside of the main body;

A reaction gas supply pipe connected to the lower portion of the reactor and supplying a reaction gas containing a carbon source, a reducing gas and an inert gas into the reactor; And

A product discharge pipe through which the carbon nanostructure and the mixed gas are discharged; And,

Wherein the catalyst, the carbon source, and the reactive gas react with each other while flowing in the reaction space to produce a carbon nanostructure.

According to an aspect of the present invention, there is further provided a diffusing plate disposed below the reaction space, wherein the at least one horizontal baffle plate is positioned at an upper portion of the diffusing plate.

According to another aspect of the present invention, the upward flow restraining member is formed by the grid members attached to the inside of the rim member.

According to another aspect of the present invention, the lift-up restraining member includes: a plurality of transverse members extending inside the frame member; And a plurality of first tilting members and a plurality of second tilting members provided between the plurality of transverse members, wherein the plurality of first tilting members and the plurality of second tilting members are inclined at an angle To the plurality of transverse members.

According to another aspect of the present invention, the ascending flow restraining member is constituted by forming a plurality of perforations in the flat plate member.

According to another aspect of the present invention, the ascending flow restraining member may be in the form of a sieve.

The horizontal baffle plate for a fluidized bed reactor and the fluidized bed reactor provided with the horizontal baffle plate for the fluidized bed reactor according to the present invention can prevent a bubble explosion in the reaction region inside the reactor body from excessively raising the powder of the catalyst and the carbon nanostructure to the upper part of the main body, So that a smooth reaction can be achieved. Also, solid particles such as catalyst and product are prevented from being separated from the reactor body, and consequently, the yield of the reaction product can be improved and a smooth process can be achieved.

1 schematically shows an example of a fluidized bed reactor for producing carbon nanotubes.
FIG. 2 shows a schematic configuration of a fluidized bed reactor for producing carbon nanotubes according to a preferred embodiment of the present invention.
3 is a perspective view showing a first embodiment of a horizontal baffle according to a preferred embodiment of the present invention.
4 is a perspective view showing a second embodiment of a horizontal baffle according to a preferred embodiment of the present invention.
5 is a perspective view showing a third embodiment of a horizontal baffle plate according to a preferred embodiment of the present invention.
6 is a perspective view showing a fourth embodiment of a horizontal interrupter according to a preferred embodiment of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS The invention will be described in more detail with reference to the embodiments of the invention shown in the accompanying drawings. It is to be understood, however, that the invention is not to be limited to the specific embodiments, but includes all modifications, equivalents, or alternatives falling within the spirit and scope of the present invention.

In the drawings, like reference numerals are used for similar elements.

The terms first, second, A, B, etc., may be used to describe various components, but the components are not limited by the terms, but may be used to distinguish one component from another Only.

The term " and / or " includes any one or a combination of the plurality of listed items.

It is to be understood that when an element is referred to as being "connected" or "connected" to another element, it is to be understood that other elements may be directly connected or connected, or intervening elements may be present.

The singular expressions include plural expressions unless otherwise specified.

It will be understood that the terms "comprises", "having", and the like have the same meanings as the features, numbers, steps, operations, elements, parts or combinations thereof described in the specification, Does not exclude the possibility that an operation, component, component, or combination thereof may be present or added.

FIG. 1 schematically shows the structure of a fluidized bed reactor for producing a carbon nanostructure. Such a fluidized bed reactor may be modified in various ways as required, but is not limited thereto.

Referring to the drawings, a fluidized bed reactor 1 has a reactor body 10, and a lower portion of the reactor body 10 is formed as a tapered region 10a. In order to heat the reactor body 10 to a high temperature, it is preferable that a heater 19 is provided outside the reactor body 10.

A raw material gas supply unit 12 is provided at the bottom of the fluidized bed reactor 1. The feed gas may be, for example, a reactive gas comprising a hydrocarbon-based gas for producing carbon nanotubes. The raw material gas is supplied to the inside of the reactor main body 10 through a raw material gas supply pipe 21 connected to the raw material gas supply unit 12. The feed gas may be preheated in the preheater 17 before being fed into the reactor body 10. The raw material gas is dispersed into the reaction space in the reactor main body 10 through the dispersing plate 13 by disposing the dispersing plate 13 below the reaction space formed inside the reactor main body 10.

A stretching part 11 may be provided on the upper part of the reactor body 10. The expander 11 is provided with a separator (not shown) for preventing the catalyst from reacting from the reactor body 10 and reaction products (for example, carbon nanostructure such as carbon nanotube or fiber) ) May be provided. A filter 18 is connected to the elongated portion 11 and the component gas filtered by the filter 18 is conveyed through the conveying pipe 23. On the other hand, a recirculation pipe 22 is connected to the expansion part 11 to recirculate part of the mixed gas discharged from the expansion part 11 to the raw material gas supply pipe 21 through the recirculation pipe 22.

A separator 14 is connected to one side of the upper portion of the reactor main body 10 through a pipe 24. The separator 14 is for separating the product from the mixed gas discharged from the reactor body 10, for example, for separating the mixed gas from the carbon nanostructure. A separator 14 is connected to one side of the reactor body 10 through a pipe 15 to collect a product such as carbon nanostructure. On the other hand, the catalyst supplier 16 is connected to the pipe 26 so that the catalyst can be supplied to the inside of the reactor main body 10 through the pipe 26. Although not shown in the drawing, the pipe 26 is provided with a blower so that the mixed gas separated from the separator 14 and the catalyst supplied from the catalyst feeder 16 can be fed into the reactor main body 10.

During the operation of the fluidized bed reactor, a fluidized bed is formed in the reaction bed filled with the bed material and the catalyst. The gas injected to the lower part of the dispersion plate 13 and discharged to the upper part moves to the upper part of the reaction area in the form of bubbles, and the phenomenon occurs that the bubbles coalesce and become larger and then explode at the upper part of the reaction area. Causing the surrounding solid particles to rise excessively to the top. For example, in a fluidized bed reactor for producing a carbon nanostructure, a bubble explosion in the reaction region excessively raises the catalyst and the powder of the carbon nanostructure to the upper portion of the reactor body 10, and consequently, the contact between the raw gas and the catalyst This does not happen smoothly. In addition, the elongated portion 11 is provided with devices for controlling the mixed gas which is separated from the reactor body 10. However, when the carbon nanostructure powder or the like excessively rises, the carbon nanostructure can be completely released It can not be prevented. Therefore, there is a problem that the yield of the carbon nanostructure is negatively affected or the entire process is obstructed.

Referring to FIG. 2, there is shown a schematic configuration of an apparatus for manufacturing a carbon nanotube according to a preferred embodiment of the present invention. The overall structure of the apparatus for producing carbon nanotubes shown in FIG. 2 is substantially similar to that of the reactor described with reference to FIG. 1, and the same components are denoted by the same reference numerals.

The carbon nanostructure manufacturing apparatus 1 includes a reactor body 10 having a reaction space formed therein, a heating unit 19 disposed outside the reactor body 10 for heating the reactor body 10, A dispersion plate 13 disposed below the reaction space formed in the interior of the body 10, and a stretching unit 11 provided on the body 10. A portion of the mixed gas separated at the elongating portion 11 is filtered at the filter 18 and is conveyed through the conveying pipe 23 and another portion of the mixed gas separated at the elongating portion 11 is conveyed to the recirculation discharge pipe 22 And is recycled to the raw gas feed pipe 21 through the feed pipe 21.

The carbon nanostructure manufacturing apparatus 1 further includes a separator 14 connected to one side of the upper portion of the reactor body 10, a collector 15 for recovering products such as carbon nanotubes separated from the separator 14, And a catalyst supplier 16 connected to one side of the bottom of the nanostructure manufacturing apparatus 1 for supplying the catalyst. At the bottom of the carbon nanostructure production apparatus 1, a raw material gas (reaction gas) supply unit 12 is provided. The raw material gas heated through the preheater 17 is supplied to the inside of the reactor main body 10 through the raw material gas supplying part 12 and the raw material gas is supplied to the reaction space of the reactor main body 10 through the dispersing plate 13 Dispersed.

According to an aspect of the present invention, at least one horizontal baffle plate 20 is provided inside the reactor body 10. 2, the horizontal baffle plate 20 is disposed so as to vertically separate the reaction space formed inside the reactor body 10 at the upper portion of the dispersion plate 13, and the raw gas, the catalyst, A plurality of through holes are formed so as to freely pass through the through hole, and it is an upward flow inhibiting member capable of suppressing an excessive upward flow. Even if the bubbles moving upward through the dispersing plate are merged and giant, the size of the bubbles decreases again as they pass through the through holes of the horizontal baffle plate 20, so that the contact area with the catalyst increases and efficient gas-solid mixing is possible .

In the example shown in FIG. 2, two horizontal interrupting plates 20 are disposed in a reaction space formed inside the reactor body 10, but this is merely an example, and in another example, 20 may be provided only one, or more than two may be provided.

The spacing of the horizontal baffle plates 20 in the reactor body and the size of the through holes are preferably determined in consideration of the size of the bubbles in the reaction zone, the particle size of the layer material, and the cross-sectional area of the reactor. Specifically, it is preferable to calculate the position where the contact area between the catalyst and the raw material gas is reduced to an appropriate level or less considering the size of the bubbles, and the size of the through hole is the maximum size of the particles The powder is free to move up and down in consideration of the diameter of the reactor and the coalesced bubbles in the reaction zone below the baffle plate 20 are re-dispersed while passing through the baffle plate 20, .

The horizontal baffle plate 20 serves to suppress the lifting force of the powder generated when the bubble explodes in the reaction zone. For example, in the fluidized bed reactor for producing carbon nanotubes, the horizontal obstruction plate 20 suppresses excessive rise of powder of the carbon nanotubes due to bubble explosion in the reaction zone. This is because, as can be seen from the embodiments shown in Figs. 3 to 6, the horizontal baffle plate 20 has a structure capable of suppressing the upward flow of the powder.

3 is a schematic perspective view of a first embodiment of a horizontal baffle plate for a fluidized bed reactor according to the present invention.

Referring to the drawing, the horizontal baffle plate 30 is provided with lattice members 32 on the inner side of a frame member 31 formed in a circular shape as a whole. The frame member 31 is configured to fit the cross section of the inner space of the reactor body 10. In the example shown in the drawing, the frame member 31 is formed in a circular shape because the reactor body 10 is cylindrical, but the shape of the frame member 31 is not limited to a circular shape and can take other shapes. A through hole 32a is formed between the lattice members 32. The lattice member 32 acts to substantially inhibit catalyst and solid product particles from rising excessively by bubble explosion within the reactor body 10. [ That is, the raw gas, the catalyst and the product can freely move through the through hole 32a formed in the horizontal baffle plate 30, but the large bubbles formed by the coalescence of the bubbles are resisted by the cross- As a result, the bubbles become small and the lift force is reduced, thereby preventing excessive synergism.

4 is a schematic perspective view of a second embodiment of a horizontal baffle plate for a fluidized bed reactor according to the present invention.

Referring to FIG. 1, the horizontal baffle plate 40 includes a generally circular frame member 41, and a plurality of transverse members 42 extend inside the frame member 41. A plurality of first inclined members 43 and a plurality of second inclined members 44 are attached between the transverse members 41. As shown in the drawing, a plurality of first inclined members 43 are attached to the transverse member 42 so as to be inclined at a predetermined angle with respect to the vertical direction, and a plurality of second inclined members 44 are also vertically And is attached to the transverse member 42 to be inclined at a constant angle. Preferably, the inclination angle of the first inclined members 43 and the inclination angles of the plurality of second inclined members 44 are equal to each other and are directed to the opposite direction. A plurality of first angled members 43 and a plurality of second transverse members 44 are alternately provided between the transverse members 42.

The transverse member 42, the plurality of first inclined members 43 and the plurality of second inclined members 44 provided in the horizontal baffle plate 40 are arranged in the reactor main body 10 in such a manner that the raw gas, So as to substantially inhibit the rise. That is, the raw gas, the catalyst and the product can freely move through the through holes formed between the transverse member 42 and the inclined members 43 and 44 in the horizontal baffle plate 40, but the large air bubbles formed by the coalescence of the bubbles, Sectional area of the member 42 and the inclined members 43 and 44. As a result, the size of the bubbles is reduced and the lifting force is reduced, thereby preventing excessive synergism.

5 is a schematic perspective view of a third embodiment of a horizontal baffle plate for a fluidized bed reactor according to the present invention.

Referring to the drawing, the horizontal baffle plate 50 is formed by forming a large number of perforations 52a in a flat plate member 52 provided inside a frame member 51. As shown in FIG. That is, a plurality of perforations 52a are formed in the flat plate member 52 having a predetermined thickness by using a perforating device (not shown), and the flat plate member 52 is attached to the inside of the frame member 51 will be.

The plate member 52 acts to substantially suppress the rise of the raw material gas, the catalyst and the product inside the reactor main body 10 in the horizontal interrupting plate 50. That is, the raw gas, the catalyst and the product can move freely through the perforations 52a, but the large bubbles formed by the coalescence of the bubbles are subjected to resistance by the cross-sectional area of the plate member 52, So that the excessive lift-up action is prevented.

6 is a schematic perspective view of a fourth embodiment of a horizontal baffle plate for a fluidized bed reactor according to the present invention.

Referring to the drawing, the horizontal baffle plate 60 is formed with a sieve-shaped member 62 inside the frame member 61, and the through-hole 62a formed in the sieve member 62 is a large- And acts to substantially prevent the catalyst and the solid product from excessively corresponding to bubble explosion by preventing bubble formation.

The horizontal baffle plate 30, 40, 50.60 described through the embodiment shown in Figs. 3 to 6 may be installed in the inner space of the reactor body 10 by one or more numbers. By the provision of the horizontal baffles 30, 40, 50 and 60, the excessive upward force of the raw gas, the catalyst and the product is suppressed, resulting in efficient contact between the raw gas and the catalyst, Can be prevented. Particularly, it is possible to prevent the powder of the carbon nanostructure from escaping to the outside of the reactor body 10 in the reactor for producing the carbon nanostructure.

10. Reactor body 11. Extension portion
12. Raw gas supply 13. Dispersion plate
21. Raw gas supply pipe 20. Horizontal baffle plate

Claims (6)

A reactor body having a reaction space formed therein;
A horizontal flow interrupting plate for vertically separating the reaction space, comprising: a frame member; and an upward flow suppressing member attached to the inside of the frame member and having a plurality of through holes formed therein;
A catalyst supply pipe for supplying a catalyst from the bottom of the reactor main body to the inside of the main body;
A reaction gas supply pipe connected to the lower portion of the reactor and supplying a reaction gas containing a carbon source, a reducing gas and an inert gas into the reactor; And
A product discharge pipe through which the carbon nanostructure and the mixed gas are discharged; And,
Wherein the catalyst, the carbon source, and the reactive gas react with each other while flowing in the reaction space to produce a carbon nanostructure. The method according to claim 1,
Further comprising a dispersion plate disposed below the reaction space,
Wherein the at least one horizontal baffle is positioned on top of the diffuser plate. The method according to claim 1,
Characterized in that the lift-up restraining member is formed by grating members attached to the inside of the rim member. The method according to claim 1,
Wherein the lift-up restraining member comprises:
A plurality of transverse members extending inside the frame member; And
A plurality of first inclined members and a plurality of second inclined members provided between the plurality of transverse members,
Wherein the plurality of first inclined members and the plurality of second inclined members are attached to the plurality of transverse members so as to be inclined at a predetermined angle with respect to a vertical direction. The method according to claim 1,
Wherein the lift-up restraining member comprises:
And forming a plurality of perforations in the flat plate member. The method according to claim 1,
Wherein the ascending flow restraining member is in the form of a sieve.

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