Preparation equipment of single-walled carbon nanotube

By designing a removable connected catalyst assembly, the stability and connectivity problems of catalyst assembly in the arc discharge method of single-wall carbon nanotube preparation equipment are solved, and the continuous preparation and production stability of single-wall carbon nanotubes are achieved.

CN119113972APending Publication Date: 2024-12-13WANHUA CHEM GRP CO LTD
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Patent Information

Application Number
CN202411263018.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-10
Publication Date
2024-12-13

AI Technical Summary

Technical Problem

In the preparation of single-wall carbon nanotubes by arc discharge method, the stability and connectivity of the catalyst assembly are difficult to ensure continuous production, resulting in the problem of production interruption.

Method used

A single-wall carbon nanotube preparation device including a catalyst vaporization chamber is designed. The catalyst assembly is detachably connected through the catalyst accommodating part and the support part, and the cathode is detachably connected to the solid catalyst, realizing the split connection of the catalyst assembly for easy replacement. With maintenance, ensure production stability.

Benefits of technology

Through this equipment, the continuous preparation of single-wall carbon nanotubes is achieved, the stability of the production equipment is improved, the replacement and maintenance of catalyst components are facilitated, and the continuous and efficient production is ensured.

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Abstract

The invention discloses preparation equipment of a single-walled carbon nanotube, and belongs to the technical field of carbon nanotube production. The production equipment comprises a main reactor, wherein the main reactor comprises a catalyst gasification cavity; the arc plasma torch assembly and the catalyst assembly are mounted on the main reactor, respectively extend into the catalyst gasification cavity of the main reactor and are spaced by a set distance; the catalyst assembly comprises a catalyst accommodating part, and the catalyst accommodating part is used for accommodating a solid catalyst matched with the catalyst accommodating part in shape; a connecting hole for connecting a cathode is formed in the bottom of the catalyst accommodating part, the cathode penetrates through the connecting hole and is detachably connected to a solid catalyst, and the catalyst accommodating part is detachably connected to the main reactor through a supporting part. According to the invention, continuous production of the single-walled carbon nanotubes can be realized.
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Description

Technical Field

[0001] The invention relates to the technical field of carbon nanotube production, and in particular to a preparation device for single-walled carbon nanotubes. Background Art

[0002] Arc discharge method is one of the commonly used methods for preparing single-walled carbon nanotubes. The principle is to introduce carbon-containing gas into a vacuum container, use transition metal as catalyst to form a receiving electrode, and use tungsten needle as anode. Argon gas is broken down and ionized by the high voltage between the cathode and anode to form a stable arc. During the arc discharge process, the metal catalyst in the receiving electrode is vaporized and forms nano-scale droplets in the reaction container. The carbon-containing gas attaches to the metal droplets under the high temperature environment in the reaction container and dehydrogenates, thereby producing single-walled carbon nanotubes.

[0003] In the arc discharge method preparation equipment, the catalyst component needs to generate a reliable and stable arc with the arc plasma torch component on the one hand, and achieve conductive connection with the cathode on the other hand, which is a key part in the production and preparation of single-walled carbon nanotubes. Therefore, providing a preparation equipment that can ensure continuous production has become a technical problem to be solved by those skilled in the art. Summary of the invention

[0004] To this end, the present invention provides a single-walled carbon nanotube preparation device capable of realizing continuous production of single-walled carbon nanotubes.

[0005] In view of the above technical problems, the present invention provides the following technical solutions:

[0006] A single-wall carbon nanotube preparation device comprises: a main reactor, the main reactor comprises a catalyst gasification chamber; an arc plasma torch assembly and a catalyst assembly mounted on the main reactor, the two respectively extend into the catalyst gasification chamber of the main reactor and are spaced apart by a set distance; the catalyst assembly comprises a catalyst accommodating portion, the catalyst accommodating portion is used to accommodate a solid catalyst having a shape matching the catalyst accommodating portion; a connecting hole for connecting a cathode is provided at the bottom of the catalyst accommodating portion, the cathode is detachably connected to the solid catalyst through the connecting hole, and the catalyst accommodating portion is detachably connected to the main reactor via a supporting portion.

[0007] Specifically, in an optional embodiment, a first mounting seat is provided on the main reactor, a connecting edge is provided at the end of the first mounting seat, a connecting hole is provided on the connecting edge, and the catalyst containing portion is detachably connected to the connecting edge of the first mounting seat through a supporting portion.

[0008] Specifically, in an optional embodiment, it also includes a reactor shell covering the outside of the main reactor, and the first mounting seat extends from the main reactor to the outside of the reactor shell.

[0009] Specifically, in an optional embodiment, the support portion includes a support plate and a support sleeve arranged on one side of the support plate, the support plate is provided with a through hole connected to the support sleeve, the catalyst holding portion is supported on the upper side of the support plate, the cathode is inserted into the support sleeve and extends along the through hole into the inner side of the catalyst holding portion.

[0010] Specifically, in an optional embodiment, the catalyst assembly further includes a cathode cooling portion, and the cathode cooling portion includes a cooling cavity surrounding the outer side of the cathode, and the cooling cavity is connected to a cooling circulation system.

[0011] Specifically, in an optional embodiment, the catalyst housing portion is spaced apart from the inner wall of the first mounting seat, and at least one annular extension edge is provided on the inner wall of the first mounting seat, and the inner side wall of the annular extension edge abuts against the outer wall of the catalyst housing portion.

[0012] Specifically, in an optional embodiment, the annular extension is located between the main reactor and the reactor shell.

[0013] Specifically, in an optional embodiment, the catalyst assembly is located on the lower side of the catalyst gasification chamber of the main reactor, and a catalyst replenishing port is provided on the upper side of the catalyst gasification chamber of the main reactor. The catalyst replenishing port is connected to the catalyst feeding system through a catalyst replenishing pipeline passing through the reactor shell.

[0014] Specifically, in an optional embodiment, the arc plasma torch assembly is installed on the main reactor at an angle, and the catalyst assembly is installed on the main reactor in a vertical direction.

[0015] Specifically, in an optional embodiment, the main reactor also includes a carbon nanotube generation chamber connected to the catalyst gasification chamber, the catalyst gasification chamber extends in a horizontal direction and has a feed port at its first end, and the carbon nanotube generation chamber extends in a vertical direction and has a discharge port at its lower end.

[0016] The technical solution of the present invention has the following technical effects compared with the prior art:

[0017] In the single-walled carbon nanotube preparation equipment provided by the present invention, the catalyst assembly includes a catalyst holding portion for holding a solid catalyst, and the catalyst holding portion can be detachably connected to the main reactor through a support portion, so that the solid catalyst can be replaced as a whole, and the cathode is detachably connected to the solid catalyst through a connecting hole, so that the various parts of the catalyst assembly can be connected in a split manner, which is convenient for replacement and maintenance of the various parts, so as to further improve the production stability of the production equipment. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings, which will help to understand the objects and advantages of the present invention, wherein:

[0019] Figure 1 It is a structural schematic diagram of a specific embodiment of the single-walled carbon nanotube preparation device of the present invention;

[0020] Figure 2 It is a partial schematic diagram of a specific embodiment of the single-walled carbon nanotube preparation device of the present invention;

[0021] Figure 3 It is a partial schematic diagram of a specific embodiment of the single-walled carbon nanotube preparation device of the present invention;

[0022] Figure 4 It is a schematic diagram of an arc plasma torch assembly in the single-walled carbon nanotube preparation device of the present invention. DETAILED DESCRIPTION

[0023] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.

[0025] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0026] In addition, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0027] like Figure 1 , Figure 2 The figure shows a specific embodiment of the single-walled carbon nanotube preparation device of the present invention, which includes a main reactor 10, wherein the main reactor 10 includes a catalyst gasification chamber 10a and a carbon nanotube generation chamber 10b which are interconnected, wherein the catalyst gasification chamber 10a extends in a horizontal direction and a first end thereof is provided with a feed port 13, and the carbon nanotube generation chamber 10b extends in a vertical direction and a lower end thereof is provided with a discharge port 14; an arc plasma torch assembly 20 and a catalyst assembly 30 installed on the main reactor 10, both of which extend into the catalyst gasification chamber 10a of the main reactor 10 respectively and are spaced apart by a set distance; the catalyst assembly 30 includes a catalyst accommodating portion 31, wherein the catalyst accommodating portion 31 is used to accommodate a solid catalyst 32 having a shape matching the catalyst accommodating portion 31; a connecting hole for connecting a cathode 33 is provided at the bottom of the catalyst accommodating portion 31, wherein the cathode 33 is connected to the solid catalyst 32 through the connecting hole, and the catalyst accommodating portion 31 is detachably connected to the main reactor 10 through a supporting portion 34. A stable electric arc is generated between the arc plasma torch assembly 20 and the catalyst assembly 30, so that the solid catalyst 32 in the catalyst assembly 30 is vaporized and enters the catalyst gasification chamber 10a to form nanometer-scale droplets; the feed gas (such as carbon-containing organic matter such as methane) enters the catalyst gasification chamber 10a along the feed port 13 of the main reactor 10 and is cracked and dehydrogenated in a high-temperature environment of more than 3000°C, and the reaction product is attached to the catalyst droplets and enters the carbon nanotube generation chamber 10b along the catalyst gasification chamber 10a to complete the growth and finally form single-walled carbon nanotubes and are discharged along the discharge port 14, thereby realizing the continuous preparation of single-walled carbon nanotubes.

[0028] In the single-walled carbon nanotube preparation equipment, the catalyst assembly 30 includes a catalyst holding portion 31 for holding a solid catalyst 32, and it can be detachably connected to the main reactor 10 through a support portion 34, which can realize the overall replacement of the solid catalyst 32. The cathode 33 is connected to the solid catalyst 32 through the connecting hole, realizing the split connection of the catalyst assembly 30, which is convenient for the replacement and maintenance of each part, so as to further improve the production stability of the production equipment.

[0029] Specifically, the solid catalyst 32 is usually made of metal materials such as iron, cobalt, nickel, molybdenum, etc., and the cathode 33 is usually made of transition metal materials such as copper, silver, etc.

[0030] In an optional embodiment, the main reactor 10 is provided with a first mounting seat 11 extending in a vertical direction, a connecting edge 111 is provided at the end of the first mounting seat 11, a connecting hole is provided on the connecting edge 111, and the catalyst holding portion 31 is detachably connected to the connecting edge 111 of the first mounting seat 11 through a supporting portion 34.

[0031] The production equipment also includes a reactor shell 40 that is covered on the outside of the main reactor 10, and a heat-insulating material is filled between the reactor shell 40 and the main reactor 10. Since the single-walled carbon nanotubes have a high requirement for the reaction temperature, in order to ensure the temperature stability of the catalyst gasification chamber 10a and the carbon nanotube generation chamber 10b, the heat-insulating material between the reactor shell 40 and the main reactor 10 can avoid excessive changes in the reaction temperature. The arc plasma torch assembly 20 and the catalyst assembly 30 extend into the inside of the main reactor 10 along the reactor shell 40, wherein the first mounting seat 11 extends from the main reactor 10 to the outside of the reactor shell 40.

[0032] Specifically, in a specific embodiment, the support portion 34 includes a support plate 341 and a support sleeve 342 disposed on one side of the support plate 341, the support plate 341 is provided with a through hole communicating with the support sleeve 342, the catalyst accommodating portion 31 is supported on the upper side of the support plate 341, and the cathode 33 is inserted into the support sleeve 342 and extends into the inner side of the catalyst accommodating portion 31 along the through hole. More specifically, a threaded hole is provided on the solid catalyst 32, and the cathode 33 is threadedly connected to the solid catalyst 32 to achieve a detachable connection between the cathode 33 and the solid catalyst 32, so that when replacing the solid catalyst 32, the cathode 33 can be removed first to facilitate the reuse of the cathode 33.

[0033] Specifically, since the cathode 33 is located outside the reactor housing 40, in order to avoid safety hazards caused by excessive temperature in the cathode 33 area, the catalyst assembly 30 also includes a cathode cooling unit, which includes a cooling chamber 351 surrounding the outside of the cathode 33, and the cooling chamber 351 is connected to a cooling circulation system. The cooling circulation system is used to circulate a coolant to achieve heat exchange between the cooling chamber 351 and the cathode 33.

[0034] More specifically, the two opposite sides of the cooling chamber 351 are connected to the cooling circulation system through cooling pipes 352 fixedly connected thereto, and the two cooling pipes 352 are connected to the cooling liquid supply pipe and the cooling liquid discharge pipe of the cooling circulation system through detachable connection structures such as flange structures. When the catalyst assembly 30 is disassembled to replace the solid catalyst 32, the connection between the cathode cooling part and the cooling circulation system is firstly released by disassembling the flange structure, and then the connection structure between the support part 34 and the first mounting seat 11 is released to realize the disassembly of the catalyst assembly 30.

[0035] Specifically, the catalyst holding portion 31 is spaced apart from the inner wall of the first mounting seat 11 to facilitate the installation and removal of the catalyst holding chamber. In order to prevent the heat in the main reactor 10 from being directly transferred to the outside of the reactor, at least one annular extension edge 112 is provided on the inner wall of the first mounting seat 11, and the inner side wall of the annular extension edge 112 abuts against the outer wall of the catalyst holding portion 31 to isolate the catalyst gasification chamber 10a of the main reactor 10 from the outside.

[0036] Specifically, the annular extension edge 112 is located between the main reactor 10 and the reactor housing 40, more specifically, the annular extension edge 112 is flush with the inner wall of the area where the main reactor 10 is located, so as to avoid heat loss as much as possible and prevent the gasified catalyst from forming droplets on the side of the annular extension edge 112 and accumulating in this area.

[0037] Specifically, in an optional embodiment, the arc plasma torch assembly 20 includes a plasma generating body 21 and an anode 22 installed inside the plasma generating body 21, the anode 22 includes a conductive tube 221 extending along a first direction and an emission nozzle 222 located at the end of the conductive tube 221; the conductive tube 221 is electrically connected to an arc generator, and the arc generator is controlled to be turned on so that an arc can be generated between the anode 22 of the arc plasma torch assembly 20 and the catalyst surface of the catalyst assembly 30; a gas channel is provided in the conductive tube 221 and the emission nozzle 222 for supplying a protective gas. More specifically, the anode 22 is made of metal tungsten, and the protective gas is argon, which is broken down and ionized by the high voltage between the cathode and cathode to form a stable arc.

[0038] The catalyst assembly 30 is located at the lower side of the catalyst gasification chamber 10a of the main reactor 10 and is installed on the main reactor 10 in a vertical direction, and the arc plasma torch assembly 20 is located at the upper side of the catalyst gasification chamber 10a of the main reactor 10 and is installed obliquely on the main reactor 10. When the arc heats the solid catalyst 32 at high temperature, the high-temperature catalyst liquid will sputter to the surroundings, and the anode 22 of the arc plasma torch assembly 20 is tilted at a certain angle (e.g., 30°-60°) to the upper surface of the solid catalyst 32 so that the argon gas blown from the surrounding of the emission nozzle 222 can quickly blow away the sputtered droplets, so that the anode 22 is not easily sputtered and ablated by the catalyst liquid.

[0039] After an arc is generated between the arc plasma torch assembly 20 and the catalyst assembly 30 to gasify the metal catalyst, the amount of catalyst in the catalyst receiving portion 31 gradually decreases, which will cause the gap between the arc plasma torch assembly 20 and the catalyst assembly 30 to be too large, and the gap between the two is insufficient to generate a stable arc, which eventually leads to the problem of production interruption. In order to ensure the continuous preparation of single-walled carbon nanotubes, a catalyst replenishing port 12 is provided on the upper side of the catalyst gasification chamber 10a of the main reactor 10, and the catalyst replenishing port 12 is connected to the catalyst feeding system through a catalyst replenishing pipeline 60 that penetrates the reactor housing 40. When the gap between the arc plasma torch assembly 20 and the catalyst assembly 30 is greater than the set threshold, the granular metal catalyst is allowed to enter the catalyst receiving portion 31 along the catalyst replenishing pipeline 60 and the catalyst replenishing port 12 by controlling the switch valve on the catalyst replenishing pipeline 60.

[0040] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. However, the obvious changes or modifications derived therefrom are still within the scope of protection of the present invention.

Claims

1. A single-walled carbon nanotube preparation device, characterized in that: include: A main reactor, the main reactor comprising a catalyst gasification chamber; An arc plasma torch assembly and a catalyst assembly mounted on the main reactor, both of which extend into the catalyst gasification chamber of the main reactor and are spaced apart by a set distance; The catalyst assembly includes a catalyst holding portion, which is used to hold a solid catalyst whose shape matches the catalyst holding portion; a connection hole for connecting a cathode is provided at the bottom of the catalyst holding portion, and the cathode is detachably connected to the solid catalyst through the connection hole; the catalyst holding portion is detachably connected to the main reactor via a supporting portion.

2. The single-walled carbon nanotube preparation device according to claim 1, characterized in that: The main reactor is provided with a first mounting seat, the end of the first mounting seat is provided with a connecting edge, the connecting edge is provided with a connecting hole, and the catalyst containing part is detachably connected to the connecting edge of the first mounting seat through a supporting part.

3. The single-walled carbon nanotube preparation device according to claim 2, characterized in that: It also includes a reactor shell which is covered on the outside of the main reactor, and the first mounting seat extends from the main reactor to the outside of the reactor shell.

4. The single-walled carbon nanotube preparation device according to claim 1, characterized in that: The support portion includes a support plate and a support sleeve arranged on one side of the support plate, the support plate is provided with a through hole connected to the support sleeve, the catalyst containing portion is supported on the upper side of the support plate, the cathode is inserted into the support sleeve and extends into the inner side of the catalyst containing portion along the through hole.

5. The single-walled carbon nanotube preparation device according to claim 1, characterized in that: The catalyst assembly further includes a cathode cooling portion, wherein the cathode cooling portion includes a cooling cavity surrounding the outer side of the cathode, and the cooling cavity is communicated with a cooling circulation system.

6. The single-walled carbon nanotube preparation device according to claim 2, characterized in that: The catalyst containing portion is spaced apart from the inner wall of the first mounting seat. The inner wall of the first mounting seat is provided with at least one annular extension edge, and the inner side wall of the annular extension edge abuts against the outer wall of the catalyst containing portion.

7. The single-walled carbon nanotube preparation device according to claim 6, characterized in that: The annular extension is located between the main reactor and the reactor shell.

8. The single-walled carbon nanotube preparation device according to claim 1, characterized in that: The catalyst assembly is located at the lower side of the catalyst gasification chamber of the main reactor. A catalyst replenishing port is provided at the upper side of the catalyst gasification chamber of the main reactor. The catalyst replenishing port is connected to the catalyst feeding system through a catalyst replenishing pipeline penetrating the reactor shell.

9. The single-walled carbon nanotube preparation device according to claim 1, characterized in that: The arc plasma torch assembly is installed on the main reactor at an angle, and the catalyst assembly is installed on the main reactor in a vertical direction.

10. The single-walled carbon nanotube preparation device according to claim 1, characterized in that: The main reactor also includes a carbon nanotube generation chamber connected to the catalyst gasification chamber, the catalyst gasification chamber extends horizontally and has a feed port at its first end, and the carbon nanotube generation chamber extends vertically and has a discharge port at its lower end.