Device for continuously preparing single-walled carbon nanotubes
By setting up a filtration mechanism in the single-walled carbon nanotube preparation device to screen the catalyst particle size, the problems of low purity and limited yield of single-walled carbon nanotubes in the prior art are solved, achieving high purity and continuous production, and meeting the needs of large-scale industry.
Patent Information
- Application Number
- CN202610027537.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-09
- Publication Date
- 2026-02-27
AI Technical Summary
Existing technologies struggle to achieve continuous production of high-quality single-walled carbon nanotubes, and existing equipment has limited output, failing to meet market demand, resulting in low purity of the single-walled carbon nanotubes.
Design an apparatus for continuous preparation of single-walled carbon nanotubes, including a horizontal reaction unit and a discharge unit. A filtration mechanism is set between the gasification section and the growth section. By screening the catalyst particle size, the quality of the material entering the growth section is controlled, the generation of by-products is reduced, the influence of high-temperature turbulence is avoided, and the purity and yield of single-walled carbon nanotubes are improved.
It has achieved high purity (over 90%) and continuous production of single-walled carbon nanotubes, reduced subsequent purification costs, and has the capability for large-scale production.
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Figure CN121573669A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of nanomaterial preparation, in particular to a device for continuously preparing single-walled carbon nanotubes. BACKGROUND
[0002] Single-walled carbon nanotubes have excellent electronic, mechanical, and mechanical properties, and have ultra-high mobility for both electrons and holes. Therefore, single-walled carbon nanotubes are determined as the most likely new device material to be applied in the future. Continuous preparation of high-quality single-walled carbon nanotubes is the basis and key to the application of single-walled carbon nanotubes. Existing research on single-walled carbon nanotubes is basically in the laboratory research stage, and there is no report on industrial large-scale production in China. Although there are many reports on the preparation of carbon nanotubes in existing patent documents and papers, the products obtained are mostly single-walled and multi-walled carbon nanotubes and various structural carbon composites, and the content of single-walled carbon nanotubes is relatively low. Since the performance of single-walled carbon nanotubes is much better than that of multi-walled carbon nanotubes and various carbon composites, how to improve the purity of single-walled carbon nanotubes is a technical problem to be solved by those skilled in the art. In addition, most of the existing carbon nanotube preparation devices cannot produce continuously, and the yield is limited, which cannot meet the market demand. Therefore, it is imperative to seek a single-walled carbon nanotube preparation device that can not only improve the purity of single-walled carbon nanotubes but also meet the continuous production requirements. SUMMARY
[0003] To solve the above technical problems, the present application provides a device for continuously preparing single-walled carbon nanotubes, which can not only ensure a high content of single-walled carbon nanotubes in the product, reduce the cost of downstream purification treatment, and modular design to ensure the convenience of later maintenance, but also has the function of continuous production, which can meet the market demand of large-scale production.
[0004] The technical scheme provided by the present application is as follows: A device for continuously preparing single-walled carbon nanotubes, comprising a reaction unit of horizontal structure and a discharging unit, the discharging unit is arranged at the discharging end of the reaction unit, the reaction unit comprises a gasification section for gasification of catalyst and a growth section for mixing catalyst and carbon source to prepare single-walled carbon nanotubes, which are arranged in sequence along the horizontal direction, and a filtering mechanism for screening the particle size of the material entering the growth section is arranged between the gasification section and the growth section.
[0005] Preferably, the gasification section comprises a gasification chamber, a gas inlet assembly one for introducing inert gas and / or active gas, a crucible melt pool, and a plasma gun arranged in the gasification chamber; The discharge port of the plasma gun is arranged opposite to the crucible melt pool, and a conveying pipeline for introducing catalyst into the gasification chamber is arranged in the plasma gun; The air inlet assembly one is arranged on the side of the corresponding surface of the plasma gun and the crucible molten pool, and is away from the filtering mechanism.
[0006] Preferably, the air inlet assembly one is annularly arranged along the side of the gasification chamber to form a vortex gas flow in the gasification chamber.
[0007] Preferably, the filtering mechanism comprises a high-temperature-resistant hollow filter plate, The lower part of the hollow filter plate is a solid part, and the upper part of the hollow filter plate is a hollow part, and the hollow part is uniformly provided with a plurality of filter holes.
[0008] Preferably, the hollow filter plate is vertically arranged, and the number of the hollow filter plates is one layer, two layers or more than two layers, When the number of the hollow filter plates is two layers or more than two layers, the filter holes on the adjacent two hollow filter plates are arranged in a staggered manner.
[0009] Preferably, the length of the hollow part in the vertical direction accounts for 1 / 4 to 1 / 2 of the total length of the hollow filter plate.
[0010] Preferably, the diameter of the filter hole is 1 to 100 mm.
[0011] Preferably, the horizontal distance between the hollow filter plate and the plane where the air outlet end of the air inlet assembly one is located is 0.3 to 2 m.
[0012] Preferably, the growth section comprises a growth chamber, an air inlet assembly two for introducing a carbon source arranged at the feeding end of the growth chamber, and a temperature control assembly arranged along the inner wall of the growth chamber, The air inlet assembly two is annularly arranged along the feeding end of the growth chamber to form a vortex gas flow in the gasification chamber. The horizontal distance between the filtering mechanism and the air outlet of the air inlet assembly two is 5 to 300 mm.
[0013] Preferably, the growth chamber is provided with an extension structure as a cooling transition discharging section, the periphery of the extension structure is provided with a temperature monitoring assembly, and the discharging port of the extension structure is in communication with a discharging unit.
[0014] The present application has the following advantages over the prior art: 1. The device for continuously preparing single-walled carbon nanotubes of the present application controls the particle size of the material entering the growth section by arranging a filtering mechanism between the gasification section and the growth section, filters out useless coarse particle catalyst through the filtering mechanism, accurately controls the mass of the catalyst entering the growth section, reduces the generation of by-products (such as multi-walled carbon nanotubes, carbon spheres, free carbon, mixed carbon, etc.), and makes the content of single-walled carbon nanotubes in the obtained product higher, and the purity can reach more than 90%. 2、The device for continuously preparing single-wall carbon nanotubes of the present application sets the gasification section and the growth section separately, and the filter mechanism set between the gasification section and the growth section can also block the high-temperature turbulent flow generated by the plasma, greatly avoiding the influence of the high-temperature turbulent flow generated by the plasma on the thermal field and flow field of the subsequent growth section, and greatly improving the product quality. BRIEF DESCRIPTION OF DRAWINGS
[0015] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments described in the present application, and other drawings can also be obtained by those skilled in the art without creative labor.
[0016] Figure 1 The structure diagram of the device for continuously preparing single-wall carbon nanotubes in the embodiment of the present application; Figure 2 The structure diagram of the filter mechanism in the embodiment of the present application.
[0017] Reference signs: 1, reaction unit; 11, gasification section; 111, gasification chamber; 112, gas inlet assembly one; 113, crucible pool; 114, plasma gun; 12, growth section; 121, growth chamber; 122, gas inlet assembly two; 123, temperature control assembly; 13, filter mechanism; 131, filter hole; 14, cooling transition discharge section; 2, discharge unit; 21, scraping mechanism. DETAILED DESCRIPTION
[0018] In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only some of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.
[0019] As Figure 1 , 2As shown, the embodiment of the present application provides a device for continuously preparing single-walled carbon nanotubes, which comprises a reaction unit 1 of horizontal structure and a discharging unit 2 arranged at the discharging end of the reaction unit 1. The reaction unit 1 comprises a gasification section 11 for gasification of catalyst and a growth section 12 for mixing catalyst with carbon source to prepare single-walled carbon nanotubes, which are arranged in sequence along the horizontal direction. A filtering mechanism 13 for screening the particle size of the material entering the growth section is arranged between the gasification section 11 and the growth section 12. The filtering mechanism 13 mainly plays a screening role. The grain size of the catalyst generated from the gasification section 11 is uneven. If the catalyst is directly screened and enters the growth section for growth without screening, some catalysts with excessively large grain size may grow into multi-walled carbon nanotubes, various carbon, or a mixture of single-walled carbon nanotubes, multi-walled carbon nanotubes and various carbon, which will seriously affect the yield of the target product single-walled carbon nanotubes, resulting in unqualified products. After screening by the filtering mechanism 13, the grain size is uniform, and the single-walled carbon nanotubes required in the growth section 12 will be grown with a high probability, which can ensure that the purity of single-walled carbon nanotubes in the product is high.
[0020] In the embodiment, the gasification section 11 comprises a gasification chamber 111, a gas inlet assembly 112 for introducing inert gas and / or active gas arranged in the gasification chamber 111, a crucible pool 113, and a plasma gun 114. The discharge port of the plasma gun 114 is arranged opposite to the crucible pool 113. The plasma gun 114 is provided with a conveying pipeline for conveying catalyst into the gasification chamber 111. The crucible pool 113 can receive the catalyst conveyed from the plasma gun 114 and forms a temperature buffer zone to receive excess heat of the plasma gun, and then most of the conveyed catalyst is subjected to a gasification process after the plasma gun 114 is powered and arced. The gas inlet assembly 112 is arranged on one side of the corresponding surface of the plasma gun 114 and the crucible pool 113, and is located on the side away from the filtering mechanism 13. The gas inlet assembly 112 comprises a plurality of gas inlet pipes. The gas introduced into the gas inlet pipes is generally inert gas in the early stage to ensure the cleanliness and high-temperature flow field of the gasification section 12, which is beneficial to the smooth progress of the gasification process. The gas introduced into the gas inlet pipes is generally active gas in the later stage to facilitate the maintenance of catalyst activity. At the same time, the gas inlet assembly 112 and the filtering mechanism 13 are located on both sides of the corresponding surface of the plasma gun 114 and the crucible pool 113, which facilitates the screening of catalyst particles through the combined action of gas flow and gravity. The catalyst particles with large particle size move downward under the action of gravity and are blocked by the filtering mechanism 13 and cannot enter the growth section 12. The catalyst particles with small particle size pass through the filtering mechanism 13 and enter the growth section 12 to catalyze the carbon source to grow into single-walled carbon nanotubes.
[0021] In the embodiment, the air inlet assembly one 112 is arranged along the side of the gasification chamber 111 to form a vortex airflow in the gasification chamber 111, the vortex airflow carries the gasified catalyst particles to move in a vortex manner in the gasification chamber 111, and the catalyst particles move to the filtering mechanism during the movement. The catalyst particles reaching the filtering mechanism 13 are filtered and screened by the filtering mechanism 13, the catalyst particles with small particle sizes enter the growth section, and the catalyst particles with large particle sizes directly sink into the crucible pool 113 or enter the airflow again to fall into the crucible pool 113 by gravity to participate in the next gasification process.
[0022] In the embodiment, as shown in Figure 2 The filtering mechanism 13 includes a high-temperature-resistant hollow filter plate, the shape and size of the hollow filter plate are consistent with the shape and size of the end of the gasification chamber 111, the lower part of the hollow filter plate is a solid part, the upper part of the hollow filter plate is a hollow part, the hollow part is uniformly provided with a plurality of filter holes 131, the plurality of filter holes 131 can first form a group of filter holes along the same straight line, and then a plurality of groups of filter holes are arranged in a spiral manner on the upper part of the hollow filter plate along the center of the hollow filter plate (this is to form a matching arrangement with the vortex airflow in the gasification chamber 111 to facilitate improving the filtering efficiency), the filter holes 131 can be circular holes or long strip-shaped circular holes formed by milling a plurality of circular holes, because the catalyst particles with small particle sizes float in the upper part of the gasification chamber 111 and the catalyst particles with large particle sizes sink to the lower part of the gasification chamber 111, the hollow filter plate is provided with the hollow part only in the upper part to be matched with the screening by gravity.
[0023] In the embodiment, the hollow filter plate is vertically arranged, and the number of the hollow filter plates is one layer, two layers or more than two layers. When the number of the hollow filter plates is two layers or more than two layers, the filter holes on the adjacent two hollow filter plates are arranged in a staggered manner. The length of the hollow part in the vertical direction accounts for 1 / 4-1 / 2 of the total length of the hollow filter plate, which can well meet the requirement that a certain amount of particles pass through the hollow part to enter the growth section to prepare single-walled carbon nanotubes, ensure high production efficiency, ensure good quality of the prepared single-walled carbon nanotubes, and well block the influence of a large amount of high-temperature disordered turbulent flow generated by the plasma gun arc on the temperature field and flow field of the rear growth section.
[0024] In the embodiment, the diameter of the filter holes 131 is 1-100 mm, and the catalyst with a particle size meeting the requirement can be obtained.
[0025] In the embodiment, the horizontal distance between the hollow filter plate and the plane where the air outlet end of the air inlet assembly one 112 is located is 0.3-2 m, and the distance between the two is appropriate to play the effect of screening by combining the airflow and gravity.
[0026] In the embodiment, the growth section 12 comprises a growth chamber 121, a gas inlet assembly 122 arranged at the feed end of the growth chamber 121 for feeding the carbon source, and a temperature control assembly 123 arranged along the inner wall of the growth chamber 121. The gas inlet assembly 122 is arranged annularly along the feed end of the growth chamber 121 to form a vortex gas flow in the gasification chamber 111. The horizontal distance between the filtering mechanism 13 and the gas outlet of the gas inlet assembly 122 is 5-300 mm, which does not affect the smooth entry of the catalyst particles into the growth chamber, and can ensure that the carbon source and the catalyst are fully mixed and uniformly distributed under the action of the gas flow of the carbon source, so that the yield and purity of the single-walled carbon nanotubes are relatively high.
[0027] In the embodiment, the temperature control assembly 123 comprises a heating unit and a heat preservation unit. The heating unit can be an electromagnetic induction heating coil or other existing heating bodies. The heat preservation unit comprises a heat preservation layer (carbon felt, graphite felt, refractory fiber, etc.) arranged along the inner wall of the growth chamber. The inner cavity structure of the gasification chamber 111 and the growth chamber 121 is preferably made of graphite, silicon carbide, etc. high-temperature refractory layer to prevent slag from polluting the product.
[0028] In the embodiment, the carbon source can be methane, ethane, propane, propyne, acetylene, acetone, etc. gaseous or gas-liquid mixed organic matter containing carbon.
[0029] In the embodiment, the growth chamber 121 is provided with an extension structure as a cooling transition discharge section 14. The cooling transition discharge section 14 is filled with heat preservation refractory material, such as Figure 1 The heat preservation refractory material is gradually thinned to ensure that the high-temperature field of the growth section does not directly contact the water cooling jacket, so as to achieve uniformity of the temperature field without being affected. The extension structure is provided with a temperature monitoring assembly. The discharge outlet of the extension structure is communicated with the discharge unit 2. The cooling transition discharge section 14 can avoid excessively high temperature during discharge.
[0030] In the embodiment, the discharge unit 2 comprises a gas material discharge end and a solid material discharge end. The gas material comprises a mixture of inert gas and carbon source gas. The solid material is almost entirely the obtained product single-walled carbon nanotubes. Since the single-walled carbon nanotubes have strong agglomeration and adhesion, in order to better discharge, a movable scraping mechanism can be arranged in the discharge extension structure to assist in discharging, so as to avoid blockage of the discharge outlet and other phenomena.
[0031] The above description of the disclosed embodiments enables those skilled in the art to carry out or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. An apparatus for the continuous preparation of single-walled carbon nanotubes, characterized in that, The device includes a horizontally oriented reaction unit and a discharge unit. The discharge unit is located at the discharge end of the reaction unit. The reaction unit includes a gasification section for catalyst gasification and a growth section for mixing the catalyst with a carbon source to prepare single-walled carbon nanotubes, arranged sequentially along the horizontal direction. A filtration mechanism for screening the particle size of the material entering the growth section is provided between the gasification section and the growth section.
2. The apparatus for continuous preparation of single-walled carbon nanotubes according to claim 1, characterized in that, The vaporization section includes a vaporization chamber, an inlet assembly for introducing inert gas and / or active gas, a crucible molten pool, and a plasma gun, all of which extend into the vaporization chamber. The plasma gun's outlet is positioned directly opposite the crucible's molten pool, and the plasma gun is equipped with a delivery pipe for introducing catalyst into the gasification chamber. The air intake assembly is located on one side of the surface corresponding to the plasma gun and the crucible molten pool, and is located on the side away from the filtration mechanism.
3. The apparatus for continuous preparation of single-walled carbon nanotubes according to claim 2, characterized in that, The air intake assembly is arranged in a ring along the side of the vaporization chamber to create a vortex airflow within the vaporization chamber.
4. The apparatus for continuous preparation of single-walled carbon nanotubes according to claim 3, characterized in that, The filtration mechanism includes a high-temperature resistant perforated filter plate. The lower part of the perforated filter plate is a solid part, and the upper part of the perforated filter plate is a perforated part, with a number of filter holes evenly distributed in the perforated part.
5. The apparatus for continuous preparation of single-walled carbon nanotubes according to claim 4, characterized in that, The perforated filter plates are arranged vertically, and the number of perforated filter plates is one, two, or more. When there are two or more layers of perforated filter plates, the filter holes on two adjacent perforated filter plates are staggered.
6. The apparatus for continuous preparation of single-walled carbon nanotubes according to claim 5, characterized in that, The length of the hollowed-out portion along the vertical direction accounts for 1 / 4 to 1 / 2 of the total length of the hollowed-out filter plate.
7. The apparatus for continuous preparation of single-walled carbon nanotubes according to claim 4, characterized in that, The pore size of the filter is 1 to 100 mm.
8. The apparatus for continuous preparation of single-walled carbon nanotubes according to claim 4, characterized in that, The horizontal distance between the perforated filter plate and the plane where the air outlet of the air intake assembly is located is 0.3 to 2 m.
9. The apparatus for the continuous preparation of single-walled carbon nanotubes according to any one of claims 1-8, characterized in that, The growth section includes a growth chamber, an air inlet assembly II for introducing a carbon source located at the feed end of the growth chamber, and a temperature control assembly arranged along the inner wall of the growth chamber. The second air intake component is arranged in a ring along the feed end of the growth chamber to form a vortex airflow in the gasification chamber; The horizontal distance between the filter mechanism and the air outlet of the second air intake assembly is 5 to 300 mm.
10. The apparatus for the continuous preparation of single-walled carbon nanotubes according to any one of claims 1-8, characterized in that, The growth chamber is provided with an extension structure as a cooling transition discharge section. A temperature monitoring component is provided around the extension structure, and the discharge port of the extension structure is connected to the discharge unit.