Cooling and feeding mechanism for preparing carbon nanotubes
By setting a cooling jacket and cooling chamber in the furnace tube feed section and using the cooling medium to absorb heat, the problem of premature volatilization of catalyst precursors under high temperature conditions was solved, thus achieving efficient preparation and safe operation of carbon nanotubes.
Patent Information
- Application Number
- CN202423049636.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-11
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2034-12-11
AI Technical Summary
During the preparation of carbon nanotubes, the high-temperature environment in the furnace tube feed section causes the catalyst precursor to volatilize prematurely, reducing the yield and increasing operational safety risks.
A cooling feeding mechanism is designed, including a furnace tube feeding section and a cooling jacket. The cooling medium flows in the cooling chamber to absorb heat, reduce the feeding temperature, and prevent the catalyst precursor from volatilizing prematurely at the furnace tube feeding end and reacting with the raw material gas.
This effectively reduced the temperature of the furnace tube feed section, ensuring that the catalyst precursor volatilized within a specific temperature range, thus improving yield and operational safety.
Smart Images
Figure CN223517474U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the preparation technical field of carbon nanotube, concretely relates to a kind of cooling feeding mechanism of preparation carbon nanotube. BACKGROUND
[0002] Carbon nanotube, also known as buckytube, is a kind of one-dimensional quantum material with special structure, its radial dimension is nanometer order, axial dimension is micron order, and both ends of the tube are basically sealed.Carbon nanotube is mainly composed of carbon atoms arranged in hexagon, which forms coaxial circular tube with several to dozens of layers.The distance between layers is fixed, about 0.34 nm, and the diameter is generally 2-20 nm.
[0003] According to the number of layers of graphene, carbon nanotubes are divided into single-walled carbon nanotubes and multi-walled carbon nanotubes, among which single-walled carbon nanotubes are more advantageous, which is reflected in the following aspects: simple structure, stable chemical properties, few structural defects, excellent electrical conductivity, good elasticity and high mechanical properties.
[0004] The ton-level production of early carbon nanotubes is realized by fixed bed / moving bed equipment.In a horizontally placed tube furnace, through ingenious devices, the continuous addition of catalyst and hydrocarbon raw materials and the continuous output of carbon nanotube products are realized, which can realize the production of first-generation carbon nanotube factory of several tons to dozens of tons per year per equipment.
[0005] Single-walled carbon nanotubes or some special raw materials as carbon source for carbon nanotube production are usually based on traditional equipment such as fluidized bed for modification, which can effectively improve the yield of multi-walled carbon nanotubes, but the yield of single-walled carbon nanotubes is still low, and the actual annual production capacity of a single equipment is only 30-50 kg.
[0006] Currently, in the development and design of larger-scale single-walled carbon nanotube production equipment, there is still a problem of pre-volatilization of raw materials.The preparation of carbon nanotubes by tube furnace involves a high-temperature environment, and the environmental temperature of the furnace tube feeding part is high.If not cooled in time, the raw materials will volatilize completely before reacting with the raw material gas after entering the furnace tube, not only reducing the yield, but also greatly increasing the operation safety of operators. SUMMARY
[0007] In view of the deficiencies of the prior art, the utility model provides a cooling feeding mechanism for preparing carbon nanotubes, which aims to reduce the feeding temperature of the furnace tube feeding part, avoid the pre-volatilization of catalyst precursors at the feeding end of the furnace tube, ensure that the catalyst precursors can volatilize in a specific temperature zone and react with the raw material gas, and at the same time ensure the operation safety of operators.
[0008] In order to achieve the above object, the utility model provides a kind of cooling feeding mechanism for preparing carbon nanotube, it is arranged in the feeding end of tubular heating furnace, including furnace tube feeding part and cooling jacket;The furnace tube feeding part is arranged in the feeding end of furnace tube, and there is operating port in the furnace tube feeding part;The feeding conduit is inserted into the furnace tube by the operating port;The outer wall of the furnace tube feeding part is wrapped with cooling jacket, and there is space between the cooling jacket and the outer wall of the furnace tube feeding part, forming cooling cavity for cooling medium to flow.
[0009] By the cooperation of furnace tube feeding part, cooling jacket and cooling cavity, the feeding conduit transports catalyst precursor into the furnace tube, and the cooling medium can flow in the cooling cavity to absorb the heat emitted by the furnace tube, reduce the feeding temperature of the furnace tube feeding part, avoid the catalyst precursor from volatilizing in advance, and ensure that the catalyst precursor can volatilize in a specific temperature zone and react with raw material gas.
[0010] Further, the lower part of the cooling jacket is connected with a liquid inlet pipe, and the upper part of the cooling jacket is connected with a liquid outlet pipe; the liquid inlet pipe and the liquid outlet pipe communicate with the cooling cavity. The cooling medium enters the cooling cavity from the liquid inlet pipe at the lower part of the cooling jacket, flows out from the liquid outlet pipe at the upper part after absorbing the heat emitted by the furnace tube, which helps to reduce the feeding temperature of the furnace tube feeding part.
[0011] Further, the liquid inlet pipe and the liquid outlet pipe are both elbow pipes; the pipe opening of the liquid inlet pipe is arranged upward, and the pipe opening of the liquid outlet pipe is arranged downward. The elbow type liquid inlet pipe and the elbow type liquid outlet pipe can change the direction of the cooling medium, realize cooling circulation, and the sealing performance of the elbow pipe is better than that of straight pipe, so that the cooling medium can enter and exit more conveniently and reliably.
[0012] Further, the feeding end of the furnace tube is provided with a furnace tube cover which can be opened and closed, and a handle is fixedly installed on the furnace tube cover. After the preparation of carbon nanotube by the tubular heating furnace is completed, the operator can open the furnace tube cover to clean the remaining reaction raw materials in the furnace tube in time.
[0013] Further, the operating port is arranged outside the furnace tube cover, and the operating port has a flange opening at the end away from the furnace tube cover, and the sealing connection plate is detachably connected with the flange opening. For example, the detachable connection is realized by bolts, clamps and other connecting members.
[0014] Further, a locking ring is arranged on the furnace tube feeding part at the end close to the cooling jacket, and the end part of the cooling jacket is fixedly installed on the locking ring.
[0015] Further, a group of fastening bolts are arranged on the end of the locking ring towards the cooling jacket, and the fastening bolts are inserted into the cooling jacket.
[0016] Further, the set of fastening bolts is provided with six or more; the fastening bolts are equally divided on the surface of the locking ring. By setting a set of evenly distributed fastening bolts, the cooling jacket can be firmly fixed on the locking ring.
[0017] Further, a fixing assembly is arranged below the furnace tube feeding part; the fixing assembly comprises a mounting plate, a fixing seat, a support rod, a connecting plate and a fastening nut; the mounting plate is arranged below the furnace tube feeding part, and the fixing seat is arranged on the mounting plate; the bottom of the support rod is fixed on the fixing seat; a pair of connecting plates are arranged on both sides of the furnace tube feeding part, and the top of the support rod penetrates through the connecting plates; and the fastening nut penetrates through the support rod to lock the support rod on the connecting plates.
[0018] Further, the furnace tube away from one end of the furnace tube feeding part is provided with a collection bin for collecting carbon nanotubes.
[0019] Further, the tubular heating furnace comprises at least one furnace tube, a heat insulating body, a cooling cover and a protective shell; the periphery of the furnace tube is provided with the heat insulating body, the outside of the heat insulating body is provided with the cooling cover, and the outside of the cooling cover is further provided with the protective shell; the protective shell blocks the periphery of the furnace tube and leaves an operation window at the feeding end of the furnace tube, and the operation window is used for arranging the furnace tube feeding part.
[0020] Further, the periphery of the furnace tube is provided with the heat insulating body, and a space is formed between the heat insulating body and the outer wall of the furnace tube; the space is divided into a plurality of heating cavities arranged along the length direction of the furnace tube, so that the space in the furnace tube corresponds to form a plurality of temperature zones; and the heating element and the temperature detection element are arranged in the heating cavities.
[0021] Further, a plurality of gas inlet pipes are led out from the side wall of the furnace tube and along the length direction of the furnace tube, and each gas inlet pipe is in communication with the inside of the furnace tube, so as to supply raw material gas to different temperature zones in the furnace tube.
[0022] Beneficial effects
[0023] The furnace tube feeding part, the feeding conduit, the cooling jacket and the cooling cavity are cooperatively arranged; the catalyst precursor is conveyed into the furnace tube through the feeding conduit; the cooling medium can flow in the cooling cavity to absorb the heat emitted by the furnace tube, so that the feeding temperature of the furnace tube feeding part is reduced, the catalyst precursor is prevented from being volatilized in advance at the feeding end of the furnace tube, the catalyst precursor can be volatilized in a specific temperature zone and react with the raw material gas, and the operation safety of the operator is ensured. BRIEF DESCRIPTION OF DRAWINGS
[0024] Figure 1 It is a schematic diagram of the overall structure of the tubular heating furnace;
[0025] Figure 2 Structure diagram of cooling feed mechanism for preparing carbon nanotube;
[0026] Figure 3 and Figure 4 Structure diagram of internal structure of tubular heating furnace;
[0027] Figure 5 and Figure 6 Structure diagram of furnace tube;
[0028] Figure 7 Front view diagram of furnace tube feed part;
[0029] Figure 8 Sectional view diagram of A-A of Figure 7 ;
[0030] Figure 9 Enlarged diagram of B in Figure 8 .
[0031] In the drawings: 1, furnace tube; 11, furnace tube feed part; 12, furnace tube cover; 121, handle; 13, operation port; 131, sealing connecting plate; 14, feed conduit; 15, locking ring; 151, fastening bolt; 16, air inlet pipe; 2, cooling jacket; 21, cooling cavity; 22, liquid inlet pipe; 23, liquid outlet pipe; 3, fixing assembly; 31, mounting plate; 32, fixing seat; 33, support rod; 34, connecting plate; 35, fastening nut; 4, collection bin; 5, heat insulation body; 51, heating cavity; 6, cooling cover; 7, protective shell. DETAILED DESCRIPTION
[0032] The embodiments of the present application are described in detail below, and the following described embodiments are exemplary and are intended to explain the present application, and cannot be understood as limiting the present application.
[0033] The preparation of carbon nanotube is to carry out high temperature reaction of raw materials containing hydrogen, catalyst precursor, growth promoter precursor and carbon source in a tubular heating furnace, the catalyst precursor is decomposed and collision-reduced into catalyst particles, the carbon source is decomposed and dissolved into the catalyst on the surface of the catalyst under the action of the catalyst, diffuses and then precipitates carbon cap, the continuous carbon source supply makes the carbon cap elongate to form carbon nanotube, and the carbon nanotube flows to the tail end of the reaction cavity with hydrogen, and finally forms macroscopic single-walled carbon nanotube of different morphologies such as thin film or sponge.
[0034] As Figure 1 , Figure 3 and Figure 4As shown, the tubular furnace includes at least one furnace tube 1, a heat insulation body 5, a cooling shroud 6, and a protective outer shell 7. The heat insulation body 5 is disposed around the outer periphery of the furnace tube 1, the cooling shroud 6 is disposed outside the heat insulation body 5, and the protective outer shell 7 is disposed outside the cooling shroud 6. The protective outer shell 7 blocks the periphery of the furnace tube 1 and provides an operating window at the feed end of the furnace tube 1 for housing the furnace tube feed section 11. The furnace tube 1 is a high-temperature resistant pipe used to contain reactants and provide heating and reaction space. The heat insulation body 5 is made of a high-temperature resistant, low-thermal-conductivity insulating material. The cooling shroud 6 helps to remove excess heat generated during the operation of the tubular furnace, protects external equipment and the environment from high temperatures, and helps control the overall temperature distribution of the tubular furnace.
[0035] like Figure 4 As shown, a heat insulation body 5 is provided around the outer periphery of the furnace tube 1. A gap exists between the heat insulation body 5 and the outer wall of the furnace tube 1, dividing the space into multiple heating chambers 51 arranged along the length of the furnace tube 1, thus forming multiple temperature zones within the furnace tube 1. Heating elements and temperature detection elements are installed within each heating chamber 51. The multiple heating chambers 51 can control the heating temperature of different temperature zones. The heating elements heat the heating chambers 51, and the temperature detection elements detect the temperature of the heating chambers 51, providing accurate and real-time temperature detection.
[0036] like Figure 4 As shown, multiple air inlet pipes 16 extend from the side wall of furnace tube 1 along its length. Each air inlet pipe 16 is connected to the interior of furnace tube 1 to supply raw material gas to different temperature zones within the furnace tube 1. By setting multiple air inlet pipes 16, it is ensured that the carbon nanotubes are supplied with the required raw material gas to different temperature zones at different growth stages, thereby improving carbon source utilization, shortening catalyst particle agglomeration time, and ultimately increasing the yield of single-walled carbon nanotubes.
[0037] like Figure 2 , Figure 7 and Figure 8 As shown, in this embodiment, the cooling feeding mechanism for preparing carbon nanotubes is set at the feeding end of the tubular heating furnace, including a furnace tube feeding section 11 and a cooling jacket 2; the furnace tube feeding section 11 is set at the feeding end of the furnace tube 1, and an operation port 13 is provided in the furnace tube feeding section 11; the feeding conduit 14 passes through the operation port 13 and extends into the furnace tube 1; the outer wall of the furnace tube feeding section 11 is wrapped with the cooling jacket 2, and a space is reserved between the cooling jacket 2 and the outer wall of the furnace tube feeding section 11 to form a cooling chamber 21 for the flow of cooling medium; a collection bin 4 for collecting carbon nanotubes is provided at one end of the furnace tube 1 away from the furnace tube feeding section 11.
[0038] Through the cooperation of the furnace tube feeding part 11, the cooling jacket 2 and the cooling cavity 21, the feeding conduit 14 can transport the catalyst precursor into the furnace tube 1, the cooling medium can flow in the cooling cavity 21 to absorb the heat emitted by the furnace tube 1, reduce the feeding temperature of the furnace tube feeding part 11, avoid the catalyst precursor from being volatilized in advance, ensure that the catalyst precursor can be volatilized in a specific temperature zone and react with the raw material gas, and ensure the operation safety of the operator.
[0039] As shown in Figure 5 and Figure 6 , in the embodiment, the lower part of the cooling jacket 2 is connected with a liquid inlet pipe 22, and the upper part of the cooling jacket 2 is connected with a liquid outlet pipe 23; the liquid inlet pipe 22 and the liquid outlet pipe 23 communicate with the cooling cavity 21. The cooling medium enters the cooling cavity 21 from the liquid inlet pipe 22 at the lower part of the cooling jacket 2, flows out from the liquid outlet pipe 23 at the upper part after absorbing the heat emitted by the furnace tube 1, and helps to reduce the feeding temperature of the furnace tube feeding part 11. The liquid inlet pipe 22 and the liquid outlet pipe 23 are both elbow pipes; the pipe opening of the liquid inlet pipe 22 is arranged upward, and the pipe opening of the liquid outlet pipe 23 is arranged downward. The elbow type liquid inlet pipe 22 and the elbow type liquid outlet pipe 23 can change the inlet and outlet directions of the cooling medium, realize the cooling circulation, and the sealing performance of the elbow pipe is better than that of the straight pipe, so that the inlet and outlet of the cooling medium are more convenient and reliable.
[0040] As shown in Figure 6 and Figure 9 , in the embodiment, the feeding end of the furnace tube 1 is provided with a furnace tube cover 12 which is arranged in an openable and closable manner; and a handle 121 is fixedly installed on the furnace tube cover 12. Through the cooperation of the furnace tube cover 12 and the handle 121, after the preparation process of carbon nanotubes by the tubular heating furnace is completed, the operator can open the furnace tube cover 12 to clean the remaining reaction raw materials in the furnace tube 1 in time. The operation port 13 is arranged outside the furnace tube cover 12; one end of the operation port 13 away from the furnace tube cover 12 is provided with a flange opening, and the sealing connection plate 131 is detachably connected with the flange opening. For example, the detachable connection is realized through connecting members such as bolts and clamps.
[0041] As shown in Figures 6 to 8 , in the embodiment, a locking ring 15 is sleeved on the furnace tube feeding part 11 close to one end of the cooling jacket 2; and the end part of the cooling jacket 2 is fixedly installed on the locking ring 15. The locking ring 15 is provided with a group of fastening bolts 151 toward one end of the cooling jacket 2; and the fastening bolts 151 penetrate into the cooling jacket 2. The group of fastening bolts 151 is provided with six or more than six; and the fastening bolts 151 are equally divided on the ring surface of the locking ring 15. Through the arrangement of the group of evenly distributed fastening bolts 151, the cooling jacket 2 can be fixed on the locking ring 15 firmly.
[0042] As shown in Figure 2As shown, in the embodiment, the fixed assembly 3 is arranged below the furnace tube feeding part 11; the fixed assembly 3 comprises a mounting plate 31, a fixed seat 32, a support rod 33, a connecting plate 34 and a fastening nut 35; the mounting plate 31 is arranged below the furnace tube feeding part 11, and the fixed seat 32 is arranged on the mounting plate 31; the bottom of the support rod 33 is fixed on the fixed seat 32; a pair of connecting plates 34 are arranged on both sides of the furnace tube feeding part 11 in an extending manner, and the top of the support rod 33 penetrates through the connecting plates 34; and the fastening nut 35 penetrates through the support rod 33 to lock the support rod 33 on the connecting plates 34. The fixed assembly 3 plays a role of supporting and fixing the furnace tube feeding part 11.
[0043] The above embodiments are exemplary, and the purpose is to illustrate the technical concept and characteristics of the utility model, so that the person skilled in the art can understand the content of the utility model and implement it, and the protection scope of the utility model cannot be limited by this. Any equivalent change or modification according to the spirit and essence of the utility model should be covered in the protection scope of the utility model.
Claims
1. A cooling feed mechanism for preparing carbon nanotubes, characterized by: The application discloses a feeding end of a tubular heating furnace, which comprises a furnace tube feeding part (11) and a cooling jacket (2). The furnace tube feeding part (11) is arranged at the feeding end of a furnace tube (1), and an operation port (13) is arranged on the furnace tube feeding part (11). A feeding pipe (14) penetrates the operation port (13) and extends into the furnace tube (1). The outer wall of the furnace tube feeding part (11) is wrapped with the cooling jacket (2), and a space is reserved between the inner wall of the cooling jacket (2) and the outer wall of the furnace tube feeding part (11) to form a cooling cavity (21) for cooling medium.
2. The cooling feed mechanism for producing carbon nanotubes according to claim 1, wherein: The lower part of the cooling jacket (2) is connected with a liquid inlet pipe (22), and the upper part of the cooling jacket (2) is connected with a liquid outlet pipe (23). The liquid inlet pipe (22) and the liquid outlet pipe (23) are communicated with the cooling cavity (21).
3. The cooling feed mechanism for producing carbon nanotubes according to claim 2, wherein: The liquid inlet pipe (22) and the liquid outlet pipe (23) are both elbow pipes. The pipe opening of the liquid inlet pipe (22) is arranged upwards, and the pipe opening of the liquid outlet pipe (23) is arranged downwards.
4. The cooling feed mechanism for producing carbon nanotubes according to claim 1, wherein: The feeding end of the furnace tube (1) is provided with a furnace tube cover (12) which can be opened and closed. The furnace tube cover (12) is fixedly provided with a handle (121).
5. The cooling feed mechanism for producing carbon nanotubes according to claim 4, wherein: The operation port (13) is arranged outside the furnace tube cover (12). The end of the operation port (13) away from the furnace tube cover (12) is provided with a flange port, and a sealing connecting plate (131) is detachably connected with the flange port.
6. The cooling feed mechanism for producing carbon nanotubes according to claim 1, wherein: A locking ring (15) is arranged on the furnace tube feeding part (11) close to one end of the cooling jacket (2). The end part of the cooling jacket (2) is fixedly arranged on the locking ring (15).
7. The cooling feed mechanism for producing carbon nanotubes according to claim 6, wherein: A group of fastening bolts (151) are arranged on one end of the locking ring (15) which is close to the cooling jacket (2). The fastening bolts (151) penetrate into the cooling jacket (2).
8. The cooling feed mechanism for producing carbon nanotubes according to claim 7, wherein: The group of fastening bolts (151) are more than six. The fastening bolts (151) are equally arranged on the ring surface of the locking ring (15).
9. The cooling feed mechanism for producing carbon nanotubes according to claim 1, wherein: A fixing assembly (3) is arranged below the furnace tube feeding part (11). The fixing assembly (3) comprises a mounting plate (31), a fixing seat (32), a supporting rod (33), a connecting plate (34) and a fastening nut (35). The mounting plate (31) is arranged below the furnace tube feeding part (11), and the fixing seat (32) is arranged on the mounting plate (31). The bottom of the supporting rod (33) is fixedly arranged on the fixing seat (32). A pair of connecting plates (34) are arranged on the two sides of the furnace tube feeding part (11), and the top of the supporting rod (33) penetrates through the connecting plates (34). The fastening nut (35) penetrates through the supporting rod (33) and locks the supporting rod (33) on the connecting plates (34).
10. The cooling feed mechanism for producing carbon nanotubes according to claim 1, wherein: The furnace tube (1) away from the furnace tube feeding part (11) is provided with a collecting bin (4) for collecting carbon nanotubes.