CN116553527B - Industrial synthesis device for single-walled carbon nanotubes - Google Patents
Industrial synthesis device for single-walled carbon nanotubes Download PDFInfo
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- CN116553527B CN116553527B CN202310733217.2A CN202310733217A CN116553527B CN 116553527 B CN116553527 B CN 116553527B CN 202310733217 A CN202310733217 A CN 202310733217A CN 116553527 B CN116553527 B CN 116553527B
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/159—Carbon nanotubes single-walled
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
Abstract
The invention discloses an industrial synthesis device of single-walled carbon nanotubes, and relates to the technical field of single-walled carbon nanotube production; the device comprises a plasma flame generating device and a low-temperature cavity connected with the top of the plasma flame generating device in a sealing way, wherein a premixing device is arranged at the top of the plasma flame generating device, and a reaction cavity is arranged between the plasma flame generating device and the premixing device; the premixing device is provided with a feeding device for providing reaction components for the premixing device, the feeding device penetrates through the top of the low-temperature cavity and enters the premixing device, the feeding device is in sealing connection with the low-temperature cavity and the premixing device, and one side of the top of the low-temperature cavity is communicated with a product collecting device. The synthesis device has the advantages of simple structure, low cost, great improvement of reaction efficiency due to the reaction structure of the large-size multiple plasma flames, more favorable generation of the carbon nano tube due to the temperature gradient design of the high-temperature region and the low-temperature region, and important promotion effect on industrial production of the single-wall carbon nano tube.
Description
Technical Field
The invention relates to the technical field of single-wall carbon nanotube production, in particular to an industrial synthesis device for single-wall carbon nanotubes.
Background
Single-walled carbon nanotubes (SWCNT), which are a novel nanomaterial, are widely used in the fields of new energy, transparent display, antistatic, semiconductors, engineering plastics, etc., due to their excellent electrical conductivity, thermal conductivity, temperature resistance, chemical resistance, mechanical properties, etc.
Currently, there are three main ways to prepare single-walled carbon nanotubes: arc methods, laser ablation methods, and chemical vapor deposition methods. The existing arc method and laser ablation method have low yield and high energy consumption, and are difficult to realize large-scale production. The floating catalytic chemical vapor deposition method is not high in yield because of the continuity of raw material supply and product collection, but is limited by the limitation of the size of a cavity of a synthesis device. The yield can be further improved by increasing the number of the reaction pipelines, but the equipment structure is complex because of excessive number of the pipelines, the consistency of the products is difficult to control, and the mass production is difficult. The method is a mode for improving productivity by increasing the size of the cavity, but because the reaction condition of the single-walled carbon nanotube is harsh, the temperature field distribution of the furnace body is changed after the size of the cavity is enlarged, vortex is formed in the cavity by air flow, the heat capacity of carrier gas is small, the temperature in the middle and at the tube wall is uneven after cold air flow is introduced, the carbon nanotube grows along the tube wall more easily, and the volume growth is not realized, so that the yield and the purity are lower.
How to design a reaction device from the angle of a single-wall carbon nano tube growth mechanism, fully realize the volume growth of the single-wall carbon nano tube, and further improve the yield of the single-wall carbon nano tube is a problem to be solved.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a single-walled carbon nanotube synthesizing device which has the advantages of high efficiency, controllability and the like, has a simple equipment structure and low cost, is easy to realize equal-proportion amplification, and has important value for batch production of single-walled carbon nanotubes.
The invention can be realized by the following technical scheme: the industrial synthesis device for the single-wall carbon nano tube comprises a plasma flame generating device and a low-temperature cavity connected with the top of the plasma flame generating device in a sealing way, wherein a premixing device is arranged at the top of the plasma flame generating device, and a reaction cavity is arranged between the plasma flame generating device and the premixing device;
the premixing device is provided with a feeding device for providing reaction components for the premixing device, the feeding device penetrates through the top of the low-temperature cavity and enters the premixing device, the feeding device is in sealing connection with the low-temperature cavity and the premixing device, and one side of the top of the low-temperature cavity is communicated with a product collecting device.
The invention further technically improves that: the plasma flame generating device comprises a high-voltage power supply assembly, a separation plate and a high-temperature insulating tube, wherein the high-temperature insulating tube is connected to the top of the separation plate in a sealing mode, a plurality of anode discharge needles are electrically connected to the high-voltage power supply assembly, each anode discharge needle penetrates through the separation plate and is uniformly distributed in the wrapping range of the high-temperature insulating tube, and a discharge head is detachably arranged at the end portion, far away from the high-voltage power supply assembly, of each anode discharge needle.
The invention further technically improves that: the reaction cavity is a cavity structure surrounded by a separation plate, a high-temperature insulating tube and a premixing device.
The invention further technically improves that: a sealing cavity is arranged in the premixing device, a plurality of microporous aeration heads are uniformly arranged at the bottom of the sealing cavity, and each microporous aeration head is in sealing connection with the sealing cavity.
The invention further technically improves that: the high-temperature insulating tube is connected with a cathode metal ring in a sealing way, and the microporous aeration head is electrically connected with the high-voltage power supply assembly through the cathode metal ring, and a gap is formed between the bottom of the microporous aeration head and the discharge head at the corresponding position.
The invention further technically improves that: at least one air outlet is arranged on the premixing device, the number of the discharge heads is at least one more than that of the microporous aeration heads, and the microporous aeration heads are in one-to-one correspondence with the positions of the discharge heads.
The invention further technically improves that: the feeding device comprises a gas pipeline and a capillary liquid inlet pipe, the capillary liquid inlet pipe is coaxially sleeved in the gas pipeline, and the gas pipeline and the capillary liquid inlet pipe are obliquely inserted into a sealing cavity of the premixing device.
The invention further technically improves that: the low-temperature cavity comprises a low-temperature cavity outer wall, the top of the low-temperature cavity outer wall is connected with a cavity cover in a sealing manner, and an observation window is arranged in the middle of the top of the cavity cover; the side wall of the outer wall of the low-temperature cavity is also provided with a pressure relief opening and is correspondingly provided with a pressure relief valve, and the top of the cavity cover is provided with a pressure gauge.
The invention further technically improves that: the product collecting device is specifically a stainless steel tank body, the inlet of the product collecting device is connected with the discharge port of the low-temperature cavity through a pipeline, and the outlet of the product collecting device is connected with the waste treatment device.
The invention further technically improves that: the top of the stainless steel tank body is provided with a back blowing port, a microporous filter plate is horizontally arranged in the stainless steel tank body near the back blowing port, and a receiving port is formed in the bottom of the stainless steel tank body.
Compared with the prior art, the invention has the following beneficial effects:
1. by arranging a plurality of plasma flames in the reaction cavity, the reaction of the carbon-containing precursor and the catalyst is more sufficient, the reaction efficiency is greatly improved, the product generation speed is further improved, and the product yield is increased;
2. the raw material supply device, the preheating device and the discharge device are integrated, so that the size of the reaction cavity is reduced, the energy is saved, and the production cost of the single-walled carbon nanotube is greatly reduced. The device has high controllability, simple structure and easy expansion production.
3. The synthesis of single-wall carbon nanotube is the process of dissolving and directional separating out carbon atom in catalyst, and the high concentration dissolution of carbon atom in catalyst in the reaction cavity is completed and the directional separating out in low temperature condition is required to form one-dimensional structure. The premixing device is arranged between the reaction cavity and the low-temperature cavity, plays a role in isolating heat, can form a low-temperature environment favorable for the growth of the carbon nano tube, and promotes the generation of products.
4. The synthesis device has the advantages of simple structure, low cost, great improvement of reaction efficiency due to the reaction structure of the large-size multiple plasma flames, more favorable generation of the carbon nano tube due to the temperature gradient design of the high-temperature region and the low-temperature region, and important promotion effect on industrial production of the single-wall carbon nano tube.
Drawings
The present invention is further described below with reference to the accompanying drawings for the convenience of understanding by those skilled in the art.
FIG. 1 is a schematic diagram of the overall device structure connection of the present invention;
FIG. 2 is a schematic diagram of a micro-porous aeration head of a premixing device according to the present invention;
fig. 3 is a structural layout of the discharge head of the present invention.
In the figure: 1. a plasma flame generating device; 2. a premixing device; 3. a feeding device; 4. a low temperature cavity; 5. a product collection device; 6. a reaction chamber; 11. a high voltage power supply assembly; 12. an anode discharge needle; 13. a partition plate; 14. a discharge head; 15. a cooling fan; 16. a high temperature insulating tube; 17. a cathode metal ring; 21. a microporous aeration head; 22. sealing the cavity; 23. an air outlet; 24. a first sealing element; 31. a gas conduit; 32. a capillary liquid inlet tube; 41. the outer wall of the low-temperature cavity; 42. a pressure relief port; 43. a cavity cover; 44. a pressure gauge; 45. an observation window; 46. a second sealing element; 47. a discharge port; 51. an exhaust gas treatment device; 52. a back-blowing port; 53. a microporous filter plate; 54. and a receiving port.
Detailed Description
In order to further describe the technical means and effects adopted by the invention for achieving the preset aim, the following detailed description is given below of the specific implementation, structure, characteristics and effects according to the invention with reference to the attached drawings and the preferred embodiment.
Referring to fig. 1-3, an industrial synthesis device for single-walled carbon nanotubes comprises a main structure including a plasma flame generating device 1, a premixing device 2, a feeding device 3, a low-temperature cavity 4, a product collecting device 5 and a reaction cavity 6;
the low-temperature cavity 4 is fixedly arranged above the plasma flame generating device 1 through bolts, the premixing device 2 is fixedly arranged at the top of the plasma flame generating device 1, the feeding device 3 penetrates through the top of the low-temperature cavity 4 to enter the premixing device 2, and the product collecting device 5 is arranged on one side of the low-temperature cavity 4 and is communicated with the inner cavity of the low-temperature cavity 4;
specifically, the plasma flame generating apparatus 1 includes a high-voltage power supply assembly 11, a partition plate 13, and a high-temperature insulating tube 16;
the high-voltage power supply assembly 11 consists of a main control circuit, a transformer and a radiator, wherein a gap is arranged between the main control circuit and the transformer, the power of the transformer is 2-50 KW, and the radiator is specifically a cooling fan 15;
a plurality of anode discharge needles 12 are electrically connected to the transformer, each anode discharge needle 12 consists of a support rod and a discharge needle body, a discharge head 14 is detachably arranged at the end part of the discharge needle body, and the discharge head 14 is conical;
the supporting rod passes through the isolation plate 13 and is connected with the transformer, the supporting rod is in sealing connection with the isolation plate 13, and the supporting rod is in sealing connection with the discharge needle body;
the high-temperature insulating tube 16 is arranged at the top of the isolation plate 13 and is connected with the isolation plate 13 in a sealing way; the top of the high-temperature insulating tube 16 is connected with a cathode metal ring 17 in a sealing way, and the cathode metal ring 17 is electrically connected with the transformer;
the reaction cavity 6 is a cavity surrounded by the isolation plate 13, the high-temperature insulating tube 16 and the premixing device 2, the high-temperature insulating tube 16 covers the discharge needle body and the discharge head 14, and the discharge needle body is uniformly distributed in the reaction cavity 6;
further, the discharge needle body and the discharge head 14 are both made of metal, preferably tungsten or 314 stainless steel; the cathode metal ring 17 is made of tungsten or 314 stainless steel;
further, the isolation plate 13 and the high-temperature insulating tube 16 are resistant to the temperature of more than 1100 ℃, and are preferably quartz plates or corundum plates, and the thickness is 2-20 mm; the height of the high-temperature insulating tube 16 is 40-100 mm, and the volume of the reaction cavity 6 can be adjusted by adjusting the height of the high-temperature insulating tube;
specifically, a sealed cavity 22 is arranged in the premixing device 2, the sealed cavity 22 is of a double-layer cavity structure, a plurality of microporous aeration heads 21 are uniformly arranged at the bottom of the sealed cavity 22, each microporous aeration head 21 is in sealing connection with the sealed cavity 22 through threads, at least one air outlet 23 is arranged in the sealed cavity 22, and the diameter range of the air outlet 23 is 20-100 mm;
the sealing cavity 22 is arranged above the cathode metal ring 17, the diameter of the sealing cavity 22 is consistent with that of the cathode metal ring 17, the sealing cavity 22 and the cathode metal ring 17 keep effective ohmic contact, and the microporous aeration head 21 is connected with the cathode metal ring 17;
further, the position distribution of the microporous aeration heads 21 corresponds to the anode discharge needles 12, gaps are arranged between the bottoms of the corresponding microporous aeration heads 21 and the discharge heads 14, and the distance of the gaps is set to be 20-100 mm; since the premixing device 2 is provided with at least one air outlet 23, the number of the discharge heads 14 is at least one more than that of the microporous aeration heads 21;
further, the sealing cavity 22 is made of metal, preferably tungsten or 314 stainless steel; the microporous aeration head is made of stainless steel or stainless titanium, the aperture is 5 um-100 um, and the shape is not limited to a cylindrical shape, a conical shape or a circular arc shape.
Specifically, the feeding device 3 comprises a gas pipeline 31 and a capillary liquid inlet pipe 32, the capillary liquid inlet pipe 32 is coaxially sleeved in the gas pipeline 31, the gas pipeline 31 and the capillary liquid inlet pipe 32 are obliquely inserted into the sealed cavity 22 of the premixing device 2 and are in sealed connection through a seal one 24, and a flow meter and a liquid supply pump are arranged at the liquid inlet end of the capillary liquid inlet pipe 32;
the outlet end of the capillary liquid inlet pipe 32 is positioned in the sealing cavity 22 and extends out of the gas pipeline 31, and the extending distance is 5-20 mm;
the inner diameter of the capillary liquid inlet pipe 32 is 0.3-1.5 mm, and the gas pipe 31 and the capillary liquid inlet pipe 32 are made of stainless steel;
specifically, the low-temperature cavity 4 comprises a low-temperature cavity outer wall 41, the top of the low-temperature cavity outer wall 41 is fixedly connected with a cavity cover 43 through threads, an observation window 45 is arranged in the middle of the top of the cavity cover 43, and the observation window 45 is positioned right above the air outlet 23 in the premixing device 2, so that the situation in the sealed cavity 22 can be observed; the side wall of the outer wall 41 of the low-temperature cavity is also provided with a pressure relief opening 42 and is correspondingly provided with a pressure relief valve, and the top of the cavity cover 43 is provided with a pressure gauge 44;
further, the cavity cover 43 is connected with the low-temperature cavity outer wall 41 in a sealing way through a high-temperature sealing ring, the sealing ring is made of PTEE, and the low-temperature cavity outer wall 41 is connected with the isolation plate 13 in a sealing way;
the feeding device 3 penetrates through the cavity cover 43 to enter the premixing device 2 and is in sealing connection with the cavity cover 43 through a second sealing piece 46;
the product collecting device 5 is specifically a stainless steel tank body, an inlet of the product collecting device is connected with a discharge hole 47 of the low-temperature cavity 4 through a pipeline, an outlet of the product collecting device is connected with a waste treatment device 51, a back blowing port is arranged at the top of the stainless steel tank body, a microporous filter plate 53 is horizontally arranged in the stainless steel tank body near the back blowing port, and a material receiving port 54 is arranged at the bottom of the stainless steel tank body;
further, the microporous filter plate 32 may be a microporous titanium plate or copper plate made of metal, or a sand core filter plate made of ceramic.
In the embodiment, the reaction cavity formed by a plurality of plasma flames is adopted, so that the reaction of the carbon-containing precursor and the catalyst is more sufficient, and the reaction efficiency is greatly improved. In addition, the raw material supply device, the premixing device and the discharge device are integrated, so that the size of the reaction cavity is reduced, the energy is saved, and the production cost of the single-walled carbon nanotube is greatly reduced. The device has high controllability, simple structure and easy expansion production;
in this embodiment, as shown in fig. 2, inert carrier gas, organic precursor, catalyst, accelerator and the like enter the premixing device 2 through the feeding device 3 for gasification, and are blown into the reaction cavity 6 through 20 microporous aeration heads with 5um for reaction;
in the present embodiment, the power of the plasma flame generating device 1 is 5KW, as shown in fig. 3, the number of the anode discharge needles 12 is 21, and the rest anode discharge needles 12 vertically correspond to the microporous aeration head 21 except for 1 anode discharge needle 12 at the center of the center;
in this example, the distance between the microporous aeration head 21 and the anode discharge electrode 12 was set to 40mm, the diameter of the reaction chamber 6 was 250mm, and the height was 80mm.
When the invention is used, firstly, the reaction cavity 6 is vacuumized and filled with inert gas nitrogen, after stabilizing for 10 minutes, a plasma flame generating device is started, the nitrogen is ionized by a discharge head 14 and a micropore aeration head 21, 20 groups of plasma flames are formed in the middle, the temperature in the reaction cavity 6 is kept stable to 1100 ℃ for 30 minutes, at the moment, the temperature in the premixing device 2 is 600-700 ℃, and the temperature in the low-temperature cavity 4 is 400-450 ℃;
then, injecting reaction precursors (including carbon-containing precursors, catalysts and accelerators) into a sealed cavity 22 of the premixing device 2, introducing the reaction precursors into a reaction cavity 6 by a microporous aeration head 21 under the action of carrier gas, carrying out catalytic cracking reaction on each reaction component under the action of high temperature, melting carbon-containing free radicals on the surface of the catalysts, discharging the carbon-containing free radicals into a low-temperature cavity 4 through an air outlet 23, and separating out carbon atoms to form flocculent single-wall carbon nanotubes;
finally, the flocculent single-walled carbon nanotube product in the low-temperature cavity 4 enters the product collecting device 5 under the action of air flow and is deposited at the bottom of the microporous filter plate 53, and after a certain amount of flocculent single-walled carbon nanotube product is accumulated, the single-walled carbon nanotube product is separated from the microporous filter plate 53 by the back-blowing port 52 and is discharged and collected from the lower material receiving port 54.
In this process, the reaction chamber 6 has three functions: 1. the microporous aeration head 21 and the discharge head 14 of the plasma flame generating device 1 form a counter electrode, and ionized inert gas forms a plasma flame; 2. the reaction cavity 6 is heated to a certain stability by the formed plasma flame, and reactants can be preheated and gasified; 3. the preheated gas is uniformly diffused to the whole reaction cavity 6 through the microporous aeration head 21, so that the synthesis reaction is more sufficient.
In addition, the function of the low-temperature cavity 4 is also important, the synthesis of the single-walled carbon nanotube is the process of dissolving and directionally precipitating carbon atoms in the catalyst, and the high-concentration dissolution of the carbon atoms in the catalyst is completed in the reaction cavity 6, so that the single-walled carbon nanotube needs to be directionally precipitated under the low-temperature condition to form a one-dimensional structure. The premixing device 2 is arranged between the reaction cavity 6 and the low-temperature cavity 4, plays a role in isolating heat, can form a low-temperature environment favorable for the growth of the carbon nano tube, and promotes the generation of products.
The present invention is not limited to the above embodiments, but is capable of modification and variation in all aspects, including those of ordinary skill in the art, without departing from the spirit and scope of the present invention.
Claims (7)
1. An industrial synthesis device for single-walled carbon nanotubes is characterized in that: the device comprises a plasma flame generating device (1) and a low-temperature cavity (4) which is connected with the top of the plasma flame generating device in a sealing way, wherein a premixing device (2) is arranged at the top of the plasma flame generating device (1), and a reaction cavity (6) is arranged between the plasma flame generating device (1) and the premixing device (2);
the premixing device (2) is provided with a feeding device (3) for providing reaction components for the premixing device, the feeding device (3) penetrates through the top of the low-temperature cavity (4) and enters the premixing device (2), the feeding device (3) is in sealing connection with the low-temperature cavity and the premixing device, and one side of the top of the low-temperature cavity (4) is communicated with a product collecting device (5);
a sealing cavity (22) is arranged in the premixing device (2), a plurality of microporous aeration heads (21) are uniformly arranged at the bottom of the sealing cavity (22), and each microporous aeration head (21) is in sealing connection with the sealing cavity (22);
the plasma flame generating device (1) comprises a high-voltage power supply assembly (11), a separation plate (13) and a high-temperature insulating tube (16), wherein the high-temperature insulating tube (16) is connected to the top of the separation plate (13) in a sealing mode, a plurality of anode discharge needles (12) are electrically connected to the high-voltage power supply assembly (11), each anode discharge needle (12) penetrates through the separation plate (13) and is uniformly distributed in the wrapping range of the high-temperature insulating tube (16), and a discharge head (14) is detachably arranged at the end part, far away from the high-voltage power supply assembly (11), of each anode discharge needle (12);
the high-temperature insulating tube (16) is connected with a cathode metal ring (17) in a sealing way, the microporous aeration head (21) is electrically connected with the high-voltage power supply assembly (11) through the cathode metal ring (17), and a gap is formed between the bottom of the microporous aeration head (21) and the discharge head (14) at the corresponding position.
2. The industrial synthesis device of single-walled carbon nanotubes according to claim 1, wherein the reaction chamber (6) is a cavity structure surrounded by a separation plate (13), a high-temperature insulating tube (16) and a premixing device (2).
3. The industrial synthesis device of single-walled carbon nanotubes according to claim 1, wherein the premixing device (2) is provided with at least one air outlet (23), and the number of the discharge heads (14) is at least one more than the number of the microporous aeration heads (21), and the microporous aeration heads (21) are in one-to-one correspondence with the positions of the discharge heads (14).
4. The industrial synthesis device of single-walled carbon nanotubes according to claim 1, wherein the feeding device (3) comprises a gas pipeline (31) and a capillary liquid inlet pipe (32), the capillary liquid inlet pipe (32) is coaxially sleeved in the gas pipeline (31), and the gas pipeline (31) and the capillary liquid inlet pipe (32) are obliquely inserted into the sealed cavity (22) of the premixing device (2).
5. The industrial synthesis device of single-walled carbon nanotubes according to claim 1, wherein the low-temperature cavity (4) comprises a low-temperature cavity outer wall (41), a cavity cover (43) is connected to the top of the low-temperature cavity outer wall (41) in a sealing manner, and an observation window (45) is arranged in the middle of the top of the cavity cover (43); the side wall of the low-temperature cavity outer wall (41) is also provided with a pressure relief opening (42) and a pressure relief valve correspondingly, and the top of the cavity cover (43) is provided with a pressure gauge (44).
6. The industrial synthesis device of single-walled carbon nanotubes according to claim 1, wherein the product collection device (5) is in particular a stainless steel tank, the inlet of which is connected with the discharge port (47) of the low-temperature cavity (4) through a pipeline, and the outlet of which is connected with the waste treatment device (51).
7. The industrial synthesis device for single-walled carbon nanotubes according to claim 6, wherein a back-blowing port is arranged at the top of the stainless steel tank, a microporous filter plate (53) is horizontally arranged in the stainless steel tank near the back-blowing port, and a material receiving port (54) is arranged at the bottom of the stainless steel tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310733217.2A CN116553527B (en) | 2023-06-20 | 2023-06-20 | Industrial synthesis device for single-walled carbon nanotubes |
Applications Claiming Priority (1)
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