CN116495725B - Carbon nanotube growth system - Google Patents

Carbon nanotube growth system Download PDF

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Publication number
CN116495725B
CN116495725B CN202310570109.8A CN202310570109A CN116495725B CN 116495725 B CN116495725 B CN 116495725B CN 202310570109 A CN202310570109 A CN 202310570109A CN 116495725 B CN116495725 B CN 116495725B
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catalyst
chamber
reaction chamber
buffer
heating
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CN116495725A (en
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丁显波
肖敏
阮超
曹礼洪
丁龙奇
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Chongqing Zhongrun New Materials Co ltd
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Chongqing Zhongrun New Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • C01B32/164Preparation involving continuous processes

Abstract

The invention belongs to the technical field of carbon nano material preparation, and particularly discloses a carbon nano tube growth system, wherein a reaction unit comprises a reaction chamber, a heating mechanism, a first vacuum mechanism, a first shielding gas mechanism, a carbon source gas mechanism and a scraping mechanism, wherein the heating mechanism is used for heating the reaction chamber and comprises an external heating structure and an internal heating structure; the scraping mechanism comprises a driving structure, an inner wall scraping plate and an inner scraping plate, wherein the driving structure is used for driving the inner wall scraping plate to rotate along the center of the reaction chamber and driving the inner scraping plate to rotate along the center shaft of the inner heating structure. By arranging the external heating structure and the internal heating structure, the uniform temperature of the growth temperature of the carbon nano tube at each position in the reaction chamber is realized. The inner wall scraping plate and the inner scraping plate are arranged, so that the carbon nanotubes can be scraped in time, the carbon nanotubes are prevented from adhering to the inner wall of the reaction chamber and affecting the heat transfer effect on the inner heating structure, and the heat transfer stability in the reaction chamber can be realized.

Description

Carbon nanotube growth system
Technical Field
The invention belongs to the technical field of preparation of carbon nano materials, and particularly relates to a carbon nano tube growth system.
Background
The carbon nano tube is taken as a typical one-dimensional nano material, is one of research hotspots in the field of material science for many years, and has wide application prospect. The synthesis methods of carbon nanotubes are various, and three methods, namely an arc method, a laser ablation method and a chemical vapor deposition method, are mainly adopted at present. The chemical vapor deposition method has the advantages of easy control of parameters, high product yield, high carbon purity, easy realization of large-scale production and most wide application in industry at present.
In the prior art, the fluidized bed is an ideal reactor for preparing the carbon nano tubes by a chemical vapor phase method, however, when the fluidized bed is used for preparing the carbon nano tubes, the following problems often exist: 1. the gas concentration of each area in the reaction chamber is not uniform, so that the growth conditions of the carbon tubes are not uniform; 2. the temperature is not uniform throughout the inside of the reaction chamber, thereby causing a difference in the growth morphology of the carbon nanotubes. In order to solve the problems, the invention provides a carbon nano tube growth system for optimizing the distribution of an air flow field and a temperature field.
Disclosure of Invention
The invention aims to provide a carbon nano tube growth system which solves the problems of low quality and low growth efficiency of carbon nano tubes caused by the influence of the growth environment of the carbon nano tubes due to the uneven gas concentration and uneven temperature in each area in a reaction chamber in the prior art.
In order to achieve the above purpose, the technical scheme of the invention is as follows: the carbon nano tube growth system comprises a control unit, and a catalyst input unit and a reaction unit which are connected with the control unit, wherein the control unit is used for controlling the catalyst input unit and the reaction unit; the catalyst input unit is used for inputting a catalyst into the reaction unit, the reaction unit comprises a reaction chamber, a heating mechanism, a first vacuum mechanism, a first shielding gas mechanism, a carbon source gas mechanism and a scraping mechanism, the heating mechanism is used for heating the reaction chamber, the heating mechanism comprises an external heating structure and an internal heating structure, the first shielding gas mechanism is used for conveying shielding gas into the reaction chamber, the carbon source gas mechanism is used for conveying carbon source gas and carrier gas into the reaction chamber, and the first vacuum mechanism is used for vacuumizing the reaction chamber; the scraping mechanism is used for scraping the carbon nano tubes on the inner wall of the reaction chamber and the carbon nano tubes outside the internal heating structure; the scraping mechanism comprises a driving structure, an inner wall scraping plate and an inner scraping plate, wherein the driving structure is used for driving the inner wall scraping plate to rotate along the center of the reaction chamber and driving the inner scraping plate to rotate along the center shaft of the inner heating structure; the reaction chamber is provided with a feed inlet and a discharge outlet, and the discharge outlet is provided with a discharge valve.
Further, the catalyst input unit comprises a jet milling chamber, wherein the jet milling chamber is used for milling the catalyst, and a catalyst inlet and a catalyst outlet are arranged on the jet milling chamber.
Further, the catalyst input unit further comprises a buffer chamber, a catalyst buffer inlet and a catalyst buffer outlet are arranged on the buffer chamber, the catalyst buffer inlet of the buffer chamber is communicated with the catalyst outlet through a first conveying structure, and the catalyst buffer outlet is communicated with a feed inlet of the reaction chamber through a second conveying structure; the buffer chamber is connected with a second vacuum mechanism and a second protective gas mechanism, the second vacuum mechanism is used for vacuumizing the buffer chamber, and the second protective gas mechanism is used for filling protective gas into the buffer chamber.
Further, a detector is arranged in the buffer chamber or an observation material window is arranged on the buffer chamber, and the detector is used for detecting the filling amount of the catalyst in the buffer chamber and sending the detection result to the control unit; the observation window is used for observing the filling amount of the catalyst in the buffer chamber.
Further, the buffer chamber and the reaction chamber are respectively provided with a pressure gauge for detecting pressure, and detected pressure data are sent to the control unit.
Further, a temperature detector is arranged in the reaction chamber; the temperature detector transmits the detected temperature data to the control unit.
Further, a screening unit is arranged in the jet milling chamber, and the screening unit screens the particle size of the catalyst.
Further, a catalyst outlet on the jet milling chamber is positioned above the buffer chamber; the first conveying structure comprises a first pipeline and a first sealing assembly, and two ends of the first pipeline are respectively connected with the catalyst buffering inlet and the catalyst outlet; the first sealing assembly is used for sealing or opening a first pipeline; the second conveying structure comprises a second pipeline and a second sealing assembly, the buffer chamber is positioned above the reaction chamber, and the second pipeline is used for connecting a catalyst buffer outlet and a feed inlet of the reaction chamber; the second seal assembly is used for sealing or opening a second pipeline.
Further, the internal heating structure comprises a plurality of heating rods, the internal scraping plates are provided with a plurality of groups, and the internal scraping plates and the heating rods are in one-to-one correspondence; the inner wall heating structure comprises a heating sleeve and a heat preservation sleeve, wherein the heating sleeve is sleeved outside the reaction chamber, and the heat preservation sleeve is sleeved outside the heating sleeve.
Further, the reaction chamber is provided with an air outlet and two air inlets, the air outlet is used for discharging air in the reaction chamber, and the air outlet is provided with an air outlet valve; the two air inlets are connected with the carbon source gas mechanism and the first protection gas mechanism, and the air inlets are provided with air inlet valves; the two air inlets are respectively positioned at the upper side and the lower side of the reaction chamber.
The working principle of the technical scheme is as follows:
the catalyst is put into a jet milling chamber for milling, and the screening unit screens out catalyst particles meeting the particle size requirement. The first conveying structure conveys catalyst particles meeting the particle size requirement into the buffer chamber, the first vacuum mechanism is opened, and the reaction chamber is vacuumized by the first vacuum mechanism; opening the first protective gas mechanism, and filling the protective gas with atmospheric pressure into the reaction chamber; and finally, opening a heating mechanism, heating the reaction chamber by the heating mechanism to 600-900 ℃, monitoring the temperature in the reaction chamber in real time by a temperature detector, and keeping constant temperature until the reaction is finished after the set temperature is reached, wherein the reaction time is usually 0.5-1 h.
An observation window or a control unit on the artificial observation buffer chamber judges the catalyst filling amount according to the height data of the catalyst detected by the detector. When a certain amount is reached, the catalyst buffer inlet of the buffer chamber is closed manually or automatically by the control unit. And then opening a second vacuum mechanism, vacuumizing the buffer chamber by the second vacuum mechanism, and then opening a second protective gas mechanism to fill protective gas with one atmosphere pressure into the buffer chamber. And then opening a catalyst buffer outlet, an air inlet valve, an air outlet valve and a first protective gas mechanism, wherein the catalyst enters the reaction chamber from the buffer chamber, and the protective gas filled by the first protective gas mechanism enables the catalyst to be in a fluidized state.
After all the catalyst in the buffer chamber enters the reaction chamber, the catalyst buffer outlet and the first protective gas mechanism are closed, the catalyst buffer inlet is opened, and the catalyst particles with the particle size are collected again. And simultaneously introducing preheated carbon source gas and carrier gas into the reaction chamber, and starting to grow the carbon nano tube in the reaction chamber. In the growth process, a driving structure is started at intervals, the driving structure drives an inner wall scraping plate and an inner scraping plate to rotate, the inner wall scraping plate scrapes carbon nano tubes on the inner wall of the reaction chamber, and the inner scraping plate scrapes the carbon nano tubes on the inner heating structure.
And after the growth of the carbon nano tube is finished, closing the air inlet valve and the air outlet valve, opening a discharge hole of the reaction chamber, and discharging the carbon nano tube from the discharge hole.
And repeating the steps to continuously produce the carbon nano tube.
The beneficial effects of this technical scheme lie in:
(1) according to the technical scheme, the external heating structure and the internal heating structure are arranged, so that the uniform temperature of the growth temperature of the carbon nanotubes at all positions in the reaction chamber is realized.
(2) According to the technical scheme, the inner wall scraping plate and the inner scraping plate are arranged, so that the carbon nanotubes can be scraped in time, the carbon nanotubes are prevented from adhering to the inner wall of the reaction chamber and affecting the heat transfer effect on the inner heating structure, and therefore the heat transfer in the reaction chamber is stable.
(3) The technical scheme enables the catalyst to be suspended by controlling the particle size of the catalyst and the flow rate of gas.
(4) According to the technical scheme, the buffer chamber is arranged, so that continuous batch production of the carbon nanotubes can be realized, the operation is simple, the production efficiency is high, the method is suitable for industrial production, and the method has good application prospects in the field of carbon nanotube synthesis.
Drawings
FIG. 1 is a schematic diagram of a carbon nanotube growth system according to the present invention;
FIG. 2 is a front view of FIG. 1;
FIG. 3 is a rear view of FIG. 1;
FIG. 4 is a schematic view showing the internal structure of the jet milling chamber in FIG. 1;
FIG. 5 is a schematic view of the internal structure of the reaction chamber;
fig. 6 is a top view of the drive structure.
Detailed Description
The following is a further detailed description of the embodiments:
reference numerals in the drawings of the specification include: the air flow crushing device comprises an air flow crushing chamber 1, a buffer chamber 2, a reaction chamber 3, a receiving chamber 4, a feeding chamber 5, a first pipeline 6, a second pipeline 7, a third pipeline 8, a sorting impeller 9, a sorting motor 10, a nozzle 11, an air inlet 12, an air outlet 13, a driving motor 14, a driving gear 15, a driven gear 16, a rotating shaft 17, an annular gear 18, an inner wall scraping plate 19, a connecting rod 20, an inner scraping plate 21, a heating rod 22 and a guide plate 23.
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The embodiment is basically as shown in the accompanying figures 1-6: a carbon nanotube growing system comprises a control unit, a catalyst input unit and a reaction unit, wherein the catalyst input unit and the reaction unit are connected with the control unit; the catalyst input unit is used for inputting the catalyst to the reaction unit, the reaction unit comprises a reaction chamber 3, a heating mechanism, a first vacuum mechanism, a first shielding gas mechanism, a carbon source gas mechanism and a scraping mechanism, the heating mechanism is used for heating the reaction chamber 3, the heating mechanism comprises an external heating structure and an internal heating structure, as shown in fig. 5, the internal heating structure comprises a plurality of heating rods 22, the internal scraping plates 21 are provided with a plurality of groups, and the internal scraping plates 21 and the heating rods 22 are in one-to-one correspondence. The inner wall heating structure comprises a heating sleeve and a heat preservation sleeve, the heating sleeve is sleeved outside the reaction chamber 3, and the heat preservation sleeve is sleeved outside the heating sleeve. The first shielding gas mechanism is used for conveying shielding gas into the reaction chamber 3, the carbon source gas mechanism is used for conveying carbon source gas and carrier gas into the reaction chamber 3, and the first vacuum mechanism is used for vacuumizing the reaction chamber 3.
The scraping mechanism is used for scraping the carbon nano tubes on the inner wall of the reaction chamber 3 and the carbon nano tubes outside the internal heating structure; the scraping mechanism comprises a driving structure, an inner wall scraping plate 19 and an inner scraping plate 21, wherein the driving structure is used for driving the inner wall scraping plate 19 to rotate along the center of the reaction chamber 3 and driving the inner scraping plate 21 to rotate along the corresponding heating rod 22. The driving structure specifically comprises a driving motor 14, an annular gear 18, a driving gear 15 and a plurality of driven gears 16, wherein the driving motor 14 is arranged above the reaction chamber 3, an output shaft of the driving motor 14 extends into the reaction chamber 3 and is connected with the driving gear 15, and magnetic fluid sealing is adopted between the output shaft and the reaction chamber. The driven gears 16 are positioned on the periphery of the driving gear 15 and meshed with the driving gear 15, the centers of the driven gears 16 are rotatably connected with rotating shafts 17, and the rotating shafts 17 are fixed at the top of the reaction chamber 3. The inner wall of the upper part of the reaction chamber 3 is provided with a ring groove, the outer turnover of the inner gear ring 18 is connected in the ring groove in a movable way, and a plurality of driven gears 16 are meshed with the inner gear ring 18. A heating rod 22 is fixed at the lower end of the rotating shaft 17, an inner wall scraping plate 19 is fixed at the lower end of the inner gear ring 18, a connecting rod 20 is fixed at the lower end of the driven gear 16, and an inner scraping plate 21 is fixed on the connecting rod 20. The distance between the inner scraper 21 and the heating rod 22, and between the inner wall scraper 19 and the inner wall of the reaction chamber 3 is 5 to 50. Mu.m, specifically 30. Mu.m.
The reaction chamber 3 is provided with a feed inlet and a discharge outlet, a discharge valve is arranged at the discharge outlet, and the discharge outlet is connected with the material receiving chamber 4. The reaction chamber 3 is provided with an air outlet 13 and two air inlets 12, the air outlet 13 is used for discharging air in the reaction chamber 3, and the air outlet 13 is provided with an air outlet valve; the two air inlets 12 are connected with a carbon source air mechanism and a first protective air mechanism, and an air inlet valve is arranged on the air inlet 12; the two air inlets 12 are respectively positioned at the upper side and the lower side of the reaction chamber 3, and a deflector 23 is arranged at the position of the air inlet 12 at the lower side, and the deflector 23 is used for upwards guiding the air at the lower side.
The catalyst input unit comprises a feeding chamber 5, a jet milling chamber 1 and a buffer chamber 2, wherein the jet milling chamber 1 is used for milling a catalyst, a catalyst inlet and a catalyst outlet are formed in the jet milling chamber 1, the feeding chamber 5 is connected with the catalyst inlet through a third pipeline 8, the feeding chamber 5 is used for adding the catalyst into the jet milling chamber 1, and an electromagnetic valve is arranged at the outlet of the feeding chamber 5.
The catalyst outlet on the jet milling chamber 1 is positioned above the buffer chamber 2, the buffer chamber 2 is provided with a catalyst buffer inlet and a catalyst buffer outlet, the catalyst buffer inlet and the catalyst outlet of the buffer chamber 2 are communicated through a first conveying structure, the first conveying structure specifically comprises a first pipeline 6 and a first sealing component, two ends of the first pipeline 6 are respectively arranged obliquely with the catalyst buffer inlet and the catalyst outlet, and the first pipeline 6 is obliquely arranged; the first sealing assembly is used to seal or open the first conduit 6. The catalyst buffer outlet is communicated with the feed inlet of the reaction chamber 3 through a second conveying structure, specifically the second conveying structure comprises a second pipeline 7 and a second sealing assembly, the buffer chamber 2 is positioned above the reaction chamber 3, and the second pipeline 7 is used for connecting the catalyst buffer outlet and the feed inlet of the reaction chamber 3; the second sealing assembly is used to seal or open the second conduit 7. In this embodiment, the first sealing component and the second sealing component are respectively installed on two sides of each pipeline by adopting a flange knife gate valve or an electromagnetic valve. The buffer chamber 2 is connected with a second vacuum mechanism and a second shielding gas mechanism, the second vacuum mechanism is used for vacuumizing the buffer chamber 2, and the second shielding gas mechanism is used for filling shielding gas into the buffer chamber 2. The buffer chamber 2 is internally provided with a detector or an observation material window is arranged on the buffer chamber 2, the detector is used for detecting the filling amount of the catalyst in the buffer chamber 2 and sending the detection result to the control unit, the detector can be a range finder, and the range finder is arranged at the top of the buffer chamber 2 and is used for detecting the height of materials; the observation window is used for observing the catalyst charge in the buffer chamber 2.
Pressure gauges for detecting pressure are arranged in the buffer chamber 2 and the reaction chamber 3, and detected pressure data are sent to the control unit. A temperature detector is arranged in the reaction chamber 3; the temperature detector transmits the detected temperature data to the control unit.
The jet milling chamber 1 is internally provided with a screening unit which screens the particle size of the catalyst. Specifically, as shown in fig. 4, the sieving unit includes a classifying impeller 9 and a classifying motor 10, the classifying motor 10 is installed above the jet mill chamber 1, the classifying impeller 9 is installed inside the jet mill chamber 1, and the classifying motor 10 is used for driving the classifying impeller 9 to operate. The catalyst inlet is arranged in the middle of the jet milling chamber 1, the catalyst outlet is arranged at the upper part of the jet milling chamber 1, and the catalyst outlet is communicated with the sorting impeller 9. The middle lower part of the jet milling chamber 1 is provided with a plurality of nozzles 11, the nozzles 11 are communicated with an externally installed compressed air pipe, and the nozzles 11 spray crushing air into the jet milling chamber 1 to achieve milling.
The specific implementation process is as follows:
the catalyst is put into the jet milling chamber 1 for milling, and the screening unit screens out catalyst particles meeting the particle size requirement. The specific screening method comprises the following steps: the sorting motor 10 drives the sorting impeller 9 to rotate, the sorting impeller 9 rotates at a high speed, the nozzle 11 is used for blowing air, collision, friction and shearing are generated to break the sorting impeller 9 into superfine materials, the materials rise along with air flow, the centrifugal force generated by the sorting impeller 9 and the centripetal force generated by the air flow viscosity function are received in the rising process, when the centrifugal force received by particles is larger than the centripetal force, the particles return to be continuously smashed, and when the centrifugal force received by the particles is smaller than the centripetal force, the particles with graded particle sizes enter and are discharged through the sorting impeller 9.
The first conveying structure conveys catalyst particles meeting the particle size requirement into the buffer chamber 2, the first vacuum mechanism is opened, and the reaction chamber 3 is vacuumized by the first vacuum mechanism; then the first protective gas mechanism is opened, and protective gas with atmospheric pressure is filled into the reaction chamber 3; and finally, a heating mechanism is opened, the heating mechanism heats the reaction chamber 3, the temperature is raised to 600-900 ℃, a temperature detector monitors the temperature in the reaction chamber 3 in real time, and the temperature is kept constant after the set temperature is reached, until the reaction is finished, and the reaction time is usually 0.5-1 h.
An observation window or a control unit on the artificial observation buffer chamber 2 judges the catalyst charge amount based on the height data of the catalyst detected by the detector. When a certain amount (for example two thirds of the time) is reached, the artificial shut-off or control unit automatically closes the catalyst buffer inlet of the buffer chamber 2. And then opening a second vacuum mechanism, vacuumizing the buffer chamber 2 by the second vacuum mechanism, and then opening a second protective gas mechanism to charge protective gas with atmospheric pressure into the buffer chamber 2. Then, a catalyst buffer outlet, an air inlet valve, an air outlet valve and a first protective gas mechanism are opened, the catalyst enters the reaction chamber 3 from the buffer chamber 2, and the protective gas filled by the first protective gas mechanism enables the catalyst to be in a fluidized state.
After all the catalyst in the buffer chamber 2 enters the reaction chamber 3, the catalyst buffer outlet and the first shielding gas mechanism are closed, the catalyst buffer inlet is opened, and the catalyst particles with the particle size are collected again. Simultaneously, preheated carbon source gas and carrier gas are introduced into the reaction chamber 3, and carbon nanotubes begin to grow in the reaction chamber 3. In the growth process, a driving structure is started at intervals, the driving structure drives the inner wall scraping plate 19 and the inner wall scraping plate 21 to rotate, the inner wall scraping plate 19 scrapes carbon nano tubes on the inner wall of the reaction chamber 3, and the inner wall scraping plate 21 scrapes carbon nano tubes on the inner heating structure. The specific driving mode of the driving structure is as follows: the driving motor 14 drives the driving gear 15 to rotate, the driving gear 15 drives the driven gear 16 to rotate, the driven gear 16 drives the inner gear ring 18 to rotate, the driven gear 16 drives the inner scraping plate 21 to rotate, and the inner gear ring 18 drives the inner wall scraping plate 19 to rotate.
And after the growth of the carbon nano tube is finished, closing the air inlet valve and the air outlet valve, opening the discharge port of the reaction chamber 3, and discharging the carbon nano tube from the discharge port.
And repeating the steps to continuously produce the carbon nano tube.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The foregoing is merely an embodiment of the present invention, and a specific structure and characteristics of common knowledge in the art, which are well known in the scheme, are not described herein, so that a person of ordinary skill in the art knows all the prior art in the application day or before the priority date of the present invention, and can know all the prior art in the field, and have the capability of applying the conventional experimental means before the date, so that a person of ordinary skill in the art can complete and implement the present embodiment in combination with his own capability in the light of the present application, and some typical known structures or known methods should not be an obstacle for a person of ordinary skill in the art to implement the present application. It should be noted that modifications and improvements can be made by those skilled in the art without departing from the structure of the present invention, and these should also be considered as the scope of the present invention, which does not affect the effect of the implementation of the present invention and the utility of the patent. The protection scope of the present application shall be subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.

Claims (6)

1. A carbon nanotube growth system, characterized by: the device comprises a control unit, a catalyst input unit and a reaction unit, wherein the catalyst input unit and the reaction unit are connected with the control unit, and the control unit is used for controlling the catalyst input unit and the reaction unit; the catalyst feeding unit is used for feeding a catalyst into the reaction unit, the catalyst feeding unit comprises a jet milling chamber (1) and a buffer chamber (2), the jet milling chamber (1) is used for milling the catalyst, a catalyst inlet and a catalyst outlet are formed in the jet milling chamber (1), a screening unit is arranged in the jet milling chamber (1), and the screening unit screens the particle size of the catalyst; the screening unit comprises a sorting impeller (9) and a sorting motor (10), the sorting motor (10) is arranged above the jet milling chamber (1), the sorting impeller (9) is arranged inside the jet milling chamber (1), and the sorting motor (10) is used for driving the sorting impeller (9) to operate; the catalyst outlet is communicated with the sorting impeller (9); the middle lower part of the jet milling chamber (1) is provided with a plurality of nozzles (11), the nozzles (11) are communicated with a compressed air pipe arranged outside, and the nozzles (11) spray compressed air into the jet milling chamber (1) to achieve milling; the reaction unit comprises a reaction chamber (3), a heating mechanism, a first vacuum mechanism, a first shielding gas mechanism, a carbon source gas mechanism and a scraping mechanism, wherein the heating mechanism is used for heating the reaction chamber (3), the heating mechanism comprises an external heating structure and an internal heating structure, and the internal heating structure comprises a plurality of heating rods (22); the external heating structure comprises a heating sleeve and a heat preservation sleeve, the heating sleeve is sleeved outside the reaction chamber (3), and the heat preservation sleeve is sleeved outside the heating sleeve; the first shielding gas mechanism is used for conveying shielding gas into the reaction chamber (3), the carbon source gas mechanism is used for conveying carbon source gas and carrier gas into the reaction chamber (3), and the first vacuum mechanism is used for vacuumizing the reaction chamber (3); the scraping mechanism is used for scraping the carbon nano tubes on the inner wall of the reaction chamber (3) and the carbon nano tubes outside the internal heating structure; the scraping mechanism comprises a driving structure, an inner wall scraping plate (19) and an inner scraping plate (21), wherein the inner scraping plate (21) is provided with a plurality of groups, and the inner scraping plate (21) and the heating rod (22) are in one-to-one correspondence; the driving structure is used for driving the inner wall scraping plate (19) to rotate along the center of the reaction chamber (3) and driving the inner scraping plate (21) to rotate along the central axis of the inner heating structure; a feed inlet and a discharge outlet are arranged on the reaction chamber (3), and a discharge valve is arranged at the discharge outlet; the buffer chamber (2) is provided with a catalyst buffer inlet and a catalyst buffer outlet, the catalyst buffer inlet of the buffer chamber (2) is communicated with the catalyst outlet through a first conveying structure, and the catalyst buffer outlet is communicated with the feed inlet of the reaction chamber (3) through a second conveying structure; the buffer chamber (2) is connected with a second vacuum mechanism and a second protective gas mechanism, the second vacuum mechanism is used for vacuumizing the buffer chamber (2), and the second protective gas mechanism is used for filling protective gas into the buffer chamber (2).
2. The carbon nanotube growth system of claim 1, wherein: a detector is arranged in the buffer chamber (2) or an observation material window is arranged on the buffer chamber (2), and the detector is used for detecting the filling amount of the catalyst in the buffer chamber (2) and sending the detection result to the control unit; the observation window is used for observing the filling amount of the catalyst in the buffer chamber (2).
3. The carbon nanotube growth system of claim 1, wherein: pressure gauges for detecting pressure are arranged in the buffer chamber (2) and the reaction chamber (3), and detected pressure data are sent to the control unit.
4. The carbon nanotube growth system of claim 1, wherein: a temperature detector is arranged in the reaction chamber (3); the temperature detector transmits the detected temperature data to the control unit.
5. The carbon nanotube growth system of claim 1, wherein: the catalyst outlet on the jet milling chamber (1) is positioned above the buffer chamber (2); the first conveying structure comprises a first pipeline (6) and a first sealing assembly, and two ends of the first pipeline (6) are respectively connected with the catalyst buffering inlet and the catalyst outlet; the first sealing assembly is used for sealing or opening a first pipeline (6); the second conveying structure comprises a second pipeline (7) and a second sealing assembly, the buffer chamber (2) is positioned above the reaction chamber (3), and the second pipeline (7) is used for connecting a catalyst buffer outlet and a feed inlet of the reaction chamber (3); the second sealing assembly is used for sealing or opening a second pipeline (7).
6. The carbon nanotube growth system of claim 1, wherein: the reaction chamber (3) is provided with an air outlet (13) and two air inlets (12), the air outlet (13) is used for discharging air in the reaction chamber (3), and the air outlet (13) is provided with an air outlet valve; the two air inlets (12) are connected with the carbon source gas mechanism and the first protection gas mechanism, and the air inlets (12) are provided with air inlet valves; the two air inlets (12) are respectively positioned at the upper side and the lower side of the reaction chamber (3).
CN202310570109.8A 2023-05-19 2023-05-19 Carbon nanotube growth system Active CN116495725B (en)

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