A carbon nanotube fluidized bed purification process and fluidized bed reaction device
The chlorine gas flow rate is controlled by inert gas purging and a sealing mechanism in the fluidized reaction chamber. Combined with the automatic cooling and collection of solid particles by a floating mechanism, the problems of chlorine matching and tail gas treatment in the fluidized purification of carbon nanotubes are solved, and an efficient carbon nanotube purification process is achieved.
Patent Information
- Application Number
- CN202311727460.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-14
- Publication Date
- 2025-09-23
- Estimated Expiration
- 2043-12-14
AI Technical Summary
In the existing fluidized bed purification process for carbon nanotubes, the amount of chlorine introduced must match the amount of carbon nanotubes delivered, otherwise it will easily lead to incomplete reaction or waste of chlorine, and the metal chlorides in the exhaust gas will form particulate matter after cooling, increasing the exhaust gas treatment pressure.
Inert gas is used to blow carbon nanotubes into the fluidized reaction chamber, and the flow of carbon nanotubes drives the sealing mechanism to control the amount of chlorine introduced. The high-temperature exhaust gas enters the cooling chamber and is cooled to form solid particles, which are automatically collected by the floating mechanism.
The precise control of the amount of chlorine introduced is achieved to avoid inadequate reaction, automatically cool and collect metal compounds in the tail gas, and reduce the pressure of tail gas treatment.
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Figure CN117699784B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of fluidized beds, in particular to a carbon nanotube fluidization purification process method and a fluidized bed reaction device. Background Art
[0002] Carbon nanotubes, due to their excellent electrical conductivity and mechanical properties, good physical and chemical stability, and low density, have broad application prospects in lithium-ion battery conductive agents, electronic devices, high-performance composite materials, catalyst supports, and other fields. Currently, carbon nanotubes have been mass-produced at low cost through chemical vapor deposition (CVD) technology.
[0003] Chinese Patent Publication No. CN111362255A discloses a fluidized bed purification process for carbon nanotubes. In a fluidized bed reactor equipped with an air inlet, an exhaust outlet, a fluidized reaction chamber, a carbon nanotube filling port, and a carbon nanotube discharge port, the carbon nanotubes to be treated react with a halogen-containing gas in the fluidized reaction chamber. The process comprises: a) adding the carbon nanotubes to be treated into the fluidized reaction chamber heated to a certain temperature; b) introducing a fluidizing gas into the fluidized reaction chamber; step b) includes: b1 ) introducing an inert gas into the fluidized reaction chamber from the air inlet at a first flow rate to fluidize the carbon nanotubes in the fluidized reaction chamber; b2) after introducing the inert gas for a certain period of time, introducing a halogen-containing gas into the fluidized reaction chamber from the air inlet at a second flow rate; b3) after introducing the halogen-containing gas for a certain period of time, repeating the above steps b1) and b2) in sequence; in step b), the second flow rate is less than the first flow rate, and the carbon nanotubes in the fluidized reaction chamber are always in a fluidized state by controlling the flow rate and time of the fluidizing gas introduced in step b).
[0004] During the carbon nanotube purification process in the above-mentioned prior art, chlorine needs to be introduced into the fluidized bed. During the carbon nanotube purification process, chlorine produces metal chlorides, which are discharged with the exhaust gas. Since the amount of chlorine introduced needs to match the amount of carbon nanotubes delivered, otherwise it is easy to cause a large amount of chlorine to be introduced, resulting in insufficient reaction, or a small amount of chlorine to be introduced, affecting the purification of carbon nanotubes. The fluidized bed in the prior art cannot solve this problem. Secondly, the metal chlorides in the exhaust gas can form particulate matter upon cooling. After being discharged with the exhaust gas, the subsequent treatment pressure of the exhaust gas increases.
[0005] To this end, we propose a fluidized bed purification process for carbon nanotubes and a fluidized bed reaction device. Summary of the Invention
[0006] The object of the present invention is to provide a fluidized bed purification process for carbon nanotubes and a fluidized bed reaction device to solve the problems raised in the above background technology.
[0007] To achieve the above objectives, the present invention provides the following technical solution: a fluidized bed purification process for carbon nanotubes, comprising:
[0008] The carbon nanotubes in the raw material tank are purged with inert gas, so that the carbon nanotubes are transported through the transport pipeline to the fluidized reaction chamber heated to a certain temperature, and the carbon nanotubes are in a fluidized state;
[0009] Chlorine gas is introduced into an air inlet pipe of the fluidized bed reactor chamber. A sealing mechanism is provided on the air inlet pipe, and a driving mechanism for driving the sealing mechanism is provided on the delivery pipeline. The driving mechanism generates a driving force by the flow of carbon nanotubes in the delivery pipeline, thereby directly controlling the on-off frequency of the sealing mechanism by the delivery rate of the carbon nanotubes.
[0010] After entering the fluidized reaction chamber, the carbon nanotubes and chlorine are subjected to high-temperature fluidization purification in the fluidized reaction chamber. After fluidization purification, the high-temperature exhaust gas containing the chlorine metal compound in the fluidized reaction chamber pushes the floating mechanism, causing the floating mechanism to operate and drive multiple cooling chambers rotatably connected to the fluidized reaction chamber to swing upward, while causing the openings of the cooling chambers to face upward, thereby allowing the high-temperature exhaust gas to enter the multiple cooling chambers for cooling. During the cooling process, the chlorine metal compound will cool and form solid particles that remain in the cooling chamber. When the pressure of the high-temperature exhaust gas in the fluidized reaction chamber decreases, the pushing force of the high-temperature exhaust gas on the floating mechanism decreases, thereby causing the cooling chamber to swing downward and the opening of the cooling chamber to swing downward, thereby causing the solid particles in the cooling chamber to fall from the opening of the cooling chamber to the collection mechanism of the fluidized reaction chamber.
[0011] After the purification is completed, an inert gas is introduced into the fluidized reaction chamber to discharge the carbon nanotubes into an external collection tank through the discharge port.
[0012] A fluidized bed reaction device, comprising a fluidized reaction chamber provided with an air inlet pipe and a material outlet, the fluidized reaction chamber being connected through a delivery pipeline, the delivery pipeline being fixedly connected to a raw material tank at one end away from the fluidized reaction chamber, and further comprising:
[0013] a sealing mechanism provided on the air intake pipe and used to seal the air intake pipe;
[0014] a driving mechanism provided in the conveying pipeline and used to drive the sealing mechanism to intermittently operate;
[0015] A heat insulation plate fixedly connected to the fluidized reaction chamber and located above the discharge port, the heat insulation plate partitioning the interior of the fluidized reaction chamber into a cooling chamber and a fluidized purification chamber from top to bottom, the air inlet pipe, the discharge port, the conveying pipeline and the fluidized purification chamber being connected;
[0016] an exhaust gas discharge pipe vertically passing through the heat insulation plate and having its upper end passing through the fluidized bed reaction chamber;
[0017] A plurality of cooling bins hinged to the exhaust pipe via hinged arms, wherein the cooling bins are hollow and have an opening on a side facing the exhaust pipe, wherein a bellows is installed in the opening, and the bellows penetrates the exhaust pipe;
[0018] A floating mechanism is provided on the heat insulation plate, and the floating mechanism is used to drive the plurality of cooling bins to swing up and down synchronously.
[0019] Preferably, the sealing mechanism includes a sealing seat integrally formed and fixed to the intake pipe, a connecting cavity is provided in the sealing seat, the connecting cavity is connected to the interior of the intake pipe, a piston is engaged in the connecting cavity, and when the piston slides up and down in the connecting cavity to a fixed position, the intake pipe can be completely closed.
[0020] Preferably, the driving mechanism includes a mounting seat fixedly connected to the conveying pipeline, the interior of the mounting seat is hollow and is horizontally rotatably connected to a rotating shaft, the part of the rotating shaft located in the mounting seat is fixed with multiple rotating plates at equal angles, the two ends of the rotating shaft passing through the mounting seat are each fixed with a swing arm, the piston is coaxially fixed with a sliding rod, the sliding rod passes through the sealing seat and can slide freely up and down, the upper end of the sliding rod is fixed with a lifting plate, the upper surface of the lifting plate and the swing arm are in a cam matching structure, a first spring is vertically installed in the connecting cavity, the elastic force of the first spring pushes against the piston and drives the piston to move upward.
[0021] Preferably, one end of the swing arm away from the rotating shaft is rotatably connected to a roller, and the roller is in rolling contact with the upper surface of the lifting plate.
[0022] Preferably, the floating mechanism includes a fixed bin vertically fixed to the bottom of the heat insulation plate, a floating plug is engaged in the fixed bin, the floating plug forms a sliding fit with the inner wall of the fixed bin, and a plurality of connecting rods are vertically fixed to the upper end face of the floating plug, the upper ends of the connecting rods pass through the heat insulation plate and can slide freely, the ends of the plurality of connecting rods passing through the cooling chamber are commonly fixed to a floating plate, a plurality of hinged arms located on the same side of the exhaust pipe are commonly hinged to a hinge rod, the lower ends of the plurality of hinge rods are hinged to the floating plate, and the floating plug is provided with a connecting unit, which is used to connect the cooling chamber and the interior of the fluidized purification chamber.
[0023] Preferably, the connecting unit includes a lifting rod that is vertically inserted into the floating plug and can slide freely. The upper end of the lifting rod is fixedly connected to a bracket, and the lower end of the lifting rod is fixedly connected to a sealing plug. The end face of the floating plug is provided with a plurality of through grooves distributed along a ring. When the upper end face of the sealing plug is against the lower end face of the floating plug, the sealing plug can close the through grooves. The lifting rod sleeve is wrapped with a second spring, and the two ends of the second spring in the direction of elastic force elastically press against the bracket and the floating plug respectively.
[0024] Preferably, the facing surfaces of the floating plug and the sealing plug are each provided with a rubber layer.
[0025] Preferably, a collection mechanism is provided in the exhaust gas exhaust pipe, and the collection mechanism includes a baffle coaxially fixed to the inner wall of the exhaust gas exhaust pipe, the outer diameter of the baffle increases from top to bottom, and the outer wall of the exhaust gas exhaust pipe is provided with a collection port corresponding to the end with the largest outer diameter of the baffle.
[0026] Preferably, when the floating plug moves upward to a fixed position, the floating plate slides on the exhaust gas exhaust pipe and closes the collecting port.
[0027] Compared with the prior art, the present invention has the following beneficial effects:
[0028] In the present invention, when carbon nanotubes are transported from a delivery pipeline to a fluidized bed reactor, the carbon nanotubes impact a rotating plate, causing the rotating plate to rotate. When the rotating shaft rotates, the roller intermittently abuts against the lifting plate and moves downward, thereby causing the sliding rod to drive the piston to move up and down. The piston can close the air inlet pipe during movement, thereby directly controlling the delivery rate of the carbon nanotubes in the delivery pipeline and the amount of chlorine introduced.
[0029] The present invention allows high-temperature exhaust gas to enter the cooling bin and the exhaust gas discharge pipe, and the cooling medium in the cooling chamber cools the exhaust gas in the cooling bin and the exhaust gas discharge pipe, thereby cooling the chlorine-containing metal compounds in the exhaust gas, so that the metal compounds form solid particles and are collected in the cooling bin. When the exhaust gas pressure in the fluidized reaction bin decreases, the floating mechanism is pushed down by the exhaust gas, thereby causing the opening of the cooling bin to face downward, so that the solidified solid particles in the cooling bin fall into the exhaust gas discharge pipe and are collected by the collecting mechanism, thereby achieving automatic cooling of the chlorine-containing metal compounds and automatic collection of the cooled solid particles.
[0030] The present invention uses the elastic support of the second spring on the bracket to make the end face of the sealing plug abut against the end face of the floating plug. As a result, when the pressure of the high-temperature exhaust gas in the fluidized bed reaction chamber increases, the high-temperature exhaust gas continuously lifts the floating plug until the bracket abuts against the bottom surface of the insulation board. As the floating plug moves upward, the floating plug and the sealing plug are separated from the state of end face abutment, thereby allowing the high-temperature exhaust gas to enter the exhaust gas exhaust pipe and the cooling chamber from the through groove. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Figure 1 Schematic diagram of the overall structure of a fluidized bed reaction device in the present invention;
[0032] Figure 2 for Figure 1 Schematic cross-sectional view of the structure;
[0033] Figure 3 for Figure 2 A magnified schematic diagram of the local structure at point A;
[0034] Figure 4 for Figure 2 A magnified schematic diagram of the local structure at point B in the middle;
[0035] Figure 5 This is a schematic diagram of the structure of the cooling chamber, exhaust gas exhaust pipe and heat insulation board after assembly in the present invention;
[0036] Figure 6 for Figure 5 A schematic cross-sectional view of the middle structure;
[0037] Figure 7 for Figure 5 Schematic diagram of the structure from a frontal perspective;
[0038] Figure 8 for Figure 5 Schematic diagram of the middle structure from an upward perspective;
[0039] Figure 9 This is a schematic diagram of the structure of the heat insulation board and the exhaust gas exhaust pipe after assembly in the present invention;
[0040] Figure 10 for Figure 9 Schematic cross-sectional view of the structure;
[0041] Figure 11 It is a structural schematic diagram of the cooling bin in the present invention;
[0042] Figure 12 for Figure 11 Schematic cross-sectional view of the structure.
[0043] In the figure, the description of each figure mark is as follows: 1. exhaust gas exhaust pipe; 2. discharge port; 3. raw material tank; 4. conveying pipeline; 5. mounting seat; 6. lifting plate; 7. sliding rod; 8. air inlet pipe; 9. sealing seat; 10. fluidized bed reaction chamber; 11. bellows; 12. cooling chamber; 13. cooling chamber; 14. heat insulation board; 15. fluidized bed purification chamber; 16. fixed chamber; 17. roller; 18. swing arm; 19. rotating plate; 20. avoidance port; 21. rotating shaft; 22. connecting chamber; 23. first spring; 24. piston; 25. hinge rod; 26. floating plate; 27. bracket; 28. second spring; 29. floating plug; 30. through groove; 31. connecting rod; 32. sealing plug; 33. collecting port; 34. baffle. DETAILED DESCRIPTION
[0044] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0045] See also Figure 1 - Figure 12The present invention provides a technical solution: a fluidized bed reaction device, comprising a fluidized reaction chamber 10 provided with an air inlet pipe 8 and a discharge port 2, the fluidized reaction chamber 10 is connected with a conveying pipeline 4, the conveying pipeline 4 is fixedly connected to a raw material tank 3 at one end away from the fluidized reaction chamber 10, the air inlet pipe 8 is connected to an external chlorine delivery pump at one end away from the fluidized reaction chamber 10, the chlorine delivery pump delivers chlorine to the air inlet pipe 8, the discharge port 2 is connected to an external finished product tank through a pipeline, a heat insulation board 14 is coaxially welded in the fluidized reaction chamber 10, the heat insulation board 14 is located above the discharge port 2, the heat insulation board 14 divides the interior of the fluidized reaction chamber 10 into a cooling chamber 13 and a fluidized purification chamber 15 from top to bottom, the air inlet pipe 8, the discharge port 2, the conveying pipeline 4 and the fluidized purification chamber 15 are connected, and an exhaust gas discharge pipe 1 is vertically passed through the heat insulation board 14 The upper end of the exhaust gas exhaust pipe 1 passes through the fluidized reaction chamber 10, and the upper end of the exhaust gas exhaust pipe 1 is connected to the external pipeline. The periphery of the exhaust gas exhaust pipe 1 is welded with multiple groups of hinged shafts from top to bottom, and a hinged arm is hinged on the hinged shaft. A cooling chamber 12 is welded at one end in the length direction of the hinged arm. The outer contour of the cooling chamber 12 is roughly fan-shaped and hollow inside. The cooling chamber 12 is provided with an opening on the side facing the exhaust gas exhaust pipe 1, and a bellows 11 is installed in the opening. A bellows socket is provided on the exhaust gas exhaust pipe 1, and the end of the bellows 11 away from the cooling chamber 12 is inserted into the bellows socket, so that the exhaust gas exhaust pipe 1 is connected to the cooling chamber 12 through the bellows 11. The cooling medium is filled in the cooling chamber 13, or a heat exchange device is installed in the cooling chamber 13. The heat exchange device or the cooling medium is used to cool the cooling chamber 12;
[0046] A sealing seat 9 is integrally formed and welded at the middle of the intake pipe 8. A connecting cavity 22 is provided in the sealing seat 9. The connecting cavity 22 is connected to the inside of the intake pipe 8. A piston 24 is engaged in the connecting cavity 22. When the piston 24 slides up and down in the connecting cavity 22 to a fixed position, the intake pipe 8 can be completely closed. A mounting seat 5 is welded on the delivery pipeline 4. The mounting seat 5 is hollow inside and is connected to a rotating shaft 21 for horizontal rotation. A plurality of rotating pieces 19 are fixedly connected at equal angles to the part of the rotating shaft 21 located in the mounting seat 5. An avoidance port 20 is provided between the mounting seat 5 and the delivery pipeline 4, so that the end of the rotating piece 19 away from the rotating shaft 21 can freely pass through the avoidance port 20. The rotating shaft 21 The two ends of the mounting seat 5 are fixed with a swing arm 18, and the piston 24 is coaxially fixed with a sliding rod 7. The sliding rod 7 passes through the sealing seat 9 and can slide freely up and down. The upper end of the sliding rod 7 is fixed with a lifting plate 6. The upper surface of the lifting plate 6 and the swing arm 18 form a cam matching structure. The end of the swing arm 18 away from the rotating shaft 21 is rotatably connected to the roller 17. The roller 17 is in rolling contact with the upper surface of the lifting plate 6. A first spring 23 is vertically installed in the communicating cavity 22. The elastic force of the first spring 23 pushes against the piston 24 and drives the piston 24 to move upward. When the carbon nanotubes are blown from the raw material tank 3 into the conveying pipeline 4, the carbon nanotubes flow in the conveying pipeline 4 and rotate against the rotating piece 19. The impact is generated, which can drive the rotating piece 19 to rotate, so that the rotating piece 19 can drive the rotating shaft 21 to rotate. When the rotating shaft 21 rotates, it will drive the swing arm 18 to rotate around the axial direction of the rotating shaft 21, thereby causing the roller 17 to rotate around the axial direction of the rotating shaft 21, and causing the roller 17 to roll with the top surface of the lifting plate 6. During rolling contact, the roller 17 generates a downward push force on the lifting plate 6, thereby causing the lifting plate 6 to drive the sliding rod 7 to move downward, and drive the piston 24 to move downward, thereby closing the air inlet pipe 8, so that the chlorine gas will be temporarily suspended from being delivered to the fluidized reaction chamber 10. When the roller 17 is out of contact with the lifting plate 6, the first A spring 23 changes from a compressed state to an extended state and drives the piston 24 to move upward, so that the chlorine in the air inlet pipe 8 can be normally transported to the fluidized bed reaction chamber 10. In this way, the chlorine can be intermittently transported to the fluidized bed reaction chamber 10, and the intermittent frequency is directly related to the rotation rate of the rotating shaft 21, and the rotation rate of the rotating shaft 21 is proportional to the rotation rate of the rotating plate 19. In addition, the rotation rate of the rotating plate 19 is directly proportional to the transportation rate of the carbon nanotubes in the transportation pipeline 4. In this way, the transportation rate of the carbon nanotubes can directly adjust the chlorine transportation rate in real time, avoiding the waste of chlorine and the insufficient reaction caused by insufficient chlorine intake.
[0047] A cylindrical fixed chamber 16 is vertically welded to the bottom of the heat insulation plate 14. Both ends of the fixed chamber 16 are open and a floating plug 29 is engaged therein. The floating plug 29 forms a sliding fit with the inner wall of the fixed chamber 16, that is, the floating plug 29 can slide up and down in the fixed chamber 16 and a plurality of connecting rods 31 are vertically fixed to the upper end surface of the floating plug 29. The upper end of the connecting rod 31 passes through the heat insulation plate 14 and can slide freely. One end of the plurality of connecting rods 31 that passes into the cooling chamber 13 is commonly fixed to the floating plate 26. The plurality of hinged arms located on the same side of the exhaust gas exhaust pipe 1 are commonly hinged to the hinge rod 25. The lower ends of the plurality of hinge rods 25 are hinged to the floating plate 26. A lifting rod is vertically passed through the floating plug 29. The lifting rod can slide freely on the floating plug 29. The upper end of the lifting rod is fixed to a cross-shaped support The bracket 27 is configured such that the outer dimensions of the bracket 27 cannot pass through the exhaust gas exhaust pipe 1. A sealing plug 32 is fixed to the lower end of the jacking rod. A plurality of through grooves 30 distributed along a ring are provided on the end surface of the floating plug 29. When the upper end surface of the sealing plug 32 abuts against the lower end surface of the floating plug 29, the sealing plug 32 can close the through groove 30. The jacking rod sleeve is wrapped with a second spring 28. The two ends of the second spring 28 elastically abut against the bracket 27 and the floating plug 29 respectively, so that initially, the second spring 28 generates an upward elastic abutting force on the bracket 27, thereby abutting the upper end surface of the sealing plug 32 against the lower end surface of the floating plug 29 and closing the through groove 30. A baffle 34 is coaxially welded to the inner wall of the exhaust gas exhaust pipe 1. The outer diameter of the baffle 34 increases from top to bottom, and an air outlet is provided in the middle of the baffle 34. The diameter of the air outlet is much smaller than the inner diameter of the exhaust pipe 1. The outer wall of the exhaust pipe 1 is provided with a collecting port 33 corresponding to the end with the largest outer diameter of the baffle 34. When the pressure of the high-temperature exhaust (chlorine-containing metal compounds) in the fluidized reaction chamber 10 increases, the high-temperature exhaust will push the floating plug 29 and drive the floating plug 29 to slide upward. When the floating plug 29 slides upward, it simultaneously drives the sealing plug 32 to move upward until the bracket 27 abuts the lower surface of the insulation board 14. At this time, as the floating plug 29 moves upward, the upper end surface of the sealing plug 32 is separated from the lower end surface of the floating plug 29, thereby allowing the high-temperature exhaust to enter the exhaust pipe 1 from the through groove 30. In addition, synchronously, when the floating plug 29 moves upward until the bracket 27 abuts the lower surface of the insulation board 14, the floating plug 29 The plug 29 drives the connecting rod 31 to move upward, so as to drive the floating plate 26 to move upward. When the floating plate 26 moves upward, it drives the hinge rod 25 to drive the hinged arm to rotate, so that the hinged arm drives the cooling bin 12 to swing downward, so that the opening of the cooling bin 12 faces upward, and then the high-temperature exhaust gas in the exhaust gas exhaust pipe 1 and the cooling bin 12 will be cooled by the cooling medium in the cooling chamber 13 or the heat exchange equipment, so that the chlorine-containing metal compounds in the exhaust gas form solid particles and are deposited in the cooling bin 12, or fall from the exhaust gas exhaust pipe 1 and accumulate on the surface of the baffle 34 to a large extent. In addition, the setting of the cooling bin 12 makes the exhaust gas enter the exhaust gas exhaust pipe 1 and pass through the cooling bin 12, so that the exhaust pressure in the exhaust gas exhaust pipe 1 is relatively small.In order to avoid the high exhaust gas escape rate affecting the collection of solid particles, after the exhaust gas enters the exhaust gas exhaust pipe 1, the exhaust gas pressure in the fluidized reaction chamber 10 gradually decreases, and the air pressure in the exhaust gas exhaust pipe 1 is lower than the air pressure in the fluidized reaction chamber 10, thereby causing the floating plug 29 to slide downward. Under the elastic push of the second spring 28 on the bracket 27, the sealing plug 32 will move upward relative to the floating plug 29, so that the upper end surface of the sealing plug 32 is against the lower end surface of the floating plug 29. In addition, preferably, a return spring (not shown in the figure) is vertically installed in the fixed chamber 16. The return spring is in a compressed state when the floating plug 29 slides upward, and when the exhaust gas pressure in the fluidized reaction chamber 10 drops, the return spring will drive The dynamic floating plug 29 slides downward smoothly, allowing the cooling chamber 12 to swing upward relatively quickly. In addition, when the floating plug 29 moves upward to a fixed position, the floating plate 26 slides on the exhaust gas exhaust pipe 1 and closes the collection port 33, allowing the high-temperature exhaust gas to fully enter the exhaust gas exhaust pipe 1 and the cooling chamber 12. In addition, the outer wall of the fluidized bed reactor 10 is provided with a discharge collection port (not shown in the figure). A baffle is installed at the discharge collection port. When the baffle is opened, the metal particles falling from the collection port 33 can be collected. In addition, the opposing surfaces of the floating plug 29 and the sealing plug 32 are each provided with a rubber layer (not shown in the figure). This ensures that when the end faces of the floating plug 29 and the sealing plug 32 abut against each other, the sealing degree of the abutting surfaces is better.
[0048] This embodiment also discloses a fluidized purification process for carbon nanotubes, comprising:
[0049] The carbon nanotubes in the raw material tank 3 are purged by inert gas, so that the carbon nanotubes are transported from the conveying pipe 4 to the fluidized reaction chamber 10 heated to a certain temperature (600°C-800°C). The carbon nanotubes are in a fluidized state. When the carbon nanotubes are blown from the raw material tank 3 to the conveying pipe 4, the carbon nanotubes flow in the conveying pipe 4 and impact the rotating piece 19, thereby driving the rotating piece 19 to rotate, so that the rotating piece 19 can drive the rotating shaft 21 to rotate. When the rotating shaft 21 rotates, it will drive the swing arm 18 to rotate around the axial direction of the rotating shaft 21, thereby causing the roller 17 to rotate around the axial direction of the rotating shaft 21, and causing the roller 17 to roll with the top surface of the lifting plate 6. During the rolling contact, the roller 17 generates a downward push force on the lifting plate 6, thereby causing the lifting plate 6 to drive the sliding rod 7 to move downward and drive the piston 2 4 moves downward, thereby closing the air inlet pipe 8, so that the chlorine gas will be temporarily suspended from being transported into the fluidized reaction chamber 10. When the roller 17 is out of contact with the lifting plate 6, the first spring 23 will be changed from a compressed state to an extended state, and drive the piston 24 to move upward, so that the chlorine gas in the air inlet pipe 8 can be normally transported into the fluidized reaction chamber 10. In this way, the chlorine gas can be intermittently transported into the fluidized reaction chamber 10, and the intermittent frequency is directly related to the rotation speed of the rotating shaft 21, and the rotation speed of the rotating shaft 21 is proportional to the rotation speed of the rotating piece 19. In addition, the rotation speed of the rotating piece 19 is directly proportional to the transport speed of the carbon nanotubes in the transport pipeline 4. In this way, the transport speed of the carbon nanotubes can directly adjust the chlorine transport speed in real time, avoiding the waste of chlorine gas and the inadequate reaction caused by insufficient chlorine gas intake;
[0050] After entering the fluidized reaction chamber 10, the carbon nanotubes and chlorine are purified by high-temperature fluidization in the fluidized reaction chamber 10. After fluidization purification, when the pressure of the high-temperature tail gas (chlorine-containing metal compounds) in the fluidized reaction chamber 10 increases, the high-temperature tail gas will push the floating plug 29 and drive the floating plug 29 to slide upward. When the floating plug 29 slides upward, it will simultaneously drive the sealing plug 32 to move upward until the bracket 27 rests against the lower surface of the insulation board 14. At this time, as the floating plug 29 moves upward, the sealing plug 32 is pushed upward. 2 is away from the lower end of the floating plug 29, thereby allowing the high-temperature exhaust gas to enter the exhaust gas exhaust pipe 1 from the through groove 30. In addition, synchronously, when the floating plug 29 moves upward until the bracket 27 abuts against the lower surface of the heat insulation plate 14, the floating plug 29 drives the connecting rod 31 to move upward, so that the floating plate 26 moves upward. When the floating plate 26 moves upward, it drives the hinge rod 25 to drive the hinge arm to rotate, so that the hinge arm drives the cooling chamber 12 to swing downward, so that the cooling chamber 12 The opening is facing upward, and then the high-temperature exhaust gas will be cooled by the cooling medium or heat exchange equipment in the cooling chamber 13 in the exhaust gas exhaust pipe 1 and the cooling chamber 12, thereby causing the chlorine-containing metal compounds in the exhaust gas to form solid particles and deposit in the cooling chamber 12, or fall from the exhaust gas exhaust pipe 1 and accumulate to a large extent on the surface of the baffle 34. In addition, the setting of the cooling chamber 12 makes it possible for the exhaust gas to have a low exhaust pressure in the exhaust gas exhaust pipe 1 after entering the exhaust gas exhaust pipe 1, thereby avoiding a high exhaust gas escape rate that affects the collection of solid particles. After the exhaust gas enters the exhaust gas exhaust pipe 1, the exhaust pressure in the fluidized reaction chamber 10 gradually decreases, and the air pressure in the exhaust gas exhaust pipe 1 is lower than the air pressure in the fluidized reaction chamber 10, thereby causing the floating plug 29 to slide downward. Under the elastic supporting force of the second spring 28 on the bracket 27, the sealing plug 32 will move upward relative to the floating plug 29, so that the upper end surface of the sealing plug 32 is against the lower end surface of the floating plug 29.
[0051] After purification is completed, the discharge port 2 is opened and inert gas is introduced into the fluidized reaction chamber 10 . The inert gas will generate turbulence on the carbon nanotubes and cause the carbon nanotubes to be discharged into an external collection tank through the discharge port 2 .
[0052] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device that includes a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations may be made to these embodiments without departing from the principles and spirit of the invention, and the scope of the invention is defined by the appended claims and their equivalents.
Claims
1. A carbon nanotube fluidization purification process, characterized in that: include: The carbon nanotubes in the raw material tank (3) are purged by inert gas, so that the carbon nanotubes are transported from the transport pipeline (4) to the fluidized reaction chamber (10) heated to a certain temperature, and the carbon nanotubes are in a fluidized state; Chlorine gas is introduced into the air inlet pipe (8) of the fluidized reaction chamber (10), a sealing mechanism is provided on the air inlet pipe (8), and a driving mechanism for driving the sealing mechanism is provided on the delivery pipeline (4), wherein the driving mechanism generates a driving force by the flow of the carbon nanotubes in the delivery pipeline (4), thereby enabling the carbon nanotube delivery rate to directly control the on-off frequency of the sealing mechanism; After entering the fluidized reaction chamber (10), the carbon nanotubes and chlorine are purified by high-temperature fluidization in the fluidized reaction chamber (10). After fluidization purification, the high-temperature tail gas containing chlorine metal compounds in the fluidized reaction chamber (10) pushes the floating mechanism, causing the floating mechanism to operate and drive multiple cooling chambers (12) connected to the fluidized reaction chamber (10) to swing upward, while making the mouth of the cooling chamber (12) face upward, thereby allowing the high-temperature tail gas to enter the multiple cooling chambers (12) for cooling. However, during the cooling process, the chlorine-containing metal compound will cool and form solid particles and remain in the cooling bin (12). When the high-temperature exhaust gas pressure in the fluidized reaction bin (10) decreases, the thrust force of the high-temperature exhaust gas on the floating mechanism decreases, thereby causing the cooling bin (12) to swing downward, and causing the opening of the cooling bin (12) to swing downward, thereby causing the solid particles in the cooling bin (12) to fall from the opening of the cooling bin (12) to the collecting mechanism of the fluidized reaction bin (10); After the purification is completed, an inert gas is introduced into the fluidized reaction chamber (10), so that the carbon nanotubes are discharged into an external collection tank through the discharge port (2).
2. A fluidized bed reaction device, comprising a fluidized reaction chamber (10) provided with an air inlet pipe (8) and a material outlet (2), wherein the fluidized reaction chamber (10) is connected to a conveying pipeline (4), and a raw material tank (3) is fixedly connected to one end of the conveying pipeline (4) away from the fluidized reaction chamber (10), characterized in that: Also includes: a sealing mechanism provided on the air intake pipe (8) and used to seal the air intake pipe (8); A driving mechanism provided in the delivery pipeline (4) and used for driving the sealing mechanism to intermittently operate; A heat insulation plate (14) fixedly connected to the fluidized reaction chamber (10) and located above the discharge port (2), wherein the heat insulation plate (14) divides the interior of the fluidized reaction chamber (10) into a cooling chamber (13) and a fluidized purification chamber (15) from top to bottom, and the air inlet pipe (8), the discharge port (2), the conveying pipeline (4) and the fluidized purification chamber (15) are connected; An exhaust gas discharge pipe (1) vertically passing through the heat insulation plate (14) and having its upper end passing through the fluidized reaction chamber (10); A plurality of cooling bins (12) hinged to the exhaust gas exhaust pipe (1) via hinged arms, the cooling bins (12) being hollow inside and having an opening on a side facing the exhaust gas exhaust pipe (1), the opening being provided with a bellows (11), and the bellows (11) penetrating the exhaust gas exhaust pipe (1); A floating mechanism is provided on the heat insulation plate (14), and the floating mechanism is used to drive the plurality of cooling bins (12) to swing up and down synchronously.
3. A fluidized bed reaction device according to claim 2, characterized in that: The sealing mechanism comprises a sealing seat (9) integrally formed and fixed to the intake pipe (8), a connecting cavity (22) being provided in the sealing seat (9), the connecting cavity (22) being connected to the interior of the intake pipe (8), a piston (24) being engaged in the connecting cavity (22), and the piston (24) being able to completely seal the intake pipe (8) when it slides up and down in the connecting cavity (22) to a fixed position.
4. A fluidized bed reaction device according to claim 3, characterized in that: The driving mechanism includes a mounting seat (5) fixed to the conveying pipeline (4), the mounting seat (5) is hollow inside and is horizontally rotatably connected to a rotating shaft (21), a portion of the rotating shaft (21) located inside the mounting seat (5) is fixed with a plurality of rotating plates (19) at equal angles, the rotating shaft (21) passes through the mounting seat (5) and is fixed with a swing arm (18) at both ends, the piston (24) is coaxially fixed with a sliding rod (7), the sliding rod (7) passes through the sealing seat (9) and can slide freely up and down, the upper end of the sliding rod (7) is fixed with a lifting plate (6), the upper surface of the lifting plate (6) and the swing arm (18) are in a cam-matching structure, a first spring (23) is vertically installed in the connecting cavity (22), the elastic force of the first spring (23) presses against the piston (24) and drives the piston (24) to move upward.
5. A fluidized bed reaction device according to claim 4, characterized in that: One end of the swing arm (18) away from the rotating shaft (21) is rotatably connected to a roller (17), and the roller (17) is in rolling contact with the upper surface of the lifting plate (6).
6. A fluidized bed reaction device according to claim 2, characterized in that: The floating mechanism includes a fixed bin (16) vertically fixed to the bottom of the heat insulation plate (14), a floating plug (29) is engaged in the fixed bin (16), the floating plug (29) and the inner wall of the fixed bin (16) form a sliding fit, and a plurality of connecting rods (31) are vertically fixed to the upper end face of the floating plug (29), the upper ends of the connecting rods (31) pass through the heat insulation plate (14) and can slide freely, and one end of the plurality of connecting rods (31) passing into the cooling chamber (13) is commonly fixed to the floating plate (26), and a plurality of hinged arms located on the same side of the exhaust gas exhaust pipe (1) are commonly hinged to a hinge rod (25), and the lower ends of the plurality of hinge rods (25) are hinged to the floating plate (26), and the floating plug (29) is provided with a connecting unit, and the connecting unit is used to connect the cooling chamber (13) and the fluidized purification chamber (15) internally.
7. A fluidized bed reaction device according to claim 6, characterized in that: The connecting unit includes a lifting rod vertically passing through the floating plug (29) and capable of sliding freely. The upper end of the lifting rod is fixedly connected to a bracket (27), and the lower end of the lifting rod is fixedly connected to a sealing plug (32). The end surface of the floating plug (29) is provided with a plurality of through grooves (30) distributed along a ring. When the upper end surface of the sealing plug (32) abuts against the lower end surface of the floating plug (29), the sealing plug (32) can close the through grooves (30). The lifting rod sleeve is wrapped with a second spring (28), and the two ends of the second spring (28) in the direction of elastic force elastically abut the bracket (27) and the floating plug (29) respectively.
8. A fluidized bed reaction device according to claim 7, characterized in that: The facing surfaces of the floating plug (29) and the sealing plug (32) are each provided with a rubber layer.
9. The fluidized bed reaction device according to claim 7, characterized in that: The exhaust gas discharge pipe (1) is provided with a collecting mechanism, the collecting mechanism comprising a baffle (34) coaxially fixed to the inner wall of the exhaust gas discharge pipe (1), the outer diameter of the baffle (34) increasing from top to bottom, and the outer wall of the exhaust gas discharge pipe (1) is provided with a collecting port (33) corresponding to the end with the largest outer diameter of the baffle (34).
10. The fluidized bed reaction device according to claim 9, characterized in that: When the floating plug (29) moves upward to a fixed position, the floating plate (26) slides on the exhaust gas discharge pipe (1) and closes the collecting port (33).
Citation Information
Patent Citations
Carbon nanotube fluidization purification process method and fluidized bed reaction device
CN111362255A
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CN117006844A