Cyclone separator and method for preparing graphene through high-pressure physical stripping method

By adopting high-pressure physical peeling method and cyclone separator design in the graphene preparation device, the problem of cumbersome loss and maintenance of graphene is solved, efficient preparation and separation of graphene is achieved, and the sealing and operation convenience of the equipment are improved.

CN119972380APending Publication Date: 2025-05-13FUJIAN JIADA GRAPHENE CO LTD
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Patent Information

Application Number
CN202510143634.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-10
Publication Date
2025-05-13

AI Technical Summary

Technical Problem

During the use of the existing graphene preparation device, the bottom collection barrel is not tightly sealed, resulting in loss of graphene material. After long-term use, the inner wall will be adhered to and accumulated by graphene, which requires regular disassembly and maintenance, and the operation is complicated.

Method used

A cyclone separator for graphene is prepared by high-pressure physical peeling method, including a cyclone separator, a cutoff assembly, a cleaning assembly and a reinforced seal assembly. The fast-loading assembly realizes the convenience of solid material collection. The cut-off assembly is used for sealing and intercepting flow, and the cleaning assembly is subject to high-pressure flushing and cleaning, which strengthens the sealing assembly and improves the sealing performance of the cyclone separation cylinder.

Benefits of technology

It effectively reduces the loss of graphene material, simplifies the cleaning and maintenance process, improves the sealing and operation convenience of the cyclone separation cylinder, and realizes efficient preparation and separation of graphene.

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Abstract

The invention relates to the technical field of graphene preparation, in particular to a cyclone separator and method for preparing graphene through a high-pressure physical stripping method.The cyclone separator comprises a cyclone separation barrel, a cut-off assembly, a cleaning assembly and a reinforced sealing assembly, and an input connecting pipe is arranged at the upper end of one side of the cyclone separation barrel; a solid material collecting tank is arranged at the lower end of the cyclone separation barrel through a quick assembly, after the inner wall of the cyclone separation barrel is subjected to graphene separation for a long time, the inner wall of the cyclone separation barrel can be subjected to high-pressure washing through a cleaning assembly, and during washing, the cyclone separation barrel and the solid material collecting tank are cut off and blocked through a cut-off assembly; and then the graphene-containing liquid is collected in a centralized mode through the liquid discharging control pipe and then is separated, the convenience of cleaning operation is improved, the cleaning effect can be improved by rotating the adjusting assembly in the period, and in addition, under the cooperation effect of the strengthening sealing assembly, sealing strengthening of the cyclone separation barrel can be conducted in combination with use of the cut-off assembly.
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Description

Technical Field

[0001] The invention relates to the technical field of graphene preparation, in particular to a cyclone separator and a method for preparing graphene by a high-pressure physical stripping method. Background Art

[0002] Graphene is a new material with carbon atoms tightly packed into a single-layer two-dimensional honeycomb lattice structure. The carbon atoms are connected by covalent bonds to form a regular hexagonal structure. This tightly packed and orderly arrangement gives graphene unique physical and chemical properties.

[0003] The invention of the existing publication number CN110817854 A discloses a device and method for preparing graphene. The device for preparing graphene includes a reactor, a cyclone separator, a washing tower and a centrifuge, and the method for preparing graphene includes: mixing the raw materials with the reaction liquid and performing a hydrothermal reaction in a closed reactor, rapidly releasing the pressure after the reaction is completed, obtaining primary graphene and graphene-containing gas through a cyclone separator, and washing the graphene-containing gas with water and then performing solid-liquid separation to obtain ultimate graphene; the raw materials include one or more of artificial graphite, natural graphite and graphene oxide; the reaction liquid includes one of water, organic solvent, carbon dioxide, inorganic salt solution or supercritical liquid. The device and method for preparing graphene provided in the present application can realize mass production of graphene, and each batch of production can reach a kilogram-level output. The equipment is easy to scale up and continuous. The above scheme prepares graphene by exfoliation through physical high pressure. In the preparation process, gas-solid mixed graphene is mainly separated by a cyclone separation device, and the graphene that cannot be separated by the cyclone separator is enhanced and separated and prepared by a washing tower, and then the required graphene is obtained by separation and drying. If the bottom collection bucket of the cyclone separator is not tightly sealed during use, the internal vortex of the device may discharge more graphene materials from the exhaust port. In addition, after the cyclone separator is used for a long time, part of the graphene will adhere to and accumulate on the inner wall, and regular disassembly and maintenance operations are required. The operation is time-consuming and labor-intensive, and it is inconvenient to use. Summary of the invention

[0004] The object of the present invention is to provide a cyclone separator and method for preparing graphene by high-pressure physical exfoliation method, so as to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solution: a cyclone separator for preparing graphene by high-pressure physical exfoliation method, comprising:

[0006] A cyclone separation cylinder, wherein an input pipe is provided at an upper end of one side of the cyclone separation cylinder, and a solid material collection tank is provided at the lower end of the cyclone separation cylinder through a quick-install component, wherein the quick-install component comprises a prismatic insert ring and an installation constraint sleeve, wherein the installation constraint sleeve is provided at the lower end of the cyclone separation cylinder, and the prismatic insert ring is provided at the upper end of the solid material collection tank;

[0007] A cut-off assembly, which is arranged on one side of the solid material collection tank, and comprises a cut-off control box, a square cut-off block and a liquid discharge control pipe. The cut-off control box is arranged horizontally on one side of the solid material collection tank close to the cyclone separation cylinder, and the square cut-off block is horizontally movably plugged into the solid material collection tank;

[0008] A cleaning assembly, wherein the cleaning assembly is rotatably arranged at the upper end of the cyclone separation cylinder, and the cleaning assembly comprises a self-rotating disc and a movable inner tube, the self-rotating disc is rotatably plugged into the upper end of the cyclone separation cylinder, an air outlet pipe is vertically arranged at the center of the self-rotating disc, the lower end of the air outlet pipe is plugged into the upper part of the cyclone separation cylinder, the movable inner tube is vertically movably arranged in the air outlet pipe, a rotation adjustment assembly is arranged on the side of the cyclone separation cylinder close to the self-rotating disc, and the rotation adjustment assembly comprises a conversion box, a control bevel gear and a switching guide plate;

[0009] The enhanced sealing component includes a first expansion gas ring and a second expansion gas ring, wherein the first expansion gas ring is arranged on the side of the solid material collection tank sleeved with the cyclone separation cylinder, and the second expansion gas ring is arranged on the side of the cyclone separation cylinder close to the rotating disk.

[0010] Preferably, a socket joint is provided at the upper end of the solid material collection tank, and the lower end of the cyclone separation cylinder is plugged into the socket joint of the solid material collection tank through a sealing ring, a prismatic insert ring is provided at the upper end of the socket joint of the solid material collection tank, a prismatic groove is sandwiched between the mounting constraint sleeve and the cyclone separation cylinder, the prismatic insert ring is plugged into the prismatic groove of the mounting constraint sleeve, an annular groove is provided on one side of the socket joint of the solid material collection tank, and a plurality of anti-stripping ball grooves are symmetrically provided on the side of the mounting constraint sleeve close to the annular groove, and mounting balls are provided in the anti-stripping ball grooves, and one side of the mounting ball passes through the anti-stripping ball groove and is plugged into the annular groove, and a constraint screw sleeve is provided on the side of the mounting constraint sleeve close to the anti-stripping ball groove through a threaded sleeve, and a plurality of mounting balls are abutted against the inner circumference of the constraint screw sleeve on the side away from the annular groove.

[0011] Preferably, a give-way slot is horizontally opened at the upper end of the solid material collection tank, the square cut-off block is horizontally movably inserted into the give-way slot, the cut-off control box is arranged on the side of the solid material collection tank close to the give-way slot, a piston chamber is opened in the cut-off control box, a discharge control pipe is arranged on the side of the square cut-off block close to the cut-off control box, and the discharge control pipe movably penetrates the piston chamber of the cut-off control box through a sealing ring.

[0012] Preferably, constraint rings are provided on both sides of the piston cavity, and a drainage control pipe is located between the two constraint rings and is sleeved with a control piston. The movable distance of the control piston between the two constraint rings is equal to the movable distance of the square truncation block in the give way groove. A liquid receiving groove is provided at the upper end of the square truncation block connected to the drainage control pipe. When the square truncation block is away from the truncation control box, the liquid receiving groove is arranged corresponding to the cyclone separation cylinder, and the cross-sectional area of ​​the square truncation block is larger than the cross-sectional area of ​​the inner cavity at the lower end of the cyclone separation cylinder.

[0013] Preferably, a first three-way joint and a second three-way joint are respectively provided on both sides of the upper end of the truncation control box, and one side of the first three-way joint and the second three-way joint are respectively connected to both sides of the piston cavity, and the side of the first three-way joint and the second three-way joint connected to the piston cavity are respectively located on the side of the two constraint rings away from the control piston.

[0014] Preferably, a bearing groove is provided at the upper end of the cyclone separation cylinder, and the rotating disk is rotated and plugged into the bearing groove through a sealed bearing, and the lower end of the air outlet pipe passes through the bearing groove and is plugged into the cyclone separation cylinder, and the air outlet pipe is located above the rotating disk and has strip guide grooves on both sides thereof, and a pushing guide plate is inserted into and penetrated on one side of the movable inner tube close to the strip guide groove, and a lifting control cylinder is embedded in the rotating disk below the pushing guide plate, and the upper end of the lifting control cylinder is connected to the lower end of the pushing guide plate.

[0015] Preferably, a sealed inner conical groove is provided at the lower end of the outlet pipe located in the cyclone separation barrel, and a cleaning head is provided at the lower end of a movable inner tube penetrating the outlet pipe. The diameter of the cleaning head is equal to that of the outlet pipe, and the upper and lower ends of the cleaning head are both arranged with conical structures. When the movable inner tube is lifted to the maximum extent, the upper conical surface of the cleaning head is inserted into the sealed inner conical groove and sealed contact. The upper and lower conical surfaces of the cleaning head are respectively inclined to penetrate and provide a plurality of first flushing holes and second flushing holes, and rubber self-closing blocks are inserted in the second flushing holes. An annular liquid groove is provided in the movable inner tube connected to the push guide plate, and a liquid connection plug is provided on one side of the annular liquid groove of the push guide plate.

[0016] Preferably, a gear groove and a toggle groove are provided at the upper end of the conversion box, and a synchronization shaft is horizontally rotatably inserted between the gear groove and the toggle groove. The synchronization shaft is located in the gear groove and the toggle groove and is respectively provided with a control bevel gear and a toggle impeller. A toggle bevel gear ring is provided at the lower end of the outer peripheral side of the turntable, and one side of the control bevel gear is meshed and connected with the toggle bevel gear ring. A diverter groove is provided below the toggle groove in the conversion box, and a switching guide plate is rotatably arranged in the diverter groove through a rotating shaft. Blowing grooves are provided on both sides of the upper end of the diverter groove and are obliquely connected to the lower ends of both sides of the toggle groove. A second air supply pipe is provided on one side of the second three-way joint, and the upper end of the second air supply pipe is connected to the lower end of the diverter groove.

[0017] Preferably, one side of the first three-way joint is connected to a first air supply pipe, the upper end of the first air supply pipe is connected and plugged with one side of the lower end of the conversion box, the second expansion air ring is embedded in the lower end of the bearing groove of the cyclone separation cylinder, one side of the second expansion air ring passes through the cyclone separation cylinder and the conversion box and is connected to the first air supply pipe and is provided with a second connecting air pipe, the first expansion air ring is sleeved on the lower end of the cyclone separation cylinder, and one side of the first expansion air ring is connected to one side of the piston groove close to the first three-way joint and is provided with a first connecting air pipe.

[0018] A method for preparing a cyclone separator for graphene using a high-pressure physical exfoliation method comprises the following steps:

[0019] Step 1: The gas-solid mixture containing graphene in the cyclone separation cylinder enters the cyclone separation cylinder from the input pipe, and a high-speed cyclone airflow is generated in the cyclone separation cylinder through the inner wall. The solid graphene adheres to the inner wall of the cyclone separation cylinder and falls down. The spiral airflow forms a second cyclone airflow at the bottom of the cyclone separation cylinder, and then is discharged from the outlet pipe and the center of the movable inner pipe for subsequent multi-stage separation and extraction of graphene;

[0020] Step 2: When a certain amount of graphene solid adheres to the inner wall of the cyclone separation cylinder, the second three-way joint injects high-pressure gas into the cut-off control box, and the high-pressure gas pushes the control piston, the drainage control pipe and the square cut-off block to move toward one side of the cyclone separation cylinder. At this time, the square cut-off block cuts off the connection between the solid material collection tank and the cyclone separation cylinder. The square cut-off block connects the drainage control pipe and the cyclone separation cylinder through the liquid receiving tank. When the square cut-off block moves to the maximum extent, the pressure is maintained first;

[0021] Step 3: The lifting control cylinder controls the guide plate and the movable inner tube to move vertically in the air outlet pipe, the cleaning head is away from the air outlet pipe and exposes the first flushing holes to the air outlet pipe, at this time, the cleaning liquid is sent into the annular liquid tank through the liquid receiving plug of the pushing guide plate, and the high-pressure cleaning liquid rushes to the inner wall of the cyclone separation cylinder through the first flushing holes and the second flushing holes, and the graphene-containing solid-liquid mixture after cleaning can also be sent to the separator and dryer for separation and extraction;

[0022] Step 4: During this period, the gas pressure of the second three-way joint can be increased. At this time, the high-pressure gas breaks through the one-way valve connected to the second air supply pipe, enters the conversion box from the second air supply pipe, and then switches the interval effect of the guide plate. The second air supply pipe is connected to the two blowing grooves in turn, and the reciprocating rotation of the driving impeller and the control bevel gear is controlled. The rotation of the rotating disk connected to the driving bevel gear ring is adjusted to realize the rotation of the cleaning head and the air outlet pipe in the cyclone separation cylinder, thereby enhancing the cleaning effect of the inner wall of the cyclone separation cylinder.

[0023] Step 5: When the cyclone separation cylinder is used normally for graphene separation, the high-pressure gas sent into the first three-way joint can enter the first expansion air ring and the second expansion air ring respectively through the first connecting air pipe and the second connecting air pipe while preventing the square cut-off block from intercepting the cyclone separation cylinder and the solid material collecting tank, thereby strengthening the sealing effect of the connection between the solid material collecting tank and the cyclone separation cylinder and the connection between the rotating disk and the cyclone separation cylinder, avoiding the possibility of external airflow entering the cyclone separation cylinder, and improving the stability of the double cyclone airflow in the cyclone separation cylinder.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] After the inner wall of the cyclone separation cylinder has been used for graphene separation for a long time, the inner wall of the cyclone separation cylinder can be flushed with high pressure through the cleaning component. During the flushing, the cyclone separation cylinder and the solid material collection tank are intercepted and sealed through the cut-off component. Then, the graphene-containing liquid is collected and separated through the drainage control pipe, thereby improving the convenience of the cleaning operation. During this period, the cleaning effect can be improved by rotating the adjustment component. In addition, with the cooperation of the enhanced sealing component, the seal of the cyclone separation cylinder can be strengthened in combination with the use of the cut-off component. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention;

[0027] Figure 2 It is a schematic diagram of the side section structure of the present invention;

[0028] Figure 3 For the present invention Figure 2 Schematic diagram of part A;

[0029] Figure 4 For the present invention Figure 3 Schematic diagram of part B;

[0030] Figure 5 For the present invention Figure 3 Schematic diagram of the C part;

[0031] Figure 6 For the present invention Figure 2 Schematic diagram of the D part;

[0032] Figure 7 For the present invention Figure 6 Schematic diagram of part E;

[0033] Figure 8 For the present invention Figure 6 Schematic diagram of the F part;

[0034] Fig. 9 For the present invention Figure 2 Schematic diagram of the G part;

[0035] Fig.10 It is a schematic side cutaway diagram of the conversion box structure of the present invention;

[0036] Fig.11 For the present invention Fig.10 Schematic diagram of the H part;

[0037] Fig.12 A schematic diagram of the structure of the cleaning head of the present invention;

[0038] Fig.13 For the present invention Fig.12 Schematic diagram of the J part;

[0039] Fig.14 It is a schematic diagram of the structure of the solid material collecting tank of the present invention.

[0040] In the figure: cyclone separation cylinder 1, input pipe 2, solid material collection tank 3, prismatic insert ring 4, installation constraint sleeve 5, annular groove 6, anti-drop ball groove 7, installation ball 8, constraint screw sleeve 9, first expansion gas ring 10, give way slide 11, square truncation block 12, truncation control box 13, discharge control pipe 14, control piston 15, liquid receiving groove 16, bearing groove 17, self-rotating disc 18, outlet pipe 19, movable inner pipe 20, strip guide groove 21, push guide plate 22, lift Lowering control cylinder 23, sealed inner conical groove 24, cleaning head 25, first flushing hole 26, second flushing hole 27, annular liquid groove 28, conversion box 29, second expansion air ring 30, first three-way joint 31, second three-way joint 32, first air supply pipe 33, first connecting air pipe 34, second connecting air pipe 35, control bevel gear 36, shifting impeller 37, shifting bevel gear ring 38, diverter groove 39, switching guide plate 40, blowing groove 41, second air supply pipe 42. DETAILED DESCRIPTION

[0041] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. 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 creative work are within the scope of protection of the present invention.

[0042] Please refer to the attached Figure 1-Figure 14 , this application provides the following technical solutions.

[0043] Embodiment 1: A cyclone separator for preparing graphene by high-pressure physical stripping method, comprising a cyclone separation cylinder 1, an input pipe 2 is provided at the upper end of one side of the cyclone separation cylinder 1, and a solid material collection tank 3 is provided at the lower end of the cyclone separation cylinder 1 through a quick-install component, the quick-install component comprises a prismatic insert ring 4 and a mounting constraint sleeve 5, the mounting constraint sleeve 5 is arranged at the lower end of the cyclone separation cylinder 1, the prismatic insert ring 4 is arranged at the upper end of the solid material collection tank 3, the upper end of the solid material collection tank 3 is provided with a sleeve joint, the lower end of the cyclone separation cylinder 1 is plugged into the sleeve joint of the solid material collection tank 3 through a sealing ring, the prismatic insert ring 4 is arranged at the upper end of the sleeve joint of the solid material collection tank 3, a prismatic groove is sandwiched between the mounting constraint sleeve 5 and the cyclone separation cylinder 1, the prismatic insert ring 4 is plugged into the prismatic groove of the mounting constraint sleeve 5, and an annular groove 6 is provided on one side of the sleeve joint of the solid material collection tank 3, the mounting A plurality of anti-slip ball grooves 7 are symmetrically provided on one side of the constraint sleeve 5 close to the annular groove 6, and mounting balls 8 are arranged in each of the anti-slip ball grooves 7, and one side of the mounting balls 8 passes through the anti-slip ball groove 7 and is inserted into the annular groove 6; a constraint screw sleeve 9 is provided on the side of the constraint sleeve 5 close to the anti-slip ball groove 7 through a threaded sleeve, and a plurality of mounting balls 8 are in contact with the inner circumference of the constraint screw sleeve 9 on the side away from the annular groove 6; a collection device or pipeline for conveying graphene materials can be additionally installed at the lower end of the solid material collecting tank 3, so that during continuous production operations, the graphene materials can be taken out by blocking the connection between the cyclone separation cylinder 1 and the solid material collecting tank 3; when the cyclone separation cylinder 1 needs to be replaced and maintained, it can be quickly connected by a one-insert and one-rotate method, while maintaining the multi-layer sealing of the sleeve, to avoid the cumbersome installation and disassembly of the flange connection.

[0044] A cut-off component is provided to cut off the cyclone separation cylinder 1 and the solid material collection tank 3. The cut-off component is provided at one side of the solid material collection tank 3. The cut-off component comprises a cut-off control box 13, a square cut-off block 12 and a drainage control pipe 14. The cut-off control box 13 is horizontally provided at one side of the solid material collection tank 3 close to the cyclone separation cylinder 1. The square cut-off block 12 is horizontally movably plugged into the solid material collection tank 3. A yielding chute 11 is horizontally provided at the upper end of the solid material collection tank 3. The square cut-off block 12 is horizontally movably plugged into the yielding chute 11. The cut-off control box 13 is provided at one side of the solid material collection tank 3 close to the yielding chute 11. A piston cavity is provided in the cut-off control box 13. The drainage control pipe 14 is provided at one side of the square cut-off block 12 close to the cut-off control box 13. The drainage control pipe 14 movably penetrates the piston cavity of the cut-off control box 13 through a sealing ring. Constraint rings are provided on both sides of the piston cavity. The drainage control pipe 14 is located at the two A control piston 15 is sleeved between the constraint rings, and the movable distance of the control piston 15 between the two constraint rings is equal to the movable distance of the square truncation block 12 in the give way slot 11. The upper end of the square truncation block 12 is connected to the discharge control pipe 14 and is penetrated by a liquid receiving groove 16. When the square truncation block 12 is away from the truncation control box 13, the liquid receiving groove 16 is arranged corresponding to the cyclone separation cylinder 1, and the cross-sectional area of ​​the square truncation block 12 is larger than the cross-sectional area of ​​the inner cavity at the lower end of the cyclone separation cylinder 1. The lower end of the cyclone separation cylinder 1 is extended. When a cyclone airflow is formed in the cyclone separation cylinder 1, the existence of the square truncation block 12 will not affect the formation of the second cyclone airflow. At the same time, the square truncation block 12 will be misaligned with the connection position between the cyclone separation cylinder 1 and the solid material collection tank 3 when the cyclone separation cylinder 1 is in normal use, further avoiding the problem that the existing installation of common valves affects the formation of the second airflow and brings out more solid materials.

[0045] The first three-way joint 31 and the second three-way joint 32 are respectively provided on both sides of the upper end of the cut-off control box 13, and one side of the first three-way joint 31 and the second three-way joint 32 are respectively connected to the two sides of the piston cavity, and the side of the first three-way joint 31 and the second three-way joint 32 connected to the piston cavity are respectively located on the side of the two constraint rings away from the control piston 15, and the movement of the discharge control pipe 14 in the cut-off control box 13 is cut off by the contact between the control piston 15 and the constraint ring, which does not affect the air supply drive control of the first three-way joint 31 and the second three-way joint 32.

[0046] A cleaning component is provided to clean the inner wall of the cyclone separation cylinder 1. The cleaning component is rotatably provided at the upper end of the cyclone separation cylinder 1. The cleaning component includes a self-rotating disc 18 and a movable inner tube 20. The self-rotating disc 18 is rotatably plugged into the upper end of the cyclone separation cylinder 1. An air outlet pipe 19 is vertically provided at the center of the self-rotating disc 18. The lower end of the air outlet pipe 19 is plugged into the upper part of the cyclone separation cylinder 1. A bearing groove 17 is provided at the upper end of the cyclone separation cylinder 1. The self-rotating disc 18 is rotatably plugged into the bearing groove 17 through a sealed bearing. The lower end of the air outlet pipe 19 penetrates the bearing groove 17 and is plugged into the cyclone separation cylinder 1. The air outlet pipe 19 is located on both sides above the self-rotating disc 18 and is penetrated by a plurality of inner tubes 20. The strip guide groove 21 and the side of the movable inner tube 20 close to the strip guide groove 21 are penetrated and inserted with a pushing guide plate 22, and the rotating disk 18 is located below the pushing guide plate 22 and is embedded with a lifting control cylinder 23, and the upper end of the lifting control cylinder 23 is connected to the lower end of the pushing guide plate 22, and the lifting control cylinder 23 can control the lifting of the movable inner tube 20. In addition, the distance between the upper end of the movable inner tube 20 and the pushing guide plate 22 is greater than the length of the strip guide groove 21. No matter how the movable inner tube 20 moves, the airflow flowing through the movable inner tube 20 will not overflow from the position of the strip guide groove 21, and a sealing piston ring can be set at the upper end of the movable inner tube 20.

[0047] The lower end of the outlet pipe 19 located in the cyclone separation cylinder 1 is provided with a sealed inner conical groove 24, and the lower end of the movable inner pipe 20 penetrating the outlet pipe 19 is provided with a cleaning head 25, the diameter of the cleaning head 25 is equal to that of the outlet pipe 19, and the upper and lower ends of the cleaning head 25 are both set in a conical structure. When the movable inner pipe 20 is lifted to the maximum extent, the upper conical surface of the cleaning head 25 is inserted into the sealed inner conical groove 24 and sealed. The upper and lower conical surfaces of the cleaning head 25 are respectively obliquely penetrated to open a plurality of first flushing holes 26 and second flushing holes 2 7. A rubber self-closing block is inserted in the second flushing hole 27. An annular liquid groove 28 is opened in the movable inner tube 20 to connect with the push guide plate 22, and a liquid connection plug is provided on one side of the annular liquid groove 28 of the push guide plate 22. The rubber self-closing block can prevent the airflow in the cyclone separation cylinder 1 from entering the annular liquid groove 28 from the second flushing hole 27. The first flushing hole 26 will be inserted into the outlet pipe 19 for sealing when the cyclone separation cylinder 1 is in normal use. The cleaning head 25 has the same diameter as the outlet pipe 19, which can avoid the disturbance of the cyclone airflow in the cyclone separation cylinder 1.

[0048] The movable inner tube 20 is vertically movable in the air outlet pipe 19. A rotation adjustment component is provided on the side of the cyclone separation cylinder 1 close to the self-rotating disk 18. The rotation adjustment component includes a conversion box 29, a control bevel gear 36 and a switching guide plate 40. A gear groove and a toggle groove are provided at the upper end of the conversion box 29. A synchronous shaft is horizontally rotated and plugged between the gear groove and the toggle groove. The synchronous shaft is located in the gear groove and the toggle groove and is respectively provided with a control bevel gear 36 and a toggle impeller 37. A toggle bevel gear ring 38 is provided at the lower end of the outer peripheral side of the self-rotating disk 18. One side of the control bevel gear 36 is meshed and connected with the toggle bevel gear ring 38. A diverter groove 39 is provided in the conversion box 29 below the toggle groove. The switching guide plate 40 is rotatably arranged in the diverter groove 39 through the rotating shaft. The two sides of the upper end of the diverter groove 39 are respectively connected to the two sides of the toggle groove The lower end is obliquely connected to form a blowing groove 41, and one side of the second three-way joint 32 is connected to form a second air supply pipe 42. The upper end of the second air supply pipe 42 is connected to the lower end of the diverter groove 39. When the rotation of the turntable 18 needs to be controlled, the second air supply pipe 42 delivers high-pressure airflow into the diverter groove 39, and the switching guide plate 40 is controlled by a small drive motor to control its reciprocating rotation in the diverter groove 39. The rotation path of the switching guide plate 40 is fixed and can only be rotated to two positions, which respectively control the connection between the second air supply pipe 42 and the two blowing grooves 41, and then after being connected with the two blowing grooves 41 respectively, the toggle impeller 37 can be controlled to rotate forward and reverse, and then under the action of the toggle bevel gear ring 38 and the control bevel gear 36 gear ratio, the slow rotation of the turntable 18 is controlled.

[0049] In this embodiment:

[0050] Embodiment 2: On the basis of embodiment 1, a strengthening sealing component is provided to strengthen the upper and lower sealing states of the cyclone separation cylinder 1 when in use, so as to prevent the external airflow from affecting the stability of the cyclone airflow in the cyclone separation cylinder 1. The strengthening sealing component comprises a first expansion air ring 10 and a second expansion air ring 30, and the first expansion air ring 10 is provided on the side of the solid material collection tank 3 which is sleeved on the cyclone separation cylinder 1, and the second expansion air ring 30 is provided on the side of the cyclone separation cylinder 1 close to the self-rotating disk 18. One side of the first three-way joint 31 is connected with a first air supply pipe 33, and the upper end of the first air supply pipe 33 is connected and plugged with one side of the lower end of the conversion box 29. The second expansion air ring 30 is embedded in the lower end of the bearing groove 17 of the cyclone separation cylinder 1, and one side of the second expansion air ring 30 passes through the cyclone separation cylinder 1 and the conversion box 29 and is connected with the first air supply pipe 33. A second connecting air pipe 35 is provided. The first expansion air ring 10 is sleeved on the lower end of the cyclone separation cylinder 1. One side of the first expansion gas ring 10 is connected to the side of the piston groove close to the first three-way joint 31 and is provided with a first connecting air pipe 34. The second three-way joint 32 is connected to the side of the second air supply pipe 42 and is provided with a one-way valve. While the second three-way joint 32 controls the discharge control pipe 14 and the square cut-off block 12, it can selectively control the rotation of the rotating disk 18. When the first three-way joint 31 delivers high-pressure gas, the high-pressure gas pushes the square cut-off block 12 not to intercept and seal the cyclone separation cylinder 1 and the solid material collection tank 3. At this time, the cyclone separation cylinder 1 is ready to perform normal separation operations, and the first three-way joint 31 continues to deliver high-pressure gas. The high-pressure gas can push the first expansion gas ring 10 and the second expansion gas ring 30 to expand, thereby realizing the contact sealing between the rotating disk 18 and the solid material collection tank 3. On the contrary, when the rotating disk 18 needs to rotate, the contact friction between the second expansion gas ring 30 and the rotating disk 18 is small, which does not affect the normal rotation of the rotating disk 18.

[0051] A method for preparing a cyclone separator for graphene using a high-pressure physical exfoliation method comprises the following steps:

[0052] Step 1: The gas-solid mixture containing graphene in the cyclone separation cylinder 1 enters the cyclone separation cylinder 1 from the input pipe 2, and a high-speed cyclone airflow is generated in the cyclone separation cylinder 1 through the inner wall. The solid graphene adheres to the inner wall of the cyclone separation cylinder 1 and falls down. The spiral airflow forms a second cyclone airflow at the bottom of the cyclone separation cylinder 1, and then is discharged from the center of the air outlet pipe 19 and the movable inner pipe 20 for subsequent multi-stage separation and extraction of graphene;

[0053] Step 2: When a certain amount of graphene solid adheres to the inner wall of the cyclone separation cylinder 1, the second three-way joint 32 injects high-pressure gas into the cut-off control box 13, and the high-pressure gas pushes the control piston 15, the drainage control pipe 14 and the square cut-off block 12 to move toward the side of the cyclone separation cylinder 1. At this time, the square cut-off block 12 cuts off the state that the solid material collection tank 3 is connected to the cyclone separation cylinder 1. The square cut-off block 12 connects the drainage control pipe 14 and the cyclone separation cylinder 1 through the liquid receiving groove 16. When the square cut-off block 12 moves to the maximum extent, the pressure is maintained first;

[0054] Step 3: The lifting control cylinder 23 controls the guide plate 22 and the movable inner tube 20 to move vertically in the air outlet pipe 19, and the cleaning head 25 is away from the air outlet pipe 19 and exposes the first flushing holes 26 to the air outlet pipe 19. At this time, the cleaning liquid is sent into the annular liquid tank 28 through the liquid receiving plug of the guide plate 22, and the high-pressure cleaning liquid rushes to the inner wall of the cyclone separation cylinder 1 through the first flushing holes 26 and the second flushing holes 27. After cleaning, the graphene-containing solid-liquid mixture can also be sent to the separator and the dryer for separation and extraction;

[0055] Step 4: During this period, the pressure of the gas delivered to the second three-way joint 32 can be increased. At this time, the high-pressure gas breaks through the one-way valve connected to the second air supply pipe 42, enters the conversion box 29 from the second air supply pipe 42, and then switches the interval effect of the guide plate 40. The second air supply pipe 42 is connected to the two blowing grooves 41 to control the reciprocating rotation of the impeller 37 and the bevel gear 36, and the rotation of the rotating disk 18 connected to the bevel gear ring 38 is adjusted to realize the rotation of the cleaning head 25 and the air outlet pipe 19 in the cyclone separation cylinder 1, thereby enhancing the cleaning effect of the inner wall of the cyclone separation cylinder 1.

[0056] Step 5: When the cyclone separation cylinder 1 is used normally for graphene separation, the high-pressure gas sent into the first three-way joint 31 can enter the first expansion air ring 10 and the second expansion air ring 30 respectively through the first connecting air pipe 34 and the second connecting air pipe 35 while preventing the square cut-off block 12 from intercepting the cyclone separation cylinder 1 and the solid material collecting tank 3, thereby strengthening the sealing effect of the connection between the solid material collecting tank 3 and the cyclone separation cylinder 1 and the connection between the rotating disk 18 and the cyclone separation cylinder 1, avoiding the possibility of external airflow entering the cyclone separation cylinder 1, and improving the stability of the double cyclone airflow in the cyclone separation cylinder 1.

[0057] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A cyclone separator for preparing graphene by high pressure physical exfoliation method, characterized in that: include: A cyclone separation cylinder (1), wherein an input pipe (2) is provided at an upper end of one side of the cyclone separation cylinder (1), and a solid material collection tank (3) is provided at the lower end of the cyclone separation cylinder (1) via a quick-installation assembly, wherein the quick-installation assembly comprises a prismatic insert ring (4) and an installation constraint sleeve (5), wherein the installation constraint sleeve (5) is provided at the lower end of the cyclone separation cylinder (1), and the prismatic insert ring (4) is provided at the upper end of the solid material collection tank (3); A cut-off assembly, the cut-off assembly being arranged on one side of the solid material collection tank (3), the cut-off assembly comprising a cut-off control box (13), a square cut-off block (12) and a liquid discharge control pipe (14), the cut-off control box (13) being arranged horizontally on one side of the solid material collection tank (3) close to the cyclone separation cylinder (1), and the square cut-off block (12) being horizontally movably plugged into the solid material collection tank (3); A cleaning component, the cleaning component is rotatably arranged at the upper end of the cyclone separation cylinder (1), the cleaning component comprises a self-rotating disc (18) and a movable inner tube (20), the self-rotating disc (18) is rotatably plugged into the upper end of the cyclone separation cylinder (1), an air outlet pipe (19) is vertically arranged at the center of the self-rotating disc (18), the lower end of the air outlet pipe (19) is plugged into the upper part of the cyclone separation cylinder (1), the movable inner tube (20) is vertically movably arranged in the air outlet pipe (19), a rotation adjustment component is arranged on one side of the cyclone separation cylinder (1) close to the self-rotating disc (18), and the rotation adjustment component comprises a conversion box (29), a control bevel gear (36) and a switching guide plate (40); A reinforced sealing assembly, comprising a first expansion gas ring (10) and a second expansion gas ring (30), wherein the first expansion gas ring (10) is arranged on a side of a solid material collection tank (3) sleeved with a cyclone separation cylinder (1), and the second expansion gas ring (30) is arranged on a side of the cyclone separation cylinder (1) close to a rotating disk (18).

2. A cyclone separator for preparing graphene by high pressure physical exfoliation method according to claim 1, characterized in that: The upper end of the solid material collection tank (3) is provided with a sleeve joint, the lower end of the cyclone separation cylinder (1) is plugged into the sleeve joint of the solid material collection tank (3) through a sealing ring, a prismatic insert ring (4) is arranged at the upper end of the sleeve joint of the solid material collection tank (3), a prismatic groove is sandwiched between the installation constraint sleeve (5) and the cyclone separation cylinder (1), the prismatic insert ring (4) is plugged into the prismatic groove of the installation constraint sleeve (5), an annular groove (6) is provided on one side of the sleeve joint of the solid material collection tank (3), and the installation constraint sleeve (5) is approximately A plurality of anti-slip ball grooves (7) are symmetrically provided on one side of the restraining sleeve (5) close to the annular groove (6), and mounting balls (8) are arranged in each of the anti-slip ball grooves (7). One side of the mounting balls (8) penetrates the anti-slip ball groove (7) and is inserted into the annular groove (6). A restraining screw sleeve (9) is provided on one side of the restraining sleeve (5) close to the anti-slip ball groove (7) through a threaded sleeve connection, and a side of the plurality of mounting balls (8) away from the annular groove (6) abuts against the inner circumference of the restraining screw sleeve (9).

3. A cyclone separator for preparing graphene by high pressure physical exfoliation method according to claim 2, characterized in that: A clearance groove (11) is horizontally provided at the upper end of the solid material collection tank (3); a square cut-off block (12) is horizontally movably inserted into the clearance groove (11); a cut-off control box (13) is arranged on a side of the solid material collection tank (3) close to the clearance groove (11); a piston cavity is provided in the cut-off control box (13); a discharge control pipe (14) is arranged on a side of the square cut-off block (12) close to the cut-off control box (13); and the discharge control pipe (14) movably penetrates the piston cavity of the cut-off control box (13) through a sealing ring.

4. A cyclone separator for preparing graphene by high pressure physical exfoliation method according to claim 3, characterized in that: Constraint rings are provided on both sides of the piston cavity. A discharge control pipe (14) is sleeved with a control piston (15) between the two constraint rings. The movable distance of the control piston (15) between the two constraint rings is equal to the movable distance of the square cut-off block (12) in the clearance groove (11). A liquid receiving groove (16) is provided at the upper end of the square cut-off block (12) and connected to the discharge control pipe (14). When the square cut-off block (12) is away from the cut-off control box (13), the liquid receiving groove (16) is arranged corresponding to the cyclone separation cylinder (1), and the cross-sectional area of ​​the square cut-off block (12) is larger than the cross-sectional area of ​​the inner cavity at the lower end of the cyclone separation cylinder (1).

5. A cyclone separator for preparing graphene by high pressure physical exfoliation method according to claim 4, characterized in that: A first three-way joint (31) and a second three-way joint (32) are respectively provided on both sides of the upper end of the cut-off control box (13); one side of the first three-way joint (31) and the second three-way joint (32) are respectively connected to both sides of the piston cavity; and the side of the first three-way joint (31) and the second three-way joint (32) connected to the piston cavity is respectively located on the side of the two restraining rings away from the control piston (15).

6. A cyclone separator for preparing graphene by high pressure physical exfoliation method according to claim 5, characterized in that: The upper end of the cyclone separation cylinder (1) is provided with a bearing groove (17), and the self-rotating disc (18) is rotatably inserted into the bearing groove (17) through a sealed bearing, and the lower end of the air outlet pipe (19) penetrates the bearing groove (17) and is inserted into the cyclone separation cylinder (1), and both sides of the air outlet pipe (19) located above the self-rotating disc (18) penetrate with strip guide grooves (21), and the side of the movable inner tube (20) close to the strip guide groove (21) penetrates and is inserted with a push guide plate (22), and the self-rotating disc (18) is located below the push guide plate (22) and is embedded with a lifting control cylinder (23), and the upper end of the lifting control cylinder (23) is connected to the lower end of the push guide plate (22).

7. A cyclone separator for preparing graphene by high pressure physical exfoliation method according to claim 6, characterized in that: The lower end of the air outlet pipe (19) located in the cyclone separation barrel (1) is provided with a sealed inner conical groove (24); the lower end of the movable inner pipe (20) penetrating the air outlet pipe (19) is provided with a cleaning head (25); the diameter of the cleaning head (25) is equal to that of the air outlet pipe (19); the upper and lower ends of the cleaning head (25) are both provided with conical structures; when the movable inner pipe (20) is lifted to the maximum extent, the upper conical surface of the cleaning head (25) is inserted into the sealed inner conical groove (24) and sealed in contact; the upper and lower conical surfaces of the cleaning head (25) are respectively obliquely penetrated to provide a plurality of first flushing holes (26) and second flushing holes (27); the second flushing holes (27) are each provided with a rubber self-closing block; the movable inner pipe (20) is provided with an annular liquid groove (28) connected to the push guide plate (22); and a liquid receiving plug is provided on one side of the annular liquid groove (28) of the push guide plate (22).

8. A cyclone separator for preparing graphene by high pressure physical exfoliation method according to claim 7, characterized in that: The upper end of the conversion box (29) is provided with a gear groove and a toggle groove, and a synchronous shaft is horizontally rotatably inserted between the gear groove and the toggle groove. The synchronous shaft is located in the gear groove and the toggle groove and is provided with a control bevel gear (36) and a toggle impeller (37) respectively. A toggle bevel gear ring (38) is provided at the lower end of the outer peripheral side of the self-rotating disk (18), and one side of the control bevel gear (36) is meshed and connected with the toggle bevel gear ring (38). A diverter groove (39) is provided below the toggle groove in the conversion box (29), and a switching guide plate (40) is rotatably arranged in the diverter groove (39) through a rotating shaft. Blowing grooves (41) are provided on both sides of the upper end of the diverter groove (39) and are obliquely connected to the lower ends of the two sides of the toggle groove. A second air supply pipe (42) is connected to one side of the second three-way joint (32), and the upper end of the second air supply pipe (42) is connected to the lower end of the diverter groove (39).

9. A cyclone separator for preparing graphene by high pressure physical exfoliation method according to claim 8, characterized in that: One side of the first three-way joint (31) is connected to a first air supply pipe (33), the upper end of the first air supply pipe (33) is connected and plugged with one side of the lower end of the conversion box (29), the second expansion air ring (30) is embedded in the lower end of the bearing groove (17) of the cyclone separation cylinder (1), one side of the second expansion air ring (30) passes through the cyclone separation cylinder (1) and the conversion box (29) and is connected to the first air supply pipe (33) and is provided with a second connecting air pipe (35), the first expansion air ring (10) is sleeved on the lower end of the cyclone separation cylinder (1), one side of the first expansion air ring (10) is connected to a side of the piston groove close to the first three-way joint (31) and is provided with a first connecting air pipe (34).

10. A method for preparing a cyclone separator for graphene using the high pressure physical exfoliation method according to any one of claims 1 to 9, characterized in that: The following steps are involved: Step 1: The gas-solid mixture containing graphene in the cyclone separation cylinder (1) enters the cyclone separation cylinder (1) from the input pipe (2), and a high-speed cyclone airflow is generated through the inner wall of the cyclone separation cylinder (1). The solid graphene adheres to the inner wall of the cyclone separation cylinder (1) and falls down. The spiral airflow forms a second cyclone airflow at the bottom of the cyclone separation cylinder (1), and then is discharged from the center of the air outlet pipe (19) and the movable inner pipe (20) for subsequent multi-stage separation and extraction of graphene; Step 2: When a certain amount of graphene solid adheres to the inner wall of the cyclone separation cylinder (1), the second three-way joint (32) injects high-pressure gas into the cut-off control box (13), and the high-pressure gas pushes the control piston (15), the discharge control pipe (14) and the square cut-off block (12) to move toward one side of the cyclone separation cylinder (1). At this time, the square cut-off block (12) cuts off the state of the solid material collection tank (3) being connected to the cyclone separation cylinder (1). The square cut-off block (12) connects the discharge control pipe (14) and the cyclone separation cylinder (1) through the liquid receiving groove (16). When the square cut-off block (12) moves to the maximum extent, the pressure is maintained first. Step 3: The lifting control cylinder (23) controls the push guide plate (22) and the movable inner tube (20) to move vertically in the air outlet pipe (19), the cleaning head (25) is away from the air outlet pipe (19) and exposes the plurality of first flushing holes (26) from the air outlet pipe (19), at which time the cleaning liquid is sent into the annular liquid tank (28) through the liquid receiving plug of the push guide plate (22), and the high-pressure cleaning liquid is rushed to the inner wall of the cyclone separation cylinder (1) through the plurality of first flushing holes (26) and the second flushing holes (27), and the graphene-containing solid-liquid mixture after cleaning can also be sent to a separator and a dryer for separation and extraction; Step 4: During this period, the pressure of the gas delivered to the second three-way joint (32) can be increased. At this time, the high-pressure gas breaks through the one-way valve connected to the second air supply pipe (42) and enters the conversion box (29) from the second air supply pipe (42). Then, under the interval action of the switching guide plate (40), the second air supply pipe (42) is connected to the two blowing grooves (41) in succession, and the reciprocating rotation of the control impeller (37) and the control bevel gear (36) is controlled. The rotation of the rotating disk (18) connected to the driving bevel gear ring (38) is adjusted, so that the cleaning head (25) and the air outlet pipe (19) can rotate in the cyclone separation cylinder (1), thereby enhancing the cleaning effect of the inner wall of the cyclone separation cylinder (1). Step 5: When the cyclone separation cylinder (1) is used normally for graphene separation, the high-pressure gas introduced into the first three-way joint (31) can enter the first expansion air ring (10) and the second expansion air ring (30) respectively through the first connecting air pipe (34) and the second connecting air pipe (35) while preventing the square truncation block (12) from intercepting the cyclone separation cylinder (1) and the solid material collection tank (3), thereby strengthening the sealing effect of the connection between the solid material collection tank (3) and the cyclone separation cylinder (1) and the connection between the rotating disk (18) and the cyclone separation cylinder (1), avoiding the possibility of external airflow entering the cyclone separation cylinder (1), and improving the stability of the double cyclone airflow in the cyclone separation cylinder (1).

Citation Information

Patent Citations

  • Device and method for preparing graphene

    CN110817854A