Doping modification device for sodium ion battery positive electrode material

Abstract

The utility model relates to the technical field of battery doping modification, and discloses a doping modification device of a sodium ion battery positive electrode material, which comprises a reaction kettle outer shell, a reaction kettle inner shell is fixedly arranged in the reaction kettle outer shell, a water inlet pipe is arranged at the left upper end of the reaction kettle outer shell in a penetrating manner, and a water outlet pipe is arranged at the right lower end of the reaction kettle outer shell in a penetrating manner; and a first rotating shaft is rotationally mounted in the middle positions of the reaction kettle outer shell and the reaction kettle inner shell. According to the doping modification device for the sodium-ion battery positive electrode material, the reaction kettle outer shell and the reaction kettle inner shell are arranged to be of a double-layer structure, a solution in the reaction kettle inner shell can be heated in a water bath, heated water can be stirred through a rotating gear ring, a connecting rod and a stirring plate, circulating water is evenly distributed, and the doping modification effect is good. The device is simple in structure and convenient to operate, the solution can be stirred in a linkage mode while heated water is stirred, uniform distribution of the reaction solution can be guaranteed, meanwhile, the liquid storage bag is extruded in a linkage mode, and a metal salt solution can be slowly dropwise added into a precipitator solution in the stirring process.

Description

Technical Field

[0001] This utility model relates to the field of battery doping modification technology, specifically to a device for doping modification of sodium-ion battery cathode materials. Background Technology

[0002] Doping modification of cathode materials for sodium-ion batteries is one of the key technologies to improve their electrochemical performance. This is mainly achieved by introducing specific elements to optimize the material's structural stability, ion diffusion kinetics, and electronic conductivity. For example, Zr-doped manganese-iron-based Prussian blue can reduce lattice stress and improve cycle stability. Co-precipitation is usually used when doping it.

[0003] The coprecipitation method described above involves weighing and dissolving a metal salt (such as nitrates, chlorides, etc.) in deionized water or a mixed solvent (such as water + ethanol) according to the stoichiometric ratio of the target material to form a homogeneous solution. Then, a precipitant (including oxalic acid, ammonium carbonate, sodium hydroxide, etc.) is added, the selection of which depends on the solubility of the target product and the reaction conditions. The metal salt solution is slowly added dropwise to the precipitant solution while it is being stirred, thus obtaining the doped battery cathode material. The above reaction needs to be carried out in a reaction vessel. The precursor prepared by the coprecipitation method is then calcined at high temperature to obtain a layered structure with a cycle life of 2000-4000 cycles.

[0004] Currently, patent CN217725534U discloses a chemical oxidation coprecipitation reaction vessel, including: a reaction vessel body, a heating and temperature control structure, and a high-efficiency stirring system; wherein the top of the reaction vessel body is provided with a pretreatment mixture inlet, a level gauge interface, a spare port, a pressure gauge interface, a stirring transmission device interface, a tank washer interface, a second temperature sensor interface, a sight glass, a vent, a manhole, a liquid inlet, a condensate vent valve interface, and a safety valve interface; the side wall of the reaction vessel body is provided with a pH sampling port, a first temperature sensor interface, a steam medium inlet, and an ear seat; the bottom of the reaction vessel body is provided with a steam medium outlet and a discharge port; the heating and temperature control structure: an insulation jacket is provided between the inner and outer walls of the reaction vessel body, and the reaction vessel body and the jacket constitute a heating and temperature control structure; an axial flow type elliptical bottom double spiral ribbon stirring blade is provided in the stirring system of the vessel body, the material spirals up along the container wall and then converges towards the central cavity to form an upper and lower convection circulation, which has a strong anti-adhesion effect. It is suitable for mixing high-viscosity materials to meet the requirements of iron oxide crystal formation.

[0005] However, the following problems still exist during the use of the co-precipitation reactor described above:

[0006] During use, the raw materials in the reactor can be mixed and stirred through the internal structure. However, when applying the doping and modification of sodium-ion battery cathode materials, the reaction temperature needs to be precisely controlled. The temperature is usually controlled at 50-60 degrees Celsius. The existing reactor uses a direct internal heating method, and it is difficult to ensure a rapid and uniform temperature distribution through internal stirring alone. Temperature fluctuations can lead to local enrichment or segregation of dopants. Utility Model Content

[0007] To address the shortcomings of existing technologies, this invention provides a doping modification device for sodium-ion battery cathode materials. By using a water bath heating method, the temperature of the reaction solution can be precisely controlled, avoiding large temperature fluctuations during the doping reaction.

[0008] This utility model provides the following technical solution: a doping modification device for sodium-ion battery cathode material, including a reaction vessel outer shell, inside which a reaction vessel inner shell is fixedly installed. A water inlet pipe is installed through the upper left end of the reaction vessel outer shell, and a water outlet pipe is installed through the lower right end of the reaction vessel outer shell. A first rotating shaft is rotatably installed at the middle position of the reaction vessel outer shell and the reaction vessel inner shell, and a stirring rod is fixedly installed at the lower end of the first rotating shaft. The stirring rod is located inside the reaction vessel inner shell. A connecting gear is fixedly installed outside the first rotating shaft, and a driving gear is meshed on the side of the connecting gear. A receiving gear is meshed on the side of the driving gear, and the receiving gear is rotatably installed on the inner surface of the reaction vessel outer shell. A rotating gear ring is meshed on the side of the receiving gear, and a connecting rod is fixedly installed at the lower end of the rotating gear ring. A stirring plate is fixedly installed on the outer surface of the connecting rod.

[0009] Furthermore, a feed pipe is provided through the upper left side of the outer shell and the inner shell of the reactor, and a liquid outlet pipe is provided through the lower end of the outer shell and the inner shell of the reactor. A sensing device is fixedly installed on the lower end of the inner surface of the inner shell of the reactor. The insulated and waterproof wire at the lower end of the sensing device passes through the outer shell and the inner shell of the reactor. With the above structure, the temperature and pH value of the solution in the inner shell of the reactor can be measured by the sensing device, which facilitates timely adjustment.

[0010] Furthermore, a second rotating shaft is fixedly installed on the upper end of the drive gear, and the second rotating shaft is rotatably connected to the outer shell of the reactor. A motor is fixedly installed on the outer surface of the upper end of the outer shell of the reactor, and the output end of the motor is connected to the second rotating shaft. Through the above structure, the second rotating shaft can be driven to rotate as the motor works.

[0011] Furthermore, a semi-circular groove is provided on the outer side of the rotating gear ring, and a limiting ball is rolled in the semi-circular groove on the rotating gear ring. A fixed track is fixedly installed on the inner surface of the outer shell of the reactor, and an annular groove is provided on the inner side of the fixed track. The limiting ball is rolled in connection with the fixed track through the annular groove on the fixed track. With the above structure, the rotating gear ring can be supported and limited under the action of the fixed track and the limiting ball, that is, the rotation of the rotating gear ring is not affected while supporting the rotating gear ring.

[0012] Furthermore, an active bevel gear is fixedly installed at the upper end of the first rotating shaft, and a driven bevel gear is meshed on the right side of the active bevel gear. A rotating screw is fixedly installed on the driven bevel gear, and the rotating screw is rotatably connected to the outer shell of the reactor. A movable sleeve is threadedly connected to the outside of the rotating screw, and a pressing plate is fixedly installed on the movable sleeve. With the above structure, the driven bevel gear can be driven to rotate as the active bevel gear rotates.

[0013] Furthermore, two guide rods are symmetrically installed on the extrusion plate, and an installation plate is fixedly installed on the outer shell of the reactor. The installation plate has two cylindrical holes, and the guide rods are slidably connected to the installation plate through the cylindrical holes. A liquid storage bladder is fixedly installed on the installation plate, and the extrusion plate and the liquid storage bladder are in close contact with each other. A sealing rubber plug is provided at the upper end of the liquid storage bladder, and a connecting pipe is installed through the lower end of the liquid storage bladder. The connecting pipe passes through the outer shell and the inner shell of the reactor, and four fan-shaped rubber diaphragms are provided inside the connecting pipe. With the above structure, the liquid storage bladder can be squeezed as the extrusion plate moves, so that the metal salt solution in the liquid storage bladder can be added to the precipitant solution.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] This sodium-ion battery cathode material doping modification device achieves a double-layered reactor by using an outer and inner shell. This allows for water bath heating of the solution within the inner shell, enabling precise temperature control. The heated water is stirred via a rotating toothed ring, connecting rod, and stirring plate, ensuring uniform distribution of the circulating water and stable, even heating of the solution, preventing large temperature fluctuations. Simultaneously, the device also stirs the solution, guaranteeing uniform distribution of the reaction solution. Furthermore, the device compresses the storage bladder, allowing the metal salt solution to be slowly added dropwise to the stirring precipitant solution, ensuring a slow and uniform doping reaction. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the overall three-dimensional structure of the present invention;

[0017] Figure 2 This is a schematic diagram of the three-dimensional cross-sectional structure of the stirring rod of this utility model;

[0018] Figure 3 This is a schematic diagram of the three-dimensional cross-sectional structure of the rotating toothed ring of this utility model;

[0019] Figure 4 This is a three-dimensional structural diagram of the connecting gear of this utility model;

[0020] Figure 5 This is a schematic diagram of the three-dimensional explosion structure of the limiting ball bearing of this utility model;

[0021] Figure 6 This utility model Figure 3 Enlarged structural diagram at point A in the middle.

[0022] In the diagram: 1. Outer shell of the reactor; 2. Inner shell of the reactor; 3. Inlet pipe; 4. Outlet pipe; 5. Liquid outlet pipe; 6. First rotating shaft; 7. Stirring rod; 8. Sensing device; 9. Connecting gear; 10. Driving gear; 11. Second rotating shaft; 12. Motor; 13. Receiving gear; 14. Rotating gear ring; 15. Limiting ball bearing; 16. Fixed track; 17. Connecting rod; 18. Stirring plate; 19. Feed pipe; 20. Driving bevel gear; 21. Driven bevel gear; 22. Rotating screw; 23. Moving sleeve; 24. Extrusion plate; 25. Guide rod; 26. Mounting plate; 27. Liquid storage bladder; 28. Connecting pipe. Detailed Implementation

[0023] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present utility model. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments.

[0024] Please see Figures 1-6This utility model provides a technical solution: a doping modification device for sodium-ion battery cathode material, including a reaction vessel outer shell 1, inside which a reaction vessel inner shell 2 is fixedly installed. A water inlet pipe 3 is installed through the upper left end of the reaction vessel outer shell 1, and a water outlet pipe 4 is installed through the lower right end of the reaction vessel outer shell 1. A first rotating shaft 6 is rotatably installed at the middle position between the reaction vessel outer shell 1 and the reaction vessel inner shell 2, and a stirring rod 7 is fixedly installed at the lower end of the first rotating shaft 6. The stirring rod 7 is located inside the reaction vessel inner shell 2. A connecting gear 9 is fixedly installed outside the first rotating shaft 6, and a driving gear 10 is meshed on the side of the connecting gear 9. A receiving gear 13 is meshed on the side of the driving gear 10, and the receiving gear 13 is rotatably installed on the inner surface of the reaction vessel outer shell 1. A rotating gear ring 14 is meshed on the side of the receiving gear 13, and a connecting rod 17 is fixedly installed at the lower end of the rotating gear ring 14. A stirring plate 18 is fixedly installed on the outer surface of the connecting rod 17. The reaction vessel outer shell 1 and the reaction vessel inner shell 2 are connected in a rotatable manner. A feed pipe 19 is provided through the upper left side of the inner shell 2 of the reactor, and a liquid outlet pipe 5 is provided through the lower ends of the outer shell 1 and the inner shell 2 of the reactor. A sensor 8 is fixedly installed on the lower end of the inner surface of the inner shell 2 of the reactor. The insulated waterproof wire at the lower end of the sensor 8 passes through the outer shell 1 and the inner shell 2 of the reactor. A second rotating shaft 11 is fixedly installed on the upper end of the drive gear 10, and the second rotating shaft 11 is rotatably connected to the outer shell 1 of the reactor. A motor 12 is fixedly installed on the upper outer surface of the outer shell 1 of the reactor, and the output end of the motor 12 is connected to the second rotating shaft 11. A semi-circular groove is provided on the outer side of the rotating gear ring 14, and a limiting ball 15 is rolled in the semi-circular groove on the rotating gear ring 14. A fixed track 16 is fixedly installed on the inner surface of the outer shell 1 of the reactor, and an annular groove is provided on the inner side of the fixed track 16. The limiting ball 15 is rolledly connected to the fixed track 16 through the annular groove on the fixed track 16.

[0025] When it is necessary to heat the solution inside the inner shell 2 of the reactor, the precipitant solution can be added to the inner shell 2 of the reactor through the feed pipe 19. Then, water heated to a specified temperature is added to the cavity formed between the outer shell 1 and the inner shell 2 of the reactor through the water inlet pipe 3 (usually heated to 60 degrees Celsius, and then transported through a water pump and an insulation pipe, i.e., both the water inlet pipe 3 and the water outlet pipe 4 are connected to an external water pump, and both the water inlet pipe 3 and the water outlet pipe 4 are insulation pipes), which starts the motor 12 (the motor 12 is set as a servo motor that can rotate in both directions, and to ensure the solution...). Due to the effect of liquid mixing and doping, the motor 12 can rotate intermittently. Because the output end of the motor 12 is connected to the second rotating shaft 11, the second rotating shaft 11 begins to rotate. Since the lower end of the second rotating shaft 11 is fixedly mounted with a drive gear 10, the drive gear 10 begins to rotate. Because the drive gear 10 meshes with the receiving gear 13, the receiving gear 13 begins to rotate. Furthermore, because the receiving gear 13 and the rotating gear ring 14 are supported and limited by the limiting ball 15, the rotating gear ring 14 begins to rotate. The lower end of the rotating gear ring 14 is equipped with a connecting... The connecting rod 17 and stirring plate 18 begin to stir the heated water, thus ensuring a uniform temperature distribution. Because the diameter of the rotating gear ring 14 is much larger than the diameter of the drive gear 10, the rotating gear ring 14 drives the connecting rod 17 and stirring plate 18 to rotate relatively slowly, thereby heating the solution inside the inner shell 2 of the reactor. Since the drive gear 10 is meshed with a connecting gear 9 on its side, the connecting gear 9 begins to rotate. Because the connecting gear 9 is installed at the lower end of the first rotating shaft 6, the first rotating shaft 6 begins to drive the stirring... Rotating rod 7 stirs the solution inside the inner shell 2 of the reactor. The temperature and pH value of the solution can be monitored by the sensing device 8 (which includes a temperature sensor and a pH detection sensor), allowing for timely adjustment of the pH value. When the monitored temperature approaches 50 degrees Celsius, the valves on the inlet pipe 3 and the outlet pipe 4 open simultaneously. That is, hot water is injected into the outer shell 1 of the reactor through the inlet pipe 3, and water is discharged from the outer shell 1 of the reactor through the outlet pipe 4. The discharged water is then heated to the specified temperature, achieving recycling and heating.

[0026] A driving bevel gear 20 is fixedly installed at the upper end of the first rotating shaft 6, and a driven bevel gear 21 is meshed on the right side of the driving bevel gear 20. A rotating screw 22 is fixedly installed on the driven bevel gear 21, and the rotating screw 22 is rotatably connected to the outer shell 1 of the reactor. A movable sleeve 23 is threadedly connected to the external of the rotating screw 22, and a pressing plate 24 is fixedly installed on the movable sleeve 23. Two guide rods 25 are symmetrically installed on the pressing plate 24. An mounting plate 26 is fixedly installed on the outer shell 1 of the reactor. Two cylindrical holes are provided on the plate 26. The guide rod 25 is slidably connected to the mounting plate 26 through the cylindrical holes provided on the mounting plate 26. A liquid storage bladder 27 is fixedly installed on the mounting plate 26. The squeezing plate 24 is in close contact with the liquid storage bladder 27. A sealing rubber plug is provided at the upper end of the liquid storage bladder 27, and a connecting pipe 28 is installed through the lower end of the liquid storage bladder 27. The connecting pipe 28 passes through the outer shell 1 and the inner shell 2 of the reactor, and four fan-shaped rubber diaphragms are provided inside the connecting pipe 28.

[0027] By removing the sealing rubber plug at the top of the reservoir 27, and then slowly pouring the metal salt solution into the reservoir 27, and then replacing the sealing rubber plug at the top of the reservoir 27, the four sector-shaped rubber diaphragms inside the connecting pipe 28 (the four sector-shaped rubber diaphragms deform under water pressure, causing water to flow out, and then stop flowing out after the water pressure is balanced) and the active bevel gear 20 fixedly installed on the first rotating shaft 6 (the first rotating shaft 6 rotates when the motor 12 is working), the active bevel gear 20 begins to rotate. Since the active bevel gear 20 meshes with the driven bevel gear 21, and a rotating screw 22 is fixedly installed on the driven bevel gear 21, the movable sleeve 23 connected to the external thread of the rotating screw 22 begins to move closer to the reservoir 27. Because a pressing plate 24 is fixedly installed on the movable sleeve 23, under the guiding and limiting action of the guide rod 25, the movable sleeve 23 and the pressing plate 24 can be kept in a safe position. 4. The horizontal plane moves left and right. At this time, the extrusion plate 24 begins to extrude the liquid storage bladder 27, and the metal salt solution in the liquid storage bladder 27 begins to be extruded and pressurized. At this time, the four fan-shaped rubber diaphragms in the connecting pipe 28 begin to deform, so as to realize the intermittent automatic addition of the metal salt solution in the liquid storage bladder 27. When the addition is completed, the rotating screw 22 is no longer connected to the moving sleeve 23, that is, the addition of the metal salt solution is completed. At this time, the metal salt solution begins to react with the precipitant solution. After the reaction is completed and the solution is allowed to stand, the solution can be taken out through the liquid outlet pipe 5 for further processing to extract the positive electrode material. Then, the motor 12 drives the second rotating shaft 11 to rotate in the opposite direction to the above, and at the same time slightly pushes the moving sleeve 23. The moving sleeve 23 is then reconnected to the rotating screw 22 by threads, and the moving sleeve 23 and the extrusion plate 24 are moved away from the liquid storage bladder 27 to facilitate the next doping modification process.

[0028] 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 alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A device for doping and modifying a sodium-ion battery cathode material, comprising a reaction vessel outer shell (1), wherein an inner reaction vessel shell (2) is fixedly installed inside the outer shell, characterized in that, Also includes: A water inlet pipe (3) is installed through the upper left end of the outer shell of the reactor (1), and a water outlet pipe (4) is installed through the lower right end of the outer shell of the reactor (1). A first rotating shaft (6) is rotatably installed in the middle position between the outer shell of the reactor (1) and the inner shell of the reactor (2). A stirring rod (7) is fixedly installed at the lower end of the first rotating shaft (6). The stirring rod (7) is located inside the inner shell of the reactor (2). A connecting gear (9) is fixedly installed on the outside of the first rotating shaft (6). A driving gear (10) is meshed on the side of the connecting gear (9). A receiving gear (13) is meshed on the side of the driving gear (10). The receiving gear (13) is rotatably installed on the inner surface of the outer shell of the reactor (1). A rotating gear ring (14) is meshed on the side of the receiving gear (13). A connecting rod (17) is fixedly installed at the lower end of the rotating gear ring (14). A stirring plate (18) is fixedly installed on the outer surface of the connecting rod (17). A feed pipe (19) is provided through the upper left side of the outer shell (1) and inner shell (2) of the reactor, and a liquid outlet pipe (5) is provided through the lower end of the outer shell (1) and inner shell (2) of the reactor. A sensing device (8) is fixedly installed on the lower end of the inner surface of the inner shell (2), and an insulated waterproof wire at the lower end of the sensing device (8) passes through the outer shell (1) and inner shell (2) of the reactor.

2. The doping modification device for sodium-ion battery cathode material according to claim 1, characterized in that: The upper end of the drive gear (10) is fixedly mounted with a second rotating shaft (11), and the second rotating shaft (11) is rotatably connected to the outer shell of the reactor (1). The outer surface of the upper end of the outer shell of the reactor (1) is fixedly mounted with a motor (12), and the output end of the motor (12) is connected to the second rotating shaft (11).

3. The doping modification device for sodium-ion battery cathode material according to claim 1 or 2, characterized in that: The outer side of the rotating toothed ring (14) is provided with a semi-circular groove, and a limiting ball (15) is rolled in the semi-circular groove on the rotating toothed ring (14). A fixed track (16) is fixedly installed on the inner surface of the reactor shell (1), and an annular groove is provided on the inner side of the fixed track (16). The limiting ball (15) is rolled in connection with the fixed track (16) through the annular groove on the fixed track (16).

4. The doping modification device for sodium-ion battery cathode material according to claim 1 or 2, characterized in that: An active bevel gear (20) is fixedly installed at the upper end of the first rotating shaft (6), and a driven bevel gear (21) is meshed on the right side of the active bevel gear (20). A rotating screw (22) is fixedly installed on the driven bevel gear (21), and the rotating screw (22) is rotatably connected to the outer shell (1) of the reactor. A movable sleeve (23) is threadedly connected to the outside of the rotating screw (22), and an extrusion plate (24) is fixedly installed on the movable sleeve (23).

5. The doping modification device for sodium-ion battery cathode material according to claim 3, characterized in that: An active bevel gear (20) is fixedly installed at the upper end of the first rotating shaft (6), and a driven bevel gear (21) is meshed on the right side of the active bevel gear (20). A rotating screw (22) is fixedly installed on the driven bevel gear (21), and the rotating screw (22) is rotatably connected to the outer shell (1) of the reactor. A movable sleeve (23) is threadedly connected to the outside of the rotating screw (22), and an extrusion plate (24) is fixedly installed on the movable sleeve (23).

6. The doping modification device for sodium-ion battery cathode material according to claim 4, characterized in that: Two guide rods (25) are symmetrically installed on the extrusion plate (24). An installation plate (26) is fixedly installed on the outer shell (1) of the reactor. Two cylindrical holes are opened on the installation plate (26). The guide rods (25) are slidably connected to the installation plate (26) through the cylindrical holes opened on the installation plate (26). A liquid storage bladder (27) is fixedly installed on the installation plate (26). The extrusion plate (24) and the liquid storage bladder (27) are in close contact with each other. A sealing rubber plug is provided at the upper end of the liquid storage bladder (27). A connecting pipe (28) is installed through the lower end of the liquid storage bladder (27). The connecting pipe (28) passes through the outer shell (1) of the reactor and the inner shell (2) of the reactor. Four fan-shaped rubber diaphragms are provided inside the connecting pipe (28).

7. The doping modification device for sodium-ion battery cathode material according to claim 5, characterized in that: Two guide rods (25) are symmetrically installed on the extrusion plate (24). An installation plate (26) is fixedly installed on the outer shell (1) of the reactor. Two cylindrical holes are opened on the installation plate (26). The guide rods (25) are slidably connected to the installation plate (26) through the cylindrical holes opened on the installation plate (26). A liquid storage bladder (27) is fixedly installed on the installation plate (26). The extrusion plate (24) and the liquid storage bladder (27) are in close contact with each other. A sealing rubber plug is provided at the upper end of the liquid storage bladder (27). A connecting pipe (28) is installed through the lower end of the liquid storage bladder (27). The connecting pipe (28) passes through the outer shell (1) of the reactor and the inner shell (2) of the reactor. Four fan-shaped rubber diaphragms are provided inside the connecting pipe (28).

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