Lithium hexafluorophosphate crystallization device convenient for sampling
By designing a lithium hexafluorophosphate crystallization device that is easy to sample, using a stirring rod and a slidable valve plate structure, the problems of inconvenience and leakage in the prior art are solved, and efficient mixing and crystallization effects are achieved.
Patent Information
- Application Number
- CN202422281115.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-19
- Publication Date
- 2025-08-01
- Estimated Expiration
- 2034-09-19
AI Technical Summary
The existing lithium hexafluorophosphate crystallization device is inconvenient to operate during the sampling process, which easily leads to leakage, and has low mixing uniformity and crystallization efficiency.
A lithium hexafluorophosphate crystallization device including a stirring rod and a sampling tube is designed. The phosphorus pentafluoride gas and lithium hexafluorophosphate liquid are fully mixed by rotating the stirring rod, and the slidable valve plate and return spring are used to achieve convenient sampling to avoid leakage.
The mixing uniformity between phosphorus pentafluoride gas and lithium hexafluorophosphate liquid is improved, the crystallization efficiency is enhanced, and the sampling process is fast and simple, avoiding sample leakage.
Smart Images

Figure CN223170361U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of lithium hexafluorophosphate production equipment, and particularly relates to a lithium hexafluorophosphate crystallization device convenient for sampling. Background Technique
[0002] As the most widely commercially used lithium-ion battery electrolyte, lithium hexafluorophosphate has good ionic conductivity and electrochemical stability, and has become the core raw material for producing lithium-ion battery electrolytes. With the rapid development of the new energy industry, its market demand has increased sharply, and the development prospect is good.
[0003] In the industrial production process of lithium hexafluorophosphate, the most stable and commonly used one is the wet preparation process. The specific steps are roughly as follows: adding lithium fluoride powder into anhydrous hydrogen fluoride to form a LiF·HF solution of lithium fluoride, then introducing phosphorus pentafluoride into the solution for reaction to produce a LiPF6·HF solution dissolving lithium hexafluorophosphate, and then the LiPF6·HF solution is cooled and crystallized, separated and dried to obtain lithium hexafluorophosphate crystals.
[0004] In order to observe the crystallization state during the crystallization process of lithium hexafluorophosphate, it is usually necessary to sample the lithium hexafluorophosphate in the crystallization device. At present, the conventional sampling method of the crystallization device controls the discharge valve on the discharge pipe to complete sampling, which is inconvenient to operate and is prone to leakage due to untimely closing of the discharge valve. Content of the Utility Model
[0005] In order to solve the above technical problems, the utility model provides a lithium hexafluorophosphate crystallization device convenient for sampling.
[0006] The technical solution of a lithium hexafluorophosphate crystallization device convenient for sampling of the utility model is as follows:
[0007] A lithium hexafluorophosphate crystallization device convenient for sampling, including a shell, an annular cavity is arranged inside the shell, a phosphorus pentafluoride gas inlet pipe communicated with the cavity is arranged on the outer wall of the shell, a plurality of air nozzles communicated with the cavity are arranged on the inner wall of the shell, a stirring rod is rotatably installed inside the shell, the stirring rod includes a rotating shaft and stirring rods, the rotating shaft and the stirring rods are hollow structures communicated with each other, a plurality of liquid outlet holes are arranged on the stirring rods, the upper end of the rotating shaft is connected with a liquid inlet pipe through a rotary joint, a driving mechanism for driving the rotating shaft to rotate is arranged on the shell, a sampling pipe is arranged at the lower end of the shell, a valve plate and a sealing plug matched with the valve plate are arranged inside the sampling pipe, the valve plate is slidably installed in the sampling pipe, the sealing plug is fixedly connected inside the sampling pipe, and a return spring for pressing the valve plate against the sealing plug is arranged inside the sampling pipe.
[0008] Furthermore, the housing includes an integrally formed cylindrical section and a conical section located at the lower end of the cylindrical section. The upper end of the cylindrical section is sealed, and a discharge pipe is provided at the lower end of the conical section. A discharge valve is provided on the discharge pipe. The cavity is arranged inside the cylindrical section, and the sampling pipe is arranged on the conical section.
[0009] Furthermore, the rotating shaft is rotatably installed at the central position of the upper end of the cylindrical section through a bearing. The upper end of the rotating shaft extends above the upper side of the cylindrical section. The stirring rods extend horizontally. A plurality of the stirring rods are arranged in multiple circles. The multiple circles of stirring rods are evenly spaced in the axial direction of the rotating shaft. Each circle of stirring rods is evenly spaced in the circumferential direction of the rotating shaft. Adjacent two circles of stirring rods are arranged staggeredly.
[0010] Furthermore, a plurality of the liquid outlet holes are arranged in multiple circles. The multiple circles of liquid outlet holes are evenly spaced in the axial direction of the stirring rod. Each circle of liquid outlet holes is evenly spaced in the circumferential direction of the stirring rod.
[0011] Furthermore, the driving mechanism includes a driving motor, a driving bevel gear, and a driven bevel gear. The driving motor is fixedly connected to the housing. The driving bevel gear is fixedly connected to the end of the output shaft of the driving motor. The driven bevel gear is coaxially and fixedly connected to the rotating shaft.
[0012] Furthermore, an exhaust pipe is provided at the upper end of the housing, and an exhaust valve is provided on the exhaust pipe.
[0013] Furthermore, a fixing ring is arranged inside the sampling pipe. The two ends of the return spring are respectively fixedly connected to the fixing ring and the valve plate. The valve plate is provided with a frustum-shaped valve hole that is smaller at the top and larger at the bottom. The sealing plug is matched with the valve hole. One side of the sealing plug facing the valve plate is fixedly connected with a fixing rod. The end of the fixing rod extends above the upper side of the fixing ring. The end of the fixing rod is fixedly connected to the inner wall of the sampling pipe through a connecting rod.
[0014] The utility model provides a lithium hexafluorophosphate crystallization device that is convenient for sampling. Compared with the prior art, its beneficial effects are:
[0015] When the lithium hexafluorophosphate crystallization device facilitating sampling of the present utility model is in use, the lithium hexafluorophosphate liquid is pressurized and enters the rotating shaft of the stirring rod through the liquid inlet pipe, and is sprayed into the shell through the liquid outlet holes on the stirring rod. The phosphorus pentafluoride gas is pressurized and added into the annular cavity through the phosphorus pentafluoride gas inlet pipe, and is sprayed into the shell from the gas nozzles, and is mixed with the hexafluorophosphoric acid liquid in the shell. During this process, the driving mechanism drives the stirring rod to rotate, and the phosphorus pentafluoride gas and the lithium hexafluorophosphate liquid are fully mixed and crystallized. When sampling is required, the sampling tube of the sampling bottle is inserted into the sampling pipe, the sampling tube pushes the valve plate upward to disengage from the sealing plug, and the material in the sampling pipe enters the sampling bottle. After sampling is completed, the sampling tube of the sampling bottle is pulled out from the sampling pipe, and the valve plate is pressed tightly on the sealing plug under the action of the return spring. Compared with the prior art, the lithium hexafluorophosphate crystallization device facilitating sampling of the present utility model improves the mixing uniformity of the phosphorus pentafluoride gas and the lithium hexafluorophosphate liquid, improves the crystallization efficiency, and the sampling is fast, simple, and avoids sample leakage. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 is a schematic structural diagram of the lithium hexafluorophosphate crystallization device facilitating sampling of the present utility model;
[0017] Figure 2 is Figure 1 the enlarged view of part A in
[0018] Figure 3 is Figure 1 the enlarged view of part B in
[0019] In the figure: 1, shell; 2, annular cavity; 3, discharge pipe; 4, discharge valve; 5, gas nozzle; 6, phosphorus pentafluoride gas inlet pipe; 7, liquid inlet pipe; 8, rotary joint; 9, exhaust pipe; 10, exhaust valve; 11, rotating shaft; 12, stirring rod; 13, liquid outlet hole; 14, driving motor; 15, driving bevel gear; 16, driven bevel gear; 17, sampling pipe; 18, fixing ring; 19, valve plate; 20, sealing plug; 21, fixing rod; 22, connecting rod; 23, return spring; 24, sampling bottle. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0020] The following further describes the present utility model in detail in conjunction with the drawings and specific embodiments:
[0021] The specific embodiment of the lithium hexafluorophosphate crystallization device facilitating sampling of the present utility model is as Figures 1 to 3As shown in the figure, it includes a housing 1. An annular cavity is provided inside the housing 1. A phosphorus pentafluoride gas inlet pipe 6 communicating with the cavity is provided on the outer wall of the housing 1. A number of nozzles 5 communicating with the cavity are provided on the inner wall of the housing 1. A stirring rod is rotatably installed inside the housing 1. The stirring rod includes a rotating shaft 11 and stirring rods 12. The rotating shaft 11 and the stirring rods 12 are hollow structures communicating with each other. A number of liquid outlet holes 13 are provided on the stirring rods 12. The upper end of the rotating shaft 11 is connected with a liquid inlet pipe 7 through a rotary joint 8. A driving mechanism for driving the rotation of the rotating shaft 11 is provided on the housing 1. A sampling pipe 17 is provided at the lower end of the housing 1. A valve plate 19 and a sealing plug 20 cooperating with the valve plate 19 are provided inside the sampling pipe 17. The valve plate 19 is slidably installed in the sampling pipe. The sealing plug 20 is fixedly connected inside the sampling pipe. A return spring 23 for pressing the valve plate 19 against the sealing plug 20 is provided inside the sampling pipe.
[0022] The housing 1 includes an integrally formed cylindrical section and a conical section located at the lower end of the cylindrical section. The upper end of the cylindrical section is sealed. A discharge pipe 3 is provided at the lower end of the conical section. A discharge valve 4 is provided on the discharge pipe 3. The cavity is arranged inside the cylindrical section. The sampling pipe 17 is arranged on the conical section. The rotating shaft 11 is rotatably installed at the central position of the upper end of the cylindrical section through a bearing. The upper end of the rotating shaft 11 extends out of the upper side of the cylindrical section. The stirring rods 12 extend horizontally. A number of stirring rods 12 are arranged in multiple circles. The multiple circles of stirring rods 12 are evenly spaced in the axial direction of the rotating shaft 11. Each circle of stirring rods 12 is evenly spaced in the circumferential direction of the rotating shaft 11. Adjacent two circles of stirring rods 12 are staggered.
[0023] A number of liquid outlet holes 13 are arranged in multiple circles. The multiple circles of liquid outlet holes 13 are evenly spaced in the axial direction of the stirring rod 12. Each circle of liquid outlet holes 13 is evenly spaced in the circumferential direction of the stirring rod 12. The driving mechanism includes a driving motor 14, a driving bevel gear 15 and a driven bevel gear 16. The driving motor 14 is fixedly connected to the housing 1. The driving bevel gear 15 is fixedly connected to the end of the output shaft of the driving motor 14. The driven bevel gear 16 is coaxially fixedly connected to the rotating shaft 11. An exhaust pipe 9 is provided at the upper end of the housing 1. An exhaust valve 10 is provided on the exhaust pipe 9. A fixing ring 18 is provided inside the sampling pipe 17. The two ends of the return spring 23 are respectively fixedly connected to the fixing ring 18 and the valve plate 19. A valve hole in the shape of a frustum of a cone with a smaller upper part and a larger lower part is provided on the valve plate 19. The sealing plug 20 is matched with the valve hole. A fixing rod 21 is fixedly connected to the side of the sealing plug 20 facing the valve plate 19. The end of the fixing rod 21 extends out of the upper side of the fixing ring 18. The end of the fixing rod 21 is fixedly connected to the inner wall of the sampling pipe 17 through a connecting rod 22.
[0024] When the lithium hexafluorophosphate crystallization device facilitating sampling of the present utility model is in use, the lithium hexafluorophosphate liquid is pressurized and enters the rotating shaft 11 of the stirring rod through the liquid inlet pipe 7, and is sprayed into the housing 1 from the liquid outlet holes 13 on the stirring rod 12. The phosphorus pentafluoride gas is pressurized and added into the annular cavity 2 through the phosphorus pentafluoride gas inlet pipe 6, and is sprayed into the housing 1 from the gas nozzles 5 to be mixed with the lithium hexafluorophosphate liquid in the housing 1. During this process, the driving mechanism drives the stirring rod to rotate, so that the phosphorus pentafluoride gas and the lithium hexafluorophosphate liquid are fully mixed and crystallized. When sampling is required, the sampling tube of the sampling bottle 24 is inserted into the sampling pipe 17. The sampling tube pushes the valve plate 19 to move upward and separate from the sealing plug 20. The material in the sampling pipe 17 enters the sampling bottle 24. After sampling is completed, the sampling tube of the sampling bottle 24 is pulled out of the sampling pipe 17, and the valve plate 19 is pressed tightly on the sealing plug 20 under the action of the return spring 23. Compared with the prior art, the lithium hexafluorophosphate crystallization device facilitating sampling of the present utility model improves the mixing uniformity of the phosphorus pentafluoride gas and the lithium hexafluorophosphate liquid, improves the crystallization efficiency, and the sampling is fast, simple and avoids sample leakage.
[0025] The above are only the preferred embodiments of the present utility model and are not intended to limit the present utility model. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present utility model shall be included in the protection scope of the present utility model.
Claims
1. A lithium hexafluorophosphate crystallization device convenient for sampling, characterized in that, It includes a housing. An annular cavity is provided inside the housing. A phosphorus pentafluoride gas inlet pipe communicating with the cavity is provided on the outer wall of the housing. A number of nozzles communicating with the cavity are provided on the inner wall of the housing. A stirring rod is rotatably installed inside the housing. The stirring rod includes a rotating shaft and stirring rods. The rotating shaft and the stirring rods are of a hollow structure communicating with each other. A number of liquid outlet holes are provided on the stirring rods. The upper end of the rotating shaft is connected to a liquid inlet pipe through a rotary joint. A driving mechanism for driving the rotating shaft to rotate is provided on the housing. A sampling pipe is provided at the lower end of the housing. A valve plate and a sealing plug cooperating with the valve plate are provided inside the sampling pipe. The valve plate is slidably installed in the sampling pipe. The sealing plug is fixedly connected inside the sampling pipe. A return spring for pressing the valve plate against the sealing plug is provided inside the sampling pipe.
2. The lithium hexafluorophosphate crystallization device facilitating sampling according to claim 1, wherein The housing includes an integrally formed cylindrical section and a conical section located at the lower end of the cylindrical section. The upper end of the cylindrical section is sealed. A discharge pipe is provided at the lower end of the conical section. A discharge valve is provided on the discharge pipe. The cavity is arranged inside the cylindrical section. The sampling pipe is arranged on the conical section.
3. The lithium hexafluorophosphate crystallization device facilitating sampling according to claim 2, wherein, The rotating shaft is rotatably installed at the central position of the upper end of the cylindrical section through a bearing. The upper end of the rotating shaft extends out of the upper side of the cylindrical section. The stirring rods extend horizontally. A number of the stirring rods are arranged in multiple circles. The multiple circles of stirring rods are evenly spaced in the axial direction of the rotating shaft. Each circle of stirring rods is evenly spaced in the circumferential direction of the rotating shaft. Adjacent two circles of stirring rods are arranged staggeredly.
4. The lithium hexafluorophosphate crystallization device convenient for sampling according to claim 3, wherein, A number of the liquid outlet holes are arranged in multiple circles. The multiple circles of liquid outlet holes are evenly spaced in the axial direction of the stirring rod. Each circle of liquid outlet holes is evenly spaced in the circumferential direction of the stirring rod.
5. The lithium hexafluorophosphate crystallization device convenient for sampling according to claim 1, wherein, The driving mechanism includes a driving motor, a driving bevel gear and a driven bevel gear. The driving motor is fixedly connected to the housing. The driving bevel gear is fixedly connected to the end of the output shaft of the driving motor. The driven bevel gear is coaxially fixedly connected to the rotating shaft.
6. The lithium hexafluorophosphate crystallization device convenient for sampling according to claim 1, wherein, An exhaust pipe is provided at the upper end of the housing. An exhaust valve is provided on the exhaust pipe.
7. The lithium hexafluorophosphate crystallization device convenient for sampling according to claim 1, wherein, A fixing ring is provided inside the sampling pipe. The two ends of the return spring are respectively fixedly connected to the fixing ring and the valve plate. A frustum-shaped valve hole with a smaller upper part and a larger lower part is provided on the valve plate. The sealing plug is matched with the valve hole. A fixing rod is fixedly connected to the side of the sealing plug facing the valve plate. The end of the fixing rod extends out of the upper side of the fixing ring. The end of the fixing rod is fixedly connected to the inner wall of the sampling pipe through a connecting rod.