Water cooling apparatus for lithium hexafluorophosphate production and method of use thereof

Abstract

The application discloses a water cooling equipment for lithium hexafluorophosphate manufacturing and a use method thereof, and belongs to the technical field of water cooling equipment. The water cooling equipment comprises a reaction kettle and a heat preservation barrel. Cooling pipes for introducing external cooling medium are coiled in the space between the heat preservation barrel and the outer wall of the reaction kettle, and form an external cooling loop. A sealing cover is internally provided with a gas filling mechanism for conveying and dispersing reaction gas into the reaction kettle. The application is provided with the gas filling mechanism, a driving assembly and a cold storage pipe. The external cooling pipe is used to preliminarily cool the kettle wall. In combination with the process that the low-temperature medium passes through the branch pipe to immediately internally cool the high-temperature gas, and the process that the first servo motor drives the receiving pipe and the porous exhaust assembly to rotate at high speed to generate strong shearing force, the "internal and external double cooling" mechanism is constructed, the local hot spots of the gas-liquid interface are completely eliminated, the large bubbles are broken into micro-bubbles to greatly increase the gas-liquid contact area, and thus the problem of low reaction efficiency is effectively solved.

Description

Technical Field

[0001] This invention relates to the field of water cooling equipment technology, and more specifically, to a water cooling equipment for the manufacture of lithium hexafluorophosphate and its method of use. Background Technology

[0002] Lithium hexafluorophosphate, as the core solute in lithium-ion battery electrolytes, directly determines the battery's performance and safety through its purity and stability. Its mainstream preparation process involves passing high-purity phosphorus pentafluoride gas into an anhydrous hydrogen fluoride solution containing dissolved lithium fluoride under low-temperature, anhydrous, and oxygen-free conditions. This reaction is strongly exothermic, and the product, lithium hexafluorophosphate, is prone to decomposition at higher temperatures. Therefore, precise and efficient cooling and temperature control are essential to maintain the reaction system within a low-temperature range of -10°C to 0°C, ensuring high selectivity and high yield, and preventing side reactions and product decomposition caused by localized overheating.

[0003] Currently, the industry generally uses indirect heat exchange methods based on water or other cooling media to cool the reactor. The most common structure is to set up a jacket or spiral coil cooling sleeve outside the reactor, in which the cooling medium circulates and exchanges heat with the internal reactants through the reactor wall.

[0004] Traditional jacketed or external coil cooling can only exchange heat from the outer wall of the reactor. The heat transfer path is long and the thermal resistance is large, resulting in a delayed cooling response. Furthermore, it is difficult to remove heat from the materials inside the reactor, especially in the central area and at the gas-liquid reaction interface, which can easily lead to a large temperature gradient, causing local overheating and affecting the uniformity of the reaction and the purity of the product. Summary of the Invention

[0005] In view of the problems existing in the prior art, the purpose of this invention is to provide a water cooling device for lithium hexafluorophosphate manufacturing and its usage method, so as to solve the above-mentioned technical problems.

[0006] To solve the above problems, the present invention adopts the following technical solution.

[0007] A water cooling device for lithium hexafluorophosphate manufacturing and its usage method are disclosed, comprising a reactor, a sealing cover on the top of the reactor, an insulation barrel covering the outer surface of the reactor, and a frame fixedly installed at the bottom of the insulation barrel; a cooling pipe for introducing an external cooling medium is coiled in the space between the insulation barrel and the outer wall of the reactor, forming an external cooling circuit; a gas filling mechanism for conveying and dispersing reaction gases into the reactor is provided inside the sealing cover; the gas filling mechanism includes a receiving cylinder fixedly connected to the bottom of the sealing cover, a ring seat rotatingly sealed inside the receiving cylinder, a receiving pipe fixedly connected to the bottom of the ring seat, and an inlet pipe fixedly connected to the top of the receiving cylinder; the bottom of the receiving pipe extends into the reactor, and a porous exhaust assembly is provided on its outer side; A cold storage pipe is coaxially arranged inside the receiving pipe. The top of the cold storage pipe passes through the receiving pipe and is provided with a gas supply pipe. Both sides of the cold storage pipe are fixedly connected to branch pipes. Heat exchange is carried out with the gas supply path of the porous exhaust assembly through the branch pipes, forming an internal cooling passage. The sealing cover is also provided with a drive assembly for driving the receiving pipe to rotate. The reactor wall is cooled by cooling pipes, and the reaction gas and surrounding liquid area flowing through the porous exhaust assembly are cooled by cold storage pipes. Combined with the drive assembly, the receiving pipe is rotated to break up bubbles and enhance mixing, so as to avoid local overheating at the gas-liquid reaction interface.

[0008] As a further aspect of the present invention: the outer circular surface of the cold storage tube is provided with a fixing block that is fixedly connected to the receiving tube; the driving assembly includes a driven gear fixedly connected to the top of the outer circular surface of the receiving tube; a first servo motor is fixedly installed on the top of the sealing cover; the output shaft of the first servo motor passes through the sealing cover and is fixedly connected to a main gear; the main gear meshes with the driven gear; a sealing sleeve is provided between the output shaft of the first servo motor and the sealing cover.

[0009] As a further embodiment of the present invention: the adjusting mechanism includes a threaded rod arranged along the axial direction of the branch pipe, with a support cylinder and a second sleeve plate respectively fixedly connected to the inner wall of the branch pipe at both ends of the threaded rod; a blocking cylinder fixedly connected to the threaded rod is provided on both sides of the second sleeve plate; a limit strip is fixedly connected to the upper and lower sides of the inner wall of the branch pipe; a slide is spirally connected to the outer circular surface of the threaded rod; a groove adapted to the limit strip is provided at the top and bottom ends of the outer circular surface of the slide; the slide is of grade S, and the magnetic slide is of grade N.

[0010] As a further embodiment of the present invention: the adjustment mechanism further includes a second servo motor fixedly connected to the top of the cold storage tube, the output end of the second servo motor is fixedly connected to a sleeve rod, the inner bottom of the sleeve rod is fixedly connected to a drive rod, the outer circular surface of the drive rod is provided with a first sleeve plate fixedly connected to the cold storage tube; the outer circular surface of the drive rod is fixedly connected to a main bevel gear arranged linearly, and one end of the threaded rod is fixedly connected to a driven bevel gear meshing with the main bevel gear.

[0011] As a further aspect of the present invention: the porous exhaust assembly further includes a porous air pipe fixedly connected to the receiving pipe, and the wall of the porous air pipe is provided with multiple exhaust holes; each exhaust hole is fixedly connected to a support plate, and a spring is fixedly connected to the outside of the support plate, and a cap for clearing the exhaust hole is fixedly connected through the spring; both sides of the outer surface of the receiving pipe are provided with limiting rods parallel to the porous air pipe, and one end of the outer circular surface of the porous air pipe is provided with a sleeve that is slidably connected to the limiting rod, and the sleeve is of grade S.

[0012] As a further aspect of the present invention: in cross-sectional view, the sleeve presents a bent plate-like structure with variable cross-sectional thickness; its upper part has a relatively thick rectangular cross-section at the connection with the limiting rod, gradually narrowing and concave to form an arc-shaped transition section as it extends downwards, the inner contour line of the arc-shaped section is parallel to the outer circumferential surface of the porous air tube and has a preset gap; the end region is further thickened and forms an abutting protrusion for abutting the cap tube to achieve unobstructed air venting.

[0013] As a further embodiment of the present invention: a feed pipe is fixedly connected to one side of the top of the sealing cover; an exhaust valve and a pressure gauge are fixedly installed on the front side of the sealing cover.

[0014] As a further aspect of the present invention: the inner wall of the heat-insulating barrel is provided with a buffer plate for supporting the cooling pipe; a pad is fixedly connected around the bottom end of the inner wall of the heat-insulating barrel, and a vent plate is fixedly connected to the upper surface of the pad; both sides of the bottom of the reactor are fixedly connected to discharge pipes, and the discharge pipes pass through the bottom of the heat-insulating barrel and are fixedly installed with discharge valves; a limiting cylinder for limiting the position of the receiving cylinder is fixedly connected to the middle of the bottom of the reactor.

[0015] A method of using a water cooling device for lithium hexafluorophosphate manufacturing, the method comprising the following steps: S1: Liquid raw materials such as anhydrous hydrogen fluoride are injected into the reactor through the feed pipe. At the same time, the external cooling medium is introduced into the cooling pipe to initially cool the reactor wall. During this process, the buffer plate absorbs the thermal stress of the pipeline, the gasket and the vent plate keep the insulation layer dry, and the pressure gauge is turned on to monitor the gas pressure in real time, so that the exhaust valve is in standby state. S2: After the reaction begins, phosphorus pentafluoride gas is introduced into the receiving pipe through the inlet pipe, receiving cylinder and ring seat, and finally released in the form of microbubbles by the porous exhaust component. At the same time, the low temperature medium is introduced into the cold storage pipe and branch pipe, so that the cold storage pipe and branch pipe can quickly absorb the heat of the high temperature reaction gas and the surrounding liquid area. S3: Start the first servo motor, drive the main gear and driven gear to rotate, and drive the receiving pipe, porous exhaust assembly and cold storage pipe to rotate at high speed in the reactor. Use the shear force generated by the rotation to break up large bubbles to increase the gas-liquid contact area. S4: The second servo motor is started according to the needs of the reaction stage, which drives the threaded rod to rotate and thus drives the slide to move axially. The magnetic sleeve is synchronously displaced by magnetic coupling, and the reaction gas flow and cooling intensity are synchronously adjusted. At the same time, the sleeve is synchronously moved by the magnetic force of the magnetic sleeve, and the sleeve is used to press the cap to clear the exhaust hole. S5: After the reaction is complete, open the double-sided discharge valves to allow the generated lithium hexafluorophosphate slurry to be discharged through the discharge pipe under gravity, thus completing the production process.

[0016] Compared with the prior art, the technical solution provided by the present invention has at least the following beneficial effects: This solution establishes a "dual cooling" mechanism by setting up a gas filling mechanism, drive components, and cold storage pipes. Based on the initial cooling of the reactor wall by external cooling pipes, it combines the "instant internal cooling" of high-temperature gas by a low-temperature medium passing through a branch pipe adjacent to the gas path. The process of starting the first servo motor to drive the receiving pipe and the porous exhaust component to rotate at high speed to generate strong shear force is achieved. This completely eliminates local hot spots at the gas-liquid interface, breaks large bubbles into microbubbles to greatly increase the gas-liquid contact area, and utilizes the rotating turbulent flow field to accelerate the uniform distribution of cooling. This effectively solves the problems of low reaction efficiency, affected product purity, and uneven bubble mixing.

[0017] By setting up an adjustment mechanism and a magnetic sliding sleeve, the motor can be started based on temperature feedback, driving the slide block to move linearly in the axial direction, thereby pulling the magnetic sliding sleeve to move synchronously. This process simultaneously changes the air intake flow cross-sectional area of ​​the porous exhaust assembly and the effective heat exchange length of the exposed branch pipe. This achieves stepless adjustment of the reaction gas flow rate without adding additional valves, and simultaneously and precisely adjusts the cooling intensity. This solves the problems of local overheating and increased side reactions caused by the independent and asynchronous response of cooling and gas supply control in traditional equipment.

[0018] By setting up an adaptive unblocking component consisting of a sleeve with magnetic attraction linkage, a limiting rod, and a cap that returns to its original position with a spring, the sleeve is simultaneously pulled down and the cap is pressed against the spring force to overcome the spring force and make a reciprocating motion of "pressing in to scrape and popping out to reset" when the gas flow is adjusted to drive the magnetic sleeve to move. This achieves the effect of automatically peeling off crystallized impurities at the orifice by using the edge of the cap like a scraper, and keeping the gas path unobstructed without adding an additional power source or stopping the machine for disassembly. This significantly improves the continuity and efficiency of lithium hexafluorophosphate production. Attached Figure Description

[0019] The accompanying drawings, which are incorporated herein and form part of the specification, illustrate embodiments of the invention and, together with the specification, further serve to explain the principles of the invention and enable those skilled in the art to practice and use the invention.

[0020] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is an internal cross-sectional view of the insulated bucket of the present invention; Figure 3 This is an internal cross-sectional view of the reactor of the present invention; Figure 4 This is a schematic diagram of the connection of the air filling mechanism of the present invention; Figure 5 This is a cross-sectional view of the internal connection of the receiving cylinder of the present invention; Figure 6 for Figure 5 Enlarged view of section A in the image; Figure 7 This is an internal cross-sectional view of the cold storage tube of the present invention; Figure 8 for Figure 7 Enlarged view of section B in the image; Figure 9 for Figure 7 A magnified view of section C in the image.

[0021] Figure label: 1. Frame; 2. Insulated container; 21. Buffer plate; 22. Pad; 23. Ventilation plate; 3. Cooling pipe; 4. Reactor; 41. Discharge pipe; 42. Discharge valve; 43. Limiting cylinder; 5. Sealing cover; 51. Feed pipe; 6. Air filling mechanism; 61. Receiving cylinder; 62. Air inlet pipe; 63. Receiving pipe; 64. Ring seat; 65. Multi-hole exhaust assembly; 651. Multi-hole air pipe; 652. Exhaust port; 653. Support plate; 654. Spring; 655. Cap; 656. Limiting rod; 657. Sleeve; 66. Driven gear; 67. First servo motor; 68. Main gear; 7. Cold storage pipe; 71. Gas transmission pipe; 72. Branch pipe; 73. Fixing block; 8. Adjustment mechanism; 81. Second servo motor; 82. Sleeve rod; 83. Drive rod; 84. First sleeve plate; 85. Main bevel gear; 86. Limiting strip; 87. Threaded rod; 88. Support cylinder; 89. Second sleeve plate; 810. Blocking cylinder; 811. Driven bevel gear; 812. Slide block; 9. Magnetic sliding sleeve; 10. Exhaust valve; 11. Pressure gauge.

[0022] As shown in the figure, specific structures and devices are marked in the figure to clearly illustrate the structure of the embodiments of the present invention. However, this is only for illustrative purposes and is not intended to limit the present invention to this specific structure, device and environment. Those skilled in the art can adjust or modify these devices and environments according to specific needs. Detailed Implementation

[0023] The following is a detailed description of a water cooling device for lithium hexafluorophosphate manufacturing and its usage method provided by the present invention, with reference to the accompanying drawings and specific embodiments. It should be noted that, to make the embodiments more detailed, the following embodiments are the best and preferred embodiments; those skilled in the art can also use other alternative methods to implement some known technologies; and the accompanying drawings are only for more specific description of the embodiments and are not intended to specifically limit the present invention.

[0024] like Figures 1 to 9 As shown, this embodiment of the invention provides a water cooling device for lithium hexafluorophosphate manufacturing and its usage method, including a reactor 4, a sealing cover 5 on the top of the reactor 4, an insulation barrel 2 wrapped around the outer surface of the reactor 4, and a frame 1 fixedly installed at the bottom of the insulation barrel 2; a cooling pipe 3 for introducing external cooling medium is coiled in the space between the insulation barrel 2 and the outer wall of the reactor 4, forming an external cooling circuit; the sealing cover 5 is provided with a gas filling mechanism 6 for conveying and dispersing reaction gas into the reactor 4; the gas filling mechanism 6 includes a receiving cylinder 61 fixedly connected to the bottom of the sealing cover 5, a ring seat 64 is rotatably sealed inside the receiving cylinder 61, a receiving pipe 63 is fixedly connected to the bottom of the ring seat 64, and an air inlet pipe 62 is fixedly connected to the top of the receiving cylinder 61; the bottom of the receiving pipe 63 extends into the interior of the reactor 4, and a porous exhaust assembly 65 is provided on its outer side; A cold storage pipe 7 is coaxially arranged inside the receiving pipe 63. The top of the cold storage pipe 7 passes through the receiving pipe 63 and is provided with a gas supply pipe 71. Both sides of the cold storage pipe 7 are fixedly connected to branch pipes 72. Heat exchange is carried out with the gas supply path of the porous exhaust assembly 65 through the branch pipes 72 to form an internal cooling passage. The sealing cover 5 is also provided with a drive assembly for driving the receiving pipe 63 to rotate. The reaction vessel 4 wall is cooled by cooling pipe 3, and the reaction gas and surrounding liquid area flowing through porous exhaust component 65 are cooled by cold storage pipe 7. Combined with the drive component, the receiving pipe 63 is driven to rotate to break bubbles and enhance mixing, so as to avoid local overheating at the gas-liquid reaction interface.

[0025] like Figures 1 to 9 As shown, the outer circular surface of the cold storage pipe 7 is provided with a fixing block 73 that is fixedly connected to the receiving pipe 63; the drive assembly includes a driven gear 66 fixedly connected to the top of the outer circular surface of the receiving pipe 63, a first servo motor 67 is fixedly installed on the top of the sealing cover 5, the output shaft of the first servo motor 67 passes through the sealing cover 5 and is fixedly connected to a main gear 68, and the main gear 68 is meshed with the driven gear 66; a sealing sleeve is provided between the output shaft of the first servo motor 67 and the sealing cover 5.

[0026] To address the issues of reduced reaction efficiency, compromised product purity, and uneven bubble mixing caused by localized overheating at the gas-liquid reaction interface within reactor 4 during lithium hexafluorophosphate manufacturing, the aforementioned technical solution is employed. The above-mentioned technical solution mainly consists of a gas filling mechanism 6, a drive assembly, and a cold storage pipe 7. In use, firstly, the reactor 4 is enclosed in an insulation container 2, with a cooling pipe 3 coiled between them. An external cooling medium is introduced into the cooling pipe 3 to initially cool the walls of the reactor 4, forming the first line of defense, reducing external heat interference and carrying away some of the reaction heat. Subsequently, the reaction gas enters the receiving cylinder 61 through the inlet pipe 62 at the top of the sealing cap 5, and then is introduced into the receiving pipe 63 through the rotating sealing ring seat 64. The gas finally enters the porous exhaust assembly 65 at different locations and disperses into the liquid inside the reactor 4 in the form of tiny bubbles. During this process, the cold storage pipe 7 located inside the receiving pipe 63 plays a crucial role. The low-temperature cooling medium enters the cold storage pipe 7 through the gas delivery pipe 71 and is diverted to the branch pipes 72 on both sides. The branch pipes 72 are adjacent to the gas supply path of the porous exhaust assembly 65. When the high-temperature reaction gas flows through this point or just exits and forms bubbles, the cold storage pipe 7 and its branch pipes 72 rapidly... The system rapidly absorbs heat from the gas and surrounding liquid, forming an internal cooling pathway. This "dual cooling" mechanism (using the external cooling pipe 3 in conjunction with the internal cold storage pipe 7) ensures the uniformity of the reaction system temperature and effectively avoids local hot spots at the gas-liquid interface. Finally, to address the issues of bubble aggregation and insufficient mixing during the rising process, the first servo motor 67 is activated, driving the main gear 68 on its output shaft to rotate. The driven gear 66, meshing with the main gear 68, drives the entire receiving pipe 63, along with the porous exhaust assembly 65 at the bottom, to rotate at high speed within the reactor 4. Since the cold storage pipe 7 is fixedly connected to the receiving pipe 63 via the fixing block 73, it also rotates accordingly. The shearing force generated by the rotation breaks large bubbles into smaller bubbles, greatly increasing the gas-liquid contact area. Simultaneously, the rotating flow field enhances the turbulence of the liquid, allowing the cooling energy of the cold storage pipe 7 to be transferred more quickly to all corners of the reactor 4, further eliminating temperature gradients.

[0027] like Figures 1 to 9 As shown, a magnetic sleeve 9 is slidably connected to one end of the outer surface of the branch pipe 72. The end of the branch pipe 72 extends to the side of the gas input end of the porous exhaust assembly 65. The magnetic sleeve 9 is configured to partially block or open the gas input channel of the porous exhaust assembly 65 when it moves along the branch pipe 72. An adjustment mechanism 8 is provided inside the branch pipe 72 to drive the magnetic sleeve 9 to move along the branch pipe 72, adjust the flow rate of the reaction gas by changing the degree of blockage of the gas input channel by the magnetic sleeve 9, and at the same time change the effective length of the heat exchange of the cooling medium.

[0028] like Figures 1 to 9As shown, the adjusting mechanism 8 includes a threaded rod 87 arranged axially along the branch pipe 72. The two ends of the threaded rod 87 are respectively provided with a support cylinder 88 and a second sleeve plate 89 fixedly connected to the inner wall of the branch pipe 72. Both sides of the second sleeve plate 89 are provided with a blocking cylinder 810 fixedly connected to the threaded rod 87. Limiting strips 86 are fixedly connected to the upper and lower sides of the inner wall of the branch pipe 72. The outer circular surface of the threaded rod 87 is spirally connected to a slide block 812. The top and bottom ends of the outer circular surface of the slide block 812 are provided with slots that are adapted to the limiting strips 86. The slide block 812 is of grade S and the magnetic sliding sleeve 9 is of grade N.

[0029] like Figures 1 to 9 As shown, the adjustment mechanism 8 also includes a second servo motor 81 fixedly connected to the top of the cold storage tube 7. The output end of the second servo motor 81 is fixedly connected to a sleeve rod 82. The inner bottom of the sleeve rod 82 is fixedly connected to a drive rod 83. The outer circular surface of the drive rod 83 is provided with a first sleeve plate 84 fixedly connected to the cold storage tube 7. The outer circular surface of the drive rod 83 is fixedly connected to a main bevel gear 85 arranged linearly. One end of the threaded rod 87 is fixedly connected to a driven bevel gear 811 that meshes with the main bevel gear 85.

[0030] To address the issues in lithium hexafluorophosphate manufacturing where dynamic changes in the reaction stages (e.g., rapid cooling to suppress explosion during the initiation phase and maintaining constant temperature for crystallization during the stable phase) cause independent and asynchronous responses in traditional equipment for cooling intensity adjustment and reactant gas (phosphorus pentafluoride) feed flow control, leading to localized overheating, increased side reactions, or uneven gas-liquid mixing within the reactor 4, this new system, based on temperature feedback from within the reactor 4, activates the second servo motor 81 when adjustments are needed. This motor's output shaft drives the sleeve rod 82 to rotate, which in turn drives the drive rod 83 at its bottom. Since the drive rod 83 is fixedly connected to the cold storage pipe 7 via the first sleeve plate 84, ensuring the stability of the central drive shaft, multiple main... The bevel gear 85 rotates accordingly and meshes with the driven bevel gear 811 located at the ends of each branch pipe 72, distributing the rotational power evenly and synchronously to all the surrounding branch pipe 72 units. During the rotation of the driven bevel gear 811, it drives the threaded rod 87 fixedly connected to it to rotate inside the branch pipe 72. The two ends of the threaded rod 87 are fixed to the inner wall of the branch pipe 72 by the support cylinder 88 and the second sleeve plate 89. The second sleeve plate 89 is provided with blocking cylinders 810 on both sides to limit the axial position of the threaded rod 87, ensuring that it only performs rotational motion. During this process, since the top and bottom ends of the slide block 812 are provided with slots that are compatible with the limiting strip 86, the slide block 812 performs linear reciprocating motion along the axial direction of the threaded rod 87 when the threaded rod 87 rotates. Since the slide block 812 is an S-pole magnetic pole, while the magnetic sleeve 9, which is slidably connected to the outer surface of the branch pipe 72, is an N-pole magnetic pole, according to the principle of opposite poles attracting each other, when the internal slide block 812 moves under the drive of the threaded rod 87, the magnetic force it generates will penetrate the pipe wall, pulling the external magnetic sleeve 9 to move synchronously along the outer surface of the branch pipe 72 and approach the receiving cylinder 61, thereby blocking the gas inlet port of the porous exhaust assembly 65; conversely, when the magnetic sleeve 9 moves away from the receiving cylinder 61, it opens the channel for the reaction gas to enter the porous exhaust assembly 65, changing the position of the magnetic sleeve 9 through the slide block 812, thereby changing the five The flow cross-sectional area of ​​the phosphorus fluoride reaction gas entering the porous exhaust assembly 65 enables stepless adjustment of the intake airflow without the need for additional valves. At the same time, the change in the position of the slide 812 inside the branch pipe 72 corresponds to the change in the flow rate of the cooling medium entering the branch pipe 72. That is, when the slide 812 is close to the cold storage pipe 7, the flow volume of the cooling channel formed by the cold storage pipe 7 and the branch pipe 72 decreases, thereby reducing the heat exchange rate accordingly. Conversely, when the slide 812 is far away from the cold storage pipe 7, the flow volume of the cooling channel formed by the cold storage pipe 7 and the branch pipe 72 increases, thereby increasing the heat exchange rate accordingly.

[0031] like Figures 1 to 9As shown, the porous exhaust assembly 65 also includes a porous air pipe 651 fixedly connected to the receiving pipe 63. The porous air pipe 651 has multiple exhaust holes 652 on its wall. Each exhaust hole 652 is fixedly connected to a support plate 653. A spring 654 is fixedly connected to the outside of the support plate 653. A cap 655 for clearing the exhaust hole 652 is fixedly connected to the spring 654. Limiting rods 656 parallel to the porous air pipe 651 are provided on both sides of the outer surface of the receiving pipe 63. A sleeve 657 slidably connected to the limiting rod 656 is provided at one end of the outer circular surface of the porous air pipe 651. The sleeve 657 is of grade S.

[0032] like Figures 1 to 9 As shown, in cross-sectional view, sleeve 657 presents a bent plate-like structure with variable cross-sectional thickness; its upper part has a relatively thick rectangular cross-section at the connection with the limiting rod 656, which gradually narrows and concaves to form an arc-shaped transition section as it extends downward. The inner contour line of this arc-shaped section is parallel to the outer circumferential surface of the porous air tube 651 and has a preset gap; the end area is further thickened and forms an abutting protrusion to abut against the cap 655 to clear the exhaust hole 652.

[0033] To address the issue that solid byproducts or crystalline particles generated during the preparation of lithium hexafluorophosphate easily clog the exhaust port 652 of the porous gas pipe 651, leading to uneven distribution of phosphorus pentafluoride gas and excessively high local pressure, the following mechanism is employed: When the adjusting mechanism 8 drives the magnetic sleeve 9 towards the receiving cylinder 61 to adjust the gas flow, the magnetic sleeve 9 uses magnetic attraction to synchronously drive the sleeve 657 to slide axially along the limiting rod 656. As the sleeve 657 moves towards the receiving cylinder 61, the abutment at its end gradually presses against the cap 655. Since the cap 655 is connected to the support plate 653 via a spring 654, the applied pressure forces the cap 655... Overcoming the spring force, the cap 655 reciprocates into the vent 652. During this process, the edge of the cap 655 scrapes away lithium hexafluorophosphate crystals and impurities adhering to the inner wall or opening of the vent 652 like a scraper. As the sleeve 657 moves, when the sleeve 657 no longer obstructs the cap 655, the restoring force of the spring 654 pushes the cap 655 back to its original position quickly. This reciprocating action of "pressing in first and then popping out" effectively destroys the structure of the blockage, peels it off and blows it away, thereby keeping the vent 652 unobstructed. This eliminates the need to stop the machine for disassembly and cleaning during the preparation of lithium hexafluorophosphate, significantly improving the continuity and efficiency of lithium hexafluorophosphate production. In this process, the sleeve 657 is designed with a variable cross-section and a bent shape to ensure that its upper end maintains a certain rigid connection with the limiting rod 656, and avoids hard friction with the porous air tube 651 through the arc transition section, thus reducing wear. The thickening of the end is intended to allow the abutment boss to concentrate its action on the cap 655, thereby increasing the impact force for unblocking.

[0034] like Figures 1 to 9 As shown, a feed pipe 51 is also fixedly connected to one side of the top of the sealing cover 5; an exhaust valve 10 and a pressure gauge 11 are also fixedly installed on the front side of the sealing cover 5.

[0035] like Figures 1 to 9 As shown, the inner wall of the heat preservation barrel 2 is provided with a buffer plate 21 for supporting the cooling pipe 3; a pad 22 is fixedly connected around the bottom of the inner wall of the heat preservation barrel 2, and a vent plate 23 is fixedly connected to the upper surface of the pad 22; both sides of the bottom of the reactor 4 are fixedly connected to discharge pipes 41, and the discharge pipes 41 pass through the bottom of the heat preservation barrel 2 and are fixedly installed with discharge valves 42; a limiting cylinder 43 for limiting the receiving cylinder 61 is fixedly connected to the middle of the bottom of the reactor 4.

[0036] Before preparing lithium hexafluorophosphate, anhydrous hydrogen fluoride and other liquid raw materials are pre-injected into the reactor 4 through the feed pipe 51. During the reaction, the pressure gauge 11 monitors the pressure changes inside the reactor in real time, providing key data for the control system to adjust the gas intake. When the reaction ends or an emergency pressure relief is required, the operator can safely discharge the residual acidic waste gas through the exhaust valve 10 to prevent overpressure explosion or splashing when the lid is opened, ensuring the safety of high-risk chemical operations. When a low-temperature medium is introduced into the cooling pipe 3 or when deformation occurs due to the heat of reaction, the buffer plate 21 acts as an elastic medium. The heat exchanger effectively absorbs the hard impact and stress concentration between the pipe body and the insulation tank 2, preventing cracking of the pipe welds and extending the service life of the cooling system. Simultaneously, a pad 22 is fixedly connected around the bottom of the inner wall of the insulation tank 2, and a vent plate 23 is fixedly connected to the upper surface of the pad 22. This not only provides a stable and level mounting base for the reactor 4, but the porous nature of the vent plate 23 also allows for the timely discharge of any small amount of leaked gas or condensate within the insulation tank 2's interlayer, preventing water accumulation that could corrode the reactor bottom or create localized hot spots, thus maintaining a dry and uniform insulation environment. After the reaction is complete, the discharge valve 42 is opened, and the generated lithium hexafluorophosphate slurry is rapidly discharged from the double-sided discharge pipes 41 under gravity, effectively avoiding the potential for uneven flow or dead zones that might result from single-sided discharge, thus improving discharge efficiency. Furthermore, the limiting cylinder 43, fixedly connected to the middle of the bottom of the reactor 4, serves to receive and limit the position of the receiving cylinder 61, ensuring that the receiving cylinder 61 remains in a central and vertical position inside the reactor 4.

[0037] A method for using a water cooling device in the manufacture of lithium hexafluorophosphate, the method comprising the following steps: S1: Liquid raw materials such as anhydrous hydrogen fluoride are injected into the reactor 4 through the feed pipe 51. At the same time, the external cooling medium is introduced into the cooling pipe 3 to initially cool the reactor wall. During this process, the buffer plate 21 absorbs the thermal stress of the pipeline, the pad plate 22 and the vent plate 23 keep the insulation layer dry, and the pressure gauge 11 is turned on to monitor the gas pressure in real time, so that the exhaust valve 10 is in standby state. S2: After the reaction begins, phosphorus pentafluoride gas is introduced into the receiving pipe 63 through the inlet pipe 62, the receiving cylinder 61 and the ring seat 64, and finally released in the form of microbubbles by the porous exhaust component 65. At the same time, the low temperature medium is introduced into the cold storage pipe 7 and the branch pipe 72, so that the cold storage pipe 7 and the branch pipe 72 can quickly absorb the heat of the high temperature reaction gas and the surrounding liquid area. S3: Start the first servo motor 67, drive the main gear 68 and the driven gear 66 to rotate, and drive the receiving pipe 63, the porous exhaust assembly 65 and the cold storage pipe 7 to rotate at high speed in the reactor, using the shear force generated by the rotation to break up large bubbles to increase the gas-liquid contact area. S4: The second servo motor 81 is started according to the needs of the reaction stage, driving the threaded rod 87 to rotate, thereby driving the slide block 812 to move axially. The magnetic sleeve 9 is synchronously displaced by magnetic coupling, and the flow rate and cooling intensity of the reaction gas are synchronously adjusted. At the same time, the sleeve 657 is synchronously moved by the magnetic force of the magnetic sleeve 9, and the sleeve 657 presses the cap 655 to clear the exhaust hole 652. S5: After the reaction is complete, open the double-sided discharge valve 42 to allow the generated lithium hexafluorophosphate slurry to be discharged through the discharge pipe 41 under gravity, thus completing the production process.

[0038] In use, this invention first injects anhydrous hydrogen fluoride and other liquid raw materials into the reactor 4 through the feed pipe 51. Then, an external cooling medium is introduced into the cooling pipe 3 to initially cool the reactor 4 wall, reducing environmental heat interference and removing some of the reaction heat. During this process, the buffer plate 21 acts as an elastic medium layer, effectively absorbing the deformation stress caused by thermal expansion and contraction of the cooling pipe 3, preventing cracking of the pipe welds. The gasket 22 and the vent plate 23 not only provide a stable base for the reactor 4 but also promptly discharge any trace amounts of leaked gas or condensate from the jacket, maintaining a dry and uniform insulation environment. Simultaneously, the pressure gauge 11 monitors the internal pressure in real time, providing data support for subsequent control, while the exhaust valve 10 is in standby mode to handle emergency pressure relief needs. After the reaction begins, phosphorus pentafluoride gas enters the receiving cylinder 61 through the inlet pipe 62 and is introduced into the receiving cylinder through the rotating sealed ring seat 64. The gas flows through pipe 63 and finally reaches the porous exhaust assembly 65, where it disperses into the liquid in the form of tiny bubbles. At the same time, the low-temperature cooling medium enters the cold storage pipe 7 through the gas supply pipe 71 and is distributed to the branch pipes 72 on both sides. Since the branch pipes 72 are close to the gas exhaust path, the cold storage pipe 7 quickly absorbs the heat from the high-temperature reaction gas and the surrounding liquid area, forming a "double cooling" mechanism with the external cooling pipe 3 to ensure uniform temperature of the reaction system and avoid local hot spots at the gas-liquid interface. In order to further enhance the mixing effect, the first servo motor 67 is started, which drives the main gear 68 and the driven gear 66 to mesh and rotate, driving the entire receiving pipe 63, the porous exhaust assembly 65 and the cold storage pipe 7 fixed on it to rotate at high speed in the reactor. Under the shearing force generated by the rotation, the large bubbles are broken into micro bubbles, which greatly increases the gas-liquid contact area. At the same time, the turbulent flow field formed accelerates the transfer of cold energy and completely eliminates the temperature gradient.Next, in response to the dynamic demands of different reaction stages (such as the need for strong cooling and low gas volume during the initiation phase, and constant temperature and high gas volume during the stable phase), the control system, based on temperature feedback, activates the second servo motor 81, driving the sleeve rod 82 and drive rod 83 to rotate. Through the meshing of the main bevel gear 85 and the driven bevel gear 811, the threaded rod 87 inside each branch pipe 72 rotates. Guided by the limit bar 86, the threaded rod 87 drives the internal slide block 812 to make axial linear motion. Utilizing the magnetic coupling between the S-level of the slide block 812 and the N-level of the external magnetic sleeve 9, the magnetic sleeve 9 is pulled to move synchronously along the outer surface of the branch pipe 72, thereby changing the degree of obstruction of the intake channel of the porous exhaust assembly 65 by the magnetic sleeve 9, thus achieving stepless adjustment of the reaction gas flow rate; and simultaneously changing the effective heat exchange length exposed by the branch pipe 72, synchronously adjusting the cooling intensity, solving the problems of traditional design The problem of asynchronous cooling and gas supply response during preparation is addressed. Furthermore, while the magnetic sleeve 9 moves axially to adjust the flow rate of the reaction gas into the porous gas pipe (651), it simultaneously drives the sleeve 657 next to the porous gas pipe 651 to move axially along the limiting rod 656 via magnetic attraction. This causes the contact boss at the end of the sleeve 657 to press against the cap 655, forcing the cap 655 to overcome the spring force of the spring 654 and reciprocate into the exhaust hole 652, scraping away crystalline impurities adhering to the orifice like a scraper. When the sleeve 657 resets, the spring 654 pushes the cap 655 back quickly. This reciprocating motion of "pressing in first, then popping out" achieves automatic unblocking without stopping the machine. Finally, after the reaction is complete and normal discharge occurs, the double-sided discharge valve 42 is opened, and the lithium hexafluorophosphate slurry is quickly discharged through the discharge pipe 41 under gravity.

[0039] This invention encompasses any substitutions, modifications, equivalent methods, and solutions made within the spirit and scope of this invention. To provide the public with a thorough understanding of this invention, specific details are described in detail in the following preferred embodiments; however, those skilled in the art will fully understand the invention even without these details. Furthermore, to avoid unnecessary misunderstanding of the essence of this invention, well-known methods, processes, procedures, components, and circuits are not described in detail.

[0040] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A water cooling device for lithium hexafluorophosphate manufacturing and a method for using the same, comprising a reaction kettle (4), a sealing cover (5) is arranged at the top of the reaction kettle (4), the outer surface of the reaction kettle (4) is wrapped with a heat preservation barrel (2), and a rack (1) is fixedly installed at the bottom of the heat preservation barrel (2); characterized in that, The space between the heat preservation barrel (2) and the outer wall of the reactor (4) is filled with a cooling pipe (3) for introducing external cooling medium, forming an external cooling circuit; the interior of the sealing cover (5) is provided with a gas filling mechanism (6) for conveying and dispersing reaction gas into the reactor (4); the gas filling mechanism (6) includes a receiving cylinder (61) fixedly connected to the bottom of the sealing cover (5), the inside of the receiving cylinder (61) is rotatably sealed with a ring seat (64), the bottom of the ring seat (64) is fixedly connected to a receiving pipe (63), and the top of the receiving cylinder (61) is fixedly connected to an air inlet pipe (62); the bottom of the receiving pipe (63) extends into the interior of the reactor (4), and its outer side is provided with a porous exhaust assembly (65). The receiving pipe (63) is coaxially provided with a cold storage pipe (7). The top of the cold storage pipe (7) passes through the receiving pipe (63) and is provided with a gas supply pipe (71). Both sides of the cold storage pipe (7) are fixedly connected to branch pipes (72). Heat exchange is carried out with the gas supply path of the porous exhaust assembly (65) through the branch pipes (72) to form an internal cooling passage. The sealing cover (5) is also provided with a drive assembly for driving the receiving pipe (63) to rotate. The wall of the reactor (4) is cooled by the cooling pipe (3), and the reaction gas and the surrounding liquid area flowing through the porous exhaust component (65) are cooled by the cold storage pipe (7). The drive component drives the receiving pipe (63) to rotate to break up bubbles and enhance mixing, so as to avoid local overheating of the gas-liquid reaction interface.

2. The water cooling apparatus for manufacturing lithium hexafluorophosphate and the method of using the same according to claim 1, wherein The outer surface of the cold storage pipe (7) is provided with a fixing block (73) that is fixedly connected to the receiving pipe (63); the drive assembly includes a driven gear (66) fixedly connected to the top of the outer surface of the receiving pipe (63); a first servo motor (67) is fixedly installed on the top of the sealing cover (5); the output shaft of the first servo motor (67) passes through the sealing cover (5) and is fixedly connected to a main gear (68); the main gear (68) meshes with the driven gear (66); a sealing sleeve is provided between the output shaft of the first servo motor (67) and the sealing cover (5).

3. The water cooling equipment for lithium hexafluorophosphate manufacturing and its method of use according to claim 2, characterized in that, A magnetic sleeve (9) is slidably connected to one end of the outer surface of the branch pipe (72). The end of the branch pipe (72) extends to the side of the gas input end of the porous exhaust assembly (65). The magnetic sleeve (9) is configured to partially block or open the gas input channel of the porous exhaust assembly (65) when it moves along the branch pipe (72). The interior of the branch pipe (72) is provided with an adjustment mechanism (8) for driving the magnetic sleeve (9) to move along the branch pipe (72), adjusting the flow rate of the reaction gas by changing the degree of blockage of the gas input channel by the magnetic sleeve (9), and simultaneously changing the effective length of the heat exchange of the cooling medium.

4. The water cooling apparatus for manufacturing lithium hexafluorophosphate according to claim 3, wherein The adjustment mechanism (8) includes a threaded rod (87) arranged axially along the branch pipe (72). The two ends of the threaded rod (87) are respectively provided with a support cylinder (88) and a second sleeve plate (89) fixedly connected to the inner wall of the branch pipe (72). Both sides of the second sleeve plate (89) are provided with a blocking cylinder (810) fixedly connected to the threaded rod (87). Limiting strips (86) are fixedly connected to the upper and lower sides of the inner wall of the branch pipe (72). The outer circular surface of the threaded rod (87) is spirally connected with a slide (812). The top and bottom ends of the outer circular surface of the slide (812) are provided with slots that are compatible with the limiting strips (86). The slide (812) is of grade S and the magnetic sliding sleeve (9) is of grade N.

5. The water cooling equipment for lithium hexafluorophosphate manufacturing and its method of use according to claim 4, characterized in that, The adjustment mechanism (8) further includes a second servo motor (81) fixedly connected to the top of the cold storage tube (7). The output end of the second servo motor (81) is fixedly connected to a sleeve rod (82). The inner bottom of the sleeve rod (82) is fixedly connected to a drive rod (83). The outer circular surface of the drive rod (83) is provided with a first sleeve plate (84) fixedly connected to the cold storage tube (7). The outer circular surface of the drive rod (83) is fixedly connected to a main bevel gear (85) arranged in a linear pattern. One end of the threaded rod (87) is fixedly connected to a driven bevel gear (811) meshing with the main bevel gear (85).

6. The water cooling equipment for lithium hexafluorophosphate manufacturing and its method of use according to claim 5, characterized in that, The porous exhaust assembly (65) further includes a porous air pipe (651) fixedly connected to the receiving pipe (63). The porous air pipe (651) has multiple exhaust holes (652) on its wall. Each exhaust hole (652) is fixedly connected to a support plate (653). A spring (654) is fixedly connected to the outside of the support plate (653). A cap (655) for unblocking the exhaust hole (652) is fixedly connected to the spring (654). Limiting rods (656) parallel to the porous air pipe (651) are provided on both sides of the outer surface of the receiving pipe (63). A sleeve (657) slidably connected to the limiting rod (656) is provided at one end of the outer circular surface of the porous air pipe (651). The sleeve (657) is of grade S.

7. The water cooling equipment for lithium hexafluorophosphate manufacturing and its method of use according to claim 6, characterized in that, In cross-sectional view, the sleeve (657) presents a bent plate-like structure with variable cross-sectional thickness; its upper part has a relatively thick rectangular cross-section at the connection with the limiting rod (656), which gradually narrows and concaves to form an arc-shaped transition section as it extends downward. The inner contour line of the arc-shaped section is parallel to the outer circumference of the porous air tube (651) and has a preset gap; the end area is further thickened and forms an abutting protrusion to abut against the cap (655) to clear the exhaust hole (652).

8. The water cooling equipment for lithium hexafluorophosphate manufacturing and its method of use according to claim 7, characterized in that, A feed pipe (51) is fixedly connected to one side of the top of the sealing cover (5); an exhaust valve (10) and a pressure gauge (11) are also fixedly installed on the front side of the sealing cover (5).

9. The water cooling equipment for lithium hexafluorophosphate manufacturing and its method of use according to claim 8, characterized in that, The inner wall of the heat-insulating barrel (2) is provided with a buffer plate (21) for supporting the cooling pipe (3); a pad (22) is fixedly connected around the bottom of the inner wall of the heat-insulating barrel (2), and a breathable plate (23) is fixedly connected to the upper surface of the pad (22); both sides of the bottom of the reactor (4) are fixedly connected to discharge pipes (41), and the discharge pipes (41) penetrate the bottom of the heat-insulating barrel (2) and are fixedly installed with discharge valves (42); a limiting cylinder (43) for limiting the receiving cylinder (61) is fixedly connected to the middle of the bottom of the reactor (4).

10. A method of using a water cooling device for lithium hexafluorophosphate manufacturing as described in any one of claims 1 to 9, characterized in that, The method of use includes the following steps: S1: Anhydrous hydrogen fluoride and other liquid raw materials are injected into the reactor (4) through the feed pipe (51). At the same time, the external cooling medium is introduced into the cooling pipe (3) to initially cool the reactor wall. During this process, the buffer plate (21) is used to absorb the thermal stress of the pipeline. The insulation layer is kept dry through the pad plate (22) and the vent plate (23). The pressure gauge (11) is turned on to monitor the gas pressure in real time, and the exhaust valve (10) is put in standby mode. S2: After the reaction begins, phosphorus pentafluoride gas is introduced into the receiving pipe (63) through the inlet pipe (62), the receiving cylinder (61) and the ring seat (64), and finally released in the form of microbubbles by the porous exhaust assembly (65). At the same time, the low temperature medium is introduced into the cold storage pipe (7) and the branch pipe (72), so that the cold storage pipe (7) and the branch pipe (72) can quickly absorb the heat of the high temperature reaction gas and the surrounding liquid area. S3: Start the first servo motor (67), drive the main gear (68) and driven gear (66) to rotate, and drive the receiving pipe (63), the porous exhaust assembly (65) and the cold storage pipe (7) to rotate at high speed in the reactor, using the shear force generated by the rotation to break up large bubbles to increase the gas-liquid contact area; S4: Start the second servo motor (81) according to the needs of the reaction stage, drive the threaded rod (87) to rotate, thereby driving the slide (812) to move axially. Use magnetic coupling to pull the magnetic sleeve (9) to move synchronously, and adjust the reaction gas flow rate and cooling intensity synchronously. At the same time, use the magnetic force of the magnetic sleeve (9) to drive the sleeve (657) to move synchronously. Use the sleeve (657) to press the cap (655) to clear the exhaust hole (652). S5: After the reaction is complete, open the double-sided discharge valve (42) so that the generated lithium hexafluorophosphate slurry is discharged through the discharge pipe (41) under gravity, thus completing the production process.

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