Continuous production device of lithium hexafluorophosphate

Abstract

The utility model discloses a continuous production device of lithium hexafluorophosphate, and belongs to the technical field of lithium hexafluorophosphate production and preparation. Aiming at the problems that a traditional device is difficult to control the size of crystallized particles, poor in product fluidity, low in separation efficiency and low in reaction heat influence reaction, the device comprises a fixing frame, and a micro-mixing mechanism and a crystallizing mechanism are arranged on the fixing frame. The micro-mixing mechanism comprises a reactor with a heat conduction pipe, a cooling assembly and a winding blade, and can be used for cooling and increasing the gas-liquid contact area; the crystallization mechanism comprises crystallization equipment, a circulating pump, a heat exchanger and a stirring assembly, and can control the size of crystallized particles through circulation; the filter adopts a composite structure of a PTFE micro-filtration membrane and flaky graphene sponge, and is corrosion-resistant and anti-blocking. The device realizes continuous production, improves the crystallization efficiency and particle uniformity, improves the reaction and solid-liquid separation efficiency, and ensures the product quality.

Description

Technical Field

[0001] This utility model belongs to the field of lithium hexafluorophosphate production and preparation technology, and in particular relates to a continuous production device for lithium hexafluorophosphate. Background Technology

[0002] In the prior art, a search revealed a Chinese patent disclosed as a "continuous lithium hexafluorophosphate generation device," with publication number "CN219150135U." This patent mainly increases the contact time between phosphorus pentafluoride and lithium fluoride hydrofluoric acid solution by setting up a primary reaction component and a secondary reaction component, thereby improving the conversion efficiency of the product and achieving continuous feeding and discharging, and continuous reaction. By setting up a first lithium fluoride silo and a second lithium fluoride silo, continuous feeding is achieved. The continuous lithium hexafluorophosphate generation device of this utility model reduces manual intervention and lowers production costs.

[0003] However, in the process of synthesizing lithium hexafluorophosphate, most devices cannot control the size of the crystal particles, resulting in inconsistent particle sizes in the finished product. This affects the flowability of the product, leading to difficulties in discharge and impacting production. Secondly, excessively small micro-particles have strong adsorption properties and are more likely to absorb moisture from the environment, affecting product quality. Utility Model Content

[0004] The purpose of this invention is to provide a continuous production device for lithium hexafluorophosphate. By setting up a crystallization mechanism, the solvent is evaporated and concentrated on the liquid surface to reach a supersaturated state, and LiPF6 is crystallized. This can effectively control the particle size of the product after crystallization, greatly improve the efficiency and effect of crystallization, and solve the problem that most devices cannot control the size of the crystallized particles, resulting in inconsistent particle sizes in the finished product.

[0005] To solve the above-mentioned technical problems, this utility model is achieved through the following technical solution:

[0006] A continuous production apparatus for lithium hexafluorophosphate includes a fixed frame (1), characterized in that: a micro-mixing mechanism (2) and a crystallization mechanism (3) are provided on the fixed frame (1), and the micro-mixing mechanism (2) includes a cooling component;

[0007] The cooling assembly includes a reactor (21) fixedly connected to a mounting frame (1), the outer wall of the reactor (21) being provided with a refrigerant outlet (22), and the outer wall of the mounting frame (1) being provided with a refrigerant inlet (221).

[0008] The crystallization mechanism (3) includes a circulation component, a stirring component, and an adjustment component. The circulation component includes a crystallization device (31) fixedly connected to a fixed frame (1). The inner bottom wall of the crystallization device (31) is connected to the end of a second pipe (33). The second pipe (33) is fixedly connected to the output end of a circulation pump (32). The circulation pump (32) is fixedly connected to the right end of a first pipe (24). A third pipe (35) is provided in communication with the outer wall of the first pipe (24). The top end of the third pipe (35) extends to the inner wall of the crystallization device (31).

[0009] A heat exchanger (34) is provided on the second pipe (33). A fourth pipe (36) is connected to the top surface of the reactor (21). A second circulation pump (361) is connected to the end of the fourth pipe (36) away from the reactor (21). A filter (362) is connected to the end of the second circulation pump (361) away from the fourth pipe (36) through a pipe. The filter (362) is on the main discharge line, i.e., the first pipe (24).

[0010] Furthermore, the inner wall of the reactor (21) is fixedly connected to two square plates (25), each of the two square plates (25) is provided with several outlets (26), the inner walls of the several outlets (26) are fixedly connected to heat conduction pipes (27), the top surface of the reactor (21) is connected to a feed pipe (23), and the bottom surface of the reactor (21) is connected to a first pipe (24).

[0011] Furthermore, the micro-mixing mechanism includes several connecting rods (28) fixedly connected to the top and bottom of several heat-conducting pipes (27), and a baffle (29) is fixedly connected to one end of the several connecting rods (28) away from the heat-conducting pipes (27).

[0012] Furthermore, a rotating rod (291) is rotatably connected between the two baffles (29), and a winding blade (292) is fixedly connected to the outer wall of the rotating rod (291).

[0013] Furthermore, the stirring assembly includes a drive motor (37) fixedly connected to the top surface of the crystallization device (31), and a rotating rod (38) is fixedly connected to the output end of the drive motor (37). The bottom end of the rotating rod (38) extends rotatably into the interior of the crystallization device (31), and a plurality of stirring blades (39) are fixedly connected to the outer wall of the rotating rod (38).

[0014] Furthermore, the regulating component includes an air outlet (391) connected to the outer wall of the crystallization device (31), a discharge pipe (392) fixedly connected to the bottom surface of the crystallization device (31), a ball valve (393) slidably connected to the inner wall of the discharge pipe (392), the outer diameter of the ball valve (393) being the same as the inner diameter of the discharge pipe (392), an adjusting rod (394) fixedly connected to the outer wall of the ball valve (393), and the right end of the adjusting rod (394) rotatably extending to the outer wall of the discharge pipe (392).

[0015] Furthermore, in the filter (362), a PTFE microfiltration membrane and a sheet graphene sponge are stacked and placed on top of each other, cut to the same size, and then rolled into a cylindrical shape, the outer diameter of which is smaller than the inner diameter of the filter 362.

[0016] Furthermore, the thickness of the PTFE microfiltration membrane is 260-280 mm, the thickness of the sheet graphene sponge is 10-15 mm, and its width is less than the internal length of the filter (362) housing.

[0017] This utility model has the following beneficial effects:

[0018] 1. By setting up a crystallization mechanism, the solvent evaporates and concentrates on the liquid surface to reach a supersaturated state, crystallizing to form LiPF6. Under the action of sedimentation, larger crystal particles are deposited at the bottom of the crystallization equipment, while smaller crystal particles enter the third pipe under the action of the first circulation pump. After mixing with the continuously flowing unsaturated solution, they re-enter the crystallization equipment for circulation. This can effectively control the particle size of the product after molding and greatly improve the efficiency and effect of crystallization.

[0019] 2. During the preparation reaction, a large amount of heat may be generated. At this time, the coolant outlet and coolant inlet can be connected and disconnected from the cooling medium respectively to cool the solution in the heat pipe and avoid affecting the reaction process. The square plate, outlet and heat pipe work together to increase the heating area and greatly improve the cooling effect. When the mixed solution flows into the heat pipe through the gap between the connecting rod and the heat pipe, the rotating rod and the winding blade work together to slow down the fluid flow speed and further improve the cooling effect. At the same time, the fluid can also drive the winding blade to rotate, so that the winding blade can divide the fluid, increase the contact area between gas and liquid, and improve the reaction speed and effect. In addition, the crystallization mechanism and the micro-mixing mechanism work together to achieve the effect of continuous production.

[0020] 3. The filter (362) consists of an overlapping PTFE microfiltration membrane and sheet graphene sponge, cut to the same size, and then rolled into a cylindrical shape. The outer diameter of the cylindrical shape is smaller than the inner diameter of the filter (362), which can be used for a long time under the corrosive effect of hydrofluoric acid environment. The double-layer structure will not be blocked by fine lithium hexafluorophosphate particles, which can improve the solid-liquid separation efficiency.

[0021] Of course, any product implementing this utility model does not necessarily need to achieve all of the advantages described above at the same time. Attached Figure Description

[0022] To more clearly illustrate the technical solutions of the embodiments of this utility model, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0023] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0024] Figure 2 This is a front cross-sectional view of the present invention.

[0025] Figure 3 This is a cross-sectional structural diagram of the heat pipe of this utility model;

[0026] Figure 4 This is a front cross-sectional view of the reactor of this utility model.

[0027] Figure 5 This utility model Figure 4 A magnified structural diagram of point A in the middle.

[0028] The attached diagram lists the components represented by each number as follows:

[0029] 1. Fixed frame; 2. Micro-mixing mechanism; 3. Crystallization mechanism; 21. Reactor; 22. Refrigerant outlet; 221. Refrigerant inlet; 23. Feed pipe; 24. First pipe; 25. Square plate; 26. Outlet; 27. Heat pipe; 28. Connecting rod; 29. ​​Baffle; 291. Rotating rod one; 292. Winding blade; 31. Crystallization equipment; 32. Circulation pump one; 33. Second pipe; 34. Heat exchanger; 35. Third pipe; 36. Fourth pipe; 361. Circulation pump two; 362. Filter; 37. Drive motor; 38. Rotating rod two; 39. Stirring blade; 391. Vent; 392. Discharge pipe; 393. Ball valve; 394. Adjusting rod. Detailed Implementation

[0030] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present utility model.

[0031] Example 1

[0032] Please see Figure 1-5 As shown, a specific application of this embodiment is a continuous production apparatus for lithium hexafluorophosphate, including a fixed frame 1, on which a micro-mixing mechanism 2 and a crystallization mechanism 3 are provided, and the micro-mixing mechanism 2 includes a cooling component.

[0033] The cooling assembly includes a reactor 21 fixedly connected to a mounting frame 1. The outer wall of the reactor 21 is connected to a refrigerant outlet 22, and the outer wall of the mounting frame 1 is connected to a refrigerant inlet 221.

[0034] The crystallization mechanism 3 includes a circulation component, a stirring component, and an adjustment component. The circulation component includes a crystallization device 31 fixedly connected to a fixed frame 1. The inner bottom wall of the crystallization device 31 is connected to the end of the second pipe 33. The second pipe 33 is fixedly connected to the output end of the circulation pump 32. The circulation pump 32 is fixedly connected to the right end of the first pipe 24. A third pipe 35 is provided in communication with the outer wall of the first pipe 24. The top end of the third pipe 35 extends to the inner wall of the crystallization device 31.

[0035] A heat exchanger 34 is installed on the second pipe 33. A fourth pipe 36 is connected to the top surface of the reactor 21. A second circulation pump 361 is connected to the end of the fourth pipe 36 away from the reactor 21. A filter 362 is connected to the end of the second circulation pump 361 away from the fourth pipe 36 through a pipe. The filter 362 is on the main discharge line, i.e., the first pipe 24. A crystallization mechanism 3 is installed on the filter 362 to make the solvent evaporate and concentrate on the liquid surface to reach a supersaturated state and crystallize to form LiPF6. Under the action of sedimentation, the larger crystal particles are deposited to the bottom of the crystallization device 31. The smaller crystal particles enter the third pipe 35 under the action of the first circulation pump 32, mix with the continuously introduced unsaturated solution, and then re-enter the crystallization device 31 for circulation, which greatly improves the efficiency and effect of crystallization.

[0036] Two square plates 25 are fixedly connected to the inner wall of reactor 21. Each square plate 25 has several outlets 26. The inner walls of the outlets 26 are fixedly connected to heat-conducting pipes 27. A feed pipe 23 is connected to the top surface of reactor 21, and a first pipe 24 is connected to the bottom surface of reactor 21. The micro-mixing mechanism includes several connecting rods 28 fixedly connected to the top and bottom of the heat-conducting pipes 27. A baffle 29 is fixedly connected to one end of the connecting rods 28 away from the heat-conducting pipes 27. A rotating rod 291 is rotatably connected between the two baffles 29. A winding blade 292 is fixedly connected to the outer wall of the rotating rod 291.

[0037] The stirring assembly includes a drive motor 37 fixedly connected to the top surface of the crystallization device 31. A rotating rod 38 is fixedly connected to the output end of the drive motor 37. The bottom end of the rotating rod 38 extends rotatably into the interior of the crystallization device 31. Several stirring blades 39 are fixedly connected to the outer wall of the rotating rod 38. By setting a micro-mixing mechanism 2, the cooling medium can be connected to and disconnected from the refrigerant outlet 22 and the refrigerant inlet 221 respectively, so as to cool the solution in the heat pipe 27 and avoid it from affecting the reaction process. Moreover, the square plate 25, the outlet 26 and the heat pipe 27 cooperate with each other to increase the heating area and greatly improve the cooling effect.

[0038] The regulating assembly includes an air outlet 391 connected to the outer wall of the crystallization device 31, a discharge pipe 392 fixedly connected to the bottom surface of the crystallization device 31, a ball valve 393 slidably connected to the inner wall of the discharge pipe 392, the outer diameter of the ball valve 393 being the same as the inner diameter of the discharge pipe 392, and an adjusting rod 394 fixedly connected to the outer wall of the ball valve 393, the right end of the adjusting rod 394 rotatably extending to the outer wall of the discharge pipe 392.

[0039] In filter 362, a PTFE microfiltration membrane and a sheet graphene sponge are stacked and cut to the same size, and then rolled into a cylindrical shape. The outer diameter of the cylindrical shape is smaller than the inner diameter of filter 362.

[0040] The PTFE microfiltration membrane is 260 mm thick, and the sheet graphene sponge is 10 mm thick. Its width is smaller than the internal length of the filter 362 housing.

[0041] Example 2

[0042] One specific application of this embodiment is as follows: A micro-mixing mechanism 2 is provided to continuously feed phosphorus pentafluoride and lithium fluoride solutions into the reactor 21 through the feed pipe 23. The square plate 25 and the outlet 26 cooperate to allow the mixture to pass sequentially through multiple heat-conducting pipes 27 and be discharged from the first pipe 24 as it flows into the fixed frame 1. This allows the two substances to react within the reactor 21 to generate LiPF6, with the reaction equation being: LiF + PF5 → LiPF6. During the reaction process, a large amount of heat may be generated. In this case, the coolant outlet 22 and coolant inlet 221 can be connected to and disconnected from the cooling medium, respectively. The solution inside the heat pipe 27 is cooled to prevent it from affecting the reaction process. The square plate 25, outlet 26 and heat pipe 27 work together to increase the heating area and greatly improve the cooling effect. When the mixed solution flows into the heat pipe 27 through the gap between the connecting rod 28 and the heat pipe 27, the rotating rod 291 and the winding blade 292 work together to slow down the flow of fluid and further improve the cooling effect. At the same time, the fluid can also drive the winding blade 292 to rotate, so that the winding blade 292 divides the fluid, increases the contact area between gas and liquid, and improves the reaction speed and effect.

[0043] With the crystallization mechanism 3 in place, after the solution is mixed, the generated LiPF6 completely dissolves in the HF solution, forming an unsaturated LiPF6 solution. This solution flows into the first pipe 24. At this point, the circulation pump 32 can be activated, allowing it to pump the solution from the first pipe 24 into the crystallization device 31 through the second pipe 33. The heat exchanger 34 heats the solution in the second pipe 33. Simultaneously, the drive motor 37 is turned on, enabling it to drive the rotating rod 38 and multiple stirring blades 39 to stir the solution. This causes the solvent to evaporate and concentrate at the liquid surface, reaching a supersaturated state, resulting in LiPF6 crystallization. Under sedimentation, larger crystal particles settle to the bottom of the crystallization device 31, while smaller crystal particles... The particles enter the third pipe 35 under the action of the circulating pump 32, mix with the continuously introduced unsaturated solution, and then re-enter the crystallization device 31 for circulation. The gas generated after crystallization is discharged through the vent 391. After the gas and liquid in the reactor 21 are completely mixed, they are first pumped to the fourth pipe 36 by the circulating pump 361, and then filtered by the filter 362 on the first pipe 24 to remove insoluble substances (LiF) from the solution. The filtered solution is circulated back to the reactor 21 until the solution is completely mixed, and then transported to the crystallization device 31 by the circulating pump 32 for crystallization. The vent 391, the discharge pipe 392, the ball valve 393, and the regulating rod 394 work together to precisely control the discharge speed by turning the regulating rod 394.

[0044] In filter 362, a PTFE microfiltration membrane and a sheet graphene sponge are stacked and cut to the same size, and then rolled into a cylindrical shape. The outer diameter of the cylindrical shape is smaller than the inner diameter of filter 362.

[0045] The PTFE microfiltration membrane is 270 mm thick, and the sheet graphene sponge is 12 mm thick. Its width is smaller than the internal length of the filter 362 housing.

[0046] Example 3

[0047] In this embodiment, except for the following contents, everything else is the same as in Embodiment 1:

[0048] In filter 362, a PTFE microfiltration membrane and a sheet of graphene sponge are stacked and cut to the same size. They are then rolled into a cylindrical shape, with the outer diameter of the cylinder being smaller than the inner diameter of filter 362.

[0049] The PTFE microfiltration membrane is 280 mm thick, and the sheet graphene sponge is 15 mm thick. Its width is smaller than the internal length of the filter 362 housing.

[0050] The preferred embodiments of this utility model disclosed above are merely illustrative of the present utility model. These preferred embodiments do not exhaustively describe all details, nor do they limit the utility model to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of this utility model, thereby enabling those skilled in the art to better understand and utilize it. This utility model is limited only by the claims and their full scope and equivalents.

Claims

1. A continuous production apparatus for lithium hexafluorophosphate, comprising a fixed frame (1), characterized in that: The fixed frame (1) is provided with a micro-mixing mechanism (2) and a crystallization mechanism (3), and the micro-mixing mechanism (2) includes a cooling component; The cooling assembly includes a reactor (21) fixedly connected to a mounting frame (1), the outer wall of the reactor (21) being provided with a refrigerant outlet (22), and the outer wall of the mounting frame (1) being provided with a refrigerant inlet (221). The crystallization mechanism (3) includes a circulation component, a stirring component, and an adjustment component. The circulation component includes a crystallization device (31) fixedly connected to a fixed frame (1). The inner bottom wall of the crystallization device (31) is connected to the end of a second pipe (33). The second pipe (33) is fixedly connected to the output end of a circulation pump (32). The circulation pump (32) is fixedly connected to the right end of a first pipe (24). A third pipe (35) is provided in communication with the outer wall of the first pipe (24). The top end of the third pipe (35) extends to the inner wall of the crystallization device (31). A heat exchanger (34) is provided on the second pipe (33). A fourth pipe (36) is connected to the top surface of the reactor (21). A second circulation pump (361) is connected to the end of the fourth pipe (36) away from the reactor (21). A filter (362) is connected to the end of the second circulation pump (361) away from the fourth pipe (36) through a pipe. The filter (362) is on the main discharge line, i.e., the first pipe (24).

2. The continuous production apparatus for lithium hexafluorophosphate according to claim 1, characterized in that, The inner wall of the reactor (21) is fixedly connected to two square plates (25), and each of the two square plates (25) is provided with several outlets (26). The inner walls of the several outlets (26) are fixedly connected to heat conduction pipes (27). The top surface of the reactor (21) is connected to a feed pipe (23), and the bottom surface of the reactor (21) is connected to a first pipe (24).

3. The continuous production apparatus for lithium hexafluorophosphate according to claim 1, characterized in that, The micro-mixing mechanism includes several connecting rods (28) fixedly connected to the top and bottom of several heat-conducting pipes (27), and a baffle (29) is fixedly connected to one end of the several connecting rods (28) away from the heat-conducting pipes (27).

4. The continuous production apparatus for lithium hexafluorophosphate according to claim 3, characterized in that, A rotating rod (291) is rotatably connected between the two baffles (29), and a winding blade (292) is fixedly connected to the outer wall of the rotating rod (291).

5. A continuous production apparatus for lithium hexafluorophosphate according to claim 1, characterized in that, The stirring assembly includes a drive motor (37) fixedly connected to the top surface of the crystallization device (31). The output end of the drive motor (37) is fixedly connected to a rotating rod (38). The bottom end of the rotating rod (38) extends rotatably into the interior of the crystallization device (31). Several stirring blades (39) are fixedly connected to the outer wall of the rotating rod (38).

6. A continuous production apparatus for lithium hexafluorophosphate according to claim 1, characterized in that, The regulating component includes an air outlet (391) connected to the outer wall of the crystallization device (31). The bottom surface of the crystallization device (31) is fixedly connected to a discharge pipe (392). A ball valve (393) is slidably connected to the inner wall of the discharge pipe (392). The outer diameter of the ball valve (393) is the same as the inner diameter of the discharge pipe (392). An adjusting rod (394) is fixedly connected to the outer wall of the ball valve (393). The right end of the adjusting rod (394) extends rotatably to the outer wall of the discharge pipe (392).

7. A continuous production apparatus for lithium hexafluorophosphate according to claim 1, characterized in that, The filter (362) consists of an overlapping PTFE microfiltration membrane and a sheet graphene sponge, cut to the same size, and then rolled into a cylindrical shape, with the outer diameter of the cylindrical shape being smaller than the inner diameter of the filter (362).

8. A continuous production apparatus for lithium hexafluorophosphate according to claim 7, characterized in that, The thickness of the PTFE microfiltration membrane is 260-280 mm, and the thickness of the sheet graphene sponge is 10-15 mm. Its width is smaller than the internal length of the filter (362) housing.

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