Ternary precursor material preparation system

Abstract

This disclosure relates to a ternary material precursor preparation system. The system includes a cylindrical reaction apparatus with a filtration assembly. The filtration assembly includes a first set of filter tubes, comprising multiple filter tubes arranged radially. The multiple sets of first filter tubes are arranged at circumferential intervals. This system allows for simultaneous precursor co-precipitation and material concentration within the reaction apparatus, avoiding particle loss and the generation of substandard products from secondary growth, thus improving the quality of the ternary precursor material product.

Description

Technical Field

[0001] This disclosure relates to a ternary precursor material preparation system. Background Technology

[0002] With the rapid development of the battery materials field, ternary materials have become one of the most widely used cathode materials due to their advantages such as good cycle performance, high specific capacity, and high energy density. Currently, the mainstream method for preparing ternary precursors in industry is the co-precipitation method. This method uses nickel salt, cobalt salt, and manganese salt solutions as raw materials, sodium hydroxide as a precipitant, and ammonia as a complexing agent. All three are introduced into a reaction vessel for reaction, and the morphology and particle size of the product are controlled by adjusting the temperature, time, pH, stirring rate, and solid content. Once the particle size reaches the predetermined value, the reaction slurry is filtered, washed, and dried to obtain the ternary precursor.

[0003] Currently, most ternary precursor manufacturers collect the mother liquor from the overflow of the reactor into an intermediate tank during the synthesis reaction, then concentrate it in a concentration tank, and finally return the concentrated material to the reactor for crystal growth. This process has several drawbacks. First, some ternary crystal nuclei are squeezed together during transport in the pump pipes, damaging the precursor surface morphology or breaking the precursor spheres. Second, when these ternary crystal nuclei leave the initial reaction system and re-enter the reactor, they cause uneven growth, resulting in ternary precursor particles of inconsistent size. The particle size distribution of the ternary precursor material directly affects key performance characteristics such as battery life. Furthermore, in applications requiring increased filtrate flow, numerous filter cartridges are typically installed in the reactor. This not only makes the filter cartridges highly susceptible to damage during the reaction but also affects the flow field distribution within the reactor, ultimately impacting the quality of the final ternary precursor product. Summary of the Invention

[0004] The purpose of this disclosure is to provide a ternary precursor material preparation system to improve the product quality of the target product, the ternary material precursor.

[0005] To achieve the above objectives, this disclosure provides a ternary precursor material preparation system. The system includes a cylindrical reaction device, in which a filtration assembly is provided. The filtration assembly includes a first filter tube group, which includes multiple filter tubes arranged radially. The number of the first filter tube groups is multiple, and the multiple groups of the first filter tube groups are evenly spaced along the circumference.

[0006] Optionally, the number of the first filter tube group is 2 to 12 groups.

[0007] Optionally, in the plurality of filter tubes of the first filter tube group, the center distance between two adjacent filter tubes is 1 to 3 times the outer diameter of the filter tube; the ratio of the center distance between the filter tube near the axis of the reaction device and the filter tube near the inner wall of the reaction device to the inner diameter of the reaction device is 1:(4 to 16); the ratio of the distance between the filter tube near the inner wall of the reaction device and the inner wall of the reaction device to the outer diameter of the filter tube is (0.1 to 10):1; and the ratio of the distance between the filter tube near the axis of the reaction device and the axis of the reaction device to the inner diameter of the reaction device is 1:(1.5 to 6).

[0008] Optionally, at least one side of the first filter tube assembly is provided with a baffle, and the baffle is fixedly connected to the plurality of filter tubes.

[0009] Optionally, the filtration assembly further includes a second filter tube group, which includes a plurality of filter tubes arranged circumferentially; the distance between the center of each of the plurality of filter tubes in the second filter tube group and the axis of the reaction device is not less than the distance between the filter tube closest to the axis of the reaction device and the axis of the reaction device in the plurality of filter tubes in the first filter tube group.

[0010] Optionally, the number of the second filter tube groups is 1 to 24. When the number of the second filter tube groups is multiple, the multiple second filter tube groups are evenly spaced along the circumference.

[0011] Optionally, the filter tube is made of a porous material, which includes at least one of metal porous materials, ceramic porous materials and polymer porous materials, and the pore size of the porous material ranges from 0.01 to 50 μm.

[0012] Optionally, in the plurality of filter tubes, the pore size of the porous material is arranged in a gradient.

[0013] Optionally, the ratio of the length of the filter tube to the height of the cylinder of the reaction device is (0.1 to 1):1, and the outer diameter of the filter tube is 10 to 200 mm.

[0014] Optionally, the filtration assembly further includes a filtrate outlet and a backwashing line, wherein the filtrate outlet is connected to the backwashing line.

[0015] Optionally, the reaction device is provided with multiple pH detection elements evenly spaced along the axial direction, which are used to detect the pH of the reaction slurry at different liquid levels.

[0016] Optionally, the system also includes:

[0017] A secondary filtration device, connected to the reaction apparatus, is used to recover the solid products obtained from the reaction apparatus;

[0018] A pressure control device is used to control the pressure within the reaction apparatus.

[0019] Through the above technical solution, the ternary precursor material preparation system disclosed herein can simultaneously carry out precursor co-precipitation reaction and material concentration within the reaction device. The reaction mother liquor can be directly discharged outside the reaction device, avoiding the problem of material particle loss. The particles do not need to be concentrated and then refluxed for growth, thus avoiding the problem of producing unqualified products due to secondary growth. The product particles are more likely to obtain better microstructure and sphericity. By setting up radially arranged filter tube components, the filtration function can be satisfied while also optimizing the flow structure within the reaction device, minimizing the occupation of the reaction space and the impact on the flow field within the reaction device, thereby further improving the quality of the ternary precursor material product.

[0020] Other features and advantages of this disclosure will be described in detail in the following detailed description section. Attached Figure Description

[0021] The accompanying drawings are provided to further illustrate the present disclosure and form part of the specification. They are used together with the following detailed description to explain the present disclosure, but do not constitute a limitation thereof. In the drawings:

[0022] Figure 1 This is a schematic diagram of a specific embodiment of the ternary precursor material preparation system provided in this disclosure.

[0023] Figure 2 This is a cross-sectional structural schematic diagram of a specific embodiment of the filter component in the ternary precursor material preparation system provided in this disclosure.

[0024] Figure 3 These are SEM images of the ternary precursor materials prepared in Example 1 and Comparative Example 1, where (a) and (b) are the results of Example 1, and (c) and (d) are the results of Comparative Example 1.

[0025] Explanation of reference numerals in the attached figures

[0026] 1. Salt solution inlet 2. Alkali solution inlet

[0027] 3 Complexing agent inlet 4 Mixing assembly

[0028] 5. Filter assembly 501 First filter tube group

[0029] 502 Second filter assembly 6 backwash line

[0030] 7 Secondary filtration device 8 Heat exchanger

[0031] 9 pH detection element 10 Reaction apparatus Detailed Implementation

[0032] The specific embodiments of this disclosure will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit this disclosure.

[0033] This disclosure provides a ternary precursor material preparation system, with reference to... Figure 1 and Figure 2 As shown, the system includes a cylindrical reaction device 10, in which a filter assembly 5 is provided. The filter assembly 5 includes a first filter tube group 501, which includes a plurality of filter tubes arranged radially.

[0034] The ternary precursor material preparation system disclosed herein concentrates the reaction slurry through the built-in filter component 5 in the reaction device 10. The reaction mother liquor can be discharged from the reaction device 10, while the precursor particles remain in the reaction device 10 to continue growing until they reach the required particle size, at which point the reaction stops. This makes it easier to obtain better microstructure and sphericity, and also ensures that the prepared precursor particles have uniform particle size and controllable dimensions. This improves operational flexibility and enables simultaneous co-precipitation reaction, slurry concentration, and particle growth within the reaction device 10. It avoids the problem of material particle loss and eliminates the need for additional external concentration equipment, reducing the impact of slurry transfer on the final product quality. It also reduces equipment investment and simplifies production operations.

[0035] In this disclosure, the terms “radial,” “circumferential,” and “axial” are relative to the reaction apparatus.

[0036] According to this disclosure, the arrangement of the first filter tube group 501 is beneficial to reducing the number of filter tubes used, minimizing the space occupied within the reaction device 10 and the impact on the flow field. (Refer to...) Figure 2 As shown, the filter tubes in the first filter tube group 501 all extend axially, and multiple filter tubes are arranged radially, so that the extension direction (radial) of the first filter tube group 501 is perpendicular to the rotation direction (circumferential) of the slurry in the reaction device 10. This ensures that a filter cake layer is not easily formed on the surface of the filter tube, thereby increasing the filtration throughput. At the same time, it can avoid the "swirling" phenomenon of the fluid, thereby improving the mixing degree of the slurry and improving the quality of the ternary precursor material product.

[0037] To improve the concentration effect, the number of the first filter tube groups 501 is multiple, and the multiple groups of the first filter tube groups 501 are arranged at intervals along the circumference. In a specific embodiment of this disclosure, the number of the first filter tube groups 501 can be 2 to 12, preferably 2 to 6, and more preferably, the multiple groups of the first filter tube groups 501 are arranged at uniform intervals along the circumference. Figure 2 The first filter tube group 501 shown has 4 groups, and the central angle between two adjacent groups is 90°.

[0038] In the first filter tube group 501, multiple filter tubes are preferably arranged at intervals and have a certain distance from the inner wall and the axis of the reaction device 10, which can avoid affecting the stirring effect, material accumulation at the side wall, and affecting product quality. In a preferred embodiment of this disclosure, among the plurality of filter tubes in the first filter tube group, the center distance between two adjacent filter tubes can be 1 to 3 times the outer diameter of the filter tube, more preferably 1.1 to 2 times; the ratio of the center distance between the filter tube near the axis of the reaction device (i.e., the innermost filter tube) and the filter tube near the inner wall of the reaction device (i.e., the outermost filter tube) to the inner diameter of the reaction device can be 1:(4 to 16), more preferably 1:(8 to 13); the ratio of the distance between the filter tube near the inner wall of the reaction device (i.e., the outermost filter tube) and the inner wall of the reaction device to the outer diameter of the filter tube can be (0.1 to 10):1, more preferably (0.3 to 3):1; the ratio of the distance between the filter tube near the axis of the reaction device (i.e., the innermost filter tube) and the axis of the reaction device to the inner diameter of the reaction device is 1:(1.5 to 6), more preferably 1:(1.5 to 3). Within the aforementioned range, the impact on the agitator can be reduced while ensuring the filtration throughput, thereby optimizing the slurry flow within the reaction device 10.

[0039] The first filter tube assembly 501 may have a baffle on at least one side in the circumferential direction, and the baffle is fixedly connected to the plurality of filter tubes. The baffle is used to protect the first filter tube assembly 501 and prevent the filter tubes from being vibrated, loosened, or damaged by the impact of the reaction slurry.

[0040] According to this disclosure, the filter assembly 5 may further include a second filter tube group 502, which is also used to concentrate and enhance the reaction slurry, and can be selected and configured as needed. (Reference) Figure 2 The second filter tube assembly 502 includes a plurality of filter tubes arranged circumferentially, and the distance between the center of the plurality of filter tubes of the second filter tube assembly 502 and the axis of the reaction device 10 is (e.g., Figure 2As shown in the figure, d2) is not less than the distance between the filter tube near the axis of the reaction device 10 and the axis of the reaction device 10 among the plurality of filter tubes of the first filter tube group 501 (e.g., Figure 2 As shown in d1); the center distance between two adjacent filter tubes can be 1 to 3 times the outer diameter of the filter tube.

[0041] According to this disclosure, the number of the second filter tube group 502 can also be multiple. In one specific embodiment of this disclosure, the number of the second filter tube group 502 can be 1 to 24 groups. When the number of the second filter tube group is multiple, the multiple groups of the second filter tube group are arranged at uniform intervals along the circumference. Figure 2 The number of the second filter tube group 502 shown is 2, and the two groups of second filter tube groups 502 are arranged opposite to each other.

[0042] According to this disclosure, the filter tubes in the second filter tube group 502 can be made of the same material and have the same dimensions as the filter tubes in the first filter tube group 501. The number of filter tubes provided in the reaction device 10 (including the total number of filter tubes in the first filter tube group 501 and the second filter tube group 502) can be determined by parameters such as the filtrate volume, the effective filtration area of ​​the filter tubes, and the filtration flux. Specifically, the number of filter tubes in the second filter tube group 502 can be 2 to 1000, and the number of filter tubes in the first filter tube group 501 can be 2 to 200.

[0043] In one specific embodiment of this disclosure, the filter tube can be made of a porous material. Specifically, the porous material can include at least one of metallic porous materials, ceramic porous materials, and polymer porous materials, preferably a metallic porous material. Compared to other porous filter materials, metallic porous materials have better permeability, and the number of filter tubes required can be reduced for the same throughput. The metallic porous material also has good strength; for example, the hardness of the metallic porous material can be 45–95 HRB. The pore size range of the porous material can be 0.01–50 μm. The above pore size range refers to the filtration accuracy of the filter tube, which can be tested according to the GB / T 30176-2013 standard method. When the filter tube is within the above filtration accuracy range, it has good filtration quality. Further, the porous material can include a filter layer and a support layer. The pore size range of the filter layer can be 0.01–20 μm, and the pore size range of the support layer can be 0.01–50 μm.

[0044] In a preferred embodiment, the pore sizes of the porous material in the plurality of filter tubes are arranged in a gradient, that is, the plurality of filter tubes have a gradient of filtration precision. Further, the plurality of filter tubes can have two filtration precisions, with the ratio of filter tubes with a first filtration precision to filter tubes with a second filtration precision being 1:(1-3). For example, when the number of filter tubes is 12, the pore size of the porous material in 6 filter tubes can be 0.5 μm, and the pore size of the porous material in 6 filter tubes can be 1 μm. In other embodiments, the plurality of filter tubes can also have three filtration precisions. For example, when the number of filter tubes is 20, the pore size of the porous material in 4 filter tubes can be 0.5 μm, the pore size of the porous material in 8 filter tubes can be 1 μm, and the pore size of the porous material in 8 filter tubes can be 2 μm. The filter tubes, with their filtration precision set in a gradient, can be activated sequentially according to the reaction progress. In the initial stage of the reaction, the filter tubes with higher filtration precision (smaller pore size in the porous material) are activated first. As the ternary precursor particles continue to grow, the filter tubes with lower filtration precision (larger pore size in the porous material) are gradually activated. The activation timing of different filter tubes can be controlled by a program or manually. By setting filter tubes with different filtration precisions, filtration can be targeted according to different reaction stages, improving raw material utilization and reducing manufacturing investment.

[0045] According to this disclosure, the shape of the filter tube is not particularly limited; it can be a filter tube with a circular, square, rectangular, or other irregular cross-section, or a combination of multiple shapes. The ratio of the length of the filter tube to the height of the cylindrical body of the reaction device 10 can be (0.1 to 1):1, the outer diameter of the filter tube can be 10 to 200 mm, and the thickness can be 1 to 120 mm. Filter tubes within the above size range can meet strength requirements, reduce the possibility of material accumulation, and reduce the occupation of reaction space.

[0046] According to this disclosure, the filter assembly 5 may further include a clear liquid collection tube connected to the first filter tube group 501 and the second filter tube group 502 respectively, for collecting the clear liquid obtained after filtration. The location and specifications of the clear liquid collection tube are not particularly limited and can be conventional in the art.

[0047] According to this disclosure, the filter assembly 5 may further include a filtrate outlet and a backwashing pipeline 6. The filtrate outlet is connected to the backwashing pipeline 6, and the backwashing pipeline 6 is used to flush the filter assembly 5 to prevent material accumulation and blockage of the filter assembly.

[0048] According to this disclosure, the reaction apparatus 10 is provided with a plurality of pH detection elements 9 evenly spaced along the axial direction, which are used to detect the pH of the reaction slurry at different liquid levels. Preferably, the number of pH detection elements 9 is 2 to 20. The height of the uppermost pH detection element 9 can be 0.6 to 0.9 times the height of the cylinder of the reaction apparatus 10; the lowermost pH detection element 9 can be installed at the bottom of the reaction apparatus 10, up to a maximum of 0.3 times the height of the cylinder of the reaction apparatus 10. During the reaction, the measured values ​​of multiple pH detection elements 9 can be acquired simultaneously. When the measured values ​​of multiple pH detection elements 9 are not significantly different, it indicates that the mixing degree of the reaction slurry in the reaction apparatus 10 is good. Maintaining the uniformity and stability of the pH within the reaction apparatus 10 is crucial for product quality. By setting multiple pH detection elements 9 at different heights, the dispersion of the reaction raw materials within the reaction apparatus 10 can be obtained relatively accurately through error analysis, and parameters such as rotation speed and raw material feed flow rate can be adjusted in a timely manner.

[0049] According to this disclosure, the reaction apparatus 10 may further include a stirring assembly 4, which is arranged along the central axis of the reaction apparatus 10. The stirring assembly 4 may include one or more sets of stirring blades evenly spaced along the axial direction; specifically, there may be 2 to 3 sets of stirring blades. The stirring blades may be conventional in the art, such as propeller-type stirring blades, turbine-type stirring blades, or combinations thereof.

[0050] According to this disclosure, the reaction apparatus 10 can be a reactor commonly used in the art, such as a batch reactor. The reaction apparatus 10 may also be equipped with a flow guide tube for guiding the reaction slurry. The reaction apparatus 10 may also be externally equipped with a heat exchange component 8, such as a jacket or coil.

[0051] This disclosure applies to the preparation of various ternary material precursors known in the art, such as nickel-cobalt-manganese precursors and nickel-cobalt-aluminum precursors. The raw material mixture is a mixture of common raw materials used in the preparation of ternary material precursors, and this disclosure does not impose any special limitations. For example, the raw material mixture may include a salt solution, an alkali solution, and a complexing agent. In one specific embodiment of this disclosure, the reaction apparatus 10 further includes a salt solution inlet 1, an alkali solution inlet 2, and a complexing agent inlet 3, for adding the salt solution, alkali solution, and complexing agent, respectively. The salt solution inlet 1, the alkali solution inlet 2, and the complexing agent inlet 3 may be further equipped with a rapid dispersion device or distributor to improve the dispersion degree of the raw materials. The rapid dispersion device or distributor may be a branch pipe type, a pressure nozzle type, a lotus-shaped type, a rotary atomizing wheel, or a combination thereof. The salt solution, alkali solution, and complexing agent can be of conventional types in the art. For example, the salt solution can be a mixture of soluble nickel salt, soluble cobalt salt, soluble manganese salt, and water, or a combination of soluble nickel salt, soluble cobalt salt, and soluble aluminum salt solutions, wherein the total molar concentration of metal ions can be 0.5–5.0 mol / L; the alkali solution can be an aqueous solution of sodium hydroxide, wherein OH... - The molar concentration can be 1.0–20.0 mol / L; the complexing agent can be ammonia, wherein the concentration of NH3 is 1–30% by weight. Furthermore, the reaction device 10 also has a slurry outlet for collecting the ternary material precursor product.

[0052] According to this disclosure, the system may further include: a secondary filtration device 7, connected to the reaction device 10, for recovering a small amount of solid product obtained from the reaction device 10 (i.e., contained in the clarified liquid of the filtration assembly 5); and a pressure control device ( Figure 1 (Not shown in the image) This pressure control device is used to control the pressure within the reaction apparatus 10, particularly the pressure on both sides of the filter assembly 5. The secondary filtration device 7 can be a common filtration device in the art, such as a filter tube, filter cloth, or filter element. The pressure control device maintains a slightly positive pressure within the reaction apparatus 10, preventing ammonia loss due to vacuum or suction filtration at high temperatures. A suitable ammonia concentration is crucial for product morphology and also reduces additional ammonia consumption. Simultaneously, the pressure control device provides additional filtration power to the filter assembly 5. When the effluent flow rate decreases, the pressure within the reaction apparatus 10 can be appropriately increased to promote the discharge of clarified liquid. The pressure control device can be a common pressure-regulating device in the art, such as a pressure pump or nitrogen pressurization device.

[0053] The method for preparing ternary precursor materials using the system provided in this disclosure can be as follows: the reaction raw materials, salt solution, complexing agent, and alkali solution are fed into the reactor near the stirring assembly through the feed pipe. Under certain reaction conditions (e.g., reaction temperature 20-100℃, reaction pressure 0-3.0MPa), a co-precipitation reaction occurs. The resulting slurry is concentrated by the filtration assembly. The concentrated slurry is discharged continuously or intermittently from the bottom outlet of the reactor to separate the ternary precursor materials. The filtered clear liquid is discharged from the reactor after optional secondary filtration through the filtration assembly's collection pipe. The pressure difference between the inside and outside of the filtration assembly is adjusted by a pressure control device. During the filtration and concentration process, the liquid level in the reactor is kept stable. The total flow rate of the raw material liquid entering the reactor at this stage is equal to the flow rate of the filtrate.

[0054] The ternary precursor material preparation system disclosed herein is simple in structure, easy to operate, and has the advantages of low investment and quick results. It can be widely used in the process of material concentration in chemical reactions, and is particularly suitable for the simultaneous synthesis and concentration of ternary precursor materials. The ternary material precursors prepared using the system disclosed herein have good microstructure and sphericity, and the particle size Span value of the ternary precursor materials is not greater than 1.

[0055] The following examples further illustrate this disclosure, but do not constitute a limitation thereof.

[0056] In the embodiments, the morphology of the ternary material precursor was detected by SEM, the particle size was analyzed by a laser particle size analyzer, and the suspended solids concentration was detected by a turbidimeter.

[0057] Example 1

[0058] Adopting such Figure 1 The system shown has a reactor volume of 800L, an inner diameter of 800mm, and a height of 1600mm. Four sets of first filter tubes are installed inside the reactor. Each set includes three filter tubes, each 1000mm long, with an inner diameter of 20mm and an outer diameter of 30mm. The center-to-center distance between adjacent filter tubes is 35mm. The outermost filter tube is 10mm from the inner wall of the reactor, the innermost filter tube is 290mm from the reactor axis, and the center-to-center distance between the outermost and innermost filter tubes is 70mm. A total of 12 filter tubes are used, all made of sintered porous metal material with a hardness of 50HRB. Six filter tubes have a pore size of 0.5μm, and six have a pore size of 1μm. A baffle is installed on the liquid-flow-facing side of each first filter tube set. The outlet of the first filter tube set is connected to a backwash line and a secondary filtration device. The reactor is equipped with two pH detection elements, with heights of 50mm and 600mm respectively on the tangent of the cylinder, and two sets of stirring paddles are set along the axis.

[0059] Deionized water was used as the initial reaction solution and heated to 60°C. The ammonia concentration and pH of the initial solution were adjusted to 3.5 g / L and 10.5, respectively. A prepared solution of nickel sulfate (2.7 mol / L total metal ion concentration), cobalt sulfate, manganese sulfate, 20% (w / w) NaOH solution, and 18.2% (w / w) ammonia solution were continuously added to the reactor, maintaining a pH of 10.85. The reaction was carried out at 60°C and 0.03 MPa. When the reaction slurry filled the reactor, it was concentrated using the first filter tube group. The 0.5 μm filter tube was opened first, and the 1 μm filter tube was opened after 24 hours of reaction. The reaction slurry was collected after a cumulative reaction time of 48 hours. A slight positive pressure was maintained throughout the reaction. When the filtration throughput needed to be increased, nitrogen gas was introduced to increase the pressure inside the reactor, maintaining a pressure difference of 0.1 MPa across the first filter tube group to promote the discharge of the filtered liquid.

[0060] The collected reaction slurry was separated to obtain nickel-cobalt-manganese ternary precursor materials, as shown in the SEM images. Figure 3 It has good sphericity, the primary crystals are plate-shaped with good morphology and dense arrangement, and there are basically no small particles. The calculated particle size Span value is 0.85. The concentration of suspended solids in the filtrate collected 24 hours before the reaction was 10 g / mL.

[0061] Example 2

[0062] The nickel-cobalt-manganese ternary precursor material was prepared according to the method of Example 1, with the difference being that four sets of first filter tubes were installed in the reactor. Each set included three filter tubes, each 1000 mm long, with an inner diameter of 20 mm and an outer diameter of 30 mm. The center-to-center distance between adjacent filter tubes was 65 mm. The outermost filter tube was 5 mm from the inner wall of the reactor, the innermost filter tube was 235 mm from the reactor axis, and the center-to-center distance between the outermost and innermost filter tubes was 160 mm. A total of 12 filter tubes were used, all made of a porous metal material with a hardness of 50 HRB. Six of the filter tubes had a pore size of 0.5 μm, and the other six had a pore size of 1 μm.

[0063] The collected reaction slurry was separated to obtain a nickel-cobalt-manganese ternary precursor material with good sphericity, primary grains that were plate-like, well-shaped and densely arranged, with virtually no small particles. The calculated particle size Span value was 0.88, and the suspended solids concentration of the filtrate collected 24 hours before the reaction was 11 g / mL.

[0064] Example 3

[0065] The nickel-cobalt-manganese ternary precursor material was prepared according to the method in Example 1, except that the filter tubes were all made of a porous metal material with a hardness of 50 HRB and a pore size of 1 μm.

[0066] The collected reaction slurry was separated to obtain a nickel-cobalt-manganese ternary precursor material with good sphericity, primary grains that were plate-like, well-shaped and densely arranged, with virtually no small particles. The calculated particle size Span value was 0.86, and the suspended solids concentration of the filtrate collected 24 hours before the reaction was 32 g / mL.

[0067] Example 4

[0068] The nickel-cobalt-manganese ternary precursor material was prepared according to the method of Example 1, with the difference being that four sets of first filter tube groups were set in the reactor, each set including 4 filter tubes, each filter tube being 1000mm long, 10mm inner diameter, and 20mm outer diameter, with a center-to-center distance of 25mm between adjacent filter tubes, the outermost filter tube being 10mm from the inner wall of the reactor, the innermost filter tube being 295mm from the center of the reactor, and the center-to-center distance between the outermost and innermost filter tubes being 65mm; two sets of second filter tube groups were added in the reactor, each set including 3 filter tubes, each filter tube being 800mm long, 10mm inner diameter, and 20mm outer diameter, with a center-to-center distance of 25mm between adjacent filter tubes, and the center of the filter tube being 350mm from the center of the reactor. There are a total of 22 filter tubes, all made of porous metal material with a hardness of 50 HRB. Among them, the pore size of the porous metal material of 11 filter tubes is 0.5 μm, and the pore size of the porous metal material of 11 filter tubes is 1 μm.

[0069] The collected reaction slurry was separated to obtain a nickel-cobalt-manganese ternary precursor material with good sphericity, primary grains that were plate-like, well-shaped and densely arranged, with virtually no small particles. The calculated particle size span value was 0.86, and the suspended solids concentration of the filtrate collected 24 hours before the reaction was 9.8 g / mL.

[0070] Comparative Example 1

[0071] The nickel-cobalt-manganese ternary precursor material was prepared according to the method of Example 1, except that the first filter tube group was removed and replaced with four baffles with a width of 100 mm and a length of 1400 mm in the same position, and an external concentrator was used.

[0072] The collected reaction slurry was separated to obtain nickel-cobalt-manganese ternary precursor materials, as shown in the SEM images. Figure 3 Its particle size is uneven, the primary grains are needle-shaped, and the calculated particle size span value is 1.02.

[0073] As can be seen from the comparison results of the examples and comparative examples, the ternary precursor material prepared by the system of this disclosure has better microstructure and sphericity, and a lower particle size Span value, which indicates higher particle uniformity.

[0074] The preferred embodiments of this disclosure have been described in detail above with reference to the accompanying drawings. However, this disclosure is not limited to the specific details of the above embodiments. Within the scope of the technical concept of this disclosure, various simple modifications can be made to the technical solutions of this disclosure, and these simple modifications all fall within the protection scope of this disclosure.

[0075] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, this disclosure will not describe the various possible combinations separately.

[0076] Furthermore, various different embodiments of this disclosure can be combined in any way, as long as they do not violate the spirit of this disclosure, they should also be regarded as the content disclosed in this disclosure.

Claims

1. A ternary precursor material preparation system, characterized in that, The system includes a cylindrical reaction device, in which a filtration assembly is provided. The filtration assembly includes a first filter tube group, which includes multiple filter tubes arranged radially. The number of first filter tube groups is multiple, and the multiple first filter tube groups are arranged at intervals along the circumference. In the first filter tube group, the center distance between two adjacent filter tubes is 1 to 3 times the outer diameter of the filter tube. The ratio of the center distance between the filter tube near the axis of the reaction device and the filter tube near the inner wall of the reaction device to the inner diameter of the reaction device is 1:(4 to 16). The ratio of the distance between the filter tube near the inner wall of the reaction device and the inner wall of the reaction device to the outer diameter of the filter tube is (0.1 to 10):

1. The ratio of the distance between the filter tube near the axis of the reaction device and the axis of the reaction device to the inner diameter of the reaction device is 1:(1.5 to 6). The filtration assembly further includes a second filter tube group, which includes a plurality of filter tubes arranged circumferentially; the distance between the center of each of the plurality of filter tubes in the second filter tube group and the axis of the reaction device is not less than the distance between the filter tube closest to the axis of the reaction device and the axis of the reaction device in the plurality of filter tubes in the first filter tube group. The filter tube is made of a porous material, and the pore sizes of the porous material are arranged in a gradient among the multiple filter tubes.

2. The system according to claim 1, wherein, The number of the first filter tube group is 2 to 12.

3. The system according to claim 1, wherein, The first filter tube assembly has a baffle on at least one side, and the baffle is fixedly connected to the plurality of filter tubes.

4. The system according to claim 1, wherein, The number of the second filter tube group is 1 to 24. When the number of the second filter tube group is multiple, the multiple second filter tube groups are evenly spaced along the circumference.

5. The system according to claim 1, wherein, The porous material includes at least one of metallic porous materials, ceramic porous materials, and polymer porous materials, and the pore size range of the porous material is 0.01~50 μm.

6. The system according to claim 1, wherein, The ratio of the length of the filter tube to the height of the cylinder of the reaction device is (0.1~1):1, and the outer diameter of the filter tube is 10~200 mm.

7. The system according to claim 1, wherein, The filtration assembly also includes a filtrate outlet and a backwashing pipeline, wherein the filtrate outlet is connected to the backwashing pipeline.

8. The system according to claim 1, wherein, The reaction device is equipped with multiple pH detection elements evenly spaced along the axial direction, which are used to detect the pH of the reaction slurry at different liquid levels.

9. The system according to claim 1, wherein, The system also includes: A secondary filtration device, connected to the reaction apparatus, is used to recover the solid products obtained from the reaction apparatus; A pressure control device is used to control the pressure within the reaction apparatus.

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