Apparatus and method for producing a positive electrode active material precursor
The described apparatus and method for producing cathode active material precursors in a single reactor address productivity and space utilization issues, achieving efficient and cost-effective production with uniform particle sizes.
Patent Information
- Application Number
- JP2025539378
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-02-21
- Filing Date
- 2024-02-21
- Publication Date
- 2026-01-27
AI Technical Summary
Existing methods for producing cathode active material precursors face challenges with low productivity, complex system configurations, poor space utilization efficiency, and variations in particle size and uniformity due to the use of continuous and batch reactors.
A manufacturing apparatus and method that involves a reactor with a solution discharge unit, including a methyl filter and nitrogen purge units, allowing continuous concentration of the precursor in a single reactor, thereby simplifying the device configuration and improving space utilization.
This approach enhances productivity and reduces investment costs while ensuring high-quality cathode active material precursor production with improved particle size uniformity and space efficiency.
Smart Images

Figure 2026502996000001_ABST
Abstract
Description
[Technical Field]
[0001] The present embodiment relates to an apparatus and method for producing a positive electrode active material precursor, and more specifically to an apparatus and method for producing a positive electrode active material precursor while continuously concentrating the precursor in one reactor. [Background technology]
[0002] In recent years, with the explosive demand for electric vehicles and the demand for increased driving distances, secondary batteries with high capacity and high energy density have been actively developed worldwide to meet this demand.
[0003] Lithium composite transition metal oxides containing transition metals such as nickel, cobalt, manganese, and aluminum are widely used as positive electrode active materials for lithium secondary batteries.
[0004] The lithium composite transition metal oxide is prepared by mixing a cathode active material precursor in the form of a hydroxide or oxyhydroxide containing a transition metal with a lithium source material and then calcining the mixture. Specifically, the cathode active material can be prepared by preparing a cathode active material precursor using a continuous reactor (CSTR) and then calcining it with the lithium source material to produce the cathode active material. Alternatively, the cathode active material can be prepared by preparing a cathode active material precursor using a batch reactor and then calcining it with the lithium source material to produce the cathode active material. A continuous reactor (CSTR) is a method in which raw materials are introduced and co-precipitated while simultaneously discharging the precursor particles. A batch reactor is a method in which a predetermined amount of raw materials are introduced into the reactor over a certain period of time, reacted, and then the precursor is discharged after the reaction is complete.
[0005] In the batch method, once the reaction is completed, the reactor is cleaned and the initial conditions are restored, and the reaction for producing the positive electrode active material is repeated, resulting in low productivity.
[0006] A cathode active material precursor produced using a continuous reactor (CSTR) can improve the productivity of the cathode active material precursor by simultaneously introducing raw materials, co-precipitating the raw materials, and discharging the precursor. The continuous reactor (CSTR) has a configuration in which raw materials are introduced and products are discharged simultaneously, resulting in a complex system configuration, increased system manufacturing costs, and poor space utilization efficiency. Furthermore, there may be variations in the residence time and reaction time of the cathode active material precursor produced in the reactor, resulting in poor particle size and particle size uniformity.
[0007] Therefore, there is a need to develop a manufacturing apparatus and method that can improve productivity, increase the space utilization efficiency of facilities, and produce high-quality cathode active material precursors. Summary of the Invention [Problem to be solved by the invention]
[0008] An object of one embodiment of the present invention is to provide a manufacturing apparatus and a manufacturing method capable of manufacturing a cathode active material precursor while continuously concentrating the precursor in a single reactor. [Means for solving the problem]
[0009] An apparatus for manufacturing a positive electrode active material precursor according to one embodiment of the present invention may include a reactor 100 for receiving and reacting reactants therein; a supply unit 200 for supplying the reactants into the reactor 100; and a solution discharge unit 300 for continuously discharging the solution from the precursor and solution produced by the reaction of the reactants inside the reactor 100 to the outside of the reactor 100. The solution discharge unit 300 may include a solution discharge pipe 310 communicating with a sidewall 110 of the reactor 100 and extending to the outside; a methyl filter unit 320 located in the solution discharge pipe 310 for separating the positive electrode active material precursor from the solution; a nitrogen purge unit 330 for purging nitrogen into the methyl filter unit 320; a shutoff unit 340 located at a rear end of the nitrogen purge unit 330; and a pressure reduction pump 350 located at a rear end of the shutoff unit 340. The methyl filter unit 320 may be located at one end of the solution discharge pipe 310 adjacent to the reactor 100.
[0010] The nitrogen purge unit 330 may include a first nitrogen purge unit 331 and a second nitrogen purge unit 332 located on both sides of the methyl filter unit 320 in the flow direction of the solution in the solution discharge pipe 310 .
[0011] The first nitrogen purge unit 331 may continuously inject nitrogen gas onto one side of the methyl filter unit 320 facing the reactor 100, and the nitrogen gas injection rate of the first nitrogen purge unit 331 may be in the range of 50 LPM to 100 LPM.
[0012] When the reactants contained in the reactor 100 exceed the highest liquid level (A1) of the reactor 100, the second nitrogen purge unit 332 may inject nitrogen gas onto the other side of the methyl filter unit 320 facing the reactor 100 to desorb precursors attached to the methyl filter unit 320, and the nitrogen gas injection speed of the second nitrogen purge unit 332 may be in the range of 250 LPM to 500 LPM.
[0013] Before the second nitrogen purge unit 332 injects nitrogen gas, the shutoff unit 340 can be turned off first.
[0014] The highest liquid level (A1) of the reactor 100 may be located at a position higher than the portion where the side wall 110 of the reactor 100 and the solution discharge pipe 310 are connected to each other, and may be located at a position of 1 / 10 or less from the top of the reactor 100. There is no particular limitation as long as the reactants do not rise and affect the reaction in the reactor 100.
[0015] The side wall 110 of the reactor 100 may be connected to communicate with the solution discharge pipe 310 at a position of at least two-fifths of the top of the entire height of the side wall 110.
[0016] The methyl filter unit 320 is fixed to the solution discharge pipe 310 by a detachable and attachable fixing member, and is replaceable.
[0017] The methyl filter unit 320 may be formed by stacking methyl filters having pore sizes ranging from 0.2 μm to 0.8 μm.
[0018] The system may include a control unit 500 for controlling the operations of the supply unit 200, the nitrogen purge unit 330, the shutoff unit 340 and the decompression pump 350.
[0019] When the control unit 500 stops the operation of the decompression pump 350, the shutoff unit 340 may be turned off.
[0020] A method for manufacturing a cathode active material precursor according to another embodiment of the present invention may include the steps of continuously feeding raw materials into a reactor, stirring and reacting them to form reactants; discharging the separated solution in the reactor to the outside of the reactor through a methyl filter unit located in a solution discharge pipe connected to a sidewall of the reactor; and purging nitrogen into the methyl filter unit when the reactants in the reactor reach a maximum liquid level in the reactor. The nitrogen purging step involves injecting nitrogen into the solution discharge pipe, and the injected nitrogen may flow from the inside of the solution discharge pipe toward the inside of the reactor.
[0021] The nitrogen purging step may be performed by closing a blocking unit located at the rear end of the solution discharge pipe and then spraying the nitrogen at a spray rate ranging from 250 LPM to 500 LPM.
[0022] In the nitrogen purging step, before closing the shutoff unit, the operation of the decompression pump located at the rear end of the shutoff unit can be stopped first.
[0023] In the solution discharging step, when the reactants in the reactor reach or exceed the lowest point of a connecting portion of a solution discharge pipe connected to the reactor and a side wall of the reactor, a pressure reducing pump located in the solution discharge pipe may be operated.
[0024] In the solution discharging step, nitrogen gas may be continuously sprayed onto one side of the methyl filter unit facing the reactor, and the nitrogen gas may be sprayed in the range of 50 LPM to 100 LPM. [Effects of the Invention]
[0025] According to one embodiment of the present invention, a cathode active material precursor can be produced while being continuously concentrated in one reactor, which has the advantage of reducing investment costs due to a simplified device configuration. Furthermore, there is an advantage that the device configuration is simplified and space utilization efficiency is improved. [Brief explanation of the drawings]
[0026] [Figure 1] 1 is a diagram schematically illustrating the configuration of an apparatus for manufacturing a positive electrode active material precursor according to an embodiment of the present invention. [Figure 2] 1 is a schematic view illustrating a methyl filter unit located inside a solution discharge pipe according to an embodiment of the present invention. [Figure 3] FIG. 10 is a schematic diagram illustrating a process of injecting nitrogen gas by operating a nitrogen purge unit according to an embodiment of the present invention. [Figure 4] FIG. 2 is a diagram schematically illustrating the configuration of a manufacturing apparatus for a positive electrode active material precursor, including a control unit. DETAILED DESCRIPTION OF THE INVENTION
[0027] In describing the present invention, terms such as "first," "second," and "third" are used to describe various parts, components, regions, layers, and / or sections, but are not limited thereto. These terms are used only to distinguish one part, component, region, layer, or section from another part, component, region, layer, or section. Thus, a first part, component, region, layer, or section described below can be referred to as a second part, component, region, layer, or section without departing from the scope of the present invention.
[0028] The terminology used herein is for the purpose of referring to particular embodiments and is not intended to limit the invention. As used herein, the singular forms "a," "an," and "the" include the plural forms unless the context clearly dictates otherwise. As used herein, the meaning of "comprising" is intended to embody certain properties, regions, areas, integers, steps, operations, elements, and / or components, and does not exclude the presence or addition of other properties, regions, areas, integers, steps, operations, elements, and / or components.
[0029] Unless otherwise defined, all terms, including technical and scientific terms, used herein have the same meaning as commonly understood by a person of ordinary skill in the art to which the present invention pertains. Terms defined in commonly used dictionaries are additionally interpreted to have a meaning consistent with the relevant technical literature and the presently disclosed content, and are not interpreted in an ideal or very formal sense unless defined.
[0030] In the drawings, the size of each component or specific parts constituting the component may be exaggerated, omitted, or illustrated schematically for convenience and clarity of explanation. Therefore, the size of each component may not completely reflect the actual size. If it is determined that a detailed description of the related notification function or configuration may unnecessarily obscure the gist of the present invention, such description will be omitted. [Example]
[0031] The following examples of the present invention are described in detail, but are given by way of example only and are not intended to limit the scope of the present invention, which is defined only by the scope of the claims that follow.
[0032] FIG. 1 is a schematic diagram illustrating the configuration of an apparatus for manufacturing a cathode active material precursor according to an embodiment of the present invention, and FIG. 2 is a schematic diagram illustrating a methyl filter unit located inside a solution discharge pipe according to an embodiment of the present invention.
[0033] Hereinafter, an apparatus for producing a positive electrode active material precursor according to one embodiment of the present invention will be specifically described with reference to FIGS.
[0034] An apparatus for manufacturing a cathode active material precursor according to an embodiment of the present invention may include a reactor 100 for receiving and reacting reactants therein; a supply unit 200 for supplying the reactants into the reactor 100; and a solution discharge unit 300 for continuously discharging the solution from among the precursor and solution produced by the reaction of the reactants in the reactor 100 to the outside of the reactor 100.
[0035] The reactor 100 may have a shape that forms a space inside to accommodate necessary components such as reactants and agitators, and specifically may include a bottom (not shown), a sidewall 110 that extends upward from the edge of the bottom and forms a container together with the bottom, and an upper cover 120 that faces the bottom (not shown) and prevents reactants inside the reactor 100 from being released to the outside. The bottom and sidewall 110 may be welded together, and the upper cover 120 may cover the upper end of the sidewall 110 using an additional fixing member.
[0036] An agitator 130 for mixing reactants introduced into the reactor 100 may be located at the center of the reactor 100. The agitator 130 may include an agitator shaft 131 and an agitator blade 132. The agitator 130 may rotate by the operation of a driver (not shown) to agitate the reactants contained in the reactor 100. The driver (not shown) is electrically connected to a controller 500 (described below) and may start or stop its operation and adjust its rotation speed by the controller 500. It is apparent that one or more agitator blades 132 may be provided, and multiple agitator blades 132 may be arranged at different heights depending on the size and needs of the reactor.
[0037] Meanwhile, a level gauge (not shown) capable of measuring a minimum liquid level (A0) and a maximum liquid level (A1) from bottom to top of the reactor 100 may be disposed in the reactor 100. The minimum liquid level (A0) is a criterion for the minimum amount of reactants to be introduced to start a reaction for producing a cathode active material precursor, and the maximum liquid level (A1) is a criterion for whether or not to operate the second nitrogen purge unit 332, which will be described in more detail in the description of the solution discharge unit 300, which will be described later.
[0038] In addition, a pH sensor unit 400 is provided inside the reactor 100 to adjust the reaction conditions.
[0039] The supply unit 200 may be located around the agitator 130. While the first and second raw material supply units 210 and 220 are shown separately in the drawings, this is for convenience of explanation; materials may be supplied through a single supply unit, or additional supply units may be located to supply different materials. Meanwhile, the reactor 100 may further include a nitrogen supply unit 230 for removing dissolved oxygen from reactants introduced into the reactor 100. Each supply unit 200 may control the start, stop, and supply rate of each reactant through a control unit 500, which will be described later. The relative positions of each supply unit may be adjusted as needed.
[0040] The solution discharge unit 300 may include a solution discharge pipe 310 communicating with the sidewall 110 of the reactor 100 and extending to the outside; a methyl filter unit 320 located in the solution discharge pipe 310 and separating the positive electrode active material precursor from the solution; a nitrogen purge unit 330 purging nitrogen into the methyl filter unit 320; a shutoff unit 340 located behind the nitrogen purge unit 330; and a pressure reduction pump 350 located behind the shutoff unit 340.
[0041] In addition, in the description of the present invention, the terms "front end / front" and "rear end / rear" may be distinguished based on the flow direction of the solution discharged to the outside from the reactor.
[0042] The solution discharge pipe 310 may be in the form of a pipe, and is not particularly limited as long as it can smoothly discharge the solution to the outside of the reactor 100 .
[0043] The solution discharge pipe 310 may be configured to penetrate the side wall 110 of the reactor 100 so that the internal space of the reactor 100 and the internal space of the solution discharge pipe 310 are in communication with each other.
[0044] The solution discharge pipe 310 may include a methyl filter unit 320 positioned across the entire cross section of the solution discharge pipe 310, which is connected to the sidewall 110 of the reactor 100. The methyl filter unit 320 may be configured by stacking a plurality of methyl filters, and the pore size of the methyl filters may be 0.1 μm to 1.0 μm, specifically 0.2 μm to 0.8 μm, and more specifically 0.4 μm to 0.6 μm. When the pore size of the methyl filter is within this range, it is advantageous for smoothly discharging the solution outside the reactor while preventing the loss of the prepared cathode active material precursor to the outside.
[0045] The methyl filter unit 320 may be fixed to the solution discharge pipe 310 by a detachable and attachable fixing member. Furthermore, when a methyl filter unit 320 needs to be replaced, the fixing member can be detached and replaced with a new methyl filter unit 320. The fixing member may include fixing holes located in the methyl filter unit 320 and the solution discharge pipe 310, respectively, and a member that fits into the fixing holes, or may be a locking fixing member. The fixing member is not particularly limited as long as it can fix the methyl filter unit 320 to the solution discharge pipe 310, discharge only the solution within the reactor 100 to the outside through the solution discharge pipe 310, and allow the positive electrode active material precursor to remain inside the reactor 100.
[0046] Meanwhile, the methyl filter unit 320 may be detachably fixed to the sidewall 110 of the reactor 100. Specifically, the methyl filter unit 320 may be positioned to cover the entire connecting portion between the reactor 100 and the solution discharge pipe 310. This is advantageous for separating the solution in the reactor 100 and discharging it to the outside through the solution discharge pipe 310.
[0047] Although not shown in the drawings, a level gauge may be further disposed at the lowest point of the portion where the solution discharge pipe 310 is connected to the side wall 110 of the reactor 100. The level gauge may be electrically connected to the control unit 500, which will be described later. When the height of the reactants charged into the reactor 100 reaches the lowest point, the control unit 500 may control and operate the pressure reducing pump 350.
[0048] The nitrogen purge unit 330 may prevent the positive electrode active material precursor from adhering to the methyl filter unit 320 or may function to remove the positive electrode active material precursor adhering to the methyl filter unit 320. Specifically, the nitrogen purge unit 330 may include a first nitrogen purge unit 331 and a second nitrogen purge unit 332, which are respectively located on both sides of the methyl filter unit 320 in the flow direction of the solution in the solution discharge pipe 310.
[0049] Referring to FIG. 3(a), which is a schematic diagram illustrating a process of injecting nitrogen gas by operating first nitrogen purge unit 331, first nitrogen purge unit 331 continuously injects nitrogen gas onto one side of methyl filter unit 320 facing reactor 100, dispersing the positive electrode active material precursor and preventing it from flowing into solution discharge pipe 310 along with the solution or adhering to methyl filter unit 320. The nitrogen gas injection rate of first nitrogen purge unit 331 may be in the range of 50 LPM to 100 LPM. When the nitrogen gas injection rate is within this range, it is advantageous in that it effectively disperses the positive electrode active material precursor without affecting the reaction of the reactants in reactor 100, thereby preventing or inhibiting its adhesion to methyl filter unit 320.
[0050] At this time, the blocking unit 340 (described later) may be maintained in an open state, and the decompression pump 350 (described later) may be in an operating state.
[0051] 1 shows the first nitrogen purge unit 331 penetrating the upper cover 120 of the reactor 100 and positioned above the portion that communicates with the sidewall 110 of the reactor 100 and the solution discharge pipe 310. However, if necessary, the first nitrogen purge unit 331 may be positioned in front of the methyl filter unit 320 and penetrating the solution discharge pipe 310. Nitrogen may also be injected directly into the methyl filter unit 320. By injecting nitrogen gas through the first nitrogen purge unit 331, it is possible to prevent or inhibit the adhesion of the positive electrode active material precursor in the reactor 100 to the methyl filter unit 320.
[0052] Also, although the first nitrogen purge unit 331 is shown as being positioned vertically in FIG. 1, it may be positioned at an angle.
[0053] In addition, the nitrogen gas outlet at the end of first nitrogen purge unit 331 may include a plurality of branch pipes, specifically, branch pipes positioned opposite each other, which is advantageous for dispersing the positive electrode active material precursor contained in the solution flowing into solution discharge pipe 310 and preventing the positive electrode active material precursor from adhering to methyl filter unit 320.
[0054] The second nitrogen purge unit 332 may be positioned to penetrate the solution discharge pipe 310, specifically, between the methyl filter unit 320 and the blocking unit 340 described later, and may inject nitrogen gas into the solution discharge pipe 310.
[0055] The second nitrogen purge unit 332 may inject nitrogen gas onto the other side of one side of the methyl filter unit 320 facing the reactor 100. Specifically, when the reactants contained within the reactor 100 exceed the maximum liquid level (A1) of the reactor 100, nitrogen gas may be injected onto the other side of the one side of the methyl filter unit 320 facing the reactor 100 to desorb the precursors attached to the methyl filter unit 320. When the solution within the reactor 100 is discharged to the outside through the solution discharge pipe 310, the cathode active material precursor produced within the reactor 100 may adhere to the methyl filter unit 320. As the amount of the cathode active material precursor attached increases, the solution discharge rate decreases, and the amount of reactants within the reactor 100 increases. When the reactants within the reactor 100 increase and reach the maximum liquid level (A1) of the reactor, the shutoff unit 340 (described below) is closed and the second nitrogen purge unit 332 is operated to inject nitrogen gas.
[0056] 3(b), which is a schematic diagram of a process of operating second nitrogen purge unit 332 to inject nitrogen gas, when the reactants in reactor 100 increase and reach the reactor's highest liquid level (A1), operation of pressure reducing pump 350 (described below) is stopped, shutoff unit 340 is turned off, and then second nitrogen purge unit 332 is operated to inject nitrogen gas. The nitrogen gas injected from second nitrogen purge unit 332 can desorb the cathode active material precursor attached to methyl filter unit 320 as it moves inside reactor 100.
[0057] In this case, the nitrogen gas injection rate of the second nitrogen purge unit 332 may be in the range of 100 LPM to 1000 LPM, specifically, in the range of 250 LPM to 500 LPM, and the injection time may be in the range of 0.1 to 1 second. When the nitrogen gas injection rate and injection time are in this range, it is advantageous in that the positive electrode active material precursor attached to the methyl filter unit 320 can be effectively desorbed while minimizing the influence on the positive electrode active material precursor manufacturing process.
[0058] The reactor 100 and the solution discharge pipe 310 may be connected to each other at a position on the side wall 110 of the reactor 100 that is lower than the highest liquid level (A1) of the reactor 100. Alternatively, the reactor 100 and the solution discharge pipe 310 may be connected to each other at a position that is at least two-fifths of the top of the side wall 110 of the reactor 100 based on the overall height. This is advantageous for improving the productivity of the entire manufacturing apparatus.
[0059] Meanwhile, the solution discharge pipe 310 may be positioned at a downward incline from the horizontal plane from the reactor 100 toward the outside of the reactor 100. This is advantageous for the solution inside the reactor 100 to be discharged to the outside of the reactor 100 through the solution discharge pipe 310 after passing through the methyl filter unit 320.
[0060] Additionally, the solution discharge pipe 310 can be positioned horizontally or according to space and other requirements.
[0061] A vacuum pump 350 may be located in the solution discharge pipe 310, specifically, behind the shutoff unit 340. By driving the vacuum pump 350, it is advantageous to separate the solution in the reactor 100 and discharge it to the outside.
[0062] The solution that passes through the methyl filter unit 320 and is discharged to the outside through the solution discharge pipe 310 may be stored in a separate storage tank or may be immediately discharged into a wastewater treatment plant.
[0063] FIG. 4 is a diagram that schematically shows the configuration of a manufacturing apparatus for a positive electrode active material precursor, including a control unit.
[0064] 4, an apparatus for manufacturing a positive electrode active material precursor according to an embodiment of the present invention may include a control unit 500. The control unit 500 may be electrically connected to the supply unit 200, the nitrogen purge unit 330, the shut-off unit 340, the decompression pump 350, and a level gauge (not shown).
[0065] When the reactants in the reactor 100 reach the highest liquid level (A1), the control unit 500 stops the operation of the pressure reducing pump 350 and / or turns off the shutoff unit 340 in response to an electrical connection of a level gauge (not shown) located at the highest liquid level (A1), and then operates the second nitrogen purge unit 332 to inject nitrogen. The speed and duration of the nitrogen injection have been described above and will not be described further.
[0066] In another embodiment of the present invention, a method for producing a positive electrode active material precursor can be provided. Specifically, the method for producing a positive electrode active material precursor can be provided by utilizing the above-described apparatus for producing a positive electrode active material precursor.
[0067] A method for producing a cathode active material precursor according to the present invention includes: continuously feeding raw materials into a reactor, stirring and reacting them to form reactants; discharging a solution from the reactor through a methyl filter unit located in a solution discharge pipe connected to a sidewall of the reactor; and purging with nitrogen by injecting nitrogen into the methyl filter unit when the reactants in the reactor reach a maximum liquid level in the reactor. The nitrogen purging step may inject nitrogen into the solution discharge pipe, and the injected nitrogen may flow from the inside of the solution discharge pipe toward the inside of the reactor.
[0068] First, a method for preparing a positive electrode active material precursor may include continuously feeding raw materials into a reactor, stirring and reacting the raw materials to form a reactant.
[0069] The raw materials for preparing a cathode active material precursor according to the present invention mainly include a metal element-containing raw material, an ammonia-containing raw material, and caustic soda, and may include additional raw materials as needed. In the drawings, the raw material supply section is divided into a first raw material supply section and a second raw material supply section, but this is not specifically defined. The raw materials may be supplied separately through any supply section, or simultaneously through a single supply section. It is also clear that additional supply sections (not shown) may be provided to supply the raw materials separately as needed.
[0070] The metal element-containing raw material may be one or more selected from metal oxides, metal salts, and metal hydroxides, and is not particularly limited as long as it is applicable to a cathode active material precursor for lithium secondary batteries. The supply rate of the metal element-containing raw material may be 300 to 2500 kg / h, and may be maintained at a constant rate or may be varied in sections. The supply rate is not particularly limited as long as it is capable of effectively producing the cathode active material precursor of the present invention.
[0071] The supply rate of the ammonia-containing raw material may be 10 to 200 kg / h. The ammonia-containing raw material may be an NH4OH solution, and is not particularly limited as long as it can effectively produce the cathode active material precursor targeted in the present invention.
[0072] Meanwhile, the caustic soda (NaOH) solution may be supplied at a rate of 100 to 2000 kg / h. The ammonia-containing raw material and caustic soda may be supplied at a constant rate within the above-mentioned supply rate range or at different rates depending on the section, and are not particularly limited as long as they can effectively produce the cathode active material precursor of the present invention.
[0073] In the present invention, it is preferable to produce a cathode active material precursor by charging the raw material solution into a reactor so that the reactor reaches a minimum liquid level (A0) or higher. When the reactor reaches a minimum liquid level (A0) or higher, it is advantageous to produce a cathode active material precursor of uniform quality.
[0074] Meanwhile, the raw material solution can be stirred by operating the stirring unit simultaneously with the introduction of the raw material solution into the reactor. At this time, the stirring speed may be in the range of 10 to 2000 rpm, specifically, 50 to 300 rpm. There are no particular limitations on the speed as long as the raw material solution can be smoothly stirred and the cathode active material precursor targeted in the present invention can be produced.
[0075] At this time, nitrogen is purged through the nitrogen supply unit 230 at a rate of 80 to 150 LPM to remove oxygen dissolved in the raw material solution.
[0076] While starting to introduce the raw material solution into the reactor 100, the shutoff unit 340 located in the solution discharge pipe 310 connected to the reactor 100 may be maintained in an open state.
[0077] Meanwhile, when the height of the reactants inside the reactor 100 rises above the lowest point where the sidewall 110 of the reactor 100 is connected to the solution discharge pipe 310, nitrogen can be purged through the first nitrogen purge unit at a spray speed of 50 LPM to 100 LPM toward the front side of the methyl filter unit 320 (based on the direction in which the solution flows from the reactor to the outside). Nitrogen can also be purged directly into the methyl filter unit 320 from the upper side. This has the advantage of dispersing the positive electrode active material precursor to prevent or inhibit adhesion to the methyl filter unit 320 and efficiently discharging only the solution inside the reactor 100 to the outside, allowing the positive electrode active material precursor to be concentrated and continuously produced.
[0078] In addition, when the height of the reactants in the reactor 100 rises above the lowest point of the portion where the side wall 110 of the reactor 100 and the solution discharge pipe 310 are connected, the decompression pump 350 can be operated. At this time, an electrical signal is transmitted from a level gauge located at the lowest point to the control unit 500, and the decompression pump 350 can be operated under the control of the control unit 500 in response.
[0079] When the height of the reactants in the reactor 100 reaches the highest liquid level (A1) of the reactor 100, the control unit 500 stops the operation of the pressure reducing pump 350 in response to an electrical signal from a level gauge (not shown), turns off the shutoff unit 340, and then operates the second nitrogen purge unit 332 to inject nitrogen gas. The nitrogen gas injection rate of the second nitrogen purge unit 332 may be in the range of 100 LPM to 1000 LPM, specifically, in the range of 250 LPM to 500 LPM, and the injection time may be in the range of 0.1 to 1 second. The nitrogen gas injected from the second nitrogen purge unit 332 may desorb the cathode active material precursor attached to the methyl filter unit 320 as it moves into the reactor 100. The operation of injecting nitrogen gas from the second nitrogen purge unit 332 may be performed one or more times continuously, and is not particularly limited. Here, the reason why the height of the reactants in reactor 100 reaches the highest liquid level (A1) of reactor 100 is because the positive electrode active material precursor adheres to methyl filter unit 320, preventing the solution from being smoothly discharged to the outside. Therefore, by operating second nitrogen purge unit 332 to inject nitrogen gas after closing shutoff unit 340 as described above, the injected nitrogen gas passes through methyl filter unit 320 and flows into reactor 100, thereby desorbing the positive electrode active material precursor adhered to methyl filter unit 320. The advantages of the nitrogen gas injection speed and injection time range have been described above and will not be discussed further.
[0080] After the second nitrogen purge unit 332 has completed the injection of nitrogen gas, the shutoff unit 340 can be opened and the decompression pump 350 can be operated.
[0081] In the present invention, when the solid content of the total mass of the reactants in the reactor 100 reaches a range of 5% to 65%, the reaction is terminated, and solid-liquid separation and subsequent processing are performed to produce a cathode active material precursor.
[0082] Although the present invention has been described with reference to the drawings illustrating an apparatus for manufacturing a cathode active material precursor, the present invention is not limited to the above-described embodiments and drawings, and may be manufactured in various different forms. It should be understood by those skilled in the art that the present invention may be embodied in other specific forms without changing the technical concept or essential features of the present invention. [Explanation of symbols]
[0083] 1: Positive electrode active material precursor manufacturing equipment 100: Reactor 110: Side wall 120: Upper cover 130: Stirring section 131: Stirring shaft 132: Stirring blade 200: Supply department 210: 1st raw material supply section 220:Second raw material supply section 230: Nitrogen supply unit 300: Solution discharge part 310:Solution discharge pipe 320: Methyl filter unit 330: Nitrogen purge unit 331: First nitrogen purge unit 332: Second nitrogen purge unit 340: Cutoff unit 350: Pressure reducing pump 400: pH sensor part A0:Minimum liquid level A1: Highest liquid level
Claims
1. a reactor 100 for containing and reacting reactants therein; A supply unit 200 for supplying reactants into the reactor 100; and a solution discharge unit 300 for continuously discharging the solution from the precursor and the solution generated by the reaction of the reactants inside the reactor 100 to the outside of the reactor 100; The solution discharge unit 300 is a solution discharge pipe 310 communicating with the side wall 110 of the reactor 100 and extending to the outside; a methyl filter unit 320 located in the solution discharge pipe 310, which separates the cathode active material precursor from the solution; a nitrogen purge unit 330 for purging nitrogen into the methyl filter unit 320; an isolation unit 340 located at the rear end of the nitrogen purge unit 330; and a decompression pump 350 located at the rear end of the blocking unit 340; The methyl filter unit 320 is located at one end of the solution discharge pipe 310 adjacent to the reactor 100. Equipment for manufacturing positive electrode active material precursors.
2. The nitrogen purge unit 330 includes: a first nitrogen purge unit 331 and a second nitrogen purge unit 332, which are respectively located on both sides of the methyl filter unit 320 in the solution flow direction of the solution discharge pipe 310; The apparatus for producing the positive electrode active material precursor according to claim 1 .
3. The first nitrogen purge unit 331 continuously injects nitrogen gas into one side of the methyl filter unit 320 facing the reactor 100. The apparatus for producing a positive electrode active material precursor according to claim 2 .
4. The nitrogen gas injection rate of the first nitrogen purge unit 331 is in the range of 50 LPM to 100 LPM. The apparatus for producing a positive electrode active material precursor according to claim 2 .
5. When the reactants contained in the reactor 100 exceed the highest liquid level (A1) of the reactor 100, The second nitrogen purge unit 332 injects nitrogen gas onto the other side of the methyl filter unit 320 facing the reactor 100, thereby desorbing precursors attached to the methyl filter unit 320. The apparatus for producing a positive electrode active material precursor according to claim 2 .
6. The nitrogen gas injection rate of the second nitrogen purge unit 332 is in the range of 250 LPM to 500 LPM. The apparatus for producing a positive electrode active material precursor according to claim 5 .
7. Before the second nitrogen purge unit 332 injects nitrogen gas, The blocking unit 340 is first closed (off). The apparatus for producing a positive electrode active material precursor according to claim 5 .
8. The highest liquid level (A1) of the reactor 100 is The reactor 100 is located at a position higher than the portion where the side wall 110 and the solution discharge pipe 310 are connected in communication with each other. The apparatus for producing a positive electrode active material precursor according to claim 5 .
9. The side wall 110 of the reactor 100 is connected to the solution discharge pipe 310 at a position of at least two-fifths of the upper part based on the overall height of the side wall 110. The apparatus for producing the positive electrode active material precursor according to claim 1 .
10. The methyl filter unit 320 is fixed to the solution discharge pipe 310 by a detachable and attachable fixing member, and is replaceable. The apparatus for producing the positive electrode active material precursor according to claim 1 .
11. The methyl filter unit 320 is formed by stacking methyl filters having pore sizes ranging from 0.2 μm to 0.8 μm. The apparatus for producing the positive electrode active material precursor according to claim 1 .
12. The control unit 500 controls the operation of the supply unit 200, the nitrogen purge unit 330, the shutoff unit 340, and the decompression pump 350. The apparatus for producing the positive electrode active material precursor according to claim 1 .
13. When the operation of the decompression pump 350 is stopped by the control unit 500, the shutoff unit 340 is turned off. The apparatus for producing a positive electrode active material precursor according to claim 12 .
14. continuously charging raw materials into a reactor and stirring and reacting to form reactants; A solution discharge step of discharging the solution in the reactor separated through a methyl filter unit located in a solution discharge pipe connected to the side wall of the reactor to the outside of the reactor; and a nitrogen purging step of injecting nitrogen into a methyl filter unit when the reactants in the reactor reach a maximum liquid level in the reactor; The nitrogen purging step involves injecting nitrogen into a solution discharge pipe, and the injected nitrogen flows from the inside of the solution discharge pipe toward the inside of the reactor. A method for producing a positive electrode active material precursor.
15. The nitrogen purging step comprises: After closing the blocking unit located at the rear end of the solution discharge pipe, It is sprayed at a spray speed in the range of 250 LPM to 500 LPM. The method for producing a positive electrode active material precursor according to claim 14 .
16. In the nitrogen purging step, Before closing the shutoff unit, the operation of the pressure reducing pump located at the rear end of the shutoff unit is stopped first. The method for producing a positive electrode active material precursor according to claim 15 .
17. In the solution discharge step, When the reactants in the reactor reach or exceed the lowest end of a connecting portion of a solution discharge pipe that is connected to the reactor and the side wall of the reactor, a pressure reducing pump located in the solution discharge pipe is operated. The method for producing a positive electrode active material precursor according to claim 14 .
18. In the solution discharge step, Nitrogen gas is continuously injected onto one side of the methyl filter unit facing the reactor. The method for producing a positive electrode active material precursor according to claim 14 .
19. The nitrogen gas is injected in the range of 50 LPM to 100 LPM. The method for producing a positive electrode active material precursor according to claim 18.
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