Precursor Manufacturing Apparatus and Precursor Manufacturing Method

JP2025519129AActive Publication Date: 2025-06-24LG CHEM LTD
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Patent Information

Application Number
JP2024569405
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2023-05-23
Filing Date
2023-05-24
Publication Date
2025-06-24
Estimated Expiration
2043-05-24

AI Technical Summary

Benefits of technology

【0011】 本発明によると、共沈反応により前駆体を製造する前駆体製造装置に適用されるpH測定システムにおいて、共沈反応タンクの外部からpHを測定できるようにpH測定部を構成することで、pHを測定するpHセンサの破損を防止して分析信頼性が向上し、pHセンサの破損によるコストを低減することができる。

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Abstract

The present invention relates to a precursor manufacturing apparatus and a precursor manufacturing method. The precursor manufacturing apparatus according to the present invention is a precursor manufacturing apparatus that produces a precursor by causing a coprecipitation reaction of raw material substances, and includes a coprecipitation reaction tank that houses a container containing a reaction product and a filtrate, and a pH measurement system that measures the pH of the filtrate. The pH measurement system includes a filter that is located inside the coprecipitation reaction tank and filters the filtrate from the container, and a pH measurement unit that is located outside the coprecipitation reaction tank and measures the pH of the filtrate filtered by the filter.
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Description

Technical Field

[0001] This application claims the benefit of priority based on Korean Patent Application No. 10-2022-0063154 filed on May 24, 2022 and Korean Patent Application No. 10-2023-0066005 filed on May 23, 2023, and all contents disclosed in the documents of the Korean patent applications are incorporated herein by reference in their entirety. The present invention relates to a precursor manufacturing apparatus and a precursor manufacturing method.

Background Art

[0002] As technology development and demand related to mobile devices increase, the demand for secondary batteries as an energy source has been rapidly increasing. Among such secondary batteries, lithium secondary batteries having high energy density, high voltage, long cycle life, and low self-discharge rate have been commercialized and widely used.

[0003] Lithium transition metal oxides are used as the positive electrode active material of lithium secondary batteries, and among them, lithium cobalt oxide of LiCoO2, which has a high operating voltage and excellent capacity characteristics, has been mainly used. However, LiCoO2 has very poor thermal characteristics due to the destabilization of the crystal structure by delithiation, and is expensive, so there is a limit to its large-scale use as a power source in fields such as electric vehicles.

[0004] As materials to replace LiCoO2, lithium manganese oxides (such as LiMnO2 or LiMn2O4), lithium iron phosphate compounds (such as LiFePO4), or lithium nickel oxides (such as LiNiO2) have been developed. Among them, research and development on lithium nickel oxides, which have a high reversible capacity of about 200 mAh / g and are easy to realize a large-capacity battery, have been more actively studied. However, LiNiO2 has worse thermal stability than LiCoO2, and when an internal short circuit occurs due to external pressure or the like in the charged state, the positive electrode active material itself is decomposed, causing problems such as battery rupture and ignition.

[0005] Therefore, as a method for maintaining the excellent reversible capacity of LiNiO2 and improving its low thermal stability, LiNi1-αCoαO2 (α = 0.1 - 0.3) in which part of nickel is replaced by cobalt, or nickel cobalt manganese (NCM) - based lithium composite metal oxides in which part of nickel is replaced by Mn and Co have been developed. In addition, in order to have excellent output characteristics and solve stability problems such as elution of metal elements, lithium transition metal oxides having a concentration gradient of metal composition have also been proposed.

[0006] When manufacturing the NCM precursor by applying the conventional coprecipitation reaction, the pH is controlled to manufacture a precursor with controlled particle growth, primary particle growth, and sphericity. This has the effect of improving the uniform firing degree and particle strength during the firing of the cathode material, and improving battery performance such as cycle life and gas generation. Therefore, it is an item that must be essentially managed during the manufacture of the precursor for improving the performance of the cathode material.

[0007] However, due to the insufficient durability of the pH sensor and the lack of reliability of the pH value inside the reactor, in practice, operators perform sampling and manage the pH using an external pH sensor, which increases the duplication of work and fatigue. In addition, in the case of a pH sensor installed inside, it lacks reliability when reused, so it must be discarded after one use, or there is a high possibility of problems such as breakage or poor contact during the reaction, which leads to defects in the precursor.

Summary of the Invention

Problems to be Solved by the Invention

[0008] One aspect of the present invention is to provide a precursor manufacturing apparatus and a precursor manufacturing method capable of improving the reliability of pH analysis.

Means for Solving the Problems

[0009] The precursor manufacturing apparatus according to an embodiment of the present invention is a precursor manufacturing apparatus that manufactures a precursor by subjecting raw material substances to a coprecipitation reaction, and includes a coprecipitation reaction tank that houses a container containing a reaction product and a filtrate, and a pH measurement system that measures the pH of the filtrate. The pH measurement system can include a filter that is located inside the coprecipitation reaction tank and filters the filtrate from the container, and a pH measurement unit that is located outside the coprecipitation reaction tank and measures the pH of the filtrate filtered by the filter.

[0010] The precursor manufacturing method according to an embodiment of the present invention is a precursor manufacturing method that manufactures a precursor by subjecting raw material substances to a coprecipitation reaction, and includes a housing process of housing the raw material substances that form a container containing a reaction product and a filtrate in a coprecipitation reaction tank, and a pH measurement process of measuring the pH of the filtrate. The pH measurement process can include a filter step of filtering the filtrate from the container through a filter located inside the coprecipitation reaction tank, and a measurement step of measuring the pH of the filtrate filtered by the filter through a pH measurement unit located outside the coprecipitation reaction tank.

Advantages of the Invention

[0011] According to the present invention, in a pH measurement system applied to a precursor manufacturing apparatus that manufactures a precursor by a coprecipitation reaction, by configuring a pH measurement unit so that the pH can be measured from outside the coprecipitation reaction tank, damage to the pH sensor for measuring the pH can be prevented, the analysis reliability can be improved, and the cost due to damage to the pH sensor can be reduced.

Brief Description of the Drawings

[0012]

Figure 1

Figure 2

Figure 3

Best Mode for Carrying Out the Invention

[0013] The objects, specific advantages, and novel features of the present invention will become more apparent from the following detailed description and preferred embodiments related to the accompanying drawings. In this specification, when assigning reference numerals to the components of each drawing, it should be noted that, as much as possible, the same components have the same numbers, even if they are shown on other drawings. Further, the present invention may be realized in various different forms and is not limited to the embodiments described herein. In describing the present invention, detailed descriptions of related known technologies that would unnecessarily obscure the gist of the present invention are omitted.

[0014] Precursor manufacturing apparatus according to an embodiment FIG. 1 is a front view showing a precursor manufacturing apparatus according to an embodiment of the present invention, FIG. 2 is a front view showing a pH measurement system in the precursor manufacturing apparatus according to an embodiment of the present invention, and FIG. 3 is a front view showing a pH measurement unit in the pH measurement system of the precursor manufacturing apparatus according to an embodiment of the present invention. Here, FIGS. 1 to 3 are reference views showing the inside of the apparatus in a perspective manner. At this time, FIG. 2 shows an enlarged view of region A in FIG. 1, and FIG. 3 shows an enlarged view of region B in FIG. 1.

[0015] Referring to FIGS. 1 to 3, a precursor manufacturing apparatus 1000 according to an embodiment of the present invention is a precursor manufacturing apparatus 1000 that coprecipitates raw materials to manufacture a precursor, and includes a coprecipitation reaction tank 200 that houses a container containing a reactant and a filtrate, and a pH measurement system 100 that measures the pH (hydrogen ion concentration) of the filtrate. The pH measurement system 100 includes a filter 120 that filters the filtrate and a pH measurement unit 110 that measures the pH of the filtrate. Further, in the precursor manufacturing apparatus 1000 according to an embodiment of the present invention, the pH measurement system 100 can further include a connection pipe P connected to the pH measurement unit 110 and a filtrate transfer pump 130 that moves the filtrate. Furthermore, the precursor manufacturing apparatus 1000 according to an embodiment of the present invention can further include a stirrer 300, a heater 400, a raw material inlet 500, a reactant discharge port 600, and a main filter 700.

[0016] More specifically, the coprecipitation reaction tank 200 has an accommodation part 200a formed therein for accommodating a container containing a reactant and a filtrate. Also, the coprecipitation reaction tank 200 is formed in a cylindrical shape, and for example, can be formed in a circular cylindrical shape.

[0017] The stirrer 300 can stir the raw material substances accommodated inside the coprecipitation reaction tank 200. Also, the stirrer 300 can include a rotating part 310 that is located inside the coprecipitation reaction tank 200 and rotates, and a motor part 320 that rotates the rotating part 310. Here, the rotating part 310 rotates inside the coprecipitation reaction tank 200 and can rotate the raw material substances to stir them.

[0018] The heater 400 can apply heat to the raw material substances accommodated inside the coprecipitation reaction tank 200. Here, the heater 400 can increase the temperature of the raw material substances to promote the coprecipitation reaction. At this time, the heater 400 can heat the raw material substances to a temperature of about 50°C, for example. On the other hand, the heater 400 can be located on the side wall of the coprecipitation reaction tank 200, for example.

[0019] The raw material inlet section 500 is connected to the upper part of the coprecipitation reaction tank 200 and can allow the raw material substances to flow into the interior of the coprecipitation reaction tank 200. That is, via the raw material inlet section 500, the raw material substances as reactants can be supplied to the accommodation section 200a of the coprecipitation reaction tank 200.

[0020] The raw material substances can include a metal solution, a caustic soda solution, and aqueous ammonia. At this time, for example, the metal solution may be a nickel-cobalt-manganese (Ni-Co-Mn) solution, and the caustic soda may be NaOH. And the caustic soda is a pH adjusting substance, and the aqueous ammonia may be a flocculant. Here, according to the degree of the pH of the filtrate measured by the pH measurement system 100, the input amount of the caustic soda can be adjusted to adjust the pH of the contents accommodated in the accommodation section 200a of the coprecipitation reaction tank 200. At this time, for example, the pH of the contents accommodated in the accommodation section 200a of the coprecipitation reaction tank 200 can be adjusted so that the pH of the filtrate becomes 10 to 12, and particles can be grown to produce a precursor.

[0021] The reactant discharge section 600 is connected to the lower part of the coprecipitation reaction tank 200 and can discharge the reactants for which the reaction inside the coprecipitation reaction tank 200 has been completed. That is, the produced precursor as a reactant can be discharged to the lower part of the coprecipitation reaction tank 200 via the reactant discharge section 600. Here, the precursor can be composed of an NCM (nickel-cobalt-manganese) precursor for a positive electrode active material. Also, the reactant discharge section 600 includes a reactant discharge valve 610 and can adjust the discharge of the reactants.

[0022] The Main Filter 700 can filter the reaction solution located inside the coprecipitation reaction tank 200. Here, after filtering a part of the reaction solution located inside the coprecipitation reaction tank 200 via the Main Filter 700 and discharging it to the outside of the coprecipitation reaction tank 200, the precursor reaction and the filtration flow rate can be confirmed.

[0023] The pH measurement system 100 can measure the pH of the filtrate contained inside the coprecipitation reaction tank 200. Here, the pH measurement system 100 can include a filter 120, a pH measurement unit 110, a connecting pipe P, and a filtrate transfer pump 130.

[0024] The filter 120 is located inside the coprecipitation reaction tank 200 and can filter the filtrate from the contained material. That is, when the raw material substance located inside the coprecipitation reaction tank 200 is generated into a reaction product and a filtrate which are the contained materials by the coprecipitation reaction, the filter 120 can filter the filtrate from the contained material. Here, by the coprecipitation reaction, in the metal solution which is the raw material substance, the metal which is the reaction product can precipitate, and the rest can be generated as the filtrate. At this time, the filtrate can include, as an example, water (H2O). Also, as another example, the filtrate can include water (H2O), aqueous ammonia, and Na2SO4, etc.

[0025] The filter 120 can be composed of a metal filter of a metal (Metal) material. Thereby, it is possible to prevent the filter 120 from being damaged by hitting the contained material accommodated inside the coprecipitation reaction tank 200. Also, it is possible to prevent chemical damage by the liquid-state contained material accommodated inside the coprecipitation reaction tank 200. At this time, the filter 120 can be composed of, for example, a stainless steel material.

[0026] The pH measurement system 100 can include a pH measurement unit 110 which is located outside the coprecipitation reaction tank 200 and measures the pH of the filtrate filtered by the filter 120. Here, the pH measurement unit 110 can include a buffer tank 111, a pH sensor 112, a fixing unit 113, a water level sensor 115, a washing water inflow unit 116, and a washing water discharge unit 117.

[0027] The buffer tank 111 is connected to the connecting pipe P and can store the filtrate filtered by the filter 120. Further, an accommodation space 111a for storing the filtrate can be formed inside the buffer tank. The pH sensor 112 can measure the pH of the filtrate stored in the buffer tank 111.

[0028] The fixing part 113 can fix the pH sensor 112 to the buffer tank 111. Here, the fixing part 113 is provided at the upper part of the buffer tank and can fix the pH sensor 112. Further, the fixing part 113 has a through hole 113a through which the pH sensor 112 penetrates inside, and can include a rubber packing 114 positioned between the through hole 113a and the pH sensor 112 so that the pH sensor 112 is press-fitted into the fixing part 113. The water level sensor 115 can measure the water level L1 of the filtrate stored in the buffer tank 111 and the water level L2 of the washing water.

[0029] The washing water inflow part 116 is connected to the upper side part of the side surface of the buffer tank 111 and can let the washing water flow into the buffer tank 111. Therefore, the inside of the buffer tank 111 can be washed with the washing water, and then the pH of the filtrate flowing into the buffer tank 111 for pH measurement can be accurately measured.

[0030] On the other hand, the washing water inflow part 116 can let the washing water flow into the buffer tank 111 so as to have a washing water level L2 higher than the filtrate level L1 of the filtrate that has flowed into the buffer tank 111. Thereby, the filtrate remaining inside the buffer tank can be completely washed. Further, the washing water flowing in through the washing water inflow part 116 may be a neutralizing solution with a pH of 7 to 8. Furthermore, the washing water can contain water.

[0031] The washing water discharge part 117 is connected to the lower part of the buffer tank 111, and the washing water flowing into the inside of the buffer tank 111 can be discharged. At this time, the washing water discharge part 117 can discharge the filtrate stored in the buffer tank 111 before washing the inside of the buffer tank 111. On the other hand, the washing water discharge part 117 can include a washing water discharge valve 118 that adjusts the discharge of the washing water or the filtrate stored in the buffer tank 111.

[0032] One side of the connecting pipe P is located inside the coprecipitation reaction tank 200 and is connected to the filter 120, and the other side extends outside the coprecipitation reaction tank 200 and can be connected to the pH measurement unit 110. The filtrate transfer pump 130 is provided on the connecting pipe P and can transfer the filtrate from the filter 120 to the buffer tank 111.

[0033] Therefore, the precursor manufacturing apparatus 1000 according to the embodiment of the present invention configured as described above can prevent damage to the pH sensor 112 that measures the pH by configuring the pH measurement unit 110 so that the pH can be measured from outside the coprecipitation reaction tank 200 during the manufacture of the precursor by the coprecipitation reaction, improve the analysis reliability, and reduce the cost due to the damage of the pH sensor 112.

[0034] Precursor manufacturing method according to an embodiment Hereinafter, a precursor manufacturing method according to an embodiment of the present invention will be described. Referring to FIGS. 1 to 3, the precursor manufacturing method according to the embodiment of the present invention is a precursor manufacturing method for manufacturing a precursor by subjecting a raw material substance to a coprecipitation reaction, including an accommodation process of accommodating a raw material substance that forms an accommodation substance including a reactant and a filtrate in the coprecipitation reaction tank 200, and a pH measurement process of measuring the pH of the filtrate. The pH measurement process can include a filtering step of filtering the filtrate from the accommodation substance through a filter 120 located inside the coprecipitation reaction tank 200, and a measuring step of measuring the pH of the filtrate filtered by the filter 120 through a pH measurement unit located outside the coprecipitation reaction tank 200.

[0035] The precursor manufacturing method according to an embodiment of the present invention is a method for manufacturing a precursor through the precursor manufacturing apparatus 1000 according to an embodiment of the present invention described above. Therefore, for the embodiment regarding this precursor manufacturing method, the content overlapping with the embodiment regarding the precursor manufacturing apparatus 1000 described above will be omitted or briefly described, and the description will focus on the differences.

[0036] More specifically, in the accommodating process, raw materials including reactants and filtrate are accommodated in the accommodating portion 200a of the coprecipitation reaction tank 200 to form an accommodation substance. Also, the accommodating process may include a raw material inflow step of flowing the raw material substance into the coprecipitation reaction tank 200 through the raw material inflow portion 500 connected to the upper part of the coprecipitation reaction tank 200. At this time, in the raw material inflow step, the raw material substance, which is a reactant, can be supplied to the accommodating portion 200a of the coprecipitation reaction tank 200 through the raw material inflow portion 500.

[0037] Then, the raw material substance flowing into the coprecipitation reaction tank 200 by the raw material inflow step can become an accommodation substance including reactants and filtrate in the coprecipitation reaction tank 200.

[0038] Here, in the accommodating process, the raw material substance is made to flow into the coprecipitation reaction tank 200, and the raw material substance that has flowed in reacts in the coprecipitation reaction tank 200 to form an accommodation substance including reactants and filtrate, so that the accommodation substance is accommodated in the coprecipitation reaction tank 200.

[0039] The raw material substance can include a metal solution, a caustic soda solution, and ammonia water. At this time, for example, the metal solution may be a nickel - cobalt - manganese (Ni - Co - Mn) solution, and the caustic soda may be NaOH. And the caustic soda is a pH adjusting substance, and the ammonia water may be a flocculant.

[0040] The stirring process can stir the raw material substances contained inside the coprecipitation reaction tank 200 via a stirrer after the accommodation process. Here, more specifically, the stirring process can be performed after the raw material substances have flowed into the inside of the coprecipitation reaction tank 200 through the raw material inflow step in the accommodation process.

[0041] At this time, the stirrer 300 can include a rotating part 310 that rotates inside the coprecipitation reaction tank 200 and a motor part 320 that rotates the rotating part 310. Here, the rotating part 310 rotates inside the coprecipitation reaction tank 200 and can rotate and stir the raw material substances.

[0042] The heating process can apply heat to the raw material substances contained inside the coprecipitation reaction tank 200 via a heater during the stirring process, or before and during the stirring process. The heating process can increase the temperature of the raw material substances via the heater 400 to promote the coprecipitation reaction. At this time, the heating process can heat the raw material substances to a temperature of about 50°C via the heater 400, for example. On the other hand, the heater 400 can be located on the side wall of the coprecipitation reaction tank 200, for example.

[0043] The pH measurement process includes a filter step and a measurement step, and can measure the pH of the filtrate via the pH measurement system 100. Here, the pH measurement system 100 can include a filter 120, a pH measurement unit 110, a connecting pipe P, and a filtrate transfer pump 130.

[0044] On the other hand, the pH measurement process can be performed after the accommodation process. Here, specifically, the pH measurement process can be performed after the raw material substances have flowed into the inside of the coprecipitation reaction tank 200 through the raw material inflow step in the accommodation process.

[0045] At this time, the pH measurement process can be performed at any one or more of the stages before, during, and after the stirring process, for example.

[0046] The filtration step can filter the filtrate from the contents through a filter 120 located inside the coprecipitation reaction tank 200. Also, in the filtration step, the filter 120 is located inside the coprecipitation reaction tank 200 and can filter the filtrate from the contents. That is, when the raw material substances located inside the coprecipitation reaction tank 200 are generated into the reactants and filtrate that are the contents by the coprecipitation reaction, the filter 120 can filter the filtrate from the contents. Here, by the coprecipitation reaction, in the metal solution which is the raw material substance, the metal which is the reactant can precipitate and the rest can be generated as the filtrate. At this time, the filtrate can contain, for example, water (H2O). Also, as another example, the filtrate can contain water (H2O), aqueous ammonia, and Na2SO4, etc.

[0047] The filter 120 can be composed of a metal filter made of a metal (Metal) material. Thereby, it is possible to prevent the filter 120 from being damaged by hitting the contents contained inside the coprecipitation reaction tank 200. Also, it is possible to prevent chemical damage by the liquid-state contents contained inside the coprecipitation reaction tank 200. At this time, the filter 120 can be made of, for example, a stainless steel material.

[0048] The measurement step can measure the pH of the filtrate filtered by the filter 120 through a pH measurement unit 110 located outside the coprecipitation reaction tank 200. Also, the measurement step can include a filtrate accommodation process and a sensor measurement process. Also, the measurement step can further include a washing water inflow process and a washing water discharge process.

[0049] In the filtrate storage step, the filtrate filtered by the filter 120 can be stored in the buffer tank 111 through the connection pipe P with one side connected to the filter 120 and the other side connected to the pH measurement unit 110. Here, in the filtrate storage step, the filtrate can be moved from the filter 120 to the buffer tank 111 through the filtrate transfer pump 130 provided on the connection pipe P. The buffer tank 111 is connected to the connection pipe P and can store the filtrate filtered by the filter 120. Also, in the buffer tank 111, a storage space 111a for storing the filtrate can be formed inside.

[0050] In the sensor measurement step, the pH of the filtrate stored in the buffer tank 111 can be measured through the pH sensor 112 of the pH measurement unit 110. In the washing water inflow step, after the sensor measurement step and when the filtrate stored in the buffer tank 111 is discharged, washing water can be made to flow into the inside of the buffer tank through the washing water inflow part connected to the upper side of the side surface of the buffer tank, and the inside of the buffer tank can be washed. At this time, the washing water discharge part 117 can discharge the filtrate stored in the buffer tank 111 before washing the inside of the buffer tank 111.

[0051] Therefore, the inside of the buffer tank 111 can be washed with washing water, and then the pH of the filtrate flowing into the inside of the buffer tank 111 for pH measurement can be accurately measured.

[0052] Also, in the washing water inflow step, the washing water flowing in through the washing water inflow part 116 may be a neutralizing solution with a pH of 7 to 8. Furthermore, the washing water can contain water.

[0053] Furthermore, in the washing water inflow step, the washing water can be made to flow in such that the water level of the washing water is higher than the water level of the filtrate that had flowed into the inside of the buffer tank in the filtrate storage step.

[0054] Then, in the washing water inflow process, the water levels L1 of the filtrate and L2 of the washing water stored in the buffer tank 111 can be measured via the water level sensor 115 and increased. The water level L2 of the washing water can be adjusted to be higher than the water level L1 of the filtrate stored in the buffer tank 111.

[0055] In the washing water discharge process, the washing water flowing into the interior of the buffer tank 111 can be discharged via the washing water discharge section 117 connected to the lower part of the buffer tank 111.

[0056] On the other hand, the precursor manufacturing method according to an embodiment of the present invention may further include a pH adjustment process of adjusting the input amount of caustic soda according to the degree of pH of the filtrate measured in the pH measurement process and adjusting the pH of the contents stored in the accommodation section 200a of the coprecipitation reaction tank 200. At this time, in the pH adjustment process, the pH of the contents stored in the accommodation section 200a of the coprecipitation reaction tank 200 can be adjusted so that the pH of the filtrate becomes 10 to 12.

[0057] Also, the precursor manufacturing method according to an embodiment of the present invention can repeatedly perform the pH measurement process and the pH adjustment process to effectively adjust the pH of the filtrate. At this time, the pH measurement process and the pH adjustment process can be performed at any one or more stages of, for example, the stage before the stirring process, the ongoing stage, and the stage after the completion of the process.

[0058] On the other hand, the precursor manufacturing method according to an embodiment of the present invention may further include a reaction solution filtration process of filtering the reaction solution in which the main filter 700 is located inside the coprecipitation reaction tank 200.

[0059] Also, in the reaction solution filtration process, after filtering a part of the reaction solution located inside the coprecipitation reaction tank 200 via the main filter 700 and discharging it outside the coprecipitation reaction tank 200, the precursor reaction and the filtration flow rate can be confirmed.

[0060] As described above, the present invention has been described in detail with reference to specific embodiments, which are for specifically explaining the present invention and the present invention is not limited thereto. It can be said that various implementations are possible by those with ordinary knowledge in the art within the scope of the technical idea of the present invention. Also, the specific protection scope of the present invention will be clarified by the appended claims.

Explanation of Reference Numerals

[0061] 100: pH measurement system 110: pH measurement unit 111: Buffer tank 111a: Accommodation space 112: pH sensor 113: Fixing part 113a: Through hole 114: Rubber packing 115: Water level sensor 116: Washing water inflow part 117: Washing water discharge part 118: Washing water discharge valve 120: Filter 130: Filtrate transfer pump 200: Coprecipitation reaction tank 200a: Accommodation part 300: Stirrer 400: Heater 500: Raw material inflow part 600: Reaction product discharge part 1000: Precursor manufacturing apparatus P: Connecting pipe

Claims

1. A precursor manufacturing apparatus for manufacturing a precursor by subjecting raw material substances to a coprecipitation reaction, comprising: a coprecipitation reaction tank for containing a container including a reactant and a filtrate; a pH measurement system for measuring the pH of the filtrate; and the pH measurement system includes: a filter located inside the coprecipitation reaction tank for filtering the filtrate from the container; a pH measurement unit located outside the coprecipitation reaction tank for measuring the pH of the filtrate filtered by the filter; The precursor manufacturing apparatus.

2. The precursor manufacturing apparatus according to claim 1, further comprising a connecting pipe having one side located inside the coprecipitation reaction tank and connected to the filter, and the other side extending outside the coprecipitation reaction tank and connected to the pH measurement unit.

3. The pH measurement unit includes: a buffer tank connected to the connecting pipe and containing the filtrate filtered by the filter; a pH sensor for measuring the pH of the filtrate contained in the buffer tank. The precursor manufacturing apparatus according to claim 2.

4. The pH sensor: penetrates the buffer tank in the vertical direction, and the lower side is located inside the buffer tank. The precursor manufacturing apparatus according to claim 3.

5. The pH measurement unit further includes a fixing portion for fixing the pH sensor to the buffer tank. The precursor manufacturing apparatus according to claim 4.

6. The fixing portion includes: a through hole is formed inside for the pH sensor to penetrate, and a rubber packing located between the through hole and the pH sensor so that the pH sensor is press-fitted into the fixing portion. The precursor manufacturing apparatus according to claim 5.

7. The precursor manufacturing apparatus according to claim 3, further comprising a filtrate transfer pump provided on the connecting pipe for transferring the filtrate from the filter to the buffer tank.

8. The pH measurement unit includes: a washing water inflow portion connected to the upper side of the side surface of the buffer tank for allowing washing water to flow into the buffer tank; a washing water discharge portion connected to the lower portion of the buffer tank for discharging the washing water flowing into the buffer tank. The precursor manufacturing apparatus according to claim 3.

9. The pH measurement unit further includes a water level sensor for measuring the water levels of the filtrate and the washing water contained in the buffer tank. The precursor manufacturing apparatus according to claim 8.

10.

10.

10. The precursor manufacturing apparatus according to claim 1, wherein the filter is a metal filter.

11. A stirrer for stirring the raw material substances accommodated inside the coprecipitation reaction tank, A heater for applying heat to the raw material substances accommodated inside the coprecipitation reaction tank, further comprising the precursor manufacturing apparatus according to claim 1.

12. A precursor manufacturing method for manufacturing a precursor by subjecting raw material substances to a coprecipitation reaction, A housing process of housing the raw material substances that form an accommodation containing reactants and filtrate in a coprecipitation reaction tank, A pH measurement process of measuring the pH of the filtrate, Including, The pH measurement process is, A filter step of filtering the filtrate from the accommodation through a filter located inside the coprecipitation reaction tank, A measurement step of measuring the pH of the filtrate filtered by the filter through a pH measurement unit located outside the coprecipitation reaction tank, A precursor manufacturing method including.

13. The measurement step is, A filtrate accommodation process of accommodating the filtrate filtered by the filter in a buffer tank through a connection pipe with one side connected to the filter and the other side connected to the pH measurement unit, A sensor measurement process of measuring the pH of the filtrate accommodated in the buffer tank through the pH sensor of the pH measurement unit, the precursor manufacturing method according to claim 12.

14. The filtrate accommodation process is, The precursor manufacturing method according to claim 13, wherein the filtrate is moved from the filter to the buffer tank through a filtrate transfer pump provided on the connection pipe.

15. The measurement step is, After the sensor measurement process, when the filtrate accommodated in the buffer tank is discharged, cleaning water is introduced into the buffer tank through a cleaning water inflow part connected to the upper side of the side surface of the buffer tank to clean the inside of the buffer tank, a cleaning water inflow process, A cleaning water discharge process of discharging the cleaning water introduced into the buffer tank through a cleaning water discharge part connected to the lower part of the buffer tank, further comprising the precursor manufacturing method according to claim 13.

16. The cleaning water inflow process is to introduce the cleaning water so that the water level of the cleaning water is higher than the water level of the filtrate that has flowed into the buffer tank by the filtrate accommodation process, the precursor manufacturing method according to claim 15.

17. After the accommodation process, a stirring process of stirring the raw material substances accommodated inside the coprecipitation reaction tank via a stirrer; The method for producing a precursor according to claim 12, further comprising a heating process of applying heat to the raw material substances accommodated inside the coprecipitation reaction tank via a heater during the stirring process, or before and during the stirring process.

Citation Information

Patent Citations

  • Method for material concentrating in ternary precursor synthesis reaction

    CN110756140A

  • Device for increasing solid content in reaction kettle

    CN209791543U

  • Device for preparing lithium-rich manganese cathode material precursor of lithium ion battery by coprecipitation method

    CN211913796U

  • Method for measuring PH of electroplating liquid

    JP1986031959A

  • Processing of waste liquid containing high concentration of metal ion

    JP1992349990A