CN114733463A - Positive electrode material precursor coprecipitation reaction equipment - Google Patents
Positive electrode material precursor coprecipitation reaction equipment Download PDFInfo
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- CN114733463A CN114733463A CN202210406122.5A CN202210406122A CN114733463A CN 114733463 A CN114733463 A CN 114733463A CN 202210406122 A CN202210406122 A CN 202210406122A CN 114733463 A CN114733463 A CN 114733463A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 233
- 239000002243 precursor Substances 0.000 title claims abstract description 100
- 238000000975 co-precipitation Methods 0.000 title claims abstract description 30
- 239000007774 positive electrode material Substances 0.000 title abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 66
- 238000001914 filtration Methods 0.000 claims abstract description 56
- 238000003756 stirring Methods 0.000 claims abstract description 34
- 239000000706 filtrate Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000010406 cathode material Substances 0.000 claims description 14
- 230000000712 assembly Effects 0.000 claims description 2
- 238000000429 assembly Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000009991 scouring Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 137
- 238000007599 discharging Methods 0.000 description 30
- 238000010517 secondary reaction Methods 0.000 description 13
- 238000004321 preservation Methods 0.000 description 11
- 230000001276 controlling effect Effects 0.000 description 9
- 239000010405 anode material Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000012066 reaction slurry Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910001039 duplex stainless steel Inorganic materials 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/11—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
- B01D29/31—Self-supporting filtering elements
- B01D29/33—Self-supporting filtering elements arranged for inward flow filtration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/50—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition
- B01D29/52—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition in parallel connection
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/62—Regenerating the filter material in the filter
- B01D29/66—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps
- B01D29/68—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps with backwash arms, shoes or nozzles
- B01D29/688—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps with backwash arms, shoes or nozzles with backwash arms or shoes acting on the cake side
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a coprecipitation reaction device for a precursor of a positive electrode material, which comprises: the reaction kettle is used for containing precursor slurry, the inner cavity of the reaction kettle is divided into a reaction area and a concentration area circumferentially arranged around the reaction area, and the upper end and the lower end of the reaction area are communicated with the concentration area to form a slurry circulation loop; the stirring assembly is arranged in a reaction zone in the reaction kettle and is used for uniformly mixing the precursor slurry in the reaction kettle; and the filtering component is arranged in the concentration area of the reaction kettle and is used for intercepting the precursor in the reaction kettle to obtain concentrated precursor slurry and filtering out the filtrate. The invention reduces the quantity of equipment and the production cost, and the slurry can also play a role of scouring the surface of the filtering component in the circulating process, thereby ensuring the continuous concentration and enrichment of materials in the filtering component.
Description
Technical Field
The invention relates to the technical field of precursor production, in particular to a coprecipitation reaction device for a precursor of a positive electrode material.
Background
The precursor slurry of the anode material is a front-end material of the anode material and plays a decisive role in the performance of the anode material. The production method of the precursor of the cathode material generally comprises the following steps: preparing mixed salt solution of nickel sulfate (or nickel chloride), cobalt sulfate (or cobalt chloride) and manganese sulfate (or manganese chloride) with a certain molar concentration, preparing alkali solution of a certain molar concentration by sodium hydroxide, and taking ammonia water of a certain concentration as a complexing agent. Adding the filtered mixed salt solution, the alkali solution and the complexing agent into a reaction kettle at a certain flow rate, controlling the stirring speed of the reaction kettle, the temperature and the pH value of the reaction slurry, performing neutralization reaction on the salt and the alkali to generate a ternary precursor crystal nucleus, gradually growing up the ternary precursor crystal nucleus, and concentrating and drying the reaction slurry after the granularity reaches a preset value to obtain the ternary precursor.
In the process of producing the precursor of the anode material by using the conventional reaction kettle, liquid only can realize the processes of reaction and gradual growth of crystal nucleus in the reaction kettle. However, for the material with slow reaction time, the main reaction kettle and the secondary reaction kettle are required to cooperate to realize the reaction process of the slurry, wherein crystal growth is realized in the main reaction kettle, particle diameter redistribution and morphology adjustment are performed in the reaction kettle, on the basis, if the liquid in the reaction kettle needs to be concentrated, a separate concentrator needs to be additionally arranged, the equipment investment is greatly increased, the time for the slurry to dissociate outside the reaction kettle is increased, and the time for the slurry to dissociate outside the reaction kettle is not expected to increase in the main actual production process.
Disclosure of Invention
The invention mainly aims to provide a coprecipitation reaction device for a precursor of a positive electrode material, and aims to solve the technical problems that in the prior art, a concentrator can only meet the requirements of more devices and high generation cost of a precursor production system.
In order to achieve the above object, there is provided according to the present invention a cathode material precursor coprecipitation reaction apparatus including:
the reaction kettle is used for containing precursor slurry, the inner cavity of the reaction kettle is divided into a reaction area and a concentration area circumferentially arranged around the reaction area, and the upper end and the lower end of the reaction area are communicated with the concentration area to form a slurry circulation loop;
the stirring component is arranged in a reaction area in the reaction kettle and is used for uniformly mixing the precursor slurry in the reaction kettle;
and the filtering component is arranged in the concentration area of the reaction kettle and is used for intercepting the precursor in the reaction kettle to obtain concentrated precursor slurry and filtering out a filtrate.
The positive electrode material precursor coprecipitation reaction equipment divides an inner cavity in the reaction kettle into a reaction area and a concentration area, the stirring assembly stirs precursor slurry in the reaction kettle to form a liquid flow when in work, the slurry circulates in the circulation loop due to the partition effect, so that the precursor slurry firstly carries out main reaction in the reaction area and then carries out secondary reaction in the concentration area, and the precursor slurry can be directly concentrated after the secondary reaction, so that the functions of the main reaction kettle, the secondary reaction kettle and a concentrator in the prior art are replaced, the equipment quantity and the production cost are reduced, the slurry can also play a role in washing the surface of the filtering assembly in the circulation process, and the continuous concentration and enrichment of materials in the slurry can be ensured.
Further, the inner cavity of the reaction kettle is divided into a reaction area and a concentration area circumferentially surrounding the reaction area through a guide cylinder arranged between the stirring assembly and the filtering assembly, and the guide cylinder is a hollow cylinder with two open ends.
Furthermore, the draft tube is fixed through an anti-rotation baffle.
Further, the draft tube is hung through a support.
Further, the diameter of the guide shell and the diameter of the reaction kettle are in the proportion range of
Furthermore, the filtering assemblies are annularly arranged in the concentration area of the reaction kettle at intervals around the stirring assembly.
Further, the input unit is used for inputting the precursor slurry into the reaction zone.
Further, the input unit comprises a feed pipe extending into the reaction vessel, and an outlet end of the feed pipe is positioned in an upper area of the reaction zone.
Further, the filter assembly is fixed in the filter core on the filter liquid pipe including filter liquid pipe, the interval that is fixed in the reation kettle, filter liquid pipe includes outer circle pipe, the inner circle pipe of laying along the radial outside-in of reation kettle, outer circle pipe, inner circle pipe are all through going out the outer clear liquid system that goes out of clear liquid pipe, outer circle pipe, inner circle pipe are the sealed tube.
Therefore, the anode material precursor coprecipitation reaction equipment divides an inner cavity in the reaction kettle into a reaction area and a concentration area, the stirring assembly stirs precursor slurry in the reaction kettle to form a liquid flow when in work, the slurry circulates in the circulation loop due to the partition effect, so that the precursor slurry firstly carries out main reaction in the reaction area and then carries out secondary reaction in the concentration area, the secondary reaction can be directly concentrated, the functions of the main reaction kettle, the secondary reaction kettle and a concentrator in the prior art are replaced, the equipment number and the production cost are reduced, the slurry can also play a role in flushing the surface of the filtering assembly in the circulation process, and the continuous concentration and enrichment of materials can be ensured.
The invention is further described with reference to the following figures and detailed description. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to assist in understanding the invention, and are included to explain the principles of the invention and not to limit the invention unduly. In the drawings:
fig. 1 is a schematic system structure diagram of a co-precipitation reaction system for precursors of positive electrode materials in the present invention.
FIG. 2 is a top view of the filter assembly mounting structure of the present invention.
Fig. 3 is a second top view of the filter assembly mounting structure of the present invention.
FIG. 4 is a schematic structural diagram of a first connection mode of the filtrate pipe and the clear liquid outlet pipe according to the present invention.
FIG. 5 is a schematic structural view of a second connection mode of the filtrate tube and the clear liquid outlet tube according to the present invention.
Fig. 6 is a schematic structural view of a third connection mode of the filtrate pipe and the clear liquid outlet pipe in the invention.
FIG. 7 is a schematic structural view of a fourth connection mode of the filtrate tube and the clear liquid outlet tube according to the present invention.
FIG. 8 is a schematic view of a reaction vessel according to the present invention.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying drawings. Those skilled in the art will be able to implement the invention based on these teachings. Before the present invention is described in detail with reference to the accompanying drawings, it is to be noted that:
the technical solutions and features provided in the present invention in the respective sections including the following description may be combined with each other without conflict.
Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
With respect to terms and units in the present invention. The terms "comprising," "having," and any variations thereof in the description and claims of this invention and the related sections are intended to cover non-exclusive inclusions.
The invention discloses a cathode material precursor coprecipitation reaction device, which comprises:
the reaction kettle 21 is used for containing precursor slurry, the inner cavity of the reaction kettle 21 is divided into a reaction area and a concentration area circumferentially arranged around the reaction area, and the upper end and the lower end of the reaction area are communicated with the concentration area to form a slurry circulation loop;
the stirring component 2 is arranged in a reaction area in the reaction kettle 21 and used for uniformly mixing the precursor slurry in the reaction kettle 21;
and the filtering assembly 23 is arranged in the concentration area of the reaction kettle 21 and is used for intercepting the precursor in the reaction kettle 21 to obtain concentrated precursor slurry and filtering out filtrate.
The inner cavity of the reaction kettle 21 is divided into a reaction area and a concentration area circumferentially surrounding the reaction area by a guide cylinder 212 arranged between the stirring assembly 2 and the filtering assembly 23, and the guide cylinder 212 is a hollow cylinder with two open ends.
The guide shell 212 is fixed by an anti-rotation baffle.
The guide shell 212 is hung through a bracket.
The diameter of the guide shell 212 and the diameter of the reaction kettle 21 are in the proportion range
And the filtering components 23 are circumferentially arranged in the concentration area of the reaction kettle 21 at intervals around the stirring component 2.
The input unit is used for inputting the precursor slurry into the reaction zone.
The input unit includes a feed pipe 211 extending into reaction vessel 21, the outlet end of feed pipe 211 being located in the upper region of the reaction zone.
The filter assembly 23 comprises a filter liquid pipe fixed in the reaction kettle 21 and a filter element fixed on the filter liquid pipe at intervals, the filter liquid pipe comprises an outer ring pipe 231 and an inner ring pipe 232 which are arranged along the radial outside-in direction of the reaction kettle 21, the outer ring pipe 231 and the inner ring pipe 232 are both connected with a clear liquid system through a clear liquid outlet pipe 233, and the outer ring pipe 231 and the inner ring pipe 232 are sealed pipes.
As shown in fig. 8, the thickener includes a reaction kettle 21 for accommodating the precursor slurry, an inner cavity of the reaction kettle 21 is divided into a reaction region and a concentration region circumferentially arranged around the reaction region, and upper and lower ends of the reaction region are both communicated with the concentration region to form a slurry circulation loop; the stirring component 22 is arranged in a reaction area in the reaction kettle 21 and used for uniformly mixing the precursor slurry in the reaction kettle 21; and the filtering component 23 is arranged in the concentration area of the reaction kettle 21 and used for intercepting the precursor in the reaction kettle 21 to obtain concentrated precursor slurry and filtering out filtrate. The inner cavity of the reaction kettle 21 is divided into a reaction area and a concentration area circumferentially surrounding the reaction area by a guide shell 4 arranged between the stirring component 22 and the filtering component 23, and the guide shell 4 is a hollow cylinder with two open ends.
Preferably, the guide shell 4 is fixed by an anti-rotation baffle. The guide shell 4 is hung through a bracket. The diameter of the guide shell 4 and the diameter of the reaction kettle 21 are in the proportion range. The filtering components 23 are circumferentially arranged in the concentration area of the reaction kettle 21 at intervals around the stirring component 22.
The input unit is used for inputting the precursor slurry into the reaction zone.
The input unit includes a feed pipe 211 extending into reaction vessel 21, the outlet end of feed pipe 211 being located in the upper region of the reaction zone.
As shown in fig. 2, the filter assembly 23 includes a filter liquid tube fixed in the reaction kettle 21, and a filter element fixed on the filter liquid tube at intervals, the filter liquid tube includes an outer ring tube 231 and an inner ring tube 232 arranged along the radial direction of the reaction kettle 21 from outside to inside, the outer ring tube 231 and the inner ring tube 232 are both externally connected to a clear liquid system through a clear liquid outlet tube 233, and both the outer ring tube 231 and the inner ring tube 232 are sealed tubes. The outer ring pipe 231 and the inner ring pipe 232 are communicated through an elbow 236.
Of course, the outer ring tube 231 and the inner ring tube 232 may also be connected in other ways as mentioned in the present invention.
The invention is further illustrated below by taking the material circulation of the ternary precursor slurry in the thickener as an example:
when the ternary precursor slurry is produced, a concentration zone at the outer side of the guide shell is required to be used as a secondary reaction zone, and a reaction zone at the inner side of the guide shell is required to be used as a main reaction zone. Therefore, after the precursor slurry enters the reaction zone, a large amount of ions are crystallized on original solid particles along with the reaction, crystals grow up, meanwhile, the ion supersaturation degree in the mixed solution is reduced, the reaction speed is reduced, the ion supersaturation degree in a short time is reduced, under the action of the stirring assembly 22, the material with low supersaturation degree enters the concentration zone for particle diameter redistribution and morphology adjustment, and the operation is circulated in the way until the final ternary precursor product is obtained. The positive electrode material precursor coprecipitation reaction equipment divides an inner cavity in the reaction kettle into a reaction area and a concentration area, the stirring assembly stirs precursor slurry in the reaction kettle to form a liquid flow when in work, the slurry circulates in the circulation loop due to the partition effect, so that the precursor slurry firstly carries out main reaction in the reaction area and then carries out secondary reaction in the concentration area, and the precursor slurry can be directly concentrated after the secondary reaction, so that the functions of the main reaction kettle, the secondary reaction kettle and a concentrator in the prior art are replaced, the equipment quantity and the production cost are reduced, the slurry can also play a role in washing the surface of the filtering assembly in the circulation process, and the continuous concentration and enrichment of materials in the slurry can be ensured.
The contents of the present invention have been explained above. Those skilled in the art will be able to implement the invention based on these teachings. All other embodiments, which can be derived by a person skilled in the art from the above description without inventive step, shall fall within the scope of protection of the present invention.
The invention also provides a coprecipitation reaction system of the precursor of the anode material, which comprises the following components:
the cathode material precursor coprecipitation reaction equipment 2 comprises a reaction kettle 21, an input unit, a stirring assembly 222 and a filtering assembly 23, wherein the reaction kettle 21 is used for accommodating precursor slurry and allowing the precursor slurry to react therein, the stirring assembly 222 is arranged in the reaction kettle 21 and is used for stirring the precursor slurry in the reaction kettle 21, and the filtering assembly 23 is arranged in the reaction kettle 21 and is used for intercepting the precursor in the reaction kettle 21 to obtain concentrated precursor slurry and filtering out filtered liquid;
go out clear subassembly, including the play clear liquid pipe 11 with filter assembly 23 play clear liquid mouth intercommunication, set up heat sink 5 on going out clear liquid pipe 11, set up the hose pump 12 in heat sink 5 rear end.
And the inlet and the outlet of the hose pump are provided with thin-wall ball valves 4.
Still including setting up the heat sink 5 on going out liquid pipe 11, heat sink 5 sets up in the front end of hose pump.
The cooling device 5 is a plate type heat exchange device, a straight pipe heat exchange device or a spiral pipe heat exchange device 5.
Also included is a regeneration assembly comprising:
a backflushing container 6 for containing backflushing gas/backflushing liquid, an outlet of the backflushing container 6 being connected with a filtrate outlet of the filter assembly 23 to be regenerated;
the air inlet control component is used for controlling the regenerated gas to be input into the backflushing container 6;
the liquid inlet control component is used for controlling the regenerated liquid to be input into the backflushing container 6;
the backflushing control component is used for controlling the regenerated gas/regenerated liquid to be output from the outlet of the backflushing container 6 to the backflushing container 6;
the pure water control component is used for controlling pure water to be input into the backflushing container 6;
wherein the outlet of the backflushing container 6 is connected with the emptying assembly.
And a heat insulation structure is arranged on the outer surface of the reaction kettle 21.
The heat preservation structure comprises a jacket 3 wrapped on the outer surface of the reaction kettle 21, and further comprises a heat preservation liquid inlet 31 and a heat preservation liquid outlet 32 which are arranged on the jacket 3.
The filtering assembly 23 is arranged in the reaction kettle 21 around the stirring assembly 222 in a circumferential direction.
The filter assembly 23 comprises a filter liquid pipe fixed in the reaction kettle 21 and filter elements fixed on the filter liquid pipe at intervals, the filter liquid pipe comprises an outer ring pipe 231 and an inner ring pipe 232 which are arranged along the radial outside-in direction of the reaction kettle 21, the outer ring pipe 231 and the inner ring pipe 232 are connected with a clear liquid outlet system through the clear liquid pipe, and the outer ring pipe 231 and the inner ring pipe 232 are sealing pipes.
The outer ring pipe 231 is connected with the clear liquid outlet pipe 11 through the outside of the clear liquid filtering pipe, and the inner ring pipe 232 is connected and communicated with the clear liquid filtering pipe through an elbow pipe.
The anode material precursor coprecipitation reaction equipment 2 comprises
The reaction kettle 21 is used for accommodating the precursor slurry and allowing the precursor slurry to react therein;
an input unit for inputting the precursor slurry into the reaction kettle 21;
the stirring component 222 is arranged in the reaction kettle 21 and is used for stirring the precursor slurry in the reaction kettle 21;
the filtering component 23 is arranged in the reaction kettle 21 and used for intercepting the precursor in the reaction kettle 21 to obtain concentrated precursor slurry and filtering out filtered liquid;
and a heat insulation structure is arranged on the outer surface of the reaction kettle 21.
The heat preservation structure comprises a jacket 3 wrapped on the outer surface of the reaction kettle 21, and further comprises a heat preservation liquid inlet 31 and a heat preservation liquid outlet 32 which are arranged on the jacket 3.
The heat preservation structure is a structure for maintaining the temperature in the reaction kettle 21 at 50-60 ℃.
A discharging pipe communicated with the inside of the reaction kettle 21 is vertically arranged at the bottom of the reaction kettle 21 downwards, the discharging pipe penetrates through the jacket 3 to the outside of the reaction kettle 21, and the cross part of the discharging pipe and the jacket 3 is welded and sealed.
The filter assembly 23 comprises a filter liquid pipe fixed in the reaction kettle 21 and filter elements fixed on the filter liquid pipe at intervals, the filter liquid pipe comprises an outer ring pipe 231 and an inner ring pipe 232 which are arranged along the radial outside-in direction of the reaction kettle 21, the outer ring pipe 231 and the inner ring pipe 232 are connected with a clear liquid outlet system through the clear liquid pipe, and the outer ring pipe 231 and the inner ring pipe 232 are sealing pipes.
The bent pipe penetrates through the jacket 3 at the bottom of the reaction kettle 21 and extends to the outside of the reaction kettle 21, and the intersection of the filter liquor pipe and the jacket 3 is welded and sealed.
The inner ring pipe 232 is disposed at a position higher than the outer ring pipe 231.
The invention discloses a coprecipitation reaction system of a precursor of a positive electrode material, which comprises:
the cathode material precursor coprecipitation reaction equipment 2 comprises a reaction kettle 21, an input unit, a stirring assembly 222 and a filtering assembly 23, wherein the reaction kettle 21 is used for accommodating precursor slurry and allowing the precursor slurry to react therein, the stirring assembly 222 is arranged in the reaction kettle 21 and is used for stirring the precursor slurry in the reaction kettle 21, and the filtering assembly 23 is arranged in the reaction kettle 21 and is used for intercepting the precursor in the reaction kettle 21 to obtain concentrated precursor slurry and filtering out filtered liquid;
and the negative pressure pumping device is connected with a filtrate outlet of the filtering assembly 23 and is used for pumping the filtrate out of the reaction kettle 21. The negative pressure clear liquid discharging device comprises a clear liquid discharging pipe 11 communicated with a clear liquid filtering outlet, a negative pressure pump communicated with the clear liquid discharging pipe 11, and a pressure transmitter 11, a pressure gauge 12, a temperature transmitter 13 and a pneumatic ball valve which are arranged on the clear liquid discharging pipe 11.
The filtering components 23 at least comprise two groups of filtering components 23, and clear liquid outlets of each group of filtering components 23 are respectively connected with the corresponding clear liquid outlet pipes 11 after being converged.
The maximum negative pressure of the negative pressure pump is-0.8 bar, and the maximum output pressure of the negative pressure pump outlet is 2-6 bar.
The filter assembly 23 comprises a filter liquid pipe fixed in the reaction kettle 21 and a filter element fixed on the filter liquid pipe at intervals, the filter liquid pipe comprises an outer ring pipe 231 and an inner ring pipe 232 which are arranged along the radial outside-in direction of the reaction kettle 21, the outer ring pipe 231 and the inner ring pipe 232 are connected with a clear liquid system through a clear liquid outlet pipe 11, and the outer ring pipe 231 and the inner ring pipe 232 are sealed pipes.
The outer circle pipe 231 is connected with a clear liquid discharging system through a clear liquid discharging pipe 11, and the inner circle pipe 232 is connected and conducted with the clear liquid discharging pipe 11 through a bent pipe.
The clear liquid outlet pipe 11 is communicated with a clear liquid filtering outlet arranged at the bottom of the reaction kettle 21.
The inner ring pipe 232 is disposed at a position higher than the outer ring pipe 231.
As shown in fig. 1, the precursor system of the present invention comprises the following structural modules: the device comprises a positive electrode material precursor coprecipitation reaction device 2, a cleaning component and a regeneration component.
The cathode material precursor coprecipitation reaction equipment 2 comprises a reaction kettle 21, an input unit, a stirring assembly 222 and a filtering assembly 23, wherein the reaction kettle 21 is used for accommodating precursor slurry and allowing the precursor slurry to react therein, the stirring assembly 222 is arranged in the reaction kettle 21 and is used for stirring the precursor slurry in the reaction kettle 21, and the filtering assembly 23 is arranged in the reaction kettle 21 and is used for intercepting the precursor in the reaction kettle 21 to obtain concentrated precursor slurry and filtering out a filtrate. And a heat insulation structure is arranged on the outer surface of the reaction kettle 21.
The heat preservation structure comprises a jacket 3 wrapped on the outer surface of the reaction kettle 21, and further comprises a heat preservation liquid inlet 31 and a heat preservation liquid outlet 32 which are arranged on the jacket 3. The heat preservation structure is a structure for maintaining the temperature in the reaction kettle 21 at 50-60 ℃. A discharging pipe communicated with the inside of the reaction kettle 21 is vertically arranged at the bottom of the reaction kettle 21 downwards, the discharging pipe penetrates through the jacket 3 to the outside of the reaction kettle 21, and the cross part of the discharging pipe and the jacket 3 is welded and sealed.
Wherein, the clear liquid outlet component comprises a clear liquid outlet pipe 11 communicated with a clear liquid outlet of the filtering component 23 and a hose pump 12 arranged on the clear liquid outlet pipe 11. And the inlet and the outlet of the hose pump are provided with thin-wall ball valves 4. Still including setting up the heat sink 5 on going out the liquid pipe 11, heat sink 5 sets up in the front end of hose pump. The cooling device 5 is a plate type heat exchange device, a straight pipe heat exchange device or a spiral pipe heat exchange device 5.
The discharging assembly is preferably a negative pressure discharging device and a negative pressure pumping device, and is connected with the filtrate outlet of the filtering assembly 23, and is used for pumping the filtrate out of the reaction kettle 21. The negative pressure clear liquid discharging device comprises a clear liquid discharging pipe 11 communicated with a clear liquid filtering outlet, a negative pressure pump communicated with the clear liquid discharging pipe 11, and a pressure transmitter 11, a pressure gauge 12, a temperature transmitter 13 and a pneumatic ball valve which are arranged on the clear liquid discharging pipe 11. The filtering components 23 at least comprise two groups of filtering components 23, and clear liquid outlets of each group of filtering components 23 are respectively connected with the corresponding clear liquid outlet pipes 11 after being converged. The maximum negative pressure of a suction inlet of the negative pressure pump is-0.8 bar, and the maximum output pressure of an outlet of the negative pressure pump is about 3 bar. The invention provides the following negative pressure discharging modes:
the vacuum pump purge characteristics are as in table 1:
TABLE 1
The discharge characteristics of the diaphragm pump are shown in table 2 below:
TABLE 2
Hose pump out characteristics are shown in table 3 below:
TABLE 3
The water ring pump out characteristics are shown in table 4 below:
TABLE 4
As can be seen from tables 1-4 above, the use of the hose pump works best in the positive electrode material precursor coprecipitation reaction system.
The regeneration assembly includes: a backflushing container 6 for containing backflushing gas/backflushing liquid, an outlet of the backflushing container 6 being connected with a filtrate outlet of the filter assembly 23 to be regenerated; the air inlet control component is used for controlling the regenerated gas to be input into the backflushing container 6; the liquid inlet control component is used for controlling the regenerated liquid to be input into the backflushing container 6; the backflushing control component is used for controlling the regenerated gas/regenerated liquid to be output from the outlet of the backflushing container 6 to the backflushing container 6;
the pure water control component is used for controlling pure water to be input into the backflushing container 6; wherein the outlet of the backflushing container 6 is connected with the emptying assembly.
The positive electrode material precursor coprecipitation reaction system is applied to the production process of the ternary precursor, ternary precursor slurry is pumped by a negative pressure pump to act on the positive electrode material precursor coprecipitation reaction equipment 2 to realize enrichment concentration and reaction, the reaction temperature of the precursor in the reaction kettle 21 is ensured by a heat insulation structure, the action of the negative pressure pump, preferably a hose pump, on the negative pressure pumping is more accurately regulated and controlled, the stability of the clear volume of the whole system is ensured, and the stable quality of the precursor product is ensured. The filter component is regenerated periodically through the regeneration component, so that the continuity of production is ensured. Because the normal working temperature of the hose pump is about 40 ℃ and can bear 50 ℃ in a short time, the temperature is preferably reduced from 60 ℃ to 40 ℃ in the negative pressure pump cooling device 5.
As shown in fig. 2-3, the filtering unit includes a filtering liquid pipe fixed in the reaction kettle 21, and a filtering assembly 235 fixed on the filtering liquid pipe at intervals, the filtering liquid pipe includes an outer ring pipe 231 and an inner ring pipe 232 arranged along the radial direction of the reaction kettle 21 from outside to inside, both the outer ring pipe 231 and the inner ring pipe 232 are externally connected with a clear liquid system through a clear liquid outlet pipe 233, and both the outer ring pipe 231 and the inner ring pipe 232 are sealed pipes.
The invention also provides the following four different connection modes of the filter liquor pipe and the liquor outlet pipe:
the first connection is shown in fig. 4: the outer ring pipe 231 is externally connected with a clear liquid discharging system through a clear liquid discharging pipe 233, and the inner ring pipe 232 and the outer ring pipe 231 are connected and communicated through a horizontal straight pipe 234. Wherein, two ends of the horizontal straight pipe 234 are respectively welded on the inner ring pipe 232 and the outer ring pipe 231 through T-shaped welding structures. When the clear liquid outlet on the reaction kettle 21 is arranged on the bottom of the reaction kettle 21, the clear liquid outlet pipe 233 can be a straight pipe which vertically extends downwards to the outside of the reaction kettle 21 and is communicated with the clear liquid outlet component; when the clear liquid outlet on the reaction vessel 21 is disposed on the side of the reaction vessel 21, the clear liquid outlet pipe 233 may be a bent pipe extending out of the reaction vessel 21 to communicate with the clear liquid outlet assembly.
The second connection is shown in fig. 5: the outer ring pipe 231 and the inner ring pipe 232 are located at the same height, the outer ring pipe 231 is externally connected with a clear liquid discharging system through a clear liquid discharging pipe 233, and the inner ring pipe 232 is connected and communicated with the clear liquid discharging pipe 233 through an elbow pipe 236. When the clear liquid outlet on the reaction kettle 21 is arranged on the bottom of the reaction kettle 21, the clear liquid outlet pipe 233 can be a straight pipe which vertically extends downwards to the outside of the reaction kettle 21 and is communicated with the clear liquid outlet component; when the clear liquid outlet on the reaction vessel 21 is disposed on the side of the reaction vessel 21, the clear liquid outlet pipe 233 may be a bent pipe extending out of the reaction vessel 21 to communicate with the clear liquid outlet assembly.
The third connection is shown in fig. 6: the setting height of the inner ring pipe 232 is higher than that of the outer ring pipe 231, the outer ring pipe 231 is externally connected with a clear liquid discharging system through a clear liquid discharging pipe 233, and the inner ring pipe 232 is connected and communicated with the clear liquid discharging pipe 233 through an elbow pipe 236. When the clear liquid outlet on the reaction kettle 21 is arranged on the bottom of the reaction kettle 21, the clear liquid outlet pipe 233 can be a straight pipe vertically extending downwards to the outside of the reaction kettle 21 and communicated with the clear liquid outlet assembly; when the clear liquid outlet on the reaction vessel 21 is disposed on the side of the reaction vessel 21, the clear liquid outlet pipe 233 may be a bent pipe extending out of the reaction vessel 21 to communicate with the clear liquid outlet assembly.
The fourth connection is shown in fig. 7: the outer ring pipe 231 and the inner ring pipe 232 are independently arranged, and the inner ring pipe 232 and the outer ring pipe 231 are respectively externally connected with a clear liquid discharging system through independent clear liquid discharging pipes 233. When the clear liquid outlet on the reaction kettle 21 is arranged on the bottom of the reaction kettle 21, the clear liquid outlet pipe 233 can be a straight pipe which vertically extends downwards to the outside of the reaction kettle 21 and is communicated with the clear liquid outlet component; when the clear liquid outlet on the reaction vessel 21 is disposed on the side of the reaction vessel 21, the clear liquid outlet pipe 233 may be a bent pipe extending out of the reaction vessel 21 to communicate with the clear liquid outlet assembly. In this connection, in order to mount the clear liquid discharge pipe 233 more easily, one end of the inner ring pipe 232 is longer than the corresponding end of the outer ring pipe 231, the clear liquid discharge pipe 233 of the inner ring is connected to and conducted with the end of the inner ring pipe 232, and the clear liquid discharge pipe 233 of the outer ring is connected to and conducted with the end of the outer ring pipe 231.
As a preferred embodiment with reference to fig. 2 to 3, the reaction kettle 21 is provided with a fixing member in the radial direction, and the inner ring pipe 232 and the outer ring pipe 231 are arranged on the fixing member from inside to outside. The fixing piece is a fixing rod 121, and two ends of the inner ring tube 232 and the outer ring tube 231 are respectively connected with the fixing rod 121 through welding; or the two ends of the inner ring tube 232 and the outer ring tube 231 are fixed on the fixing rod 121 through the hoop 1221. The inner ring pipe 232 and the outer ring pipe 231 are arc pipes. The filter assembly 23 comprises four filter units, and the central angle of the arc-shaped pipe is 60 degrees.
When the filtering component is installed, the upper end and the lower end of the filtering component can be fixed or only the lower end of the filtering component is fixed. When the filter assembly is installed, the lower end of the filter assembly is connected to the mounting hole formed in the upper end of the filter liquid pipe through threads, and the upper end of the filter assembly is fixedly connected with the reaction kettle through angle steel. The filter component can adopt one of a titanium alloy filter element, a 316 stainless steel filter element, a 2205 duplex stainless steel filter element, a silicon carbide material, PVDF and other materials. The single end is fixed on the filter assembly, and the filter element is broken when the length of the filter assembly is long, so that the double end fixing is adopted when the filter assembly with the length of more than 500mm is applied to the thickener of the invention.
Therefore, the temperature reduction device is arranged on the clear liquid outlet pipe in the production operation process of the cathode material precursor coprecipitation reaction system, so that the secondary reaction of reactants in the filtrate is inhibited, the growth of crystals in the clear liquid outlet pipe is inhibited, and the problem of blockage of the clear liquid outlet pipe generated after the secondary reaction kettle and the concentrator are combined into a whole is effectively solved; the rear end of heat sink sets up the hose pump on going out the liquid pipe, the excellent negative pressure pumping function of hose pump has guaranteed on the one hand that the strained clear liquid can carry out stable output under negative pressure environment, the environment of the little positive pressure clear liquid that original dependence main reation kettle and inferior reation kettle realized has been solved, another convenience is under the guarantee of the heat sink of its front end setting, the characteristic that hose pump self is not high temperature resistant has been agreed with well, the normal use of hose pump has been ensured, from this heat sink and hose pump have realized the mutual gain in the functional effect.
It should be noted that the structural features of the above four connection modes can be combined into other connection modes by arranging, and these connection modes are also within the protection scope of the present invention.
The contents of the present invention have been explained above. Those skilled in the art will be able to implement the invention based on these teachings. All other embodiments, which can be derived by a person skilled in the art from the above description without inventive step, shall fall within the scope of protection of the present invention.
Claims (8)
1. Positive pole material precursor coprecipitation reaction equipment, its characterized in that includes:
the reaction kettle (21) is used for containing precursor slurry, the inner cavity of the reaction kettle (21) is divided into a reaction area and a concentration area circumferentially arranged around the reaction area, and the upper end and the lower end of the reaction area are communicated with the concentration area to form a slurry circulation loop;
the stirring assembly (22) is arranged in a reaction zone in the reaction kettle (21) and is used for stirring the precursor slurry in the reaction kettle (21);
and the filtering component (23) is arranged in the concentration area of the reaction kettle (21) and is used for intercepting the precursor in the reaction kettle (21) to obtain concentrated precursor slurry and filtering out filtrate.
2. The cathode material precursor coprecipitation reaction apparatus according to claim 1, wherein an inner cavity of the reaction vessel (21) is divided into a reaction region and a concentration region circumferentially surrounding the reaction region by a guide cylinder (212) disposed between the stirring assembly (22) and the filtering assembly (23), and the guide cylinder (212) is a hollow cylinder with two open ends.
3. The cathode material precursor coprecipitation reaction apparatus of claim 2, wherein the guide shell (212) is fixed by an anti-rotation baffle.
4. The cathode material precursor coprecipitation reaction apparatus of claim 2, wherein the guide shell (212) is hung by a bracket.
5. The cathode material precursor coprecipitation reaction apparatus of claim 1, wherein the filter assemblies (23) are circumferentially spaced around the stirring assembly (22) in a concentration zone of the reaction vessel (21).
6. The cathode material precursor co-precipitation reaction device according to claim 1, wherein the input unit is configured to input a precursor slurry into the reaction zone.
7. The cathode material precursor coprecipitation reaction apparatus of claim 7, wherein the input unit comprises a feed pipe (211) extending into the reaction vessel (21), and an outlet end of the feed pipe (211) is located in an upper region of the reaction zone.
8. The cathode material precursor coprecipitation reaction apparatus according to claim 1, wherein the filter assembly (23) includes a filter solution tube fixed in the reaction vessel (21), and a filter element fixed on the filter solution tube at intervals, the filter solution tube includes an outer ring tube (231) and an inner ring tube (232) arranged along a radial direction of the reaction vessel (21) from outside to inside, the outer ring tube (231) and the inner ring tube (232) are both connected to a clear solution system through a clear solution outlet tube (233), and the outer ring tube (231) and the inner ring tube (232) are both sealed tubes.
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