CN114931919A - Positive electrode material precursor coprecipitation reaction equipment and coprecipitation reaction system - Google Patents
Positive electrode material precursor coprecipitation reaction equipment and coprecipitation reaction system Download PDFInfo
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- CN114931919A CN114931919A CN202210366790.XA CN202210366790A CN114931919A CN 114931919 A CN114931919 A CN 114931919A CN 202210366790 A CN202210366790 A CN 202210366790A CN 114931919 A CN114931919 A CN 114931919A
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- 239000002243 precursor Substances 0.000 title claims abstract description 280
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 182
- 238000000975 co-precipitation Methods 0.000 title claims abstract description 100
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 284
- 238000003756 stirring Methods 0.000 claims abstract description 130
- 239000002002 slurry Substances 0.000 claims abstract description 114
- 238000007599 discharging Methods 0.000 claims abstract description 71
- 238000010992 reflux Methods 0.000 claims abstract description 47
- 239000010406 cathode material Substances 0.000 claims abstract description 44
- 230000001276 controlling effect Effects 0.000 claims abstract description 38
- 239000000706 filtrate Substances 0.000 claims abstract description 24
- 230000001105 regulatory effect Effects 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims description 96
- 238000000034 method Methods 0.000 claims description 23
- 238000010926 purge Methods 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 31
- 239000006228 supernatant Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 39
- 238000011010 flushing procedure Methods 0.000 description 27
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- 238000000429 assembly Methods 0.000 description 24
- 238000004519 manufacturing process Methods 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 239000010405 anode material Substances 0.000 description 18
- 230000008569 process Effects 0.000 description 17
- 239000000463 material Substances 0.000 description 16
- 238000009434 installation Methods 0.000 description 14
- 230000004907 flux Effects 0.000 description 12
- 239000007789 gas Substances 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000012065 filter cake Substances 0.000 description 9
- 230000008929 regeneration Effects 0.000 description 9
- 238000011069 regeneration method Methods 0.000 description 9
- 238000003466 welding Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 6
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- 238000004140 cleaning Methods 0.000 description 5
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- 239000012066 reaction slurry Substances 0.000 description 4
- 239000012266 salt solution Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 2
- 229940044175 cobalt sulfate Drugs 0.000 description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000011565 manganese chloride Substances 0.000 description 2
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- 229940099607 manganese chloride Drugs 0.000 description 2
- 229940099596 manganese sulfate Drugs 0.000 description 2
- 239000011702 manganese sulphate Substances 0.000 description 2
- 235000007079 manganese sulphate Nutrition 0.000 description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
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- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 229910001039 duplex stainless steel Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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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
- B01J19/1868—Stationary reactors having moving elements inside resulting in a loop-type movement
- B01J19/1881—Stationary reactors having moving elements inside resulting in a loop-type movement externally, i.e. the mixture leaving the vessel and subsequently re-entering it
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
-
- 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
- B01J19/0053—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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00182—Controlling or regulating processes controlling the level of reactants in the reactor vessel
-
- 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)
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Abstract
The invention discloses a coprecipitation reaction device for a precursor of a positive electrode material, which comprises a main body; a filter assembly; a stirring unit; the backflow unit is used for refluxing the precursor slurry in the main body to the reaction kettle; a supernatant discharging unit for discharging the filtrate to the outside of the main body; the first liquid level control unit comprises a clear valve for regulating and controlling the discharge flow of the filtered liquid, and the clear valve is used for controlling the interlocking of a first liquid level meter arranged on the reaction kettle; and the second liquid level control unit comprises a second liquid level meter arranged on the main body and a reflux valve used for regulating and controlling the reflux amount of the concentrated precursor slurry, and the second liquid level meter and the reflux valve are controlled in an interlocking manner. The invention also discloses a coprecipitation reaction system formed by the coprecipitation reaction equipment for the precursor of the cathode material. The invention ensures the stability of the system and the quality of the finally produced product.
Description
Technical Field
The invention relates to the technical field of precursor production, in particular to a coprecipitation reaction device and a coprecipitation reaction system for a precursor of a positive electrode material.
Background
The precursor slurry 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 filtering, washing and drying the reaction slurry after the granularity reaches a preset value to obtain the ternary precursor.
In order to improve the solid content of the precursor slurry and optimize the shape of the precursor, a concentration device which integrates the filtering and concentrating functions with the stirring function is provided in the market and is used for concentrating the ternary precursor after reaction in the reaction kettle, so that the enrichment and concentration of the precursor slurry are realized. The applicant finds that the technical problems of unstable liquid level of a reaction kettle and unstable liquid level in concentration equipment often occur in the production process, so that the product quality of the obtained precursor of the cathode material is unstable.
Disclosure of Invention
In practical production research, the applicant finds that technical problems of unstable liquid level of a reaction kettle and unstable liquid level in concentration equipment often occur in the production process, and the technical problems can cause unstable product quality of the obtained anode material precursor. Specifically, the method comprises the following steps: the sum of the total amount of the slurry in the reaction kettle and the total amount of the slurry in the concentration equipment determines the working volume of the whole coprecipitation reaction system, and the working volume determines the total retention time of reaction materials and the concentration of the materials in the reaction kettle and also influences the stirring flow field. If the liquid level in the reaction kettle and the concentration equipment is too low, the total volume of the slurry is too small, so that the retention time is shortened at a higher concentration, the clear flux of the filtered liquid of the system is influenced at a higher concentration, the reaction is not completely carried out due to the shortened retention time, so that the penetration and the material waste are caused, and if the liquid level is too low, the upper paddle is failed and the stirring effect is influenced; if the liquid level is too high, the total stirring power will increase, resulting in an excessive stirring load. Therefore, the invention also provides a coprecipitation reaction device for the anode material precursor, aiming at the problem, so as to solve the technical problems that the liquid level of the reaction kettle is unstable and the liquid level of the coprecipitation reaction device for the anode material precursor is unstable in the prior art, and further cause the quality of the obtained anode precursor product to be unstable.
In order to achieve the above object, the present invention provides a co-precipitation reaction apparatus for precursors of positive electrode materials, comprising
A body for containing a precursor slurry;
the filtering component is arranged in the main body and used for intercepting the precursor in the main body to obtain concentrated precursor slurry and filtering out filtrate;
the stirring unit is arranged in the main body and is used for stirring the precursor slurry in the main body;
the pump unit is used for pumping the precursor slurry in the reaction kettle into the main body;
the backflow unit is used for refluxing the precursor slurry in the main body to the reaction kettle;
the supernatant discharging unit is used for discharging the filtered liquid out of the main body;
the first liquid level control unit comprises a clear liquid outlet valve for regulating and controlling the discharge flow of the filtered clear liquid, and the clear liquid outlet valve is used for controlling the first liquid level meter arranged on the reaction kettle in an interlocking manner;
and the second liquid level control unit comprises a second liquid level meter arranged on the main body and a reflux valve used for regulating and controlling the reflux amount of the concentrated precursor slurry, and the second liquid level meter and the reflux valve are controlled in an interlocking manner.
Furthermore, the first liquid level meter and the clear valve are subjected to interlocking control in a PID control mode.
Furthermore, go out the qing dynasty unit including connecting filtering component and filtering clear liquid export to the play qing dynasty outside the main part manage, set up the play qing dynasty pump on going out the qing dynasty pipe, it sets up on going out the qing dynasty pipe to go out the clear valve.
Furthermore, go out the scavenge valve including setting up manometer, play clear flowmeter, play clear pneumatic ball valve on going out the scavenge pipe.
Furthermore, the second liquid level meter and the return valve are controlled in an interlocking manner in a PID control mode.
Further, the backflow unit comprises a backflow pipe connecting the main body and the reaction kettle, and the backflow valve is arranged on the backflow pipe.
Further, the return valve is an electric regulating valve.
Furthermore, a backflow stop valve is further arranged on the backflow pipe.
Further, the pump material unit includes the inlet pipe of connecting reation kettle and main part, sets up charge-in pump, feeding flowmeter and the pneumatic ball valve of feeding on the inlet pipe.
A co-precipitation reaction system comprising:
the reaction kettle is used for reacting reactants therein to generate precursor slurry;
the anode material precursor coprecipitation reaction equipment comprises a main body, a filtering assembly and a stirring unit, wherein the filtering assembly and the stirring unit are installed in the main body, the main body is used for accommodating precursor slurry, and the filtering assembly is used for intercepting the precursor in the main body to obtain concentrated precursor slurry and filtering out a filtrate; the stirring unit is used for stirring the precursor slurry in the main body;
the pump unit is used for pumping the precursor slurry in the reaction kettle into the main body;
the backflow unit is used for refluxing the precursor slurry in the main body to the reaction kettle;
the supernatant discharging unit is used for discharging the filtered liquid out of the main body;
the first liquid level control unit comprises a first liquid level meter arranged on the reaction kettle and a clear liquid outlet valve used for regulating and controlling the discharge flow of the filtered clear liquid, and the first liquid level meter and the clear liquid outlet valve are in interlocking control;
and the second liquid level control unit comprises a second liquid level meter arranged on the main body and a reflux valve used for regulating and controlling the reflux amount of the concentrated precursor slurry, and the second liquid level meter and the reflux valve are controlled in an interlocking manner.
Therefore, the clear liquid outlet valve and the first liquid level meter are controlled in an interlocking mode through the first liquid level control unit, namely the opening degree of the clear liquid outlet valve is correspondingly adjusted according to the reading of the first liquid level control unit, so that the liquid level in the reaction kettle is controlled to be kept stable in the production process; and the second liquid level meter and the reflux valve are subjected to interlocking control through the second liquid level control unit, namely, the opening degree of the reflux valve is correspondingly adjusted according to the reading of the second liquid level control unit, so that the liquid level in the anode material precursor coprecipitation reaction equipment main body is controlled to be kept stable in the production process. The size of the clear liquid outlet quantity of the filtered liquid of the main body is consistent with the size of the liquid inlet quantity of the reaction kettle, and the liquid level of the ternary precursor slurry in the main body is controlled to be kept stable, so that the total reaction residence time of the ternary precursor slurry, the concentration of materials in the reaction kettle, the stirring flow field and the system clear liquid outlet quantity are ensured, and the stable quality of the finally produced ternary precursor product of the anode material is ensured.
The invention also provides a coprecipitation reaction device for the precursor of the anode material, which is used for solving the problems of different sizes of particles of the precursor product, breakage of a filter assembly and damage to the surfaces of the particles caused by improper arrangement positions of the stirring blades in the prior art.
The applicant finds that in actual production research, when the stirring paddle and the filtering component are arranged too far, precursor slurry can not be sufficiently stirred, and the problem that the size of precursor product particles is uneven is caused; when the stirring paddle blade and the filter assembly are arranged too close to each other, the end part of the stirring paddle blade on the radial direction of the tank body can be in contact with a filter cake formed by the filter surface of the filter assembly or directly form stronger acting force on the filter surface of the filter assembly by stirring formed fluid, or indirectly act on the filter surface of the filter assembly through the stronger acting force formed by the filter cake on the filter surface of the filter assembly, so that the filter assembly is broken and the particle surface of a precursor product is damaged.
In order to achieve the above object, the present invention provides a cathode material precursor coprecipitation reaction apparatus, including:
a tank for containing a precursor slurry;
the input unit is used for inputting the precursor slurry into the tank body;
the stirring assembly is arranged in the tank body and is used for stirring the precursor slurry in the tank body;
the filtering component is annularly distributed in the tank body around the stirring component and is used for intercepting the precursor in the tank body to obtain concentrated precursor slurry and filtering out filtrate;
the end part of the stirring blade of the stirring assembly in the radial direction of the tank body forms a first cylindrical surface in the circumferential direction during stirring, the positions, closest to the stirring blade, of all the filtering assemblies are connected into a second cylindrical surface in the circumferential direction, and the ratio of the distance between the first cylindrical surface and the second cylindrical surface in the radial direction to the inner diameter of the tank body is 5% -15%.
Further, the ratio of the distance between the first cylindrical surface and the second cylindrical surface in the radial direction to the inner diameter of the can body is 6% -8%.
Further, the distance between the first cylindrical surface and the second cylindrical surface in the radial direction is 15-25 mm.
Further, the distance between the first cylindrical surface and the second cylindrical surface in the radial direction is 100-150 mm.
Further, the ratio of the width of the gap to the inner diameter of the main body is 6-8%.
Further, the stirring linear speed of the stirring component is 5-10 m/s.
Further, the stirring linear speed of the stirring component is 7-8 m/s.
Further, the filter assembly is a metal filter element.
Furthermore, the filtering component comprises a filtering liquid pipe fixed in the main body and a filtering component fixed on the filtering liquid pipe at intervals, the filtering liquid pipe comprises an outer ring pipe and an inner ring pipe which are arranged along the radial direction of the main body from outside to inside, the outer ring pipe and the inner ring pipe are connected with a clear liquid outlet system through the clear liquid outlet pipe, and the outer ring pipe and the inner ring pipe are sealed pipes.
Furthermore, the outer ring pipe is connected with a clear liquid outlet system through a clear liquid outlet pipe, and the inner ring pipe is connected and communicated with the clear liquid outlet pipe through a bent pipe.
Furthermore, the outer ring pipe and the inner ring pipe are independently arranged, and the inner ring pipe and the outer ring pipe are respectively externally connected with a clear liquid discharging system through independent clear liquid discharging pipes.
Further, the arrangement position of the inner ring pipe is higher than that of the outer ring pipe.
Therefore, the anode material precursor coprecipitation reaction equipment solves the problems of different sizes of precursor product particles, breakage of the filter assembly and damage to the particle surface caused by improper arrangement of the stirring blade and the filter assembly, and the problem of uneven sizes of the precursor product particles; when the stirring paddle and the filter component are arranged too close to each other, the end part of the stirring paddle in the radial direction of the tank body can be in contact with a filter cake formed on the surface of the filter element or fluid formed by stirring forms stronger acting force on the surface of the filter element, so that the filter component is broken, and the particle surface of a precursor product is damaged.
The applicant finds that the installation structure of the filtering assembly directly influences the filtering flux of the concentration equipment and the output flow of the obtained filtered liquid when the filtering assembly of the concentration equipment is installed, the traditional filtering assembly is installed by a single-layer filter element, the installation mode of the traditional filtering assembly causes the filtering flux to be small, the output flow of the filtered liquid to be small, the output flow of the whole precursor production system is directly influenced, and the production efficiency of the precursor is reduced.
The invention also provides a cathode material precursor coprecipitation reaction device, which aims to solve the technical problem that the production efficiency of the cathode material precursor coprecipitation reaction device is reduced due to the installation structure of the filter assembly in the prior art.
In order to achieve the above object, according to an aspect of the present invention, there is provided a cathode material precursor coprecipitation reaction apparatus including:
a body for containing a ternary precursor slurry;
an input unit for inputting the ternary precursor slurry into the main body;
a stirring component arranged in the main body and used for stirring the ternary precursor slurry in the main body,
the filter assembly comprises a filter liquid pipe fixed in the main body and filter elements fixed on the filter liquid pipe at intervals, the filter liquid pipe comprises an outer ring pipe and an inner ring pipe which are arranged from outside to inside along the radial direction of the main body, the outer ring pipe and the inner ring pipe are both externally connected with a clear liquid outlet system through the clear liquid outlet pipe, and the outer ring pipe and the inner ring pipe are both sealed pipes;
and the mounting position of the filter element on the outer ring pipe and the mounting position of the filter assembly on the inner ring pipe are arranged in a staggered manner.
Therefore, in the positive electrode material precursor coprecipitation reaction equipment, the outer ring pipe and the inner ring pipe are arranged to ensure that the filter assemblies are distributed in the main body in the circumferential direction, and the installation positions of the filter assemblies are increased, so that more filter assemblies are allowed to be installed, the filter flux and the clear volume of the filter assemblies are greatly increased, and the filter elements on the inner ring and the outer ring are installed in a staggered mode on the installation positions of the filter elements, so that the staggered installation has the advantages that: the filter element is convenient to mount inside and outside, and the inner ring and the outer ring of the filter element cannot block and interfere with each other when being mounted; the second does benefit to the stirring subassembly when stirring, and the thick liquids in the main part contacts each filter core, has guaranteed the filter flux on the one hand, and on the other hand has guaranteed that the thick liquids erodes the filter cake that each filter core surface formed at flow in-process, prevents that the filter cake from blockking each other because of the filter core and leading to quick deposit, and then does benefit to the assurance of filter flux, has guaranteed the filter flux of whole anode material precursor coprecipitation reaction equipment and the output flow of straining the clear liquid from this.
The invention provides a cathode material precursor coprecipitation reaction device which provides the following connection modes of a plurality of different filter liquor tubes and a plurality of different clear liquor outlet tubes.
Furthermore, the outer ring pipe is externally connected with a clear liquid outlet system through a clear liquid outlet pipe, and the inner ring pipe and the outer ring pipe are connected and communicated through a horizontal straight pipe. Two ends of the horizontal straight pipe are required to be welded to the inner ring pipe and the outer ring pipe respectively through T-shaped welding.
Furthermore, the outer ring pipe is externally connected with a clear liquid outlet system through a clear liquid outlet pipe, and the inner ring pipe is connected and communicated with the clear liquid outlet pipe through a bent pipe. Compared with the T-shaped welding at two ends of a horizontal straight pipe, the connecting mode is quicker, more convenient and simpler.
Furthermore, the outer ring pipe and the inner ring pipe are independently arranged, and the inner ring pipe and the outer ring pipe are respectively externally connected with a clear liquid discharging system through independent clear liquid discharging pipes. Compared with the T-shaped welding at two ends of a horizontal straight pipe, the connecting mode is quicker and more convenient, and the independent liquid outlet pipe is more convenient to install.
Furthermore, one end part of the inner ring pipe is longer than the corresponding end part of the outer ring pipe, the clear liquid outlet pipe of the inner ring is connected and communicated with the end part of the inner ring pipe, and the clear liquid outlet pipe of the outer ring is connected and communicated with the end part of the outer ring pipe. Because the horizontal straight pipe, the inner ring pipe and the outer ring pipe respectively form a T shape, a full penetration welding seam is required to be carried out at the joint, so that the connection mode is quicker, simpler and more convenient than the T-shaped welding at the two ends of the horizontal straight pipe, and the independent liquid outlet pipe is more convenient to install.
Further, the arrangement position of the inner ring pipe is higher than that of the outer ring pipe. This kind of inner circle pipe compares in the condition of inner circle pipe with outer lane pipe same height with the position connected mode of pipe, and the installation is dismantled more conveniently to the filtering component, and the installation of the filtering component of being convenient for is overhauld.
Further, the clear liquid outlet pipe is a pipeline which is vertically arranged downwards.
Furthermore, a fixing piece is radially arranged in the main body, and the inner ring pipe and the outer ring pipe are arranged on the fixing piece from inside to outside.
Furthermore, the fixing piece is a fixing rod, and two ends of the inner ring tube and the outer ring tube are respectively connected with the fixing rod through welding; or the two ends of the inner ring tube and the outer ring tube are fixed on the fixed rod through the hoop pieces.
Further, the inner ring pipe and the outer ring pipe are both arc pipes.
Further, the filter assembly comprises four filter units, and the central angle of the arc-shaped pipe is 75-80 degrees.
The technical means for solving the problem that the filter cake influences the filtering flux in the prior art is to perform back flushing on the filtering component through back flushing equipment, however, some back flushing structures in the prior art can easily cause damage to the filtering component in concentration equipment, and some back flushing structures can not realize thorough back flushing of the filter element.
The invention also provides a coprecipitation reaction system for the precursor of the cathode material, which aims to solve the problems that some backflushing structures in the prior art can easily cause the leakage of a filter assembly in concentration equipment, and some backflushing structures can not realize the thorough backflushing of a filter element.
In order to achieve the above object, there is provided according to the present invention a cathode material precursor coprecipitation reaction system including:
a body for containing a precursor slurry;
an input unit for inputting the precursor slurry into the main body;
the stirring assembly is arranged in the main body and is used for stirring the precursor slurry in the main body;
the filtering component is arranged in the main body and used for intercepting the precursor in the main body to obtain concentrated precursor slurry and filtering out filtrate;
and the back flushing device is used for back flushing regeneration of the filtering component, and the one-time back flushing amount of the back flushing device is 1-2 times of the total volume of the filtering component which is back flushed at one time.
The applicant finds in research that backflushing the filter assemblies in groups can effectively ensure the backflushing effect,
furthermore, at least two groups of filtering assemblies are arranged in the main body, and the primary recoil quantity of the recoil device is 1-2 times of the total volume of one group of filtering assemblies.
Further, the recoil apparatus includes:
the backflushing container is used for containing backflushing gas/backflushing liquid, and an outlet of the backflushing container is connected with a filtered liquid outlet of the filtering component to be regenerated;
the gas inlet control assembly is used for controlling the regenerated gas to be input into the backflushing container;
the liquid inlet control assembly is used for controlling regenerated liquid to be input into the backflushing container;
and the backflushing control assembly is used for controlling the regenerated gas/regenerated liquid to be output from the backflushing container through the outlet of the backflushing container.
Furthermore, the liquid outlet control assembly comprises a back-flushing pipe connected with a liquid outlet of the back-flushing container and a pneumatic ball valve arranged on the back-flushing pipe.
Furthermore, the backflushing pipe is branched out of the backflushing side pipe corresponding to each group of filtering assemblies, a manual ball valve is arranged on each backflushing side pipe, and each group of filtering assemblies is connected with the backflushing container through the backflushing side pipe.
Furthermore, a sight glass is arranged on each recoil side pipe.
Further, the air inlet control assembly comprises an air inlet pipe connected with an air source, and a pneumatic ball valve, a pressure gauge and a stop valve which are arranged on the air inlet pipe.
Further, the feed liquor control assembly comprises a feed liquor pipe connected with the regeneration liquid source and a manual ball valve arranged on the feed liquor pipe.
Further, the volume of the backflush container is 1.5 to 2.5 times of the volume of the filter assembly which is backflushed once.
The filter element is characterized by further comprising a clear water discharging assembly and a pure water control assembly, wherein the clear water discharging assembly is used for discharging filtered clear water, the pure water control assembly is respectively connected with the clear water discharging assembly and the backflushing device, and the pure water control assembly is used for controlling pure water to enter the clear water discharging assembly and the backflushing device.
Thus, the ratio of the volume of the backflush vessel to the volume of the filter element in the filter element regeneration system of the present invention substantially ensures that the solution in the backflush vessel is sufficient to backflush the filter cake structure thoroughly on all filter element surfaces.
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 invention and their equivalents and not limit it unduly. In the 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 invention and their equivalents and not limit it unduly. In the drawings:
FIG. 1 is a schematic diagram of a system configuration of a precursor production system according to 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 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 tube and the clear liquid outlet tube according to the present 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 topographical view of a ternary precursor product obtained in accordance with one through sixteen examples of the present invention.
FIG. 9 is a schematic view of the position relationship between the stirring assembly and the filtering assembly according to the present invention.
Fig. 10 is a schematic illustration of the filter cake of the present invention attached to the filtration surface of the filter assembly proximate the agitator blades.
Fig. 11 is a schematic view showing that the installation position of the filter element on the outer ring pipe and the installation position of the filter assembly on the inner ring pipe are arranged in a staggered manner.
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 practice the invention based on these descriptions. 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 in the related section are intended to cover a non-exclusive inclusion.
The invention discloses a coprecipitation reaction device of a precursor of a positive electrode material, which comprises
A main body 21 for containing a precursor slurry;
a filtering assembly 23 installed in the main body 21 for intercepting the precursor in the main body 21 to obtain a concentrated precursor slurry and filtering out a filtrate;
a stirring unit 22 installed in the main body 21 for stirring the precursor slurry in the main body 21;
the pump unit is used for pumping the precursor slurry in the reaction kettle 1 into the main body 21;
the backflow unit is used for refluxing the precursor slurry in the main body 21 to the reaction kettle 1;
a clear-out unit for discharging the filtered clear liquid to the outside of the main body 21;
the first liquid level control unit comprises a clear valve for regulating and controlling the discharge flow of the filtered liquid, and the clear valve is used for interlocking control with a first liquid level meter 31 arranged on the reaction kettle;
and the second liquid level control unit comprises a second liquid level meter 51 arranged on the main body 21 and a reflux valve 52 used for regulating and controlling the reflux amount of the concentrated precursor slurry, and the second liquid level meter 51 and the reflux valve 52 are controlled in an interlocking manner.
The first liquid level meter 31 and the cleaning valve are subjected to interlocking control in a PID control mode.
The discharging unit comprises a discharging pipe 41 for connecting the filtered liquid outlet of the filtering component 23 to the outside of the main body 21 and a discharging pump 42 arranged on the discharging pipe 41, and the discharging valve is arranged on the discharging pipe 41.
The discharging valve comprises a pressure gauge 322, a discharging flow meter 323 and a discharging pneumatic ball valve 321 which are arranged on the discharging pipe 41.
The second liquid level meter 51 and the return valve 52 are controlled in an interlocking manner by a PID control method.
The reflux unit comprises a reflux pipe connecting the main body 21 and the reaction kettle 1, and the reflux valve 52 is arranged on the reflux pipe.
The return valve 52 is an electrically operated regulator valve.
The return pipe is also provided with a return cut-off valve 7.
The pumping unit includes a feeding pipe 61 connecting the reaction vessel 1 and the main body 21, a feeding pump 62 provided on the feeding pipe 61, a feeding flowmeter 63, and a feeding pneumatic ball valve 64.
A co-precipitation reaction system comprising:
a reaction kettle 1 for reacting reactants therein to generate precursor slurry;
the cathode material precursor coprecipitation reaction equipment 2 comprises a main body 21, a filter assembly 23 and a stirring unit 22, wherein the filter assembly 23 is installed in the main body 21, the main body 21 is used for containing precursor slurry, and the filter assembly 23 is used for intercepting the precursor in the main body 21 to obtain concentrated precursor slurry and filtering out filtrate; the stirring unit 22 is used for stirring the precursor slurry in the main body 21;
the pump unit is used for pumping the precursor slurry in the reaction kettle 1 into the main body 21;
the backflow unit is used for refluxing the precursor slurry in the main body 21 to the reaction kettle 1;
a clear-out unit for discharging the filtered clear liquid to the outside of the main body 21;
the first liquid level control unit comprises a first liquid level meter 31 arranged on the reaction kettle 1 and a clear outlet valve used for regulating and controlling the discharge flow of the filtered clear liquid, and the first liquid level meter 31 and the clear outlet valve are controlled in an interlocking manner;
and the second liquid level control unit comprises a second liquid level meter 51 arranged on the main body 21 and a reflux valve 52 used for regulating and controlling the reflux amount of the concentrated precursor slurry, and the second liquid level meter 51 and the reflux valve 52 are controlled in an interlocking manner.
The invention discloses a coprecipitation reaction device for a precursor of a positive electrode material, which comprises:
a tank 21 for containing a precursor slurry;
an input unit for inputting the precursor slurry into the tank 21;
the stirring component 22 is arranged in the tank body 21 and is used for stirring the precursor slurry in the tank body 21;
the filtering component 23 is annularly distributed in the tank body 21 around the stirring component 22 and is used for intercepting the precursor in the tank body 21 to obtain concentrated precursor slurry and filtering out filtrate;
the positions of the end parts of the stirring blades of the stirring components 22 in the radial direction of the tank body 21 during stirring are all positioned on a first virtual cylindrical surface, the positions of all the filter surfaces of the filter components, which are closest to the stirring blades, are all positioned on a second virtual cylindrical surface, and the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 5-15%.
The ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction to the inner diameter of the can body 21 is 6-8%.
The volume of the tank body 21 is 50-100L, and the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 20-40 mm.
The volume of the tank body 21 is 0.6-8m 3 And the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 100-150 mm.
The stirring linear speed of the stirring component 22 is 5-10 m/s.
The stirring linear speed of the stirring component 22 is 7-8 m/s.
The filter assembly 23 is including being fixed in the filter liquor pipe in the jar body 21, the interval is fixed in the filter core 235 on the filter liquor pipe, the filter liquor pipe includes outer lane pipe 231, the inner circle pipe 232 of laying along jar body 21 radial outside-in, outer lane pipe 231, inner circle pipe 232 are all through going out the external clear liquid system of clear liquid pipe 233, outer lane pipe 231, inner circle pipe 232 are the sealed tube.
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 a bent pipe 236.
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.
The inner ring pipe 232 is disposed at a position higher than the outer ring pipe 231.
The invention discloses a coprecipitation reaction device for a precursor of a positive electrode material, which comprises:
a main body 21 for containing a precursor slurry;
an input unit for inputting the precursor slurry into the main body 21;
the stirring component 22 is arranged in the main body 21 and is used for stirring the precursor slurry in the main body 21;
the filtering component 23 comprises a plurality of filtering units annularly arranged in the main body 21 around the stirring component 22, and is used for intercepting the precursor in the main body 21 to obtain concentrated precursor slurry and filtering out filtrate;
the filter assembly 23 comprises a filter liquid pipe fixed in the main body 21 and filter elements 235 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 from outside to inside along the radial direction of the main body 21, the outer ring pipe 231 and the inner ring pipe 232 are both externally connected with a clear liquid discharging system through a clear liquid discharging pipe 233, and the outer ring pipe 231 and the inner ring pipe 232 are both sealed pipes;
the installation position of the filter element 235 on the outer ring pipe 231 and the installation position of the filter element 235 on the inner ring pipe 232 are arranged in a staggered manner.
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.
The outer ring pipe 231 is externally connected with a clear liquid outlet system through a clear liquid outlet pipe 233, and the inner ring pipe 232 is connected and communicated with the clear liquid outlet pipe 233 through a bent pipe 236.
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.
One end of the inner ring tube 232 is longer than the corresponding end of the outer ring tube 231, the inner ring tube 232 is connected and communicated with the inner ring tube 233, and the outer ring tube 231 is connected and communicated with the outer ring tube 233.
The inner ring pipe 232 is disposed at a position higher than the outer ring pipe 231.
The clear liquid outlet pipe 233 is a pipe arranged vertically downward.
The main body 21 is provided with a fixing member in the radial direction, and the inner ring tube 232 and the outer ring tube 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 both arc pipes.
The filter assembly 23 comprises four filter units, and the central angle of the arc-shaped pipe is 75-80 degrees.
Positive pole material precursor coprecipitation reaction system includes:
a main body 21 for containing a precursor slurry;
an input unit for inputting the precursor slurry into the main body 21;
a stirring assembly 22 disposed in the main body 21 for stirring the precursor slurry in the main body 21;
the filtering component 235 is arranged in the main body 21 and used for intercepting the precursor in the main body 21 to obtain concentrated precursor slurry and filtering out filtered liquid;
and the back flushing device is used for back flushing regeneration of the filter assembly 235, and the one-time back flushing amount of the back flushing device is 1-2 times of the total volume of the filter assembly 235 which is back flushed at one time.
At least two groups of filter assemblies 235 are arranged in the main body 21, and the primary recoil quantity of the recoil device is 1-2 times of the total volume of one group of filter assemblies 235.
The recoil device includes:
a backflushing container 8 for containing backflushing gas/backflushing liquid, an outlet of the backflushing container 8 being connected with a filtrate outlet of the filter assembly 235 to be regenerated;
the air inlet control component is used for controlling the regenerated gas to be input into the backflushing container 8;
the liquid inlet control component is used for controlling the regenerated liquid to be input into the backflushing container 8;
and the backflushing control component is used for controlling the regenerated gas/regenerated liquid to be output from the backflushing container 8 through the outlet of the backflushing container 8.
The liquid outlet control assembly comprises a backflushing pipe connected with the liquid outlet of the backflushing container 8 and a pneumatic ball valve 112 arranged on the backflushing pipe 111.
The backflushing pipe is branched out of the backflushing side pipe 111 corresponding to each group of filtering assemblies 235, a manual ball valve 112 is arranged on each backflushing side pipe 111, and each group of filtering assemblies 235 are connected with the backflushing container 8 through the backflushing side pipes 111 respectively.
A sight glass 113 is arranged on each recoil side pipe 111.
The air inlet control assembly comprises an air inlet pipe 91 connected with an air source, and a pneumatic ball valve 92, a pressure gauge 93 and a stop valve 94 which are arranged on the air inlet pipe 91.
The liquid inlet control assembly comprises a liquid inlet pipe 10 connected with a regeneration liquid source and a manual ball valve 11 arranged on the liquid inlet pipe 10.
The volume of the backflush vessel 8 is 1.5-2.5 times the volume of the filter assembly 235 that is backflushed at a time.
The device comprises a cleaning component and a pure water control component, wherein the cleaning component is used for discharging filtered liquid, the pure water control component is respectively connected with the cleaning component and the backflushing device, and the pure water control component is used for controlling pure water to enter the cleaning component and the backflushing device.
The cathode material precursor coprecipitation reaction equipment and the cathode material precursor coprecipitation reaction equipment are suitable for production of precursors, and are particularly suitable for application in production of ternary precursors.
As shown in fig. 1, the coprecipitation reaction system of the invention comprises the following structural modules: comprises a reaction kettle 1 and anode material precursor coprecipitation reaction equipment 2; the pumping unit is used for pumping the ternary precursor slurry in the reaction kettle 1 into the main body 21; the backflow unit is used for refluxing concentrated ternary precursor slurry obtained by the main body 21 under the action of the filtering assembly 23 and the stirring unit 22 to the reaction kettle 1; a clear-out unit for discharging the filtered clear liquid to the outside of the main body 21; the liquid inlet and outlet control unit is used for controlling the clear liquid outlet quantity of the filtered liquid of the main body 21 to be consistent with the liquid inlet quantity of the reaction kettle 1; the main body liquid level control unit is used for controlling the liquid level of the ternary precursor slurry in the main body 21 to be kept stable; a filter assembly regeneration system.
Wherein the cathode material precursor coprecipitation reaction equipment 2 comprises: a body 21 for containing a ternary precursor slurry; an input unit for inputting the ternary precursor slurry into the main body 21; the stirring assembly 22 is arranged in the main body 21 and is used for stirring the ternary precursor slurry in the main body 21; and the filtering assembly 23 comprises a plurality of filtering units annularly arranged in the main body 21 around the stirring assembly 22, and is used for intercepting the precursor in the main body 21 to obtain concentrated ternary precursor slurry and filtering out filtrate.
The following further explains improvements made by the present invention in relation to the technical problems of unstable liquid level of the reaction vessel in the positive electrode material precursor coprecipitation system and unstable liquid level in the concentration equipment.
As shown in FIG. 1, the apparatus for coprecipitation reaction of precursors of positive electrode material in the present invention comprises
A main body 21 for containing a precursor slurry; a filtering assembly 23 installed in the main body 21 for intercepting the precursor in the main body 21 to obtain a concentrated precursor slurry and filtering out a filtrate; a stirring unit 22 installed in the main body 21 for stirring the precursor slurry in the main body 21; the pump unit is used for pumping the precursor slurry in the reaction kettle 1 into the main body 21; the backflow unit is used for refluxing the precursor slurry in the main body 21 to the reaction kettle 1; a clear-out unit for discharging the filtered clear liquid to the outside of the main body 21; the first liquid level control unit comprises a clear valve for regulating and controlling the discharge flow of the filtered liquid, and the clear valve is used for interlocking control with a first liquid level meter 31 arranged on the reaction kettle; the second liquid level control unit comprises a second liquid level meter 51 arranged on the main body 21 and a reflux valve 52 used for regulating and controlling the reflux amount of the concentrated precursor slurry, and the second liquid level meter 51 and the reflux valve 52 are controlled in an interlocking manner. The first liquid level meter 31 and the purge valve are controlled in an interlocking manner in a PID control mode. The discharging unit comprises a discharging pipe 41 for connecting the filtered liquid outlet of the filtering component 23 to the outside of the main body 21 and a discharging pump 42 arranged on the discharging pipe 41, and the discharging valve is arranged on the discharging pipe 41. The discharging valve comprises a pressure gauge 322, a discharging flow meter 323 and a discharging pneumatic ball valve 321 which are arranged on the discharging pipe 41. The second liquid level meter 51 and the return valve 52 are controlled in an interlocking manner by a PID control method. The reflux unit comprises a reflux pipe connecting the main body 21 and the reaction kettle 1, and the reflux valve 52 is arranged on the reflux pipe. The return valve 52 is an electrically operated regulator valve. And the return pipe is also provided with a return cut-off valve 7. The pumping unit includes a feeding pipe 61 connecting the reaction vessel 1 and the main body 21, a feeding pump 62 provided on the feeding pipe 61, a feeding flowmeter 63, and a feeding pneumatic ball valve 64.
A co-precipitation reaction system comprising: the reaction kettle 1 is used for reacting reactants therein to generate precursor slurry; the cathode material precursor coprecipitation reaction equipment 2 comprises a main body 21, a filter assembly 23 and a stirring unit 22, wherein the filter assembly 23 is installed in the main body 21, the main body 21 is used for containing precursor slurry, and the filter assembly 23 is used for intercepting the precursor in the main body 21 to obtain concentrated precursor slurry and filtering out filtrate; the stirring unit 22 is used for stirring the precursor slurry in the main body 21; the pump unit is used for pumping the precursor slurry in the reaction kettle 1 into the main body 21; the backflow unit is used for refluxing the precursor slurry in the main body 21 to the reaction kettle 1; a clear-out unit for discharging the filtered clear liquid to the outside of the main body 21; the first liquid level control unit comprises a first liquid level meter 31 arranged on the reaction kettle 1 and a clear outlet valve used for regulating and controlling the discharge flow of the filtered clear liquid, and the first liquid level meter 31 and the clear outlet valve are controlled in an interlocking manner; the second liquid level control unit comprises a second liquid level meter 51 arranged on the main body 21 and a reflux valve 52 used for regulating and controlling the reflux amount of the concentrated precursor slurry, and the second liquid level meter 51 and the reflux valve 52 are controlled in an interlocking manner.
The working flow of the coprecipitation reaction system under the improvement is as follows: under the condition that the feeding flow of the reaction kettle 1 is constant, the first liquid level meter 31 on the reaction kettle 1 monitors the liquid level change of the reaction kettle 1 and sends a liquid level change signal to a controller controlled in a PID control mode, when the liquid level of the first liquid level meter 31 is monitored to be higher than a set liquid level threshold value, the total stirring power is increased if no adjustment is carried out at the moment, so that the stirring overload is caused, and the valve opening of the pneumatic clean air ball valve 321 is increased through PID control at the moment; when the situation that the liquid level of the first liquid level meter 31 is lower than the set liquid level threshold value is monitored, the total volume of slurry is small, so that the retention time is shortened due to high concentration, the clear liquid outlet flux of a filtered liquid of the system can be influenced due to high concentration, the reaction cannot be completely carried out due to shortened retention time, the liquid level is too low, and if the total volume of the slurry is lower than the upper paddle, the upper paddle fails to work, so that the stirring effect is influenced, and therefore the opening degree of the valve of the pneumatic purge ball valve 321 is reduced through PID control at the moment, so that the liquid level stability of the reaction kettle 1 is ensured. Under the condition that the feeding flow of the main body 21 is constant, the second liquid level meter 51 on the main body 21 monitors the liquid level in the main body 21 in real time, when the second liquid level meter 51 monitors that the liquid level of the main body 21 is higher than a threshold value, the problem of overload stirring caused by increase of total stirring power can also occur, and the problem of material waste caused by filter assembly penetration can also occur, especially the problem that a filter element component made of plastic material is damaged, so that the filter element is broken, and therefore the opening degree of the return valve 52 needs to be increased through PID control at the moment; when the second liquid level meter 51 monitors that the liquid level of the main body 21 is higher than the threshold value, the flux of the filter assembly cannot reach the expectation, and if the flux is lower than the upper paddle, the upper paddle fails to work, and the stirring effect is affected, and at this time, the opening degree of the return valve 52 needs to be reduced through PID control, so that the liquid level in the main body 21 is stabilized.
According to the invention, the reaction retention time of the ternary precursor slurry in the reaction kettle and the filtration pressure difference of the filtration component in the anode material precursor coprecipitation reaction equipment are ensured by controlling the size of the clear liquid outlet amount of the main body to be consistent with the liquid inlet amount of the reaction kettle and controlling the liquid level of the ternary precursor slurry in the main body to be kept stable, so that the quality of the finally produced product is ensured to be stable. The obtained filtrate can be used by other ingredients of the coprecipitation reaction system.
The following further describes the improvement of the present invention in the structural relationship between the stirring component and the filtering component of the cathode material precursor coprecipitation reaction apparatus.
As shown in fig. 9, the apparatus for co-precipitating a precursor of a positive electrode material according to the present invention includes: a tank 21 for containing a precursor slurry; an input unit for inputting the precursor slurry into the tank 21; the stirring component 22 is arranged in the tank body 21 and is used for stirring the precursor slurry in the tank body 21; the filtering component 23 is annularly arranged in the tank body 21 around the stirring component 22 and is used for intercepting the precursor in the tank body 21 to obtain concentrated precursor slurry and filtering out filtrate; the positions of the ends of the stirring blades of the stirring assembly 22 in the radial direction of the tank body 21 during stirring are all located on a first virtual cylindrical surface, the positions of all the filtering surfaces of the filtering assemblies closest to the stirring blades are all located on a second virtual cylindrical surface, and the ratio of the distance d between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 5-15%. The ratio of the distance d between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction to the inner diameter of the can body 21 is 6% -8%. The volume of the tank body 21 is 50-100L, and the distance d between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 20-40 mm. The volume of the tank body 21 is 0.6-8m 3 And the distance d between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 100-150 mm. The stirring linear speed of the stirring component 22 is 5-10 m/s. The stirring linear speed of the stirring component 22 is 7-8 m/s. The filtering assembly 23 comprises a filtering liquid pipe fixed in the tank body 21 and a filtering liquid pipe fixed on the filtering liquid pipe at intervalsThe filter element 235, the filter liquid pipe includes outer lane pipe 231, the inner circle pipe 232 of laying along jar body 21 radial outside-in, outer lane pipe 231, inner circle pipe 232 are all through going out the external clear liquid system that goes out of clear liquid pipe 233, outer lane pipe 231, inner circle pipe 232 are the sealed tube. The outer ring pipe 231 is externally connected with a clear liquid outlet system through a clear liquid outlet pipe 233, and the inner ring pipe 232 is connected and communicated with the clear liquid outlet pipe 233 through a bent pipe 236. 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. The inner ring pipe 232 is disposed at a position higher than the outer ring pipe 231.
The precursor reaction is a salt-alkali neutralization reaction, nickel sulfate (or nickel chloride), cobalt sulfate (or cobalt chloride) and manganese sulfate (or manganese chloride) are prepared into a mixed salt solution with a certain molar concentration, sodium hydroxide is prepared into an alkali solution with a certain molar concentration, and ammonia water with a certain concentration is used as a complexing agent. All prepared solutions are filtered to remove solid impurities and then can enter the next link. Adding the filtered 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 the ternary precursor crystal nucleus, and filtering, washing and drying the reaction slurry after the granularity reaches a preset value to obtain the ternary precursor. In the process, the sodium hydroxide and the ammonia water are mixed and then added into the reaction kettle, so that the production line is simplified. If the doped ternary precursor needs to be prepared, the dopant solution can be added into the reaction kettle in the reaction process, and the doped ternary precursor is obtained after the reaction is finished. The following examples were conducted with the same ingredients, concentrations of ingredients, reaction temperatures, and pH values in each step.
The first embodiment is as follows: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 5%, and the stirring linear speed of the stirring assembly 22 is 5 m/s. In the cathode material precursor coprecipitation reaction apparatus in the first embodiment, the size of the ternary precursor product obtained by the cathode material precursor coprecipitation reaction apparatus in the application process of producing the ternary precursor by the actual cathode material precursor coprecipitation reaction apparatus is uniform, and the particle surface is not damaged.
Example two: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 10%, and the stirring linear speed of the stirring assembly 22 is 3 m/s. In the second embodiment, the positive electrode material precursor coprecipitation reaction equipment is used for producing the ternary precursor in the actual application process of the positive electrode material precursor coprecipitation reaction equipment, so that the obtained ternary precursor product has uniform particle size and no damage to the particle surface.
Example three: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 15%, and the stirring linear speed of the stirring assembly 22 is 8 m/s. In the third embodiment, the positive electrode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor product with uniform particle size and no damage to the particle surface in the application process of producing the ternary precursor by using the actual positive electrode material precursor coprecipitation reaction apparatus.
Example four: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 6%, and the stirring linear speed of the stirring assembly 22 is 7 m/s. In the fourth embodiment, the positive electrode material precursor coprecipitation reaction apparatus is used to produce the ternary precursor in the actual application process of the positive electrode material precursor coprecipitation reaction apparatus, and the obtained ternary precursor product has uniform particle size and no damage on the particle surface.
Example five: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 7%, and the stirring linear speed of the stirring assembly 22 is 7.5 m/s. In the fifth embodiment, the positive electrode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor product with uniform particle size and no damage to the particle surface in the application process of producing the ternary precursor by using the actual positive electrode material precursor coprecipitation reaction apparatus.
Example six: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 8%, and the stirring linear speed of the stirring assembly 22 is 8 m/s. In the sixth embodiment, the cathode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor product with uniform particle size and no damage to the particle surface in the application process of producing the ternary precursor by using the actual cathode material precursor coprecipitation reaction apparatus.
Example seven: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 6%, and the stirring linear speed of the stirring assembly 22 is 7 m/s. In the seventh embodiment, the positive electrode material precursor coprecipitation reaction apparatus is used to produce the ternary precursor in an actual application process of the positive electrode material precursor coprecipitation reaction apparatus, and the obtained ternary precursor product has uniform particle size and no damage on the particle surface.
Example eight: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 7%, and the stirring linear speed of the stirring assembly 22 is 7.5 m/s. In the embodiment eight, the positive electrode material precursor coprecipitation reaction equipment obtains a ternary precursor product with uniform particle size and no damage to the particle surface in the application process of producing the ternary precursor by using the actual positive electrode material precursor coprecipitation reaction equipment.
Example nine: the ratio of the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction of the tank body 21 to the inner diameter of the tank body 21 is 8%, and the stirring linear speed of the stirring assembly 22 is 8 m/s. In the ninth embodiment, the cathode material precursor coprecipitation reaction apparatus is used to produce the ternary precursor in the actual application process of the cathode material precursor coprecipitation reaction apparatus, so that the obtained ternary precursor product has uniform particle size and no damage to the particle surface.
The volume of the tank body 21 is 50-100L, and the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 20-40 mm.
Example eleven: the tank body 21 has a volume of 50L, and the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 20 mm. The stirring linear speed of the stirring assembly 22 is 8 m/s. In the eleventh embodiment, the cathode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor product having a uniform particle size and a non-damaged particle surface in the application process of producing the ternary precursor by using the actual cathode material precursor coprecipitation reaction apparatus.
Example twelve: the tank body 21 has a volume of 80L, and the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 30 mm. The stirring linear speed of the stirring assembly 22 is 8 m/s. In the twelfth embodiment, the cathode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor product with uniform particle size and no damage to the particle surface in the application process of the actual cathode material precursor coprecipitation reaction apparatus to produce the ternary precursor.
Example thirteen: the tank body 21 has a volume of 100L, and the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 40 mm. The stirring linear speed of the stirring assembly 22 is 8 m/s. In the thirteenth embodiment, the cathode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor product having a uniform particle size and a non-damaged particle surface in an application process of producing the ternary precursor by using the actual cathode material precursor coprecipitation reaction apparatus.
The manufacturing testing machines are suitable for the eleventh, twelfth and thirteenth embodiments, and are used for measuring data before actual production and production processes are determined, and the obtained data can be used for determining the production processes by users.
The volume of the tank body 21 is 0.6-8m 3 And the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 100-150 mm.
Example fourteen: the volume of the tank body 21 is 0.6m 3 And the distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 100 mm. The stirring linear speed of the stirring component 22 is 8 m/s. In the fourteenth embodiment, the positive electrode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor in the application process of producing the ternary precursor by using the actual positive electrode material precursor coprecipitation reaction apparatusThe particle size of the body-driving product is uniform, and the surface of the particle is not damaged.
Example fifteen: the volume of the tank body 21 is 5m 3 The distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 120 mm. The stirring linear speed of the stirring component 22 is 8 m/s. In the fifteenth embodiment, the positive electrode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor product having a uniform particle size and a non-damaged particle surface in an application process of producing the ternary precursor by using the actual positive electrode material precursor coprecipitation reaction apparatus.
Example sixteen: the volume of the tank body 21 is 8m 3 The distance between the first virtual cylindrical surface and the second virtual cylindrical surface in the radial direction is 150 mm. The stirring linear speed of the stirring component 22 is 8 m/s. In the sixteenth embodiment, the cathode material precursor coprecipitation reaction apparatus is used to obtain a ternary precursor product with uniform particle size and no damage to the particle surface in the application process of the actual cathode material precursor coprecipitation reaction apparatus to produce the ternary precursor.
The embodiments fourteen, fifteen and sixteen are mainly applicable to practical cathode material precursor coprecipitation reaction production equipment.
Microscopic representation of the precursor products obtained in the first to sixteenth embodiments is provided. As shown in fig. 8, it can be seen from the microscopic schematic diagram that the obtained ternary precursor product has uniform particle size and no damage on the particle surface. Other structural modules in the cathode material precursor coprecipitation reaction equipment applied to the cathode material precursor coprecipitation reaction equipment in all the embodiments can be existing modules, or structural modules improved in the invention can be adopted, and when the anode material precursor coprecipitation reaction equipment is used in combination with other improved structural modules in the invention, the production effects of the precursors are mutually enhanced.
The following further illustrates the improvement of the present invention in the backflush structure of the filter assembly:
as shown in fig. 1, the positive electrode material precursor coprecipitation reaction system includes:
a main body 21 for containing a precursor slurry; an input unit for inputting the precursor slurry into the main body 21; a stirring assembly 22 disposed in the main body 21 for stirring the precursor slurry in the main body 21; the filtering component 235 is arranged in the main body 21 and used for intercepting the precursor in the main body 21 to obtain concentrated precursor slurry and filtering out filtered liquid; and the back flushing device is used for back flushing regeneration of the filter assembly 235, and the one-time back flushing amount of the back flushing device is 1-2 times of the total volume of the filter assembly 235 which is back flushed at one time. At least two groups of filter assemblies 235 are arranged in the main body 21, and the primary recoil quantity of the recoil device is 1-2 times of the total volume of one group of filter assemblies 235. The recoil device includes: a backflushing container 8 for containing backflushing gas/backflushing liquid, an outlet of the backflushing container 8 being connected with a filtrate outlet of the filter assembly 235 to be regenerated; the air inlet control component is used for controlling the regenerated gas to be input into the backflushing container 8; the liquid inlet control assembly is used for controlling regenerated liquid to be input into the backflushing container 8; and the backflushing control component is used for controlling the regenerated gas/regenerated liquid to be output from the backflushing container 8 through the outlet of the backflushing container 8. The liquid outlet control assembly comprises a back-flushing pipe connected with a liquid outlet of the back-flushing container 8 and a pneumatic ball valve 112 arranged on the back-flushing pipe 111. The backflushing pipe is branched out of the backflushing side pipe 111 corresponding to each group of filtering assemblies 235, a manual ball valve 112 is arranged on each backflushing side pipe 111, and each group of filtering assemblies 235 are connected with the backflushing container 8 through the backflushing side pipes 111 respectively.
A sight glass 113 is arranged on each recoil side pipe 111. The air inlet control assembly comprises an air inlet pipe 91 connected with an air source, and a pneumatic ball valve 92, a pressure gauge 93 and a stop valve 94 which are arranged on the air inlet pipe 91. The liquid inlet control assembly comprises a liquid inlet pipe 10 connected with a regeneration liquid source and a manual ball valve 11 arranged on the liquid inlet pipe 10. The volume of the backflush vessel 8 is 1.5-2.5 times the volume of the filter assembly 235 that is backflushed at a time. The filter is characterized by further comprising a clear discharging assembly and a pure water control assembly, wherein the clear discharging assembly is used for discharging filtered liquid, the pure water control assembly is respectively connected with the clear discharging assembly and the backflushing device, and the pure water control assembly is used for controlling pure water to enter the clear discharging assembly and the backflushing device. And during backflushing, different buffering modes are selected according to different material requirements. The advantages of backflushing liquid for backflushing are that: the wear to the filtering component is smaller, and the oxygen partial pressure in the material is not influenced; the advantages of gas back flushing are: better control and fewer valves. Therefore, when the device is used specifically, different backflushing modes can be selected according to different material properties.
Under the condition that other experimental conditions are the same, the applicant performs a backflushing test on the condition that the primary backflushing amount of the filter assembly 235 is 1, 1.5 and 2 times of the total volume of the filter assembly 235 which is backflushed once, and under the condition, the filter assembly which is backflushed once can be guaranteed to be backflushed completely, the condition that the backflushing of the filter assembly 235 is incomplete is avoided, and the condition that the filter assembly 235 penetrates through the filter assembly 235 is avoided.
Under the condition that other experimental conditions are the same, four groups of filter assemblies 235 are arranged in the main body 21, and the applicant performs a backflushing test on the backflushing device with the primary backflushing amount being 1, 1.5 and 2 times of the total volume of the group of filter assemblies 235, so that the backflushing of the backflushing device can be ensured to be just completely backflushed, the condition that the backflushing of the filter assemblies 235 is incomplete is avoided, and the condition that the filter assemblies 235 penetrate through the filter assemblies is avoided.
Fig. 10 is a schematic diagram of the attachment of the filter cake to the filter assembly 235. The positive electrode material precursor coprecipitation reaction system can ensure that a filter assembly which is backflushed once is just backflushed completely during backflushing, the condition that the backflushing of the filter assembly 235 is incomplete is not caused, and the condition that the filter assembly 235 penetrates through the filter assembly is also avoided.
Because the filtered liquid contains 10-15% of sodium sulfate, the sodium sulfate is easy to crystallize in the back flushing pipeline of the clear water outlet pipeline box, and therefore the pure water component allows pure water to enter the clear water outlet pipeline and the back flushing pipeline for flushing.
The situation of penetration can be observed through the sight glass, and whether the filter element is observed to have good precision or generate turbidity of different degrees is observed.
The following further describes the improvement of the present invention in the filter module mounting structure of the cathode material precursor coprecipitation reaction apparatus.
As shown in fig. 2 to 3, the apparatus for coprecipitation reaction of a precursor of a positive electrode material according to the present invention includes: a main body 21 for containing a precursor slurry; an input unit for inputting the precursor slurry into the main body 21; a stirring assembly 22 disposed in the main body 21 for stirring the precursor slurry in the main body 21; the filtering component 23 comprises a plurality of filtering units annularly arranged in the main body 21 around the stirring component 22, and is used for intercepting the precursor in the main body 21 to obtain concentrated precursor slurry and filtering out filtrate; the filter assembly 23 comprises a filter liquid pipe fixed in the main body 21 and a filter element 235 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 main body 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.
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 main body 21 is arranged on the bottom of the main body 21, the clear liquid outlet pipe 233 can be a straight pipe extending vertically downwards to the outside of the main body 21 to communicate with the clear liquid outlet assembly; when the clear liquid outlet of the main body 21 is disposed on the side of the main body 21, the clear liquid outlet pipe 233 may be a bent pipe extending out of the main body 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 main body 21 is arranged on the bottom of the main body 21, the clear liquid outlet pipe 233 can be a straight pipe extending vertically downwards to the outside of the main body 21 and communicated with the clear liquid outlet assembly; when the clear liquid outlet of the main body 21 is disposed on the side of the main body 21, the clear liquid outlet pipe 233 may be a bent pipe extending out of the main body 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 a bent pipe 236. When the clear liquid outlet on the main body 21 is arranged on the bottom of the main body 21, the clear liquid outlet pipe 233 can be a straight pipe extending vertically downwards to the outside of the main body 21 and communicated with the clear liquid outlet assembly; when the clear liquid outlet of the main body 21 is disposed on the side of the main body 21, the clear liquid outlet pipe 233 may be a bent pipe extending out of the main body 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 main body 21 is arranged on the bottom of the main body 21, the clear liquid outlet pipe 233 can be a straight pipe extending vertically downwards to the outside of the main body 21 to communicate with the clear liquid outlet assembly; when the clear liquid outlet of the main body 21 is disposed on the side of the main body 21, the clear liquid outlet pipe 233 may be a bent pipe extending out of the main body 21 to communicate with the clear liquid outlet assembly. In this connection, in order to install the clear liquid tube 233 more easily, one end of the inner ring tube 232 is longer than the corresponding end of the outer ring tube 231, the clear liquid tube 233 of the inner ring is connected to and conducted with the end of the inner ring tube 232, and the clear liquid tube 233 of the outer ring is connected to and conducted with the end of the outer ring tube 231.
Preferably, with reference to fig. 2 to 3, a fixing member is radially disposed inside the main body 21, and the inner ring tube 232 and the outer ring tube 231 are disposed 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 both 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 75-80 degrees. As shown in fig. 11, the installation position of the filter insert 235 in the outer ring pipe 231 is offset from the installation position of the filter insert 235 in the inner ring pipe 232.
The filter assembly 235 may be fixed at both the upper and lower ends or only at the lower end. When the filtering component is installed, the lower end of the filtering component is connected to the mounting hole formed in the upper end of the filtering liquid pipe through threads, and the upper end of the filtering component is fixedly connected with the main body 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 when the length of the filter assembly is longer, the filter element can be broken, so that when the filter assembly with the length of more than 500mm is applied to the anode material precursor coprecipitation reaction equipment, the double end is fixed.
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.
When the precursor system is applied to ternary precursor production, the specific composition of the reaction kettle 1 can be determined according to the reaction time of specific materials because the reaction time of materials with different proportions and different compositions is different, for example, when the reaction time of ternary precursor slurry is relatively short, the reaction kettle 1 only adopts a main reaction kettle; when the reaction of the ternary precursor slurry is slow, the reaction kettle 1 adopts a structure that the main reaction kettle is connected with the secondary reaction kettle. The ternary precursor slurry firstly enters a reaction kettle 1 for reaction and then enters an anode material precursor coprecipitation reaction device 2, enrichment and concentration of the ternary precursor slurry are achieved in the anode material precursor coprecipitation reaction device 2, the clear volume of the filtered liquid of a main body is controlled to be consistent with the liquid inlet volume of the reaction kettle and the liquid level of the ternary precursor slurry in the main body is controlled to be kept stable in the operation process of the ternary anode material precursor coprecipitation reaction device, therefore, the system can stably operate, the quality of the ternary precursor product is stable, the filtering assembly is fully regenerated periodically through a filtering assembly regeneration system, and the filtering flux of the filtering assembly is guaranteed.
The contents of the present invention have been explained above. Those skilled in the art will be able to practice the invention based on these descriptions. 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 (10)
1. The positive electrode material precursor coprecipitation reaction equipment is characterized by comprising
A body (21) for containing a precursor slurry;
a filtering assembly (23) mounted in the main body (21) for intercepting the precursor in the main body (21) to obtain a concentrated precursor slurry and filtering out a filtrate;
a stirring unit (22) which is installed in the main body (21) and is used for stirring the precursor slurry in the main body (21);
the pump unit is used for pumping the precursor slurry in the reaction kettle (1) into the main body (21);
the backflow unit is used for refluxing the precursor slurry in the main body (21) to the reaction kettle (1);
a clear-out unit for discharging the filtered clear liquid out of the main body (21);
the first liquid level control unit comprises a clear valve for regulating and controlling the discharge flow of the filtered clear liquid, and the clear valve is used for interlocking control with a first liquid level meter (31) arranged on the reaction kettle;
the second liquid level control unit comprises a second liquid level meter (51) arranged on the main body (21) and a backflow valve (52) used for regulating and controlling the backflow amount of the concentrated precursor slurry, and the second liquid level meter (51) and the backflow valve (52) are controlled in an interlocking mode.
2. The battery cathode material precursor coprecipitation reaction device of claim 1, wherein the first liquid level meter (31) and the purge valve are interlockingly controlled by a PID control method.
3. The battery cathode material precursor coprecipitation reaction device of claim 2, wherein the purge unit comprises a purge pipe (41) for connecting a filtrate outlet of the filter assembly (23) to the outside of the main body (21), and a purge pump (42) arranged on the purge pipe (41), and the purge valve is arranged on the purge pipe (41).
4. The battery cathode material precursor coprecipitation reaction device according to claim 2, wherein the purge valve comprises a pressure gauge (322), a purge flow meter (323) and a purge pneumatic ball valve (321) which are arranged on the purge pipe (41).
5. The battery cathode material precursor coprecipitation reaction apparatus according to claim 1, wherein the second level meter (51) and the return valve (52) are interlockingly controlled by a PID control method.
6. The battery cathode material precursor coprecipitation reaction apparatus of claim 5, wherein the reflux unit comprises a reflux pipe connecting the main body (21) and the reaction vessel (1), and the reflux valve (52) is disposed on the reflux pipe.
7. The battery cathode material precursor coprecipitation reaction apparatus of claim 5, wherein the return valve (52) is an electrically operated regulating valve.
8. The battery cathode material precursor coprecipitation reaction device according to claim 5, wherein a reflux shut-off valve (7) is further provided on the reflux pipe.
9. The battery cathode material precursor coprecipitation reaction apparatus of claim 1, wherein the pump unit comprises a feed pipe (61) connecting the reaction vessel (1) and the body (21), a feed pump (62) disposed on the feed pipe (61), a feed flow meter (63), and a feed pneumatic ball valve (64).
10. A coprecipitation reaction system, comprising:
the reaction kettle (1) is used for reacting reactants therein to generate precursor slurry;
the cathode material precursor coprecipitation reaction equipment (2) comprises a main body (21), a filtering assembly (23) and a stirring unit (22), wherein the filtering assembly (23) is installed in the main body (21), the main body (21) is used for containing precursor slurry, and the filtering assembly (23) is used for intercepting the precursor in the main body (21) to obtain concentrated precursor slurry and filtering out filtrate; the stirring unit (22) is used for stirring the precursor slurry in the main body (21);
the pump unit is used for pumping the precursor slurry in the reaction kettle (1) into the main body (21);
the backflow unit is used for refluxing the precursor slurry in the main body (21) to the reaction kettle (1);
a clear-out unit for discharging the filtered clear liquid out of the main body (21);
the first liquid level control unit comprises a first liquid level meter (31) arranged on the reaction kettle (1) and a clear outlet valve used for regulating and controlling the discharge flow of the filtered clear liquid, and the first liquid level meter (31) and the clear outlet valve are controlled in an interlocking manner;
the second liquid level control unit comprises a second liquid level meter (51) arranged on the main body (21) and a backflow valve (52) used for regulating and controlling the backflow amount of the concentrated precursor slurry, and the second liquid level meter (51) and the backflow valve (52) are controlled in an interlocking mode.
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