CN109663560B - Ternary positive electrode material precursor reaction kettle - Google Patents
Ternary positive electrode material precursor reaction kettle Download PDFInfo
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- CN109663560B CN109663560B CN201910086204.4A CN201910086204A CN109663560B CN 109663560 B CN109663560 B CN 109663560B CN 201910086204 A CN201910086204 A CN 201910086204A CN 109663560 B CN109663560 B CN 109663560B
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 157
- 239000002243 precursor Substances 0.000 title claims abstract description 27
- 239000007774 positive electrode material Substances 0.000 title claims description 12
- 230000006911 nucleation Effects 0.000 claims abstract description 34
- 238000010899 nucleation Methods 0.000 claims abstract description 34
- 230000002093 peripheral effect Effects 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 25
- 239000002002 slurry Substances 0.000 claims description 23
- 239000010406 cathode material Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008139 complexing agent Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 2
- 239000010405 anode material Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
Abstract
The invention relates to a ternary anode material precursor reaction kettle, which comprises a reaction kettle body, wherein a feed inlet, a discharge outlet and a fixed mounting port are arranged on the reaction kettle body; the device also comprises a nucleation reaction device, a first flow dividing and collecting device and a second flow dividing and collecting device; the nucleation reaction device comprises an inner rotor and an outer stator, the peripheral edge of the outer stator is fixed on a fixed mounting port of the reaction kettle body, the inner rotor is positioned in a stator cavity of the outer stator, and an inclined clearance channel is formed between the inclined outer side wall of the inner rotor and the inclined inner side wall of the outer stator; the first flow dividing and collecting device comprises a first flow dividing valve, the first flow dividing valve is provided with a first inflow port, a first flow dividing port and a second flow dividing port, the second flow dividing and collecting device comprises a second flow dividing valve, the second flow dividing valve is provided with a second inflow port, a third flow dividing port and a fourth flow dividing port, the first flow dividing port and the third flow dividing port are communicated with a feeding port on the reaction kettle body, and the second flow dividing port and the fourth flow dividing port are communicated with an inlet of the nucleation reaction device.
Description
Technical Field
The invention belongs to the field of preparation equipment of ternary cathode material precursors of lithium batteries, and particularly relates to a ternary cathode material precursor reaction kettle.
Background
The nickel-cobalt-manganese ternary anode material is a novel anode material which appears in recent years, and is widely applied to the industries of novel energy sources, mineral extraction, metal smelting, material processing and the like due to the advantages of low cost, good environmental protection, high capacity, good cycle performance and the like.
At present, in a plurality of synthesis methods of ternary positive electrode material precursors, the operation of a coprecipitation synthesis method is relatively simple, and the morphology and the size of a product can be regulated and controlled by controlling the precipitation condition in the material precipitation process. Among them, many factors influencing the synthesis of ternary positive electrode material precursors, such as PH, ammonia concentration, solid content, liquid flow, reaction atmosphere, temperature, etc., especially PH, are favorable to the generation of crystal nuclei when PH is higher, and the growth of secondary spheres when PH is lower, but if the morphology and size of the product are regulated by controlling PH, the number and size of particles cannot be precisely controlled, and certain side effects are brought.
In the existing synthesis method, to realize accurate control of the above-mentioned precipitation conditions, it is difficult to realize the control by a single reaction kettle; in addition, for products with the requirements on the size and granularity, the diameter distance of the ternary precursor is controlled by a plurality of reaction kettles to be realized barely, so that the manufacturing cost of the ternary positive electrode material is increased, and the quantity and the size of the particles are difficult to accurately control by adopting the existing reaction kettles.
In view of this, it is an object of the present invention to provide a ternary cathode material precursor reaction vessel.
Disclosure of Invention
The invention aims at: the ternary positive electrode material precursor reaction kettle is provided, and ternary positive electrode material precursor products with different granularity specifications, wider particle size and higher regularity are prepared.
In order to achieve the above purpose, the invention adopts the following technical scheme: the reaction kettle comprises a reaction kettle body, wherein a feed port, a discharge port and a fixed mounting port are formed in the reaction kettle body, and a stirring device is arranged on the reaction kettle body;
the device also comprises a nucleation reaction device, a first flow dividing and collecting device and a second flow dividing and collecting device;
the nucleation reaction device comprises an inner rotor and an outer stator, wherein the inner rotor is of a rotor structure, the appearance of the rotor structure is of an inverted truncated cone shape, the outer stator is of a stator structure, a stator cavity is arranged in the stator structure, the stator cavity is of a funnel shape, and the shape and the size of the stator cavity are matched with those of the inner rotor;
the first flow dividing and collecting device comprises a first flow dividing valve, wherein the first flow dividing valve is provided with a first inflow port, a first flow dividing port and a second flow dividing port, a first control valve is arranged for the first flow dividing port, and a second control valve is arranged for the second flow dividing port; the second flow dividing and collecting device comprises a second flow dividing valve, the second flow dividing valve is provided with a second inflow port, a third flow dividing port and a fourth flow dividing port, a third control valve is arranged for the third flow dividing port, and a fourth control valve is arranged for the second flow dividing port;
in the assembled state, the peripheral edge of the outer stator is fixed on a fixed mounting port of the reaction kettle body, the inner rotor is positioned in a stator cavity of the outer stator, an inclined clearance channel is formed between the inclined outer side wall of the inner rotor and the inclined inner side wall of the outer stator, the upper end of the clearance channel is an inlet of the nucleation reaction device, and the lower end of the clearance channel is an outlet of the nucleation reaction device;
the first shunt opening and the third shunt opening are both communicated with a feed inlet on the reaction kettle body, and the second shunt opening and the fourth shunt opening are both communicated with an inlet of the nucleation reaction device; the split ratio of the first split valve is the same as that of the second split valve;
in the working state, the reaction raw materials are split through the first splitter valve and the second splitter valve according to the same split ratio; when the first control valve and the third control valve are opened, the split reaction raw materials enter the reaction kettle body from a feed inlet on the reaction kettle body and quickly form a first batch of crystal nuclei under the stirring of the stirring device, and when the reaction raw materials continue to enter the reaction kettle body from the feed inlet on the reaction kettle body, the generated precipitate can cover the outer surface of the first batch of crystal nuclei and continue to grow on the basis of the first batch of crystal nuclei; when the second control valve and the fourth control valve are opened, the split reaction raw materials enter the gap channel between the inner rotor and the outer stator from the inlet of the nucleation reaction device, a second batch of crystal nuclei are rapidly formed in the gap channel, the second batch of crystal nuclei slowly fall into the reaction kettle body under the action of gravity, a third batch and a fourth batch of crystal nuclei can be formed in the reaction process by adjusting the second control valve and the fourth control valve, and the nth batch of crystal nuclei are formed by analogy and fall into the reaction kettle body; thus, preparing ternary positive electrode material precursors with various diametral distance specifications;
the bottom of the reaction kettle body is also provided with a concentrating chamber, the concentrating chamber comprises a cavity, the cavity is divided into an upper concentrating chamber and a lower concentrating chamber by a filter layer, the bottom of the upper concentrating chamber is provided with a slurry outlet, and the bottom of the lower concentrating chamber is provided with a clear liquid outlet;
the device also comprises a bottom valve, the bottom valve comprises a first valve, a second valve and a connecting rod, the first valve and the second valve are fixed on the connecting rod at intervals, the first valve is arranged corresponding to a discharge hole of the reaction kettle body, and the second valve is arranged corresponding to a slurry outlet of the upper concentrating chamber;
the foot valve has two operating states: in a first working state, the first valve covers the discharge port of the reaction kettle body to close the discharge port of the reaction kettle body, and meanwhile, the second valve is opened relative to the slurry outlet of the upper concentrating chamber; under the second working condition, the second valve covers the slurry outlet of the upper concentrating chamber so as to close the slurry outlet of the upper concentrating chamber, and meanwhile, the first valve is opened relative to the discharge port of the reaction kettle body.
The relevant content explanation in the technical scheme is as follows:
1. in the scheme, the filter layer adopts a ceramic membrane filter layer, and the range of the filter pore diameter in the ceramic membrane filter layer is 1-3 um.
2. In the scheme, the device further comprises a circulating pump, wherein an input port of the circulating pump is communicated with the upper concentrating cavity, and an output port of the circulating pump is communicated with the reaction kettle body.
3. In the scheme, the system also comprises a PH sensor, a controller and a metering pump; the PH sensor is arranged in the reaction kettle body and used for detecting the PH value in the reaction kettle body, the output end of the PH sensor is connected to the input end of the controller, the output end of the controller is connected with the input end of the metering pump, and the output end of the metering pump is connected with the second inflow port of the second flow dividing valve and used for outputting alkali liquor for regulating the PH value.
4. In the above scheme, the device further comprises a third flow distributing and collecting device, wherein the third flow distributing and collecting device comprises a third flow distributing valve, and the third flow distributing valve is provided with a third inflow port, a fifth flow distributing port and a sixth flow distributing port;
the first diverter valve is used for diverting the nickel-cobalt-manganese mixed salt solution in the reaction raw material, the second diverter valve is used for diverting the alkali solution in the reaction raw material, and the third diverter valve is used for diverting the complexing agent solution in the reaction raw material.
5. In the above scheme, the inner rotor adopts a permanent magnet rotor.
6. In the above scheme, the inclination direction of the clearance channel is inclined from top to bottom to the axial center.
7. In the scheme, the width range of the clearance channel is 1 mm-2 mm.
The working principle and the advantages of the invention are as follows:
the invention relates to a ternary anode material precursor reaction kettle, which comprises a nucleation reaction device, a first flow distribution and collection device and a second flow distribution and collection device, wherein the nucleation reaction device comprises an inner rotor and an outer stator, the inner rotor is of a rotor structure, the appearance of the rotor structure is of an inverted truncated cone shape, the outer stator is of a stator structure, a stator cavity is arranged in the stator structure, the stator cavity is of a funnel shape, and the shape and the size of the stator cavity are matched with those of the inner rotor; the first flow dividing and collecting device comprises a first flow dividing valve, the first flow dividing valve is provided with a first inflow port, a first flow dividing port and a second flow dividing port, a first control valve is arranged for the first flow dividing port, a second control valve is arranged for the second flow dividing port, the second flow dividing and collecting device comprises a second flow dividing valve, the second flow dividing valve is provided with a second inflow port, a third flow dividing port and a fourth flow dividing port, a third control valve is arranged for the third flow dividing port, and a fourth control valve is arranged for the fourth flow dividing port;
in the assembled state, the peripheral edge of the outer stator is fixed on a fixed mounting port of the reaction kettle body, the inner rotor is positioned in a stator cavity of the outer stator, an inclined clearance channel is formed between the inclined outer side wall of the inner rotor and the inclined inner side wall of the outer stator, the upper end of the clearance channel is an inlet of the nucleation reaction device, and the lower end of the clearance channel is an outlet of the nucleation reaction device; the first shunt port is communicated with a feed port on the reaction kettle body, and the second shunt port is communicated with an inlet of the nucleation reaction device; the third split-flow port is communicated with a feed port on the reaction kettle body, and the fourth split-flow port is communicated with an inlet of the nucleation reaction device;
under the state that the inner rotor rotates at a high speed relative to the outer stator, the reaction raw materials entering the gap channel are driven to be quickly mixed, nucleate and precipitate, crystal nuclei with smaller granularity generated in the gap channel slowly fall into the reaction kettle body through the inclined arrangement of the gap channel, and the reaction raw materials entering from the feed inlet of the reaction kettle body and the content proportion and the speed proportion of the reaction raw materials entering from the inlet of the nucleation reaction device are controlled by controlling the opening and closing of the first shunt opening and the second shunt opening in the first shunt and flow collecting device, so that the ternary anode material precursors with various different particle sizes are prepared.
The method has good reliability and low cost, adopts a single reaction kettle body, and simultaneously carries out nucleation and particle growth under the same PH value, and can effectively control the nucleation rate and the number of crystal nuclei by adjusting the first and second shunt valves, thereby preparing the ternary positive electrode material precursor product with wider particle size and higher regularity.
Drawings
The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way. In addition, the shapes, proportional sizes, and the like of the respective components in the drawings are merely illustrative for aiding the understanding of the present application, and are not particularly limited. Those skilled in the art who have the benefit of the teachings of this application may select various possible shapes and scale dimensions to practice this application as the case may be. In the drawings:
FIG. 1 is a cross-sectional view of a precursor reactor of the present embodiment;
fig. 2 is an enlarged view of fig. 1 at a in the present embodiment.
In the above figures: 1. a reaction kettle body; 10. a feed inlet; 11. a discharge port; 2. a nucleation reaction device; 20. an inner rotor; 21. an outer stator; 22. an inlet; 23. an outlet; 24. a clearance channel; 3. a first current and flow dividing device; 30. an inflow port; 31. a first control valve; 32. a second control valve; 4. a concentrating chamber; 40. a first valve; 41. a second valve; 42. a connecting rod; 43. a filter layer; 44. a circulation pump; 45. an upper concentrating chamber; 46. a lower concentrating chamber; 5. a stirring rod; 50. stirring paddles; 51. a stirring motor; 6. a second split-flow header; 60. an inflow port; 61. a third control valve; 62. a fourth control valve; 7. A PH sensor; 70. a controller; 71. metering pump.
Description of the embodiments
The invention is further described below with reference to the accompanying drawings and examples:
examples: ternary positive electrode material precursor reaction kettle
Referring to fig. 1, the reactor comprises a reactor body 1, wherein a feed inlet 10, a discharge outlet 11 and a fixed mounting opening positioned on a reactor cover of the reactor body 1 are arranged on the reactor body 1. Be equipped with agitating unit on the reation kettle body 1, this agitating unit includes agitator motor 51 and stirring rod 5, stirring rod 5 stretches into the inside of the reation kettle body 1 by fixed mounting mouth, and agitator motor 51 is connected to stirring rod 5 upper end, and a plurality of stirring rake 50 are connected to stirring rod 5 lower extreme region, and stirring motor 51 drive stirring rod 5 axial rotation to drive stirring rake 50 and stir.
Also comprises a nucleation reaction device 2, a first flow dividing and collecting device 3 and a second flow dividing and collecting device 6.
Referring to fig. 2, the nucleation reaction device 2 includes an inner rotor 20 and an outer stator 21, the inner rotor 20 is a rotor structure, the outer shape of the rotor structure is an inverted truncated cone, the outer stator 21 is a stator structure, the inside of the stator structure is provided with a stator cavity, the stator cavity is funnel-shaped, and the shape and size of the stator cavity are matched with those of the inner rotor 20. In this embodiment, the inner rotor 20 is a permanent magnet rotor, and the surface materials of the inner rotor 20 and the outer stator 21 are polytetrafluoroethylene.
The first flow dividing and collecting device 3 comprises a first flow dividing valve, the first flow dividing valve is provided with an inflow port 30, a first flow dividing port and a second flow dividing port, a first control valve 31 is arranged for the first flow dividing port, a second control valve 32 is arranged for the second flow dividing port, and electromagnetic valves are adopted for the first control valve 31 and the second control valve 32; the second flow dividing and collecting device 6 comprises a second flow dividing valve, the second flow dividing valve is provided with a second inflow port 60, a third flow dividing port and a fourth flow dividing port, a third control valve 61 is arranged for the third flow dividing port, and a fourth control valve 62 is arranged for the second flow dividing port; wherein, the third control valve 61 and the fourth control valve 62 are electromagnetic valves. In this embodiment, the first control valve 31 and the third control valve 61 are the same set of reaction control valves, and the second control valve 32 and the fourth control valve 62 are also the same set of reaction control valves, and the two sets of reaction control valves may be opened and controlled simultaneously or may be opened and controlled separately.
In this embodiment, a first flow dividing and collecting device 3 and a second flow dividing and collecting device 6 are adopted, wherein the first flow dividing valve is used for dividing the nickel-cobalt-manganese mixed salt solution in the reaction raw material, the second flow dividing valve is used for dividing the alkaline solution in the reaction raw material, and the complexing agent solution can be mixed into the nickel-cobalt-manganese mixed salt solution or can be mixed into the alkaline solution. In fact, a third flow dividing and collecting device may also be provided, comprising a third flow dividing valve having a third inflow opening, a fifth flow dividing opening for which a fifth control valve is provided, and a sixth flow dividing opening for which a sixth control valve is provided; at this time, the first diverter valve is used for the reposition of redundant personnel of nickel cobalt manganese mixed salt solution in the reaction raw materials, and the second diverter valve is used for the reposition of redundant personnel of alkali solution in the reaction raw materials, and the third diverter valve is used for the reposition of redundant personnel of complexing agent solution in the reaction raw materials. The number of the current dividing and collecting devices in the embodiment is not limited.
In the assembled state, the outer peripheral edge of the outer stator 21 is fixed on a fixed mounting port of the reaction kettle body 1, which is positioned on the kettle cover, the center of the inner rotor 20 is connected with the stirring rod 5, and the inner rotor 20 is positioned in a stator cavity of the outer stator 21. An inclined gap channel 24 is formed between the inclined outer side wall of the inner rotor 20 and the inclined inner side wall of the outer stator 21, the upper end of the gap channel 24 is the inlet 22 of the nucleation reaction device 2, the lower end is the outlet 23 of the nucleation reaction device 2, and in this embodiment, the width of the gap channel 24 is 1mm. In fact, the width of the clearance channel 24 may also be set to 1.5mm, 2mm, etc., not limited to 1mm of the present application. In addition, the inner rotor 20 and the stirring rod 5 may be fixedly connected, and at this time, the rotation speeds of the stirring motor 51 and the inner rotor 20 may be the same, and in practice, the rotation speeds of the inner rotor 20 and the stirring rod 5 may be independently controlled by rotationally connecting the inner rotor 20 and the stirring rod 5.
The first split-flow port is communicated with a feed port 10 on the reaction kettle body 1, and the second split-flow port is communicated with an inlet 22 of the nucleation reaction device 2; the third split-flow port is communicated with the feeding port 10 on the reaction kettle body 1, and the fourth split-flow port is communicated with the inlet 22 of the nucleation reaction device 2.
The embodiment also comprises a PH sensor 7, a controller 70, a metering pump 71 and a second current and flow dividing device 6. The PH sensor 7 is arranged in the reaction kettle body 1 and used for detecting the PH value in the reaction kettle body 1, the output end of the PH sensor 7 is connected to the input end of the controller 70, the output end of the controller 70 is connected with the input end of the metering pump 71, and the output end of the metering pump 71 is connected with the second inflow port 60 of the second shunt valve and used for outputting alkali liquor or acid liquor for regulating the PH value. In operation, the PH sensor 7 monitors the PH value in the reaction kettle body 1 in real time, and feeds back the PH value to the controller 70, and the controller 70 controls the output of the metering pump 71 according to the received PH information, so as to control the PH value in the reaction kettle body 1.
In the operating state, the stirring motor 51 drives the stirring rod 5, the inner rotor 20 and the stirring paddle 50 to rotate at a high speed. The mixed sulfate solution, complexing agent and alkali liquor are respectively delivered to a first flow distributing and collecting device 3 according to the following formula 4:1, splitting the split ratio; when the first control valve 31 and the third control valve 61 are opened, the split reaction raw materials enter the reaction kettle body 1 from the feed inlet 10 on the reaction kettle body 1 and quickly form first crystal nuclei under the stirring of the stirring device, and when the reaction raw materials continue to enter the reaction kettle body 1 from the feed inlet 10 on the reaction kettle body 1, the generated precipitate can cover the outer surface of the first crystal nuclei and continue to grow on the basis of the first crystal nuclei; when the second control valve 32 and the fourth control valve 62 are opened, the split reaction raw materials enter a gap channel 24 between the inner rotor 20 and the outer stator 21 through an inlet 22 of the nucleation reaction device 2, a second crystal nucleus is rapidly formed in the gap channel 24, the second crystal nucleus slowly falls into the reaction kettle body 1 under the action of gravity, then continues to grow into particles with different particle sizes from the first crystal nucleus by the second crystal nucleus, a third crystal nucleus and a fourth crystal nucleus can be formed by adjusting the opening and closing of the second control valve and the fourth control valve 62 in the reaction process, and an nth crystal nucleus is formed by analogy and falls into the reaction kettle body 1; therefore, a plurality of ternary positive electrode material precursors with different particle diameters are prepared, and the nucleation rate can be effectively controlled, so that a ternary precursor product with wider particle diameter distance is prepared. Of course, the flow dividing ratio of the flow dividing and collecting valve can be freely adjusted according to the product requirement, and the feed inlet 10 of the reaction kettle body 1 and/or the inlet 22 of the nucleation reaction device 2 can be cut off, so that the generation of crystal nuclei or particles with different specifications can be effectively controlled.
In addition, in this embodiment, a concentrating chamber 4 is further disposed at the bottom of the reaction kettle body 1, the concentrating chamber 4 includes a cavity, the cavity is divided into an upper concentrating chamber 45 and a lower concentrating chamber 46 by a filtering layer 43, a slurry outlet is disposed at the bottom of the upper concentrating chamber 45, and a clear liquid outlet is disposed at the bottom of the lower concentrating chamber 46. Wherein, the filter layer 43 adopts a ceramic membrane filter layer, the range of the filter aperture in the ceramic membrane filter layer is 1-3 um, and specifically, the ceramic membrane filter layer with the filter aperture of 2 um can be adopted, and the ceramic membrane filter layers with the filter apertures of 1 um, 3um and the like can also be adopted, so that the filter is not limited to the aperture of the present application.
The bottom valve comprises a first valve 40, a second valve 41 and a connecting rod 42, wherein the first valve 40 and the second valve 41 are fixed on the connecting rod 42 at intervals, the first valve 40 is arranged corresponding to the discharge port 11 of the reaction kettle body 1, and the second valve 41 is arranged corresponding to the slurry outlet of the upper concentration chamber 45. By rotating the bottom valve, the discharge port 11 of the reaction kettle body 1 or the slurry outlet of the upper concentrating chamber 45 can be selectively opened.
The foot valve has two operating states: in the first working state, the first valve 40 covers the discharge port 11 of the reaction kettle body 1 to close the discharge port 11 of the reaction kettle body 1, and the second valve 41 is opened relative to the slurry outlet of the upper concentrating chamber 45; in the second working state, the second valve 41 covers the slurry outlet of the upper concentrating chamber 45 to close the slurry outlet of the upper concentrating chamber 45, and at the same time, the first valve 40 is opened relative to the discharge port 11 of the reaction kettle body 1. The embodiment further comprises a circulating pump 44, wherein an input port of the circulating pump 44 is communicated with the upper concentrating chamber 45, and an output port of the circulating pump 44 is communicated with the reaction kettle body 1.
In the reaction process, in the first working state of the bottom valve, slurry in the reaction kettle body 1 flows into the upper concentrating chamber 45, and in the second working state of the bottom valve, part of clear liquid in the slurry flows into the lower concentrating chamber 46 through the filter layer 43. After the slurry outlet is opened, the concentrated slurry can also flow into the reaction kettle body 1 again through the liquid inlet 10 of the reaction kettle body 1 by the circulating pump 44. Because the higher the solid content of the slurry is, the better the appearance of granulation, namely the spherical quality is, if the solid content of the slurry needs to be improved, the clear liquid outlet is opened to remove clear liquid, and the slurry can be continuously enriched.
It will be understood that when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
In the description of the present application, unless otherwise indicated, the meaning of "a plurality" in the description of the present application is two or more.
The use of the terms "comprises" or "comprising" to describe combinations of elements, components, or steps herein also contemplates embodiments consisting essentially of such elements, components, or steps. By using the term "may" herein, it is intended that any attribute described as "may" be included is optional.
Multiple elements, components, parts or steps can be provided by a single integrated element, component, part or step. Alternatively, a single integrated element, component, part or step may be divided into separate plural elements, components, parts or steps. The disclosure of "a" or "an" to describe an element, component, section or step is not intended to exclude other elements, components, sections or steps.
It is to be understood that the above description is intended to be illustrative, and not restrictive. Many embodiments and many applications other than the examples provided will be apparent to those of skill in the art upon reading the above description. The scope of the present teachings should, therefore, be determined not with reference to the above description, but instead should be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are incorporated herein by reference for the purpose of completeness. The omission of any aspect of the subject matter disclosed herein in the preceding claims is not intended to forego such subject matter, nor should the applicant be deemed to have such subject matter not considered to be part of the subject matter of the disclosed application.
The above list of detailed descriptions is only specific to practical embodiments of the present application, and they are not intended to limit the scope of the present application, and all equivalent embodiments or modifications that do not depart from the spirit of the technical spirit of the present application are included in the scope of the present application.
Claims (8)
1. The reaction kettle comprises a reaction kettle body, wherein a feed port, a discharge port and a fixed mounting port are formed in the reaction kettle body, and a stirring device is arranged on the reaction kettle body;
the method is characterized in that: the device also comprises a nucleation reaction device, a first flow dividing and collecting device and a second flow dividing and collecting device;
the nucleation reaction device comprises an inner rotor and an outer stator, wherein the inner rotor is of a rotor structure, the appearance of the rotor structure is of an inverted truncated cone shape, the outer stator is of a stator structure, a stator cavity is arranged in the stator structure, the stator cavity is of a funnel shape, and the shape and the size of the stator cavity are matched with those of the inner rotor;
the first flow dividing and collecting device comprises a first flow dividing valve, wherein the first flow dividing valve is provided with a first inflow port, a first flow dividing port and a second flow dividing port, a first control valve is arranged for the first flow dividing port, and a second control valve is arranged for the second flow dividing port; the second flow dividing and collecting device comprises a second flow dividing valve, the second flow dividing valve is provided with a second inflow port, a third flow dividing port and a fourth flow dividing port, a third control valve is arranged for the third flow dividing port, and a fourth control valve is arranged for the second flow dividing port;
in the assembled state, the peripheral edge of the outer stator is fixed on a fixed mounting port of the reaction kettle body, the inner rotor is positioned in a stator cavity of the outer stator, an inclined clearance channel is formed between the inclined outer side wall of the inner rotor and the inclined inner side wall of the outer stator, the upper end of the clearance channel is an inlet of the nucleation reaction device, and the lower end of the clearance channel is an outlet of the nucleation reaction device;
the first shunt opening and the third shunt opening are both communicated with a feed inlet on the reaction kettle body, and the second shunt opening and the fourth shunt opening are both communicated with an inlet of the nucleation reaction device; the split ratio of the first split valve is the same as that of the second split valve;
in the working state, the reaction raw materials are split through the first splitter valve and the second splitter valve according to the same split ratio; when the first control valve and the third control valve are opened, the split reaction raw materials enter the reaction kettle body from a feed inlet on the reaction kettle body and quickly form a first batch of crystal nuclei under the stirring of the stirring device, and when the reaction raw materials continue to enter the reaction kettle body from the feed inlet on the reaction kettle body, the generated precipitate can cover the outer surface of the first batch of crystal nuclei and continue to grow on the basis of the first batch of crystal nuclei; when the second control valve and the fourth control valve are opened, the split reaction raw materials enter the gap channel between the inner rotor and the outer stator from the inlet of the nucleation reaction device, a second batch of crystal nuclei are rapidly formed in the gap channel, the second batch of crystal nuclei slowly fall into the reaction kettle body under the action of gravity, a third batch and a fourth batch of crystal nuclei can be formed in the reaction process by adjusting the second control valve and the fourth control valve, and the nth batch of crystal nuclei are formed by analogy and fall into the reaction kettle body; thus, preparing ternary positive electrode material precursors with various diametral distance specifications;
the bottom of the reaction kettle body is also provided with a concentrating chamber, the concentrating chamber comprises a cavity, the cavity is divided into an upper concentrating chamber and a lower concentrating chamber by a filter layer, the bottom of the upper concentrating chamber is provided with a slurry outlet, and the bottom of the lower concentrating chamber is provided with a clear liquid outlet;
the device also comprises a bottom valve, the bottom valve comprises a first valve, a second valve and a connecting rod, the first valve and the second valve are fixed on the connecting rod at intervals, the first valve is arranged corresponding to a discharge hole of the reaction kettle body, and the second valve is arranged corresponding to a slurry outlet of the upper concentrating chamber;
the foot valve has two operating states: in a first working state, the first valve covers the discharge port of the reaction kettle body to close the discharge port of the reaction kettle body, and meanwhile, the second valve is opened relative to the slurry outlet of the upper concentrating chamber; under the second working condition, the second valve covers the slurry outlet of the upper concentrating chamber so as to close the slurry outlet of the upper concentrating chamber, and meanwhile, the first valve is opened relative to the discharge port of the reaction kettle body.
2. The ternary cathode material precursor reaction kettle according to claim 1, wherein: the filter layer adopts a ceramic membrane filter layer, and the range of the filter pore diameter in the ceramic membrane filter layer is 1-3 um.
3. The ternary cathode material precursor reaction kettle according to any one of claims 1, wherein: the device also comprises a circulating pump, wherein an input port of the circulating pump is communicated with the upper concentrating cavity, and an output port of the circulating pump is communicated with the reaction kettle body.
4. The ternary cathode material precursor reaction kettle according to claim 1, wherein: the system also comprises a PH sensor, a controller and a metering pump; the PH sensor is arranged in the reaction kettle body and used for detecting the PH value in the reaction kettle body, the output end of the PH sensor is connected to the input end of the controller, the output end of the controller is connected with the input end of the metering pump, and the output end of the metering pump is connected with the second inflow port of the second flow dividing valve and used for outputting alkali liquor for regulating the PH value.
5. The ternary cathode material precursor reaction kettle according to claim 1, wherein: the device also comprises a third flow distributing and collecting device, wherein the third flow distributing and collecting device comprises a third flow distributing valve, and the third flow distributing valve is provided with a third inflow port, a fifth flow distributing port and a sixth flow distributing port; the first diverter valve is used for diverting the nickel-cobalt-manganese mixed salt solution in the reaction raw material, the second diverter valve is used for diverting the alkali solution in the reaction raw material, and the third diverter valve is used for diverting the complexing agent solution in the reaction raw material.
6. The ternary cathode material precursor reaction kettle according to claim 1, wherein: the inner rotor adopts a permanent magnet rotor.
7. The ternary cathode material precursor reaction kettle according to claim 4 or 5, wherein: the inclination direction of the clearance channel is inclined from top to bottom to the axial center.
8. The ternary cathode material precursor reaction kettle according to claim 1, wherein: the width of the clearance channel ranges from 1mm to 2mm.
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