CN113441097A - Cobalt carbonate production system and method - Google Patents
Cobalt carbonate production system and method Download PDFInfo
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- CN113441097A CN113441097A CN202010225035.0A CN202010225035A CN113441097A CN 113441097 A CN113441097 A CN 113441097A CN 202010225035 A CN202010225035 A CN 202010225035A CN 113441097 A CN113441097 A CN 113441097A
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- 229910021446 cobalt carbonate Inorganic materials 0.000 title claims abstract description 71
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 title claims abstract description 71
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 190
- 239000000463 material Substances 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 21
- 239000002562 thickening agent Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 230000008719 thickening Effects 0.000 claims description 11
- 239000012452 mother liquor Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- 230000001502 supplementing effect Effects 0.000 claims description 6
- 239000013067 intermediate product Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 19
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 7
- KKTCWAXMXADOBB-UHFFFAOYSA-N azanium;hydrogen carbonate;hydrate Chemical compound [NH4+].O.OC([O-])=O KKTCWAXMXADOBB-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 150000001868 cobalt Chemical class 0.000 description 4
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 239000010405 anode material Substances 0.000 description 2
- -1 cobalt oxyhydroxide Chemical compound 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 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
-
- 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
- B01J19/0066—Stirrers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/06—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a cobalt carbonate production system and a cobalt carbonate production method, wherein the system comprises at least four reaction kettles, the four reaction kettles comprise a first reaction kettle, a second reaction kettle, a third reaction kettle and a fourth reaction kettle, the reaction kettles are all provided with side feed inlets, the middle parts of the reaction kettles are all provided with discharge overflow ports, the bottoms of the reaction kettles are all provided with bottom valves, the side feed inlets of the second reaction kettle and the fourth reaction kettle are all connected with the discharge overflow port of the first reaction kettle, the side feed inlet of the third reaction kettle is connected with the discharge overflow port of the second reaction kettle, and the discharge overflow port of the upper stage reaction kettle is higher than the side feed inlet of the lower stage reaction kettle. The method ensures the continuity and stability of cobalt carbonate growth, enables the cobalt carbonate particles to grow step by step in the reactor-separating reaction process, is beneficial to obtaining finished cobalt carbonate particles with larger particle size and better consistency, and improves the production efficiency.
Description
Technical Field
The invention belongs to the technical field of cobalt carbonate, and particularly relates to a cobalt carbonate production system and a cobalt carbonate production method.
Background
At present, lithium ion batteries are widely applied to the 3C field, such as smart phones, cameras, unmanned aerial vehicles and the like, and the performance and cost of the lithium ion batteries depend on the performance and cost of the lithium ion battery anode materials to a great extent; at present, the anode material in the 3C field is mainly lithium cobaltate, has high specific capacity, stable structure and no memory effect, and is a novel green secondary battery; lithium cobaltate is mainly formed by sintering cobaltosic oxide and a lithium source at high temperature, wherein the lithium source is mainly lithium hydroxide and lithium carbonate, and the cobaltosic oxide is mainly formed by roasting cobalt carbonate or cobalt oxyhydroxide at low temperature, wherein the cobalt carbonate can be used for sintering the lithium cobaltate with good appearance, large particles and high tap density; cobalt carbonate is a precursor of lithium cobaltate, the physicochemical properties of the cobalt carbonate are inherited to a certain extent, and the physicochemical properties of the cobalt carbonate, such as tap density, specific surface area and the like, have important influence on the lithium cobaltate.
The preparation of cobalt carbonate is mainly that ammonium bicarbonate water solution and cobalt salt are nucleated and grow in a reaction kettle by controlling pH, temperature, rotating speed, solid content and the like, and finally spherical or spheroidal cobalt carbonate is generated. Chinese patent publication No. CN108190971A discloses a method and system for preparing cobalt carbonate, which uses seed crystals to prepare cobalt carbonate, on one hand, the yield and preparation efficiency of cobalt carbonate are improved, on the other hand, small-particle-size cobalt carbonate seed crystals are used to control the particle size of large-particle-size cobalt carbonate in the reaction mother liquor, so as to ensure the consistency and stability of large-particle-size cobalt carbonate grown by continuous process, but still more manual intermittent operations exist, and the production efficiency is not high; the invention patent with publication number CN108275729 discloses a system and a method for preparing cobalt carbonate, wherein a thickener structure is added, so that the efficiency of continuous operation is improved, but the cobalt carbonate cannot grow fully after nucleation, and finally obtained cobalt carbonate particles have small particle size and cannot meet the requirements on quality.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art, and provide a cobalt carbonate production system and method capable of improving production efficiency and increasing particle size of a cobalt carbonate particle finished product.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the utility model provides a cobalt carbonate production system, includes four at least reation kettle, four reation kettle include first reation kettle, second reation kettle, third reation kettle and fourth reation kettle, reation kettle all is provided with the side feed inlet, the middle part all is provided with ejection of compact overflow mouth, the bottom all is provided with the bottom valve, and second reation kettle and fourth reation kettle's side feed inlet all links to each other with first reation kettle's ejection of compact overflow mouth, and third reation kettle's side feed inlet links to each other with second reation kettle's ejection of compact overflow mouth, and last one-level reation kettle's ejection of compact overflow mouth is higher than next one-level reation kettle's side feed inlet.
Furthermore, top return ports are formed in the tops of the reaction kettles, liquid discharge overflow pipes are mounted on the upper portions of the reaction kettles, overflow grooves and thickening machines are correspondingly arranged on the four reaction kettles, the liquid discharge overflow ports of the liquid discharge overflow pipes are connected with the feeding ports of the overflow grooves, the discharge ports of the overflow grooves are connected to the thickening machines, and cobalt carbonate materials obtained after thickening by the thickening machines enter the reaction kettles again through the top return ports.
Furthermore, the structure and the volume of the four reaction kettles are the same, the volume below the liquid discharge overflow port in the reaction kettle is the effective volume of the reaction kettle, and the horizontal plane of the discharge overflow port divides the effective volume into an upper part and a lower part which are equal.
Further, be equipped with the stirring rake in the reation kettle, the stirring rake includes (mixing) shaft and anchor formula oar, the top of anchor formula oar is provided with oblique oar, the one end of oblique oar is installed on the (mixing) shaft, the other end with the top fixed connection of anchor formula oar.
Furthermore, a flow baffle plate is fixedly mounted on a top cover of the reaction kettle, is positioned on the outer side of the stirring paddle and extends downwards to the inside of the reaction kettle close to the junction of the straight cylinder and the U-shaped bottom of the reaction kettle.
Further, be equipped with the inlet pipe in the reation kettle, inlet pipe swing joint is in reation kettle top cap, and inlet pipe lower extreme tip is bent to the (mixing) shaft.
Further, the oblique paddle comprises two blades, and the blades of the oblique paddle are inclined downwards by 45 degrees relative to the horizontal plane.
The production method using the cobalt carbonate production system comprises the following steps:
s1, adding raw materials into a first reaction kettle for reaction;
s2, after the first reaction kettle completely reacts, opening the discharging overflow port to transfer the material above the discharging overflow port to a second reaction kettle, and then supplementing raw materials to the first reaction kettle and the second reaction kettle to enable the first reaction kettle and the second reaction kettle to continue to react;
s3, after the materials in the first reaction kettle and the second reaction kettle are completely reacted, opening the discharge overflow ports of the first reaction kettle and the second reaction kettle, correspondingly transferring the materials above the discharge overflow ports to a fourth reaction kettle and a third reaction kettle respectively, and supplementing raw materials to enable the materials in all the reaction kettles to continue to react;
and S4, after all the reaction is completed, discharging all the materials in the four reaction kettles through the bottom valves to obtain finished product materials.
Furthermore, in the reaction process of each reaction kettle, the upper mother liquor is conveyed to the overflow groove through the liquor drainage overflow pipe, then is pumped into the thickener for thickening, and the thickened slurry is conveyed to the reaction kettle for continuous growth.
Further, S1 reacts until 9-11 mu m cobalt carbonate crystal nuclei are obtained, S2 reacts until 13-15 mu m cobalt carbonate intermediate products are obtained, and S3 reacts until 17-19 mu m cobalt carbonate finished products are obtained.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts a form of separated kettle reaction to enable cobalt carbonate to grow into large granules from small granules step by step, a discharge overflow port is arranged on the kettle wall, side feed inlets of a second reaction kettle and a fourth reaction kettle are both connected with a discharge overflow port of a first reaction kettle, a discharge overflow port of the second reaction kettle is connected with a side feed inlet of a third reaction kettle, when the first reaction kettle completely reacts, the discharge overflow port is opened to transfer materials to the second reaction kettle, then raw materials are supplemented to the first reaction kettle and the second reaction kettle to enable the materials to continue to react, when the materials in the first reaction kettle and the second reaction kettle respectively completely react, the discharge overflow ports of the first reaction kettle and the second reaction kettle are opened to correspondingly transfer the materials to the fourth reaction kettle and the third reaction kettle respectively, the raw materials are supplemented to enable the materials in all the reaction kettles to continue to react, and after all the materials are completely reacted, and (4) discharging all the materials in the four reaction kettles through the bottom valves to obtain large-particle finished product materials. By adopting the production method, a continuous production process can be formed, the consistency of the sub-kettles is controlled by cascade connection of the multi-stage growth reaction kettles and division of the multi-stage growth reaction kettles at the overflow ports at the same relative height, so that the growth continuity and stability of the cobalt carbonate are ensured, the cobalt carbonate particles grow step by step in the sub-kettle reaction process, the finished product cobalt carbonate particles with larger particle size and better consistency can be obtained, and the production efficiency is improved.
(2) The invention uses the combined paddle of the inclined paddle and the anchor type paddle in the reaction kettle, the flow velocity of the anchor type paddle is faster near the inner wall of the reaction kettle relative to the middle area, the inclined paddle is added at the top of the anchor type paddle, the mixing effect of the middle part can be improved, the anchor type paddle is matched with the flow baffle plate for use, so that the material liquid rotates/rolls in a more comprehensive direction in the growth process, the stirring and mixing are more uniform, in addition, the end of the feeding pipe bends to the stirring shaft, the pipe orifice is close to the stirring paddle, the cobalt carbonate material liquid is dispersed more rapidly, and the cobalt carbonate crystal growth is facilitated.
(3) In the reaction process of each reaction kettle, the upper mother liquor is discharged to the overflow groove in time, then is sent to the thickener for thickening, and the thickened slurry can be conveyed to the reaction kettle again for continuous growth, so that the cobalt carbonate finished product material with higher yield can be obtained, the whole process does not need manual operation, and the labor is saved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a structural diagram of reaction kettles in a cobalt carbonate production system according to the present invention;
FIG. 2 is a structural diagram between any one of the reaction vessels and the overflow vessel and thickener corresponding to the reaction vessel in the cobalt carbonate production system according to the present invention;
FIG. 3 is a simple structure diagram of any one reaction vessel in the cobalt carbonate production system of the present invention;
in the figures, the reference numbers correspond to the following numbers:
1-reaction kettle 2-overflow trough 3-thickener
4-liquid discharge overflow pipe 5-discharge overflow port 6-bottom valve
7-side feed inlet 8-top return port 9-anchor type paddle
10-inclined paddle 11-baffle plate 12-feeding pipe
101-first reaction kettle 102-second reaction kettle
103-a third reaction kettle 104-a fourth reaction kettle.
Detailed Description
In order to facilitate understanding of the invention, the invention will be described more fully and in detail with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
The cobalt carbonate production system according to a specific embodiment of the present invention, as shown in fig. 1 to 3, includes four reaction kettles 1, which are a first reaction kettle 101, a second reaction kettle 102, a third reaction kettle 103, and a fourth reaction kettle 104, respectively. Top backward flow mouth 8, one side all are provided with side feed inlet 7, opposite side middle part all are provided with ejection of compact overflow mouth 5, flowing back overflow pipe 4 is all installed on upper portion, the bottom all is provided with bottom valve 6 have all been seted up at reation kettle 1's top.
The side feed inlets 7 of the second reaction kettle 102 and the fourth reaction kettle 104 are connected with the discharge overflow port 5 of the first reaction kettle 101, and the side feed inlet 7 of the third reaction kettle 103 is connected with the discharge overflow port 5 of the second reaction kettle 102.
The four reaction kettles 1 are correspondingly provided with an overflow trough 2 and a thickener 3. The flowing back overflow mouth of reation kettle 1's flowing back overflow pipe 4 links to each other with the pan feeding mouth of overflow launder 2, and the discharge gate of overflow launder 2 is connected to thickener 3, and the cobalt carbonate material accessible reation kettle's that obtains after thickener 3 is dense top backward flow mouth 8 gets into reation kettle 1 again to can obtain the cobalt carbonate finished product material of higher output, and whole process need not manual operation, comparatively uses manpower sparingly.
In the above embodiment, the discharge overflow 5 of the first reaction vessel 101 is higher than the side feed inlet 7 of the second reaction vessel 102. The discharge overflow 5 of the second reaction vessel 102 is higher than the side feed inlets 7 of the third reaction vessel 103 and the fourth reaction vessel 104.
In the above embodiment, the four reaction tanks 1 have the same structure and volume. The volume of the reaction kettle 1 below the liquid discharge overflow port is the effective volume of the reaction kettle 1. The horizontal plane of the discharge overflow port 5 can divide the effective volume into an upper part and a lower part which are equal. Like this, four reation kettle 1 all divide the cauldron in the ejection of compact overflow mouth of same relative height (the ejection of compact overflow mouth of different cauldron is highly unanimous to the cauldron bottom), control the uniformity of dividing the cauldron to guarantee the continuity and the stability of cobalt carbonate growth.
In a preferred embodiment, the four reaction kettles 1 have the same volume and are all 500L, and the volume of the overflow groove 2 is 1m3The filtering speed of the thickener is 300L/h, and after being thickened by the thickener 3, the slurry is pumped into the reaction kettle 1 again for continuous growth.
In a preferred embodiment, the stirring paddle of the reaction kettle 1 comprises a stirring shaft and an anchor paddle 9, the top end of the anchor paddle 9 is provided with a slant paddle 10, one end of the slant paddle 10 is installed on the stirring shaft, and the other end is fixedly connected with the top end of the anchor paddle 9. Preferably, the number of the inclined paddles 10 is 2, and the inclined paddles 10 are inclined downwards by 45 degrees relative to the horizontal plane.
In a preferred embodiment, a flow baffle plate 11 is fixedly installed on the top cover of the reaction kettle 1, and the flow baffle plate 11 is located outside the stirring paddle in the reaction kettle 1 and extends downwards to the inside of the reaction kettle 1 near the junction of the straight cylinder and the U-shaped bottom of the reaction kettle 1.
Anchor formula oar 9 is near 1 inner wall of reation kettle for the regional velocity of flow in middle part relatively fast, increases oblique oar 10 at anchor formula oar 9 top, can improve the mixed effect at middle part, uses with keeping off a cooperation of class board 11 for the rotatory direction that rolls of material liquid is more comprehensive in the growth process, and the stirring mixes more evenly.
In a preferred embodiment, a feeding pipe 12 is respectively arranged at two sides of the stirring paddle in the reaction kettle 1, and the feeding pipe 12 is movably connected to the top cover of the reaction kettle 1. The pipe orifice at the lower end of the feed pipe 12 is close to the stirring paddle, and the tail end is bent to the stirring shaft, so that the cobalt carbonate feed liquid is dispersed more rapidly, and the growth of cobalt carbonate crystals is facilitated.
The method for producing cobalt carbonate of one embodiment of the present invention comprises the following steps: the production method comprises the steps of producing four reaction kettles 1, opening a discharge overflow port 5 to transfer materials above the discharge overflow port 5 to a second reaction kettle 102 after a first reaction kettle 1 completely reacts, supplementing raw materials to the first reaction kettle 101 and the second reaction kettle 102 to enable the materials to continuously react, opening the discharge overflow ports 5 of the first reaction kettle 101 and the second reaction kettle 102 after the materials in the first reaction kettle 101 and the second reaction kettle 102 completely react respectively, correspondingly transferring the materials above the discharge overflow port 5 to a fourth reaction kettle 104 and a third reaction kettle 103 respectively, supplementing the raw materials to enable the materials in all the reaction kettles 1 to continuously react, and discharging all the materials in the four reaction kettles 1 through a bottom valve 6 after all the materials in the four reaction kettles 1 completely react to obtain finished product materials.
By adopting the production method, a continuous production process can be formed, and the cobalt carbonate particles grow step by step in the reactor separation reaction process through the cascade connection of the multistage growth reaction kettles, so that the finished product cobalt carbonate particles with larger particle size and better consistency can be obtained, and the production efficiency is improved.
The specific production method comprises the following steps:
firstly, pumping qualified ammonium bicarbonate water solution into a first reaction kettle 101 to serve as base solution, wherein the volume of the base solution is 1/5-1/3 of that of a reaction kettle 1, and the pH value of the base solution is controlled to be 7.8-8.3; after heating to 54-58 ℃, starting a motor for stirring, simultaneously pumping an ammonium bicarbonate water solution and a cobalt salt solution through a metering pump, controlling the flow rate ratio to be 0.9-1.0 and the pH value to be 7.3-7.8, and reacting for 15-20 hours; and the mother liquor on the upper layer is conveyed to an overflow groove 2 through a liquor drainage overflow pipe 4, then is pumped into a thickener 3 for thickening, and the thickened slurry is conveyed into a reaction kettle 1 for continuous growth to obtain cobalt carbonate crystal nuclei with the particle size of 9-11 microns.
Keeping the first reaction kettle 101 stirred, and stopping adding the raw materials; opening a discharge overflow port 5 of the first reaction kettle 101 and a side feed port 7 of the second reaction kettle 102, and conveying the material above the discharge overflow port 5 to the second reaction kettle 102 through the side feed port 7; pumping qualified ammonium bicarbonate water solution and cobalt salt solution into the first reaction kettle 101 and the second reaction kettle 102 through a metering pump for continuous reaction, wherein the flow rate ratio is 0.9-1.0, the reaction lasts for 15-20 hours, the mother liquor on the upper layer in the reaction process is conveyed to an overflow tank 2 through a liquor drainage overflow pipe 4, then the mother liquor is pumped into a thickener 3 for thickening, and the thickened slurry is conveyed into the reaction kettle 1 for continuous growth; obtaining a cobalt carbonate intermediate product with the particle size of 13-15 mu m.
Keeping the first reaction kettle 101 and the second reaction kettle 102 stirred, and stopping adding the raw materials; opening the discharge overflow ports 5 of the first reaction kettle 101 and the second reaction kettle 102 and the side feed ports 7 of the third reaction kettle 103 and the fourth reaction kettle 104, and respectively conveying the materials above the discharge overflow ports 5 of the first reaction kettle 101 and the second reaction kettle 102 to the fourth reaction kettle 104 and the third reaction kettle 103 through the side feed ports 7; and pumping qualified ammonium bicarbonate water solution and cobalt salt solution into the four reaction kettles simultaneously for reaction, wherein the flow rate ratio is 0.9-1.0, reacting for 15-20 hours, and finally obtaining a cobalt carbonate finished product with the particle size of 17-19 mu m, and discharging the cobalt carbonate finished product from a bottom valve of the reaction kettle.
In the above embodiment, in the reaction process of the reaction kettle 1, the mother liquor on the upper layer is conveyed to the overflow tank 2 through the liquid discharge overflow pipe 4, and then is pumped into the thickener 3 for thickening, and the thickened slurry is conveyed into the reaction kettle 1 for continuous growth.
The foregoing is considered as illustrative of the preferred embodiments of the invention and is not to be construed as limiting the invention in any way. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (10)
1. The utility model provides a cobalt carbonate production system, a serial communication port, includes four at least reation kettle (1), four reation kettle (1) are including first reation kettle (101), second reation kettle (102), third reation kettle (103) and fourth reation kettle (104), reation kettle (1) all is provided with side feed inlet (7), the middle part all is provided with ejection of compact overflow mouth (5), the bottom all is provided with bottom valve (6), side feed inlet (7) of second reation kettle (102) and fourth reation kettle (104) all link to each other with ejection of compact overflow mouth (5) of first reation kettle (101), side feed inlet (7) of third reation kettle (103) link to each other with ejection of compact overflow mouth (5) of second reation kettle (102), ejection of compact overflow mouth (5) of last one-level reation kettle (1) are higher than side feed inlet (7) of next-level reation kettle (1).
2. The cobalt carbonate production system according to claim 1, wherein top return ports (8) are formed in the tops of the reaction kettles (1), liquid discharge overflow pipes (4) are installed on the upper portions of the reaction kettles, overflow chutes (2) and thickeners (3) are correspondingly arranged on the four reaction kettles (1), the liquid discharge overflow ports of the liquid discharge overflow pipes (4) are connected with the feed ports of the overflow chutes (2), the discharge ports of the overflow chutes (2) are connected to the thickeners (3), and cobalt carbonate materials obtained after thickening by the thickeners (3) enter the reaction kettles (1) again through the top return ports (8).
3. The cobalt carbonate production system according to claim 2, characterized in that the four reaction kettles (1) have the same structure and volume, the volume of the reaction kettle (1) below the liquid discharge overflow port is the effective volume of the reaction kettle (1), and the horizontal plane of the discharge overflow port (5) divides the effective volume into an upper part and a lower part which are equal.
4. The cobalt carbonate production system according to any one of claims 1 to 3, wherein a stirring paddle is arranged in the reaction kettle (1), the stirring paddle comprises a stirring shaft and an anchor paddle (9), the top end of the anchor paddle (9) is provided with an inclined paddle (10), one end of the inclined paddle (10) is installed on the stirring shaft, and the other end of the inclined paddle is fixedly connected with the top end of the anchor paddle (9).
5. The cobalt carbonate production system according to claim 4, wherein a flow baffle plate (11) is fixedly installed on the top cover of the reaction kettle (1), and the flow baffle plate (11) is located outside the stirring paddle and extends downwards to the inside of the reaction kettle (1) near the junction of the straight barrel and the U-shaped bottom of the reaction kettle.
6. The cobalt carbonate production system according to claim 4, characterized in that a feed pipe (12) is arranged in the reaction kettle (1), the feed pipe (12) is movably connected to the top cover of the reaction kettle (1), and the lower end tip of the feed pipe (12) is bent towards the stirring shaft.
7. Cobalt carbonate production system according to claim 4, characterized in that the tilt paddle (10) comprises two blades, the blades of the tilt paddle (10) being inclined 45 ° downwards with respect to the horizontal plane.
8. A production method using the cobalt carbonate production system according to any one of claims 1 to 7, comprising the steps of:
s1, adding raw materials into a first reaction kettle (101) for reaction;
s2, after the first reaction kettle (101) completely reacts, opening the discharge overflow port (5) to transfer the material above the discharge overflow port (5) to the second reaction kettle (102), and then supplementing raw materials to the first reaction kettle (101) and the second reaction kettle (102) to enable the first reaction kettle (101) and the second reaction kettle (102) to continue to react;
s3, after the materials in the first reaction kettle (101) and the second reaction kettle (102) are completely reacted respectively, opening the discharge overflow ports (5) of the first reaction kettle (101) and the second reaction kettle (102), correspondingly transferring the materials above the discharge overflow ports (5) to a fourth reaction kettle (104) and a third reaction kettle (103) respectively, and supplementing raw materials to enable the materials in all the reaction kettles (1) to continue to react;
and S4, after all reactions are completed, discharging all the materials in the four reaction kettles (1) through the bottom valves (6) to obtain finished product materials.
9. The cobalt carbonate production method according to claim 8, characterized in that during the reaction of each reaction kettle (1), the mother liquor at the upper layer is conveyed to the overflow trough (2) through the drainage overflow pipe (4), and then is pumped into the thickener (3) for thickening, and the thickened slurry is conveyed into the reaction kettle (1) for further growth.
10. The method for producing cobalt carbonate according to claim 8 or 9, wherein S1 is reacted to obtain 9-11 μm cobalt carbonate crystal nuclei, S2 is reacted to obtain 13-15 μm cobalt carbonate intermediate products, and S3 is reacted to obtain 17-19 μm cobalt carbonate finished products.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010225035.0A CN113441097A (en) | 2020-03-26 | 2020-03-26 | Cobalt carbonate production system and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010225035.0A CN113441097A (en) | 2020-03-26 | 2020-03-26 | Cobalt carbonate production system and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024011625A1 (en) * | 2022-07-15 | 2024-01-18 | 宁德时代新能源科技股份有限公司 | Continuous reaction system, manganese iron oxalate precursor, lithium manganese iron phosphate, preparation method, and secondary battery |
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| CN108172892A (en) * | 2017-11-28 | 2018-06-15 | 清远佳致新材料研究院有限公司 | Multistage continuity method synthesis size distribution is concentrated, the preparation method of multiple types presoma |
| CN108275729A (en) * | 2018-01-23 | 2018-07-13 | 荆门市格林美新材料有限公司 | A kind of system and method preparing cobalt carbonate |
| CN109368709A (en) * | 2018-11-26 | 2019-02-22 | 荆门市格林美新材料有限公司 | A kind of cobalt carbonate, cobaltosic oxide particle size controlling production technology |
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| CN108172892A (en) * | 2017-11-28 | 2018-06-15 | 清远佳致新材料研究院有限公司 | Multistage continuity method synthesis size distribution is concentrated, the preparation method of multiple types presoma |
| CN108275729A (en) * | 2018-01-23 | 2018-07-13 | 荆门市格林美新材料有限公司 | A kind of system and method preparing cobalt carbonate |
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| WO2024011625A1 (en) * | 2022-07-15 | 2024-01-18 | 宁德时代新能源科技股份有限公司 | Continuous reaction system, manganese iron oxalate precursor, lithium manganese iron phosphate, preparation method, and secondary battery |
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Address after: 17-8 Lu Gu Lu Tian Lu, Changsha high tech Development Zone, Changsha City, Hunan Province Applicant after: Hunan Shanshan Energy Technology Co.,Ltd. Address before: 17-8 Lu Gu Lu Tian Lu, Changsha high tech Development Zone, Changsha City, Hunan Province Applicant before: HUNAN SHANSHAN ENERGY TECHNOLOGY Co.,Ltd. Address after: 17-8 Lu Gu Lu Tian Lu, Changsha high tech Development Zone, Changsha City, Hunan Province Applicant after: BASF Shanshan battery material Co.,Ltd. Address before: 17-8 Lu Gu Lu Tian Lu, Changsha high tech Development Zone, Changsha City, Hunan Province Applicant before: Hunan Shanshan Energy Technology Co.,Ltd. |
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Application publication date: 20210928 |