CN108786708A - A kind of dense bucket control system and the method using the system synthesis ternary precursor - Google Patents
A kind of dense bucket control system and the method using the system synthesis ternary precursor Download PDFInfo
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- CN108786708A CN108786708A CN201810896711.XA CN201810896711A CN108786708A CN 108786708 A CN108786708 A CN 108786708A CN 201810896711 A CN201810896711 A CN 201810896711A CN 108786708 A CN108786708 A CN 108786708A
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- slurry
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- dense bucket
- reaction kettle
- underflow
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000015572 biosynthetic process Effects 0.000 title claims description 16
- 238000003786 synthesis reaction Methods 0.000 title claims description 16
- 239000002243 precursor Substances 0.000 title description 7
- 239000002002 slurry Substances 0.000 claims abstract description 76
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 238000010992 reflux Methods 0.000 claims abstract description 37
- 239000007787 solid Substances 0.000 claims abstract description 35
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000005086 pumping Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 57
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 36
- 239000007789 gas Substances 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 229910021529 ammonia Inorganic materials 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- SEVNKUSLDMZOTL-UHFFFAOYSA-H cobalt(2+);manganese(2+);nickel(2+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mn+2].[Co+2].[Ni+2] SEVNKUSLDMZOTL-UHFFFAOYSA-H 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- 238000012423 maintenance Methods 0.000 claims description 6
- 238000007600 charging Methods 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims 1
- 229940099596 manganese sulfate Drugs 0.000 claims 1
- 239000011702 manganese sulphate Substances 0.000 claims 1
- 235000007079 manganese sulphate Nutrition 0.000 claims 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims 1
- 235000019698 starch Nutrition 0.000 claims 1
- 239000008107 starch Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 5
- 238000010923 batch production Methods 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 4
- 239000010406 cathode material Substances 0.000 abstract description 2
- 230000005484 gravity Effects 0.000 abstract description 2
- 238000004062 sedimentation Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- OVAQODDUFGFVPR-UHFFFAOYSA-N lithium cobalt(2+) dioxido(dioxo)manganese Chemical compound [Li+].[Mn](=O)(=O)([O-])[O-].[Co+2] OVAQODDUFGFVPR-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- BDRTVPCFKSUHCJ-UHFFFAOYSA-N molecular hydrogen;potassium Chemical compound [K].[H][H] BDRTVPCFKSUHCJ-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000010792 warming 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to ternary cathode material of lithium ion battery preparing technical field, more particularly to a kind of method synthesizing nickel-cobalt-manganese ternary presoma using dense bucket control system.The present invention will be in reactor bottom slurry pumping to dense bucket by the pump on feed pipe, there is no stirrings in dense bucket, sedimentation is carried out by gravity and realizes separation of solid and liquid, then underflow is back in reaction kettle and improves solid content, while clear liquid is arranged by going out outside pigging road；Present invention could apply to continuous production upgradings, can be used for Batch Process and propose production upgrading, can be opened in the arbitrary process of production.When the system operation, by improving feed flow rate, the outer parallelism example of clear liquid can be improved, underflow flow velocity can be changed by underflow reflux line valve opening size.The present invention can effectively reduce production cost, reduce operation difficulty, improve safety；The presoma produced through the invention has more excellent physical and chemical index, while sintered positive electrode has better performance.
Description
Technical field
The present invention relates to ternary cathode material of lithium ion battery preparing technical field, more particularly to a kind of dense bucket control of application
The method of system synthesis nickel-cobalt-manganese ternary presoma processed.
Background technology
Currently, the fast development of electric vehicle and hybrid vehicle promotes advancing by leaps and bounds for lithium ion battery technology.
Anode material for lithium-ion batteries at present, if cobalt acid lithium, LiFePO4, LiMn2O4 are all with the low defect of capacity, it is impossible to meet
The requirement of the following Development of Electric Vehicles.And nickle cobalt lithium manganate has many advantages, such as that specific capacity is high, thermal stability is good and cheap, is
Most potential one kind in anode material for lithium-ion batteries has good application prospect in electric automobiles.
Nickel cobalt manganese hydroxide, i.e. nickel-cobalt-manganese ternary presoma synthesize nickel cobalt manganese by the way that lithium source is added by high temperature sintering
Sour lithium.Size, pattern, structure of ternary precursor etc. have a direct impact the technical indicator of nickle cobalt lithium manganate, therefore, presoma
It is most important to the production of ternary material.Currently, preparing the common method crystalline hydroxides in order to control of nickel cobalt manganese hydroxide
Coprecipitation, during precursor synthesis, the solid content of precursor pulp is concentrated mainly on 5~10%, properly increases and contains admittedly
Amount can improve product pattern, improve product tap density, the pattern of product is more regular, and second particle surface is more fine and close；Together
When extend the reaction kettle slurry residence time, presoma nucleus stablizes growth under high pH systems, and crystallinity is improved, more has
Replace from lattice out and reduce the generation of dephasign conducive to impurity, the presoma crystallinity of generation is more preferable, pattern is more regular
Micro mist is reduced, impurity content is substantially reduced, and tap density is promoted, to make sintered positive electrode have higher energy close
Degree.It is using thickener to put forward solid mode mainstream at present, and thickener presence involves great expense, daily operation maintenance cost is larger, occupies
The larger disadvantage in space；Thickener be used as power by high pure nitrogen simultaneously, and liquid is cleared outside through filter stick, there are blocking risk,
There is also security risks for internal high pressure environment.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide one kind capable of effectively reducing production cost, reduces
Operation difficulty improves safety；And the dense bucket control system of continuous production and Batch Process can be applied to simultaneously and applied to be somebody's turn to do
The method of system synthesis ternary precursor.
In order to achieve the above object, the present invention designed by a kind of dense bucket control system, it include it is dense bucket and into
Pipe material, backflow of slurry pipeline, goes out pigging road at underflow reflux line；One end of the feed pipe is arranged in reactor bottom,
The other end leads to dense bucket top；One end of backflow of slurry pipeline is arranged on dense bucket top, and the other end leads to reaction kettle top；
One end of underflow reflux line is arranged in dense bucket bottom, and the other end leads to reaction kettle top and connect with backflow of slurry pipeline；
The one end for going out pigging road is arranged on dense bucket top；On underflow reflux line, it is equipped with diaphragm valve successively from close dense bucket
One, expansion joint one, vibrator, expansion joint two and visor one；On feed pipe, it is equipped with ball valve successively from close reaction kettle
One, expansion joint three, pump, expansion joint four, damper, ball valve two, counterbalance valve, visor two；On going out pigging road, from close to dense bucket
Place is equipped with ball valve three, visor three, electromagnetic flowmeter, spinner flowmeter, diaphragm valve two successively；It is equipped with and regards on backflow of slurry pipeline
Mirror four；It is additionally provided with gas pipeline on dense bucket top, gas pipeline is equipped with shut-off valve；Feed pipe and backflow of slurry pipeline it
Between be equipped with connecting pipe, the connecting pipe be equipped with ball valve, connecting pipe close to feed pipe one end be arranged in expansion joint four
Between damper.
Above-mentioned control system by the pump on feed pipe by reactor bottom slurry pumping to dense bucket, in dense bucket
There is no stirrings, and carrying out sedimentation by gravity realizes separation of solid and liquid, and then underflow is back in reaction kettle and improves solid content, together
When clear liquid by go out outside pigging road arrange.This control system by feed pipe, underflow reflux line, backflow of slurry pipeline, go out it is clear
Pipeline maintains level stability in dense bucket, and the pressure of slurry in dense bucket, clear liquid is kept to stablize relatively；Dense bucket pipe flow speed control
Working method processed is as follows：Row's+V backflow of slurry outside V chargings=V underflow reflux+V clear liquids, it is dense when keeping V backflow of slurry > 0
Level stability in bucket, pipeline pressure are stablized, and can accurately control flow velocity in the precision of desired value ± 5L/h by diaphragm valve, respectively
Mobility status can be observed by corresponding pipeline visor in pipeline.This control system is by increasing external vibrator and expansion simultaneously
Section optimizes underflow reflux line, by the sustained vibration of vibrator, effectively reduces the blocking risk of underflow pipeline；?
Increase counterbalance valve on feed pipe, foreign matter in reaction kettle is effectively intercepted at counterbalance valve, reduces foreign matter to dense bucket operation
It influences, and can be observed by visor above counterbalance valve, find to be cleared up in time when foreign matter accumulation is serious；By diaphragm valve,
Electromagnetic flowmeter stability contorting clear liquid effluent stream amount；Increase backflow of slurry pipeline simultaneously, part size passes through backflow of slurry pipeline
It is back in reaction kettle to stablize liquid level in reaction kettle；Connecting pipe is equipped between feed pipe and backflow of slurry pipeline,
The connecting pipe is equipped with ball valve, when pump feed rate is excessive, can influence the dense dense efficiency of bucket, can be by adjusting the valve
Gate is made a part of slurry and is directly back in reaction kettle；The filling that the gases such as nitrogen or argon gas are carried out above dense bucket is close
Envelope effectively reduces the oxidative phenomena that solid process is put forward in ternary precursor synthesis.
This control system can be applied to continuous production upgrading, can be used for Batch Process and proposes production upgrading, can be in life
It is opened in the arbitrary process of production.When the system operation, by improving feed flow rate, the outer parallelism example of clear liquid can be improved, is led to
Underflow flow velocity can be changed by crossing underflow reflux line valve opening size, and underflow flow velocity, which improves opposite underflow solid content, to drop
Low, underflow flow velocity reduces opposite underflow solid content and can improve, and situation can be controlled as needed.This control system can have
Effect solves the problems such as dense bucket operation stability is poor, safety is poor, uncontrollable.
A kind of method using above-mentioned dense bucket control system synthesis of ternary presoma designed by the present invention, including it is as follows
Specific steps：
(1) according to the dense bucket of reaction kettle spatial choice, pipe fitting is installed, and reduces bend pipe, flat pipe as far as possible；
(2) by the sodium hydroxide of nickel cobalt manganese salt solution, concentration 80-320g/L that concentration of metal ions is 1.0-3.0mol/L
Solution, concentration 8%-30% ammonium hydroxide be added reaction kettle simultaneously, 50-70 DEG C of reaction temperature, rotating speed is controlled in 100-300rpm；Dimension
Hold pH value 10.0-12.0, ammonia density 1.0-20.0g/L, and be continually fed into the gases such as nitrogen or argon gas to slurry in reaction kettle into
Row protection；It promotes pH with slurry solid content raising in reaction kettle and is significantly grown to prevent tablet degree, pH promotes amplitude and exists
0.05-1.5 is increased according to solid content and is increased；
(3) it is extracted in slurry to dense bucket out of reaction kettle by pumping, by underflow being back in reaction kettle after dense,
It will be arranged outside clear liquid, achieve the purpose that improve reaction kettle slurry solid content, and by gases such as nitrogen or argon gas to outer loop
Slurry is protected；By feed pipe, underflow reflux line, backflow of slurry pipeline, go out liquid level in the dense bucket of pigging road maintenance
Stablize, the pressure of slurry in dense bucket, clear liquid is kept to stablize relatively；Dense bucket pipe flow speed control working method is as follows：V is fed
Row's+V backflow of slurry outside=V underflow reflux+V clear liquids；Backflow of slurry, underflow reflux are kept, underflow reflux line diaphragm valve is passed through
Liquid measure is cleared outside control underflow return flow indirect control and reaches required ratio, and is accurately controlled outside by going out pigging road diaphragm valve
Liquid proportional is cleared in 0-80%, reaction kettle slurry solid content and the outer discharge capacity account mode of dense bucket clear liquid are as follows：
(4) the nickel cobalt manganese hydroxide of institute's overflow precipitates after separation of solid and liquid with containing potassium hydroxide or hydroxide after reacting
The solution of sodium configuration washs several hours, then several times with pure water rinsing, wherein being configured containing potassium hydroxide or sodium hydroxide molten
The concentration of liquid is controlled in 0.1-0.5mol/L；
(5) the nickel cobalt manganese hydroxide filter cake after washing is good is done by drying equipments such as disk dryer or rotary kilns
Nickel cobalt manganese presoma that is dry, finally being synthesized.
Nickel cobalt manganese solution can come from nickel chloride, cobalt chloride, manganese chloride, nickel sulfate, cobaltous sulfate, sulphur in the step (2)
The one or several kinds of sour manganese, nickel nitrate, cobalt nitrate, manganese nitrate etc..
The temperature control of the solution and pure water of potassium hydroxide or the sodium hydroxide configuration of washing in the step (4) exists
50-80℃。
Drying temperature is at 120-250 DEG C in the step (5), drying time 2-20h.
The present invention is solid by carrying, and extends the synthesis reactor slurry residence time, and presoma nucleus stablizes life under high pH systems
Long, crystallinity is improved, effectively reduces the generation of dephasign and reduce the impurity in lattice；It can be carried in batch technology
High crystal seed quantity extends reactor feed time promotion output per single reactor；The presoma produced through the invention has more excellent
Physical and chemical index, while sintered positive electrode have better performance.
Description of the drawings
Fig. 1 is the structural schematic diagram of the dense bucket control system of the present invention.
Fig. 2 is the nickel cobalt manganese persursor material pictorial diagram obtained using the method for the present invention Batch Process.
Fig. 3 is the nickel cobalt manganese persursor material pictorial diagram obtained using the method for the present invention continuous production.
Fig. 4 is the model nickel cobalt manganese persursor material pictorial diagram of the same race for not using the method for the present invention to produce.
Fig. 5 is the nickel cobalt manganese persursor material that the method for the present invention is prepared and the model nickel cobalt of the same race for not using this method
The XRD of manganese persursor material is compared.
Fig. 6 is the nickel cobalt manganese persursor material that the method for the present invention is prepared and the model nickel cobalt of the same race for not using this method
The impurity content of manganese persursor material compares.
Specific implementation mode
Present invention work is further illustrated with reference to embodiment, but invention is not limited to specific embodiment.
Embodiment 1：
A kind of dense bucket control system as shown in Figure 1, including it is dense bucket 1 and feed pipe 2, underflow reflux line 3,
Backflow of slurry pipeline 4 goes out pigging road 5；One end of the feed pipe is arranged in reactor bottom, and the other end leads on dense bucket
Portion；One end of backflow of slurry pipeline is arranged on dense bucket top, and the other end leads to reaction kettle top；One end of underflow reflux line
It is arranged in dense bucket bottom, the other end leads to reaction kettle top and connect with the lower end of backflow of slurry pipeline；Go out the one of pigging road
End is arranged on dense bucket top；On underflow reflux line, it is equipped with diaphragm valve 1, expansion joint one successively from close dense bucket
7, vibrator 8, expansion joint 29 and visor 1；On feed pipe, from ball valve 1, swollen is equipped with from the reaction kettle successively
Swollen section 3 12, pump 13, expansion joint 4 14, damper 15, ball valve 2 16, counterbalance valve 17, visor 2 18；On going out pigging road, from
It is equipped with ball valve 3 19, visor 3 20, electromagnetic flowmeter 21, spinner flowmeter 22, diaphragm valve 2 23 successively at dense bucket；?
Backflow of slurry pipeline is equipped with visor 4 24；It is additionally provided with gas pipeline 25 on dense bucket top, gas pipeline is equipped with shut-off valve
26；Between feed pipe and reflux line be equipped with connecting pipe 27, the connecting pipe be equipped with ball valve 28, connecting pipe close into
One end of pipe material is arranged between expansion joint four and damper.
Embodiment 2：
A method of using dense bucket control system synthesis of ternary presoma, including following steps：
(1) in-site installation dense bucket control system, including various pipelines and accessory as described in Example 1；
(2) the nickel cobalt manganese salt solution that configuration concentration of metal ions is 2.0mol/L, configuration concentration of sodium hydroxide solution 200g/
L configures ammonia concn 9.5%；Sodium hydroxide solution, ammonium hydroxide are added into reaction kettle base solution, adjusting ammonia density is 3.5-5.5g/
L, pH value is 10.0-12.0；Reaction kettle, reaction temperature 50- is added simultaneously in nickel cobalt manganese salt solution, sodium hydroxide solution, ammonium hydroxide
70 DEG C, rotating speed is controlled in 100-300rpm, and maintains pH value 10.0-12.0, ammonia density 3.5-5.5g/L；And it is continually fed into nitrogen
Or the gases such as argon gas protect slurry in reaction kettle；PH is promoted to prevent tablet with slurry solid content raising in reaction kettle
Degree is significantly grown, and pH promotes amplitude in 0.05-1.5, is increased and is increased according to solid content；
(3) it is extracted in slurry to dense bucket out of reaction kettle by air driven pump, by the way that underflow is back to reaction after dense
In kettle, it will be arranged outside clear liquid, achieve the purpose that improve reaction kettle slurry solid content, and follow outside by gases such as nitrogen or argon gas
The slurry of ring is protected；By feed pipe, underflow reflux line, backflow of slurry pipeline, go out in the dense bucket of pigging road maintenance
Level stability keeps the pressure of slurry in dense bucket, clear liquid to stablize relatively；Dense bucket pipe flow speed control working method is as follows：V
Row's+V backflow of slurry outside charging=V underflow reflux+V clear liquids；Keep backflow of slurry, underflow reflux, by underflow reflux line every
Liquid measure is cleared outside film valve control underflow return flow indirect control and reaches required ratio, and is accurately controlled by going out pigging road diaphragm valve
The outer liquid proportional that clears of system is 55 ± 3%；Reaction kettle slurry solid content and the outer discharge capacity account mode of dense bucket clear liquid are as follows：
(4) the nickel cobalt manganese hydroxide of institute's overflow precipitates after separation of solid and liquid with containing potassium hydroxide or hydroxide after reacting
The solution of sodium configuration washs several hours, then several times with pure water rinsing, wherein being configured containing potassium hydroxide or sodium hydroxide molten
The concentration of liquid is controlled in 0.3mol/L；
(5) the nickel cobalt manganese hydroxide filter cake after washing is dried by pan dryer, drying temperature is in 120-
250 DEG C, drying time 2-20h is to get to the nickel cobalt manganese persursor material finally synthesized.
Embodiment 3：
A method of using dense bucket control system synthesis of ternary presoma, including following steps：
(1) in-site installation dense bucket control system, including various pipelines and accessory as described in Example 1；
(2) the nickel cobalt manganese salt solution that configuration concentration of metal ions is 2.0mol/L, configuration concentration of sodium hydroxide solution 200g/
L configures ammonia concn 9.5%；Sodium hydroxide solution, ammonium hydroxide are added into reaction kettle base solution, adjusting ammonia density is 8.5-9.5g/
L, pH value is 10.0-12.0；Reaction kettle, reaction temperature 50- is added simultaneously in nickel cobalt manganese salt solution, sodium hydroxide solution, ammonium hydroxide
70 DEG C, rotating speed is controlled in 100-300rpm, and maintains pH value 10.0-12.0, ammonia density 8.5-9.5g/L；And it is continually fed into nitrogen
Or the gases such as argon gas protect slurry in reaction kettle；PH is promoted to prevent tablet with slurry solid content raising in reaction kettle
Degree is significantly grown, and pH promotes amplitude in 0.05-1.5, is increased and is increased according to solid content；
(3) it is extracted in slurry to dense bucket out of reaction kettle by air driven pump, by the way that underflow is back to reaction after dense
In kettle, it will be arranged outside clear liquid, achieve the purpose that improve reaction kettle slurry solid content, and follow outside by gases such as nitrogen or argon gas
The slurry of ring is protected；By feed pipe, underflow reflux line, backflow of slurry pipeline, go out in the dense bucket of pigging road maintenance
Level stability keeps the pressure of slurry in dense bucket, clear liquid to stablize relatively；Dense bucket pipe flow speed control working method is as follows：V
Row's+V backflow of slurry outside charging=V underflow reflux+V clear liquids；Keep backflow of slurry, underflow reflux, by underflow reflux line every
Liquid measure is cleared outside film valve control underflow return flow indirect control and reaches required ratio, and is accurately controlled by going out pigging road diaphragm valve
The outer liquid proportional that clears of system is 40 ± 3%；Reaction kettle slurry solid content and the outer discharge capacity account mode of dense bucket clear liquid are as follows：
(4) the hydroxide hydroxide of institute's overflow precipitates after separation of solid and liquid with containing potassium hydroxide or hydrogen-oxygen after reacting
The solution for changing sodium configuration washs several hours, then several times with pure water rinsing, wherein configured containing potassium hydroxide or sodium hydroxide
The concentration of solution is controlled in 0.4mol/L；
(5) the nickel cobalt manganese hydroxide filter cake after washing is dried by pan dryer, drying temperature is in 120-
250 DEG C, drying time 2-20h is to get to the nickel cobalt manganese persursor material finally synthesized.
Embodiment 4：
A method of using dense bucket control system synthesis of ternary presoma, including following steps：
(1) in-site installation dense bucket control system, including various pipelines and accessory as described in Example 1；
(2) the nickel cobalt manganese salt solution that configuration concentration of metal ions is 2.0mol/L, configuration concentration of sodium hydroxide solution 200g/
L configures ammonia concn 9.5%；Deionized water is added into sealing reaction kettle, speed of agitator 220rpm is warming up to 70 DEG C, leads to nitrogen
Gas shields such as gas or argon gas 2 hours or more, sodium hydroxide solution, ammonium hydroxide are added into bottom liquid, and adjustings ammonia density is 12.0-
13.0g/L, pH value 10.0-12.0；Reaction kettle is added simultaneously in nickel cobalt manganese salt solution, sodium hydroxide solution, ammonium hydroxide, and is maintained
PH value 10.0-12.0, ammonia density 12.0-13.0g/L；PH is promoted to prevent tablet degree with slurry solid content raising in reaction kettle
It significantly grows, pH promotes amplitude in 0.05-1.5, is increased and is increased according to solid content；
(3) it is extracted in slurry to dense bucket out of reaction kettle by air driven pump, by the way that underflow is back to reaction after dense
In kettle, it will be arranged outside clear liquid, achieve the purpose that improve reaction kettle slurry solid content, and follow outside by gases such as nitrogen or argon gas
The slurry of ring is protected；By feed pipe, underflow reflux line, backflow of slurry pipeline, go out in the dense bucket of pigging road maintenance
Level stability keeps the pressure of slurry in dense bucket, clear liquid to stablize relatively；Dense bucket pipe flow speed control working method is as follows：V
Row's+V backflow of slurry outside charging=V underflow reflux+V clear liquids；Keep backflow of slurry, underflow reflux, by underflow reflux line every
Liquid measure is cleared outside film valve control underflow return flow indirect control and reaches required ratio, and is accurately controlled by going out pigging road diaphragm valve
The outer liquid proportional that clears of system is 80 ± 3%；Reaction kettle slurry solid content and the outer discharge capacity account mode of dense bucket clear liquid are as follows：
(4) the hydroxide hydroxide of institute's overflow precipitates after separation of solid and liquid with containing potassium hydroxide or hydrogen-oxygen after reacting
The solution for changing sodium configuration washs several hours, then several times with pure water rinsing, wherein configured containing potassium hydroxide or sodium hydroxide
The concentration of solution is controlled in 0.2mol/L；
(5) the nickel cobalt manganese hydroxide filter cake after washing is dried by 220 DEG C of rotary kiln to get to final synthesis
Nickel cobalt manganese persursor material.
Claims (5)
1. a kind of dense bucket control system, it is characterised in that：Including dense bucket and feed pipe, underflow reflux line, slurry
Reflux line goes out pigging road；One end of the feed pipe is arranged in reactor bottom, and the other end leads to dense bucket top；Slurry
Expect that one end of reflux line is arranged on dense bucket top, the other end leads to reaction kettle top；One end of underflow reflux line is arranged
In dense bucket bottom, the other end leads to reaction kettle top and is connect with the lower end of backflow of slurry pipeline；The one end for going out pigging road is set
It sets on dense bucket top；On underflow reflux line, it is equipped with diaphragm valve one, expansion joint one, vibration successively from close dense bucket
Device, expansion joint two and visor one；On feed pipe, from ball valve one, expansion joint three, pump, swollen is equipped with from the reaction kettle successively
Swollen section four, damper, ball valve two, counterbalance valve, visor two；On going out pigging road, from be equipped with successively from the dense bucket ball valve three,
Visor three, electromagnetic flowmeter, spinner flowmeter, diaphragm valve two；Visor four is equipped on backflow of slurry pipeline；On dense bucket top
It is additionally provided with gas pipeline, gas pipeline is equipped with shut-off valve；Connecting pipe is equipped between feed pipe and backflow of slurry pipeline, it should
Connecting pipe is equipped with ball valve, and connecting pipe is arranged close to one end of feed pipe between expansion joint four and damper.
2. a kind of method using dense bucket control system synthesis of ternary presoma described in claim 1, it is characterised in that：Including
Following specific steps：
(1) according to the dense bucket of reaction kettle spatial choice, pipe fitting is installed, and reduces bend pipe, flat pipe as far as possible；
(2) concentration of metal ions is molten for nickel cobalt manganese salt solution, the sodium hydroxide of concentration 80-320g/L of 1.0-3.0mol/L
Liquid, concentration 8%-30% ammonium hydroxide be added reaction kettle simultaneously, 50-70 DEG C of reaction temperature, rotating speed is controlled in 100-300rpm；It maintains
PH value 10.0-12.0, ammonia density 1.0-20.0g/L, and be continually fed into the gases such as nitrogen or argon gas and slurry in reaction kettle is carried out
Protection；It promotes pH with slurry solid content raising in reaction kettle and is significantly grown to prevent tablet degree, pH promotes amplitude in 0.05-
1.5, it is increased and is increased according to solid content；
(3) it is extracted in slurry to dense bucket out of reaction kettle by pumping, it, will be clear by underflow being back in reaction kettle after dense
It is arranged outside liquid, achievees the purpose that improve reaction kettle slurry solid content, and by gases such as nitrogen or argon gas to the slurry of outer loop
It is protected；By feed pipe, underflow reflux line, backflow of slurry pipeline, go out level stability in the dense bucket of pigging road maintenance,
The pressure of slurry in dense bucket, clear liquid is kept to stablize relatively；Dense bucket pipe flow speed control working method is as follows：V chargings=V is dense
Starch row's+V backflow of slurry outside reflux+V clear liquids；Backflow of slurry, underflow reflux are kept, is controlled by underflow reflux line diaphragm valve dense
Liquid measure is cleared outside slurry return flow indirect control and reaches required ratio, and is accurately controlled by going out pigging road diaphragm valve and outer cleared liquid
For ratio in 0-80%, reaction kettle slurry solid content and the outer discharge capacity account mode of dense bucket clear liquid are as follows：
(4) the nickel cobalt manganese hydroxide of institute's overflow, which is precipitated, after reacting is matched after separation of solid and liquid with containing potassium hydroxide or sodium hydroxide
The solution set washs several hours, then several times with pure water rinsing, wherein the solution containing potassium hydroxide or sodium hydroxide configuration
Concentration is controlled in 0.1-0.5mol/L；
(5) the nickel cobalt manganese hydroxide filter cake after washing is good is dried by drying equipments such as disk dryer or rotary kilns,
The nickel cobalt manganese presoma finally synthesized.
3. a kind of method using dense bucket control system synthesis of ternary presoma according to claim 2, feature exist
In：In the step (2) nickel cobalt manganese solution can come from nickel chloride, cobalt chloride, manganese chloride, nickel sulfate, cobaltous sulfate, manganese sulfate,
The one or several kinds of nickel nitrate, cobalt nitrate, manganese nitrate etc..
4. a kind of method using dense bucket control system synthesis of ternary presoma according to claim 2, feature exist
In：The solution of potassium hydroxide or sodium hydroxide configuration and the temperature of pure water of washing in the step (4) are controlled in 50-80
℃。
5. a kind of method using dense bucket control system synthesis of ternary presoma according to claim 2, feature exist
In：Drying temperature is at 120-250 DEG C in the step (5), drying time 2-20h.
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| CN111921267A (en) * | 2020-07-23 | 2020-11-13 | 华友新能源科技（衢州）有限公司 | Method for stably separating mother liquor in precursor synthesis |
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