CN109449430A - A kind of system and method for continous way production nickel cobalt manganese presoma - Google Patents
A kind of system and method for continous way production nickel cobalt manganese presoma Download PDFInfo
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- CN109449430A CN109449430A CN201811503195.6A CN201811503195A CN109449430A CN 109449430 A CN109449430 A CN 109449430A CN 201811503195 A CN201811503195 A CN 201811503195A CN 109449430 A CN109449430 A CN 109449430A
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- reaction kettle
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- reaction
- metal salt
- inlet tube
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 190
- 239000007788 liquid Substances 0.000 claims abstract description 53
- 229910052751 metal Inorganic materials 0.000 claims abstract description 44
- 239000002184 metal Substances 0.000 claims abstract description 44
- 239000012266 salt solution Substances 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 34
- 239000002562 thickening agent Substances 0.000 claims abstract description 20
- 239000008139 complexing agent Substances 0.000 claims abstract description 9
- 239000012452 mother liquor Substances 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 18
- 230000032683 aging Effects 0.000 claims description 17
- 238000000975 co-precipitation Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 239000000908 ammonium hydroxide Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- WQABCVAJNWAXTE-UHFFFAOYSA-N dimercaprol Chemical compound OCC(S)CS WQABCVAJNWAXTE-UHFFFAOYSA-N 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 5
- 235000005979 Citrus limon Nutrition 0.000 claims description 5
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000001630 malic acid Substances 0.000 claims description 5
- 235000011090 malic acid Nutrition 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 claims description 3
- 244000248349 Citrus limon Species 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 3
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 3
- 229910015450 Ni1-x-yCoxMny(OH)2 Inorganic materials 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229960001051 dimercaprol Drugs 0.000 claims description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 3
- 229940039790 sodium oxalate Drugs 0.000 claims description 3
- FGGPAWQCCGEWTJ-UHFFFAOYSA-M sodium;2,3-bis(sulfanyl)propane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(S)CS FGGPAWQCCGEWTJ-UHFFFAOYSA-M 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims 1
- 230000007812 deficiency Effects 0.000 abstract description 2
- 239000011572 manganese Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 230000029087 digestion Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000009938 salting Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 244000131522 Citrus pyriformis Species 0.000 description 2
- 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 2
- 238000010923 batch production Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- 208000012826 adjustment disease Diseases 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 210000004262 dental pulp cavity Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 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 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- ZAUUZASCMSWKGX-UHFFFAOYSA-N manganese nickel Chemical compound [Mn].[Ni] ZAUUZASCMSWKGX-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
-
- 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
Abstract
The present invention provides a kind of system and methods of continous way production nickel cobalt manganese presoma.A kind of system of continous way production nickel cobalt manganese presoma, comprising: female reaction kettle, mother's reaction kettle are connected with metal salt solution inlet tube, liquid alkaline inlet tube, complex solution inlet tube, and mother's reaction kettle is additionally provided with discharge port；The thickener or centrifuge being connected to the discharge port of female reaction kettle；The thickener or the centrifuge are parallel with multiple sub- reaction kettles；Each sub- reaction kettle is also connected with metal salt solution inlet tube, liquid alkaline inlet tube, complex solution inlet tube, and each sub- reaction kettle is equipped with overflow port.The present invention solves the problems, such as liquid alkaline existing for traditional mode of production system and complexing agent utilization rate is low and the problem of production stability deficiency.
Description
Technical field
The present invention relates to chemical technology fields, system and side more particularly, to a kind of continous way production nickel cobalt manganese presoma
Method.
Background technique
Lithium ion battery has energy density height, has a safety feature, has extended cycle life as a kind of clean secondary energy sources
The characteristics of, it is widely used in the fields such as electronic product, new-energy automobile, energy storage device.Positive electrode is as lithium ion battery
Important component, performance will have a direct impact on the performance of lithium ion battery.The positive electrode of most application prospect is at present
Nickle cobalt lithium manganate, it is to be made by the presoma and lithium salts of nickel cobalt manganese by calcining.
When producing nickel cobalt manganese presoma, the solid content in reaction kettle is often improved using the method for concentration, after concentration
Presoma return to reaction kettle, mother liquor is then discharged into mother liquor tank, liquid alkaline and complex solution in mother liquor caused not to obtain fully
It recycles.In addition, reaction kettle generally uses a metal salt pipe, a liquid alkaline pipe, three root canal of a complex solution pipe charging, when
When metal salt, liquid alkaline or larger complex solution inlet amount, regional area excessive concentration will cause, influence the stabilization of reaction process
Property.
In view of this, the present invention is specifically proposed.
Summary of the invention
The system that the first object of the present invention is to provide a kind of continous way production nickel cobalt manganese presoma, system solves the problem
The problem of liquid alkaline existing for traditional mode of production system and the low problem and production stability deficiency of complexing agent utilization rate.
The second object of the present invention is to provide a kind of method of continous way production nickel cobalt manganese presoma, and this method can connect
It is continuous to utilize liquid alkaline and complexing agent, the utilization rate of two kinds of raw materials is improved, while realizing the steady production of serialization.
In order to achieve the goal above, the present invention provides following technical schemes:
A kind of system of continous way production nickel cobalt manganese presoma, comprising:
Female reaction kettle, mother's reaction kettle are connected with metal salt solution inlet tube, liquid alkaline inlet tube, complex solution feed liquor
Pipe, mother's reaction kettle are additionally provided with discharge port；
The thickener or centrifuge being connected to the discharge port of female reaction kettle；
The thickener or the centrifuge are parallel with multiple sub- reaction kettles；Each sub- reaction kettle is also connected with metal
Salting liquid inlet tube, liquid alkaline inlet tube, complex solution inlet tube, and each sub- reaction kettle is equipped with overflow port.
As described above, the core of system provided by the present invention is: it is anti-that a female reaction kettle is connected in parallel multiple sons
Kettle is answered, working principle is as follows.
Firstly, by metal salt solution inlet tube, liquid alkaline inlet tube, complex solution inlet tube respectively by metal salt solution,
Liquid alkaline and complex solution are added in female reaction kettle, carry out coprecipitation reaction, obtain slurry.
Then the slurry that female reaction kettle obtains enters thickener or centrifuge by discharge port, by being concentrated or being centrifuged, obtains
Mother liquor (material after concentration can return to female reaction kettle and continue to participate in reaction, the material after centrifugation can continue it is subsequent be centrifuged,
The processing such as dry).
Obtained mother liquor is separately added into the sub- reaction kettle of multiple parallel connections, while metal is added to every sub- reaction kettle respectively
Salting liquid, liquid alkaline and complex solution (being added by the inlet tube being respectively arranged), make to occur respectively altogether in every sub- reaction kettle
Precipitation reaction；The material that every sub- reaction kettle obtains finally is subjected to subsequent processing (including be centrifuged, dry) respectively, is obtained not
Same or identical nickel cobalt manganese presoma.
In summary, system of the invention is mainly realized by female reaction kettle and the mechanical structure of multiple sub- reaction kettle parallel connections
Liquid alkaline and complexing agent are used repeatedly, to improve utilization rate, for certain techniques or certain form of presoma,
Complex solution additional amount in sub- reaction kettle can even be reduced to zero；In addition the inlet tube of sub- reaction kettle is increased from traditional three
If making in kettle that more evenly, reaction process is more stable for feed distribution to four；Third, multiple sub- reaction kettles are in parallel connection, mutually not
Interference, can produce different types of continous way nickel cobalt manganese presoma, and do not restricted by female reaction kettle product type.
System suitable provided by the present invention prepares any type of nickel cobalt manganese presoma.
In the present invention, the connection between centrifuge and sub- reaction kettle can be collected by mother liquor (filtrate being centrifuged)
Pond is realized, i.e., using mother liquor collecting pit as the terminal of mother liquor.
In the above structure basis, system of the invention can be also further improved, specific as follows.
Preferably, connected between the thickener or the centrifuge and each sub- reaction kettle by flow control valve
It is logical.
Control mother liquor by flow control valve and enter the speed of sub- reaction kettle, so control the reaction in sub- reaction kettle into
Journey, the additional amount of convenient constantly adjustment reaction raw materials, to meet actual product demand.
Preferably, the overflow port of all sub- reaction kettles is connected to an ageing tank jointly；
Alternatively, the overflow port of each sub- reaction kettle is respectively communicated with an ageing tank.
The metal salt composition that group reaction kettle is added is identical, and the type of obtained nickel cobalt manganese presoma is identical, then may be used
To share ageing tank, simplify equipment and operation；If the metal salt composition that sub- reaction kettle is added is different, before obtained nickel cobalt manganese
The type for driving body is different, then needs that ageing tank is separately provided.
Preferably, the ageing tank is sequentially connected centrifuge, dryer.
Centrifuge, dryer are set, another centrifugation and drying process are carried out to material, obtains presoma.
Preferably, blender and heater are equipped in female reaction kettle and each sub- reaction kettle.
The condition and process of coprecipitation reaction are adjusted by control blender and heater.
Preferably, each heater is connected with thermostat.
Preferably, the thickener is equipped with concentration material outlet and mother liquor outlet, the mother liquor outlet and multiple sons
Reaction kettle connection；The concentration material outlet is connected to female reaction kettle.
Concentration material returns in female reaction kettle by concentration material outlet, continues to participate in coprecipitation reaction, realizes female reaction
It, can be by the batch production (precipitating of female reaction kettle when the batch production mode of kettle, i.e. sub- reaction kettle in parallel using thickener
Mode) it is connected as one with continous way production (coprecipitation mode of sub- reaction kettle).
The present invention also provides a kind of methods of continous way production nickel cobalt manganese presoma, including the following steps:
Step A: metal salt solution, liquid alkaline and complex solution are added in female reaction kettle, coprecipitation reaction is carried out, is expected
Slurry；
Step B: the slurry is concentrated or is centrifuged, mother liquor is obtained；
The mother liquor: being separately added into the sub- reaction kettle of multiple parallel connections by step C, while respectively to each sub- reaction kettle
Metal salt solution, liquid alkaline and complex solution is added, makes that coprecipitation reaction occurs respectively in each sub- reaction kettle, it respectively will be every
The precipitating that a sub- reaction kettle obtains carries out subsequent processing, obtains similar and different nickel cobalt manganese presoma.
Identical as the working principle of system described above, method of the invention is reacted by liquid alkaline and complex solution in mother
Being used repeatedly between kettle and sub- reaction kettle improves the reaction stability in raw material availability and sub- reaction kettle, also
Increase presoma type.
On this basis, the process conditions of this method and type of feed can also be improved, specific as follows.
Preferably, the gold that the composition for the metal salt solution being added in female reaction kettle is added with each sub- reaction kettle
The composition for belonging to salting liquid is identical or different.
The composition for the metal salt solution being added between female reaction kettle and sub- reaction kettle and each sub- reaction kettle can be identical
Or it is different, to prepare the nickel cobalt manganese presoma of identical or different type.Since female reaction kettle and sub- reaction kettle and each height are anti-
It is independent for answering between kettle, therefore can arbitrarily select the type of metal salt solution.
Preferably, the composition for the metal salt solution that multiple sub- reaction kettles are added is identical or different.
Preferably, it when carrying out the concentration, obtains also obtaining concentration material while mother liquor, the concentration material is returned
Mother's reaction kettle, participates in coprecipitation reaction.
Preferably, the molecular formula of the nickel cobalt manganese presoma is Ni1-x-yCoxMny(OH)2, by molar fraction, 0≤x < 1,
0≤y<1.As x=0, presoma is nickel manganese presoma；As y=0, presoma is nickel cobalt presoma.
Preferably, in female reaction kettle and each sub- reaction kettle coprecipitation reaction condition are as follows: pH is 10~
13.5, reaction temperature is 40~70 DEG C.
Preferably, the liquid alkaline being added in female reaction kettle and each sub- reaction kettle be selected from sodium hydrate aqueous solution and
One or both of aqueous sodium carbonate is with the mixture of any ratio.
Preferably, female reaction kettle and the interior complexing agent being added of each sub- reaction kettle are malic acid, tartaric acid, lemon
Lemon acid, oxalic acid, ammonium hydroxide, disodium ethylene diamine tetraacetate, dimercaprol dimercaptopropanol, sulfosalicylic acid, sodium oxalate, sodium citrate, malic acid
Any one or more in sodium, mercaptoethylmaine and sodium dimercaptopropane sulfonate is with the mixture of any ratio.
Preferably, the solvent of the metal salt solution and the complex solution is separately selected from pure water, ethyl alcohol, ethyl alcohol
Aqueous solution, propyl alcohol and propyl alcohol aqueous solution in any one or a few with the mixture of any ratio.
Preferably, the concentration of the metal salt solution is 0.5~4mol/L, and the concentration of the liquid alkaline is 1~20mol/L.
Preferably, in the step C, the mother liquor is separately added into the flow velocity of the sub- reaction kettle of multiple parallel connections are as follows: 100~
1500L/h。
Preferably, the subsequent processing is followed successively by centrifugation, drying.
To sum up, compared with prior art, invention achieves following technical effects:
(1) utilization rate for improving liquid alkaline and complexing agent, saves cost of material；
(2) the chemical kinetics stability of coprecipitation reaction is improved, is provided to prepare the ternary precursor of high-quality
Prerequisite；
(3) multiple sub- reaction kettles are in parallel connection, do not interfere with each other, can produce different types of continous way nickel cobalt manganese forerunner
Body enriches product type.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the schematic diagram for the system that continous way provided in an embodiment of the present invention produces nickel cobalt manganese presoma；
Fig. 2 is the sub- reaction kettle F of the present invention2Produce 811 presoma scanning electron microscope (SEM) photographs；
Fig. 3 is the sub- reaction kettle F of the present invention3Produce 622 presoma scanning electron microscope (SEM) photographs；
Fig. 4 is the sub- reaction kettle F of the present invention4Produce 523 presoma scanning electron microscope (SEM) photographs；
Appended drawing reference:
Mother's 1- reaction kettle, 2- diaphragm pump, 3- thickener, 4- metering pump, 5- reaction kettle, 6- ageing tank.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with the drawings and specific embodiments, but
Be it will be understood to those of skill in the art that it is following described embodiments are some of the embodiments of the present invention, rather than it is whole
Embodiment is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, ability
Domain those of ordinary skill every other embodiment obtained without making creative work, belongs to guarantor of the present invention
The range of shield.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same
Or production firm person is not specified in instrument, is the conventional products that can be obtained by commercially available purchase.
A kind of system of continous way production nickel cobalt manganese presoma, including female reaction kettle, mother's reaction kettle are connected with metal
Salting liquid inlet tube, liquid alkaline inlet tube, complex solution inlet tube, mother's reaction kettle are equipped with discharge port；
The thickener being connected to the discharge port of female reaction kettle, thickener is equipped with concentration material outlet and mother liquor goes out
Mouthful, the mother liquor outlet is connected to multiple sub- reaction kettles；The concentration material outlet is connected to female reaction kettle.
The mother liquor outlet of the thickener is parallel with multiple sub- reaction kettles；Each sub- reaction kettle is also connected with metal salt
Solution inlet tube, liquid alkaline inlet tube, complex solution inlet tube, each sub- reaction kettle are equipped with overflow port.
The overflow port of each sub- reaction kettle is respectively communicated with an ageing tank.The ageing tank be sequentially connected centrifuge,
Dryer.
Blender and heater are equipped in mother's reaction kettle and each sub- reaction kettle；Each heater connects
It is connected to thermostat.
System above can be used for the production of any type nickel cobalt manganese presoma, and production procedure is as follows.
Firstly, by metal salt solution inlet tube, liquid alkaline inlet tube, complex solution inlet tube respectively by metal salt solution,
Liquid alkaline and complex solution are added in female reaction kettle, carry out coprecipitation reaction, obtain slurry.
Then the slurry that female reaction kettle obtains enters thickener by discharge port, and concentration material and clearly is obtained after concentration
Liquid, concentration material return to female reaction kettle and continue to participate in reaction；Obtained clear liquid is separately added into the sub- reaction kettle of multiple parallel connections, together
When metal salt solution, liquid alkaline and complex solution be added to every sub- reaction kettle respectively (added by the inlet tube being respectively arranged
Enter), make that coprecipitation reaction occurs respectively in every sub- reaction kettle；After the precipitating for finally respectively obtaining every sub- reaction kettle carries out
Continuous processing (including be centrifuged, dry), obtains similar and different nickel cobalt manganese presoma.
For different types of nickel cobalt manganese presoma, the condition reacted using above system is variant.
To prepare Ni1-x-yCoxMny(OH)2Nickel cobalt manganese presoma for, by molar fraction, 0≤x < 1,0≤y < 1,
Suitable reaction condition is as follows.
Preferably, in female reaction kettle and each sub- reaction kettle coprecipitation reaction condition are as follows: pH is 10~
13.5, reaction temperature is 40~70 DEG C；
Preferably, the liquid alkaline being added in female reaction kettle and each sub- reaction kettle be selected from sodium hydrate aqueous solution and
One or both of aqueous sodium carbonate is with the mixture of any ratio；
Preferably, female reaction kettle and the interior complexing agent being added of each sub- reaction kettle are malic acid, tartaric acid, lemon
Lemon acid, oxalic acid, ammonium hydroxide, disodium ethylene diamine tetraacetate, dimercaprol dimercaptopropanol, sulfosalicylic acid, sodium oxalate, sodium citrate, malic acid
Any one or more in sodium, mercaptoethylmaine and sodium dimercaptopropane sulfonate is with the mixture of any ratio；
Preferably, the solvent of the metal salt solution and the complex solution is separately selected from pure water, ethyl alcohol, ethyl alcohol
Aqueous solution, propyl alcohol and propyl alcohol aqueous solution in any one or a few with the mixture of any ratio；
Preferably, the concentration of the metal salt solution is 0.5~4mol/L, and the concentration of the liquid alkaline is 1~20mol/L；
Preferably, the mother liquor is separately added into the flow velocity of the sub- reaction kettle of multiple parallel connections are as follows: 100-1500L/h；
Preferably, the subsequent processing is followed successively by centrifugation, drying.
Compared to traditional production system and technique, each embodiment of the present invention is had at least the following advantages:
1, liquid alkaline and complexing agent utilization rate are high；
2, the presoma type that same production system produces simultaneously is more；
3, stable production process, therefore obtained product quality is high.
Embodiment 1
Three kinds of presomas are prepared using system as shown in Figure 1, which includes female reaction kettle, the 1 (figure of mother's reaction kettle
Middle label is1) there are three feed pipes, respectively metal salt solution A for connection1Feed pipe, liquid alkaline B feed pipe, complex solution C charging
Pipe, there are one discharge nozzles.The discharge nozzle of female reaction kettle 1 is connected to thickener 3 by diaphragm pump 2, and thickener 3 is equipped with concentration material
Outlet and mother liquor outlet, mother liquor outlet passes through three metering pumps 4 respectively and three sub- reaction kettles 5 (are respectively labeled as F in figure2、F3、
F4) connection, concentration material outlet is connected to female reaction kettle 1.In addition three sub- reaction kettles are also respectively equipped with three feed pipes,
Respectively metal salt solution feed pipe, liquid alkaline feed pipe and complex solution feed pipe.Three sub- reaction kettles 5 are also respectively connected old
Change slot 6 and (is respectively labeled as T in figure1、T2、T3)。
The presoma of 811,622 and 523 three types is produced using above system, production procedure is as follows.
By the metal salt solution A of 2mol/L1(Ni:Co:Mn=8:1:1), the liquid alkaline B and ammonium hydroxide C of 5mol/L by 3 into
Expects pipe is pumped into female reaction kettle F respectively1In reacted, control reaction kettle pH be 11, reaction temperature be 55 DEG C.It is dense by thickener
Contracting, concentration material return to female reaction kettle F1, mother liquor M then constantly flows into each sub- reaction kettle F2、F3、F4In.It is controlled and is flowed by metering pump
Enter each sub- reaction kettle F2、F3、F4Flow, namely to 200L/h, 100L/h and 300L/h.
By the metal salt solution A of 2mol/L1(Ni:Co:Mn=8:1:1), the liquid alkaline B of 5mol/L, ammonium hydroxide C and partial mother liquid
M (flow 200L/h) is pumped into sub- reaction kettle F by 4 feed pipes respectively2Middle progress continous way production.Controlling reaction kettle pH is
11, reaction temperature is 55 DEG C, gained presoma overflow to ageing tank T1, digestion time 5h is then centrifuged for, dries, when drying
Between be 10h, obtain 811 continous way presomas, as shown in Figure 2.
By the metal salt solution A of 2mol/L2(Ni:Co:Mn=6:2:2), the liquid alkaline B of 5mol/L, ammonium hydroxide C and partial mother liquid
M (flow 100L/h) is pumped into sub- reaction kettle F by 4 feed pipes respectively3Middle progress continous way production.Controlling reaction kettle pH is
11, reaction temperature is 55 DEG C, gained presoma overflow to ageing tank T2, digestion time 6h is then centrifuged for, dries, when drying
Between be 8h, obtain 622 continous way presomas, as shown in Figure 3.
By the metal salt solution A of 2mol/L3(Ni:Co:Mn=5:2:3), the liquid alkaline B of 5mol/L, ammonium hydroxide C and partial mother liquid
M (flow 300L/h) is pumped into sub- reaction kettle F by 4 feed pipes respectively4Middle progress continous way production.Controlling reaction kettle pH is
11, reaction temperature is 55 DEG C, gained presoma overflow to ageing tank T3, digestion time 4h is then centrifuged for, dries, when drying
Between be 12h, obtain 523 continous way presomas, as shown in Figure 4.
Comparative example
For the comparative example there is no female reaction kettle is arranged, specific production procedure is as follows.
By the metal salt solution A of 2mol/L1(Ni:Co:Mn=8:1:1), the liquid alkaline B and ammonium hydroxide C of 5mol/L by 3 into
Expects pipe is pumped into reaction kettle F respectively2Middle progress continous way production.Controlling reaction kettle pH is 11, and reaction temperature is 55 DEG C, gained forerunner
Body overflow is to ageing tank T1, digestion time 5h is then centrifuged for, dries, and drying time 10h obtains 811 continous way forerunners
Body.
By the metal salt solution A of 2mol/L2(Ni:Co:Mn=6:2:2), the liquid alkaline B and ammonium hydroxide C of 5mol/L by 3 into
Feed pipe is pumped into reaction kettle F respectively3Middle progress continous way production.Controlling reaction kettle pH is 11, and reaction temperature is 55 DEG C, before gained
Body overflow is driven to ageing tank T2, digestion time 6h is then centrifuged for, dries, and drying time 8h obtains 622 continous way forerunners
Body.
By the metal salt solution A of 2mol/L3(Ni:Co:Mn=5:2:3), the liquid alkaline B and ammonium hydroxide C of 5mol/L by 3 into
Feed pipe is pumped into reaction kettle F respectively4Middle progress continous way production.Controlling reaction kettle pH is 11, and reaction temperature is 55 DEG C, before gained
Body overflow is driven to ageing tank T3, digestion time 4h is then centrifuged for, dries, and drying time 12h obtains 523 continous way forerunners
Body.
The results are shown in Table 1 for the production of embodiment 1 and comparative example.
Each index of presoma made from 1 the present embodiment of table and comparative example compares
Data can be seen that from table 1, and continous way production method of the invention can greatly improve ammonium hydroxide utilization rate, reduces it and disappears
Consumption, while production stability also increases.In addition, in the present embodiment only by taking three sub- reaction kettles as an example, it, can in actual production
Increase and decrease sub- reaction kettle quantity as needed, for example, two, four or more.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of system of continous way production nickel cobalt manganese presoma characterized by comprising
Female reaction kettle, mother's reaction kettle are connected with metal salt solution inlet tube, liquid alkaline inlet tube, complex solution inlet tube, institute
It states female reaction kettle and is additionally provided with discharge port；
The thickener or centrifuge being connected to the discharge port of female reaction kettle；
The thickener or the centrifuge are parallel with multiple sub- reaction kettles；It is molten that each sub- reaction kettle is also connected with metal salt
Liquid inlet tube, liquid alkaline inlet tube, complex solution inlet tube, and each sub- reaction kettle is respectively equipped with overflow port.
2. system according to claim 1, which is characterized in that the thickener or the centrifuge and each son are anti-
It answers and is connected between kettle by metering pump.
3. system according to claim 1, which is characterized in that the overflow port of all sub- reaction kettles is connected to one jointly
Ageing tank；
Alternatively, the overflow port of each sub- reaction kettle is respectively communicated with an ageing tank.
4. system according to claim 3, which is characterized in that the ageing tank is sequentially connected another centrifuge, drying
Machine.
5. system according to claim 1, which is characterized in that be all provided in mother's reaction kettle and each sub- reaction kettle
There are blender and heater；
Preferably, each heater is connected with thermostat；
Preferably, the thickener is equipped with concentration material and exports and mother liquor outlet, and the mother liquor outlet described sub is reacted with multiple
Kettle connection；The concentration material outlet is connected to female reaction kettle.
6. a kind of method of continous way production nickel cobalt manganese presoma, characterized in that it comprises the following steps:
Step A: metal salt solution, liquid alkaline and complex solution are added in female reaction kettle, coprecipitation reaction is carried out, obtains slurry；
Step B: the slurry is concentrated or is centrifuged, mother liquor is obtained；
The mother liquor: being separately added into the sub- reaction kettle of multiple parallel connections by step C, while being added respectively to each sub- reaction kettle
Metal salt solution, liquid alkaline and complex solution make that coprecipitation reaction occurs respectively in each sub- reaction kettle, respectively by each institute
It states the precipitating that sub- reaction kettle obtains and carries out subsequent processing, obtain similar and different nickel cobalt manganese presoma.
7. according to the method described in claim 6, it is characterized in that, the composition for the metal salt solution being added in mother's reaction kettle
It is identical or different with the composition of the metal salt solution of each sub- reaction kettle addition；
Preferably, the composition for the metal salt solution that multiple sub- reaction kettles are added is identical or different；
Preferably, it when carrying out the concentration, obtains also obtaining concentration material while mother liquor, it will be described in concentration material return
Female reaction kettle participates in coprecipitation reaction.
8. according to the method described in claim 6, it is characterized in that, the molecular formula of the nickel cobalt manganese presoma is Ni1-x-yCoxMny
(OH)2, by molar fraction, 0≤x < 1,0≤y < 1；
Preferably, in female reaction kettle and each sub- reaction kettle coprecipitation reaction condition are as follows: pH is 10~13.5, instead
Answering temperature is 40~70 DEG C.
9. the method according to claim 6 or 8, which is characterized in that in mother's reaction kettle and each sub- reaction kettle
The liquid alkaline of addition is selected from one or both of sodium hydrate aqueous solution and aqueous sodium carbonate with the mixture of any ratio；
Preferably, female reaction kettle and the interior complexing agent being added of each sub- reaction kettle are malic acid, tartaric acid, lemon
Acid, oxalic acid, ammonium hydroxide, disodium ethylene diamine tetraacetate, dimercaprol dimercaptopropanol, sulfosalicylic acid, sodium oxalate, sodium citrate, natrium malicum,
Any one or more in mercaptoethylmaine and sodium dimercaptopropane sulfonate is with the mixture of any ratio；
Preferably, the solvent of the metal salt solution and the complex solution is separately selected from the water of pure water, ethyl alcohol, ethyl alcohol
Any one or a few in the aqueous solution of solution, propyl alcohol and propyl alcohol is with the mixture of any ratio.
10. according to the method described in claim 9, it is characterized in that, the concentration of the metal salt solution be 0.5~4mol/L,
The concentration of the liquid alkaline is 1~20mol/L；
Preferably, in the step C, the mother liquor is separately added into the flow velocity of the sub- reaction kettle of multiple parallel connections are as follows: 100-
1500L/h；
Preferably, the subsequent processing is followed successively by centrifugation, drying.
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