CN109860542A - A kind of preparation method of lithium ion anode material presoma - Google Patents
A kind of preparation method of lithium ion anode material presoma Download PDFInfo
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- CN109860542A CN109860542A CN201811587149.9A CN201811587149A CN109860542A CN 109860542 A CN109860542 A CN 109860542A CN 201811587149 A CN201811587149 A CN 201811587149A CN 109860542 A CN109860542 A CN 109860542A
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- nickel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The present invention relates to a kind of preparation methods of lithium ion anode material presoma, its chemical formula is NixCoyMn1-x-y (OH) 2 or NixCoyAl1-x-y (OH) 2,0.18 < x < 0.99,0 < y < 0.8, the present invention has uniform clad, it reduces material to react with electrolyte, so that material circulation and high rate performance be made to have a distinct increment, high temperature storage is obviously improved;The present invention can more preferably control in material Li dissolution rate in water by using mixed solvent and Li solution control whole system pH, can be with rock-steady structure, so that material property be made to have clear improvement.
Description
Technical field
The invention belongs to technical field of new energy material preparation, in particular to prepared by precursor of lithium ionic cell positive material
Method.
Background technique
It further decreases as lithium ion battery energy density is further increased with cost, is led in electric car and energy storage
Domain is widely used, and lithium ion battery self discharge has very the life and reliability of electric car and energy-storage system
Important influence,
And this market also proposed higher performance requirement to new energy industry, specific energy, high-temperature behavior, the service life, from
Electric discharge etc., research has shown that, the quantity for reducing the micro powder granule in lithium ion anode material can effectively improve self discharge
Can, the presence of micro mist affects the self discharge of battery in terms of two two, that is, increases side reaction and the micro-short circuit of inside battery,
And increasing with micro mist, it influences more serious, in addition, the presence of micro mist can deteriorate the high-temperature storage performance of battery, makes battery
Capacity attenuation during storage, internal resistance increase, and phenomena such as along with flatulence, therefore, in actual production, need strict control
The distribution of particles of material avoids Dmin too small.
So being that each anode material for lithium-ion batteries factory needs the work being rigid in checking up in the production process to the control of micro mist
Sequence, the content of micro mist directly determine the storage life of battery, and more seriously the presence of micro mist is likely to cause the interior of battery
Portion's short circuit, causes battery to generate heat in charge and discharge process, is finally likely to result in the explosion of battery, therefore, studies micro mist to electricity
The influence of pond performance has certain practical significance.
Want to improve this status, it is necessary to solve the problems, such as in presoma micro powder granule during the reaction, as its name suggests,
Micro mist is that in the reaction system, not exclusively the residence time is inadequate in reaction kettle in other words for reaction, causes partial size small, the present invention
Using a filter device, the particle that overflow goes out will be reacted and be classified, after micro powder granule is filtered, be back to reaction kettle again
In, the reaction was continued, and the particle of fully reacting is flowed out along filter device, into subsequent processing.Its is easy to operate, the degree of automation
Height, control are accurate.And the production that can work continuously, while improving micro powder granule, and maintain the original compacted density of product.
Summary of the invention
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of anode material for lithium ion battery,
With uniform clad, reduces material and reacted with electrolyte, so that material circulation and high rate performance is made to have a distinct increment, high temperature
Storage is obviously improved.
The second object of the present invention is to provide a kind of anode material for lithium ion battery preparation method, by using mixing
Solvent and Li solution control whole system pH can more preferably control in material Li dissolution rate in water, can with rock-steady structure, from
And material property is made to have clear improvement.
In order to achieve the above object, the present invention has following technical scheme:
A kind of preparation method of lithium ion anode material presoma of the invention, chemical formula NixCoyMn1-x-y(OH)2
Or NixCoyAl1-x-y(OH)2, 0.18 < x < 0.99,0 < y < 0.8, this method comprises the following steps that:
It A, is the solution of 0.49~3mol/L, element in solution by nickel salt, cobalt salt, manganese salt or aluminium salt preparation solution, concentration
It can be nickel cobalt, nickel manganese, nickel cobalt manganese, any one in nickel cobalt aluminium;
B, compound concentration is the aqueous slkali of 1.4~10mol/L;
C, compound concentration is the enveloping agent solution of 2~12mol/L;
D, with metering pump or constant flow pump by above-mentioned solution A, B, C are entered in reaction kettle 4 by pipeline 1, pipeline 2, pipeline 3,
It controls flow and is passed through protective gas, mixing speed 80- in 10.0-14.0 in 0.01-900L/h, 35-80 DEG C of temperature, reaction pH
800r/min, after reacting in a kettle, the material pump that overflow goes out is squeezed into filter device 5, and the aperture of filter core is in 2-
5um, micro powder granule will pass through filter core 7 with liquid, and bulky grain can flow into surge tank 9 along the pipeline 8 inside filter core, stream
Little particle solution out, as pipeline 6 is back in reaction kettle, the reaction was continued;So circulation, is able to achieve continuous production, buffers
The product of tank can enter subsequent processing;
E, reaction terminates, and will be separated by solid-liquid separation, and is washed with deionized and is separated by solid-liquid separation resulting positive electrode material precursor, finally
It is dried, that is, lithium ion battery presoma of the present invention is prepared.
Wherein, resulting presoma is spherical nickel cobalt manganese hydroxide or spherical nickel-cobalt aluminium hydroxide.
Wherein, in the step A, nickel salt is any one in nickel sulfate, nickel chloride, nickelous carbonate, nickel acetate or nickel nitrate
Kind or any two or more composition;The cobalt salt is appointing in cobaltous sulfate, cobalt chloride, cobalt carbonate, cobalt acetate or cobalt nitrate
It anticipates a kind of or any two or more composition;The manganese salt is in manganese sulfate, manganese chloride, manganese acetate, manganese carbonate or manganese nitrate
Any one or any two or more compositions;The aluminium salt is aluminium chloride, aluminum sulfate, aluminum acetate, aluminum nitrate, aluminium carbonate
Or any one or any two or more compositions in sodium metaaluminate.
Wherein, in the step B, aqueous slkali is any one in sodium hydroxide, potassium hydroxide and lithium hydroxide or appoints
It anticipates two or more compositions;
Wherein, in the step C, complexing agent is ammonium hydroxide, ammonium hydrogencarbonate, citric acid, ammonium carbonate, ethylenediamine and ethylenediamine tetraacetic
Any one or any two or more compositions in two acid disodiums;
Wherein, in the step D, the filter core aperture of the filter is 0.001-5um, between.
Wherein, in the step E, 4 overflow of reaction kettle goes out material, is squeezed into filtering dress device by the pressure of pump, will
Gradation, bulky grain flow out inside the filter core, less than filter core aperture micro powder granule follow liquid in a form of slurry with
Across filter core outer wall, into filtering container in, then with pump by its have micro powder granule backflow of slurry into reaction kettle, after
Continuous reaction, wherein the material for filtering the core is PP, PE, or ceramics, after bulky grain flows out inside filter core, into subsequent processing
In, by the method, micro powder granule secondary response again can be allowed, continuous production is realized, obtain the narrow presoma of particle diameter distribution.
Wherein, nickel salt is preferably sulfuric acid nickel;Cobalt salt is preferably sulfuric acid cobalt;Manganese salt is preferably sulfuric acid manganese;Aluminium salt is preferably partially
Sodium aluminate.
Beneficial effect
The present invention has the advantages that the micro powder granule generated in reaction was carried out in a form of slurry using filter device
Filter classification, by the micro mist backflow of slurry isolated, into reaction kettle, the reaction was continued, easy to operate, high degree of automation, control essence
It is quasi-.And the production that can work continuously, while improving micro powder granule, and maintain the original compacted density of product.
Detailed description of the invention
Attached drawing 1: the process flow diagram of the prior art;
Attached drawing 2: the present invention removes little particle process flow diagram;
Attached drawing 3: the SEM figure that 1 equipment of the embodiment of the present invention obtains;
Attached drawing 4: the embodiment of the present invention 2 removes the SEM figure after little particle;
Attached drawing 5: the embodiment of the present invention 3 removes the SEM figure after little particle.
In figure, 1-1, pipeline 1-1;1-2, pipeline 1-2;1-3, pipeline 1-3;1-4, reaction kettle;1-5, pipeline 1-5;1-6,
Surge tank;1, pipeline 1;2, pipeline 2;3, pipeline 3;4, reaction kettle 4;5, filter;6, pipeline 6;7, filtration core 7;8, pipeline 8;
9, surge tank.
Specific embodiment
For a further understanding of the present invention, the present invention is made below in conjunction with specification and specific preferred embodiment further
Description, but protection scope not thereby limiting the invention.
Embodiment 1
By nickel nitrate, cobalt nitrate, manganese nitrate in molar ratio be respectively Ni:Co:Mn=0.60:0.10:0.30 ratio match
Solution A processed, concentration 2.3mol/L prepare the potassium hydroxide solution B of 4.2mol/L, and compound concentration is that the ammonium hydroxide of 5.0mol/L is molten
Liquid C, with metering pump by tri- kinds of solution of A, B, C respectively with the flow of 700L/h, 350L/h, 90L/h along process pipeline 1, pipe
Road 2, pipeline 3 enter in process reaction kettle 4, and under the conditions of nitrogen protection, gas flow 25m3/h controls anti-temperature of reaction kettle
It is 50 DEG C, pH value 12.3, speed of agitator 200r/min, after starting reaction, the overflow from reaction kettle relies on liquid along pipeline 5
Potential difference is flowed to naturally in the surge tank 6 of process, successive reaction, and the material of surge tank 6 is separated by solid-liquid separation;It is washed with deionized
It is separated by solid-liquid separation resulting presoma, finally in 110 DEG C of drying.Gained presoma is represented by Ni0.60Co0.10Mn0.30
(OH)2.(the present embodiment can be explained by attached drawing 1) in D50:10.0um, Dmin 0.198um
Embodiment 2
By nickel sulfate, cobaltous sulfate, manganese sulfate in molar ratio be respectively Ni:Co:Mn=0.85:0.05:0.10 ratio match
Solution A processed, concentration 2.0mol/L prepare the sodium hydroxide solution B of 6.5mol/L, and compound concentration is the ammonium hydroxide of 10.0mol/L
Solution C, with metering pump by tri- kinds of solution of A, B, C respectively with the flow of 60L/h, 32L/h, 5L/h, along process pipeline 1, pipeline
2, pipeline 3 enters in the reaction kettle 4 of process, and under the conditions of nitrogen protection, gas flow 3m3/h controls anti-temperature of reaction kettle
It is 60 DEG C, pH value 13.0, speed of agitator 300r/min starts after reacting 4h, is got with pump from reaction kettle, into the mistake of process
Device 5 is filtered, 7 aperture of filter core uses 3um, pressure 4kg, and bulky grain flows into the buffering of process with the pipeline 8 of process inside filter core
In tank 9, by entering in filtering container 5 outside filter core 7, the pump of pipeline 6 along process returns work for little particle and a part of liquid
In the reaction kettle 4 of sequence, the reaction was continued, continuous production;The material of surge tank 9 is separated by solid-liquid separation;Solid-liquid is washed with deionized
Separating obtained presoma, finally in 110 DEG C of drying;Gained presoma is represented by Ni0.85Co0.05Mn0.10 (OH) 2.
D50:8.0um, Dmin 3.05um/ obtain product and see attached drawing 3 (the present embodiment can be explained by 2 equipment of attached drawing)
Embodiment 3
By nickel nitrate, cobalt acetate, aluminum sulfate in molar ratio be respectively Ni:Co:Al=0.89:0.03:0.08 ratio match
Solution A processed, concentration 1.5mol/L prepare the sodium hydroxide solution B of 4mol/L, and compound concentration is the ammonia spirit of 8.0mol/L
C is entered tri- kinds of solution of A, B, C in reaction kettle 4 with metering pump with the flow of 150L/h, 70L/h, 4L/h respectively, is protected in nitrogen
Under the conditions of shield, gas flow 2m3/h, controlling anti-temperature of reaction kettle is 70 DEG C, pH value 12.6, speed of agitator 180r/min,
Start after reacting 6h, got with pump from reaction kettle, into the filter device 5 of process, 7 aperture of filter core uses 5um, pressure 6kg, greatly
Particle flows into the surge tank 9 of process with the pipeline 8 of process inside filter core, and little particle and liquid outside filter core 7 by entering
Filter container in, along process pipeline 6 with pump return process reaction kettle 4 in the reaction was continued, continuous production;The object of surge tank 9
Material is separated by solid-liquid separation;It is washed with deionized and is separated by solid-liquid separation resulting presoma, finally in 110 DEG C of drying;Gained forerunner
Body is represented by Ni0.89Co0.03Al0.08 (OH) 2.D50:15.0um, Dmin4.95um are (interpretable originally by 2 equipment of attached drawing
Embodiment).
The Applicant declares that the present invention is explained by the above embodiments, the present invention is made is further described, cannot
Assert that specific implementation of the invention is only limited to these instructions.It should be bright for those skilled in the art
, under the early periods for not departing from present inventive concept, several simple deductions or substitution are made to the present invention, all fall within guarantor of the invention
It protects within range and the open scope.
Claims (8)
1. a kind of preparation method of lithium ion anode material presoma, chemical formula NixCoyMn1-x-y(OH)2Or
NixCoyAl1-x-y(OH)2, 0.18 < x < 0.99,0 < y < 0.8, it is characterised in that: this method comprises the following steps that:
A, by the solution that nickel salt, cobalt salt, manganese salt or aluminium salt prepare solution, concentration is 0.49~3mol/L, element can be in solution
It is nickel cobalt, nickel manganese, nickel cobalt manganese, any one in nickel cobalt aluminium;
B, compound concentration is the aqueous slkali of 1.4~10mol/L;
C, compound concentration is the enveloping agent solution of 2~12mol/L;
D, with metering pump or constant flow pump by above-mentioned solution A, B, C are entered in reaction kettle 4 by pipeline 1, pipeline 2, pipeline 3, control
Flow is passed through protective gas, mixing speed 80-800r/ in 10.0-14.0 in 0.01-900L/h, 35-80 DEG C of temperature, reaction pH
Min, after reacting in a kettle, the material that overflow goes out, which pumps, to be squeezed into filter device 5, and the aperture of filter core is micro- in 2-5um
Powder particles will with liquid pass through filter core 7, bulky grain can along the pipeline 8 inside filter core, flow into surge tank 9 in, outflow it is small
Particle solution, as pipeline 6 is back in reaction kettle, the reaction was continued;So circulation, is able to achieve continuous production, the production of surge tank
Product can enter subsequent processing;
E, reaction terminates, and will be separated by solid-liquid separation, and is washed with deionized and is separated by solid-liquid separation resulting positive electrode material precursor, finally carries out
It is dried, that is, lithium ion battery presoma of the present invention is prepared.
2. a kind of lithium ion battery precursor preparation method according to claim 1, it is characterised in that: resulting presoma
For spherical nickel cobalt manganese hydroxide or spherical nickel-cobalt aluminium hydroxide.
3. a kind of lithium ion battery precursor preparation method according to claim 1, it is characterised in that: in the step A,
Nickel salt is any one or any two or more compositions in nickel sulfate, nickel chloride, nickelous carbonate, nickel acetate or nickel nitrate;
The cobalt salt is any one or any two or more combinations in cobaltous sulfate, cobalt chloride, cobalt carbonate, cobalt acetate or cobalt nitrate
Object;The manganese salt is any one or any two or more in manganese sulfate, manganese chloride, manganese acetate, manganese carbonate or manganese nitrate
Composition;The aluminium salt is any one in aluminium chloride, aluminum sulfate, aluminum acetate, aluminum nitrate, aluminium carbonate or sodium metaaluminate or appoints
It anticipates two or more compositions.
4. a kind of lithium ion battery precursor preparation method according to claim 1, it is characterised in that: in the step B,
Aqueous slkali is any one or any two or more compositions in sodium hydroxide, potassium hydroxide and lithium hydroxide;
5. a kind of lithium ion battery precursor preparation method according to claim 1, it is characterised in that: in the step C,
Complexing agent be ammonium hydroxide, ammonium hydrogencarbonate, citric acid, in two acid disodium of ammonium carbonate, ethylenediamine and ethylenediamine tetraacetic any one or
Any two or more composition;
6. a kind of lithium ion battery precursor preparation method according to claim 1, it is characterised in that: in the step D,
The filter core aperture of the filter is 0.001-5um, between.
7. a kind of lithium ion battery precursor preparation method according to claim 1, it is characterised in that: in the step E,
4 overflow of reaction kettle goes out material, is squeezed into filtering dress device by the pressure of pump, by gradation, bulky grain is in filter core
Portion's outflow, the micro powder granule less than filter core aperture follows liquid in a form of slurry with the outer wall for passing through filter core, into filtering
In container, then with pumping by its backflow of slurry with micro powder granule into reaction kettle, the reaction was continued, wherein filtering the material of the core
For PP, PE, or ceramics, after bulky grain flows out inside filter core, into subsequent processing, by the method, micro powder granule can be allowed
Secondary response again realizes continuous production, obtains the narrow presoma of particle diameter distribution.
8. a kind of lithium ion battery precursor preparation method according to claim 1, it is characterised in that: nickel salt is preferred sulphur
Sour nickel;Cobalt salt is preferably sulfuric acid cobalt;Manganese salt is preferably sulfuric acid manganese;Aluminium salt is preferred sodium metaaluminate.
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Cited By (2)
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CN111036161A (en) * | 2019-12-27 | 2020-04-21 | 中冶瑞木新能源科技有限公司 | System and method for preparing ternary precursor with narrow particle size distribution |
CN112191212A (en) * | 2020-12-02 | 2021-01-08 | 河南科隆新能源股份有限公司 | Reaction kettle and method for preparing precursor of lithium ion battery anode material |
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