CN107611423A - A kind of preparation method of nickel-cobalt-manganese ternary presoma - Google Patents
A kind of preparation method of nickel-cobalt-manganese ternary presoma Download PDFInfo
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- CN107611423A CN107611423A CN201710751638.2A CN201710751638A CN107611423A CN 107611423 A CN107611423 A CN 107611423A CN 201710751638 A CN201710751638 A CN 201710751638A CN 107611423 A CN107611423 A CN 107611423A
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- nickel
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- ternary presoma
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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
Abstract
A kind of preparation method of nickel-cobalt-manganese ternary presoma disclosed by the invention, comprises the following steps：1) mixed slurry, is prepared in the co-precipitation of nickel cobalt manganese mixed liquor, alkali lye and complexing agent；2), the mixed slurry is washed and adjusts viscosity and solid content is to suitable parameters；3) mixed slurry, is subjected to mist projection granulating, obtains granule materials；4), the granule materials are dried, obtain nickel-cobalt-manganese ternary presoma, the atomic ratio of the nickel-cobalt-manganese ternary presoma is NixCoyMnz(OH)2, wherein the ＜ z ＜ 0.30 of 0.50≤x ＜, 1.00,0 ＜ y ＜ 0.20,0.The quality for the nickel-cobalt-manganese ternary persursor material that preparation method provided by the invention obtains is higher, and preparation technology is simple.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, more particularly to a kind of system of nickel-cobalt-manganese ternary presoma
Preparation Method.
Background technology
With the continuous lifting of electrokinetic cell energy density requirement, tertiary cathode material（NCM）It is increasingly becoming mainstream applications.
Current domestic tertiary cathode material enterprise technology still has gap with external, mainly based on NCM111,523 and 622, only works as liter
Science and technology, Bei Terui minorities enterprise have grasped NCM811 and NCA production technologies, start small lot production.Domestic tertiary cathode material
Still in feudal lords vyiying for the throne the stage, leading enterprise is not yet molded for enterprise.Forerunner of the nickel cobalt manganese hydroxide as tertiary cathode material
Body, vital effect is played during prepared by tertiary cathode material.
The main method for preparing precursor of nickel-cobalt-lithium-manganese-oxide in the prior art is：The first step matches somebody with somebody nickel cobalt manganese mixed liquor
System, obtained feed liquid and the co-precipitation of precipitating reagent and complexing agent are crystallized；Second step washed to slurry, dried, mixed,
The processes such as sieving, iron removaling prepare nickel cobalt manganese unit or polynary hydroxide precursor.Its process chart is as shown in figure 1, Fig. 1 is
The existing process chart for preparing nickel cobalt manganese hydroxide.
The preparation method for the nickel cobalt manganese hydroxide that prior art provides, the reaction controlling process when preparing small-particulate materials
It is not sufficiently stable, easily causes the unstable of quality, improve cost.
The content of the invention
In view of the shortcomings of the prior art and defect, the present invention provide a kind of preparation method of nickel-cobalt-manganese ternary presoma, this
The quality for the nickel-cobalt-manganese ternary persursor material that the preparation method that invention provides obtains is higher, and preparation technology is simple.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of nickel-cobalt-manganese ternary presoma, the preparation method comprise the following steps,
（1）Nickel cobalt manganese mixed liquor, alkali lye and the complexing agent co-precipitation that molar concentration is 1.5mol/L~1.8mol/L are prepared into
To mixed slurry, the mol ratio of nickel, cobalt and manganese is (0.5~1) in the nickel cobalt manganese mixed liquor：a：B, 0 ＜ a ＜ 0.20,0 ＜ b
＜ 0.30；Mixing speed in coprecipitation process is 800r/min~1100r/min；PH value in coprecipitation process for 11~
13；The temperature of co-precipitation is 40 DEG C~70 DEG C, and the atomic ratio of the nickel-cobalt-manganese ternary presoma is NixCoyMnz(OH)2, wherein
The ＜ z ＜ 0.30 of 0.50≤x ＜, 1.00,0 ＜ y ＜ 0.20,0；
（2）The mixed slurry is washed and adjusts viscosity and solid content is to suitable parameters, solid content is 20%~50%, viscosity
For 0cp~500cp；
（3）The mixed slurry is subjected to mist projection granulating, obtains granule materials, the atomisation pressure of the mist projection granulating is 0.1MPa
~0.5MPa；The tower chamber temperature of the mist projection granulating is 300 DEG C~500 DEG C.
（4）The granule materials are dried, obtain nickel-cobalt-manganese ternary presoma, the atom of the nickel-cobalt-manganese ternary presoma
Than for NixCoyMnz(OH)2, wherein the ＜ z ＜ 0.30 of 0.50≤x ＜, 1.00,0 ＜ y ＜ 0.20,0.
Further, step（1）The alkali lye is sodium hydroxide solution, content 5mol/L；.
Further, step（1）Described complexing agent is sodium citrate, content 1.25g/L.
Further, step（1）Described in coprecipitation process in pH value be 11~12.
Further, step（1）Described in mixing speed in coprecipitation process be 1000r/min.
Further, step（1）Described in the temperature that is co-precipitated be 45 DEG C~50 DEG C.
Further, rate-determining steps（1）Atmosphere in coprecipitation process is nitrogen atmosphere or inert gas atmosphere.
Preferably, rate-determining steps（1）Atmosphere in coprecipitation process is nitrogen atmosphere.
Further, step（2）Described in solid content be 20%~30%.
Further, step（3）Described in the atomisation pressure of mist projection granulating be 0.3MPa；The tower chamber temperature of the mist projection granulating
Spend for 300 DEG C.
Compared with prior art, beneficial effects of the present invention are：Test result indicates that method provided by the invention is prepared into
The tap density of the nickel-cobalt-manganese ternary presoma arrived is 1.50g/cm3~1.90g/cm3。
Brief description of the drawings
Fig. 1 is the process chart of existing preparation nickel cobalt manganese hydroxide；
Fig. 2 is the process chart of nickel cobalt manganese hydroxide preparation method provided in an embodiment of the present invention；
Fig. 3 is 3000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 1 is prepared；
Fig. 4 is 5000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 1 is prepared；
Fig. 5 is 3000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 2 is prepared；
Fig. 6 is 5000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 2 is prepared；
Fig. 7 is 5000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 3 is prepared；
Fig. 8 is 10000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 3 is prepared.
Embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.
A kind of preparation method of nickel-cobalt-manganese ternary presoma, the preparation method comprise the following steps,
（1）Nickel cobalt manganese mixed liquor, alkali lye and the complexing agent co-precipitation that molar concentration is 1.5mol/L~1.8mol/L are prepared into
To mixed slurry, the mol ratio of nickel, cobalt and manganese is (0.5~1) in the nickel cobalt manganese mixed liquor：a：B, 0 ＜ a ＜ 0.20,0 ＜ b
＜ 0.30；Mixing speed in coprecipitation process is 800r/min~1100r/min；PH value in coprecipitation process for 11~
13；The temperature of co-precipitation is 40 DEG C~70 DEG C, and the atomic ratio of the nickel-cobalt-manganese ternary presoma is NixCoyMnz(OH)2, wherein
The ＜ z ＜ 0.30 of 0.50≤x ＜, 1.00,0 ＜ y ＜ 0.20,0；
（2）The mixed slurry is washed and adjusts viscosity and solid content is to suitable parameters, solid content is 20%~50%, viscosity
For 0cp~500cp；
（3）The mixed slurry is subjected to mist projection granulating, obtains granule materials, the atomisation pressure of the mist projection granulating is 0.1MPa
~0.5MPa；The tower chamber temperature of the mist projection granulating is 300 DEG C~500 DEG C.
（4）The granule materials are dried, obtain nickel-cobalt-manganese ternary presoma, the atom of the nickel-cobalt-manganese ternary presoma
Than for NixCoyMnz(OH)2, wherein the ＜ z ＜ 0.30 of 0.50≤x ＜, 1.00,0 ＜ y ＜ 0.20,0.
Step（1）The alkali lye is sodium hydroxide solution, content 5mol/L；.
Step（1）Described complexing agent is sodium citrate, content 1.25g/L.
Step（1）Described in coprecipitation process in pH value be 11~12.
Step（1）Described in mixing speed in coprecipitation process be 1000r/min.
Step（1）Described in the temperature that is co-precipitated be 45 DEG C~50 DEG C.
Rate-determining steps（1）Atmosphere in coprecipitation process is nitrogen atmosphere or inert gas atmosphere.
Rate-determining steps（1）Atmosphere in coprecipitation process is nitrogen atmosphere.
Step（2）Described in solid content be 20%~30%.
Step（3）Described in the atomisation pressure of mist projection granulating be 0.3MPa；The tower chamber temperature of the mist projection granulating is 300
℃。
Embodiment 1
Using NiSO4、CoSO4、MnSO4It is 1.6mol/L nickel cobalt manganese mixed liquors that raw material prepares total concentration in preparing tank, will
To mixed liquor be delivered to feed liquid storage tank, Ni in mixed liquor：Co：Mn mol ratio is 5:2:3, and sodium citrate is added
In feed liquid storage tank, stirring makes its content reach 1.25g/L；The sodium hydroxide solution for preparing 5mol/L is delivered to alkali lye storage
Bucket；Using measuring pump, feed liquid, alkali lye containing complexing agent simultaneously flow through flowmeter and enter reactor, and it is nitrogen to control reactor atmosphere
Gas atmosphere, reactor speed of agitator are 1000r/min, and pH 11.60, temperature is 45 DEG C；Slurry is flowed to after reactor is stable
Aging tank, suspension of the meso-position radius at 1.5 μm is obtained, suspension addition ceramic membrane washer is washed and lifted and contains admittedly
Amount, obtain the mixed slurry that solid content is 20%；Mixed slurry is pumped into mist projection granulating tower to be granulated, controls the atomisation pressure to be
0.3MPa, spray tower tower cavity temperature are 300 DEG C, and it is 110 DEG C to collect cloth bag temperature.By obtained material it is toasted, mixing, sieve
Divide, obtain 1.5 micron order monocrystalline type persursor material NixCoyMnz (OH) after iron removaling2。
The nickel-cobalt-manganese ternary persursor material that embodiment 1 obtains is scanned into Electronic Speculum to test, test result such as Fig. 3,4,
Fig. 3 is 3000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 1 is prepared, and Fig. 4 is implemented for the present invention
5000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that example 1 is prepared.
The nickel-cobalt-manganese ternary presoma being prepared according to the method test embodiment of the present invention 1 described in above-mentioned technical proposal
Tap density, test result is that the tap density of nickel-cobalt-manganese ternary presoma that the embodiment of the present invention 1 is prepared reaches
1.61g/cm3。
Embodiment 2
Using NiSO4、CoSO4、MnSO4 It is 1.8mol/L nickel cobalt manganese mixed liquors that raw material prepares total concentration in preparing tank, will
To mixed liquor be delivered to feed liquid storage tank, Ni in mixed liquor：Co：Mn mol ratio is 5:2:3, and sodium citrate is added
In feed liquid storage tank, stirring makes its content reach 1.25g/L；The sodium hydroxide solution for preparing 5mol/L is delivered to alkali lye storage
Bucket；Using measuring pump, feed liquid, alkali lye containing complexing agent simultaneously flow through flowmeter and enter reactor, and it is nitrogen to control reactor atmosphere
Gas atmosphere, reactor speed of agitator are 1000r/min, and pH 11.00, temperature is 45 DEG C；Slurry is flowed to after reactor is stable
Aging tank, suspension of the meso-position radius at 3.0 μm is obtained, suspension addition ceramic membrane washer is washed and lifted and contains admittedly
Amount, obtain the mixed slurry that solid content is 30%；Mixed slurry is pumped into mist projection granulating tower to be granulated, controls the atomisation pressure to be
0.3MPa, spray tower tower cavity temperature are 300 DEG C, and it is 110 DEG C to collect cloth bag temperature.By obtained material it is toasted, mixing, sieve
Divide, obtain 1.5 micron order monocrystalline type persursor material NixCoyMnz (OH) after iron removaling2。
The nickel-cobalt-manganese ternary persursor material that embodiment 2 obtains is scanned into Electronic Speculum to test, test result such as Fig. 5,6,
Fig. 5 is 3000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 2 is prepared, and Fig. 6 is implemented for the present invention
5000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that example 2 is prepared.
The nickel-cobalt-manganese ternary presoma being prepared according to the method test embodiment of the present invention 2 described in above-mentioned technical proposal
Tap density, test result is that the tap density of nickel-cobalt-manganese ternary presoma that the embodiment of the present invention 2 is prepared reaches
1.85g/cm3。
Embodiment 3
Using NiSO4、CoSO4、MnSO4 It is 1.8mol/L nickel cobalt manganese mixed liquors that raw material prepares total concentration in preparing tank, will
To mixed liquor be delivered to feed liquid storage tank, Ni in mixed liquor：Co：Mn mol ratio is 17:2:1, and sodium citrate is added
Enter in feed liquid storage tank, stirring makes its content reach 1.25g/L；The sodium hydroxide solution for preparing 5mol/L is delivered to alkali lye storage
Bucket；Using measuring pump, feed liquid, alkali lye containing complexing agent simultaneously flow through flowmeter and enter reactor, and it is nitrogen to control reactor atmosphere
Gas atmosphere, reactor speed of agitator are 1000r/min, and pH 11.40, temperature is 50 DEG C；Slurry is flowed to after reactor is stable
Aging tank, suspension of the meso-position radius at 1.0 μm is obtained, suspension addition ceramic membrane washer is washed and lifted and contains admittedly
Amount, obtain the mixed slurry that solid content is 30%；Mixed slurry is pumped into mist projection granulating tower to be granulated, controls the atomisation pressure to be
0.3MPa, spray tower tower cavity temperature are 300 DEG C, and it is 110 DEG C to collect cloth bag temperature.By obtained material it is toasted, mixing, sieve
Divide, obtain 1.0 micron order monocrystalline type persursor material NixCoyMnz (OH) after iron removaling2。
The nickel-cobalt-manganese ternary persursor material that embodiment 3 obtains is scanned into Electronic Speculum to test, test result such as Fig. 7,8,
Fig. 7 is 5000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that the embodiment of the present invention 3 is prepared, and Fig. 8 is implemented for the present invention
10000 times of scanning electron microscope (SEM) photographs of the nickel cobalt manganese hydroxide that example 3 is prepared.
The nickel-cobalt-manganese ternary presoma being prepared according to the method test embodiment of the present invention 3 described in above-mentioned technical proposal
Tap density, test result is that the tap density of nickel-cobalt-manganese ternary presoma that the embodiment of the present invention 3 is prepared reaches
1.32g/cm3。
The present invention is described in detail above in association with embodiment and exemplary example, but these explanations are simultaneously
It is not considered as limiting the invention.It will be appreciated by those skilled in the art that without departing from the spirit and scope of the invention,
A variety of equivalencing, modification or improvement can be carried out to technical solution of the present invention and embodiments thereof, these each fall within the present invention
In the range of.Protection scope of the present invention is determined by the appended claims.
Claims (11)
- A kind of 1. preparation method of nickel-cobalt-manganese ternary presoma, it is characterised in that：The preparation method comprises the following steps,（1）Nickel cobalt manganese mixed liquor, alkali lye and the complexing agent co-precipitation that molar concentration is 1.5mol/L~1.8mol/L are prepared into To mixed slurry, the mol ratio of nickel, cobalt and manganese is (0.5~1) in the nickel cobalt manganese mixed liquor：a：B, 0 ＜ a ＜ 0.20,0 ＜ b ＜ 0.30；Mixing speed in coprecipitation process is 800r/min~1100r/min；PH value in coprecipitation process for 11~ 13；The temperature of co-precipitation is 40 DEG C~70 DEG C, and the atomic ratio of the nickel-cobalt-manganese ternary presoma is NixCoyMnz(OH)2, wherein The ＜ z ＜ 0.30 of 0.50≤x ＜, 1.00,0 ＜ y ＜ 0.20,0；（2）The mixed slurry is washed and adjusts viscosity and solid content is to suitable parameters, solid content is 20%~50%, viscosity For 0cp~500cp；（3）The mixed slurry is subjected to mist projection granulating, obtains granule materials, the atomisation pressure of the mist projection granulating is 0.1MPa ~0.5MPa；The tower chamber temperature of the mist projection granulating is 300 DEG C~500 DEG C.
- 2.（4）The granule materials are dried, obtain nickel-cobalt-manganese ternary presoma, the atomic ratio of the nickel-cobalt-manganese ternary presoma For NixCoyMnz(OH)2, wherein the ＜ z ＜ 0.30 of 0.50≤x ＜, 1.00,0 ＜ y ＜ 0.20,0.
- A kind of 3. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1, it is characterised in that：Step（1）Institute It is sodium hydroxide solution to state alkali lye, content 5mol/L；.
- A kind of 4. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1, it is characterised in that：Step（1）It is described Complexing agent be sodium citrate, content 1.25g/L.
- A kind of 5. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1, it is characterised in that：Step（1）In PH value in described coprecipitation process is 11~12.
- A kind of 6. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1, it is characterised in that：Step（1）In Mixing speed in the coprecipitation process is 1000r/min.
- A kind of 7. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1, it is characterised in that：Step（1）In The temperature of the co-precipitation is 45 DEG C~50 DEG C.
- A kind of 8. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1, it is characterised in that：Rate-determining steps （1）Atmosphere in coprecipitation process is nitrogen atmosphere or inert gas atmosphere.
- A kind of 9. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1 or 7, it is characterised in that：Control step Suddenly（1）Atmosphere in coprecipitation process is nitrogen atmosphere.
- A kind of 10. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1, it is characterised in that：Step（2）In Described solid content is 20%~30%.
- A kind of 11. preparation method of nickel-cobalt-manganese ternary presoma according to claim 1, it is characterised in that：Step（3）In The atomisation pressure of the mist projection granulating is 0.3MPa；The tower chamber temperature of the mist projection granulating is 300 DEG C.
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| CN108565455A (en) * | 2018-05-30 | 2018-09-21 | 北京石油化工学院 | A kind of method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor |
| CN112225262A (en) * | 2020-10-13 | 2021-01-15 | 中科(马鞍山)新材料科创园有限公司 | High-nickel quaternary precursor material, and preparation method and preparation system thereof |
| CN112652762A (en) * | 2020-12-21 | 2021-04-13 | 中科(马鞍山)新材料科创园有限公司 | Single-crystal-structure ternary lithium battery positive electrode precursor material and preparation method and application thereof |
| CN113292112A (en) * | 2021-05-21 | 2021-08-24 | 上海大学 | Preparation method of high-nickel ternary positive electrode precursor |
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Application publication date: 20180119 |