CN107572603A - A kind of preparation method of the spherical NCM presomas of small grain size - Google Patents
A kind of preparation method of the spherical NCM presomas of small grain size Download PDFInfo
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- CN107572603A CN107572603A CN201710751639.7A CN201710751639A CN107572603A CN 107572603 A CN107572603 A CN 107572603A CN 201710751639 A CN201710751639 A CN 201710751639A CN 107572603 A CN107572603 A CN 107572603A
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Abstract
A kind of preparation method of the spherical NCM presomas of small grain size disclosed by the invention, comprises the following steps：（1）Mixed ion solutions, wherein Ni are prepared into after being mixed using nickel sulfate, cobaltous sulfate, manganese sulfate2+、Co2+、Mn2+Total concentration be 1.5 2.0mol/L, Ni in the mixed ion solutions2+：Co2+：Mn2+Mol ratio is 5：2：3 or 6：2：2；（2）Mixed ion solutions are subjected to equimolar synthetic reaction with 2 3L/h flow and liquid caustic soda solution and ammoniacal liquor, regulation ammoniacal liquor flow control ammonia value is maintained at 8~11g/L, 45~60 DEG C of reaction temperature, and between pH scopes 10.00 12.00, speed of agitator is 800 1000rpm；Reaction time is 8~12h；（3）By step（2）Synthetic product be incubated and be aged, by pressure filtration washing, drying, drying temperature is 100~150 DEG C, and spherical little particle nickel cobalt manganese presoma Ni is obtained after 5~16h of constant temperaturexCoyMn1‑x‑y(OH)2.Crystallinity height, component uniformly spherical little particle nickel cobalt manganese presoma can be obtained using the preparation method of the present invention.
Description
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries, the system of more particularly to a kind of spherical NCM presomas of small grain size
Preparation Method.
Background technology
Demand with the fast development of lithium rechargeable battery, especially automobile power cell further increases, to three
First positive electrode various aspects of performance is proposed new requirement.At the same time, the Homogeneous synthesis to ternary anode material precursor,
Size distribution and pattern control, component segregation and Control of Impurities etc. it is also proposed new requirement.
Nickel-cobalt-manganese ternary material precursor is the basic material for preparing tertiary cathode material, its particle size and tap density
Etc. the performance and cycle performance that can directly affect anode material for lithium-ion batteries.At present, it is industrial using continuous co-precipitation
The particle diameter of nickel-cobalt-manganese ternary presoma prepared by method is mostly 7-15 μm, although this reduces the resistivity of ternary material powder,
But the migration path of lithium ion is added so that concentration polarization easily occurs between ternary material and electrolyte.Comparatively, granule
The structure of the ternary material in footpath is more complete, and specific discharge capacity is higher, and high rate performance is also preferable.Secondly, in bulky grain ternary material
The less little particle of many particle diameters can be generated in presoma production process, this strong influence cyclicity of lithium ion battery
Can, especially for high-nickel material.
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 the spherical NCM presomas of small grain size,
Crystallinity height, component uniformly spherical little particle nickel cobalt manganese presoma can be obtained using the preparation method of the present invention.
To achieve the above object, the present invention uses following technical scheme.
A kind of preparation method of the spherical NCM presomas of small grain size, the preparation method comprise the following steps,
（1）By the water soluble salt of Ni water soluble salt, Co water soluble salt and Mn according to Ni：Co ：Mn mol ratios
For x：y：1-x-y is mixed and is prepared mixed ion solutions, wherein Ni2+、Co2+、Mn2+Total concentration be 1.5-2.0mol/L, institute
State Ni in mixed ion solutions2+：Co2+：Mn2+Mol ratio is 5：2：3 or 6：2：2；
（2）The mixed ion solutions are added continuously in reactor and concentrated ammonia liquor and liquid caustic soda solution with certain flow 2-3L/h
Coprecipitation reaction is carried out, while adjusts ammoniacal liquor flow to control the ammonia value of supernatant to be maintained at 8~11g/L, reaction temperature
For 45~60 DEG C, regulation liquid caustic soda flow controls pH scopes between 10.00-12.00, speed of agitator 800-1000rpm；Reaction
Time is 8~12h, and nickel content is controlled in 0.02~0.04mg/L in the supernatant in reactor.
（3）By step（2）Synthetic product be incubated and be aged, then be by pressure filtration washing, drying, drying temperature
100~150 DEG C, spherical little particle nickel cobalt manganese presoma Ni of the present invention is obtained after 5~16h of constant temperaturexCoyMn1-x-y(OH)2。
Further, step（1）Described Ni2+、Co2+、Mn2+Total concentration be 1.6-1.8mol/L.
Further, step（2）Described liquid caustic soda solution is the sodium hydroxide solution containing 2-10mol/L.
Preferably, step（2）Described liquid caustic soda solution is the sodium hydroxide solution containing 5mol/L.
Further, step is being carried out（2）Before, mixed ion solutions and liquid caustic soda solution are removed using bag filtering is considered with pipeline
Iron.
Further, step（3）Described PH scope controls are between 11-12.
Further, when targeted particle size D50 is 3~4 μm, step（3）It is 8~10h to control the reaction time, targeted particle size
When D50 is 4~5 μm, step（3）It is 10~12h to control the reaction time.
Further, step（2）Described mixing speed control is 900-1000rpm.
Compared with prior art, beneficial effects of the present invention are：Crystallinity can be obtained using the preparation method of the present invention
The uniform spherical little particle nickel cobalt manganese presoma of high, component.
Brief description of the drawings
Fig. 1 is the granularity graph in the embodiment of the present invention 1.
Fig. 2 is to obtain 3000 times of electron microscopes of nickel cobalt manganese hydroxide in the embodiment of the present invention 1.
Fig. 3 is to obtain 10000 times of electron microscopes of nickel cobalt manganese hydroxide in the embodiment of the present invention 1.
Fig. 4 is to obtain 3000 times of electron microscopes of nickel cobalt manganese hydroxide in the embodiment of the present invention 2.
Fig. 5 is to obtain 10000 times of electron microscopes of nickel cobalt manganese hydroxide in the embodiment of the present invention 2.
Fig. 6 is to obtain 3000 times of electron microscopes of nickel cobalt manganese hydroxide in the embodiment of the present invention 3.
Fig. 7 is to obtain 10000 times of electron microscopes of nickel cobalt manganese hydroxide in the embodiment of the present invention 3.
Embodiment
Below by the present invention is described in detail, the features and advantages of the invention will become more with these explanations
To be clear, clear and definite.
A kind of preparation method of the spherical NCM presomas of small grain size, the preparation method comprise the following steps,
（1）By the water soluble salt of Ni water soluble salt, Co water soluble salt and Mn according to Ni：Co ：Mn mol ratios
For x：y：1-x-y is mixed and is prepared mixed ion solutions, wherein Ni2+、Co2+、Mn2+Total concentration be 1.5-2.0mol/L, institute
State Ni in mixed ion solutions2+：Co2+：Mn2+Mol ratio is 5：2：3 or 6：2：2；
（2）The mixed ion solutions are added continuously in reactor and concentrated ammonia liquor and liquid caustic soda solution with certain flow 2-3L/h
Coprecipitation reaction is carried out, while adjusts ammoniacal liquor flow to control the ammonia value of supernatant to be maintained at 8~11g/L, reaction temperature
For 45~60 DEG C, regulation liquid caustic soda flow controls pH scopes between 10.00-12.00, speed of agitator 800-1000rpm；Reaction
Time is 8~12h, and nickel content is controlled in 0.02~0.04mg/L in the supernatant in reactor.
（3）By step（2）Synthetic product be incubated and be aged, then be by pressure filtration washing, drying, drying temperature
100~150 DEG C, spherical little particle nickel cobalt manganese presoma Ni of the present invention is obtained after 5~16h of constant temperaturexCoyMn1-x-y(OH)2。
Further, step（1）Described Ni2+、Co2+、Mn2+Total concentration be 1.6-1.8mol/L.
Step（2）Described liquid caustic soda solution is the sodium hydroxide solution containing 2-10mol/L.
Step（2）Described liquid caustic soda solution is the sodium hydroxide solution containing 5mol/L.
Carrying out step（2）Before, mixed ion solutions and liquid caustic soda solution are filtered and pipeline iron removaling using bag is considered.
Step（3）Described PH scope controls are between 11-12.
When targeted particle size D50 is 3~4 μm, step（3）It is 8~10h to control the reaction time, and targeted particle size D50 is 4~5 μm
When, step（3）It is 10~12h to control the reaction time.
Step（2）Described mixing speed control is 900-1000rpm.
Embodiment 1
（1）The water soluble salt of Ni water soluble salt, Co water soluble salt and Mn is mixed and is configured to the aqueous solution, obtain mixing from
Sub- solution, wherein the hybrid ionic concentration that the mixed ion solutions include Ni2+, Co2+ and Mn2+ is 1 .6mol/L, Ni2
+ ：Co2+ ：Mn2+ mol ratios are 5：2：3；
（2）Configuration concentration is 5 .0mol/L sodium hydroxide solution；
（3）Will（1）The mixed ion solutions are added continuously in reactor and aqueous slkali and ammoniacal liquor with certain flow 3.0L/h
Equimolar synthetic reaction is carried out, and constantly regulate liquid caustic soda flow controls the pH value of reaction to be adjusted simultaneously between 11.6 ± 0.1
Ammoniacal liquor flow controls the ammonia value of supernatant to be maintained at 11.2 ± 0.2g/L, and the temperature of reactor is 45 DEG C, mixing speed is
1000rpm；
（4）By step（3）Synthetic product by press filtration, wash, be dried to obtain tertiary cathode material NCM presomas, gained three
First presoma-nickel cobalt manganese hydroxide particle diameter distribution is narrow, and component is uniform, and size tunable, and impurity is low（Such as Fig. 2 and Fig. 3 institutes
Show）.
Embodiment 2
The invention provides a kind of preparation method of NCM presomas manganese, this method comprises the following steps：
（1）The water soluble salt of Ni water soluble salt, Co water soluble salt and Mn is mixed and is configured to the aqueous solution, obtain mixing from
Sub- solution, wherein the hybrid ionic concentration that the mixed ion solutions include Ni2+, Co2+ and Mn2+ is 1 .8mol/L, Ni2
+：Co2+：Mn2+ mol ratios are 6：2：2；
（2）Configuration concentration is 5 .0mol/L sodium hydroxide solution；
（3）Will（1）The mixed ion solutions are added continuously in reactor and aqueous slkali and ammoniacal liquor with certain flow 3.0L/h
Equimolar synthetic reaction is carried out, and constantly regulate liquid caustic soda flow controls the pH value of reaction to be adjusted simultaneously between 11.5 ± 0.1
Ammoniacal liquor flow controls the ammonia value of supernatant to be maintained at 10.2 ± 0.2g/L, and the temperature of reactor is 55 DEG C, mixing speed is
950rpm；
（4）By step（4）Synthetic product by press filtration, wash, be dried to obtain tertiary cathode material NCM presomas.Gained three
First presoma-nickel cobalt manganese hydroxide particle diameter distribution is narrow, and component is uniform, and size tunable, and impurity is relatively low（Such as Fig. 4 and Fig. 5 institutes
Show）.
Embodiment 3
The invention provides a kind of preparation method of NCM presomas, this method comprises the following steps：
（1）The water soluble salt of Ni water soluble salt, Co water soluble salt and Mn is mixed and is configured to the aqueous solution, obtain mixing from
Sub- solution, wherein the hybrid ionic concentration that the mixed ion solutions include Ni2+, Co2+ and Mn2+ is 1 .8mol/L, Ni2
+：Co2+：Mn2+ mol ratios are 6：2：2；
（2）Configuration concentration is 5 .0mol/L sodium hydroxide solution；
（3）Will（1）The mixed ion solutions are added continuously in reactor and aqueous slkali and ammoniacal liquor with certain flow 2.0L/h
Equimolar synthetic reaction is carried out, and constantly regulate liquid caustic soda flow controls the pH value of reaction to be adjusted simultaneously between 11.4 ± 0.1
Ammoniacal liquor flow controls the ammonia value of supernatant to be maintained at 8.2 ± 0.2g/L, and the temperature of reactor is 60 DEG C, mixing speed is
900rpm；
（4）By step（4）Synthetic product by press filtration, wash, be dried to obtain tertiary cathode material NCM presomas.Gained three
First presoma-nickel cobalt manganese hydroxide particle diameter distribution is narrow, and component is uniform, and size tunable, and impurity is relatively low（Such as Fig. 6 and Fig. 7 institutes
Show）.
Experimental data statistical form
| Project | Experiment 1 | Experiment 2 | Experiment 3 | Experiment 4 | Experiment 5 |
| Salinity mol/L | 1.6 | 1.6 | 1.8 | 1.8 | 1.8 |
| Salt flow L/h | 2.0 | 2.5 | 2.0 | 2.5 | 3.0 |
| Mixing speed/rpm | 1000 | 950 | 1000 | 950 | 900 |
| React pH | 11.6±0.1 | 11.5±0.1 | 11.6±0.1 | 11.5±0.1 | 11.4±0.1 |
| Reaction temperature/DEG C | 45 | 50 | 50 | 55 | 60 |
| D50/ μm of granularity | 3.01 | 5.04 | 3.12 | 4.11 | 4.99 |
| Tap density g/cm3 | 2.02 | 2.17 | 2.07 | 2.21 | 2.27 |
The present invention is described in detail above in association with embodiment and exemplary example, but these explanations can not
It is interpreted as limitation of the present invention., can be with 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 are carried out to technical solution of the present invention and embodiments thereof, these each fall within the model of the present invention
In enclosing.Protection scope of the present invention is determined by the appended claims.
Claims (8)
- A kind of 1. preparation method of the spherical NCM presomas of small grain size, it is characterised in that：The preparation method comprises the following steps,（1）By the water soluble salt of Ni water soluble salt, Co water soluble salt and Mn according to Ni：Co ：Mn mol ratios For x：y：1-x-y is mixed and is prepared mixed ion solutions, wherein Ni2+、Co2+、Mn2+Total concentration be 1.5-2.0mol/L, institute State Ni in mixed ion solutions2+：Co2+：Mn2+Mol ratio is 5：2：3 or 6：2：2；（2）The mixed ion solutions are added continuously in reactor and concentrated ammonia liquor and liquid caustic soda solution with certain flow 2-3L/h Coprecipitation reaction is carried out, while adjusts ammoniacal liquor flow to control the ammonia value of supernatant to be maintained at 8~11g/L, reaction temperature For 45~60 DEG C, regulation liquid caustic soda flow controls pH scopes between 10.00-12.00, speed of agitator 800-1000rpm；Reaction Time is 8~12h, and nickel content is controlled in 0.02~0.04mg/L in the supernatant in reactor；（3）By step（2）Synthetic product be incubated and be aged, then by pressure filtration washing, drying, drying temperature is 100~ 150 DEG C, spherical little particle nickel cobalt manganese presoma Ni of the present invention is obtained after 5~16h of constant temperaturexCoyMn1-x-y(OH)2。
- A kind of 2. preparation method of the spherical NCM presomas of small grain size according to claim 1, it is characterised in that：Step（1） Described Ni2+、Co2+、Mn2+Total concentration be 1.6-1.8mol/L.
- A kind of 3. preparation method of the spherical NCM presomas of small grain size according to claim 1, it is characterised in that：Step（2） Described liquid caustic soda solution is the sodium hydroxide solution containing 2-10mol/L.
- A kind of 4. preparation method of the spherical NCM presomas of small grain size according to claim 1 or 3, it is characterised in that：Step （2）Described liquid caustic soda solution is the sodium hydroxide solution containing 5mol/L.
- A kind of 5. preparation method of the spherical NCM presomas of small grain size according to claim 1, it is characterised in that：Carry out Step（2）Before, mixed ion solutions and liquid caustic soda solution are filtered and pipeline iron removaling using bag is considered.
- A kind of 6. preparation method of the spherical NCM presomas of small grain size according to claim 1, it is characterised in that：Step（2） Described mixing speed control is 900-1000rpm.
- A kind of 7. preparation method of the spherical NCM presomas of small grain size according to claim 1, it is characterised in that：Step（3） Described PH scope controls are between 11-12.
- A kind of 8. preparation method of the spherical NCM presomas of small grain size according to claim 1, it is characterised in that：Target grain When degree D50 is 3~4 μm, step（3）It is 8~10h to control the reaction time, when targeted particle size D50 is 4~5 μm, step（3）Control Reaction time is 10~12h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574094A (en) * | 2019-01-24 | 2019-04-05 | 广东迈纳科技有限公司 | A kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide |
| CN110451585A (en) * | 2019-05-11 | 2019-11-15 | 浙江美都海创锂电科技有限公司 | A kind of nickelic, long circulating monocrystalline method for preparing anode material of lithium-ion battery |
| WO2020220662A1 (en) * | 2019-04-28 | 2020-11-05 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, positive electrode pole, lithium ion secondary battery and apparatus |
| CN115893515A (en) * | 2022-10-14 | 2023-04-04 | 宜宾光原锂电材料有限公司 | Novel positive electrode material precursor and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104201367A (en) * | 2014-04-18 | 2014-12-10 | 宁夏东方钽业股份有限公司 | High-density small-particle-size nickel-cobalt-manganese hydroxide and preparing method thereof |
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2017
- 2017-08-28 CN CN201710751639.7A patent/CN107572603A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104201367A (en) * | 2014-04-18 | 2014-12-10 | 宁夏东方钽业股份有限公司 | High-density small-particle-size nickel-cobalt-manganese hydroxide and preparing method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574094A (en) * | 2019-01-24 | 2019-04-05 | 广东迈纳科技有限公司 | A kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide |
| CN109574094B (en) * | 2019-01-24 | 2022-03-08 | 广东迈纳科技有限公司 | Preparation method of nickel-cobalt-aluminum hydroxide with stable particle size and particle size distribution |
| WO2020220662A1 (en) * | 2019-04-28 | 2020-11-05 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, positive electrode pole, lithium ion secondary battery and apparatus |
| CN110451585A (en) * | 2019-05-11 | 2019-11-15 | 浙江美都海创锂电科技有限公司 | A kind of nickelic, long circulating monocrystalline method for preparing anode material of lithium-ion battery |
| CN115893515A (en) * | 2022-10-14 | 2023-04-04 | 宜宾光原锂电材料有限公司 | Novel positive electrode material precursor and preparation method thereof |
| CN115893515B (en) * | 2022-10-14 | 2024-03-26 | 宜宾光原锂电材料有限公司 | Preparation method of nickel-cobalt-containing hydroxide positive electrode material precursor |
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Application publication date: 20180112 |