CN109574094A - A kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide - Google Patents
A kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide Download PDFInfo
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- CN109574094A CN109574094A CN201910067280.0A CN201910067280A CN109574094A CN 109574094 A CN109574094 A CN 109574094A CN 201910067280 A CN201910067280 A CN 201910067280A CN 109574094 A CN109574094 A CN 109574094A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The present invention provides a kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide, preparation method for control target, finds nucleation by experimental data and Screening PH or critical supernatant Ni that crystal is grown up with D50 (the volume percentile of the cumulative particle sizes of sample partial size corresponding when reaching 50%)2+Residual concentration passes through dynamic regulation pH value or the Ni of supernatant2+Residual concentration, so that the particle size and its distribution of nickel cobalt aluminium hydroxide fluctuates in smaller range, the standard deviation of D50 granularity is dropped to 0.1 or less by 0.6 by preparation method of the invention, the standard deviation of size distribution drops to 0.05 or less by 0.15, stable process control ensure that finished product nickel cobalt aluminium hydroxide stability, it largely improves in hydroxide preparation process and the consistency of final finished, so as to improve the stability of positive electrode and the consistency of battery core performance.
Description
Technical field
The present invention relates to nickel cobalt aluminium hydroxide preparation field, especially a kind of stable particle size and its distribution nickel cobalt aluminium hydrogen
The preparation method of oxide.
Background technique
With the promotion of lithium ion battery energy density, nickelic anode is becoming a kind of lithium ion battery of extremely hot topic just
Pole material is highly suitable on the power battery of high-energy density due to its characteristic with high capacity.Lot of domestic and international electricity
Core factory all has begun using nickelic positive electrode, and is applied on popular electric car, uses on tesla's automobile
It is nickel cobalt aluminium positive electrode.According to current present Research, have following two using nickelic system's positive electrode that Co and Al is adulterated
Kind advantage: the first this material uses more a small amount of Co, overcomes Co inadequate resource and its price wave to a certain extent
Dynamic defect；The addition of 2nd Al can improve the stability of positive electrode, and the doping of Al and Co can improve nickelic to a certain extent
It is the instable defect of cathode material structure.The synergistic effect of tri- kinds of elements of Ni, Co, Al, so that material has discharge capacity
Height, the advantage of stable circulation are kind of nickelic system's positive electrodes of awfully hot door.
The stability of nickel cobalt aluminium positive electrode particle size and its distribution is extremely important to the consistency of battery core performance, and nickel cobalt
The presoma raw material that aluminium positive electrode generallys use are nickel cobalt aluminium hydroxide, and the granularity and granularity of nickel cobalt aluminium hydroxide
Distribution can be inherited by nickel cobalt aluminium positive electrode.The nickel cobalt aluminium hydroxide of stable particle size and its distribution is prepared in summary
Object directly affects the stability of nickel cobalt aluminium positive electrode, then influences the consistency of battery core performance.
Summary of the invention
In order to overcome the disadvantages mentioned above of the prior art, the object of the present invention is to provide a kind of stable particle size and its distribution nickel
The preparation method of cobalt aluminium hydroxide can prepare the nickel cobalt aluminium hydrogen-oxygen that particle size stable is fixed and size distribution is stable by the method
The consistency of compound, stability and battery core performance for raising positive electrode is extremely important.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide, comprising the following steps: (1) by nickel salt
It is dissolved in deionized water with cobalt salt, nickel cobalt mixed liquor is made；(2) sodium metaaluminate is dissolved in sodium hydroxide solution, it is molten that aluminium is made
Liquid；(3) nickel cobalt mixed liquor, aluminum solutions and required complexing agent and precipitating reagent are added in reaction kettle, are stirred, by altogether
Precipitation reaction generates nickel cobalt aluminium hydroxide particles；
(4) when granularity D50 (i.e. the volume percentile of the cumulative particle sizes of sample partial size corresponding when reaching 50%)
When reaching targeted particle size, and when granularity presentation ascendant trend, the injection of sodium hydroxide flow is increased, PH is promoted, promotes more polycrystalline
The generation of core, to prevent particle growth.When granularity D50 reaches target, and when granularity presentation downward trend, reduce hydroxide
The injection of sodium flow reduces PH, reduces the production rate of nucleus, promote particle growth.
As a further improvement of the present invention: (5) (4) step being replaced using step, (5) the step includes:
(5) it is control target with D50, finds nucleation and Screening PH that crystal is grown up is B1, using B1 as control center value,
Dynamic regulation PH dynamic fluctuation between (B1-X, B1, B1+X) this three, wherein the regulation of 0.1≤X≤0.5, PH by adjusting
The injection rate of precipitating reagent is realized.
As a further improvement of the present invention: (4) step is replaced using step (6), the step (6) include: (6) with
D50 is control target, finds nucleation and critical supernatant Ni that crystal is grown up2+Residual concentration (does not precipitate complete in ie in solution
Ni2+) range be C~Dppm, centered on C~Dppm, dynamic regulation Ni2+Residual concentration (< C, C~D, > D) this three
Dynamic fluctuation in a range, Ni2+The regulation of residual concentration is realized by adjusting the injection rate of precipitating reagent.
The chemical general formula of the nickel cobalt aluminium hydroxide is Ni1-a-cCoaAlc(OH)2+c(0.05≤a≤0.20,0.01
≤c≤0.10)。
As a further improvement of the present invention: the step (1) in, the nickel salt be nickel chlorate, nickel nitrate or nickel sulphur
One of hydrochlorate, the cobalt salt are one of cobalt chlorate, cobalt nitrate or cobalt sulfate, and nickel, cobalt metal ion
Total concentration is in 1-2mol/L.
As a further improvement of the present invention: the step (2) in, the Al of the aluminum solutions3+Concentration in 0.05-
0.5mol/L, the concentration of sodium hydroxide solution is in 1-2mol/L.
As a further improvement of the present invention: the step (3) in, the precipitating reagent be sodium hydroxide, sodium carbonate or carbonic acid
One of hydrogen sodium, concentration is in 2-10mol/L.
As a further improvement of the present invention: the step (3) in, the complexing agent be ammonium hydroxide, ethylenediamine tetra-acetic acid, second
One of edetate disodium or glycine, concentration is in 3-15mol/L.
As a further improvement of the present invention: the step (3) in, the PH of reaction kettle is controlled in 10.5-12.5.
As a further improvement of the present invention: the step (3) in, the control of the temperature of reaction kettle is at 30-70 DEG C, reaction kettle
Mixing speed in 200-500rad/min.
As a further improvement of the present invention: Screening PH is confirmed by the experimental data that granularity fluctuates, such as PH exists
The process grown up is presented in 11.20-11.29 granularity, and the process of decline, critical PH is presented in PH granularity between 11.31-11.40
Value is it is confirmed that the variation for 11.30, PH is regulated and controled by precipitating reagent injection rate.
As a further improvement of the present invention: critical supernatant Ni2+The experiment number that residual concentration range is fluctuated by granularity
According to confirmation, such as Ni2+Residual concentration in 150ppm or more, grow up, and Ni2+ residual concentration is being less than 70ppm by granularity presentation
When, granularity, which is presented, to be reduced, critical supernatant Ni2+Residual concentration range is it is confirmed that be 70-150ppm, Ni2+Residual concentration
Variation is regulated and controled by the injection rate of precipitating reagent.
Compared with prior art, the beneficial effects of the present invention are:
The stability of nickel cobalt aluminium hydroxide is to determine the stability deciding factor of positive electrode；And positive electrode
Stability is the key factor of battery core consistency again.The present invention provides a kind of stable particle size and its distribution nickel cobalt aluminium hydrogen-oxygens
The preparation method of compound, substantially increases in nickel cobalt aluminium hydroxide preparation process and the consistency of final finished, so as to improve
The stability of positive electrode, and then improve the consistency of battery core performance.
Detailed description of the invention
Fig. 1 is table 1.
Fig. 2 is table 2.
Fig. 3 is table 3.
Fig. 4 is table 4.
Fig. 5 is comparative example and the comprehensive finished product SEM comparison diagram of embodiment.
Fig. 6 is the fluctuation comparison diagram of comparative example and embodiment granularity.
Fig. 7 is the fluctuation comparison diagram of comparative example and embodiment size distribution.
Specific embodiment
Now in conjunction with Detailed description of the invention, the present invention is further described with embodiment:
Nickel cobalt aluminium hydroxide Ni is prepared in case of the present invention0.92Co0.05Al0.03(OH)2.03, the granularity D50 of particle is big
Small is 10.5 μm.(1) nickel salt and cobalt salt the following steps are included: be dissolved in deionized water, obtained nickel cobalt mixed liquor by preparation method；
Nickel and cobalt total concentration in nickel cobalt mixed liquor are 2mol/L.(2) sodium metaaluminate is dissolved in 2mol/L sodium hydroxide solution, is made
Aluminum solutions；Aluminum concentration in aluminum solutions is 0.1mol/L.(3) by nickel cobalt mixed liquor, aluminum solutions and required complexing agent and precipitating
Agent is added in reaction kettle, is stirred, and generates nickel cobalt aluminium hydroxide particles by coprecipitation reaction；Precipitating reagent uses concentration
For the sodium hydroxide solution of 7.5mol/L；The ammonia spirit that complexing agent is 10mol/L using concentration；The volume of reaction kettle is 5m3,
Using the double-deck pusher stirring, speed of agitator 200r/min；It is 55 DEG C, in reaction kettle that reaction kettle, which controls reaction process temperature,
Ammonia density is 11g/L in reaction solution；Reaction solution PH in reaction kettle is controlled in 10.5-12.5.(4) the coprecipitated of a period of time is passed through
It forms sediment and reacts, by the rule of experimental data, find PH critical value and be about 11.28, critical Ni2+Concentration be 40-100ppm.
Comparative example 1
(5) traditional control method is used, when granularity D50 reaches 10.5 μm or so, and ascendant trend is presented in granularity, is added
The injection of big sodium hydroxide flow promotes pH value to 11.28 or more, promotes the generation of more nucleus, to prevent particle growth.
(6) when granularity D50 reaches 10.5 μm or so, and downward trend is presented in granularity, the injection of sodium hydroxide flow is reduced, so that PH
Value drop to 11.28 hereinafter, reduce nucleus production rate, promote particle growth.
Every 4 hours to the nickel cobalt aluminium hydroxide Ni generated in reaction kettle0.92Co0.05Al0.03(OH)2.03Particle sampling
Once, 5 days data are acquired altogether.
With reference to Fig. 1, table 1 is the fluctuation tables of data of the fluctuation of comparative example granularity and size distribution.
Embodiment 1
(5) control method for using dynamic PH, when granularity D50 reaches 10.5 μm or so, and long main trend is presented in granularity,
PH value is adjusted to 11.30, after stablizing 60min, PH is adjusted to 11.28, stablizes 60min, and pH value is adjusted to 11.26, stablizes
60min is recycled with this；
(6) when granularity D50 reaches 10.5 μm or so, and reduction trend is presented in granularity, pH value is adjusted to 11.26, surely
After determining 60min, PH is adjusted to 11.28, and after stablizing 60min, pH value is adjusted to 11.30, stablizes 60min, as circulation.
Every 4 hours to the nickel cobalt aluminium hydroxide Ni generated in reaction kettle0.92Co0.50Al0.03(OH)3.03Particle sampling
Once, 5 days data are acquired altogether.
With reference to Fig. 2, table 2 is the fluctuation tables of data of the fluctuation of 1 granularity of case study on implementation and size distribution.
Embodiment 2
(5) using Ni in dynamic supernatant2+Control method, when granularity D50 reaches 10.5 μm or so, and granularity presentation length
When main trend, increases the injection rate of sodium hydroxide pellets agent, more nucleus are generated, the Ni in supernatant2+Control 40ppm
Hereinafter, after continuing 60min；The injection rate for reducing sodium hydroxide pellets agent, the Ni in supernatant2+Regulate and control to 40-100ppm model
In enclosing, after continuing for 60min；The injection rate for reducing sodium hydroxide pellets agent, the Ni in supernatant2+Regulate and control to 100ppm with
On, after continuing 60min；With this step cycle.
(6) when granularity D50 reaches 10.5 μm or so, when reduction trend is presented in granularity, reduction sodium hydroxide pellets agent
Injection rate reduces the generation of nucleus, so that particle growth, the Ni in supernatant2+Regulate and control to 100ppm or more, continues 60min
Afterwards；The injection rate for increasing sodium hydroxide pellets agent, the Ni in supernatant2+Regulate and control between 40-100ppm, after continuing 60min；
The injection rate for continuing increase sodium hydroxide pellets agent, the Ni in supernatant2+After regulating and controlling to 40ppm hereinafter, continuing 60min；With
This circulation.
Every 4 hours to the nickel cobalt aluminium hydroxide Ni generated in reaction kettle0.92Co0.05Al0.03(OH)2.03Particle sampling
Once, 5 days data are acquired altogether.
With reference to Fig. 3, table 3 is the fluctuation tables of data of the fluctuation of 2 granularity of case study on implementation and size distribution.
With reference to Fig. 4, table 4 is the comparative analysis tables of data of the parameters of finished product prepared by comparative example and embodiment 1,2.
With reference to Fig. 4,5,6 and 7, compare the parameters of finished product prepared by comparative example and embodiment 1,2, it is known that embodiment 1,
The finished product of 2 preparations is higher than the consistency of finished product prepared by comparative example, can deduce that preparation method of the invention can be largely
Improve the consistency of nickel cobalt aluminium hydroxide precursor.
In conclusion after those skilled in the art read file of the present invention, according to the technique and scheme of the present invention with
Technical concept is not necessarily to creative mental labour and makes other various corresponding conversion schemes, belongs to the model that the present invention is protected
It encloses.
Claims (10)
1. a kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide, it is characterised in that: the following steps are included:
(1) nickel salt and cobalt salt are dissolved in deionized water, nickel cobalt mixed liquor is made；
(2) sodium metaaluminate is dissolved in sodium hydroxide solution, aluminum solutions are made；
(3) nickel cobalt mixed liquor, aluminum solutions and required complexing agent and precipitating reagent are added in reaction kettle, are stirred, pass through
Coprecipitation reaction generates nickel cobalt aluminium hydroxide particles；
(4) when granularity D50 (i.e. the volume percentile of the cumulative particle sizes of sample partial size corresponding when reaching 50%) reaches
When controlling target, and when granularity presentation ascendant trend, the injection of precipitating agent flux is increased, PH is promoted, promotes the production of more nucleus
It is raw, to prevent particle growth.When granularity D50 reaches control target, and when granularity presentation downward trend, reduce precipitating reagent stream
The injection of amount reduces PH, reduces the production rate of nucleus, promote particle growth.
2. a kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide, it is characterised in that: using step (5) come
(4) instead of step, (5) the step includes:
It (5) is control mesh with D50 (i.e. the volume percentile of the cumulative particle sizes of sample partial size corresponding when reaching 50%)
Mark, finds nucleation and Screening PH that crystal is grown up is B1, and using B1 as control center value, dynamic regulation PH is in (B1-X, B1, B1+
X) dynamic fluctuation between this three, wherein the regulation of 0.1≤X≤0.5, PH are realized by adjusting the injection rate of precipitating reagent.
3. a kind of preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide, it is characterised in that: using step (6) come
(4) instead of step, the step (6) includes:
It (6) is control mesh with D50 (i.e. the volume percentile of the cumulative particle sizes of sample partial size corresponding when reaching 50%)
Mark finds nucleation and critical supernatant Ni that crystal is grown up2+Residual concentration (does not precipitate complete Ni in ie in solution2+) range
For C~Dppm, centered on C~Dppm, dynamic regulation Ni2+Residual concentration is in (< C, C~D, > D) dynamic within the scope of these three
Fluctuation, Ni2+The regulation of residual concentration is realized by adjusting the injection rate of precipitating reagent.
4. a kind of according to claim 1, preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide described in 2 or 3,
It is characterized by: the chemical general formula for the nickel cobalt aluminium hydroxide being prepared is Ni1-a-cCoaAlc(OH)2+c(wherein, 0.05≤a
≤0.20,0.01≤c≤0.10)。
5. a kind of according to claim 1, preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide described in 2 or 3,
It is characterized by: the step (1) in, the nickel salt is one of nickel chlorate, nickel nitrate or nickel sulfate, the cobalt
Salt is one of cobalt chlorate, cobalt nitrate or cobalt sulfate, and the total concentration of nickel, cobalt metal ion is in 1-2mol/L.
6. a kind of according to claim 1, preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide described in 2 or 3,
It is characterized by: the step (2) in, the Al of the aluminum solutions3+Concentration in 0.05-0.5mol/L, the sodium hydroxide solution
Concentration is in 1-2mol/L.
7. a kind of according to claim 1, preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide described in 2 or 3,
It is characterized by: the step (3) in, the precipitating reagent is one of sodium hydroxide, sodium carbonate or sodium bicarbonate, and concentration exists
2-10mol/L。
8. a kind of according to claim 1, preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide described in 2 or 3,
It is characterized by: the step (3) in, the complexing agent be ammonium hydroxide, ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate or sweet ammonia
One of acid, concentration is in 3-15mol/L.
9. a kind of according to claim 1, preparation method of stable particle size and its distribution nickel cobalt aluminium hydroxide described in 2 or 3,
It is characterized by: the step (3) in, the PH of reaction kettle is controlled in 10.5-12.5.
10. a kind of according to claim 1, preparation side of stable particle size and its distribution nickel cobalt aluminium hydroxide described in 2 or 3
Method, it is characterised in that: the step (3) in, the temperature of reaction kettle is controlled at 30-70 DEG C, and the mixing speed of reaction kettle is in 200-
500rad/min。
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Cited By (4)
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| CN110808369A (en) * | 2019-09-19 | 2020-02-18 | 宜宾光原锂电材料有限公司 | Preparation method of low-sodium-sulfur nickel-cobalt-aluminum ternary precursor |
| CN110931776A (en) * | 2019-12-24 | 2020-03-27 | 中南大学 | Preparation method of nickel-cobalt-manganese ternary positive electrode material precursor with multi-level distribution of particle sizes |
| CN114349068A (en) * | 2021-12-03 | 2022-04-15 | 宜宾光原锂电材料有限公司 | Preparation method of large-particle-size nickel-cobalt-aluminum ternary cathode material precursor |
| CN115092976A (en) * | 2022-07-08 | 2022-09-23 | 金驰能源材料有限公司 | Preparation method of precursor with high specific surface area and high tap density |
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| CN110931776A (en) * | 2019-12-24 | 2020-03-27 | 中南大学 | Preparation method of nickel-cobalt-manganese ternary positive electrode material precursor with multi-level distribution of particle sizes |
| CN110931776B (en) * | 2019-12-24 | 2021-02-02 | 中南大学 | Preparation method of nickel-cobalt-manganese ternary positive electrode material precursor with multi-level distribution of particle sizes |
| CN114349068A (en) * | 2021-12-03 | 2022-04-15 | 宜宾光原锂电材料有限公司 | Preparation method of large-particle-size nickel-cobalt-aluminum ternary cathode material precursor |
| CN115092976A (en) * | 2022-07-08 | 2022-09-23 | 金驰能源材料有限公司 | Preparation method of precursor with high specific surface area and high tap density |
| CN115092976B (en) * | 2022-07-08 | 2023-10-24 | 金驰能源材料有限公司 | Preparation method of precursor with high specific surface area and high tap density |
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