CN107963672B - The preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus - Google Patents
The preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus Download PDFInfo
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- C01P2004/50—Agglomerated particles
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- 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 invention discloses partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus and preparation method thereof, the preparation method includes the following steps: by using Ni in reaction kettle reaction product filtered fluid during control presoma coprecipitation reaction2+Concentration, to prepare the middle partial size nickel cobalt manganese hydroxide precursor of D50=8~15 μm.Preparation method of the present invention improves the uniformity of the size distribution of presoma, particle sphericity is more preferable and the whisker of surface one time uniformly, it is thick rodlike, promote the compacted density of positive electrode and can be to avoid the protrusion problem in coating process；After being sintered positive electrode, since compactness itself is good, increases in terms of the secondary ball particle thermal stability of formation, also significantly promote the thermal stability and security performance of material.
Description
Technical field
The present invention relates to technical field of new energy material preparation, and in particular to partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus
Object and preparation method thereof.
Background technique
It is the nickel cobalt manganese hydroxide that is prepared of host element as presoma using nickel-cobalt-manganese ternary element, prepares nickle cobalt lithium manganate
Positive electrode is high with its battery specific energy density, occupies the advantages that small in size is widely used in digital 3C and electric passenger vehicle neck
Domain.Due to being influenced during the preparation process by different governing factors, resulting nickel cobalt manganese hydroxide is in the side such as pattern, jolt ramming
Face has very big difference, to directly affect the performance of positive electrode after sintering.
Positive electrode is the key that lithium ion battery, and presoma is the key that positive electrode, and the battery to have had just must
The presoma that need have had.Anode material for lithium-ion batteries pattern, size distribution and tap density and its synthetic method are close
It is related.Tap density can be improved using the nickel cobalt manganese hydroxide of Co deposited synthesis, be greatly improved the processable type of material
Property.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the technological deficiency of background technique, partial size in a kind of coarse-grain palpus is provided
Nickel cobalt manganese hydroxide and preparation method thereof.The present invention is by using anti-in reaction kettle during control presoma coprecipitation reaction
Answer Ni in product filtered fluid2+Concentration, come partial size nickel cobalt manganese hydroxide precursor in preparing；Preparation method of the present invention mentions
The uniformity of the size distribution of presoma is risen, particle sphericity is more preferable and the whisker of surface one time is uniform, thick rodlike, promotes anode
The compacted density of material and can be to avoid the protrusion problem in coating process, after being sintered positive electrode, due to compactness itself
It is good, it increases in terms of the secondary ball particle thermal stability of formation, also significantly promotes the thermal stability and security performance of material.
The present invention solves technological means used by above-mentioned technical problem are as follows:
The preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus, by using control presoma coprecipitation reaction
Ni in reaction kettle reaction product filtered fluid in the process2+Concentration, to prepare the middle partial size nickel cobalt manganese of D50=8~15 μm
Hydroxide precursor.
The preparation method of partial size nickel cobalt manganese hydroxide, includes the following steps: in the coarse-grain palpus
(1) by soluble nickel salt, cobalt salt, manganese salt according to molar ratio needed for nickel cobalt manganese in hydroxide, i.e. nickel cobalt manganese hydrogen
Oxide chemistry general formula Ni1-x-yCoxMny(OH)2, wherein it is molten to be configured to mixed metal salt for 0.1≤x≤0.3,0.1≤y≤0.3
Then precipitating reagent and complexing agent is respectively configured in liquid；
(2) deionized water is added into reaction kettle under agitation, is passed through step (1) precipitating reagent and complexing agent system
It at mother liquor, and is passed through inert gas and carries out atmosphere protection, the entire reaction mechanism mechanism of reaction all needs sufficient inert gas to be protected；
(3) by step (1) mixed salt solution, precipitating reagent and the continual reaction for being passed through stirring of complexing agent
Coprecipitation reaction is carried out in kettle, nucleus is constantly formed and grown up, and when feed liquid reaches reaction kettle overflow port, is started from reaction kettle bottom
Portion releases about 100~200ml feed liquid, filters immediately, obtains filtered filtrate, Ni in accurate filtrates tested2+Concentration, work as object
Material granularity D50 stops charging when reaching 12 ± 0.5 μm, shuts down after continuing 0.5~2h of stirring；
(4) step (3) resulting material is aged, the material after ageing is centrifuged by alkali cleaning, dries, be sieved, removing
Partial size nickel cobalt manganese hydroxide in coarse-grain palpus is obtained after iron.
Preferably, in the step (1), total concentration of metal ions is 0.5~2.5mol/ in the mixed salt solution
L。
Preferably, in the step (1), the precipitating reagent is KOH, NaOH, Na2CO3In any one or a few.
It is highly preferred that the precipitating reagent is NaOH in the step (1).
Preferably, in the step (1), the precipitant concentration is 2~10mol/L.
Preferably, in the step (1), the complexing agent is ammonium hydroxide, ammonium sulfate, disodium ethylene diamine tetraacetate, sulfo group water
Poplar acid, any one or a few in glycine.
It is highly preferred that the complexing agent is ammonium sulfate in the step (1).
Preferably, in the step (1), the complexing agent concentration is 2~15mol/L.
Preferably, in the step (2), the additional amount of the deionized water is the 20~60% of reaction kettle effective volume.
Preferably, in the step (2), the mother liquor accounts for the 20~60% of reaction kettle effective volume, the mother liquor pH value
It is 10.00~12.50, ammonia value is 2~15g/L, and temperature is 40~65 DEG C.
Preferably, in the step (2), the inert gas is one or both of nitrogen or argon gas.
Preferably, in the step (3), the coprecipitation reaction temperature is 40~65 DEG C.
Preferably, in the step (3), the pH of the coprecipitation reaction is 10.00~12.50.
Preferably, in the step (3), the revolving speed when coprecipitation reaction is 200~1000 rpmo
Preferably, it in the step (3), is accurately tested using ICP (inductively coupled plasma atomic emission spectrometer)
Ni in filtrate2+Concentration.
Preferably, in the step (3), Ni in the 5min~2h test first-time filtrate of interval2+Concentration, it is ensured that Ni2+Concentration is protected
It holds within 0~1000ppm, if Ni2+Concentration is more than 1000 ppm, then the pH value in reaction kettle is increased, to Ni2+Concentration decline
After keep existing pH value.
It is highly preferred that in the step (3), Ni in the 1h test first-time filtrate of interval2+Concentration, it is ensured that Ni2+Concentration is maintained at
Within 0~1000ppm, if Ni2+Concentration is more than 1000ppm, then the pH value in reaction kettle is increased, to Ni2+It is kept after concentration decline
Existing pH value.
Preferably, in the step (3), partial size nickel cobalt manganese hydroxide granularity D50 is 8~15 μm in the coarse-grain palpus,
Tap density is 2.0~2.4g/cm3, whisker is thick rodlike.
Basic principle of the invention:
The present invention passes through Ni in solution during the reaction2+Content control the pH value of reaction, Ni2+Content is higher
When, increase pH value, Ni2+When content is relatively low, pH value is reduced, Ni is only allowed2+Content fluctuates in normal range value, so that reaction
PH value fluctuation is small, but can guarantee the normal growth of presoma, until reaching required granularity；Before being prepared by the method
Body is driven, good sphericity, tap density is big, and whisker is thick, and interior void is few, is conducive to the circulation longevity of positive electrode after raising sintering
Life.
Compared with prior art, technical solution of the present invention has the advantages that
(1) during the present invention is using control precursor synthesis, the concentration value tested in supernatant regulates and controls the lifting of pH,
The stability and consistency of nickel cobalt manganese hydroxide are promoted to stability contorting presoma surface whisker morphology and tap density；
(2) preparation method of the present invention improves the uniformity of the size distribution of presoma, and particle sphericity is more preferable and surface
Whisker is uniform, thick rodlike, and whisker is between slice shape and sheet；
(3) present invention is promoted the physicochemical property of corresponding positive electrode, is promoted just by the granularity and pattern of control presoma
The compacted density of pole material and can be to avoid the protrusion problem in coating process；
(4) nickel cobalt manganese hydroxide of the present invention is after being sintered positive electrode, since compactness itself is good, the secondary ball of formation
It increases in terms of particle thermal stability, also significantly promotes the thermal stability and security performance of material.
Detailed description of the invention
Partial size nickel cobalt manganese hydroxide amplifies 5000 times in the coarse-grain palpus that Fig. 1 is prepared for the embodiment of the present invention 1
SEM figure；
Partial size nickel cobalt manganese hydroxide amplifies 20000 times in the coarse-grain palpus that Fig. 2 is prepared for the embodiment of the present invention 1
SEM figure.
Specific embodiment
In order to better understand the content of the present invention, it is described further combined with specific embodiments below with attached drawing.Ying Li
Solution, these embodiments are only used for that the present invention is further described, rather than limit the scope of the invention.In addition, it should also be understood that, In
After having read the contents of the present invention, person skilled in art makes some nonessential changes or adjustment to the present invention, still belongs to
In protection scope of the present invention.
Embodiment 1
(1) nickel sulfate, cobaltous sulfate and manganese sulfate are configured to mixing salt solution in proportion, wherein total concentration of metal ions
For 1.5mol/L, nickel, cobalt, three element of manganese ratio be 0.5: 0.2: 0.3, the sodium hydroxide for then preparing 5mol/L respectively is molten
The ammonium sulfate of liquid and 9mol/L；
(2) the nickel cobalt manganese mixing salt solution, sodium hydroxide solution and the ammonium sulfate that prepare individually are pumped into and have been had been loaded with
It imitates in the reaction kettle of 40% deionized water of volume and is stirred, mixing speed 1000rpm, control sodium hydroxide solution and sulphur
The flow velocity of acid ammonium solution makes mixed solution pH value 11.50, and at 50 DEG C, reaction kettle whole process is passed through temperature of reaction kettle constant control
Nitrogen protection；When feed liquid reaches reaction kettle overflow port, starts to release about 200ml feed liquid from reactor bottom, filter immediately,
Filtered filtrate is obtained with Ni in the accurate filtrates tested of ICP (inductively coupled plasma atomic emission spectrometer)2+Concentration,
A Ni is tested per hour2+Concentration, it is ensured that Ni2+Concentration is maintained within 0~1000ppm.If Ni2+Concentration is more than 1000ppm,
The pH value in reaction kettle is then increased, to Ni2+Existing pH value is kept after concentration decline, granularity D50 stops when reaching 12 ± 0.5 μm
Charging, shuts down after continuing 0.5~2h of stirring；
(3) the nickel cobalt manganese hydroxide precursor that step (2) obtains is put into hot water kettle and is washed, by the forerunner after washing
Body is put into baking oven, takes out after freeze-day with constant temperature 20h under 120 DEG C of environment, is sieved after cooling, removes iron, obtains partial size nickel in coarse-grain palpus
Cobalt manganese hydroxide.
Partial size nickel cobalt manganese hydroxide sampling in step (3) the coarse-grain palpus is subjected to SEM (see Fig. 1 and Fig. 2) and jolt ramming
Density measurement, wherein D50 is 12.5 μm, and tap density is 2.38 g/cm3, whisker is thick rodlike.
Comparative example 1
(1) nickel chloride, cobalt chloride and manganese piece are configured to mixing salt solution in proportion, wherein always concentration of metal ions is
1.5mol/L, nickel, cobalt, three element of manganese ratio be 0.6: 0.2: 0.2, then respectively prepare 6mol/L sodium hydroxide solution and
The ammonia spirit of 9mol/L；
(2) the nickel cobalt manganese mixing salt solution, sodium hydroxide solution and the ammonia spirit that prepare individually are pumped into and are had been loaded with effectively
It in the reaction kettle of 50% deionized water of volume and is stirred, mixing speed 500rpm, controls sodium hydroxide solution and ammonium hydroxide
The flow velocity of solution makes mixed solution pH value 11.80, and for temperature of reaction kettle constant control at 60 DEG C, reaction kettle whole process is passed through nitrogen guarantor
Shield；When feed liquid reaches reaction kettle overflow port, start to release presoma in about 20ml feed liquid test feed liquid from reactor bottom
Granularity, the pH value of reaction is adjusted according to the growth tendency of granularity, and stability contorting grows based on 1~1.5 μm in every 8h, grew
When low, pH value in reaction is reduced；When growing too fast, then pH value in reaction is increased.Stop charging when granularity D50 reaches 12 ± 0.5 μm,
It is shut down after continuing 0.5~2h of stirring；
(3) the nickel cobalt manganese hydroxide precursor that step (2) obtains is put into hot water kettle and is washed, by the forerunner after washing
Body is put into baking oven, and freeze-day with constant temperature takes out afterwards for 24 hours under 120 DEG C of environment, is sieved after cooling, removes iron, obtains partial size nickel in coarse-grain palpus
Cobalt manganese hydroxide.
Partial size nickel cobalt manganese hydroxide sampling in step (3) the coarse-grain palpus is subjected to SEM and tap density test, wherein
D50 is 12.0 μm, tap density 2.10g/cm3, whisker is fine strip shape.
Comparative example 2
(1) nickel sulfate, cobaltous sulfate and manganese sulfate are configured to mixing salt solution in proportion, wherein total concentration of metal ions
For 1.5mol/L, nickel, cobalt, three element of manganese ratio be 0.8: 0.1: 0.1, the sodium hydroxide for then preparing 9mol/L respectively is molten
The ammonia spirit of liquid and 9mol/L；
(2) the nickel cobalt manganese mixing salt solution, sodium hydroxide solution and the ammonia spirit that prepare individually are pumped into and are had been loaded with effectively
It in the reaction kettle of 60% deionized water of volume and is stirred, mixing speed 600rpm, controls sodium hydroxide solution and ammonium hydroxide
The flow velocity of solution makes mixed solution pH value 12.00, and for temperature of reaction kettle constant control at 40 DEG C, reaction kettle whole process is passed through nitrogen guarantor
Shield；When feed liquid reaches reaction kettle overflow port, start to release presoma in about 20ml feed liquid test feed liquid from reactor bottom
Granularity, the pH value of reaction is adjusted according to the growth tendency of granularity, and stability contorting grows based on 1~1.5 μm in every 8h, grew
When low, pH value in reaction is reduced；When growing too fast, then pH value in reaction is increased.Stop charging when granularity D50 reaches 12 ± 0.5 μm,
It is shut down after continuing 0.5~2h of stirring；
(3) the nickel cobalt manganese hydroxide precursor that step (2) obtains is put into hot water kettle and is washed, by the forerunner after washing
Body is put into baking oven, takes out after freeze-day with constant temperature 20h under 120 DEG C of environment, is sieved after cooling, removes iron, obtains partial size nickel in coarse-grain palpus
Cobalt manganese hydroxide.
Partial size nickel cobalt manganese hydroxide sampling in step (3) the coarse-grain palpus is subjected to SEM and tap density test, wherein
D50 is 12.0 μm, tap density 2.02g/cm3, whisker is fine strip shape.
By embodiment 1 and comparative example 1, comparative example 2 it is found that during coprecipitation reaction mixing speed and reaction pH value
Stationary value to the importance of reaction product；Embodiment 1 passes through to solution Ni in reaction process2+Continue to monitor, pH can be made
Value obtains stable control, and comparative example 1 and comparative example 2 according to the every 8h of the granularity of presoma grow 1~1.5 μm to control pH,
Meeting to influence the direction of growth of crystal grain in reaction process, so that whisker becomes elongated, eventually becomes thin so that pH fluctuation is larger
Strip particle.
Above description is not the limitation to invention, and the present invention is also not limited to the example above.The common skill of the art
For art personnel in the essential scope of invention, the variations, modifications, additions or substitutions made also should belong to protection scope of the present invention.
Claims (8)
1. the preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus, which is characterized in that by using control presoma
Ni in reaction kettle reaction product filtered fluid during coprecipitation reaction2+Concentration, to prepare D50=8~15 μm, jolt ramming
Density is 2.0~2.4g/cm3, whisker be thick rodlike middle partial size nickel cobalt manganese hydroxide precursor；
The preparation method of partial size nickel cobalt manganese hydroxide, includes the following steps: in a kind of coarse-grain palpus
(1) by soluble nickel salt, cobalt salt, manganese salt according to molar ratio needed for nickel cobalt manganese in hydroxide, i.e. nickel cobalt manganese hydroxide
Object chemical general formula Ni1-x-yCoxMny(OH)2, wherein 0.1≤x≤0.3,0.1≤y≤0.3, are configured to mixed salt solution, so
After precipitating reagent and complexing agent is respectively configured；
(2) deionized water is added into reaction kettle under agitation, is passed through step (1) precipitating reagent and mother is made in complexing agent
Liquid, and be passed through inert gas and carry out atmosphere protection；
(3) by step (1) mixed salt solution, precipitating reagent and complexing agent is continual is passed through in the reaction kettle of stirring
Coprecipitation reaction is carried out, nucleus is constantly formed and grown up, and when feed liquid reaches reaction kettle overflow port, starts to put from reactor bottom
100~200ml feed liquid out filters immediately, obtains filtered filtrate, Ni in accurate filtrates tested2+Concentration, work as material size
D50 stops charging when reaching 12 ± 0.5 μm, shuts down after continuing 0.5~2h of stirring；
(4) step (3) resulting material is aged, by the material after ageing by alkali cleaning centrifugation, dry, sieving, except after iron
Obtain partial size nickel cobalt manganese hydroxide in coarse-grain palpus；
In the step (1), the complexing agent is ammonium hydroxide, ammonium sulfate, disodium ethylene diamine tetraacetate, sulfosalicylic acid, glycine
In any one or a few；
In the step (3), Ni in the 5min~2h test first-time filtrate of interval2+Concentration, it is ensured that Ni2+Concentration is maintained at 0~
Within 1000ppm, if Ni2+Concentration is more than 1000ppm, then the pH value in reaction kettle is increased, to Ni2+Keep existing after concentration decline
There is pH value.
2. the preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus as described in claim 1, it is characterised in that: institute
It states in step (1), total concentration of metal ions is 0.5~2.5mol/L in the mixed salt solution.
3. the preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus as described in claim 1, it is characterised in that: institute
It states in step (1), the precipitant concentration is 2~10mol/L.
4. the preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus as described in claim 1, it is characterised in that: institute
It states in step (1), the complexing agent concentration is 2~15mol/L.
5. the preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus as described in claim 1, it is characterised in that: institute
It states in step (2), the additional amount of the deionized water is the 20~60% of reaction kettle effective volume, and the mother liquor, which accounts for reaction kettle, to be had
The 20~60% of volume are imitated, the mother liquor pH value is 10.00~12.50, and ammonia value is 2~15mol/L, and temperature is 40~65 DEG C.
6. the preparation method of partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus as described in claim 1, which is characterized in that institute
It states in step (3), the coprecipitation reaction temperature is 40~65 DEG C, and the pH of coprecipitation reaction is 10.00~12.50, described total
Revolving speed when precipitation reaction is 200~1000rpm.
7. partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus, which is characterized in that using described in claim 1~6 any one
Method is prepared.
8. partial size nickel cobalt manganese hydroxide in a kind of coarse-grain palpus as claimed in claim 7, which is characterized in that in the coarse-grain palpus
Partial size nickel cobalt manganese hydroxide granularity D50 is 8~15 μm, and tap density is 2.0~2.4g/cm3, whisker is thick rodlike.
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| CN109250764B (en) * | 2018-08-30 | 2020-11-10 | 华友新能源科技（衢州）有限公司 | Preparation method of power type medium-particle-size nickel-cobalt-manganese precursor material |
| CN109686966B (en) * | 2018-12-05 | 2020-06-23 | 华友新能源科技（衢州）有限公司 | Ultra-large-particle-size nickel-cobalt-manganese hydroxide for energy storage and preparation method thereof |
| CN111106345A (en) * | 2020-01-04 | 2020-05-05 | 华友新能源科技（衢州）有限公司 | Microcrystalline refined nickel-cobalt-manganese composite hydroxide and ternary cathode material prepared from same |
| CN113299904B (en) * | 2021-05-24 | 2022-11-15 | 宁波容百新能源科技股份有限公司 | High-nickel precursor material, and preparation method and application thereof |
| CN114645329B (en) * | 2022-03-30 | 2023-08-01 | 宁波容百新能源科技股份有限公司 | Nickel-cobalt-manganese hydroxide with high nickel and low cobalt fine whisker and preparation method thereof |
| CN115012036B (en) * | 2022-05-31 | 2023-10-03 | 宁波容百新能源科技股份有限公司 | Fine whisker small-particle-size nickel cobalt manganese hydroxide and preparation method thereof |
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