CN108529687A - A kind of preparation method of hydroxide nickel cobalt manganese - Google Patents
A kind of preparation method of hydroxide nickel cobalt manganese Download PDFInfo
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- CN108529687A CN108529687A CN201810381788.3A CN201810381788A CN108529687A CN 108529687 A CN108529687 A CN 108529687A CN 201810381788 A CN201810381788 A CN 201810381788A CN 108529687 A CN108529687 A CN 108529687A
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- nickel cobalt
- cobalt manganese
- hydroxide
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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
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
Abstract
A kind of preparation method of hydroxide nickel cobalt manganese provided by the invention, is related to material preparation method technical field.The preparation method of the hydroxide nickel cobalt manganese include prepare nickel, cobalt, manganese mixing salt solution, prepare aqueous slkali, prepare reaction paste, filtering, ball milling and spray drying step.By ball milling and spray drying, the size distribution of ternary precursor can be controlled, it is ensured that the granularity of ternary precursor it is uniform, consistent.By the above method, the high ternary precursor of even particle size distribution, grain size consistency can be produced, is conducive to produce high performance nickel-cobalt-manganese ternary material.
Description
Technical field
The present invention relates to material preparation method technical fields, in particular to a kind of preparation side of hydroxide nickel cobalt manganese
Method.
Background technology
Currently, the mainstream production technology of ternary material is：Nickel cobalt manganese hydroxide (hereinafter referred to as ternary precursor) and lithium
Source dry mixing and then high temperature sintering are crushed, except iron, sieving packaging.Therefore the size distribution of ternary material depends mainly on three
The size distribution of first material precursor, so there be very high want in ternary material factory to the size distribution requirements of ternary material precursor
It asks.
And in ternary material precursor production process, the technological parameter for influencing granularity is more, such as：Nickel cobalt manganese salt is dense
Solution ph control when speed is added in degree, reaction kettle bottom liquid caustic soda concentration, reaction kettle base solution temperature, nickel cobalt manganese salt, nickel cobalt manganese salt is added
System, reaction kettle mixing speed etc. can have an impact ternary precursor size distribution.So as to cause the grain of ternary material precursor
Degree is unevenly distributed, and grain size consistency is poor, and ternary material cycle performance is caused to decline.
Invention content
In view of this, the purpose of the present invention includes providing a kind of preparation method of hydroxide nickel cobalt manganese, pass through ball milling and spray
Mist drying process enables to the size tunable of ternary precursor, produces the high ternary of even particle size distribution, grain size consistency
The problem of material overcomes granular precursor size unevenness in traditional handicraft, ternary material cycle performance is caused to decline, has pole
Big market application prospect and promotional value.
The present invention improves its technical problem using technical solution below to realize.
The preparation method of hydroxide nickel cobalt manganese provided by the invention, includes the following steps：
Prepare the mixing salt solution of nickel, cobalt, manganese.
Prepare aqueous slkali.
Reaction paste is prepared, the mixing salt solution and the aqueous slkali are mixed to form reaction paste, react life
At ternary precursor.
Filtering is filtered reaction product, washs after the completion of waiting for the reaction paste reaction.
Slurry after filtration step is carried out ball milling by ball milling.
Spray drying, the slurry after ball milling step is spray-dried, and obtains ternary precursor hydroxide nickel cobalt manganese.
Further, in the mixing salt solution step for preparing nickel, cobalt, manganese, the salt of the nickel, cobalt, manganese is configured to
The mixing salt solution of 100g/L to 200g/L.
Further, described to prepare in aqueous slkali step, the concentration of sodium hydroxide solution is configured to 0.5mol/L extremely
6mol/L。
Further, described to prepare in reaction paste step, it is also necessary to it is added complexing agent, it is the mixing salt solution, described
Aqueous slkali and the complexing agent are mixed, are stirred jointly, form the reaction paste.
Further, described to prepare in reaction paste step, by the mixing salt solution, the aqueous slkali and the complexing
Agent mixing, stirring, control mixing speed are 200r/min to 1000r/min；Control the reaction paste temperature be 30 DEG C extremely
60 DEG C, pH value is 10 to 13.
Further, the ball milling step includes pre-grinding and fine grinding, the slurry after the filtration step is first carried out described in
Pre-grinding, then carry out the fine grinding.
Further, in the pre-grinding step, using Ball-stirring mill, pre- time consuming is 0.5 hour to 10 hours；The fine grinding
In step, using sand mill, the fine grinding time is 0.5 hour to 20 hours.
Further, in the pre-grinding step, pre-grinding electricity is 0.1Kwh/Kg to 20Kwh/Kg；In the fine milling step,
Pre-grinding electricity is 0.5Kwh/Kg to 20Kwh/Kg.
Further, in the spray drying step, control inlet air temperature is 100 DEG C to 350 DEG C, and leaving air temp is 80 DEG C
To 120 DEG C.
Further, in the spray drying step, using drying machine with centrifugal spray, the drying machine with centrifugal spray is controlled
Rotating speed be 5000r/min to 30000r/min；Or use pressure drying spraying machine, the atomization of the pressure drying spraying machine
Pressure is 0.05MPa to 0.75MPa.
A kind of preparation method of hydroxide nickel cobalt manganese provided by the invention, the advantageous effect with the following aspects：
The preparation method of hydroxide nickel cobalt manganese provided by the invention, including prepare nickel, cobalt, the mixing salt solution of manganese, preparation
Aqueous slkali prepares reaction paste, filtering, ball milling and spray drying step.By ball milling and drying process with atomizing, three can be controlled
The size distribution of first presoma, it is ensured that the granularity of ternary precursor it is uniform, consistent.The preparation method energy of the hydroxide nickel cobalt manganese
The high ternary precursor of even particle size distribution, grain size consistency is produced, overcomes in traditional handicraft granular precursor size not
, the problem of causing ternary material cycle performance to decline, is conducive to produce high performance nickel-cobalt-manganese ternary material, has very big
Market application prospect and promotional value.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is a kind of flow chart of the preparation method for hydroxide nickel cobalt manganese that the specific embodiment of the invention provides；
Fig. 2 is the ternary precursor sample that the preparation method for the hydroxide nickel cobalt manganese that the specific embodiment of the invention provides obtains
Electron microscope.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being usually described and illustrated herein in the accompanying drawings is implemented
The component of example can be arranged and be designed with a variety of different configurations.
Therefore, below the detailed description of the embodiment of the present invention to providing in the accompanying drawings be not intended to limit it is claimed
The scope of the present invention, but be merely representative of the present invention selected embodiment.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without creative efforts belongs to the model that the present invention protects
It encloses.
In the description of the present invention, it is to be understood that, the orientation or positional relationship of the instructions such as term "upper", "lower" is base
In orientation or positional relationship shown in the drawings, or product of the present invention using when the orientation or positional relationship usually put, or
Person is the orientation or positional relationship that those skilled in the art usually understand, is merely for convenience of description of the present invention and simplification of the description,
It does not indicate or imply the indicated equipment or element must have a particular orientation, with specific azimuth configuration and operation, because
This is not considered as limiting the invention.
" first ", " second " etc. of the present invention, is only used to distinguish between description, has no special meaning.
In the description of the present invention, it is also necessary to which explanation is unless specifically defined or limited otherwise, term " setting ",
" installation " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；Can be
It is connected directly, it can also be indirectly connected through an intermediary.It for the ordinary skill in the art, can be with concrete condition
Understand the concrete meaning of above-mentioned term in the present invention.
In ternary material precursor production process, the technological parameter for influencing granularity is very more, such as：Nickel cobalt manganese salt is dense
Solution ph control when speed is added in degree, reaction kettle bottom liquid caustic soda concentration, reaction kettle base solution temperature, nickel cobalt manganese salt, nickel cobalt manganese salt is added
System, reaction kettle mixing speed etc. can have an impact presoma size distribution.Therefore, the ternary material precursor produced at present
Size distribution disqualification rate is higher.Being uniformly distributed for granularity is controlling difficulties in ternary material production, and cost is higher.
In order to overcome drawbacks described above, present applicant proposes a kind of preparation methods of hydroxide nickel cobalt manganese, pass through ball milling and spray
Mist drying process can control the size distribution of ternary precursor, it is ensured that the granularity of ternary precursor it is uniform, consistent.The hydrogen
The preparation method of cobalt nickel oxide manganses can produce the high ternary precursor of even particle size distribution, grain size consistency, overcome tradition
Granular precursor size is uneven in technique, the problem of causing ternary material cycle performance to decline, and is conducive to produce high performance
Nickel-cobalt-manganese ternary material.
Fig. 1 is a kind of flow chart of the preparation method for hydroxide nickel cobalt manganese that the specific embodiment of the invention provides, and is please referred to
Fig. 1.
The preparation method of hydroxide nickel cobalt manganese provided in this embodiment, includes the following steps：
S1：Prepare the mixing salt solution of nickel, cobalt, manganese.
The salt of nickel, cobalt, manganese is configured to the mixing salt solution of 100g/L to 200g/L.
Optionally, nickel, cobalt, manganese salt include but not limited to nickel chloride, nickel sulfate, nickel nitrate, cobalt chloride cobaltous sulfate, nitric acid
Cobalt, manganese chloride, manganese sulfate.
S2：Prepare aqueous slkali.
Sodium hydroxide solution is configured to a concentration of 0.5mol/L to 6mol/L.
S3：Prepare reaction paste.
Above-mentioned mixing salt solution, aqueous slkali are mixed, and complexing agent are added, complexing agent uses ammonium hydroxide, prepares ammonium hydroxide
A concentration of 1mol/L to 8mol/L.
Mixing salt solution, aqueous slkali and complexing agent are added with scheduled flow in reaction kettle, common mixing, stirring, shape
At reaction paste.
Preferably, the mixing speed for controlling reaction kettle is 200r/min to 1000r/min；Control reaction paste temperature be
30 DEG C to 60 DEG C, pH value is 10 to 13.Reaction paste occurs chemical reaction and generates ternary precursor, the nucleus of ternary precursor by
Gradually grow up.
S4：Filtering.
After the completion of waiting for reaction paste reaction, reaction product is filtered, is washed.It should be noted that being filtered, washed
Number can be it is one or many, can be by least one of deionized water and absolute ethyl alcohol cleaning solution to reaction product
It is washed.Washing times are depending on actual product demand.
S5：Ball milling.
By the slurry after filtration step, i.e. reaction product carries out ball milling.
Preferably, ball milling step includes pre-grinding and fine grinding, by the slurry after filtration step, i.e. reaction product first carries out
Pre-grinding, then carry out fine grinding.
In pre-grinding step, using Ball-stirring mill pre-grinding, the pre- time consuming of reaction product is 0.5 hour to 10 hours；Or with
Voltameter, pre-grinding electricity are 0.1Kwh/Kg to 20Kwh/Kg.
In fine milling step, using sand mill fine grinding, the fine grinding time of reaction product is 0.5 hour to 20 hours；Or with
Voltameter, pre-grinding electricity are 0.5Kwh/Kg to 20Kwh/Kg.
S6：Spray drying.
By the slurry after fine grinding, i.e. reaction product is spray-dried, and obtains ternary precursor hydroxide nickel cobalt manganese.It is excellent
Selection of land, the inlet air temperature for controlling spray drying device are 100 DEG C to 350 DEG C, and leaving air temp is 80 DEG C to 120 DEG C.
For example, spray drying device uses drying machine with centrifugal spray, the rotating speed for controlling drying machine with centrifugal spray is 5000r/
Min to 30000r/min.Or spray drying device uses Pressuresprayingdrier, the atomization pressure of control pressure spray dryer
Power is 0.05MPa to 0.75MPa.Even-grained ternary precursor hydroxide nickel cobalt manganese can be thus obtained, chemical formula is：
NixCoyMnz(OH)2, wherein x+y+z=1.
Specific embodiment
1) by NiCl2·6H2O、CoCl2·6H2O and MnCl2·4H2O is configured to mixing salt solution, the wherein concentration of three
Respectively 150g/L, 150g/L and 125g/L.
2) take the sodium hydroxide solution of 2mol/L as aqueous slkali；Take the ammonium hydroxide of 2mol/L as complexing agent, by salt-mixture
Solution, aqueous slkali and ammonium hydroxide mixing are reacted, and controlling reaction temperature is 45 DEG C or so, pH value 11.5, mixing speed
For 300r/min.
After reaction, reaction product is filtered, and profit is washed with deionized 3 times, absolute ethyl alcohol washing 2
It is secondary.
3) ball milling：To first agitated mill pre-grinding 2 hours of reaction product, by sand mill fine grinding 3.5 hours.
4) it is spray-dried：Spray drying device uses Pressuresprayingdrier, the atomizing pressure of Pressuresprayingdrier to set
For 0.4MPa, charging rate 30mL/min, inlet air temperature is 300 DEG C, and leaving air temp is 110 DEG C, obtains ternary precursor
NixCoyMnz(OH)2(wherein, x+y+z=1).
Fig. 2 is the ternary precursor sample that the preparation method for the hydroxide nickel cobalt manganese that the specific embodiment of the invention provides obtains
Electron microscope.
Pass through nickel cobalt manganese hydroxide precursor Ni obtained by the above method1/3Co1/3Mn1/3(OH)2Granule-morphology is more advised
It is whole, it is mostly spherical, and even particle distribution, size is between 10 μm to 20 μm, as shown in Figure 2.
In conclusion a kind of preparation method of hydroxide nickel cobalt manganese provided by the invention has the beneficial of the following aspects
Effect：
A kind of preparation method of hydroxide nickel cobalt manganese provided by the invention, including prepare nickel, cobalt, manganese mixing salt solution,
It prepares aqueous slkali, prepare reaction paste, filtering, ball milling and spray drying step.By ball milling and drying process with atomizing, using stirring
After mixing mill pre-grinding, dried using sand mill fine grinding, then spray-dried equipment, this preparation method can control ternary precursor
Size distribution, it is ensured that the granularity of ternary precursor it is uniform, consistent.In traditional mainstream production technology, by adjusting coprecipitated
The factor controllings presoma size distribution such as mixing speed and solution flow rate is compared during prepared by drop method, what the application proposed
The adjustment of preparation method size distribution is easier to realize.
The preparation method of the hydroxide nickel cobalt manganese is largely reduced to each factor during production presoma
Condition requirement, can produce the high ternary precursor of even particle size distribution, grain size consistency, overcome presoma in traditional handicraft
Granular size is uneven, the problem of causing ternary material cycle performance to decline, and is conducive to produce high performance nickel-cobalt-manganese ternary material
Material has great market application prospect and promotional value.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the present invention can have various changes, combination and variation.All within the spirits and principles of the present invention, made by
Any modification, equivalent substitution, improvement and etc. should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of hydroxide nickel cobalt manganese, which is characterized in that include the following steps：
Prepare the mixing salt solution of nickel, cobalt, manganese；
Prepare aqueous slkali；
Reaction paste is prepared, the mixing salt solution and the aqueous slkali are mixed to form reaction paste, react generation three
First presoma；
Filtering is filtered reaction product, washs after the completion of waiting for the reaction paste reaction；
Slurry after filtration step is carried out ball milling by ball milling；
Spray drying, the slurry after ball milling step is spray-dried, and obtains ternary precursor hydroxide nickel cobalt manganese.
2. the preparation method of hydroxide nickel cobalt manganese according to claim 1, which is characterized in that described to prepare nickel, cobalt, manganese
In mixing salt solution step, the salt of the nickel, cobalt, manganese is configured to the mixing salt solution of 100g/L to 200g/L.
3. the preparation method of hydroxide nickel cobalt manganese according to claim 1, which is characterized in that described to prepare aqueous slkali step
In, the concentration of sodium hydroxide solution is configured to 0.5mol/L to 6mol/L.
4. the preparation method of hydroxide nickel cobalt manganese according to claim 1, which is characterized in that described to prepare reaction paste step
In rapid, it is also necessary to complexing agent be added, the mixing salt solution, the aqueous slkali and the complexing agent are mixed, stirred jointly, are formed
The reaction paste.
5. the preparation method of hydroxide nickel cobalt manganese according to claim 4, which is characterized in that described to prepare reaction paste step
In rapid, the mixing salt solution, the aqueous slkali and the complexing agent are mixed, stirring, control mixing speed is 200r/min
To 1000r/min；The temperature for controlling the reaction paste is 30 DEG C to 60 DEG C, and pH value is 10 to 13.
6. the preparation method of hydroxide nickel cobalt manganese according to claim 1, which is characterized in that the ball milling step includes pre-
Mill and fine grinding, first carry out the pre-grinding, then carry out the fine grinding by the slurry after the filtration step.
7. the preparation method of hydroxide nickel cobalt manganese according to claim 6, which is characterized in that in the pre-grinding step, adopt
With Ball-stirring mill, pre- time consuming is 0.5 hour to 10 hours；In the fine milling step, using sand mill, the fine grinding time is 0.5 small
Up to 20 hours.
8. the preparation method of hydroxide nickel cobalt manganese according to claim 6, which is characterized in that in the pre-grinding step, in advance
Electric mill amount is 0.1Kwh/Kg to 20Kwh/Kg；In the fine milling step, pre-grinding electricity is 0.5Kwh/Kg to 20Kwh/Kg.
9. the preparation method of hydroxide nickel cobalt manganese according to claim 1, which is characterized in that the spray drying step
In, control inlet air temperature is 100 DEG C to 350 DEG C, and leaving air temp is 80 DEG C to 120 DEG C.
10. the preparation method of hydroxide nickel cobalt manganese according to claim 9, which is characterized in that the spray drying step
In, using drying machine with centrifugal spray, the rotating speed for controlling the drying machine with centrifugal spray is 5000r/min to 30000r/min；Or
Person uses Pressuresprayingdrier, and the atomizing pressure of the Pressuresprayingdrier is 0.05MPa to 0.75MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN105140473A (en) * | 2015-07-23 | 2015-12-09 | 苏州迪思伏新能源科技有限公司 | Synthesis method for lithium-rich manganese-based layered oxide material of secondary lithium-ion spherical battery |
| CN107180950A (en) * | 2017-04-17 | 2017-09-19 | 张保平 | A kind of ternary cathode material of lithium ion battery NCM, NCA spray drying process preparation method |
| CN107658460A (en) * | 2017-10-18 | 2018-02-02 | 重庆特瑞新能源材料有限公司 | A kind of preparation method of modified nickel-cobalt-manganese multi material |
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2018
- 2018-04-25 CN CN201810381788.3A patent/CN108529687A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105140473A (en) * | 2015-07-23 | 2015-12-09 | 苏州迪思伏新能源科技有限公司 | Synthesis method for lithium-rich manganese-based layered oxide material of secondary lithium-ion spherical battery |
| CN107180950A (en) * | 2017-04-17 | 2017-09-19 | 张保平 | A kind of ternary cathode material of lithium ion battery NCM, NCA spray drying process preparation method |
| CN107658460A (en) * | 2017-10-18 | 2018-02-02 | 重庆特瑞新能源材料有限公司 | A kind of preparation method of modified nickel-cobalt-manganese multi material |
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| 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: 20180914 |