CN109037670A - A kind of method of continuity preparation little particle ternary precursor material - Google Patents
A kind of method of continuity preparation little particle ternary precursor material Download PDFInfo
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- CN109037670A CN109037670A CN201810752767.8A CN201810752767A CN109037670A CN 109037670 A CN109037670 A CN 109037670A CN 201810752767 A CN201810752767 A CN 201810752767A CN 109037670 A CN109037670 A CN 109037670A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
A kind of method of continuity preparation little particle ternary precursor material, is dissolved in water for the raw material including nickel salt, cobalt salt, manganese salt, obtains ternary mixed solution a；Using lye as precipitating reagent b；Ammonium hydroxide is as complexing agent c；One or more of polyvinyl alcohol, sodium oxalate, tartaric acid, triethanolamine are dissolved in water, wiring solution-forming d；There is N2Or liquid water in bottom is added in the reaction kettle of inert gas shielding, it heats up 50~70 DEG C, opens 200~800rpm of stirring；B, c and d first is added after mixing evenly, control b, c and d additional amount come adjust the pH value in reaction kettle be 10~12, after 0.01~0.2mol/L of concentration of 3~8g/L of ammonia content and solution d, tetra- kinds of solution of above-mentioned a, b, c, d are controlled into requirement by the concentration of the above pH value, ammonia content and solution d, four kinds of solution flow velocitys are controlled to be pumped into reaction kettle, coprecipitation reaction is carried out, and controlling material in reactor solid content simultaneously is 80~150g/L；Continuous discharge obtains 3 μm~5 μm precipitate particles；The precipitate particles obtain ternary precursor material by ageing, washing, drying.
Description
Technical field
The present invention relates to a kind of methods for preparing ion battery little particle ternary precursor material.
Background technique
Major part manufacturer prepares the ternary precursor material of conventional particle size (10 μm~15 μm) using continuity method at present,
Not only yield is high for the method, but also lot stability is good.But in the ternary precursor material for preparing low particle size (3 μm~5 μm)
When material, in order to obtain the preferable particle of pattern, be all made of batch process production, i.e., by the high solids content of material in kettle (200~
250g/L), particle growth rate is reduced, extends granule growth time, to obtain preferable sphericity.But the method not only yield
It is low, and open kettle every time and be both needed to reconfigure bottom liquid, a large amount of pure water, steam, electric energy, person works' amount etc. are expended, life is increased
Produce cost.In addition, the lot stability of batch process production is also poor.
Summary of the invention
The object of the present invention is to provide it is a kind of in the industrial production can continuous production preparation there is good spherical morphology
The ternary precursor material of lithium ion battery low particle size (3 μm~5 μm).
The purpose of the present invention is what is be achieved through the following technical solutions:
Raw material including nickel salt, cobalt salt, manganese salt is dissolved in water, obtains ternary mixed solution a；Using lye as precipitating
Agent b；Ammonium hydroxide is as complexing agent c；One or more of polyvinyl alcohol, sodium oxalate, tartaric acid, triethanolamine are dissolved in water, matched
At solution d；
There is N2Or liquid water in bottom is added in the reaction kettle of inert gas shielding, it heats up 50~70 DEG C, unlatching stirring 200~
800rpm；First be added b, c and d after mixing evenly, control b, c and d additional amount come adjust the pH value in reaction kettle be 10~12,
After 0.01~0.2mol/L of concentration of 3~8g/L of ammonia content and solution d, tetra- kinds of solution of above-mentioned a, b, c, d are pressed into the above pH value, ammonia
Content and the control of the concentration of solution d require, and control four kinds of solution flow velocitys and are pumped into reaction kettle, carry out coprecipitation reaction, and same
When control material in reactor solid content be 80~150g/L；Continuous discharge obtains 3 μm~5 μm precipitate particles；Described
Precipitate particles obtain ternary precursor material by ageing, washing, drying.
The preferred concentration of solution d is 0.01~0.06mol/L in reaction kettle of the present invention, and material in reactor preferably contains admittedly
Amount is 100~130g/L.
Between the ternary mixed solution a concentration preferably 1.5~2.0mol/L.
The lye is preferably sodium hydroxide or sodium carbonate liquor.
The preferred concentration of the lye is 5~10mol/L.
By the dense of one or more of polyvinyl alcohol, sodium oxalate, tartaric acid, triethanolamine wiring solution-forming d soluble in water
Degree.Preferably concentration is 2~5mol/L.
The ammonium hydroxide preferably use mass fraction for 18% ammonium hydroxide.
Due to, in order to obtain the preferable spheric granules of pattern, needing solid content 200 in strict control kettle in prior art production
~250g/L is caused to be produced using batch process, not only increases production cost, the stability of product is greatly reduced.But
How in the condition of continuous production 3 μm~5 μm this little particles and the preferable spheric granules of pattern obtained, inventor is also always
Grope in research.Until inventor is found surprisingly that by the pH value control of material in reactor be 10~12,3~8g/L of ammonia content
Afterwards, solid content control is added solution d and controls solution in reaction kettle simultaneously in 80~150g/L in further reaction kettle
Under these conditions of 0.01~0.2mol/L of d concentration synergistic effect, it may be implemented that continuous production obtains little particle and pattern is preferable
3 μm~5 μm ternary precursor spheric granules.
The persursor material is the hydroxide of nickel cobalt manganese Metal, molecular formula NixCoyMnz(OH)2, wherein
0.3≤x≤1,0.03≤y≤1, x+y+Z=1.
The preferred tartaric acid of solution d.
Detailed description of the invention
Fig. 1 is Ni prepared by the embodiment of the present invention 10.8Co0.1Mn0.1(OH)2Ternary precursor SEM figure.
Fig. 2 is Ni prepared by the present embodiment 20.6Co0.2Mn0.2(OH)2Ternary precursor material SEM figure.
Fig. 3 is Ni manufactured in the present embodiment0.5Co0.2Mn0.3(OH)2Ternary precursor material SEM figure.
Specific embodiment
Following embodiment is intended to illustrate invention rather than of the invention is further limited.
Embodiment 1
Weigh 19kg NiSO4·6(H2O)、2.5kg CoSO4·7H2O、1.54kg MnSO4·H2O is dissolved in 50L heat
In (50 DEG C) pure water, it is 1.8mol/L that ternary solution concentration, which is made,.Solution after mixing evenly successively passes through iron remover and micropore
Filter obtains solution as ternary liquid a；32% liquid alkaline 16L is weighed, pure water is added and is diluted to the lye that concentration is 5mol/L
As precipitating reagent b；The ammonium hydroxide of 5L 18% is weighed as complexing agent c；It weighs 0.65kg sodium oxalate to be dissolved in 2.4L pure water, match
It is set to the solution d that concentration is 2mol/L.
There is N212L pure water is added in the 20L reaction kettle of protection, is warming up to 55 DEG C and opens stirring, revolving speed 600rpm.
B, c and 300mL d solution is added, makes pH value 11 in kettle, ammonia content 6g/L, solution d concentration is 0.05mol/L.With wriggling
A solution is pumped into reaction kettle by pump with the flow velocity of 15mL/min, is controlled the flow velocity of b, c, d, so that pH value in kettle is remained 11, ammonia
Content is 6g/L, and solution d concentration is 0.05mol/L, solid content 110g/L, starts coprecipitation reaction.When precipitate particles ruler
It is very little reach 3 μm after, overflow go out material by ageing, washing, drying obtain Ni0.8Co0.1Mn0.1(OH)2Ternary precursor material
Material.Fig. 1 is Ni prepared by the present embodiment 10.6Co0.2Mn0.2(OH)2Ternary precursor material, particle size are 3 μm or so, can be with
Find out that sphericity is fine.
Embodiment 2
Weigh 15.8kg NiSO4·6(H2O)、5.6kg CoSO4·7H2O、3.4kg MnSO4·H2O is dissolved in 50L heat
In (50 DEG C) pure water, it is 2.0mol/L that ternary solution concentration, which is made,.Solution after mixing evenly successively passes through iron remover and micropore
Filter obtains solution as ternary liquid a；32% liquid alkaline 16L is weighed, pure water is added and is diluted to the lye that concentration is 8mol/L
As precipitating reagent b；The ammonium hydroxide of 7.5L 18% is weighed as complexing agent c；0.46kg tartaric acid is weighed to be dissolved in 1.5L pure water,
It is configured to the solution d that concentration is 2mol/L.
There is N212L pure water is added in the 20L reaction kettle of protection, is warming up to 50 DEG C and opens stirring, revolving speed 800rpm.
B, c and 180mL d solution is added, makes pH value 11.5 in kettle, ammonia content 7g/L, solution d concentration is 0.03mol/L.With compacted
A solution is pumped into reaction kettle by dynamic pump with the flow velocity of 15mL/min, is controlled the flow velocity of b, c, d, is remained pH value in kettle
11.5, ammonia content 7g/L, solution d concentration are 0.03mol/L, solid content 130g/L, start coprecipitation reaction.Work as sediment
After particle size reaches 4 μm, the material that overflow goes out obtains Ni by ageing, washing, drying0.6Co0.2Mn0.2(OH)2Ternary forerunner
Body material.
Fig. 2 is Ni prepared by the present embodiment 20.6Co0.2Mn0.2(OH)2Ternary precursor material, particle size are 4 μm of left sides
The right side, sphericity are fine.
Embodiment 3
Weigh 9.9kg NiSO4·6(H2O)、4.2kg CoSO4·7H2O、3.9kg MnSO4·H2O is dissolved in 50L heat
In (50 DEG C) pure water, it is 1.5mol/L that ternary solution concentration, which is made,.Solution after mixing evenly successively passes through iron remover and micropore
Filter obtains solution as ternary liquid a；32% liquid alkaline 16L is weighed, pure water is added and is diluted to the lye that concentration is 5mol/L
As precipitating reagent b；The ammonium hydroxide of 7.5L 18% is weighed as complexing agent c；280mL triethanolamine is weighed, is diluted to concentration with pure water
For 2mol/L solution as dispersing agent (surfactant) d.
There is N212L pure water is added in the 20L reaction kettle of protection, is warming up to 65 DEG C and opens stirring, revolving speed 600rpm.
B, c and 120mL d solution is added, makes pH value 10.5 in kettle, ammonia content 8g/L, dispersant concentration 0.02mol/L.With compacted
A solution is pumped into reaction kettle by dynamic pump with the flow velocity of 15mL/min, is controlled the flow velocity of b, c, d, is remained pH value in kettle
10.5, ammonia content 8g/L, dispersant concentration 0.02mol/L, solid content 100g/L start coprecipitation reaction.Work as precipitating
After composition granule size reaches 5 μm, the material that overflow goes out obtains Ni by ageing, washing, drying0.5Co0.2Mn0.3(OH)2Before ternary
Drive body material.
Fig. 3 is Ni manufactured in the present embodiment0.5Co0.2Mn0.3(OH)2Ternary precursor material, particle size are 3-5 μm, ball
Shape degree is fine.
Comparative example 1
It is compared with embodiment 1.Weigh 19kg NiSO4·6(H2O)、2.5kg CoSO4·7H2O、1.54kg MnSO4·
H2O is dissolved in hot (50 DEG C) pure water of 80L, and it is 1.8mol/L that ternary solution concentration, which is made,.Solution after mixing evenly successively passes through
Iron remover and millipore filter are crossed, obtains solution as ternary liquid a；32% liquid alkaline 16L is weighed, pure water is added and is diluted to concentration
For 5mol/L lye as precipitating reagent b；The ammonium hydroxide of 5L 18% is weighed as complexing agent c；0.65kg sodium oxalate is weighed to be dissolved in
In 2.4L pure water, it is configured to the solution d that concentration is 2mol/L.
There is N212L pure water is added in the 20L reaction kettle of protection, is warming up to 55 DEG C and opens stirring, revolving speed 600rpm.
B, c and 300mL d solution is added, makes pH value 11 in kettle, ammonia content 6g/L, solution d concentration is 0.05mol/L.With wriggling
A solution is pumped into reaction kettle by pump with the flow velocity of 15mL/min, is controlled the flow velocity of b, c, d, so that pH value in kettle is remained 11, ammonia
Content is 6g/L, and solution d concentration is 0.05mol/L, solid content 70g/L, starts coprecipitation reaction.When precipitate particles size
After reaching 3 μm, the material that overflow goes out obtains Ni by ageing, washing, drying0.8Co0.1Mn0.1(OH)2Ternary precursor material,
It was found that the particle sphericity come out is poor.
Comparative example 2
It is compared with embodiment 2.Weigh 15.8kg NiSO4·6(H2O)、5.6kg CoSO4·7H2O、3.4kg MnSO4·
H2O is dissolved in hot (50 DEG C) pure water of 50L, and it is 2.0mol/L that ternary solution concentration, which is made,.Solution after mixing evenly successively passes through
Iron remover and millipore filter are crossed, obtains solution as ternary liquid a；32% liquid alkaline 16L is weighed, pure water is added and is diluted to concentration
For 8mol/L lye as precipitating reagent b；The ammonium hydroxide of 7.5L 18% is weighed as complexing agent c；Weigh 0.46kg winestone acid dissolution
In 1.5L pure water, it is configured to the solution d that concentration is 2mol/L.
There is N212L pure water is added in the 20L reaction kettle of protection, is warming up to 50 DEG C and opens stirring, revolving speed 800rpm.
B, c and 30mL d solution is added, makes pH value 11.5 in kettle, ammonia content 7g/L, dispersant concentration 0.005mol/L.With compacted
A solution is pumped into reaction kettle by dynamic pump with the flow velocity of 15mL/min, is controlled the flow velocity of b, c, d, is remained pH value in kettle
11.5, ammonia content 7g/L, solution d concentration are 0.005mol/L, solid content 130g/L, start coprecipitation reaction.Work as precipitating
After composition granule size reaches 4 μm, the material that overflow goes out obtains Ni by ageing, washing, drying0.6Co0.2Mn0.2(OH)2Before ternary
Body material is driven, inventor has found that its particle surface is uneven, and sphericity is poor.
Comparative example 3
It is compared with embodiment 2.Weigh 15.8kg NiSO4·6(H2O)、5.6kg CoSO4·7H2O、3.4kg MnSO4·
H2O is dissolved in hot (50 DEG C) pure water of 50L, and it is 2.0mol/L that ternary solution concentration, which is made,.Solution after mixing evenly successively passes through
Iron remover and millipore filter are crossed, obtains solution as ternary liquid a；32% liquid alkaline 16L is weighed, pure water is added and is diluted to concentration
For 8mol/L lye as precipitating reagent b；The ammonium hydroxide of 7.5L 18% is weighed as complexing agent c；Weigh 0.46kg winestone acid dissolution
In 1.5L pure water, it is configured to the solution d that concentration is 2mol/L.
There is N212L pure water is added in the 20L reaction kettle of protection, is warming up to 50 DEG C and opens stirring, revolving speed 800rpm.
B, c and 2100mL d solution is added, makes pH value 11.5 in kettle, ammonia content 7g/L, solution d concentration is 0.3mol/L.With compacted
A solution is pumped into reaction kettle by dynamic pump with the flow velocity of 15mL/min, is controlled the flow velocity of b, c, d, is remained pH value in kettle
11.5, ammonia content 7g/L, solution d concentration are 0.3mol/L, solid content 130g/L, start coprecipitation reaction.Invention human hair
Existing particle is unable to reach 4 μm of target sizes.
Claims (8)
1. a kind of method of continuity preparation little particle ternary precursor material, which is characterized in that will include nickel salt, cobalt salt, manganese
Raw material including salt is dissolved in water, obtains ternary mixed solution a；Using lye as precipitating reagent b；Ammonium hydroxide is as complexing agent c；By poly- second
One or more of enol, sodium oxalate, tartaric acid, triethanolamine are dissolved in water, wiring solution-forming d；There is N2Or inert gas is protected
Liquid water in bottom is added in the reaction kettle of shield, heats up 50~70 DEG C, opens 200~800rpm of stirring；B, c and d is first added to stir evenly
Afterwards, control b, c and d additional amount come adjust the pH value in reaction kettle be 10~12, the concentration of 3~8g/L of ammonia content and solution d
After 0.01~0.2mol/L, tetra- kinds of solution of above-mentioned a, b, c, d are controlled into requirement by the concentration of the above pH value, ammonia content and solution d,
It controls four kinds of solution flow velocitys to be pumped into reaction kettle, carries out coprecipitation reaction, and control material in reactor solid content simultaneously and be
80~150g/L；Continuous discharge obtains 3 μm~5 μm precipitate particles；The precipitate particles are by ageing, washing, drying
Obtain ternary precursor material.
2. the method according to claim 1, wherein the concentration of solution d is 0.01~0.06mol/ in reaction kettle
L, the material solid content in reaction kettle are 100~130g/L.
3. method according to claim 1 or 2, which is characterized in that the concentration of the ternary mixed solution a 1.5~
Between 2.0mol/L.
4. method according to claim 1 or 2, which is characterized in that the lye is sodium hydroxide or sodium carbonate liquor.
5. method according to claim 1 or 4, which is characterized in that the concentration of lye is 5~10mol/L.
6. method according to claim 1 or 2, which is characterized in that by polyvinyl alcohol, sodium oxalate, tartaric acid, triethanolamine
One or more of wiring solution-forming d soluble in water concentration be 2~5mol/L.
7. method according to claim 1 or 2, which is characterized in that the persursor material is the hydrogen of nickel cobalt manganese Metal
Oxide, molecular formula NixCoyMnz(OH)2, wherein 0.3≤x≤1,0.03≤y≤1, x+y+Z=1.
8. method according to claim 1 or 2, which is characterized in that the solution d tartaric acid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110451587A (en) * | 2019-08-23 | 2019-11-15 | 东莞市宏湖智能装备有限公司 | A kind of ternary precursor preparation system |
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Application publication date: 20181218 |