CN107459069B - A method of reducing nickel cobalt aluminium presoma sulfur content - Google Patents
A method of reducing nickel cobalt aluminium presoma sulfur content Download PDFInfo
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- CN107459069B CN107459069B CN201710744895.3A CN201710744895A CN107459069B CN 107459069 B CN107459069 B CN 107459069B CN 201710744895 A CN201710744895 A CN 201710744895A CN 107459069 B CN107459069 B CN 107459069B
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- nickel cobalt
- cobalt aluminium
- aluminium presoma
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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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of methods for reducing nickel cobalt aluminium presoma sulfur content.The sulfate radical for being adsorbed on nickel cobalt aluminium presoma surface can be removed using lye such as traditional sodium hydroxide, lithium hydroxides, it is and bad to sulfate radical removal effect in nickel cobalt aluminium presoma crystal structure, it is difficult to meet requirement of the power battery anode material to impurity sulfur content.Nickel cobalt aluminium mixed metal solution, sodium hydroxide and ammonium hydroxide are added in reaction kettle the present invention simultaneously, by controlling reaction condition, obtain nickel cobalt aluminium presoma；It is transferred in washing kettle after nickel cobalt aluminium presoma removing mother liquor and is washed and starched and washed, then be dried, be sieved, obtain sulfur content≤1000ppm nickel cobalt aluminium presoma.Washing solution of the invention is at low cost, and washing process is simple, strong operability, high-efficient, to nickel cobalt aluminium presoma microscopic appearance without destruction, be it is a kind of be suitable for industrial technique, there is practical value.
Description
Technical field
The invention belongs to lithium ion battery nickel cobalt aluminium positive electrode material precursor technical field, especially a kind of reduction nickel cobalt aluminiums
The method of presoma sulfur content.
Background technique
With the fast development of electric automobile market, power lithium-ion battery is as one of its core component by industry
It pays high attention to.It is adversely affected since impurity has the security performance of battery, chemical property, cycle life etc., it is used for
Requirement of the positive electrode of lithium ion power in terms of Control of Impurities is very harsh.
Nickel cobalt lithium aluminate (NCA) positive electrode is one of positive electrode of power lithium-ion battery, using co-precipitation legal system
Standby NCA mainly has following 3 process routes: (1) preparing Ni using coprecipitation1-x-yCoxAly(OH)2, then mixed with Li salt
Sintering preparation NCA；(2) using nickel cobalt mixed metal solution co-precipitation preparation Ni1-xCox(OH)2, then in Ni1-xCox(OH)2Table
Bread covers Al (OH)3, finally NCA is prepared with Li salt mixed sintering；(3) using nickel cobalt mixed metal solution co-precipitation preparation Ni1- xCox(OH)2, then by Ni1-xCox(OH)2Sintering preparation NCA is mixed together with the source Al, Li salt.
In process route (1), when solution of metal sulfates being selected to prepare nickel cobalt aluminium presoma for raw material, nickel cobalt aluminium forerunner
Body sulfur content is very high.Sulfur content is mainly derived from sulfate radical, is on the one hand to be present in nickel cobalt aluminium presoma due to suction-operated
On the other hand the sulfate radical on surface is due to nickel and cobalt is+divalent, aluminium is+trivalent, it is present in nickel cobalt aluminium under charge balance effect
Sulfate radical in presoma crystal structure.It can be removed using lye such as traditional sodium hydroxide, lithium hydroxides and be adsorbed on nickel cobalt
The sulfate radical on aluminium presoma surface, and it is bad to sulfate radical removal effect in nickel cobalt aluminium presoma crystal structure, it is difficult to meet dynamic
Requirement of the power cell positive material to impurity sulfur content.Therefore, it is badly in need of developing a kind of side for reducing nickel cobalt aluminium presoma sulfur content
Method.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the problems of the above-mentioned prior art, a kind of reduction nickel cobalt is provided
The method of aluminium presoma sulfur content.
For this purpose, the present invention adopts the following technical scheme that: a method of nickel cobalt aluminium presoma sulfur content being reduced, including such as
Lower step:
1) nickel cobalt aluminium mixed metal solution, sodium hydroxide and ammonium hydroxide are added in reaction kettle simultaneously, item is reacted by control
Part obtains nickel cobalt aluminium presoma precipitating and mother liquor, nickel cobalt aluminium presoma is obtained after mother liquor is removed；
2) the nickel cobalt aluminium presoma in step 1) is transferred in washing kettle and is washed；
3) it washes and starches: washing solution being added into the washing kettle of step 2), opens stirring, after reaching wash time, then removes
Solution is washed, washing and starching number is 1-2 times；
4) it washes: washing water being added into the washing kettle after washing and starching, open stirring, after reaching wash time, then go
Except washing water；
5) the nickel cobalt aluminium presoma for obtaining step 4) is dry, and sieving obtains sulfur content≤1000ppm nickel cobalt aluminium forerunner
Body.
The reaction condition that the present invention refers to refers to: by control charging rate make reaction residence time 12h-32h, instead
Answer 48 DEG C -61 DEG C of temperature, pH value 10.80-11.35, ammonia value 6.0gL-1-10g·L-1, mixing speed 600rpm-700rpm and
N2Atmosphere.
Supplement as above-mentioned technical proposal, the chemical general formula of the nickel cobalt aluminium presoma are NixCoyAlz(OH)2+z,
Middle x+y+z=1, and 0.75≤x < 1.00,0 < y≤0.15,0 < z≤0.05.
Supplement as above-mentioned technical proposal, the washing kettle inside are equipped with 2-8 block baffle, are evenly distributed；Washing
The agitating paddle of kettle has 1-3 layers, and bottom agitating paddle is pusher agitating paddle；The blade quantity of every layer of agitating paddle is 2-6.
Supplement as above-mentioned technical proposal, in step 3), the washing solution is 0.1-2.0molL-1Carbonic acid
One of hydrogen sodium, sodium carbonate, formic acid, sodium formate, acetic acid, sodium acetate, oxalic acid, sodium oxalate, sodium hydroxide, ammonium hydroxide are a variety of
Mixed solution, the pH value for washing solution is 9.0-14.0.
In supplement as above-mentioned technical proposal, step 3) and step 4), the solid content of nickel cobalt aluminium precursor pulp is 10-
70%.
Supplement as above-mentioned technical proposal, in step 3), the revolving speed of stirring is 50-400rpm.
Supplement as above-mentioned technical proposal, in step 4), the revolving speed of stirring is 50-400rpm.
Supplement as above-mentioned technical proposal, in step 3), wash temperature is 40-80 DEG C, wash time 0.5-5h.
Supplement as above-mentioned technical proposal, in step 4), wash temperature is 40-80 DEG C, wash time 0.5-5h.
Supplement as above-mentioned technical proposal, in step 4), washing water is deionized water, distilled water or pure water.
Of the invention be particular in that provides a kind of washing solution and its washing process, can be by nickel cobalt aluminium presoma sulphur
Content is down to 1000ppm or less.
Washing solution of the invention is at low cost, and washing process is simple, strong operability, high-efficient, to nickel cobalt aluminium presoma
Microscopic appearance is a kind of suitable for industrial technique, has practical value without destruction.
Detailed description of the invention
Fig. 1 is FESEM photo of the nickel cobalt aluminium granular precursor of the embodiment of the present invention 1 at 1000 times；
Fig. 2 is FESEM photo of the nickel cobalt aluminium granular precursor at 1000 times after the embodiment of the present invention 1 is washed.
Specific embodiment
Embodiment 1
(1) nickel cobalt aluminium mixed metal solution, sodium hydroxide, ammonium hydroxide are passed through in reaction kettle simultaneously, pass through control charging speed
Degree makes the residence time 20h-22h of reaction, 59 DEG C -61 DEG C of reaction temperature, pH value 11.00-11.10, ammonia value 7.5gL-1-
8.0g·L-1, mixing speed 600rpm-610rpm, N2Atmosphere obtains nickel cobalt aluminium presoma precipitating and mother liquor, after mother liquor is removed
Nickel cobalt aluminium presoma is obtained, FESEM photo is as shown in Fig. 1.
(2) the nickel cobalt aluminium presoma in step (1) is transferred in washing kettle and is washed, 2 pieces are equipped with inside washing kettle
Baffle is evenly distributed；Agitating paddle is 1 layer, and bottom agitating paddle is pusher agitating paddle；The blade quantity of every layer of agitating paddle is
3.
(3) it washes and starches: washing solution being added into washing kettle, opens stirring.Washing solution is 0.4molL-1Sodium bicarbonate
Solution, and it is 9.0-12.0 that sodium hydroxide solution, which is added, to adjust pH.The solid content of slurry is 20%；The revolving speed of stirring is
300rpm；Wash temperature is 60 DEG C, wash time 1h.It washes and starches altogether 2 times.
(4) it washes: washing water being added into washing kettle, open stirring.The solid content of slurry is 10%-70%；Stirring
Revolving speed is 50rpm-400rpm；Wash temperature is 40 DEG C -80 DEG C, wash time 0.5h-5h, then removes washing water.
(5) the nickel cobalt aluminium presoma of removal washing water in step (4) is dried, is sieved, the nickel cobalt after being washed
Aluminium presoma, sulfur content 670ppm.The FESEM photo of nickel cobalt aluminium presoma is as shown in Fig. 2.Pass through comparison diagram 1 and Fig. 2
It is found that the microscopic appearance of the nickel cobalt aluminium presoma after washing does not change.
Embodiment 2
(1) nickel cobalt aluminium mixed metal solution, sodium hydroxide, ammonium hydroxide are passed through in reaction kettle simultaneously, pass through control charging speed
Degree makes the residence time 30h-32h of reaction, 54 DEG C -56 DEG C of reaction temperature, pH value 10.80-10.90, ammonia value 6.0gL-1-
6.5g·L-1, mixing speed 650rpm-660rpm, N2Atmosphere obtains nickel cobalt aluminium presoma precipitating and mother liquor, after mother liquor is removed
Obtain nickel cobalt aluminium presoma.
(2) the nickel cobalt aluminium presoma in step (1) is transferred in washing kettle and is washed, 4 pieces are equipped with inside washing kettle
Baffle is evenly distributed；Agitating paddle is 2 layers, and bottom agitating paddle is pusher agitating paddle；The blade quantity of every layer of agitating paddle is
4.
(3) it washes and starches: washing solution being added into washing kettle, opens stirring.Washing solution is 0.8molL-1Sodium formate is molten
Liquid, and it is 10.0-12.0 that ammonia spirit, which is added, to adjust pH.The solid content of slurry is 60%；The revolving speed of stirring is 100rpm；Washing
Temperature is 70 DEG C, wash time 4h.It washes and starches altogether 2 times.
(4) it washes: washing water being added into washing kettle, open stirring.The solid content of slurry is 50%；The revolving speed of stirring is
150rpm；Wash temperature is 60 DEG C, wash time 4h, then removes washing water.
(5) the nickel cobalt aluminium presoma of removal washing water in step (4) is dried, is sieved, the nickel cobalt after being washed
The microscopic appearance of aluminium presoma, sulfur content 790ppm, the nickel cobalt aluminium presoma after washing does not change.
Embodiment 3
(1) nickel cobalt aluminium mixed metal solution, sodium hydroxide, ammonium hydroxide are passed through in reaction kettle simultaneously, pass through control charging speed
Degree makes the residence time 12h-14h of reaction, 48 DEG C -50 DEG C of reaction temperature, pH value 11.25-11.35, ammonia value 9.5gL-1-
10g·L-1, mixing speed 690rpm-700rpm, N2Atmosphere obtains nickel cobalt aluminium presoma precipitating and mother liquor, after mother liquor is removed
Obtain nickel cobalt aluminium presoma.
(2) the nickel cobalt aluminium presoma in step (1) is transferred in washing kettle and is washed, 8 pieces are equipped with inside washing kettle
Baffle is evenly distributed；Agitating paddle is 3 layers, and bottom agitating paddle is pusher agitating paddle；The blade quantity of every layer of agitating paddle is
4.
(3) it washes and starches: washing solution being added into washing kettle, opens stirring.Washing solution is 1.5molL-1Sodium formate is molten
Liquid, and it is 12.0-14.0 that sodium hydroxide solution, which is added, to adjust pH.The solid content of slurry is 40%；The revolving speed of stirring is 150rpm；
Wash temperature is 45 DEG C, wash time 4h.It washes and starches altogether 1 time.
(4) it washes: washing water being added into washing kettle, open stirring.The solid content of slurry is 20%；The revolving speed of stirring is
300rpm；Wash temperature is 70 DEG C, wash time 2h, then removes washing water.
(5) the nickel cobalt aluminium presoma of removal washing water in step (4) is dried, is sieved, the nickel cobalt after being washed
The microscopic appearance of aluminium presoma, sulfur content 930ppm, the nickel cobalt aluminium presoma after washing does not change.
Examples detailed above is citing of the invention, although disclosing highly preferred embodiment of the present invention and attached for the purpose of illustration
Figure, however it is not intended to limit the present invention, anyone skilled in the art is not departing from the present invention and appended right
It is required that spirit and scope in, various substitutions, changes and modifications are all possible.Therefore, the present invention should not be limited to best reality
Apply example and attached drawing disclosure of that.
Claims (8)
1. a kind of method for reducing nickel cobalt aluminium presoma sulfur content, which comprises the steps of:
1) nickel cobalt aluminium mixed metal solution, sodium hydroxide and ammonium hydroxide are added in reaction kettle simultaneously, by controlling reaction condition, are obtained
To nickel cobalt aluminium presoma precipitating and mother liquor, nickel cobalt aluminium presoma is obtained after mother liquor is removed；
2) the nickel cobalt aluminium presoma in step 1) is transferred in washing kettle and is washed；2-8 is housed inside the washing kettle
Block baffle is evenly distributed；The agitating paddle of washing kettle has 1-3 layers, and bottom agitating paddle is pusher agitating paddle；Every layer of agitating paddle
Blade quantity be 2-6；
3) it washes and starches: washing solution being added into the washing kettle of step 2), opens stirring, after reaching wash time, then removes washing
Solution, washing and starching number is 1-2 times；
4) it washes: washing water being added into the washing kettle after washing and starching, open stirring, after reaching wash time, then remove and wash
Wash water；
5) the nickel cobalt aluminium presoma for obtaining step 4) is dry, and sieving obtains sulfur content≤1000ppm nickel cobalt aluminium presoma；
In step 3), the washing solution is 0.1-2.0molL-1Sodium bicarbonate, sodium carbonate, sodium formate, sodium acetate, grass
One of sour sodium or a variety of mixed solutions, the pH value that washing solution is adjusted with sodium hydroxide or ammonium hydroxide is 9.0-14.0.
2. the method according to claim 1 for reducing nickel cobalt aluminium presoma sulfur content, which is characterized in that before the nickel cobalt aluminium
The chemical general formula for driving body is NixCoyAlz(OH)2+z, wherein x+y+z=1, and 0.75≤x < 1.00,0 < y≤0.15,0 < z≤
0.05。
3. it is according to claim 1 or 2 reduce nickel cobalt aluminium presoma sulfur content method, which is characterized in that step 3) and
In step 4), the solid content of nickel cobalt aluminium precursor pulp is 10-70%.
4. the method according to claim 1 or 2 for reducing nickel cobalt aluminium presoma sulfur content, which is characterized in that in step 3),
The revolving speed of stirring is 50-400rpm.
5. the method according to claim 1 or 2 for reducing nickel cobalt aluminium presoma sulfur content, which is characterized in that in step 4),
The revolving speed of stirring is 50-400rpm.
6. the method according to claim 1 or 2 for reducing nickel cobalt aluminium presoma sulfur content, which is characterized in that in step 3),
Wash temperature is 40-80 DEG C, wash time 0.5-5h.
7. the method according to claim 1 or 2 for reducing nickel cobalt aluminium presoma sulfur content, which is characterized in that in step 4),
Wash temperature is 40-80 DEG C, wash time 0.5-5h.
8. the method according to claim 1 or 2 for reducing nickel cobalt aluminium presoma sulfur content, which is characterized in that in step 4),
Washing water is deionized water, distilled water or pure water.
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| CN108767218A (en) * | 2018-05-21 | 2018-11-06 | 金川集团股份有限公司 | A kind of post-processing approach that battery is prepared with nickel cobalt aluminium hydroxide |
| CN108946827B (en) * | 2018-07-03 | 2020-09-29 | 华友新能源科技（衢州）有限公司 | Ultra-small particle size nickel-cobalt-manganese hydroxide and preparation method thereof |
| CN109704412A (en) * | 2018-12-05 | 2019-05-03 | 郑州中科新兴产业技术研究院 | A kind of retired lithium-ion-power cell nickle cobalt lithium manganate tertiary cathode material recycling and reusing method |
| CN112441624A (en) * | 2019-08-30 | 2021-03-05 | 荆门市格林美新材料有限公司 | Preparation method of nickel-cobalt-aluminum precursor with high tap density and low impurity content |
| CN111847529A (en) * | 2020-07-23 | 2020-10-30 | 华友新能源科技（衢州）有限公司 | Method for removing sulfur content in hydroxide precursor |
| CN112079397A (en) * | 2020-08-28 | 2020-12-15 | 蜂巢能源科技有限公司 | Method for washing lithium-rich carbonate precursor |
| CN112357969A (en) * | 2020-10-19 | 2021-02-12 | 江苏集萃托普索清洁能源研发有限公司 | Method for removing nickel-cobalt-aluminum precursor impurity phase |
| CN112194202A (en) * | 2020-10-19 | 2021-01-08 | 荆门市格林美新材料有限公司 | Method for reducing sulfur content of large-particle impurities of nickel-cobalt-manganese ternary precursor |
| CN114684871A (en) * | 2020-12-28 | 2022-07-01 | 天津国安盟固利新材料科技股份有限公司 | Method for reducing sulfur content of sulfate system lithium ion battery positive electrode material precursor |
| CN112713269B (en) * | 2020-12-31 | 2021-10-29 | 浙江帕瓦新能源股份有限公司 | Production system and production method for reducing content of sodium ions and sulfate ions in precursor of positive electrode material |
| CN116675265B (en) * | 2023-07-27 | 2023-11-07 | 宜宾光原锂电材料有限公司 | Nickel-copper-iron-manganese precursor, preparation method thereof, washing method thereof, positive electrode material and battery |
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