CN114044542A - Nickel-cobalt-manganese ternary precursor and preparation method thereof - Google Patents

Nickel-cobalt-manganese ternary precursor and preparation method thereof Download PDF

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CN114044542A
CN114044542A CN202111285076.XA CN202111285076A CN114044542A CN 114044542 A CN114044542 A CN 114044542A CN 202111285076 A CN202111285076 A CN 202111285076A CN 114044542 A CN114044542 A CN 114044542A
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cobalt
nickel
value
ternary precursor
stage
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李军军
李航
刘梅红
王孝猛
王小敏
杜一举
琚少罕
赵子涵
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Huayou New Energy Technology Quzhou Co ltd
Zhejiang Huayou Cobalt Co Ltd
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Huayou New Energy Technology Quzhou Co ltd
Zhejiang Huayou Cobalt Co Ltd
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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
    • 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
    • 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
    • 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
    • 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 nickel-cobalt-manganese ternary precursor and a preparation method thereof. The preparation method comprises the following steps: preparing a mixed salt solution by using nickel, cobalt and manganese soluble salts as raw materials and pure water; adding the mixed salt solution, alkali liquor and ammonia water into a reaction kettle, controlling the temperature, the rotating speed, the ammonia value and the residence time, wherein the reaction is divided into a first stage with a high pH value and a second stage with a low pH value, the first stage is mainly crystal nucleation, the second stage is mainly crystal growth, and oxidizing gas is introduced when the second stage reacts until the granularity of crystals is 1.1-3.0 mu m until the D50 of the slurry reaches a set range; the pH value of the high pH value is 11.60-12.60, and the pH value of the low pH value is 10.4-11.40; and washing and drying the synthesized slurry to obtain the low-sodium-sulfur nickel-cobalt-manganese ternary precursor. The invention leads the material to be oxidized by introducing the oxidizing gas in the crystal growth stage, thereby reducing the surface energy of the particles, reducing the inclusion of sulfate ions, sodium ions and the like caused by agglomeration and reunion, and meeting the indexes of low sodium and low sulfur content.

Description

Nickel-cobalt-manganese ternary precursor and preparation method thereof
Technical Field
The invention belongs to the technical field of precursors of ternary nickel-cobalt-manganese cathode materials of lithium ion batteries, and particularly relates to a low-sodium-sulfur nickel-cobalt-manganese ternary precursor and a preparation method thereof.
Background
Environmental protection and energy crisis have become the core of social sustainable development, reduce the dependence on fossil energy, develop sustainable renewable energy and energy storage system, and have important meaning to improve energy utilization, environmental protection, solve the energy crisis. The lithium ion battery is the secondary battery which has the most application prospect and the fastest development at present, and as the application of the lithium ion battery in the fields of electric automobiles, mobile equipment and the like is gradually strengthened, the development of the lithium ion battery with higher performance is urgent.
The nickel cobalt lithium manganate (NCM) material has the advantages of high specific capacity, low price and the like, is one of the anode materials of the lithium ion battery, the preparation of a precursor by a coprecipitation method is the mainstream choice of manufacturers at present, and the used metal salt raw material is most widely sulfate. In the preparation process, sulfate ions and sodium ions can be adsorbed on the surfaces of the particles and can be included in the particles, and the sulfate ions and the sodium ions can be continuously retained in the subsequent sintering process of the anode material, so that the performance of the battery is seriously influenced finally.
Patent CN107459069A mentions a preparation method of a low-sulfur nickel-cobalt-aluminum precursor, the prepared ternary precursor is washed by a push type stirring kettle, the washing alkali liquor is 0.1-2 mol/L washing liquid, and the S content after washing is lower than 1000 ppm. Patent CN107611383A proposes a method for preparing a low-sulfur high-tap density nickel-cobalt-manganese ternary precursor, which comprises preparing nickel-cobalt-manganese hydroxide by an intermittent process that is performed by crystal nucleation and crystal growth in stages, increasing the density of nickel-cobalt-manganese hydroxide particles and reducing unqualified materials by a synthesis process of "stop reaction, settling, removing supernatant liquid, and starting reaction" in the crystal growth stage, and washing with low-concentration alkali solution and drying to obtain the low-sulfur high-tap density nickel-cobalt-manganese ternary precursor. The preparation method of the above patent is somewhat cumbersome, cannot be continuously produced, and requires special washing equipment.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a low-sodium-sulfur nickel-cobalt-manganese ternary precursor.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a nickel-cobalt-manganese ternary precursor comprises the following steps:
1) preparing a mixed salt solution by using nickel, cobalt and manganese soluble salts as raw materials and pure water;
2) adding the mixed salt solution, alkali liquor and ammonia water into a reaction kettle, controlling the temperature, the rotating speed, the ammonia value and the residence time, wherein the reaction is divided into a first stage with a high pH value and a second stage with a low pH value, the first stage is mainly crystal nucleation, the second stage is mainly crystal growth, and oxidizing gas is introduced when the second stage reacts until the granularity of crystals is 1.1-3.0 mu m until the D50 of the slurry reaches a set range;
the pH value of the high pH value is 11.60-12.60, and the pH value of the low pH value is 10.4-11.40;
3) washing and drying the slurry synthesized in the step 2) to obtain the low-sodium-sulfur nickel-cobalt-manganese ternary precursor.
The method leads the material to be oxidized to a certain extent by introducing the oxidizing gas in the crystal growth stage, thereby reducing the surface energy of the particles and reducing the inclusion of sulfate ions, sodium ions and the like caused by agglomeration and reunion.
Further, the chemical formula of the nickel-cobalt-manganese ternary precursor is NixCoyMnz(OH)2Wherein x + y + z is 1, x is more than 0.2 and less than 0.90, y is more than 0.1 and less than 0.3, and z is more than 0.1 and less than 0.3.
Further, in the step 1), the soluble salts of nickel, cobalt and manganese are sulfates, chlorides or nitrates of nickel, cobalt and manganese.
Further, in the step 2), the total concentration of the mixed salt solution is 1.5-2.5 mol/L, the concentration of the alkali liquor is 8.0-12.0 mol/L, and the concentration of the ammonia water is 15-25%.
Further, in the step 2), the temperature is 50-65 ℃, the rotating speed is 100-300 rpm, the ammonia value is 4-9 g/L, and the retention time is 30-130 h.
Further, in the step 2), the introduced oxidizing gas is oxygen or a mixed gas containing oxygen.
Further, in the step 2), the speed of introducing the oxidizing gas is 0.1-50L/min, and the total introducing amount is 0.2-1.0 m3The rate and total amount of feed are based on the oxygen in the oxidizing gas. When the amount of the introduced oxidizing gas is too small, the oxidation degree of the material is insufficient. Conversely, the morphology of the particles changes.
The invention also provides a nickel-cobalt-manganese ternary precursor prepared by the preparation method, wherein the nickel-cobalt-manganese ternary precursor D50 is 2.0-5.0 mu m, the S content is less than or equal to 800ppm, and the Na content is less than or equal to 50 ppm.
The invention has the following beneficial effects: the operation is simple, the continuous production can be realized, and the energy consumption is low; the prepared nickel-cobalt-manganese ternary precursor D50 is 2.0-5.0 mu m, the S content is less than or equal to 800ppm, and the Na content is less than or equal to 50 ppm.
Drawings
The invention is further described with reference to the drawings and the detailed description.
FIG. 1 is a SEM image at 5000X of Ni-Co-Mn hydroxide particles provided in example 1 of the present invention;
FIG. 2 is a SEM image at 5000 times of Ni-Co-Mn hydroxide particles provided in example 2 of the present invention;
FIG. 3 is a SEM image at 5000 times of Ni-Co-Mn hydroxide particles provided in example 3 of the present invention;
fig. 4 is a SEM image of 5000 times of the nickel cobalt manganese hydroxide particles provided in comparative example 1 of the present invention.
Fig. 5 is a SEM image of 5000 times of the nickel cobalt manganese hydroxide particles provided in comparative example 2 of the present invention.
Detailed Description
In order to facilitate understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the following specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The use of the term of art in this document is for the purpose of describing particular embodiments and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or prepared by an existing method.
Example 1
Low sodium sulfur Ni0.6Co0.2Mn0.2(OH)2Ternary precursor, D50 of 4.0 μm, S content of 770ppm, Na content of 35ppm, the preparation process is as follows:
(1) according to Ni0.6Co0.2Mn0.2(OH)2Preparing a salt solution according to the molar ratio of medium nickel, cobalt and manganese, wherein the total concentration is 2.0 mol/L; the concentration of the prepared alkali liquor is 10mol/L, and the concentration of the prepared ammonia water is 20%.
(2) Adding 1000-4000L of pure water as a base solution before starting up, adjusting the pH value of the base solution to 11.70-11.90 and the ammonia value to 5-6 g/L, stirring at a rotating speed of 150rpm and a temperature of 55 ℃, simultaneously adding the nickel-cobalt-manganese salt solution, the sodium hydroxide solution and the ammonia water into the reaction kettle, and standing for 50-90 hours.
(3) After the reaction is started, the first stage mainly takes nucleation as the main, the pH value is 11.70-11.90, the ammonia value is 5-6 g/L, and the duration is 0.1-0.5 h, and then the second stage enters a nuclear growth stage, and the pH value is adjusted to 10.7-10.8, and the ammonia value is 5-6 g/L.
(4) In the growth stage of the step (3), air is introduced at a rate of 10L/min and an introduction amount of 0.5m when the particle size reaches 1.1 μm3When D50 reached 4.0. mu.m, the reaction was stopped.
(5) And washing, drying and removing iron from the synthesized nickel-cobalt-manganese hydroxide to obtain a final product.
Example 2
Low sodium sulfur Ni0.6Co0.2Mn0.2(OH)2The ternary precursor, D50, was 3.0 μm, the S content was 730ppm, the Na content was 30ppm, and it was prepared as follows:
(1) according to Ni0.6Co0.2Mn0.2(OH)2Preparing a salt solution according to the molar ratio of medium nickel, cobalt and manganese, wherein the total concentration is 2.5 mol/L; the concentration of the prepared alkali liquor is 12mol/L, and the concentration of the prepared ammonia water is 25%.
(2) Adding 1000-4000L of pure water as a base solution before starting up, adjusting the pH value of the base solution to 12.40-12.60, adjusting the ammonia value to 8-9 g/L, stirring at a rotating speed of 300rpm and at a temperature of 60 ℃, simultaneously adding the nickel-cobalt-manganese salt solution, the sodium hydroxide solution and the ammonia water into the reaction kettle, and keeping for 100-130 h.
(3) After the reaction is started, the first stage mainly takes nucleation as the main, the pH value is 12.40-12.60, the ammonia value is 8-9 g/L, and the duration is 0.1-0.5 h, and then the second stage enters a nuclear growth stage, and the pH value is adjusted to 11.0-11.3, and the ammonia value is 8-9 g/L.
(4) In the growth stage of the step (3), air is introduced at a rate of 0.1L/min and an introduction amount of 1.0m when the particle size reaches 2.0 μm3When D50 reached 3.0. mu.m, the reaction was stopped.
(5) And washing, drying and removing iron from the synthesized nickel-cobalt-manganese hydroxide to obtain a final product.
Example 3
Low sodium sulfur Ni0.6Co0.2Mn0.2(OH)2Ternary precursor, D50 of 4.0 μm, S content of 780ppm, Na content of 45ppm, the preparation process is as follows:
(1) according to Ni0.6Co0.2Mn0.2(OH)2Preparing salt solution with the molar ratio of medium nickel, cobalt and manganese, and concentrating the salt solutionThe degree is 2.5 mol/L; the concentration of the prepared alkali liquor is 12mol/L, and the concentration of the prepared ammonia water is 25%.
(2) Adding 1000-4000L of pure water as a base solution before starting up, adjusting the pH value of the base solution to 11.60-11.80, adjusting the ammonia value to 4-5 g/L, stirring at a rotating speed of 100rpm and at a temperature of 60 ℃, simultaneously adding the nickel-cobalt-manganese salt solution, the sodium hydroxide solution and the ammonia water into the reaction kettle, and keeping the mixture for 40-60 hours.
(3) After the reaction is started, the first stage mainly takes nucleation as the main, the pH value is 11.60-11.80, the ammonia value is 4-5 g/L, the duration is 0.1-0.5 h, and then the second stage enters a nuclear growth stage, and the pH value is adjusted to 10.7-10.9, and the ammonia value is 4-5 g/L.
(4) In the growth stage of the step (3), air is introduced at a rate of 50L/min and an introduction amount of 0.2m when the grain size reaches 3.0 μm3When D50 reached 4.0. mu.m, the reaction was stopped.
(5) And washing, drying and removing iron from the synthesized nickel-cobalt-manganese hydroxide to obtain a final product.
Comparative example 1
Low sodium sulfur Ni0.6Co0.2Mn0.2(OH)2The ternary precursor, D50, was 4.0 μm, the S content was 730ppm, the Na content was 30ppm, and it was prepared as follows:
(1) according to Ni0.6Co0.2Mn0.2(OH)2Preparing a salt solution according to the molar ratio of medium nickel, cobalt and manganese, wherein the total concentration is 2.0 mol/L; the concentration of the prepared alkali liquor is 10mol/L, and the concentration of the prepared ammonia water is 20%.
(2) Adding 1000-4000L of pure water as a base solution before starting up, adjusting the pH value of the base solution to 11.70-11.90 and the ammonia value to 5-6 g/L, stirring at a rotating speed of 150rpm and a temperature of 55 ℃, simultaneously adding the nickel-cobalt-manganese salt solution, the sodium hydroxide solution and the ammonia water into the reaction kettle, and standing for 50-90 hours.
(3) After the reaction is started, the first stage mainly takes nucleation as the main, the pH value is 11.70-11.90, the ammonia value is 5-6 g/L, and the duration is 0.1-0.5 h, and then the second stage enters a nuclear growth stage, and the pH value is adjusted to 10.7-10.8, and the ammonia value is 5-6 g/L.
(4) In the growth stage of the step (3), air is introduced at a rate of 1.1 μm500L/min, the input of which is 6.0m3When D50 reached 4.0. mu.m, the reaction was stopped.
(5) And washing, drying and removing iron from the synthesized nickel-cobalt-manganese hydroxide to obtain a final product.
Comparative example 2
Low sodium sulfur Ni0.6Co0.2Mn0.2(OH)2The ternary precursor, D50, was 4.0 μm, the S content was 1150ppm, the Na content was 70ppm, and it was prepared as follows:
(1) according to Ni0.6Co0.2Mn0.2(OH)2Preparing a salt solution according to the molar ratio of medium nickel, cobalt and manganese, wherein the total concentration is 2.0 mol/L; the concentration of the prepared alkali liquor is 10mol/L, and the concentration of the prepared ammonia water is 20%.
(2) Adding 1000-4000L of pure water as a base solution before starting up, adjusting the pH value of the base solution to 11.70-11.90 and the ammonia value to 5-6 g/L, stirring at a rotating speed of 150rpm and a temperature of 55 ℃, simultaneously adding the nickel-cobalt-manganese salt solution, the sodium hydroxide solution and the ammonia water into the reaction kettle, and standing for 50-90 hours.
(3) After the reaction is started, the first stage mainly takes nucleation as the main, the pH value is 11.70-11.90, the ammonia value is 5-6 g/L, and the duration is 0.1-0.5 h, and then the second stage enters a nuclear growth stage, and the pH value is adjusted to 10.7-10.8, and the ammonia value is 5-6 g/L.
(4) In the growth stage of the step (3), air is introduced at a rate of 10L/min and an introduction amount of 0.1m when the particle size reaches 1.1 μm3When D50 reached 4.0. mu.m, the reaction was stopped.
(5) And washing, drying and removing iron from the synthesized nickel-cobalt-manganese hydroxide to obtain a final product.
As can be seen from example 1 and comparative example 1, when the amount of the oxidizing gas is excessively increased, primary crystal grains are delaminated and the crystal grains are dislocated and stacked, resulting in a change in morphology of the primary particles from "plate-like" to "rib-like".
It can be seen from example 1 and comparative example 2 that sodium sulfur of the product cannot be improved when the supply of the oxidizing gas is insufficient.

Claims (10)

1. A preparation method of a nickel-cobalt-manganese ternary precursor is characterized by comprising the following steps:
1) preparing a mixed salt solution by using nickel, cobalt and manganese soluble salts as raw materials and pure water;
2) adding the mixed salt solution, alkali liquor and ammonia water into a reaction kettle, controlling the temperature, the rotating speed, the ammonia value and the residence time, wherein the reaction is divided into a first stage with a high pH value and a second stage with a low pH value, the first stage is mainly crystal nucleation, the second stage is mainly crystal growth, and oxidizing gas is introduced when the second stage reacts until the granularity of crystals is 1.1-3.0 mu m until the D50 of the slurry reaches a set range;
the pH value of the high pH value is 11.60-12.60, and the pH value of the low pH value is 10.4-11.40;
3) washing and drying the slurry synthesized in the step 2) to obtain the low-sodium-sulfur nickel-cobalt-manganese ternary precursor.
2. The method of claim 1, wherein the formula of the nickel-cobalt-manganese ternary precursor is NixCoyMnz(OH)2Wherein x + y + z is 1, x is more than 0.2 and less than 0.90, y is more than 0.1 and less than 0.3, and z is more than 0.1 and less than 0.3.
3. The method for preparing the nickel-cobalt-manganese ternary precursor according to claim 1 or 2, wherein in step 1), the soluble salts of nickel, cobalt and manganese are sulfates, chlorides or nitrates of nickel, cobalt and manganese.
4. The method for preparing the nickel-cobalt-manganese ternary precursor according to claim 1 or 2, wherein in the step 2), the total concentration of the mixed salt solution is 1.5-2.5 mol/L, the concentration of the alkali solution is 8.0-12.0 mol/L, and the concentration of the ammonia water is 15-25%.
5. The method for preparing the nickel-cobalt-manganese ternary precursor according to claim 1 or 2, wherein in the step 2), the temperature is 50-65 ℃, the rotation speed is 100-300 rpm, the ammonia value is 4-9 g/L, and the retention time is 30-130 h.
6. The method for preparing the nickel-cobalt-manganese ternary precursor according to claim 1 or 2, wherein the introduced oxidizing gas in the step 2) is oxygen or a mixed gas including oxygen.
7. The method for preparing the nickel-cobalt-manganese ternary precursor according to claim 1 or 2, wherein in the step 2), the rate of introducing the oxidizing gas is 0.1 to 50L/min, and the total amount of introducing the oxidizing gas is 0.2 to 1.0m3The rate and total amount of feed are based on the oxygen in the oxidizing gas.
8. The method for preparing the nickel-cobalt-manganese ternary precursor according to claim 1 or 2, wherein in the step 2), D50 of the slurry is set to be 2 to 5 μm.
9. The method for preparing the nickel-cobalt-manganese ternary precursor according to claim 1 or 2, wherein the prepared nickel-cobalt-manganese ternary precursor has an S content of 800ppm or less and an Na content of 50ppm or less.
10. The nickel-cobalt-manganese ternary precursor prepared by the preparation method of any one of claims 1 to 7 is characterized in that the nickel-cobalt-manganese ternary precursor D50 is 2.0-5.0 μm, the S content is less than or equal to 800ppm, and the Na content is less than or equal to 50 ppm.
CN202111285076.XA 2021-11-01 2021-11-01 Nickel-cobalt-manganese ternary precursor and preparation method thereof Pending CN114044542A (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN115072804A (en) * 2022-07-08 2022-09-20 金驰能源材料有限公司 Method for regulating and controlling XRD diffraction intensity ratio of crystal faces of precursor (101) and precursor (001)
CN115286050A (en) * 2022-08-05 2022-11-04 宁波容百新能源科技股份有限公司 Ternary precursor material and preparation method thereof

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CN107611383A (en) * 2017-08-25 2018-01-19 浙江华友钴业股份有限公司 A kind of preparation method of the nickel-cobalt-manganese ternary presoma of low-sulfur high-tap density
CN111170375A (en) * 2020-01-07 2020-05-19 万华化学集团股份有限公司 Ternary positive electrode material precursor and preparation method thereof
CN111732132A (en) * 2020-07-06 2020-10-02 金驰能源材料有限公司 Nickel-cobalt-manganese core-shell structure precursor, preparation method thereof and positive electrode material
CN113415830A (en) * 2021-08-24 2021-09-21 金驰能源材料有限公司 Preparation method of lithium ion battery anode material precursor

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Publication number Priority date Publication date Assignee Title
CN107611383A (en) * 2017-08-25 2018-01-19 浙江华友钴业股份有限公司 A kind of preparation method of the nickel-cobalt-manganese ternary presoma of low-sulfur high-tap density
CN111170375A (en) * 2020-01-07 2020-05-19 万华化学集团股份有限公司 Ternary positive electrode material precursor and preparation method thereof
CN111732132A (en) * 2020-07-06 2020-10-02 金驰能源材料有限公司 Nickel-cobalt-manganese core-shell structure precursor, preparation method thereof and positive electrode material
CN113415830A (en) * 2021-08-24 2021-09-21 金驰能源材料有限公司 Preparation method of lithium ion battery anode material precursor

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115072804A (en) * 2022-07-08 2022-09-20 金驰能源材料有限公司 Method for regulating and controlling XRD diffraction intensity ratio of crystal faces of precursor (101) and precursor (001)
CN115072804B (en) * 2022-07-08 2024-02-02 金驰能源材料有限公司 Method for regulating XRD diffraction intensity ratio of precursor (101) and (001) crystal faces
CN115286050A (en) * 2022-08-05 2022-11-04 宁波容百新能源科技股份有限公司 Ternary precursor material and preparation method thereof

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