CN112441627A - Method for inhibiting twin crystals of nickel-cobalt-manganese ternary precursor - Google Patents
Method for inhibiting twin crystals of nickel-cobalt-manganese ternary precursor Download PDFInfo
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- C01G53/00—Compounds of nickel
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- 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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- 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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Abstract
The invention discloses a method for inhibiting a nickel-cobalt-manganese ternary precursor twin crystal, which comprises the following steps: respectively preparing a nickel-cobalt-manganese ternary solution, liquid caustic soda, an ammonia water solution and a water-soluble dispersant solution; adding pure water, an ammonia water solution and liquid caustic soda into a reaction kettle to prepare a base solution, introducing nitrogen into the reaction kettle added with the base solution, and heating the reaction kettle added with the base solution; adding the nickel-cobalt-manganese ternary solution, liquid alkali, an ammonia water solution and a water-soluble dispersant solution into a reaction kettle with a base solution in a parallel flow mode, starting the reaction kettle with the base solution to stir, discharging the obtained nickel-cobalt-manganese ternary precursor crude product with the target particle size into an ageing tank, washing and removing impurities, dehydrating, drying, mixing, screening, removing iron and packaging to obtain the nickel-cobalt-manganese ternary precursor finished product. The invention can reduce the generation of precursor twin crystal, and the prepared ternary precursor has uniform particles, good sphericity, no obvious twin crystal interface in the appearance of secondary particles and no microcrack.
Description
Technical Field
The invention belongs to the field of synthesis of new energy battery material precursors, and particularly relates to a method for inhibiting twin crystals of a nickel-cobalt-manganese ternary precursor.
Background
The nickel-cobalt-manganese ternary precursor is the most important raw material for preparing the lithium ion battery anode material, and the main preparation method of the ternary precursor is that a nickel-cobalt-manganese metal salt solution, liquid caustic soda and ammonia water are simultaneously added into a reaction kettle for coprecipitation reaction, twin crystals (the twin crystals refer to crystals with mirror symmetry orientation relation formed by two crystals along a common crystal face and are called twin crystal faces) are usually generated in the process of nucleation of the coprecipitation reaction, ellipsoidal or multi-head-shaped particle appearance secondary particles are formed in the process of gradual growth of the twin crystal nuclei, the existence of the twin crystals aggravates the anisotropy of lattice expansion and shrinkage among crystal grains, microcracks are generated on the twin crystal faces, and the microcracks are inherited to the anode material prepared by the precursor. The contact of the anode material containing the microcracks and the electrolyte can aggravate the side reaction of the anode material and the electrolyte, so that the battery has serious capacity attenuation, and the existence of twin crystals can also make the gaps among the anode material particles larger, so that higher compaction density is difficult to obtain, and the volume energy density of the battery is lower.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for inhibiting the Ni-Co-Mn ternary precursor twin crystal, which can reduce the generation of precursor twin crystal, and the prepared ternary precursor has uniform particles, good sphericity, no obvious twin crystal interface on the appearance of secondary particles and no microcrack.
The invention adopts the following technical scheme:
a method for inhibiting twins of a nickel-cobalt-manganese ternary precursor is characterized by comprising the following steps:
(1) respectively preparing a nickel-cobalt-manganese ternary solution, liquid alkali, an ammonia water solution and a water-soluble dispersant solution, wherein the concentration of the nickel-cobalt-manganese ternary solution is 80-120 g/L, and the mass fraction of the water-soluble dispersant solution is 30-60%;
(2) adding pure water, an ammonia water solution and liquid caustic soda into a reaction kettle to prepare a base solution with the pH of 10.2-11.8, the ammonia concentration of 8.5-10.5 g/L and the total alkalinity of 20-28 g/L, introducing nitrogen into the reaction kettle added with the base solution, and heating the reaction kettle added with the base solution to 50-70 ℃;
(3) adding the nickel-cobalt-manganese ternary solution, liquid alkali, an ammonia water solution and a water-soluble dispersant solution into a reaction kettle added with a base solution in a parallel flow mode, and stirring the reaction kettle added with the base solution to obtain a nickel-cobalt-manganese ternary precursor crude product with a target particle size;
(4) discharging the nickel-cobalt-manganese ternary precursor crude product with the target particle size into an aging tank, washing, removing impurities, dehydrating, drying, mixing, screening, removing iron, and packaging to obtain a nickel-cobalt-manganese ternary precursor finished product.
The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal is characterized in that the water-soluble dispersant solution in the step (1) is one or more of sodium dodecyl sulfate, coconut diethanolamide, methyl high hydrogen silicone oil emulsion and hydroxyl silicone oil emulsion.
The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal is characterized in that in the step (1), the mass fraction of the liquid caustic soda is 30-40%, and the mass fraction of the ammonia water solution is 15-25%.
The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal is characterized in that the flow of nitrogen introduced into the reaction kettle with the base solution in the step (2) is 0.5m3/h～2.0m3/h。
The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal is characterized in that in the step (3), the flow rate of adding the nickel-cobalt-manganese ternary solution into the reaction kettle with the base solution is 200-600L/h, the flow rate of adding the liquid alkali into the reaction kettle with the base solution is 80-220L/h, the flow rate of adding the ammonia water solution into the reaction kettle with the base solution is 25-65L/h, and the flow rate of adding the water-soluble dispersant solution into the reaction kettle with the base solution is 10-30L/h; the stirring speed of the reaction kettle added with the base solution is 120 rpm-240 rpm.
The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal is characterized in that the addition amount of the base solution in the reaction kettle in the step (3) is 60-75% of the volume of the reaction kettle.
The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal is characterized in that the target median diameter of the nickel-cobalt-manganese ternary precursor coarse product with the target particle diameter in the step (3) is 10-15 mu m.
The invention has the beneficial technical effects that: according to the invention, a proper amount of water-soluble dispersant is added in the process of preparing the nickel-cobalt-manganese ternary cathode material precursor, so that the dispersibility of secondary particles of the precursor in a reaction system is increased, the generation of twin crystals of the precursor can be reduced, the added dispersant is an environment-friendly dispersant, the dispersant plays a role in dispersing particles only in a reaction stage, and can be removed in a washing stage, so that the environment is not polluted, and the physicochemical indexes of the product are not influenced. The ternary precursor prepared by the invention has uniform particles, good sphericity, no obvious twin crystal interface in the appearance of secondary particles and no microcrack.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Referring to fig. 1, the method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal of the invention comprises the following steps:
(1) respectively preparing a nickel-cobalt-manganese ternary solution, liquid alkali, an ammonia water solution and a water-soluble dispersant solution, wherein the concentration of the nickel-cobalt-manganese ternary solution is 80-120 g/L, the mass fraction of the water-soluble dispersant solution is 30-60%, the mass fraction of the liquid alkali is 30-40%, and the mass fraction of the ammonia water solution is 15-25%. The water-soluble dispersant solution is one or more of sodium dodecyl sulfate, coconut diethanolamide, methyl high hydrogen silicone oil emulsion and hydroxyl silicone oil emulsion.
(2) Adding 4.0-4.5 m of the mixture into a reaction kettle3Preparing a base solution with pH of 10.2-11.8, ammonia concentration of 8.5-10.5 g/L and total alkalinity of 20-28 g/L by using pure water, 200-400L of ammonia water solution and 30-60L of liquid alkali, introducing nitrogen into a reaction kettle added with the base solution, wherein the flow rate of introducing the nitrogen into the reaction kettle added with the base solution is 0.5m3/h～2.0m3H is used as the reference value. Heating the reaction kettle added with the base solution to 50-70 ℃;
(3) adding the nickel-cobalt-manganese ternary solution, liquid alkali, an ammonia water solution and a water-soluble dispersant solution into a reaction kettle with a base solution in a parallel flow mode, wherein the adding amount of the base solution in the reaction kettle is 60-75% of the volume of the reaction kettle. And starting the reaction kettle added with the base solution to stir at the stirring speed of 120-240 rpm to obtain a nickel-cobalt-manganese ternary precursor crude product with the target median diameter of 10-15 mu m, and stopping feeding. The flow rate of adding the nickel-cobalt-manganese ternary solution into the reaction kettle added with the base solution is 200L/h-600L/h, the flow rate of adding the liquid caustic soda into the reaction kettle added with the base solution is 80L/h-220L/h, the flow rate of adding the ammonia water solution into the reaction kettle added with the base solution is 25L/h-65L/h, and the flow rate of adding the water-soluble dispersant solution into the reaction kettle added with the base solution is 10L/h-30L/h.
(4) Discharging the nickel-cobalt-manganese ternary precursor crude product with the target particle size into an aging tank, washing, removing impurities, dehydrating, drying, mixing, screening, removing iron, and packaging to obtain a nickel-cobalt-manganese ternary precursor finished product.
Example 1
Respectively preparing a nickel-cobalt-manganese ternary solution with the concentration of 80g/L, liquid caustic soda with the mass fraction of 30%, an ammonia water solution with the mass fraction of 15% and a water-soluble dispersant solution with the mass fraction of 30%. The water-soluble dispersant solution is a mixture formed by lauryl sodium sulfate and hydroxyl silicone oil emulsion, and the molar ratio of the lauryl sodium sulfate to the hydroxyl silicone oil is 1: 2.
To 6.5m3Adding 4.0m into the reaction kettle3Preparing pure water, 200L of 15% ammonia water solution by mass fraction and 30L of 30% liquid alkali into base solution with pH of 10.2, ammonia concentration of 8.5g/L and total alkalinity of 20g/L, introducing nitrogen into the reaction kettle with the base solution, wherein the flow rate of introducing the nitrogen into the reaction kettle with the base solution is 0.5m3H is used as the reference value. The reaction kettle with the added base solution was heated to 50 ℃.
Respectively adding the nickel-cobalt-manganese ternary solution, the liquid caustic soda, the ammonia water solution and the water-soluble dispersant solution into a reaction kettle added with the base solution in parallel flow at the flow rates of 200L/h, 80L/h, 25L/h and 10L/h through a flowmeter, starting stirring the reaction kettle added with the base solution at the stirring speed of 120rpm and the reaction temperature of 50 ℃ until particles grow up.
And when the particle D50 reaches 10.0 mu m, stopping feeding to obtain a nickel-cobalt-manganese ternary precursor crude product with the target particle size. Discharging the nickel-cobalt-manganese ternary precursor crude product with the target particle size into an aging tank, washing, removing impurities, dehydrating, drying, mixing, screening, removing iron, and packaging to obtain a nickel-cobalt-manganese ternary precursor finished product.
Example 2
Respectively preparing 100g/L of nickel-cobalt-manganese ternary solution, 32% of liquid alkali, 16% of ammonia water solution and 35% of water-soluble dispersant solution. The water-soluble dispersant solution is a mixture formed by lauryl sodium sulfate and hydroxyl silicone oil emulsion, and the molar ratio of the lauryl sodium sulfate to the hydroxyl silicone oil is 1: 2.
To 6.5m3Adding 4.2m into a reaction kettle3Preparing pure water, 230L of 16% ammonia water solution and 55L of 32% liquid alkali into base solution with pH of 11.0, ammonia concentration of 10.4g/L and total alkalinity of 24g/L, and addingIntroducing nitrogen into the reaction kettle added with the base solution, wherein the flow of the nitrogen introduced into the reaction kettle added with the base solution is 1.5m3H is used as the reference value. The reaction kettle with the added base solution was heated to 55 ℃.
Respectively adding the nickel-cobalt-manganese ternary solution, the liquid caustic soda, the ammonia water solution and the water-soluble dispersant solution into a reaction kettle added with the base solution in parallel flow at the flow rates of 380L/h, 115L/h, 38L/h and 13L/h through a flowmeter, starting stirring the reaction kettle added with the base solution at the stirring speed of 180rpm and the reaction temperature of 55 ℃ until particles grow up.
And when the particle D50 reaches 13.0 mu m, stopping feeding to obtain a nickel-cobalt-manganese ternary precursor crude product with the target particle size. Discharging the nickel-cobalt-manganese ternary precursor crude product with the target particle size into an aging tank, washing, removing impurities, dehydrating, drying, mixing, screening, removing iron, and packaging to obtain a nickel-cobalt-manganese ternary precursor finished product.
Example 3
Respectively preparing a nickel-cobalt-manganese ternary solution with the concentration of 120g/L, liquid caustic soda with the mass fraction of 40%, an ammonia water solution with the mass fraction of 25% and a water-soluble dispersant solution with the mass fraction of 60%. The water-soluble dispersant solution is a mixture formed by lauryl sodium sulfate and hydroxyl silicone oil emulsion, and the molar ratio of the lauryl sodium sulfate to the hydroxyl silicone oil is 1: 2.
To 6.5m3Adding 4.5m into the reaction kettle3Preparing pure water, 400L of 25% ammonia water solution by mass fraction and 60L of 40% liquid alkali into base solution with pH of 11.8, ammonia concentration of 10.5g/L and total alkalinity of 28g/L, introducing nitrogen into the reaction kettle with the base solution, wherein the flow rate of introducing the nitrogen into the reaction kettle with the base solution is 2.0m3H is used as the reference value. The reaction kettle with the added base solution was heated to 70 ℃.
Respectively adding the nickel-cobalt-manganese ternary solution, the liquid caustic soda, the ammonia water solution and the water-soluble dispersant solution into a reaction kettle added with the base solution in parallel at the flow rates of 600L/h, 220L/h, 65L/h and 30L/h through a flowmeter, starting the reaction kettle added with the base solution to stir at the stirring speed of 240rpm and the reaction temperature of 70 ℃ until particles grow up.
And when the particle D50 reaches 15.0 mu m, stopping feeding to obtain a nickel-cobalt-manganese ternary precursor crude product with the target particle size. Discharging the nickel-cobalt-manganese ternary precursor crude product with the target particle size into an aging tank, washing, removing impurities, dehydrating, drying, mixing, screening, removing iron, and packaging to obtain a nickel-cobalt-manganese ternary precursor finished product.
Comparative example 1
Respectively preparing 100g/L of nickel-cobalt-manganese ternary solution, 32% of liquid alkali, 16% of ammonia water solution and 5% of water-soluble dispersant solution. The water-soluble dispersant solution is a mixture formed by lauryl sodium sulfate and hydroxyl silicone oil emulsion, and the molar ratio of the lauryl sodium sulfate to the hydroxyl silicone oil is 1: 2.
To 6.5m3Adding 4.2m into a reaction kettle3Preparing pure water, 230L of 16 mass percent ammonia water solution and 55L of 32 mass percent liquid alkali into base solution with the pH of 11.0, the ammonia concentration of 10.4g/L and the total alkalinity of 24g/L, introducing nitrogen into the reaction kettle with the base solution, wherein the flow rate of introducing the nitrogen into the reaction kettle with the base solution is 1.5m3H is used as the reference value. The reaction kettle with the added base solution was heated to 55 ℃.
Respectively adding the nickel-cobalt-manganese ternary solution, the liquid caustic soda, the ammonia water solution and the water-soluble dispersant solution into a reaction kettle added with the base solution in parallel flow at the flow rates of 380L/h, 115L/h, 38L/h and 13L/h through a flowmeter, starting stirring the reaction kettle added with the base solution at the stirring speed of 100rpm and the reaction temperature of 55 ℃ until particles grow up.
And when the particle D50 reaches 13.0 mu m, stopping feeding to obtain a nickel-cobalt-manganese ternary precursor crude product with the target particle size. Discharging the nickel-cobalt-manganese ternary precursor crude product with the target particle size into an aging tank, washing, removing impurities, dehydrating, drying, mixing, screening, removing iron, and packaging to obtain a nickel-cobalt-manganese ternary precursor finished product.
The mass fraction of the water-soluble dispersant solution prepared in the comparative example 1 is 5%, the reaction stirring speed is 100rpm, the reaction stirring speed is lower than the process control range, and the prepared ternary precursor has uneven particles, poor sphericity and obvious twins generated by secondary particles.
Claims (7)
1. A method for inhibiting twins of a nickel-cobalt-manganese ternary precursor is characterized by comprising the following steps:
(1) respectively preparing a nickel-cobalt-manganese ternary solution, liquid alkali, an ammonia water solution and a water-soluble dispersant solution, wherein the concentration of the nickel-cobalt-manganese ternary solution is 80-120 g/L, and the mass fraction of the water-soluble dispersant solution is 30-60%;
(2) adding pure water, an ammonia water solution and liquid caustic soda into a reaction kettle to prepare a base solution with the pH of 10.2-11.8, the ammonia concentration of 8.5-10.5 g/L and the total alkalinity of 20-28 g/L, introducing nitrogen into the reaction kettle added with the base solution, and heating the reaction kettle added with the base solution to 50-70 ℃;
(3) adding the nickel-cobalt-manganese ternary solution, liquid alkali, an ammonia water solution and a water-soluble dispersant solution into a reaction kettle added with a base solution in a parallel flow mode, and stirring the reaction kettle added with the base solution to obtain a nickel-cobalt-manganese ternary precursor crude product with a target particle size;
(4) discharging the nickel-cobalt-manganese ternary precursor crude product with the target particle size into an aging tank, washing, removing impurities, dehydrating, drying, mixing, screening, removing iron, and packaging to obtain a nickel-cobalt-manganese ternary precursor finished product.
2. The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal according to claim 1, wherein the water-soluble dispersant solution in the step (1) is one or more of sodium dodecyl sulfate, coconut diethanolamide, methyl high hydrogen silicone oil emulsion and hydroxyl silicone oil emulsion.
3. The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal according to claim 1 or 2, wherein the mass fraction of the liquid alkali in the step (1) is 30-40%, and the mass fraction of the ammonia water solution is 15-25%.
4. The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal as claimed in claim 2, wherein the flow rate of nitrogen introduced into the reaction kettle with the base solution in the step (2) is 0.5m3/h～2.0m3/h。
5. The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal as claimed in claim 2, wherein the flow rate of the nickel-cobalt-manganese ternary solution added into the reaction kettle with the base solution in the step (3) is 200L/h to 600L/h, the flow rate of the liquid alkali added into the reaction kettle with the base solution is 80L/h to 220L/h, the flow rate of the ammonia water solution added into the reaction kettle with the base solution is 25L/h to 65L/h, and the flow rate of the water-soluble dispersant solution added into the reaction kettle with the base solution is 10L/h to 30L/h; the stirring speed of the reaction kettle added with the base solution is 120 rpm-240 rpm.
6. The method for inhibiting the nickel-cobalt-manganese ternary precursor twin crystal as claimed in claim 5, wherein the amount of the base solution added to the reaction kettle in the step (3) is 60-75% of the volume of the reaction kettle.
7. The method for inhibiting the twinning of the Ni-Co-Mn ternary precursor of claim 5, wherein the target median diameter of the coarse Ni-Co-Mn ternary precursor with the target particle diameter in the step (3) is 10-15 μm.
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Cited By (6)
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| CN113582256A (en) * | 2021-09-28 | 2021-11-02 | 金驰能源材料有限公司 | High-nickel single crystal positive electrode material, precursor thereof and preparation method of precursor |
| CN113651372A (en) * | 2021-10-19 | 2021-11-16 | 金驰能源材料有限公司 | Discontinuous growth preparation method of high-sphericity twinning-particle-free precursor |
| CN114084917A (en) * | 2022-01-24 | 2022-02-25 | 金驰能源材料有限公司 | Nickel-cobalt-manganese ternary precursor with XRD diffraction bifurcation double peak and preparation method thereof |
| CN114477315A (en) * | 2022-02-25 | 2022-05-13 | 荆门市格林美新材料有限公司 | Synthesis method of nickel-cobalt-manganese ternary positive electrode material precursor |
| CN114804232A (en) * | 2022-05-16 | 2022-07-29 | 南通金通储能动力新材料有限公司 | Hollow ternary positive electrode material precursor and preparation method thereof |
| CN115140782A (en) * | 2022-04-27 | 2022-10-04 | 南通金通储能动力新材料有限公司 | Lithium-rich manganese-based positive electrode material precursor with core-shell structure and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101202343A (en) * | 2006-12-15 | 2008-06-18 | 中国电子科技集团公司第十八研究所 | Lithium ion battery positive pole material cobalt nickel oxide manganses lithium and method for making same |
| CN102751485A (en) * | 2012-07-17 | 2012-10-24 | 中国电子科技集团公司第十八研究所 | Preparation method of composite cathode material for lithium ion battery |
| CN103825014A (en) * | 2014-01-09 | 2014-05-28 | 北京理工大学 | Preparation method of lithium ion battery high-voltage cathode material lithium nickel manganese composite oxide |
| CN106892464A (en) * | 2017-03-03 | 2017-06-27 | 北京理工大学 | A kind of preparation method of ternary anode material precursor |
| CN108585065A (en) * | 2018-04-17 | 2018-09-28 | 广东迈纳科技有限公司 | A kind of nickelic ternary anode material precursor and preparation method thereof |
| CN109449435A (en) * | 2018-11-01 | 2019-03-08 | 广东佳纳能源科技有限公司 | The preparation method of semidefinite form positive electrode material precursor and positive electrode material precursor obtained, positive electrode, lithium ion battery and application |
| CN111646521A (en) * | 2020-06-02 | 2020-09-11 | 格林美股份有限公司 | Preparation method of high-dispersity and high-nickel ternary precursor material |
-
2020
- 2020-11-13 CN CN202011272565.7A patent/CN112441627A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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