CN114291850A - Method for controlling morphology of ternary precursor in preparation process of ternary precursor - Google Patents
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Abstract
The invention discloses a method for controlling the morphology of a ternary precursor in the preparation process of the ternary precursor, which comprises the steps of introducing a metal salt solution, a complexing agent solution, a precipitator solution and a required atmosphere into a reaction kettle I, and carrying out coprecipitation reaction to prepare a ternary precursor crystal nucleus for later use, wherein the particle size of the crystal nucleus is D90/3 SPAN-D90/2 SPAN; and (3) introducing a metal salt solution, a complexing agent solution, a precipitator solution and a required atmosphere into a reaction kettle II, carrying out coprecipitation reaction, introducing crystal nuclei to continue coprecipitation reaction until the average particle size of the particles grows to 85% -95% of the target particle size, stopping feeding until the particle size D50 is stabilized to the target particle size, and thus obtaining the slurry containing the precursor material. The invention controls the particle size distribution by adjusting the input amount of small particles in the continuous process operation process, thereby ensuring that D50 achieves long-term stability, enabling the pH in the continuous process not to be influenced by the particle size distribution, realizing free adjustment, releasing the parameter linkage effect and enabling each parameter to be used as a means for adjusting the morphology.
Description
Technical Field
The invention relates to a preparation method of a ternary precursor, in particular to a method for controlling the morphology of the ternary precursor in the preparation process of the ternary precursor.
Background
At present, the lithium ion battery occupies a larger market share in the field of wide portable electronic equipment by virtue of the advantages of high specific capacity, long cycle life, low self-discharge rate, no memory effect, environmental friendliness and the like, and is generally recognized as the most development potential power battery for the electric vehicle. The ternary nickel-cobalt-manganese/aluminum cathode material is an important lithium ion battery cathode material, has the important advantages of better performance than lithium cobaltate, lower cost than lithium cobaltate, higher energy density than lithium iron phosphate and the like, and gradually becomes a mainstream cathode material of an automobile power battery. The performances of the lithium ion battery anode material, such as cycle performance, safety stability, energy density and the like, are greatly dependent on the quality and physicochemical properties of the precursor. With the application of lithium ion batteries in the field of electric vehicles, the requirements for the endurance of materials of the lithium ion batteries are gradually increased. Although the current 5 series, 6 series and other middle and low nickel materials still occupy more than half of the markets of ternary materials, the future industry forecast will be 8 series, 9 series and other high nickel materials, and enterprises related to the ternary materials are also arranged in a way of carrying out high nickel synthesis technology.
When the ternary positive electrode material precursor is used for preparing the lithium battery positive electrode material, the prepared lithium battery positive electrode material has better cycle performance when the ternary positive electrode material precursor has uniform granularity and concentrated distribution, and is more suitable for power batteries. In order to better exert the excellent performance of the ternary cathode material, the preparation of the precursor is crucial to the production of the ternary cathode material, and the physical and chemical indexes of the final sintered product are directly determined by the quality (morphology, particle size distribution, specific surface area, impurity content, tap density and the like) of the precursor. The preparation method of the ternary anode material precursor mainly adopts a hydroxide coprecipitation process, and comprises the steps of dissolving raw materials in deionized water, mixing according to a certain molar ratio, and then using NaOH as a precipitator and ammonia water as a complexing agent to prepare the high-density spherical hydroxide precursor. In the synthesis of the ternary precursor, strong linkage relation exists among the parameters, a set of parameters corresponds to the synthesis of a product in the traditional continuous method, and the particle size distribution, the content and the proportion of main elements, the tap density, the specific surface area, the content of impurity elements and the morphological characteristics of the product are all fixed, so that obstacles are brought to the technical development of the precursor.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for controlling the appearance of a ternary precursor in the preparation process, and the method solves the problems that one set of parameters corresponds to the synthesis of one product in the traditional ternary precursor preparation process, and the appearance of the precursor product cannot be flexibly controlled.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for controlling the morphology of a ternary precursor in the preparation process of the ternary precursor comprises the following steps:
(1) preparing a metal salt solution, a precipitator solution and a complexing agent solution, wherein the metal salt solution is an aqueous solution containing nickel salt, cobalt salt, manganese salt or aluminum salt;
(2) introducing a metal salt solution, a complexing agent solution, a precipitator solution and a required atmosphere into a reaction kettle I, and carrying out coprecipitation reaction to prepare a ternary precursor crystal nucleus for later use, wherein the particle size of the crystal nucleus is D90/3 SPAN-D90/2 SPAN;
(3) introducing a metal salt solution, a complexing agent solution, a precipitator solution and a required atmosphere into a reaction kettle II, carrying out coprecipitation reaction, introducing the crystal nucleus obtained in the step (2) to continue coprecipitation reaction when the average particle size of particles grows to 85% -95% of the target particle size, stopping feeding until the particle size D50 is stabilized to the target particle size, and obtaining slurry containing a precursor material;
(4) and (4) stirring the slurry containing the precursor material obtained in the step (3), aging, washing, drying, screening and removing iron to obtain the precursor of the ternary cathode material.
In the step (2), process regulation and control are carried out according to the technological parameters of designing the crystal nucleus structure, and coprecipitation reaction is carried out to prepare a ternary precursor crystal nucleus for later use.
In the step (3), a base solution is prepared according to the process requirements, a metal salt solution, a complexing agent solution, a precipitator solution and a required atmosphere are introduced into a reaction kettle II, process regulation and control are carried out according to process parameters meeting the requirements of a precipitation structure, continuous process synthesis of particles with required particle sizes is carried out, when the average particle size of the particles grows to 85% -95% of the target particle size, crystal nuclei obtained in the step (2) are introduced to regulate the particle size distribution, coprecipitation reaction is continuously carried out until the particle size D50 is stabilized to the target particle size, continuous material receiving can be started, and slurry containing precursor materials is obtained.
Further, when the nickel-cobalt-manganese ternary precursor is prepared, the metal salt solution is an aqueous solution containing nickel salt, cobalt salt and manganese salt, and the molar ratio of the nickel salt to the cobalt salt to the manganese salt is x: y: (1-x-y), wherein x is more than or equal to 0.3 and less than 1.0, y is more than or equal to 0.3 and less than 1.0, and the total concentration of metal ions in the metal salt solution is 0.2-2.5 mol/L; when the nickel-cobalt-aluminum ternary precursor is prepared, the metal salt solution is a mixed salt solution prepared from nickel salt and cobalt salt and an aluminum salt solution prepared from aluminum salt, and the molar ratio of nickel to cobalt to aluminum in the metal salt solution is x: y: (1-x-y), wherein x is more than or equal to 0.8 and less than 1.0, y is more than or equal to 0 and less than 0.2, the total concentration of nickel ions and cobalt ions in the mixed salt solution is 0.2-2.5 mol/L, and the concentration of aluminum ions in the aluminum salt solution is 0.05-0.5 mol/L; the nickel salt, the cobalt salt, the manganese salt and the aluminum salt are at least one of sulfate, nitrate and halogen salt.
Further, the precipitant solution is a sodium hydroxide solution with a mass concentration of 12-35%, and the complexing agent solution is an ammonia water solution with a mass concentration of 1-28%.
Further, in the step (2), the reaction temperature is controlled to be 40-80 ℃, the pH value is 11.0-13.0, the ammonia concentration is 1-17 g/L, and the stirring speed is 500-1200 rpm.
Further, in the step (3), the reaction temperature is controlled to be 40-80 ℃, the pH value is 10.0-12.0, the ammonia concentration is 1-17 g/L, and the stirring speed is 200-1000 rpm.
Further, the feeding amount of the metal salt solution in the step (2) and the step (3) is 1/20-1/10 of the volume of the reaction kettle; the feeding amount of the crystal nucleus per hour is 30-80% of the mass of the particles in the reaction kettle II. The mode of stabilizing the particle diameter D50 is adjusted by controlling the amount of the crystal nuclei introduced.
Further, the average particle size of the particles in the step (3) is a particle size distribution D50 value, and the target particle size is 4-20 μm.
Further, the crystal nucleus in the step (3) is introduced in the form of one or combination of a plurality of forms of manual feeding, mechanical feeding and automatic feeding; the crystal nucleus is introduced in one or a combination of a plurality of modes of slurry input, wet material input and dry material input.
Further, the atmosphere in the step (2) and the step (3) is one or more of air, oxygen, nitrogen, helium and argon.
In the conventional continuous process method, the reaction temperature, the feeding concentration, the feeding flow, the stirring speed and the ammonia-nickel ratio need to be determined preferentially, the pH is adjusted by combining the growth acceleration and the growth rate of the granularity in the reaction process, and the balance between the particle growth rate and the nucleation rate is controlled, so that the long-term stability of D50 in the process operation process is ensured, and the continuous and stable output of the product slurry is realized. The invention controls the particle size distribution by adjusting the input amount of small particles in the continuous process operation process, thereby ensuring that D50 achieves long-term stability, enabling the pH in the continuous process not to be influenced by the particle size distribution, realizing free adjustment, releasing the parameter linkage effect and enabling each parameter to be used as a means for adjusting the morphology. The morphology determines the performance, the higher the consistency of the morphology of the particles is, the more consistent the performance is, the smaller the "erosion point" effect is, the risk of local structural collapse caused by the transition output of the performance of a certain point in the particles can be reduced, and thus the electrochemical performance of the final material is improved.
The invention has the beneficial effects that: according to the method for controlling the morphology of the ternary precursor in the preparation process, the input quantity of small particles in the continuous process operation process is adjusted to control the particle size distribution, so that the long-term stability of D50 is ensured, the pH is not influenced by the particle size distribution in the continuous process, the free adjustment is realized, the parameter linkage effect can be liberated, and each parameter can be used as a means for morphology adjustment.
Drawings
FIG. 1 shows the morphology of a sample prepared in example 1 of the present invention under an electron microscope;
FIG. 2 is an electron microscope image of a sample prepared in comparative example 1 of the present invention;
FIG. 3 is an electron microscope image of a sample prepared in example 2 of the present invention;
FIG. 4 shows the morphology of a sample prepared in comparative example 2 according to the present invention under an electron microscope.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
using deionized water to mix nickel sulfate, cobalt sulfate and manganese sulfate according to the proportion of Ni: co: preparing a metal mixed salt solution with the Mn of 55:05:40 of 2mol/L, preparing a solution with the concentration of 10mol/L by using deionized water for sodium hydroxide, and diluting an ammonia water solution to the concentration of 10 mol/L.
Opening a 100L small particle reaction kettle, adding 50L of base solution, opening and stirring at the stirring speed of 900rpm, opening a mold temperature controller connected with a small particle reaction kettle jacket, heating the solution in the reaction kettle to 60 ℃, and keeping the temperature constant; introducing nitrogen flow of 2L/min into the reaction kettle for 2 hours, adding 10mol/L NaOH solution to adjust the pH of the base solution to 11.85, and adding 10mol/L ammonia water solution to adjust the ammonia concentration to 0.25 mol/L. After the adjustment is finished, starting salt, alkali and ammonia feeding pumps to continuously feed, controlling the feeding flow rates to be 2L/h, 0.5L/h and 100mL/h respectively, controlling the reaction pH to be 11.80-11.90 and the ammonia concentration to be 0.2-0.3 mol/L in the process, controlling the particle D50 to be 1.8-2.4 mu m, continuously feeding, performing sphericity optimization by using a thickener, and maintaining the particle size to slowly grow the dao crystal nucleus small particles. The method comprises the steps of reconfiguring a base solution by using a continuous reaction kettle, adjusting parameters to a required range, controlling the pH of the reaction to be 11.40-11.50, controlling the ammonia concentration to be 0.2-0.3 mol/L, connecting the small-particle reaction kettle and the continuous reaction kettle by using a feed pump when the particle size grows to be 3.3 mu m, starting the feed pump, controlling the addition amount of crystal nuclei to be (20-60) g/h, controlling the particle size D50 to be stable at 3.8-4.0 mu m, starting material collection, periodically carrying out continuous material treatment, pulping for 30min by using a 70 ℃ 1mol/L NaOH solution with the temperature 5 times that of the solid obtained by separation, and carrying out solid-liquid separation. Then washing with hot water of 80 ℃ until the impurity content reaches the standard. And drying in an oven at 140 ℃ for 16h to obtain the product.
Example 2:
using deionized water to mix nickel sulfate, cobalt sulfate and manganese sulfate according to the proportion of Ni: co: preparing a metal mixed salt solution with the Mn of 80:10:10 of 2mol/L, preparing sodium hydroxide into a solution with the concentration of 10mol/L by using deionized water, and diluting an ammonia water solution to the concentration of 10 mol/L.
Opening a 100L reaction kettle, adding 50L base solution, opening and stirring at the stirring speed of 900rpm, opening a mold temperature controller connected with a small particle reaction kettle jacket, heating the solution in the small particle reaction kettle to 60 ℃, and keeping the temperature constant. Introducing nitrogen flow of 2L/min into a reaction kettle for 2 hours continuously, adding 10mol/L NaOH solution to adjust the pH of a base solution to 11.55, adding 10mol/L ammonia water solution to adjust the ammonia concentration to 0.25mol/L, opening a salt, alkali and ammonia feeding pump to continuously feed after the adjustment is finished, controlling the feeding flow to be 2L/h, 0.5L/h and 100mL/h respectively, controlling the reaction pH to be 11.50-11.60 in the initial process, controlling the ammonia concentration to be 0.1-0.2 mol/L, controlling the crystal nucleus small particles D50 to be 3.0-4.5 mu m, continuously feeding, and optimizing the sphericity by using a thickener to maintain the slow growth of the particle size. The method comprises the steps of reconfiguring a base solution by adopting a continuous reaction kettle, adjusting parameters to a required range, controlling the pH value of the reaction to be 11.10-11.20, controlling the ammonia concentration to be 0.1-0.2 mol/L, connecting a small particle kettle and the continuous kettle by using a feeding pump when the particle size grows to 9.5 mu m, starting the feeding pump, controlling the crystal nucleus addition amount to be (20-60) g/h, controlling the particle size to be stabilized at 9.5-10.5 mu m, and starting material collection. The continuous material treatment is carried out regularly, pulping is carried out for 30min by using NaOH solution with the temperature of 70 ℃ and the concentration of 1mol/L, wherein the NaOH solution is 5 times of the solid obtained by separation, and the solid and the liquid are separated. Then washing with hot water of 80 ℃ until the impurity content reaches the standard, and drying in an oven of 120 ℃ for 24h to obtain the product.
Comparative example 1:
using deionized water to mix nickel sulfate, cobalt sulfate and manganese sulfate according to the proportion of Ni: co: preparing a metal mixed salt solution with the Mn of 55:05:40 of 2mol/L, preparing a solution with the concentration of 10mol/L by using deionized water for sodium hydroxide, and diluting an ammonia water solution to the concentration of 10 mol/L.
Opening a 100L reaction kettle, adding 50L base solution, opening and stirring at the stirring speed of 900rpm, opening a mold temperature machine connected with a reaction kettle jacket, heating the solution in the reaction kettle to 60 ℃, and keeping the temperature constant; introducing nitrogen flow of 2L/min into the reaction kettle for 2 hours, adding 10mol/L NaOH solution to adjust the pH of the base solution to 11.85, and adding 10mol/L ammonia water solution to adjust the ammonia concentration to 0.25 mol/L. After the adjustment is finished, a salt, alkali and ammonia feeding pump is started to continuously feed materials, the feeding flow rates are controlled to be 2L/h, 0.5L/h and 100mL/h respectively, the reaction pH is controlled to be 11.80-11.90 in the initial reaction process, the ammonia concentration is 0.2-0.3 mol/L, when the particle size grows to 3.8 mu m, the pH is gradually increased to 12.0-12.1, the particle size is controlled to be stable at 3.8-4.0 mu m, material collection is started, continuous material treatment is periodically performed, 5 times of the separated solid amount of a 70 ℃ 1MNaOH solution is used for pulping for 30min, and solid-liquid separation is performed. Then washing with hot water of 80 ℃ until the impurity content reaches the standard. And drying in an oven at 140 ℃ for 16h to obtain the product.
Comparative example 2:
using deionized water to mix nickel sulfate, cobalt sulfate and manganese sulfate according to the proportion of Ni: co: preparing a metal mixed salt solution with the Mn of 80:10:10 of 2mol/L, preparing sodium hydroxide into a solution with the concentration of 10mol/L by using deionized water, and diluting an ammonia water solution to the concentration of 10 mol/L.
Opening a 100L reaction kettle, adding 50L base solution, opening and stirring at the stirring speed of 900rpm, opening a mold temperature machine connected with a jacket of the reaction kettle, heating the solution in the reaction kettle to 60 ℃, and keeping the temperature constant. Introducing nitrogen flow of 2L/min into a reaction kettle for 2 hours continuously, adding 10mol/L NaOH solution to adjust the pH of a base solution to 11.25, adding 10mol/L ammonia water solution to adjust the ammonia concentration to 0.25mol/L, opening a salt, alkali and ammonia feeding pump to continuously feed after the adjustment is finished, controlling the feeding flow to be 2L/h, 0.5L/h and 100mL/h respectively, controlling the reaction pH to be 11.20-11.30 in the initial process, controlling the ammonia concentration to be 0.1-0.2 mol/L, gradually increasing the pH to 11.50-11.60 when the particle size grows to 9.5 mu m, controlling the particle size to be stable at 9.5-10.5 mu m, and starting to collect materials. The continuous material treatment is carried out regularly, pulping is carried out for 30min by using NaOH solution with the temperature of 70 ℃ and the concentration of 1mol/L, wherein the NaOH solution is 5 times of the solid obtained by separation, and the solid and the liquid are separated. Then washing with hot water of 80 ℃ until the impurity content reaches the standard, and drying in an oven of 120 ℃ for 24h to obtain the product.
Claims (9)
1. A method for controlling the morphology of a ternary precursor in a preparation process of the ternary precursor is characterized by comprising the following steps of:
(1) preparing a metal salt solution, a precipitator solution and a complexing agent solution, wherein the metal salt solution is an aqueous solution containing nickel salt, cobalt salt, manganese salt or aluminum salt;
(2) introducing a metal salt solution, a complexing agent solution, a precipitator solution and a required atmosphere into a reaction kettle I, and carrying out coprecipitation reaction to prepare a ternary precursor crystal nucleus for later use, wherein the particle size of the crystal nucleus is D90/3 SPAN-D90/2 SPAN;
(3) introducing a metal salt solution, a complexing agent solution, a precipitator solution and a required atmosphere into a reaction kettle II, carrying out coprecipitation reaction, introducing the crystal nucleus obtained in the step (2) to continue coprecipitation reaction when the average particle size of particles grows to 85% -95% of the target particle size, stopping feeding until the particle size D50 is stabilized to the target particle size, and obtaining slurry containing a precursor material;
(4) and (4) stirring the slurry containing the precursor material obtained in the step (3), aging, washing, drying, screening and removing iron to obtain the precursor of the ternary cathode material.
2. The method of claim 1 for controlling the morphology of ternary precursors during their preparation, wherein: when the nickel-cobalt-manganese ternary precursor is prepared, the metal salt solution is an aqueous solution containing nickel salt, cobalt salt and manganese salt, and the molar ratio of the nickel salt to the cobalt salt to the manganese salt is x: y: (1-x-y), wherein x is more than or equal to 0.3 and less than 1.0, y is more than or equal to 0.3 and less than 1.0, and the total concentration of metal ions in the metal salt solution is 0.2-2.5 mol/L; when the nickel-cobalt-aluminum ternary precursor is prepared, the metal salt solution is a mixed salt solution prepared from nickel salt and cobalt salt and an aluminum salt solution prepared from aluminum salt, and the molar ratio of nickel to cobalt to aluminum in the metal salt solution is x: y: (1-x-y), wherein x is more than or equal to 0.8 and less than 1.0, y is more than or equal to 0 and less than 0.2, the total concentration of nickel ions and cobalt ions in the mixed salt solution is 0.2-2.5 mol/L, and the concentration of aluminum ions in the aluminum salt solution is 0.05-0.5 mol/L; the nickel salt, the cobalt salt, the manganese salt and the aluminum salt are at least one of sulfate, nitrate and halogen salt.
3. The method of claim 1 for controlling the morphology of ternary precursors during their preparation, wherein: the precipitator solution is a sodium hydroxide solution with the mass concentration of 12-35%, and the complexing agent solution is an ammonia water solution with the mass concentration of 1-28%.
4. The method of claim 1 for controlling the morphology of ternary precursors during their preparation, wherein: in the step (2), the reaction temperature is controlled to be 40-80 ℃, the pH value is 11.0-13.0, the ammonia concentration is 1-17 g/L, and the stirring speed is 500-1200 rpm.
5. The method of claim 1 for controlling the morphology of ternary precursors during their preparation, wherein: in the step (3), the reaction temperature is controlled to be 40-80 ℃, the pH value is 10.0-12.0, the ammonia concentration is 1-17 g/L, and the stirring speed is 200-1000 rpm.
6. The method of claim, wherein the morphology of the ternary precursor is controlled during its preparation, and wherein: the feeding amount of the metal salt solution in the step (2) and the step (3) is 1/20-1/10 of the volume of the reaction kettle; the feeding amount of the crystal nucleus per hour is 30-80% of the mass of the particles in the reaction kettle II.
7. The method of claim 1 for controlling the morphology of ternary precursors during their preparation, wherein: the average particle size of the particles in the step (3) is a particle size distribution D50 value, and the target particle size is 4-20 μm.
8. The method of claim 1, wherein the morphology of the ternary precursor is controlled during its preparation, and wherein: the crystal nucleus is introduced in the step (3) in the form of one or combination of a plurality of forms of manual feeding, mechanical feeding and automatic feeding; the crystal nucleus is introduced in one or a combination of a plurality of modes of slurry input, wet material input and dry material input.
9. The method of claim 1, wherein the morphology of the ternary precursor is controlled during its preparation, and wherein: and (3) requiring one or more of air, oxygen, nitrogen, helium and argon to be in the atmosphere.
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| CN114804234A (en) * | 2022-05-18 | 2022-07-29 | 宁夏中化锂电池材料有限公司 | NCM/NCA core-shell structure ternary precursor material and preparation method thereof |
| CN115285959A (en) * | 2022-07-06 | 2022-11-04 | 宜宾天原海丰和泰有限公司 | Low-cost continuous production method of iron phosphate |
| CN115974174A (en) * | 2022-12-07 | 2023-04-18 | 宜宾光原锂电材料有限公司 | Sodium ion battery positive electrode material precursor and preparation method thereof |
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