CN115385399B - Nickel-cobalt-manganese ternary precursor and intermittent preparation process thereof - Google Patents
Nickel-cobalt-manganese ternary precursor and intermittent preparation process thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of lithium ion battery materials, and discloses a nickel-cobalt-manganese ternary precursor and an intermittent preparation method thereof. In the nucleation stage, the pH value and the alkalinity are controlled to obtain crystal nuclei with better dispersibility and sphericity; after the nucleation stage is finished, the precursor material with good sphericity and high compaction density is obtained by entering a growth stage and precisely distributing and controlling the flow. The prepared precursor secondary particles are spherical, the primary particles are laminated, and the thickness of the laminated layers is 50-400 nm; the particle diameter D50 is 2.0-4.0 mu m, and the tap density is 2.0-2.3 g/cm 3 Specific surface area of 5-15 m 2 And/g. The preparation method of the target nickel-cobalt-manganese precursor is realized by means of conventional process parameter adjustment, material separation and the like, and has the advantages of simple process, strong operability and no additional cost.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a nickel-cobalt-manganese ternary precursor and a preparation method thereof.
Background
In the field of hydroxide ternary precursor materials, compared with precursors produced by a continuous process, precursors produced by an intermittent process have the advantages of good particle consistency, strong index adjustability and the like, and can meet more severe application scenes. The intermittent ternary precursor is usually prepared by matching two products with large and small particle sizes, and the two products with large particle sizes have great difference in process adopted by the two products and are required to be prepared independently.
The intermittent large-particle-size ternary precursor has a large proportion in practical application, determines most of the properties of the corresponding positive electrode material, and has wide and deep preparation research. And the preparation research of the intermittent small-particle-size precursor is relatively less. Although the small-particle-size precursor is matched with the large-particle-size precursor in a lower proportion, the small-particle-size precursor still has a great influence on the whole performance of the large-particle-size precursor, for example, the particle size distribution of the small-particle-size precursor determines the micro-powder condition of the positive electrode material to a great extent, and the capacity of the positive electrode material is directly influenced.
At present, research on intermittent small-particle-size precursors in the industry is mainly focused on controllable preparation and parameter adjustment of the small-particle-size precursors, and the controllable preparation research on precursors with smaller particle-size ranges of D50 ranging from 2 mu m to 4 mu m is less. Patent document with the publication number of CN107834064B discloses a high-nickel small-particle-size nickel cobalt manganese hydroxide and a preparation method thereof, wherein the method prepares a small-particle-size ternary precursor by concentrating more small-particle slurry outside a kettle and then growing the slurry, and the contents such as precursor shape regulation and the like are not involved. The patent document with the authority of publication number CN112086616B discloses a preparation method of a large (010) crystal face nickel cobalt manganese or nickel cobalt manganese aluminum layered cathode material, which is characterized in that a large (010) area flaky crystal nucleus is synthesized firstly, and then a large (010) area medium-large particle size precursor is synthesized on the basis, wherein the method is used for regulating and controlling the medium-large particle size (010) face, and the primary particle size of the method is about 3 mu m and is not suitable for precursor products with the particle size of 2-4 mu m.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a small-particle-size nickel-cobalt-manganese ternary precursor with good sphericity, high tap density and high specific surface area and a preparation method thereof.
In order to achieve the above object, the present invention provides the following specific technical solutions.
First, the invention provides a Ni-Co-Mn ternary precursor with a chemical molecular formula of Ni x Co y Mn 1-x-y (OH) 2 Wherein x is more than or equal to 0.70 and less than 1.0, and y is more than or equal to 0 and less than 0.3; the precursor secondary particles are spherical, the primary particles are laminated, and the thickness of the laminated layers is 50-400 nm; the particle diameter D50 of the precursor is 2.0-4.0 mu m, and the tap density is 2.0-2.3 g/cm 3 Specific surface area of 5-15 m 2 /g。
Secondly, the invention provides an intermittent preparation method of the nickel-cobalt-manganese ternary precursor, which comprises the following steps:
(1) Preparing a nickel-cobalt-manganese mixed salt solution, a precipitator solution and a complexing agent solution;
(2) Preparing a reaction kettle bottom solution;
(3) Adding the nickel-cobalt-manganese mixed salt solution prepared in the step (1), the precipitator solution and the complexing agent solution into the bottom solution of the reaction kettle in parallel, and controlling the adding speed of the nickel-cobalt-manganese mixed salt solution to be V 1 The pH value of a system in the reaction kettle is adjusted to 11.0-13.0, and the alkalinity is adjusted to 20-40 g/L; stopping the reaction when the reaction slurry reaches the target granularity D1 to obtain crystal nucleus slurry;
(4) The crystal nucleus slurry is evenly conveyed into N growing kettles, wherein N is a natural number and is more than or equal to 2 and less than or equal to 10; adding the nickel-cobalt-manganese mixed salt solution, the precipitant solution and the complexing agent solution prepared in the step (1) into each growth kettle in parallel; the pH value of the reaction system is regulated to be 10.0-12.0, and the alkalinity is regulated to be 15-30 g/L;
when the N value is 2, the speed of adding the nickel-cobalt-manganese mixed salt solution into each growth kettle is V 2 ；
When N is a natural number and N is more than or equal to 3 and less than or equal to 10, the speed of adding the nickel-cobalt-manganese mixed salt solution into each growth kettle is 2V 2 /N；
(5) Stopping the reaction when the granularity of the reaction slurry in the step (4) reaches the target granularity D2, and obtaining the nickel-cobalt-manganese ternary precursor after aging, solid-liquid separation, washing and drying the solid phase of the reaction slurry.
Further, in some preferred embodiments of the present invention, the nickel, cobalt, manganese salt of the nickel cobalt manganese mixed salt solution is at least one of sulfate, nitrate, chloride salt.
Further, the total concentration of metal ions in the nickel-cobalt-manganese mixed salt solution is 1.0-2.5 mol/L.
Further, in some preferred embodiments of the present invention, the precipitant is sodium hydroxide, and the concentration of the precipitant solution is 5-10 mol/L; the complexing agent is ammonia water, and the concentration of the complexing agent solution is 6-12 mol/L.
Further, in some preferred embodiments of the present invention, the pH value of the bottom solution of the reaction kettle is 11.0-13.0, and the alkalinity is 20-40 g/L.
Further, in some preferred embodiments of the present invention, the target particle size D1 is d50=1.0 to 3.0 μm; the target particle size D2 is d50=2.0 to 4.0 μm.
Further, in a part of the preferred embodiments of the present invention, the temperature of the reaction system in the step (3) is controlled to 50 to 80 ℃ and the stirring speed is 500 to 800rpm.
Further, in a part of the preferred embodiments of the present invention, the temperature of the reaction system in the step (4) is controlled to be 50-80 ℃ and the stirring speed is 400-700 rpm.
Further, in a part of the preferred embodiment of the present invention, during the reaction of step (3) and step (4), the concentration is carried out by a thickener.
Further, at the end of the reaction in the step (4), the solid content of the reaction system is 400-800 g/L.
The precursor material is prepared by an intermittent process, and in a nucleation stage, crystal nuclei with good dispersibility and sphericity are obtained by controlling the pH value and the alkalinity; after the nucleation stage is finished, the precursor material with good sphericity and high compaction density is obtained by entering a growth stage and precisely distributing and controlling the flow.
Compared with the prior art, the invention has the following obvious beneficial effects:
(1) The invention provides a process for intermittently preparing a ternary nickel-cobalt-manganese precursor with a very small particle size, which realizes the regulation and control of primary particles and secondary particles of the nickel-cobalt-manganese precursor with the very small particle size;
(2) The preparation method of the target nickel-cobalt-manganese precursor is realized by means of conventional technological parameter adjustment, material distribution and the like, and has the advantages of simple process, strong operability and no additional cost;
(3) The precursor material prepared by the invention has small granularity, high tap density and large specific surface area, is a small-particle-size ternary precursor with excellent performance, and has wide application prospect in the aspects of single crystal materials, high-compaction materials and high-power materials.
Drawings
FIG. 1 is a 10000-fold scanning electron microscope image of a ternary nickel-cobalt-manganese precursor prepared in example 1;
FIG. 2 is a 10000-fold scanning electron microscope image of the ternary nickel-cobalt-manganese precursor prepared in example 2;
FIG. 3 is a 10000-fold scanning electron microscope image of the ternary nickel-cobalt-manganese precursor prepared in example 3;
FIG. 4 is a 10000-fold scanning electron microscope image of the ternary nickel-cobalt-manganese precursor prepared in example 4;
fig. 5 is a 10000-fold scanning electron microscope image of the nickel-cobalt-manganese ternary precursor prepared in comparative example 1.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
The invention firstly provides a nickel-cobalt-manganese ternary precursor, the chemical molecular formula of which is Ni x Co y Mn 1-x-y (OH) 2 Wherein x is more than or equal to 0.70 and less than 1.0, and y is more than or equal to 0 and less than 0.3; the precursor secondary particles are spherical, the primary particles are laminated, and the thickness of the laminated layers is 50-400 nm; the particle diameter D50 of the precursor is 2.0-4.0 mu m, and the tap density is 2.0-2.3 g/cm 3 Specific surface area of 5-15 m 2 /g。
The research shows that the primary particle thickness of the nickel-cobalt-manganese ternary precursor is closely related to the area of the (010) crystal face, and the adjustment of the (010) crystal face in a certain range can be realized by adjusting the primary particle thickness of the precursor.
The precursor material provided by the invention takes main index parameters such as (010) crystal face, tap density, specific surface area and the like into consideration, is a small-particle-size ternary precursor with excellent performance, and has wide application prospects in the aspects of monocrystalline materials, high-compaction materials and high-power materials.
The invention further provides an intermittent preparation method of the nickel-cobalt-manganese ternary precursor, which comprises the following steps:
(1) Preparing a nickel-cobalt-manganese mixed salt solution, a precipitator solution and a complexing agent solution;
(2) Preparing a reaction kettle bottom solution;
(3) Adding the nickel-cobalt-manganese mixed salt solution prepared in the step (1), the precipitator solution and the complexing agent solution into the bottom solution of the reaction kettle in parallel, and controlling the adding speed of the nickel-cobalt-manganese mixed salt solution to be V 1 The pH value of a system in the reaction kettle is adjusted to 11.0-13.0, and the alkalinity is adjusted to 20-40 g/L; stopping the reaction when the reaction slurry reaches the target granularity D1 to obtain crystal nucleus slurry;
(4) The crystal nucleus slurry is evenly conveyed into N growing kettles, wherein N is a natural number and is more than or equal to 2 and less than or equal to 10; adding the nickel-cobalt-manganese mixed salt solution, the precipitant solution and the complexing agent solution prepared in the step (1) into each growth kettle in parallel; the pH value of the reaction system is regulated to be 10.0-12.0, and the alkalinity is regulated to be 15-30 g/L;
when the N value is 2, the speed of adding the nickel-cobalt-manganese mixed salt solution into each growth kettle is V 2 ；
When N is a natural number and N is more than or equal to 3 and less than or equal to 10, the speed of adding the nickel-cobalt-manganese mixed salt solution into each growth kettle is 2V 2 /N；
(5) Stopping the reaction when the granularity of the reaction slurry in the step (4) reaches the target granularity D2, and obtaining the nickel-cobalt-manganese ternary precursor after aging, solid-liquid separation, washing and drying the solid phase of the reaction slurry.
According to the invention, the crystal nucleus slurry is evenly distributed into the growth reaction kettles, and the flow of the nickel-cobalt-manganese mixed salt solution is regulated according to the quantity of the distributed reaction kettles. The adding speed of the nickel-cobalt-manganese mixed salt solution in the nucleation stage is V 1 The quantity of the growth reaction kettles is different, and the adding speed of the nickel-cobalt-manganese mixed salt solution of each growth reaction kettle is directly related. When the number of the growth reaction kettles is 2, the adding speed of the nickel-cobalt-manganese mixed salt solution of the 2 growth reaction kettles in the growth stage is V respectively 2 As the number of growth reaction kettles increases, the addition rate of the nickel-cobalt-manganese mixed salt solution of each growth reaction kettle is adjusted downwards, for example: if the number of the reaction kettles in the growth stage is 5, the flow rate of the nickel-cobalt-manganese mixed salt solution of each growth reaction kettle is 2V 2 5; if the number of the growth reaction kettles is 8, the flow rate of the nickel-cobalt-manganese mixed salt solution of each growth reaction kettle is 2V 2 /8. In general, as the number of growth reactors increases, the rate of addition of the nickel cobalt manganese mixed salt solution per growth reactor decreases.
After the crystal nucleus slurry is evenly distributed to the growth reaction kettles, the flow of the nickel-cobalt-manganese mixed metal salt is regulated according to the quantity of the branch kettles, so that the obtained granularity is consistent after the same growth period of different quantities of crystal seeds; and obtaining precursors with laminated primary particles and laminated thickness of 50-400 nm, wherein the number of the growth reaction kettles is more than 2 and not more than 10. Along with the increase of the number of the growth reaction kettles, the seed crystal amount in each growth kettle is small, so that the growth period is consistent with the granularity, the particle growth is slow, primary particles can be thicker, and the tap density can be reduced.
In some specific embodiments, the nickel, cobalt and manganese salt in the nickel-cobalt-manganese mixed salt solution is at least one of sulfate, nitrate and chloride. The total concentration of metal ions in the nickel-cobalt-manganese mixed salt solution is 1.0-2.5 mol/L, preferably 1.5-2.5 mol/L.
In some specific embodiments, sodium hydroxide is selected as a precipitant, and the concentration of the sodium hydroxide solution is 5-10 mol/L; ammonia water is selected as a complexing agent, and the concentration of the ammonia water solution is 6-12 mol/L.
In some specific embodiments, preparing a reaction kettle bottom solution, and adjusting the pH value of the reaction kettle bottom solution to be 11.0-13.0, wherein the alkalinity is 20-40 g/L.
In some embodiments, the control target particle size D1 is d50=1.0 to 3.0 μm, and the control target particle size D2 is d50=2.0 to 4.0 μm.
In some embodiments, the temperature of the reaction system in step (3) is controlled to 50-80 ℃ and the stirring speed is 500-800 rpm.
In some embodiments, the temperature of the reaction system in step (4) is controlled to be 50-80 ℃, and the stirring speed is 400-700 rpm.
In some embodiments, during the reaction of step (3) and step (4), the concentration is achieved by a thickener.
Further, at the end of the reaction in the step (4), the solid content of the reaction system is 400 to 800g/L, preferably 400 to 600g/L.
In some specific embodiments, 10-15 wt% alkali solution is used to age the reaction slurry, the aging temperature is 50-80 ℃, and the aging reaction time is 60-120 min; the pH value of the washing end point is controlled to be 7.5-8.5; the drying temperature is 130-160 ℃.
Further description will be given below by way of specific examples.
Example 1
(1) According to formula Ni 0.70 Co 0.2 Mn 0.1 (OH) 2 Preparing 2mol/L nickel-cobalt-manganese mixed metal salt solution; preparing 8mol/L sodium hydroxide solution; preparing 10mol/L ammonia water solution;
(2) 200L of pure water was added to a reaction vessel having a volume of 300L, the temperature was controlled to 70℃and the stirring speed was controlled to 700rpm, and a pH value was adjusted to 12.90.+ -. 0.10 by introducing a sodium hydroxide solution. And (3) introducing the solution in the step (1) into the bottom solution of the reaction kettle, wherein the flow rate of the nickel-cobalt-manganese mixed metal salt solution is 100ml/min, adjusting the flow rate of the sodium hydroxide solution after the reaction starts, stabilizing the pH value in the kettle to 12.90+/-0.10, controlling the concentration of ammonium ions in the kettle to be about 30g/L, and maintaining for 2h. The particle size of the reaction slurry was measured to be 2.0.+ -. 0.5. Mu.m.
(3) Pumping the slurry in the step (2) into 2 300L growth kettles respectively at the same flow rate, heating to 75 ℃, and controlling the stirring rotation speed to 600rpm; and (3) introducing ammonia water solution to adjust the alkalinity in the kettle to be 12g/L, introducing the solution in the step (1) into the bottom solution of the reaction kettle, and introducing the solution in the step (1), wherein the flow rate of the nickel-cobalt-manganese mixed metal salt solution is 600ml/min, controlling the concentration of ammonium ions in the kettle to be about 25g/L, and stopping the reaction until the pH value is 11.80+/-0.10 and the slurry D50 is detected to be 3.5+/-0.5 mu m. Concentrating by a thickener, and controlling the solid content of the slurry at the time of stopping the reaction to be 600g/L.
(4) Aging, washing, filtering and drying the reaction product obtained in the step (3), wherein the aging temperature is 75 ℃ and the aging reaction time is 120min; the pH value of the washing end point is controlled to be 7.5-8.5; the drying temperature was 140 ℃.
Fig. 1 is an SEM image of the precursor prepared in example 1. The obtained precursor D50 is 2.8 mu m, the tap density is 2.16g/cm and the specific surface area is 13.79m 2 /g。
Example 2
Example 2 differs from example 1 in that: step (3) is different.
The step (3) of this embodiment specifically includes: pumping the slurry in the step (2) into 3 300L growth kettles respectively at the same flow rate, heating to 75 ℃, and controlling the stirring rotation speed to 600rpm; and (3) introducing ammonia water solution to adjust the alkalinity in the kettle to be 12g/L, introducing the solution in the step (1) into the bottom solution of the reaction kettle, and introducing the solution in the step (1), wherein the flow rate of the nickel-cobalt-manganese mixed metal salt solution is 400ml/min, controlling the concentration of ammonium ions in the kettle to be about 25g/L, and stopping the reaction until the pH value is 11.80+/-0.10 and the slurry D50 is detected to be 3.5+/-0.5 mu m.
Fig. 2 is an SEM image of the precursor prepared in example 2. The obtained front partThe D50 of the precursor is 3.1 mu m, the tap density is 2.30g/cm and the specific surface area is 10.96m 2 /g。
Example 3
Example 3 differs from example 1 in that: step (3) is different.
The step (3) of this embodiment specifically includes: pumping the slurry in the step (2) into 5 300L growth kettles at the same flow rate, heating to 75 ℃, and controlling the stirring rotation speed to 600rpm; and (3) introducing ammonia water solution to adjust the alkalinity in the kettle to be 12g/L, introducing the solution in the step (1) into the bottom solution of the reaction kettle, and introducing the solution in the step (1), wherein the flow rate of the nickel-cobalt-manganese mixed metal salt solution is 240ml/min, controlling the concentration of ammonium ions in the kettle to be about 25g/L, and stopping the reaction until the pH value is 11.80+/-0.10 and the slurry D50 is detected to be 3.5+/-0.5 mu m.
Fig. 3 is an SEM image of the precursor prepared in example 3. The obtained precursor D50 is 3.3 mu m, the tap density is 2.21g/cm and the specific surface area is 10.04m 2 /g。
Example 4
Example 4 differs from example 1 in that: step (3) is different.
The step (3) of this embodiment specifically includes: pumping the slurry in the step (2) into 8 300L growth kettles at the same flow rate, heating to 75 ℃, and controlling the stirring rotation speed to 600rpm; and (3) introducing ammonia water solution to adjust the alkalinity in the kettle to be 12g/L, introducing the solution in the step (1) into the bottom solution of the reaction kettle, and introducing the solution in the step (1), wherein the flow rate of the nickel-cobalt-manganese mixed metal salt solution is 150ml/min, controlling the concentration of ammonium ions in the kettle to be about 25g/L, and stopping the reaction until the pH value is 11.80+/-0.10 and the slurry D50 is detected to be 3.5+/-0.5 mu m.
Fig. 4 is an SEM image of the precursor prepared in example 4. The obtained precursor D50 is 3.6 mu m, the tap density is 2.28g/cm and the specific surface area is 9.21m 2 /g。
Comparative example 1
(1) According to formula Ni 0.70 Co 0.2 Mn 0.1 (OH) 2 Preparing 2mol/L nickel-cobalt-manganese mixed metal salt solution; preparing 8mol/L sodium hydroxide solution; preparing 10mol/L ammonia water solution;
(2) 200L of pure water was added to a reaction vessel having a volume of 300L, the temperature was controlled to 70℃and the stirring speed was controlled to 700rpm, and a pH value was adjusted to 10.90.+ -. 0.10 by introducing a sodium hydroxide solution. And (3) introducing the solution in the step (1) into the bottom solution of the reaction kettle, wherein the flow rate of the nickel-cobalt-manganese mixed metal salt solution is 100ml/min, adjusting the flow rate of the sodium hydroxide solution after the reaction starts, stabilizing the pH value in the kettle to 10.90+/-0.10, controlling the concentration of ammonium ions in the kettle to be about 10g/L, maintaining the growth under the condition until the slurry D50 is detected to be 3.5+/-0.5 mu m, and stopping the reaction.
(3) Aging, washing, filtering and drying the reaction product obtained in the step (2), wherein the aging temperature is 75 ℃ and the aging reaction time is 120min; the pH value of the washing end point is controlled to be 7.5-8.5; the drying temperature was 140 ℃.
Fig. 5 is an SEM image of the precursor prepared in comparative example 1. The obtained precursor D50 is 3.4 mu m, the tap density is 1.9g/cm and the specific surface area is 3.70m 2 /g。
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (7)
1. Intermittent preparation method of nickel-cobalt-manganese ternary precursor, wherein chemical molecular formula of nickel-cobalt-manganese ternary precursor is Ni x Co y Mn 1-x-y (OH) 2 Wherein x is more than or equal to 0.70 and less than 1.0, and y is more than or equal to 0 and less than 0.3; the secondary particles of the nickel-cobalt-manganese ternary precursor are spherical, the primary particles are laminated, and the thickness of the laminated layers is 50-400 nm; the particle diameter D50 of the nickel-cobalt-manganese ternary precursor is 2.0-4.0 mu m, and the tap density is 2.0-2.3 g/cm 3 Specific surface area of 5-15 m 2 /g; the preparation method is characterized by comprising the following steps of:
(1) Preparing a nickel-cobalt-manganese mixed salt solution, a precipitator solution and a complexing agent solution;
(2) Preparing a reaction kettle bottom solution;
(3) Adding the nickel-cobalt-manganese mixed salt solution prepared in the step (1), the precipitator solution and the complexing agent solution into the bottom solution of the reaction kettle in parallel, and controlling the adding speed of the nickel-cobalt-manganese mixed salt solution to be V 1 Regulating the pH value of the system in the reaction kettle to be 11.0-13.0 and the alkalinity to be 20-40 g/L; stopping the reaction when the reaction slurry reaches the target granularity D1 to obtain crystal nucleus slurry;
(4) The crystal nucleus slurry is evenly conveyed into N growing kettles, wherein N is a natural number and is more than or equal to 2 and less than or equal to 10; adding the nickel-cobalt-manganese mixed salt solution, the precipitant solution and the complexing agent solution prepared in the step (1) into each growth kettle in parallel; regulating the pH value of the reaction system to be 10.0-12.0 and the alkalinity to be 15-30 g/L;
when the N value is 2, the speed of adding the nickel-cobalt-manganese mixed salt solution into each growth kettle is V 2 ；
When N is a natural number and N is more than or equal to 3 and less than or equal to 10, the speed of adding the nickel-cobalt-manganese mixed salt solution into each growth kettle is 2V 2 /N；
(5) Stopping the reaction when the granularity of the reaction slurry in the step (4) reaches the target granularity D2, and obtaining the nickel-cobalt-manganese ternary precursor after aging, solid-liquid separation, washing and drying the solid phase of the reaction slurry.
2. The batch process of claim 1 wherein the nickel, cobalt and manganese salt of the nickel cobalt manganese mixed salt solution is at least one of sulfate, nitrate and chloride; the total concentration of metal ions in the nickel-cobalt-manganese mixed salt solution is 1.0-2.5 mol/L.
3. The batch process of claim 1 wherein said precipitant is sodium hydroxide and said precipitant solution has a concentration of 5 to 10mol/L; the complexing agent is ammonia water, and the concentration of the complexing agent solution is 6-12 mol/L.
4. The batch process of claim 1 wherein the pH of the reaction vessel bottoms is 11.0 to 13.0 and the alkalinity is 20 to 40g/L.
5. The batch process according to claim 1, wherein the target particle size D1 is d50=1.0 to 3.0 μm; the target particle size D2 is d50=2.0 to 4.0 μm.
6. The batch production process according to claim 1, wherein the temperature of the reaction system in the step (3) is controlled to 50 to 80 ℃ and the stirring speed is 500 to 800rpm; the temperature of the reaction system in the step (4) is controlled to be 50-80 ℃, and the stirring speed is 400-700 rpm.
7. The batch process of claim 1 wherein during the steps (3) and (4) the reaction is concentrated by a concentrator; and (3) after the reaction in the step (4) is finished, the solid content of the reaction system is 400-800 g/L.
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