Preparation device and preparation method of high-tap-density ternary precursor material

文档序号:496030 发布日期:2022-01-07 浏览:9次 中文

阅读说明:本技术 一种高振实三元前驱体材料的制备装置及制备方法 (Preparation device and preparation method of high-tap-density ternary precursor material ) 是由 许开华 黎俊 张坤 李涛 陈龙 李聪 于 2021-09-02 设计创作,主要内容包括:本发明公开了一种高振实三元前驱体材料的制备装置,包括晶种反应釜(1)、浓密机(7)、晶种槽(8),晶种反应釜分别与浓密机、晶种槽连接,晶种反应釜与晶种槽之间连接的管道与浓密机连接;晶种反应釜内安装有搅拌器(2)、挡板(5),晶种反应釜(1)的内壁安装有导流筒(3)。制备方法为:配制镍、钴、锰的混合硫酸盐溶液;配制底液并通入保护气体;将混合盐溶液、工业液碱、氨水加入到上层桨叶高度处并开启搅拌器;浓密机抽取上清液再返回晶种反应釜,再向晶种槽中溢流;将晶种颗粒通入到晶种反应釜中继续反应,得到目标粒径物料后再经过处理得到高振实三元前驱体材料。本发明制备出的材料振实密度高、颗粒均一性好。(The invention discloses a preparation device of a high-tap ternary precursor material, which comprises a seed crystal reaction kettle (1), a thickener (7) and a seed crystal tank (8), wherein the seed crystal reaction kettle is respectively connected with the thickener and the seed crystal tank, and a pipeline connected between the seed crystal reaction kettle and the seed crystal tank is connected with the thickener; a stirrer (2) and a baffle (5) are arranged in the seed crystal reaction kettle, and a guide cylinder (3) is arranged on the inner wall of the seed crystal reaction kettle (1). The preparation method comprises the following steps: preparing a mixed sulfate solution of nickel, cobalt and manganese; preparing base liquid and introducing protective gas; adding the mixed salt solution, the industrial liquid caustic soda and the ammonia water to the upper layer of the blade and starting a stirrer; the thickener extracts supernatant fluid, returns to the seed crystal reaction kettle and overflows into the seed crystal tank; and introducing the seed crystal particles into a seed crystal reaction kettle to continue reacting to obtain a material with a target particle size, and then processing to obtain the high-tap-density ternary precursor material. The material prepared by the invention has high tap density and good particle uniformity.)

1. The preparation device of the high-tap ternary precursor material is characterized by comprising a seed crystal reaction kettle (1), a thickener (7) and a seed crystal tank (8), wherein the seed crystal reaction kettle (1) is connected with the thickener (7) through a pipeline provided with a valve; install agitator (2) in seed crystal reation kettle (1), draft tube (3) are installed to the inside wall of seed crystal reation kettle (1), and baffle (5) are installed to the lateral wall of seed crystal reation kettle (1).

2. The apparatus for preparing high tap density ternary precursor material according to claim 1, wherein the stirrer (2) is provided with a stirring paddle (4), the stirring paddle (4) comprises an upper layer paddle (9) and a lower layer paddle (6), the upper layer paddle (9) is arranged in the middle of the stirrer (2), and the guide cylinder (3) is arranged around the upper layer paddle (9); the lower paddle (6) is arranged at the lower part of the stirrer (2).

3. The apparatus for preparing a ternary precursor material with high tap density according to claim 2, wherein the upper layer blade (9) is one of a flap-open type blade and a disc turbine type blade, the blade inclination angle of the upper layer blade (9) is 45-75 °, the stirring diameter is 0.5-0.8 times the inner diameter of the guide cylinder (3), and the inner diameter of the guide cylinder (3) is 0.5-0.7 times the inner diameter of the seed crystal reaction kettle (1).

4. The apparatus for preparing high tap density ternary precursor material according to claim 1, wherein the pipeline-mounted valve connected between the seed reaction kettle (1) and the seed tank (8) is located on the pipeline between the thickener (7) and the seed tank (8).

5. A method for preparing a high tap ternary precursor material based on any of claims 1-4, comprising the steps of:

step (I): preparing a mixed salt solution of nickel sulfate, cobalt sulfate and manganese sulfate; the molar ratio of nickel ions, cobalt ions and manganese ions in the mixed salt solution is x: y (100-x-y), wherein x is more than or equal to 60 and less than or equal to 98, y is more than or equal to 0 and less than or equal to 20, and the sum of the concentration of the nickel ions, the concentration of the cobalt ions and the concentration of the manganese ions in the mixed salt solution is 1-3 mol/L;

step (II): preparing a base solution in a seed crystal reaction kettle, and introducing protective gas into the seed crystal reaction kettle; the base solution comprises industrial liquid alkali and ammonia water, the pH value of the base solution is 11-12.5, the concentration of the ammonia water in the base solution is 5-20 g/L, and the temperature of the base solution is 40-60 ℃;

step (three): adding the mixed salt solution into the upper layer blade height position in a seed crystal reaction kettle at the flow rate of 300-600L/h, the industrial liquid caustic soda with the concentration of 8-12 mol/L at the flow rate of 60-120L/h and the ammonia water with the concentration of 0.5-2 mol/L at the flow rate of 20-50L/h for coprecipitation reaction, and starting a stirrer; extracting supernatant from the materials in the seed crystal reaction kettle through a thickener, returning the materials in the thickener to the seed crystal reaction kettle, and continuously overflowing the materials in the seed crystal reaction kettle to a seed crystal tank when the particle size of the material particles in the seed crystal reaction kettle reaches 0.3-0.6 times of the target particle size;

step (IV): introducing the seed crystal material in the seed crystal groove into a seed crystal reaction kettle, wherein the seed crystal material introduced into the seed crystal reaction kettle is 1/5-1/2 of the volume of the seed crystal reaction kettle; adding the mixed salt solution into the lower paddle height in a seed crystal reaction kettle at the flow rate of 200-400L/h and the industrial liquid caustic soda with the concentration of 8-12 mol/L at the flow rate of 40-100L/h and the ammonia water with the concentration of 0.5-2 mol/L at the flow rate of 10-40L/h, starting a stirrer to continue coprecipitation reaction, and stopping the reaction after precursor particles with target particle size are obtained;

step (V): and (3) sequentially carrying out aging, centrifuging, washing, drying and magnetic foreign matter removal treatment on the precursor particles to obtain the high-tap-density ternary precursor material.

6. The method for preparing a high tap density ternary precursor material as claimed in claim 5, wherein the process conditions of the coprecipitation reaction in step (III) are as follows: the reaction temperature is 40-60 ℃, the pH is 10-11, and the concentration of ammonia water is 5-10 g/L; the stirring speed of the stirrer is 200rpm-600 rpm.

7. The method for preparing a high tap density ternary precursor material according to claim 5, wherein the stirring speed of the stirrer in the step (IV) is 200rpm to 500 rpm.

Technical Field

The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation device and a preparation method of a high-tap ternary precursor material.

Background

As a new secondary clean and renewable energy source, the lithium ion battery has the advantages of high energy, high voltage, rapid charge and discharge and the like, is widely applied to the fields of electric tools, mobile phones, digital cameras, notebook computers, instruments and meters and the like, has great potential in the electric automobile industry, and has shown a strong development trend. The anode material is used as a key material of the lithium ion battery, directly influences the performance of the lithium ion battery, the cost accounts for over 40%, and the specific gravity of the anode material in the lithium ion battery is high. The lithium ion battery anode material mainly comprises lithium cobaltate, lithium iron phosphate, lithium manganate, ternary materials of lithium nickel cobalt manganese oxide, lithium nickel cobalt aluminate and the like, wherein the ternary materials have higher reversible capacity and low cost and become the lithium ion power battery anode material with the most application prospect at present, and the structural performance of the ternary anode material is mainly influenced by the physical and chemical properties of a precursor material. The industrialization mode of the ternary precursor material mainly adopts a coprecipitation preparation method, and the structural performance of the ternary precursor material is directly influenced by the control of precipitation and crystallization.

The invention patent of patent No. CN103482711A discloses a method for preparing a precursor of a ternary positive electrode material of a lithium ion battery by ultrasonic assistance, wherein an ultrasonic assistance method is adopted in the coprecipitation preparation process and the washing process of the precursor, so that a precursor conforming to the hydroxide with high tap density can be obtained, but the preparation process adopts an ultrasonic assistance mode, the high tap density ternary precursor needs higher shearing force in the synthesis process, the ultrasonic assistance method is adopted in the coprecipitation preparation process of the ternary precursor to prepare the precursor conforming to the hydroxide with high tap density, but the energy consumption in the preparation process is lower than that in the coprecipitation preparation processLarge size and high cost. In the application of patent No. CN111039331A, a certain amount of sodium chloroborate (Na) is added in the process of preparing the high-nickel ternary precursor by a coprecipitation method3B6O10Cl) to adjust the crystal face growth of primary particles in the precursor, so that the interface adhesion among the primary particles is improved, a more compact and dense secondary ball is obtained, sodium chloroborate is added in the coprecipitation process to adjust the crystal face growth of the precursor particles, the interface adhesion is increased, and then the precursor particles which are combined compactly and densely are prepared. The application with the patent number of CN109225069A improves the stability and consistency of products caused by uneven stirring by adding an anti-deposition device at the bottom of the reaction kettle, and prepares a ternary anode precursor material with small particle size, high tap density, narrow distribution and uniformity, but the method directly reduces the effective volume of the reaction kettle, which is equivalent to sacrificing the productivity to improve the consistency of the materials.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a preparation device and a preparation method for preparing a high-tap ternary precursor material which has high tap density and good particle uniformity and is beneficial to improving the stability and energy density of a cathode material.

The invention adopts the following technical scheme:

the preparation device of the high-tap ternary precursor material is characterized by comprising a seed crystal reaction kettle (1), a thickener (7) and a seed crystal tank (8), wherein the seed crystal reaction kettle (1) is connected with the thickener (7) through a pipeline provided with a valve; install agitator (2) in seed crystal reation kettle (1), draft tube (3) are installed to the inside wall of seed crystal reation kettle (1), and baffle (5) are installed to the lateral wall of seed crystal reation kettle (1).

The device for preparing the high-tap ternary precursor material is characterized in that a stirring paddle (4) is installed on the stirrer (2), the stirring paddle (4) comprises an upper paddle (9) and a lower paddle (6), the upper paddle (9) is installed in the middle of the stirrer (2), and the guide cylinder (3) is installed around the upper paddle (9); the lower paddle (6) is arranged at the lower part of the stirrer (2).

The preparation device of the high tap ternary precursor material is characterized in that the upper-layer paddle (9) is one of a flap-opening paddle and a disc turbine paddle, the blade inclination angle of the upper-layer paddle (9) is 45-75 degrees, the stirring diameter is 0.5-0.8 times of the inner diameter of the guide cylinder (3), and the inner diameter of the guide cylinder (3) is 0.5-0.7 times of the inner diameter of the seed crystal reaction kettle (1).

The device for preparing the high-tap ternary precursor material is characterized in that a valve installed on a pipeline connected between the seed crystal reaction kettle (1) and the seed crystal tank (8) is positioned on a pipeline between the thickener (7) and the seed crystal tank (8).

The preparation method of the preparation device based on the high-tap ternary precursor material is characterized by comprising the following steps of:

step (I): preparing a mixed salt solution of nickel sulfate, cobalt sulfate and manganese sulfate; the molar ratio of nickel ions, cobalt ions and manganese ions in the mixed salt solution is x: y (100-x-y), wherein x is more than or equal to 60 and less than or equal to 98, y is more than or equal to 0 and less than or equal to 20, and the sum of the concentration of the nickel ions, the concentration of the cobalt ions and the concentration of the manganese ions in the mixed salt solution is 1-3 mol/L;

step (II): preparing a base solution in a seed crystal reaction kettle, and introducing protective gas into the seed crystal reaction kettle; the base solution comprises industrial liquid alkali and ammonia water, the pH value of the base solution is 11-12.5, the concentration of the ammonia water in the base solution is 5-20 g/L, and the temperature of the base solution is 40-60 ℃;

step (three): adding the mixed salt solution into the upper layer blade height position in a seed crystal reaction kettle at the flow rate of 300-600L/h, the industrial liquid caustic soda with the concentration of 8-12 mol/L at the flow rate of 60-120L/h and the ammonia water with the concentration of 0.5-2 mol/L at the flow rate of 20-50L/h for coprecipitation reaction, and starting a stirrer; extracting supernatant from the materials in the seed crystal reaction kettle through a thickener, returning the materials in the thickener to the seed crystal reaction kettle, and continuously overflowing the materials in the seed crystal reaction kettle to a seed crystal tank when the particle size of the material particles in the seed crystal reaction kettle reaches 0.3-0.6 times of the target particle size;

step (IV): introducing the seed crystal material in the seed crystal groove into a seed crystal reaction kettle, wherein the seed crystal material introduced into the seed crystal reaction kettle is 1/5-1/2 of the volume of the seed crystal reaction kettle; adding the mixed salt solution into the lower paddle height in a seed crystal reaction kettle at the flow rate of 200-400L/h and the industrial liquid caustic soda with the concentration of 8-12 mol/L at the flow rate of 40-100L/h and the ammonia water with the concentration of 0.5-2 mol/L at the flow rate of 10-40L/h, starting a stirrer to continue coprecipitation reaction, and stopping the reaction after precursor particles with target particle size are obtained;

step (V): and (3) sequentially carrying out aging, centrifuging, washing, drying and magnetic foreign matter removal treatment on the precursor particles to obtain the high-tap-density ternary precursor material.

The preparation method of the preparation device of the high tap density ternary precursor material is characterized in that the process conditions of the coprecipitation reaction in the step (III) are as follows: the reaction temperature is 40-60 ℃, the pH is 10-11, and the concentration of ammonia water is 5-10 g/L; the stirring speed of the stirrer is 200rpm-600 rpm.

The preparation method of the preparation device of the high tap density ternary precursor material is characterized in that the stirring speed of the stirrer in the step (IV) is 200-500 rpm.

The invention has the beneficial technical effects that: in the coprecipitation reaction process of the precursor, a seed crystal process and a seed crystal growth process in the preparation of the precursor are respectively controlled, the shear distribution in the crystallization process of the seed crystal is improved, a certain radial flow is ensured below a feeding position by controlling the structural sizes of a stirrer and a guide cylinder, the rapid mixing of a mixed salt solution and a precipitator in a crystal nucleus area is promoted, the mixing efficiency and the shear distribution in the nucleation and crystallization process of the seed crystal are improved, and the seed crystal with compact particles and good consistency and dispersibility is prepared; by controlling the addition of the seed crystal, the growth rate of the precursor particles is ensured to be consistent and stable in the growth process of the seed crystal, the ordered assembly of the precursor particles is promoted, and the ternary precursor material with high tap density and good uniformity is prepared. The material prepared by the invention has high tap density and good particle uniformity, and is beneficial to improving the stability and energy density of the anode material.

Drawings

FIG. 1 is a schematic diagram of the apparatus of the present invention;

FIG. 2 shows the surface morphology and the cross-sectional morphology of the seed crystal of the ternary precursor material prepared in example 1;

FIG. 3 shows the surface morphology of the finished ternary precursor material with high tap density.

Detailed Description

Referring to fig. 1, the device for preparing a high tap density ternary precursor material of the present invention comprises a seed crystal reaction kettle 1, a thickener 7 and a seed crystal tank 8, wherein the seed crystal reaction kettle 1 is connected with the thickener 7 through a pipeline provided with a valve, the seed crystal reaction kettle 1 is connected with the seed crystal tank 8 through a pipeline provided with a valve, a pipeline connected between the seed crystal reaction kettle 1 and the seed crystal tank 8 is connected with the thickener 7 through a pipeline provided with a valve, and the seed crystal tank 8 is connected with the seed crystal reaction kettle 1 through a pipeline provided with a valve; the valve installed on the pipeline connected between the seed crystal reaction kettle 1 and the seed crystal tank 8 is positioned on the pipeline between the thickener 7 and the seed crystal tank 8. Install agitator 2 in the seed crystal reation kettle 1, agitator 4 is installed to agitator 2, and agitator 4 includes upper paddle 9 and lower floor's paddle 6, and upper paddle 9 is installed in the middle part of agitator 2, and lower floor's paddle 6 is installed in the lower part of agitator 2. The upper layer blade 9 is one of a flap opening type blade and a disc turbine type blade, the blade inclination angle of the upper layer blade 9 is 45-75 degrees, the stirring diameter is 0.5-0.8 times of the inner diameter of the guide shell 3, and the inner diameter of the guide shell 3 is 0.5-0.7 times of the inner diameter of the seed crystal reaction kettle 1. The inner wall of the crystal seed reaction kettle 1 is provided with a guide shell 3, and the guide shell 3 is arranged around the upper paddle 9. The side wall of the seed crystal reaction kettle 1 is provided with a baffle 5.

The preparation method of the preparation device of the high-tap ternary precursor material comprises the following steps:

step (I): preparing a mixed salt solution of nickel sulfate, cobalt sulfate and manganese sulfate; the molar ratio of nickel ions, cobalt ions and manganese ions in the mixed salt solution is x: y (100-x-y), wherein x is more than or equal to 60 and less than or equal to 98, y is more than or equal to 0 and less than or equal to 20, and the sum of the concentration of the nickel ions, the concentration of the cobalt ions and the concentration of the manganese ions in the mixed salt solution is 1-3 mol/L; industrial liquid caustic soda with the concentration of 8-12 mol/L is used as a precipitator solution, and ammonia water with the concentration of 0.5-2 mol/L is used as a complexing agent solution.

Step (II): preparing a base solution in the seed crystal reaction kettle 1, and introducing protective gas into the seed crystal reaction kettle 1; the base solution is prepared from a precipitator solution and a complexing agent solution, the pH of the base solution is 11-12.5, the concentration of ammonia water in the base solution is 5-20 g/L, and the temperature of the base solution is 40-60 ℃.

Step (three): adding the mixed salt solution at the flow rate of 300-600L/h, the precipitant solution at the flow rate of 60-120L/h and the complexing agent solution at the flow rate of 20-50L/h into the horizontal position of an upper paddle 9 in the seed crystal reaction kettle 1 for coprecipitation reaction, and starting a stirrer 2; the process conditions of the coprecipitation reaction are as follows: the reaction temperature is 40-60 ℃, the pH is 10-11, the concentration of ammonia water is 5-10 g/L, and the stirring speed of the stirring paddle is 200-600 rpm. Extracting supernatant from the material in the seed crystal reaction kettle 1 through a thickener 7, returning the material in the thickener 7 to the seed crystal reaction kettle 1, stabilizing the reaction conditions when the particle size of the material particles in the seed crystal reaction kettle 1 reaches 0.3-0.6 times of the target particle size, and continuously overflowing the material in the seed crystal reaction kettle 1 into a seed crystal tank 8.

Step (IV): introducing the seed crystal material in the seed crystal tank 8 into the seed crystal reaction kettle 1, wherein the seed crystal material introduced into the seed crystal reaction kettle 1 is 1/5-1/2 of the volume of the seed crystal reaction kettle 1; and adding the mixed salt solution at the flow rate of 200-400L/h, the precipitant solution at the flow rate of 40-100L/h and the complexing agent solution at the flow rate of 10-40L/h into the horizontal position of the lower paddle 6 in the seed crystal reaction kettle 1, starting the stirrer 2 to continue the coprecipitation reaction, and stopping the reaction until the precursor particles grow to the target particle size D50. The stirring speed of the stirrer 2 is 200rpm to 500 rpm.

Step (V): and aging the precursor particles to obtain a spherical precursor, and carrying out centrifugation, washing, drying, magnetic foreign matter removal and other treatments to obtain the high-tap-density ternary precursor material.

Example 1

Preparing a mixed salt solution of nickel sulfate, cobalt sulfate and manganese sulfate; the molar ratio of nickel ions to cobalt ions to manganese ions in the mixed salt solution is 8:1:1, and the sum of the concentration of the nickel ions, the concentration of the cobalt ions and the concentration of the manganese ions in the mixed salt solution is 2 mol/L; industrial liquid alkali with the concentration of 8mol/L is used as a precipitator solution, and ammonia water with the concentration of 1mol/L is used as a complexing agent solution.

Preparing a base solution in the seed crystal reaction kettle 1, and introducing protective gas into the seed crystal reaction kettle 1; the base solution is prepared from a precipitator solution and a complexing agent solution, the pH of the base solution is 11-11.6, the concentration of ammonia water in the base solution is 5-10 g/L, and the temperature of the base solution is 40-50 ℃.

Adding the mixed salt solution at the flow rate of 600L/h, the precipitant solution at the flow rate of 110L/h-120L/h and the complexing agent solution at the flow rate of 45L/h-50L/h to the horizontal position of an upper layer paddle 9 in the seed crystal reaction kettle 1, and carrying out coprecipitation reaction under the stirring speed of 500rpm-600rpm of a stirring paddle; the upper layer of the blades 9 are hinged opening blades, the blade inclination angle of the upper layer of the blades 9 is 55 degrees, the stirring diameter is 0.65 times of the inner diameter of the guide shell 3, and the inner diameter of the guide shell 3 is 0.7 times of the inner diameter of the crystal seed reaction kettle 1. The process conditions of the coprecipitation reaction are as follows: the reaction temperature is 40-42 ℃, the pH is 10-10.2, and the concentration of ammonia water is 5-6 g/L. Extracting supernatant from the material in the seed crystal reaction kettle 1 through a thickener 7, returning the material in the thickener 7 to the seed crystal reaction kettle 1, stabilizing reaction conditions when the particle size of the material particles in the seed crystal reaction kettle 1 reaches 0.6 times of the target particle size D50, and continuously overflowing the material in the seed crystal reaction kettle 1 into a seed crystal tank 8.

Introducing the seed crystal material in the seed crystal tank 8 into the seed crystal reaction kettle 1; and adding the mixed salt solution at the flow rate of 400L/h, the precipitant solution at the flow rate of 90L/h-100L/h and the complexing agent solution at the flow rate of 35L/h-40L/h to the horizontal position of the lower layer paddle 6 in the seed crystal reaction kettle 1, starting the stirrer 2 to continue coprecipitation reaction, and stopping the reaction until precursor particles grow to the target particle size D50. The stirring speed of the stirrer 2 is 450rpm-500 rpm.

And aging the precursor particles to obtain a spherical precursor, and carrying out centrifugation, washing, drying, magnetic foreign matter removal and other treatments to obtain the high-tap-density ternary precursor material.

The surface morphology and the profile morphology of the ternary precursor material seed crystal prepared in example 1 are shown in fig. 2; the surface topography of the finished high tap ternary precursor material is shown in fig. 3.

Example 2

Preparing a mixed salt solution of nickel sulfate, cobalt sulfate and manganese sulfate; the molar ratio of nickel ions to cobalt ions to manganese ions in the mixed salt solution is 88:6:6, and the sum of the concentration of the nickel ions, the concentration of the cobalt ions and the concentration of the manganese ions in the mixed salt solution is 2 mol/L; industrial liquid alkali with the concentration of 8mol/L is used as a precipitator solution, and ammonia water with the concentration of 1mol/L is used as a complexing agent solution.

Preparing a base solution in the seed crystal reaction kettle 1, and introducing protective gas into the seed crystal reaction kettle 1; the base solution is prepared from a precipitator solution and a complexing agent solution, the pH of the base solution is 11.2-11.8, the concentration of ammonia water in the base solution is 8-13 g/L, and the temperature of the base solution is 45-55 ℃.

Adding the mixed salt solution at the flow rate of 500L/h, the precipitant solution at the flow rate of 90L/h-100L/h and the complexing agent solution at the flow rate of 40L/h-45L/h to the horizontal position of an upper layer blade 9 in the seed crystal reaction kettle 1, and carrying out coprecipitation reaction under the stirring speed of 450rpm-550rpm of a stirring paddle; the upper layer of the blades 9 are hinged opening blades, the blade inclination angle of the upper layer of the blades 9 is 55 degrees, the stirring diameter is 0.65 times of the inner diameter of the guide shell 3, and the inner diameter of the guide shell 3 is 0.6 times of the inner diameter of the crystal seed reaction kettle 1. The process conditions of the coprecipitation reaction are as follows: the reaction temperature is 50-52 ℃, the pH is 10.4-10.6, and the concentration of ammonia water is 7-8 g/L. Extracting supernatant from the material in the seed crystal reaction kettle 1 through a thickener 7, returning the material in the thickener 7 to the seed crystal reaction kettle 1, stabilizing reaction conditions when the particle size of the material particles in the seed crystal reaction kettle 1 reaches 0.6 times of the target particle size D50, and continuously overflowing the material in the seed crystal reaction kettle 1 into a seed crystal tank 8.

Introducing the seed crystal material in the seed crystal tank 8 into the seed crystal reaction kettle 1; and adding the mixed salt solution at the flow rate of 350L/h, the precipitant solution at the flow rate of 62L/h-70L/h and the complexing agent solution at the flow rate of 28L/h-35L/h to the horizontal position of the lower layer paddle 6 in the seed crystal reaction kettle 1, starting the stirrer 2 to continue coprecipitation reaction, and stopping the reaction until precursor particles grow to the target particle size D50. The stirring speed of the stirrer 2 is 400rpm to 450 rpm.

And aging the precursor particles to obtain a spherical precursor, and carrying out centrifugation, washing, drying, magnetic foreign matter removal and other treatments to obtain the high-tap-density ternary precursor material.

Example 3

Preparing a mixed salt solution of nickel sulfate, cobalt sulfate and manganese sulfate; the molar ratio of nickel ions to cobalt ions to manganese ions in the mixed salt solution is 96:2:2, and the sum of the concentration of nickel ions, the concentration of cobalt ions and the concentration of manganese ions in the mixed salt solution is 2 mol/L; industrial liquid alkali with the concentration of 8mol/L is used as a precipitator solution, and ammonia water with the concentration of 1mol/L is used as a complexing agent solution.

Preparing a base solution in the seed crystal reaction kettle 1, and introducing protective gas into the seed crystal reaction kettle 1; the base solution is prepared from a precipitator solution and a complexing agent solution, the pH of the base solution is 11.4-12.0, the concentration of ammonia water in the base solution is 8-15 g/L, and the temperature of the base solution is 50-60 ℃.

Adding the mixed salt solution at the flow rate of 400L/h, the precipitant solution at the flow rate of 72L/h-80L/h and the complexing agent solution at the flow rate of 35L/h-40L/h to the horizontal position of an upper layer paddle 9 in the seed crystal reaction kettle 1, and carrying out coprecipitation reaction under the stirring speed of a stirring paddle of 400rpm-500 rpm; the upper layer of the blades 9 are hinged opening blades, the blade inclination angle of the upper layer of the blades 9 is 55 degrees, the stirring diameter is 0.65 times of the inner diameter of the guide shell 3, and the inner diameter of the guide shell 3 is 0.5 times of the inner diameter of the crystal seed reaction kettle 1. The process conditions of the coprecipitation reaction are as follows: the reaction temperature is 58-60 ℃, the pH value is 10.8-11, and the concentration of ammonia water is 9-10 g/L. Extracting supernatant from the material in the seed crystal reaction kettle 1 through a thickener 7, returning the material in the thickener 7 to the seed crystal reaction kettle 1, stabilizing reaction conditions when the particle size of the material particles in the seed crystal reaction kettle 1 reaches 0.6 times of the target particle size D50, and continuously overflowing the material in the seed crystal reaction kettle 1 into a seed crystal tank 8.

Introducing the seed crystal material in the seed crystal tank 8 into the seed crystal reaction kettle 1; and adding the mixed salt solution at the flow rate of 300L/h, the precipitant solution at the flow rate of 54L/h-60L/h and the complexing agent solution at the flow rate of 24L/h-30L/h to the horizontal position of the lower layer paddle 6 in the seed crystal reaction kettle 1, starting the stirrer 2 to continue coprecipitation reaction, and stopping the reaction until precursor particles grow to the target particle size D50. The stirring speed of the stirrer 2 is 350-400 rpm.

And aging the precursor particles to obtain a spherical precursor, and carrying out centrifugation, washing, drying, magnetic foreign matter removal and other treatments to obtain the high-tap-density ternary precursor material.

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