CN113735182A - Preparation method of large-particle-size aluminum-coated cobaltosic oxide - Google Patents

Preparation method of large-particle-size aluminum-coated cobaltosic oxide Download PDF

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CN113735182A
CN113735182A CN202110980495.9A CN202110980495A CN113735182A CN 113735182 A CN113735182 A CN 113735182A CN 202110980495 A CN202110980495 A CN 202110980495A CN 113735182 A CN113735182 A CN 113735182A
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aluminum
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cobaltosic oxide
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谭玉虎
汤玲花
赵宗明
岳心圆
杨姬蓉
符敏
王平德
王飞
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Lanzhou Jinchuan Advangced Materials Technology Co ltd
Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
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    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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Abstract

A preparation method of large-particle-size aluminum-coated cobaltosic oxide comprises the following steps: preparing a solution, carrying out a synthesis reaction, coating an aluminum source, filtering, washing and drying. The invention realizes the rapid growth of the particles by the application of the additive; the aluminum source coated can be uniformly distributed in the cobaltosic oxide, and the aluminum source coated by hydroxyl groups is successfully realized.

Description

Preparation method of large-particle-size aluminum-coated cobaltosic oxide
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for preparing a high-voltage lithium cobaltate battery positive electrode material precursor aluminum-coated cobaltosic oxide.
Background
The lithium ion battery is a new green secondary battery, and has the advantages of high voltage, high capacity, small volume, light weight, long cycle life, good safety performance, no memory effect and the like, and is widely applied to various portable electronic products (mobile phones, PDAs, notebook computers, ipods and the like), and will become a main power source of electric vehicles and hybrid vehicles, and is considered to be the secondary battery with the most competitive and most development potential. In recent years, the high-speed development of portable electronic products has higher and higher requirements on the lightness and thinness of batteries, on one hand, the compacted density of the battery material needs to be ensured to be close to the theoretical density, and on the other hand, higher requirements on the gram specific capacity of lithium cobaltate are also provided. One of the most common cobalt sources for synthesizing lithium cobaltate is Co3O4, and the quality of the cobalt source directly influences the performance of the battery.
Portable electronic devices put increasing demands on battery performance, lithium cobaltate is developing towards high voltage, high compaction and high cycle performance, and the mainstream development direction of lithium battery electrode materials is basically determined, namely, the energy (mainly volume energy density) of the lithium battery is improved, and the lithium battery is still the basic development direction of small lithium batteries in the coming years. There are two main approaches to increasing energy density, either increasing the capacity of the battery material or increasing the operating voltage of the battery.
One of the effective methods for improving the working voltage of the battery is to improve the charging voltage of the material, and the structural stability and the surface morphology of the material can be effectively changed by doping modification or surface coating and other technical means on the lithium cobaltate, so that the commercial application of the high-voltage lithium cobaltate material is realized.
Therefore, it is important for the raw material cobaltosic oxide to prepare large-particle-size coated cobaltosic oxide.
The prior preparation process of hydroxyl large-particle-size aluminum-coated cobaltosic oxide has the following problems:
1. the grain diameter is difficult to grow, the proportion of small grains (micro powder) is high, and the influence on the subsequent preparation of the anode material is large;
2. the doping preparation method by adding the aluminum source into the solution has the defects of poor product appearance, small tap density and increased specific surface area, and the reason for the result is that Ksp (Co (OH)2】=1.6×10-15，Ksp【Al(OH)3】=1.9×10-33When the pH value of the composite is about 8.0, the precipitation speed of the aluminum ions is greatly higher than that of the cobalt ions. The rate of formation of Al (OH)3 is significantly greater than that of Co (OH)2Speed of formation of Al (OH)3The particles prevent the cobalt hydroxide from agglomerating and crystallizing to grow, so that the appearance of the final product is poor.
3. The aluminum source can not be uniformly dispersed in the cobaltosic oxide, and the aluminum content can not meet the design requirement.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of large-particle-size cobalt aluminum tetraoxide, which has the advantages of large particle size, compact appearance and uniform distribution of an aluminum source.
The invention relates to a preparation method of large-particle-size aluminum-coated cobaltosic oxide, which comprises the following steps of:
a. preparing a solution A with the cobalt concentration of Xg/L by taking cobalt salt as a raw material, preparing a solution B with the concentration of Yg/L by taking sodium hydroxide as a raw material, adding an ammonia water solution with the volume of 0.04-0.06 times and the concentration of 180-200g/L into the solution B, preparing an aluminum source solution with the concentration of Zg/L, and storing the prepared solution for later use;
b. a fixed volume of hot, pure water was added to each kettle as the synthesis buffer, and a certain amount of additives were added. Controlling the temperature and stirring in the process, then sequentially adding the solution A and the solution B, adjusting the flow rate of the solution A by stages, adjusting and controlling the pH =7.8-8.6 by stages, stabilizing the flow rate of the solution B according to the pH, synthesizing the solution B for 18-20 hours until the granularity reaches the required index, and performing subsequent processes;
c. after the synthesis is finished, the PH value of the fine adjustment system is 8.0-8.4, the adding flow of the aluminum source solution is controlled, the solution with a certain volume is added into a synthesis 1 kettle within 2-4 hours, the aging is carried out for 1 hour, and the next procedure is carried out after the aluminum source is fully combined;
d. after the coating is finished, the slurry is centrifugally washed by deionized water at the temperature of 80-100 ℃, dried at the temperature of 100-.
And in the step a, the cobalt salt is cobalt nitrate.
In the step a, the concentration of the solution A is 110-120g/L, the concentration of the solution B is 250-300g/L, and the concentration Z of the aluminum source is 4-6 g/L.
The addition amount in the step b is as follows: 3-7L.
The flow rate of the solution A in the step B is 100-400L/h, and the flow rate of the solution B is 200-300L/h.
The flow rate of the solution A in the step b is adjusted in stages as follows: 1-15 h: 400L/h, after 15 h: 100L/h; the pH is adjusted in stages as: 1-10 h: 8.4-8.6, 10-15 h: 8.2-8.4, after 15 h: 7.8-8.2.
In the step c, the flow of the aluminum source is 200-400L/h, and the aluminum source is added in a downward liquid adding mode in a spraying mode.
The aluminum content of the large-particle-size aluminum-coated cobaltosic oxide in the step d is 2500-6000 ppm.
Compared with the prior art, the invention has the following advantages: the rapid growth of the particles is realized through the application of the additive; the aluminum source coated can be uniformly distributed in the cobaltosic oxide, and the aluminum source coated by hydroxyl groups is successfully realized.
Drawings
FIG. 1 is a flow chart of a process employing the present invention.
FIG. 2 is an SEM image of a cobalt hydroxide product obtained by the preparation method of the invention.
FIG. 3 is an SEM image of a calcined product obtained by the preparation method of the invention.
FIG. 4 is an EDS diagram of the product obtained by the preparation method of the invention.
FIG. 5 is a scanned graph of large particle size aluminum-coated cobaltosic oxide prepared by the preparation method of the present invention.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the large-particle-size aluminum-coated cobaltosic oxide shown in the figure 1 comprises the following steps of:
a. preparing a solution A with the cobalt concentration of Xg/L by taking cobalt salt as a raw material, preparing a solution B with the concentration of Yg/L by taking sodium hydroxide as a raw material, adding an ammonia water solution with the volume of 0.04-0.06 times and the concentration of 180-200g/L into the solution B, preparing an aluminum source solution with the concentration of Zg/L, and storing the prepared solution for later use;
b. a fixed volume of hot, pure water was added to each kettle as the synthesis buffer, and a certain amount of additives were added. Controlling the temperature and stirring in the process, then sequentially adding the solution A and the solution B, adjusting the flow rate of the solution A by stages, adjusting and controlling the pH =7.8-8.6 by stages, stabilizing the flow rate of the solution B according to the pH, synthesizing the solution B for 18-20 hours until the granularity reaches the required index, and performing subsequent processes;
c. after the synthesis is finished, the PH value of the fine adjustment system is 8.0-8.4, the adding flow of the aluminum source solution is controlled, the solution with a certain volume is added into a synthesis 1 kettle within 2-4 hours, the aging is carried out for 1 hour, and the next procedure is carried out after the aluminum source is fully combined;
d. after the coating is finished, the slurry is centrifugally washed by deionized water at the temperature of 80-100 ℃, dried at the temperature of 100-.
In the step a, the cobalt salt is cobalt nitrate, the concentration of the solution A is 110-120g/L, the concentration of the solution B is 250-300g/L, and the concentration Z of the aluminum source is 4-6 g/L; the addition amount in the step b is as follows: 3-7L, the flow rate of the solution A is 400L/h, the flow rate of the solution B is 200L/h, and the flow rate of the solution A is adjusted by stages as follows: 1-15 h: 400L/h, after 15 h: 100L/h; the pH is adjusted in stages as: 1-10 h: 8.4-8.6, 10-15 h: 8.2-8.4, after 15 h: 7.8-8.2; in the step c, the flow of the aluminum source is 200-400L/h, the adding mode of the aluminum source is a downward liquid adding mode, and the aluminum source is added in a spraying mode; the amount of aluminum contained in the large-particle-size aluminum-containing cobaltosic oxide in the step d is 2500-.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
1. Preparing a cobalt solution with the cobalt concentration of 115g/L as an A solution, a B solution with the concentration of 260g/L and an aluminum source solution with the concentration of 5.5 g/L. And adding 0.05 time volume of ammonia water solution with the concentration of 180g/L into the solution B.
2. Adding 1m of the mixture into each kettle3The hot purified water of (2) was used as a synthesis buffer, and 5L of an additive was added. Controlling the temperature at 74-76 ℃, stirring at the rotating speed of 35HZ, and then sequentially adding the solution A and the solution B, wherein the flow rate of the solution A is controlled as follows: 1-15 h: 400 +/-5L/h; after 15 h: 100 +/-5L/h; and then, controlling the pH =7.8-8.6 according to the process, stabilizing the flow of the solution B, synthesizing for 20-25 hours, and performing subsequent procedures after D50 reaches 15.0-16.0 um.
3. After the synthesis is finished, the PH value of the system is adjusted to 8.3, the adding flow of the aluminum source solution is controlled to be 300 +/-5L/h, the aluminum source is added into the synthesis kettle within 3 hours, and the next procedure is carried out after the aging is carried out for 1 hour.
4. Centrifugally washing the slurry with deionized water at 85 ℃ for 3 hours, drying at 110 ℃, and calcining in a rotary kiln at 750-800 ℃ to obtain the large-particle-size aluminum-coated cobaltosic oxide product.
Figure DEST_PATH_IMAGE001
Figure 888241DEST_PATH_IMAGE002
Figure 867698DEST_PATH_IMAGE004
By adopting high-concentration and high-flow solution and adjusting the process flow and the pH stage, the particle size distribution after synthesis is uniform, the product has no micro powder and compact appearance; the additive is adopted, so that the rapid growth of the particles is realized; the aluminum source is added in a spraying mode by adopting a mode of coating the aluminum source, the coated aluminum source is uniformly infiltrated, the product is compact in shape and shape, and the use requirement of high-voltage lithium cobalt oxide is met.
The above description is only for the preferred embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept thereof within the scope of the present invention.

Claims (8)

1. A preparation method of large-particle-size aluminum-coated cobaltosic oxide is characterized by comprising the following steps of:
a. preparing a solution A with the cobalt concentration of Xg/L by taking cobalt salt as a raw material, preparing a solution B with the concentration of Yg/L by taking sodium hydroxide as a raw material, adding an ammonia water solution with the volume of 0.04-0.06 times and the concentration of 180-200g/L into the solution B, preparing an aluminum source solution with the concentration of Zg/L, and storing the prepared solution for later use;
b. adding hot pure water with a fixed volume as a synthesis buffer solution into each kettle, and adding a certain amount of additives;
controlling the temperature and stirring in the process, then sequentially adding the solution A and the solution B, adjusting the flow rate of the solution A by stages, adjusting and controlling the pH =7.8-8.6 by stages, stabilizing the flow rate of the solution B according to the pH, synthesizing the solution B for 18-20 hours until the granularity reaches the required index, and performing subsequent processes;
c. after the synthesis is finished, the PH value of the fine adjustment system is 8.0-8.4, the adding flow of the aluminum source solution is controlled, the solution with a certain volume is added into a synthesis 1 kettle within 2-4 hours, the aging is carried out for 1 hour, and the next procedure is carried out after the aluminum source is fully combined;
d. after the coating is finished, the slurry is centrifugally washed by deionized water at the temperature of 80-100 ℃, dried at the temperature of 100-.
2. The method for preparing large-particle-size aluminum-coated cobaltosic oxide according to claim 1, wherein the method comprises the following steps: and in the step a, the cobalt salt is cobalt nitrate.
3. The method for preparing large-particle-size aluminum-coated cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step a, the concentration of the solution A is 110-120g/L, the concentration of the solution B is 250-300g/L, and the concentration Z of the aluminum source is 4-6 g/L.
4. The method for preparing large-particle-size aluminum-coated cobaltosic oxide according to claim 1, wherein the method comprises the following steps: the addition amount in the step b is as follows: 3-7L.
5. The method for preparing large-particle-size aluminum-coated cobaltosic oxide according to claim 1, wherein the method comprises the following steps: the flow rate of the solution A in the step B is 100-400L/h, and the flow rate of the solution B is 200-300L/h.
6. The method for preparing large-particle-size aluminum-coated cobaltosic oxide according to claim 1, wherein the method comprises the following steps: the flow rate of the solution A in the step b is adjusted in stages as follows: 1-15 h: 400L/h, after 15 h: 100L/h; the pH is adjusted in stages as: 1-10 h: 8.4-8.6, 10-15 h: 8.2-8.4, after 15 h: 7.8-8.2.
7. The method for preparing large-particle-size aluminum-coated cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step c, the flow of the aluminum source is 200-400L/h, and the aluminum source is added in a downward liquid adding mode in a spraying mode.
8. The method for preparing large-particle-size aluminum-coated cobaltosic oxide according to claim 1, wherein the method comprises the following steps: the aluminum content of the large-particle-size aluminum-coated cobaltosic oxide in the step d is 2500-6000 ppm.
CN202110980495.9A 2021-08-25 2021-08-25 Preparation method of large-particle-size aluminum-coated cobaltosic oxide Pending CN113735182A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114604881A (en) * 2022-03-24 2022-06-10 昆明理工大学 Preparation method of hydroxyl nano-alumina with controllable hydroxyl content
CN115259237A (en) * 2022-06-30 2022-11-01 金川集团股份有限公司 Method for eliminating cobalt hydroxide micropowder

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114604881A (en) * 2022-03-24 2022-06-10 昆明理工大学 Preparation method of hydroxyl nano-alumina with controllable hydroxyl content
CN114604881B (en) * 2022-03-24 2022-11-25 昆明理工大学 Preparation method of hydroxyl nano-alumina with controllable hydroxyl content
CN115259237A (en) * 2022-06-30 2022-11-01 金川集团股份有限公司 Method for eliminating cobalt hydroxide micropowder

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