CN214486904U

CN214486904U - Device for preparing layered precursors in various proportions

Info

Publication number: CN214486904U
Application number: CN202120770459.5U
Authority: CN
Inventors: 欧阳毅; 高炯信; 邱天; 郭美鑫; 汪镇涛; 肖亚威
Original assignee: Huayou New Energy Technology Quzhou Co ltd; Zhejiang Huayou Cobalt Co Ltd
Current assignee: Huayou New Energy Technology Quzhou Co ltd; Zhejiang Huayou Cobalt Co Ltd
Priority date: 2021-04-15
Filing date: 2021-04-15
Publication date: 2021-10-26
Anticipated expiration: 2031-04-15

Abstract

The utility model discloses a device for preparing layered precursors with various proportions. The utility model discloses a reation kettle I, reation kettle II, the overflow pipe, the circulating pump, go out clarified pump I, go out clarified pump II, mother liquor pond and thick liquids groove, reation kettle I meets through overflow pipe and reation kettle II, the import of circulating pump meets with reation kettle II, the export of circulating pump meets with reation kettle I, I bottom of reation kettle meets with the import of going out clarified pump I, reation kettle II's bottom meets with the import of going out clarified pump II, the export of going out clarified pump I and going out clarified pump II all meets with the mother liquor pond, reation kettle I and reation kettle II's top is equipped with the raw materials import, reation kettle I and reation kettle II's bottom all is equipped with the discharge valve, the discharge valve meets with the thick liquids groove, reation kettle I and reation kettle II's inside all is equipped with agitating unit. The utility model discloses can design the precursor granule that obtains stratiform nuclear shell structure according to required product requirement, synthesize the precursor of the different proportion main content of multiple stratiform.

Description

Device for preparing layered precursors in various proportions

Technical Field

The utility model relates to a ternary precursor synthesizer, especially a device of preparation multiple proportion stratiform precursor.

Background

The lithium ion battery has a huge application prospect in the new energy automobile market by virtue of the characteristics of high capacity, low pollution, high power and the like, and the ternary precursor has a good development space when being used as the anode of the lithium ion battery due to strong comprehensive performance. The ternary material is one of the positive electrode materials of the lithium battery, has the advantages of good safety, high gram specific capacity, low price and the like, becomes one of the development directions of the lithium battery industry in the future, and has mature application technology and good market prospect.

In recent years, the operating voltage of consumer lithium batteries is higher and higher, and the requirements on the mass energy density, safety performance and the like of the cathode material are also higher and higher. The prior technical method for improving the high-voltage performance of the lithium ion battery comprises bulk phase doping, a core-shell structure and the like; the lithium battery anode material with the core-shell structure is the most fully researched and widely applied consumer lithium battery anode material at present. The core-shell structure is considered to be a structure with flexible and variable performance adjustment, can realize the doping of a core pure phase and a shell, or different pure phases of the core and the shell, and can develop the doping of concentration gradient from the core to the shell.

The core-shell structure generally adopts a material structure with a more stable structure and high rate performance as a shell, because in the lithium ion battery, the shell is directly contacted with the electrolyte, the shell layer is impacted by the electrolyte lithium ions, the lithium ions migrate into the first station of the migration in the charge-discharge process, and the crystal structure collapse of the lithium ion battery starts from the surface shell layer; the core of the core-shell structure is a core-shell structure anode material with a layered structure, the core part of the core-shell structure can ensure the mass energy density, and the shell part of the core-shell structure has better high-temperature stability and can simultaneously meet the requirements of high energy density and high safety performance.

However, the precursors prepared at present have the problems of uneven distribution of shells, complex device and high investment.

SUMMERY OF THE UTILITY MODEL

Be difficult to obtain the lamellar nucleocapsid structure to present coprecipitation preparation precursor in-process, the utility model provides a device of multiple proportion lamellar precursor body, it can be according to the required product of required product requirement design preparation and obtain the precursor granule of lamellar nucleocapsid structure, makes the nucleocapsid structure element distribution of precursor granule even to improve the security performance, the cyclicity ability and the specific capacity of the anodal material of follow-up preparation.

Therefore, the utility model discloses a technical scheme is: the device for preparing the layered precursors with various proportions comprises a reaction kettle I, a reaction kettle II, an overflow pipe, a circulating pump, a cleaning pump I, a cleaning pump II, a mother liquor pool and a slurry tank, wherein the reaction kettle I is connected with the reaction kettle II through the overflow pipe, the inlet of the circulating pump is connected with the reaction kettle II, the outlet of the circulating pump is connected with the reaction kettle I, the bottom of the reaction kettle I is connected with the inlet of the cleaning pump I, the bottom of the reaction kettle II is connected with the inlet of the cleaning pump II, the outlets of the cleaning pump I and the cleaning pump II are connected with the mother liquor pool, the tops of the reaction kettle I and the reaction kettle II are provided with raw material inlets, the bottoms of the reaction kettle I and the reaction kettle II are provided with discharge valves, the discharge valves are connected with the slurry tank, and the insides of the reaction kettle I and the reaction kettle II are provided with stirring devices; the filter rods are arranged inside the reaction kettle I and the reaction kettle II, the filter rods in the reaction kettle I are connected with the discharge pump I through pipelines, and the filter rods in the reaction kettle II are connected with the discharge pump II through pipelines.

In the device for preparing the layered precursors with various proportions, the horizontal height of the interface of the reaction kettle I connected with the overflow pipe is higher than that of the reaction kettle II.

According to the device for preparing the layered precursors in various proportions, the liquid level in the reaction kettle I is ensured to be stable by interlocking the cleaning pump I with the liquid level in the reaction kettle I.

According to the device for preparing the layered precursors in various proportions, the discharge pump II is interlocked with the liquid level in the reaction kettle II, so that the liquid level in the reaction kettle II is stable.

The device for preparing the layered precursors in various proportions is characterized in that a regulating valve is arranged between a circulating pump and a reaction kettle I, and the regulating valve is linked with a cleaning pump I and a cleaning pump II to jointly control the liquid level stability of the reaction kettle I and the reaction kettle II.

The utility model discloses the beneficial effect who has as follows: the utility model solves the problems that the layered core-shell structure precursor is difficult to obtain in the process of preparing the precursor by coprecipitation at present, and the precursor particles with different uniform proportion internal structures are prepared according to the problems of the cycle life, the stability and the like of the precursor at present; precursor particles with a layered core-shell structure can be designed and prepared according to the requirements of required products, various layered precursors with different proportion main contents are synthesized, the internal structure of the precursor is effectively improved, and the problem of unstable structure of the nickel-cobalt-manganese-based oxide anode material is solved. The utility model is simple in operation, the nucleocapsid structure element of the precursor granule that obtains distributes evenly, has further promoted holistic structural stability, and the better improvement the positive electrode material's of follow-up preparation security performance, cyclicity performance and specific capacity, realized the production of one set of multiple product of device. The utility model discloses but the wide application is in the production technology of lithium cell positive pole material precursor, especially is applicable to the production technology of multiple stratiform lithium cell positive pole material precursor.

Drawings

Fig. 1 is a schematic structural view of the present invention;

in figure 1, 1 is reation kettle I, 2 is the filter rod, 3 is the slurry tank, 4 is the pump I of going out the clear, 5 is the pump II of going out the clear, 6 is the mother liquor pond, 7 is reation kettle II, 8 is the circulating pump, 9 is the overflow pipe, 10 is the governing valve, 11 is agitating unit, 12 is the discharge valve.

Detailed Description

Referring to the attached figure 1, the device for preparing the layered precursors with various proportions comprises a reaction kettle I, a reaction kettle II, an overflow pipe, a circulating pump, a cleaning pump I, a cleaning pump II, a mother liquor pool and a slurry tank, wherein the reaction kettle I is connected with the reaction kettle II through the overflow pipe, an inlet of the circulating pump is connected with the reaction kettle II, an outlet of the circulating pump is connected with the reaction kettle I, the bottom of the reaction kettle I is connected with an inlet of the cleaning pump I, the bottom of the reaction kettle II is connected with an inlet of the cleaning pump II, outlets of the cleaning pump I and the cleaning pump II are connected with the mother liquor pool, raw material inlets are formed in the tops of the reaction kettle I and the reaction kettle II, discharge valves are arranged at the bottoms of the reaction kettle I and the reaction kettle II and are connected with the slurry tank, and stirring devices are arranged inside the reaction kettle I and the reaction kettle II; the filter rods are arranged inside the reaction kettle I and the reaction kettle II, the filter rods in the reaction kettle I are connected with the discharge pump I through pipelines, and the filter rods in the reaction kettle II are connected with the discharge pump II through pipelines.

The difference of another embodiment is that the level of the interface of the reaction kettle I connected with the overflow pipe is higher than that of the reaction kettle II.

The difference of another embodiment is that the discharge pump I is interlocked with the liquid level in the reaction kettle I to ensure the liquid level in the reaction kettle I to be stable.

The difference of the other embodiment is that the discharge pump II is interlocked with the liquid level in the reaction kettle II to ensure the stability of the liquid level in the reaction kettle II.

The difference of another embodiment lies in that a regulating valve is arranged between a circulating pump and a reaction kettle I, and the regulating valve is interlocked with a cleaning pump I and a cleaning pump II to jointly control the liquid level stability of the reaction kettle I and the reaction kettle II.

The utility model discloses an operating procedure as follows:

step 1, according to the requirements of metal elements in a required layered precursor, preparing a metal liquid I and a metal liquid II by adopting one or more of nickel sulfate, cobalt sulfate, manganese sulfate, nickel nitrate, cobalt nitrate, manganese nitrate, nickel chloride, cobalt chloride, manganese chloride, aluminum sulfate, aluminum nitrate and aluminum chloride respectively; the metal liquid I and the metal liquid II are not the same substance;

step 2, preparing a sodium hydroxide solution with the mass concentration of 3-32.5%;

step 3, preparing ammonia water with the mass concentration of 3-22% as a complexing agent;

step 4, adding pure water into the reaction kettle I until the pure water overflows the bottom layer stirring paddle, and then adding the sodium hydroxide solution prepared in the step 2 and the ammonia water prepared in the step 3 to form a bottom solution for starting up the reaction;

step 5, adding the metal liquid I prepared in the step 1, the sodium hydroxide solution prepared in the step 2 and the ammonia water prepared in the step 3 into a reaction kettle I in a concurrent flow manner for reaction, and controlling the reaction temperature, the pH value, the ammonia concentration and the stirring rotating speed;

step 6, continuing feeding according to the step 5, gradually raising the liquid level of the reaction kettle I, overflowing the slurry to the reaction kettle II through an overflow pipe, starting a discharge pump I when the liquid level of the reaction kettle II reaches the total height 1/3 in the tank and above, and enabling the mother liquor in the reaction kettle I to enter a mother liquor pool through the filter stick and the discharge pump I;

step 7, adding the metal liquid II prepared in the step 1, the sodium hydroxide solution prepared in the step 2 and the ammonia water prepared in the step 3 into a reaction kettle II in a concurrent flow manner for reaction, controlling the reaction temperature, the pH value, the ammonia concentration and the stirring rotating speed, starting a discharging pump II, and enabling the mother liquor in the reaction kettle II to enter a mother liquor pool through a filter stick and the discharging pump II;

step 8, starting a circulating pump according to the layered requirement of a target precursor, preparing precursors with uniform laminated structures in different proportions by controlling the flow of the circulating pump, and preparing precursors with multilayer annular core-shell structures by discontinuously controlling the input of metal liquids in different proportions; when the concentrations of the metal liquid I and the metal liquid II are constant, the metal liquid I and the metal liquid II in different proportions are controlled to be introduced, so that precursors with different proportions of annular multilayer core-shell structures can be prepared, and precursors with different proportions of primary particle laminated structures can also be prepared by controlling the flow of a circulating pump of a reaction kettle; when the concentrations of the metal liquid I and the metal liquid II are set to be linearly changed, the method can be used for preparing precursor products in concentration gradient distribution;

and 9, stopping feeding when the granularity of the materials in the reaction kettle meets the required requirement, opening a discharge valve of the reaction kettle, and conveying the materials to the subsequent process for treatment.

In the synthesis process, metal liquid with different proportions is put into the primary and secondary kettles, and the two kettles are continuously mixed through overflow and a circulating pump, so that the sizes of primary particles with different proportions in the kettles are uniformly controlled, the sizes of the primary particles with different proportions can be controlled to be 20-2000 nm, the primary particles are uniformly distributed in a laminated manner, metal liquid with different proportions can be put into the metal liquid feeding groove in a staged mode, precursors of annular layer structures with different proportions and different sizes are controlled, and the thicknesses of the annular layers with different proportions are 0.1-10 mu m.

Claims

1. The device for preparing the layered precursors in various proportions is characterized by comprising a reaction kettle I (1), a reaction kettle II (7), an overflow pipe (9), a circulating pump (8), a clear liquid outlet pump I (4), a clear liquid outlet pump II (5), a mother liquid pool (6) and a slurry tank (3);

the reaction kettle I (1) is connected with the reaction kettle II (7) through an overflow pipe (9), the inlet of a circulating pump (8) is connected with the reaction kettle II (7), the outlet of the circulating pump (8) is connected with the reaction kettle I (1), the bottom of the reaction kettle I (1) is connected with the inlet of a supernatant pump I (4), the bottom of the reaction kettle II (7) is connected with the inlet of a supernatant pump II (5), and the outlets of the supernatant pump I (4) and the supernatant pump II (5) are connected with a mother liquor pool (6);

the top parts of the reaction kettle I (1) and the reaction kettle II (7) are provided with raw material inlets, the bottom parts of the reaction kettle I (1) and the reaction kettle II (7) are respectively provided with a discharge valve (12), and the discharge valves (12) are connected with the slurry tank (3);

stirring devices (11) are arranged in the reaction kettle I (1) and the reaction kettle II (7);

the filter stick cleaning device is characterized in that filter sticks (2) are arranged inside the reaction kettle I (1) and the reaction kettle II (7), the filter sticks (2) in the reaction kettle I (1) are connected with the cleaning pump I (4) through pipelines, and the filter sticks (2) in the reaction kettle II (7) are connected with the cleaning pump II (5) through pipelines.

2. The apparatus for preparing multi-ratio layered precursors of claim 1, wherein: the horizontal height of the interface of the reaction kettle I (1) connected with the overflow pipe (9) is higher than that of the reaction kettle II (7).

3. The apparatus for preparing multi-ratio layered precursors of claim 1, wherein: go out liquid level chain in clarified pump I (4) and reation kettle I (1), guarantee that the liquid level in reation kettle I (1) is stable.

4. The apparatus for preparing multi-ratio layered precursors of claim 1, wherein: and the discharge pump II (5) is interlocked with the liquid level in the reaction kettle II (7), so that the stability of the liquid level in the reaction kettle II (7) is ensured.

5. The apparatus for preparing multi-ratio layered precursors of claim 1, wherein: be equipped with governing valve (10) between circulating pump (8) and reation kettle I (1), governing valve (10) are chain with play clear pump I (4), play clear pump II (5), and the liquid level in controlling reation kettle I (1) and reation kettle II (7) jointly is stable.