Full-automatic positive lithium supplement material continuous production device and production method thereof

Abstract

The invention provides a full-automatic continuous production device and method for a positive electrode lithium supplement agent material, and belongs to the technical field of positive electrode material production equipment. According to the continuous production device, a stock bin, a high mixing machine, a box-type furnace, a crusher, a screening machine and a bagging machine are sequentially connected through a material conveying pipe, the crusher, the screening machine and the bagging machine are located in a drying room, the material conveying pipe is a cylindrical 304 stainless steel pipe capable of being freely bent, a spiral rotatable crawler belt is embedded in the material conveying pipe, and a signal sensor is arranged in the material conveying pipe. The automatic feeding device can automatically receive a feeding signal of a previous workshop section device and automatically transfer materials into a next workshop section device. According to the device, one-key full-process preparation from the raw materials to the positive electrode lithium supplementing agent material is realized, and the preparation process only needs to set a program in advance without manual participation, so that the preparation efficiency of the positive electrode lithium supplementing agent material can be greatly improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of positive electrode material production equipment, and in particular relates to a full-automatic positive electrode lithium supplement material continuous production device and a production method thereof. Background Art

[0002] During the first cycle of the battery, there are processes such as the formation of negative electrode SEI, deactivation of negative electrode material particles due to shedding, and irreversible deposition of lithium metal, which consume the active lithium of the positive electrode and reduce the available energy of the battery. By increasing the content of active lithium source, the loss of active lithium in the first cycle of charge and discharge is pre-compensated. This process is called "pre-lithiation or lithium replenishment". Therefore, lithium replenishment technology can pre-compensate for the loss of active lithium in the first cycle of charge and discharge, thereby improving the first cycle coulomb efficiency of the battery, and then improving the battery energy density and cycle performance.

[0003] Lithium replenishment technology is divided into negative electrode replenishment and positive electrode replenishment. Negative electrode replenishment often uses lithium foil, lithium ribbon and other metal lithium as a lithium replenisher, which has extremely high requirements for device operation and environment, so it has not been industrialized for many years; positive electrode replenisher materials have reduced sensitivity to the environment, and the battery preparation process is highly compatible, and are gradually promoted and applied downstream. The lithium replenishers that are currently receiving more market attention are lithium-rich nickel oxide (LNO) and lithium-rich lithium iron oxide (LFO) and their doped and modified forms. Among them, LNO was first industrialized in the ternary-silicon negative electrode system. LFO has a higher lithium replenishment capacity (actual performance exceeds 650mAh / g), and has a higher cost-effectiveness than LNO. It is considered to be a second-generation positive electrode lithium replenisher that can replace LNO. At present, positive electrode replenisher material manufacturers such as Defang Nano, Shanshan, and Xia Tungsten are competing for layout, ushering in the era of lithium replenishers.

[0004] CN217450111U discloses an integrated device for washing, filtering and drying positive electrode materials for lithium ion batteries, which includes a kettle, a filter element and a jacket; CN209752982U provides an integrated device for filtering and crushing a precursor of lithium battery positive electrode materials, which includes a filter press, a feed pipe, a silo, a bipolar pair of rollers, and a concave material trough; CN218637064U discloses a processing device for lithium battery positive electrode materials, including a stirring component and a filtering component; the surface of the processing device is connected with a stirring component that runs through it, and the side surface is connected with a filtering component that runs through it. The stirring filter integrates the stirring link and the filtering link, which can eliminate the transportation time in the stirring link and the filtering link, thereby improving the overall work efficiency. However, the integrated device disclosed in the above patent is only a post-processing device for positive electrode materials, and has a single type of use. There is no integrated continuous device for the preparation of positive electrode lithium replenisher materials. In addition, the existing positive electrode lithium replenisher material preparation devices are mostly intermittent production devices with low intelligence and complicated operation. They require a lot of manual participation, which is not conducive to improving efficiency, and therefore cannot meet the needs of positive electrode material preparation. Summary of the invention

[0005] The present invention provides a fully automatic continuous production device for positive electrode lithium replenisher materials and a production method thereof. The device can realize the full process preparation from raw materials to positive electrode lithium replenisher materials with one click, and the preparation process only needs to set the program in advance without manual participation, which can greatly improve the preparation efficiency of positive electrode lithium replenisher materials.

[0006] In order to achieve the above-mentioned purpose, the present invention provides a fully automatic continuous production device for positive electrode lithium supplement materials, wherein six work section devices including a silo, a high-speed mixer, a box furnace, a crusher, a screener and a bagger are connected in sequence through a feed pipe, and the crusher, the screener and the bagger are located in a drying room, wherein the feed pipe is a cylindrical freely bendable 304 stainless steel pipe with an embedded spiral rotatable crawler and a built-in signal sensor, which can automatically receive the discharge signal of the previous work section device and automatically transfer the material to the next work section device.

[0007] Preferably, an automatic sensor is installed below the silo. When a feed signal is received, the valve at the bottom of the silo opens and automatically discharges quantitative material into the feed pipe.

[0008] Preferably, the feed port of the high-speed mixer is connected to the feed pipe through a flange, and an automatic operation sensor is installed in the high-speed mixer. When the automatic operation sensor detects that the feeding at the feed port is completed, the valve automatically closes, and the high-speed mixer automatically operates according to the set program. After the mixing is completed, the discharge port valve automatically opens, and the feed pipe at one end of the discharge port automatically operates to transport the material to the box furnace.

[0009] Preferably, an automatic feed port is installed in the box-type furnace, and the automatic feed port is connected to the feed pipe through a flange. A quality sensor is also provided in the box-type furnace. When receiving the set mass material, the signal is transmitted to the feed pipe connected to the feed port, the feed pipe automatically stops feeding, and the box-type furnace automatically closes the feed port valve. The box-type furnace automatically runs according to the set program. After sintering is completed, the material automatically cools down, and the upper insulation layer in the box-type furnace cavity automatically opens. The box-type furnace cavity has built-in scrapers and vacuum material collection devices. When the box-type furnace temperature sensor recognizes that the temperature drops to room temperature, the scrapers and vacuum material collection devices automatically collect the material in the sagger into the feed pipe, and the feed pipe transfers the material to the air flow pulverizer in the drying room.

[0010] Preferably, the feed port and the discharge port of the air flow pulverizer are connected to the feed pipe by flange means. After the air flow pulverizer receives the automatic feeding completion signal from the feed pipe, the feed port valve is automatically closed, and the air flow pulverizer automatically runs. The air flow pulverizer has a built-in particle size detection unit, which automatically adjusts the pulverizing time and pulverizing pressure by detecting the particle size. After the pulverizing is completed, the material is transported to the screening machine through the feed pipe.

[0011] Preferably, the feed port and the discharge port of the screening machine are connected to the feed pipe by flange means. After the screening machine receives the feeding completion signal from the feed pipe, the feed port valve is automatically closed, and the screening machine automatically runs according to the set program. The screening machine has a built-in automatic discharge device to transport the screened materials to the feed pipe. The feed pipe starts running after detecting the feeding signal and transports the materials to the bagging machine.

[0012] Preferably, the feeding port of the bagging machine is connected to the feeding pipe by flange means, and the bagging machine is equipped with a quality sensor to automatically vacuum pack and seal materials of a set mass, wherein the bagging machine and the feeding pipe do not operate at the same time.

[0013] The present invention also provides a method for producing a positive electrode lithium supplement material using the continuous production device described in any one of the above technical solutions, comprising the following steps:

[0014] Add enough raw materials into the silo, and start the program with one button through the intelligent control cabinet. The valve at the bottom of the silo opens, and the materials are quantitatively fed into the feeding pipe. The feeding pipe detects the entry of materials and starts running automatically, and transports the materials to the high-speed mixer.

[0015] After the high-speed mixer detects the incoming material information, it opens the inlet valve. After the feeding of the conveying pipe is completed, the inlet valve of the high-speed mixer is closed, and the high-speed mixer starts to run automatically according to the set program. After the mixing is completed, the outlet valve automatically opens and transmits the signal to the conveying pipe. At this time, the material is automatically discharged to the conveying pipe under the stirring action of the high-speed mixer blades. The conveying pipe detects the entry of the material and starts to run automatically, and conveys the material to the box furnace;

[0016] After the box-type furnace detects the incoming material information, it opens the feed inlet valve. After the feeding of the feeding pipe is completed, the box-type furnace automatically closes the feed inlet valve and automatically operates according to the set program. When the operation is completed and the material temperature drops to room temperature, the box-type furnace discharge port opens, and the scraper and vacuum device in the insulation layer above the box-type furnace automatically transport the material in the sagger to the feeding pipe. The feeding pipe detects the entry of the material and automatically starts to operate, and transports the material to the airflow mill in the drying room;

[0017] After the airflow mill detects the incoming material information, the feed inlet valve is opened. After the feeding of the feeding pipe is completed, the airflow mill feed inlet valve is closed and automatically operates according to the set program. When the operation is completed, the airflow mill outlet is automatically opened, and the vacuum device of the airflow mill transports the material to the feeding pipe. After the feeding pipe detects the incoming material information, it automatically operates and transports the material to the screening machine.

[0018] After the screening machine detects the incoming material information, it opens the feed inlet valve. After the feeding of the feeding pipe is completed, the screening machine feed inlet valve is closed and automatically operates according to the set program. When the operation is completed, the screening machine outlet automatically opens, and the vacuum device of the screening machine transports the material to the feeding pipe. After the feeding pipe detects the incoming material information, it automatically operates and transports the material to the bagging machine.

[0019] After the bagging machine detects the incoming material information, it opens the feed port valve, and the material begins to be transmitted to the bagging machine through the feed pipe. After the material transmission is completed, the feed port valve of the bagging machine automatically closes, and the material is vacuum-sealed to obtain the positive electrode lithium supplement material.

[0020] As a preferred embodiment, the raw materials added to the silo are LiOH / Li2O / Li2CO3 / LiNO3 powder and Fe2O3 / FePO4 / / Fe(NO 3)3 / FeCl3 / FeSO4 powder, the two are mixed in a ratio of lithium iron (5-6):1;

[0021] The mixing time of the raw materials in the high-speed mixer is 10-60 minutes, and the line speed is 20-30m / s;

[0022] The sintering temperature of the raw materials in the box furnace is 800-1000°C, the sintering time is 1-8h, the heating rate is 1-10°C / min, and the nitrogen flow rate is 1-10L / min;

[0023] The particle size of the obtained positive electrode lithium supplement material is 200-500 meshes.

[0024] Preferably, compared with manual operation between various process sections, the specific capacity of the positive electrode lithium replenisher material produced by the fully automatic positive electrode lithium replenisher material continuous production device that integrates various process sections and automatically transmits the material through a conveying pipe is at least 8% higher.

[0025] Compared with the prior art, the advantages and positive effects of the present invention are:

[0026] 1. The present invention develops a fully automatic continuous production device for positive electrode lithium supplement materials. The device is composed of a feeding pipe that connects six sections of the feeding section (silo), mixing section (high-speed mixer), sintering section (box furnace), crushing section (crusher), screening section (screening machine), and bagging section (bagging machine) in sequence. After the program is set by the intelligent control cabinet and started with one button, each section can cooperate closely to complete the process from raw materials to products without human intervention.

[0027] 2. Compared with the traditional positive electrode lithium replenisher material preparation device (which is an intermittent production device), which has a low degree of intelligence and requires a lot of manual participation, the fully automatic positive electrode lithium replenisher material continuous production device provided by the present invention can realize the production process from raw materials to products with one click, thereby increasing the stability of product batches; and due to the characteristics of the material absorbing water and being easy to deteriorate, the sintered material is directly transferred to the drying room through the feed pipe, thereby reducing the time the material stays in the air and reducing the risk of product deterioration. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 A schematic diagram of a fully automatic positive electrode lithium supplement material continuous production device provided by an embodiment of the present invention, wherein:

[0029] 1- Silo, 2- Drying room, 3- Conveying pipe, 4- Intelligent control cabinet, 5- High-speed mixer, 6- Box furnace, 7- Air flow mill, 8- Screening machine, 9- Bagging machine. DETAILED DESCRIPTION

[0030] The technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. It should be noted that the various section devices (high mixer, box furnace, air flow mill, screening machine, bagging machine) in the following fully automatic continuous production device for positive electrode lithium supplement materials are all commercialized devices.

[0031] In an embodiment of the present invention, a fully automatic positive electrode lithium supplement material continuous production device is provided, such as Figure 1 As shown, the six working section devices, namely, the silo (1), the high-speed mixer (5), the box furnace (6), the crusher (7), the screener (8) and the bagging machine (9), are connected in sequence through a conveying pipe, and the crusher (7), the screener (8) and the bagging machine (9) are located in a drying room with a dew point of -30°C, wherein the conveying pipe (3) is a cylindrical, freely bendable 304 stainless steel pipe with a spiral rotatable crawler embedded therein and a built-in signal sensor, which can automatically receive the discharge signal of the previous working section device and automatically transfer the material to the next working section device.

[0032] In a preferred embodiment, an automatic sensor is installed below the silo (1). When a feed signal is received, the valve at the bottom of the silo will open and automatically discharge quantitative materials into the feed pipe (3).

[0033] In a preferred embodiment, the feed port of the high-speed mixer (5) is connected to the feed pipe (3) through a flange, and the high-speed mixer (5) is equipped with an automatic operation sensor. After the automatic operation sensor detects that the feed port is fed, the feed port valve of the high-speed mixer (5) is automatically closed, and the high-speed mixer (5) automatically operates according to the set program. After the mixing is completed, the discharge port valve automatically opens, and the feed pipe at one end of the discharge port automatically operates to transport the material to the next stage device.

[0034] In a preferred embodiment, an automatic feed port is provided in the box-type furnace (6), and the automatic feed port is connected to the feed pipe (3) through a flange. The box-type furnace (6) is provided with a mass sensor. When receiving a set mass of material, a signal is transmitted to the feed pipe (3) connected to the feed port, and the feed pipe (3) automatically stops feeding. The box-type furnace (6) automatically closes the feed port valve. The box-type furnace (6) automatically operates according to the set program. After sintering is completed, the material automatically cools down. The upper insulation layer in the furnace cavity of the box-type furnace (6) automatically opens. A scraper and a vacuum material collection device are built into the furnace cavity of the box-type furnace (6). When the temperature sensor of the box-type furnace (6) recognizes that the temperature has dropped to room temperature, the scraper and the vacuum material collection device automatically collect the material in the sagger into the feed pipe (3), and the feed pipe (3) transfers the material to the air flow pulverizer (7) in the drying room (2).

[0035] In a preferred embodiment, the feed port and the discharge port of the air flow pulverizer (7) are connected to the feed pipe (3) by flange means. After the air flow pulverizer (7) receives the automatic feeding completion signal from the feed pipe (3), the feed port valve is automatically closed, and the air flow pulverizer (7) automatically operates. The air flow pulverizer (7) has a built-in particle size detection function, and automatically adjusts the pulverization time and pulverization pressure by detecting the particle size. After the pulverization is completed, the material is transported to the screening machine (8) through the feed pipe (3).

[0036] In a preferred embodiment, the feed port and the discharge port of the screening machine (8) are connected to the feed pipe (3) by flange means. After the screening machine (8) receives a signal indicating that the feeding is completed from the feed pipe (3), the feed port valve is automatically closed, and the screening machine (8) automatically operates according to a set program. The screening machine (8) is equipped with a built-in automatic discharge device to transport the screened material to the feed pipe (3). After the feed pipe (3) detects the feeding signal, it starts to operate and transports the material to the bagging machine.

[0037] In a preferred embodiment, the feeding port of the bagging machine (9) is connected to the feeding pipe (3) by flange means, and the bagging machine (9) is equipped with a quality sensor, which can automatically vacuum pack and seal materials of a set mass, and the bagging machine (9) and the feeding pipe (3) do not operate at the same time.

[0038] The embodiment of the present invention also provides a method for producing a positive electrode lithium supplement material using the above-mentioned continuous production device, comprising the following steps:

[0039] A sufficient amount of raw materials is added to the silo (1), and after the program is set by the intelligent control cabinet (4) and one-key start is performed, the valve at the bottom of the silo (1) is opened, and the materials are quantitatively fed into the feed pipe (3). The feed pipe (3) automatically starts to operate when it detects the entry of materials, and transports the materials to the high-speed mixer (5);

[0040] After the high-speed mixer (5) detects the incoming material information, it opens the inlet valve. After the feeding of the conveying pipe (3) is completed, the inlet valve of the high-speed mixer (5) is closed, and the high-speed mixer (5) starts to automatically operate according to the set program. After the mixing is completed, the outlet valve automatically opens and transmits the signal to the conveying pipe (3). At this time, the material is automatically discharged to the conveying pipe (3) under the stirring action of the blades of the high-speed mixer (5). The conveying pipe (3) detects that the material has entered and automatically starts to operate, and conveys the material to the box furnace (6);

[0041] After the box-type furnace (6) detects the incoming material information, it opens the feed inlet valve. After the feeding of the feeding pipe (3) is completed, the box-type furnace (6) automatically closes the feed inlet valve and automatically operates according to the set program. When the operation is completed and the material temperature drops to room temperature, the discharge port of the box-type furnace (6) is opened, and the scraper and vacuum device in the insulation layer above the box-type furnace (6) automatically transport the material in the sagger to the feeding pipe (3). The feeding pipe (3) detects the entry of the material and automatically starts to operate, and transports the material to the air flow mill (7) in the drying room (2);

[0042] After the air flow mill (7) detects the incoming material information, the feed inlet valve is opened. After the feeding of the feeding pipe (3) is completed, the feed inlet valve of the air flow mill (7) is closed and automatically operates according to the set program. When the operation is completed, the discharge port of the air flow mill (7) is automatically opened, and the vacuum device of the air flow mill (7) transports the material to the feeding pipe (3). After the feeding pipe (3) detects the incoming material information, it automatically operates and transports the material to the screening machine (8);

[0043] After the screening machine (8) detects the incoming material information, the feeding port valve is opened. After the feeding of the feeding pipe (3) is completed, the feeding port valve of the screening machine (8) is closed and automatically operates according to the set program. When the operation is completed, the discharge port of the screening machine (8) is automatically opened, and the vacuum device of the screening machine (8) transports the material to the feeding pipe (3). After the feeding pipe (3) detects the incoming material information, it automatically operates and transports the material to the bagging machine (9);

[0044] After the bagging machine (9) detects the incoming material information, it opens the feed inlet valve, and the material begins to be transmitted to the bagging machine (9) through the feed pipe (3). After the material transmission is completed, the feed inlet valve of the bagging machine (9) is automatically closed, and the material is vacuum-sealed to obtain the positive electrode lithium supplement material.

[0045] Example 1

[0046] Set up program: Set up automated production program.

[0047] Feeding: LiOH powder and Fe2O3 powder are loaded into the silo, and the silo automatically feeds the two materials into the high-speed mixer according to the molar ratio of 5.5:1.

[0048] Mixing: After receiving the signal that the material feeding is completed, the high-speed mixer automatically runs. The mixing time is 20 minutes and the line speed is 25m / s to fully mix the two materials.

[0049] Sintering: The mixed materials are transported to the box furnace through the feed pipe. After the material transmission is completed, the box furnace automatically runs according to the set program. The sintering temperature is 900℃, the sintering time is 5h, the heating rate is 5℃ / min, and the nitrogen flow rate is 5L / min.

[0050] Crushing: After sintering, the material enters the air flow mill through the transmission of the scraper, vacuum collector and feed pipe. After the air flow mill receives the material transmission, it starts to run and crushes the material. The air flow pressure is 0.6MPa.

[0051] Screening: The crushed material is transferred to the screening machine (8) through the material conveying pipe. After receiving the signal indicating that the material transfer is completed, the screening machine (8) starts to operate and screens the material. The aperture of the screen is 400 meshes.

[0052] Bagging: After screening, the material is transferred to the bagging machine through the conveying pipe. After receiving the signal that the material transfer is completed, the bagging machine vacuum bags the material.

[0053] Example 2

[0054] Set up program: Set up automated production program.

[0055] Feeding: Li2O powder and / Fe(NO 3)3 The powder is loaded into the silo, and the silo automatically feeds the two materials into a high-speed mixer in a lithium-iron ratio of 6:1 (molar ratio).

[0056] Mixing: After receiving the signal that the material feeding is completed, the high-speed mixer automatically runs. The mixing time is 20 minutes and the line speed is 25m / s to fully mix the two materials.

[0057] Sintering: The mixed materials are transported to the box furnace through the feed pipe. After the material transmission is completed, the box furnace automatically runs according to the set program. The sintering temperature is 950℃, the sintering time is 1h, the heating rate is 1℃ / min, and the nitrogen flow rate is 10L / min.

[0058] Crushing: After sintering, the material enters the air flow mill through the transmission of the scraper, vacuum collector and feed pipe. After the air flow mill receives the material transmission, it starts to run and crushes the material. The air flow pressure is 0.6MPa.

[0059] Screening: The crushed material is transferred to the screening machine (8) through the material conveying pipe. After receiving the signal indicating that the material transfer is completed, the screening machine (8) starts to operate and screens the material. The aperture of the screen is 400 meshes.

[0060] Bagging: After screening, the material is transferred to the bagging machine through the conveying pipe. After receiving the signal that the material transfer is completed, the bagging machine vacuum bags the material.

[0061] Example 3

[0062] Set up program: Set up automated production program.

[0063] Feeding: LiNO3 powder and / Fe(NO 3)3 The powder is loaded into the silo, and the silo automatically feeds the two materials into a high-speed mixer in a lithium-iron ratio of 5.1:1 (molar ratio).

[0064] Mixing: After receiving the signal that the material feeding is completed, the high-speed mixer automatically runs. The mixing time is 20 minutes and the line speed is 25m / s to fully mix the two materials.

[0065] Sintering: The mixed materials are transported to the box furnace through the feed pipe. After the material transmission is completed, the box furnace automatically runs according to the set program. The sintering temperature is 850℃, the sintering time is 3h, the heating rate is 10℃ / min, and the nitrogen flow rate is 10L / min.

[0066] Crushing: After sintering, the material enters the air flow mill through the transmission of the scraper, vacuum collector and feed pipe. After the air flow mill receives the material transmission, it starts to run and crushes the material. The air flow pressure is 0.6MPa.

[0067] Screening: The crushed material is transferred to the screening machine (8) through the material conveying pipe. After receiving the signal indicating that the material transfer is completed, the screening machine (8) starts to operate and screens the material. The aperture of the screen is 400 meshes.

[0068] Bagging: After screening, the material is transferred to the bagging machine through the conveying pipe. After receiving the signal that the material transfer is completed, the bagging machine vacuum bags the material.

[0069] Comparative Example 1

[0070] Compared with Example 1, all steps are manually operated.

[0071] Feeding: LiOH powder and Fe2O3 powder were manually added into the high-speed mixer at a molar ratio of 5.5:1, and the mixing time was set to 20 min and the linear speed was set to 25 m / s to fully mix the two materials.

[0072] Sintering: The mixed materials are manually transferred to a box furnace, and the box furnace is set with a sintering temperature of 900°C, a sintering time of 5h, a heating rate of 5°C / min, and a nitrogen flow rate of 5L / min.

[0073] Crushing: After sintering, the materials are manually transferred to the air flow mill for crushing, and the air flow pressure is 0.6MPa.

[0074] Screening: The crushed material is manually transferred to a screening machine (8) and screened with a screen aperture of 400 mesh.

[0075] Bagging: The screened materials are manually transferred to the bagging machine, which vacuum bags the materials.

[0076] Comparative Example 2

[0077] Compared with Example 1, all the operation steps are completed by the reported semi-automatic positive electrode material production equipment.

[0078] Feeding: LiOH powder and Fe2O3 powder were manually added into the high-speed mixer at a molar ratio of 5.5:1, and the mixing time was set to 20 min and the linear speed was set to 25 m / s to fully mix the two materials.

[0079] Sintering: The mixed materials are manually transferred to a box furnace, and the box furnace is set with a sintering temperature of 900°C, a sintering time of 5h, a heating rate of 5°C / min, and a nitrogen flow rate of 5L / min.

[0080] Crushing: After sintering, the materials are manually transferred to the air flow mill for crushing, and the air flow pressure is 0.6MPa.

[0081] Screening: The crushed material is automatically transferred from the feeding pipe to the screening machine (8) for screening. The screen has an aperture of 400 mesh.

[0082] Bagging: The screened materials are automatically transferred to the bagging machine through the conveying pipe, and the bagging machine vacuum bags the materials.

[0083] Performance Testing

[0084] The positive electrode lithium supplement material prepared in Examples 1-3 and Comparative Examples 1-2 was mixed with a conductive agent (Super-P) and a binder PVDF in a mass ratio of 80:10:10 to prepare a slurry, which was coated on an aluminum foil and dried in a small compartment of a glove box to form an electrode sheet. A 1 mol / L LiPF6 electrolyte (the volume ratio of ethylene carbonate and diethyl carbonate in the solvent = 1:1) was used, a polypropylene microporous membrane was used as a separator, and a lithium sheet was used as a negative electrode to assemble a button cell. The electrochemical performance was tested on a blue battery test system, with constant current charge and discharge at 0.05C and a voltage range of 2.5-4.5v. The results are shown in Table 1 (10 sets of parallel data in each group).

[0085] Table 1 Capacity data of the embodiment

[0086]

[0087]

[0088] It can be seen from the data in Table 1 that the positive electrode prepared by the fully automatic positive electrode lithium replenisher material continuous production device has excellent capacity performance, and compared with the traditional positive electrode lithium replenisher material preparation device, the integrated device has a simpler operation process, higher efficiency, large processing capacity, and is suitable for large-scale production.

[0089] Table 2 Capacity data of different batches of examples and comparative examples

[0090]

[0091] It can be seen from the data in Table 2 that the batch stability of the positive electrode lithium replenisher material prepared by the fully automatic positive electrode lithium replenisher material continuous production device is better. This is because the uncontrollable factors of human (errors in each manual operation) and environment (preventing H2O and CO2 in the air from reacting with the material) are eliminated in the material preparation process.

[0092] Table 3 Preparation efficiency comparison

[0093] Time Example 1 20h Comparative Example 1 25h Comparative Example 2 22h

[0094] It can be seen from the data in Table 3 that the fully automatic continuous production device for positive electrode lithium supplement materials can complete production in a shorter time and has higher efficiency than fully manual operation and semi-automatic operation.

Claims

1. A fully automatic continuous production device for positive electrode lithium supplement material, characterized in that: The six working sections of silo, high-speed mixer, box furnace, crusher, screener and bagger are connected in sequence through the conveying pipe, and the crusher, screener and bagger are located in the drying room. Among them, the conveying pipe is a cylindrical and freely bendable 304 stainless steel pipe with a spiral rotatable track and a built-in signal sensor. It can automatically receive the discharge signal of the previous working section device and automatically transfer the material to the next working section device.

2. The continuous production device according to claim 1, characterized in that: An automatic sensor is installed under the silo. When the feed signal is received, the valve at the bottom of the silo opens and automatically discharges quantitative materials into the feed pipe.

3. The continuous production device according to claim 1, characterized in that: The feed port of the high-speed mixer is connected to the feed pipe through a flange. An automatic operation sensor is installed in the high-speed mixer. When the automatic operation sensor detects that the feeding at the feed port is completed, the valve automatically closes, and the high-speed mixer automatically operates according to the set program. After the mixing is completed, the discharge port valve automatically opens, and the feed pipe at one end of the discharge port automatically operates to transport the material to the box furnace.

4. The continuous production device according to claim 1, characterized in that: An automatic feed port is installed in the box-type furnace, and the automatic feed port is connected to the feed pipe through a flange. A quality sensor is also provided in the box-type furnace. When receiving the set mass material, the signal is transmitted to the feed pipe connected to the feed port, and the feed pipe automatically stops feeding. The box-type furnace automatically closes the feed port valve, and the box-type furnace automatically runs according to the set program. After sintering is completed, the material automatically cools down, and the upper insulation layer in the box-type furnace cavity automatically opens. The box-type furnace cavity has a built-in scraper and a vacuum material collection device. When the box-type furnace temperature sensor recognizes that the temperature has dropped to room temperature, the scraper and the vacuum material collection device automatically collect the material in the sagger into the feed pipe, and the feed pipe transfers the material to the air flow pulverizer in the drying room.

5. The continuous production device according to claim 1, characterized in that: The feed port and discharge port of the air flow mill are connected to the feed pipe by flange. After the air flow mill receives the signal that the automatic feeding is completed through the feed pipe, the feed port valve is automatically closed and the air flow mill runs automatically. The air flow mill has a built-in particle size detection unit, which automatically adjusts the crushing time and crushing pressure by detecting the particle size. After the crushing is completed, the material is transported to the screening machine through the feed pipe.

6. The continuous production device according to claim 1, characterized in that: The feed port and discharge port of the screening machine are connected to the feed pipe by flange. After receiving the feeding completion signal from the feed pipe, the screening machine automatically closes the feed port valve, and the screening machine automatically runs according to the set program. The screening machine has a built-in automatic discharge device to transport the screened materials to the feed pipe. The feed pipe starts to run after detecting the feeding signal and transports the materials to the bagging machine.

7. The continuous production device according to claim 1, characterized in that: The feeding port of the bagging machine is connected to the feeding pipe by flange. The bagging machine is equipped with a quality sensor to automatically vacuum pack and seal the materials of set quality. The bagging machine and the feeding pipe do not operate at the same time.

8. A method for producing positive electrode lithium supplement material using the continuous production device according to any one of claims 1 to 7, characterized in that: The following steps are involved: Add enough raw materials into the silo, and start the program with one button through the intelligent control cabinet. The valve at the bottom of the silo opens, and the materials are quantitatively fed into the feeding pipe. The feeding pipe detects the entry of materials and starts running automatically, and transports the materials to the high-speed mixer. After the high-speed mixer detects the incoming material information, it opens the inlet valve. After the feeding of the conveying pipe is completed, the inlet valve of the high-speed mixer is closed, and the high-speed mixer starts to run automatically according to the set program. After the mixing is completed, the outlet valve automatically opens and transmits the signal to the conveying pipe. At this time, the material is automatically discharged to the conveying pipe under the stirring action of the high-speed mixer blades. The conveying pipe detects the entry of the material and starts to run automatically, and conveys the material to the box furnace; After the box-type furnace detects the incoming material information, it opens the feed inlet valve. After the feeding of the feeding pipe is completed, the box-type furnace automatically closes the feed inlet valve and automatically operates according to the set program. When the operation is completed and the material temperature drops to room temperature, the box-type furnace discharge port opens, and the scraper and vacuum device in the insulation layer above the box-type furnace automatically transport the material in the sagger to the feeding pipe. The feeding pipe detects the entry of the material and automatically starts to operate, and transports the material to the airflow mill in the drying room; After the airflow mill detects the incoming material information, the feed inlet valve is opened. After the feeding of the feeding pipe is completed, the airflow mill feed inlet valve is closed and automatically operates according to the set program. When the operation is completed, the airflow mill outlet is automatically opened, and the vacuum device of the airflow mill transports the material to the feeding pipe. After the feeding pipe detects the incoming material information, it automatically operates and transports the material to the screening machine. After the screening machine detects the incoming material information, it opens the feed inlet valve. After the feeding of the feeding pipe is completed, the screening machine feed inlet valve closes and automatically runs according to the set program. When the operation is completed, the screening machine outlet automatically opens, and the vacuum device of the screening machine transports the material to the feeding pipe. After the feeding pipe detects the incoming material information, it automatically runs and transports the material to the bagging machine. After the bagging machine detects the incoming material information, it opens the feed port valve, and the material begins to be transmitted to the bagging machine through the feed pipe. After the material transmission is completed, the feed port valve of the bagging machine automatically closes, and the material is vacuum-sealed to obtain the positive electrode lithium supplement material.

9. The method according to claim 8, characterized in that The raw materials added to the silo are LiOH / Li2O / Li2CO3 / LiNO3 powder and Fe2O3 / FePO4 / Fe(NO 3)3 / FeCl3 / FeSO4 powder, the two are mixed in a ratio of lithium iron (5-6):1; The mixing time of the raw materials in the high-speed mixer is 10-60 minutes, and the line speed is 20-30m / s; The sintering temperature of the raw materials in the box furnace is 800-1000°C, the sintering time is 1-8h, the heating rate is 1-10°C / min, and the nitrogen flow rate is 1-10L / min; The particle size of the obtained positive electrode lithium supplement material is 200-500 meshes.

10. The method according to claim 8 or 9, characterized in that: Compared with manual operation between various work-section devices, the specific capacity of the positive electrode lithium replenisher material produced by the fully automatic positive electrode lithium replenisher material continuous production device that integrates each work-section device with automatic transmission through a conveying pipe is at least 8% higher.

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