Large silicon monoxide pre-magnesium or lithium negative electrode material preparation equipment and large silicon monoxide pre-magnesium or lithium negative electrode material preparation method
By designing an integrated large-scale silicon oxide premagnesium or lithium negative electrode material preparation equipment, the problems of uneven material mixing, insufficient reaction and excessive grain size in traditional equipment are solved, and efficient and uniform material preparation is achieved, improving the performance and stability of lithium batteries.
Patent Information
- Application Number
- CN202510401108.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-01
- Publication Date
- 2025-05-02
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Traditional silicon oxide pre-magnesium or lithium equipment have problems such as uneven material mixing, insufficient reaction in the volatilization process, and excessive grains in the cooling stage, resulting in unstable performance of the negative electrode material and difficult to meet the needs of high-performance lithium batteries.
A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment is designed, including an external circulation cooling device, a magnesium or lithium evaporation furnace, a rotary feeding barrel, a steam mixing chamber, a silicon oxide evaporation chamber, a vacuum unit, a raw material lifting device and a control component. The equipment performs steam ratio adjustment and uniform mixing through the steam mixing chamber, controls the condensation temperature using a rotary feeding barrel, and quickly cools down the external circulation cooling device, and evaporates and reacts under a vacuum environment.
The equipment simplifies the process flow, improves production efficiency and material uniformity, effectively improves the first-time Coulomb efficiency and overall battery performance of the negative electrode material, and ensures the stability and high quality of the material.
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Figure CN119909613A_ABST
Abstract
Description
Technical Field
[0001] The present application belongs to the field of battery material technology, and specifically relates to a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation device and method. Background Art
[0002] In recent years, with the widespread application of miniaturized devices, higher and higher requirements have been placed on power supply performance. Due to its high energy density and good cycle life, lithium-ion batteries have gradually become the most widely used form of power supply and are widely used in mobile phones, laptops, power tools, electric vehicles, energy storage devices, and small household appliances. The current market demand for lithium batteries is growing, especially driven by electric vehicles and energy storage devices, and the lithium-ion battery industry is experiencing large-scale expansion.
[0003] The negative electrode material of lithium-ion batteries is mainly graphite, but with the increase in application demand, the performance of graphite materials can no longer meet the requirements for higher battery capacity. Therefore, researchers have developed silicon dioxide (SiO x ) and other silicon-based materials as negative electrode materials to improve the capacity and charge-discharge performance of the battery. Silicon-based materials, especially silicon oxide, have attracted widespread attention due to their high theoretical specific capacity. However, silicon oxide will form electrochemically inert substances such as lithium silicate and lithium oxide during the first charge and discharge process, resulting in a low first coulombic efficiency. Therefore, pre-magnesium or lithium treatment of silicon oxide has become an effective means to improve the first coulombic efficiency.
[0004] Traditional silicon oxide pre-magnesium or lithium equipment mostly adopts the method of first grinding and mixing, and then heating and volatilization. In this process, there are several problems: (1) Raw material pretreatment: In existing solutions, silicon oxide and magnesium powder or lithium powder usually need to be ground and mixed for a long time to maximize the contact area between the materials. This process is time-consuming and increases equipment energy consumption, seriously affecting production efficiency.
[0005] (2) Simple heating volatilization treatment: In traditional equipment, after the pretreatment of silicon dioxide and magnesium or lithium, heating volatilization treatment is usually carried out in a separate heating device. In this process, due to the lack of a precise mixing reaction mechanism, the contact between magnesium or lithium vapor and silicon dioxide is often uneven, resulting in low reaction efficiency, affecting the uniformity of the final product and battery performance.
[0006] (3) Insufficient grain control: During the magnesium thermal reaction, due to inaccurate material temperature control, larger crystal particles are often formed, especially the formation of magnesium silicate. These large crystal particles will block the pore structure of the negative electrode material. The blocked pores affect the electrolyte permeability of the material, further causing the volume expansion of the lithium battery during the charge and discharge process, and the performance degradation, which cannot stably meet the needs of high-performance lithium batteries.
[0007] (4) Lack of reasonable control of the cooling process: In the existing technology, the cooling of materials often adopts natural cooling or simple forced cooling methods, and lacks precise control of the cooling rate, which leads to further growth of grains and affects the uniformity of the final material and the performance of the negative electrode material.
[0008] In summary, there are several problems with traditional silicon oxide pre-magnesium or lithium equipment, such as uneven material mixing, inadequate reaction during volatilization, and easy formation of large crystal particles during the cooling stage, which block the pores. These problems lead to significant volume expansion of the prepared negative electrode material, unstable performance, and difficulty in application in applications with high battery performance requirements. Summary of the invention
[0009] The purpose of this application is to solve the problems of the prior art and to provide a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation device and method.
[0010] In order to solve the technical problem, the technical solution of the present application is: a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment, including an external circulation cooling device, a magnesium or lithium evaporation furnace, a rotating material receiving cylinder, a material receiving chamber, a steam mixing chamber, a silicon oxide evaporation chamber, a vacuum unit, a raw material lifting device, a raw material crucible and a control component; The raw material lifting device is arranged at the bottom of the silicon oxide evaporation chamber, the raw material crucible is placed in the raw material lifting device, the raw material lifting device is used to lift the silicon oxide raw material in the raw material crucible to the silicon oxide evaporation chamber, the top of the silicon oxide evaporation chamber is connected to the steam mixing chamber through a valve, the top of the steam mixing chamber is connected to the material receiving chamber, the rotating material receiving cylinder is installed in the material receiving chamber, the top of the material receiving chamber is connected to the vacuum unit through a pipeline, and the top of the magnesium or lithium evaporation furnace is connected to the steam mixing chamber through a valve; The air inlet end of the external circulation cooling device is connected to the top of the magnesium or lithium evaporation furnace and the top of the material receiving chamber through pipelines, and the air outlet end of the external circulation cooling device is connected to the bottom of the magnesium or lithium evaporation furnace and the bottom of the silicon oxide evaporation chamber through pipelines; The bottom of the magnesium or lithium evaporation furnace and the bottom of the silicon oxide evaporation chamber are also connected to argon supply components respectively; The external circulation cooling device, the magnesium or lithium evaporation furnace, the rotary material receiving cylinder, the steam mixing chamber, the vacuum unit and the raw material lifting device are electrically connected to the control component respectively.
[0011] Preferably, the steam mixing chamber comprises a magnesium or lithium steam connecting pipe, a magnesium or lithium steam distributor, a steam mixing cavity and a mixed steam outlet; The bottom of the steam mixing cavity is connected to the silicon dioxide evaporation chamber through a valve, and the top of the steam mixing cavity is connected to the material receiving chamber through a mixed steam outlet; The magnesium or lithium steam distributor comprises an annular cavity and a top cover plate, wherein the annular cavity is arranged along the periphery of the bottom surface of the top cover plate, the top cover plate installs the annular cavity in the steam mixing cavity, and the periphery of the bottom surface of the top cover plate is sealed and fixedly connected to the top of the steam mixing cavity, a through hole is opened in the center of the top cover plate, and the mixed steam outlet passes through the through hole and is sealed and connected thereto, the outer wall of the annular cavity, the top cover plate and the top of the raw material crucible form a mixing chamber, the annular cavity is provided with a plurality of magnesium or lithium steam distribution ports facing the mixing chamber, the top of the raw material crucible is provided with a plurality of silicon dioxide steam distribution ports, and the axial direction of the magnesium or lithium steam distribution ports is perpendicular to the axial direction of the silicon dioxide steam distribution ports; A magnesium or lithium steam connecting pipe is connected to the side of the steam mixing cavity near the top, one end of the magnesium or lithium steam connecting pipe is connected to the magnesium or lithium evaporation furnace, and the other end of the magnesium or lithium steam connecting pipe is connected to the annular cavity.
[0012] Preferably, a first graphite ring is provided at the top of the raw material crucible extending upward, wherein a silicon oxide vapor distribution port is provided at the top of the raw material crucible outside the first graphite ring; a second graphite ring is provided at the mixed steam outlet extending downward, the first graphite ring and the second graphite ring are nested up and down, wherein the first graphite ring and the second graphite ring are not in contact, and the first graphite ring does not contact the top cover plate, and the second graphite ring does not contact the top of the raw material crucible; The number of the magnesium or lithium vapor distribution ports is twice the number of the silicon oxide vapor distribution ports, and two magnesium or lithium vapor distribution ports are provided corresponding to one silicon oxide vapor distribution port; A third graphite ring is arranged on the top of the silicon oxide vapor distribution port, and the opening of the silicon oxide vapor distribution port is adjusted by rotating the third graphite ring.
[0013] Preferably, a magnesium or lithium feed port and a first steam regulating valve are provided on the top of the magnesium or lithium evaporation furnace, the magnesium or lithium feed port is used to add magnesium or lithium granular materials into the magnesium or lithium evaporation furnace, the first steam regulating valve is used to control the evaporation amount of magnesium or lithium steam entering the steam mixing chamber, and an argon gas inlet interface is provided at the bottom of the magnesium or lithium evaporation furnace, the argon gas inlet interface is connected to the argon gas supply assembly, and the argon gas inlet interface is used to introduce micro-pressure argon gas into the magnesium or lithium evaporation furnace.
[0014] Preferably, the top of the magnesium or lithium evaporation furnace is also connected to a steam mixing chamber via a magnesium or lithium steam connecting pipe, and the first steam regulating valve is used to control the evaporation amount of the magnesium or lithium steam entering the magnesium or lithium steam connecting pipe; An aisle heater is arranged on the periphery of the magnesium or lithium steam connecting pipe to control the temperature of the magnesium or lithium steam entering the steam mixing chamber.
[0015] Preferably, a second steam regulating valve is provided between the bottom of the steam mixing chamber and the top of the silicon oxide evaporation chamber; an argon gas inlet interface is also provided at the bottom of the silicon oxide evaporation chamber, and the argon gas inlet interface is used to introduce micro-pressure argon gas into the silicon oxide evaporation chamber.
[0016] Preferably, a discharging platform is provided on one side of the receiving chamber, and the discharging platform is flush with the plane where the bottom of the receiving chamber is located. The discharging platform is provided with a discharging trolley, and the discharging trolley is used to move the rotating receiving cylinder out of the receiving chamber and perform final material collection on the discharging platform. The receiving chamber is connected to the vacuum unit through a filter.
[0017] Preferably, the air inlet end of the external circulation cooling device is connected to the top of the magnesium or lithium evaporation furnace and the top of the receiving chamber through a first cold air pipe, and the air outlet end of the external circulation cooling device is connected to the bottom of the magnesium or lithium evaporation furnace and the bottom of the silicon oxide evaporation chamber through a second cold air pipe.
[0018] Preferably, a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation method is to use the large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment to prepare silicon oxide pre-magnesium or lithium material, and the specific steps are: Step 1: Raw material pretreatment and evaporation; Step 1-1: adding magnesium or lithium granules to a magnesium or lithium evaporation furnace, then closing the feed port to prevent oxygen from entering, ensuring the stability of the furnace environment, setting the maximum heating temperature of the magnesium or lithium evaporation furnace to 1600° C. through a control component, adjusting the temperature in the magnesium or lithium evaporation furnace through a temperature regulating device to control the evaporation rate of the magnesium or lithium granules, and converting the magnesium or lithium granules into magnesium or lithium vapor; Step 1-2: Load the silicon oxide raw material into the raw material crucible, and use the raw material lifting device to transport it to the silicon oxide evaporation chamber. The furnace environment is maintained at a set vacuum state of <1Pa by the vacuum unit to ensure that there is no impurity interference during the silicon oxide evaporation process; set the maximum heating temperature of the silicon oxide evaporation chamber to 1600°C through the control component to convert the silicon oxide raw material into silicon oxide vapor; Step 2: Steam mixing and reaction: Open the valve, and magnesium or lithium vapor and silicon oxide vapor enter the steam mixing chamber. The ratio of the two vapors is 1:1~1.04. The magnesium or lithium vapor and silicon oxide vapor are mixed through the physical process of mutual diffusion to form pre-magnesium or lithium silicon oxide vapor; Step 3: Material collection and cooling; the pre-magnesium or lithium silicon dioxide vapor enters the receiving chamber, and the pre-magnesium or lithium silicon dioxide vapor is evenly deposited on the surface of the rotating receiving cylinder. The rotating speed of the rotating receiving cylinder is 2~10r / min. Step 4: material cooling; the temperature of the magnesium or lithium evaporation furnace and the silicon oxide evaporation chamber is reduced to below 600°C by introducing slightly pressurized argon gas, and then an external circulation cooling device is used to quickly remove the heat of the magnesium or lithium evaporation furnace, the receiving chamber and the silicon oxide evaporation chamber to ensure uniform cooling of the material; after the cooling is completed, the vacuum unit is started to discharge the residual argon gas in the furnace, and after the pressure inside and outside the furnace is balanced, the furnace door of the receiving chamber is opened, and the rotating receiving cylinder is removed to obtain silicon oxide pre-magnesium or lithium material; Step 5: Finished product processing; the collected silicon monoxide pre-magnesium or lithium material needs to be screened to ensure uniform particle size. After processing, the silicon monoxide pre-magnesium or lithium material is used as the negative electrode material of the lithium battery.
[0019] Preferably, the particle size of the magnesium or lithium particle material in step 1 is ≤20 mm.
[0020] Preferably, in step 5, the collected silicon monoxide pre-magnesium or lithium material also needs to be subjected to quality inspection, including particle size distribution, composition uniformity and chemical stability, to ensure that it meets the lithium battery application standards.
[0021] Compared with the prior art, the advantages of this application are: (1) The present application provides a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation device, including a magnesium or lithium evaporation furnace and a silicon oxide evaporation chamber, magnesium or lithium granular materials are added to the magnesium or lithium evaporation furnace, silicon oxide raw materials are loaded into a raw material crucible, and are transported to the silicon oxide evaporation chamber by a raw material lifting device, the magnesium or lithium evaporation furnace and the silicon oxide evaporation chamber are heated separately, and the evaporated steam is mixed in proportion in a steam mixing chamber, and the mixed steam is deposited on a rotating receiving cylinder through argon gas and a rotating cylinder control; the rotating receiving cylinder rotates and maintains an appropriate cooling rate to control the grain size of the material and avoid grain growth caused by excessive temperature; (2) The present application eliminates the previous grinding and mixing process of magnesium powder or lithium powder and silicon oxide in the traditional process, and instead directly places the magnesium powder or lithium powder particles in the magnesium or lithium evaporation furnace, and directly places the silicon oxide raw material in the silicon oxide evaporation chamber, which greatly reduces the previous processing steps, simplifies the entire process flow, improves production efficiency and reduces equipment energy consumption; (3) The present application adopts a steam mixing chamber to adjust the ratio and evenly mix silicon dioxide vapor and magnesium or lithium vapor, and uses a first steam regulating valve and a second steam regulating valve to accurately control the ratio of the two vapors, thereby ensuring that silicon dioxide vapor and magnesium or lithium vapor are evenly mixed in the mixing chamber according to a set ratio, thereby improving the reaction uniformity of the material and effectively improving the first coulombic efficiency of the negative electrode material and the overall battery performance; (4) The present application adopts a rotating collecting cylinder to collect materials. The appropriate collection temperature is controlled by adjusting the rotation speed of the collecting cylinder to ensure that the grain size of the material is uniform. The design of the rotating collecting cylinder enables the material to be uniformly deposited during the condensation process, avoiding the problem of excessive grain growth caused by excessive temperature, thereby obtaining silicon oxide pre-magnesium or lithium material with uniform particle size and improving the stability of the material; (5) The present application uses an external circulation cooling device to take away the heat through the cold air pipe, quickly reducing the temperature in the receiving chamber. The rapid cooling function of the external circulation cooling system can achieve rapid cooling of the material, effectively control the grain growth of the material, avoid the irregular growth of grains that occurs during long-term natural cooling, and ensure the stability of the material; (6) The evaporation and reaction of silicon dioxide and magnesium or lithium in the present application are carried out in a set vacuum environment (<1Pa), and a vacuum unit is used to maintain a low-pressure environment. Evaporation and reaction in a vacuum environment can effectively reduce the impact of impurities, improve the purity of the reaction, and ensure that the materials react evenly without interference from impurities, thereby improving the quality of the product; (7) In the present application, magnesium or lithium vapor enters the mixing chamber from the magnesium or lithium vapor distribution port through the magnesium or lithium vapor distributor, and silicon dioxide vapor enters the mixing chamber from the silicon dioxide vapor distribution port at the same time. The positions of the two vapor distribution ports correspond to each other, which increases the degree of steam mixing. At the same time, the first graphite ring and the second graphite ring are nested in the mixing chamber, which lengthens the mixed gas flow path and time, allowing the two vapors to be fully mixed. In the present application, the two high-temperature evaporation gas flows are controlled by a valve to control the evaporation amount, so as to achieve a good mixing ratio. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 This is a schematic diagram of the structure of a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation device of the present application; Figure 2 It is a structural schematic diagram of the steam mixing chamber of the present application; Figure 3 It is a schematic diagram of the top view of the raw material crucible of the present application.
[0023] Description of reference numerals: 1. External circulation cooling device, 2. Argon gas inlet interface, 3. Magnesium or lithium evaporation furnace, 4. First cold air pipeline, 5. Magnesium or lithium feed port, 6. First steam regulating valve, 7. Discharging platform, 8. Discharging trolley, 9. Rotating collecting cylinder, 10. Aisle heater, 11. Receiving chamber, 12. Steam mixing chamber, 13. Filter, 14. Second steam regulating valve, 15. Silicon oxide evaporation chamber, 16. Vacuum unit, 17. Raw material lifting device, 18. Raw material crucible, 19. Second cold air pipeline; 12-1, magnesium or lithium steam connecting pipe, 12-2, magnesium or lithium steam distributor, 12-3, steam mixing chamber, 12-4, first graphite ring, 12-5, second graphite ring, 12-6, mixed steam outlet; 12-2-1, annular cavity, 12-2-2, top cover plate; 12-2-1-1, magnesium or lithium vapor distribution port; 12-2-2-1, through hole; 18-1. Silicon dioxide vapor distribution port 18-1-1, the third graphite ring. DETAILED DESCRIPTION
[0024] The present application is described in detail below in conjunction with the accompanying drawings and specific embodiments, but the present application is not limited to these embodiments. The present application covers any substitution, modification, equivalent method and scheme made on the essence and scope of the present application. In order to make the public have a thorough understanding of the present application, specific details are described in detail in the following embodiments of the present application, and those skilled in the art can fully understand the present application without the description of these details.
[0025] like Figure 1 As shown, the present application discloses a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment, including an external circulation cooling device 1, a magnesium or lithium evaporation furnace 3, a rotating material receiving cylinder 9, a material receiving chamber 11, a steam mixing chamber 12, a silicon oxide evaporation chamber 15, a vacuum unit 16, a raw material lifting device 17, a raw material crucible 18 and a control component; The raw material lifting device 17 is arranged at the bottom of the silicon oxide evaporation chamber 15, and the raw material crucible 18 is placed in the raw material lifting device 17. The raw material lifting device 17 is used to lift the silicon oxide raw material in the raw material crucible 18 to the silicon oxide evaporation chamber 15. The top of the silicon oxide evaporation chamber 15 is connected to the steam mixing chamber 12 through a valve, and the top of the steam mixing chamber 12 is connected to the material receiving chamber 11. The rotary material receiving cylinder 9 is installed in the material receiving chamber 11, and the top of the material receiving chamber 11 is connected to the vacuum unit 16 through a pipeline. The top of the magnesium or lithium evaporation furnace 3 is connected to the steam mixing chamber 12 through a valve; The air inlet end of the external circulation cooling device 1 is connected to the top of the magnesium or lithium evaporation furnace 3 and the top of the material receiving chamber 11 through pipelines, and the air outlet end of the external circulation cooling device 1 is connected to the bottom of the magnesium or lithium evaporation furnace 3 and the bottom of the silicon oxide evaporation chamber 15 through pipelines; The bottom of the magnesium or lithium evaporation furnace 3 and the bottom of the silicon oxide evaporation chamber 15 are also connected to argon supply components respectively; The external circulation cooling device 1, the magnesium or lithium evaporation furnace 3, the rotary material collecting cylinder 9, the steam mixing chamber 12, the vacuum unit 16 and the raw material lifting device 17 are electrically connected to the control component respectively.
[0026] like Figure 2 As shown, preferably, the steam mixing chamber 12 includes a magnesium or lithium steam connecting pipe 12-1, a magnesium or lithium steam distributor 12-2, a steam mixing cavity 12-3 and a mixed steam outlet 12-6; The bottom of the steam mixing chamber 12-3 is connected to the silicon oxide evaporation chamber 15 through a valve, and the top of the steam mixing chamber 12-3 is connected to the material receiving chamber 11 through a mixed steam outlet 12-6; The magnesium or lithium steam distributor 12-2 comprises an annular cavity 12-2-1 and a top cover plate 12-2-2. The annular cavity 12-2-1 is arranged along the bottom periphery of the top cover plate 12-2-2. The top cover plate 12-2-2 installs the annular cavity 12-2-1 in the steam mixing cavity 12-3. The bottom periphery of the top cover plate 12-2-2 is sealed and fixedly connected to the top of the steam mixing cavity 12-3. A through hole 12-2-2-1 is opened in the center of the top cover plate 12-2-2. The mixed steam outlet 12-2-2 is provided at the top of the steam mixing cavity 12-3. -6 passes through the through hole 12-2-2-1 and is sealed and connected thereto. The outer wall of the annular cavity 12-2-1, the top cover plate 12-2-2 and the top of the raw material crucible 18 form a mixing chamber. The annular cavity 12-2-1 is provided with a plurality of magnesium or lithium vapor distribution ports 12-2-1-1 facing the mixing chamber. The top of the raw material crucible 18 is provided with a plurality of silicon dioxide vapor distribution ports 18-1. The axial direction of the magnesium or lithium vapor distribution ports 12-2-1-1 is perpendicular to the axial direction of the silicon dioxide vapor distribution ports 18-1. The side of the steam mixing cavity 12-3 near the top is connected with a magnesium or lithium steam connecting pipe 12-1, one end of the magnesium or lithium steam connecting pipe 12-1 is connected to the magnesium or lithium evaporation furnace 3, and the other end of the magnesium or lithium steam connecting pipe 12-1 is connected to the annular cavity 12-2-1.
[0027] like Figure 2 , 3 As shown, preferably, a first graphite ring 12-4 is extended upward from the top of the raw material crucible 18, wherein a silicon oxide vapor distribution port 18-1 is arranged at the top of the raw material crucible 18 outside the first graphite ring 12-4; a second graphite ring 12-5 is extended downward from the mixed steam outlet 12-6, and the first graphite ring 12-4 and the second graphite ring 12-5 are nested up and down, wherein the first graphite ring 12-4 and the second graphite ring 12-5 are not in contact, and the first graphite ring 12-4 does not contact the top cover plate 12-2-2, and the second graphite ring 12-5 does not contact the top of the raw material crucible 18; The number of the magnesium or lithium vapor distribution ports 12-2-1-1 is twice the number of the silicon dioxide vapor distribution ports 18-1, and two magnesium or lithium vapor distribution ports 12-2-1-1 are provided corresponding to one silicon dioxide vapor distribution port 18-1; A third graphite ring 18-1-1 is disposed on the top of the silicon dioxide vapor distribution port 18-1, and the opening of the silicon dioxide vapor distribution port 18-1 is adjusted by rotating the third graphite ring 18-1-1.
[0028] The first graphite ring 12-4 and the second graphite ring 12-5 have the same structure, which is a common cylindrical structure. The third graphite ring 18-1-1 is a circular plate structure, and the size of the reserved opening on the plate is the same as the size of the silicon dioxide vapor distribution opening 18-1.
[0029] The steam evaporated from the magnesium or lithium evaporation furnace 3 passes through the aisle heater 10 to heat the steam temperature to the same temperature as the silicon oxide steam to prevent condensation after the steam is mixed; the magnesium or lithium vapor enters the mixing chamber from the magnesium or lithium vapor distribution port 12-2-1-1 through the magnesium or lithium vapor connecting pipe 12-1 and the magnesium or lithium vapor distributor 12-2, and the silicon oxide vapor enters the mixing chamber from the silicon oxide vapor distribution port 18-1. The positions of the two steam distribution ports correspond to each other, which increases the steam mixing degree. The first graphite ring 12-4 and the second graphite ring 12-5 are nested up and down, which lengthens the mixed airflow path and time, so that the two steams can be fully mixed.
[0030] The preparation method of the present application is a direct mixing of two steams, and the evaporation amount of two high-temperature evaporation air flows is controlled by a valve to achieve a good mixing ratio.
[0031] like Figure 1 As shown, preferably, a magnesium or lithium feed port 5 and a first steam regulating valve 6 are provided on the top of the magnesium or lithium evaporation furnace 3, the magnesium or lithium feed port 5 is used to add magnesium or lithium granular materials into the magnesium or lithium evaporation furnace 3, the first steam regulating valve 6 is used to control the evaporation amount of magnesium or lithium steam entering the steam mixing chamber 12, and an argon gas inlet interface 2 is provided at the bottom of the magnesium or lithium evaporation furnace 3, the argon gas inlet interface 2 is connected to the argon gas supply component, and the argon gas inlet interface 2 is used to introduce micro-pressure argon gas into the magnesium or lithium evaporation furnace 3.
[0032] like Figure 1 , 2 As shown, preferably, the top of the magnesium or lithium evaporation furnace 3 is also connected to the steam mixing chamber 12 through a magnesium or lithium steam connecting pipe 12-1, and the first steam regulating valve 6 is used to control the evaporation amount of the magnesium or lithium steam entering the magnesium or lithium steam connecting pipe 12-1; An aisle heater 10 is arranged on the periphery of the magnesium or lithium steam connecting pipe 12 - 1 to control the temperature of the magnesium or lithium steam entering the steam mixing chamber 12 .
[0033] like Figure 1As shown, preferably, a second steam regulating valve 14 is provided between the bottom of the steam mixing chamber 12 and the top of the silicon oxide evaporation chamber 15; an argon gas inlet interface 2 is also provided at the bottom of the silicon oxide evaporation chamber 15, and the argon gas inlet interface 2 is used to introduce micro-pressure argon gas into the silicon oxide evaporation chamber 15.
[0034] like Figure 1 As shown, preferably, a discharging platform 7 is provided on one side of the receiving chamber 11, and the discharging platform 7 is flush with the plane where the bottom of the receiving chamber 11 is located. The discharging platform 7 is provided with a discharging trolley 8, and the discharging trolley 8 is used to move the rotating receiving cylinder 9 out of the receiving chamber 11 and perform final material collection on the discharging platform 7. The receiving chamber 11 is connected to the vacuum unit 16 through the filter 13.
[0035] like Figure 1 As shown, preferably, the air inlet end of the external circulation cooling device 1 is connected to the top of the magnesium or lithium evaporation furnace 3 and the top of the receiving chamber 11 through the first cold air pipe 4, and the air outlet end of the external circulation cooling device 1 is connected to the bottom of the magnesium or lithium evaporation furnace 3 and the bottom of the silicon oxide evaporation chamber 15 through the second cold air pipe 19.
[0036] like Figure 1 , 2 As shown, preferably, a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation method, using the large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment to prepare silicon oxide pre-magnesium or lithium material, the specific steps are: Step 1: Raw material pretreatment and evaporation; Step 1-1: adding magnesium or lithium granules to a magnesium or lithium evaporation furnace 3, then closing the feed port to prevent oxygen from entering and ensuring the stability of the furnace environment, setting the maximum heating temperature of the magnesium or lithium evaporation furnace 3 to 1600° C. through a control component, adjusting the temperature in the magnesium or lithium evaporation furnace 3 through a temperature regulating device to control the evaporation rate of the magnesium or lithium granules, and converting the magnesium or lithium granules into magnesium or lithium vapor; Step 1-2: Load the silicon oxide raw material into the raw material crucible 18, and use the raw material lifting device 17 to transport it to the silicon oxide evaporation chamber 15. The furnace environment is maintained at a set vacuum state of <1Pa by the vacuum unit 16 to ensure that there is no impurity interference during the silicon oxide evaporation process; set the maximum heating temperature of the silicon oxide evaporation chamber 15 to 1600°C through the control component to convert the silicon oxide raw material into silicon oxide vapor; Step 2: Steam mixing and reaction; Open the valve, magnesium or lithium vapor and silicon oxide vapor enter the steam mixing chamber 12, the ratio of the two vapors is 1:1~1.04, magnesium or lithium vapor and silicon oxide vapor are mixed by a physical process of mutual diffusion to form pre-magnesium or lithium silicon oxide vapor; Step 3: Material collection and cooling; the pre-magnesium or lithium silicon dioxide vapor enters the collecting chamber 11, and the pre-magnesium or lithium silicon dioxide vapor is uniformly deposited on the surface of the rotating collecting cylinder 9, and the rotating speed of the rotating collecting cylinder 9 is 2~10r / min, Step 4: material cooling; the temperature of the magnesium or lithium evaporation furnace 3 and the silicon oxide evaporation chamber 15 is reduced to below 600°C by introducing slightly pressurized argon gas, and then the heat of the magnesium or lithium evaporation furnace 3, the receiving chamber 11 and the silicon oxide evaporation chamber 15 is quickly removed by using the external circulation cooling device 1 to ensure uniform cooling of the material; after the cooling is completed, the vacuum unit 16 is started to discharge the residual argon gas in the furnace, and after the pressure inside and outside the furnace is balanced, the furnace door of the receiving chamber 11 is opened, and the rotating receiving cylinder 9 is removed to obtain silicon oxide pre-magnesium or lithium material; Step 5: Finished product processing; the collected silicon monoxide pre-magnesium or lithium material needs to be screened to ensure uniform particle size. After processing, the silicon monoxide pre-magnesium or lithium material is used as the negative electrode material of the lithium battery.
[0037] Preferably, the particle size of the magnesium or lithium particle material in step 1 is ≤20 mm.
[0038] Preferably, in step 5, the collected silicon monoxide pre-magnesium or lithium material also needs to be subjected to quality inspection, including particle size distribution, composition uniformity and chemical stability, to ensure that it meets the lithium battery application standards.
[0039] This application uses a steam regulating valve to accurately control the steam ratio and evenly mix the steam in the mixing chamber. Alternative solutions include: Dynamically adjustable injection system: Use nozzles for dynamic injection to control the flow and velocity of silicon oxide vapor and magnesium or lithium vapor, and adjust the mixing ratio of the vapor through precision injectors.
[0040] Stirring mixer: A high-speed rotating agitator is added to the mixing chamber to mix the two steams evenly through mechanical stirring to achieve a more efficient mixing effect.
[0041] In this application, the material collection adopts a rotating collection cylinder to control the collection temperature and deposition uniformity. Alternative solutions include: Static cooling collection tray: The rotating collecting cylinder is replaced with a static cooling collection tray, and multiple cooling channels are set inside it. The temperature of the collection tray surface is adjusted by liquid cooling or air cooling to avoid excessive growth of material grains.
[0042] Vibrating receiving barrel: Use a vibrating receiving barrel instead of a rotating receiving barrel. The vibration device can control the uniformity of material deposition in the barrel by adjusting the vibration frequency, thereby achieving a similar effect to a rotating receiving barrel.
[0043] This application uses an external circulation cooling device to quickly cool through the cold air pipeline. Alternative solutions include: Internal water cooling system: There is a cooling water pipeline inside the receiving chamber, which absorbs heat through circulating cooling water to achieve cooling. Compared with external circulation cooling, this method can reduce the material temperature more directly.
[0044] Heat exchange plate cooling: Use a cooling device with a heat exchange plate. The plate is attached to the outside of the receiving chamber, and the heat in the receiving chamber is transferred to the external cooling medium through efficient heat conduction.
[0045] In this application, a vacuum unit is used to maintain a low-pressure environment to reduce interference from impurities. Alternative solutions include: Inert gas environment: Use high-purity argon environment instead of vacuum environment, and remove impurities in the air by filling argon to maintain the purity of the reaction environment. Although it is not a complete vacuum, high-purity argon can also effectively prevent material oxidation and improve the purity of the product.
[0046] Semi-vacuum environment: Using a semi-vacuum (such as a pressure of about 10 to 50Pa), the effect of reducing impurities can be achieved by partial vacuuming and mixing with inert gas, avoiding the high cost of full vacuum equipment.
[0047] This application uses argon-assisted flow to ensure uniform vapor deposition. Alternative solutions include: Gas diffusion plate: A porous diffusion plate is added inside the steam mixing chamber so that the steam is evenly distributed behind the diffusion plate, thereby improving the uniformity of deposition.
[0048] Gas drainage device: Nitrogen (rather than argon) is introduced around the receiving barrel through a multi-point gas drainage device for uniform drainage to help uniform deposition and cooling of vapor on the deposition surface.
[0049] Dynamic injection systems and stirring mixers can more finely adjust the steam ratio and uniformity, making the material react more fully and are suitable for processes that require higher precision control.
[0050] The static cooling collection plate and the vibrating collection cylinder are alternatives to the rotating collection cylinder and are respectively suitable for occasions with higher requirements on the collection temperature and processes with higher requirements on the deposition uniformity.
[0051] Internal water cooling systems provide a more direct cooling method at the collection point than heat exchange plate cooling, facilitating precise temperature control during the cooling process.
[0052] High-purity argon atmosphere and semi-vacuum can achieve similar anti-oxidation functions without relying on high vacuum equipment, while reducing equipment complexity and operating costs.
[0053] As an alternative to argon-assisted flow, the gas diffusion plate and gas guide device can improve the uniformity of steam distribution and effectively enhance the uniformity of reaction products.
[0054] Example 1 The preparation process of silicon oxide pre-magnesium or lithium material in this application is as follows: Step 1: Raw material pretreatment and evaporation; Magnesium or lithium raw materials are heated and evaporated: Feeding process: First, magnesium or lithium granular material (particle size ≤ 20 mm) is added into the magnesium or lithium evaporation furnace 3 through the magnesium or lithium feed port 5, and then the magnesium or lithium feed port 5 is closed to prevent oxygen from entering and ensure the stability of the furnace environment.
[0055] Temperature control: The magnesium or lithium evaporation furnace 3 can be heated to a maximum temperature of 1600°C, and the temperature in the furnace is adjusted by a temperature regulating device to control the evaporation rate of magnesium or lithium. The accuracy of temperature control directly determines the effect of subsequent steam mixing, so the present application uses a temperature control sensor to provide real-time feedback and adjust the temperature in the furnace.
[0056] Silicon oxide evaporation: Silicon oxide evaporation process: The silicon oxide raw material is loaded into the raw material crucible 18 and transported to the silicon oxide evaporation chamber 15 using the raw material lifting device 17. The furnace environment is maintained at a set vacuum state of <1Pa by the vacuum unit 16 to ensure that there is no impurity interference during the silicon oxide evaporation process.
[0057] Temperature setting: The maximum heating temperature of the silicon oxide evaporation chamber 15 is also 1600° C., thereby converting silicon oxide into steam and entering the steam mixing chamber 12 .
[0058] Step 2: Steam mixing and reaction The steam mixing chamber 12 is a key component for achieving the mixing reaction of silicon dioxide and magnesium or lithium vapor. The two steams enter the steam mixing chamber 12 according to a set ratio through their respective steam regulating valves (the first steam regulating valve 6 and the second steam regulating valve 14).
[0059] Mixing reaction process: In the vapor mixing chamber, magnesium or lithium vapor and silicon dioxide vapor are mixed through a physical process of mutual diffusion to form a pre-magnesium or lithium silicon dioxide material.
[0060] In order to ensure the uniformity of mixing, a vortex stirring device is designed inside the mixing chamber to enhance the mutual contact between steam and improve the uniformity and efficiency of the reaction.
[0061] Step 3: Material collection and cooling The rotating collecting cylinder 9 is located in the collecting chamber 11 and is responsible for collecting the material after the steam is condensed and deposited.
[0062] Collection method: Rotation control: By adjusting the rotation speed of the rotating collecting drum, the collection temperature of the condensed material can be adjusted to avoid excessively high temperature on the collection surface leading to grain growth. The surface temperature of the rotating collecting drum is controlled within an appropriate range so that the material is deposited evenly while the grain growth is effectively controlled.
[0063] Step 4: Cooling process: After the material is collected, the temperature in the furnace is lowered to below 600°C by introducing slightly-pressure argon gas, and then the heat in the furnace is quickly removed by using an external circulation cooling device 1 to ensure uniform cooling of the material.
[0064] After cooling, start the vacuum unit 16 to discharge the residual argon in the furnace. After maintaining the pressure balance inside and outside the furnace, open the furnace door of the receiving chamber 11, use the discharge trolley 8 to move the rotating receiving cylinder out and carry out the final material collection on the second-layer discharge platform 7.
[0065] Step 5: Finished product processing The collected materials need to be screened to ensure uniform particle size and remove possible large particle impurities. After processing, the materials are used as negative electrode materials for lithium batteries. The collected materials are tested for quality, including particle size distribution, composition uniformity, and chemical stability, to ensure that they meet the standards for lithium battery applications.
[0066] Comparative Example 1 The current technical implementation scheme for silicon dioxide pre-magnesium or lithium usually includes the following main steps to complete the preparation of negative electrode materials: 1) Raw material pretreatment: The raw materials of silicon oxide and magnesium or lithium are first processed through grinding and mixing processes to increase the contact area of the materials and create greater surface activity for subsequent reactions. Grinding is usually carried out in equipment such as ball mills to obtain relatively fine powders and improve the mixing effect and reaction rate between materials.
[0067] 2) Heating volatilization treatment: After raw material pretreatment, silicon oxide and magnesium or lithium raw materials are placed in a heating device for volatilization treatment. In this step, the heating device gradually increases the temperature to convert magnesium or lithium into a vapor state and react chemically with silicon oxide. The volatilization reaction is usually carried out in a closed reaction chamber to ensure full contact with the steam and maintain a stable reaction environment. The whole process involves adjusting the evaporation temperature to control the volatilization rate and diffusion degree of the steam.
[0068] 3) Steam mixing reaction: After silicon oxide and magnesium or lithium raw materials are heated to a certain temperature, the generated silicon oxide vapor contacts and reacts with magnesium or lithium vapor in the steam mixing area. In this process, magnesium or lithium vapor and silicon oxide are mixed through physical mechanisms such as diffusion, and chemical reactions occur, thereby achieving pre-magnesium or pre-lithium treatment of silicon oxide. In order to improve the uniformity of the material, mixing equipment such as cyclone separators or gas agitators are usually used to promote uniform mixing of the reactants.
[0069] 4) Material collection and cooling: After the mixing reaction, the materials generated by the reaction need to be cooled and collected. Cooling usually adopts natural cooling or simple forced cooling, such as by passing cold air or placing the materials in a cooler. The purpose of cooling is to reduce the reaction temperature to a suitable level so that the materials can be safely collected. In this process, the cooled material is collected in the collecting device, and a rotating collection drum or a static collection tank is usually used to complete the deposition and collection of the material. The collected material is a silicon oxide negative electrode material containing magnesium or lithium, which can be used in subsequent lithium battery manufacturing processes.
[0070] 5) Finished product processing: After cooling and collection, the obtained materials need to be further processed in order to be used in the preparation of negative electrode materials for batteries.
[0071] The silicon dioxide pre-magnesium or lithium material prepared by the equipment and method of the present application is applied to the battery, with an initial discharge capacity of 1859 mAh / g, an initial coulombic efficiency of 86.4%, and a 0.5C 100-cycle capacity retention rate of 94%, which greatly improves the quality of the battery.
[0072] The application works as follows: like Figures 1 to 3 As shown, the present application discloses a novel silicon oxide pre-magnesium or lithium equipment, which aims to achieve more efficient preparation of silicon oxide negative electrode materials and improve their charge and discharge performance. The raw material lifting device 17 is responsible for lifting the silicon oxide raw material to the silicon oxide evaporation chamber 15 to ensure the raw material supply during the evaporation process. The magnesium or lithium evaporation furnace 3 is used to heat the magnesium or lithium raw material and convert it into steam form. The steam mixing chamber 12 connects the magnesium or lithium evaporation furnace 3 and the silicon oxide evaporation chamber 15 to mix the steam from the two evaporation chambers. The receiving chamber 11 and the rotating receiving cylinder 9 constitute a closed collection unit for uniformly collecting the mixed pre-magnesium or lithium silicon oxide. The external circulation cooling device 1 is connected to the magnesium or lithium evaporation furnace 3 and the receiving chamber 11 through the cold air pipe 4, which is used for rapid cooling to prevent excessive growth of material grains. The present application can efficiently and stably prepare high-quality silicon oxide pre-magnesium or lithium materials, and provides reliable technical support for improving the first coulomb efficiency of lithium batteries.
[0073] The raw materials of this application enter their respective evaporation chambers from the feed port for heating treatment; the evaporated steam is mixed in proportion in the mixing chamber; the mixed steam is deposited on the receiving barrel through argon gas and rotating cylinder control; the receiving barrel rotates and maintains an appropriate cooling rate to control the grain size of the material and avoid grain growth caused by excessive temperature. This application evaporates silicon oxide and magnesium (or lithium) raw materials at high temperature and uniformly mixes the steam through the mixing chamber to finally obtain silicon oxide material pre-treated with magnesium or lithium; the rotating receiving barrel is used to effectively control the size of the condensed grains, thereby improving the uniformity of the material and the performance of the final battery.
[0074] This application eliminates the simplified process of raw material grinding and mixing steps Technical solution: Silicon oxide and magnesium (or lithium) powders are directly processed through the evaporation chamber, eliminating the previous grinding and mixing steps.
[0075] Quantitative effect: The process flow is shortened by 20% and production efficiency is increased by about 15%.
[0076] In this application, magnesium or lithium vapor and silicon dioxide vapor are adjusted in proportion and uniformly mixed. Technical solution: The ratio of silicon dioxide vapor to magnesium or lithium vapor is precisely controlled by steam regulating valves (a first steam regulating valve 6 and a second steam regulating valve 14 ), and uniform mixing is achieved in the steam mixing chamber 12 .
[0077] Quantitative effect: Reaction uniformity increased by about 30%, and the first coulombic efficiency increased to more than 85%.
[0078] Application and temperature control of the rotary receiving drum in this application Technical solution: Utilize the rotating collecting barrel 9 to control the collecting temperature by adjusting the rotation speed, avoid the growth of grains and ensure uniform deposition.
[0079] Quantitative effect: The grain size is reduced to an average of less than 30 microns, and the uniformity of particle size distribution is improved by 20%.
[0080] The rapid cooling system of the external circulation cooling device of the present invention Technical solution: The external circulation cooling device 1 quickly reduces the temperature in the furnace through the cold air pipe, ensuring that the collected materials reach the set cooling temperature in a short time.
[0081] Quantitative effect: The cooling time is shortened by 40%, the grain growth is controlled within the set range, and the large grain generation rate is effectively suppressed to less than 5%.
[0082] This application evaporation and mixing reaction under vacuum environment Technical solution: Under the action of the vacuum unit 16, silicon dioxide and magnesium or lithium are evaporated and mixed in a low-pressure (<1Pa) environment.
[0083] Quantitative effect: The impurity content in the reaction environment is reduced by 90%, and the material purity is increased to more than 99%.
[0084] Argon-assisted flow control of mixed steam in this application Technical solution: During the steam mixing process, slightly-pressure argon gas is introduced through the argon gas inlet interface 2 to assist the uniform distribution and deposition of the steam.
[0085] Quantitative effect: The deposition uniformity of the mixed vapor is improved by about 25%, and the content of uneven particles in the finished product is reduced by 10%.
[0086] The present application is a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment, which can produce 400kg of products in a single furnace.
[0087] The present application adopts the method of directly placing magnesium powder (or lithium powder) particles in the magnesium or lithium evaporation furnace 3, eliminating the previous grinding and mixing steps, and achieving a more efficient preparation process by optimizing the process arrangement inside the equipment, greatly shortening the overall production time.
[0088] The present application uniformly mixes magnesium or lithium vapor with silicon dioxide vapor in a specific vapor mixing chamber, thereby ensuring that the two vapors are fully contacted and pre-reacted in proportion, thereby improving the uniformity and reaction efficiency of the material, and further improving the coulombic efficiency of the final product.
[0089] The present application effectively controls the cooling rate during the collection process, preventing excessive grain growth due to excessively high temperature, thereby obtaining a negative electrode material with uniform particles and good pore structure, thereby improving the performance and stability of the product.
[0090] The present application provides a large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation device, including a magnesium or lithium evaporation furnace and a silicon oxide evaporation chamber, magnesium or lithium granular materials are added to the magnesium or lithium evaporation furnace, silicon oxide raw materials are loaded into a raw material crucible, and are transported to the silicon oxide evaporation chamber using a raw material lifting device, the magnesium or lithium evaporation furnace and the silicon oxide evaporation chamber are heated separately, the evaporated steam is mixed in proportion in a steam mixing chamber, and the mixed steam is deposited on a rotating receiving cylinder through argon gas and a rotating cylinder control; the rotating receiving cylinder rotates and maintains an appropriate cooling rate to control the grain size of the material and avoid grain growth caused by excessive temperature.
[0091] The present application eliminates the preliminary grinding and mixing steps of magnesium powder or lithium powder and silicon oxide in the traditional process, and instead places the magnesium powder or lithium powder particles directly in the magnesium or lithium evaporation furnace, and places the silicon oxide raw material directly in the silicon oxide evaporation chamber, which greatly reduces the preliminary processing steps, simplifies the entire process flow, improves production efficiency and reduces equipment energy consumption.
[0092] The present application adopts a steam mixing chamber to adjust the ratio and evenly mix silicon dioxide vapor and magnesium or lithium vapor, and uses a first steam regulating valve and a second steam regulating valve to accurately control the ratio of the two vapors, thereby ensuring that silicon dioxide vapor and magnesium or lithium vapor are evenly mixed in the mixing chamber at a set ratio, thereby improving the reaction uniformity of the material and effectively improving the first coulombic efficiency of the negative electrode material and the overall battery performance.
[0093] The present application adopts a rotating collecting barrel to collect materials, and controls the appropriate collection temperature by adjusting the rotation speed of the collecting barrel to ensure the uniformity of the material grain size. The design of the rotating collecting barrel enables the material to be evenly deposited during the condensation process, avoiding the problem of excessive grain growth caused by excessively high temperature, thereby obtaining silicon oxide pre-magnesium or lithium material with uniform particle size and improving the stability of the material.
[0094] The present application uses an external circulation cooling device to take away heat through the cold air pipe, quickly lowering the temperature in the material receiving room. The rapid cooling function of the external circulation cooling system can achieve rapid cooling of the material, effectively control the grain growth of the material, avoid the irregular grain growth that occurs during long-term natural cooling, and ensure the stability of the material.
[0095] In the present application, the evaporation and reaction of silicon dioxide and magnesium or lithium are carried out in a set vacuum environment (<1Pa), and a vacuum unit is used to maintain a low-pressure environment. Evaporation and reaction in a vacuum environment can effectively reduce the impact of impurities, improve the purity of the reaction, and ensure that the materials react evenly without interference from impurities, thereby improving the quality of the product.
[0096] In the present application, magnesium or lithium vapor enters the mixing chamber from the magnesium or lithium vapor distribution port through the magnesium or lithium vapor distributor, and silicon dioxide vapor enters the mixing chamber from the silicon dioxide vapor distribution port at the same time. The positions of the two steam distribution ports correspond to each other, which increases the steam mixing degree; at the same time, the first graphite ring and the second graphite ring are nested up and down in the mixing chamber, which lengthens the mixed airflow path and time, allowing the two steams to be fully mixed. In the present application, the two high-temperature evaporation airflows control the evaporation amount through a valve, so as to achieve a good mixing ratio.
[0097] The preferred embodiments of the present application are described in detail above, but the present application is not limited to the above embodiments, and various changes can be made within the knowledge scope of ordinary technicians in this field without departing from the purpose of the present application.
[0098] Many other changes and modifications can be made without departing from the concept and scope of the present application.It should be understood that the present application is not limited to specific embodiments, and the scope of the present application is defined by the appended claims.
Claims
1. A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment, characterized in that: It comprises an external circulation cooling device (1), a magnesium or lithium evaporation furnace (3), a rotating material receiving cylinder (9), a material receiving chamber (11), a steam mixing chamber (12), a silicon oxide evaporation chamber (15), a vacuum unit (16), a raw material lifting device (17), a raw material crucible (18) and a control component; The raw material lifting device (17) is arranged at the bottom of the silicon oxide evaporation chamber (15), and the raw material crucible (18) is placed in the raw material lifting device (17). The raw material lifting device (17) is used to lift the silicon oxide raw material in the raw material crucible (18) to the silicon oxide evaporation chamber (15). The top of the silicon oxide evaporation chamber (15) is connected to the steam mixing chamber (12) through a valve. The top of the steam mixing chamber (12) is connected to the material receiving chamber (11). The rotating material receiving cylinder (9) is installed in the material receiving chamber (11). The top of the material receiving chamber (11) is connected to the vacuum unit (16) through a pipeline. The top of the magnesium or lithium evaporation furnace (3) is connected to the steam mixing chamber (12) through a valve. The air inlet end of the external circulation cooling device (1) is connected to the top of the magnesium or lithium evaporation furnace (3) and the top of the material receiving chamber (11) through pipelines, and the air outlet end of the external circulation cooling device (1) is connected to the bottom of the magnesium or lithium evaporation furnace (3) and the bottom of the silicon dioxide evaporation chamber (15) through pipelines; The bottom of the magnesium or lithium evaporation furnace (3) and the bottom of the silicon oxide evaporation chamber (15) are also connected to argon gas supply components respectively; The external circulation cooling device (1), the magnesium or lithium evaporation furnace (3), the rotating material collecting cylinder (9), the steam mixing chamber (12), the vacuum unit (16) and the raw material lifting device (17) are respectively electrically connected to the control component.
2. A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment according to claim 1, characterized in that: The steam mixing chamber (12) comprises a magnesium or lithium steam connecting pipe (12-1), a magnesium or lithium steam distributor (12-2), a steam mixing cavity (12-3) and a mixed steam outlet (12-6); The bottom of the steam mixing cavity (12-3) is connected to the silicon dioxide evaporation chamber (15) via a valve, and the top of the steam mixing cavity (12-3) is connected to the material receiving chamber (11) via a mixed steam outlet (12-6); The magnesium or lithium steam distributor (12-2) comprises an annular cavity (12-2-1) and a top cover plate (12-2-2); the annular cavity (12-2-1) is arranged along the bottom periphery of the top cover plate (12-2-2); the top cover plate (12-2-2) installs the annular cavity (12-2-1) in the steam mixing cavity (12-3); and the bottom periphery of the top cover plate (12-2-2) is sealed and fixedly connected to the top of the steam mixing cavity (12-3); a through hole (12-2-2-1) is opened in the center of the top cover plate (12-2-2); and a mixed steam outlet (12-2-2) is provided at the top of the steam mixing cavity (12-3). 12-6) passes through the through hole (12-2-2-1) and is sealed and connected thereto, the outer wall of the annular cavity (12-2-1), the top cover plate (12-2-2) and the top of the raw material crucible (18) form a mixing chamber, the annular cavity (12-2-1) is provided with a plurality of magnesium or lithium vapor distribution ports (12-2-1-1) facing the mixing chamber, the top of the raw material crucible (18) is provided with a plurality of silicon dioxide vapor distribution ports (18-1), and the axial direction of the magnesium or lithium vapor distribution ports (12-2-1-1) is perpendicular to the axial direction of the silicon dioxide vapor distribution ports (18-1); A magnesium or lithium steam connecting pipe (12-1) is connected to the side of the steam mixing cavity (12-3) close to the top; one end of the magnesium or lithium steam connecting pipe (12-1) is connected to the magnesium or lithium evaporation furnace (3); and the other end of the magnesium or lithium steam connecting pipe (12-1) is connected to the annular cavity (12-2-1).
3. A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment according to claim 2, characterized in that: A first graphite ring (12-4) is provided on the top of the raw material crucible (18) extending upward, wherein a silicon oxide vapor distribution port (18-1) is provided on the top of the raw material crucible (18) outside the first graphite ring (12-4); a second graphite ring (12-5) is provided on the bottom of the mixed vapor outlet (12-6), wherein the first graphite ring (12-4) and the second graphite ring (12-5) are nested in an up-and-down manner, wherein the first graphite ring (12-4) and the second graphite ring (12-5) are not in contact with each other, and the first graphite ring (12-4) does not contact the top cover plate (12-2-2), and the second graphite ring (12-5) does not contact the top of the raw material crucible (18); The number of the magnesium or lithium vapor distribution ports (12-2-1-1) is twice the number of the silicon dioxide vapor distribution ports (18-1), and two magnesium or lithium vapor distribution ports (12-2-1-1) are provided corresponding to one silicon dioxide vapor distribution port (18-1); A third graphite ring (18-1-1) is arranged on the top of the silicon dioxide vapor distribution port (18-1), and the opening of the silicon dioxide vapor distribution port (18-1) is adjusted by rotating the third graphite ring (18-1-1).
4. A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment according to claim 2, characterized in that: The magnesium or lithium evaporation furnace (3) is provided with a magnesium or lithium feed port (5) and a first steam regulating valve (6) at the top. The magnesium or lithium feed port (5) is used to add magnesium or lithium granular material into the magnesium or lithium evaporation furnace (3). The first steam regulating valve (6) is used to control the evaporation amount of magnesium or lithium steam entering the steam mixing chamber (12). The magnesium or lithium evaporation furnace (3) is provided with an argon gas inlet interface (2) at the bottom. The argon gas inlet interface (2) is connected to an argon gas supply component. The argon gas inlet interface (2) is used to introduce micro-pressure argon gas into the magnesium or lithium evaporation furnace (3).
5. A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment according to claim 4, characterized in that: The top of the magnesium or lithium evaporation furnace (3) is also connected to the steam mixing chamber (12) via a magnesium or lithium steam connecting pipe (12-1), and the first steam regulating valve (6) is used to control the evaporation amount of the magnesium or lithium steam entering the magnesium or lithium steam connecting pipe (12-1); An aisle heater (10) is arranged on the periphery of the magnesium or lithium steam connecting pipe (12-1) to control the temperature of the magnesium or lithium steam entering the steam mixing chamber (12).
6. A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation device according to claim 1, characterized in that: A second steam regulating valve (14) is provided between the bottom of the steam mixing chamber (12) and the top of the silicon oxide evaporation chamber (15); an argon gas inlet interface (2) is also provided at the bottom of the silicon oxide evaporation chamber (15), and the argon gas inlet interface (2) is used to introduce micro-pressure argon gas into the silicon oxide evaporation chamber (15).
7. A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation device according to claim 1, characterized in that: A discharging platform (7) is provided on one side of the material receiving chamber (11), and the discharging platform (7) is flush with the plane where the bottom of the material receiving chamber (11) is located. The discharging platform (7) is provided with a discharging trolley (8), and the discharging trolley (8) is used to move the rotating material receiving cylinder (9) out of the material receiving chamber (11) and perform final material collection on the discharging platform (7). The material receiving chamber (11) is connected to a vacuum unit (16) via a filter (13).
8. A large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment according to claim 1, characterized in that: The air inlet end of the external circulation cooling device (1) is connected to the top of the magnesium or lithium evaporation furnace (3) and the top of the material receiving chamber (11) through a first cold air pipeline (4), and the air outlet end of the external circulation cooling device (1) is connected to the bottom of the magnesium or lithium evaporation furnace (3) and the bottom of the silicon dioxide evaporation chamber (15) through a second cold air pipeline (19).
9. A method for preparing a large-scale silicon oxide pre-magnesium or lithium negative electrode material, characterized in that: The large-scale silicon oxide pre-magnesium or lithium negative electrode material preparation equipment according to any one of claims 1 to 8 is used to prepare silicon oxide pre-magnesium or lithium material, and the specific steps are: Step 1: Raw material pretreatment and evaporation; Step 1-1: adding magnesium or lithium granules to a magnesium or lithium evaporation furnace (3), then closing the feed port to prevent oxygen from entering and ensuring a stable furnace environment, setting the maximum heating temperature of the magnesium or lithium evaporation furnace (3) to 1600° C. through a control component, adjusting the temperature in the magnesium or lithium evaporation furnace (3) through a temperature regulating device to control the evaporation rate of the magnesium or lithium granules, and converting the magnesium or lithium granules into magnesium or lithium vapor; Step 1-2: Load the silicon oxide raw material into the raw material crucible (18), and use the raw material lifting device (17) to transport it to the silicon oxide evaporation chamber (15). The environment in the furnace is maintained at a set vacuum state of <1Pa by the vacuum unit (16) to ensure that there is no impurity interference during the silicon oxide evaporation process; set the maximum heating temperature of the silicon oxide evaporation chamber (15) to 1600°C through the control component to convert the silicon oxide raw material into silicon oxide vapor; Step 2: steam mixing and reaction; opening the valve, magnesium or lithium steam and silicon oxide steam enter the steam mixing chamber (12), the ratio of the two steams is 1:1~1.04, the magnesium or lithium steam and silicon oxide steam are mixed by the physical process of mutual diffusion to form pre-magnesium or lithium silicon oxide steam; Step 3: Material collection and cooling; the pre-magnesium or lithium silicon dioxide vapor enters the collecting chamber (11), and the pre-magnesium or lithium silicon dioxide vapor is uniformly deposited on the surface of the rotating collecting cylinder (9). The rotating speed of the rotating collecting cylinder (9) is 2-10 r / min. Step 4: material cooling; the temperature of the magnesium or lithium evaporation furnace (3) and the silicon oxide evaporation chamber (15) is reduced to below 600°C by introducing slightly pressurized argon gas, and then the heat of the magnesium or lithium evaporation furnace (3), the material receiving chamber (11) and the silicon oxide evaporation chamber (15) is quickly removed by using an external circulation cooling device (1) to ensure uniform cooling of the material; after the cooling is completed, the vacuum unit (16) is started to discharge the residual argon gas in the furnace, and after the pressure inside and outside the furnace is balanced, the furnace door of the material receiving chamber (11) is opened, and the rotating material receiving cylinder (9) is removed to obtain silicon oxide pre-magnesium or lithium material; Step 5: Finished product processing; the collected silicon monoxide pre-magnesium or lithium material needs to be screened to ensure uniform particle size. After processing, the silicon monoxide pre-magnesium or lithium material is used as the negative electrode material of the lithium battery.
10. A method for preparing a large-scale silicon oxide pre-magnesium or lithium negative electrode material according to claim 9, characterized in that: In step 1, the particle size of the magnesium or lithium particle material is ≤20 mm; in step 5, the collected silicon oxide pre-magnesium or lithium material also needs to be quality tested, including particle size distribution, composition uniformity and chemical stability, to ensure that it meets the lithium battery application standards.
Citation Information
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