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CN-122010066-A - Phosphorus-carbon negative electrode material production device and preparation method

CN122010066ACN 122010066 ACN122010066 ACN 122010066ACN-122010066-A

Abstract

The invention relates to the technical field of battery cathode materials, in particular to a phosphorus-carbon cathode material production device and a preparation method, comprising the following operation steps of placing active carbon in a closed container and then carrying out vacuum heat treatment on the closed container; injecting molten white phosphorus into a closed container according to a certain proportion, mechanically stirring and uniformly mixing, heating the closed container, continuously stirring, regulating the temperature in the closed container to the conversion temperature, preserving heat, cooling the closed container, injecting alkali liquor into the closed container after cooling, heating and alkali washing, discharging waste gas generated during the alkali washing out of the closed container, further treating, washing, drying and packaging. The invention solves the problem of difficult combination of white phosphorus and active carbon by adopting a specific device, realizes the preparation of the phosphorus-carbon negative electrode material by taking low-cost white phosphorus as a phosphorus source, obviously reduces the production cost of the phosphorus-carbon negative electrode material, and has the advantages of safe and efficient preparation method, easy operation and no influence on the deposition efficiency of phosphorus.

Inventors

  • WANG YU
  • WANG JUAN
  • GUO YIMING
  • HU JIAJIA
  • MENG QINGSHI
  • QI XINGGUO
  • LI SHUJUN

Assignees

  • 溧阳中科海钠科技有限责任公司

Dates

Publication Date
20260512
Application Date
20241111

Claims (10)

  1. 1. The preparation method of the phosphorus-carbon negative electrode material is characterized by comprising the following operation steps: S1, placing activated carbon in a closed container, and then carrying out vacuum heat treatment on the closed container to discharge the activated carbon and air and moisture in the closed container; s2, injecting molten white phosphorus into the closed container according to a proportion, and mechanically stirring and uniformly mixing; S3, heating and continuously stirring the closed container to convert white phosphorus into phosphorus vapor and adsorbing the phosphorus vapor in the pore canal of the activated carbon; S4, adjusting the temperature in the closed container to a conversion temperature and preserving heat to convert the phosphorus vapor adsorbed in the pore canal of the activated carbon into red phosphorus; S5, cooling the closed container, injecting alkali liquor into the closed container after cooling, heating and alkali washing to remove residual white phosphorus, and discharging waste gas generated in the process out of the closed container for further treatment; s6, washing, drying and packaging.
  2. 2. The method for preparing a phosphorus-carbon negative electrode material according to claim 1, wherein in the step S1, heating is started synchronously during vacuum heat treatment, the closed container is firstly vacuumized to a vacuum degree of less than or equal to-0.1 MPa and heated to 150-300 ℃, then the temperature is kept for 2-24 hours and the vacuum degree is maintained to less than or equal to-0.1 MPa, and the temperature is reduced to 80-240 ℃ and maintained after the temperature is kept, so that the step S2 is performed.
  3. 3. The method for producing a carbon-phosphorus anode material according to claim 1, wherein in step S3, the temperature in the sealed container is raised to 350 to 400 ℃.
  4. 4. The method according to claim 1, wherein in the step S4, the conversion temperature is 260-300 ℃.
  5. 5. The method according to claim 1, wherein in step S5, the temperature in the sealed container is 40-100deg.C after the cooling treatment.
  6. 6. The preparation method of the phosphorus-carbon anode material according to claim 1, wherein in the step S5, inert gas is injected after the temperature reduction treatment, the pressure of a closed container is monitored, alkali liquid is injected when the vacuum degree is more than or equal to 0MPa, the temperature in the closed container is controlled to be 60-100 ℃ after the alkali liquid is injected, inert gas is introduced into the closed container for purging during alkali washing, so that the generated waste gas is discharged and transferred to environmental protection equipment for the next treatment.
  7. 7. The method for preparing a phosphorus-carbon negative electrode material according to claim 1, wherein in the step S6, the material is washed until the material is neutral, and the drying and the packaging are performed in a vacuum environment.
  8. 8. The phosphorus carbon negative electrode material production device is characterized by comprising a cover body (4) and a conversion tank (14) which are detachably connected and have independent heating functions, wherein an air inlet (11), an air outlet (5), a water injection port (10), a charging port (12) and a pressure release valve (23) are arranged on the cover body (4), a check valve (15) is connected to the charging port (12), a pressure gauge (1) for monitoring the air pressure in the conversion tank (14) is further arranged on the cover body (4), the pressure gauge (1) is communicated with the conversion tank (14) through a pressure gauge buffer (2), and a stirring mechanism and a thermocouple (24) are arranged in the conversion tank (14).
  9. 9. The phosphorus carbon cathode material production device of claim 8, wherein the pressure gauge buffer (2) comprises a shell and a cooling liquid pipe positioned in the shell, the cooling liquid pipe is of a serpentine structure, one end of the cooling liquid pipe is a cooling liquid inlet (21), the other end of the cooling liquid pipe is a cooling liquid outlet (22), a cooling net (23) is further connected below a horizontal section part of the cooling liquid pipe, the cooling net (23) is of a flat-top conical structure, a large opening end of the cooling net is connected with the horizontal section part, and a small opening end of the cooling net is downward.
  10. 10. The phosphorus carbon cathode material production device of claim 8, further comprising a conversion tank supporting seat (18), wherein the conversion tank (14) is fixedly connected with a turnover shaft (7), the conversion tank (14) is rotatably connected to the conversion tank supporting seat (18) through the turnover shaft (7), and the turnover shaft (7) is connected with a turnover structure (3) for controlling the rotation of the turnover shaft (7).

Description

Phosphorus-carbon negative electrode material production device and preparation method Technical Field The invention relates to the technical field of battery cathode materials, in particular to a phosphorus-carbon cathode material production device and a preparation method. Background With the rapid development of industries such as new energy automobiles, smart grids and the like, the demand for high-performance batteries is increasing. The phosphorus-carbon anode material is expected to occupy important position in future battery markets by virtue of the advantages of high energy density, good safety, long cycle life and the like. Meanwhile, along with continuous progress of research and development technology and further reduction of production cost, the application range of the phosphorus-carbon anode material is also continuously expanded. Common phosphorus sources include white phosphorus, black phosphorus and red phosphorus, wherein the white phosphorus is easy to spontaneously ignite, and the black phosphorus has higher cost, so that red phosphorus with stable performance is selected in the preparation of the phosphorus-carbon negative electrode, and the red phosphorus is compounded with the activated carbon in an evaporation deposition mode. Specifically, in the technical route, red phosphorus is mixed with active carbon, the red phosphorus is heated to be converted into phosphorus vapor, the phosphorus vapor is deposited to be converted into white phosphorus, and the white phosphorus is cooled to be converted into red phosphorus. To avoid spontaneous ignition of the residual white phosphorus due to incomplete conversion, CS 2 is typically introduced or lye is used to dissolve or react to remove the white phosphorus. Obviously, if white phosphorus is directly used as a phosphorus source, the process can be effectively simplified, and the cost can be reduced. However, the activated carbon is stored with O 2 due to the developed pores, white phosphorus is easy to react with O 2 to generate P 2O5, and the activated carbon is easy to absorb water, and water reacts with the white phosphorus to generate highly toxic phosphine gas. Therefore, the combination of white phosphorus and activated carbon has been a difficult technical problem to solve. In order to solve the problem, the prior art adopts a liquid phase method, such as ethylenediamine assisted phosphorus conversion and active carbon compounding, and avoids the problem of spontaneous combustion of white phosphorus, but in terms of preparation technology, the steps of liquid phase treatment and post-treatment operation are added, and no matter safety and environment, personnel protection and environmental protection equipment are added, and additional matching and investment are required. In addition, solvated phosphorus diffuses more difficult into the pores of the activated carbon than does phosphorus vapor molecules, and introduced solvent molecules can form competitive adsorption with phosphorus, affecting deposition efficiency. In the phosphorus chemical industry, white phosphorus is prepared by smelting phosphate ore, then red phosphorus, black phosphorus and other phosphorus are further prepared by taking the white phosphorus as a basic raw material, so that the preparation of the phosphorus-carbon negative electrode by taking the white phosphorus as a phosphorus source has obvious process and cost advantages, but the problem that the white phosphorus and the active carbon are difficult to compound is solved, and the risk of inflammability in the use process of the white phosphorus is avoided. For this purpose, the present application is proposed. Disclosure of Invention In view of the above-mentioned shortcomings of the prior art, the present invention provides a device for producing a phosphorus-carbon negative electrode material and a preparation method thereof. In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps: in one aspect, the invention provides a preparation method of a phosphorus-carbon anode material, which comprises the following operation steps: S1, placing activated carbon in a closed container, and then carrying out vacuum heat treatment on the closed container to discharge the activated carbon and air and moisture in the closed container; s2, injecting molten white phosphorus into the closed container according to a proportion, and mechanically stirring and uniformly mixing; S3, heating and continuously stirring the closed container to convert white phosphorus into phosphorus vapor and adsorbing the phosphorus vapor in the pore canal of the activated carbon; S4, adjusting the temperature in the closed container to a conversion temperature and preserving heat to convert the phosphorus vapor adsorbed in the pore canal of the activated carbon into red phosphorus; S5, cooling the closed container, injecting alkali liquor into the closed container after cooling,