Preparation method and system of carbonized particles

Abstract

A high-temperature reaction zone is arranged at a position close to the bottom of a carbonization fluidized bed, a low-temperature reaction zone is arranged at a position close to an outlet of the carbonization fluidized bed, and an overflow pipe is arranged between the high-temperature reaction zone and the low-temperature reaction zone. During preparation, magnesium oxide and other heat carrier particles and polymer particles are introduced into the low-temperature reaction area and are in countercurrent contact with fluidizing gas for compounding and carbonization, and basically cured particles move to the high-temperature reaction area through the overflow pipe and are fully carbonized. The method has the advantages that the heat carrier particles are used for effectively dispersing polymer particles such as resin, softening adhesion during high-temperature carbonization is avoided, the effect of continuous operation is achieved, and porous carbonized particles can be formed after the heat carrier particles are dissolved subsequently. According to the method, the grinding energy consumption and cost can be reduced, the carbonization degree control at different temperatures can be realized, and the energy can be saved and the material consumption can be reduced during subsequent activation.

Description

Technical Field

[0001] The present application relates to the technical field of electrochemical energy storage electrode materials or environmentally friendly materials, and in particular, to a method and system for preparing carbonized particles. Background Art

[0002] Devices based on clean electrochemical energy storage mechanisms, such as various secondary batteries, supercapacitors, lithium-ion capacitors or their hybrid devices, are important electrical energy storage systems and have made great progress in recent years. The positive electrode materials of supercapacitors and lithium-ion capacitors are porous activated carbon with large specific surface area. Secondary batteries such as lithium-ion negative electrode materials (silicon-carbon negative electrode) also use porous activated carbon with large specific surface area as a fixed carrier of silicon particles, which accounts for about 50% of the weight of the silicon-carbon negative electrode.

[0003] Porous carbon is mainly composed of biomass or organic polymers as precursors, and is composed of carbonization (dehydrogenation, deoxidation or other elements at high temperature) and activation (pore formation) steps. Among them, in the carbonization process, some precursor particles will become soft and sticky at high temperatures, forming particularly large sticky agglomerates, resulting in uncontrollable particle size and density. At the same time, there is also a wall sticking phenomenon, which is particularly difficult to operate in engineering. For the huge carbonized agglomerates or particles generated, they have to be ground into small particles before proceeding to the subsequent steps. The strength of the agglomerates after carbonization is particularly large. Therefore, a large amount of mechanical energy is required, making the carbonization process cumbersome to operate, high energy consumption, high cost, and the resulting product quality is low. Summary of the invention

[0004] In order to solve the above problems, the present application provides a method and system for preparing carbonized particles, which utilizes heat carrier particles to achieve the purpose of dispersing polymer particles (i.e., organic precursor particles) at a relatively low temperature, thereby making it difficult for the carbonized particles to grow or form agglomerates, avoiding subsequent grinding and other steps, and effectively reducing the consumption of mechanical energy. In addition, by setting up a two-stage variable temperature carbonization fluidized bed, the compounding and carbonization can be easily controlled in engineering, and the carbonized product can be easily activated, further reducing the cost.

[0005] In a first aspect, the present application provides a method for preparing carbonized particles, the method comprising: Under the action of fluidizing gas, the polymer particles and the heat carrier particles are placed at 200°C-400°C for the first high temperature treatment, and after 0.5 h-20 h, a composite carbonized material is obtained; Continue to raise the temperature to 500°C-950°C, perform a second high temperature treatment, and after 0.5 h-20 h, obtain the carbonized particles; Wherein, the polymer particles include at least one of epoxy resin, phenolic resin, urea-formaldehyde resin, unsaturated resin and polycarbonate resin; the heat carrier particles include at least one of magnesium oxide, sodium chloride, potassium chloride, calcium chloride, calcium oxide, sodium silicate, calcium carbonate, sodium carbonate and magnesium carbonate.

[0006] Furthermore, the mass ratio of the polymer particles to the heat carrier particles is 1:(1-3).

[0007] Further, the diameter of the polymer particles is 5 μm-50 μm; The diameter of the heat carrier particles is 50 μm-200 μm.

[0008] Furthermore, the temperature of the first high temperature treatment is 270°C-360°C.

[0009] Furthermore, the temperature of the second high temperature treatment is 750°C-900°C, and the time of the second high temperature treatment is 3 h-12 h.

[0010] Further, the fluidizing gas includes at least one of N2, CO, H2, Ar, He, CO2 and CH4.

[0011] Furthermore, the first high temperature treatment process includes: The heat carrier particles are fluidized under the action of the fluidizing gas, the polymer particles melt and soften at a temperature of 200° C.-400° C., and are bonded and solidified with the fluidized heat carrier particles to obtain the composite carbonized material.

[0012] In a second aspect, the present application provides a system for preparing carbonized particles, the system being used to perform the method for preparing carbonized particles described in the first aspect, the system comprising: a carbonization fluidized bed; A porous distribution plate is arranged in the carbonization fluidized bed, and the porous distribution plate divides the carbonization fluidized bed into a low-temperature reaction zone and a high-temperature reaction zone; The low temperature reaction zone is provided with a mixed raw material inlet, and the mixed raw material inlet is used to introduce polymer particles and heat carrier particles into the low temperature reaction zone; the low temperature reaction zone is used to perform a first high temperature treatment on the polymer particles and the heat carrier particles to obtain a composite carbonized material; The high temperature reaction zone is used to perform a second high temperature treatment on the composite carbonized material to convert it into carbonized particles; the high temperature reaction zone is provided with a fluidizing gas inlet, and the fluidizing gas inlet is used to introduce fluidizing gas into the carbonization fluidized bed to fluidize the mixed raw materials and composite carbonized material in the carbonization fluidized bed.

[0013] Furthermore, an overflow pipe is provided outside the carbonization fluidized bed, one end of the overflow pipe is connected to the low-temperature reaction zone, and the other end is connected to the high-temperature reaction zone; the composite carbonized material flows to the high-temperature reaction zone through the overflow pipe; The carbonization fluidized bed is provided with an exhaust gas outlet, and the fluidizing gas is discharged from the carbonization fluidized bed through the exhaust gas outlet; The carbonization fluidized bed is provided with a carbonization material outlet, and the carbonized particles are discharged from the high-temperature reaction zone along the carbonization material outlet.

[0014] In a third aspect, the present application provides carbonized particles obtained by the method for preparing carbonized particles according to the first aspect, wherein the particle size of the carbonized particles is 5 μm-80 μm.

[0015] In summary, the present application includes at least one of the following beneficial technical effects: 1. A method for preparing carbonized particles provided in the present application, wherein heat carrier particles are introduced to disperse polymer particles at high temperature, and the obtained composite carbonized material is further heated to be carbonized to convert it into carbonized particles; the method can control the particle size of directly carbonized particles to be within a few μm to tens of μm, thereby avoiding agglomeration of polymer particles at high temperature or forming large-size particles, saving operation steps such as grinding, avoiding the risk of subsequent grinding introducing impurities, and reducing grinding energy consumption and cost; the method can also realize carbonization degree control at different temperatures, which can save energy and reduce material consumption during subsequent activation; the number of preparation equipment is reduced by 20%, the equipment investment is reduced by 25%-30%, the mechanical energy consumed in production is greatly reduced, and the preparation time is shortened by about 50%-90%, the carbonization cost is saved by 50%-60%, and the grinding cost is saved by 70%-90%; 2. The present application provides a system for preparing carbonized particles. The porous distribution plate provided in the system divides the carbonization fluidized bed into a low-temperature reaction zone and a high-temperature reaction zone, and can respectively perform the first high-temperature treatment and the second high-temperature treatment on the heat carrier particles, polymer particles and composite carbonization materials, thereby realizing precise control of the temperature of the carbonization process; by adjusting the temperature and fluidizing gas flow rate of the low-temperature reaction zone and the high-temperature reaction zone, the entire carbonization process is made more stable and controllable; 3. The carbonized particles obtained by the preparation method of carbonized particles provided in the present application have a particle size of 5 μm-80 μm. The carbonized particles of this size do not need to be ground and can directly participate in subsequent activation and other treatments to prepare porous electrode carbon, thereby achieving the effect of continuous operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the description of the embodiments of the present application will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0017] Figure 1 A flow chart of a method for preparing carbonized particles provided in an embodiment of the present application is shown; Figure 2 A structural diagram of a system for preparing carbonized particles proposed in an embodiment of the present application is shown.

[0018] Description of reference numerals: 1. Carbonized fluidized bed; 11. Porous distribution plate; 12. Low temperature reaction zone; 121. Mixed raw material inlet; 13. High temperature reaction zone; 131. Fluidizing gas inlet; 14. Overflow pipe; 15. Exhaust gas outlet; 16. Carbonized material outlet. DETAILED DESCRIPTION

[0019] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0020] In the drawings, the size of the constituent elements, the thickness of the layer or the area may be exaggerated for the sake of clarity. Therefore, any implementation of the present disclosure is not necessarily limited to the size shown in the drawings, and the shapes and sizes of the components in the drawings do not reflect the true proportions. In addition, the drawings schematically show ideal examples, and any implementation of the present disclosure is not limited to the shapes or values ​​shown in the drawings.

[0021] In the related art, the process of preparing porous electrode carbon mainly includes two steps: carbonization and activation, and the carbonization step is particularly important. The traditional carbonization method will cause the precursor particles to soften and stick together at high temperatures, forming difficult-to-control agglomerates, which not only affects the particle size and density distribution of the carbonized particles, but also increases the difficulty and cost of subsequent grinding treatment. In addition, the formation of agglomerates may also lead to the destruction of the pore structure and reduce the specific surface area and electrochemical activity of the carbonized particles. Therefore, there is an urgent need for an innovative carbonization technology that can achieve an efficient carbonization process while maintaining the dispersibility of the precursor particles, which is conducive to the subsequent preparation of high-performance, low-cost porous carbon electrode materials.

[0022] See also Figure 1 , Figure 1 A flow chart of a method for preparing carbonized particles provided in an embodiment of the present application is shown, and the specific operation steps include: S1: Under the action of fluidizing gas, the polymer particles and the heat carrier particles are placed at 200°C-400°C for the first high temperature treatment, and after 0.5 h-20 h, a composite carbonized material is obtained; S2: Continue to raise the temperature to 500 ℃-950 ℃ for a second high temperature treatment. After 0.5 h-20 h, carbonized particles are obtained.

[0023] The polymer particles include at least one of epoxy resin, phenolic resin, urea-formaldehyde resin, unsaturated resin and polycarbonate resin; the heat carrier particles include at least one of magnesium oxide, sodium chloride, potassium chloride, calcium chloride, calcium oxide, sodium silicate, calcium carbonate, sodium carbonate and magnesium carbonate.

[0024] In specific implementation, the polymer particles are mixed with the heat carrier particles under the action of the fluidizing gas and subjected to high temperature treatment. This method can effectively disperse the polymer particles, prevent them from softening at high temperatures and forming particularly large viscous agglomerates, and is more helpful in controlling the particle size and density of the carbonized particles.

[0025] By introducing heat carrier particles, the growth of particles during the carbonization process is inhibited, and the carbonized particles will not grow excessively; it also helps to reduce the wall adhesion of polymer particles during the carbonization process, making engineering operations more convenient; the heat carrier particles also serve as heat transfer media to accelerate heat conduction and improve the uniformity and efficiency of the carbonization process. The heat carrier particles provided in the embodiments of the present application have the advantages of high stability, small diameter, and good fluidity. By using batch preparation, the production capacity per unit time can be increased by 3 to 10 times.

[0026] In a specific implementation, the generated carbonized particles with heat carrier particles can be used to obtain porous carbonized particles by removing the heat carrier particles, which can reduce the activation time by 30%-50%.

[0027] In a specific implementation, the chloride in the heat carrier particles can be used at a temperature below 780°C, and the sodium silicate, carbonate, magnesium oxide and calcium oxide can be used at a temperature below 950°C.

[0028] In some embodiments, the mass ratio of polymer particles to heat carrier particles is 1:(1-3).

[0029] In a specific implementation, the mass ratio of the polymer particles to the heat carrier particles can be 1:1, 1:1.5, 1:2, 1:2.5 or 1:3.

[0030] In specific implementation, within the above mass ratio range, the number of heat carrier particles is sufficient to effectively disperse the polymer particles, prevent them from agglomerating into large particles during the high-temperature carbonization process, keep the carbonized particles small and uniform, and create favorable conditions for the subsequent activation step.

[0031] In some embodiments, the polymer particles have a diameter of 5 μm to 50 μm; The diameter of the heat carrier particles is 50 μm-200 μm.

[0032] In practice, small-sized polymer particles tend to form finer carbonized particles, while large-sized heat carrier particles help maintain the dispersion of these fine particles and prevent polymer particles from agglomerating at high temperatures. Large-sized heat carrier particles can also provide a larger surface area, which is conducive to the rapid transfer of heat, and because polymer particles are smaller, they can absorb heat and undergo carbonization reactions faster, thereby improving the heat transfer efficiency of the entire process.

[0033] In some embodiments, the temperature of the first high temperature treatment is 270°C-360°C.

[0034] In some embodiments, the temperature of the second high temperature treatment is 750° C.-900° C., and the time of the second high temperature treatment is 3 h-12 h.

[0035] In some embodiments, the fluidizing gas includes at least one of N2, CO, H2, Ar, He, CO2, and CH4.

[0036] In a specific implementation, inert gases such as N2, Ar, and He can provide a relatively oxygen-free environment during the carbonization process to prevent the polymer particles from undergoing oxidation reactions at high temperatures.

[0037] In specific implementation, the fluidizing gas not only plays a fluidizing role, but also carries the heat carrier particles for uniform distribution, ensuring that the polymer particles can fully contact the heat and undergo a carbonization reaction.

[0038] In some embodiments, the first high temperature treatment process includes: The heat carrier particles are fluidized under the action of the fluidizing gas, the polymer particles melt and soften at a temperature of 200°C-400°C, and are bonded and solidified with the fluidized heat carrier particles to obtain a composite carbonized material.

[0039] In specific implementation, under the action of fluidizing gas, the heat carrier particles are fluidized, which helps to distribute more evenly, further enhance the dispersion effect of polymer particles, and avoid their agglomeration and wall adhesion at high temperature. After the polymer particles are melted and softened, they are more likely to contact and bond with the heat carrier particles to form a more uniform composite carbonized material.

[0040] In some embodiments, the curing time is 1 min-10 min. Preferably, the curing time is 3 min-6 min.

[0041] See also Figure 2 , Figure 2 A system for preparing carbonized particles provided in an embodiment of the present application is shown, which specifically includes: Carbonized fluidized bed 1; A porous distribution plate is provided in the carbonization fluidized bed 1, and the porous distribution plate divides the carbonization fluidized bed 1 into a low-temperature reaction zone 12 and a high-temperature reaction zone 13; The low temperature reaction zone 12 is provided with a mixed raw material inlet 121, and the mixed raw material inlet 121 is used to introduce polymer particles and heat carrier particles into the low temperature reaction zone 12; the low temperature reaction zone 12 is used to perform a first high temperature treatment on the polymer particles and the heat carrier particles to obtain a composite carbonized material; The high temperature reaction zone 13 is used to perform a second high temperature treatment on the composite carbonized material to convert it into carbonized particles; the high temperature reaction zone 13 is provided with a fluidizing gas inlet 131, and the fluidizing gas inlet 131 is used to introduce fluidizing gas into the carbonizing fluidized bed 1 to make the mixed raw materials and composite carbonized materials in the carbonizing fluidized bed 1 in a fluidized state.

[0042] In specific implementation, the system can prepare carbonized particles with excellent pore structure by precisely controlling the carbonization process; through the design of a two-stage temperature carbonization fluidized bed 1, precise control of the temperature of the carbonization process is achieved, and carbonized particles suitable for activation can be directly prepared without grinding treatment, thereby simplifying the production process and reducing production costs.

[0043] In some embodiments, the low temperature reaction zone 12 and the high temperature reaction zone 13 are respectively provided with temperature control devices, and the temperatures of the low temperature reaction zone 12 and the high temperature reaction zone 13 are controlled to remain constant for a period of time through a preset program.

[0044] In some embodiments, an overflow pipe 14 is disposed outside the carbonization fluidized bed 1 , one end of the overflow pipe 14 is connected to the low-temperature reaction zone 12 , and the other end is connected to the high-temperature reaction zone 13 ; the composite carbonized material flows to the high-temperature reaction zone 13 through the overflow pipe 14 .

[0045] In specific implementation, by setting up the overflow pipe 14, it is helpful to quickly transport the composite carbonized material formed in the low-temperature reaction zone 12 to the high-temperature reaction zone 13. On the one hand, it avoids blockage of the low-temperature reaction zone 12, allowing solid particles and fluidizing gas to continuously enter the low-temperature reaction zone 12 to ensure the smooth progress of the first high-temperature reaction; on the other hand, it accelerates the process of further carbonization of the composite carbonized material and improves the reaction efficiency.

[0046] In some embodiments, a tail gas outlet 15 is further provided on the carbonization fluidized bed 1 , and the fluidizing gas is discharged from the carbonization fluidized bed 1 through the tail gas outlet 15 .

[0047] In specific implementation, by setting the tail gas outlet 15, the organic gas and water vapor generated in the low-temperature reaction zone 12 can escape from the carbonization fluidized bed 1 in the shortest time without contacting the materials in the high-temperature reaction zone 13, thereby avoiding adhesion or the generation of impurities such as amorphous carbon, which can improve the product quality by 20%-30%.

[0048] In some embodiments, a carbonized material outlet 16 is further provided on the carbonized fluidized bed 1 , and the carbonized particles are discharged from the high-temperature reaction zone 13 along the carbonized material outlet 16 .

[0049] In specific implementation, by providing the carbonized material outlet 16 , the obtained carbonized particles can be quickly discharged from the carbonization fluidized bed 1 , thereby avoiding over-carbonization and making the carbonization process more controllable.

[0050] The present application provides a carbonized particle obtained by the above preparation method, wherein the particle size of the carbonized particle is 5 μm-80 μm. In the subsequent activation treatment, no further grinding is required, and the carbonized particle can be directly used for the activation treatment to achieve the effect of continuous operation.

[0051] In specific implementation, the surface reaction activity of the carbonized particles in this size range is higher, which is conducive to sufficient contact and reaction with the activator in the subsequent activation process, so that the activator can more easily penetrate into the interior of the particles, react with carbon atoms and form pores, and finally form a more open and connected pore structure, thereby improving the conductivity and capacitance properties of the product porous electrode carbon.

[0052] In order to enable those skilled in the art to more clearly understand the present application, a method and system for preparing carbonized particles of the present application are now described in detail through the following examples.

[0053] Example Example 1 1. Load a large amount of heat carrier particles (magnesium oxide, particle size 50 μm-100 μm) into the carbonization fluidized bed through the mixed raw material inlet and accumulate in the high-temperature reaction zone; introduce fluidizing gas (95% CO, 5% He) into the carbonization fluidized bed from the fluidizing gas inlet to put the heat carrier particles in a fluidized state; 2. Raise the temperature in the high-temperature reaction zone to 920°C-950°C, and the fluidizing gas and heat carrier particles pass through the porous distribution plate and enter the low-temperature reaction zone, and then form a bed layer of a certain height; 3. The polymer particles (phenolic resin, particle size 6 μm-9 μm) with a mass ratio of 1:1 to the heat carrier particles are introduced into the low-temperature reaction zone of the carbonization fluidized bed along the mixed raw material inlet, and the temperature is controlled at 200 ℃-300 ℃ for the first high-temperature treatment. After the polymer particles are rapidly melted and softened at high temperature, they are dispersed by a large number of heat carrier particles to form small composite particles (particle size 3 μm-30 μm), which are solidified after 3 minutes to obtain composite carbonized materials; a large amount of organic gas generated during the carbonization process moves upward and is discharged from the carbonization fluidized bed through the tail gas outlet; 4. With the continuous feeding of particles, the composite carbonized materials in the low-temperature reaction zone continue to increase, and move downward through the porous distribution plate and the overflow pipe to reach the high-temperature reaction zone. The temperature of the high-temperature reaction zone is controlled at 920 ℃-950 ℃ for the second high-temperature treatment; 5. The composite carbonized particles in the high-temperature reaction zone are in contact with the high-temperature gas and the high-temperature heat carrier particles, and are further carbonized for 3 hours. The proportion of the obtained carbonized particles having a particle size of 5 μm-6 μm is greater than 90%, and the obtained carbonized particles are discharged from the carbonization fluidized bed along the carbonization material outlet; 6. The above process can be operated continuously by continuously introducing gas and particles.

[0054] Example 2 1. Load a large amount of heat carrier particles (potassium oxide, particle size 100 μm-200 μm) into the carbonization fluidized bed through the mixed raw material inlet and accumulate in the high-temperature reaction zone; introduce fluidizing gas (90% nitrogen 10% CH4) into the carbonization fluidized bed from the fluidizing gas inlet to put the heat carrier particles in a fluidized state; 2. Raise the temperature in the high-temperature reaction zone to 500°C-700°C, and the fluidizing gas and heat carrier particles pass through the porous distribution plate and enter the low-temperature reaction zone, and then form a bed layer of a certain height; 3. The polymer particles (90% phenolic resin + 10% urea-formaldehyde resin, particle size 40 μm-50 μm) with a mass ratio of 1:2 to the heat carrier particles are introduced into the low-temperature reaction zone of the carbonization fluidized bed along the mixed raw material inlet, and the temperature is controlled at 350 ℃-400 ℃ for the first high-temperature treatment. After the polymer particles are rapidly melted and softened at high temperature, they are dispersed by a large number of heat carrier particles to form small composite particles (particle size 3 μm-30 μm), which are solidified after 5 minutes to obtain composite carbonized materials; a large amount of organic gas generated during the carbonization process moves upward and is discharged from the carbonization fluidized bed through the tail gas outlet; 4. With the continuous feeding of particles, the composite carbonized materials in the low-temperature reaction zone continue to increase, and move downward through the porous distribution plate and the overflow pipe to reach the high-temperature reaction zone. The temperature of the high-temperature reaction zone is controlled at 500 ℃-700 ℃ for the second high-temperature treatment; 5. The composite carbonized particles in the high temperature reaction zone are in contact with the high temperature gas and the high temperature heat carrier particles, and are further carbonized for 20 hours. The proportion of the obtained carbonized particles having a particle size of 35 μm-45 μm is greater than 85%, and the obtained carbonized particles are discharged from the carbonization fluidized bed along the carbonization material outlet; 6. The above process can be operated continuously by continuously introducing gas and particles.

[0055] Example 3 1. Load a large amount of heat carrier particles (sodium silicate, particle size 150 μm-200 μm) into the carbonization fluidized bed through the mixed raw material inlet and accumulate in the high-temperature reaction zone; introduce fluidizing gas (50% Ar, 50% He) into the carbonization fluidized bed from the fluidizing gas inlet to put the heat carrier particles in a fluidized state; 2. Raise the temperature in the high-temperature reaction zone to 900°C-950°C, and the fluidizing gas and heat carrier particles pass through the porous distribution plate and enter the low-temperature reaction zone, and then form a bed layer of a certain height; 3. The polymer particles (30% phenolic resin + 30% unsaturated resin + 40% polycarbonate resin, particle size 3 μm-12 μm) with a mass ratio of 2:3 to the heat carrier particles are introduced into the low-temperature reaction zone of the carbonization fluidized bed through the mixed raw material inlet, and the temperature is controlled at 300 ℃-400 ℃ for the first high-temperature treatment. After the polymer particles are rapidly melted and softened at high temperature, they are dispersed by a large number of heat carrier particles to form small composite particles (particle size 3 μm-30 μm), which are solidified after 1 minute to obtain composite carbonized materials; a large amount of organic gas generated during the carbonization process moves upward and is discharged from the carbonization fluidized bed through the tail gas outlet; 4. With the continuous feeding of particles, the composite carbonized materials in the low-temperature reaction zone continue to increase, and move downward through the porous distribution plate and the overflow pipe to reach the high-temperature reaction zone. The temperature of the high-temperature reaction zone is controlled at 900 ℃-950 ℃ for the second high-temperature treatment; 5. The composite carbonized particles in the high temperature reaction zone are in contact with the high temperature gas and the high temperature heat carrier particles, and are further carbonized for 10 hours. The proportion of the obtained carbonized particles having a particle size of 2 μm-8 μm is greater than 85%, and the obtained carbonized particles are discharged from the carbonization fluidized bed along the carbonization material outlet; 6. The above process can be operated continuously by continuously introducing gas and particles.

[0056] Example 4 1. Load a large amount of heat carrier particles (50% magnesium oxide + 2% calcium oxide + 10% magnesium carbonate + 38% calcium carbonate, particle size 100μm-150μm) into the carbonization fluidized bed through the mixed raw material inlet and accumulate in the high-temperature reaction zone; introduce fluidizing gas (90% nitrogen, 10% H2) into the carbonization fluidized bed from the fluidizing gas inlet to put the heat carrier particles in a fluidized state; 2. The temperature in the high temperature reaction zone is raised to 820°C, and the fluidizing gas and heat carrier particles pass through the porous distribution plate and enter the low temperature reaction zone, and then form a bed layer of a certain height; 3. The polymer particles (50% epoxy resin + 50% unsaturated resin, particle size 10 μm-30 μm) with a mass ratio of 1:1 to the heat carrier particles are introduced into the low-temperature reaction zone of the carbonization fluidized bed along the mixed raw material inlet, and the temperature is controlled at 200 ℃-400 ℃ for the first high-temperature treatment. After the polymer particles are rapidly melted and softened at high temperature, they are dispersed by a large number of heat carrier particles to form small composite particles (particle size 3 μm-30 μm), which are solidified after 6 minutes to obtain composite carbonized materials; a large amount of organic gas generated during the carbonization process moves upward and is discharged from the carbonization fluidized bed through the tail gas outlet; 4. With the continuous feeding of particles, the composite carbonized materials in the low-temperature reaction zone continue to increase, and move downward through the porous distribution plate and the overflow pipe to reach the high-temperature reaction zone. The temperature of the high-temperature reaction zone is controlled at 820 °C for the second high-temperature treatment; 5. The composite carbonized particles in the high temperature reaction zone are in contact with the high temperature gas and the high temperature heat carrier particles, and are further carbonized for 0.5 hours. The proportion of the obtained carbonized particles having a particle size of 7 μm-25 μm is greater than 85%. The obtained carbonized particles are discharged from the carbonization fluidized bed along the carbonization material outlet; 6. The above process can be operated continuously by continuously introducing gas and particles.

[0057] Example 5 1. Load a large amount of heat carrier particles (sodium oxide, particle size 50 μm-70 μm) into the carbonization fluidized bed through the mixed raw material inlet and accumulate in the high-temperature reaction zone; introduce fluidizing gas (90% nitrogen, 10% H2) into the carbonization fluidized bed from the fluidizing gas inlet to put the heat carrier particles in a fluidized state; 2. The temperature in the high-temperature reaction zone is raised to 750°C, and the fluidizing gas and heat carrier particles pass through the porous distribution plate and enter the low-temperature reaction zone, and then form a bed layer of a certain height; 3. The polymer particles (50% epoxy resin + 50% unsaturated resin, particle size 30 μm-50 μm) with a mass ratio of 1:2 to the heat carrier particles are introduced into the low-temperature reaction zone of the carbonization fluidized bed through the mixed raw material inlet, and the temperature is controlled at 280 ℃-360 ℃ for the first high-temperature treatment. After the polymer particles are rapidly melted and softened at high temperature, they are dispersed by a large number of heat carrier particles to form small composite particles (particle size 3 μm-30 μm, and solidified after 3 minutes to obtain composite carbonized materials); a large amount of organic gas generated during the carbonization process moves upward and is discharged from the carbonization fluidized bed through the tail gas outlet; 4. With the continuous feeding of particles, the composite carbonized materials in the low-temperature reaction zone continue to increase, and move downward through the porous distribution plate and the overflow pipe to reach the high-temperature reaction zone. The temperature of the high-temperature reaction zone is controlled at 750 °C for the second high-temperature treatment; 5. The composite carbonized particles in the high temperature reaction zone are in contact with the high temperature gas and the high temperature heat carrier particles, and are further carbonized for 12 hours. The proportion of the obtained carbonized particles having a particle size of 2 μm-6 μm is greater than 85%, and the obtained carbonized particles are discharged from the carbonization fluidized bed along the carbonization material outlet; 6. The above process can be operated continuously by continuously introducing gas and particles.

[0058] Example 6 1. Load a large amount of heat carrier particles (sodium carbonate, particle size 70 μm-150 μm) into the carbonization fluidized bed through the mixed raw material inlet and accumulate in the high-temperature reaction zone; introduce fluidizing gas (75% CO2, 30% N2) into the carbonization fluidized bed from the fluidizing gas inlet to put the heat carrier particles in a fluidized state; 2. Raise the temperature in the high-temperature reaction zone to 800°C-850°C, and the fluidizing gas and heat carrier particles pass through the porous distribution plate and enter the low-temperature reaction zone, and then form a bed layer of a certain height; 3. The polymer particles (unsaturated resin, particle size 5 μm-12 μm) with a mass ratio of 1:3 to the heat carrier particles are introduced into the low-temperature reaction zone of the carbonization fluidized bed along the mixed raw material inlet, and the temperature is controlled at 270 ℃-320 ℃ for the first high-temperature treatment. After the polymer particles are rapidly melted and softened at high temperature, they are dispersed by a large number of heat carrier particles to form small composite particles (particle size 3 μm-30 μm), which are solidified after 1-3 minutes to obtain composite carbonized materials; a large amount of organic gas generated during the carbonization process moves upward and is discharged from the carbonization fluidized bed through the tail gas outlet; 4. With the continuous feeding of particles, the composite carbonized materials in the low-temperature reaction zone continue to increase, and move downward through the porous distribution plate and the overflow pipe to reach the high-temperature reaction zone. The temperature of the high-temperature reaction zone is controlled at 800 ℃ 850 ℃ for the second high-temperature treatment; 5. The composite carbonized particles in the high temperature reaction zone are in contact with the high temperature gas and the high temperature heat carrier particles, and are further carbonized for 6 hours. The proportion of the obtained carbonized particles having a particle size of 4 μm-10 μm is greater than 75%, and the obtained carbonized particles are discharged from the carbonization fluidized bed along the carbonization material outlet; 6. The above process can be operated continuously by continuously introducing gas and solid.

[0059] In summary, the method and system for preparing carbonized particles proposed in this application have the advantages of effectively dispersing polymer particles such as resins with heat carrier particles to avoid softening and sticking during carbonization, thereby achieving the purpose of continuous operation. After the heat carrier particles are subsequently dissolved, porous carbonized particles can be formed. This method can reduce grinding energy consumption and costs, and can also achieve carbonization degree control at different temperatures, which can save energy and reduce material consumption during subsequent activation.

[0060] The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the various embodiments can be referenced to each other.

[0061] Although the preferred embodiments of the present application have been described, those skilled in the art may make additional changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the embodiments of the present application.

[0062] Finally, it should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or terminal device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or terminal device. In the absence of further restrictions, the elements defined by the sentence "including one..." do not exclude the existence of other identical elements in the process, method, article or terminal device including the elements.

[0063] The above is a detailed introduction to the preparation method and system of carbonized particles provided by the present application. Specific examples are used in this article to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method of the present application and its core idea; at the same time, for general technical personnel in this field, according to the idea of ​​the present application, there will be changes in the specific implementation method and application scope. In summary, the content of this specification should not be understood as a limitation on the present application.

Claims

1. A method for preparing carbonized particles, characterized in that: The method comprises: Under the action of fluidizing gas, the polymer particles and the heat carrier particles are placed at 200°C-400°C for the first high temperature treatment, and after 0.5 h-20 h, a composite carbonized material is obtained; Continue to raise the temperature to 500°C-950°C, perform a second high temperature treatment, and after 0.5 h-20 h, obtain the carbonized particles; Wherein, the polymer particles include at least one of epoxy resin, phenolic resin, urea-formaldehyde resin, unsaturated resin and polycarbonate resin; the heat carrier particles include at least one of magnesium oxide, sodium chloride, potassium chloride, calcium chloride, calcium oxide, sodium silicate, calcium carbonate, sodium carbonate and magnesium carbonate.

2. The method for preparing carbonized particles according to claim 1, characterized in that: The mass ratio of the polymer particles to the heat carrier particles is 1:(1-3).

3. The method for preparing carbonized particles according to claim 1, characterized in that: The diameter of the polymer particles is 5 μm-50 μm; The diameter of the heat carrier particles is 50 μm-200 μm.

4. The method for preparing carbonized particles according to claim 1, characterized in that: The temperature of the first high temperature treatment is 270°C-360°C.

5. The method for preparing carbonized particles according to claim 1, characterized in that: The temperature of the second high temperature treatment is 750°C-900°C, and the time of the second high temperature treatment is 3 h-12 h.

6. The method for preparing carbonized particles according to claim 1, characterized in that: The fluidizing gas includes at least one of N2, CO, H2, Ar, He, CO2 and CH4.

7. The method for preparing carbonized particles according to claim 1, characterized in that: The process of the first high temperature treatment comprises: The heat carrier particles are fluidized under the action of the fluidizing gas, the polymer particles melt and soften at a temperature of 200° C.-400° C., and are bonded and solidified with the fluidized heat carrier particles to obtain the composite carbonized material.

8. A system for preparing carbonized particles, characterized in that: The system is used to perform the method for preparing carbonized particles according to any one of claims 1 to 7, and the system comprises: a carbonization fluidized bed; A porous distribution plate is arranged in the carbonization fluidized bed, and the porous distribution plate divides the carbonization fluidized bed into a low-temperature reaction zone and a high-temperature reaction zone; The low temperature reaction zone is provided with a mixed raw material inlet, and the mixed raw material inlet is used to introduce polymer particles and heat carrier particles into the low temperature reaction zone; the low temperature reaction zone is used to perform a first high temperature treatment on the polymer particles and the heat carrier particles to obtain a composite carbonized material; The high temperature reaction zone is used to perform a second high temperature treatment on the composite carbonized material to convert it into carbonized particles; the high temperature reaction zone is provided with a fluidizing gas inlet, and the fluidizing gas inlet is used to introduce fluidizing gas into the carbonization fluidized bed to fluidize the mixed raw materials and composite carbonized material in the carbonization fluidized bed.

9. The system for preparing carbonized particles according to claim 8, characterized in that: An overflow pipe is arranged outside the carbonization fluidized bed, one end of the overflow pipe is connected to the low-temperature reaction zone, and the other end is connected to the high-temperature reaction zone; the composite carbonized material flows to the high-temperature reaction zone through the overflow pipe; The carbonization fluidized bed is provided with an exhaust gas outlet, and the fluidizing gas is discharged from the carbonization fluidized bed through the exhaust gas outlet; The carbonization fluidized bed is provided with a carbonization material outlet, and the carbonized particles are discharged from the high-temperature reaction zone along the carbonization material outlet.

10. A carbonized particle obtained by the method for preparing carbonized particles according to any one of claims 1 to 7, characterized in that: The particle size of the carbonized particles is 5 μm-80 μm.

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