Continuous fluidized apparatus and method for steam-activated porous carbon

Abstract

The application relates to the technical field of porous carbon material preparation, and relates to a continuous fluidization equipment and method for water vapor activated porous carbon. The equipment comprises a fluidized bed reactor, a feeding mechanism, a water vapor preheating mechanism, a discharging mechanism, a heating mechanism and an intelligent control system; the fluidized bed reactor of the application can adapt to the activation process requirements of porous carbon preparation, can strengthen the gas-solid mixing effect, guarantee the smooth and efficient promotion of the reaction, accurately control the product quality, and optimize the stability and safety of the overall operation. Meanwhile, the water vapor preheating mechanism is used to preheat water vapor, and the water vapor enters the pre-activation section and the deep activation section in two ways, the accurate regulation and control of the pore size distribution of the porous carbon are realized, and the intelligent control system is used to automatically adjust the feeding, heating, activation and discharging and other operations, the whole system has high automation, the real-time monitoring and feedback regulation of key parameters are realized through the intelligent control system, and manual intervention is reduced.

Description

Technical Field

[0001] This application relates to the field of porous carbon material preparation technology, and more specifically, to a continuous fluidization apparatus and method for steam-activated porous carbon. Background Technology

[0002] Carbon has a strong bonding ability and can form a variety of carbon materials, among which porous carbon materials have attracted much attention due to their advantages such as large specific surface area, adjustable pore size, and good chemical stability. Common preparation methods for porous carbon include activation methods, template methods, and sol-gel methods. Activation methods are divided into physical and chemical activation. Physical methods use water vapor or carbon dioxide as activating agents, creating pores at high temperatures, but the interaction force is weak. Chemical methods use chemical reagents, which can obtain a large specific surface area, but highly corrosive reagents can easily cause pore collapse and corrosion of equipment, while mild reagents result in high activation temperatures or insufficient pore structure control. Template methods are divided into hard and soft template methods. Hard template methods can obtain ordered structures, but the template agent is highly toxic and costly; soft template methods have gentle template removal, but the process is complex and difficult to scale up. Sol-gel methods are simple to operate and have mild conditions, but drying can easily cause pore collapse, and they often need to be combined with template methods.

[0003] From an industrial production perspective, these methods still face numerous challenges in practical applications. In activation processes using fluidized beds as the core equipment, traditional fluidized bed operations are mostly batch-based, resulting in long production cycles (over 16 hours per batch) and low equipment utilization. Batch-to-batch reaction parameters fluctuate significantly, leading to product performance variations of ±15% and poor stability. Frequent heating and cooling consumes high energy, and fine carbon particles easily escape, resulting in low material utilization. Furthermore, existing technologies employ rotary kilns for continuous activation of porous carbon, but rotary kilns suffer from low heat transfer efficiency and uneven material mixing, leading to low product yields (typically below 20%). Additionally, the large temperature distribution within the kiln results in poor product uniformity (specific surface area fluctuations can reach ±20%). Moreover, the large equipment footprint and high energy consumption further increase production costs.

[0004] With the rapid development of energy, environmental protection, chemical industry and other fields, high specific surface area (≥1800m²) is becoming increasingly important. 2 Porous carbon with a specific pore size distribution (e.g., mesopores ≥ 60%) exhibits significant advantages in high-end applications. Fluidized bed reactors are commonly used for the activation and preparation of porous carbon, achieving efficient activation through sufficient gas-solid two-phase contact. Compared to equipment such as rotary kilns, this allows for more precise control of product performance. However, fluidized bed equipment for porous carbon has not yet been widely adopted in the market, primarily due to issues such as discontinuous production, poor product quality stability, high energy and material losses, and insufficient control over the activation process.

[0005] Therefore, developing a fluidized bed equipment and method that can achieve continuous production, precise control of the activation process, and reduced energy consumption and material loss is of great significance for promoting the upgrading of the porous carbon industry.

[0006] In view of this, the present invention is proposed. Summary of the Invention

[0007] The purpose of this application is to provide a continuous fluidization device and method for steam-activated porous carbon, aiming to break through the bottlenecks of traditional technology and achieve efficient, stable, and low-cost large-scale production of porous carbon.

[0008] To achieve the above objectives, in a first aspect, the present invention provides a continuous fluidization device for steam-activated porous carbon, comprising: a fluidized bed reactor, a feeding mechanism, a steam preheating mechanism, a discharging mechanism, a heating mechanism, and an intelligent control system;

[0009] The fluidized bed reactor includes a top settling section, a pre-activation section, and a deep activation section connected sequentially from top to bottom. A narrowing section is provided between adjacent sections. The cone angle of the narrowing section is ≤30°, and the diameter of the top settling section is > the diameter of the pre-activation section is > the diameter of the deep activation section.

[0010] The top settling section is provided with a feeding port and a tail gas discharge port; the pre-activation section is provided with a stirring device; the narrowing section between the pre-activation section and the deep activation section is provided with a first gas distributor; the bottom of the deep activation section is provided with a discharge port and a second gas distributor.

[0011] The feeding mechanism is connected to the feeding port, the steam preheating mechanism is connected to both the first gas distributor and the second gas distributor, the unloading mechanism is connected to the discharge port, and the heating mechanism is sleeved on the outside of the pre-activation section and the deep activation section.

[0012] The intelligent control system is electrically connected to the feeding mechanism, the steam preheating mechanism, the unloading mechanism, and the heating mechanism, respectively.

[0013] In an optional embodiment, the height-to-diameter ratio (H / D) of the pre-activated section is 3-5, and the height-to-diameter ratio (H / D) of the deep-activated section is 1.5-3.

[0014] In an optional embodiment, the steam preheating mechanism includes a steam generating mechanism, a main gas generating pipe, a preheating furnace, a first pipeline, and a second pipeline. The outlet of the steam generating mechanism is connected to the main gas generating pipe, the main gas generating pipe is connected to the preheating furnace, the outlet of the preheating furnace is connected to the first pipeline and the second pipeline, the first pipeline is connected to the first gas distributor, and the second pipeline is connected to the second gas distributor.

[0015] In an optional embodiment, the continuous fluidization device for steam-activated porous carbon further includes a gas carrier mechanism connected to the main gas production pipe.

[0016] In an optional embodiment, the first gas distributor is an annular porous tube structure, arranged circumferentially along the inner wall of the corresponding narrowed section, with the opening direction inclined upward at 45°, the pore diameter 1~3mm, and the opening ratio 1.5~3%;

[0017] And / or, the second gas distributor is a disc-shaped perforated plate, horizontally positioned at the bottom of the deep activation section, with a pore diameter of 2~4mm and an opening rate of 2~4%.

[0018] In an optional embodiment, a spiral agitator is provided in the pre-activation section, and the spiral agitator extends below the material level by a distance of 1 / 2 to 1 / 8 of the diameter of the pre-activation section.

[0019] In an optional embodiment, the rotational speed of the spiral agitator is 50~200 r / min;

[0020] And / or, the blades of the spiral agitator are rotatably mounted on the agitator shaft; the rotation angle of the blades is 30°-60°.

[0021] In an optional implementation, the intelligent control system includes monitoring sensors and an adjustment module;

[0022] The monitoring sensor includes:

[0023] The temperature sensor is used to monitor the activation temperature of the pre-activation section and the deep activation section;

[0024] A level sensor used to monitor the material level in the fluidized bed reactor;

[0025] A mass flow sensor used to monitor the mass flow rate of the material discharged at the outlet;

[0026] Material property sensors are used for real-time monitoring of material properties within the fluidized bed reactor;

[0027] The adjustment module includes:

[0028] A heating adjustment module for regulating the heating power of the heating mechanism based on the temperature sensor;

[0029] An infeed / outfeed adjustment module for regulating the rotational speed of the feeding mechanism and the opening degree of the unloading mechanism based on the material level sensor and the mass flow sensor;

[0030] A steam regulation module for adjusting the steam flow rate of the steam preheating mechanism according to the material characteristic sensor;

[0031] An interlocking control module for automatically executing shutdown, cutting off the gas supply, and initiating emergency cooling operations when the detection indicators of the temperature sensor, the level sensor, the mass flow sensor, and the material characteristic sensor exceed the limits.

[0032] Secondly, the present invention provides a continuous fluidization method for steam-activated porous carbon using a continuous fluidization apparatus for steam-activated porous carbon as described in any of the foregoing embodiments, comprising the following steps:

[0033] (1) Continuous feeding: Carbon raw material is continuously fed into the fluidized bed reactor through the feed port of the top settling section, and the air is isolated by the sealed structure. The intelligent control system controls the feeding rate.

[0034] (2) Pre-activation: In the pre-activation section, the heating mechanism is controlled to heat the pre-activation section to 800~1000℃, and the steam preheating mechanism is controlled to introduce steam and carrier gas into the first gas distributor to form a bubbling fluidized state with an apparent gas velocity of 0.04-0.12m / s. The carbon raw material is in contact with preheated steam at 500~600℃ to react.

[0035] (3) Deep activation: The carbon raw material enters the deep activation section, and the heating mechanism is controlled to heat the deep activation section to 800~1000℃. The steam preheating mechanism is controlled to introduce steam and carrier gas into the second gas distributor to form a turbulent fluidization state with an apparent gas velocity of 0.12-0.3m / s. The carbon raw material reacts with preheated steam at 500~600℃.

[0036] (4) Continuous discharge: The activated product is continuously discharged at high temperature through the discharge port at the bottom of the deep activation section;

[0037] The total residence time of the carbon raw material in the reactor is controlled to be 4-10 hours by the intelligent control system.

[0038] In an optional embodiment, the particle size of the carbon raw material is ≤200μm;

[0039] And / or, the carrier gas introduced is one or a combination of nitrogen, argon, and helium;

[0040] And / or, the flow rate-to-volume ratio of the water vapor to the carrier gas is 10-100%;

[0041] And / or, the yield of the prepared porous carbon product is ≥25%, and the specific surface area is ≥1200 m². 2 / g, pore volume ≥0.8cm 3 / g, with 2-50nm mesoporous content ≥60%.

[0042] The beneficial effects of the present invention through the above technical solution are as follows:

[0043] The continuous fluidization equipment for steam-activated porous carbon provided by this invention, by segmenting the fluidized bed reactor and controlling the diameter of the top settling section to be greater than that of the pre-activation section to be greater than that of the deep activation section, and connecting adjacent sections with a narrowing section, can adapt to the activation process requirements of porous carbon preparation. It can enhance the gas-solid mixing effect, ensure the stable and efficient progress of the reaction, accurately control the product quality, and optimize the stability and safety of the overall operation. Simultaneously, this invention utilizes a steam preheating mechanism to preheat steam, which is then divided into two streams: one entering the pre-activation section via a first gas distributor, and the other entering the deep activation section via a second gas distributor. This two-stage segmented design of pre-activation and deep activation, combined with precise temperature control and gas distribution, achieves accurate regulation of the pore size distribution of porous carbon. The proportion of mesopores in the product can reach over 60%, meeting the specific pore structure requirements of different application scenarios. Furthermore, an intelligent control system automates the feeding, heating, activation, and discharging operations, resulting in a high degree of automation. The intelligent control system enables real-time monitoring and feedback adjustment of key parameters, reducing manual intervention. This invention achieves true continuous production, solving the problems of low production efficiency and poor product consistency inherent in traditional batch operations. Equipment utilization is increased by over 50%, product performance stability is significantly improved, and specific surface area fluctuations are controlled within ±5%, enhancing the controllability and safety of the production process. It is particularly suitable for large-scale industrial production.

[0044] Other features and advantages of this application will be described in detail in the following detailed description section. Attached Figure Description

[0045] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0046] Figure 1 A schematic diagram of the structure of the continuous fluidization device for steam-activated porous carbon provided in this application;

[0047] Figure 2 A schematic diagram of the intelligent control system in the continuous fluidization equipment for steam-activated porous carbon provided in this application;

[0048] Figure 3 A process flow diagram of the continuous fluidization method for steam-activated porous carbon provided in this application.

[0049] Icons: 100 - Continuous fluidized bed reactor for steam-activated porous carbon; 110 - Fluidized bed reactor; 111 - Top settling section; 1111 - Feed port; 1112 - Tail gas outlet; 112 - Pre-activation section; 113 - Deep activation section; 1131 - Discharge port; 114 - Reduction section; 115 - Stirring device; 116 - First gas distributor; 117 - Second gas distributor; 118 - Metal filter column; 119 - Pulse pipe; 120 - Feeding mechanism; 130 - Steam preheating mechanism; 131 - Steam generation mechanism; 13 2-Main gas production pipe; 133-Preheating furnace; 134-First pipeline; 135-Second pipeline; 140-Unloading mechanism; 150-Heating mechanism; 160-Intelligent control system; 161-Monitoring sensor; 1611-Temperature sensor; 1612-Level sensor; 1613-Mass flow sensor; 1614-Material characteristic sensor; 162-Regulation module; 1621-Heating regulation module; 1622-Infeed / Discharge regulation module; 1623-Steam regulation module; 1624-Interlock regulation module; 170-Carrier gas mechanism. Detailed Implementation

[0050] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. The components of the embodiments of this application described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0051] In the description of this application, it should be noted that the terms "inner" and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product is in use. They are used only for the convenience of describing this application and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this application. Furthermore, the terms "first," "second," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0052] In the description of this application, it should also be noted that, unless otherwise expressly specified and limited, the terms "setup" and "connection" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.

[0053] This study found that conventional porous carbon fluidized bed equipment suffers from problems such as discontinuous production mode, poor product quality stability, high energy consumption and material loss, and insufficient control of the activation process. Specifically:

[0054] The production mode is discontinuous: batch operation, with a single batch cycle taking more than 16 hours, and the effective utilization rate of equipment is less than 30%, making it difficult to meet the needs of large-scale production.

[0055] Poor product quality stability: large fluctuations in reaction parameters between batches, with the specific surface area of ​​porous carbon often fluctuating by ±15%, and poor consistency in pore size distribution, failing to meet the stability requirements of high-end applications.

[0056] High energy consumption and material loss: Frequent heating and cooling wastes energy, resulting in high energy consumption per ton of product; fine carbon powder is easily escaped with airflow, and the material utilization rate is usually less than 85%, increasing production costs.

[0057] Insufficient control over the activation process: Single-stage fluidized beds make it difficult to achieve step-by-step control of "pre-activation-deep activation", making it impossible to optimize activation conditions in stages, resulting in low precision in pore size distribution control and difficulty in accurately matching the mesopore / micropore ratio to application requirements.

[0058] Based on this, please refer to Figure 1 and Figure 2 This application provides a continuous fluidization device 100 for steam-activated porous carbon, comprising: a fluidized bed reactor 110, a feeding mechanism 120, a steam preheating mechanism 130, a discharging mechanism 140, a heating mechanism 150, and an intelligent control system 160. The above structure and its connection relationship will be described in detail below:

[0059] (1) Fluidized bed reactor 110.

[0060] In this invention, the fluidized bed reactor 110 serves as the reaction mechanism for porous carbon. The fluidized bed reactor 110 includes a top settling section 111, a pre-activation section 112, and a deep activation section 113 connected sequentially from top to bottom. A narrowing section 114 is provided between adjacent sections, and the cone angle of the narrowing section 114 is ≤30°. The diameter of the top settling section 111 is > the diameter of the pre-activation section 112 is > the diameter of the deep activation section 113. The top settling section 111 is provided with a feed port 1111 and a tail gas discharge port 1112. The pre-activation section 112 is provided with a stirring device 115. The narrowing section 114 between the pre-activation section 112 and the deep activation section 113 is provided with a first gas distributor 116. The bottom of the deep activation section 113 is provided with a discharge port 1131 and a second gas distributor 117.

[0061] In this invention, the fluidized bed reactor 110 is segmented, with different reaction sections having different functions and diameters. This is to adapt to the activation process requirements for porous carbon preparation, which can enhance the gas-solid mixing effect, ensure the smooth and efficient progress of the reaction, accurately control the product quality, and optimize the overall operational stability and safety.

[0062] Among them, the top settling section 111 has the largest diameter, which can reduce the airflow velocity. After the raw material enters through the feed port 1111, preliminary gas-solid separation can be achieved, preventing unreacted small particles from being directly discharged with the exhaust gas and reducing raw material waste. At the same time, the settling section can buffer the airflow, making the reaction environment of the subsequent pre-activation section 112 more stable. The exhaust gas can also be discharged in an orderly manner through a dedicated emission port, facilitating subsequent treatment and reducing environmental pressure. In addition, a metal filter column 118 is also installed at the top of the top settling section 111, which effectively reduces the escape of fine particulate matter and significantly improves material utilization. At the same time, a pulse pipe 119 is also installed at the top of the top settling section 111. By introducing backflushing air into it, the metal filter column 118 can be backflushed to prevent it from clogging.

[0063] The diameter of the pre-activation section 112 is smaller than that of the top settling section 111. This size design allows for a moderate airflow velocity. This section serves as the initial activation reaction for the raw materials, ensuring sufficient contact between the raw materials and the activating gas without excessively short residence time due to excessive flow velocity, thus guaranteeing sufficient initial activation and laying the foundation for subsequent deep activation. The stirring device 115 in the pre-activation section 112 further improves the uniformity of gas-solid mixing, solves the problem of material agglomeration, and makes the temperature and concentration fields more uniform, allowing each raw material particle to participate uniformly in the pre-activation reaction, ensuring the consistency of product performance after subsequent deep activation. The stirring device 115 is a spiral agitator, and the distance the spiral agitator extends below the material level is 1 / 2 to 1 / 8 of the diameter of the pre-activation section 112. The rotation speed of the spiral agitator is 50~200 r / min; the blades of the spiral agitator are rotatably mounted on the stirring shaft; the rotation angle of the blades is 30°-60°.

[0064] The deep activation section 113, being the smallest in diameter, has the fastest airflow velocity. This rapid airflow enhances the interaction between the activating gas and the material, meeting the requirements for deep activation of porous carbon and contributing to the formation of porous carbon products with high porosity and large specific surface area. Furthermore, the discharge port 1131 at the bottom of this section allows for the timely discharge of the deeply activated porous carbon, preventing the product from being consumed due to over-activation.

[0065] The narrowing section 114 between adjacent sections guides the smooth transition of airflow and material, avoiding the formation of vortices at the section junction and reducing energy loss. The cone angle ≤30° design prevents material accumulation at the transition point, while also conforming to the characteristics of a conical fluidized bed. This ensures a higher airflow velocity in the lower section to maintain fluidization, while gradually reducing the flow velocity in the upper section to suppress fine particle separation, reduce material entrainment losses, ensure stable gas-solid two-phase flow, and allow the activation reaction to proceed continuously.

[0066] The first gas distributor 116 is located in the narrowed section 114 between the pre-activation section 112 and the deep activation section 113. It redistributes the gas entering the deep activation section 113, ensuring that the activating gas passes evenly through the material layer. This prevents excessively high or low gas concentrations in localized areas, guaranteeing a uniform deep activation reaction and improving the yield of porous carbon products. The first gas distributor 116 is an annular porous tube structure, circumferentially arranged along the inner wall of the corresponding narrowed section 114. The opening direction is obliquely upward at 45°, with a pore diameter of 1~3mm and an opening ratio of 1.5~3%.

[0067] The second gas distributor 117 is located at the bottom of the deep activation section 113. It allows the introduced activation gas (water vapor) to enter the reaction zone uniformly, providing stable fluidization power for the bottom material and ensuring that the material is always in a good fluidization state, avoiding "dead zones" and ensuring efficient deep activation. The second gas distributor 117 is a disc-shaped perforated plate, horizontally positioned at the bottom of the deep activation section 113, with a pore diameter of 2~4mm and an opening ratio of 2~4%.

[0068] Furthermore, the present invention also specifies that the height-to-diameter ratio H / D of the pre-activated section 112 is 3~5, and the height-to-diameter ratio H / D of the deep-activated section 113 is 1.5~3.

[0069] The height-to-diameter ratio of the pre-activation section 112 ensures sufficient reaction space height for both the pre-activation section 112 and the deep activation section 113. This prevents insufficient material residence time due to a short reaction section, ensuring that the raw materials complete preliminary dehydration, degassing, or mild oxidation, laying the foundation for deep activation. Combined with the stirring device 115 in the pre-activation section 112, the longer reaction height allows for sufficient transmission of stirring disturbances, preventing material stratification or airflow short-circuiting, ensuring uniform contact between the raw materials and the activation gas, and resulting in a more stable temperature and concentration field. This height-to-diameter ratio also complements the large-diameter design of the top settling section 111, smoothly reducing airflow velocity, minimizing material entrainment, and providing a smooth transition for materials entering the deep activation section 113.

[0070] The high-to-diameter ratio of the deep activation section 113 allows for more concentrated airflow velocity, enhancing the impact and contact strength between the activating gas and the material, and improving pore-forming efficiency. The shorter reaction height controls the material residence time, preventing the porous carbon from being over-activated due to prolonged residence, while also reducing airflow resistance and energy loss. This high-to-diameter ratio can be matched with the bottom second gas distributor 117 to ensure uniform diffusion of the activating gas, while facilitating the rapid discharge of the deeply activated material from the bottom outlet 1131, ensuring continuous production.

[0071] The gradient design of the two-stage high-aspect-ratio section, transitioning from a "long-stage slow reaction" to a "short-stage strong reaction," is well-suited to the reactor's variable-diameter structure, which is "coarse at the top and fine at the bottom." The pre-activation stage 112, with its larger aspect ratio, ensures sufficient reaction, while the deep activation stage 113, with its smaller aspect ratio, enhances reaction efficiency. This not only meets the gradient process requirements for porous carbon preparation but also maintains the fluidization stability of the entire fluidized bed through size synergy, preventing material accumulation or airflow turbulence at the junction of the two stages.

[0072] (2) Feeding mechanism 120.

[0073] The feeding mechanism 120 is used to provide reaction raw materials to the fluidized bed reactor 110. The feeding mechanism 120 is connected to the feeding port 1111. In this invention, the feeding mechanism 120 is a screw feeding device. The screw feeding device is connected through the feeding port 1111 and equipped with a sealing structure to achieve continuous feeding of raw materials and air isolation. In this invention, the screw conveyor is used to feed the raw materials, which can ensure continuous feeding of raw materials and controllable feeding amount, thereby improving the quality stability of the product and enabling continuous production.

[0074] (3) Steam preheating mechanism 130.

[0075] The steam preheating mechanism 130 is used to introduce preheated steam into the fluidized bed reactor 110. The steam acts as an activator to activate the raw materials. In this invention, the steam preheating mechanism 130 is simultaneously connected to the first gas distributor 116 and the second gas distributor 117. The first gas distributor 116 and the second gas distributor 117 can be used to fully disperse the preheated steam, ensuring its uniform distribution and more uniform contact with the raw materials.

[0076] Specifically, the steam preheating mechanism 130 of the present invention includes a steam generating mechanism 131, a main gas generating pipe 132, a preheating furnace 133, a first pipeline 134, and a second pipeline 135. The outlet of the steam generating mechanism 131 is connected to the main gas generating pipe 132, the main gas generating pipe 132 is connected to the preheating furnace 133, the outlet of the preheating furnace 133 is connected to the first pipeline 134 and the second pipeline 135, the first pipeline 134 is connected to the first gas distributor 116, and the second pipeline 135 is connected to the second gas distributor 117.

[0077] The steam generated by the steam generating mechanism 131 enters the main gas generating pipe 132, and is then heated by the preheating furnace 133. After heating, it is introduced into the first pipeline 134 and the second pipeline 135, and then enters the pre-activation section 112 and the deep activation section 113 through the first gas distributor 116 and the second gas distributor 117, respectively, to activate the raw materials.

[0078] Since this invention also requires the introduction of inert carrier gas into the fluidized bed reactor 110 to achieve fluidization, the continuous fluidization device 100 for steam-activated porous carbon in this invention further includes a carrier gas mechanism 170, which is connected to the gas production main pipe 132. By connecting the carrier gas mechanism 170 to the gas production main pipe 132, the carrier gas can be heated simultaneously, and the carrier gas can also be introduced through the first gas distributor 116 and the second gas distributor 117. The introduced inert carrier gas is one or a combination of nitrogen, argon, and helium.

[0079] (4) Unloading mechanism 140.

[0080] The unloading mechanism 140 is connected to the discharge port 1131. In this invention, the unloading mechanism 140 unloads material through a plug valve, and the amount of material unloaded can be adjusted by controlling the opening of the plug valve.

[0081] (5) Heating mechanism 150.

[0082] The heating mechanism 150 is used to heat the fluidized bed reactor 110 to activate it at a temperature of 800~1000℃. Specifically, the heating mechanism 150 in this invention is sleeved on the outside of the pre-activation section 112 and the deep activation section 113. The temperatures of the pre-activation section 112 and the deep activation section 113 can be controlled independently, which makes it easy to adjust different activation temperatures.

[0083] (6) Intelligent control system 160.

[0084] The intelligent control system 160 is electrically connected to the feeding mechanism 120, the steam preheating mechanism 130, the unloading mechanism 140, and the heating mechanism 150, respectively, thereby realizing full control over feeding, activation, unloading, and heating, achieving full intelligence.

[0085] The intelligent control system 160 includes a monitoring sensor 161 and an adjustment module 162.

[0086] The monitoring sensors 161 include: a temperature sensor 1611 for monitoring the activation temperature of the pre-activation section 112 and the deep activation section 113; a level sensor 1612 for monitoring the material inventory in the fluidized bed reactor 110; a mass flow sensor 1613 for monitoring the mass flow rate of the discharge at the discharge port 1131; and a material characteristic sensor 1614 for real-time monitoring of material characteristics (such as particle size, humidity, density, etc.) in the fluidized bed reactor 110.

[0087] The adjustment module 162 includes: a heating adjustment module 1621 for adjusting the heating power of the heating mechanism 150 according to the temperature sensor 1611; an infeed / outfeed adjustment module 1622 for adjusting the rotation speed of the feeding mechanism 120 and the opening of the unloading mechanism 140 according to the material level sensor 1612 and the mass flow sensor 1613; a steam adjustment module 1623 for adjusting the steam flow rate of the steam preheating mechanism 130 according to the material characteristic sensor 1614; and an interlock adjustment module 1624 for automatically executing shutdown, cutting off the gas supply, and starting emergency cooling operations after the detection indicators of the temperature sensor 1611, the material level sensor 1612, the mass flow sensor 1613, and the material characteristic sensor 1614 exceed the limits.

[0088] In this invention, temperature sensors 1611, level sensors 1612, mass flow sensors 1613, and material characteristic sensors 1614 installed in the fluidized bed reactor 110 are used to monitor the reaction temperature, level, and material characteristics in the fluidized bed reactor 110 in real time. This facilitates fully automatic real-time regulation and interlocking control of the reaction parameters in the fluidized bed reactor 110, ensuring the stability of product quality and timely regulation of the activation process.

[0089] In addition, please see Figure 3 The present invention also provides a continuous fluidization method for activating porous carbon with steam using the above-mentioned continuous fluidization device 100 for activating porous carbon with steam, comprising the following steps:

[0090] (1) Continuous feeding: Carbon raw material (particle size ≤200μm) is continuously fed into fluidized bed reactor 110 through feeding port 1111 of top settling section 111. Air is isolated by a sealed structure to control the feeding rate;

[0091] (2) Pre-activation: In the pre-activation section 112, the heating mechanism 150 controls the heating of the pre-activation section 112 to 800~1000℃, and the steam preheating mechanism 130 controls the introduction of steam and carrier gas into the first gas distributor 116 to form a bubbling fluidized state with an apparent gas velocity of 0.04-0.12m / s. The carbon raw material reacts with the preheated steam at 500~600℃. The inert carrier gas introduced is one or a combination of nitrogen, argon, and helium. The flow rate-to-volume ratio of activation steam to inert carrier gas is 10-100%.

[0092] (3) Deep activation: The carbon raw material enters the deep activation section 113. The heating mechanism 150 is controlled to heat the deep activation section 113 to 800~1000℃. The steam preheating mechanism 130 is controlled to introduce steam and carrier gas into the second gas distributor 117 to form a turbulent fluidization state with an apparent gas velocity of 0.12-0.3m / s. The carbon raw material reacts with the preheated steam at 500~600℃. The inert carrier gas introduced is one or a combination of nitrogen, argon, and helium. The flow rate-to-volume ratio of activation steam to inert carrier gas is 10-100%.

[0093] (4) Continuous discharge: The activated product is continuously discharged at high temperature through the discharge port 1131 at the bottom of the deep activation section 113; the total residence time of the carbon raw material in the reactor is controlled by the intelligent control system 160 to be 4-10 hours. The yield of the prepared porous carbon product is ≥25%, and the specific surface area is ≥1200m². 2 / g, pore volume ≥0.8cm 3 / g, with 2-50nm mesoporous content ≥60%.

[0094] The present invention will be further described below with reference to specific embodiments.

[0095] Example 1

[0096] Pine-based biochar is used as raw material, with a particle size of 5-15 μm. Continuous activation is performed using the steam-activated porous char continuous fluidization equipment 100 provided by this invention.

[0097] Equipment parameters: The top settling section 111 has a diameter of 1.2m and a height of 1.5m; the pre-activation section 112 has a diameter of 0.8m and a height of 3.6m, with a height-to-diameter ratio of 4.5; the deep activation section 113 has a diameter of 0.6m and a height of 1.5m, with a height-to-diameter ratio of 2.5. The spiral agitator in the pre-activation section 112 extends 0.2m below the material level and rotates at 100 r / min. The first gas distributor 116 is an annular porous tube structure, circumferentially arranged along the inner wall of the corresponding narrowing section 114, with the opening direction angled upwards at 45°, an aperture of 2mm, and an opening rate of 2%; the second gas distributor 117 is a disc-shaped porous plate, horizontally positioned at the bottom of the deep activation section 113, with an aperture of 3mm and an opening rate of 3%.

[0098] Process parameters: Feeding rate 85 kg / h; temperature of pre-activation section 112 880℃±4℃, apparent gas velocity 0.08 m / s; temperature of deep activation section 113 920℃±2℃, apparent gas velocity 0.18 m / s; steam preheating temperature 550℃; residence time 6.5 hours.

[0099] The product yield was 31.5%, and the specific surface area was 1920 m². 2 / g, total pore volume 1.15cm³ 3 / g, with 68% being mesoporous (2-50nm).

[0100] Example 2

[0101] Petroleum coke was used as raw material, with a particle size of 2-8 μm. The equipment parameters remained the same as in Example 1.

[0102] Adjust the process parameters as follows: feed rate 70 kg / h; temperature of pre-activation section 112 920℃±3℃, apparent gas velocity 0.06 m / s; temperature of deep activation section 113 960℃±2℃, apparent gas velocity 0.22 m / s; steam preheating temperature 580℃; residence time 8 hours.

[0103] The product yield was 28.8%, and the specific surface area was 2150 m². 2 / g, total pore volume 1.28cm³ 3 / g, with a mesoporous content of 72%. Electrochemical tests show that the specific capacitance reaches 285F / g at a current density of 1A / g.

[0104] Example 3

[0105] Coconut shell charcoal was used as the raw material, with a particle size of 8-12 μm. The equipment parameters were kept consistent with those in Example 1.

[0106] Process parameters: Feeding rate 90 kg / h; temperature of pre-activation section 112 860℃±4℃, apparent gas velocity 0.10 m / s; temperature of deep activation section 113 900℃±3℃, apparent gas velocity 0.20 m / s; steam preheating temperature 530℃; residence time 5.5 hours.

[0107] The product yield was 33.2%, and the specific surface area was 1850 m². 2 / g, total pore volume 1.05cm³ 3 / g, with well-developed micropores and a microporosity of 75%, making it particularly suitable for VOCs adsorption.

[0108] Example 4

[0109] Coal tar pitch-based spherical activated carbon was used as raw material, with a particle size of 10-20 μm. The equipment parameters were consistent with those in Example 1.

[0110] Process parameters: Feeding rate 75 kg / h; temperature of pre-activation section 112 940℃±5℃, apparent gas velocity 0.07 m / s; temperature of deep activation section 113 980℃±2℃, apparent gas velocity 0.25 m / s; steam preheating temperature 590℃; residence time 7 hours.

[0111] The product yield was 27.5%, and the specific surface area was 2050 m². 2 / g, total pore volume 1.35cm³ 3 / g, with a concentrated pore size distribution (2-4nm), high strength, and a wear rate of only 3.5%.

[0112] Example 5

[0113] Phenolic resin charcoal was used as the raw material, with a particle size of 1-5 μm. The equipment parameters were kept consistent with those in Example 1.

[0114] Process parameters: Feeding rate 60 kg / h; temperature of pre-activation section 112 900℃±3℃, apparent gas velocity 0.05 m / s; temperature of deep activation section 113 950℃±2℃, apparent gas velocity 0.15 m / s; steam preheating temperature 560℃; residence time 9 hours.

[0115] The product yield was 25.8%, and the specific surface area was 2250 m². 2 / g, total pore volume 1.18cm³ 3 / g, with a microporosity of 85% and excellent electrical conductivity, it is suitable for supercapacitor electrode materials.

[0116] Example 6

[0117] Walnut shell charcoal was used as the raw material, with a particle size of 15-25 μm. The equipment parameters were consistent with those in Example 1.

[0118] Process parameters: Feeding rate 100 kg / h; temperature of pre-activation section 112 820℃±4℃, apparent gas velocity 0.12 m / s; temperature of deep activation section 113 880℃±3℃, apparent gas velocity 0.28 m / s; steam preheating temperature 510℃; residence time 4.5 hours.

[0119] The product yield was 35.5%, and the specific surface area was 1650 m². 2 / g, total pore volume 0.95cm³ 3 / g, with well-developed mesopores and a mesopore rate of 70%, suitable for macromolecular adsorption and catalyst support.

[0120] Example 7

[0121] Using the equipment and raw materials from Example 1, a 72-hour continuous operation stability test was conducted. The intelligent control system 160 automatically adjusted process parameters based on online detection signals: it activated the backup heating unit when temperature fluctuations exceeded ±6℃; it fine-tuned the steam flow rate based on the product's specific surface area (fluctuations controlled within ±8%); and it automatically adjusted the discharge valve opening based on changes in material inventory. During operation, product indicators remained stable: yield 31.2% ± 1.8%, specific surface area 1900-1950 m². 2 / g, with mesoporous components accounting for 67%-70%.

[0122] Example 8

[0123] Using the raw materials and process parameters of Example 1, only the equipment parameters were adjusted.

[0124] Equipment parameters: The top settling section 111 has a diameter of 1.2m and a height of 1.5m; the pre-activation section 112 has a diameter of 0.8m and a height of 2.4m, with a height-to-diameter ratio of 3; the deep activation section 113 has a diameter of 0.6m and a height of 1.8m, with a height-to-diameter ratio of 3. The spiral agitator in the pre-activation section 112 extends 0.15 meters below the material level and rotates at 50 r / min. The first gas distributor 116 is an annular porous tube structure, circumferentially arranged along the inner wall of the corresponding narrowing section 114, with the opening direction angled upwards at 45°, an aperture of 1mm, and an opening rate of 3%; the second gas distributor 117 is a disc-shaped porous plate, horizontally positioned at the bottom of the deep activation section 113, with an aperture of 2mm and an opening rate of 4%.

[0125] The product yield was 32.8%, and the specific surface area was 1780 m². 2 / g, total pore volume 0.95cm³ 3 / g, with well-developed mesopores and a mesopore rate of 70%, suitable for macromolecular adsorption and catalyst support.

[0126] Example 9

[0127] Equipment parameters: The top settling section 111 has a diameter of 1.2m and a height of 1.5m; the pre-activation section 112 has a diameter of 0.8m and a height of 4m, with a height-to-diameter ratio of 5; the deep activation section 113 has a diameter of 0.6m and a height of 0.9m, with a height-to-diameter ratio of 1.5. The spiral agitator in the pre-activation section 112 extends 0.4m below the material level and rotates at 200 r / min. The first gas distributor 116 is an annular porous tube structure, circumferentially arranged along the inner wall of the corresponding narrowing section 114, with the opening direction angled upwards at 45°, an aperture of 3mm, and an opening rate of 1.5%; the second gas distributor 117 is a disc-shaped porous plate, horizontally positioned at the bottom of the deep activation section 113, with an aperture of 4mm and an opening rate of 4%.

[0128] The product yield was 33.5%, and the specific surface area was 2050 m². 2 / g, total pore volume 1.1cm 3 / g, with well-developed mesopores and a mesopore rate of 62%, making it suitable for macromolecular adsorption and catalyst support.

[0129] Comparative Example 1

[0130] Using the same raw materials as in Example 1, activation was performed at 850°C for 12 hours in a conventional fixed-bed reactor, with steam directly introduced without preheating. The product yield was 22.5%, and the specific surface area was 1650 m². 2 / g, total pore volume 0.82cm³ 3 / g, mesoporous content 41%. Specific capacitance is 195F / g, and product performance varies significantly between batches (specific surface area fluctuates by ±18%).

[0131] Comparative Example 2

[0132] Using the same raw materials as in Example 2, steam activation was performed in a conventional rotary kiln. The temperature was controlled at 900°C, the activation time was 14 hours, and the steam flow rate was similar. The resulting product had a specific surface area of ​​only 1350 m². 2 / g, yield 22%, uneven pore size distribution, mesoporous proportion 45%.

[0133] Comparative Example 3

[0134] Using the same raw materials as in Example 3, steam activation was carried out in an intermittent fluidized bed. The temperature was controlled at 880°C, the activation time was 10 hours, and the steam flow rate was similar. Due to the inability to achieve continuous and stable operation, the product performance fluctuated greatly: yield 25-32%, specific surface area 1500-1800 m². 2 / g, mesoporous content 50-65%, product quality is unstable.

[0135] Comparative Example 4

[0136] Using the same raw materials, process parameters, and core equipment structure as in Example 1, only the height-to-diameter ratio of the two activation sections was adjusted: the height-to-diameter ratio of the pre-activation section was 2.0; and the height-to-diameter ratio of the deep activation section was 3.5.

[0137] Reaction phenomena: insufficient fluidization space in the pre-activation section and local back-mixing; decreased fluidization intensity in the deep activation section and wider gas-solid contact time distribution.

[0138] Product performance: Yield 29.1%, specific surface area 1750m² / g, total pore volume 1.01cm³ / g, mesoporous content 58% (not reaching ≥60%), performance fluctuation ±8%.

[0139] Comparative Example 5

[0140] Using the same raw materials, process parameters, and main equipment structure as in Example 1, only the gas distributor parameters were adjusted: the first gas distributor had an aperture of 4 mm and an opening ratio of 4%; the second gas distributor had an aperture of 1 mm and an opening ratio of 1.5%.

[0141] Reaction phenomena: concentrated airflow injection and increased material entrainment in the pre-activation section; uneven gas distribution and local dead zones in the deep activation section.

[0142] Product performance: Yield 29.5%, specific surface area 1700m² / g, total pore volume 0.98cm³ / g, mesoporous content 56% (not reaching ≥60%).

[0143] Comparative Example 6

[0144] Using the same raw materials and equipment structure as in Example 1, only the process parameters were adjusted: the pre-activation section temperature was 780℃ and the apparent gas velocity was 0.03m / s; the deep activation section temperature was 1020℃ and the apparent gas velocity was 0.32m / s; the steam preheating temperature was 480℃, and the residence time remained unchanged.

[0145] Reaction phenomena: The temperature in the pre-activation section is too low and the gas velocity is insufficient, resulting in incomplete material activation; the temperature in the deep activation section is too high and the gas velocity exceeds the standard, leading to excessive local ablation and a significant increase in material entrainment.

[0146] Product performance: Yield 28.8%, specific surface area 1680m² / g, total pore volume 0.96cm³ / g, mesoporous content 55%, specific capacitance 220F / g.

[0147] In summary, the continuous fluidization equipment 100 for steam-activated porous carbon provided by the present invention, by segmenting the fluidized bed reactor 110 and controlling the diameter of the top settling section 111 to be greater than the diameter of the pre-activation section 112 to be greater than the diameter of the deep activation section 113, and connecting adjacent sections with a narrowing section 114, can adapt to the activation process requirements of porous carbon preparation. It can not only enhance the gas-solid mixing effect and ensure the stable and efficient progress of the reaction, but also accurately control the product quality and optimize the overall stability and safety of operation. Meanwhile, this invention utilizes a steam preheating mechanism 130 to preheat steam, which is then divided into two streams: one entering the pre-activation section 112 via a first gas distributor 116, and the other entering the deep activation section 113 via a second gas distributor 117. Through this two-stage segmented design of pre-activation and deep activation, combined with precise temperature control and gas distribution, precise control of the pore size distribution of porous carbon is achieved. The proportion of mesopores in the product can reach over 60%, meeting the specific pore structure requirements of different application scenarios. Furthermore, the intelligent control system 160 automates the feeding, heating, activation, and discharging operations, resulting in a high degree of automation for the entire system. The intelligent control system 160 enables real-time monitoring and feedback adjustment of key parameters, reducing manual intervention. This invention achieves true continuous production, solving the problems of low production efficiency and poor product consistency in traditional batch operations. Equipment utilization is increased by over 50%, product performance stability is significantly improved, and specific surface area fluctuation is controlled within ±5%, enhancing the controllability and safety of the production process. This invention is particularly suitable for large-scale industrial production.

[0148] It should be noted that, where there is no conflict, the features in the embodiments of this application can be combined with each other.

[0149] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. A continuous fluidization apparatus for steam-activated porous carbon, characterized by, include: Fluidized bed reactor, feeding mechanism, steam preheating mechanism, unloading mechanism, heating mechanism and intelligent control system; The fluidized bed reactor includes a top settling section, a pre-activation section, and a deep activation section connected sequentially from top to bottom. A narrowing section is provided between adjacent sections. The cone angle of the narrowing section is ≤30°, and the diameter of the top settling section is > the diameter of the pre-activation section is > the diameter of the deep activation section. The top settling section is provided with a feeding port and a tail gas discharge port; the pre-activation section is provided with a stirring device; the narrowing section between the pre-activation section and the deep activation section is provided with a first gas distributor; the bottom of the deep activation section is provided with a discharge port and a second gas distributor. The feeding mechanism is connected to the feeding port, the steam preheating mechanism is connected to both the first gas distributor and the second gas distributor, the unloading mechanism is connected to the discharge port, and the heating mechanism is sleeved on the outside of the pre-activation section and the deep activation section. The intelligent control system is electrically connected to the feeding mechanism, the steam preheating mechanism, the unloading mechanism, and the heating mechanism, respectively. The height-to-diameter ratio (H / D) of the pre-activated section is 3~5, and the height-to-diameter ratio (H / D) of the deep-activated section is 1.5~3. The first gas distributor is an annular porous tube structure, arranged circumferentially along the inner wall of the corresponding narrowed section, with the opening direction inclined upward at 45°, the pore diameter 1~3mm, and the opening ratio 1.5~3%; The second gas distributor is a disc-shaped perforated plate, horizontally positioned at the bottom of the deep activation section, with a pore diameter of 2-4 mm and an opening ratio of 2-4%. The intelligent control system includes monitoring sensors and an adjustment module. The monitoring sensors include: a temperature sensor for monitoring the activation temperature of the pre-activation section and the deep activation section; a level sensor for monitoring the material inventory in the fluidized bed reactor; a mass flow sensor for monitoring the mass flow rate of the discharged material at the outlet; and a material characteristic sensor for real-time monitoring of the material characteristics in the fluidized bed reactor. The adjustment module includes: a heating adjustment module for adjusting the heating power of the heating mechanism according to the temperature sensor; an infeed / outfeed adjustment module for adjusting the rotation speed of the feeding mechanism and the opening degree of the unloading mechanism according to the material level sensor and the mass flow sensor; a steam adjustment module for adjusting the steam flow rate of the steam preheating mechanism according to the material characteristic sensor; and an interlock adjustment module for automatically executing shutdown, cutting off the gas supply, and initiating emergency cooling operations after the detection indicators of the temperature sensor, the material level sensor, the mass flow sensor, and the material characteristic sensor exceed the limits.

2. The continuous fluidized apparatus for water vapor-activated porous carbon of claim 1, wherein, The steam preheating mechanism includes a steam generating mechanism, a main gas generating pipe, a preheating furnace, a first pipeline, and a second pipeline. The outlet of the steam generating mechanism is connected to the main gas generating pipe, the main gas generating pipe is connected to the preheating furnace, the outlet of the preheating furnace is connected to the first pipeline and the second pipeline, the first pipeline is connected to the first gas distributor, and the second pipeline is connected to the second gas distributor.

3. The continuous fluidized apparatus for water vapor-activated porous carbon of claim 2, wherein, The continuous fluidization equipment for steam-activated porous carbon also includes a gas carrier mechanism, which is connected to the main gas production pipe.

4. The continuous fluidized apparatus for water vapor-activated porous carbon of claim 1, wherein, The pre-activation section is equipped with a spiral stirring blade, and the spiral stirring blade penetrates below the material level by a distance of 1 / 2 to 1 / 8 of the diameter of the pre-activation section.

5. The continuous fluidized apparatus for water vapor-activated porous carbon of claim 4, wherein, The rotational speed of the spiral agitator is 50~200 r / min; And / or, the blades of the spiral agitator are rotatably mounted on the agitator shaft; the rotation angle of the blades is 30°-60°.

6. A continuous fluidization method of the steam-activated porous carbon using the continuous fluidization apparatus of the steam-activated porous carbon according to any one of claims 1 to 5, characterized by, Includes the following steps: (1) Continuous feeding: Carbon raw material is continuously fed into the fluidized bed reactor through the feed port of the top settling section, and the air is isolated by the sealed structure. The intelligent control system controls the feeding rate. (2) Pre-activation: In the pre-activation section, the heating mechanism is controlled to heat the pre-activation section to 800~1000℃, and the steam preheating mechanism is controlled to introduce steam and carrier gas into the first gas distributor to form a bubbling fluidized state with an apparent gas velocity of 0.04-0.12m / s. The carbon raw material is in contact with preheated steam at 500~600℃ to react. (3) Deep activation: The carbon raw material enters the deep activation section, and the heating mechanism is controlled to heat the deep activation section to 800~1000℃. The steam preheating mechanism is controlled to introduce steam and carrier gas into the second gas distributor to form a turbulent fluidization state with an apparent gas velocity of 0.12-0.3m / s. The carbon raw material reacts with preheated steam at 500~600℃. (4) Continuous discharge: The activated product is continuously discharged at high temperature through the discharge port at the bottom of the deep activation section; The total residence time of the carbon raw material in the reactor is controlled to be 4-10 hours by the intelligent control system.

7. The continuous fluidization method for steam-activated porous carbon according to claim 6, characterized in that, The particle size of the carbon raw material is ≤200μm; And / or, the carrier gas introduced is one or a combination of nitrogen, argon, and helium; And / or, the flow rate-to-volume ratio of the water vapor to the carrier gas is 10-100%; And / or, the yield of the prepared porous carbon product is ≥25%, and the specific surface area is ≥1200 m². 2 / g, pore volume ≥0.8cm 3 / g, with 2-50nm mesoporous content ≥60%.

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