A large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs

Abstract

This invention relates to a large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flakes, comprising: a flake forming assembly, including a spinning module, an electric field control device, a material transport module, and a solution preparation module; the spinning module includes a micro-region air supply device composed of a gas mixing unit and a gas transport unit, a positive nozzle spinneret, and a negative nozzle spinneret; an environmental parameter control assembly; a material pretreatment assembly, including a pressure equalization and shaping module, a pressure equalization and shaping module controller, a drying device, and an organic component removal device; and a composite calcination assembly, including a microwave pulse device, a quantitative oxygen delivery device, a high-temperature resistant gradient differential conveyor belt, a stripping roller, and a high-temperature calcination device. Compared with existing technologies, this invention achieves efficient, continuous, and large-scale production, improves the macroscopic structural stability of the fiber flakes, realizes high-precision control of the spinning solution synthesis reaction, and optimizes the microstructure and performance.

Description

Technical Field

[0001] This invention relates to the field of inorganic nanofiber preparation technology, and in particular to a large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flakes. Background Technology

[0002] Porous ceramic nanofibers possess high temperature resistance and chemical stability, along with high specific surface area, high porosity, and abundant open sites due to their porous structure. The three-dimensional fluffy flocs constructed from them further expand their application range, showing promising prospects in fireproofing, heat insulation, air filtration, adsorption separation, and sound absorption and noise reduction. However, existing porous ceramic nanofiber preparations based on electrospinning still have significant shortcomings in structural control. On the one hand, the overall structural stability of flocs composed of porous ceramic nanofibers is poor, easily collapsing and delaminating under pressure or deformation. On the other hand, the current production rate of porous nanofiber-based elastic ceramic flocs is low due to the inherent limitations of ordinary electrospinning. These problems severely restrict the continuous, high-speed, and large-scale preparation of porous ceramic nanofiber flocs.

[0003] Currently, some researchers in this field have conducted studies. Patent CN201010237944.2 discloses a porous silicon carbide fiber and its preparation method. It utilizes the precipitation-grading principle to modulate an electrospinnable polysilane suspension, achieving electrospinning of an extremely dilute polysilane solution and introducing a large number of mesoporous structures. However, the pore distribution obtained by this method is uneven, and the fiber pore structure is difficult to precisely control, resulting in poor fiber mechanical properties. Patent CN202010035821.4 discloses an airflow-assisted electrospinning nozzle and its usage method. This increases the yield of electrospinned nanofibers through airflow assistance and can effectively reduce fiber fineness. However, the device suffers from insufficient air-electric field coupling stability, making it difficult to control the jet morphology and obtain structurally stable nanofiber aggregates. Patent ZL202411182158.5 discloses a continuous production system for ultrafine fiber porous materials based on electrostatic air-jet spinning and a method for preparing ultrafine fiber porous materials. It employs a vertical spinning method, which enhances the ability to control the fiber structure to some extent. However, the resulting flakes are still mainly layered, with a structure prone to delamination, and the thickness is adjusted only by a single pressure roller. Stress concentration easily occurs during the pressure process, leading to edge warping, surface deformation, and more severe delamination. Furthermore, the material is prone to springback after leaving the pressure roller, resulting in poor thickness stability, difficulty in effective control, and poor overall material quality.

[0004] Therefore, there is an urgent need to construct a large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs. By synergistically controlling fiber forming and pore structure evolution during continuous preparation, the system can achieve controllable construction of fiber pore structures and stable formation of floc macrostructures. Based on this, the preparation efficiency of porous ceramic nanofibers can be improved, thereby realizing the efficient and continuous large-scale preparation of porous nanofiber-based elastic ceramic flocs. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of the existing technology by providing a large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs. This system achieves efficient, continuous, and large-scale production, significantly improves the macroscopic structural stability of the fiber flocs, enables high-precision control of the spinning solution synthesis reaction, efficiently and uniformly constructs the porous structure inside the fiber, innovates the calcination process, synergistically optimizes the microstructure and performance, and achieves refined and automated control of the entire process.

[0006] The objective of this invention can be achieved through the following technical solutions: This invention provides a large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs, comprising: The flake forming assembly includes a spinning module, an electric field control device, a material transport module, and a solution preparation module. The spinning module, located above the material transport module, includes a micro-area air supply device composed of a gas mixing unit and a gas transport unit, a positive-nozzle spinneret, and a negative-nozzle spinneret. The solution preparation module includes a reaction tank, an in-situ infrared analyzer, a viscosity detector, and a vacuum assembly for solution concentration, along with a stirring unit located inside the reaction tank. A multi-directional mixed gas transport device is provided around the reaction tank. A light shield and a dot matrix light source are placed outside the reaction tank. The outlet at the bottom of the reaction tank is connected to the liquid inlet of each spinneret. The electric field control device is connected to each spinneret. An environmental parameter control component includes distributed air outlets and an environmental temperature and humidity controller; the distributed air outlets are located at the four corners of the floc forming component. The material pretreatment assembly includes a pressure equalization and shaping module, a pressure equalization and shaping module controller, a drying device, and an organic component removal device; the organic component removal device includes an ultraviolet irradiation device, an ultraviolet-resistant porous conveyor belt, and a negative pressure suction device; the drying device is located below the pressure equalization and shaping module; the nanofiber flocs undergo surface homogenization and thickness shaping treatment under a heating environment; the ultraviolet irradiation device is located above the ultraviolet-resistant porous conveyor belt, and the negative pressure suction device is located below the ultraviolet-resistant porous conveyor belt; A composite calcination assembly includes a microwave pulse device, a quantitative oxygen delivery device, a high-temperature resistant gradient differential conveyor belt, a stripping roller, and a high-temperature calcination device. The quantitative oxygen delivery device has an oxygen-enriched mixed gas outlet and an oxygen-deficient mixed gas outlet at its bottom, separated by a partition. The microwave pulse device is located in the oxygen-enriched calcination zone, and the high-temperature calcination device is located in the oxygen-deficient calcination zone. The microwave pulse device is positioned above the high-temperature resistant gradient differential conveyor belt, and a stripping roller is positioned between adjacent conveying surfaces of the belt. The high-temperature calcination device is located below the belt. The fiber flocs are rapidly heated in the microwave pulse device, causing the amorphous phase structure to quickly transform into a large number of uniformly sized nucleation sites, while simultaneously rapidly bridging the voids remaining in the fibers after side group removal. Subsequently, high-temperature calcination is performed in an oxygen-deficient atmosphere to weaken the oxygen ion diffusion and exchange rate, inhibit grain growth, and obtain ceramic nanofibers with fine grains and uniform pore structure.

[0007] Furthermore, the gas mixing unit includes a gas inlet, a mixing chamber, and a mixing chamber gas outlet. The gas inlet is connected to the mixing chamber and the mixing chamber gas outlet below. The gas inlet includes a room temperature high humidity gas inlet, a room temperature dry gas inlet, and a high temperature dry gas inlet. The gas transmission unit includes: a top primary air supply plate, a primary air supply channel, and a buffer chamber; a bottom secondary air supply plate, a buffer chamber gas outlet, and a secondary air supply channel; and a bottom tertiary air supply plate, a tertiary air supply channel, and a grid plate.

[0008] Furthermore, the pressure equalization and shaping module includes a parallel distribution of pressure rollers and a sensing layer located on the surface of the pressure rollers. The position of the pressure rollers can be adjusted up and down to control the material feeding and output angles and the shaping height.

[0009] Furthermore, the stirring unit includes a drive motor, a transmission assembly connected to the drive motor, a mechanical stirring rod, and stirring blades connected to the outer wall of the mechanical stirring rod.

[0010] Furthermore, the multi-directional mixed gas conveying device is evenly distributed in the four directions of the reaction tank, and there are four such multi-directional mixed gas conveying devices, which are evenly distributed around the reaction tank. The light shield is located outside the reaction vessel, and the dot matrix light source is located outside the light shield. The outer layer of the light shield is equipped with a dot matrix light source, and each side of the light shield has 35 light sources arranged in an array. The material of the light shield is not limited to metal plate, carbon plate, or polymer plate.

[0011] Furthermore, the liquid preparation module also includes a stirring tank and an injection pump. The stirring tank is located above the reaction vessel. The injection pump is connected to the stirring tank at the top and to the feed port on the reaction vessel at the bottom via an adapter. The reaction vessel shell is equipped with a condenser pipe.

[0012] Furthermore, the gas transmission unit has 256 to 1024 bottom three-stage air supply channels, an airflow velocity of 0.1 to 10 m / s, an airflow temperature adjustable from 10 to 60°C, and an airflow humidity adjustable from 15 to 99%.

[0013] Furthermore, the feeding angle and output angle of the pressure equalization and shaping module are adjustable within the range of 10~50°, the shaping height is adjustable within the range of 1~20cm, and the conveyor belt running speed is adjustable within the range of 1~25m / min; the temperature of the drying device is adjustable from 25~300℃.

[0014] Furthermore, the emission wavelength of the ultraviolet irradiation device is adjustable from 150 to 400 nm, and the power is set from 40 to 350 W / dm. 2 The UV-resistant porous conveyor belt is a porous, hollow type, with a moving speed of 1~25m / min; the material of the UV-resistant porous conveyor belt is selected from one or more of the following: metal materials, polymer materials, rubber materials, or fiber-reinforced composite materials.

[0015] Furthermore, the quantitative oxygen delivery device can periodically switch between delivering oxidizing gas and inert gas, and independently control each oxygen-enriched mixed gas outlet and oxygen-deficient mixed gas outlet. The volume fraction of oxygen in oxygen-enriched calcination is controlled at ≥40%, and the volume fraction of oxygen in oxygen-deficient calcination is controlled at 3%~18%. The oxidizing gas is one of air and oxygen, and the auxiliary gas is one or more of nitrogen, xenon, radon, argon, helium, krypton, and neon. The microwave pulse device has a pulse power of 10~500kW, a pulse width of 0.1~5s, and a pulse interval of 0.1~0.5Hz; the heating temperature of the high-temperature calcination device is 250~1500℃. The high-temperature resistant gradient differential conveyor belt is distributed in a stepped manner, with different movement speeds at each stage, ranging from 1 to 25 m / min. The structure can be hollow, fully enclosed, or grid-type, and the material is selected from metals, ceramics, carbon, and their composite materials.

[0016] Electric field control equipment includes, but is not limited to, positive and negative voltage static power supplies, pulse high voltage power supplies, and AC power supplies, with a voltage range of -110~110kV during spinning.

[0017] The prepared porous ceramic nanofibers have diameters of 100–800 nm, pore sizes of 0.5–80 nm, and total pore volumes of 0.1–1 cm³. 3 / g, specific surface area of ​​50~1500m² 2 / g, single fiber tensile strength 0.1~2GPa.

[0018] Compared with the prior art, the present invention has the following advantages: (1) Efficient, continuous and large-scale production has been achieved: By integrating the four units of “floc forming - environmental control - material pretreatment - composite calcination” into a complete production line, the system has realized continuous and large-scale manufacturing from raw material preparation to the final ceramic floc product, which has improved production efficiency and met the needs of industrial application.

[0019] (2) Significantly improved the macroscopic structural stability of the fiber flocs: In terms of molding: The spinning module utilizes the synergistic effect of "electric field-airflow field" and a micro-area air supply device to rapidly solidify the jet into crimped nanofibers. These crimped fibers dynamically entangle with each other in the air, forming a three-dimensional interwoven fiber network, ultimately obtaining a fluffy floc substrate with strong internal cohesion, thus avoiding simple layered accumulation from the source.

[0020] In terms of shaping: The pressure equalization and shaping module applies controllable gradient pressure to the fluffy fiber flocs through an adjustable pressure roller group with a sensing layer, so as to achieve slow and uniform compaction and shaping, thereby obtaining a stable precursor flocs with a flat surface, uniform thickness and not easy to spring back, which solves the problems of stress concentration, edge lifting and delamination caused by traditional single pressure rollers.

[0021] (3) High-precision control of the spinning solution synthesis reaction was achieved: In the solution preparation module, a design combining a light shield and a dot matrix light source was adopted. By controlling the illumination conditions (opening the light shield to trigger the reaction, closing the light shield and turning on the dot matrix light source to terminate the reaction), the chain extension and end-capping reactions of the inorganic polymer precursor can be precisely controlled, thereby ensuring the uniformity of the molecular weight and structure of the spinning solution, laying the foundation for the subsequent preparation of fibers with consistent performance.

[0022] (4) The organic component removal equipment combines ultraviolet irradiation with negative pressure suction. Ultraviolet irradiation generates hydroxyl radicals to decompose the organic template, while negative pressure suction promotes the free radicals and decomposition products to penetrate the interior of the flocs, thereby achieving rapid, uniform and thorough removal of organic components inside the fiber, thus introducing a rich and uniformly distributed porous structure into the fiber.

[0023] (5) The calcination process was innovated and the microstructure and performance were optimized in a synergistic way: the composite calcination unit adopted a new two-step process of "microwave pulse oxygen-enriched rapid nucleation" and "oxygen-deficient high temperature inhibiting grain growth".

[0024] In the oxygen-rich region, the microwave pulse device provides high peak power, enabling the rapid and uniform generation of numerous crystal nuclei from the amorphous precursor and aiding in the pore closure. In the oxygen-deficient region, the high-temperature calcination device operates in a low-oxygen atmosphere, significantly inhibiting oxygen ion diffusion and grain growth. This synergistic process ultimately yields ceramic nanofibers with fine grains, abundant grain boundaries, and a uniform pore structure. This structure endows them with high specific surface area (similar to the adsorption properties of activated carbon), excellent mechanical properties (single fiber tensile strength 0.1~2 GPa), and high-temperature resistance, making them a type of thermally regenerable and recyclable "white activated carbon."

[0025] (6) The system achieves refined and automated control of the entire process: It integrates a variety of control and monitoring devices, such as an environmental temperature and humidity controller, an in-situ infrared analyzer, a viscosity detector, a pressure equalization and shaping module controller, and a quantitative oxygen delivery device that can independently control gas components and flow rates. These devices together achieve refined and automated control of key process parameters such as spinning environment, solution state, forming pressure, and calcination atmosphere, ensuring the stability and repeatability of product quality. Attached Figure Description

[0026] Figure 1 A schematic diagram of a large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs; Figure 2 This is a schematic diagram of the solution preparation module; Figure 3 This is a schematic diagram of a light shield; Figure 4 This is a schematic diagram of a dot matrix light source; Figure 5 This is a magnified view of a portion of the spinning module; Figure 6 A schematic diagram of a micro-area air supply device; Figure 7 This is a schematic diagram of the voltage equalization and shaping module.

[0027] Figure reference numerals: 1-Spinning module; 2-Electric field control equipment; 3-Material transfer module; 4-Liquid preparation module; 5-Distributed gas outlet; 6-Temperature and humidity controller; 7-Equalizing and shaping module; 8-Equalizing and shaping module controller; 9-Drying device; 10-Organic component removal equipment; 11-Ultraviolet irradiation device; 12-UV resistant porous conveyor belt; 13-Negative pressure suction device; 14-Microwave pulse device; 15-Oxygen-enriched mixed gas outlet; 16-Separator; 17-Quantitative oxygen delivery device; 18-Oxygen-deficient mixed gas outlet; 19-High temperature gradient differential conveyor belt; 20-Peeling roller; 21-High temperature calcination device; 101-Gas mixing unit; 1011-Ambient temperature high humidity gas conveying port; 1012-Ambient temperature dry gas conveying port; 1013-High temperature dry gas conveying port; 1014-Blending chamber; 1015-Blending chamber gas outlet; 102-Gas transfer unit; 1021 1022- Primary air supply plate; 1023- Buffer chamber; 1024- Secondary air supply plate; 1025- Gas outlet of buffer chamber; 1026- Secondary air supply channel; 1027- Tertiary air supply plate; 1028- Tertiary air supply channel; 1029- Grille plate; 103- Forward nozzle spinneret; 104- Offset nozzle spinneret; 401- Reaction tank; 402- Feed port; 403- Agitation unit; 4031- Agitation blades ; 4032-Drive motor; 4033-Transmission assembly; 4034-Mechanical stirring rod; 404-In-situ infrared analyzer; 405-Viscosity detector; 406-Condensation pipeline; 407-Discharge port; 408-Vacuum assembly; 409-Multi-directional mixed gas conveying device; 410-Injection pump; 411-Adapter; 412-Mixing tank; 413-Light shield; 414-Dot matrix light source; 701-Pressure roller assembly; 702-Sensing layer. Detailed Implementation

[0028] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments. Any component models, manufacturing methods, materials, structures, or composition ratios not explicitly described in this technical solution are considered common technical features disclosed in the prior art.

[0029] Example 1 This embodiment provides a large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs, such as... Figure 1-7 As shown, it includes: The flake forming assembly includes a spinning module 1, an electric field control device 2, a material transfer module 3, and a liquid preparation module 4. The spinning module 1 is located above the material transfer module 3 and includes a micro-area air supply device composed of a gas mixing unit 101 and a gas transfer unit 102, a positive nozzle spinneret 103, and a negative nozzle spinneret 104. The liquid preparation module 4 includes a reaction tank 401, an in-situ infrared analyzer 404, a viscosity detector 405, and a vacuum assembly 408 for solution concentration, as well as a stirring unit 403 located inside the reaction tank 401. A multi-directional mixed gas delivery device 409 is provided around the reaction tank 401. A light shield 413 and a dot matrix light source 414 are placed outside the reaction tank 401. The discharge port 407 at the bottom of the reaction tank 401 is connected to the liquid inlet of each spinneret. The electric field control device 2 is connected to each spinneret. An environmental parameter control component includes a distributed air outlet 5 and an environmental temperature and humidity controller 6; the distributed air outlet 5 is located at the four corners of the floc forming component. The material pretreatment assembly includes a pressure equalization and shaping module 7, a pressure equalization and shaping module controller 8, a drying device 9, and an organic component removal device 10; the organic component removal device 10 includes an ultraviolet irradiation device 11, an ultraviolet-resistant porous conveyor belt 12, and a negative pressure suction device 13; the drying device 9 is located below the pressure equalization and shaping module 7; the nanofiber flocs undergo surface homogenization and thickness shaping treatment under a heating environment; the ultraviolet irradiation device 11 is located above the ultraviolet-resistant porous conveyor belt 12, and the negative pressure suction device 13 is located below the ultraviolet-resistant porous conveyor belt 12; The composite calcination assembly includes a microwave pulse device 14, a quantitative oxygen delivery device 17, a high-temperature resistant gradient differential conveyor belt 19, a stripping roller 20, and a high-temperature calcination device 21. The quantitative oxygen delivery device 17 has an oxygen-enriched mixed gas outlet 15 and an oxygen-deficient mixed gas outlet 18 at its bottom, which are separated by a partition 16. The microwave pulse device 14 is distributed in the oxygen-enriched calcination zone, and the high-temperature calcination device 21 is distributed in the oxygen-deficient calcination zone. The microwave pulse device 14 is located above the high-temperature resistant gradient differential conveyor belt 19, and the stripping roller 20 is located between adjacent conveying surfaces of the high-temperature resistant gradient differential conveyor belt 19. The high-temperature calcination device 21 is located below the high-temperature resistant gradient differential conveyor belt 19. The fiber flocs are rapidly heated in the microwave pulse device 14, which rapidly transforms the amorphous phase structure into a large number of uniformly sized nucleation sites, and at the same time rapidly fills the voids in the fiber after the side groups are removed. Then, high-temperature calcination is carried out in an oxygen-deficient atmosphere to reduce the diffusion and exchange rate of oxygen ions and inhibit grain growth, resulting in ceramic nanofibers with fine grains and uniform pore structure.

[0030] Example 2 This embodiment provides a large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs, such as... Figure 1-7 As shown, it includes: The flake forming assembly includes a spinning module 1, an electric field control device 2, a material transfer module 3, and a liquid preparation module 4. The spinning module 1 is located above the material transfer module 3 and includes a micro-area air supply device composed of a gas mixing unit 101 and a gas transfer unit 102, a positive nozzle spinneret 103, and a negative nozzle spinneret 104. The liquid preparation module 4 includes a reaction tank 401, an in-situ infrared analyzer 404, a viscosity detector 405, and a vacuum assembly 408 for solution concentration, as well as a stirring unit 403 located inside the reaction tank 401. A multi-directional mixed gas delivery device 409 is provided around the reaction tank 401. A light shield 413 and a dot matrix light source 414 are placed outside the reaction tank 401. The discharge port 407 at the bottom of the reaction tank 401 is connected to the liquid inlet of each spinneret. The electric field control device 2 is connected to each spinneret. An environmental parameter control component includes a distributed air outlet 5 and an environmental temperature and humidity controller 6; the distributed air outlet 5 is located at the four corners of the floc forming component. The material pretreatment assembly includes a pressure equalization and shaping module 7, a pressure equalization and shaping module controller 8, a drying device 9, and an organic component removal device 10; the organic component removal device 10 includes an ultraviolet irradiation device 11, an ultraviolet-resistant porous conveyor belt 12, and a negative pressure suction device 13; the drying device 9 is located below the pressure equalization and shaping module 7; the nanofiber flocs undergo surface homogenization and thickness shaping treatment under a heating environment; the ultraviolet irradiation device 11 is located above the ultraviolet-resistant porous conveyor belt 12, and the negative pressure suction device 13 is located below the ultraviolet-resistant porous conveyor belt 12; The composite calcination assembly includes a microwave pulse device 14, a quantitative oxygen delivery device 17, a high-temperature resistant gradient differential conveyor belt 19, a stripping roller 20, and a high-temperature calcination device 21. The quantitative oxygen delivery device 17 has an oxygen-enriched mixed gas outlet 15 and an oxygen-deficient mixed gas outlet 18 at its bottom, which are separated by a partition 16. The microwave pulse device 14 is distributed in the oxygen-enriched calcination zone, and the high-temperature calcination device 21 is distributed in the oxygen-deficient calcination zone. The microwave pulse device 14 is located above the high-temperature resistant gradient differential conveyor belt 19, and the stripping roller 20 is located between adjacent conveying surfaces of the high-temperature resistant gradient differential conveyor belt 19. The high-temperature calcination device 21 is located below the high-temperature resistant gradient differential conveyor belt 19. The fiber flocs are rapidly heated in the microwave pulse device 14, which rapidly transforms the amorphous phase structure into a large number of uniformly sized nucleation sites, and at the same time rapidly fills the voids in the fiber after the side groups are removed. Then, high-temperature calcination is carried out in an oxygen-deficient atmosphere to reduce the diffusion and exchange rate of oxygen ions and inhibit grain growth, resulting in ceramic nanofibers with fine grains and uniform pore structure.

[0031] In a specific embodiment, the gas mixing unit 101 includes a gas inlet, a mixing chamber 1014 and a mixing chamber gas outlet 1015. The gas inlet is connected to the mixing chamber 1014 and the mixing chamber gas outlet 1015 below. The gas inlet includes a normal temperature high humidity gas inlet 1011, a normal temperature dry gas inlet 1012 and a high temperature dry gas inlet 1013. The gas transmission unit 102 includes: a top primary air supply plate 1021, a primary air supply channel 1022, and a buffer chamber 1023; a secondary air supply plate 1024, a buffer chamber gas outlet 1025, and a secondary air supply channel 1026 located below 1023; and a bottom tertiary air supply plate 1027, a tertiary air supply channel 1028, and a grid plate 1029.

[0032] In a specific embodiment, the pressure equalization and shaping module 7 includes a parallel distribution of pressure rollers 701 and a sensing layer 702 located on the surface of the pressure rollers. The position of the pressure rollers 701 can be adjusted up and down to control the material feeding and output angle and the shaping height.

[0033] In a specific embodiment, the stirring unit 403 includes a drive motor 4032, a transmission assembly 4033 connected to the drive motor 4032, a mechanical stirring rod 4034, and stirring blades 4031 connected to the outer wall of the mechanical stirring rod 4034.

[0034] In a specific embodiment, the multi-directional mixed gas conveying device 409 is evenly distributed in the four directions of the reaction tank 401. There are four multi-directional mixed gas conveying devices 409 in total, which are evenly distributed around the reaction tank 401. The light shield 413 is located outside the reaction vessel 401, and the dot matrix light source 414 is located outside the light shield 413. The dot matrix light source 414 is provided on the outer layer of the light shield 413, and each side of the light shield 413 is arranged in an array of 35 light sources. The material of the light shield is not limited to metal plate, carbon plate, or polymer plate.

[0035] In a specific embodiment, the liquid preparation module 4 further includes a stirring tank 412 and an injection pump 410. The stirring tank 412 is located above the reaction tank 401. The injection pump 410 is connected to the stirring tank 412 at the top and to the feed port 402 on the reaction tank 401 at the bottom via an adapter 411. A condenser pipe 406 is provided inside the outer shell of the reaction tank 401.

[0036] In a specific embodiment, the number of bottom three-stage air supply channels of the gas transmission unit 102 is 256 to 1024, the airflow velocity is 0.1 to 10 m / s, the airflow temperature is adjustable from 10 to 60°C, and the airflow humidity is adjustable from 15 to 99%.

[0037] In a specific embodiment, the feeding angle and output angle of the pressure equalization and shaping module 7 are adjustable in the range of 10~50°, the shaping height is adjustable in the range of 1~20cm, and the conveyor belt running speed is adjustable in the range of 1~25m / min; the temperature of the drying device 9 is adjustable in the range of 25~300℃.

[0038] In a specific embodiment, the emission wavelength of the ultraviolet irradiation device 11 is adjustable from 150 to 400 nm, and the power is set to 40 to 350 W / dm. 2 The UV-resistant porous conveyor belt 12 is porous and hollow, with a moving speed of 1~25m / min; the material of the UV-resistant porous conveyor belt 12 is selected from one or more of metal materials, polymer materials, rubber materials or fiber-reinforced composite materials.

[0039] In a specific embodiment, the quantitative oxygen delivery device 17 can periodically switch between delivering oxidizing gas and inert gas, and independently control each oxygen-enriched mixed gas outlet 15 and oxygen-deficient mixed gas outlet 18. The volume fraction of oxygen in oxygen-enriched calcination is controlled at ≥40%, and the volume fraction of oxygen in oxygen-deficient calcination is controlled at 3%~18%. The oxidizing gas is one of air and oxygen, and the auxiliary gas is one or more of nitrogen, xenon, radon, argon, helium, krypton, and neon. The microwave pulse device 14 has a pulse power of 10~500kW, a pulse width of 0.1~5s, and a pulse interval of 0.1~0.5Hz; the heating temperature of the high-temperature calcination device 21 is 250~1500℃. The high-temperature resistant gradient differential conveyor belt 19 is distributed in a stepped manner, with different movement speeds at each stage. The movement speed ranges from 1 to 25 m / min. The structure can be hollow, fully enclosed, or grid-type, and the material is selected from metal, ceramic, carbon, and their composite materials.

[0040] The electric field control device 2 includes, but is not limited to, positive and negative voltage static power supplies, pulse high voltage power supplies, and AC power supplies, with a voltage range of -110~110kV during spinning.

[0041] The prepared porous ceramic nanofibers have diameters of 100–800 nm, pore sizes of 0.5–80 nm, and total pore volumes of 0.1–1 cm³. 3 / g, specific surface area of ​​50~1500m² 2 / g, single fiber tensile strength 0.1~2GPa.

[0042] The above description of the embodiments is provided to enable those skilled in the art to understand and use the invention. It will be apparent to those skilled in the art that various modifications can be made to these embodiments, and the general principles described herein can be applied to other embodiments without inventive effort. Therefore, the present invention is not limited to the above embodiments, and any improvements and modifications made by those skilled in the art based on the disclosure of the present invention without departing from the scope of the invention should be within the protection scope of the present invention.

Claims

1. A large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs, characterized in that, include: The floc forming assembly includes a spinning module (1), an electric field control device (2), a material transfer module (3), and a liquid preparation module (4); the spinning module (1) is located above the material transfer module (3) and includes a micro-area air supply device composed of a gas mixing unit (101) and a gas transfer unit (102), a positive nozzle spinneret (103), and a negative nozzle spinneret (104); the liquid preparation module (4) includes a reaction tank (401), an in-situ infrared analyzer (404), and a viscosity analyzer. The detector (405) and the vacuum assembly (408) for solution concentration are located inside the reaction vessel (401), and the stirring unit (403) is located inside the reaction vessel (401). A multi-directional mixed gas conveying device (409) is provided around the reaction vessel (401). A light shield (413) and a dot matrix light source (414) are placed outside the reaction vessel (401). The discharge port (407) at the bottom of the reaction vessel (401) is connected to the liquid inlet of each spinneret. The electric field control device (2) is connected to each spinneret. The environmental parameter control component includes a distributed air outlet (5) and an environmental temperature and humidity controller (6). The material pretreatment component includes a pressure equalization and shaping module (7), a pressure equalization and shaping module controller (8), a drying device (9), and an organic component removal device (10); the organic component removal device (10) includes an ultraviolet irradiation device (11), an ultraviolet-resistant porous conveyor belt (12), and a negative pressure suction device (13); the drying device (9) is located below the pressure equalization and shaping module (7); The composite calcination assembly includes a microwave pulse device (14), a quantitative oxygen delivery device (17), a high-temperature gradient differential conveyor belt (19), a stripping roller (20), and a high-temperature calcination device (21). The quantitative oxygen delivery device (17) has an oxygen-enriched mixed gas outlet (15) and an oxygen-deficient mixed gas outlet (18) at its bottom, which are separated by a partition (16). The microwave pulse device (14) is located in the oxygen-enriched calcination zone, and the high-temperature calcination device (21) is located in the oxygen-deficient calcination zone. The microwave pulse device (14) is located above the high-temperature gradient differential conveyor belt (19), and a stripping roller (20) is located between adjacent conveying surfaces of the high-temperature gradient differential conveyor belt (19). The high-temperature calcination device (21) is located below the high-temperature gradient differential conveyor belt (19).

2. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The gas mixing unit (101) includes a gas inlet, a mixing chamber (1014) and a mixing chamber gas outlet (1015). The gas inlet is connected to the mixing chamber (1014) and the mixing chamber gas outlet (1015) below. The gas inlet includes a normal temperature high humidity gas inlet (1011), a normal temperature dry gas inlet (1012) and a high temperature dry gas inlet (1013). The gas transmission unit (102) includes: a primary air supply plate (1021), a primary air supply channel (1022), and a buffer chamber (1023) at the top; a secondary air supply plate (1024), a buffer chamber gas outlet (1025), and a secondary air supply channel (1026) located below (1023); and a tertiary air supply plate (1027), a tertiary air supply channel (1028), and a grid plate (1029) at the bottom.

3. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The pressure equalization and shaping module (7) includes a parallel distribution of pressure rollers (701) and a sensing layer (702) located on the surface of the pressure rollers. The position of the pressure rollers (701) can be adjusted up and down to control the material feeding and output angle and shaping height.

4. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The stirring unit (403) includes a drive motor (4032), a transmission assembly (4033) connected to the drive motor (4032), a mechanical stirring rod (4034), and stirring blades (4031) connected to the outer wall of the mechanical stirring rod (4034).

5. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The multi-directional mixed gas conveying device (409) is evenly distributed in the four directions of the reaction tank (401). There are four multi-directional mixed gas conveying devices (409) in total, which are evenly distributed around the reaction tank (401). The light shield (413) is located outside the reaction vessel (401), and the dot matrix light source (414) is located outside the light shield (413). The outer layer of the light shield (413) is provided with a dot matrix light source (414), and each side of the light shield (413) is arranged in an array of 35 light sources.

6. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The liquid preparation module (4) also includes a stirring tank (412) and an injection pump (410). The stirring tank (412) is located above the reaction tank (401). The injection pump (410) is connected to the stirring tank (412) above and to the feed port (402) on the reaction tank (401) below via an adapter (411). The reaction tank (401) has a condenser pipe (406) inside its outer shell.

7. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The gas transmission unit (102) has 256 to 1024 bottom three-stage air supply channels, an airflow velocity of 0.1 to 10 m / s, an airflow temperature adjustable from 10 to 60°C, and an airflow humidity adjustable from 15 to 99%.

8. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The feeding angle and output angle of the equalizing and shaping module (7) are adjustable in the range of 10~50°, the shaping height is adjustable in the range of 1~20cm, and the conveyor belt running speed is adjustable in the range of 1~25m / min; the temperature of the drying device (9) is adjustable in the range of 25~300℃.

9. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The ultraviolet irradiation device (11) has an adjustable emission wavelength of 150~400nm and a power setting of 40~350W / dm. 2 The UV-resistant porous conveyor belt (12) is porous and hollow, and its moving speed is 1~25m / min. The material of the UV-resistant porous conveyor belt (12) is selected from one or more of metal materials, polymer materials, rubber materials or fiber-reinforced composite materials.

10. The large-scale continuous manufacturing system for porous nanofiber-based elastic ceramic flocs according to claim 1, characterized in that, The quantitative oxygen delivery device (17) can periodically switch between delivering oxidizing gas and inert gas, and independently control each oxygen-enriched mixed gas outlet (15) and oxygen-deficient mixed gas outlet (18). The volume fraction of oxygen in oxygen-enriched calcination is controlled at ≥40%, and the volume fraction of oxygen in oxygen-deficient calcination is controlled at 3%~18%. The microwave pulse device (14) has a pulse power of 10~500kW, a pulse width of 0.1~5s, and a pulse interval of 0.1~0.5Hz; the heating temperature of the high-temperature calcination device (21) is 250~1500℃. The high-temperature resistant gradient differential conveyor belt (19) is distributed in a stepped manner, with different movement speeds at each stage. The movement speed ranges from 1 to 25 m / min. The structure can be hollow, fully enclosed, or grid-type, and the material is selected from metal, ceramic, carbon, and their composite materials.

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