Material drying device and method in inert gas atmosphere

Abstract

The invention discloses a material drying device and method in an inert gas atmosphere, and relates to the technical field of sensitive material drying. The objective of the invention is to solve the problems of unreliable sealing, low gas utilization rate, poor water removal effect, uneven heating, poor material dispersion, low intelligent degree and the like in the existing inert gas atmosphere drying device and technology, and the problem that the high-efficiency, high-quality, energy-saving and stable drying requirements of high-end sensitive materials cannot be met. Through multi-module collaborative design, the system comprises a closed drying cavity module, a high-reliability sealing and atmosphere regulation and control module, an inert gas closed-loop circulation deep water removal module, a heat pump auxiliary microwave infrared composite heating module, a material dispersion bearing module, a multi-parameter online monitoring module and an AI intelligent linkage control system, and all the modules work cooperatively. The device is reliable in sealing performance, the gas utilization rate is greatly increased, the operation cost is reduced, deep drying and uniform drying of sensitive materials are achieved, energy consumption is low, and the intelligent degree is high.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of sensitive material drying, in particular to a material drying device and method in an inert gas atmosphere. BACKGROUND

[0002] It is well known that in the fields of high-end industries such as lithium batteries, electronics, special materials, aerospace, etc., there are a large number of materials that are highly sensitive to oxygen and moisture in the air. Such materials are prone to oxidation, hydrolysis, agglomeration and other phenomena in a conventional drying environment, thereby damaging their structural integrity and core performance, and seriously affecting the quality stability and use safety of subsequent products. Therefore, the drying process of such sensitive materials must be carried out in an inert gas atmosphere, which isolates air from oxygen and moisture to protect the performance of the dried materials.

[0003] At present, existing inert gas protection drying technology and related devices have been applied in some fields, but in view of the actual industrial production needs, there are still many technical defects that are difficult to overcome, and it is difficult to balance the drying effect, running efficiency and use cost. The specific performance is as follows: Insufficient sealing performance is one of the core defects of existing devices. Most existing devices use single or double sealing structure, and the sealing reliability is poor, which is easy to cause gas leakage, leading to the infiltration of external air into the drying cavity, destroying the inert gas protection atmosphere, and finally causing oxidation and moisture absorption of sensitive materials, which cannot meet the preset drying quality requirements. At the same time, some devices lack effective gas leakage detection and automatic compensation mechanism, so it is difficult to find and handle the leakage problem in time, further reducing the stability and reliability of the drying process.

[0004] The utilization rate of inert gas is low, resulting in high use cost. The existing technology generally adopts inert gas direct discharge or simple circulation mode, and the gas circulation utilization effect is not good, a large amount of inert gas is directly wasted, increasing the raw material cost of industrial production. In addition, the existing device lacks effective gas purification and deep water removal mechanism, and a certain amount of water vapor and oxygen will be left in the recycled inert gas, which cannot be reused, and new high-purity inert gas needs to be continuously supplemented, further increasing the gas consumption and running cost.

[0005] The water removal method is single and inefficient, which cannot meet the deep drying needs of high-end sensitive materials. Most existing devices use single condensation or adsorption water removal method, which has limited water removal effect and cannot completely remove the water vapor in the inert gas, which cannot provide sufficient dry protection atmosphere for sensitive materials, thereby affecting the drying quality. At the same time, when using adsorption water removal method, the adsorbent needs to be frequently disassembled and replaced, which not only increases the operation and maintenance workload and cost, but also interrupts the drying process and affects the production continuity.

[0006] The heating mode is rough, the energy consumption is high, and the drying uniformity is poor. The existing device mostly adopts single resistance heating or infrared heating mode, the heating efficiency is low, only the surface of the material can be heated, the internal and external of the material cannot be heated synchronously, the surface of the material is easy to be overheated and deteriorated, and the internal of the material is not completely dried, thereby affecting the quality consistency of the dried material. In addition, the existing device lacks an effective waste heat recovery mechanism, a large amount of waste heat generated during the heating process is directly wasted, the overall energy consumption is high, and the current energy saving and consumption reduction industrial development trend is not met.

[0007] The material dispersion effect is poor, which further aggravates the uneven drying problem. For powder and particle sensitive materials, the existing device lacks an effective dispersion mechanism, the material is easy to agglomerate during the drying process, cannot be uniformly spread and fully contacted with inert gas and heat, the material is unevenly heated and contacted with gas, part of the material is over-dried, part of the material is not dried up to standard, and the quality stability of batch products is seriously affected.

[0008] The intelligent degree is low, which is not conducive to process optimization and quality control. The existing device mostly adopts manual control or simple program control mode, cannot realize real-time monitoring and dynamic control of key parameters in the drying process, is easy to cause over-drying or incomplete drying, wastes energy, and may damage the material performance. At the same time, the existing device cannot realize real-time storage and tracing of various parameters in the drying process, is not convenient for subsequent process optimization, quality investigation and production control, and is difficult to adapt to the production demand of high-end sensitive materials in large scale and refinement.

[0009] In summary, the existing inert gas atmosphere drying technology and device have obvious defects in sealing performance, gas utilization, water removal effect, heating efficiency, material dispersion and intelligent control, and cannot meet the efficient, high-quality, energy-saving and stable drying demand of high-end sensitive materials. A technical and reliable inert gas atmosphere drying device and method with strong adaptability are needed to fill the gap in the existing technology and promote the technical upgrading of related industries. SUMMARY

[0010] (I) Technical problems solved In view of the problems of unreliable sealing, low gas utilization rate, poor water removal effect, uneven heating, poor material dispersion and low intelligent degree of the existing inert gas atmosphere drying device and technology, the present application provides a material drying device and method in inert gas atmosphere.

[0011] (II) Technical solutions To achieve the above object, the present application provides the following technical solutions: A material drying device in an inert gas atmosphere, comprising a sealed drying cavity module, a high-reliability sealing and atmosphere control module, an inert gas closed-loop circulation deep water removal module, a heat pump assisted microwave infrared composite heating module, a material dispersion and bearing module, a multi-parameter online monitoring module and an AI intelligent linkage control system, each functional module is mechanically connected or electrically connected, and works cooperatively; The inert gas closed-loop circulation deep water removal module integrates membrane separation water removal, adsorption regeneration water removal and condensation water removal triple water removal technology, realizes inert gas closed-loop circulation utilization rate ≥ 95%; The heat pump assisted microwave infrared composite heating module integrates heat pump waste heat recovery, microwave heating and infrared heating triple technology, realizes waste heat recovery utilization rate ≥ 70%; The AI intelligent linkage control system can dynamically control the running state of each module according to the multi-parameter online monitoring data, and realizes on-demand energy supply.

[0012] Further, the high-reliability sealing and atmosphere control module adopts a triple sealing structure, cooperates with a hydraulic locking mechanism and a gas leakage automatic compensation unit.

[0013] Further, the inert gas closed-loop circulation deep water removal module comprises a high-purity inert gas source, a gas buffer tank, a membrane separation water removal assembly, an adsorption regeneration water removal assembly, a condensation water remover, a gas-liquid separator, a circulating fan and a gas purification module; The adsorption regeneration water removal assembly adopts a molecular sieve + activated alumina composite adsorbent, and can realize online heating regeneration by using the waste heat recovered by the heat pump.

[0014] Further, the heat pump assisted microwave infrared composite heating module comprises a heat pump unit, a microwave heating assembly, an infrared heating assembly and a temperature zoning control system, the temperature control precision is ± 0.5 ℃, and the temperature range is 25~220 ℃ adjustable.

[0015] Further, the material dispersion and bearing module comprises a multilayer quartz hollow tray, a rotary drive assembly and an ultrasonic dispersion assembly, can avoid material agglomeration, and ensures that the material is heated and contacted with airflow uniformly.

[0016] Further, the multi-parameter online monitoring module comprises an oxygen content sensor, a dew point sensor, a laser moisture sensor, a multi-channel temperature sensor, a pressure sensor and an energy consumption monitoring sensor, can collect each parameter in real time and transmit to the AI intelligent linkage control system.

[0017] The present application also provides a material drying method in an inert gas atmosphere, comprising the following steps: Step 1: loading and sealing detection, ensuring that the material is uniformly laid, the cavity is sealed qualified, providing a basis for subsequent drying; Step 2: Vacuum inert gas multi-stage replacement, through the repeated operation of vacuumizing by the linkage of a rotary vane pump + a Roots pump and filling high-purity inert gas, the oxygen content and dew point in the cavity are quickly reduced; Step 3: Heat pump assisted microwave infrared composite heating drying, through composite heating, closed loop circulating air flow and material dispersion synergy, rapid heating and water vapor desorption of the material are realized; Step 4: AI intelligent linkage regulation, according to the dynamic adjustment of the operation of each module based on multi-parameter monitoring data, deep water removal and on-demand energy supply are ensured; Step 5: Standard shutdown and pressure maintaining cooling, cooling under the protection of inert gas to avoid moisture absorption of the material; Step 6: Protective discharge and cavity cleaning, realizing continuous production preparation; through multi-step cooperation, the unit water removal energy consumption is ensured to be ≤3000kJ / kg, and the drying effect meets the standard.

[0018] Further, in the vacuum inert gas multi-stage replacement step, the vacuum degree is ≤1×10⁻³MPa, the replacement number is 1~2 times, the oxygen content in the cavity after replacement is ≤8ppm, and the dew point is ≤50℃Td.

[0019] Further, in the heat pump assisted microwave infrared composite heating drying step, microwave heating realizes synchronous heating inside and outside the material, infrared heating assists in maintaining uniform temperature, and the heat pump unit recovers the waste heat in the condensation water removal and adsorption regeneration processes for cavity heat preservation and adsorbent regeneration.

[0020] Further, in the AI intelligent linkage regulation step, the heating power, circulating air volume and water removal module operating state can be dynamically adjusted according to the material moisture, oxygen content, dew point and other parameters, over-drying is avoided, and the material performance consistency is ensured.

[0021] (Three) Beneficial effects Compared with the prior art, the present application provides a material drying device and method in an inert gas atmosphere, which has the following beneficial effects: The material drying device and method in an inert gas atmosphere, the present application adopts a multiple sealing structure cooperating with a gas leakage detection and automatic compensation mechanism, which can effectively block gas leakage, ensure the high sealing property of the drying cavity, and prevent external air from penetrating. At the same time, the cavity sealing property is monitored in real time by a gas leakage detection sensor, and once a leakage problem is found, the automatic gas supplement unit can be started in time to supplement high-purity inert gas, maintain a stable micro-positive pressure atmosphere inside the cavity, fundamentally avoid oxidation and moisture absorption of sensitive materials due to contact with air, and ensure the performance consistency of the dried materials.

[0022] The present application can thoroughly purify the inert gas carrying water vapor in the drying process by the inert gas closed loop circulation design, combined with multiple depth water removal and gas purification technology, remove the water vapor, oxygen and other impurities in the inert gas, realize the repeated circulation of the inert gas, significantly improve the gas utilization rate, and reduce the waste of inert gas. At the same time, without frequent supplement of new high-purity inert gas, the consumption cost of inert gas is effectively reduced, and the economy and environmental protection are considered. In addition, the adsorption water removal assembly can realize online regeneration by using system waste heat, without frequent disassembly and replacement of adsorbent, reducing operation and maintenance workload and cost, and ensuring the continuity of the drying process.

[0023] The present application combines multiple water removal technologies to form a synergistic water removal system, which can remove water vapor in inert gas in layers and thoroughly, and can realize deep water removal effect, provide a dry protective atmosphere for sensitive materials, effectively avoid the influence of residual water vapor on the performance of materials, meet the deep drying needs of high-end sensitive materials, and improve the drying quality.

[0024] The present application adopts a heat pump assisted microwave infrared composite heating mode, microwave heating can realize synchronous heating inside and outside the material, improve the heating efficiency, and infrared heating can assist in maintaining the uniformity of the cavity temperature, effectively solving the problems of uneven heating and inconsistent drying of materials inside and outside in the existing device, and ensuring the quality consistency of the dried materials. At the same time, the heat pump unit can efficiently recover the waste heat generated in the processes of heating and water removal, and recycle the waste heat for cavity insulation, gas heating and other links, greatly reducing the waste of waste heat and the overall energy consumption, and meeting the industrial development trend of energy saving and consumption reduction.

[0025] The present application sets a special material dispersion bearing module, which can effectively break the agglomeration phenomenon of powder and granular materials through the synergistic action of rotary drive and ultrasonic dispersion, make the materials evenly spread, increase the contact area of the materials with inert gas and heat, ensure the uniformity of the materials in heating and gas, avoid the problems of excessive local drying or incomplete drying, significantly improve the quality stability of batch products, and adapt to the drying needs of different types and forms of sensitive materials.

[0026] The present application is equipped with a multi-parameter online monitoring module and an AI intelligent linkage control system, which can collect various key parameters in the drying process in real time, analyze and process the parameters through AI algorithm, and dynamically control the running state of each module to realize on-demand energy supply, avoid excessive drying or incomplete drying, save energy, and protect material performance. At the same time, the system can automatically store all parameters in the drying process, which is convenient for subsequent parameter query, process optimization, quality tracing and abnormal troubleshooting, improves the fine level of production control, and adapts to the large-scale and fine production needs of high-end sensitive materials. BRIEF DESCRIPTION OF DRAWINGS

[0027] Figure 1Process schematic diagram of the closed drying cavity module of the present application; Figure 2 Process schematic diagram of the high-reliability sealing and atmosphere control module of the present application; Figure 3 Process schematic diagram of the deep water removal module of the present application; Figure 4 Process schematic diagram of the heat pump assisted microwave infrared composite heating module of the present application; Figure 5 Process schematic diagram of the material dispersion and bearing module of the present application; Figure 6 Process schematic diagram of the multi-parameter online monitoring module of the present application; Figure 7 Process schematic diagram of the AI intelligent linkage control system of the present application. DETAILED DESCRIPTION

[0028] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the scope of the present application.

[0029] Please refer to Figures 1 to 7 The present application is a material drying device in an inert gas atmosphere, which comprises a closed drying cavity module, a high-reliability sealing and atmosphere control module, an inert gas closed-loop circulation deep water removal module, a heat pump assisted microwave infrared composite heating module, a material dispersion and bearing module, a multi-parameter online monitoring module, and an AI intelligent linkage control system. The functional modules are mechanically or electrically connected and work cooperatively. The inert gas closed-loop circulation deep water removal module integrates membrane separation water removal, adsorption regeneration water removal, and condensation water removal triple water removal technologies. The heat pump assisted microwave infrared composite heating module integrates heat pump waste heat recovery, microwave heating, and infrared heating triple technologies, achieving a waste heat recovery utilization rate of ≥70%. The AI intelligent linkage control system can dynamically control the operating state of each module according to multi-parameter online monitoring data, and realizes on-demand energy supply.

[0030] In the present scheme, the high-reliability sealing and atmosphere control module adopts a triple sealing structure (inner layer fluororubber sealing + middle layer metal labyrinth sealing + outer layer vacuum sealing), cooperates with a hydraulic locking mechanism and a gas leakage automatic compensation unit, and has a cavity gas leakage rate of ≤1.0×10-6Pa·L / s. The micro-positive pressure of the cavity can be maintained at 0.02-0.05 MPa. The three-seal structure of "inner fluorine rubber elastic sealing layer (high-temperature resistance ≥ 250°C Td) + middle metal labyrinth sealing layer + outer vacuum sealing washer" is adopted, and the sealing property of the sealed dry cavity module is strengthened by cooperating with the cabin door hydraulic locking mechanism, so that the air leakage rate is controlled at ; at the same time, the air leakage detection sensor and the automatic air supplement unit are additionally provided, the air leakage detection sensor monitors the sealing property of the cavity in real time, when air leakage is detected, the automatic air supplement unit timely supplements high-purity inert gas to maintain the micro-positive pressure of 0.02-0.05 MPa inside the cavity, and air infiltration into the cavity to destroy the inert gas atmosphere is prevented. The sealing reliability of the sealed dry cavity is further improved, the three-seal structure cooperates with the hydraulic locking mechanism to greatly reduce the air leakage rate of the cavity, ensures that the cavity maintains a stable inert gas atmosphere for a long time, avoids material oxidation and moisture absorption caused by air leakage; the high-temperature-resistant fluorine rubber sealing layer is suitable for the heating working condition (temperature range 25-220°C) of the device, and the durability of the sealing structure is improved; the air leakage automatic compensation mechanism realizes real-time monitoring and dynamic adjustment of the sealing property, without manual intervention, and the stability and automation degree of the device operation are improved; the micro-positive pressure maintenance design further prevents air infiltration, provides a stable atmosphere basis for subsequent deep water removal and precise temperature control, and guarantees the performance consistency of the dried material.

[0031] In the present scheme, the inert gas closed loop circulation deep water removal module comprises a high-purity inert gas source, a gas buffer tank, a membrane separation water removal assembly, an adsorption regeneration water removal assembly, a condensation water remover, a gas-liquid separator, a circulating fan and a gas purification module; the adsorption regeneration water removal assembly uses a molecular sieve + activated alumina composite adsorbent, and the waste heat recovered by the heat pump can be used for online heating regeneration. The adsorption regeneration water removal assembly uses a molecular sieve and activated alumina composite adsorbent, and is connected with the pipeline of the heat pump unit, and the waste heat recovered by the heat pump unit is used for online heating regeneration of the adsorbent (regeneration temperature 120-150℃Td); the condensation water removal assembly is driven by the waste heat of the heat pump, and the cooling temperature can be adjusted at 0-10℃; the membrane separation water removal assembly uses a pervaporation membrane, and the water vapor interception rate is ≥99.9%, the three water removal assemblies cooperate to realize deep purification of inert gas, and then the gas is purified by the gas purification module and returned to the cavity to ensure the recycling rate and gas purity. The reliability of the closed loop circulation of inert gas and the deep water removal effect are strengthened, the operation and maintenance cost and gas loss are reduced, the high-purity inert gas source cooperates with the three water removal assemblies and the gas purification module to ensure that the dew point of the purified gas is ≤70℃, the oxygen content is ≤3ppm, the deep water removal and oxygen removal are realized, the material oxidation and moisture absorption are prevented; the adsorbent online regeneration design uses the waste heat of the heat pump without additional energy consumption, and the adsorbent does not need to be replaced frequently, which reduces the operation and maintenance cost by more than 50%; the heat pump waste heat driven condensation water removal further improves the waste heat utilization rate and reduces the overall energy consumption of the device; the high water vapor interception rate of the pervaporation membrane and the dehydration effect of the gas-liquid separator ensure the dryness of the circulating gas and improve the drying efficiency, while the inert gas recycling rate is ≥95%, which greatly reduces the gas consumption cost; the gas buffer tank ensures the pressure stability of the closed loop gas path, avoiding the influence of airflow fluctuation on the uniformity of drying.

[0032] In the present scheme, the heat pump auxiliary microwave infrared composite heating module comprises a heat pump unit, a microwave heating assembly (frequency 2450 MHz, power 1-5 kW adjustable), an infrared heating assembly (power 0.5-3 kW adjustable), and a temperature zoning control system, with temperature control accuracy ±0.5℃ and temperature range 25-220℃ adjustable. The heating uniformity and temperature control accuracy are improved, the waste heat recovery effect is strengthened, the energy consumption is further reduced, the drying efficiency is improved, the microwave infrared composite heating realizes synchronous heating of the inside and outside of the material, the heating rate is increased by more than 80% compared with traditional heating, the problems of overheating of the material surface and incomplete drying of the inside of the material are avoided, and the drying uniformity is improved; the temperature zoning control system and high-precision temperature control design ensure uniform temperature field of the cavity (temperature difference ≤±1℃), guarantee the consistency of batch material drying, and avoid local material deterioration; the heating power and temperature are adjustable, which adapts to the drying needs of different materials (such as low-temperature drying sensitive materials and high-temperature rapid drying temperature-resistant materials); the heat pump unit cooperates with the double heating assembly, the waste heat recovery utilization rate is ≥70%, combined with the precise regulation and control of temperature zoning, energy waste is avoided, unit water removal energy consumption is further reduced, and energy consumption is ensured to be ≤3000 kJ / kg; far infrared heating pipe auxiliary heating improves the stability of the cavity atmosphere temperature, and reduces the influence of temperature fluctuation on drying effect.

[0033] In the present scheme, the material dispersion carrying module comprises a multi-layer quartz hollow tray, a rotary drive assembly (rotational speed 0.5-8 r / min adjustable) and an ultrasonic dispersion assembly (power 0.3-1.5 kW adjustable), which can avoid material agglomeration and ensure uniform heating and air flow contact of the material. Each layer of tray is equipped with an independent ultrasonic dispersion unit, the rotary drive assembly drives the tray to rotate at low speed, and the ultrasonic dispersion assembly continuously works to break the material agglomeration, so that the material is evenly spread, the contact area between the material and inert gas is increased, and the quartz glass material avoids metal pollution. The pull-out tray is suitable for batch loading and continuous production. The problem of powder material agglomeration is solved, the uniformity of material heating and air flow contact is improved, the drying efficiency and material purity are further improved, the core effects include: ultrasonic dispersion + rotary tray cooperation, effectively breaking the material agglomeration, making the material evenly spread, avoiding incomplete drying inside caused by agglomeration, improving drying uniformity and drying rate, the overall drying rate is increased by more than 50% compared with the prior art; multi-layer independent tray and independent ultrasonic dispersion unit can realize synchronous drying of batch materials, improve production efficiency, and adapt to continuous production requirements; quartz glass material avoids metal pollution, ensures the purity of high-end sensitive materials such as electronic grade and lithium battery grade, and meets the drying requirements of high-end materials; the hollow tray design and rotary action increase the contact area between the material and inert gas, accelerate water vapor desorption, and further improve the drying efficiency; the rotational speed and power are adjustable, which adapts to the dispersion and drying needs of materials of different particle sizes and forms, and improves the adaptability of the device.

[0034] In the present scheme, the multi-parameter online monitoring module includes an oxygen content sensor (detection range 0~10ppm), a dew point sensor (detection range 80~20℃), a laser moisture sensor (detection accuracy ±0.01%), a multi-channel temperature sensor, a pressure sensor and an energy consumption monitoring sensor, which can collect various parameters in real time and transmit them to the AI intelligent linkage control system. All sensors are electrically connected to the AI intelligent linkage control system, real-time acquisition of corresponding parameters and transmission to the control system, automatic triggering of alarm when the parameters exceed the set range, providing accurate data support for AI intelligent control, realizing traceability and controllability of the drying process. Realize accurate monitoring of all parameters in the drying process, provide support for AI intelligent control, improve the stability of the device and the repeatability of the drying process, high-precision sensors ensure the accuracy of the detection of key parameters such as oxygen content, dew point and material moisture, providing accurate basis for AI intelligent control, ensuring that the atmosphere parameters in the cavity are stable (oxygen content ≤3ppm, dew point ≤70℃), and the material moisture meets the standard (≤50ppm); The multi-channel temperature sensor monitors the temperature of the cavity and the material in real time, and cooperates with the temperature zoning control system to improve the temperature control accuracy and temperature field uniformity; The energy consumption monitoring sensor monitors the power consumption and gas consumption of the device in real time, providing data support for AI on-demand energy control, further optimizing the energy consumption ratio; The laser moisture sensor monitors the material moisture in real time, avoids excessive drying or incomplete drying, reduces energy consumption and protects material performance; The abnormal alarm function can timely find out problems such as air leakage and sensor failure, avoid material deterioration and device damage, and improve the operation safety; All parameters are stored in real time, which is convenient for process optimization and quality traceability, and meets the strict requirements of high-end material industrialization.

[0035] The present application also provides a material drying method in an inert gas atmosphere, comprising the following steps: charging and sealing detection, vacuum inert gas multi-stage replacement, heat pump assisted microwave infrared composite heating drying, AI intelligent linkage control and deep water removal, standard shutdown and pressure maintaining cooling, protective discharge and cavity cleaning; The method can realize unit moisture removal energy consumption ≤3000kJ / kg, the drying rate is improved by more than 50% compared with the prior art, the oxygen content in the cavity after drying is ≤3ppm, and the dew point is ≤70℃.

[0036] Step 1: charging and sealing detection, ensuring uniform placement of materials, qualified cavity sealing, providing a basis for subsequent drying; Step 2: vacuum inert gas multi-stage replacement, through the repeated operation of rotary vane pump+roots pump linkage vacuumizing and filling high-purity inert gas, quickly reducing the oxygen content and dew point in the cavity; Step 3: heat pump assisted microwave infrared composite heating drying, through composite heating, closed loop circulating air flow, material dispersion cooperation, realizing rapid heating and water vapor desorption of materials; Step 4: AI intelligent linkage regulation, dynamically adjust the operation of each module according to multi-parameter monitoring data, ensure deep water removal and on-demand energy supply; Step 5: meet the shutdown and pressure cooling, cool down under the protection of inert gas, avoid material moisture absorption; Step 6: protective discharge and cavity cleaning, realize continuous production preparation; the whole process through multi-step cooperation, ensure that the unit water removal energy consumption ≤3000kJ / kg, drying effect meets the standard.

[0037] In this scheme, in the vacuum inert gas multi-stage replacement step, the vacuum degree , replacement times 1~2 times, oxygen content in the cavity after replacement ≤8ppm, dew point ≤50℃Td. Improve the adaptability and flexibility of the drying method, ensure that the replacement effect and heating effect adapt to the material characteristics, the linkage structure of rotary vane pump + roots pump can quickly extract to the limit vacuum degree , shorten the replacement time and improve the replacement efficiency; AI automatically adjusts the replacement times, accurately controls the initial water and oxygen content according to the material sensitivity, avoids excessive replacement of energy waste, and insufficient replacement of material deterioration, and considers energy consumption and drying effect; preset drying temperature can be adjusted, adapt to different temperature-sensitive materials (such as low-temperature drying of organic photosensitive materials, high-temperature rapid drying of lithium battery materials), expand the application range of the method; flexible adjustment of temperature and replacement times further ensures the performance consistency of the dried materials, and avoids material structure damage caused by mismatched process parameters.

[0038] In this scheme, in the heat pump assisted microwave infrared composite heating and drying step, microwave heating realizes synchronous heating inside and outside the material, infrared heating assists to maintain uniform temperature, heat pump unit recovers waste heat in the condensation and adsorption regeneration process, which is used for cavity insulation and adsorbent regeneration. Targeted control logic ensures that the oxygen content and dew point in the cavity are always stable in the target range, eliminates material oxidation and moisture absorption, and ensures drying effect; adsorbent regeneration uses heat pump waste heat, without additional energy consumption, further reducing energy consumption; reduce power and air volume when the material moisture approaches the target, avoid over-drying, not only save energy, but also prevent materials from agglomeration, performance degradation and other problems caused by over-drying; dynamic regulation ensures the collaborative work of each module, avoids energy waste and process fluctuation, ensures that the unit water removal energy consumption is stable ≤3000kJ / kg, and improves the stability of energy consumption ratio; without manual intervention, improve the automation degree and process stability of the drying method.

[0039] In this scheme, in the AI intelligent linkage regulation step, the heating power, circulating air volume, and water removal module operating state can be dynamically adjusted according to the material moisture, oxygen content, dew point and other parameters, to avoid excessive drying and ensure the consistency of material performance. The material type is clear, covering the main forms of high-end sensitive materials, expanding the application range of the method, and adapting to lithium batteries, electronics, special materials and other fields; the target water content is ≤50ppm, and can be adjusted as needed to meet the strict use requirements of different materials and ensure that the performance of the dried material meets the standards; the protective discharge design is matched with the clear material type to avoid moisture absorption, oxidation or damage of different forms of materials during the discharge process, further protecting the material performance; it adapts to different water content requirements, improves the universality of the method, and reduces the limitations of industrial application.

[0040] Example 1: Drying of lithium battery ternary positive electrode powder material (high sensitive powder material).

[0041] This example is for lithium battery ternary positive electrode powder (LiNi0.5Co0.2Mn0.3O2) , which is a high water and oxygen sensitive powder, easy to absorb moisture and oxidize. The target water content after drying is ≤30ppm, and the oxygen content in the cavity during drying needs to be strictly controlled to ≤2ppm and the dew point to ≤75℃ to avoid material oxidation and deterioration affecting the electrochemical performance. The material particle size is 1-10μm, which is easy to agglomerate, and the dispersion effect needs to be strengthened. The drying batch is 5kg.

[0042] The parameters of each core module are as follows: The closed drying cavity module adopts 316L stainless steel integrated cavity, the heat preservation layer thickness is 70mm, the heat loss is ≤4%, the adjustable pressure relief valve sets the pressure relief pressure to 0.08MPa, and the bottom liquid guide port is sealed connected with the gas-liquid separator.

[0043] High-reliability sealing and atmosphere control module: three-seal structure normally in use, hydraulic locking hatch ensures air leakage rate ; vacuum displacement assembly adopts rotary vane pump + roots pump linkage, limit vacuum degree ; automatic air supplement unit supplements high-purity argon (purity ≥99.9995%), maintains the cavity micro-positive pressure to 0.03MPa.

[0044] Inert gas closed-loop circulation deep water removal module: argon is used as inert gas, the gas buffer tank is stabilized to 0.04MPa; the condensation water removal assembly cooling temperature is set to 8℃, the membrane separation water removal assembly water vapor interception rate is ≥99.92%; the adsorption regeneration water removal assembly uses molecular sieve + activated alumina composite adsorbent, the regeneration temperature is set to 135℃, and the heat pump waste heat is used for online regeneration; the circulating fan drives the gas flow speed to be set to 2m / s, and the gas circulation utilization rate is ≥96%.

[0045] Heat pump auxiliary microwave infrared composite heating module: the heat pump unit normally recovers waste heat, the microwave heating assembly power is set to 3.5kW (frequency 2450MHz), and the infrared heating assembly power is set to 1.5kW; the temperature partition control system temperature control accuracy is ±0.5℃, the cavity temperature is set to 120℃, the cavity internal temperature difference is ≤±0.8℃, and the waste heat recovery utilization rate is ≥72%.

[0046] Material dispersion bearing module: 5-layer quartz glass hollow tray (pore diameter 0.2mm) is used, the material laying thickness is ≤10mm; the rotation driving assembly rotation speed is set to 4r / min, the ultrasonic dispersion assembly power is set to 0.8kW (frequency 40kHz), each layer of tray is independently ultrasonically dispersed, and the powder pre-dispersion time is 4min.

[0047] Multi-parameter online monitoring module: the oxygen content sensor detection range is 0~10ppm (accuracy ±0.05ppm), the dew point sensor detection range is 80~20℃ (accuracy ±1℃), and the laser moisture sensor detection accuracy is ±0.01%; the multi-way temperature sensor is arranged in the cavity 4 regions and the material interior respectively, the pressure sensor monitors the cavity pressure (range 0.1~0.3MPa) in real time, and the energy consumption monitoring sensor records the power consumption in real time.

[0048] AI intelligent linkage control system: preset process parameters, real-time reception of each sensor data, dynamic regulation and control of each module operation, unit moisture removal energy consumption control ≤2800kJ / kg, abnormal situation automatic alarm and record.

[0049] Implementation method steps: Step 1: loading and sealing detection, 5kg of lithium battery ternary positive electrode powder is evenly laid on 5 layers of quartz tray, the ultrasonic dispersion assembly is started for pre-dispersion for 4min to break the material agglomeration; the hatch is closed and hydraulically locked, the AI system starts sealing detection, confirms the air leakage rate , and enters the next step.

[0050] Step 2: vacuum inert gas multi-stage replacement, start the vacuum replacement assembly, vacuumize to , pressure maintaining for 2.5min; fill high-purity argon to 0.035MPa, pressure maintaining for 1.5min; repeat replacement for 2 times, the oxygen content in the cavity is ≤1.8ppm after replacement is completed, and the dew point is ≤76℃.

[0051] Step 3: composite heating and drying, start the heat pump unit, microwave heating assembly and infrared heating assembly, and run according to the preset parameters; start the water removal module and circulating fan to form an argon closed loop circulation; start the material dispersion module, the tray rotates at 4r / min, and the ultrasonic dispersion assembly continuously works.

[0052] Step 4: AI intelligent linkage regulation, real-time collection of oxygen content, dew point, material moisture and other parameters, when the dew point > 75℃, increase the condensation water removal power, start the membrane separation and adsorption regeneration linkage; when the material moisture is close to 30ppm, reduce the microwave power to 2kW, the infrared power to 1kW, and the circulating air flow to 1.5m / s.

[0053] Step 5: standard shutdown and pressure holding cooling, when the material moisture ≤30ppm, oxygen content ≤2ppm, dew point ≤75℃, stable maintenance for 60min, determine that the drying is up to standard; turn off heating, ultrasonic, circulating fan and water removal module, keep the heat pump and automatic air supplement unit, cool the material to ≤35℃.

[0054] Step 6: protective discharge and cavity cleaning, open the hatch under the protection of 0.03MPa micro-positive pressure argon, quickly take out the dried powder and transfer it into sealed packaging; start the cavity cleaning program, use argon closed loop to purge the cavity and remove residual dust.

[0055] The drying cycle of this implementation is 2.8h, which is 42% shorter than the existing technology; after drying, the powder moisture content is 27ppm, the oxygen content is 1.6ppm, and the dew point is 77℃, all meeting the preset requirements; the powder has no agglomeration and oxidation, and the electrochemical performance (specific capacity, cycle stability) has no decay; the unit moisture removal energy consumption is 2750kJ / kg, which is 65% lower than the existing device; the argon recycling rate is 96.3%, which greatly reduces the gas consumption cost; the whole process is automatically operated without manual intervention, the parameters are traceable, and it meets the needs of large-scale drying of lithium battery positive electrode powder.

[0056] Example 2: Drying of electronic grade polyimide film (low temperature resistant film material).

[0057] This example is for electronic grade polyimide film (thickness 50μm), which belongs to low temperature resistant, easy to absorb moisture film type sensitive material, temperature resistance ≤80℃, target moisture content after drying ≤40ppm, oxygen content in the cavity ≤3ppm, dew point ≤70℃ during drying, to avoid deformation and oxidation of the film; the material batch is 20 (single size 300mm×300mm), which needs to avoid film damage and wrinkles.

[0058] The parameters of each core module are as follows: The closed drying cavity module: the thickness of the heat preservation layer is 60mm, the heat loss is ≤5%, the adjustable pressure relief valve is set to 0.06MPa, the inner wall of the cavity is polished and treated to prevent adhesion, to avoid film adhesion.

[0059] High-reliability sealing and atmosphere regulation module: three-seal structure is enabled, hydraulic locking hatch ensures the air leakage rate ; the ultimate vacuum degree of the vacuum replacement assembly ; The automatic air supplementing unit supplements high-purity nitrogen (purity ≥ 99.9995%) to maintain a micro-positive pressure of 0.025 MPa in the cavity.

[0060] The inert gas closed-loop circulation deep water removal module uses nitrogen as the inert gas, and the gas buffer tank is stabilized at 0.035 MPa; the cooling temperature of the condensation water removal assembly is set to 5°C, and the water vapor interception rate of the membrane separation water removal assembly is ≥ 99.9%; the regeneration temperature of the adsorption regeneration water removal assembly is set to 125°C, and the heat pump waste heat is regenerated online; the circulating fan drives the airflow speed to be set to 1.2 m / s, and the gas circulation utilization rate is ≥ 95.5%.

[0061] The heat pump assisted microwave infrared composite heating module: the microwave heating assembly power is set to 1.5 kW (frequency 2450 MHz), and the infrared heating assembly power is set to 0.8 kW; the temperature partition control system temperature control accuracy is ± 0.5°C, the cavity temperature is set to 70°C, the cavity internal temperature difference is ≤ ± 1°C, and the waste heat recovery utilization rate is ≥ 70%.

[0062] The material dispersion bearing module: a 3-layer quartz glass hollow tray (pore diameter 0.3 mm) is used, and a high-temperature-resistant silicone pad is laid on the tray surface to avoid film damage; the rotation driving assembly speed is set to 1 r / min, and the ultrasonic dispersion assembly is turned off (to avoid film damage); the film is laid flat on the tray without wrinkles or overlaps.

[0063] The multi-parameter online monitoring module: the oxygen content, dew point, and laser moisture sensor operate according to standard parameters, the multi-channel temperature sensor focuses on monitoring the tray area temperature to avoid local overheating causing film deformation; the pressure sensor monitors the cavity micro-positive pressure in real time.

[0064] The AI intelligent linkage control system: preset low-temperature drying process parameters, focus on controlling heating power and circulating air flow, avoid excessive temperature, real-time monitor film moisture changes, and prevent over-drying.

[0065] Implementation method steps: Step 1: loading and sealing detection, 20 polyimide films are laid on the silicone pad of the 3-layer quartz tray to ensure no wrinkles or overlaps; the hatch is closed and hydraulically locked, and the AI system detects the cavity air leakage rate , and the next step is entered.

[0066] Step 2: multi-stage replacement of vacuum inert gas, vacuum to , pressure maintaining for 2 min; fill high-purity nitrogen to 0.03 MPa, pressure maintaining for 1 min; repeat replacement 1 time, the oxygen content in the cavity is ≤ 2.8 ppm, and the dew point is ≤ 71°C after replacement is completed.

[0067] Step 3: Composite heating and drying, start the heat pump unit, microwave heating assembly (1.5 kW), infrared heating assembly (0.8 kW); start the water removal module and circulating fan (1.2 m / s) to form a nitrogen closed loop circulation; start the material dispersion module, the tray rotates slowly at 1 r / min, and the ultrasonic dispersion assembly is turned off.

[0068] Step 4: AI intelligent linkage regulation, real-time collection of temperature, dew point, and material moisture parameters, when the cavity temperature fluctuates > ± 0.5℃, fine-tune the microwave and infrared power; when the dew point > 70℃, start the membrane separation and adsorption regeneration linkage to maintain stable dew point.

[0069] Step 5: meet the standard and keep pressure cooling, when the material moisture ≤ 40 ppm, oxygen content ≤ 3 ppm, dew point ≤ 70℃, stable maintenance for 45 min, determine the drying is up to standard; turn off the heating, circulating fan and water removal module, keep the heat pump and automatic air supplement unit, cool the film to ≤ 35℃.

[0070] Step 6: protective discharge and cavity cleaning, open the hatch under 0.025 MPa micro-positive pressure nitrogen protection, gently take out the dried film to avoid breakage; use nitrogen closed loop to purge the cavity to remove residual impurities.

[0071] The drying cycle of this implementation is 3.2h, which is 35% shorter than existing low-temperature drying devices; after drying, the film moisture content is 38ppm, the oxygen content is 2.7ppm, and the dew point is 72℃, meeting the requirements of electronic grade; the film is not deformed, broken or oxidized, and the surface flatness is good; the unit moisture removal energy consumption is 2900kJ / kg, which is 62% lower than existing devices; the nitrogen recycling rate is 95.7%, the operating cost is significantly reduced; the whole process is stable and controlled at low temperature, which meets the drying needs of low-temperature sensitive materials such as low-temperature resistant films.

[0072] Example 3: Drying of active metal titanium particles (highly oxidized sensitive particle materials).

[0073] This example is aimed at active metal titanium particles (particle size 0.5~2mm), which belong to highly oxidized sensitive particles and are easily oxidized and discolored in air. The target moisture content after drying is ≤ 20ppm, and the oxygen content in the cavity during drying must be ≤ 1ppm and the dew point must be ≤ 80℃; the material batch is 8kg, the particles are not agglomerated, and the particle abrasion during drying must be avoided.

[0074] The parameters of each core module are as follows: The sealed drying cavity module: the thickness of the heat preservation layer is 80mm, the heat loss is ≤ 3.5%, the adjustable pressure relief valve is set to 0.1MPa, the bottom liquid guide port is sealed well to avoid air leakage.

[0075] High-reliability sealing and atmosphere regulation module: three-seal structure is fully enabled, hydraulic locking hatch ensures air leakage rate ; vacuum replacement assembly limit vacuum degree ; automatic air supplement unit supplements high-purity argon (purity ≥ 99.9998%), maintains a micro-positive pressure of 0.04 MPa in the cavity.

[0076] Inert gas closed loop circulation deep water removal module: the gas buffer tank is stabilized at 0.045 MPa; the cooling temperature of the condensation water removal assembly is set to 10°C, and the water vapor interception rate of the membrane separation water removal assembly is ≥ 99.95%; the regeneration temperature of the adsorption regeneration water removal assembly is set to 145°C, and the heat pump waste heat is regenerated online; the circulating fan drives the gas flow speed to be set to 2.5 m / s, and the gas circulation utilization rate is ≥ 97%.

[0077] Heat pump assisted microwave infrared composite heating module: the microwave heating assembly power is set to 4 kW (frequency 2450 MHz), and the infrared heating assembly power is set to 2 kW; the temperature partition control system temperature control accuracy is ± 0.5°C, the cavity temperature is set to 160°C, the cavity internal temperature difference is ≤ ± 0.7°C, and the waste heat recovery utilization rate is ≥ 73%.

[0078] Material dispersion bearing module: 4 layers of quartz glass hollow tray (pore diameter 0.5 mm) are used, and the material laying thickness is ≤ 12 mm; the rotation driving assembly speed is set to 2 r / min (to avoid particle abrasion), and the ultrasonic dispersion assembly is closed (no particle agglomeration requirement); the tray surface is treated to prevent abrasion, reducing particle impact abrasion.

[0079] Multi-parameter online monitoring module: the oxygen content sensor detection accuracy is improved to ± 0.03 ppm, the dew point sensor detection range is 80~20°C (accuracy ± 1°C), and the laser moisture sensor detection accuracy is ± 0.01%; the oxygen content parameter is monitored, and when abnormal, air supplement and alarm are immediately started.

[0080] AI intelligent linkage control system: preset high-purity atmosphere drying parameters, strengthen oxygen content and dew point control logic, when oxygen content > 1 ppm, immediately start automatic air supplement and circulating fan speed up, ensure stable atmosphere.

[0081] Implementation method steps: Step 1: loading and sealing detection, 8 kg of titanium particles are evenly laid on 4 layers of quartz tray, ensuring that the particles are not stacked; the hatch is closed and hydraulically locked, and the AI system detects the cavity air leakage rate , and the next step is entered.

[0082] Step 2: vacuum inert gas multi-stage replacement, vacuum to 7 × 10⁻ 4 MPa, pressure maintaining for 3 min; fill high-purity argon to 0.04 MPa, pressure maintaining for 2 min; repeat replacement 2 times, the oxygen content in the cavity is ≤ 0.8 ppm after replacement is completed, and the dew point is ≤ 81°C.

[0083] Step 3: Composite heating and drying, start the heat pump unit, microwave heating assembly (4 kW), infrared heating assembly (2 kW); start the water removal module and circulating fan (2.5 m / s) to form an argon closed loop circulation; start the material dispersion module, the tray rotates slowly at 2r / min, and the ultrasonic dispersion assembly is turned off.

[0084] Step 4: AI intelligent linkage regulation, real-time collection of oxygen content, dew point, and material moisture parameters, when the oxygen content > 0.9 ppm, immediately start the automatic gas supplement unit and increase the circulating fan speed to 2.8 m / s; when the dew point > 80℃, start the three water removal assemblies to quickly reduce the dew point; when the material moisture is close to 20 ppm, reduce the microwave power to 2.5 kW and the infrared power to 1.2 kW.

[0085] Step 5: Drying to standard and pressure maintaining cooling, when the material moisture ≤ 20 ppm, the oxygen content ≤ 1 ppm, and the dew point ≤ 80℃, stable maintenance for 90 min, the drying is determined to be up to standard; turn off the heating, circulating fan, and water removal module, and keep the heat pump and automatic gas supplement unit, cool the titanium particles to ≤ 35℃.

[0086] Step 6: Protective discharge and cavity cleaning, open the hatch under the protection of 0.04 MPa micro-positive pressure argon, quickly take out the titanium particles and transfer them into sealed packaging; use argon closed loop to purge the cavity to remove residual particles and impurities.

[0087] The drying cycle of this implementation is 3.5 h, which is 40% shorter than the existing active metal drying device; after drying, the titanium particle moisture content is 18 ppm, the oxygen content is 0.7 ppm, and the dew point is 79℃, which fully meets the requirements of high oxidation sensitive materials; the titanium particles are not oxidized, not worn, and not agglomerated, and the surface color is uniform; the unit moisture removal energy consumption is 2700 kJ / kg, which is 68% lower than the existing device; the argon recycling rate is 97.2%, which greatly saves gas cost; the whole process is protected by high-purity gas atmosphere, and the automatic control meets the needs of large-scale drying of active metal particles.

[0088] In summary, the three examples cover three typical materials: high sensitive powder, low temperature resistant film, and high oxidation sensitive particles, which are all realized based on the device and method described in the claims of the present application, the parameters of each module are reasonably matched and work stably, the implementation effect is remarkable, which fully proves the practicality, adaptability, and outstanding advantages of energy saving, high efficiency, and high reliability of the present application, and it can be widely applied to the drying of various oxidation sensitive and moisture sensitive materials.

[0089] Although embodiments of the present application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the application, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A material drying apparatus under an inert gas atmosphere, characterized by, The application relates to a high-reliability sealing and atmosphere control module, an inert gas closed-loop circulation deep water removal module, a heat pump auxiliary microwave infrared composite heating module, a material dispersion and bearing module, a multi-parameter online monitoring module and an AI intelligent linkage control system, mechanical connection or electrical connection between the functional modules, and collaborative work.

2. The material drying device in an inert gas atmosphere according to claim 1, characterized by The high-reliability sealing and atmosphere control module adopts a triple-sealing structure, cooperates with a hydraulic locking mechanism and a gas leakage automatic compensation unit.

3. The apparatus for drying a material in an inert gas atmosphere according to claim 1, wherein The inert gas closed-loop circulation deep water removal module comprises a high-purity inert gas source, a gas buffer tank, a membrane separation water removal assembly, an adsorption regeneration water removal assembly, a condenser, a gas-liquid separator, a circulating fan and a gas purification module; the adsorption regeneration water removal assembly adopts a molecular sieve + activated alumina composite adsorbent, and can realize online heating regeneration by using the waste heat recovered by the heat pump.

4. The material drying apparatus under inert gas atmosphere according to claim 1, wherein The heat pump auxiliary microwave infrared composite heating module comprises a heat pump unit, a microwave heating assembly, an infrared heating assembly and a temperature partition control system, and the temperature control precision is + / - 0.5 DEG C, and the temperature range is 25-220 DEG C.

5. The apparatus for drying a material in an inert gas atmosphere according to claim 1, wherein The material dispersion and bearing module comprises a multi-layer quartz hollow tray, a rotary driving assembly and an ultrasonic dispersion assembly, can avoid material agglomeration, and ensures that the material is uniformly heated and contacted with airflow.

6. The material drying apparatus under inert gas atmosphere according to claim 1, wherein The multi-parameter online monitoring module comprises an oxygen content sensor, a dew point sensor, a laser moisture sensor, a multi-channel temperature sensor, a pressure sensor and an energy consumption monitoring sensor, can collect various parameters in real time and transmit the parameters to the AI intelligent linkage control system.

7. A material drying method in an inert gas atmosphere, based on the material drying apparatus in an inert gas atmosphere according to any one of claims 1 to 6, characterized by, The application also discloses a drying method. The application also discloses a drying method. In the heat pump auxiliary microwave infrared composite heating drying step, microwave heating realizes synchronous temperature rise inside and outside the material, infrared heating assists in maintaining temperature uniformity, the heat pump unit recovers waste heat in the condensation water removal and adsorption regeneration process, and is used for cavity heat preservation and adsorbent regeneration. ​ ​ ​ ​ 8. The apparatus and method for drying a material under an inert gas atmosphere according to claim 7, wherein In the vacuum inert gas multi-stage replacement step, the vacuum degree is 1~2 times, the oxygen content in the cavity after replacement is ≤8ppm, and the dew point is ≤50℃Td.

9. The apparatus and method for drying a material under an inert gas atmosphere according to claim 7, wherein ​ 10. The apparatus and method for drying a material under an inert gas atmosphere according to claim 7, wherein In the AI intelligent linkage regulation step, the heating power, the circulating air volume and the operation state of the water removal module can be dynamically adjusted according to the parameters such as material moisture, oxygen content and dew point, so as to avoid excessive drying and ensure the consistency of material performance.

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