Alcohol displacement vessel and method for aerogels and aerogel composites
By layering materials, directional fluid injection and discharge, magnetically coupled stirring, and low-temperature, low-pressure inert atmosphere control, the problem of low alcohol replacement efficiency in aerogels and composite materials has been solved, achieving efficient and safe solvent replacement.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- CHANGSHA RONGLAN MACHINERY
- Filing Date
- 2026-02-13
- Publication Date
- 2026-05-15
AI Technical Summary
Existing alcohol replacement processes for aerogels and aerogel composites are inefficient, time-consuming, and consume large amounts of solvent, making them unsuitable for large-sized and irregularly shaped components. Furthermore, existing improvement schemes pose safety risks or lack applicability.
The material placement components are stacked in layers, and the directional fluid injection and discharge, magnetically coupled stirring system enhances the flow field disturbance non-contactly, while the low-temperature and low-pressure inert atmosphere environment is controlled to synergistically improve solvent diffusion and displacement efficiency.
It significantly shortens the replacement cycle, reduces solvent consumption, improves adaptability to large and irregularly shaped components, and ensures operational safety and product quality stability.
Smart Images

Figure CN121695787B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of material preparation technology, and in particular, to an alcohol displacement container and method for aerogels and aerogel composite materials. Background Technology
[0002] Aerogels and their composites are typically prepared using the sol-gel method, which includes steps such as aging, solvent replacement, and supercritical drying. The solvent replacement step aims to replace water and reaction byproducts within the pores of the wet gel with organic solvents (such as alcohols) with lower surface tension, thereby mitigating the capillary forces that damage the three-dimensional network structure of the gel during subsequent drying.
[0003] Currently, conventional displacement processes typically involve immersing the wet gel sample in a large amount of displacement solvent, relying on the diffusion of the solute's natural concentration gradient for displacement. This method has significant drawbacks: firstly, it has low displacement efficiency and a long cycle, especially for large-sized products or those with complex irregular structures, often requiring multiple rounds of displacement using solvents tens of times the gel volume, taking several days or even weeks; secondly, it consumes a huge amount of solvent, and the internal space utilization of conventional displacement containers is low, further exacerbating solvent waste and production costs.
[0004] To improve displacement efficiency, several improvement schemes have been proposed in existing technologies. For example, one scheme uses microwave-assisted heating to accelerate the movement of solvent molecules, but this technology is mainly suitable for roll or thin flat products, with limited applicability to bulk and irregularly shaped components, and insufficient adaptability to industrial production. Another scheme attempts to introduce ultrasonic vibration combined with inert gas pressurization to enhance the mass transfer process; however, this method is also more suitable for products with specific shapes and may lead to increased shrinkage of the final product, affecting its thermal insulation performance. In addition, there are schemes that place the displacement process in a high-temperature and high-pressure reactor, utilizing subcritical conditions to improve efficiency; however, this equipment is a high-pressure vessel, posing significant safety risks, and the high investment and operating costs limit its application in large-scale production. Summary of the Invention
[0005] This invention provides an alcohol displacement container and method for aerogels and aerogel composites. By stacking materials in layers in the placement components, injecting and discharging liquids in a directional manner through the inlet and outlet components, enhancing the flow field disturbance non-contactly through a magnetically coupled stirring system, and maintaining a low-temperature, low-pressure, inert atmosphere in the environmental system, the efficiency of solvent diffusion and displacement is synergistically improved. This solves the technical problems of low efficiency, long cycle, large solvent consumption, and difficulty in adapting to large-size and irregularly shaped components in existing displacement processes.
[0006] According to one aspect of the present invention, an alcohol displacement container for aerogels and aerogel composites is provided, comprising: a sealed cavity having an upper opening and a cover plate sealing the upper opening for providing a sealed cavity; a material placement assembly inserted into the inner cavity of the sealed cavity through the upper opening for layering material within the inner cavity of the sealed cavity; an inlet / outlet liquid assembly disposed on the sealed cavity for injecting alcohol displacement solvent and / or desiccant along the inner wall of the sealed cavity and draining liquid from the bottom of the sealed cavity; a magnetically coupled stirring system disposed on the side of the sealed cavity in a relatively grouped arrangement for transmitting torque through magnetic non-contact to achieve a completely sealed stirring process, increasing the turbulence effect by adjusting the rotation speed and controlling the turbulence flow direction to improve the solvent diffusion efficiency, thereby improving the displacement efficiency; and an environmental control system for providing and maintaining a low-temperature, low-pressure, inert gas environment for alcohol displacement of the material.
[0007] Furthermore, the magnetic coupling stirring system includes a stirring paddle, an explosion-proof motor, a magnetic coupler, and an electrical control cabinet. The explosion-proof motor drives the magnetic coupler to rotate, which in turn drives the stirring paddle to rotate. The explosion-proof motor is connected to an external electrical control cabinet, which adjusts the speed and disturbance flow direction. By adjusting the speed and controlling the disturbance flow direction, the disturbance effect is increased, thereby improving the solvent diffusion efficiency and enhancing the displacement efficiency.
[0008] Furthermore, the environmental control system includes: a temperature environment control system for maintaining a constant low-temperature environment within the sealed cavity; and a gas environment control system for maintaining a constant low-pressure inert gas environment within the sealed cavity.
[0009] Furthermore, the temperature environment control system includes an overall insulation layer laid outside the sealed cavity; the temperature environment control system also includes a heating and cooling unit and a temperature display. The heating and cooling unit is connected to the sealed cavity through an external heating coil to heat the inner cavity of the sealed cavity, and the temperature display is installed inside the sealed cavity to realize temperature monitoring. The heating and cooling unit and the temperature display are electrically connected. The temperature display monitors and feeds back the temperature signal of the inner cavity of the sealed cavity to the heating and cooling unit in real time. The control unit inside the heating and cooling unit compares the temperature signal with the preset target temperature value, and then automatically adjusts the output power to heat or cool. Finally, the sealed cavity is continuously heated or cooled through the external coil to achieve temperature control inside the cavity.
[0010] Furthermore, the gas environment control system includes an inert gas inlet, a pressure display, and a breather valve installed in the sealed cavity; inert gas is introduced through the inlet to maintain a preset pressure in the sealed cavity, and the pressure display monitors it in real time; the breather valve maintains the pressure stability inside the sealed cavity, preventing damage to the sealed cavity due to pressure fluctuations, and reducing the evaporation loss of alcohol replacement solvent and external pollution.
[0011] Furthermore, the longitudinal section of the inner cavity of the sealed cavity is circular, elliptical, or capsule-shaped; the liquid inlet and outlet assembly includes an inlet and an outlet, the inlet is located in the arc-shaped area of the sealed cavity so that the reagent injected through the inlet flows along the arc-shaped surface, and the outlet is located at the bottom of the sealed cavity.
[0012] Furthermore, the storage assembly includes multiple shelves that are detachably installed in the sealed cavity. The shelves are assembled according to the size and specifications of the material to be replaced, ensuring that the material is placed one shelf at a time to improve the utilization of container space and reduce the consumption of replacement media.
[0013] According to another aspect of the present invention, an alcohol replacement method for aerogels and aerogel composite materials is also provided, using the aforementioned alcohol replacement container for aerogels and aerogel composite materials, comprising the following steps: S100, opening the cover, loading the bottom shelf according to the material size and placing the material, adding one shelf and one layer of material sequentially until the material is placed; S200, calculating the total mass of alcohol replacement solvent required based on the material filling amount; S300, injecting alcohol replacement solvent from the inlet and allowing the alcohol replacement solvent to flow slowly along the inner wall surface to avoid the alcohol replacement solvent directly impacting the material and causing material damage; S400, closing the cover and checking the airtightness of the sealed cavity, while simultaneously injecting inert gas to a preset pressure; S500, starting the magnetic coupling stirring system for stirring, observing the stirring effect through the observation window and ensuring that... Damage to materials; S600, set the parameters of the integrated heating and cooling machine, turn on the integrated heating and cooling machine to heat the sealed cavity, and observe the temperature and pressure display instruments to ensure that the temperature and pressure are within the normal and safe range; S700, check the status inside the sealed cavity through the observation window at preset time intervals; S800, replace the alcohol replacement solvent in the sealed cavity at preset time intervals; S900, repeat steps S200 to S800 until the replacement process is completed, turn off the integrated heating and cooling machine and the magnetic coupling stirring system in sequence, and check the temperature and pressure display instruments. Under safe conditions, open the cover plate and take out the top layer of product and the top shelf in sequence from top to bottom, and so on, until all products are taken out. Then drain the alcohol replacement solvent in the sealed cavity through the liquid outlet.
[0014] Further, in step S800, the alcohol replacement solvent in the sealed cavity is replaced, specifically as follows: S801, turn off the integrated heating and cooling unit; S802, after the temperature drops to room temperature, turn off the magnetic coupling stirring system; S803, open the outlet to drain the alcohol replacement solvent from the sealed cavity; S804, inject the alcohol replacement solvent into the inlet to the preset amount, and allow the alcohol replacement solvent to flow slowly along the inner wall.
[0015] Furthermore, after step S300, the following steps are added: 1% desiccant is added to the alcohol replacement solvent through the inlet and the solvent is agitated at a constant speed using a magnetically coupled stirring system to improve the replacement efficiency; and / or after step S800, the following steps are added: 5% desiccant is added to the alcohol replacement solvent during or after discharge, and the solvent is stirred for 1-2 hours and then allowed to stand for 10 minutes to achieve the reuse of the alcohol replacement solvent.
[0016] Further, in step S400, an inert gas inlet is connected to the outside of the sealed cavity, and inert gas is filled in according to the preset settings of the pressure display and the breathing valve, so that the sealed cavity is kept at constant pressure and reaches the initial pressure index value required for replacement. The initial pressure index value is obtained as follows: S401, calculation of material filling amount. In order to increase the material filling amount and improve the utilization rate of alcohol replacement solvent, ethanol is used as the alcohol representative for calculation. The sealed cavity is equipped with a movable shelf (4), and the minimum filling amount is set to 60%; S402, calculation of inert gas filling pressure value. In order to maintain the pressure in the alcohol replacement container to reach the preset pressure value, a certain amount of inert gas needs to be pre-filled. The pre-filling nitrogen pressure is calculated and designed based on the pressure and temperature setting range.
[0017] Further, step S401 specifically involves: considering the replacement effect, setting the replacement pressure ≥ 0.5 MPa to ensure the replacement effect; considering safety performance, the replacement solvent ethanol is a volatile, flammable, and explosive substance, so the set pressure value is ≤ 1.0 MPa, i.e., the replacement pressure should be controlled between 0.5 MPa and 1 MPa; considering the replacement effect, setting the replacement temperature ≥ 80℃ to ensure the replacement effect; considering safety performance, the replacement solvent ethanol is a volatile, flammable, and explosive substance, so the set temperature value is ≤ 90℃, i.e., the replacement temperature is controlled between 80 and 90℃; calculating and designing the maximum filling capacity of the equipment based on the pressure and temperature setting range; at 20℃, the initial gauge pressure is zero, i.e., the absolute pressure value is 101 kPa, and at 80℃, the set final gauge pressure is 500 kPa, i.e., the absolute pressure value is 601 kPa; based on the fact that the amount of nitrogen in the initial and final states remains unchanged, the ideal gas law is used:
[0018] P 氮气1 V 氮气1 =nRT
[0019] Among them, P 氮气1 Where n is the initial nitrogen pressure, n is the amount of substance, R is a constant, and V is the initial nitrogen pressure. 氮气1 Where T is the volume of the gas phase inside the container and K is the temperature. The volume ratio of the gas phase space when the temperature is increased from 20℃ to 80℃ is given by the following formula:
[0020] V 氮气1(20℃) / V 氮气1(80℃) =T20℃ P 氮气1(80℃) / (T) 80℃ P 氮气1(20℃) )
[0021] According to Dalton's law of partial pressures:
[0022] P 总 =P 乙醇 +P 氮气
[0023] Where: P 总 It is the total pressure, P 乙醇 It is the partial pressure of ethanol, P 氮气 It is the partial pressure of nitrogen;
[0024] P 总20℃ =101 kPa, P 总80℃ =601 kPa, P 乙醇(20℃) ≈5.8kPa, P 乙醇(80℃) ≈116 kPa; Calculate the partial pressure of nitrogen:
[0025] P 氮气1(20℃) =95.2kPa
[0026] P 氮气1(80℃) =485kPa
[0027] Substituting into the formula for the volume ratio of nitrogen gas phase, we obtain the following formula:
[0028] V 氮气1(80℃) = V 氮气1(20℃) 0.2365
[0029] During the heating process from 20℃ to 80℃, the mass of liquid ethanol remains unchanged:
[0030] m 乙醇20℃ =m 乙醇80℃
[0031] Where, m 乙醇20℃ This is the mass of liquid ethanol at 20℃, m 乙醇80℃ This refers to the mass of liquid ethanol at 80℃;
[0032] Right now:
[0033] ρ 80℃ ×(V) 总 - V 氮气1(80℃) )=ρ 20℃ ×(V) 总 - V 氮气1(20℃) )
[0034] Among them, V 总 This refers to the total volume, and the density ρ of ethanol at 20℃. 20℃The density ρ of ethanol at 80℃ is 0.789. 80℃ It is 0.736;
[0035] We can obtain:
[0036] V 氮气1(20℃) / V 总 =8.60%
[0037] That is: the maximum filling amount is 1-8.60%=91.40%; when the filling amount is increased from 20℃ to 80℃, and the final gauge pressure is set at 500kPa, the maximum allowable filling amount is 91.40%; according to the above method, the filling amount when the final gauge pressure is 500kPa and the temperature reaches 90℃ is 88.77%; considering equipment utilization and equipment safety, the filling amount is set to 60%-80%.
[0038] Further, step S402 specifically involves: setting the final temperature to 80℃, the filling amount to 60%, and the final gauge pressure to 500 kPa; the filling amount is based on the ideal gas law:
[0039] P 氮气2 V 氮气2 =nRT
[0040] Among them, P 氮气2 It is the final nitrogen pressure, V 氮气2 It is the final gas volume inside the container;
[0041] Because the container is sealed, the amount of nitrogen gas remains constant, that is:
[0042] P 氮气2(80℃) V 氮气2(80℃) / (RT) 80℃ )= P 氮气2(20℃) V 氮气2(20℃) / (RT) 20℃ )
[0043] Calculate V based on the ethanol expansion coefficient. 氮气2(20℃) and V 氮气2(80℃) and V 总 Ratio:
[0044] V 氮气2(20℃) ×(1+△T×γ (20~80℃) )=V 氮气2(80℃)
[0045] Where, γ (20~80℃) The coefficient of thermal expansion of ethanol at 20–80°C is 1.1 × 10⁻⁶. -3 ℃ -1 , T is the temperature change; since the filling amount is 60%, that is:
[0046] V 氮气2(20℃) =40%Vtank
[0047] V 氮气2(80℃) =37.5%V tank
[0048] Among them, V tank It is the total capacity;
[0049] We can obtain:
[0050] P 氮气2(20℃) =377kPa
[0051] Calculated using the above method, the final gauge pressure is 0.5-1.0 MPa, the final temperature is 80-90℃, and the filling rate is 60-80%.
[0052] The present invention has the following beneficial effects:
[0053] 1. The material placement assembly allows materials to be stacked in layers, improving the space utilization rate within the sealed cavity, increasing the single replacement throughput, and accommodating the orderly loading of different sizes, especially large and irregularly shaped components. From a process layout perspective, this reduces the amount of alcohol replacement solvent consumed per unit product, laying the foundation for reducing overall alcohol replacement solvent consumption.
[0054] 2. The inlet and outlet liquid assembly is designed to inject liquid along the inner wall and drain it from the bottom, forming a top-down directional displacement solvent flow path. This flow direction design can be combined with the flow field generated by the magnetically coupled stirring system to form a more effective overall circulation. It is beneficial to effectively discharge waste liquid (or mixed liquid with high water content) that has participated in the displacement and whose density may have changed from the bottom, avoiding disorderly mixing of new and old solvents in the cavity, thereby promoting the renewal efficiency of alcohol displacement solvent and reducing unnecessary retention and waste of alcohol displacement solvent.
[0055] 3. The magnetically coupled stirring system uses a completely sealed, non-contact transmission method, with pairs of components installed on the sidewall of the sealed cavity. It generates controllable forced convection and turbulent disturbances by magnetically driving the internal stirring structure. This active and adjustable (speed and direction) fluid disturbance directly and continuously acts on the alcohol displacement solvent in the cavity, enhancing the mass transfer boundary layer renewal rate of the alcohol displacement solvent outside the gel channels of the material. This accelerates the diffusion rate of the alcohol displacement solvent into the internal channels of the material gel and the rate at which residual water molecules in the channels are removed from the bulk solution of the material. It is a dynamic enhancement method to improve displacement efficiency and shorten the cycle.
[0056] 4. The environmental control system provides and maintains a low-temperature, low-pressure, inert gas environment, creating conditions for efficient displacement in terms of thermodynamics and chemical stability. The low-temperature environment helps reduce the evaporation loss of alcohol solvents and operational risks. The low-pressure (slightly negative pressure) environment can promote the removal of residual liquid in the gel channels by moderately reducing external pressure without introducing high-pressure risks. The inert atmosphere effectively isolates oxygen and water vapor, preventing unnecessary oxidation or hygroscopic side reactions of solvents and / or gel materials during the displacement process, ensuring the quality stability of the displacement process and the final product.
[0057] In addition to the objectives, features, and advantages described above, the present invention has other objectives, features, and advantages. The invention will now be described in further detail with reference to the figures. Attached Figure Description
[0058] The accompanying drawings, which form part of this invention, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an undue limitation of the invention. In the drawings:
[0059] Figure 1 This is a schematic diagram of the structure of an alcohol displacement container for aerogel and aerogel composite materials according to a preferred embodiment of the present invention;
[0060] Figure 2 This is a schematic diagram of the structure of the magnetic coupling stirring system of the preferred embodiment of the present invention, showing the direction of the stirring change.
[0061] Figure 3 This is a schematic diagram of the installation and assembly of the shelf according to a preferred embodiment of the present invention.
[0062] Legend:
[0063] 1. Cover plate; 2. Sealed cavity; 3. Magnetic coupling stirring system; 4. Shelf; 5. Breathing valve; 6. Inert gas inlet; 7. Pressure display; 8. Liquid inlet / outlet assembly; 9. Integrated heating and cooling unit; 10. External heating coil; 11. Temperature display. Detailed Implementation
[0064] The embodiments of the present invention will be described in detail below with reference to the accompanying drawings. However, the present invention can be implemented in many different ways as defined and covered below. Unless otherwise stated, the raw materials and reagents used in the following embodiments are commercially available or can be prepared by known methods.
[0065] like Figure 1As shown, the alcohol displacement container for aerogels and aerogel composites in this embodiment includes: a sealed cavity 2 with an upper opening and a cover plate 1 sealing the upper opening for providing a sealed cavity; a material placement assembly inserted into the inner cavity of the sealed cavity 2 through the upper opening for layering the material within the inner cavity of the sealed cavity 2; an inlet / outlet liquid assembly 8 disposed on the sealed cavity 2 for injecting alcohol displacement solvent and / or desiccant along the inner wall of the sealed cavity 2 and draining the liquid from the bottom of the sealed cavity 2; a magnetically coupled stirring system 3 disposed on the side of the sealed cavity 2 in a relatively grouped arrangement for transmitting torque through magnetic non-contact to achieve a completely sealed stirring process, increasing the turbulence effect by adjusting the speed and controlling the turbulence flow direction to improve the solvent diffusion efficiency, thereby improving the displacement efficiency; and an environmental control system for providing and maintaining a low-temperature, low-pressure, inert gas environment for alcohol displacement of the material. This invention relates to an alcohol displacement container made of aerogel and aerogel composite materials. The placement component allows materials to be stacked in layers, improving the space utilization within the sealed cavity 2. This increases the single displacement throughput and can accommodate the orderly loading of components of different sizes, especially large and irregularly shaped components. From a process layout perspective, this reduces the amount of alcohol displacement solvent used per unit product, laying the foundation for reducing overall alcohol displacement solvent consumption. The inlet and outlet liquid assembly 8 is designed to inject along the inner wall and drain from the bottom, forming a top-down directional displacement solvent flow path. This flow design can be combined with the flow field generated by the magnetically coupled stirring system 3 to form a more efficient overall circulation. It facilitates the effective discharge of waste liquid (or mixtures with high water content) that has participated in the displacement and whose density may have changed from the bottom, avoiding disorderly mixing of old and new solvents within the cavity. This, in turn, promotes the renewal efficiency of the alcohol displacement solvent and reduces unnecessary retention and waste of the alcohol displacement solvent. The magnetically coupled stirring system 3 is installed in pairs on the side wall of the sealed cavity using a completely sealed, non-contact transmission method. It generates controllable forced convection and turbulent disturbance through magnetic drive of the internal stirring structure. This active and adjustable (speed and direction) fluid disturbance directly and continuously acts on the alcohol replacement solvent in the cavity, enhancing the mass transfer boundary layer renewal rate of the alcohol replacement solvent outside the gel channels of the material. This accelerates the diffusion rate of the alcohol replacement solvent into the internal channels of the material gel and the rate at which residual water molecules in the channels are removed from the bulk solution of the material. It is a dynamic enhancement method to improve replacement efficiency and shorten the cycle. The environmental control system provides and maintains a low-temperature, low-pressure, inert gas environment, creating conditions for efficient displacement in terms of thermodynamics and chemical stability. The low-temperature environment helps reduce the evaporation loss of alcohol solvents and operational risks. The low-pressure (slightly negative pressure) environment can promote the removal of residual liquid in the gel channels by moderately reducing external pressure without introducing high-pressure risks. The inert atmosphere effectively isolates oxygen and water vapor, preventing unnecessary oxidation or hygroscopic side reactions of solvents and / or gel materials during the displacement process, ensuring the quality stability of the displacement process and the final product.This invention relates to an alcohol replacement container for aerogels and aerogel composites. Through the organic combination of high-utilization, well-organized loading, directional solvent flow path design, non-contact, controllable flow field enhancement, and low-temperature, low-pressure, inert atmosphere maintenance, the solvent replacement process is systematically optimized from four dimensions: space utilization, macroscopic flow, microscopic mass transfer, and environmental control. While ensuring operational safety and product quality, it significantly shortens the solvent replacement cycle of aerogels and their composites, substantially reduces solvent consumption, and particularly improves process adaptability and efficiency for large-size and irregularly shaped products. This effectively overcomes the technical bottlenecks of existing replacement methods, such as low efficiency, high cost, and limited applicability. Optionally, an observation window is provided on the cover plate 1.
[0066] like Figure 1 and Figure 2As shown, in this embodiment, the magnetically coupled stirring system 3 includes a stirring paddle, an explosion-proof motor, a magnetic coupler, and an electrical control cabinet. The explosion-proof motor drives the magnetic coupler to rotate, which in turn drives the stirring paddle to rotate. The explosion-proof motor is connected to an external electrical control cabinet, which adjusts the rotation speed and disturbance flow direction. By adjusting the rotation speed and controlling the disturbance flow direction, the disturbance effect is increased, thereby improving the solvent diffusion efficiency and enhancing the displacement efficiency. The application of the magnetic coupler enables non-contact torque transmission, achieving complete physical isolation and static sealing between the explosion-proof motor (drive end) and the stirring paddle (working end). This eliminates the risk of solvent leakage that may occur at the rotating shaft of the sealed cavity and removes the source of contamination caused by wear of dynamic seals. It ensures that the displacement process is carried out safely and cleanly in a strictly sealed inert gas environment, which in turn helps maintain the stable conditions set by the environmental control system. The combination of explosion-proof motor and electrical control cabinet provides a precise, reliable and programmable power and control core; the electrical control cabinet allows operators to precisely adjust the speed of the drive motor and control the rotation direction of the stirring paddle (such as forward, reverse or periodic reversal), thereby achieving active and flexible control of stirring intensity and flow field pattern; this adjustable disturbance allows the flow state of the displacement solvent in the container to be optimized according to the material loading conditions (such as different configurations of stacked placement components), avoiding the formation of flow dead zones and enhancing fluid mixing and mass transfer throughout the displacement space. Adjustable stirring intensity and flow direction control are the core mechanisms for improving displacement efficiency. By increasing the rotation speed or changing the flow direction, the stirring paddle can generate stronger turbulence or form a specific circulating flow field within the sealed cavity 2. This enhanced fluid disturbance directly acts on the macroscopic flow path established by the inlet and outlet liquid components 8, more effectively disrupting the diffusion boundary layer formed by the concentration difference on the surface of the gel material, accelerating the penetration of fresh solvent into the gel channels; it also promotes the rapid dispersion and discharge of water or impurities displaced from the gel, thereby significantly accelerating the mass transfer rate of the displacement process and shortening the time required to achieve the desired displacement effect. This magnetically coupled stirring system 3 ensures process safety and cleanliness through non-contact sealed transmission, and provides an active, controllable, and efficient means of enhancing fluid dynamics for the displacement process with precisely programmable stirring; by optimizing the movement of fluid micro-elements, it directly intervenes in the diffusion mass transfer bottleneck in the displacement process, thereby shortening the displacement cycle and improving displacement efficiency.
[0067] like Figure 1As shown, in this embodiment, the environmental control system includes: a temperature environment control system for maintaining a constant low-temperature environment within the sealed cavity 2; and a gas environment control system for maintaining a constant low-pressure inert gas environment within the sealed cavity 2. The temperature environment control system maintains a constant low-temperature environment within the sealed cavity 2. This low-temperature environment significantly reduces the saturated vapor pressure of the displacement solvent (especially volatile organic solvents such as alcohols), thereby minimizing solvent evaporation loss during the displacement process. This not only reduces solvent consumption and operating costs but also improves operational safety and helps maintain the pressure stability set by the gas environment control system. Furthermore, the low-temperature environment effectively suppresses potential side reactions or structural relaxation of the gel material in the solvent, providing a stable and controllable reaction condition for the displacement process and ensuring the structural integrity of the final product. The gas environment control system maintains a constant low-pressure inert gas environment within the sealed chamber 2. This inert gas environment (such as nitrogen or argon) completely eliminates oxygen and water vapor, providing chemical protection for the gel material and solvent. This completely eliminates the risks of oxidation, combustion, or structural damage to the gel network due to contact with moisture, ensuring the stability and reliability of the replacement process and product quality. The constant low-pressure environment also acts on the replacement process from a physical perspective. Without introducing the risks of high-pressure equipment, this low-pressure environment creates a small outward pressure difference between the inside and outside of the gel material. This pressure difference helps overcome the surface tension and viscous resistance of the liquid within the gel pores, thereby promoting the smooth extraction of residual solvent and moisture from the pores by the externally flowing fresh replacement solvent. This plays a role in enhancing the mass transfer process in conjunction with the inlet / outlet liquid assembly 8 and the magnetically coupled stirring system 3. This low-pressure environment also reduces the risk of abnormal pressure increases within the chamber due to factors such as operating temperature fluctuations, further improving the safety of the entire system. The environmental control system provides a highly controllable, safe, and efficient foundation for the entire solvent replacement process from three dimensions: thermodynamic stability, chemical inertness protection, and synergistic physical mass transfer. The temperature environmental control system reduces material consumption and risks, while the gas environmental control system fundamentally eliminates the potential risks of side reactions such as oxidation and hydration, and enhances replacement mass transfer through constant low-pressure physical processes. The synergy between the two ensures that the replacement process can be carried out under optimal and stable conditions, providing environmental protection for achieving the ultimate goal of high-efficiency, high-quality, low-consumption, and high-safety replacement.
[0068] like Figure 1As shown, in this embodiment, the temperature environment control system includes an overall insulation layer laid outside the sealed cavity 2; the temperature environment control system also includes a heating and cooling unit 9 and a temperature display 11. The heating and cooling unit 9 is connected to the sealed cavity 2 through an external heating coil 10 to heat the inner cavity of the sealed cavity 2. The temperature display 11 is installed in the inner cavity of the sealed cavity 2 to realize temperature monitoring. The heating and cooling unit 9 and the temperature display 11 are electrically connected. The temperature display 11 monitors and feeds back the temperature signal of the inner cavity of the sealed cavity 2 to the heating and cooling unit 9 in real time. The control unit inside the heating and cooling unit 9 compares the temperature signal with the preset target temperature value, and then automatically adjusts the output power to heat or cool. Finally, the sealed cavity 2 is continuously heated or cooled through the external coil to realize the control of the temperature inside the cavity. The overall insulation layer is directly laid on the outside of the sealed cavity 2, providing efficient thermal insulation. This reduces the heat exchange between the working environment inside the cavity and the external environment, thus laying the physical foundation for establishing and maintaining a stable and uniform temperature field inside. This not only reduces the energy consumption burden of the subsequent integrated cooling and heating unit 9, but also effectively avoids uncontrollable interference to the replacement process caused by ambient temperature fluctuations, ensuring the repeatability and consistency of the process. The integrated heating and cooling unit 9, the external heating coil 10, the temperature display 11, and their closed-loop control circuit together constitute a precise and automated dynamic temperature control system. The temperature display 11, as a sensing element, monitors the actual temperature inside the cavity in real time. This measurement signal is immediately fed back to the control unit of the integrated heating and cooling unit 9. The control unit compares the measured value with the preset target temperature (e.g., the required constant low temperature) and performs calculations based on the deviation using an internal control algorithm (such as PID control). Subsequently, the integrated heating and cooling unit 9 automatically and continuously adjusts its output power (for heating or cooling) and performs efficient heat exchange with the cavity through the external heating coil 10. This closed-loop feedback control mechanism enables the system to actively and in real time compensate for temperature fluctuations inside the cavity caused by factors such as heat from chemical reactions, fluid flow, or minor heat loss through the insulation layer, thereby achieving high-precision and dynamically stable control of the cavity temperature. The temperature environment control system's ability to regulate heating and cooling in both directions provides high flexibility for the displacement process. It can maintain a constant low-temperature environment below ambient temperature when needed to reduce solvent evaporation and suppress side reactions (as mentioned above), and can also provide controllable heating at specific process stages (such as initial heating to reduce solvent viscosity or post-process heating for recovery). This bidirectional and precise temperature control capability allows the temperature profile of the entire displacement process to be programmed according to different materials or process optimization requirements, thereby ensuring the core displacement effect while potentially further optimizing the efficiency and adaptability of the entire process.The temperature environment control system provides a highly stable, precise, controllable, and flexible temperature environment for the displacement process through the synergistic effects of thermal insulation, closed-loop feedback, and bidirectional temperature regulation. It not only passively reduces energy loss but also actively and in real time maintains the specific temperature conditions required by the process, thereby ensuring that the displacement reaction takes place under optimal and most stable thermodynamic conditions. This is not only the foundation for achieving low solvent volatility and process safety but also a guarantee for stable displacement rate, consistent product quality, and process repeatability.
[0069] like Figure 1As shown, in this embodiment, the gas environment control system includes an inert gas inlet 6, a pressure display 7, and a breathing valve 5 installed in the sealed cavity 2; inert gas is introduced through the inlet to maintain a preset pressure inside the sealed cavity 2, and the pressure display 7 monitors it in real time; the breathing valve 5 maintains the pressure inside the sealed cavity 2 to prevent damage to the sealed cavity 2 due to pressure fluctuations, and reduces the evaporation loss of alcohol replacement solvent and external pollution. The inert gas inlet 6, together with the preset pressure maintenance mechanism, establishes a controlled, chemically inert gaseous environment. By introducing inert gas (such as nitrogen or argon), the system can actively replace and vent the air in the sealed cavity 2, thereby creating a protective atmosphere around the material that isolates it from oxygen and moisture. This completely eliminates the chemical basis for potential safety hazards such as oxidation and combustion of solvents (especially alcohols) during operation, and also prevents moisture intrusion that could damage the gel structure or alter solvent properties, fundamentally ensuring the basic chemical stability of the displacement process and the quality of the final product. Maintaining this inert gas environment at a preset low pressure (e.g., slightly negative pressure) can create a small directional pressure gradient inside and outside the gel, which helps to promote the removal of residual liquid from the pores and synergistically enhances the displacement mass transfer process. The pressure display 7, as the system's sensing element, enables real-time and intuitive monitoring of the internal pressure of the cavity, providing crucial status feedback for operators or potential automated control systems. This allows for effective monitoring of the achievement of preset pressure targets, the integrity of the system seal, and dynamic pressure changes throughout the replacement process. This is a prerequisite for achieving accurate and reliable pressure control and a vital link in ensuring process repeatability and operational safety. The breather valve 5, as the system's pressure safety and stabilization element, passively and automatically responds to pressure fluctuations. When the internal pressure exceeds its set safety upper limit due to temperature fluctuations, liquid injection, liquid discharge, gas dissolution, or gas release, the breather valve 5 automatically opens to release pressure, preventing damage to the cavity due to overpressure. When the pressure falls below its set lower limit, it draws in inert gas to replenish the pressure, preventing deformation of the cavity due to excessive negative pressure. This not only directly protects the structural safety of the sealed cavity 2 but also effectively maintains the stability of the preset pressure range during dynamic processes, thereby reducing abnormal solvent evaporation losses caused by drastic pressure changes and continuously blocking the intrusion of external contaminated air, thus reinforcing the integrity of the inert gas environment. The gas environment control system, through the synergistic effect of actively establishing an inert low-pressure environment, real-time monitoring of pressure status, and automatic stabilization of pressure range, constructs a safe, stable, and clean physicochemical space for the entire replacement process. This not only eliminates the risks of chemical reactions such as combustion and oxidation at the source, but also enhances replacement efficiency by maintaining a stable low-pressure environment. Furthermore, the automatic adjustment function of the breather valve 5 ensures the safety of the equipment and the continuous and stable operation of the process, thereby achieving the invention's goal of safe, efficient, and high-quality replacement.
[0070] like Figure 1 As shown, in this embodiment, the longitudinal cross-section of the inner cavity of the sealed cavity 2 is circular, elliptical, or capsule-shaped; the liquid inlet / outlet assembly 8 includes an inlet and an outlet. The inlet is located in the arc-shaped area of the sealed cavity 2 so that the reagent injected through the inlet flows along the arc-shaped surface, and the outlet is located at the bottom of the sealed cavity 2. The specific longitudinal cross-sectional shape (circular, elliptical, or capsule-shaped) of the inner cavity of the sealed cavity 2 has hydrodynamic and structural advantages; these smooth arc-shaped curved surface structures can effectively avoid the flow dead zones or eddy current stagnation zones that occur in traditional rectangular or angular containers; when the displacement solvent flows in the cavity or is driven by the magnetically coupled stirring system 3, the smooth arc surface is conducive to forming a smoother and more uniform overall circulating flow field, so that the solvent can more effectively contact and flow through each layer of material loaded on the placement assembly, thereby creating favorable container conditions for improving displacement uniformity and efficiency on a macroscopic scale; when this type of shape is subjected to the internal and external pressure difference established by the gas environment control system, the stress distribution is more uniform, which helps to improve structural stability and safety. The design of the liquid inlet / outlet assembly 8, especially the placement of the liquid inlet in the curved surface area of the cavity, aims to optimize the initial injection flow pattern of the solvent. When the alcohol-based displacement solvent (or containing a desiccant) is injected from the curved surface area, it will naturally flow downwards along the tangential or oblique arc. It can utilize the momentum of the fluid itself to induce a wall-adhering flow near the side wall of the container, which helps to initially form a certain directional flow trend before the start of stirring and better couples with the subsequent stirring flow field. This avoids the solvent directly impacting the material or causing splashing, and is conducive to the solvent wetting and displacing the material more gently and evenly. Placing the outlet at the bottom of the chamber is the most reasonable and efficient design, conforming to the basic principles of gravity settling and density stratification. During the displacement process, the heavier liquids containing more water or impurities, as well as the small amount of insoluble matter that may exist when standing, will naturally settle to the bottom of the container. Placing the outlet at the bottom ensures that these displacement waste liquids, sediments, or mixed liquid layers of different densities can be discharged from the container most effectively and thoroughly, thereby avoiding their accumulation and recycling in the container. This ensures the purity of the fresh displacement solvent and the displacement driving force, which is an important step in achieving efficient displacement and solvent conservation. The cavity shape and liquid inlet / outlet layout design of this invention are based on a comprehensive consideration of fluid mechanics, mass transfer processes, and structural design. The smooth arc-shaped cavity provides a foundation for the uniformity of the internal flow field and structural safety. The arc-shaped liquid inlet enables the gentle and orderly introduction of the solvent. The bottom liquid outlet ensures the effective and complete discharge of waste liquid. The combination of these three factors optimizes the macroscopic flow path and renewal efficiency of the replacement solvent in the container. This, combined with the microscopic disturbances generated by the magnetically coupled stirring system 3, forms a highly efficient mass transfer circulation system from macroscopic to microscopic and from injection to discharge, thereby improving the overall replacement efficiency, ensuring replacement uniformity, and reducing solvent consumption.
[0071] like Figure 1and Figure 3 As shown, in this embodiment, the storage assembly includes multiple storage racks 4, which are detachably installed inside the sealed cavity 2. The storage racks 4 are assembled according to the size specifications of the materials to be replaced, ensuring that materials are placed one layer of rack 4 at a time to improve container space utilization and reduce the consumption of replacement media. The detachable storage racks 4 and their assembly characteristics provide high process adaptability and flexibility. Operators can flexibly adjust the layout and spacing of the storage racks 4 or select suitable rack structures according to the actual shape and volume of materials to be replaced in different batches, of different sizes, and especially various irregular shapes. This maximizes the utilization of the effective internal space of the sealed cavity 2, ensuring that materials can be stacked tightly, neatly, and stably regardless of their shape, thereby directly increasing the single-pass throughput and meeting the process requirements for efficient replacement of large-sized and irregularly shaped components. The stacking of materials in layers of shelving 4 constitutes a standardized and modular loading pattern. This layered structure creates regular and uniform gaps between the materials. These gaps provide a pre-defined flow path throughout the entire loading body for the displacement solvent injected by the inlet / outlet liquid assembly 8 and the fluid driven by the magnetically coupled stirring system 3. The solvent can flow more smoothly and evenly across the surface and surrounding area of each layer of material, effectively avoiding flow blockage or short circuits caused by excessively dense or irregular material stacking. Structurally, this ensures sufficient and uniform contact between the displacement medium and the surface of all materials, laying the foundation for improving overall displacement uniformity. By improving space utilization and reducing media consumption, more materials to be treated can be loaded within a unit volume of sealed cavity 2. The total amount of displacement solvent (alcohols) required to immerse and displace these materials is significantly reduced compared to traditional random stacking methods, solving the problem of excessive solvent waste and reducing the solvent usage cost and subsequent waste liquid treatment load of a single displacement process from the source. The loading assembly, through its adjustable and modular design, achieves high-density and highly organized material loading. This not only directly improves the equipment's processing capacity and economic efficiency from a space utilization perspective, but also optimizes the macroscopic flow path of the solvent in the material pile from a fluid distribution perspective. This ensures that the replacement medium can act efficiently and uniformly on all materials, thereby reducing the consumption of replacement solvent without sacrificing the replacement effect, and enhancing the device's adaptability to different specifications, especially irregularly shaped products.
[0072] The alcohol replacement method for aerogels and aerogel composites in this embodiment uses the aforementioned alcohol replacement container for aerogels and aerogel composites, and includes the following steps: S100, open the cover plate 1, load the bottom shelf 4 according to the material size and place the material, adding one shelf 4 and one layer of material sequentially until the material is placed; S200, calculate the total mass of alcohol replacement solvent required based on the material filling amount; S300, inject the alcohol replacement solvent from the inlet and allow the alcohol replacement solvent to flow slowly along the inner wall surface to avoid the alcohol replacement solvent directly impacting the material and causing material damage; S400, close the cover plate 1 and check the airtightness of the sealed cavity 2, while injecting inert gas to a preset pressure; S500, start the magnetic coupling stirring system 3 to stir, observe the stirring effect through the observation window and ensure that no damage is caused to the material; S60 0. Set the parameters of the integrated heating and cooling unit 9, turn on the integrated heating and cooling unit 9 to heat the sealed chamber 2, and observe the temperature display 11 and pressure display 7 at the same time to ensure that the temperature and pressure are within the normal and safe range; S700. Check the state inside the sealed chamber 2 through the observation window at preset time intervals; S800. Replace the alcohol replacement solvent in the sealed chamber 2 at preset time intervals; S900. Repeat steps S200 to S800 until the replacement process is completed. Turn off the integrated heating and cooling unit 9 and the magnetic coupling stirring system 3 in sequence, and check the temperature display 11 and pressure display 7. Open the cover plate 1 in a safe state, and take out the top layer of products and the top layer of shelves 4 from top to bottom, and so on, until all products are taken out. Then drain the alcohol replacement solvent in the sealed chamber 2 through the liquid outlet. Step S100, with its layer-by-layer, cumulative placement, ensures standardized, high-density, and repeatable orderly loading of materials within the replacement container. The physical separation created by the racks 4 provides uniform gaps for solvent flow in each layer of material and its surroundings, avoiding compression, deformation, or flow channel blockage caused by traditional stacking methods. This loading structure guarantees the fundamental conditions for sufficient and uniform contact between the solvent and all material surfaces, a prerequisite for efficient and uniform replacement. Step S200, calculating the required total solvent mass based on the loading volume, demonstrates the method's precision and economy, changing the extensive model of excessive solvent use based on experience in traditional replacement. By accurately calculating the required solvent amount based on the actual material loading volume (directly related to space utilization), the minimum necessary solvent usage can be precisely controlled from the process source, reducing solvent consumption and costs.The slow injection along the inner wall in step S300 and the observation and ensuring that stirring does not damage the material in step S500 together constitute a physical protection mechanism for the material throughout the process. By controlling the flow direction and flow rate of the injected fluid, high-velocity fluid is prevented from directly impacting the surface of the brittle gel material and causing structural damage. By monitoring the stirring intensity through the observation window, it is ensured that the flow field disturbance generated by magnetic stirring is sufficient to enhance mass transfer without being so violent as to cause collision or friction damage between materials. This ensures that the enhanced mass transfer process does not come at the expense of product integrity. The systematic environmental establishment and monitoring in steps S400 and S600, along with the reverse-sequence safety shutdown in step S900, together constitute a safe, controllable, and stable closed-loop process environment. Through inert gas replacement and airtightness testing, an inert low-pressure basic environment is established, isolating oxygen and moisture. Subsequently, the precise temperature control by the integrated heating and cooling unit 9 stabilizes the key process parameter of temperature within the optimized range. Continuous observation of temperature and pressure throughout the process enables real-time monitoring of the process status. Finally, strict safety shutdown and unloading sequences ensure the safety of the process endpoint and operation. This series of steps systematically manages the thermodynamic, chemical, and operational risks of the replacement process. The solvent replacement at preset time intervals in step S800 combines two strategies: magnetic stirring to enhance mass transfer and periodic renewal of the replacement medium. Stirring continuously disrupts the diffusion boundary layer at the microscopic level, accelerating replacement. Meanwhile, the periodic replacement of the nearly saturated old solvent maintains the maximum concentration difference (i.e., mass transfer driving force) between the solvent inside and outside the gel at the macroscopic level. The combination of these two methods ensures that the replacement process is always carried out efficiently under a high driving force, thereby significantly shortening the total time required to achieve the same replacement effect and solving the problem of long replacement cycles. This invention provides an alcohol replacement method for aerogels and aerogel composites. Through a series of rigorous and coordinated steps—"structured loading, precise metering, gentle operation, environmental control, dynamic replacement, and safe closed-loop"—the method organically integrates and orderly utilizes the functions of each subsystem of the alcohol replacement container. This not only achieves comprehensive and refined control over material integrity, solvent consumption, environmental parameters, and operational safety during the replacement process, but more importantly, through a dynamic process combining enhanced stirring and timed liquid replacement, it systematically shortens the replacement cycle and significantly reduces solvent consumption while ensuring replacement quality. This makes solvent replacement of large-size and irregularly shaped aerogel products a stable and repeatable industrial operation that is highly efficient, low-consumption, safe, and adaptable.
[0073] In this embodiment, the replacement of the alcohol displacement solvent in the sealed cavity 2 in step S800 is specifically as follows: S801, turn off the integrated heating and cooling unit 9; S802, after the temperature drops to room temperature, turn off the magnetic coupling stirring system 3; S803, open the outlet to drain the alcohol displacement solvent in the sealed cavity 2 completely; S804, inject the alcohol displacement solvent into the inlet to a preset amount and allow the alcohol displacement solvent to flow slowly along the inner wall surface. Step S801, which involves shutting down the integrated heating and cooling unit 9, and step S802, which involves shutting down the agitator after cooling down, constitute a pretreatment step that ensures safety and process stability. Stopping heating allows the system temperature (controlled by the temperature environment system) to naturally drop to room temperature, which can significantly reduce the vapor pressure and fluidity of the replacement solvent. This reduces the safety risks such as flash evaporation and vapor escape that may occur when the solvent is opened for discharge due to excessively high temperature and vigorous evaporation, and also reduces solvent evaporation loss. After cooling down, shutting down the agitator stops the magnetically coupled agitator system 3 from disturbing, which is conducive to the stabilization of the gas-liquid two phases in the container and allows any possible suspended solids to settle. This creates a calmer and more orderly working condition for subsequent clear liquid-solid separation and thorough discharge, avoiding material displacement or resuspension of settled impurities that may occur when directly discharging under vigorous agitation. Step S803, by opening the outlet and draining the waste liquid, achieves a synergy between gravity settling and bottom discharge design, resulting in efficient and thorough discharge of the waste liquid. After stirring stops and the system settles, the waste liquid, which has a high density and contains a large amount of displaced water or impurities, as well as possible trace solid particles, will settle or accumulate at the bottom of the sealed cavity 2 with a smooth arc surface. Discharge is carried out through the outlet located at the lowest point, ensuring that this portion of the displaced waste liquid with reduced efficiency is discharged from the system to the maximum extent and thoroughly. This directly cuts off the possibility of the waste liquid circulating in the system, preparing for the injection of fresh solvent and the reconstruction of the maximum concentration diffusion driving force, thereby improving the displacement efficiency and reducing the number of solvent cycles. Step S804, which involves injecting new solvent to a preset amount and allowing it to flow slowly along the inner wall, is the starting step for completing solvent replacement and initiating a new round of efficient replacement. The precise injection of the preset amount of new solvent, calculated based on the filling volume, inherits the principles of precision and economy from step S200, avoiding solvent waste. Furthermore, the method of allowing the solvent to flow slowly along the inner wall utilizes the fluid dynamics design of the arc-shaped flow guide, enabling the fresh solvent to smoothly and evenly refill the cavity and wet the material. This avoids direct impact of the liquid flow on the stationary material and any fragile gel structures that may form, achieving a lossless transition during the batch replacement process of the old and new solvents.
[0074] In this embodiment, after step S300, the following steps are added: 1% desiccant is added to the alcohol replacement solvent through the inlet and the solvent is agitated at a constant speed by the magnetically coupled stirring system 3 to improve the replacement efficiency; and / or after step S800, the following steps are added: 5% desiccant is added to the alcohol replacement solvent during or after discharge, and the solvent is stirred for 1-2 hours and then allowed to stand for 10 minutes to achieve the reuse of the alcohol replacement solvent. The addition of a small amount of desiccant (1%) to the displacement solvent after step S300, followed by uniform stirring, introduces a physicochemical synergistic enhancement method in the main displacement process. The addition of the desiccant can form a local microenvironment with a stronger affinity for water in the solvent. In the uniform flow field created by magnetic coupling stirring, these desiccant particles can be fully dispersed. Their huge specific surface area provides water absorption, which can continuously and dynamically absorb water diffused from the gel channels into the solvent, thereby effectively reducing the water content of the solvent on the outside of the gel. This is equivalent to maintaining and increasing the concentration difference (chemical potential gradient) of water inside and outside the material gel, that is, strengthening the mass transfer driving force of the displacement process. Thus, without increasing the temperature or pressure, the rate of water molecule diffusion from the gel to the solvent is gently increased, ultimately improving the displacement efficiency. The step S800, followed by the addition of a larger amount of desiccant (5%) to the discharged waste alcohol solvent and a stirring-settling process, allows for offline regeneration of the replaced waste solvent, achieving resource recycling. This step is for waste solvents that have completed one round of replacement and whose water content has significantly increased. The addition of a higher proportion of desiccant and thorough stirring aims to maximize the contact between the desiccant and the waste solvent. Through the strong water absorption properties of the desiccant, most of the dissolved water in the waste solvent is absorbed and fixed. The subsequent settling process facilitates the sedimentation or separation of the desiccant (and the absorbed water). Through this treatment, the water content of the waste solvent is significantly reduced, and its effectiveness as a replacement solvent is partially restored, thus giving it the potential to be reused in the next round of replacement or for other purposes. This opens up a way to reduce the consumption of fresh solvent and reduce waste liquid discharge from the end of the process. The desiccant process optimizes the economy and environmental friendliness of the displacement process from two different dimensions: process intensification and resource regeneration. Adding a small amount of desiccant during the process serves as a mild chemical aid, maintaining high mass transfer driving force by reducing the water content of the solvent, thereby increasing the displacement rate. The subsequent high-dose desiccant treatment of the waste solvent aims to recover and regenerate solvent resources, a direct measure to reduce unit consumption and waste emissions. The combination of these two approaches reflects the invention's comprehensive consideration of reducing operating costs and achieving green production while pursuing high efficiency.
[0075] In this embodiment, in step S400, an inert gas inlet is connected to the sealed cavity 2, and inert gas is filled in according to the preset settings of the pressure display instrument 7 and the breathing valve 5, so that the sealed cavity 2 is kept at a constant pressure and reaches the initial pressure index value required for replacement. The initial pressure index value is obtained as follows: S401, calculation of material filling amount: In order to increase the material filling amount and improve the utilization rate of alcohol replacement solvent, ethanol is used as the alcohol representative for calculation. The sealed cavity 2 is equipped with a movable shelf 4, and the minimum filling amount is set to 60%; S402, calculation of inert gas filling pressure value: In order to maintain the pressure in the alcohol replacement container to reach the preset pressure value, a certain amount of inert gas needs to be pre-filled. The pre-filling nitrogen pressure is calculated and designed based on the pressure and temperature setting range. In step S401, a minimum filling volume of 60% is set, establishing a lower limit for the space utilization rate of material loading. This ensures that the effective volume of the container is fully and efficiently utilized in each replacement operation, avoiding solvent waste caused by insufficient filling volume. This maximizes the amount of material that can be processed per unit volume of replacement solvent, thereby improving solvent utilization. This is a key process parameter control for reducing unit consumption and improving production efficiency. In step S402, the pre-charge nitrogen pressure is calculated and designed based on pressure and temperature settings. This achieves precise and predictable control of the initial inert gas pressure, abandoning the traditional practice of repeatedly charging and discharging gas based on experience. By establishing a theoretical or empirical calculation model between pressure, temperature, and inert gas quantity, the required pre-charge inert gas pressure value can be directly calculated based on preset process objectives (such as the required micro-negative pressure or specific pressure environment). This makes the establishment of process starting conditions more scientific, accurate, and repeatable, laying an accurate foundation for the entire replacement process to proceed in a stable and controllable pressure environment. It avoids the fluctuations that may occur in process consistency (such as solvent boiling point and diffusion rate) caused by improper initial pressure values. An external inert gas inlet is connected, and gas is filled according to the preset settings of the pressure display 7 and the breathing valve 5. This closed-loop control method automates and ensures the establishment and safety of the inert environment and pressure setting. Through real-time feedback from the pressure display 7, the operation can accurately fill the chamber pressure to the initial pressure index value calculated in step S402. The preset settings of the breathing valve 5 provide an automatic protection upper limit for this pressure setting value. The combination of these two not only ensures the accurate and rapid establishment of the target pressure environment, but also prevents the risk of overpressure due to misoperation, ensuring the stable and safe operation of the gas environment control system. Optionally, the alcohol replacement solvent, in addition to the ethanol (C2H5OH) specifically used in the examples, can usually be other low-grade alcohol organic solvents that can effectively replace water and have low surface tension.Alternatively, alcohol replacement solvents can also be methanol (CH3OH), isopropanol (C3H7OH, often referring to isopropanol), n-propanol (C3H7OH), tert-butanol (C4H9OH), etc. These solvents are all miscible with water, have significantly lower surface tension than water, and have relatively moderate boiling points, which are beneficial for their effective removal in subsequent drying steps (such as supercritical drying), thereby reducing damage to the gel network structure. In actual processes, the specific selection of solvents needs to comprehensively consider their replacement efficiency, impact on gel materials, safety, cost, and compatibility with subsequent processes.
[0076] In this embodiment, step S401 specifically involves: considering the replacement effect, setting the replacement pressure ≥ 0.5 MPa to ensure the replacement effect; considering safety performance, the replacement solvent ethanol is a volatile, flammable, and explosive substance, and the set pressure value is ≤ 1.0 MPa, that is, the replacement pressure should be controlled between 0.5 MPa and 1 MPa; considering the replacement effect, setting the replacement temperature ≥ 80°C to ensure the replacement effect; considering safety performance, the replacement solvent ethanol is a volatile, flammable, and explosive substance, and the set temperature value is ≤ 90°C, that is, the replacement temperature is controlled between 80°C and 90°C; calculating and designing the maximum filling capacity of the equipment based on the pressure and temperature setting range; at 20°C, the initial gauge pressure is zero, that is, the absolute pressure value is 101 kPa, and at 80°C, the set final gauge pressure is 500 kPa, that is, the absolute pressure value is 601 kPa; based on the fact that the amount of nitrogen in the initial and final states remains unchanged, the ideal gas law is used:
[0077] P 氮气1 V 氮气1 =nRT
[0078] Among them, P 氮气1 Where n is the initial nitrogen pressure, n is the amount of substance, R is a constant, and V is the initial nitrogen pressure. 氮气1 Where T is the volume of the gas phase inside the container and K is the temperature. The volume ratio of the gas phase space when the temperature is increased from 20℃ to 80℃ is given by the following formula:
[0079] V 氮气1(20℃) / V 氮气1(80℃) =T 20℃ P 氮气1(80℃) / (T) 80℃ P 氮气1(20℃) )
[0080] According to Dalton's law of partial pressures:
[0081] P 总 =P 乙醇 +P 氮气
[0082] Where: P 总 It is the total pressure, P 乙醇 It is the partial pressure of ethanol, P 氮气It is the partial pressure of nitrogen; P 总20℃ =101 kPa, P 总80℃ =601 kPa, P 乙醇(20℃) ≈5.8kPa, P 乙醇(80℃) ≈116 kPa; Calculate the partial pressure of nitrogen:
[0083] P 氮气1(20℃) =95.2kPa
[0084] P 氮气1(80℃) =485kPa
[0085] Substituting into the formula for the volume ratio of nitrogen gas phase, we obtain the following formula:
[0086] V 氮气1(80℃) = V 氮气1(20℃) 0.2365
[0087] During the heating process from 20℃ to 80℃, the mass of liquid ethanol remains unchanged:
[0088] m 乙醇20℃ =m 乙醇80℃
[0089] Where, m 乙醇20℃ This is the mass of liquid ethanol at 20℃, m 乙醇80℃ This refers to the mass of liquid ethanol at 80℃;
[0090] Right now:
[0091] ρ 80℃ ×(V) 总 - V 氮气1(80℃) )=ρ 20℃ ×(V) 总 - V 氮气1(20℃) )
[0092] Among them, V 总 This refers to the total volume, and the density ρ of ethanol at 20℃. 20℃ The density ρ of ethanol at 80℃ is 0.789. 80℃ It is 0.736;
[0093] We can obtain:
[0094] V 氮气1(20℃) / V 总 =8.60%
[0095] That is: the maximum filling amount is 1-8.60%=91.40%; when the filling amount is increased from 20℃ to 80℃, and the final gauge pressure is set at 500kPa, the maximum allowable filling amount is 91.40%; according to the above method, the filling amount when the final gauge pressure is 500kPa and the temperature reaches 90℃ is 88.77%; considering equipment utilization and equipment safety, the filling amount is set to 60%-80%. The optimal ranges for displacement pressure (0.5MPa-1.0MPa) and displacement temperature (80℃-90℃) are defined to balance the core contradiction between displacement efficiency and operational safety. Setting a lower limit for pressure (≥0.5MPa) and a lower limit for temperature (≥80℃) is based on the consideration of improving the displacement effect, because under moderate heating and pressurization conditions, the solvent diffusion coefficient increases, viscosity decreases, and gel shrinkage stress decreases, thereby effectively enhancing the mass transfer process and shortening the displacement time. Setting an upper limit for pressure (≤1.0MPa) and an upper limit for temperature (≤90℃) addresses the volatile, flammable, and explosive characteristics of ethanol solvent, fundamentally avoiding the risks of overpressure, leakage, and even combustion and explosion caused by a sharp rise in vapor pressure due to excessive temperature and pressure, and strictly controlling the process conditions within the safety boundaries. This limitation defines a clear operating window that is both efficient and safe for the entire displacement process. Based on the ideal gas law and Dalton's law of partial pressures, the maximum filling volume (e.g., 91.40%) and the set filling volume range (60%-80%) are quantitatively calculated and limited to achieve synergistic optimization of equipment safety, solvent utilization, and process reliability. This calculation model comprehensively considers the increase in total system pressure caused by the expansion of liquid ethanol and the changes in the partial pressure of gaseous nitrogen and ethanol vapor during heating. By accurately calculating the maximum allowable space ratio for liquid phase volume expansion at specific final pressures (e.g., 500 kPa gauge pressure) and temperatures (e.g., 80℃, 90℃), the maximum material filling volume within the safe range is derived. This provides a quantitative and preventative safety design criterion to prevent the system pressure from exceeding the safety limit (1.0 MPa) due to overfilling and liquid phase expansion after heating. Setting the actual operating filling volume at 60%-80% is below the theoretical safety upper limit, further reserving a safety margin for unforeseen fluctuations, while also taking into account equipment space utilization and operational convenience, ensuring the inherent safety and stable operation of the process. By elevating core process parameters (pressure, temperature, and filling volume) from qualitative descriptions to quantitative calculations and collaborative constraints, this approach clearly demonstrates how thermodynamic and physicochemical principles can be used to pursue displacement efficiency (by setting lower limits for pressure and temperature) while strictly ensuring process safety (by setting upper limits for pressure and temperature and calculating the maximum filling volume based on safe pressure). The final filling volume setting range of 60%-80% represents an optimized balance point that integrates theoretical safety limits, equipment utilization, and engineering practice margins. This transforms the entire technical solution from a vague concept into a well-defined, logically consistent, safe, controllable, and repeatable industrial process solution.
[0096] In this embodiment, step S402 specifically involves: setting the final temperature to 80°C, the filling amount to 60%, and the final gauge pressure to 500 kPa; the filling amount is based on the ideal gas law:
[0097] P 氮气2 V 氮气2 =nRT
[0098] Among them, P 氮气2 It is the final nitrogen pressure, V 氮气2 It is the final gas volume inside the container;
[0099] Because the container is sealed, the amount of nitrogen gas remains constant, that is:
[0100] P 氮气2(80℃) V 氮气2(80℃) / (RT) 80℃ )= P 氮气2(20℃) V 氮气2(20℃) / (RT) 20℃ )
[0101] Calculate V based on the ethanol expansion coefficient. 氮气2(20℃) and V 氮气2(80℃) and V 总 Ratio:
[0102] V 氮气2(20℃) ×(1+△T×γ (20~80℃) )=V 氮气2(80℃)
[0103] Where, γ (20~80℃) The coefficient of thermal expansion of ethanol at 20–80°C is 1.1 × 10⁻⁶. -3 ℃ -1 , T is the temperature change; since the filling amount is 60%, that is:
[0104] V 氮气2(20℃) =40%V tank
[0105] V 氮气2(80℃) =37.5%V tank
[0106] Among them, V tank It is the total capacity;
[0107] We can obtain:
[0108] P 氮气2(20℃) =377kPa
[0109] Calculated using the above method, the final gauge pressure is 0.5-1.0 MPa, the final temperature is 80-90℃, and the filling volume is 60-80%. This provides specific, quantified process parameters and a safe operating window, elevating process control from experience-based operation to precise engineering control. By limiting the final displacement gauge pressure to 0.5-1.0 MPa, the final temperature to 80-90℃, and the filling volume to 60-80%, an optimized and safe operating range is established for the entire displacement process. This range ensures sufficient kinetic driving force for the displacement process to improve efficiency at the lower limits of pressure and temperature, while its upper limits directly avoid safety risks such as equipment overpressure, excessive solvent evaporation, and even combustion and explosion caused by excessive pressure or temperature, providing clear boundary conditions for the safe and stable operation of the process. Based on the ideal gas law and the principle of thermal expansion of liquids, a specific calculation method for pre-charge inert gas pressure is provided, realizing the scientific, precise, and predictable setting of initial process conditions. This calculation model comprehensively considers two aspects of changes caused by temperature rise in a closed system: first, the liquid solvent (ethanol) expands due to heat and occupies more volume, thereby compressing the initial space of the inert gas (nitrogen); second, the gas pressure change caused by the temperature rise itself. Through the given formula, the required initial pre-charge nitrogen pressure (such as 377 kPa in the example) can be accurately calculated under the set final temperature, filling amount, and final pressure target. This transforms the process of establishing an inert environment before replacement from a step that requires repeated adjustments into a precisely set and controllable operation that can be completed in one go, ensuring the consistency of the initial state of each process. This is the key to process repeatability and predictable results. The calculations reveal the intrinsic correlations and constraints among key parameters (filling volume, temperature, and pressure), providing a theoretical basis and quantitative tools for process optimization and safety design. The calculation method clearly shows that the maximum safe filling volume is not a fixed value, but is strongly correlated with the set final temperature and the allowable final pressure. This guides operators to calculate the maximum allowable filling volume in reverse, based on the actual equipment's safe pressure threshold and the desired process temperature, thereby maximizing single-batch throughput and solvent utilization without sacrificing safety margins. This quantitative correlation based on physical principles enables process design to combine flexibility, economy, and inherent safety. The key control parameters (filling volume, temperature, and pressure) of the entire replacement process are transformed from an empirically defined range into a closed-loop system based on physical principles that can be precisely calculated and predicted. This not only provides specific parameter ranges to ensure the safe and efficient operation of the process, but also offers a scientific method that enables operators to accurately set the initial state of the process based on specific conditions (such as container pressure resistance and target temperature) and understand the interactions between parameters. This enhances the feasibility, controllability, and licensability of the technical solution, demonstrating a rigorous engineering transformation from technical conception to reliable industrial application.
[0110] The relationship between the design specifications of the replacement pressure vessel and the pre-charge nitrogen pressure is shown in Table 1:
[0111]
[0112] According to the table above, the initial pre-charge nitrogen pressure should be between 276 kPa and 465 kPa, which meets the required specifications.
[0113] The advantages of this process design lie in its balance of efficiency, safety, and controllability. First, by optimizing the filling rate to 60-80%, processing efficiency is ensured while providing ample safety space for material expansion. Second, the process conditions are scientifically set: pre-charging with nitrogen at 276-465 kPa at room temperature reduces energy consumption and operational complexity; the displacement temperature is precisely controlled at 80-90℃, a range that effectively drives the displacement reaction and prevents excessive material volatilization or decomposition. Finally, the displacement container integrates multiple safety mechanisms, ensuring inherent safety throughout the entire operation under direct monitoring.
[0114] In practice, an alcohol displacement container for aerogels and their composites is provided, specifically a low-pressure displacement container that can significantly improve the displacement efficiency of aerogel products and reduce the amount of displacement solvent used. The displacement container includes: a sealed cavity 2, with an inert gas filling port 6 on the sealed cavity, through which inert gas is filled to maintain a certain pressure inside the cavity; a breather valve 5 and a pressure display 7 are used to monitor the pressure inside the container and maintain the overall safety performance; a heating and cooling unit 9 and the sealed cavity 2 are connected by an external heating coil 10, and a temperature display 11 is used to monitor and control the temperature of the displacement medium inside the container; a magnetic coupling stirring system 3 increases the disturbance of the medium, increases the contact between the displacement medium and the product surface, and improves the displacement efficiency; the sealed cavity is also equipped with a movable shelf 4, which can be assembled according to the size and specifications of the product to be replaced, improving the space utilization of the container and reducing the consumption of the displacement medium; an alcohol displacement solvent (with added desiccant) is added through the inlet and outlet (inlet / outlet assembly 8) to facilitate the replacement of the displacement medium, improve the displacement effect, and reduce the cost of the alcohol displacement solvent.
[0115] The container is covered with an overall insulation layer to maintain the temperature stability of the replacement solution and the sample to be replaced in different environments; the container is connected to an external temperature display to monitor the temperature changes of the replacement solution inside the container in real time; the container is connected to an external integrated heating and cooling unit, which is connected to the heating and cooling coils at the bottom of the container, and can adjust the temperature of the replacement solution inside the container according to the temperature value required for the replacement process to achieve a constant temperature state.
[0116] A magnetic coupling stirring system 3 is installed on the outer walls of the left and right sides of the cavity. The stirring paddle drives the magnetic coupler to rotate through an explosion-proof motor. The motor is connected to an external electrical control cabinet to adjust the speed and the direction of disturbance flow. By adjusting the speed and controlling the direction of disturbance flow, the disturbance effect is increased, thereby improving the diffusion efficiency of the solvent and thus improving the displacement efficiency.
[0117] The magnetically coupled stirring system 3 inside the container reverses its stirring direction every 2 hours to improve the agitation effect and avoid situations where there is no replacement fluid or poor agitation in local areas during unidirectional circulation. Furthermore, the container has a removable shelf 4 with a vertical spacing of 100mm, which can selectively hold products to be replaced according to their different shapes and thicknesses to maximize the use of container space.
[0118] By adding 1% desiccant to the alcohol replacement medium through the inlet / outlet liquid assembly 8 and subjecting it to uniform agitation, the replacement efficiency can be further improved.
[0119] After each round of replacement is completed, add 5% of the desiccant to the bottom of the container, stir for 1-2 hours, and let stand for 10 minutes. The replacement solvent can be reused, improving the utilization rate of the replacement solvent and significantly reducing costs.
[0120] Furthermore, the breather valve 5 in the safety accessories can quickly vent the gas in the container, reducing the risk of excessive pressure inside the container; the magnetically coupled stirring system 3 can control the safety of the circuit.
[0121] The present invention has the following beneficial effects:
[0122] 1. This invention significantly enhances the molecular motion rate during the displacement process by adding a water-absorbing agent and introducing the synergistic effects of heating, pressurization, and stirring, thereby greatly improving the displacement efficiency. Compared with the 14-30 day cycle required by traditional processes, this technology can shorten the displacement cycle to 2-3 days;
[0123] 2. This invention employs low-pressure and relatively low-temperature reaction conditions, combined with a magnetically coupled stirring system 3, a highly sealed container, a container breather valve 5, and a temperature and pressure display device, which comprehensively improves the safety control level of the replacement process and effectively prevents potential risks caused by the flammable, explosive, and volatile properties of the replacement solvent.
[0124] 3. This invention optimizes reaction conditions and process flow, significantly improving container space utilization and greatly reducing the amount of displacement solvent used. Specifically, the amount of displacement solvent used is reduced from 15-30 times the original product weight to 3-5 times; the container space utilization rate is increased from 20-40% to 60-80%.
[0125] A method for alcohol replacement of aerogels and their composites is provided, comprising: a. opening the cover plate 1 to the limiting device; b. placing the product into the rack 4 according to the product size and fixing it in the U-shaped groove on the inner wall; stacking the rack 4 layer by layer, one layer of product at a time, until the product placement is complete; c. calculating the required total mass of alcohol and drawing the alcohol into the inlet (flowing along the inner wall of the cavity), taking care not to aim the flowing liquid directly at the product to avoid damage; d. closing the cover plate 1, tightening the locking bolts, and checking the airtightness of the container; e. stirring with the magnetically coupled stirring system 3, observing through the observation window. f. Observe whether the stirring effect is good and whether it will cause damage to the product; h. Set the parameters of the integrated heating and cooling machine 9, turn on the integrated heating and cooling machine 9 to heat the container, and at the same time observe the temperature display 11 and pressure display 7. The temperature and pressure should be within the normal and safe range; g. Check the state inside the container through the observation window at the specified time; h. Replace the alcohol in the container at the specified time, turn off the integrated heating and cooling machine 9, and after the temperature drops to room temperature, turn off the magnetic coupling stirring system 3, open the liquid outlet, and drain the alcohol in the container completely. Repeat the cef step. After the replacement process is completed, turn off the integrated heating and cooling machine 9 and the magnetic coupling stirring system 3 in sequence, and check the temperature display 11 and pressure display 7. Under the condition of ensuring safety, take out the top layer of product and the top shelf 4 in the container, the second layer of product and the second shelf 4, and so on, until all the products are taken out. Then drain the alcohol in the container through the liquid outlet.
[0126] Based on the above method, the pressure during the replacement process is solidified and monitored within a specified range by a sealed cavity 2, an inert gas filling port 6, and a pressure display instrument 7; the temperature of the alcohol is controlled by a heating and cooling unit 9 and a temperature display instrument 11; the replacement effect is accelerated by a magnetically coupled stirring system 3; and the filling amount of insulation materials of different thicknesses and sizes is optimized by a shelf 4. A comparison of the replacement process of this invention with the traditional replacement process is shown in Table 2.
[0127]
[0128] The table above, through specific data comparison, intuitively demonstrates the multidimensional and significant advantages of the replacement process of this invention compared to traditional replacement processes: In terms of single-batch processing capacity, the maximum replacement sample mass increases from 50 kg to 200 kg, resulting in a substantial improvement in processing efficiency; in terms of process cycle, the replacement time is shortened from 14-30 days to 2-3 days, demonstrating a highly significant efficiency improvement; in terms of resource consumption, the amount of replacement solvent used is reduced from 750-1500 kg to 600-1000 kg, resulting in greater resource conservation; and in terms of equipment efficiency, the replacement container capacity required to achieve the same or even higher processing volumes is reduced from 500-700 L to 300-400 L, resulting in higher equipment space utilization. In summary, the data in Table 2 comprehensively demonstrate that this invention has achieved comprehensive and outstanding technological progress in improving processing efficiency, shortening the production cycle, reducing raw material consumption, and optimizing equipment utilization.
[0129] Matters not covered in this invention are common knowledge.
[0130] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0131] The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.
[0132] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. An alcohol displacement container for aerogels and aerogel composite materials, characterized in that, include: A sealed cavity (2) having an upper opening and a cover plate (1) sealing the upper opening, for providing a sealed cavity; The placement assembly is inserted into the inner cavity of the sealed cavity (2) through the top opening, and is used to place the material in layers in the inner cavity of the sealed cavity (2); The inlet / outlet liquid assembly (8) is arranged on the sealed cavity (2) and is used to inject alcohol replacement solvent or alcohol replacement solvent and desiccant along the inner wall of the sealed cavity (2) and drain the liquid from the bottom of the sealed cavity (2); The magnetic coupling stirring system (3) is arranged on the side of the sealed cavity (2) and arranged in a relatively grouped manner. It is used to achieve a completely sealed stirring process by transmitting torque through magnetic non-contact. The stirring effect is increased by adjusting the speed and controlling the turbulence flow direction, thereby improving the solvent diffusion efficiency and thus improving the displacement efficiency. An environmental control system is used to provide and maintain a low-temperature, low-pressure, inert gas environment for alcohol displacement of materials; To ensure effective replacement, the replacement pressure is set to ≥0.5MPa. For safety reasons, since the replacement solvent ethanol is volatile, flammable, and explosive, the set pressure is ≤1.0MPa, meaning the replacement pressure should be controlled between 0.5MPa and 1MPa. To ensure effective replacement, the replacement temperature is set to ≥80℃. For safety reasons, since the replacement solvent ethanol is volatile, flammable, and explosive, the set temperature is ≤90℃, meaning the replacement temperature is controlled between 80 and 90℃. The material filling rate is set at 60%-80%.
2. The alcohol displacement container for aerogels and aerogel composite materials according to claim 1, characterized in that, The magnetic coupling stirring system (3) includes a stirring paddle, an explosion-proof motor, a magnetic coupler, and an electrical control cabinet; The magnetic coupler is driven to rotate by an explosion-proof motor, which in turn drives the agitator to rotate. The explosion-proof motor is connected to an external electrical control cabinet. The speed and disturbance flow direction are adjusted through the electrical control cabinet. By adjusting the speed and controlling the disturbance flow direction, the disturbance effect is increased, thereby improving the diffusion efficiency of the solvent and enhancing the displacement efficiency.
3. The alcohol displacement container for aerogels and aerogel composite materials according to claim 1, characterized in that, The environmental control system includes: Temperature environment control system, used to maintain a constant low temperature environment inside the sealed cavity (2); A gas environment control system is used to maintain a constant low-pressure inert gas environment within a sealed cavity (2).
4. The alcohol displacement container for aerogels and aerogel composite materials according to claim 3, characterized in that, The temperature environment control system includes an integral insulation layer laid outside the sealed cavity (2); The temperature environment control system also includes a heating and cooling unit (9) and a temperature display (11). The heating and cooling unit (9) is connected to the sealed cavity (2) through an external heating coil (10) to heat the cavity inside the sealed cavity (2). The temperature display (11) is installed inside the sealed cavity (2) to monitor the temperature. The heating and cooling unit (9) is electrically connected to the temperature display (11). The temperature display (11) monitors and feeds back the temperature signal of the cavity inside the sealed cavity (2) to the heating and cooling unit (9) in real time. The control unit inside the heating and cooling unit (9) compares the temperature signal with the preset target temperature value and then automatically adjusts the output power to heat or cool. Finally, the sealed cavity (2) is continuously heated or cooled through the external coil to achieve control of the cavity temperature.
5. The alcohol displacement container for aerogels and aerogel composite materials according to claim 3, characterized in that, The gas environment control system includes an inert gas filling port (6), a pressure display (7), and a breathing valve (5) installed in a sealed cavity (2). Inert gas is introduced through the air inlet to maintain a preset pressure in the sealed cavity (2), and the pressure is monitored in real time by the pressure display instrument (7); The pressure inside the sealed cavity (2) is kept stable by the breather valve (5) to prevent damage to the sealed cavity (2) due to pressure fluctuations, and to reduce the evaporation loss of alcohol replacement solvent and external pollution.
6. The alcohol displacement container for aerogels and aerogel composites according to any one of claims 1 to 5, characterized in that, The longitudinal section of the inner cavity of the sealed cavity (2) is circular, elliptical or capsule-shaped; The liquid inlet and outlet assembly (8) includes an inlet and an outlet. The inlet is located in the arc area of the sealed cavity (2) so that the reagent injected through the inlet flows along the arc surface. The outlet is located at the bottom of the sealed cavity (2).
7. An alcohol displacement container for aerogels and aerogel composites according to any one of claims 1 to 5, characterized in that, The storage assembly includes multiple shelves (4), which are detachably installed in the inner cavity of the sealed cavity (2). The shelves (4) are assembled according to the size specifications of the material to be replaced, ensuring that the material is placed in layers of shelves (4) to improve the utilization of container space and reduce the consumption of replacement media.
8. A method for alcohol substitution in aerogels and aerogel composites, characterized in that, The alcohol replacement container using the aerogel and aerogel composite material as described in claim 1 has an environmental control system including a temperature environment control system and a gas environment control system. The temperature environment control system includes a heating and cooling unit (9) and a temperature display (11). The heating and cooling unit (9) is connected to the sealed cavity (2) via an external heating coil (10) to heat the inner cavity of the sealed cavity (2). The temperature display (11) is installed in the inner cavity of the sealed cavity (2) to monitor the temperature. The gas environment control system includes a breathing valve (5) and a pressure display (7). The breathing valve (5) maintains the pressure inside the sealed cavity (2) and inert gas is introduced through the air inlet to maintain the preset pressure inside the sealed cavity (2). The pressure display (7) monitors the pressure in real time. The storage component includes multiple shelves (4), which are detachably installed in the inner cavity of the sealed cavity (2). The system includes the following steps: S100. Open the cover (1), load the bottom shelf (4) according to the material size and place the material, and add the material layer by layer according to the shelf (4) and the material layer by layer until the material is placed. S200. Calculate the total mass of alcohol replacement solvent required based on the material filling amount; S300: Inject alcohol replacement solvent into the inlet and allow it to flow slowly along the inner wall to avoid direct impact of the alcohol replacement solvent on the material and causing damage to the material. S400, close the cover (1) and check the airtightness of the sealed cavity (2), while injecting inert gas to the preset pressure; S500, start the magnetic coupling stirring system (3) to stir, observe the stirring effect through the observation window and ensure that the material is not damaged; S600, set the parameters of the integrated cooling and heating unit (9), turn on the integrated cooling and heating unit (9) to heat the sealed cavity (2), and at the same time observe the temperature display (11) and pressure display (7) to ensure that the temperature and pressure are within the normal and safe range; S700. Check the state inside the sealed cavity (2) through the observation window at preset time intervals; S800. Replace the alcohol replacement solvent in the sealed cavity (2) according to the preset time interval; S900, repeat steps S200 to S800 until the replacement process is completed. In sequence, turn off the integrated heating and cooling machine (9) and the magnetic coupling stirring system (3), and check the temperature display (11) and pressure display (7). Ensure that it is safe to open the cover plate (1), and take out the top layer of products and the top layer of shelves (4) from top to bottom. Continue in this manner until all products are taken out. Then drain the alcohol replacement solvent in the sealed cavity (2) through the outlet. The material filling rate is set at 60%-80%.
9. The method for alcohol replacement of aerogels and aerogel composites according to claim 8, characterized in that, In step S800, the alcohol replacement solvent in the sealed cavity (2) is replaced, specifically as follows: S801, Turn off the integrated cooling and heating unit (9); S802. After the temperature drops to room temperature, turn off the magnetic coupling stirring system (3). S803. Open the outlet to drain the alcohol replacement solvent from the sealed chamber (2); S804. Inject the alcohol replacement solvent into the inlet to the preset amount, and allow the alcohol replacement solvent to flow slowly along the inner wall surface.
10. The method for alcohol replacement of aerogels and aerogel composites according to claim 8 or 9, characterized in that, After step S300, add the following step: add 1% desiccant to the alcohol replacement solvent through the inlet and agitate it at a constant speed using a magnetically coupled stirring system (3) to improve the replacement efficiency; and / or Add a step after step S800: When or after the alcohol replacement solvent is discharged, add 5% of the dosage of desiccant to the alcohol replacement solvent, keep stirring for 1-2 hours and let stand for 10 minutes to achieve the reuse of the alcohol replacement solvent.
11. The method for alcohol replacement of aerogels and aerogel composites according to claim 8 or 9, characterized in that, In step S400, an inert gas inlet is connected to the sealed cavity (2), and inert gas is filled in according to the preset settings of the pressure display (7) and the breathing valve (5), so that the sealed cavity (2) is kept at a constant pressure and reaches the initial pressure index value required for replacement. The initial pressure index value is obtained as follows: S401, Calculation of material filling amount: In order to increase the material filling amount and improve the utilization rate of alcohol replacement solvent, ethanol is used as the alcohol representative for calculation. The sealed cavity (2) is equipped with a movable shelf (4), and the minimum filling amount is set to 60%. Step S401 is as follows: Considering the replacement effect, the replacement pressure is set to ≥0.5MPa to ensure the replacement effect; From a safety perspective, the replacement solvent ethanol is a volatile, flammable and explosive substance, and the set pressure value is ≤1.0MPa, that is, the replacement pressure should be controlled between 0.5MPa and 1MPa; Considering the displacement effect, the displacement temperature is set to ≥80℃ to ensure the displacement effect; From a safety perspective, the replacement solvent ethanol is a volatile, flammable and explosive substance, and the set temperature value is ≤90℃, that is, the replacement temperature is controlled at 80~90℃; The maximum filling capacity of the equipment is calculated and designed based on the pressure and temperature setting range. At 20℃, the initial gauge pressure is zero, which is an absolute pressure of 101 kPa. When the temperature reaches 80℃, the final gauge pressure is set to 500 kPa, which is an absolute pressure of 601 kPa. Based on the fact that the amount of nitrogen remains constant in both the initial and final states, we apply the ideal gas law: P 氮气1 V 氮气1 =nRT Among them, P 氮气1 Where n is the initial nitrogen pressure, n is the amount of substance, R is a constant, and V is the initial nitrogen pressure. 氮气1 It is the volume of the gas phase inside the container; T is the temperature value, in K. When the temperature is increased from 20℃ to 80℃, the volume ratio of the gas phase space is given by the following formula: V 氮气1(20℃) / V 氮气1(80℃) =T 20℃ P 氮气1(80℃) / (T 80℃ P 氮气1(20℃) ) According to Dalton's law of partial pressures: P 总 =P 乙醇 +P 氮气 Where: P 总 It is the total pressure, P 乙醇 It is the partial pressure of ethanol, P 氮气 It is the partial pressure of nitrogen; P 总20℃ =101 kPa,P 总80℃ =601 kPa,P 乙醇(20℃) ≈5.8kPa,P 乙醇(80℃) ≈116kPa: Calculate the partial pressure of nitrogen: P 氮气1(20℃) =95.2kPa P 氮气1(80℃) =485kPa Substituting into the formula for the volume ratio of nitrogen gas phase, we obtain the following formula: V 氮气1(80℃) = V 氮气1(20℃) 0.2365 During the heating process from 20℃ to 80℃, the mass of liquid ethanol remains unchanged: m 乙醇20℃ =m 乙醇80℃ Where, m 乙醇20℃ This is the mass of liquid ethanol at 20℃, m 乙醇80℃ This refers to the mass of liquid ethanol at 80℃; Right now: ρ 80℃ ×(V 总 - V 氮气1(80℃) )=ρ 20℃ ×(V 总 - V 氮气1(20℃) ) Among them, V 总 This refers to the total volume, and the density ρ of ethanol at 20℃. 20℃ The density ρ of ethanol at 80℃ is 0.
789. 80℃ It is 0.736; We can obtain: V 氮气1(20℃) / V 总 =8.60% That is, the maximum filling amount is 1 - 8.60% = 91.40%; When the filling temperature is increased from 20℃ to 80℃, and the final gauge pressure is set at 500kPa, the maximum allowable filling rate is 91.40%. The filling rate calculated using the above method is 88.77% when the final gauge pressure is 500 kPa and the temperature reaches 90°C. Considering both equipment utilization and safety, the filling rate is set at 60%-80%. S402, Calculation of inert gas pressure: In order to maintain the pressure inside the alcohol replacement container at the preset pressure value, a certain amount of inert gas needs to be pre-charged. The pre-charge nitrogen pressure is calculated and designed based on the pressure and temperature setting range. Step S402 is as follows: The final temperature is set at 80℃, the filling rate at 60%, and the final gauge pressure at 500 kPa; the filling rate is based on the ideal gas law. P 氮气2 V 氮气2 =nRT Among them, P 氮气2 It is the final nitrogen pressure, V 氮气2 It is the final gas volume inside the container; Because the container is sealed, the amount of nitrogen gas remains constant, that is: P 氮气2(80℃) V 氮气2(80℃) / (RT 80℃ )=P 氮气2(20℃) V 氮气2(20℃) / (RT 20℃ ) Calculate V based on the ethanol expansion coefficient. 氮气2(20℃) and V 氮气2(80℃) and V 总 Ratio: V 氮气2(20℃) ×(1+△T×γ (20~80℃) )=V 氮气2(80℃) Where, γ (20~80℃) The coefficient of thermal expansion of ethanol at 20–80°C is 1.1 × 10⁻⁶. -3 ℃ -1 △T is the temperature change; since the filling amount is 60%, that is: V 氮气2(20℃) =40%V tank V 氮气2(80℃) =37.5%V tank Among them, V tank It is the total capacity; We can obtain: P 氮气2(20℃) =377kPa Calculated using the above method, the final gauge pressure is 0.5-1.0 MPa, the final temperature is 80-90℃, and the filling rate is 60-80%.