High-efficiency hydrogen purification device and method suitable for ultrahigh-temperature working condition

Abstract

The invention discloses an efficient hydrogen purification device suitable for an ultra-high-temperature working condition. The efficient hydrogen purification device comprises a pressure-bearing shell; the Getter material bed layer is arranged in the pressure bearing shell; the heating system is used for heating the Getter material bed layer, and the heating system is configured to maintain the operation temperature of the Getter material bed layer at 600 DEG C + / -10 DEG C; the invention further discloses an efficient hydrogen purification method suitable for the ultrahigh-temperature working condition. According to the invention, high-efficiency purification of hydrogen under high-temperature and high-pressure conditions is realized, the impurity content is obviously reduced, the service life of the device is prolonged, and reliable technical support is provided for industrial hydrogen purification.

Description

Technical Field

[0001] This invention relates to the field of information technology, and in particular to a high-efficiency hydrogen purification device suitable for ultra-high temperature operating conditions. Background Technology

[0002] In industrial production and the energy sector, hydrogen, as a clean and efficient energy carrier, has irreplaceable value, especially in applications under high temperature and high pressure environments, where the purity of hydrogen directly affects the system's operational efficiency and safety. However, current technologies for purifying hydrogen under high-temperature conditions still face many challenges and urgently need breakthroughs to meet industrial demands.

[0003] Existing hydrogen purification methods often exhibit significant shortcomings under high-temperature conditions. Many traditional solutions struggle to adapt to extreme environments in terms of material selection and process design, leading to equipment susceptibility to corrosion, poor purification efficiency, and even threats to system operational stability. Particularly during long-term operation, material surfaces are prone to degradation, gradually reducing impurity removal capabilities. This not only increases maintenance costs but also limits the technology's application in a wider range of scenarios.

[0004] A deeper challenge lies in effectively controlling the complex reactions between materials and hydrogen under high temperature and pressure conditions, which is a core technical hurdle. Particularly concerning is the crucial factor of material surface condition. Without a stable protective mechanism, materials can be corroded upon contact with hydrogen, potentially triggering unnecessary side reactions such as generating other gaseous impurities that contaminate hydrogen purity. For instance, in some industrial settings, the inner wall material of purification devices gradually deteriorates after prolonged exposure to hydrogen at high temperatures. This not only shortens equipment lifespan but also makes it difficult to effectively adsorb impurities, significantly reducing purification efficiency. More specifically, in some high-temperature reactors, if the material surface is not specially treated, micro-cracks may appear in the early stages of operation. These cracks expand over time, ultimately causing the entire purification process to fail.

[0005] Therefore, how to effectively suppress corrosion and side reactions by optimizing the surface state of materials under high temperature and high pressure conditions, while ensuring the efficient removal of impurities, has become a key problem that urgently needs to be solved in the field of hydrogen purification. Summary of the Invention

[0006] This invention provides a high-efficiency hydrogen purification device suitable for ultra-high temperature operating conditions, mainly comprising: A pressure-bearing housing; a Getter material bed disposed within the pressure-bearing housing; and a heating system configured to maintain the operating temperature of the Getter material bed at 600℃±10℃.

[0007] Further, the process includes: passing the raw hydrogen gas to be purified through a bed containing getter material; reacting the raw hydrogen gas with the getter material at a temperature of 600℃±10℃ to remove impurity gases from the raw hydrogen gas; evacuating the system before introducing the raw hydrogen gas, and then, under an inert atmosphere or a high-purity hydrogen atmosphere, heating the system to 600℃ and holding it at that temperature for a period of time to activate the getter material and stabilize its surface state.

[0008] Furthermore, the pressure-bearing shell includes: the pressure-bearing shell is made of a high-chromium-nickel alloy material; the inner surface of the pressure-bearing shell is electropolished; after the electropolishing treatment, the inner surface is subjected to high-temperature oxidation pretreatment to form a dense Cr2O3 protective film or Al2O3 protective film; the Cr2O3 protective film or the Al2O3 protective film covers the inner surface, and the inner surface forms an enclosing structure for the Getter material bed.

[0009] Furthermore, the Getter material bed includes: the Getter material is a zirconium-vanadium-iron alloy or a zirconium-iron alloy; the zirconium-vanadium-iron alloy or the zirconium-iron alloy is filled into the pressure-bearing shell to form the Getter material bed; the Getter material bed is in contact with the heating system, and the heating system heats the zirconium-vanadium-iron alloy or the zirconium-iron alloy to 600℃±10℃.

[0010] Furthermore, the heating system includes: the heating system is disposed outside the pressure-bearing shell to conduct heat to the Getter material bed; the heating system monitors the operating temperature of the Getter material bed; the heating system adjusts the heating power according to the operating temperature to maintain the operating temperature within the range of 600℃±10℃.

[0011] Furthermore, the system vacuuming process includes: evacuating the pressure-bearing shell and the Getter material bed; after vacuuming, introducing high-purity nitrogen to replace the gas inside the pressure-bearing shell; after the high-purity nitrogen replacement, programmatically heating the heating system to 600°C; after programmatically heating to 600°C, introducing high-purity hydrogen to activate the Getter material bed; and maintaining the temperature for a period of time during the activation process to stabilize the surface state of the zirconium-vanadium-iron alloy or the zirconium-iron alloy.

[0012] Furthermore, the raw material hydrogen passes through a bed of Getter material, including: the raw material hydrogen entering the pressure-bearing shell; the raw material hydrogen flowing through the Getter material bed; the Getter material bed being maintained at 600℃±10℃ under the action of the heating system; the raw material hydrogen contacting the zirconium-vanadium-iron alloy or the zirconium-iron alloy; after the contact reaction, the purified hydrogen flowing out from the pressure-bearing shell.

[0013] Furthermore, the electropolishing process includes: electropolishing the inner surface; cleaning the inner surface after electropolishing; drying the inner surface after cleaning; and performing the high-temperature oxidation pretreatment after drying.

[0014] The technical solutions provided by the embodiments of the present invention may include the following beneficial effects: This invention discloses a high-efficiency hydrogen purification device and method suitable for ultra-high temperature operating conditions. Addressing the challenges of material corrosion, low impurity removal efficiency, and insufficient system stability during hydrogen purification under high-temperature environments, this invention achieves a fusion solution of high-efficiency purification and long-term stable operation through innovative design. The invention uses a high-chromium-nickel alloy to construct the pressure-bearing shell, and forms a dense protective film through electropolishing and high-temperature oxidation pretreatment, effectively inhibiting hydrogen corrosion and methane generation. Simultaneously, a specific zirconium alloy is selected as the getter material, exhibiting excellent impurity adsorption and methane cracking capabilities under precisely controlled operating temperatures. Furthermore, this invention ensures the surface stability of the getter material through vacuuming, inert atmosphere replacement, and programmed temperature activation steps, thereby improving purification efficiency. Ultimately, this invention achieves high-efficiency hydrogen purification under high temperature and high pressure conditions, significantly reducing impurity content and extending the device's service life, providing reliable technical support for industrial hydrogen purification. Attached Figure Description

[0015] Figure 1 This is a flowchart of a high-efficiency hydrogen purification device suitable for ultra-high temperature conditions according to the present invention. Detailed Implementation

[0016] To further understand the content of this invention, a detailed description of the invention is provided in conjunction with the accompanying drawings and embodiments. The specific embodiments described herein are for illustrative purposes only and are not intended to limit the invention. It should also be noted that, for ease of description, only the parts relevant to the invention are shown in the accompanying drawings.

[0017] like Figure 1 This embodiment of a high-efficiency hydrogen purification device suitable for ultra-high temperature operating conditions may specifically include: S1, a high-efficiency hydrogen purification device suitable for ultra-high temperature conditions, comprising a pressure-bearing shell, a Getter material bed disposed within the pressure-bearing shell, and a heating system for heating the Getter material bed, characterized in that the heating system is configured to maintain the operating temperature of the Getter material bed at 600℃±10℃.

[0018] To address the heating requirements of a high-efficiency hydrogen purification device suitable for ultra-high temperature conditions, a precisely temperature-controlled heating component is configured. This component is tightly integrated with a Getter material bed within a pressure-bearing shell, ensuring uniform heat transfer to the bed and stabilizing its temperature within a preset range. Real-time temperature data is acquired from the heating component and compared with the preset temperature range to determine if heating power adjustment is necessary. If the temperature deviates from the target value, the heating component power is dynamically adjusted to maintain stable operating temperature of the Getter material bed. Based on the power adjustment of the heating component, the temperature distribution of the Getter material bed is continuously monitored. For areas with uneven temperature distribution, the heat conduction path is adjusted to ensure uniformity of the temperature field across the entire bed. Feedback information from the temperature distribution is used to optimize the operating parameters of the heating component. To address potential heat loss under high-temperature conditions, insulation measures are implemented to further ensure the temperature stability of the Getter material bed during high-temperature hydrogen purification.

[0019] For example, the generation steps are as follows: 1. For example, when configuring a heating component in a high-efficiency hydrogen purification device suitable for ultra-high temperature conditions, a resistance wire wound heater can be used as a component for precise temperature control. It is uniformly wrapped around the outside of the pressure-bearing shell and tightly bonded to the Getter material bed through a heat-conducting medium. This allows heat to penetrate evenly from the shell wall into the bed interior, avoiding the formation of hot spots, thereby maintaining the bed temperature within a preset range and improving the efficiency of hydrogen purification and the effect of impurity removal. 2. In one possible implementation, real-time temperature data from the heating element can be obtained through embedded thermocouple sensors. These sensors are distributed at different locations in the bed to collect data, which is then compared with a preset temperature range, such as 600 degrees Celsius ± 10 degrees Celsius. If the temperature is detected to be too low, the power input is increased to rapidly raise the temperature. This helps to correct deviations in a timely manner and maintain the stability of the operating temperature, thereby ensuring that the Getter material's catalytic activity for the cracking of impurities such as methane is fully utilized at high temperatures, which is beneficial for obtaining hydrogen products with higher purity. 3. Specifically, based on the power adjustment of the heating components, the temperature distribution is continuously monitored. Infrared thermal imaging technology can be used to scan the bed cross-section. For local temperature unevenness, such as overcooling in the edge areas, the heat conduction path can be optimized by adjusting the position of the internal heat-conducting fins. This can balance the consistency of the temperature field, reduce material stress caused by thermal gradients, and help extend the service life of the device and ensure the continuity of the purification process. 4. In one possible implementation, when optimizing the operating parameters of the heating component after obtaining feedback information from the temperature distribution, PID control logic can be introduced to fine-tune the power output. Simultaneously, to address heat loss under high-temperature conditions, a ceramic fiber insulation layer is used to wrap the exterior of the shell. This effectively reduces heat loss, further ensuring the temperature stability of the Getter material bed during hydrogen purification, which is beneficial for achieving the ultimate removal of difficult-to-remove impurities such as methane, and improving overall purification performance.

[0020] S2, the pressure-bearing shell is made of high-chromium-nickel alloy material, and its inner surface is pretreated by electropolishing and high-temperature oxidation to form a dense protective film.

[0021] For the material selection of the pressure-bearing shell, a high-chromium-nickel alloy is chosen to construct the shell, adapting to the operational requirements under high temperature and high pressure environments while ensuring sufficient corrosion resistance, thus completing the initial material construction. After the material construction is completed, the inner surface of the pressure-bearing shell is electropolished to remove minor surface defects and impurities, forming a smooth inner surface, laying the foundation for the subsequent formation of the protective film. After the inner surface smoothing is completed, the pressure-bearing shell undergoes a high-temperature oxidation pretreatment. By controlling the heating conditions, a dense oxide protective film is formed on the inner surface. This protective film effectively isolates the shell from external environmental corrosion, enhancing durability. After the protective film is formed, the inner surface of the pressure-bearing shell is inspected to ensure that the uniformity and density of the protective film meet preset standards, thereby ensuring the stable operation of the pressure-bearing shell under high-temperature environments and meeting the material protection requirements of the hydrogen purification device.

[0022] For example, the generation steps are as follows: 1. For example, when using high-chromium-nickel alloy materials to make pressure-bearing shells, 310S stainless steel can be selected as the specific material. This alloy contains a high proportion of chromium and nickel elements, which can maintain structural integrity under high temperature and high pressure environments and help prevent embrittlement caused by hydrogen permeation. This can improve the overall life of the shell and reduce the frequency of maintenance.

[0023] In one possible implementation, the material is formed into a shell shape using a precision casting process, ensuring a uniform wall thickness distribution, thereby providing a stable substrate for subsequent surface treatment. This method supports the reliability of the device in the hydrogen purification process from the perspective of material durability.

[0024] 2. In one possible implementation, when electropolishing the inner surface of the pressure-bearing shell, an electrolyte is used for immersion and an electric current is applied to uniformly dissolve the surface metal atoms, removing minute defects and impurities and forming a mirror-like smooth inner surface. This treatment is beneficial for reducing surface roughness, thereby reducing impurity adhesion points and effectively preventing localized corrosion in a hydrogen environment.

[0025] For example, in a hydrogen purification device, such a smooth surface can optimize gas flow and create ideal conditions for high-temperature oxidation pretreatment, supporting the uniform formation of a protective film and enhancing the sealing performance of the device from a surface optimization perspective.

[0026] 3. For example, during the high-temperature oxidation pretreatment, the pressure shell is placed in a temperature-controlled furnace and gradually heated to a preset high temperature while an oxygen atmosphere is introduced, so that the chromium or aluminum elements on the inner surface are oxidized to form a dense Cr2O3 or Al2O3 protective film. This film is uniform and dense in thickness, which can prevent hydrogen molecules from penetrating the matrix material and is beneficial to inhibiting methane generation and hydrogen corrosion reaction.

[0027] In one possible implementation, the quality of the membrane is controlled by monitoring the oxidation time and temperature gradient, thereby ensuring the continuity and adhesion of the membrane. From the perspective of protection mechanism, this supports the stable operation of the housing under ultra-high temperature conditions and extends the service life of the device.

[0028] 4. In one possible implementation, when inspecting the inner surface after the protective film is formed, a scanning electron microscope is used to observe the microstructure of the film layer and X-ray diffraction is used to analyze its composition to ensure that the uniformity and density meet the preset standards. This inspection is beneficial to detect potential defects early and thus avoid the risk of failure during operation.

[0029] For example, in hydrogen purification applications, this validation process can confirm the reliability of the housing protection capability, supporting the adaptability of the entire device to high temperature and high pressure environments from a quality assurance perspective and improving the stability of purification efficiency.

[0030] S3, the Getter material is a zirconium-vanadium-iron system or a zirconium-iron system alloy.

[0031] As a getter material, the zirconium-vanadium-iron or zirconium-iron alloy first requires precise proportioning and smelting of raw materials to ensure the uniformity of the alloy composition. During smelting, impurity content is controlled to obtain high-purity alloy materials. Starting from the high-purity alloy material obtained from smelting, it is processed into particle shapes suitable for bed filling. The particle size and shape are standardized to ensure uniform gas flow during subsequent use. The processed alloy particles need to be activated in a specific environment. During activation, temperature and atmosphere conditions are controlled to form active sites on the alloy surface, enhancing its adsorption capacity for impurity gases. The activated alloy particles are then filled into the bed within the pressure-bearing shell. During filling, uniform particle distribution is ensured to achieve efficient capture of impurities in hydrogen gas, thus achieving the goal of using the zirconium-vanadium-iron or zirconium-iron alloy as a getter material.

[0032] For example, the generation steps are as follows: 1. The zirconium-vanadium-iron alloy is used as a gas-getting material. When making precise proportions, the proportion of zirconium element needs to be controlled at a high level to enhance the stability of hydrogen adsorption. The melting is carried out in a vacuum induction melting furnace. The oxide impurities are removed by multiple remeltings to obtain the alloy material. This method can improve the purity of the alloy and reduce the risk of subsequent hydrogen corrosion.

[0033] 2. Starting from the obtained alloy material, mechanical crushing and sieving methods are used when processing it into particles to unify the particle diameter to a specific range in order to optimize the gas flow path. For example, in the bed filling, the particle gaps are ensured to be evenly distributed to avoid local blockage. This processing helps to maintain the pressure stability during the hydrogen purification process.

[0034] 3. For the processed particles, during the activation treatment, they are placed in a hydrogen atmosphere and gradually heated to a preset temperature to generate a metal hydride layer on the surface as an active site. For example, by controlling the heating rate, particle agglomeration is prevented, thereby improving the cracking efficiency of impurities such as methane. This treatment can significantly enhance the catalytic activity of the alloy and extend its service life.

[0035] 4. Starting with the activated particles, vibration filling technology is used when filling the pressure-bearing shell to ensure consistent particle density. For example, combined with the pretreatment of the inner surface of the shell, such as electropolishing to form a protective film, the efficient capture of hydrogen impurities can be achieved. This filling method can optimize the bed performance and achieve the purification goal of the alloy as a getter material.

[0036] S4, a method for efficient hydrogen purification suitable for ultra-high temperature conditions, comprising passing the raw hydrogen to be purified through a bed of Getter material, and reacting the raw hydrogen with the Getter material at a temperature of 600℃±10℃ to remove impurity gases.

[0037] The raw hydrogen gas to be purified is introduced into a bed containing getter material. Maintaining a temperature of 600°C ± 10°C ensures sufficient contact between the hydrogen gas and the getter material, promoting a chemical reaction between impurity gases and the material surface, forming a pre-purified hydrogen gas stream. This pre-purified hydrogen stream is then further catalytically decomposed by the continuous high-temperature environment inside the getter material bed, converting residual methane impurities into simple adsorbable compounds, ensuring a further reduction in impurity concentration and obtaining a deeply purified hydrogen stream. The deeply purified hydrogen stream is continuously monitored. As it passes through the end of the getter material bed, the content of residual impurities is detected in real time. If the detected value exceeds a preset threshold, the hydrogen flow rate through the bed is adjusted to extend the contact reaction time, obtaining a final hydrogen stream that meets purity requirements. The final hydrogen stream is then exited from the getter material bed and cooled through a cooling channel within the pressure vessel to ensure it reaches a suitable temperature for subsequent use before leaving the device, while maintaining the quality of ultra-high purity hydrogen, thus completing the purification process.

[0038] In one embodiment, the raw hydrogen gas to be purified is introduced into a bed containing getter material. By maintaining a temperature of 600 degrees Celsius ± 10 degrees Celsius, the hydrogen gas comes into contact with the material. This promotes the chemical reaction between impurity gases such as water vapor and oxygen and the surface of the getter. For example, in fuel cell production scenarios, the raw hydrogen gas contains a small amount of carbon dioxide. This contact reaction will convert the carbon dioxide into a fixable compound, thereby forming a pre-purified hydrogen gas flow. This is beneficial to improving the efficiency of subsequent purification because the preliminary removal of impurities reduces the downstream burden and ensures a more efficient and stable overall process.

[0039] Specifically, for the initially purified hydrogen stream, the residual methane impurities are further catalytically decomposed using the continuous high-temperature environment inside the bed. This catalytic process involves the cracking of methane molecules into carbon and hydrogen at high temperatures. Then, the carbon is adsorbed by the getter and converted into simple compounds. For example, in aerospace hydrogen supply, residual methane may affect fuel purity if it is not decomposed. This conversion step ensures that the impurity concentration is reduced, resulting in a deeply purified hydrogen stream. The beneficial effects are that it significantly improves the removal rate of stubborn impurities, avoids the risk of penetration, and extends the service life of the device.

[0040] In one embodiment, the deep-purified hydrogen flow is continuously monitored, and the residual impurity content is detected in real time at the end of the bed. If it exceeds a preset threshold, the flow rate is adjusted to extend the contact time. For example, in high-end metallurgical applications, when nitrogen residue is detected to exceed the standard, the flow rate is slowed down to allow more reaction opportunities, thereby obtaining a final hydrogen flow that meets the purity requirements. This monitoring and adjustment is beneficial for dynamically optimizing the purification effect, preventing impurity fluctuations from affecting product quality, and improving the adaptability of the device.

[0041] Specifically, after the final hydrogen gas is exited from the bed, it is cooled through a cooling channel in the pressure-bearing shell to ensure that the outlet temperature is suitable for subsequent use while maintaining ultra-high purity. For example, in semiconductor manufacturing lines, the cooled hydrogen is directly used for wafer cleaning. This treatment helps prevent the high-temperature hydrogen from corroding downstream equipment and maintains purity integrity, thus improving the overall reliability of hydrogen quality after the purification process is completed.

[0042] S5, the method further includes a system activation step, in which the system is first evacuated before the raw material hydrogen is introduced, and then the system is heated to 600°C and kept at that temperature for a period of time under an inert atmosphere or a high-purity hydrogen atmosphere to activate the Getter material and stabilize its surface state.

[0043] Before system operation, the entire device undergoes initial treatment. First, a vacuum system is used to adjust the internal environment to a low-pressure state to remove residual gases and moisture, ensuring the purity of the subsequent activation process and creating a closed environment free from impurities. In this closed environment, an inert gas or high-purity hydrogen is introduced as a protective atmosphere to prevent oxidation or contamination of the material surface during heating. Simultaneously, the heating device is activated, and the temperature is gradually increased to the target high-temperature range according to a preset program and maintained for a period of time to ensure the internal structure of the material is adjusted to a suitable state. After the internal structure of the material is adjusted to a suitable state, the high-temperature environment is maintained. By controlling the flow rate and pressure of the atmosphere, the protective atmosphere is evenly distributed on the material surface, promoting the full exposure of active sites and forming a stable reaction interface. After a stable reaction interface is formed, the flow rate of the protective atmosphere is gradually reduced, while monitoring the changes in the material surface state to ensure that the active sites remain in optimal condition. This lays the foundation for the subsequent introduction of hydrogen and impurity removal, completing the system activation steps to activate the getter material and stabilize its surface state.

[0044] In one possible implementation, during the initial treatment of the device, the internal environment is adjusted to a low-pressure state by using a vacuum device, such as a rotary vane pump or a turbomolecular pump, to reduce the pressure to below 1 Pa. This effectively removes residual gases and moisture, preventing these impurities from reacting with the material at subsequent high temperatures and causing surface passivation. This is beneficial for improving the purity of the activation process and forming a closed environment free from impurities, thus providing a reliable basis for material activation.

[0045] It should be noted that this vacuuming operation also prevents residual oxygen in the air, reduces the risk of oxidation, and ensures the stability of material performance.

[0046] For example, in semiconductor manufacturing, this process is similar to the pre-preparation of a vacuum chamber, which can significantly reduce the defect rate and improve the purity of hydrogen output. In one possible implementation, an inert gas such as argon or high-purity hydrogen is introduced as a protective atmosphere in a closed environment free from impurities, for example, at a flow rate of 0.1-1 L / min. Simultaneously, a resistance heating device is activated, and the temperature is gradually increased from room temperature to 600°C according to a linear heating program and maintained for 2-4 hours. This prevents oxidation or contamination of the material surface and ensures that the internal structure of the material is adjusted to a suitable state, which is beneficial for activating the crystal structure of the material and enhancing its adsorption capacity.

[0047] It should be noted that this uniform distribution of the protective atmosphere can suppress hydrogen embrittlement at high temperatures and extend the life of the device.

[0048] For example, in fuel cell applications, this step is similar to catalyst pre-activation, which improves hydrogen purification efficiency and reduces impurity penetration. In one possible implementation, after the internal structure of the material is adjusted to a suitable state, a high-temperature environment is maintained, and the atmosphere flow rate and pressure are controlled by adjusting valves to ensure that the protective atmosphere is evenly distributed on the material surface, for example, by using a porous distributor to achieve uniform coverage. This promotes the full exposure of active sites on the material surface and the formation of a stable reaction interface, which is beneficial for improving the reaction rate against impurities and optimizing purification performance.

[0049] It should be noted that this uniform distribution can avoid local overheating and ensure consistent overall material activity.

[0050] For example, in the aerospace field, this process is similar to the heat treatment of alloy materials, which can enhance high-temperature resistance and support a stable supply of ultra-high purity hydrogen. In one possible implementation, after a stable reaction interface is formed, the flow rate of the protective atmosphere is gradually reduced, for example, from the initial flow rate to zero, while the state changes of the material surface are monitored by temperature sensors and surface analyzers to ensure that the active sites remain in an optimal state. This lays the foundation for the subsequent introduction of raw material hydrogen and the removal of impurities, and completes the system activation step to activate the getter material and stabilize its surface state, which is beneficial for achieving efficient hydrogen purification and maintaining long-term operation.

[0051] It should be noted that this monitoring can adjust parameters in a timely manner to prevent surface deactivation.

[0052] For example, in high-end metallurgical applications, this step is similar to furnace atmosphere control, which can significantly reduce the content of impurities such as methane and improve the purity of hydrogen in the product.

[0053] S21, the high chromium nickel alloy material is 310S stainless steel or nickel-based alloy Inconel 600 or Inconel 601, and the electropolishing treatment is followed by an oxidation pretreatment at 980℃ for 2 hours.

[0054] For the selection of the pressure-bearing shell material, the high-chromium-nickel alloy material is determined to be 310S stainless steel or nickel-based alloys Inconel 600 or Inconel 601 to meet the requirements of use under high temperature and high pressure environments, obtaining an initial shell substrate for subsequent surface treatment. Starting from the initial shell substrate, surface electropolishing is performed to improve the smoothness of the inner surface and reduce microscopic defects, obtaining a smoothed shell intermediate. The smoothed shell intermediate undergoes an oxidation pretreatment at a high temperature, specifically at nearly 1000 degrees Celsius for several hours, forming a dense oxide protective layer, obtaining a final shell with corrosion resistance. From this final shell, it is used to load a Getter material bed to ensure stable structural performance under high-temperature operating conditions, completing the construction of the hydrogen purification equipment.

[0055] For example, when selecting a high-chromium-nickel alloy material, 310S stainless steel is chosen to withstand high-temperature and high-pressure environments. This material contains a high proportion of chromium and nickel, which can form a stable oxide layer to resist corrosion, thereby obtaining an initial shell substrate. This choice helps to enhance overall durability in subsequent processing because it provides a solid base and avoids the problem of rapid deterioration in a hydrogen environment.

[0056] In one possible implementation, the use of the nickel-based alloy Inconel 600 ensures the structural integrity of the housing at sustained high temperatures due to its excellent oxidation resistance. This results in extended equipment life and reduced maintenance requirements, further supporting continuity from material selection to surface treatment.

[0057] In one possible implementation, the initial shell substrate is electropolished to remove the surface inhomogeneity layer through an electrochemical method, thereby improving the smoothness of the inner surface and reducing micro-defects, resulting in a smoothed shell intermediate. This treatment reduces the risk of hydrogen permeation because a smooth surface minimizes stress concentration points, thus improving compatibility with oxidation pretreatment. The beneficial effects include improving the shell's ability to withstand high-pressure environments and preventing potential crack propagation.

[0058] For example, an oxidation pretreatment is performed on the smoothed shell intermediate to form a dense oxide protective layer at high temperature for several hours. This layer is mainly composed of chromium oxide and acts as a barrier to inhibit hydrogen corrosion and carbon reaction, resulting in a final shell with corrosion resistance. This step enhances the results of the previous smoothing process because the oxide layer depends on the uniformity of the smooth substrate. The beneficial effect is that it significantly improves the stability of the shell during hydrogen purification and prevents side reactions such as methane generation.

[0059] In one possible implementation, the final shell is used to load the Getter material bed, ensuring stable structural performance under high-temperature operating conditions. This loading method utilizes the corrosion-resistant properties of the shell to protect the internal materials from environmental influences, completing the construction of the hydrogen purification equipment. The beneficial effect of this is that it achieves efficient impurity removal because the stable shell supports the catalytic activity of the Getter material. Overall, a complementary chain is formed from material selection to final construction, improving the reliability and purification efficiency of the equipment.

[0060] S22, the protective film is a Cr2O3 or Al2O3 film, used to inhibit hydrogen corrosion and the reaction of matrix carbon to generate methane.

[0061] For the inner surface treatment of the pressure-bearing shell, electropolishing is used to smooth the surface of the high-chromium-nickel alloy material, reducing surface roughness and improving surface finish to form a uniform base layer, providing conditions for the subsequent formation of the protective film. On the electropolished base layer, a high-temperature oxidation pretreatment is performed. By controlling the oxidation environment and temperature, a dense oxide protective film is formed on the inner surface. This protective film, either chromium oxide or aluminum oxide, is used to shield the substrate material from direct contact with high-temperature, high-pressure hydrogen. The generated oxide protective film is tested for thickness and uniformity to determine if it meets the preset protection standards. If the test results meet the requirements, the inner surface is applied to the hydrogen purification environment to reduce the possibility of methane formation from the reaction of carbon in the substrate with hydrogen. After the protective film is applied, the condition of the inner surface of the pressure-bearing shell is monitored regularly. Wear or corrosion signs of the protective film are obtained from operational data. Operating parameters are adjusted promptly for any abnormalities to ensure the protective film continuously inhibits hydrogen corrosion and methane formation, guaranteeing the stability of the hydrogen purification process.

[0062] For example, the generation steps are as follows: 1. For example, during the surface treatment of the inner surface of the pressure-bearing housing, electropolishing is used to smooth the surface of the high-chromium-nickel alloy material, which can effectively reduce surface roughness and improve surface smoothness, forming a uniform base layer. This treatment helps to provide ideal conditions for the subsequent formation of a protective film, because a smooth surface can promote the uniform adhesion of the oxide film, thereby enhancing the overall protective performance.

[0063] 2. In one possible implementation, the base layer after electropolishing undergoes a high-temperature oxidation pretreatment. By precisely controlling the oxidation environment and temperature, a dense oxide protective film is generated on the inner surface. The protective film is a chromium oxide film or an aluminum oxide film, which is used to shield the substrate material from direct contact with high-temperature and high-pressure hydrogen. This shielding effect can significantly reduce the risk of hydrogen erosion to the material and prevent the substrate carbon from reacting to form methane, thereby extending the service life of the device and improving the efficiency of hydrogen purification.

[0064] 3. For example, the generated oxide protective film is tested for its thickness and uniformity to determine whether it meets the preset protection standard. If the test results meet the requirements, the inner surface is applied to the hydrogen purification environment to reduce the possibility of the matrix carbon reacting with hydrogen to generate methane. This test process involves using an optical microscope or a scanning electron microscope to observe the film structure to ensure that the film thickness is uniformly distributed at the micrometer level, thereby avoiding failure caused by local weak points and providing reliable material protection for the purification process.

[0065] 4. In one possible implementation, after the protective film is applied, the condition of the inner surface of the pressure-bearing shell is monitored regularly, and signs of wear or corrosion of the protective film are obtained from the operating data. In case of abnormalities, the operating parameters are adjusted in a timely manner to ensure that the protective film continuously inhibits hydrogen erosion and methane generation, and to ensure the stability of the hydrogen purification process.

[0066] For example, in actual operation, if localized corrosion of the membrane is detected, parameters can be adjusted by reducing the hydrogen flow rate or increasing inert gas protection. This kind of monitoring can detect problems early, prevent small defects from evolving into major failures, thereby maintaining the efficient operation of the device and reducing maintenance costs.

[0067] 5. For example, from multiple perspectives, the implementation of high-temperature oxidation pretreatment can be optimized in combination with different alloy types. For instance, for 310S stainless steel, a chromium oxide film is formed by heating it in air to a specified temperature, while for Inconel 600 alloy, an oxygen-containing atmosphere can be used to generate an aluminum oxide film. These methods support each other because the chromium oxide film provides good oxidation resistance, while the aluminum oxide film enhances high-temperature stability, together ensuring the effect of inhibiting hydrogen corrosion at 600 degrees Celsius.

[0068] 6. In one possible implementation, specific methods for detecting thickness and uniformity include non-destructive testing, such as ultrasonic thickness gauges, for quantifying film parameters and comparing them with preset standards.

[0069] For example, if the standard requires the film thickness to be at least several micrometers and the uniformity deviation to be less than a certain percentage, then the compliance can be judged by data analysis. This method can support the realization of the protection standard from both the perspectives of accuracy and reliability, thus providing a solid foundation for subsequent applications.

[0070] 7. Exemplary examples of extended periodic monitoring involve integrated sensor systems that extract signs of wear from operational data such as temperature, pressure, and gas composition.

[0071] For example, if data shows an abnormally high hydrogen concentration, it may indicate that the membrane corrosion is intensifying. In this case, adjusting parameters such as the cooling rate can support each other from both preventative and responsive perspectives, jointly maintaining the integrity of the protective membrane and ultimately ensuring the stability of the hydrogen purification process from methane generation interference.

[0072] S31, the zirconium-vanadium-iron alloy or zirconium-iron alloy has methane cracking catalytic activity and impurity adsorption capacity at 600℃.

[0073] An initial material bed is obtained from a zirconium-vanadium-iron alloy or a zirconium-iron alloy. This material bed is placed inside a pressure vessel, and the operating temperature is maintained within a preset range by a heating system to ensure that the surface active sites of the material are activated at high temperatures for subsequent methane cracking and impurity adsorption processes. Based on the activation of the surface active sites of the material bed, the input hydrogen stream induces a catalytic cracking reaction between methane molecules and the material surface under high-temperature conditions, decomposing methane into carbon and hydrogen. Simultaneously, the decomposed carbon elements are fixed on the material surface, forming a stable solid deposit. During the formation of this solid deposit, the material's high adsorption capacity is used to selectively capture other trace impurities in the hydrogen, binding impurity molecules inside or on the surface of the material to generate stable compound structures, reducing impurity residues in the gas stream. After the impurities are captured and stable compound structures are formed, the temperature stability of the material bed and the gas flow rate are continuously maintained to ensure the sustained performance of the methane cracking catalytic activity and impurity adsorption capacity, completing the efficient purification process of hydrogen.

[0074] For example, after obtaining the initial material bed from a zirconium-vanadium-iron alloy or a zirconium-iron alloy, it is placed inside a pressure-bearing shell made of a high-chromium-nickel alloy, and the operating temperature is maintained at about 600 degrees Celsius by a heating system. This activates the active sites on the material surface, because the high-temperature environment promotes the rearrangement of alloy atoms, forming more exposed metal sites, which is beneficial to subsequent reactions. This activation process has the beneficial effect of improving the material's methane cracking efficiency and avoiding the problem of slow reaction kinetics at low temperatures, thereby ensuring a more thorough purification process.

[0075] In one possible implementation, based on the activation of active sites on the surface of the material bed, when the feed hydrogen gas is introduced, methane molecules undergo catalytic cracking with the surface at high temperature, decomposing methane into carbon and hydrogen, and fixing carbon elements to form solid deposits. This cracking reaction helps prevent methane from penetrating the bed, because the solid deposits are stably attached and do not release back into the gas flow, resulting in technical effects such as significantly reducing the methane concentration in the outlet hydrogen to below 1 ppb, supporting the overall efficiency of the purification unit.

[0076] For example, in response to the formation of solid deposits on the material surface, the high adsorption capacity of the material is used to selectively capture other impurities, such as moisture or carbon dioxide, and combine them to form stable compounds. This capture process is achieved through internal vacancies or surface complexation of the material. The beneficial effect is to reduce residual impurities in the airflow because the stable compounds are not easily desorbed, thereby extending the operating cycle of the device and maintaining high-purity output.

[0077] In one possible implementation, after impurities are captured and stable compounds are formed, maintaining bed temperature stability and gas flow rate can ensure the sustained performance of methane cracking catalytic activity and adsorption capacity. This maintenance method is achieved through feedback control of the heating system, which helps to avoid uneven reaction caused by temperature fluctuations, resulting in effects such as achieving continuity and stability in the hydrogen purification process, and ultimately achieving efficient purification.

[0078] For example, in practical applications such as semiconductor manufacturing, the alloy bed is used to process hydrogen sources containing trace amounts of methane. Through the activation and pyrolysis steps described above, impurities can be reduced to extremely low levels. This method, from material preparation to gas flow treatment, ensures that each step supports the other, resulting in an overall improvement in purification efficiency.

[0079] In one possible implementation, considering the high-purity hydrogen requirements of the aerospace industry, a combination of a pressure-bearing shell and a heating system is used to adsorb and extend the solid deposits formed by pyrolysis. This can handle complex mixtures of impurities. This extension is beneficial for adapting to different operating conditions because it strengthens the thought chain from decomposition to capture, supporting the reliable operation of the device in harsh environments.

[0080] For example, further examining the matter, in fuel cell applications, the step of maintaining the gas flow rate is linked to the aforementioned capture process, which can prevent performance degradation caused by the accumulation of impurities. This linkage brings beneficial effects such as extending the life of the fuel cell, and is supported by multiple aspects such as temperature control and adsorption capacity, forming a consistent purification argument.

[0081] S41, when the raw material hydrogen passes through the bed, the operating space velocity is set to 5000 h⁻¹, the raw material hydrogen pressure is 1.0 MPa, and the methane content is 10 ppm.

[0082] An initial gas stream with a preset methane content is obtained from the hydrogen input. This gas stream is introduced into the bed of the purification unit at a preset pressure, maintained within a specified range to ensure uniform gas distribution. Inside the bed, the operating space velocity is set to a predetermined value to ensure sufficient contact between the gas stream and the getter material. The gas stream reacts with the material at a high temperature, initially reducing the impurity content. For the gas stream after the initial reaction, the bed temperature is maintained within a specified high-temperature range to promote a deeper chemical reaction between methane impurities and the getter material, ensuring the methane content gradually decreases to the target range. A gas stream after the deep reaction is obtained from the bed output. The methane impurities in this gas stream have been effectively removed, completing the purification process of the hydrogen feedstock under specified space velocity and pressure conditions, achieving the expected purity requirements.

[0083] For example, in the process of purifying raw material hydrogen, the operation of obtaining the initial gas flow from the input end can ensure the initial control of methane impurities. This method stabilizes the input quality by setting the methane content by a preset value, which is beneficial to the improvement of subsequent purification efficiency. This is because a uniformly distributed gas flow can avoid uneven reaction caused by excessively high local concentrations, thereby making the overall purification process more reliable.

[0084] In one possible implementation, the input gas flow is assumed to originate from upstream of an industrial hydrogen production line and be transported via pipeline to the inlet valve of the purification unit. At this point, the pressure is maintained within a specified range, such as atmospheric pressure to medium pressure. This facilitates the diffusion of gas molecules within the bed, avoids potential turbulence interference under high pressure, and thus improves the uniformity of contact with the getter material. Such a design can reduce the risk of impurity residue.

[0085] Specifically, the setting of the operating space velocity within the bed is designed to ensure sufficient contact between the gas flow and the getter material. This step controls the gas flow rate by a predetermined value to ensure sufficient reaction time, which is beneficial for initially reducing the impurity content. This is because the reaction under high temperature conditions can accelerate the breaking of chemical bonds, thereby effectively capturing impurities such as oxygen or nitrogen compounds.

[0086] In one possible implementation, the getter material is a zirconium-based alloy-filled bed. When the gas stream passes through at a moderate space velocity, an adsorption reaction occurs on the material surface, initially separating impurities from the gas stream. This not only improves the efficiency of the initial purification stage but also lays the foundation for subsequent deep reactions, avoiding purity fluctuations caused by impurity accumulation.

[0087] It should be noted that maintaining the bed temperature within the specified high-temperature range is for the gas stream that has undergone preliminary reaction, promoting the deep chemical reaction of methane impurities. This temperature control is beneficial for activating the cracking pathway of methane molecules, because high temperature can provide enough energy for methane to undergo carbon-hydrogen bond breaking and recombination with the getter, thereby gradually reducing the methane content to the target range.

[0088] In one possible implementation, the bed is equipped with heating elements such as resistance wires to ensure uniform temperature distribution. When the gas flows through, methane molecules are catalytically decomposed into carbon and hydrogen on the surface of the getter. The carbon is absorbed by the material, which results in a significant impurity removal effect and supports a stable improvement in overall purity.

[0089] Specifically, the entire purification process is completed by obtaining the gas stream after deep reaction from the output end. This method ensures the effective removal of methane impurities and helps to achieve the expected purity requirements because the output gas stream has been processed under specified space velocity and pressure conditions, thereby providing high-purity hydrogen support for applications such as semiconductor manufacturing.

[0090] In one possible implementation, the output is connected to a detection instrument to monitor the residual methane level. If it meets the standard, it is directly delivered to downstream equipment. This not only verifies the reliability of the purification process, but also optimizes the long-term operating performance of the device through continuous monitoring, avoiding potential losses caused by impurity backtracking issues.

[0091] S211, the electropolishing process makes the inner surface roughness Ra less than 0.4 μm, and then the high-temperature oxidation pretreatment is carried out under the protection of high-purity argon gas.

[0092] For the treatment of the inner surface of the pressure-bearing shell, the selected stainless steel material is first electropolished to ensure that the surface roughness reaches below a preset threshold, forming a smooth base surface and providing uniform contact conditions for subsequent treatments. On the smooth base surface after electropolishing, high-purity argon is used as a protective atmosphere, and the treated shell is placed in a high-temperature environment for oxidation pretreatment. By controlling the atmosphere conditions, a stable oxide layer is formed on the surface to improve corrosion resistance. Following the oxidation pretreatment, the shell surface undergoes subsequent system activation preparation. The internal environment of the shell is subjected to programmed temperature rise under an inert atmosphere to ensure the stability and consistency of the surface oxide layer, laying the foundation for further applications. After the surface oxide layer stabilizes, the atmosphere inside the shell is adjusted. By gradually introducing a specific gas environment, the surface treatment effect is verified, ensuring that the combined electropolishing and high-temperature oxidation pretreatment achieves the target requirements for inner surface roughness and corrosion resistance.

[0093] In one possible implementation, the selected stainless steel material is electropolished to ensure that the surface roughness is below a preset threshold, forming a smooth base surface. This operation removes the surface uneven layer through electrochemical methods, making the base surface smooth and uniform, thereby providing a better adhesion base for subsequent oxidation pretreatment and helping to improve the uniformity of the overall treatment.

[0094] For example, in practical applications, selecting an electrolyte with a suitable current density for polishing can effectively reduce surface micro-defects, resulting in higher surface quality and improving the sealing performance of the housing under high pressure.

[0095] Specifically, on the smooth base surface after electropolishing, high-purity argon is used as a protective atmosphere to place the treated shell in a high-temperature environment for oxidation pretreatment. By controlling the atmosphere conditions, a stable oxide layer is formed on the surface to improve corrosion resistance. This pretreatment promotes the surface oxidation reaction at high temperature, forming a dense oxide film layer to prevent further corrosion.

[0096] For example, in a stainless steel casing, high-temperature oxidation can generate a chromium oxide layer, which acts as a barrier to prevent oxygen penetration, thereby extending the casing's service life and contributing to long-term stability in hydrogen production.

[0097] In one possible implementation, the shell surface after oxidation pretreatment is prepared for subsequent system activation by performing a programmed temperature rise treatment on the internal environment of the shell under an inert atmosphere to ensure the stability and consistency of the surface oxide layer, laying the foundation for further applications. This temperature rise process gradually activates the active sites on the material surface, making the oxide layer bond more tightly with the substrate.

[0098] For example, by slowly increasing the temperature to avoid thermal stress cracking, the integrity of the oxide layer can be maintained, which is beneficial to the surface reaction efficiency when subsequent gases are introduced.

[0099] Specifically, after the surface oxide layer stabilizes, the atmosphere inside the shell is adjusted. By gradually introducing a specific gas environment, the surface treatment effect is verified to ensure that the surface roughness and corrosion resistance of the inner surface meet the target requirements after the combination of electropolishing and high-temperature oxidation pretreatment. This adjustment includes the transition from inert gas to reactive gas and testing the surface response to the gas.

[0100] For example, verifying the stability of the oxide layer before introducing hydrogen can confirm the treatment effect, provide a reliable environment for producing ultra-high purity hydrogen, and benefit the overall system performance optimization.

[0101] In one possible implementation, the above process forms a continuous chain from electropolishing to oxidation pretreatment to activation preparation, with each step enhancing surface properties.

[0102] For example, a smooth base surface directly affects the uniform formation of the oxide layer, while a stable oxide layer ensures surface consistency during activation. The final verification step integrates the aforementioned effects to jointly support the durability of the shell in a high-pressure hydrogen environment, which is beneficial for reducing impurity adsorption and improving purity.

[0103] Specifically, from multiple perspectives, electropolishing can be expanded to include various electrolyte formulations.

[0104] For example, acidic solutions are used for stubborn oxide scale, while alkaline solutions are suitable for fine polishing. These approaches support each other, ensuring flexibility in roughness control and making it suitable for various types of stainless steel. Similarly, high-temperature oxidation pretreatment can be adjusted within different temperature ranges.

[0105] For example, the medium-temperature zone focuses on oxide layer thickness, while the medium-high temperature zone emphasizes density. These mutually supportive approaches enrich the optimization path for corrosion resistance.

[0106] In one possible implementation, the procedural warm-up for system activation preparation can be carried out in stages.

[0107] For example, stabilizing the structure by first heating at a low speed and then activating the surface by heating at a high speed ensures consistency, while the gradual introduction of atmosphere adjustment can include multiple rounds of cyclic verification.

[0108] For example, testing with a small flow rate of gas before applying it at full flow rate allows for comprehensive confirmation of the treatment effect from multiple perspectives, which is beneficial to achieving the final goal: an inner surface roughness Ra of less than 0.4 μm and high-temperature oxidation pretreatment under high-purity argon protection.

[0109] S212, after the high-temperature oxidation pretreatment, the thickness of the protective film is 1-5 μm.

[0110] After selecting a specific stainless steel material for the pressure-bearing shell, its inner surface is electropolished to improve surface smoothness and reduce microscopic defects. Subsequently, it undergoes oxidation pretreatment in a high-temperature, high-purity inert gas environment to form an initial protective layer. After the initial protective layer forms, the ambient temperature and time of the oxidation pretreatment are controlled, and the gas flow rate and pressure are adjusted to ensure the protective layer gradually thickens and achieves a uniform distribution. Based on the uniform distribution of the protective layer, its thickness is continuously monitored, and local process parameters are adjusted for areas where the thickness does not meet the standard to ensure the overall protective layer thickness is controlled within the predetermined range. After thickness control is completed, the surface quality of the protective layer is inspected to obtain its microstructural characteristic data. Minor non-uniformities discovered during the inspection are then further optimized to ensure the final protective layer thickness meets the target requirements after high-temperature oxidation pretreatment.

[0111] For example, the generation steps are as follows: 1. For example, after selecting a specific stainless steel material for the pressure-bearing shell, its inner surface is electropolished. This treatment removes the irregular layer on the surface through an electrochemical method, improving surface smoothness and reducing micro-defects. This results in a more stable substrate, which is beneficial for the adhesion of the subsequent oxide layer. For example, in actual operation, the shell is immersed in an electrolyte and an electric current is applied to gradually dissolve the surface protrusions, thereby obtaining a mirror-like inner wall. This can reduce the adsorption of gas impurities. Subsequently, an oxidation pretreatment is performed in a high-temperature, high-purity inert gas environment to form an initial protective layer. This pretreatment generates a chromium oxide layer on the stainless steel surface by controlling the oxygen partial pressure, which is beneficial for blocking hydrogen permeation. For example, the shell is heated to a specified temperature in a furnace and an inert gas mixed with a small amount of oxygen is introduced. The initial layer thickness gradually accumulates, providing a preliminary anti-corrosion barrier.

[0112] 2. For example, after the initial protective layer is formed, the ambient temperature and time of the oxidation pretreatment are controlled. By adjusting the gas flow rate and pressure, the protective layer is ensured to gradually thicken and reach a uniform distribution. This control method optimizes the oxidation kinetics process and helps avoid local over-thickness or under-thinness. For example, during the treatment, a flow meter is used to adjust the inert gas input rate, while a pressure gauge is monitored to maintain a stable atmosphere. Temperature uniformity results in a consistent layer thickness. Building upon the initial layer, the density of the layer is further enhanced. For example, if the initial layer has already covered the surface, the oxidation reaction is allowed to penetrate deeper by extending the time, gradually thickening to a uniform state. This can bring about the beneficial effect of improving overall durability.

[0113] 3. For example, based on the uniform distribution of the protective layer, the thickness of the layer is continuously monitored. Local process parameters are adjusted for areas where the thickness does not meet the standard to ensure that the overall thickness of the protective layer is controlled within a predetermined range. This monitoring is carried out by observing the layer thickness changes in real time through optical or electron microscopy, which is beneficial for timely intervention in unevenness problems. For example, if the thickness of a certain area is found to be too low during monitoring, the oxygen concentration or heating time is increased locally to make adjustments, resulting in a precise control effect. After the aforementioned uniform distribution, the thickness is ensured to be stable and hydrogen-induced reactions are avoided. For example, the thickness data is obtained by scanning the surface with a probe, and the parameters are optimized for the deviation area, which can bring about the beneficial effect of improving the stability of the material.

[0114] 4. For example, after thickness control is completed, the surface quality of the protective layer is inspected to obtain its microstructure characteristics. For minor inhomogeneities found during the inspection, secondary optimization is performed to ensure that the final protective layer thickness meets the target requirements after high-temperature oxidation pretreatment. This inspection uses scanning electron microscopy to analyze the microstructure, which is beneficial for identifying grain boundaries or defects. For example, the cross-section of the oxide layer can be magnified during inspection to quantify porosity and crystal arrangement. If inhomogeneities are found, optimization is performed through additional heat treatment or chemical etching, resulting in the technical effect of layer quality optimization. Building on the aforementioned thickness control, the structural integrity is further improved. For example, the thickness data is re-verified after secondary processing to ensure that it meets the target, which can bring the beneficial effect of enhanced corrosion resistance.

[0115] S51, the vacuum is evacuated to less than 10 Pa, and then a high-purity nitrogen replacement system is introduced. Subsequently, the temperature is increased to 600°C and high-purity hydrogen is introduced for activation for 8 hours.

[0116] First, the device undergoes initial treatment by evacuating the internal pressure to below a preset low-pressure threshold to ensure a high vacuum environment. Then, high-purity nitrogen is introduced for purging to remove residual impurities, creating a clean initial environment. Based on this clean initial environment, the internal temperature is gradually increased to a predetermined high-temperature range while maintaining a stable nitrogen atmosphere to ensure no interference from other gases during the heating process, forming a stable high-temperature activation state. In this stable high-temperature activation state, the gas environment is switched, and high-purity hydrogen is introduced and maintained for a period of time to activate the surface properties of the internal materials, generating the activated material structure. After the activated material structure is formed, the high-temperature conditions are maintained and the hydrogen flow rate is monitored to ensure the activation process continues until the preset activation time is reached, completing the entire activation process and meeting the objective of evacuating the vacuum to below the preset threshold, introducing high-purity nitrogen for purging, and then gradually increasing the temperature and introducing high-purity hydrogen for activation.

[0117] For example, in the initial processing stage of the device, a high vacuum state is achieved by evacuating the internal pressure to below a preset low-pressure threshold. This process effectively removes contaminants such as oxygen and moisture from the air, preventing oxidation of the material surface during subsequent activation, thereby improving the purity and activity of the material. For example.

[0118] In one possible implementation, a vacuum system combining a rotary vane pump and a molecular pump is used to first roughly pump to a medium vacuum level, and then finely pump to a high vacuum level to ensure a clean environment. This helps to create an impurity-free initial environment, resulting in the beneficial effect of improved material activation efficiency.

[0119] In one possible implementation, the temperature is programmed to rise to a predetermined high temperature range based on a clean initial environment, while maintaining a stable nitrogen atmosphere. This method prevents material degradation caused by oxygen intrusion during heating. Nitrogen, as an inert gas, can evenly distribute heat and promote a uniform temperature gradient, thereby forming a stable high-temperature state to be activated, which is beneficial to the uniformity of subsequent hydrogen activation.

[0120] For example, in laboratory-scale setups, a slow heating rate controlled at a few degrees per minute can reduce thermal stress damage to materials and enhance the stability of the overall structure.

[0121] For example, switching to high-purity hydrogen and maintaining the activation treatment can activate the surface properties of the material because the hydrogen reacts with the material at high temperatures to remove the surface oxide layer and generate an activated structure with greater adsorption capacity. This process improves the hydrogen capture performance of the material, which is beneficial to gas purification efficiency in industrial applications. For example.

[0122] In one possible implementation, hydrogen flow is controlled at a constant rate for several hours to activate the porous material surface, which can uniformly activate the surface and support the continuity from the initial vacuum to the final activation.

[0123] In one possible implementation, maintaining a high temperature and monitoring the hydrogen flow rate until the preset activation time ensures that activation is complete. This monitoring prevents local overactivation or underactivation caused by flow fluctuations, resulting in the beneficial effect of consistent material properties. This achieves the goal of purging the vacuum to below the preset threshold, then introducing high-purity nitrogen for replacement, followed by programmed heating and the introduction of high-purity hydrogen for activation.

[0124] For example, on the production line, flow meters are used to adjust in real time to ensure optimized material structure after activation and support consistency across multiple batches.

[0125] The above description is only a preferred embodiment of the present invention. It should be noted that those skilled in the art can make several improvements and additions without departing from the principle of the present invention, and these improvements and additions should also be considered within the scope of protection of the present invention.

Claims

1. A high-efficiency hydrogen purification device suitable for ultra-high temperature operating conditions, characterized in that, include: Pressure-bearing shell; Getter material bed disposed within the pressure-bearing shell; A heating system is provided for heating the Getter material bed, the heating system being configured to maintain the operating temperature of the Getter material bed at 600℃±10℃.

2. A method for efficient hydrogen purification suitable for ultra-high temperature operating conditions, characterized in that, include: The hydrogen gas to be purified is passed through a bed containing Getter material. At a temperature of 600℃±10℃, the raw material hydrogen is brought into contact with the Getter material to react and remove impurity gases from the raw material hydrogen. Before introducing the raw material hydrogen, the system is evacuated, and then the system is heated to 600°C and held at that temperature for a period of time under an inert atmosphere or a high-purity hydrogen atmosphere to activate the Getter material and stabilize its surface state.

3. The high-efficiency hydrogen purification device suitable for ultra-high temperature operating conditions as described in claim 1, characterized in that, The pressure-bearing housing includes: The pressure-bearing shell is made of high-chromium-nickel alloy material; The inner surface of the pressure-bearing shell is electropolished. After the electropolishing treatment, the inner surface is subjected to high-temperature oxidation pretreatment to form a dense Cr2O3 protective film or Al2O3 protective film. The Cr2O3 protective film or the Al2O3 protective film covers the inner surface, and the inner surface forms an enclosing structure for the Getter material bed.

4. The high-efficiency hydrogen purification device suitable for ultra-high temperature operating conditions as described in claim 1, characterized in that, The Getter material bed includes: The Getter material is a zirconium-vanadium-iron alloy or a zirconium-iron alloy; The zirconium-vanadium-iron alloy or the zirconium-iron alloy is filled into the pressure-bearing shell to form the Getter material bed; The Getter material bed is in contact with the heating system, which heats the zirconium-vanadium-iron alloy or the zirconium-iron alloy to 600℃±10℃.

5. The high-efficiency hydrogen purification device suitable for ultra-high temperature operating conditions as described in claim 1, characterized in that, The heating system includes: The heating system is located outside the pressure-bearing shell and conducts heat to the Getter material bed. The heating system monitors the operating temperature of the Getter material bed; The heating system adjusts the heating power according to the operating temperature to maintain the operating temperature within the range of 600℃±10℃.

6. The method for efficient hydrogen purification under ultra-high temperature conditions as described in claim 2, characterized in that, The system is evacuated, including: The pressure-bearing shell and the Getter material bed are evacuated; After the vacuum is drawn, high-purity nitrogen is introduced to replace the gas inside the pressure-bearing shell; After the high-purity nitrogen gas is used for purging, the heating system is programmed to be heated to 600°C. After the process heats up to 600°C, high-purity hydrogen is introduced to activate the Getter material bed. The activation process involves maintaining a certain temperature for a period of time to stabilize the surface state of the zirconium-vanadium-iron alloy or the zirconium-iron alloy.

7. The method for efficient hydrogen purification under ultra-high temperature conditions as described in claim 2, characterized in that, The raw material hydrogen gas passes through a bed packed with getter material, including: The raw material hydrogen gas enters the pressure-bearing shell; The raw material hydrogen flow passes through the Getter material bed; The Getter material bed is maintained at 600℃±10℃ under the action of the heating system; The raw material hydrogen gas comes into contact with the zirconium-vanadium-iron alloy or the zirconium-iron alloy; After the contact reaction, the purified hydrogen gas flows out from the pressure vessel.

8. The high-efficiency hydrogen purification device suitable for ultra-high temperature operating conditions as described in claim 3, characterized in that, The electropolishing process includes: The inner surface is electrolytically polished; The inner surface is cleaned after electropolishing; The inner surface is dried after cleaning; The high-temperature oxidation pretreatment is performed after drying.

Images