Deep hydrogen removal device and method for helium purification

Abstract

The invention discloses a deep hydrogen removal device and method for helium purification, and relates to the technical field of gas purification, the method comprises a pretreatment unit, the pretreatment unit comprises a pre-filter and a gas flow adjusting device which are connected in sequence, and the pretreatment unit is used for pretreating untreated helium; the core purification unit comprises a first-stage adsorption tower and a second-stage adsorption tower which are arranged in series, the first-stage adsorption tower is filled with an efficient dehydrogenation metal getter, and the second-stage adsorption tower is filled with a chemical active oxide adsorbent; the dehydrogenation module is used for carrying out dehydrogenation treatment on the pretreated helium twice; the post-treatment monitoring unit comprises a precise filter and an online hydrogen analyzer which are connected in sequence, and is used for precisely filtering the helium subjected to dehydrogenation treatment twice, detecting the content of hydrogen in the helium subjected to precise filtering, and sending the detected hydrogen to the online hydrogen analyzer; the problem that high working efficiency is difficult to guarantee while hydrogen is deeply removed to the sub-ppm level in an existing helium purification technology can be solved.

Description

Technical Field

[0001] This application relates to the field of gas purification technology, and in particular to a deep hydrogen removal device and method for helium purification. Background Technology

[0002] In the field of high-purity helium preparation and recovery, the deep removal of hydrogen impurities remains a core technical challenge for the industry. Helium, as an inert rare gas, is widely used in aerospace, semiconductors, nuclear energy, and cutting-edge scientific research. These applications place extremely stringent requirements on the purity of helium, especially the content of light impurities such as hydrogen. For example, in the aerospace field, helium is often used as a propellant pressurizing gas or a protective gas for precision instruments, requiring a hydrogen content of less than 0.5 ppm to ensure the safety and reliability of the system.

[0003] Traditional helium purification processes, such as cryogenic condensation, pressure swing adsorption (PSA), or catalytic oxidation, all have significant limitations when faced with the specific requirement of separating hydrogen and helium. Because hydrogen and helium molecules have extremely similar molecular diameters and boiling points, cryogenic condensation is inefficient and energy-intensive; PSA has limited selective adsorption capacity for hydrogen, making it difficult to achieve deep purification from ppm to sub-ppm levels; and while catalytic oxidation can convert hydrogen to water, it requires complex dehydration steps and may introduce other byproducts.

[0004] In summary, existing technologies cannot achieve stable and economical removal of hydrogen content from helium from high concentrations (e.g., ≤1000ppm) to extremely low levels (e.g., sub-ppm, 0.5ppm) while ensuring high efficiency, thus failing to meet the stringent requirements for ultra-high purity helium in aerospace and other fields. Summary of the Invention

[0005] The purpose of this application is to provide a deep hydrogen removal device and method for helium purification, which can solve the problem that existing helium purification technologies are unable to achieve deep hydrogen removal to the sub-ppm level while ensuring high working efficiency.

[0006] To achieve the above objectives, this application provides the following solution: In a first aspect, this application provides a deep hydrogen removal device for helium purification, comprising: The pretreatment unit includes a pre-filter and a gas flow regulating device connected in sequence, for pretreating untreated helium gas, the pretreatment including preliminary filtration and adjustment of helium gas flow rate; The core purification unit includes a primary adsorption tower and a secondary adsorption tower arranged in series. The primary adsorption tower is filled with a highly efficient dehydrogenating metal getter, and the secondary adsorption tower is filled with a chemically active oxide adsorbent. The core purification unit is used to perform two dehydrogenation treatments on the pretreated helium. The post-processing monitoring unit includes a precision filter and an online hydrogen analyzer connected in sequence. The post-processing monitoring unit is used to perform precision filtration on the helium after two dehydrogenation treatments and monitor the hydrogen content in the precision-filtered helium. The pretreatment unit, the core purification unit, and the post-treatment monitoring unit are connected in series.

[0007] Optionally, the gas flow regulating device includes: A mass flow meter, used to measure the real-time mass flow rate or standard volume flow rate of helium after preliminary filtration; A regulating valve is used to control the flow rate of helium gas after preliminary filtration.

[0008] Optionally, the effective dehydrogenation metal getter is a porous alloy containing zirconium, vanadium, iron, titanium, and copper; the chemically active oxide adsorbent is a composite material with porous oxide as a carrier and loaded with catalytically active metal components.

[0009] Optionally, the primary adsorption tower and the secondary adsorption tower are detachable structures, and the outer walls of both the primary adsorption tower and the secondary adsorption tower are provided with heat dissipation structures.

[0010] Optionally, the deep hydrogen removal device for helium purification further includes a control unit, the control unit comprising: Temperature sensors are respectively installed inside the primary adsorption tower and the secondary adsorption tower to monitor the temperature inside the primary adsorption tower and the secondary adsorption tower in real time. Pressure sensors are installed at the inlet and outlet of the core purification unit to monitor the pressure difference between the inlet and outlet of the core purification unit in real time. The PLC controller receives temperature signals from the temperature sensor, differential pressure signals from the pressure sensor, helium flow rate signals from the gas flow regulator, and hydrogen concentration signals from the online hydrogen analyzer. Based on all the received signals, it adjusts the gas flow regulator in real time to control the helium flow.

[0011] Optionally, the step of controlling the gas flow rate regulation device in real time according to all received signals to control the helium flow rate specifically includes: when the temperature of any temperature sensor rises abnormally above a set safety threshold, or the pressure difference of the core purification unit continues to increase above an allowable value, or the hydrogen concentration continues to exceed a preset concentration, the PLC controller regulates the gas flow rate regulation device to execute an instruction to reduce the helium flow rate.

[0012] Secondly, this application provides a deep hydrogen removal method for helium purification, comprising: The hydrogen-containing helium gas is pretreated by a pretreatment unit, which includes preliminary filtration and adjustment of the helium flow rate. The pretreated helium undergoes two dehydrogenation treatments through the core purification unit; the first treatment uses a highly efficient dehydrogenation metal getter, and the second treatment uses a chemically active oxide adsorbent. The helium gas after two dehydrogenation processes is precisely filtered by the post-processing monitoring unit, and the hydrogen content in the precisely filtered helium gas is monitored, ultimately outputting high-purity helium gas.

[0013] Optionally, the hydrogen-containing helium space velocity during the first dehydrogenation treatment is 500 h⁻¹. -1 up to 2000 h -1 The contact time between hydrogen-containing helium gas and the highly efficient dehydrogenating metal getter is 2 to 10 seconds.

[0014] Optionally, the deep hydrogen removal method for helium purification further includes: The working status of the two adsorbents is determined by monitoring the temperature changes of the two adsorbent beds in the core purification unit. When the temperature of either adsorbent bed rises abnormally, the helium flow rate is adjusted or the adsorbent replacement procedure is executed.

[0015] Optionally, the loading amount of the high-efficiency dehydrogenating metal getter is calculated in the following way: m=(C in ×F×t) / (η×ρ); In the formula, m is the mass of the required high-efficiency dehydrogenation metal getter, and C in η is the hydrogen volume concentration at the inlet of the core purification unit, F is the standard volume flow rate of helium, t is the design operating cycle, η is the design hydrogen absorption efficiency of the high-efficiency dehydrogenation metal getter, and ρ is the density of hydrogen under standard conditions.

[0016] According to the specific embodiments provided in this application, the following technical effects are disclosed: This application provides a deep hydrogen removal device and method for helium purification. A pre-filter in the pretreatment unit initially removes solid particles and oil mist from the raw helium gas, preventing contamination or blockage of the downstream adsorbent. Simultaneously, a gas flow regulating device precisely controls the helium flow rate entering the core purification unit, ensuring a stable and optimized contact time between hydrogen and the adsorbent. The pretreatment unit avoids the purification efficiency decline caused by flow fluctuations or impurity interference in traditional methods, improving the overall process stability and economy, and creating reliable conditions for subsequent deep purification. The core purification unit uses a primary adsorption tower and a secondary adsorption tower connected in series, filled with a high-efficiency dehydrogenating metal getter and a chemically active oxide adsorbent, respectively. The first stage uses the high-efficiency dehydrogenating metal getter to perform high-capacity, partially reversible chemical and physical adsorption of hydrogen, rapidly removing the main hydrogen load (e.g., from ≤1000ppm to single-digit ppm levels). The second stage uses the catalytic oxidation of the chemically active oxide adsorbent to convert residual trace hydrogen into water and adsorb it, achieving "refining" from ppm to sub-ppm levels. The core purification unit fundamentally solves the separation problem caused by the similar molecular properties of hydrogen and helium, stably removing hydrogen from helium from ≤1000ppm to ≤0.5ppm, thus meeting the stringent requirements of ultra-high purity helium in aerospace and other fields. The purified helium is then precisely filtered (filtration accuracy up to 0.01 micrometers or higher) by a precision filter in the post-treatment unit, trapping ultrafine particles that may be carried away from the adsorbent bed, ensuring the absolute cleanliness of the output gas. An online hydrogen analyzer monitors the hydrogen content in real time, enabling process quality control. The post-treatment monitoring unit effectively prevents byproduct residues or secondary pollution, avoiding the complexity of the additional dehydration step required by traditional catalytic oxidation methods and simplifying the post-treatment process. This application constructs a systematic process route of "pretreatment - two-stage composite deep purification - post-treatment monitoring" and adopts a composite purification mechanism of "highly efficient physicochemical adsorption + deep catalytic conversion," achieving the ultimate removal of hydrogen from helium. This ensures full process controllability from raw material pretreatment and two-stage deep purification to terminal monitoring, improving the operational reliability and consistency of the device. Through the collaboration of each unit, this application achieves deep hydrogen removal without introducing other products, maintaining the simplicity of the process flow, thereby ensuring high working efficiency and reducing energy consumption and maintenance costs. It is particularly suitable for industrial scenarios that require a continuous and stable supply of ultra-high purity helium. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 A functional module diagram of a deep hydrogen removal device for helium purification provided in an embodiment of this application; Figure 2 A functional module schematic diagram of a deep hydrogen removal device for helium purification provided in another embodiment of this application; Figure 3 This application provides a schematic flowchart of a deep hydrogen removal method for helium purification according to one embodiment.

[0019] In the picture: 100. Pretreatment unit; 101. Pre-filter; 102. Gas flow regulating device; 200. Core purification unit; 201. Primary adsorption tower; 202. Secondary adsorption tower; 300. Post-processing monitoring unit; 301. Precision filter; 302. Online hydrogen analyzer; 400. Control Unit. Detailed Implementation

[0020] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0021] To make the above-mentioned objectives, features and advantages of this application more apparent and understandable, the application will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0022] In one exemplary embodiment, such as Figure 1 As shown, a deep hydrogen removal device for helium purification is provided, which, according to the process flow, includes a pretreatment unit 100, a core purification unit 200, and a post-treatment monitoring unit 300, wherein: The pretreatment unit 100 receives raw helium (untreated hydrogen-containing helium) and performs pretreatment. It includes a pre-filter 101 and a gas flow regulating device 102 connected in sequence. The pre-filter 101 is preferably a high-efficiency particulate filter with a filtration accuracy of not less than 1 micrometer. It is used to filter out solid particles, oil mist, and other mechanical impurities that may be carried in the raw helium, preventing them from contaminating or clogging the downstream adsorbent, thus achieving preliminary filtration. The gas flow regulating device 102 is used to precisely control the flow rate of helium entering the core purification unit 200, creating stable process conditions for subsequent deep purification.

[0023] The core purification unit 200 is the core component of the deep hydrogen removal device for helium purification, enabling deep hydrogen removal. Its inlet is connected to the outlet of the pretreatment unit 100 via a pipeline. The core purification unit 200 includes a primary adsorption tower 201 and a secondary adsorption tower 202 connected in series. The primary adsorption tower 201 is filled with a highly efficient dehydrogenating metal getter, and the secondary adsorption tower 202 is filled with a chemically active oxide adsorbent. The two adsorption towers are connected in series; the primary adsorption tower 201 first removes the main load, and then the secondary adsorption tower 202 performs "refining." This collaborative purification mechanism is key to achieving deep hydrogen removal in this application.

[0024] The post-treatment monitoring unit 300 ensures the final purity and quality of the output helium. Its inlet is connected to the outlet of the core purification unit 200 (i.e., the secondary adsorption tower 202) via a pipeline. The post-treatment monitoring unit 300 includes a precision filter 301 and an online hydrogen analyzer 302 connected in sequence. The precision filter 301 has a higher filtration accuracy than the pre-filter 101, typically reaching 0.01 micrometers or higher, and is used to trap trace amounts of adsorbent dust or other ultrafine particles that may be carried out during the purification process, ensuring the cleanliness of the output gas. The online hydrogen analyzer 302 is used for real-time, continuous monitoring of the hydrogen concentration in the final purified helium. The online hydrogen analyzer 302 preferably employs a high-sensitivity gas chromatograph, laser spectrometer, or dedicated electrochemical hydrogen sensor, with a detection limit of at least 0.1 ppm to ensure accurate determination of whether the product gas meets the purity requirement of ≤0.5 ppm.

[0025] In this implementation, the pre-filter 101 in the pretreatment unit 100 initially filters and removes solid particles and oil mist from the raw helium gas, preventing contamination or blockage of the downstream adsorbent. Simultaneously, the gas flow regulating device 102 precisely controls the helium flow rate entering the core purification unit 200, ensuring a stable and optimized contact time between hydrogen and the adsorbent. The pretreatment unit 100 avoids the decrease in purification efficiency caused by flow fluctuations or impurity interference in traditional methods, improving the overall process stability and economy, and creating reliable conditions for subsequent deep purification. The core purification unit 200 uses a primary adsorption tower 201 and a secondary adsorption tower 202 connected in series, filled with a high-efficiency dehydrogenating metal getter and a chemically active oxide adsorbent, respectively. The first stage uses the high-efficiency dehydrogenating metal getter to perform high-capacity, physical and chemical adsorption of hydrogen, rapidly removing the main hydrogen load (e.g., from ≤1000ppm to single-digit ppm levels). The second stage uses the catalytic oxidation of the chemically active oxide adsorbent to convert residual trace hydrogen into water and adsorb it, achieving "refining" from ppm to sub-ppm levels. The core purification unit 200 fundamentally solves the separation problem caused by the similar molecular properties of hydrogen and helium, stably removing hydrogen from helium from ≤1000ppm to ≤0.5ppm, thus meeting the stringent requirements of ultra-high purity helium in aerospace and other fields. The purified helium is then precisely filtered by the precision filter 301 in the post-treatment unit (filtration accuracy up to 0.01 microns or higher), trapping ultrafine particles that may be carried away from the adsorbent bed, ensuring the absolute cleanliness of the output gas. The online hydrogen analyzer 302 monitors the hydrogen content in real time, enabling process quality control. The post-treatment monitoring unit 300 effectively prevents byproduct residue or secondary contamination, avoids the complexity of the additional dehydration step required by traditional catalytic oxidation methods, and simplifies the post-treatment process. This application constructs a systematic process route of "pretreatment - two-stage composite deep purification - post-treatment monitoring" and adopts a composite purification mechanism of "high-efficiency physicochemical adsorption + deep catalytic conversion" to achieve the ultimate removal of hydrogen from helium. This ensures the controllability of the entire process from raw material pretreatment and two-stage deep purification to terminal monitoring, improving the operational reliability and consistency of the device. Through the synergy of each unit, this application maintains the simplicity of the process flow while achieving deep hydrogen removal, reducing energy consumption and maintenance costs, making it particularly suitable for industrial scenarios requiring a continuous and stable supply of ultra-high purity helium.

[0026] As an optional implementation, the gas flow regulating device 102 specifically includes a mass flow meter and a regulating valve (an electrically operated regulating valve in this embodiment). The mass flow meter is used to accurately measure the real-time mass flow rate or standard volume flow rate of the raw material helium, and the regulating valve is used to control the flow rate of the helium after preliminary filtration (in this embodiment, space velocity is used to represent the helium flow rate).

[0027] In this implementation method, by employing a closed-loop flow control scheme including a mass flow meter and a regulating valve, the gas space velocity entering the core purification unit 200 can be strictly controlled within the optimal process window. Space velocity is a key parameter determining the contact time between hydrogen and the adsorbent. If the space velocity is too low, although the contact time is long, the equipment's processing capacity is low, making it uneconomical; if the space velocity is too high, the contact time is insufficient, and the hydrogen is carried out before it can fully react, leading to a decrease in purification efficiency or even penetration. This implementation method, through precise space velocity control, ensures that regardless of fluctuations in the inlet gas load, hydrogen and the two-stage adsorbent can achieve an optimized and stable reaction contact time. This is an important prerequisite for achieving stable and efficient deep dehydrogenation, directly improving the purification efficiency and operational economy of the entire deep hydrogen removal device for helium purification.

[0028] As an alternative implementation method, the high-efficiency dehydrogenation metal getter is a porous alloy body made of multiple metal elements such as zirconium (Zr), vanadium (V), iron (Fe), titanium (Ti), and copper (Cu) through a special sintering process. It possesses extremely high specific surface area and abundant active sites. Its working principle is mainly based on the strong chemisorption of hydrogen molecules. It can efficiently capture and solidify hydrogen into stable metal hydrides within a wide temperature range from room temperature to relatively low temperatures (-50℃ ~ +80℃), thereby achieving the bulk removal of the vast majority of hydrogen (e.g., over 90%) from helium. This high-efficiency dehydrogenation metal getter features large hydrogen absorption capacity, good kinetic performance, and partially reversible adsorption. Its designed hydrogen absorption efficiency can reach over 1000 liters of hydrogen per kilogram of adsorbent.

[0029] As an alternative implementation method, chemically active oxide adsorbents typically use high-specific-surface-area alumina (Al2O3) or other porous ceramics as a support, loaded with active metals such as palladium (Pd), platinum (Pt), and manganese (Mn) or their oxides. Its working principle differs from that of the primary adsorption tower 201, primarily relying on a catalytic oxidation mechanism. When helium gas containing trace amounts of residual hydrogen passes through the secondary adsorption tower 202, under the catalytic action of the chemically active oxide adsorbent, hydrogen (H2) reacts with trace amounts of oxygen (O2) that may be present in the helium or with oxygen in the adsorbent lattice, generating water (H2O). The generated water molecules are then captured and fixed by the strong physical adsorption capacity of the adsorbent support.

[0030] The core innovation of this application lies in its two-stage composite purification process, which uses a "high-efficiency dehydrogenating metal getter" and a "chemically active oxide adsorbent" in series. The first stage utilizes the high-capacity, irreversible chemical adsorption characteristics of the high-efficiency dehydrogenating metal getter for hydrogen, acting like a "hydrogen storage tank" to rapidly and significantly remove the main hydrogen load from the feed gas, reducing the concentration from hundreds of ppm to single ppm levels. This solves the problem of efficiency degradation in traditional methods at higher hydrogen concentrations. The second stage utilizes the catalytic oxidation function of the chemically active oxide adsorbent to specifically target the trace amounts of hydrogen remaining after the first stage, converting it into water and adsorbing it, acting like a "precision polisher" to achieve a breakthrough from ppm to sub-ppm. This "division of labor and cooperation, step-by-step breakthrough" strategy overcomes the contradiction between capacity and precision faced by single purification technologies, and is the fundamental reason why this application can consistently achieve a purification index of ≤0.5 ppm.

[0031] As an optional implementation, both the primary adsorption tower 201 and the secondary adsorption tower 202 adopt a detachable modular cylindrical structure. Each adsorption tower has a finned or coiled heat dissipation structure on its exterior. The inlet and outlet of each adsorption tower are connected using quick-connect couplings.

[0032] This implementation method, with its modular and detachable design, allows for easy removal of the entire adsorption tower from the pipeline when a stage of the adsorbent reaches saturation or deactivation. The tower can then be replaced with a spare or transported to a dedicated area for adsorbent replacement and regeneration. This significantly simplifies maintenance, reduces downtime, and improves the availability and ease of maintenance of the deep hydrogen removal unit for helium purification. The external heat dissipation structure effectively dissipates heat generated during the adsorption reaction (especially the chemisorption heat of the first stage), preventing excessively high local temperatures in the adsorbent bed from affecting adsorption performance or even damaging the adsorbent. This ensures the purification process proceeds under safe and stable temperature conditions, extending the adsorbent's lifespan.

[0033] As an optional implementation, see [link to implementation details]. Figure 2 The deep hydrogen removal device for helium purification also includes a control unit 400, which includes: Temperature sensors are respectively installed inside the primary adsorption tower 201 and the secondary adsorption tower 202 to monitor the temperature inside the primary adsorption tower 201 and the secondary adsorption tower 202 in real time. Pressure sensors are respectively installed at the inlet and outlet of the core purification unit 200 to monitor the pressure difference between the inlet and outlet of the core purification unit 200 in real time. The PLC controller receives temperature signals from the temperature sensor, differential pressure signals from the pressure sensor, helium flow rate signals from the gas flow regulator 102, and hydrogen concentration signals from the online hydrogen analyzer 302. Based on all the received signals, the PLC controller adjusts the gas flow regulator 102 in real time to control the helium flow rate.

[0034] As an optional implementation, the step of controlling the gas flow rate regulation device 102 in real time according to all received signals to control the helium flow rate specifically includes: when the temperature of any temperature sensor rises abnormally above the set safety threshold, or the pressure difference of the core purification unit 200 continues to increase above the allowable value, or the hydrogen concentration continues to exceed the preset concentration, the PLC controller regulates the regulating valve of the gas flow rate regulation device 102 to execute the instruction to reduce the helium flow rate.

[0035] In this embodiment, the mass flow meter feeds back the measurement signal to the control unit 400, and the control unit 400 determines the process space velocity (e.g., 500 h⁻¹) based on a preset process space velocity value. -1 up to 2000 h -1 Based on the range and cross-sectional area of ​​the adsorption tower, the corresponding target volumetric flow rate is calculated, and the opening degree of the electric regulating valve is controlled by the output signal to achieve precise and stable flow rate regulation.

[0036] In implementing this method, this application incorporates key parameters such as temperature, pressure difference, and purity into real-time monitoring and closed-loop control. An abnormally high bed temperature may indicate rapid adsorbent saturation and a vigorous reaction, and is also an important indirect indicator of the remaining adsorbent capacity. An increased system pressure difference may indicate adsorbent pulverization, bed caking, or filter blockage. The intelligent monitoring and coordinated control of these parameters by the control unit 400 provides advanced warning and automatic protection for the operating status of the deep hydrogen removal device for helium purification. It not only ensures that the purity of the output helium meets standards at all times but also prevents the equipment from operating under abnormal conditions, avoiding irreversible damage to the adsorbent, and significantly improving the safety, reliability, and intelligence level of the device operation.

[0037] As an optional implementation, the online hydrogen analyzer 302 employs a trace hydrogen analyzer based on transducer laser absorption spectroscopy (TDLAS). Trace hydrogen analyzers based on transducer laser absorption spectroscopy offer advantages such as fast response time (down to the second level), high sensitivity (detection limit down to the ppb level), accurate measurement, good stability, and no need for carrier gas.

[0038] In this implementation method, a high-sensitivity laser absorption spectroscopy trace hydrogen analyzer serves as the final "judge" of purity, providing ultimate assurance for achieving the deep hydrogen removal target of this application. Its extremely high sensitivity ensures accurate detection of hydrogen concentrations as low as 0.5 ppm, providing a reliable basis for quality control. The rapid response capability allows for immediate monitoring of even minor fluctuations in the purification process or near-deterioration of the adsorbent, providing timely feedback signals to the control unit 400 for rapid adjustment or early warning. This online, real-time, and precise monitoring method elevates product quality control from post-process laboratory sampling inspection to continuous in-process monitoring, significantly improving the consistency and reliability of the product gas quality, a necessary condition for meeting the stringent quality requirements of aerospace and other fields.

[0039] In summary, the deep hydrogen removal device for helium purification provided in this application, through the synergistic effect of the aforementioned units and their specific implementation methods, constitutes a complete technical system encompassing raw material pretreatment, two-stage composite deep purification, product end-product assurance, and end-to-end intelligent monitoring. It not only innovatively combines the advantages of both chemical adsorption and catalytic oxidation mechanisms in principle, solving the technical bottleneck of deep hydrogen removal, but also ensures the high efficiency, stability, safety, and maintainability of the technology through precise flow control, modular design, intelligent monitoring, and scientific calculations in engineering implementation. This effectively meets the urgent needs of high-end industries such as aerospace and semiconductors for ultra-high purity helium.

[0040] Based on the same inventive concept, this application also provides a method for deep hydrogen removal in helium purification. The solution provided by this method is similar to the solution described above. Therefore, the specific limitations of one or more embodiments of the deep hydrogen removal method for helium purification provided below can be found in the limitations of the deep hydrogen removal device for helium purification described above, and will not be repeated here.

[0041] In one exemplary embodiment, such as Figure 3 As shown, a deep hydrogen removal method for helium purification is provided, specifically including: Step 101: The hydrogen-containing helium gas is pretreated by the pretreatment unit 100, the pretreatment including preliminary filtration and adjustment of the helium flow rate.

[0042] In this embodiment, the raw helium gas to be purified is introduced into a deep hydrogen removal device for helium purification. The raw helium gas first enters the pretreatment unit 100. The initial hydrogen concentration in the raw helium gas is typically no higher than 1000 ppm, and it may contain particulate impurities. In the pre-filter 101, solid particles, oil, and other mechanical impurities in the raw helium gas are effectively filtered out. Subsequently, the purified raw helium gas enters the gas flow regulating device 102. The control unit 400, according to preset process parameters (such as target space velocity), precisely controls the volumetric flow rate of helium within a certain range by adjusting the valve opening in the gas flow regulating device 102. The purpose of this step is to provide clean and stable flow rate raw gas for the subsequent core purification process, avoiding flow fluctuations or impurities from impacting or damaging the adsorbent performance. Precise control of the flow rate (or space velocity) is crucial to ensuring sufficient and constant contact reaction time between hydrogen and the adsorbent.

[0043] Step 102: The pretreated helium is subjected to two dehydrogenation treatments through the core purification unit 200; the first treatment is performed by a highly efficient dehydrogenation metal getter; the second treatment is performed by a chemically active oxide adsorbent.

[0044] In this embodiment, helium gas, after preliminary purification and flow regulation, flows from the pretreatment unit 100 and enters the core purification unit 200. The helium gas first passes through a primary adsorption tower 201. In the primary adsorption tower 201, the helium gas comes into full contact with a highly efficient dehydrogenating metal getter. The highly efficient dehydrogenating metal getter, through its abundant active metal sites on its surface and within its pores, exerts a strong chemical adsorption effect on hydrogen molecules. The hydrogen molecules are dissociated into hydrogen atoms and diffuse into the alloy lattice, forming stable metal hydrides, which are then irreversibly fixed. This process can remove the vast majority of hydrogen from the helium gas, rapidly reducing the hydrogen concentration from an initial level of several hundred ppm to ppm or even lower. This process is typically accompanied by slight exothermic activity, which can be monitored by a temperature sensor 203.

[0045] Subsequently, the helium gas, having undergone primary deep dehydrogenation and significantly reduced hydrogen concentration, enters the secondary adsorption tower 202. In the secondary adsorption tower 202, the helium gas comes into contact with the chemically active oxide adsorbent. For the remaining hydrogen gas, which is already at a very low concentration (e.g., a few ppm to sub-ppm), the chemically active oxide adsorbent performs catalytic oxidation. Under the action of the catalyst active component (such as palladium), the remaining hydrogen gas and trace amounts of oxygen carried in the helium gas (or lattice oxygen provided by the adsorbent) undergo an oxidation reaction at a lower temperature, generating water vapor. The generated water molecules are immediately and firmly captured by the high specific surface area carrier of the chemically active oxide adsorbent (such as alumina) through physical adsorption. This process achieves the final "sweeping" of trace hydrogen gas, reducing its concentration to a minimum of 0.5 ppm or even lower. Through the synergistic treatment of the two adsorption towers, the hydrogen gas in the helium gas is deeply and thoroughly removed.

[0046] Step 103: The helium gas after two dehydrogenation treatments is precisely filtered by the post-processing monitoring unit 300, and the hydrogen content in the precisely filtered helium gas is monitored, and finally high-purity helium gas is output.

[0047] In this embodiment, the helium gas, which has undergone deep dehydrogenation and flows out from the secondary adsorption tower 202 of the core purification unit 200, enters the post-processing monitoring unit 300. The helium gas first passes through a precision filter 301, where any extremely fine particles that may be generated during the purification process (such as trace amounts of powder generated by friction of the adsorbent) are ultimately intercepted, ensuring the absolute cleanliness of the output gas and meeting the requirements for use in precision instruments. Then, the clean helium gas flows through an online hydrogen analyzer 302. The online hydrogen analyzer 302 performs real-time, online, and accurate measurement of the residual hydrogen concentration in the helium gas and continuously transmits the concentration data to the control unit 400.

[0048] The control unit 400 compares and judges the hydrogen concentration value detected by the online hydrogen analyzer 302 with the preset target value (e.g., ≤0.5ppm). If the detected value remains consistently lower than the target value, it indicates that the purification process is operating normally and the product gas is qualified. At this time, the purified high-purity helium gas (purity ≥99.999%, H2≤0.5ppm) can be delivered to the point of use or storage device. If the online hydrogen analyzer 302 detects an abnormal rise in hydrogen concentration and exceeds the alarm threshold, the control unit 400 will immediately issue an audible and visual alarm and can take corresponding measures according to the preset program, such as reducing the processing volume, prompting maintenance, or automatically shutting down, thereby ensuring the absolute reliability of the product gas quality.

[0049] By implementing steps 101 to 103 above, the deep hydrogen removal method for helium purification provided in this application can systematically purify helium containing hydrogen impurities (≤1000ppm) to an ultra-high purity level (H2≤0.5ppm) that meets the highest standards required for aerospace and other applications. The entire method has a clear process flow, with each step having a defined function and being interconnected. Combined with automated control, it achieves efficient, stable, and reliable industrial applications of deep hydrogen removal.

[0050] As an optional implementation, the hydrogen-containing helium space velocity during the first dehydrogenation treatment is 500 h⁻¹. -1 up to 2000 h -1 The contact time between hydrogen-containing helium gas and the highly efficient dehydrogenating metal getter is 2 to 10 seconds.

[0051] As an optional implementation, the deep hydrogen removal method for helium purification further includes: The working status of the two adsorbents is determined by monitoring the temperature changes of the two adsorbent beds in the core purification unit 200. When the temperature of either adsorbent bed rises abnormally, the helium flow rate is adjusted or the adsorbent replacement procedure is executed.

[0052] As an optional implementation, by monitoring the pressure difference of the core purification unit 200 and the hydrogen concentration in the output helium, if the pressure difference is detected to continuously increase beyond the allowable value or the hydrogen concentration is detected to continuously exceed the preset concentration, a procedure to reduce the helium flow rate is executed.

[0053] As an optional implementation, before or during the design phase of the deep hydrogen removal unit for helium purification, the minimum loading amount of high-efficiency dehydrogenation metal getter required for the primary adsorption tower 201 is precisely calculated based on the maximum inlet hydrogen concentration of the raw helium, the designed processing flow rate, the planned operating cycle (or adsorbent replacement cycle), the nominal hydrogen absorption efficiency of the selected high-efficiency dehydrogenation metal getter, and the hydrogen density. The calculation formula is: m=(C in ×F×t) / (η×ρ); In the formula, m is the mass (in kilograms) of the required high-efficiency dehydrogenation metal getter, and C in The hydrogen volume concentration at the inlet of the core purification unit 200 (unit: ppm, needs to be converted to volume fraction for calculation), F is the standard volumetric flow rate of helium (unit: standard cubic meters / hour), t is the design operating cycle (unit: hours), η is the design hydrogen absorption efficiency of the high-efficiency dehydrogenation metal getter (unit: standard liters of hydrogen / kg of adsorbent), and ρ is the density of hydrogen under standard conditions (unit: kg / standard cubic meter). To ensure reliability, the actual filling amount is usually multiplied by a safety factor of 1.5 to 2.0 based on the above calculated value m.

[0054] By implementing this method and introducing this scientific quantitative calculation formula, this application changes the traditional, crude approach of relying on experience to estimate adsorbent dosage. This formula comprehensively considers core variables such as inlet gas load (concentration × flow rate), operating time, and adsorbent performance, enabling precise calculation of the minimum theoretical adsorbent dosage required to meet specific purification tasks and operating cycles. Furthermore, a safety factor is added to ensure that, even in the face of fluctuations in inlet gas concentration or slight degradation of adsorption performance over long-term operation, the adsorption tower still has sufficient buffer capacity to prevent premature hydrogen penetration, thus guaranteeing the absolute reliability and stability of the purification effect of the deep hydrogen removal device for helium purification throughout the entire operating cycle. This achieves a balance between precise technical design and economic cost optimization.

[0055] 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.

[0056] This document uses specific examples to illustrate the principles and implementation methods of this application. The descriptions of the above embodiments are only for the purpose of helping to understand the methods and core ideas of this application. Furthermore, those skilled in the art will recognize that, based on the ideas of this application, there will be changes in the specific implementation methods and application scope. Therefore, the content of this specification should not be construed as a limitation of this application.

Claims

1. A deep hydrogen removal device for helium purification, characterized in that, The deep hydrogen removal device for helium purification includes: The pretreatment unit includes a pre-filter and a gas flow regulating device connected in sequence, for pretreating untreated helium gas, the pretreatment including preliminary filtration and adjustment of helium gas flow rate; The core purification unit includes a primary adsorption tower and a secondary adsorption tower arranged in series. The primary adsorption tower is filled with a highly efficient dehydrogenating metal getter, and the secondary adsorption tower is filled with a chemically active oxide adsorbent. The core purification unit is used to perform two dehydrogenation treatments on the pretreated helium. The post-processing monitoring unit includes a precision filter and an online hydrogen analyzer connected in sequence. The post-processing monitoring unit is used to perform precision filtration on the helium after two dehydrogenation treatments and monitor the hydrogen content in the precision-filtered helium. The pretreatment unit, the core purification unit, and the post-treatment monitoring unit are connected in series.

2. The deep hydrogen removal device for helium purification according to claim 1, characterized in that, The gas flow regulating device includes: A mass flow meter, used to measure the real-time mass flow rate or standard volume flow rate of helium after preliminary filtration; A regulating valve is used to control the flow rate of helium gas after preliminary filtration.

3. The deep hydrogen removal device for helium purification according to claim 1, characterized in that, The effective dehydrogenation metal getter is a porous alloy containing zirconium, vanadium, iron, titanium, and copper; the chemically active oxide adsorbent is a composite material with porous oxide as a carrier and loaded with catalytically active metal components.

4. The deep hydrogen removal device for helium purification according to claim 1, characterized in that, The primary adsorption tower and the secondary adsorption tower are detachable structures, and both the primary adsorption tower and the secondary adsorption tower have heat dissipation structures on their outer walls.

5. The deep hydrogen removal device for helium purification according to claim 1 or 2, characterized in that, The deep hydrogen removal device for helium purification also includes a control unit, which includes: Temperature sensors are respectively installed inside the primary adsorption tower and the secondary adsorption tower to monitor the temperature inside the primary adsorption tower and the secondary adsorption tower in real time. Pressure sensors are installed at the inlet and outlet of the core purification unit to monitor the pressure difference between the inlet and outlet of the core purification unit in real time. The PLC controller receives temperature signals from the temperature sensor, differential pressure signals from the pressure sensor, helium flow rate signals from the gas flow regulator, and hydrogen concentration signals from the online hydrogen analyzer. Based on all the received signals, it adjusts the gas flow regulator in real time to control the helium flow.

6. The deep hydrogen removal device for helium purification according to claim 5, characterized in that, The method of controlling the gas flow rate regulation device in real time according to all received signals to control the helium flow rate specifically includes: when the temperature of any temperature sensor rises abnormally above the set safety threshold, or the pressure difference of the core purification unit continues to increase above the allowable value, or the hydrogen concentration continues to exceed the preset concentration, the PLC controller regulates the gas flow rate regulation device to execute the instruction to reduce the helium flow rate.

7. A deep hydrogen removal method for helium purification, characterized in that, The deep hydrogen removal method for helium purification includes: The hydrogen-containing helium gas is pretreated by a pretreatment unit, which includes preliminary filtration and adjustment of the helium flow rate. The pretreated helium undergoes two dehydrogenation treatments through the core purification unit; the first treatment uses a highly efficient dehydrogenation metal getter, and the second treatment uses a chemically active oxide adsorbent. The helium gas after two dehydrogenation processes is precisely filtered by the post-processing monitoring unit, and the hydrogen content in the precisely filtered helium gas is monitored, ultimately outputting high-purity helium gas.

8. The deep hydrogen removal method for helium purification according to claim 7, characterized in that, The hydrogen-containing helium space velocity during the first dehydrogenation process is 500 h⁻¹. -1 up to 2000 h -1 The contact time between hydrogen-containing helium gas and the highly efficient dehydrogenating metal getter is 2 to 10 seconds.

9. The deep hydrogen removal method for helium purification according to claim 7, characterized in that, The deep hydrogen removal method for helium purification also includes: The working status of the two adsorbents is determined by monitoring the temperature changes of the bed layers of the two adsorbents in the core purification unit. When the bed temperature of either adsorbent rises abnormally, the helium flow rate is adjusted or the adsorbent replacement procedure is executed.

10. The deep hydrogen removal method for helium purification according to claim 7, characterized in that, The loading amount of the high-efficiency dehydrogenating metal getter is calculated in the following way: m=(C in ×F×t) / (η×ρ); In the formula, m is the mass of the required high-efficiency dehydrogenation metal getter, and C in η is the hydrogen volume concentration at the inlet of the core purification unit, F is the standard volume flow rate of helium, t is the design operating cycle, η is the design hydrogen absorption efficiency of the high-efficiency dehydrogenation metal getter, and ρ is the density of hydrogen under standard conditions.

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