A natural gas crude helium selective adsorption and impurity removal purification device and a working method thereof

Abstract

The application discloses a natural gas crude helium selective adsorption and impurity removal and purification device and a working method thereof, and belongs to the technical field of natural gas crude helium purification. The device comprises a first sealing valve, a first-stage shell, a second sealing valve, a second-stage shell, a third sealing valve, a third-stage shell, a flange for sealing the third-stage shell, a first low-temperature plate system, a second low-temperature plate system, a third low-temperature plate system and a male and female head. The first-stage shell, the second-stage shell and the third-stage shell are connected with the first sealing valve, the second sealing valve and the third sealing valve through flanges at front and rear ends respectively, and the rear flange of the third-stage shell is connected with the flange for sealing the third-stage shell. The first low-temperature plate system, the second low-temperature plate system and the third low-temperature plate system are arranged in the first-stage shell, the second-stage shell and the third-stage shell respectively. The application improves the helium purification efficiency and adsorption cycle stability through staged low-temperature adsorption, reduces energy consumption, and provides an efficient and feasible technical scheme for natural gas crude helium purification.

Description

Technical Field

[0001] This invention belongs to the field of crude helium purification technology for natural gas, and in particular relates to a selective adsorption purification device for crude helium in natural gas and its working method. Background Technology

[0002] Against the backdrop of ever-increasing demand for energy and industrial gases, helium, as a strategic resource with unique physical properties such as ultra-low boiling point, high thermal conductivity, and chemical inertness, plays an indispensable role in high-end fields such as aerospace, cryogenic superconductivity, and semiconductor manufacturing. However, helium is scarce in nature, and extracting crude helium from natural gas and purifying it has become one of the important ways to obtain helium.

[0003] Currently, the main purification technologies for crude helium from natural gas include cryogenic condensation, pressure swing adsorption (PSA), and membrane separation. While cryogenic condensation can achieve high-purity helium separation, it consumes a huge amount of energy and involves complex equipment. PSA requires extremely high-performance adsorbents, and its adsorption and desorption processes have limited efficiency. Membrane separation's separation effect is limited by the selectivity and permeation flux of the membrane material, making it difficult to meet the demands of large-scale, high-purity helium purification. Furthermore, existing purification devices suffer from structural design flaws, such as insufficient sealing leading to gas leakage, a simplistic combination of cryogenic plate systems affecting adsorption efficiency, and significant heat transfer losses in connecting components. These issues severely restrict the efficiency and economic viability of crude helium purification from natural gas.

[0004] Currently, the technical solutions for helium purification include:

[0005] A helium purification system capable of removing hydrogen and neon (CN114988377B) is disclosed. This patent focuses on removing hydrogen and neon impurities from helium. However, the system has the following technical shortcomings: First, the impurity treatment mechanism is singular and cannot meet the needs of comprehensive purification; second, the process is complex, resulting in high maintenance difficulty and poor deployment flexibility; third, at the connection between the refrigeration unit and the device, there is significant loss of cold air and a high risk of helium leakage, which greatly affects the system's operational stability and helium purity.

[0006] A lightweight, adsorption- and desorption-resistant adsorption tower and its coating process, helium purification system and method (CN119303406A). This patent focuses on structural innovation of the adsorption tower and optimization of the coating process. The adsorption tower is constructed using lightweight materials, reducing transportation and installation costs. A unique coating process is applied inside the adsorption tower, improving the bonding stability between the adsorbent and the tower body. However, this patent does not fully consider the differences in adsorption characteristics of different impurity gases under different temperature and pressure conditions, and lacks an efficient selective adsorption strategy for the removal of common impurities such as methane, nitrogen, and hydrogen.

[0007] A system and method for cryogenic separation and purification of crude helium gas (CN118203949A) is disclosed. This patent is primarily based on the principle of cryogenic separation, achieving separation by gradually cooling the crude helium gas and utilizing the phase transition differences of different impurity gases at low temperatures. However, this method consumes a large amount of energy and poses severe challenges to the sealing and material properties of the equipment in cryogenic environments. Furthermore, the separation effect is poor for some impurity gases with similar boiling points (such as nitrogen and hydrogen), making it unsuitable for selective adsorption purification of crude helium from natural gas.

[0008] Therefore, developing a highly efficient, energy-saving, and reliable device for the selective adsorption and purification of crude helium in natural gas is of great practical significance for improving the purification efficiency of crude helium in natural gas and reducing production costs. Summary of the Invention

[0009] To address the aforementioned technical problems, this invention relates to a crude helium selective adsorption purification device for natural gas and its operating method, aiming to achieve efficient, energy-saving, and stable separation of multiple components of natural gas by optimizing the device structure and improving the workflow.

[0010] To achieve the above objectives, the present invention provides the following technical solution:

[0011] A crude helium selective adsorption purification device for natural gas includes a first sealing valve, a primary shell, a second sealing valve, a secondary shell, a third sealing valve, a tertiary shell, a flange sealing the tertiary shell, a first cryogenic plate system, a second cryogenic plate system, a third cryogenic plate system, and male and female connectors.

[0012] The specific connection relationships are as follows: the front and rear ends of the primary, secondary, and tertiary shells are connected to the first, second, and third sealing valves respectively via flanges, and the rear flange of the tertiary shell is connected to the flange sealing the tertiary shell. The first, second, and third cryogenic plate systems are located inside the primary, secondary, and tertiary shells respectively.

[0013] Furthermore, the primary, secondary, and tertiary shells are each equipped with a refrigerant inlet, a refrigerant outlet, and a regeneration gas outlet. Both the refrigerant inlet and outlet are provided with male and female connectors.

[0014] Furthermore, the first, second, and third sealing valves each include an actuator, a valve seat, a valve disc, a first rotating shaft, a second rotating shaft, a fixing cover for the first seal, a first seal, a second seal, and a fixing cover for the second seal.

[0015] The specific connection relationship is as follows: the valve disc is located inside the valve seat and is connected to the first rotating shaft and the second rotating shaft. The actuator is connected to the valve disc through the first rotating shaft. The first seal and the second seal are respectively assembled on both sides of the valve disc through the fixing cover plate of the first seal and the fixing cover plate of the second seal.

[0016] Furthermore, the valve disc has an adjustable rotation range of 0°-90°, and the valve disc is provided with a bidirectional sealing groove structure. The valve disc achieves bidirectional sealing through a first sealing element and a second sealing element.

[0017] Furthermore, the cross-sectional shape of both the first and second seals is a shape consisting of a curved section connected to a straight section.

[0018] Furthermore, the first, second, and third cryogenic plate systems are all composed of multiple cryogenic plates connected in series and in parallel.

[0019] Furthermore, the cryogenic plate is composed of a refrigerant channel and fins. The refrigerant channel can be cylindrical or other shapes. The fins can be cuboid or other shapes. The surface of the fins is coated with a selective adsorbent.

[0020] Furthermore, the male and female connectors include a first male pipe, a second male pipe, a third male pipe, a male flange, a female flange, a seal for the male and female flanges, a first female pipe, a second female pipe, a third female pipe, a connector for the second and third male pipes, a heat insulation ring, and a connector for the second and third female pipes.

[0021] The specific connection relationships are as follows: the male flange is connected to the first and third pipes of the male connector, the male connector fitting is connected to the second and third pipes of the male connector, the fitting is connected to the insulation ring, the female flange is connected to the first and second pipes of the female connector, the female connector fitting is connected to the second and third pipes of the female connector, the sealing element is located between the male and female flanges, and the insulation ring is in contact with the female connector fitting.

[0022] Furthermore, the cross-section of the third tube of the male connector and the second tube of the female connector are both rectangular threaded, but not limited to rectangular threaded. The first tube of the male connector is provided with a male evacuation port, and the first tube of the female connector is provided with a female evacuation port.

[0023] A method for operating the above-mentioned crude natural gas helium selective adsorption purification device is as follows:

[0024] When the natural gas crude helium selective adsorption purification device is in operation, a vacuum operation is first performed on the device using a vacuum pump to remove the original gas inside. Then, the first, second, and third cryogenic plate systems are cooled, and then the first, second, and third sealing valves are opened sequentially. As the raw gas passes through the primary, secondary, and tertiary shells, impurities are selectively adsorbed by the cryogenic plate systems. The purified helium is then extracted and collected. Afterward, the first, second, and third sealing valves are closed sequentially, and the first, second, and third cryogenic plate systems are heated to regenerate the gas molecules adsorbed on the cryogenic plate systems. The regenerated gas from the primary, secondary, and tertiary shells is discharged through the regeneration gas outlets on the shells, and finally, the discharged gas is recovered.

[0025] The beneficial effects of this invention are as follows:

[0026] 1. A three-stage gradient low-temperature plate system (80K / 40K / 15K) and surface-functionalized adsorbents are synergistically designed to achieve... , , Through the stepwise removal of impurity gases, the helium recovery rate is increased to over 95%, and the purity is higher than 99.999%.

[0027] 2. The cryogenic plate system employs a combination of series and parallel connections, optimizing fluid distribution and heat and mass transfer efficiency. Furthermore, the combination of the cryogenic plate system and the type of adsorbent on the cryogenic plate surface can be adjusted according to the composition of the feed gas, making it suitable for purification of different gas sources. In addition, through cryogenic adsorption and controlled temperature regeneration, energy consumption can be reduced by 30% to 50% compared to traditional high-temperature desorption processes.

[0028] 3. The male and female connectors adopt a quick-plug connection structure, reducing the difficulty of assembly. The rectangular thread design, combined with the heat insulation ring and the pipe cross-section, effectively reduces heat loss.

[0029] 4. The double-sided sealing groove and special cross-section sealing element of the sealed valve have a leakage rate of less than [percentage missing] under high pressure (maximum 5 MPa) and low temperature (minimum 4.5 K) conditions. .

[0030] 5. This invention employs a modular design for easy online maintenance, and individual modules can be isolated in case of failure. Furthermore, the modular design allows for flexible addition or removal of processing modules based on the composition of the raw gas, enabling rapid deployment of the device on mobile platforms such as vehicle-mounted or skid-mounted units. Attached Figure Description

[0031] Figure 1 A schematic diagram of a crude helium selective adsorption purification unit for natural gas.

[0032] Figure 2A schematic cross-sectional view of a crude helium selective adsorption depurification and purification unit for natural gas.

[0033] Figure 3 This is a schematic diagram of the structure of a sealing valve;

[0034] Figure 4 A cross-sectional structural diagram of a sealing valve;

[0035] Figure 5 for Figure 4 A magnified view of a portion at point H;

[0036] Figure 6 A schematic diagram of the sealing element for a sealing valve;

[0037] Figure 7 This is a schematic diagram of the low-temperature plate.

[0038] Figure 8 This is a schematic diagram of the refrigerant cycle in a low-temperature plate system.

[0039] Figure 9 A schematic diagram of the cross-sectional structure of the male and female heads;

[0040] Figure 10 This is a flowchart of the process for a crude helium selective adsorption purification unit for natural gas.

[0041] The reference numerals in the figures include:

[0042] 1 is the first sealing valve, 101 is the actuator, 102 is the valve seat, 103 is the valve disc, 104 is the first rotating shaft, 105 is the second rotating shaft, 106 is the fixing cover plate of the first sealing element, 107 is the first sealing element, 108 is the second sealing element, 109 is the fixing cover plate of the second sealing element, 110 is the sealing groove for sealing the first rotating shaft, 111 is the fixing hole, 2 is the primary housing, 201 is the refrigerant inlet for cooling the first cryogenic plate system, 202 is the refrigerant outlet for cooling the first cryogenic plate system, and 203 is the regeneration port of the primary housing. Gas outlet; 204 is the front flange of the primary shell; 205 is the rear flange of the primary shell; 3 is the second sealing valve; 4 is the secondary shell; 401 is the refrigerant inlet for cooling the second cryogenic plate system; 402 is the refrigerant outlet for cooling the second cryogenic plate system; 403 is the regeneration gas outlet of the secondary shell; 404 is the front flange of the secondary shell; 405 is the rear flange of the secondary shell; 5 is the third sealing valve; 6 is the tertiary shell; 601 is the refrigerant inlet for cooling the third cryogenic plate system; 602 is the refrigerant outlet for cooling the third cryogenic plate system. The refrigerant outlet is 603, the regeneration gas outlet of the third-stage shell is 604, the front flange of the third-stage shell is 605, the rear flange of the third-stage shell is 7, the flange sealing the third-stage shell is 8, the cryogenic plate is 801, the refrigerant flow channel is 802, the fins are x1, the first cryogenic plate system is x2, the second cryogenic plate system is x3, the third cryogenic plate system is A, the male and female connectors are 9, the first pipe of the male connector is 901, the evacuation port of the male connector is 901, the second pipe of the male connector is 10, the male flange is 11, the female flange is 12, and the male and female flanges are 13. Seals, 14 is the first pipe of the female connector, 1401 is the evacuation port of the female connector, 15 is the second pipe of the female connector, 16 is the third pipe of the male connector, 17 is the male connector connector, 18 is the heat insulation ring, 19 is the female connector connector, 20 is the third pipe of the female connector, L1 is the dehydration and deacidification device, L2 is the cooler, L3 is the buffer tank, L4 is the natural gas crude helium selective adsorption purification device, P1 is the first mechanical pump, P2 is the second mechanical pump, P3 is the third mechanical pump, S1 is the first collection device, S2 is the second collection device, and S3 is the third collection device. Detailed Implementation

[0043] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments. However, the following embodiments are only for explaining the present invention, and the scope of protection of the present invention should include all the contents of the claims. Moreover, through the description of the following embodiments, those skilled in the art can fully implement all the contents of the claims of the present invention.

[0044] Example

[0045] like Figure 1 , 2As shown, the crude helium selective adsorption purification device for natural gas provided in this embodiment mainly consists of three adsorption units connected in series. The first adsorption unit includes a first sealing valve 1, a first-stage shell 2, and a first cryogenic plate system x1; a second sealing valve 3, a second-stage shell 4, and a second cryogenic plate system x2; and a third sealing valve 5, a third-stage shell 6, and a third cryogenic plate system x3.

[0046] The connection methods for each stage of the shell are as follows:

[0047] The front end of the first sealing valve 1 is connected to the raw gas inlet pipeline, and the rear end is connected to the front end of the first-stage shell 2 via a flange; the rear end of the first-stage shell 2 is connected to the front end of the second sealing valve 3 via a flange; the rear end of the second sealing valve 3 is connected to the front end of the second-stage shell 4 via a flange; the rear end of the second-stage shell 4 is connected to the front end of the third sealing valve 5 via a flange; the rear end of the third sealing valve 5 is connected to the front end of the third-stage shell 6 via a flange; the rear end of the third-stage shell 6 is sealed by a sealing flange.

[0048] Each stage of the shell has its own independent cryogenic plate system:

[0049] The first-stage housing 2 houses the first-stage cryogenic plate system x1; the second-stage housing 4 houses the second-stage cryogenic plate system x2; and the third-stage housing 6 houses the third-stage cryogenic plate system x3.

[0050] Furthermore, the locations of the aforementioned flange structure, refrigerant inlet, and refrigerant outlet are as follows: Figure 1 As shown, it specifically includes:

[0051] The refrigerant inlet 201 for cooling the first cryogenic plate system, the refrigerant outlet 202 for cooling the first cryogenic plate system, the regeneration gas outlet 203 for the primary shell, the front flange 204 for the primary shell, and the rear flange 205 for the primary shell.

[0052] The refrigerant inlet 401 for cooling the second cryogenic plate system, the refrigerant outlet 402 for cooling the second cryogenic plate system, the regeneration gas outlet 403 for the secondary shell, the front flange 404 for the secondary shell, and the rear flange 405 for the secondary shell.

[0053] The refrigerant inlet 601 for cooling the third cryogenic plate system, the refrigerant outlet 602 for cooling the third cryogenic plate system, the regeneration gas outlet 603 for the third-stage shell, the front flange 604 for the third-stage shell, the rear flange 605 for the third-stage shell, and the flange 7 for sealing the third-stage shell.

[0054] like Figure 3-6 As shown, the sealing valve (taking the first sealing valve as an example) includes:

[0055] Actuator 101 is used to drive the valve to open and close, with a rotation range of 0° (closed) to 90° (fully open); valve seat 102 constitutes the main structure of the valve; valve disc 103 is installed in the valve seat via a first rotating shaft 104 and a second rotating shaft 105; a first sealing element 107 and a second sealing element 108 are provided with fixing holes 111, which are respectively installed on both sides of the valve disc via fixing cover plates (fixing cover plate 106 of the first sealing element and fixing cover plate 109 of the second sealing element).

[0056] The low-temperature plate system, such as Figure 7 , 8 As shown, it consists of multiple cryogenic plates 8 arranged in a series-parallel hybrid configuration. Each cryogenic plate 8 includes: a refrigerant channel 801, made of copper tubing, through which refrigerants such as liquid nitrogen and liquid helium are circulated; and fins 802, which are rectangular structures made of aluminum alloy and coated with an adsorbent.

[0057] like Figure 9 As shown, the male and female connector A includes a first male pipe 9, a second male pipe 10, a third male pipe 16, a male flange 11, a female flange 12, a sealing element 13 for the male and female flanges, a first female pipe 14, a second female pipe 15, a third female pipe 20, a male connector 17, a heat insulation ring 18, and a female connector 10.

[0058] The specific connection relationships are as follows: Male flange 11 is connected to male first pipe 9 and male third pipe 16 respectively; male connector 17 is connected to male second pipe 10 and male third pipe 16 respectively; male connector 17 is connected to heat insulation ring 18; female flange 12 is connected to female first pipe 14 and female second pipe 15 respectively; female connector 19 is connected to female second pipe 15 and female third pipe 20 respectively; the sealing element 13 of the male and female flanges is located between male flange 11 and female flange 12; heat insulation ring 18 is in contact with female connector 19. Male first pipe 9 is provided with male evacuation port 901, and female first pipe 14 is provided with female evacuation port 1401.

[0059] like Figure 10 As shown, Figure 10 This is a flowchart of the process of a crude helium selective adsorption purification unit for natural gas, wherein: L1 is a dehydration and deacidification unit, L2 is a cooler, L3 is a buffer tank, L4 is a crude helium selective adsorption purification unit for natural gas, P1 is the first mechanical pump, P2 is the second mechanical pump, P3 is the third mechanical pump, S1 is the first collection device, S2 is the second collection device, and S3 is the third collection device.

[0060] To adsorb methane from crude natural gas ( ), nitrogen ( ),hydrogen( For example, the low-temperature plate system is specially configured as follows:

[0061] First low-temperature plate system x1: operating temperature 70-90K (preferably 80K), used for adsorbing methane ( );

[0062] Second low-temperature plate system x2: operating temperature 30-45 K (preferably 40 K), used for nitrogen adsorption ( ) and the remaining methane ( );

[0063] Third low-temperature plate system x3: operating temperature 10-20 K (preferably 15 K), used for deep adsorption of hydrogen ( ) and the remaining nitrogen gas ( It outputs high-purity helium gas.

[0064] Adsorbent preparation:

[0065] The fin 802 surface of the first low-temperature plate system x1 is coated with coconut shell activated carbon adsorbent;

[0066] The fin 802 surface of the second low-temperature plate system x2 is coated with an activated carbon-metal-organic framework composite adsorbent.

[0067] The surface of the fins 802 of the third low-temperature plate system x3 is coated with an activated carbon-metal-organic framework composite adsorbent containing nano-sized copper oxide particles. It utilizes the principle of chemical adsorption reaction between hydrogen and copper oxide to deeply remove hydrogen.

[0068] The working method of the natural gas crude helium selective adsorption depurification and purification device provided in this embodiment is as follows:

[0069] S1: System preparation phase

[0070] Vacuuming to High vacuum.

[0071] S2: Staged start-up of the refrigeration system

[0072] The first stage uses liquid nitrogen cooling to reduce the x1 system to 80 K;

[0073] The second stage uses liquid helium cooling to bring the x2 system down to 40 K;

[0074] The third stage uses liquid helium refrigeration to reduce the x3 system temperature to 15 K.

[0075] S3: Adsorption stage.

[0076] The mixed gas enters the system at a pressure of 0.1-0.3 MPa;

[0077] Primary shell: over 99% methane ( ) is adsorbed by the x1 system;

[0078] Secondary shell: 95% or more nitrogen ( ) is adsorbed by the x2 system;

[0079] Third-stage shell: over 99% hydrogen ( It is adsorbed by the x3 system.

[0080] The purified helium (purity ≥ 99.999%) is discharged from the outlet of the third-stage shell.

[0081] S4: Regeneration phase

[0082] Regeneration: The x1 system is heated to 320-350 K and collected through the primary regeneration gas outlet;

[0083] Regeneration: The x2 system is heated to 100-130 K and collected through the secondary regeneration gas outlet;

[0084] Regeneration: The x3 system is heated to 60-80 K and collected through the three-stage regeneration gas outlet.

[0085] After regeneration is complete, the cooling-adsorption cycle is repeated.

[0086] The above description is merely a specific embodiment of this application, enabling those skilled in the art to understand or implement this application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of this application. Therefore, this application is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features claimed herein.

Claims

1. A selective adsorption purification device for crude helium in natural gas, characterized in that, include: The first sealing valve (1), the first-stage housing (2), the second sealing valve (3), the second-stage housing (4), the third sealing valve (5), and the third-stage housing (6) are connected in series. The flange at the rear end of the sealing three-stage housing (7); The first cryogenic plate system (x1) in the first-stage shell, the second cryogenic plate system (x2) in the second-stage shell, and the third cryogenic plate system (x3) in the third-stage shell. Male and female connectors (A) for connecting refrigerant lines; Each stage of the casing is equipped with a refrigerant inlet, a refrigerant outlet, and a regeneration gas outlet; The first low-temperature plate system (x1), the second low-temperature plate system (x2), and the third low-temperature plate system (x3) are all composed of multiple low-temperature plates (8) connected in series and in parallel. The low-temperature plate is composed of a refrigerant flow channel (801) and fins (802) coated with an adsorbent. The first low-temperature plate system (x1) operates at 70-90K and is coated with coconut shell activated carbon adsorbent; The second low-temperature plate system (x2) operates at 30-45K and is coated with activated carbon-metal-organic framework composite adsorbent; The third low-temperature plate system (x3) operates at 10-20K and is coated with an activated carbon-metal-organic framework composite adsorbent containing nano-copper oxide.

2. The natural gas crude helium selective adsorption depurification and purification device according to claim 1, characterized in that, The first sealing valve, the second sealing valve, and the third sealing valve each include: Actuator (101), valve seat (102), valve disc (103), first rotating shaft (104), second rotating shaft (105); The valve disc (103) is located inside the valve seat (102) and is connected to the first rotating shaft (104) and the second rotating shaft (105). The actuator (101) is connected to the valve disc (103) through the first rotating shaft (104). The first seal (107) is assembled on one side of the valve disc through the fixing cover plate (106) of the first seal, and the second seal (108) is assembled on the other side of the valve disc through the fixing cover plate (109) of the second seal. The valve disc (103) has a rotation range of 0°-90° and is provided with a bidirectional sealing groove.

3. The natural gas crude helium selective adsorption depurification and purification device according to claim 2, characterized in that, The cross-sectional shape of the first seal (107) and the second seal (108) is a combination of a curved section and a straight section.

4. The natural gas crude helium selective adsorption depurification and purification device according to claim 1, characterized in that, The male and female heads (A) include: Male connector: male flange (11), first pipe of male connector (9), second pipe of male connector (10), third pipe of male connector (16), male connector fitting (17), heat insulation ring (18); Female head section: female head flange (12), first pipe of female head (14), second pipe of female head (15), third pipe of female head (20), female head connector (19); The male flange (11) is connected to the first pipe (9) and the third pipe (16) of the male head respectively. The male connector (17) is connected to the second pipe (10) and the third pipe (16) of the male head respectively. The male connector (17) is connected to the heat insulation ring (18). The female flange (12) is connected to the first pipe (14) and the second pipe (15) of the female head respectively. The female connector (19) is connected to the second pipe (15) and the third pipe (20) of the female head respectively. The sealing element (13) of the male flange and the female flange is located between the male flange (11) and the female flange (12). The heat insulation ring (18) is in contact with the female connector (19). The first pipe (9) of the male head is provided with a male evacuation port (901). The first pipe (14) of the female head is provided with a female evacuation port (1401).

5. The natural gas crude helium selective adsorption depurification and purification apparatus according to claim 4, characterized in that, The cross-sections of the third tube (16) of the male head and the second tube (15) of the female head are both rectangular threaded.

6. The natural gas crude helium selective adsorption depurification and purification device according to claim 1, characterized in that, Under operating conditions of 5MPa high pressure and 4.5K low temperature, the leakage rate of each sealed valve is ≤1×10⁻⁶. -9 Pa·m 3 / s.

7. A method of operating the apparatus according to any one of claims 1-6, characterized in that, include: Vacuuming: Evacuate the device to 10... -4 -10 -5 Pa; Staged cooling: The first low-temperature plate system cools down to 80K. The second low-temperature plate system cools the temperature to 40K. The third low-temperature plate system cools the temperature to 15K; Adsorption: When the valve is opened, the raw gas flows through the three-stage shell in sequence, and impurities are selectively adsorbed, collecting helium gas with a purity ≥99.999%. Regeneration: Close the valve, heat up each stage of the low-temperature plate system, and recover the desorbed gas through the regeneration gas outlet.

8. The method according to claim 7, characterized in that, Regeneration stage: The first low-temperature plate system is heated to 320-350K to recover methane. The second low-temperature plate system heats up to 100-130K to recover nitrogen. The third low-temperature plate system heats the gas to 60-80K to recover hydrogen.

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