Device and method for purifying helium from hydrogen-helium mixed gas

Abstract

The invention discloses a device for purifying helium from hydrogen-helium mixed gas. The device comprises a gas input pipe; the input end of the stable pressure output unit is communicated with the output end of the gas input pipe, and the gas input by the gas input pipe is output at stable pressure; the plurality of treatment tanks are annularly and sequentially communicated end to end; a blocking valve is arranged between every two treatment tanks; the head ends of the plurality of treatment tanks are respectively communicated with the output end of the pressure stabilizing output unit through respective lead-in valves; the tail ends of the plurality of treatment tanks are respectively communicated with the head end of the gas output pipe through respective discharge valves; the moisture treatment unit is arranged at the tail end of the gas output pipe and is used for separating moisture of gas in the gas output pipe; the tank body cleaning unit is respectively communicated with the tail end of the treatment tank through a waste gas valve and is used for extracting gas in the treatment tank; according to the invention, hydrogen in the hydrogen-helium mixed gas is reacted and consumed by adopting a chemical reaction, the final products are solid substances and water, and new impurity gas cannot be formed in the purified helium.

Description

Technical Field

[0001] The present invention relates to the field of gas purification, and in particular to a device and method for purifying helium from a hydrogen-helium mixed gas. Background Art

[0002] Since hydrogen and helium have very similar molecular weights, melting points, and boiling points, distillation cannot effectively separate them. Currently, the purification technology for hydrogen and helium mixed gases mainly relies on adsorption, membrane separation, and optimization of hybrid processes, as follows:

[0003] 1. Adsorption dehydrogenation technology. The combined process of "pressure swing adsorption + membrane separation + adsorption dehydrogenation" has been a breakthrough in recent years. Its advantages include: high safety, avoiding the flammability and explosion risks of traditional cryogenic distillation; low energy consumption, reducing energy consumption through room temperature operation; and resource utilization, with the separated hydrogen being reusable in industrial applications (such as fuel cells). However, this technology requires a large amount of equipment, is complex to implement, and is difficult to operate. Furthermore, there is currently no large-scale gas processing capability, and it is still in the laboratory stage.

[0004] 2. Membrane separation technology. MOFs membrane: Metal-organic framework materials (MOFs) have become a research hotspot in the field of membrane separation due to their high specific surface area and adjustable porosity. Experiments have shown that the separation coefficient of MOFs membranes for He / CH4 can reach more than 10, and the performance is further improved after molecular simulation optimization. However, it is easily degraded in high temperature, high humidity or corrosive environments, and its industrial application is limited. Mixed matrix membrane: Combining the flexibility of polymer materials with the screening ability of MOFs, some commercial membranes have achieved a helium purity of 99.99%. However, membrane separation technology requires multi-stage membrane stacking to achieve high purity, and the membrane materials are expensive and have a limited lifespan.

[0005] 3. Multi-stage separation process. Using spiral plate structure and multi-level separation network, the separation efficiency is improved through physical long path design, which is suitable for industrial mixed gas processing. Through three-stage compressor and hydrogen storage alloy (such as Ti 0.8 Zr 0.2 Cr 0.8 Mn 1.2 ) achieves helium purity 5N (99.999%) and hydrogen recovery rate of 99%.

[0006] 4. Improved traditional processes. Cryogenic distillation remains the mainstream technology for helium extraction from natural gas, but it consumes a lot of energy (accounting for approximately 40% of the total cost) and relies on feed gas with a high helium concentration (typically >0.1%). Pressure swing adsorption (PSA): This process uses multiple adsorption towers operating alternately to process low-concentration helium (such as BOG flash gas), but requires integration with membrane separation or adsorption dehydrogenation to improve efficiency. Summary of the Invention

[0007] In view of the above-mentioned defects of the prior art, the purpose of the present invention is to provide an apparatus and method for purifying helium from a hydrogen-helium mixture gas, which adopts a completely different path from all existing ideas for purifying helium from a hydrogen-helium mixture gas. That is, a chemical reaction consumes the hydrogen in the hydrogen-helium mixture gas, and the final products are solid matter and water, and no new impurity gas is formed in the purified helium.

[0008] The objective of the present invention is achieved through such technical solution:

[0009] The device for purifying helium from hydrogen-helium mixed gas comprises:

[0010] Gas inlet pipe;

[0011] A pressure-stabilizing output unit, the input end of which is connected to the output end of the gas input pipe, outputting the gas inputted from the gas input pipe at a stable pressure;

[0012] A plurality of treatment tanks are connected end to end in a ring-shaped manner; a blocking valve is provided between each treatment tank; the head ends of the plurality of treatment tanks are connected to the output end of the voltage stabilizing output unit through respective inlet valves;

[0013] A gas output pipe, wherein the tail ends of the plurality of treatment tanks are connected to the head end of the gas output pipe through respective discharge valves;

[0014] The moisture processing unit is arranged at the tail end of the gas output pipe to separate the moisture from the gas in the gas output pipe;

[0015] The tank cleaning unit is connected to the tail end of the treatment tank through the exhaust valve to extract the gas in the treatment tank;

[0016] The processing tank includes: a ceramic tank body, a hydrogen-reduced oxide whose product is a solid, an electromagnetic heating component, and a heat recovery component; the interior of the ceramic tank body is hollow, the head end is connected to the output end of the voltage-stabilizing output unit, and the tail end is connected to the tank cleaning unit and the gas output pipe; the hydrogen-reduced oxide whose product is a solid is accommodated in the ceramic tank body; the electromagnetic heating component is arranged on the outside of the ceramic tank body, facing the hydrogen-reduced oxide whose product is a solid, and the electromagnetic heating component heats the hydrogen-reduced oxide whose product is a solid through high-frequency current; the heat recovery component, with a heat absorption end arranged at the tail end of the ceramic tank body and a heat release end arranged at the head end of the ceramic tank body, heats the gas flowing out of the ceramic tank body with the heat of the gas flowing into the ceramic tank body.

[0017] Furthermore, the ceramic tank body comprises:

[0018] The head is barrel-shaped and has an air inlet at the bottom that is connected to the voltage-stabilizing output unit; the open end surface of the head is provided with a ring-shaped receiving groove of the tank body;

[0019] The tail portion is barrel-shaped, with the same internal diameter as the head portion, and an air outlet is provided at the bottom thereof, which is connected to the voltage stabilizing output unit and the tank cleaning unit; the open end surface of the tail portion is provided with a tank annular protrusion matching the tank annular receiving groove;

[0020] The high-temperature sealing ring of the tank body is arranged in the tank body receiving groove; after the head and tail are combined, the annular receiving groove of the tank body and the annular protrusion of the tank body are squeezed against each other; the high-temperature sealing ring of the tank body seals the tank body; the product is a solid hydrogen-reduced oxide contained in the receiving cavity formed by the head and tail parts.

[0021] Furthermore, the ceramic tank body further comprises:

[0022] The bottom tube is made of ceramic and is barrel-shaped. It is buckled on the inner bottom surface of the tail and faces the air outlet. The side wall of the bottom tube is provided with a bottom vent hole. The inner bottom surface of the tail is provided with a bottom ring-shaped receiving groove that matches the lower end surface of the bottom tube. A bottom high-temperature sealing ring is provided in the bottom ring-shaped receiving groove.

[0023] The center tube is made of ceramic material and is open at both ends. It is arranged between the outer bottom surface of the bottom tube and the inner bottom surface of the head, facing the air inlet; the inner wall of the center tube near the end of the bottom tube is provided with a penetrating internal vent hole; the inner side surface of the center tube, the inner bottom surface of the head, and the outer bottom surface of the bottom tube enclose an inner cavity; the inner bottom surface of the head is provided with a head-middle annular receiving groove matching the upper end of the center tube, and a head-middle high-temperature sealing ring is provided in the head-middle annular receiving groove; the outer bottom surface of the bottom tube is provided with a tail-middle annular receiving groove matching the lower end of the center tube, and a tail-middle high-temperature sealing ring is provided in the tail-middle annular receiving groove;

[0024] The outer tube is made of ceramic and is open at both ends. It is arranged between the outer bottom surface of the bottom tube and the inner bottom of the head, and is sleeved on the outside of the central tube. The inner wall of the outer tube at one end close to the inner bottom surface of the head is provided with a penetrating external vent; the inner side of the outer tube, the outer side of the central tube, the inner bottom surface of the head, and the bottom surface of the bottom tube form a middle cavity; the inner and outer sides of the outer tube, the inner side surface of the head, the inner side surface of the tail, and the outer side surface of the bottom tube form an outer cavity; the inner bottom surface of the head is provided with a head outer annular receiving groove matching the upper end of the outer tube, and a head outer high-temperature sealing ring is provided in the head outer annular receiving groove; the outer bottom surface of the bottom tube is provided with a tail outer annular receiving groove matching the lower end of the outer tube, and a tail outer high-temperature sealing ring is provided in the tail outer annular receiving groove;

[0025] The product is a solid hydrogen-reduced oxide contained in the inner cavity, the middle cavity and the outer cavity.

[0026] Furthermore, the ceramic tank body further comprises:

[0027] The inner rod is made of ceramic and has an openable and closable internal hollow structure. It is housed within the inner cavity, with its outer surface in sealed contact with the inner side of the central tube. The top of the inner rod is provided with an inner air inlet grille, and the top and bottom of the inner rod are provided with air outlet grilles. The inner rod contains a solid hydrogen-reduced oxide product. The lower portion of the inner rod is provided with an inner air outlet hole corresponding to the inner air vent hole.

[0028] The middle ring tube is made of ceramic and has an openable and closable internal hollow structure. Its outer contour is tubular, and its outer surface is in sealed contact with the inner side of the peripheral tube, and its inner surface is in sealed contact with the outer side of the central tube. The top of the middle ring tube is provided with a middle air outlet grille, and the bottom of the middle ring tube is provided with a middle air inlet grille. The middle ring tube contains a hydrogen-reduced oxide whose product is a solid. The lower portion of the middle ring tube is provided with a middle air inlet corresponding to the inner air vent, and the upper portion of the middle ring tube is provided with a middle air outlet corresponding to the outer air vent.

[0029] The outer ring tube is made of ceramic and has an internal hollow structure that can be opened and closed. Its outer contour is in the shape of a tube. Its outer surface is in contact and sealed with the inner side surfaces of the head and tail, and its inner surface is in contact and sealed with the inner side surface of the outer ring. The top of the outer ring tube is provided with an outer air intake grille, and the bottom of the outer ring tube is provided with an outer air outlet grille. The product placed in the outer ring tube is a solid hydrogen-reduced oxide; the lower part of the outer ring tube is provided with an outer air outlet corresponding to the bottom air vent, and the upper part of the outer ring tube is provided with an outer air intake corresponding to the outer air outlet.

[0030] Furthermore, the inner rod comprises an inner top section, a plurality of inner reaction sections, and an inner bottom section connected in sequence;

[0031] The inner top section is a tubular structure with two ends open, the upper end of the inner top section is open and faces the air inlet of the head, and the lower end is fixedly connected to the upper end of the adjacent inner reaction section;

[0032] The inner reaction section comprises an inner reaction chamber and an inner support tube; the upper end of the inner reaction chamber is provided with an inner air inlet grille, and the lower end is provided with an inner air outlet grille; the inner reaction chamber contains a hydrogen-reduced oxide whose product is a solid, and both ends of the inner support tube are open;

[0033] The upper end of the inner bottom section is an open structure, which is connected and fixed to the inner support tube of the adjacent inner reaction section. The side of the inner bottom section is provided with a plurality of inner air outlet holes; when the inner bottom section is located at the bottom of the central tube, the inner air outlet holes are connected to the inner ventilation holes;

[0034] The middle ring tube includes a middle top section, several middle reaction sections, and a middle bottom section connected in sequence;

[0035] The lower end of the middle top section is an open structure, with a plurality of middle air outlet holes provided on the side, and the lower end is fixedly connected to the upper end of the adjacent middle reaction section; when the middle top section is located at the top of the central tube, the middle air outlet holes are connected to the external air vents;

[0036] The middle reaction section comprises: a middle reaction chamber and a middle support tube; the middle reaction chamber is provided with a middle air outlet grille at the upper end and a middle air inlet grille at the lower end; the middle reaction chamber contains hydrogen-reduced oxides whose products are solids, and the middle support tube is open at both ends;

[0037] The upper end of the middle bottom section is an open structure, which is connected and fixed to the middle support tube of the adjacent middle reaction section. The side of the middle bottom section is provided with a number of middle air inlet holes. When the middle bottom section is located at the bottom of the peripheral tube, the middle opening is connected to the inner air vent.

[0038] The outer ring tube includes an outer top section, a plurality of outer reaction sections, and an outer bottom section connected in sequence;

[0039] The lower end of the outer top section is an open structure, with a plurality of external air inlet holes provided on the side, and the lower end is fixedly connected to the upper end of the adjacent outer reaction section; when the outer top section is located at the inner bottom of the head, the external air inlet holes are connected to the external air vents;

[0040] The outer reaction section comprises an outer reaction chamber and an outer support tube; the upper end of the outer reaction chamber is provided with an outer air inlet grille, and the lower end is provided with an outer air outlet grille; the outer reaction chamber contains a hydrogen-reduced oxide whose product is a solid, and both ends of the outer support tube are open;

[0041] The upper end of the outer bottom section is an open structure, which is connected and fixed to the outer support tube of the adjacent outer reaction section. Several outgoing air holes are provided on the side of the outer bottom section; when the outer bottom section is located at the inner bottom of the tail, the outgoing air holes are connected to the bottom vent holes.

[0042] Furthermore, the product is a solid hydrogen-reduced oxide comprising ferrosoferric oxide and copper oxide;

[0043] The content of copper oxide in the plurality of inner reaction sections decreases as the distance from the top of the inner cavity increases;

[0044] The content of copper oxide in the middle reaction sections increases as the distance from the top of the middle cavity increases;

[0045] The content ratio of copper oxide contained in the plurality of outer reaction sections decreases as the distance from the top of the outer cavity increases;

[0046] The number of inner reaction sections, middle reaction sections, and outer reaction sections is the same;

[0047] The multiple inner reaction chambers of the inner reaction section, the multiple middle reaction chambers of the middle reaction section, and the multiple outer reaction chambers of the outer reaction section are kept at the same horizontal height from the inner bottom surface of the head to the inner bottom surface of the tail; the electromagnetic heating assembly includes the same number of electromagnetic heating rings as the inner reaction sections, and each electromagnetic heating ring is directly opposite to the height of each inner reaction chamber in the inner reaction section.

[0048] Furthermore, the inner reaction chamber includes an upper rod and a lower rod connected by a threaded seal; an inner annular groove is provided on the outer surface of the upper rod and / or the lower rod; an annular inner high-temperature sealing ring is provided in the inner annular groove, and when the inner reaction chamber is placed in the inner cavity, the inner high-temperature sealing ring and the inner side surface of the central tube are pressed and fixed against each other, sealing the upper and lower sides thereof;

[0049] The middle reaction chamber comprises a middle upper ring disc and a middle lower ring disc connected by a threaded seal; a middle annular groove is provided on the outer surface of the middle upper ring disc and / or the middle lower ring disc; a ring-shaped middle and high temperature sealing ring is provided in the middle annular groove; when the middle reaction chamber is placed in the middle cavity body, the middle and high temperature sealing ring is pressed and fixed against the outer side surface of the central tube and the inner side surface of the peripheral tube, thereby sealing the upper and lower sides thereof;

[0050] The outer reaction chamber includes an outer upper ring disk and an outer lower ring disk connected by threaded sealing; an outer annular groove is provided on the outer surface of the outer upper ring disk and / or the outer lower ring disk; an annular outer high-temperature sealing ring is provided in the outer annular groove. When the outer reaction chamber is placed in the outer cavity body, the outer high-temperature sealing ring and the outer side surface, the inner side surface of the head or the inner side surface of the tail of the outer tube are squeezed and fixed to each other, sealing the upper and lower sides thereof.

[0051] 8Furthermore,

[0052] The ferrosoferric oxide is in the form of a filament with a length of not less than 1 micron and a diameter of not more than 200 nanometers, and the copper oxide is in the form of a nanorod;

[0053] The upper and lower ends of the inner reaction chamber, the middle reaction chamber and the outer reaction chamber are all provided with asbestos mesh filters;

[0054] The asbestos mesh filter diameter at the top and bottom of the inner reaction section is not greater than 1 micron, and the asbestos mesh filter diameter between the top and bottom of the inner reaction section is not less than 1 micron;

[0055] The asbestos mesh filter diameter at the top and bottom of the middle reaction section is not greater than 1 micron, and the asbestos mesh filter diameter between the top and bottom of the middle reaction section is not less than 1 micron;

[0056] The asbestos mesh filter diameter at the top and bottom of the outer reaction section is not greater than 1 micron, and the asbestos mesh filter diameter between the top and bottom of the outer reaction section is not less than 1 micron.

[0057] Further,

[0058] A transparent observation window is provided on the head or tail;

[0059] The moisture treatment unit includes: a pressure reduction and temperature reduction component and a centrifugal separation component;

[0060] The heat recovery assembly includes: a copper heat-absorbing heat exchanger, a copper heat-releasing heat exchanger, a circulating heat exchange medium, and a heat exchange pump; the copper heat-absorbing heat exchanger is arranged at the rear end of the ceramic tank; the copper heat-releasing heat exchanger is arranged at the head end of the ceramic tank; the circulating heat exchange medium connects the copper heat-absorbing heat exchanger and the copper heat-releasing heat exchanger; the heat exchange pump drives the circulating heat exchange medium to circulate between the copper heat-absorbing heat exchanger and the copper heat-releasing heat exchanger;

[0061] The blocking valve is arranged at the gas outlet end of the upstream treatment tank; a clean valve is also provided between each treatment tank; the clean valve and the introduction valve on each treatment tank are integrated into a multi-way control valve; the blocking valve, the discharge valve and the exhaust valve on each treatment tank are integrated into a multi-way control valve.

[0062] The device and method for purifying helium from a hydrogen-helium mixed gas include the following steps:

[0063] S1. Close all inlet valves and outlet valves, and open all other valves;

[0064] S2. Start the tank cleaning unit to vacuum all the processing tanks until a predetermined vacuum degree is reached and then close the tank cleaning unit;

[0065] S3. Close all exhaust valves and open all inlet valves to keep the pressure of the treatment tank consistent with the output end of the pressure-stabilizing output unit;

[0066] S4. After repeating steps S2 and S3 a certain number of times, follow step S2;

[0067] S5. Start the electromagnetic heating assembly to heat the hydrogen-reduced oxide, and energize the electromagnetic heating ring so that it heats the hydrogen-reduced oxide alternately at a frequency of 40 kHz and 200 kHz until the temperature of the hydrogen-reduced oxide rises to 550 degrees Celsius and then maintains the hydrogen-reduced oxide between 500 and 600 degrees Celsius;

[0068] S6. Select a treatment tank as the head tank, and the adjacent upstream treatment tank as the tail pipe;

[0069] S7, close all the exhaust valves; close the clean valve on the head tank, open the exhaust valve on the head tank; close the blocking valve on the tail tank,

[0070] S8. Set the output pressure of the pressure-stabilizing output unit to be greater than the static pressure of the device and greater than the external atmospheric pressure of the device; then open the inlet valve between the pressure-stabilizing output unit and the header tank;

[0071] S9, open the discharge valve between the head tank and the gas output pipe;

[0072] S10, turning on the heat exchange pump, the pressure reduction and temperature reduction component, and the centrifugal separation component; the pressure reduction and temperature reduction component controls the condensation of part of the water in the purified helium output from the gas output pipe;

[0073] S11. Observe the color of ferroferric oxide in each treatment tank through a transparent observation window in real time;

[0074] When you need to replace any treatment tank, the steps are as follows:

[0075] SX1. The adjacent processing tank upstream of the head tank that needs to be replaced is used as the new tail tank, and the adjacent processing tank downstream of the head tank that needs to be replaced is used as the new head tank;

[0076] SX2. Open the inlet valve between the new header tank and the pressure-stabilizing output unit, the outlet valve between the tail tank and the gas discharge pipe, and the clean valve and shut-off valve between the original header tank and the tail tank. Simultaneously, close the inlet valve between the original header tank and the pressure-stabilizing output unit, the outlet valve between the original tail tank and the gas discharge pipe, and the clean valve and shut-off valve between the new tail tank and the treatment tank to be replaced.

[0077] SX3, remove the treatment tank that needs to be replaced;

[0078] When you need to replace any treatment tank, the steps are as follows:

[0079] SS1. Add the treatment tank to be replaced into the device;

[0080] SS2. Open the exhaust valve of the replaced treatment tank and start the tank cleaning unit to vacuum the replaced treatment tank. When the vacuum degree in the replaced treatment tank reaches the requirement, close the tank cleaning unit.

[0081] SS3. Open the inlet valve between the replaced treatment tank and the pressure-stabilizing output unit. When the pressure inside the replaced treatment tank is consistent with the pressure at the output end of the pressure-stabilizing output unit, close the inlet valve between the replaced treatment tank and the pressure-stabilizing output unit.

[0082] SS4. After repeating steps SS2 and SS3 a certain number of times, follow step SS2.

[0083] SS5. Use the replaced treatment tank as the new tail tank, open the discharge valve between the new tail tank and the gas output pipe, the clean valve and the shut-off valve between the new tail tank and the upstream treatment tank; close the discharge valve between the new tail tank and the upstream treatment tank and the gas output pipe.

[0084] Due to the adoption of the above technical solution, the present invention has the following advantages:

[0085] 1. This invention uses a chemical reaction to specifically absorb hydrogen. The reaction products are water and solids (). It does not add new impurities to the helium gas, reduces the hydrogen content in the hydrogen helium gas, and avoids the addition of other gaseous impurities. The absorption of hydrogen can be controlled throughout the purification process to achieve the desired helium concentration.

[0086] 2. By installing multiple process tanks, the absorption reaction capacity of hydrogen can be increased, and the helium concentration can be raised, while also ensuring continuous production. Specifically, by arranging multiple process tanks in a ring and controlling them through multiple valves, when a process tank needs maintenance or replacement of hydrogen-reduced oxides, the process tank in need of maintenance can be removed from the production line without affecting production, significantly improving production efficiency and reducing production costs.

[0087] 3. Using copper oxide and ferroferric oxide, two hydrogen-reducible oxides, can ensure a better heating effect during electromagnetic heating. (Copper oxide has a poor heating efficiency, while ferroferric oxide has a higher heating efficiency). At the same time, after copper oxide is reduced to copper, it can act as a catalyst to increase the reaction rate of ferroferric oxide and hydrogen. Compared with pure ferroferric oxide, the conversion efficiency can be increased from 60-70% to more than 95%, thereby achieving a more efficient reaction. The specific principle is as follows:

[0088] Electron transfer and charge balance: The introduction of Cu can adjust the electron distribution of Fe3O4. 2+ and Fe 3+ The mixed valence state of Cu forms local charge compensation through Cu doping, reducing Fe 3+ For example, XPS analysis of Cu-doped Fe3O4 shows that Cu 2+ with Fe 3+ Charge transfer occurs between them, optimizing the surface electronic state.

[0089] d-band center regulation: The d orbital of Cu hybridizes with the Fe 3d orbital of Fe3O4, bringing the d-band center closer to the Fermi level and enhancing the adsorption and dissociation ability of H2

[0090] Surface reconstruction and defect generation: The addition of Cu promotes electrochemical reconstruction of the Fe3O4 surface, forming a Cu-FeOOH mixed phase. For example, under alkaline conditions, the Cu-Fe3O4 precursor generates FeOOH rich in oxygen vacancies through a "dissolution-redeposition" process, significantly increasing the active site density.

[0091] Synergistic adsorption effect: Cu atoms and Fe atoms on the Fe₃O₄ surface synergistically adsorb H₂ molecules, reducing the activation energy for H₂ dissociation. DFT calculations show that the H adsorption energy at the Cu-Fe₃O₄ interface is approximately 0.2 eV lower than that of pure Fe₃O₄.

[0092] Step-by-step reduction acceleration: The reduction of Fe3O4 is usually carried out in two steps (Fe 3+ →Fe 2+ →Fe), the introduction of Cu can preferentially reduce Fe 3+ , shortening the overall reaction path. For example, Cu / Fe3O4 can complete Fe 3+ Complete reduction of pure Fe3O4 requires 400℃.

[0093] The catalytic effect of Cu can reduce the reoxidation of Fe intermediates and improve the reaction selectivity. For example, in a hydrogen atmosphere, the stability of Cu / Fe3O4 is more than three times higher than that of pure Fe3O4.

[0094] Other advantages, objects and features of the present invention will be described in part in the following description and, in part, will be apparent to those skilled in the art based on an examination of the following or may be learned from the practice of the invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0095] Figure 1 1 is a schematic top view of the structure of the device for purifying helium from a hydrogen-helium mixed gas in this embodiment;

[0096] Figure 2 1 is a schematic diagram of a partial front view of the structure of the device for purifying helium from a hydrogen-helium mixture in this embodiment;

[0097] Figure 3 This is a schematic front view of the processing tank and related structures in this embodiment;

[0098] Figure 4 Schematic diagram of the longitudinal cross-sectional structure of the processing tank in this embodiment;

[0099] Figure 5 yes Figure 4 Enlarged structural diagram at point A in the middle.

[0100] Figure 6 yes Figure 4 Enlarged structural diagram at point B in the middle.

[0101] Figure 7 yes Figure 4 Enlarged structural diagram at point C in the middle.

[0102] Figure 8 Schematic diagram of the flow of the gas to be treated in the treatment tank in this embodiment;

[0103] Figure: 1. Gas inlet pipe; 2. Voltage-stabilizing output unit; 31. Ceramic tank body; 311. Head; 3111. Air inlet; 312. Tail; 3121. Air outlet; 32. High-temperature sealing ring of tank body; 33. Bottom tube; 331. Bottom vent hole; 34. Center tube; 341. Inner vent hole; 35. Outer tube; 351. Outer vent hole; 36. Inner rod; 361. Inner top section; 36211. Inner air intake grille; 362 12. Internal air outlet grille; 36213. Upper rod; 36214. Lower rod; 36215. Internal high-temperature sealing ring; 3622. Internal support tube; 363. Internal bottom section; 3631. Internal air outlet; 37. Middle ring tube; 371. Middle top section; 3711. Middle air outlet; 37211. Middle air inlet grille; 37212. Middle air outlet grille; 37213. Middle upper ring plate; 37214. Middle lower ring plate; 37215. Middle high High-temperature sealing ring; 3722. Middle support tube; 373. Middle bottom section; 3731. Middle air inlet; 38. Outer ring tube; 381. Outer top section; 3811. Outer air inlet; 38211. Outer air inlet grille; 38212. Outer air grille; 38213. Outer upper ring plate; 38214. Outer lower ring plate; 38215. Outer high-temperature sealing ring; 3822. Outer support tube; 383. Outer bottom section; 3831. Outer air inlet; 39. Hydrogen reduction of oxides; 41. Electromagnetic heating ring; 421. Copper endothermic heat exchanger; 422. Copper exothermic heat exchanger; 423. Circulating heat exchange medium; 424. Heat exchange pump; 43. Transparent observation window; 5. Gas output pipe; 61. Pressure reduction and cooling component; 62. Centrifugal separation component; 7. Tank cleaning unit; 81. Cleaning valve; 82. Inlet valve; 91. Blocking valve; 92. Discharge valve; 93. Exhaust valve; 10. Asbestos mesh. DETAILED DESCRIPTION

[0104] The present invention will be further described below with reference to the embodiments.

[0105] Example:

[0106] like Figure 1 、 Figure 2 As shown, the device for purifying helium from hydrogen-helium mixed gas comprises:

[0107] Gas inlet pipe 1;

[0108] The pressure-stabilizing output unit 2 has an input end connected to the output end of the gas input pipe 1, and outputs the gas inputted from the gas input pipe 1 at a stable pressure;

[0109] Several processing tanks are connected end to end in a ring-shaped manner; a blocking valve 91 is provided between each processing tank; the head ends of the several processing tanks are connected to the output end of the voltage stabilizing output unit 2 through their respective inlet valves 82;

[0110] Gas output pipe 5, the tail ends of the several processing tanks are connected to the head end of the gas output pipe 5 through their respective discharge valves 92;

[0111] The moisture processing unit is provided at the tail end of the gas output pipe 5 to separate the moisture from the gas in the gas output pipe 5;

[0112] The tank cleaning unit 7 is connected to the tail end of the treatment tank through the exhaust valve 93 to extract the gas in the treatment tank;

[0113] The processing tank includes: a ceramic tank body 31, a hydrogen-reduced oxide 39 whose product is a solid, an electromagnetic heating component, and a heat recovery component; the ceramic tank body 31 is hollow inside, the head end is connected to the output end of the voltage-stabilizing output unit 2, and the tail end is connected to the tank cleaning unit 7 and the gas output pipe 5; the hydrogen-reduced oxide 39 whose product is a solid is accommodated in the ceramic tank body 31; the electromagnetic heating component is arranged on the outside of the ceramic tank body 31, facing the hydrogen-reduced oxide 39 whose product is a solid, and the electromagnetic heating component heats the hydrogen-reduced oxide 39 whose product is a solid through high-frequency current; the heat recovery component, the heat absorption end is arranged at the tail end of the ceramic tank body 31, and the heat release end is arranged at the head end of the ceramic tank body 31, and the heat of the gas flowing out of the ceramic tank body 31 is used to heat the gas flowing into the ceramic tank body 31.

[0114] The chemical reaction specifically absorbs hydrogen, reducing its content. The resulting solid hydrogen-reduced oxides include copper oxide, iron oxide, and ferroferric oxide, all of which react and adsorb hydrogen. A cyclic production system allows for replacement of the hydrogen-reduced oxide reagent without disrupting production.

[0115] The reaction conditions of hydrogen reduction of oxide 39, in which the product is a solid, are achieved through an electromagnetic heating component, ensuring that the reaction process does not exchange with the outside air and that the gas is pure.

[0116] like Figure 4 As shown, the ceramic tank body 31 includes:

[0117] The head 311 is barrel-shaped and has an air inlet 3111 at the bottom that is connected to the voltage-stabilizing output unit 2; the open end surface of the head 311 is provided with a tank body annular receiving groove;

[0118] The tail portion 312 is barrel-shaped, with the same internal diameter as the head portion 311, and has an air outlet 3121 at its bottom that communicates with the voltage stabilizing output unit 2 and the tank cleaning unit 7; the open end surface of the tail portion 312 is provided with a tank annular protrusion that matches the tank annular receiving groove;

[0119] The high-temperature sealing ring 32 of the tank body is arranged in the tank body receiving groove; after the head 311 and the tail 312 are combined, the annular receiving groove of the tank body and the annular protrusion of the tank body are squeezed against each other; the high-temperature sealing ring 32 of the tank body seals the tank body; the product is a solid hydrogen-reduced oxide 39 contained in the receiving cavity formed by the head 311 and the tail 312.

[0120] The tank body features a split upper and lower structure, facilitating replacement of the hydrogen-reduced oxide 39 contained within. Furthermore, the ceramic material does not hinder the electromagnetic heating assembly from heating the hydrogen-reduced oxide 39, minimizing energy waste. High-temperature sealing rings can be made of high-temperature-resistant materials that do not react with helium or hydrogen, such as ceramic fiber gaskets or high-silica cloth, which are squeezed to create a seal. Furthermore, increasing the pressure of the other gases being purified can prevent external gases from entering the treatment tank.

[0121] like Figure 4 、 5 As shown in , 6, and 7, in this embodiment, the ceramic tank body 31 further includes:

[0122] The bottom tube 33 is made of ceramic and is barrel-shaped. It is buckled onto the inner bottom surface of the tail portion 312 and faces the air outlet 3121. The side wall of the bottom tube 33 is provided with a bottom vent hole 331 extending therethrough. The inner bottom surface of the tail portion 312 is provided with a bottom annular receiving groove that matches the lower end surface of the bottom tube 33. A bottom high-temperature sealing ring is provided in the bottom annular receiving groove.

[0123] The center tube 34 is made of ceramic and is open at both ends. It is arranged between the outer bottom surface of the bottom tube 33 and the inner bottom surface of the head 311, facing the air inlet 3111; the inner wall of the center tube 34 near the end of the bottom tube 33 is provided with a penetrating internal vent 341; the inner side surface of the center tube 34, the inner bottom surface of the head 311, and the outer bottom surface of the bottom tube 33 enclose an inner cavity; the inner bottom surface of the head 311 is provided with a head-center annular receiving groove that matches the upper end of the center tube 34, and a head-center high-temperature sealing ring 37215 is provided in the head-center annular receiving groove; the outer bottom surface of the bottom tube 33 is provided with a tail-center annular receiving groove that matches the lower end of the center tube 34, and a tail-center high-temperature sealing ring 37215 is provided in the tail-center annular receiving groove;

[0124] The outer tube 35 is made of ceramic and is open at both ends. It is arranged between the outer bottom surface of the bottom tube 33 and the inner bottom of the head 311, and is sleeved on the outside of the central tube 34. The inner wall of the outer tube 35 at one end close to the inner bottom surface of the head 311 is provided with a penetrating external vent 351; the inner side of the outer tube 35, the outer side of the central tube 34, the inner bottom surface of the head 311, and the bottom surface of the bottom tube 33 form a middle cavity; the inner and outer sides of the outer tube 35, the inner side surface of the head 311, the inner side surface of the tail 312, and the outer side surface of the bottom tube 33 form an outer cavity; the inner bottom surface of the head 311 is provided with a head outer annular receiving groove that matches the upper end of the outer tube 35, and the head outer annular receiving groove is provided with a head outer high-temperature sealing ring 38215; the outer bottom surface of the bottom tube 33 is provided with a tail outer annular receiving groove that matches the lower end of the outer tube 35, and the tail outer annular receiving groove is provided with a tail outer high-temperature sealing ring 38215;

[0125] The product is a solid hydrogen-reduced oxide 39 contained in the inner cavity, the middle cavity and the outer cavity.

[0126] The bottom tube 33, the center tube 34 and the outer tube 35 are arranged in the ceramic tank body 31 to guide the gas to be purified to stay in the ceramic tank body 31 for as long as possible, and to contact the hydrogen-reduced oxide 39 for a longer time, thereby reacting more hydrogen.

[0127] like Figure 5 、 6 As shown in FIG. 7 , in this embodiment, the ceramic tank body 31 further includes:

[0128] The inner rod 36 is made of ceramic and has an openable and closable hollow structure. It is housed within the inner cavity, with its outer surface in sealed contact with the inner side of the central tube 34. An inner air inlet grille 36211 is provided at the top of the inner rod 36, and air outlet grilles are provided at the top and bottom of the inner rod 36. The inner rod 36 contains a solid hydrogen-reduced oxide 39 as a product. An inner air outlet hole 3631 is provided at the bottom of the inner rod 36, corresponding to the inner air vent 341.

[0129] The middle ring tube 37 is made of ceramic and has an openable and closable hollow interior. Its outer contour is tubular, with its outer surface in sealed contact with the inner side of the outer tube 35 and its inner surface in sealed contact with the outer side of the central tube 34. A middle air outlet grille 37212 is provided at the top of the middle ring tube 37, and a middle air inlet grille 37211 is provided at the bottom of the middle ring tube 37. The middle ring tube 37 contains a solid hydrogen-reduced oxide 39 as a product. A middle air inlet hole 3731 corresponding to the inner air vent 341 is provided at the bottom of the middle ring tube 37, and a middle air outlet hole 3711 corresponding to the outer air vent 351 is provided at the top of the middle ring tube 37.

[0130] The outer ring tube 38 is made of ceramic material, has an internal hollow structure that can be opened and closed, and has a tubular outer contour. Its outer surface is in contact and sealed with the inner side surfaces of the head 311 and the tail 312, and its inner surface is in contact and sealed with the inner side surface of the outer ring; the top of the outer ring tube 38 is provided with an outer air intake grille 38211, and the bottom of the outer ring tube 38 is provided with an outer air outlet grille 38212; the outer ring tube 38 contains a hydrogen-reduced oxide 39 whose product is a solid; the lower part of the outer ring tube 38 is provided with an outer air outlet 3831 corresponding to the bottom air vent 331, and the upper part of the outer ring tube 38 is provided with an outer air intake 3811 corresponding to the outer air vent 351.

[0131] A hydrogen-reducing oxide 39 containing device matching each cavity is provided in the ceramic tank body 31, so that the hydrogen-reducing oxide 39 reagent can be replaced more quickly and conveniently.

[0132] In this embodiment, the inner rod 36 includes an inner top section 361, a plurality of inner reaction sections, and an inner bottom section 363 connected in sequence;

[0133] The inner top section 361 is a tubular structure with openings at both ends. The upper end of the inner top section 361 is open facing the air inlet 3111 of the head 311, and the lower end is fixedly connected to the upper end of the adjacent inner reaction section.

[0134] The inner reaction section includes an inner reaction chamber and an inner support tube 3622. The upper end of the inner reaction chamber is provided with an inner air inlet grille 36211, and the lower end is provided with an inner air outlet grille 36212. The inner reaction chamber contains a hydrogen-reduced oxide 39, the product of which is a solid. The inner support tube 3622 is open at both ends.

[0135] The upper end of the inner bottom section 363 is open and connected to the inner support tube 3622 of the adjacent inner reaction section. The side of the inner bottom section 363 is provided with a plurality of inner air outlet holes 3631. When the inner bottom section 363 is located at the bottom of the central tube 34, the inner air outlet holes 3631 are connected to the inner vent hole 341.

[0136] The middle ring tube 37 includes a middle top section 371, several middle reaction sections, and a middle bottom section 373 connected in sequence;

[0137] The lower end of the middle top section 371 is an open structure, with a plurality of middle air outlet holes 3711 provided on the side. The lower end is fixedly connected to the upper end of the adjacent middle reaction section. When the middle top section 371 is located at the top of the central tube 34, the middle air outlet holes 3711 are connected to the external air vents 351.

[0138] The middle reaction section includes a middle reaction chamber and a middle support tube 3722. The middle reaction chamber is provided with a middle air outlet grille 37212 at the upper end and a middle air inlet grille 37211 at the lower end. The middle reaction chamber contains a solid hydrogen-reduced oxide 39, and the middle support tube 3722 is open at both ends.

[0139] The upper end of the middle bottom section 373 is an open structure, which is connected and fixed to the middle support tube 3722 of the adjacent middle reaction section. The side of the middle bottom section 373 is provided with a plurality of middle air inlet holes 3731. When the middle bottom section 373 is located at the bottom of the outer tube 35, the middle opening is connected to the inner air vent 341.

[0140] The outer ring tube 38 includes an outer top section 381, a plurality of outer reaction sections, and an outer bottom section 383 connected in sequence;

[0141] The lower end of the outer top section 381 is an open structure, with a plurality of external air inlet holes 3811 provided on the side. The lower end is fixedly connected to the upper end of the adjacent outer reaction section. When the outer top section 381 is located at the bottom of the head section 311, the external air inlet holes 3811 are connected to the external air vents 351.

[0142] The outer reaction section includes an outer reaction chamber and an outer support tube 3822. The upper end of the outer reaction chamber is provided with an outer air inlet grille 38211, and the lower end is provided with an outer air outlet grille 38212. The outer reaction chamber contains a hydrogen-reduced oxide 39, the product of which is a solid. The outer support tube 3822 is open at both ends.

[0143] The upper end of the outer bottom section 383 is an open structure, which is connected and fixed to the outer support tube 3822 of the adjacent outer reaction section. The side of the outer bottom section 383 is provided with several outgoing air holes 3831; when the outer bottom section 383 is located at the bottom of the tail section 312, the outgoing air holes 3831 are connected to the bottom vent hole 331.

[0144] The hydrogen-reduced oxide 39 containing device in each cavity is set to a multi-stage structure, which is convenient for disassembling the containing hydrogen-reduced oxide 39 reagent, and can also better match the electromagnetic heating component on the outside of the ceramic tank body 31, effectively heating the hydrogen-reduced oxide 39 to a suitable temperature, avoiding excessive temperature in some areas, resulting in a decrease in reaction rate.

[0145] At the same time, the multi-stage structure can guide the gas to be purified to turbulent flow in the support tube between each section. Compared with filling the entire support tube with hydrogen-reduced oxide 39, the flow direction of the gas can be changed each time the gas enters the reaction chamber from the support tube, so that the gas can more fully utilize the hydrogen-reduced oxide 39, reduce the use of hydrogen-reduced oxide 39, effectively improve efficiency and reduce costs.

[0146] like Figure 4 As shown, the product is a solid hydrogen-reduced oxide 39 including ferrosoferric oxide and copper oxide;

[0147] The content of copper oxide in the plurality of inner reaction sections decreases as the distance from the top of the inner cavity increases;

[0148] The content of copper oxide in the middle reaction sections increases as the distance from the top of the middle cavity increases;

[0149] The content ratio of copper oxide contained in the plurality of outer reaction sections decreases as the distance from the top of the outer cavity increases;

[0150] The number of inner reaction sections, middle reaction sections, and outer reaction sections is the same;

[0151] The multiple inner reaction chambers of the inner reaction section, the multiple middle reaction chambers of the middle reaction section, and the multiple outer reaction chambers of the outer reaction section are kept at the same horizontal height from the inner bottom surface of the head 311 to the inner bottom surface of the tail 312; the electromagnetic heating assembly includes the same number of electromagnetic heating rings 41 as the inner reaction sections, and each electromagnetic heating ring 41 is directly opposite to the height of each inner reaction chamber in the inner reaction section.

[0152] Compared with ferroferric oxide, copper oxide has a lower reaction rate with hydrogen, but the copper element reduced to it can effectively catalyze the reaction rate of ferroferric oxide and hydrogen. Therefore, after the copper oxide is reduced, the small amount of copper element generated will float in the gas into the next reaction chamber under the action of the airflow. Therefore, the copper oxide content in the downstream reaction chamber can be lower, which can reduce costs and ensure a better reaction rate.

[0153] According to the direction of gas flow, gradually reducing the proportion of copper oxide can increase the hydrogen

[0154] In this embodiment, the inner reaction chamber includes an upper rod 36213 and a lower rod 36214 connected by a threaded seal. The outer surface of the upper rod 36213 and / or the lower rod 36214 is provided with an inner annular groove. An annular inner high-temperature sealing ring 36215 is provided within the inner annular groove. When the inner reaction chamber is placed in the inner cavity, the inner high-temperature sealing ring 36215 and the inner surface of the central tube 34 are pressed and fixed against each other, sealing the upper and lower sides thereof.

[0155] The middle reaction chamber includes a middle upper ring disc 37213 and a middle lower ring disc 37214 connected by a threaded seal; the outer surface of the middle upper ring disc 37213 and / or the middle lower ring disc 37214 is provided with a middle annular groove; an annular middle and high temperature sealing ring 37215 is provided in the middle annular groove. When the middle reaction chamber is placed in the middle cavity, the middle and high temperature sealing ring 37215 is pressed and fixed against the outer surface of the central tube 34 and the inner surface of the peripheral tube 35, thereby sealing the upper and lower sides thereof;

[0156] The outer reaction chamber includes an outer upper ring disk 38213 and an outer lower ring disk 38214 connected by threaded sealing; an outer annular groove is provided on the outside of the outer upper ring disk 38213 and / or the outer lower ring disk 38214; an annular outer high-temperature sealing ring 38215 is provided in the outer annular groove. When the outer reaction chamber is placed in the outer cavity body, the outer high-temperature sealing ring 38215 and the outer side surface of the outer tube 35, the inner side surface of the head 311 or the inner side surface of the tail 312 are squeezed and fixed to each other to seal the upper and lower sides.

[0157] The high-temperature sealing rings in this example are all made of ceramic fiber gaskets and high-silica cloth materials, which do not react with gas and serve as isolation seals and embedded fillers to relatively stably fix the container (inner rod 36, middle ring tube 37, outer ring tube 38) containing hydrogen reduced oxide 39 in the ceramic tank body 31.

[0158] In this embodiment, the ferrosoferric oxide is a filamentous structure with a length of not less than 1 micron and a diameter of not more than 200 nanometers, and the copper oxide is a nanorod;

[0159] The upper and lower ends of the inner reaction chamber, the middle reaction chamber, and the outer reaction chamber are all provided with asbestos mesh 10 for filtration;

[0160] The filter diameter of the asbestos mesh 10 at the top and bottom of the inner reaction section is not greater than 1 micron, and the filter diameter of the asbestos mesh 10 between the top and bottom of the inner reaction section is not less than 1 micron;

[0161] The filter diameter of the asbestos mesh 10 at the top and bottom of the middle reaction section is not greater than 1 micron, and the filter diameter of the asbestos mesh 10 between the top and bottom of the middle reaction section is not less than 1 micron;

[0162] The filtration diameter of the asbestos mesh 10 at the top and bottom of the outer reaction section is not greater than 1 micron, and the filtration diameter of the asbestos mesh 10 between the top and bottom of the outer reaction section is not less than 1 micron.

[0163] The filamentous ferroferric oxide can effectively wrap the copper oxide powder. After the copper oxide powder is reduced, it can be released to a certain extent as the ferroferric oxide is simultaneously reduced, so that it can better enter the next reaction chamber with the flow of gas to promote the reaction of the next reaction chamber, thereby making full use of the ferroferric oxide and improving the reaction efficiency.

[0164] The ferroferric oxide in this embodiment can be formed into Fe3O4 filaments through a soluble template (such as silk fibroin, gelatin), and then calcined to remove organic matter to obtain pure Fe3O4 filaments, or Fe3O4 precursors (such as FeCl3 and polymer material composites) can be used as raw materials to form fibers through electrospinning, and pure Fe3O4 nanofibers can be obtained after calcination, or the crystallization process can be controlled in a closed reactor to directly generate Fe3O4 fibrous structures.

[0165] In this embodiment, a transparent observation window 43 is provided on the head portion 311 or the tail portion 312;

[0166] The moisture treatment unit includes a pressure reduction and temperature reduction assembly 61 and a centrifugal separation assembly 62. The pressure reduction and temperature reduction assembly 61 uses a pressure reduction valve in conjunction with a cooling device to reduce the gas's dew point, thereby condensing the water in the gas. This is then separated by a cyclone centrifuge. If the moisture content requirement is higher, cryogenic distillation can be performed to more thoroughly separate the water from the gas.

[0167] The heat recovery component includes: a copper heat-absorbing heat exchanger 421, a copper heat-releasing heat exchanger 422, a circulating heat exchange medium 423, and a heat exchange pump 424; the copper heat-absorbing heat exchanger 421 is arranged at the rear end of the ceramic tank 31; the copper heat-releasing heat exchanger 422 is arranged at the head end of the ceramic tank 31; the circulating heat exchange medium 423 connects the copper heat-absorbing heat exchanger 421 and the copper heat-releasing heat exchanger 422; the heat exchange pump 424 drives the circulating heat exchange medium 423 to circulate between the copper heat-absorbing heat exchanger 421 and the copper heat-releasing heat exchanger 422;

[0168] The blocking valve 91 is arranged at the outlet end of the upstream treatment tank; a clean valve 81 is also provided between each treatment tank; the clean valve 81 and the introduction valve 82 on each treatment tank are integrated into a multi-way control valve; the blocking valve 91, the discharge valve 92 and the exhaust valve 93 on each treatment tank are integrated into a multi-way control valve.

[0169] The transparent observation window 43 is made of high temperature resistant glass. The clean valve 81 is provided to ensure that the gas in the pipeline between adjacent ceramic tanks 31 will not be contaminated due to the influence of replacing the ceramic tank 31. In this way, after the new ceramic tank 31 is installed, the impurity gas can be replaced more quickly and better.

[0170] The device and method for purifying helium from a hydrogen-helium mixed gas include the following steps:

[0171] S1. Close all inlet valves 82 and outlet valves 92, and open all other valves;

[0172] S2, start the tank cleaning unit 7 to vacuum all the processing tanks until a predetermined vacuum degree is reached and then close the tank cleaning unit 7;

[0173] S3, close all exhaust valves 93, open all inlet valves 82, and make the pressure of the treatment tank consistent with the output end of the voltage stabilizing output unit 2;

[0174] S4. After repeating steps S2 and S3 a certain number of times, proceed to step S2. The specific number of operations can be used to detect the gas discharged through the exhaust valve 93. When the concentration of the impurity gas is reduced to a certain level, proceed to step S5.

[0175] S5. Start the electromagnetic heating assembly to heat the hydrogen-reduced oxide 39. Power the electromagnetic heating ring 41 so that it alternately heats the hydrogen-reduced oxide 39 at a frequency of 40 kHz and 200 kHz until the temperature of the hydrogen-reduced oxide 39 rises to 550 degrees Celsius and then maintains the temperature of the hydrogen-reduced oxide 39 between 500 and 600 degrees Celsius.

[0176] In terms of heating efficiency, Fe3O4 has both ferromagnetic and dielectric properties, resulting in higher overall losses and is suitable for low-frequency, high-efficiency heating. CuO relies on high conductivity, exhibiting significant eddy current effects at high frequencies, but with negligible magnetic losses. Regarding heating efficiency, Fe3O4's hysteresis losses are positively correlated with its magnetic permeability, while its eddy current losses are proportional to the square of its conductivity and the square of its frequency. CuO's eddy current losses are dominated by its conductivity, and its skin effect is significant at high frequencies.

[0177] The optimal frequencies for Fe3O4 and CuO are approximately 200kHz and 40kHz, respectively. Therefore, alternating heating can effectively heat them both to the reaction temperature. During the reaction process, this can prevent Fe3O4 and CuO from being unable to maintain the optimal reaction temperature in time due to endothermic reaction.

[0178] S6. Select a treatment tank as the head tank, and the adjacent upstream treatment tank as the tail pipe;

[0179] S7, close all the exhaust valves 93; close the clean valve 81 on the head tank, open the exhaust valve of the head tank; close the blocking valve 91 on the tail tank,

[0180] S8. Set the output pressure of the pressure-stabilizing output unit 2 to be greater than the static pressure of the device and greater than the external atmospheric pressure of the device; then open the inlet valve 82 between the pressure-stabilizing output unit 2 and the header tank;

[0181] S9, open the discharge valve 92 between the head tank and the gas output pipe 5;

[0182] S10, turning on the heat exchange pump 424, the pressure reduction and temperature reduction component 61, and the centrifugal separation component 62; the pressure reduction and temperature reduction component 61 controls the condensation of part of the water in the purified helium gas output from the gas output pipe 5;

[0183] S11, observing the color of ferroferric oxide in each processing tank through the transparent observation window 43 in real time;

[0184] When you need to replace any treatment tank, the steps are as follows:

[0185] SX1. The adjacent processing tank upstream of the head tank that needs to be replaced is used as the new tail tank, and the adjacent processing tank downstream of the head tank that needs to be replaced is used as the new head tank;

[0186] SX2, open the inlet valve 82 between the new head tank and the pressure-stabilizing output unit 2, the discharge valve 92 between the tail tank and the gas discharge pipe, and the clean valve 81 and the shut-off valve 91 between the original head tank and the tail tank. At the same time, close the inlet valve 82 between the original head tank and the pressure-stabilizing output unit 2, the discharge valve 92 between the original tail tank and the gas discharge pipe, and the clean valve 81 and the shut-off valve 91 between the new tail tank and the treatment tank to be replaced.

[0187] SX3, remove the treatment tank that needs to be replaced;

[0188] When a ceramic tank 31 needs maintenance or the hydrogen reduction oxide 39 reagent inside needs to be replaced, continuous production can be carried out in the terminal production line. The process only needs to follow the following steps: SS1. Add the treatment tank to be replaced into the device;

[0189] SS2, open the exhaust valve 93 of the replaced treatment tank, start the tank cleaning unit 7 to vacuum the replaced treatment tank, and when the vacuum level in the replaced treatment tank reaches the required level, close the tank cleaning unit 7;

[0190] SS3. Open the inlet valve 82 between the replaced treatment tank and the pressure-stabilizing output unit 2. When the pressure inside the replaced treatment tank is consistent with the pressure at the output end of the pressure-stabilizing output unit 2, close the inlet valve 82 between the replaced treatment tank and the pressure-stabilizing output unit 2.

[0191] SS4. After repeating steps SS2 and SS3 a certain number of times, follow step SS2.

[0192] SS5. Use the replaced processing tank as the new tail tank, open the discharge valve 92 between the new tail tank and the gas output pipe 5, and the clean valve 81 and the blocking valve 91 between the new tail tank and the upstream processing tank; close the discharge valve 92 between the new tail tank, the upstream processing tank and the gas output pipe 5.

[0193] In the process of switching to a new head tank and tail tank, the rate of the purified gas can be appropriately lowered. After replacing the new head tank and tail tank, some of the purified gas may enter the tail tank without being processed by the preset number of ceramic tank bodies 31. Therefore, the rate is reduced and the reaction time is extended to ensure that the purified concentration will not be affected by the replacement of the ceramic tank body 31 and will not experience large negative fluctuations.

[0194] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not limiting. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention can be modified or replaced by equivalents without departing from the purpose and scope of the technical solutions, which should all be included in the scope of the claims of the present invention.

Claims

1. A device for purifying helium from a hydrogen-helium mixture, characterized in that: include: Gas inlet pipe; A pressure-stabilizing output unit, the input end of which is connected to the output end of the gas input pipe, outputting the gas inputted from the gas input pipe at a stable pressure; A plurality of treatment tanks are connected end to end in a ring-shaped manner; a blocking valve is provided between each treatment tank; the head ends of the plurality of treatment tanks are connected to the output end of the voltage stabilizing output unit through respective inlet valves; A gas output pipe, wherein the tail ends of the plurality of treatment tanks are connected to the head end of the gas output pipe through respective discharge valves; The moisture processing unit is arranged at the tail end of the gas output pipe to separate the moisture from the gas in the gas output pipe; The tank cleaning unit is connected to the tail end of the treatment tank through the exhaust valve to extract the gas in the treatment tank; The processing tank includes: a ceramic tank body, a hydrogen-reduced oxide whose product is a solid, an electromagnetic heating component, and a heat recovery component; the interior of the ceramic tank body is hollow, the head end is connected to the output end of the voltage-stabilizing output unit, and the tail end is connected to the tank cleaning unit and the gas output pipe; the hydrogen-reduced oxide whose product is a solid is accommodated in the ceramic tank body; the electromagnetic heating component is arranged on the outside of the ceramic tank body, facing the hydrogen-reduced oxide whose product is a solid, and the electromagnetic heating component heats the hydrogen-reduced oxide whose product is a solid through high-frequency current; the heat recovery component, with a heat absorption end arranged at the tail end of the ceramic tank body and a heat release end arranged at the head end of the ceramic tank body, heats the gas flowing out of the ceramic tank body with the heat of the gas flowing into the ceramic tank body.

2. The device for purifying helium from a hydrogen-helium mixed gas according to claim 1, characterized in that: The ceramic tank body comprises: The head is barrel-shaped and has an air inlet at the bottom that is connected to the voltage-stabilizing output unit; the open end surface of the head is provided with a ring-shaped receiving groove of the tank body; The tail portion is barrel-shaped, with the same internal diameter as the head portion, and an air outlet is provided at the bottom thereof, which is connected to the voltage stabilizing output unit and the tank cleaning unit; the open end surface of the tail portion is provided with a tank annular protrusion matching the tank annular receiving groove; The high-temperature sealing ring of the tank body is arranged in the tank body receiving groove; after the head and tail are combined, the annular receiving groove of the tank body and the annular protrusion of the tank body are squeezed against each other; the high-temperature sealing ring of the tank body seals the tank body; the product is a solid hydrogen-reduced oxide contained in the receiving cavity formed by the head and tail parts.

3. The device for purifying helium from hydrogen-helium mixed gas according to claim 2, characterized in that: The ceramic tank body also includes: The bottom tube is made of ceramic and is barrel-shaped. It is buckled on the inner bottom surface of the tail and faces the air outlet. The side wall of the bottom tube is provided with a bottom vent hole. The inner bottom surface of the tail is provided with a bottom ring-shaped receiving groove that matches the lower end surface of the bottom tube. A bottom high-temperature sealing ring is provided in the bottom ring-shaped receiving groove. The center tube is made of ceramic material and is open at both ends. It is arranged between the outer bottom surface of the bottom tube and the inner bottom surface of the head, facing the air inlet; the inner wall of the center tube near the end of the bottom tube is provided with a penetrating internal vent hole; the inner side surface of the center tube, the inner bottom surface of the head, and the outer bottom surface of the bottom tube enclose an inner cavity; the inner bottom surface of the head is provided with a head-middle annular receiving groove matching the upper end of the center tube, and a head-middle high-temperature sealing ring is provided in the head-middle annular receiving groove; the outer bottom surface of the bottom tube is provided with a tail-middle annular receiving groove matching the lower end of the center tube, and a tail-middle high-temperature sealing ring is provided in the tail-middle annular receiving groove; The outer tube is made of ceramic and is open at both ends. It is arranged between the outer bottom surface of the bottom tube and the inner bottom of the head, and is sleeved on the outside of the central tube. The inner wall of the outer tube at one end close to the inner bottom surface of the head is provided with a penetrating external vent; the inner side of the outer tube, the outer side of the central tube, the inner bottom surface of the head, and the bottom surface of the bottom tube form a middle cavity; the inner and outer sides of the outer tube, the inner side surface of the head, the inner side surface of the tail, and the outer side surface of the bottom tube form an outer cavity; the inner bottom surface of the head is provided with a head outer annular receiving groove matching the upper end of the outer tube, and a head outer high-temperature sealing ring is provided in the head outer annular receiving groove; the outer bottom surface of the bottom tube is provided with a tail outer annular receiving groove matching the lower end of the outer tube, and a tail outer high-temperature sealing ring is provided in the tail outer annular receiving groove; The product is a solid hydrogen-reduced oxide contained in the inner cavity, the middle cavity and the outer cavity.

4. The device for purifying helium from hydrogen-helium mixed gas according to claim 3, characterized in that: The ceramic tank body also includes: The inner rod is made of ceramic and has an openable and closable internal hollow structure. It is housed within the inner cavity, with its outer surface in sealed contact with the inner side of the central tube. The top of the inner rod is provided with an inner air inlet grille, and the top and bottom of the inner rod are provided with air outlet grilles. The inner rod contains a solid hydrogen-reduced oxide product. The lower portion of the inner rod is provided with an inner air outlet hole corresponding to the inner air vent hole. The middle ring tube is made of ceramic and has an openable and closable internal hollow structure. Its outer contour is tubular, and its outer surface is in sealed contact with the inner side of the peripheral tube, and its inner surface is in sealed contact with the outer side of the central tube. The top of the middle ring tube is provided with a middle air outlet grille, and the bottom of the middle ring tube is provided with a middle air inlet grille. The middle ring tube contains a hydrogen-reduced oxide whose product is a solid. The lower portion of the middle ring tube is provided with a middle air inlet corresponding to the inner air vent, and the upper portion of the middle ring tube is provided with a middle air outlet corresponding to the outer air vent. The outer ring tube is made of ceramic and has an internal hollow structure that can be opened and closed. Its outer contour is in the shape of a tube. Its outer surface is in contact and sealed with the inner side surfaces of the head and tail, and its inner surface is in contact and sealed with the inner side surface of the outer ring. The top of the outer ring tube is provided with an outer air intake grille, and the bottom of the outer ring tube is provided with an outer air outlet grille. The product placed in the outer ring tube is a solid hydrogen-reduced oxide; the lower part of the outer ring tube is provided with an outer air outlet corresponding to the bottom air vent, and the upper part of the outer ring tube is provided with an outer air intake corresponding to the outer air outlet.

5. The device for purifying helium from hydrogen-helium mixed gas according to claim 4, characterized in that: The inner rod comprises an inner top section, a plurality of inner reaction sections, and an inner bottom section connected in sequence; The inner top section is a tubular structure with two ends open, the upper end of the inner top section is open and faces the air inlet of the head, and the lower end is fixedly connected to the upper end of the adjacent inner reaction section; The inner reaction section comprises an inner reaction chamber and an inner support tube; the upper end of the inner reaction chamber is provided with an inner air inlet grille, and the lower end is provided with an inner air outlet grille; the inner reaction chamber contains a hydrogen-reduced oxide whose product is a solid, and both ends of the inner support tube are open; The upper end of the inner bottom section is an open structure, which is connected and fixed to the inner support tube of the adjacent inner reaction section. The side of the inner bottom section is provided with a plurality of inner air outlet holes; when the inner bottom section is located at the bottom of the central tube, the inner air outlet holes are connected to the inner ventilation holes; The middle ring tube includes a middle top section, several middle reaction sections, and a middle bottom section connected in sequence; The lower end of the middle top section is an open structure, with a plurality of middle air outlet holes provided on the side, and the lower end is fixedly connected to the upper end of the adjacent middle reaction section; when the middle top section is located at the top of the central tube, the middle air outlet holes are connected to the external air vents; The middle reaction section comprises: a middle reaction chamber and a middle support tube; the middle reaction chamber is provided with a middle air outlet grille at the upper end and a middle air inlet grille at the lower end; the middle reaction chamber contains hydrogen-reduced oxides whose products are solids, and the middle support tube is open at both ends; The upper end of the middle bottom section is an open structure, which is connected and fixed to the middle support tube of the adjacent middle reaction section. The side of the middle bottom section is provided with a number of middle air inlet holes. When the middle bottom section is located at the bottom of the peripheral tube, the middle opening is connected to the inner air vent. The outer ring tube includes an outer top section, a plurality of outer reaction sections, and an outer bottom section connected in sequence; The lower end of the outer top section is an open structure, with a plurality of external air inlet holes provided on the side, and the lower end is fixedly connected to the upper end of the adjacent outer reaction section; when the outer top section is located at the inner bottom of the head, the external air inlet holes are connected to the external air vents; The outer reaction section comprises an outer reaction chamber and an outer support tube; the upper end of the outer reaction chamber is provided with an outer air inlet grille, and the lower end is provided with an outer air outlet grille; the outer reaction chamber contains a hydrogen-reduced oxide whose product is a solid, and both ends of the outer support tube are open; The upper end of the outer bottom section is an open structure, which is connected and fixed to the outer support tube of the adjacent outer reaction section. Several outgoing air holes are provided on the side of the outer bottom section; when the outer bottom section is located at the inner bottom of the tail, the outgoing air holes are connected to the bottom vent holes.

6. The device for purifying helium from hydrogen-helium mixed gas according to claim 5, characterized in that: The product is a solid hydrogen-reduced oxide including ferrosoferric oxide and copper oxide; The content of copper oxide in the plurality of inner reaction sections decreases as the distance from the top of the inner cavity increases; The content of copper oxide in the middle reaction sections increases as the distance from the top of the middle cavity increases; The content ratio of copper oxide contained in the plurality of outer reaction sections decreases as the distance from the top of the outer cavity increases; The number of inner reaction sections, middle reaction sections, and outer reaction sections is the same; The multiple inner reaction chambers of the inner reaction section, the multiple middle reaction chambers of the middle reaction section, and the multiple outer reaction chambers of the outer reaction section are kept at the same horizontal height from the inner bottom surface of the head to the inner bottom surface of the tail; the electromagnetic heating assembly includes the same number of electromagnetic heating rings as the inner reaction sections, and each electromagnetic heating ring is directly opposite to the height of each inner reaction chamber in the inner reaction section.

7. The device for purifying helium from hydrogen-helium mixed gas according to claim 6, characterized in that: The inner reaction chamber includes an upper rod and a lower rod connected by a threaded seal; the outer surface of the upper rod and / or the lower rod is provided with an inner annular groove; the inner annular groove is provided with an annular inner high-temperature sealing ring. When the inner reaction chamber is placed in the inner cavity, the inner high-temperature sealing ring and the inner side surface of the central tube are pressed and fixed against each other, sealing the upper and lower sides thereof; The middle reaction chamber comprises a middle upper ring disc and a middle lower ring disc connected by a threaded seal; a middle annular groove is provided on the outer surface of the middle upper ring disc and / or the middle lower ring disc; a ring-shaped middle and high temperature sealing ring is provided in the middle annular groove; when the middle reaction chamber is placed in the middle cavity body, the middle and high temperature sealing ring is pressed and fixed against the outer side surface of the central tube and the inner side surface of the peripheral tube, thereby sealing the upper and lower sides thereof; The outer reaction chamber includes an outer upper ring disk and an outer lower ring disk connected by threaded sealing; an outer annular groove is provided on the outer surface of the outer upper ring disk and / or the outer lower ring disk; an annular outer high-temperature sealing ring is provided in the outer annular groove. When the outer reaction chamber is placed in the outer cavity body, the outer high-temperature sealing ring and the outer side surface, the inner side surface of the head or the inner side surface of the tail of the outer tube are squeezed and fixed to each other, sealing the upper and lower sides thereof.

8. The device for purifying helium from hydrogen-helium mixed gas according to claim 7, characterized in that: The ferrosoferric oxide is in the form of a filament with a length of not less than 1 micron and a diameter of not more than 200 nanometers, and the copper oxide is in the form of a nanorod; The upper and lower ends of the inner reaction chamber, the middle reaction chamber and the outer reaction chamber are all provided with asbestos mesh filters; The asbestos mesh filter diameter at the top and bottom of the inner reaction section is not greater than 1 micron, and the asbestos mesh filter diameter between the top and bottom of the inner reaction section is not less than 1 micron; The asbestos mesh filter diameter at the top and bottom of the middle reaction section is not greater than 1 micron, and the asbestos mesh filter diameter between the top and bottom of the middle reaction section is not less than 1 micron; The asbestos mesh filter diameter at the top and bottom of the outer reaction section is not greater than 1 micron, and the asbestos mesh filter diameter between the top and bottom of the outer reaction section is not less than 1 micron.

9. The device for purifying helium from a hydrogen-helium mixed gas according to claim 8, characterized in that: A transparent observation window is provided on the head or tail; The moisture treatment unit includes: a pressure reduction and temperature reduction component and a centrifugal separation component; The heat recovery assembly includes: a copper heat-absorbing heat exchanger, a copper heat-releasing heat exchanger, a circulating heat exchange medium, and a heat exchange pump; the copper heat-absorbing heat exchanger is arranged at the rear end of the ceramic tank; the copper heat-releasing heat exchanger is arranged at the head end of the ceramic tank; the circulating heat exchange medium connects the copper heat-absorbing heat exchanger and the copper heat-releasing heat exchanger; the heat exchange pump drives the circulating heat exchange medium to circulate between the copper heat-absorbing heat exchanger and the copper heat-releasing heat exchanger; The blocking valve is arranged at the gas outlet end of the upstream treatment tank; a clean valve is also provided between each treatment tank; the clean valve and the introduction valve on each treatment tank are integrated into a multi-way control valve; the blocking valve, the discharge valve and the exhaust valve on each treatment tank are integrated into a multi-way control valve.

10. The device and method for purifying helium from a hydrogen-helium mixed gas according to claim 9, characterized in that: The following steps are involved: S1. Close all inlet valves and outlet valves, and open all other valves; S2. Start the tank cleaning unit to vacuum all the processing tanks until a predetermined vacuum degree is reached and then close the tank cleaning unit; S3. Close all exhaust valves and open all inlet valves to keep the pressure of the treatment tank consistent with the output end of the pressure-stabilizing output unit; S4. After repeating steps S2 and S3 a certain number of times, follow step S2; S5. Start the electromagnetic heating assembly to heat the hydrogen-reduced oxide, and energize the electromagnetic heating ring so that it heats the hydrogen-reduced oxide alternately at a frequency of 40 kHz and 200 kHz until the temperature of the hydrogen-reduced oxide rises to 550 degrees Celsius and then maintains the hydrogen-reduced oxide between 500 and 600 degrees Celsius; S6. Select a treatment tank as the head tank, and the adjacent upstream treatment tank as the tail pipe; S7, close all the exhaust valves; close the clean valve on the head tank, open the exhaust valve on the head tank; close the blocking valve on the tail tank, S8. Set the output pressure of the pressure-stabilizing output unit to be greater than the static pressure of the device and greater than the external atmospheric pressure of the device; then open the inlet valve between the pressure-stabilizing output unit and the header tank; S9, open the discharge valve between the head tank and the gas output pipe; S10, turning on the heat exchange pump, the pressure reduction and temperature reduction component, and the centrifugal separation component; the pressure reduction and temperature reduction component controls the condensation of part of the water in the purified helium output from the gas output pipe; S11. Observe the color of ferroferric oxide in each treatment tank through a transparent observation window in real time; When you need to replace any treatment tank, the steps are as follows: SX1. The adjacent processing tank upstream of the head tank that needs to be replaced is used as the new tail tank, and the adjacent processing tank downstream of the head tank that needs to be replaced is used as the new head tank; SX2. Open the inlet valve between the new header tank and the pressure-stabilizing output unit, the outlet valve between the tail tank and the gas discharge pipe, and the clean valve and shut-off valve between the original header tank and the tail tank. Simultaneously, close the inlet valve between the original header tank and the pressure-stabilizing output unit, the outlet valve between the original tail tank and the gas discharge pipe, and the clean valve and shut-off valve between the new tail tank and the treatment tank to be replaced. SX3, remove the treatment tank that needs to be replaced; When you need to replace any treatment tank, the steps are as follows: SS1. Add the treatment tank to be replaced into the device; SS2. Open the exhaust valve of the replaced treatment tank and start the tank cleaning unit to vacuum the replaced treatment tank. When the vacuum degree in the replaced treatment tank reaches the requirement, close the tank cleaning unit. SS3. Open the inlet valve between the replaced treatment tank and the pressure-stabilizing output unit. When the pressure inside the replaced treatment tank is consistent with the pressure at the output end of the pressure-stabilizing output unit, close the inlet valve between the replaced treatment tank and the pressure-stabilizing output unit. SS4. After repeating steps SS2 and SS3 a certain number of times, follow step SS2. SS5. Use the replaced treatment tank as the new tail tank, open the discharge valve between the new tail tank and the gas output pipe, the clean valve and the shut-off valve between the new tail tank and the upstream treatment tank; close the discharge valve between the new tail tank and the upstream treatment tank and the gas output pipe.

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