A purification device system and method for oxygen, nitrogen and crude neon-helium gas

Abstract

The present invention relates to a purification device system and method for oxygen, nitrogen and crude neon and helium gases. Based on non-cryogenic gas purification technology, the dehydrogenation of crude neon and helium gases is coupled with the regeneration of nitrogen deoxygenation adsorbent, and the nitrogen purification is coupled with the regeneration process of oxygen removal of carbon dioxide and water. The oxygen, nitrogen and crude neon and helium gases can be purified and impurities removed in a linked manner, thereby realizing efficient purification of nitrogen, oxygen and crude neon and helium gases.

Description

Technical Field

[0001] The present invention relates to the technical field of gas separation, and particularly to a purification device system and method for oxygen, nitrogen and crude neon-helium gas. Background Art

[0002] At present, the purification of air separation nitrogen, the purification of air separation oxygen, and the removal of hydrogen and nitrogen from air separation crude neon-helium mainly rely on cryogenic distillation means. Especially in the process of removing hydrogen and nitrogen from air separation crude neon-helium, due to the extremely low boiling points of neon and helium, the pressure required for the cryogenic distillation process is extremely high, further making the equipment for deep purification and purification of crude neon-helium bulky, and the equipment has extremely high requirements for thermal insulation. For the purification processes of air separation nitrogen and air separation oxygen, for example, CN112229143A discloses a device for producing oxygen and nitrogen by separating air through cryogenic distillation, which includes a raw air compressor, a precooling system, a purification system, a medium-pressure air booster, a low-pressure air booster, an air separation cold box, and an oxygen booster connected in sequence. The purification cost of this device is relatively high, and its application is limited in industrial production. For electronic-grade ultra-high-purity nitrogen with a volume purity higher than 99.9999%, it is usually obtained by purifying air separation high-purity nitrogen, that is, nitrogen with a volume purity ≥ 99.999% through a purifier. However, there is also the problem that the purifier is expensive, and its working condition is high temperature. In addition, the getter needs to be replaced regularly, and the use cost is relatively high.

[0003] The non-cryogenic method is a new gas separation means developed since the 1990s. Compared with the cryogenic distillation method, the non-cryogenic gas separation has the advantages of fast response speed, operability at room temperature, compact equipment structure, high separation coefficient between different components of the gas, and being more suitable for the separation of precision systems than cryogenic distillation.

[0004] CN117566701A discloses a device for purifying crude neon-helium by the non-cryogenic method, which includes a buffer tank, a catalytic device, a room-temperature adsorption device, a membrane separation and enrichment neon-helium device, and a cryogenic quantum adsorption device. The inlet of the buffer tank is connected to the outlet of air separation crude neon-helium, the outlet of the buffer tank is connected to a relay compressor, and the catalytic device is connected behind the relay compressor. An oxygen addition catalytic device and a hydrogen addition catalytic device are respectively installed in the catalytic device. The outlet of the catalytic device is connected to a crude neon-helium and catalytic device, which is connected to a heat exchanger to recover heat and then connected to a cooler for cooling. The outlet of the cooler is connected to the relay compressor, and after pressurization, it enters the room-temperature adsorption device. The room-temperature adsorption device is sequentially connected to a membrane separation and enrichment neon-helium device and a cryogenic quantum adsorption device behind. However, this device is only applicable to the purification of crude neon-helium gas and cannot achieve the coordinated purification and impurity removal of air separation nitrogen, air separation oxygen, and air separation crude neon-helium, with certain application limitations.

[0005] Therefore, in view of the shortcomings of the prior art, there is an urgent need to provide a device system that can achieve coordinated and efficient purification of air-separated nitrogen, air-separated oxygen, and air-separated crude neon and helium. Summary of the invention

[0006] The object of the present invention is to provide a purification device system and method for oxygen, nitrogen and crude neon-helium gases, wherein the nitrogen, oxygen and crude neon-helium gases produced by an air separation device are linked and purified and impurities removed by non-cryogenic gas separation technology, thereby obtaining high-purity nitrogen, high-purity oxygen and a neon-helium mixed gas.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a purification device system for oxygen, nitrogen and crude neon helium, the purification device system comprising a heat exchanger, the heat exchanger being provided with a nitrogen inlet, a nitrogen outlet, an oxygen inlet, an oxygen outlet, a crude neon helium inlet, a crude neon helium outlet, a dehydrogenation neon helium inlet and a dehydrogenation neon helium outlet; the nitrogen outlet and the crude neon helium outlet are both connected to a deoxygenation tower, the deoxygenation tower discharges high-purity nitrogen and dehydrogenation neon helium, the dehydrogenation neon helium enters the heat exchanger from the dehydrogenation neon helium inlet and is discharged from the dehydrogenation neon helium outlet, and then enters a permeation membrane assembly and an impurity adsorption tower in sequence.

[0009] The oxygen outlet is connected to the first supercharger, the hydrocarbon removal device and the heat balancer in sequence. The oxygen discharged from the heat balancer flows through the heat exchanger and enters the carbon dioxide and water adsorption tower and the nitride removal device in sequence. The discharged oxygen flows through the heat exchanger again and enters the oxygen purification tower. The high-purity nitrogen part discharged from the deoxygenation tower enters the carbon dioxide and water adsorption tower for purging, takes out carbon dioxide and water, and returns to the pipeline where the nitrogen outlet is located after carbon dioxide and water are removed by the nitrogen drying device.

[0010] The purification device system also includes an ice dryer, which is used to provide a cold source for the impurity adsorption tower and the oxygen purification tower.

[0011] The oxygen, nitrogen and crude neon-helium purification device system provided by the present invention can purify and remove impurities in nitrogen, oxygen and crude neon-helium produced by an air separation device. Specifically, the air separation nitrogen is reheated through a heat exchanger and then deoxygenated in a deoxygenation tower to obtain high-purity nitrogen; the air separation oxygen is reheated and pressurized by a heat exchanger and a first supercharger, and then hydrocarbons are removed by a hydrocarbon removal device, and then CO2 and H2O are adsorbed by a carbon dioxide and water adsorption tower, and then NO is removed in a nitride removal device. xIt is reduced to N2 and O2, and finally high-purity oxygen is obtained through the oxygen purification tower; the hydrogen removal from the crude neon-helium gas separated by air and the purification process of the air-separated nitrogen are linked. When the oxygen absorption of the deoxidation tower is saturated, the heated crude neon-helium gas is introduced to remove hydrogen in the crude neon-helium gas while realizing the regeneration of nitrogen purification; after the hydrogen is removed, the crude neon-helium gas is introduced into the permeable membrane module and the impurity adsorption tower to obtain a neon-helium mixed gas; there is a linkage between the purification of air-separated nitrogen and the purification of air-separated oxygen, that is, a part of the purified nitrogen is used as the regeneration gas source for oxygen purification, and the discharged nitrogen converges with the air-separated nitrogen.

[0012] Preferably, the outlet of the crude neon-helium gas is connected to the deoxidation tower through an electric heater.

[0013] The deoxidation tower includes a first deoxidation tower and a second deoxidation tower that operate and regenerate alternately.

[0014] The "alternate operation and regeneration" means that when the first deoxidation tower is working, the second deoxidation tower is regenerating, and vice versa, when the second deoxidation tower is working, the first deoxidation tower is regenerating.

[0015] Preferably, the permeable membrane module includes a first permeable membrane, a second permeable membrane, and a third permeable membrane connected in sequence along the flow direction of the hydrogen-removed neon-helium gas. The first permeable membrane, the second permeable membrane, and the third permeable membrane are each independently provided with a permeate side and a non-permeate side.

[0016] The non-permeate side of the first permeable membrane is provided with an exhaust gas outlet.

[0017] The waste gas discharged from the non-permeate side of the second permeable membrane flows through a first booster valve and then returns to the first permeable membrane. The pressure gas source of the first booster valve comes from the inlet of the hydrogen-removed neon-helium gas.

[0018] The waste gas discharged from the non-permeate side of the third permeable membrane flows through a second booster valve and then returns to the first permeable membrane. The pressure gas source of the second booster valve comes from the waste gas discharged from the non-permeate side of the second permeable membrane.

[0019] The exhaust gas outlet described in the present invention is directly connected to the atmosphere or recycled and enters the Ne enrichment system.

[0020] Preferably, the outlet of the impurity adsorption tower is connected to a neon-helium gas refining system.

[0021] The impurity adsorption tower includes a first impurity adsorption tower and a second impurity adsorption tower that operate and regenerate alternately.

[0022] The waste gas desorbed by the re-warming of the regenerated impurity adsorption tower is safely discharged through the impurity adsorption tower exhaust pipeline.

[0023] Preferably, the carbon dioxide and water adsorption tower includes a first adsorption tower and a second adsorption tower that operate and regenerate alternately.

[0024] Part of the high-purity nitrogen discharged from the deoxidation tower enters the high-purity nitrogen system, part enters the first permeable membrane, and part flows through the heat balancer and the second booster and enters the regenerated carbon dioxide and water adsorption tower.

[0025] Part of the high-purity nitrogen enters the first permeable membrane to increase the partial pressure of Ne+N2 in the crude neon-helium gas, thereby increasing the recovery rate of Ne+He in the first permeable membrane; part enters the regenerated carbon dioxide and water adsorption tower to purge the adsorbent in the carbon dioxide and water adsorption tower to desorb and carry away the carbon dioxide and water adsorbed by the adsorbent.

[0026] Preferably, the oxygen purification tower includes a first purification tower and a second purification tower that operate and regenerate alternately.

[0027] The outlet of the oxygen purification tower is independently connected to the high-purity oxygen system and the vacuum pump respectively.

[0028] The high-purity oxygen discharged from the oxygen purification tower can enter the high-purity oxygen system or can be directly evacuated after entering the vacuum pump.

[0029] Preferably, the ice dryer is provided with a refrigerant outlet and a refrigerant inlet. The refrigerant outlet is independently connected to the inlet of the cold quantity supply chamber of the impurity adsorption tower, the inlet of the cold quantity supply chamber of the oxygen purification tower, and the inlet of the refrigerant heat exchange pipeline respectively. The refrigerant inlet is independently connected to the outlet of the cold quantity supply chamber of the impurity adsorption tower, the outlet of the cold quantity supply chamber of the oxygen purification tower, and the outlet of the refrigerant heat exchange pipeline respectively. The inlet of the refrigerant heat exchange pipeline is connected to the outlet of the refrigerant heat exchange pipeline through the heat exchanger.

[0030] Preferably, the refrigerant inlet is provided with a first pressure sensor and a second pressure sensor.

[0031] Before being put into use, the impurity adsorption tower and the oxygen purification tower in the present invention are cooled by an ice dryer to reach the working temperature range.

[0032] In a second aspect, the present invention provides a method for purifying oxygen, nitrogen, and crude neon-helium gas. The purification method is carried out by the oxygen, nitrogen, and crude neon-helium gas purification device system described in the first aspect. The purification method includes the following steps:

[0033] (1) The air separation nitrogen is physically deoxidized after being reheated by the first heat exchange to obtain high-purity nitrogen;

[0034] (2) The air separation crude neon-helium gas enters the oxygen absorption saturated environment formed after the physical deoxidation in step (1) for hydrogen removal. The obtained hydrogen-removed neon-helium gas is reheated by the second heat exchange and then subjected to membrane separation and impurity adsorption in sequence to obtain a neon-helium mixed gas;

[0035] (3) The air-separated oxygen undergoes the third heat exchange and reheating, pressurization, catalytic hydrocarbon removal, the first heat recovery and the second heat recovery, carbon dioxide and water adsorption treatment, and nitride removal treatment in sequence. The obtained oxygen undergoes the fourth heat exchange and reheating and is then purified to obtain high-purity oxygen.

[0036] The high-purity nitrogen gas in step (1) enters the water vapor environment formed after the carbon dioxide and water adsorption treatment in step (3) for purging, then takes out the carbon dioxide and water, and returns to the physical deoxygenation in step (1) after the water vapor removal treatment.

[0037] During the impurity adsorption in step (2) and the purification process in step (3), cold circulation is provided.

[0038] The purification method of oxygen, nitrogen and crude neon and helium provided by the present invention can purify and remove impurities in nitrogen, oxygen and crude neon and helium produced by an air separation device. Specifically, the air separation nitrogen is reheated through a heat exchanger and then physically deoxygenated at room temperature; the air separation oxygen is reheated and pressurized and then C is removed by high-temperature physical catalysis. m H n , and then adsorb CO2 and H2O at room temperature; then, NO x Reduced to N2 and O2, and finally the volume concentration of N2 and O2 is controlled below 0.3ppm by temperature variable adsorption; the dehydrogenation of crude neon-helium gas in air separation is linked with the nitrogen purification process in air separation. When the nitrogen purification tower is saturated with oxygen, heated crude neon-helium gas is introduced to realize nitrogen purification regeneration and remove H2 in the crude neon-helium gas at the same time; after hydrogen is removed, the crude neon-helium gas is combined with membrane separation and low-temperature adsorption to control the volume concentration of impurity nitrogen below 0.1ppm; air separation nitrogen purification and air separation oxygen purification are linked, that is, the purified nitrogen part is used as the regeneration gas source for oxygen purification, and the discharged nitrogen merges with the air separation nitrogen.

[0039] Preferably, the temperature of the air separation nitrogen after the first heat exchange and rewarming in step (1) is 20-30°C, for example, 20°C, 22°C, 25°C, 28°C or 30°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0040] Preferably, the purity of the high-purity nitrogen in step (1) is ≥ 7N, for example, 7N or 99.99999%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0041] Preferably, the physical deoxygenation in step (1) comprises deoxygenation and regeneration which are performed simultaneously, and oxygen desorption and dehydrogenation of crude neon and helium gas from air separation are performed during the regeneration process.

[0042] Before the dehydrogenation described in step (2), the air separation crude neon-helium gas is heated to 180 - 205 °C. For example, it can be 180 °C, 185 °C, 190 °C, 200 °C or 205 °C, but it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0043] The membrane separation described in step (2) includes the first membrane separation, the second membrane separation, and the third membrane separation carried out in sequence. The waste gas discharged after the first membrane separation is discharged to the atmosphere or recycled for treatment. The waste gas discharged after the second membrane separation is pressurized and returned to the first membrane separation. The waste gas discharged after the third membrane separation is pressurized and returned to the first membrane separation.

[0044] Part of the high-purity nitrogen gas described in step (1) enters the first membrane separation and converges with the dehydrogenated neon-helium gas.

[0045] The impurity adsorption described in step (2) includes adsorption and regeneration carried out simultaneously. During the adsorption process, the temperature is controlled at -100 to -84 °C, and during the regeneration process, the temperature is controlled at -10 to 0 °C to realize the desorption of the adsorbed impurity gas.

[0046] During the adsorption process, the temperature is controlled at -100 to -84 °C. For example, it can be -100 °C, -95 °C, -90 °C or -84 °C, but it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0047] During the regeneration process, the temperature is controlled at -10 to 0 °C. For example, it can be -10 °C, -8 °C, -5 °C, -2 °C or 0 °C, but it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0048] Preferably, the volume concentration of hydrogen in the dehydrogenated neon-helium gas described in step (2) ≤ 0.9 ppm, and the volume concentration of nitrogen ≥ 72%.

[0049] The volume concentration of hydrogen in the dehydrogenated neon-helium gas ≤ 0.9 ppm. For example, it can be 0.9 ppm, 0.8 ppm, 0.7 ppm, 0.6 ppm or 0.5 ppm, but it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0050] The volume concentration of nitrogen in the dehydrogenated neon-helium gas ≥ 72%. For example, it can be 72%, 73%, 75%, 78% or 80%, but it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0051] Preferably, the volume concentration of nitrogen in the dehydrogenated neon-helium gas after the first membrane separation ≤ 33%, the volume concentration of nitrogen in the dehydrogenated neon-helium gas after the second membrane separation ≤ 4.7%, and the volume concentration of nitrogen in the dehydrogenated neon-helium gas after the third membrane separation ≤ 0.3%.

[0052] The volume concentration of nitrogen in the hydrogen, neon, and helium gas after the first membrane separation is ≤ 33%, and can be, for example, 33%, 30%, 25%, 20%, or 15%, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0053] The volume concentration of nitrogen in the hydrogen, neon, and helium gas after the second membrane separation is ≤ 4.7%, and can be, for example, 4.7%, 4.5%, 4%, 3.5%, or 3%, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0054] The volume concentration of nitrogen in the hydrogen, neon, and helium gas after the third membrane separation is ≤ 0.3%, and can be, for example, 0.3%, 0.25%, 0.2%, 0.15%, or 0.1%, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0055] Preferably, the volume concentration of hydrogen in the neon-helium mixture gas in step (2) is ≤ 0.2 ppm, and the volume concentration of nitrogen is ≤ 0.1 ppm.

[0056] The volume concentration of hydrogen in the neon-helium mixture gas is ≤ 0.2 ppm, and can be, for example, 0.2 ppm, 0.18 ppm, 0.15 ppm, 0.12 ppm, or 0.1 ppm, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0057] The volume concentration of nitrogen in the neon-helium mixture gas is ≤ 0.1 ppm, and can be, for example, 0.1 ppm, 0.08 ppm, 0.05 ppm, 0.02 ppm, or 0.01 ppm, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0058] Preferably, the end point of the pressurization in step (3) is 7 - 18 ata(A), and can be, for example, 7 ata(A), 10 ata(A), 12 ata(A), 15 ata(A), or 18 ata(A), but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0059] Preferably, the temperature of the catalytic hydrocarbon removal in step (3) is 270 - 320 °C, and can be, for example, 270 °C, 280 °C, 300 °C, 310 °C, or 320 °C, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0060] The carbon dioxide and water adsorption treatment in step (3) includes adsorption and regeneration performed simultaneously. During the regeneration process, the high-purity nitrogen gas in step (1) is heated at 170-200° C. and then enters the water vapor environment formed after the carbon dioxide and water adsorption treatment for purging. For example, the temperature may be 170° C., 180° C., 185° C., 190° C. or 200° C., but is not limited to the listed values. Other values ​​within the numerical range not listed are also applicable.

[0061] The temperature of the nitride removal treatment in step (3) is 320-350°C, for example, 320°C, 330°C, 340°C, 345°C or 350°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0062] The purification treatment in step (3) includes nitrogen and argon adsorption treatment and regeneration analysis performed simultaneously.

[0063] Preferably, the purity of the high-purity oxygen is ≥6N, and the total volume concentration of nitrogen and argon in the high-purity oxygen is ≤0.3ppm.

[0064] The purity of the high-purity oxygen is ≥ 6N, for example, it can be 6N or 7N, but it is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0065] The total volume concentration of nitrogen and argon in the high-purity oxygen is ≤0.3ppm, for example, it can be 0.3ppm, 0.25ppm, 0.2ppm, 0.15ppm or 0.1ppm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0066] Compared with the prior art, the present invention has the following beneficial effects:

[0067] The oxygen, nitrogen and crude neon-helium purification device system provided by the present invention can purify and remove impurities in nitrogen, oxygen and crude neon-helium produced by an air separation device. Specifically, the air separation nitrogen is reheated through a heat exchanger and then deoxygenated in a deoxygenation tower to obtain high-purity nitrogen; the air separation oxygen is reheated and pressurized by a heat exchanger and a first supercharger, and then hydrocarbons are removed by a hydrocarbon removal device, and then CO2 and H2O are adsorbed by a carbon dioxide and water adsorption tower, and then NO is removed in a nitride removal device. xIt is reduced to N2 and O2, and finally high-purity oxygen is obtained through the oxygen purification tower; the hydrogen removal from the air separation crude neon-helium gas is linked with the air separation nitrogen purification process. When the oxygen absorption of the deoxidation tower is saturated, heated crude neon-helium gas is introduced to remove hydrogen in the crude neon-helium gas while realizing the regeneration of nitrogen purification; after hydrogen removal, the crude neon-helium gas is introduced into the permeable membrane module and the impurity adsorption tower to obtain a neon-helium mixed gas; there is a linkage between the air separation nitrogen purification and the air separation oxygen purification, that is, part of the purified nitrogen is used as the regeneration gas source for oxygen purification, and the discharged nitrogen converges with the air separation nitrogen; by using the purification device system to conduct linked purification of oxygen, nitrogen and crude neon-helium gas, nitrogen can be purified to an impurity oxygen volume concentration of less than 0.1 ppm; oxygen can be purified to a total volume concentration of impurities nitrogen and argon of less than 0.3 ppm; crude neon-helium gas can be purified to an impurity hydrogen volume concentration of less than 0.2 ppm and a nitrogen volume concentration of less than 0.1 ppm. Description of the Drawings

[0068] Figure 1 It is a schematic structural diagram of the purification device system for oxygen, nitrogen and crude neon-helium gas provided in Embodiment 1 of the present invention.

[0069] Wherein: 1. First shut-off valve; 2. Second shut-off valve; 3. Third shut-off valve; 4. Fourth shut-off valve; 5. Fifth shut-off valve; 6. Second deoxidation tower; 7. First deoxidation tower; 8. Sixth shut-off valve; 9. Seventh shut-off valve; 10. Eighth shut-off valve; 11. Ninth shut-off valve; 12. Tenth shut-off valve; 13. Heat balancer; 14. Second booster; 15. Eleventh shut-off valve; 16. Twelfth shut-off valve; 17. Thirteenth shut-off valve; 18. Fourteenth shut-off valve; 19. Fifteenth shut-off valve; 20. Sixteenth shut-off valve; 21. Second adsorption tower; 22. First adsorption tower; 23. Seventeenth shut-off valve; 24. Eighteenth shut-off valve; 25. Nineteenth shut-off valve; 26. Nitride removal device; 27. Twentieth shut-off valve; 28. Twenty-first shut-off valve; 29. Twenty-second shut-off valve; 30. Second purification tower; 31. First purification tower; 32. Twenty-third shut-off valve; 33. Twenty-fourth shut-off valve; 34. Twenty-fifth shut-off valve; 35. Twenty-sixth shut-off valve; 36. Vacuum pump; 37. Twenty-seventh shut-off valve; 38. Twenty-eighth shut-off valve; 39. Twenty-ninth shut-off valve; 40. Thirtieth shut-off valve; 41. Thirty-first shut-off valve; 42-1. First pressure sensor; 42-2. Second pressure sensor; 43. Nitrogen inlet; 44. Oxygen inlet; 45. Cold end inlet; 46. Coarse neon-helium inlet; 47. First hot end inlet; 48. Third hot end inlet; 49. Second hot end inlet; 50. Second hot end outlet; 51. Third hot end outlet; 52. First hot end outlet; 53. Coarse neon-helium outlet; 54. Cold end outlet; 55. Oxygen outlet; 56. Nitrogen outlet; 57. Heat exchanger; 58. First booster; 59. Electric heater; 60. Hydrocarbon removal device; 61. Nitrogen drying device; 62. Thirty-second shut-off valve; 63. Thirty-third shut-off valve; 64. Thirty-fourth shut-off valve; 65. First permeable membrane; 66. Thirty-fifth shut-off valve; 67. First booster valve; 68. Second booster valve; 69. Second permeable membrane; 70. Thirty-sixth shut-off valve; 71. Third permeable membrane; 72. Thirty-seventh shut-off valve; 73. Thirty-eighth shut-off valve; 74. First impurity adsorption tower; 75. Second impurity adsorption tower; 76. Thirty-ninth shut-off valve; 77. Fortieth shut-off valve. Detailed implementation manners

[0070] The technical solution of the present invention will be further described below through specific implementation manners. Those skilled in the art should understand that the embodiments are only for helping to understand the present invention and should not be regarded as specific limitations on the present invention.

[0071] The present invention provides a purification device system for oxygen, nitrogen and coarse neon-helium. The purification device system includes a heat exchanger, and the heat exchanger is provided with a nitrogen inlet, a nitrogen outlet, an oxygen inlet, an oxygen outlet, a coarse neon-helium inlet, a coarse neon-helium outlet, a hydrogen-removed neon-helium inlet and a hydrogen-removed neon-helium outlet.

[0072] The nitrogen outlet is connected to a deoxidation tower. The crude neon-helium gas outlet is connected to the deoxidation tower through an electric heater. The deoxidation tower includes a first deoxidation tower and a second deoxidation tower that operate alternately and are regenerated. The deoxidation tower discharges high-purity nitrogen and hydrogen-removed neon-helium gas. The hydrogen-removed neon-helium gas enters a heat exchanger from the hydrogen-removed neon-helium gas inlet and is discharged from the hydrogen-removed neon-helium gas outlet, and then successively enters a permeable membrane module and an impurity adsorption tower. The impurity adsorption tower includes a first impurity adsorption tower and a second impurity adsorption tower that operate alternately and are regenerated. The outlet of the impurity adsorption tower is connected to a neon-helium gas refining system.

[0073] The permeable membrane module includes a first permeable membrane, a second permeable membrane, and a third permeable membrane that are successively connected along the flow direction of the hydrogen-removed neon-helium gas. The first permeable membrane, the second permeable membrane, and the third permeable membrane are each independently provided with a permeate side and a non-permeate side. An exhaust gas outlet is provided on the non-permeate side of the first permeable membrane. The exhaust gas discharged from the non-permeate side of the second permeable membrane flows through a first booster valve and then returns to the first permeable membrane. The pressure air source of the first booster valve comes from the hydrogen-removed neon-helium gas inlet. The exhaust gas discharged from the non-permeate side of the third permeable membrane flows through a second booster valve and then returns to the first permeable membrane. The pressure air source of the second booster valve comes from the exhaust gas discharged from the non-permeate side of the second permeable membrane.

[0074] The oxygen outlet is successively connected to a first booster, a hydrocarbon removal device, and a heat balancer. The oxygen discharged from the heat balancer flows through a heat exchanger and then successively enters a carbon dioxide and water adsorption tower and a nitride removal device. The discharged oxygen flows through the heat exchanger again and then enters an oxygen purification tower. The carbon dioxide and water adsorption tower includes a first adsorption tower and a second adsorption tower that operate alternately and are regenerated. The oxygen purification tower includes a first purification tower and a second purification tower that operate alternately and are regenerated. The outlet of the oxygen purification tower is independently connected to a high-purity oxygen system and a vacuum pump respectively.

[0075] Part of the high-purity nitrogen discharged from the deoxidation tower enters the high-purity nitrogen system, part enters the first permeable membrane, part flows through the heat balancer and a second booster, enters the regenerated carbon dioxide and water adsorption tower for purging to carry out carbon dioxide and water, and after removing carbon dioxide and water through a nitrogen drying device, returns to the pipeline where the nitrogen outlet is located.

[0076] The purification device system further includes an ice dryer, which is used to provide a cold source for the impurity adsorption tower and the oxygen purification tower; the ice dryer is provided with a refrigerant outlet and a refrigerant inlet, the refrigerant outlet is independently connected to the cold quantity supply chamber inlet of the impurity adsorption tower, the cold quantity supply chamber inlet of the oxygen purification tower, and the refrigerant heat exchange pipeline inlet respectively, and the refrigerant inlet is independently connected to the cold quantity supply chamber outlet of the impurity adsorption tower, the cold quantity supply chamber outlet of the oxygen purification tower, and the refrigerant heat exchange pipeline outlet respectively, and the refrigerant heat exchange pipeline inlet is connected to the refrigerant heat exchange pipeline outlet through the heat exchanger; the refrigerant inlet is provided with a first pressure sensor and a second pressure sensor.

[0077] The present invention also provides a purification method for oxygen, nitrogen, and crude neon-helium gas. The purification method is carried out by the purification device system for oxygen, nitrogen, and crude neon-helium gas, and the purification method includes the following steps:

[0078] (1) Physically deoxygenate the air separation nitrogen at 20-30°C obtained after the first heat exchange and rewarming to obtain high-purity nitrogen with a purity ≥ 7N; the physical deoxygenation includes deoxygenation and regeneration carried out simultaneously, and during the regeneration process, oxygen desorption and hydrogen removal from the air separation crude neon-helium gas are carried out.

[0079] (2) Heat the air separation crude neon-helium gas to 180-205°C and then enter the oxygen absorption saturation environment formed after the physical deoxygenation in step (1) for hydrogen removal. The obtained hydrogen-removed neon-helium gas is reheated through the second heat exchange and then subjected to membrane separation and impurity adsorption in sequence to obtain a neon-helium mixed gas; the volume concentration of hydrogen in the hydrogen-removed neon-helium gas ≤ 0.9 ppm, and the volume concentration of nitrogen ≥ 72%; the volume concentration of hydrogen in the neon-helium mixed gas ≤ 0.2 ppm, and the volume concentration of nitrogen ≤ 0.1 ppm;

[0080] The membrane separation includes first membrane separation, second membrane separation, and third membrane separation carried out in sequence. The waste gas discharged after the first membrane separation is discharged to the atmosphere or recycled and treated. The waste gas discharged after the second membrane separation is pressurized and returned to the first membrane separation. The waste gas discharged after the third membrane separation is pressurized and returned to the first membrane separation; a part of the high-purity nitrogen in step (1) enters the first membrane separation and converges with the hydrogen-removed neon-helium gas; the volume concentration of nitrogen in the hydrogen-removed neon-helium gas after the first membrane separation ≤ 33%, the volume concentration of nitrogen in the hydrogen-removed neon-helium gas after the second membrane separation ≤ 4.7%, and the volume concentration of nitrogen in the hydrogen-removed neon-helium gas after the third membrane separation ≤ 0.3%;

[0081] The impurity adsorption includes adsorption and regeneration carried out simultaneously. During the adsorption process, the temperature is controlled at -100 to -84°C, and during the regeneration process, the temperature is controlled at -10 to 0°C to realize the desorption of the adsorbed impurity gas.

[0082] (3)The oxygen separated by air separation is reheated through the third heat exchanger, pressurized to 7-18 ata(A), catalytically dehydrocarbonized at 270-320 °C, subjected to the first heat recovery and the second heat recovery, carbon dioxide and water adsorption treatment, and nitride removal treatment at 320-350 °C. The obtained oxygen is reheated through the fourth heat exchanger and then purified to obtain high-purity oxygen; the purity of the high-purity oxygen ≥ 6N, and the total volume concentration of nitrogen and argon in the high-purity oxygen ≤ 0.3 ppm;

[0083] The carbon dioxide and water adsorption treatment includes adsorption and regeneration carried out simultaneously. During the regeneration process, a part of the high-purity nitrogen in step (1) is heated to 170-200 °C and then enters the water vapor environment formed after the carbon dioxide and water adsorption treatment for purging, and then carbon dioxide and water are carried out, and after passing through the water vapor removal treatment, it returns to the physical deoxidation in step (1);

[0084] The purification treatment includes nitrogen and argon adsorption treatment and regeneration analysis carried out simultaneously;

[0085] During the impurity adsorption in step (2) and the purification treatment in step (3), cold energy is cyclically supplied.

[0086] The technical solution of the present invention will be further described below through specific embodiments.

[0087] Example 1

[0088] This example provides a purification device system for oxygen, nitrogen and crude neon-helium, as Figure 1 shown, the nitrogen, oxygen and crude neon-helium come from the air separation product gas.

[0089] The nitrogen inlet pipeline is connected to the nitrogen inlet 43 of the heat exchanger 57 through the first stop valve 1. The nitrogen outlet 56 of the heat exchanger 57 is simultaneously connected to the inlet of the fourth stop valve 4, the inlet of the fifth stop valve 5, and the outlet of the nitrogen drying device 61; the outlet of the fourth stop valve 4 is simultaneously connected to the outlet of the eighth stop valve 10 and the inlet of the first deoxidation tower 7; the outlet of the fifth stop valve 5 is simultaneously connected to the outlet of the ninth stop valve 11 and the inlet of the second deoxidation tower 6.

[0090] The inlets of the eighth stop valve 10 and the ninth stop valve 11 are jointly connected to the outlet of the electric heater 59; the inlet of the electric heater 59 is connected to the crude neon-helium outlet 53 of the heat exchanger 57. The crude neon-helium inlet 46 of the heat exchanger 57 is connected to the outlet of the third stop valve 3, and the inlet of the third stop valve 3 is connected to the crude neon-helium inlet pipeline.

[0091] The outlet of the first deoxidation tower 7 is simultaneously connected to the inlet of the seventh stop valve 9 and the inlet of the thirty-third stop valve 63; the outlet of the second deoxidation tower 6 is simultaneously connected to the inlet of the sixth stop valve 8 and the inlet of the thirty-second stop valve 62; the outlets of the sixth stop valve 8 and the seventh stop valve 9 are simultaneously connected to the first hot end inlet 47 of the heat exchanger 57; the outlets of the thirty-second stop valve 62 and the thirty-third stop valve 63 are simultaneously connected to the inlet of the tenth stop valve 12, the high-purity nitrogen system, and the inlet of the thirty-fourth stop valve 64; the outlet of the tenth stop valve 12 is connected to the cold end inlet of the heat balancer 13, and the cold end outlet of the heat balancer 13 is connected to the inlet of the second booster 14. The outlet of the second booster 14 is simultaneously connected to the inlet of the eleventh stop valve 15 and the inlet of the twelfth stop valve 16.

[0092] The outlet of the eleventh stop valve 15 is simultaneously connected to the outlet of the fifteenth stop valve 19 and the inlet of the first adsorption tower 22; the outlet of the twelfth stop valve 16 is simultaneously connected to the outlet of the sixteenth stop valve 20 and the inlet of the second adsorption tower 21; the outlet of the first adsorption tower 22 is simultaneously connected to the inlet of the thirteenth stop valve 17 and the inlet of the eighteenth stop valve 24; the outlet of the second adsorption tower 21 is simultaneously connected to the inlet of the fourteenth stop valve 18 and the inlet of the seventeenth stop valve 23; the outlets of the thirteenth stop valve 17 and the fourteenth stop valve 18 are jointly connected to the inlet of the nitrogen drying device 61.

[0093] The first hot end outlet 52 of the heat exchanger 57, the outlet of the thirty-fourth stop valve 64, the outlet of the first booster valve 67, and the outlet of the second booster valve 68 are jointly connected to the inlet of the first permeable membrane 65; the outlet of the first permeable membrane 65 is connected to the inlet of the thirty-fifth stop valve 66, and the outlet of the thirty-fifth stop valve 66 is connected to the inlet of the second permeable membrane 69; the outlet of the second permeable membrane 69 is connected to the inlet of the thirty-sixth stop valve 70, the outlet of the thirty-sixth stop valve 70 is connected to the inlet of the third permeable membrane 71, and the outlet of the third permeable membrane 71 is simultaneously connected to the inlet of the thirty-seventh stop valve 72 and the inlet of the thirty-eighth stop valve 73; the outlet of the thirty-seventh stop valve 72 is connected to the inlet of the first impurity adsorption tower 74, and the outlet of the first impurity adsorption tower 74 is connected to the inlet of the thirty-ninth stop valve 76; the outlet of the thirty-eighth stop valve 73 is connected to the inlet of the second impurity adsorption tower 75, and the outlet of the second impurity adsorption tower 75 is connected to the inlet of the fortieth stop valve 77; the outlets of the thirty-ninth stop valve 76 and the fortieth stop valve 77 are jointly connected to the neon-helium refining system.

[0094] The exhaust outlet of the second permeable membrane 69 is connected to the inlet of the first booster valve 67, and the exhaust outlet of the third permeable membrane 71 is connected to the inlet of the second booster valve 68.

[0095] The oxygen inlet pipeline is connected to the oxygen inlet 44 of the heat exchanger 57 through the second shut-off valve 2. The oxygen outlet 55 of the heat exchanger 57 is connected to the inlet of the first booster 58. The outlet of the first booster 58 is connected to the inlet of the hydrocarbon removal device 60. The outlet of the hydrocarbon removal device 60 is connected to the hot-end inlet of the heat balancer 13. The hot-end outlet of the heat balancer 13 is connected to the second hot-end inlet 49 of the heat exchanger 57; the second hot-end outlet 50 of the heat exchanger 57 is simultaneously connected to the inlet of the fifteenth shut-off valve 19 and the inlet of the sixteenth shut-off valve 20; the outlet of the seventeenth shut-off valve 23 and the outlet of the eighteenth shut-off valve 24 are jointly connected to the inlet of the nineteenth shut-off valve 25. The outlet of the nineteenth shut-off valve 25 is connected to the inlet of the nitride removal device 26; the outlet of the nitride removal device 26 is connected to the inlet of the twentieth shut-off valve 27. The outlet of the twentieth shut-off valve 27 is connected to the third hot-end inlet 48 of the heat exchanger 57. The third hot-end outlet 51 of the heat exchanger 57 is simultaneously connected to the inlet of the twenty-first shut-off valve 28 and the inlet of the twenty-second shut-off valve 29.

[0096] The outlet of the twenty-first shut-off valve 28 is connected to the inlet of the first purification tower 31, and the inlet of the twenty-second shut-off valve 29 is connected to the inlet of the second purification tower 30; the outlet of the second purification tower 30 is simultaneously connected to the inlet of the twenty-third shut-off valve 32 and the inlet of the twenty-fifth shut-off valve 34; the outlet of the first purification tower 31 is simultaneously connected to the inlet of the twenty-fourth shut-off valve 33 and the inlet of the twenty-sixth shut-off valve 35; the outlet of the twenty-third shut-off valve 32 and the outlet of the twenty-fourth shut-off valve 33 are jointly connected to the high-purity oxygen system; the outlet of the twenty-fifth shut-off valve 34 and the outlet of the twenty-sixth shut-off valve 35 are jointly connected to the suction port of the vacuum pump 36, and the exhaust port of the vacuum pump 36 is safely emptied.

[0097] In the device of the present invention, the ice dryer provides cold source supplement for the system, where A-1 and A-2 represent refrigerants; the refrigerant outlet of the ice dryer is simultaneously connected to the inlet of the thirtieth shut-off valve 40, the inlet of the thirty-first shut-off valve 41, and the cold quantity supply chambers of the first purification tower 31 and the second purification tower 30; the outlet of the thirtieth shut-off valve 40 is connected to the cold-end inlet 45 of the heat exchanger 57, and the outlet of the thirty-first shut-off valve 41 is simultaneously connected to the cold quantity supply chamber of the second impurity adsorption tower 75 and the cold quantity supply chamber of the first impurity adsorption tower 74.

[0098] The outlet of the cold quantity supply chamber of the first impurity adsorption tower 74 is connected to the inlet of the twenty-seventh shut-off valve 37, and the outlet of the cold quantity supply chamber of the second impurity adsorption tower 75 is connected to the inlet of the twenty-eighth shut-off valve 38; the outlets of the cold quantity supply chambers of the first purification tower 31 and the second purification tower 30, the outlet of the twenty-seventh shut-off valve 37, the outlet of the twenty-eighth shut-off valve 38, and the outlet of the twenty-ninth shut-off valve 39 are jointly connected to the refrigerant inlet of the ice dryer; the inlet of the twenty-ninth shut-off valve 39 is connected to the cold-end outlet 54 of the heat exchanger 57; a first pressure sensor 42-1 and a first pressure sensor 42-2 are provided at the refrigerant inlet of the ice dryer.

[0099] The method for purifying oxygen, nitrogen, and crude neon-helium gas using the purification device system specifically includes the following steps:

[0100] Before the start of the purification device system, the pipelines in the purification device system need to be purged and replaced. The conditions are as follows: purge with nitrogen at 4 atm for 5.5 h, and then evacuate to vacuum 3 times until the oxygen content at the outlet of the pipelines in the purification device system drops below 0.1 ppm. After the replacement of the pipelines in the purification device system is completed, first perform pipeline pressure holding, and the nitrogen in the pipelines is not emptied temporarily. Check whether the instrument and electric control of the system display normally. After the inspection of the instrument and electric control components is completed, vent the nitrogen in the pipelines and evacuate to vacuum below 10 Pa.

[0101] Open the first stop valve 1. Nitrogen flows through the nitrogen outlet 56 of the heat exchanger 57 through the nitrogen inlet 43 and enters the second deoxidation tower 6 or the first deoxidation tower 7. The second deoxidation tower 6 and the first deoxidation tower 7 are used alternately, that is, when the second deoxidation tower 6 is working, the first deoxidation tower 7 is regenerated, and vice versa. The following takes the first deoxidation tower 7 working and the second deoxidation tower 6 regenerating as an example:

[0102] Open the fourth stop valve 4 and the thirty-third stop valve 63 successively. After nitrogen removes trace oxygen through the first deoxidation tower 7, the volume purity of nitrogen reaches 7N and is used in high-purity nitrogen applications. After the first deoxidation tower 7 works for 0.9 T, open the third stop valve 3. The crude neon-helium gas flows through the heat exchanger 57 through the crude neon-helium gas inlet 46 and enters the electric heater 59 through the crude neon-helium gas outlet 53. The crude neon-helium gas is heated to 190 °C by the electric heater 59. After the working time of the first deoxidation tower 7 ends, open the eighth stop valve 10. The heated crude neon-helium gas is introduced into the first deoxidation tower 7 to remove the impurity hydrogen in the crude neon-helium gas while consuming the oxygen adsorbed by the deoxidizer. At this time, the volume concentration of hydrogen in the hydrogen-removed crude neon-helium gas ≤ 0.9 ppm.

[0103] The hydrogen-removed crude neon-helium gas flows through the first hot end inlet 47 of the heat exchanger 57 and enters the first permeable membrane 65 through the first hot end outlet 52 to preliminarily remove nitrogen with a volume concentration ≥ 72% in the crude neon-helium gas. It should be noted here that 95% of He and 73% of Ne in the crude neon-helium gas enter the permeate side of the first permeable membrane 65 through the dissolution and diffusion of the membrane, and the volume concentration of nitrogen on the permeate side drops to ≤ 33%. The waste gas on the non-permeate side of the first permeable membrane 65 can be directly discharged to the atmosphere, and the volume concentration of nitrogen in the waste gas is 82%. In addition, open the thirty-fourth stop valve 64, and a part of the high-purity nitrogen after nitrogen purification converges with the hydrogen-removed crude neon-helium gas.

[0104] Open the thirty-fifth stop valve 66. The gas at the outlet of the permeate side of the first permeable membrane 65 enters the second permeable membrane 69. 83% of He and 48% of Ne in the gas at the outlet of the permeate side of the first permeable membrane 65 enter the permeate side of the second permeable membrane 69 through the dissolution and diffusion of the membrane; the waste gas on the non-permeate side of the second permeable membrane 69 is pressurized by the first booster valve 67 and returns to the gas inlet of the first permeable membrane 65.

[0105] Further, open the thirty-sixth shut-off valve 70. The gas at the permeate side outlet of the second permeation membrane 69 enters the third permeation membrane 71. 71% of He and 32% of Ne in the gas at the low-pressure side outlet of the second permeation membrane 69 enter the permeate side of the third permeation membrane 71 through dissolution and diffusion through the membrane. The waste gas on the non-permeate side of the third permeation membrane 71 is pressurized by the second booster valve 68 and then returned to the gas inlet of the first permeation membrane 65. It should be noted here that the pressure gas source AM-1 of the first booster valve 67 comes from the first hot-end inlet 47 of the heat exchanger 57, and the pressure gas source AM-2 of the second booster valve 68 comes from the waste gas on the non-permeate side of the second permeation membrane 69.

[0106] The volume concentration of impurity nitrogen gas in the gas at the permeate side outlet of the third permeation membrane 71 is 0.3%, and it enters the first impurity adsorption tower 74 or the second impurity adsorption tower 75. It should be noted here that the first impurity adsorption tower 74 and the second impurity adsorption tower 75 are used alternately. When the first impurity adsorption tower 74 is working, the second impurity adsorption tower 75 is regenerated. Conversely, the second impurity adsorption tower 75 is working and the first impurity adsorption tower 74 is regenerated. The first impurity adsorption tower 74 and the second impurity adsorption tower 75 are set to work at -90 °C and regenerate at 0 °C.

[0107] Further, before the first impurity adsorption tower 74 and the second impurity adsorption tower 75 are put into use, they are cooled first. Open the twenty-seventh shut-off valve 37, the twenty-eighth shut-off valve 38, the twenty-ninth shut-off valve 39, the thirtieth shut-off valve 40, and the thirty-first shut-off valve 41, and start the ice dryer to cool the first impurity adsorption tower 74 and the second impurity adsorption tower 75 to -90 °C. At the same time, the second purification tower 30 and the first purification tower 31 are also cooled and used to adsorb trace impurity gases in the oxygen separated by air. It should be pointed out here that it takes 45 minutes for the first impurity adsorption tower 74, the second impurity adsorption tower 75, the second purification tower 30, and the first purification tower 31 to be cooled below -90 °C. Therefore, according to the actual situation of on-site commissioning, the ice dryer is preferably started first. In this embodiment, taking the first impurity adsorption tower 74 working and the second impurity adsorption tower 75 regenerating as an example:

[0108] After the first impurity adsorption tower 74 and the second impurity adsorption tower 75 are cooled to -90 °C, open the thirty-seventh shut-off valve 72 and the thirty-ninth shut-off valve 76. The gas at the permeate side outlet of the third permeation membrane 71 enters the first impurity adsorption tower 74 to adsorb and remove trace N2 and other impurity gases in the hydrogen, neon, and helium gases. The neon-helium mixed gas at the outlet of the first impurity adsorption tower 74 goes to the neon-helium refining system. It should be noted here that when the first impurity adsorption tower 74 is working, the second impurity adsorption tower 75 is reheated by its own electric tracing band, and the waste gas desorbed and analyzed during reheating is safely discharged through the adsorption tower evacuation pipeline.

[0109] Further, after the working conditions of the nitrogen purification and the processes of removing hydrogen and nitrogen from the crude neon-helium gas in the present invention become stable, open the second stop valve 2. Oxygen passes through the oxygen inlet 44 of the heat exchanger 57 and flows out through the oxygen outlet 55 into the first booster 58. After the oxygen is boosted to 7 ata(A), it enters the hydrocarbon removal device 60, where trace hydrocarbons in the oxygen are catalytically removed at 300°C. It should be noted here that trace hydrocarbons are decomposed into CO2, H2O, and NO in the hydrocarbon removal device 60. x , and CO2 and H2O are adsorbed and removed through the subsequent second adsorption tower 21 or the first adsorption tower 22, and N2 and Ar are adsorbed and removed through the second purification tower 30 or the first purification tower 31.

[0110] Further, the oxygen at the outlet of the hydrocarbon removal device 60 exchanges heat with a part of the high-purity nitrogen through the hot-end flow path of the heat balancer 13, and the heat of the oxygen at the outlet of the hydrocarbon removal device 60 is recovered for the first time; the oxygen at the hot end of the heat balancer 13 passes through the second hot-end inlet 49 of the heat exchanger 57 and flows out through the second hot-end outlet 50, and the heat of the oxygen at the outlet of the hydrocarbon removal device 60 is recovered for the second time.

[0111] The second adsorption tower 21 and the first adsorption tower 22 are used alternately. That is, when the second adsorption tower 21 is working, the first adsorption tower 22 is regenerated; conversely, when the first adsorption tower 22 is working, the second adsorption tower 21 is regenerated, and the regeneration gas source is high-purity nitrogen. In this embodiment, taking the first adsorption tower 22 working and the second adsorption tower 21 being regenerated as an example:

[0112] Open the fifteenth stop valve 19 and the eighteenth stop valve 24. The oxygen at the second hot-end outlet 50 of the heat exchanger 57 enters the first adsorption tower 22 to adsorb and remove the decomposition products CO2 and H2O of trace hydrocarbons. At the same time, open the tenth stop valve 12, start the second booster 14, open the twelfth stop valve 16 and the fourteenth stop valve 18, and the high-purity nitrogen at 170°C after heating is used to purge the adsorbent in the second adsorption tower 21, and the CO2 and H2O adsorbed by the adsorbent are desorbed and carried away. The purging nitrogen at the outlet of the second adsorption tower 21 is purified by the nitrogen drying device 61 and then returns to the inlet of the second deoxidation tower 6 or the first deoxidation tower 7.

[0113] Further, open the nineteenth stop valve 25. After removing CO2 and H2O, the oxygen decomposes NO at 320°C through the nitride removal device 26 x into N2 and O2. Open the twentieth stop valve 27. The high-temperature gas at the outlet of the nitride removal device 26 passes through the third hot-end inlet 48 of the heat exchanger 57 and flows out through the third hot-end outlet 51 to exchange heat with other process streams, and after cooling, it enters the second purification tower 30 or the first purification tower 31. It should be noted here that the second purification tower 30 and the first purification tower 31 are used alternately. That is, when the second purification tower 30 is working, the first purification tower 31 is regenerated; conversely, when the first purification tower 31 is working, the second purification tower 30 is regenerated. In this embodiment, taking the second purification tower 30 working and the first purification tower 31 being regenerated as an example:

[0114] Open the twenty-second stop valve 29 and the twenty-third stop valve 32, and the oxygen at the third hot end outlet 51 of the heat exchanger 57 enters the second purification tower 30 to remove N2 and Ar, and then goes to the high-purity oxygen use occasion.

[0115] In this embodiment, the purification device system is used to purify oxygen, nitrogen and crude neon and helium in a linked manner, and the nitrogen is purified to a volume concentration of impurity oxygen below 0.1ppm; the oxygen is purified to a total volume concentration of impurity nitrogen and argon below 0.3ppm; the crude neon and helium are purified to a volume concentration of impurity hydrogen below 0.2ppm, and a volume concentration of nitrogen below 0.1ppm, thereby achieving efficient purification of air-separated oxygen, air-separated nitrogen and air-separated crude neon and helium.

[0116] Example 2

[0117] This embodiment provides a purification device system for oxygen, nitrogen and crude neon and helium. The difference from Embodiment 1 is that the second permeable membrane 69 and the third permeable membrane 71 are not provided, and the outlet gas on the permeation side of the first permeable membrane 65 directly enters the first impurity adsorption tower 74 or the second impurity adsorption tower 75, and the rest is the same as Embodiment 1.

[0118] In this embodiment, since the permeable membrane assembly is only provided with the first permeable membrane 65, the nitrogen in the dehydrogenated neon-helium gas cannot be effectively separated and removed, and thus the volume concentration of the impurity nitrogen in the obtained neon-helium mixed gas is too high.

[0119] Example 3

[0120] This embodiment provides a purification device system for oxygen, nitrogen and crude neon and helium. The difference from Embodiment 1 is that the thirty-fourth stop valve 64 and the pipeline where it is located are not provided, and the rest are the same as Embodiment 1.

[0121] In this embodiment, the thirty-fourth stop valve and the pipeline where it is located are not provided, so that the high-purity nitrogen gas and the crude neon and helium gas after hydrogen removal cannot be merged, thereby reducing the recovery rate of Ne+He of the first permeable membrane.

[0122] Comparative Example 1

[0123] This comparative example provides a purification device for oxygen, nitrogen and crude neon and helium. The purification of the oxygen and nitrogen is carried out by using the device disclosed in CN112229143A for producing oxygen and nitrogen by separating air through cryogenic distillation. The purification of the crude neon and helium is carried out by using the device disclosed in CN117566701A for purifying crude neon and helium by non-cryogenic method. The two devices are operated separately.

[0124] The purification device for oxygen, nitrogen, and crude neon-helium gas provided in this comparative example cannot achieve linked purification and impurity removal. Separately purifying oxygen, nitrogen, and crude neon-helium gas through different devices will increase production costs and is limited in industrial production applications.

[0125] In summary, the purification device system for oxygen, nitrogen, and crude neon-helium gas provided by the present invention can perform linked purification and impurity removal on the nitrogen, oxygen, and crude neon-helium gas produced by the air separation device. Specifically, the air separation nitrogen is reheated through a heat exchanger and then deoxygenated in a deoxygenation tower to obtain high-purity nitrogen; the air separation oxygen is reheated and pressurized by using a heat exchanger and a first booster, then the hydrocarbons are removed by a hydrocarbon removal device, and then CO2 and H2O are adsorbed by a carbon dioxide and water adsorption tower, and then NO x is reduced to N2 and O2 in a nitride removal device, and finally high-purity oxygen is obtained through an oxygen purification tower; the hydrogen removal of the air separation crude neon-helium gas is linked with the purification process of the air separation nitrogen. When the deoxygenation tower is saturated with oxygen absorption, heated crude neon-helium gas is introduced to realize the regeneration of nitrogen purification while removing hydrogen in the crude neon-helium gas; after hydrogen removal, the crude neon-helium gas is introduced into a permeable membrane module and an impurity adsorption tower to obtain a neon-helium mixed gas; there is a linkage between the purification of the air separation nitrogen and the purification of the air separation oxygen, that is, part of the purified nitrogen is used as the regeneration gas source for oxygen purification, and the discharged nitrogen converges with the air separation nitrogen; by using the purification device system to perform linked purification on oxygen, nitrogen, and crude neon-helium gas, the nitrogen can be purified to an impurity oxygen volume concentration of less than 0.1 ppm; the oxygen can be purified to an overall volume concentration of impurities nitrogen and argon of less than 0.3 ppm; the crude neon-helium gas can be purified to an impurity hydrogen volume concentration of less than 0.2 ppm and a nitrogen volume concentration of less than 0.1 ppm.

[0126] The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention fall within the protection scope and the disclosure scope of the present invention.

Claims

1. A purification device system for oxygen, nitrogen and crude neon-helium gas, characterized in that, The purification device system includes a heat exchanger, which is provided with a nitrogen inlet, a nitrogen outlet, an oxygen inlet, an oxygen outlet, a crude neon-helium inlet, a crude neon-helium outlet, a hydrogen-removed neon-helium inlet, and a hydrogen-removed neon-helium outlet; the nitrogen outlet and the crude neon-helium outlet are both connected to a deoxidation tower, the deoxidation tower discharges high-purity nitrogen and hydrogen-removed neon-helium, and the hydrogen-removed neon-helium enters the heat exchanger from the hydrogen-removed neon-helium inlet and is discharged from the hydrogen-removed neon-helium outlet, and then sequentially enters a permeable membrane module and an impurity adsorption tower; the permeable membrane module includes a first permeable membrane, a second permeable membrane, and a third permeable membrane connected in sequence along the flow direction of the hydrogen-removed neon-helium, and the first permeable membrane, the second permeable membrane, and the third permeable membrane are respectively independently provided with a permeate side and a non-permeate side; The oxygen outlet is sequentially connected with a first booster, a hydrocarbon removal device, and a heat balancer, the oxygen discharged from the heat balancer flows through the heat exchanger and then sequentially enters a carbon dioxide and water adsorption tower and a nitride removal device, and the discharged oxygen flows through the heat exchanger again and enters an oxygen purification tower; a part of the high-purity nitrogen discharged from the deoxidation tower enters the high-purity nitrogen system, a part enters the first permeable membrane, a part flows through the heat balancer and a second booster, enters the carbon dioxide and water adsorption tower for purging to carry out carbon dioxide and water, and returns to the pipeline where the nitrogen outlet is located after removing carbon dioxide and water through a nitrogen drying device; The purification device system further includes an ice dryer, which is used to provide a cold source for the impurity adsorption tower and the oxygen purification tower.

2. The purification device system according to claim 1, wherein, The crude neon-helium outlet is connected to the deoxidation tower through an electric heater; The deoxidation tower includes a first deoxidation tower and a second deoxidation tower that operate and regenerate alternately.

3. The purification device system according to claim 1, wherein, The non-permeate side of the first permeable membrane is provided with an exhaust gas outlet; The exhaust gas discharged from the non-permeate side of the second permeable membrane flows through a first booster valve and returns to the first permeable membrane, and the pressure air source of the first booster valve comes from the hydrogen-removed neon-helium inlet; The exhaust gas discharged from the non-permeate side of the third permeable membrane flows through a second booster valve and returns to the first permeable membrane, and the pressure air source of the second booster valve comes from the exhaust gas discharged from the non-permeate side of the second permeable membrane.

4. The purification device system according to claim 1, wherein The outlet of the impurity adsorption tower is connected to a neon-helium refining system; The impurity adsorption tower includes a first impurity adsorption tower and a second impurity adsorption tower that operate and regenerate alternately.

5. The purification device system according to claim 1, characterized in that, The carbon dioxide and water adsorption tower includes a first adsorption tower and a second adsorption tower that operate and regenerate alternately.

6. The purification device system according to claim 1, characterized in that, The oxygen purification tower includes a first purification tower and a second purification tower that operate and regenerate alternately; The outlet of the oxygen purification tower is independently connected to a high-purity oxygen system and a vacuum pump respectively.

7. The purification device system according to claim 1, characterized in that, The ice dryer is provided with a refrigerant outlet and a refrigerant inlet, the refrigerant outlet is independently connected to the cold quantity supply chamber inlet of the impurity adsorption tower, the cold quantity supply chamber inlet of the oxygen purification tower, and the refrigerant heat exchange pipeline inlet respectively, the refrigerant inlet is independently connected to the cold quantity supply chamber outlet of the impurity adsorption tower, the cold quantity supply chamber outlet of the oxygen purification tower, and the refrigerant heat exchange pipeline outlet respectively, and the refrigerant heat exchange pipeline inlet is communicated with the refrigerant heat exchange pipeline outlet through the heat exchanger.

8. A purification method for oxygen, nitrogen and crude neon-helium gas, characterized in that, The purification method is carried out by the purification device system of oxygen, nitrogen and crude neon and helium according to any one of claims 1 to 7, and the purification method comprises the following steps: (1) After the first heat exchange and reheating, the air separation nitrogen is physically deoxygenated to obtain high-purity nitrogen; (2) the crude neon-helium gas from air separation enters the oxygen-saturated environment formed after the physical deoxygenation in step (1) to be dehydrogenated, and the dehydrogenated neon-helium gas is subjected to the second heat exchange and rewarming, and then sequentially subjected to the first membrane separation, the second membrane separation, the third membrane separation, and impurity adsorption to obtain a neon-helium mixed gas; (3) The air-separated oxygen undergoes the third heat exchange and reheating, pressurization, catalytic hydrocarbon removal, the first heat recovery and the second heat recovery, carbon dioxide and water adsorption treatment, and nitride removal treatment in sequence. The obtained oxygen undergoes the fourth heat exchange and reheating and is then purified to obtain high-purity oxygen. Part of the high-purity nitrogen in step (1) enters the first membrane separation and merges with the dehydrogenation neon and helium, and part of it enters the water vapor environment formed after the carbon dioxide and water adsorption treatment in step (3) for purging, and then takes out carbon dioxide and water, and returns to the physical deoxygenation in step (1) after water vapor removal treatment; During the impurity adsorption in step (2) and the purification treatment in step (3), cold energy is circulated and supplied.

9. The purification method according to claim 8, wherein The physical deoxygenation in step (1) includes deoxygenation and regeneration performed simultaneously, wherein oxygen desorption and dehydrogenation of crude neon and helium gas from air separation are performed during the regeneration process; In step (2), the crude neon-helium gas from the air separation is heated to 180-205° C. before the dehydrogenation; Step (2) the waste gas discharged after the first membrane separation is discharged into the atmosphere or recovered for treatment, the waste gas discharged after the second membrane separation is pressurized and returned to the first membrane separation, and the waste gas discharged after the third membrane separation is pressurized and returned to the first membrane separation; The impurity adsorption in step (2) includes adsorption and regeneration performed simultaneously. During the adsorption process, the temperature is controlled at -100 to -84°C, and during the regeneration process, the temperature is controlled at -10 to 0°C, so as to achieve the decomposition of the adsorbed impurity gas.

10. The purification method according to claim 8, wherein, The temperature of the catalytic hydrocarbon removal in step (3) is 270-320°C; The carbon dioxide and water adsorption treatment in step (3) includes adsorption and regeneration performed simultaneously. During the regeneration process, the high-purity nitrogen gas in step (1) is heated at 170-200° C. and then enters the water vapor environment formed after the carbon dioxide and water adsorption treatment for purging. The temperature of the nitride removal treatment in step (3) is 320-350°C; The purification treatment in step (3) includes nitrogen and argon adsorption treatment and regeneration analysis performed simultaneously.

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