A siphon refrigeration krypton-xenon refining device

Abstract

The present invention provides a siphon-type refrigeration krypton-xenon refining device, comprising a main heat exchanger, a deoxidation tower, a refined krypton tower, a refined xenon tower, a refined krypton condenser, and a multi-effect condenser. The feed gas accumulates cold energy in the main heat exchanger. A reboiler is provided in the deoxidation tower, through which the feed gas transfers heat with the medium in the deoxidation tower. The refined krypton tower receives and rectifies the bottom still liquid of the deoxidation tower. The refined krypton tower receives and rectifies the bottom still liquid of the refined krypton tower. The refined xenon tower receives and rectifies the gas condensate at the top of the deoxidation tower. The refined krypton condenser receives the feed gas flowing through the reboiler and the gas at the top of the refined krypton tower, and performs heat exchange. The multi-effect condenser receives and performs heat exchange with the gas at the top of the deoxidation tower and the refined xenon tower. The cold source gas flows through the refined krypton condenser via a compressor, is then injected into the multi-effect condenser, and returns to the refined krypton condenser to form a closed-loop circulation. The krypton-xenon refining device of the present invention reduces production costs and increases the speed of collecting or releasing cold energy.

Description

Technical Field

[0001] The present invention relates to the technical field of gas separation, and in particular to a krypton-xenon refining device with siphon refrigeration. Background Art

[0002] The content of krypton and xenon gases in the atmosphere is about 1.138x10 -6 , 0.0857x10 -6 After trace amounts of krypton and xenon gases enter an air separation unit, such as a cryogenic distillation tower, along with air, the high-boiling-point components—krypton, xenon, hydrocarbons (primarily methane), and fluorides—mostly accumulate in the liquid oxygen in the low-pressure tower. By transferring the liquid oxygen from the low-pressure tower to a krypton-added distillation tower (commonly known as a lean krypton tower), a lean krypton-xenon concentrate with a krypton-xenon content of 0.2-0.3% Kr+Xe is produced. The methane content in this lean krypton-xenon concentrate is approximately 0.3-0.4%. Excessive methane content in oxygen (generally no more than 0.5%) is extremely dangerous. Therefore, pre-emptive removal of methane from the lean krypton-xenon concentrate not only improves equipment safety but also increases the krypton-xenon concentration in the lean krypton-xenon concentrate. In the known method, the krypton-depleted xenon concentrate is first pressurized to a critical pressure of 5.5 MPa and vaporized. The pressure is then reduced to 1.0 MPa before entering a methane purification unit. In the methane purification unit, oxygen and methane react chemically at a temperature of 480-500°C over a palladium catalyst, decomposing the methane into carbon dioxide and water. The residual methane content in the krypton-depleted xenon concentrate is less than 1x10 -6 , and then carbon dioxide and water are removed by molecular sieve adsorption; the raw gas after removing methane enters the first-level distillation tower to obtain a krypton-xenon mixture.

[0003] Conventional refining equipment uses a krypton-xenon mixture as the feed gas, and a mixture of nitrogen and liquid nitrogen as the cooling source. Krypton and xenon are separated and further purified through multi-stage distillation. This method is lengthy and consumes a large amount of liquid nitrogen as the cooling source, increasing production costs and reducing the efficiency of krypton and xenon purification.

[0004] In view of this, the present invention provides a krypton-xenon refining device with siphon refrigeration to solve the technical problems existing in the background technology. Summary of the Invention

[0005] In order to solve the above technical problems, the present invention provides a krypton-xenon refining device with siphon refrigeration, comprising:

[0006] a main heat exchanger, through which the raw gas passes and accumulates cold energy;

[0007] A deoxidation tower, wherein a reboiler is provided in the deoxidation tower, and the feed gas transfers heat with the medium in the deoxidation tower through the reboiler;

[0008] a refinement tower, which receives the bottom liquid from the deoxidation tower and performs rectification;

[0009] a desulfurization tower, which receives the bottom liquid from the clarifier tower and performs rectification;

[0010] a xenon refinement tower, which receives the condensed gas from the top of the de-kr tower and distills it to produce xenon liquid;

[0011] a refined krypton condenser, which receives the feed gas flowing through the reboiler and the top gas of the refined krypton tower and performs heat exchange;

[0012] A multi-effect condenser, which receives gas from the top of the krypton removal tower and the xenon refinement tower and performs heat exchange;

[0013] The cold source gas flows through the fine krypton condenser through the compressor to collect cold energy, and then is injected into the multi-effect condenser to release cold energy, and the cold source gas flowing through the multi-effect condenser returns to the fine krypton condenser to form a closed loop.

[0014] Furthermore, a deoxidation tower condenser is provided in conjunction with the deoxidation tower;

[0015] The gas at the top of the deoxidation tower flows through the deoxidation tower condenser to be liquefied to produce liquid oxygen product M3 or is transported to the deoxidation tower for heat and mass transfer.

[0016] Furthermore, the raw gas pipeline flowing through the reboiler is connected to the first gas-liquid separator;

[0017] The gas-liquid mixture separated by the first gas-liquid separator flows into the fine krypton condenser and then returns to the deoxidation tower.

[0018] Furthermore, the raw gas pipeline at the rear end of the refined krypton condenser is connected to the second gas-liquid separator;

[0019] The gas phase and liquid phase of the raw gas separated by the second gas-liquid separator are returned to different heights of the deoxidation tower through the transmission pipeline respectively.

[0020] Furthermore, the cold source flowing through the deoxidation tower condenser is liquid nitrogen, and the liquid nitrogen flows through the main heat exchanger through the conveying pipeline after passing through the deoxidation tower condenser for heat exchange.

[0021] Furthermore, the refined krypton product M5 is produced by flowing through the refined krypton condenser or returned to the refined krypton tower.

[0022] Furthermore, the krypton-xenon refining device further includes a recovery tower;

[0023] The gas at the top of the recovery tower flows through the multiple-effect condenser and enters the fourth gas-liquid separator for gas-liquid separation.

[0024] Furthermore, the gas pipeline at the top of the refined xenon tower flowing through the multi-effect condenser is connected to the third gas-liquid separator for gas-liquid separation;

[0025] The liquid phase separated by the third gas-liquid separator is returned to the xenon refinement tower or transported to the recovery tower.

[0026] Furthermore, the bottom liquid of the deoxidation tower is returned to the recovery tower.

[0027] The above technical solutions of the present invention have at least the following technical effects:

[0028] 1. In the krypton-xenon refining device of the present invention, the cold source gas forms a siphon effect during the flow between the refined krypton condenser and the multi-effect condenser, achieving self-circulation of the refrigerant and increasing the collection or release rate of cold energy. This cold energy circulation system not only reduces the consumption of liquid nitrogen and production costs, but also realizes efficient utilization of the cold energy in the krypton-xenon refining device.

[0029] 2. In the embodiment of the present application, the raw gas undergoes primary heat exchange in the main heat exchanger and then undergoes secondary heat exchange in the reboiler to accumulate cold energy. The raw liquid with accumulated cold energy enters the refined krypton condenser to provide cold energy for the cold source gas and realize cold energy recovery. The raw gas then passes through the second gas-liquid separator to achieve gas-liquid separation and then enters the deoxidation tower for gas-liquid mass transfer and heat exchange to improve the deoxidation efficiency of the raw gas-liquid mixture. The krypton-xenon enriched liquid is produced to provide raw materials for the refined krypton tower and the refined xenon tower.

[0030] 3. The krypton-xenon refining device of the embodiment of the present application has a short process flow and can efficiently realize the preparation of krypton and xenon gases;

[0031] The embodiments of the present invention also include other advantages, which are detailed in the specific embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 This is a schematic diagram of the process system structure of the krypton-xenon refining device in the embodiment of this application;

[0033] Figure 2 for Figure 1 Schematic diagram of the raw material gas condensation cycle process structure;

[0034] Figure 3 for Figure 1 Schematic diagram of the preparation process of refined krypton;

[0035] Figure 4 for Figure 1 Schematic diagram of the liquid nitrogen cooling energy cycle process structure;

[0036] Figure 5 for Figure 1 Schematic diagram of the liquid oxygen preparation process structure in the middle deoxidation tower;

[0037] Figure 6 for Figure 1 Schematic diagram of the process structure for removing krypton from medium-enriched xenon liquid;

[0038] Figure 7 for Figure 1 Schematic diagram of the process structure of medium-precision xenon preparation;

[0039] Figure 8 for Figure 1 Schematic diagram of the process structure for recovering residual krypton or residual xenon;

[0040] Figure 9 for Figure 1 Schematic diagram of the siphon cooling energy cycle process structure.

[0041] Reference numerals:

[0042] 100. Krypton-xenon refining unit; 1. Main heat exchanger; 2. Deoxidation tower; 3. Reboiler; 4. Deoxidation tower condenser; 5. First gas-liquid separator; 6. First regulating valve; 7. Refining krypton tower; 8. Refining krypton condenser; 9. Second gas-liquid separator; 10. Second regulating valve; 11. Third regulating valve; 12. Compressor; 13. Deoxidation tower; 14. Refining xenon tower; 15. Recovery tower; 16. Multi-effect condenser; 17. Third gas-liquid separator; 18. Fourth gas-liquid separator. DETAILED DESCRIPTION

[0043] To make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the following will be combined with the appended drawings of the embodiments of the present invention. Figure 1-9 The technical solutions of the embodiments of the present invention are clearly and completely described as shown. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the described embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field fall within the scope of protection of the present invention.

[0044] A siphon refrigeration krypton-xenon refining device 100 includes a main heat exchanger 1, a deoxidation tower 2, a refining krypton tower 7, a deoxidation tower 13, a refining xenon tower 14, a refining krypton condenser 8, and a multi-effect condenser 16. The raw gas passes through the main heat exchanger 1 and accumulates cold energy. The deoxidation tower 2 is provided with a reboiler 3, and the raw gas transfers heat with the medium in the deoxidation tower 2 through the reboiler 3. The refining krypton tower 7 receives the bottom kettle liquid of the deoxidation tower 2 and distills it. The deoxidation tower 13 receives the bottom kettle liquid of the refining krypton tower 7 and distills it. The refining xenon tower 1 4 receives the condensate from the top of the xenon removal tower 13 and distills it to produce xenon liquid; the fine xenon condenser 8 receives the feed gas flowing through the reboiler 3 and the gas from the top of the fine xenon tower 7 and performs heat exchange; the multi-effect condenser 16 receives the gas from the top of the xenon removal tower 13 and the fine xenon tower 14 and performs heat exchange; wherein, the cold source gas flows through the fine xenon condenser 8 through the compressor 12 to collect cold energy, and is then injected into the multi-effect condenser 16 to release cold energy, and the cold source gas flowing through the multi-effect condenser 16 returns to the fine xenon condenser 8 to form a closed loop circulation.

[0045] As shown in Figures 1-9, the present invention provides a krypton-xenon refining device with siphon refrigeration, wherein the krypton-xenon refining device 100 includes a main heat exchanger 1, a deoxidation tower 2, a refined krypton tower 7, a deoxygenation tower 13, a refined xenon tower 14, a refined krypton condenser 8, and a multi-effect condenser 16. The raw gas rich in krypton and xenon from the purification process has an initial temperature of 15-25°C and a pressure of 18-20 bar. The main components of the raw gas are: oxygen ≥ 99.5%, methane ≤ 10 ppb, krypton ≥ 1500 ppm, xenon ≥ 300 ppm, and other components are trace amounts of carbon dioxide, nitrous oxide, carbon tetrafluoride, etc. The raw gas is introduced into the first inlet 18 of the main heat exchanger 1. 1Enters and is discharged from its corresponding outlet 19, in this process, it exchanges heat with the cold source and accumulates cold energy. After passing through the main heat exchanger, the temperature of the raw gas is reduced to -120~-126℃; a reboiler 3 is provided in the deoxidation tower 2, and the reboiler is preferably located at the bottom of the deoxidation tower. The raw gas enriched with cold energy enters from the inlet end of the reboiler 3 and is discharged from the outlet end of the reboiler. In the process of flowing through the reboiler, it transfers heat with the liquid medium rich in krypton and xenon in the deoxidation tower 2. The raw gas condenses in the reboiler and further releases heat to liquefy. The liquid absorbs heat and boils and evaporates, causing light components such as oxygen to evaporate and overflow from the top of the deoxidation tower, and the heavy component kettle liquid accumulates at the bottom of the deoxidation tower. The heavy component kettle liquid is the krypton-xenon-rich raw material liquid; the krypton tower 7 receives the bottom kettle liquid of the deoxidation tower 2 and distills it. During the distillation process in the krypton tower, the bottom kettle liquid of the krypton tower accumulates and is then transported to the deoxidation tower for krypton removal treatment. The gas at the top of the krypton tower enters the krypton condenser for heat transfer and liquefaction to prepare the krypton product M5; the deoxidation tower 13 receives the bottom kettle liquid of the krypton tower 7 and distills it. The bottom kettle liquid is xenon-rich liquid, which enters the lower part of the deoxygenation tower and exchanges heat with the steam in the deoxygenation tower through mass transfer. The high-boiling-point components are continuously accumulated at the bottom of the tower, and the low-boiling-point components are discharged from the top of the deoxygenation tower and are subsequently collected for xenon. The bottom kettle liquid of the deoxygenation tower is then subjected to subsequent rectification and purification. The refined xenon tower 14 receives the condensate from the top of the deoxygenation tower 13, and the xenon-rich liquid is rectified in the refined xenon tower. The gas from the top of the refined xenon tower enters the multi-effect condenser for liquefaction treatment and is returned to the refined xenon tower for circulation and enrichment. The xenon concentration of the kettle liquid enriched at the bottom of the refined xenon tower gradually increases. Improve and produce electronic grade xenon product M6, wherein the purity of xenon product M6 is ≥99.9999995%; the refined krypton condenser 8 receives the raw gas flowing through the reboiler 3 and the top gas of the refined krypton tower 7 and performs heat exchange, and the raw gas flowing through the reboiler is transferred to the cold source gas in the refined krypton condenser as a cold source, thereby realizing the cold energy recovery and utilization of the cold source gas; the multi-effect condenser 16 receives the top gas of the dexenon tower 13 and the refined xenon tower 14 and performs heat exchange; the top gas of the dexenon tower is discharged from the first inlet end 34 of the multi-effect condenser 16 1 Enter and be discharged from the corresponding outlet end, the gas at the top of the deoxygenation tower is liquefied in the multi-effect condenser and then returned to the reflux port of the deoxygenation tower or transported to the refined xenon tower; wherein, the cold source gas is carbon tetrafluoride, the initial pressure of carbon tetrafluoride is 24~26bar, the temperature is 35~38℃, and the carbon tetrafluoride gas is compressed from the first inlet end 28 of the refined xenon condenser 8 by the compressor 12 1 The cold energy of the raw gas flowing through the reboiler in the refined krypton condenser is transferred to the cold source gas, which absorbs the cold energy and stores it, and then flows out from the fourth inlet port 40 of the multi-effect condenser 16. 4The cold source gas enters and is discharged from the corresponding outlet port 41, releasing cold energy in the multi-effect condenser, and the cold source gas flowing through the multi-effect condenser 16 returns to the fine krypton condenser 8 to form a closed loop circulation; the cold source gas realizes cold source absorption in the fine krypton condenser and releases and transfers cold energy in the multi-effect condenser; the gas at the top of the dekrypton tower and the fine xenon tower passes through the multi-effect condenser for cold source absorption, so as to realize the liquefaction of the corresponding gas intermediates to meet the process requirements.

[0046] The krypton-xenon refining device of the present invention has a short process flow and can efficiently realize the preparation of krypton and xenon gases. The cold source gas forms a siphon effect during the process between the refined krypton condenser and the multi-effect condenser, realizing self-circulation of the refrigerant and increasing the collection or release rate of cold energy. The cold energy circulation system provided by this arrangement not only reduces the consumption of liquid nitrogen and production costs, but also realizes the efficient utilization of the cold energy in the krypton-xenon refining device.

[0047] In another embodiment of the present application, Figure 3 As shown:

[0048] A deoxidation tower condenser 4 is provided in conjunction with the deoxidation tower 2; the raw material liquid rich in krypton and xenon is heat-exchanged with the raw material gas flowing through the reboiler in the deoxidation tower, and the heat energy is transferred to the kettle liquid in the deoxidation tower, thereby achieving the boiling of light components such as oxygen and overflowing the top gas of the deoxidation tower 2 containing a high concentration of oxygen, which is discharged from the second inlet end 26 of the deoxidation tower condenser 4. 2 Enter and be discharged from the corresponding outlet port 27, in the deoxygenation condenser, the oxygen-rich gas is heat exchanged with liquid nitrogen and liquefied, and the liquefied oxygen-containing liquid can be used as the industrial oxygen product M3 output value liquid oxygen tank storage, or transported to the top of the deoxygenation tower 2 and the steam rising in the deoxygenation tower for further heat and mass transfer to achieve the increase of oxygen concentration; the gas from the top of the deoxygenation tower can also be connected to the exhaust pipeline and connected to the second inlet port 20 of the main heat exchanger. 2 , and discharged from the corresponding outlet port 21 of the main heat exchanger. Through the emptying line P1, the gas at the top of the deoxidation tower can be emptied and the cold energy can be recovered, thereby improving the cold energy collection of the raw gas in the main heat exchanger.

[0049] In another embodiment of the present application, Figure 3 As shown;

[0050] The raw gas pipeline flowing through the reboiler 3 is connected to the first gas-liquid separator 5, and the raw gas-liquid mixture is separated into gas and liquid in the first gas-liquid separator 5, and the gas phase is vented. The liquid phase of the raw gas is throttled to 15-19 bar after passing through the first regulating valve 6 on the raw gas pipeline, and is discharged from the third inlet end 32 of the refined krypton tower condenser. 3The raw material liquid enters and is discharged from the corresponding outlet port 33. In the refined krypton condenser 8, the raw material liquid serves as a cold source for the carbon tetrafluoride gas. When passing through the refined krypton condenser, the raw material liquid is vaporized in small amounts. At this time, the raw material gas-liquid mixture can be returned to the deoxidation tower for mass transfer and heat exchange to improve the deoxidation of the raw material liquid.

[0051] In another embodiment of the present application, Figure 2 As shown:

[0052] The raw gas pipeline at the rear end of the refined krypton condenser 8 is connected to the second gas-liquid separator 9; the raw gas-liquid mixture is discharged from the condenser at the top of the refined krypton tower and enters the second gas-liquid separator for gas-liquid separation. The separated liquid phase is throttled to 4~7bar through the third regulating valve 11, and enters the tower from the middle and upper part of the deoxidation tower 2 for mass exchange and heat exchange with the rising steam; the gas phase separated from the second gas-liquid separator 9 is throttled to 4~7bar through the second regulating valve 10, and enters the tower from the middle and upper part of the deoxidation tower for mass exchange and heat exchange with the top reflux liquid to achieve deoxygenation of the raw gas; it should be noted that the raw liquid gas phase and liquid phase separated by the second gas-liquid separator 9 are returned to different heights of the deoxidation tower 2 through the transmission pipeline respectively, so as to achieve countercurrent mass transfer and heat exchange for the best result. In this embodiment, the raw gas undergoes heat exchange in the main heat exchanger and then undergoes secondary heat exchange in the reboiler to accumulate cold energy. The raw liquid with accumulated cold energy then enters the refined krypton condenser to provide cold energy for the cold source gas and to recycle the condensed material. The raw gas then passes through the second gas-liquid separator to achieve gas-liquid separation and then enters the deoxidation tower for gas-liquid mass transfer and heat exchange to improve the deoxidation efficiency of the raw gas-liquid mixture. Krypton-xenon enriched liquid is then produced to provide feedstock for the refined krypton tower and refined xenon tower.

[0053] In another embodiment of the present application, Figure 4 As shown:

[0054] The cold source flowing through the deoxidation tower condenser 4 is liquid nitrogen, the initial pressure of the liquid nitrogen is 12~13 bar, and the temperature is about -186℃. The liquid nitrogen flows through the first inlet end 24 of the deoxidation tower condenser 4. 1 The nitrogen gas enters and is discharged from the corresponding outlet port 25, and can exchange heat with the gas from the top of the deoxidation tower in the deoxidation tower condenser 4, thereby providing cold energy for oxygen liquefaction, and the temperature rises to -160~-170℃; the nitrogen gas flowing through the deoxidation tower condenser is transported from the third inlet port 22 of the main heat exchanger 1 through the transmission pipeline. 3 After entering and exiting the corresponding outlet 23, the cold-energy-rich nitrogen undergoes heat exchange with the feed gas in the main heat exchanger, raising the nitrogen temperature to -50°C to -40°C. This allows for the recovery of nitrogen cold energy and accumulation of cold energy in the feed gas. In this embodiment, this cold energy utilization circuit P2 fully utilizes the cold energy of liquid nitrogen, improving its utilization rate. The nitrogen flowing through the main heat exchanger, carrying cold energy, continues to enter the feed liquid purification process for further cold energy recovery.

[0055] In another embodiment of the present application, Figure 5 As shown:

[0056] The bottom kettle liquid of the deoxidation tower enters the refinery tower 7 for distillation separation, and the gas at the top of the refinery tower is distilled from the second inlet end 30 of the refinery condenser 8. 2 It enters and is discharged from the corresponding outlet port 31, undergoes heat exchange and liquefaction in the refined krypton condenser, and produces refined krypton product M5 after liquefaction, or returns to the refined krypton tower 7 through the reflux port of the refined krypton tower for cyclic enrichment to achieve the purification of the krypton product; it should be noted that the liquid or gas-liquid mixed state discharged from the outlet port of the refined krypton condenser is regulated according to the working state of the refined krypton tower. In the initial stage, it should return from the reflux port of the refined krypton tower after passing through the krypton condenser until the enriched krypton meets the concentration requirement and the refined krypton product M5 is produced.

[0057] In another embodiment of the present application, Figure 1-9 As shown:

[0058] The krypton-xenon refining device 100 further includes a recovery tower 15; the top gas of the recovery tower 15 is discharged from the third inlet end 38 of the multi-effect condenser 16; 3 The gas enters and is discharged from the corresponding outlet 39, undergoes heat exchange and liquefaction in the multi-effect condenser, and then enters the fourth gas-liquid separator 18 for gas-liquid separation. The gas phase separated by the fourth gas-liquid separator is discharged through the exhaust pipeline P3, and the liquid phase is returned to the deoxidation tower 2 for recycling through the transfer pipeline P5, or enters the recovery tower through the recovery tower reflux port for cyclic enrichment. The recovery tower bottom liquid is output from the system through the transfer pipeline P6 to enter the subsequent process. In this embodiment, the recovery tower serves as a backup reactor to treat the deoxidation tower bottom liquid or to treat the xenon product waste liquid for recovery, thereby improving the refined processing capacity of the krypton-xenon refining device.

[0059] In one embodiment of the present application, Figure 7 As shown:

[0060] The top gas of the refined xenon tower is supplied from the second inlet end 36 of the multi-effect condenser 16. 2 The gas is discharged from the corresponding outlet port 37 and the gas pipeline at the top of the xenon refinement tower flowing through the multi-effect condenser 16 is connected to the third gas-liquid separator 17. The gas at the top of the xenon refinement tower undergoes heat exchange and liquefaction in the multi-effect condenser, and then enters the third gas-liquid separator for gas-liquid separation. The gas phase separated by the third gas-liquid separator is discharged through the transmission pipeline P4 or returned to the pre-concentration system for treatment, and the liquid phase is returned to the xenon refinement tower through the transmission pipeline for circulated enrichment. The distillation residue with a low xenon concentration produced by the xenon refinement tower is transported to the recovery tower 15 for subsequent recovery and treatment.

[0061] In another embodiment of the present application, Figure 6 As shown;

[0062] The bottom liquid of the krypton removal tower 13 is returned to the recovery tower 15. When the krypton and xenon content in the bottom liquid of the krypton removal tower is reduced to a preset content, it can be transported to the recovery tower through the return liquid pipeline for further purification.

[0063] The working method or working principle of the present invention:

[0064] When the krypton-xenon refining device of the embodiment of the present application is in operation, the raw gas rich in krypton-xenon components from the purification process is fed into the first inlet port 18 of the main heat exchanger 1. 1 The raw gas enters and is discharged from its corresponding outlet 19. In this process, it exchanges heat with the cold source and accumulates cold energy. After passing through the main heat exchanger, the temperature of the raw gas is reduced to -120~-126℃. A reboiler 3 is provided in the deoxidation tower 2. The reboiler is preferably located at the bottom of the deoxidation tower. The raw gas enriched with cold energy enters from the inlet of the reboiler 3 and is discharged from the outlet of the reboiler. In the process of flowing through the reboiler, it transfers heat with the liquid medium rich in krypton and xenon in the deoxidation tower 2. The raw gas further releases heat and liquefies in the reboiler. The kettle liquid in the deoxidation tower absorbs heat and boils and evaporates, causing the light component oxygen to evaporate and overflow from the top of the deoxidation tower, and the heavy component kettle liquid accumulates at the bottom of the deoxidation tower. The heavy component kettle liquid is the krypton-xenon-rich raw material liquid; the krypton refiner receives the bottom kettle liquid of the deoxidation tower 2 and distills it. During the distillation process in the krypton refiner, the bottom kettle liquid of the krypton refiner accumulates and is then transported to the deoxidation tower for krypton removal treatment. The gas at the top of the krypton refiner enters the krypton refiner condenser for heat transfer and liquefaction to prepare the krypton product M5; the deoxidation tower 13 receives the bottom kettle liquid of the krypton refiner 7 The kettle liquid is distilled, and the bottom kettle liquid of the trough of the refining tower is xenon-rich liquid. The xenon-rich liquid enters the lower part of the deoxygenation tower and exchanges heat with the steam in the deoxygenation tower through mass transfer. The high-boiling point components are continuously accumulated at the bottom of the tower, and the low-boiling point components are discharged from the top of the deoxygenation tower and are subsequently collected for xenon. The bottom kettle liquid of the deoxygenation tower is then subjected to subsequent distillation and purification; the refining xenon tower 14 receives the condensate of the gas at the top of the deoxygenation tower 13, and the xenon-rich liquid is distilled in the refining xenon tower. The gas at the top of the refining xenon tower enters the multi-effect condenser for liquefaction treatment and returns to the refining xenon tower for circulation and enrichment. The xenon concentration in the kettle liquid accumulated at the bottom of the refined xenon tower gradually increases and produces electronic grade xenon product M6; the refined krypton condenser 8 receives the raw gas flowing through the reboiler 3 and the gas at the top of the refined krypton tower 7 and performs heat exchange. The raw gas flowing through the reboiler is transferred to the cold source gas in the refined krypton condenser as a cold source, thereby realizing the recovery and utilization of the cold energy of the cold source gas; the multi-effect condenser 16 receives the gas at the top of the dexenon tower 13 and the refined xenon tower 14 and performs heat exchange; the gas at the top of the dexenon tower is discharged from the first inlet 34 of the multi-effect condenser 16. 1 The gas at the top of the dexenon tower is liquefied in the multi-effect condenser and then returned to the reflux port of the dexenon tower or transported to the refined xenon tower; the cold source gas is carbon tetrafluoride, which is discharged from the first inlet port 28 of the refined xenon condenser 8 through the compressor 12. 1The cold energy of the raw gas flowing through the reboiler in the refined krypton condenser is transferred to the cold source gas, which absorbs the cold energy and stores it, and then flows out from the fourth inlet port 40 of the multi-effect condenser 16. 4 The cold source gas enters and is discharged from the corresponding outlet port 41, releasing cold energy in the multi-effect condenser, and the cold source gas flowing through the multi-effect condenser 16 returns to the fine krypton condenser 8 to form a closed loop circulation; the cold source gas realizes cold source absorption in the fine krypton condenser and releases and transfers cold energy in the multi-effect condenser; the gas at the top of the dekrypton tower and the fine xenon tower passes through the multi-effect condenser for cold source absorption, so as to realize the liquefaction of the corresponding gas intermediates to meet the process requirements.

[0065] In the present invention, unless otherwise clearly specified and limited, for example, it can be a fixed connection, a detachable connection, or an integrated connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, it can be internal communication between two elements or an interaction relationship between two elements. Unless otherwise clearly specified and limited, ordinary technicians in this field can understand the specific meanings of the above terms in the present invention according to specific circumstances.

[0066] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A krypton-xenon refining device with siphon refrigeration, characterized in that: include: A main heat exchanger (1), wherein the raw gas passes through the main heat exchanger (1) and accumulates cold energy; A deoxidation tower (2), wherein a reboiler (3) is provided in the deoxidation tower (2), and the raw gas transfers heat with the medium in the deoxidation tower (2) through the reboiler (3); A refinement tower (7), wherein the refinement tower (7) receives the bottom liquid of the deoxidation tower (2) and performs rectification; a desulfurization tower (13), wherein the desulfurization tower (13) receives the bottom liquid of the sulfide tower (7) and performs rectification; a xenon refinement tower (14), wherein the xenon refinement tower (14) receives the gas condensate from the top of the deoxygenation tower (13) and distills it to produce xenon liquid; a refined krypton condenser (8), wherein the refined krypton condenser (8) receives the raw gas flowing through the reboiler (3) and the top gas of the refined krypton tower (7) and performs heat exchange; a multi-effect condenser (16), wherein the multi-effect condenser (16) receives gas from the top of the de-krypton tower (13) and the refined xenon tower (14) and performs heat exchange; The cold source gas flows through the fine krypton condenser (8) through the compressor (12) to collect cold energy, and then is injected into the multi-effect condenser (16) to release cold energy, and the cold source gas flowing through the multi-effect condenser (16) returns to the fine krypton condenser (8) to form a closed loop cycle; A deoxidation tower condenser (4) is provided in conjunction with the deoxidation tower (2); The gas at the top of the deoxidation tower (2) flows through the deoxidation tower condenser (4) to be liquefied and then produces liquid oxygen product M3 or is transported to the deoxidation tower (2) for heat and mass transfer; The cold source flowing through the deoxidation tower condenser (4) is liquid nitrogen, and the liquid nitrogen flows through the main heat exchanger (1) through the conveying pipeline after passing through the deoxidation tower condenser (4) for heat exchange; The cooling gas is carbon tetrafluoride.

2. The krypton-xenon refining device with siphon refrigeration as claimed in claim 1, characterized in that: The raw gas pipeline flowing through the reboiler (3) is connected to the first gas-liquid separator (5); The gas-liquid mixture separated by the first gas-liquid separator (5) flows into the refined krypton condenser (8) and then returns to the deoxidation tower (2).

3. The krypton-xenon refining device with siphon refrigeration as claimed in claim 1, characterized in that: The raw gas pipeline at the rear end of the refined krypton condenser (8) is connected to the second gas-liquid separator (9); The gas phase and liquid phase of the raw gas separated by the second gas-liquid separator (9) are returned to different heights of the deoxidation tower (2) through the transmission pipeline respectively.

4. The krypton-xenon refining device with siphon refrigeration as claimed in claim 1, characterized in that: The refined krypton product M5 is produced by flowing through the refined krypton condenser (8) or returned to the refined krypton tower (7).

5. The krypton-xenon refining device with siphon refrigeration as claimed in claim 1, characterized in that: The krypton-xenon refining device (100) further includes a recovery tower (15); The gas at the top of the recovery tower (15) flows through the multi-effect condenser (16) and enters the fourth gas-liquid separator (18) for gas-liquid separation.

6. The krypton-xenon refining device with siphon refrigeration as claimed in claim 5, characterized in that: The gas pipeline at the top of the refined xenon tower flowing through the multi-effect condenser (16) is connected to the third gas-liquid separator (17) for gas-liquid separation; The liquid phase separated by the third gas-liquid separator (17) is returned to the xenon refinement tower (14) or transported to the recovery tower (15).

7. The krypton-xenon refining device with siphon refrigeration as claimed in claim 5, characterized in that: The bottom liquid of the deoxygenation tower (13) is returned to the recovery tower (15).

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