CN115560541A - Hydrocone type refrigerated krypton-xenon refining device - Google Patents

Hydrocone type refrigerated krypton-xenon refining device Download PDF

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Publication number
CN115560541A
CN115560541A CN202210848488.8A CN202210848488A CN115560541A CN 115560541 A CN115560541 A CN 115560541A CN 202210848488 A CN202210848488 A CN 202210848488A CN 115560541 A CN115560541 A CN 115560541A
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China
Prior art keywords
krypton
tower
gas
condenser
xenon
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CN202210848488.8A
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Chinese (zh)
Inventor
黄保华
刘媛媛
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Shanghai Huanyuyuanchuang Industrial Co ltd
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Shanghai Huanyuyuanchuang Industrial Co ltd
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Priority to CN202210848488.8A priority Critical patent/CN115560541A/en
Publication of CN115560541A publication Critical patent/CN115560541A/en
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/028—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04745—Krypton and/or Xenon
    • F25J3/04751—Producing pure krypton and/or xenon recovered from a crude krypton/xenon mixture
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/34—Krypton
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/36—Xenon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The invention provides a siphon type refrigerating krypton-xenon refining device which comprises a main heat exchanger, a deoxygenation tower, a refined krypton tower, a krypton-removing tower, a refined xenon tower, a refined krypton condenser and a multi-effect condenser, wherein the main heat exchanger is connected with the main heat exchanger; the raw material gas is automatically stored in the heat exchanger; a reboiler is arranged in the deoxygenation tower, and the feed gas transfers heat with a medium in the deoxygenation tower through the reboiler; the krypton rectifying tower receives and rectifies the tank bottom kettle liquid of the deoxygenation tower; the krypton-removing tower receives and rectifies the tank bottom kettle liquid of the krypton-refining tower; a rectification xenon tower receives and rectifies the gas condensate at the top of the krypton-removing tower; the refined krypton condenser receives the feed gas flowing through the reboiler and the top gas of the refined krypton tower and carries out heat exchange; the multi-effect condenser receives gas at the top ends of the krypton-removing tower and the refined xenon tower and exchanges heat; the cold source gas flows through the refined krypton condenser through the compressor, then is injected into the multi-effect condenser and returns to the refined krypton condenser to form closed-loop circulation. The krypton-xenon refining device reduces the production cost and improves the collection or release speed of cold energy.

Description

Hydrocone type refrigerated krypton-xenon refining device
Technical Field
The invention relates to the technical field of gas separation, in particular to a siphon type refrigerating krypton-xenon refining device.
Background
The content of krypton and xenon in the atmosphere is about 1.138x10 -6 、0.0857x10 -6 After a trace amount of krypton-xenon gas enters an air separation device such as a low-temperature rectification tower along with air, most of high-boiling-point components such as krypton, xenon, hydrocarbon (mainly methane) and fluoride are accumulated in liquid oxygen of a low-pressure tower, the liquid oxygen of the low-pressure tower is conveyed to a krypton-additional rectification tower (commonly called a poor krypton tower), so that a krypton-xenon-poor concentrate with the content of krypton and xenon of 0.2 to 0.3 percent and the content of Kr + Xe can be prepared, and the krypton-poor xenon is concentrated into the xenon-poor concentrateThe content of methane in the product is about 0.3 to 0.4 percent. Too high a methane content in oxygen (generally not exceeding 0.5%) is extremely dangerous. In view of this, the methane in the poor krypton-xenon concentrate is removed in advance, which not only can improve the safety performance of the equipment, but also can further improve the concentration of krypton and xenon in the poor krypton-xenon concentrate. In the known method, the krypton-xenon-depleted concentrate is pressurized to the critical pressure of 5.5MPa and vaporized, the pressure is reduced to 1.0MPa, the obtained product enters a methane purification device, oxygen and methane are subjected to chemical reaction in the methane purification device through a palladium catalyst at the temperature of 480-500 ℃, the methane is decomposed into carbon dioxide and water, and the content of residual methane in the krypton-xenon-depleted concentrate is lower than 1x10 -6 Then removing carbon dioxide and water by molecular sieve adsorption; and (4) feeding the feed gas without methane into a first-stage rectifying tower to obtain the krypton-xenon mixture.
The general refining equipment uses a krypton-xenon mixture as a raw material gas, uses a nitrogen and liquid nitrogen mixed gas as a cold source, separates and obtains krypton and xenon by additionally arranging a multi-stage rectification mode, and further purifies the krypton and the xenon. The method has long flow and large consumption of cold source liquid nitrogen, thereby increasing the production cost and reducing the purification efficiency of krypton and xenon.
In view of the above, the present invention provides a siphon-type refrigeration refining apparatus for krypton and xenon to solve the technical problems in the background art.
Disclosure of Invention
In order to solve the technical problem, the invention provides a siphon-type refrigerating krypton-xenon refining device, which comprises:
the feed gas passes through the main heat exchanger and stores cold energy;
the device comprises a deoxygenation tower, wherein a reboiler is arranged in the deoxygenation tower, and a feed gas is subjected to heat transfer with a medium in the deoxygenation tower through the reboiler;
the krypton rectifying tower receives and rectifies tank bottom kettle liquid of the deoxygenation tower;
the krypton removal tower receives and rectifies tank bottom kettle liquid of the refined krypton tower;
the refined xenon tower receives the gas condensate at the top of the krypton removal tower and rectifies the gas condensate to produce xenon liquid;
the refined krypton condenser receives the feed gas flowing through the reboiler and the top gas of the refined krypton tower and carries out heat exchange;
the multi-effect condenser receives gas at the top ends of the krypton-removing tower and the refined xenon tower and performs heat exchange;
cold source gas flows through the refined krypton condenser through the compressor to collect cold energy, then is injected into the multi-effect condenser to release the cold energy, and the cold source gas flowing through the multi-effect condenser returns to the refined krypton condenser to form closed-loop circulation.
Further, a condenser of the deoxygenation tower is arranged in cooperation with the deoxygenation tower;
the gas at the top end of the deoxygenation tower flows through the deoxygenation tower condenser to be liquefied to produce a liquid oxygen product M 3 Or transferring the product to a deoxygenation tower for heat and mass transfer.
Further, a feed gas pipeline flowing through the reboiler is connected into a first gas-liquid separator;
the gas-liquid mixture separated by the first gas-liquid separator flows into a fine krypton condenser and then returns to the deoxygenation tower.
Further, a raw material gas pipeline at the rear end of the refined krypton condenser is connected to a second gas-liquid separator;
the gas phase and the liquid phase of the raw material gas separated by the second gas-liquid separator are respectively returned to different heights of the deoxygenation tower through conveying pipelines.
Furthermore, a cold source flowing through the condenser of the deoxygenation tower is liquid nitrogen, and the liquid nitrogen flows through the main heat exchanger through a conveying pipeline after passing through the condenser of the deoxygenation tower to perform heat exchange.
Further, the refined krypton product M is produced by flowing through the refined krypton condenser 5 Or returned to the fine krypton column.
Further, the krypton-xenon refining device also comprises a recovery tower;
and the gas at the top end of the recovery tower flows through the multi-effect condenser and enters a fourth gas-liquid separator for gas-liquid separation.
Further, a gas pipeline at the top end of the xenon rectifying tower flowing through the multi-effect condenser is connected to a third gas-liquid separator and is subjected to gas-liquid separation;
the liquid phase separated by the third gas-liquid separator is returned to the fine xenon column or sent to the recovery column.
Further, the tank bottom liquid of the krypton removing tower returns to the recovery tower.
The technical scheme of the invention at least comprises the following technical effects:
1. in the krypton-xenon refining device provided by the embodiment of the application, the cold source gas forms a siphon effect in the process between the refined krypton condenser and the multi-effect condenser, so that the self-circulation of the refrigerant is realized, and the collection or release speed of cold energy can be increased; the cold energy circulating system not only reduces the consumption of liquid nitrogen and the production cost, but also realizes the efficient utilization of the cold energy in the krypton-xenon refining device;
2. the raw material gas is subjected to primary heat exchange by the autonomous heat exchanger, secondary heat exchange is carried out through the reboiler, cold energy accumulation is realized, raw material liquid accumulating the cold energy enters the refined krypton condenser to provide cold energy for cold source gas, cold energy recycling is realized, gas-liquid separation is realized through the second gas-liquid separator, and then the raw material liquid enters the deoxygenation tower to carry out gas-liquid mass transfer heat exchange, so that the deoxygenation efficiency of a raw material gas-liquid mixture is improved, and prepared krypton-xenon enriched liquid provides raw materials for the refined krypton tower and the refined xenon tower;
3. the krypton-xenon refining device is short in process flow, and can efficiently realize preparation of krypton and xenon;
the embodiment of the invention also comprises other advantages, which are detailed in specific embodiments.
Drawings
FIG. 1 is a schematic diagram of a flow system of a krypton-xenon refining apparatus in an embodiment of the present application;
FIG. 2 is a schematic view of the process of the feed gas condensation cycle shown in FIG. 1;
FIG. 3 is a schematic diagram of a process for preparing refined krypton in FIG. 1;
FIG. 4 is a schematic diagram of a liquid nitrogen cold energy circulation flow in FIG. 1;
FIG. 5 is a schematic diagram showing a liquid oxygen preparation process of the deoxygenator column of FIG. 1;
FIG. 6 is a schematic diagram of a process for removing krypton from the xenon-rich liquid in FIG. 1;
FIG. 7 is a schematic diagram of the flow chart for the preparation of refined xenon in FIG. 1;
FIG. 8 is a schematic diagram of a process for recovering krypton residues or xenon residues in FIG. 1;
FIG. 9 is a schematic view of the siphon-type cold energy cycle of FIG. 1.
Reference numerals:
100. a krypton-xenon refining device; 1. a primary heat exchanger; 2. a deoxygenation tower; 3. a reboiler; 4. a deoxygenation tower condenser; 5. a first gas-liquid separator; 6. a first regulating valve; 7. a fine krypton tower; 8. a refined krypton condenser; 9. a second gas-liquid separator; 10. a second regulating valve; 11. a third regulating valve; 12. a compressor; 13. a krypton removal column; 14. a fine xenon column; 15. a recovery tower; 16. a multi-effect condenser; 17. a third gas-liquid separator; 18. and a fourth gas-liquid separator.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 9 of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention, are within the scope of the invention.
A siphon type refrigeration krypton-xenon refining device 100 comprises a main heat exchanger 1, a deoxygenation tower 2, a refined krypton tower 7, a krypton-removing tower 13, a refined xenon tower 14, a refined krypton condenser 8 and a multi-effect condenser 16; the raw material gas passes through the main heat exchanger 1 and accumulates cold energy; a reboiler 3 is arranged in the deoxygenation tower 2, and the feed gas is in heat transfer with a medium in the deoxygenation tower 2 through the reboiler 3; the krypton rectifying tower 7 receives and rectifies the tank bottom liquid of the deoxygenation tower 2; the krypton-removing tower 13 receives and rectifies the tank bottom kettle liquid of the krypton-refining tower 7; the refined xenon tower 14 receives the gas condensate at the top of the krypton-removing tower 13 and rectifies the gas condensate to produce xenon liquid; the refined krypton condenser 8 receives the feed gas flowing through the reboiler 3 and the top gas of the refined krypton tower 7 and carries out heat exchange; the multi-effect condenser 16 receives the top gas of the krypton-removing tower 13 and the refined xenon tower 14 and carries out heat exchange; wherein, cold source gas flows through the fine krypton condenser 8 through the compressor 12 to collect cold energy, then is injected into the multi-effect condenser 16 to release the cold energy, and the cold source gas flowing through the multi-effect condenser 16 returns to the fine krypton condenser 8 to form closed-loop circulation.
As shown in figures 1-9: the invention provides a siphon type refrigerating krypton-xenon refining device, wherein the krypton-xenon refining device 100 comprises a main heat exchanger 1, a deoxygenation tower 2, a refined krypton tower 7, a krypton removing tower 13, a refined xenon tower 14, a refined krypton condenser 8 and a multi-effect condenser 16; the initial temperature of the raw material gas rich in krypton-xenon from the purification process is 15-25 ℃, the pressure is 18-20bar, and the main component content of the raw material gas is as follows: oxygen is more than or equal to 99.5 percent, methane is less than or equal to 10ppb, krypton is more than or equal to 1500ppm, xenon is more than or equal to 300ppm, and other components comprise trace carbon dioxide, nitrous oxide, carbon tetrafluoride and the like; the raw gas is from the first inlet end 18 of the main heat exchanger 1 1 The raw material gas enters and is discharged from a corresponding outlet end 19, heat exchange is carried out with a cold source in the process, cold energy is accumulated, and the temperature of the raw material gas is reduced to-120 to-126 ℃ after passing through a main heat exchanger; a reboiler 3 is arranged in the deoxygenation tower 2, the reboiler is preferably arranged at the bottom of the deoxygenation tower, the cold energy-enriched feed gas enters from the inlet end of the reboiler 3 and is discharged from the outlet end of the reboiler, the feed gas and the krypton-xenon-enriched liquid medium in the deoxygenation tower 2 are subjected to heat transfer in the process of flowing through the reboiler, the feed gas is condensed in the reboiler to further release heat and be liquefied, and the kettle liquid in the deoxygenation tower absorbs heat to be boiled and evaporated, so that light components such as oxygen are evaporated and overflow from the top end of the deoxygenation tower, and heavy component kettle liquid is accumulated at the bottom end of the deoxygenation tower, namely krypton-xenon-enriched feed liquid; the refined krypton tower 7 receives and rectifies the tank bottom kettle liquid of the deoxygenation tower 2, the tank bottom kettle liquid is conveyed to the krypton-removing tower for krypton removal treatment after being accumulated in the tank bottom kettle liquid of the refined krypton tower in the rectification process of the refined krypton tower, and the gas at the top end of the refined krypton tower enters a refined krypton condenser for heat transfer and liquefaction to prepare a krypton product M 5 (ii) a The krypton-removing tower 13 receives and rectifies the bottom kettle liquid of the krypton-removing tower 7, the bottom kettle liquid of the krypton-removing tower is a xenon-rich liquid, the xenon-rich liquid enters the lower part of the krypton-removing tower and exchanges mass and heat with steam in the krypton-removing tower, high-boiling components are continuously accumulated at the bottom of the tower, low-boiling components are discharged from the top of the krypton-removing tower and are subjected to subsequent xenon collection, and the bottom kettle liquid of the krypton-removing tower is subjected to subsequent rectification and purification; the refined xenon tower 14 receives the gas condensate at the top of the krypton-removing tower 13, the xenon-rich liquid in the refined xenon tower is rectified, and the gas at the top of the refined xenon tower enters a multi-effect condenser for liquefactionAnd returning to the refined xenon tower for cyclic enrichment, gradually increasing the concentration of the xenon in the kettle liquid enriched at the bottom of the refined xenon tower and producing an electronic grade xenon product M 6 Wherein the xenon product M 6 The purity is more than or equal to 99.9999995%; the refined krypton condenser 8 receives the feed gas flowing through the reboiler 3 and the top gas of the refined krypton tower 7, carries out heat exchange, and the feed gas flowing through the reboiler is used as a cold source in the refined krypton condenser and is transmitted to the cold source gas, so that the cold energy of the cold source gas is recycled; the multi-effect condenser 16 receives the top gas of the krypton-removing tower 13 and the refined xenon tower 14 and carries out heat exchange; the top gas of the krypton-removing tower flows from the first inlet end 34 of the multi-effect condenser 16 1 The gas enters and is discharged from a corresponding outlet end, and the gas at the top of the krypton-removing tower is liquefied in a multi-effect condenser and then returns to a reflux port of the krypton-removing tower or is conveyed to a refined xenon tower; wherein the cold source gas is carbon tetrafluoride, the initial pressure of the carbon tetrafluoride is 24 to 26bar, the temperature is 35 to 38 ℃, and the carbon tetrafluoride gas passes through a compressor 12 from a first inlet end 28 of a fine krypton condenser 8 1 Enters and is discharged from a corresponding outlet end 29, the cold energy of the feed gas flowing through the reboiler in the fine krypton condenser is transferred to the cold source gas, the cold source gas absorbs the cold energy to store the energy and then flows from a fourth inlet end 40 of the multi-effect condenser 16 4 Enters and is discharged from the corresponding outlet end 41, the cold energy is released in the multi-effect condenser, and the cold source gas flowing through the multi-effect condenser 16 returns to the refined krypton condenser 8 to form closed-loop circulation; the cold source gas realizes cold source absorption in the refined krypton condenser and releases and transfers cold energy in the multi-effect condenser; the top gases of the krypton-removing tower and the refined xenon tower are absorbed by a cold source through a multi-effect condenser so as to realize the liquefaction of corresponding gas intermediates and meet the process requirements.
The krypton-xenon refining device is short in process flow, and can efficiently realize preparation of krypton and xenon; the cold source gas forms a siphon effect in the process of the flow between the fine krypton condenser and the multi-effect condenser, so that the self-circulation of the refrigerant is realized, and the collection or release speed of cold energy can be increased; the cold energy circulating system not only reduces the consumption of liquid nitrogen and the production cost, but also realizes the efficient utilization of the cold energy in the krypton-xenon refining device.
In another embodiment of the present application, as shown in fig. 3:
a deoxygenation tower condenser 4 is arranged in cooperation with the deoxygenation tower 2; the krypton-xenon-rich raw material liquid exchanges heat with the raw material gas flowing through the reboiler in the deoxygenation tower, and heat energy is transferred to the kettle liquid in the deoxygenation tower, so that light components such as oxygen are boiled and overflow, the gas at the top end of the deoxygenation tower 2 contains high-concentration oxygen, and the light components are boiled and overflow from the second inlet end 26 of the condenser 4 of the deoxygenation tower 2 Enters and is discharged from a corresponding outlet end 27, the oxygen-enriched gas and the liquid nitrogen exchange heat and are liquefied in the deoxidizing condenser, and the liquefied oxygen-containing liquid can be used as an industrial oxygen product M 3 The output value is stored in a liquid oxygen tank, or is conveyed to the top of the deoxygenation tower 2 to further transfer heat and mass with the rising steam in the deoxygenation tower, so that the oxygen concentration is improved; the top gas of the self-deoxidation tower can also be connected to the second inlet end 20 of the main heat exchanger by an emptying pipeline 2 And is discharged from the corresponding outlet end 21 of the main heat exchanger, through the evacuation line P 1 The gas at the top end of the deoxygenation tower can be emptied and the cold energy can be recovered, so that the cold energy collection of the feed gas in the main heat exchanger is improved.
In another embodiment of the present application, as shown in FIG. 3;
a feed gas pipeline flowing through the reboiler 3 is connected into a first gas-liquid separator 5, a raw material gas-liquid mixture is subjected to gas-liquid separation in the first gas-liquid separator 5, a gas phase is discharged, a liquid phase of the feed gas is throttled to 15 to 19bar after passing through a first regulating valve 6 on the feed gas pipeline, and a third inlet end 32 of a condenser of the krypton rectifying tower is connected with a third inlet end 32 of the condenser of the krypton rectifying tower 3 Enters and is discharged from a corresponding outlet end 33, the raw material liquid in the refined krypton condenser 8 is used as a cold source of carbon tetrafluoride gas, and is gasified by a small amount when passing through the refined krypton condenser; at the moment, the raw material gas-liquid mixture can return to the deoxygenation tower for mass transfer and heat exchange so as to improve the deoxygenation of the raw material liquid.
In another embodiment of the present application, as shown in fig. 2:
a raw material gas pipeline at the rear end of the refined krypton condenser 8 is connected to a second gas-liquid separator 9; discharging a raw material gas-liquid mixture from a condenser at the top of the refined krypton tower, allowing the raw material gas-liquid mixture to enter a second gas-liquid separator for gas-liquid separation, throttling a separated liquid phase to 4-7 bar through a third regulating valve 11, and allowing the separated liquid phase to enter the tower from the middle upper part of the deoxygenation tower 2 for exchanging heat with ascending steam; the gas phase separated from the second gas-liquid separator 9 is throttled to 4 to 7bar through a second regulating valve 10, enters the tower from the middle upper part of the deoxygenation tower, and exchanges heat with the top reflux liquid to realize the deoxygenation of the feed gas; it should be noted that the gas phase and the liquid phase of the raw material liquid separated by the second gas-liquid separator 9 are respectively returned to the different heights of the deoxygenation column 2 through the conveying pipelines, so as to realize the best countercurrent mass transfer heat exchange. In the embodiment, the raw material gas is subjected to secondary heat exchange through the reboiler after being subjected to heat exchange by the main heat exchanger, cold energy accumulation is realized, then the raw material liquid accumulating the cold energy enters the fine krypton condenser to provide cold energy for cold source gas, condensation recycling is realized, then gas-liquid separation is realized through the second gas-liquid separator, and then the raw material liquid enters the deoxygenation tower to perform gas-liquid mass transfer heat exchange, so that the deoxygenation efficiency of a raw material gas-liquid mixture is improved, and the prepared krypton-xenon enriched liquid provides raw materials for the fine krypton tower and the fine xenon tower.
In another embodiment of the present application, as shown in fig. 4:
the cold source flowing through the condenser 4 of the oxygen removal tower is liquid nitrogen, the initial pressure of the liquid nitrogen is 12-13bar, the temperature is about-186 ℃, and the liquid nitrogen passes through the first inlet end 24 of the condenser 4 of the oxygen removal tower 1 Enters and is discharged from a corresponding outlet end 25, and can exchange heat with the gas at the top of the self-deoxidation tower in a condenser 4 of the deoxidation tower so as to provide cold energy for the liquefaction of the oxygen, and the temperature is raised to minus 160 to minus 170 ℃; the nitrogen flowing through the condenser of the deoxygenating tower passes through the conveying pipeline from the third inlet end 22 of the main heat exchanger 1 3 And the nitrogen rich in cold energy enters and is discharged from the corresponding outlet end 23, the heat exchange is carried out between the nitrogen rich in cold energy and the feed gas in the main heat exchanger, and the temperature of the nitrogen is raised to minus 50 to minus 40 ℃, so that the cold energy of the nitrogen is recycled, and the cold energy accumulation of the feed gas is realized. In this embodiment, the cold energy utilization line P 2 The liquid nitrogen cold energy can be fully utilized, and the utilization rate of the liquid nitrogen cold energy is improved; the nitrogen flowing through the main heat exchanger carries cold energy to continue to enter the raw material liquid purification process to continue to recover the cold energy.
In another embodiment of the present application, as shown in fig. 5:
the bottom residue of the deoxygenation tower enters a rectification krypton tower 7 for rectification and separation, and the gas at the top end of the rectification krypton tower automatically rectifies the second inlet end 30 of the krypton condenser 8 2 Enters and is discharged from a corresponding outlet end 31, exchanges heat in a fine krypton condenser and is liquefied, and a fine krypton product M is produced after liquefaction 5 Or returning the purified krypton product to the refined krypton tower 7 through a reflux port of the refined krypton tower for cyclic enrichment to purify the krypton product; it should be noted that the liquid state or gas-liquid mixed state discharged from the outlet end of the fine krypton condenser is regulated and controlled according to the working state of the fine krypton tower, and the liquid state or gas-liquid mixed state from the fine krypton condenser at the initial stage should be returned from the reflux port of the fine krypton tower until enriched krypton meets the concentration requirement, and then the fine krypton product M is produced 5 。
In another embodiment of the present application, as shown in FIGS. 1-9:
the krypton-xenon refining apparatus 100 further comprises a recovery column 15; the gas at the top end of the recovery tower 15 flows from the third inlet end 38 of the multi-effect condenser 16 3 Enters and is discharged from the corresponding outlet end 39, exchanges heat in the multi-effect condenser and is liquefied, and then enters the fourth gas-liquid separator 18 for gas-liquid separation; the gas phase separated by the fourth gas-liquid separator passes through an evacuation line P 3 Emptying, passing liquid phase through a delivery pipe P 5 Returning to the deoxygenation tower 2 for recycling, or entering a recovery tower through a reflux port of the recovery tower for recycling and enrichment; the bottom kettle liquid of the recovery tower passes through a conveying pipeline P 6 And the output system enters a subsequent process. In the embodiment, the recovery tower can be used as a spare reactor for treating the tank bottom liquid of the krypton-removing tower or treating the xenon product waste liquid for recovery, so that the fine treatment capacity of the krypton-xenon refining device is improved.
In one embodiment of the present application, as shown in fig. 7:
the top gas of the refined xenon tower is from the second inlet end 36 of the multi-effect condenser 16 2 And is discharged from the corresponding outlet end 37, the top end gas pipeline of the xenon rectifying tower flowing through the multi-effect condenser 16 is connected into the third gas-liquid separator 17, the top end gas flow of the xenon rectifying tower is subjected to heat exchange and liquefaction in the multi-effect condenser, then enters the third gas-liquid separator for gas-liquid separation, and the gas phase separated by the third gas-liquid separator passes through the conveying pipeline P 4 Emptying or returning to a pre-concentration system for treatment, and returning the liquid phase to a refined xenon tower through a conveying pipeline for cyclic enrichment; the rectification raffinate with low xenon concentration produced by the xenon rectifying tower is conveyed to a recovery tower 15 for carrying outAnd (5) subsequent recovery treatment.
In another embodiment of the present application, as shown in FIG. 6;
and returning the tank bottom kettle liquid of the krypton-removing tower 13 to the recovery tower 15, and when the content of krypton and xenon in the tank bottom kettle liquid of the krypton-removing tower is reduced to a preset content, conveying the tank bottom kettle liquid to the recovery tower through a liquid return pipeline for further purification.
The working method or working principle of the invention is as follows:
in the krypton-xenon refining apparatus of the embodiment of the present application, during operation, the krypton-xenon-component-rich raw material gas from the purification process is supplied from the first inlet end 18 of the main heat exchanger 1 1 The raw material gas enters and is discharged from a corresponding outlet end 19, heat exchange is carried out with a cold source in the process, cold energy is accumulated, and the temperature of the raw material gas is reduced to-120 to-126 ℃ after passing through a main heat exchanger; a reboiler 3 is arranged in the deoxygenation tower 2, the reboiler is preferably arranged at the bottom of the deoxygenation tower, the cold-energy-enriched feed gas enters from the inlet end of the reboiler 3 and is discharged from the outlet end of the reboiler, the feed gas is subjected to heat transfer with a krypton-xenon-rich liquid medium in the deoxygenation tower 2 in the process of flowing through the reboiler, the feed gas is further subjected to heat release liquefaction in the reboiler, kettle liquid in the deoxygenation tower absorbs heat to be boiled and evaporated, so that light-component oxygen is evaporated and overflows from the top end of the deoxygenation tower, heavy-component kettle liquid is accumulated at the bottom end of the deoxygenation tower, and the heavy-component kettle liquid is krypton-xenon-rich raw material liquid; the refined krypton tower receives and rectifies the tank bottom kettle liquid of the deoxygenation tower 2, the tank bottom kettle liquid is conveyed to the krypton-removing tower for krypton-removing treatment after being accumulated in the tank bottom kettle liquid of the refined krypton tower in the rectification process of the refined krypton tower, and the gas at the top end of the refined krypton tower enters the refined krypton condenser for heat transfer and liquefaction to prepare a krypton product M 5 (ii) a The krypton-removing tower 13 receives and rectifies the tank bottom kettle liquid of the krypton-removing tower 7, the tank bottom kettle liquid of the krypton-removing tower is a xenon-rich liquid, the xenon-rich liquid enters the lower part of the krypton-removing tower and exchanges mass transfer with steam in the krypton-removing tower, high-boiling components are continuously accumulated at the bottom of the tower, low-boiling components are discharged from the top of the krypton-removing tower and are subsequently collected for xenon, and the tank bottom kettle liquid of the krypton-removing tower is subsequently rectified and purified; the refined xenon tower 14 receives the gas condensate at the top of the krypton-removing tower 13, the xenon-rich liquid in the refined xenon tower is rectified, the gas at the top of the refined xenon tower enters a multi-effect condenser for liquefaction and returns to the refined xenon tower for circulating enrichment, and the concentration of the xenon in the kettle liquid enriched at the bottom of the refined xenon tower is gradually increasedPromoting and producing electronic grade xenon product M 6 (ii) a The refined krypton condenser 8 receives the feed gas flowing through the reboiler 3 and the top gas of the refined krypton tower 7, carries out heat exchange, and the feed gas flowing through the reboiler is used as a cold source in the refined krypton condenser and is transmitted to the cold source gas, so that the cold energy of the cold source gas is recycled; the multi-effect condenser 16 receives the top gas of the krypton-removing tower 13 and the refined xenon tower 14 and carries out heat exchange; the top gas of the krypton-removing tower flows from the first inlet end 34 of the multi-effect condenser 16 1 The gas enters and is discharged from a corresponding outlet end, and the gas at the top of the krypton-removing tower is liquefied in a multi-effect condenser and then returns to a reflux port of the krypton-removing tower or is conveyed to a refined xenon tower; the cold source gas is carbon tetrafluoride, and the carbon tetrafluoride gas passes through the compressor 12 from the first inlet end 28 of the refined krypton condenser 8 1 Enters and is discharged from the corresponding outlet end 28, the cold energy of the feed gas flowing through the reboiler in the fine krypton condenser is transferred to the cold source gas, the cold source gas absorbs the cold energy to store energy and then is discharged from the fourth inlet end 40 of the multi-effect condenser 16 4 Enters and is discharged from the corresponding outlet end 41, the cold energy is released in the multi-effect condenser, and the cold source gas flowing through the multi-effect condenser 16 returns to the refined krypton condenser 8 to form closed-loop circulation; the cold source gas realizes cold source absorption in the refined krypton condenser and releases and transfers cold energy in the multi-effect condenser; the top gases of the krypton-removing tower and the refined xenon tower are absorbed by a cold source through a multi-effect condenser so as to realize the liquefaction of corresponding gas intermediates and meet the process requirements.
In the present invention, unless otherwise explicitly specified or limited, for example, it may be fixedly attached, detachably attached, or integrated; can be mechanically or electrically connected; the terms may be directly connected or indirectly connected through an intermediate agent, and may be used for communicating the inside of two elements or interacting relation of two elements, unless otherwise specifically defined, and the specific meaning of the terms in the present invention can be understood by those skilled in the art according to specific situations.
The foregoing is a preferred embodiment of the present invention, and it should be noted that it would be apparent to those skilled in the art that various modifications and enhancements can be made without departing from the principles of the invention, and such modifications and enhancements are also considered to be within the scope of the invention.

Claims (9)

1. A kind of hydrocone type refrigerated krypton-xenon refining plant, characterized by that, including:
the device comprises a main heat exchanger (1), wherein raw gas passes through the main heat exchanger (1) and accumulates cold energy;
the device comprises a deoxygenation tower (2), wherein a reboiler (3) is arranged in the deoxygenation tower (2), and feed gas is in heat transfer with a medium in the deoxygenation tower (2) through the reboiler (3);
the krypton rectifying tower (7), wherein the krypton rectifying tower (7) receives and rectifies the tank bottom liquid of the deoxygenation tower (2);
the krypton-removing tower (13), wherein the krypton-removing tower (13) receives and rectifies the tank bottom liquid of the krypton-refining tower (7);
the xenon rectifying tower (14) receives the gas condensate at the top of the krypton-removing tower (13) and rectifies the gas condensate to produce xenon liquid;
a refined krypton condenser (8), wherein the refined krypton condenser (8) receives the feed gas flowing through the reboiler (3) and the top gas of the refined krypton tower (7) and carries out heat exchange;
the multi-effect condenser (16) receives gas at the top ends of the krypton-removing tower (13) and the refined xenon tower (14) and carries out heat exchange;
cold source gas flows through the fine krypton condenser (8) through the compressor (12) to collect cold energy, then the cold energy is injected into the multi-effect condenser (16) to release the cold energy, and the cold source gas flowing through the multi-effect condenser (16) returns to the fine krypton condenser (8) to form closed-loop circulation.
2. The hydrocone type refrigerated krypton-xenon refining apparatus of claim 1, wherein: a deoxygenation tower condenser (4) is arranged in cooperation with the deoxygenation tower (2);
the gas at the top end of the deoxygenation tower (2) flows through the deoxygenation tower condenser (4) to be liquefied to produce a liquid oxygen product M 3 Or is conveyed to the inside of the deoxygenation tower (2) for heat and mass transfer.
3. The hydrocone type refrigerated krypton-xenon refining apparatus of claim 1, wherein: a feed gas pipeline flowing through the reboiler (3) is connected into a first gas-liquid separator (5);
the gas-liquid mixture separated by the first gas-liquid separator (5) flows into a refined krypton condenser (8) and then returns to the deoxygenation tower (2).
4. The apparatus of claim 2, wherein the hydrocone type refrigeration krypton-xenon refining apparatus comprises: a raw material gas pipeline at the rear end of the refined krypton condenser (8) is connected to a second gas-liquid separator (9);
the gas phase and the liquid phase of the raw material gas separated by the second gas-liquid separator (9) respectively return to different heights of the deoxygenation tower (2) through conveying pipelines.
5. The hydrocone type refrigerated krypton-xenon refining apparatus of claim 1, wherein: the cold source flowing through the condenser (4) of the deoxygenation tower is liquid nitrogen, and the liquid nitrogen flows through the main heat exchanger (1) through a conveying pipeline after passing through the condenser (4) of the deoxygenation tower for heat exchange.
6. The hydrocone type refrigerated krypton-xenon refining apparatus of claim 1, wherein: flowing through the refined krypton condenser (8) to produce refined krypton product M 5 Or returned to the refined krypton column (7).
7. The hydrocone type refrigerated krypton-xenon refining apparatus of claim 1, wherein: the krypton-xenon refining device (100) further comprises a recovery tower (15);
and the gas at the top end of the recovery tower (15) flows through the multi-effect condenser (16) and enters a fourth gas-liquid separator (18) for gas-liquid separation.
8. The hydrocone type refrigerated krypton-xenon refining apparatus of claim 7, wherein: a gas pipeline at the top end of the xenon rectifying tower flowing through the multi-effect condenser (16) is connected into a third gas-liquid separator (17) and is subjected to gas-liquid separation;
the liquid phase separated by the third gas-liquid separator (17) is returned to the xenon refining column (14) or sent to the recovery column (15).
9. The hydrocone type refrigerated krypton-xenon refining apparatus of claim 7, wherein: and the tank bottom liquid of the krypton-removing tower (13) returns to the recovery tower (15).
CN202210848488.8A 2022-07-19 2022-07-19 Hydrocone type refrigerated krypton-xenon refining device Pending CN115560541A (en)

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CN202210848488.8A CN115560541A (en) 2022-07-19 2022-07-19 Hydrocone type refrigerated krypton-xenon refining device

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CN202210848488.8A CN115560541A (en) 2022-07-19 2022-07-19 Hydrocone type refrigerated krypton-xenon refining device

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115060042A (en) * 2022-07-27 2022-09-16 郑州耀强化工产品有限公司 Hydrocone type refrigerated krypton-xenon refining device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115060042A (en) * 2022-07-27 2022-09-16 郑州耀强化工产品有限公司 Hydrocone type refrigerated krypton-xenon refining device

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