CN116518646A - Production system and process for producing high-purity krypton-xenon product by adopting mixed refrigerant - Google Patents

Production system and process for producing high-purity krypton-xenon product by adopting mixed refrigerant Download PDF

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Publication number
CN116518646A
CN116518646A CN202310488889.1A CN202310488889A CN116518646A CN 116518646 A CN116518646 A CN 116518646A CN 202310488889 A CN202310488889 A CN 202310488889A CN 116518646 A CN116518646 A CN 116518646A
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xenon
tower
krypton
condenser
mixed refrigerant
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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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    • 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
    • F25J3/0228—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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00—Noble gases; Compounds thereof
    • C01B23/001—Purification or separation processes of noble gases
    • C01B23/0036—Physical processing only
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/04—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa
    • C09K5/041—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa for compression-type refrigeration systems
    • 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
    • F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
    • 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
    • F25J3/04278—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using external refrigeration units, e.g. closed mechanical or regenerative refrigeration units
    • 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
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/12—External refrigeration with liquid vaporising loop
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/66—Closed external refrigeration cycle with multi component refrigerant [MCR], e.g. mixture of hydrocarbons
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/902—Details about the refrigeration cycle used, e.g. composition of refrigerant, arrangement of compressors or cascade, make up sources, use of reflux exchangers etc.

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  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
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Abstract

The invention provides a production system and a process for producing a high-purity krypton-xenon product by adopting a mixed refrigerant, which belong to the technical field of high-purity krypton-xenon product production, and the production system for producing the high-purity krypton-xenon product by adopting the mixed refrigerant comprises a high-purity krypton-xenon production device and a mixed refrigerant device for providing a cold source for the high-purity krypton-xenon production device; the mixed refrigerant device comprises a condenser for providing a cold source for the high-purity krypton-xenon production device, mixed refrigerant is injected into the condenser, the mixed refrigerant comprises a mixed refrigerant I, a mixed refrigerant II and a mixed refrigerant III, and the mixed refrigerant device provides cold source circulation for the condenser at the top of each rectifying tower through a thermal coupling process; according to the invention, the first mixed refrigerant and the second mixed refrigerant are supplied once, so that the stable operation requirement can be met, the third mixed refrigerant can be reused, and the cold energy utilization rate is high; the prepared product is stable, and industrial oxygen can be produced as a byproduct while the high-purity krypton-xenon product is obtained.

Description

Production system and process for producing high-purity krypton-xenon product by adopting mixed refrigerant
Technical Field
The invention relates to the technical field of high-purity krypton-xenon product production, in particular to a production system and a production process for producing a high-purity krypton-xenon product by adopting a mixed refrigerant.
Background
The high-purity krypton-xenon product is used as an indispensable key material in the semiconductor manufacturing process, and new growth power is injected for technological innovation trends such as 5G and the like. Krypton and xenon are large molecular weight inert gases, and the properties of krypton and xenon determine that krypton and xenon have irreplaceable functions in the field of high-end manufacturing, particularly in the field of integrated circuit manufacturing and space technology, the requirements are increasing in recent years, the supply increment is slow, and the contradiction between supply and demand is increasing.
The process technology for producing the rare gas krypton-xenon product in China has low cost and is limited to the property of krypton-xenon at present, generally, low-temperature nitrogen or liquid nitrogen is adopted as a production process of five towers or six towers matched with a refrigerant, the refrigerant needs to be supplemented for many times, the process route of a production device is complex, the operation stability performance is poor, and the product purity needs to be improved. For example, chinese patent publication No. CN 212390705U discloses a device for refining rare gas krypton-xenon and producing ultra-pure oxygen, comprising a liquid oxygen storage tank and a nitrogen recycle compressor, wherein the liquid oxygen storage tank is connected with a primary concentration tower through a liquid oxygen pump and a cryogenic adsorption tower; the bottom liquid phase outlet of the primary concentration tower is connected with a catalytic oxidation system with a high-pressure throttle valve at the tail end; the high-pressure throttle valve sequentially passes through a tube side of a back cooler, a secondary concentration tower, a krypton-xenon deoxidization tower and a gas heating device to be connected with a krypton-xenon separation tower for storing and separating krypton-xenon, the bottom of the krypton-xenon separation tower is connected with a xenon filling system through a first valve, and the middle upper part of the krypton-xenon separation tower is connected with the krypton-xenon filling system through a second valve.
Therefore, there is a need to provide a production system and process for producing high purity krypton-xenon products using mixed refrigerants to solve the above-mentioned problems of the prior art.
Disclosure of Invention
In view of this, the invention provides a production system and a process for producing high-purity krypton-xenon products by using mixed refrigerants, wherein the mixed refrigerant I and the mixed refrigerant II are supplied once, so that the stable operation requirement can be met, the mixed refrigerant III can be reused, and the cold energy utilization rate is high.
In order to achieve the above purpose, the invention provides a production system and a process for producing a high-purity krypton-xenon product by adopting a mixed refrigerant, which adopts the following technical scheme:
a production system for producing a high-purity krypton-xenon product by adopting a mixed refrigerant comprises a high-purity krypton-xenon production device and a mixed refrigerant device for providing a cold source for the high-purity krypton-xenon production device;
the high-purity krypton-xenon production device comprises a main heat exchanger connected with an air source, a deoxidizing unit connected with an outlet of the main heat exchanger, a krypton production unit connected with the deoxidizing unit, a xenon production unit connected with a liquid outlet of the krypton production unit, and a recovery unit connected with the liquid outlet of the xenon production unit, wherein an outlet of the recovery unit is connected with the xenon production unit and used for recovering xenon;
The mixed refrigerant device comprises a condenser for providing a cold source for the high-purity krypton-xenon production device, wherein mixed refrigerant is injected into the condenser, the mixed refrigerant comprises a mixed refrigerant I, a mixed refrigerant II and a mixed refrigerant III, the mixed refrigerant I is liquid nitrogen, and the mixed refrigerant II is 80% CF 4 And 20% O 2 The third mixed refrigerant is CF 4 The mixed condensing agent provides a condensing source for the deoxidizing unit, the krypton production unit and the xenon production unit respectively.
Further, the deoxidizing unit comprises a deoxidizing tower connected with the outlet of the main heat exchanger through a pipeline, a purifier connected with the liquid phase outlet at the bottom of the deoxidizing tower through a pipeline, and a first separator connected with the gas phase outlet at the top of the deoxidizing tower through a pipeline, wherein the mixed refrigerant device is connected with the first separator and the gas phase outlet at the top of the deoxidizing tower for providing a cold source, and a first liquid phase outlet of the first separator is connected with a second inlet of the deoxidizing tower through a pipeline for refluxing condensed liquid.
Further, the krypton production unit comprises a pure krypton tower connected with an outlet of the deoxidizing unit through a pipeline, a second separator connected with a gas phase outlet at the top of the pure krypton tower through a pipeline, a liquid phase outlet at the bottom of the pure krypton tower is connected with the xenon production unit through a pipeline, a mixed refrigerant device is connected with the second separator for providing a cold source, and a first outlet of the second separator is connected with a second inlet of the pure krypton tower through a pipeline for refluxing condensed liquid.
Further, the xenon production unit comprises a crude xenon tower connected with the krypton production unit through a pipeline, and a pure xenon tower connected with a second outlet of the crude xenon tower through a pipeline, wherein a gas phase outlet at the top of the crude xenon tower and a gas phase outlet at the top of the pure xenon tower are connected with a mixed refrigerant device through pipelines, the gas phase at the top of the crude xenon tower exchanges heat and then flows back fully, the pure xenon gas flows to an inlet of the pure xenon tower after components are rectified, the gas phase at the top of the pure xenon tower exchanges heat and then flows back fully, and a high-purity xenon product is obtained at a liquid phase outlet at the bottom of the pure xenon tower after rectification.
Further, the recovery unit comprises a recovery tower connected with a liquid phase outlet at the bottom of the crude xenon tower through a pipeline, and a separator III connected with a second inlet of the recovery tower through a pipeline, and a gas phase outlet at the top of the recovery tower is connected with a second inlet of the recovery tower through a third inlet of a mixed refrigerant device, a third outlet of the mixed refrigerant device, a third inlet of the separator III, and a liquid phase outlet of the separator; the extraction outlet in the recovery tower is connected with the third inlet of the crude xenon tower, and the third gas phase outlet of the separator is discharged to the atmosphere through a seventh regulating valve; the liquid phase outlet at the bottom of the recovery tower is discharged to the atmosphere.
Further, the mixed refrigerant device comprises a deoxidizing tower top condenser, a pure krypton tower top condenser, a xenon tower top condenser, a mixed refrigerant I, a mixed refrigerant II and a mixed refrigerant III, wherein the externally-supplemented mixed refrigerant I is connected with a krypton tower condenser fourth inlet through a pure krypton tower top condenser third inlet, an evaporation gas outlet, a ninth regulating valve, a deoxidizing top condenser second inlet and a deoxidizing top condenser second outlet, the externally-supplemented mixed refrigerant II is connected with the krypton tower top condenser second inlet through a krypton tower top condenser second inlet, a krypton tower top condenser second outlet, a xenon tower condenser fourth inlet, a xenon tower condenser gas phase outlet, a tenth regulating valve and a third tee joint, the externally-supplemented mixed refrigerant III is connected with the deoxidizing tower top condenser third inlet, and the deoxidizing tower top condenser top gas phase is connected with a main heat exchanger (1) third inlet and a third regulating valve.
A production process for producing a high-purity krypton-xenon product by adopting a mixed refrigerant comprises the following steps:
step one: after heat exchange of the raw material gas through the main heat exchanger, the raw material gas enters the deoxidizing tower through the first regulating valve, and heat and cold rectification are respectively provided through the first electric heater at the tower bottom and the condenser at the top of the deoxidizing tower, wherein the temperature of the raw material gas is as follows: 20-30 ℃, the pressure is: 0.65Mpa, the flow is: 800Nm/h, gas phase fraction: 1, krypton and xenon contents are respectively: 1000-2000 ppm, 20-200 ppm;
step two: enabling a gas phase after primary rectification purification of the raw material liquid entering the deoxidizing tower in the first step to enter a condenser at the top of the deoxidizing tower and a main heat exchanger respectively through a first tee joint, recovering part of cold energy through the main heat exchanger, and then, enabling the cold energy to enter a back cooler, and enabling crude krypton-xenon liquid at the bottom of the deoxidizing tower to enter a purifier; temperature of crude krypton-xenon liquid at the bottom of the deoxidizing tower: -129.2 to-129.5 ℃, and the mole fraction of krypton and xenon is as follows: 99.97 to 99.99 percent;
step three: the gas phase in the second step enters a condenser at the top of the deoxidizing tower through a first tee joint to be liquefied and then enters a first separator, a liquid phase outlet at the bottom of the first separator flows back to a second inlet of the deoxidizing tower, and a second liquid phase outlet of the first separator flows to an industrial oxygen storage tank through an eleventh regulating valve; the liquid phase temperature of the industrial oxygen is as follows: -164 to-166 ℃, and the molar purity is not lower than 99.98%;
Step four: the crude krypton-xenon liquid in the deoxidizing tower kettle in the second step is connected with a purifier through a fourth regulating valve, and the gas phase at the outlet of the purifier is discharged into the pure krypton tower; purifier outlet temperature: the mole fraction of krypton and xenon is between 30 ℃ and 35 ℃ below zero: 99.995 to 99.999 percent;
step five: in the fourth step, the raw material gas of the pure krypton tower is rectified through a condenser at the top of the pure krypton tower and an electric heater II, after multiple gasification liquefaction, the gas phase of the pure krypton tower is liquefied through the condenser at the top of the pure krypton tower and then flows back into the pure krypton tower to a liquid phase outlet at the bottom of the second separator, the second liquid phase outlet of the second separator is connected with a krypton vaporizer through a fifth regulating valve, and the purity of krypton gas at the inlet of the krypton vaporizer is 99.9998%;
step six: in the fifth step, the liquid phase outlet at the bottom of the pure krypton tower is connected with the first inlet (43) of the crude xenon tower, and the xenon content of the liquid phase outlet at the bottom of the pure krypton tower is 99.98%;
step seven: in the step six, raw material gas of the crude xenon tower is rectified through a xenon tower condenser and a heater, after gasification and liquefaction are carried out for many times, gas phase of the top of the crude xenon tower is liquefied through a xenon tower top condenser (12) and then flows back into a crude xenon tower (11), a second outlet of the crude xenon tower enters the pure xenon tower through an eleventh regulating valve, and the gas phase xenon content of the second outlet of the crude xenon tower is 99.999 percent, and the temperature is-90 ℃;
Step eight: in the step seven, a liquid phase outlet at the bottom of the crude xenon tower is connected with a first inlet of the recovery tower, the xenon content at the liquid phase outlet at the bottom of the crude xenon tower is 90%, and the temperature is-70 ℃;
step nine: in the seventh step, the raw material gas of the pure xenon tower is rectified by a xenon tower condenser and a heater, and after gasification and liquefaction for many times, the gas phase at the top of the pure xenon tower is liquefied by the xenon tower condenser and then flows back into the pure xenon tower, a liquid phase outlet at the bottom of the pure xenon tower is connected with a xenon gasifier through an eighth regulating valve, the purity of the xenon gas at the liquid phase outlet at the bottom of the pure xenon tower is 99.9998%, and the temperature is-86 ℃;
step ten: in the step eight, the raw material gas of the recovery tower is rectified by a xenon tower condenser and a heater, and after gasification and liquefaction are carried out for a plurality of times, the gas at the top of the recovery tower is partially liquefied by the xenon tower condenser and then flows back to a separator III, the gas phase of the separator III is discharged to the atmosphere by a seventh regulating valve, and the discharge capacity is 0.03Nm 3 And/h, the temperature is-115 ℃ and the pressure is 0.6MPa;
step eleven: in the step ten, the liquid phase outlet of the separator flows back into the recovery tower, the crude xenon is pumped in the recovery tower, the liquid phase outlet at the bottom of the recovery tower is discharged to the atmosphere, and the discharge amount is 0.04Nm 3 And/h, the temperature is-78 ℃ and the pressure is 0.6MPa;
step twelve: in the step ten, the recovery tower is pumped to a third inlet of the crude xenon tower, and the content of the pumped xenon is as follows: 89%, at-85 ℃;
Step thirteen: the mixed refrigerant III flows to a condenser at the top of the deoxidizing tower, the gas phase at the top of the condenser at the top of the deoxidizing tower is reheated by a main heat exchanger, the temperature of the mixed refrigerant III is minus 183 ℃, and the pressure is 0.65MPa;
step fourteen: delivering the re-heated gas in the thirteenth step to a back cooler through a third regulating valve to continuously recover cold energy, wherein the temperature of the re-heated gas is minus 69 ℃ and the pressure is 0.7MPa;
fifteen steps: the mixed refrigerant I reaches the condenser at the top of the krypton tower, and is liquefied and circulated through a ninth regulating valve and the condenser at the top of the deoxidizing tower, wherein the temperature of the mixed refrigerant I is minus 178 ℃ and the pressure is 0.4MPa;
step sixteen: and the mixed refrigerant II is liquefied by the condenser at the top of the krypton tower and then enters the condenser at the top of the xenon tower, the gas phase outlet of the condenser at the xenon tower enters the second inlet of the condenser at the top of the krypton tower through a tenth regulating valve and a third tee joint, and the mixed refrigerant II is circularly reciprocated, wherein the temperature of the mixed refrigerant II is minus 110 ℃, and the pressure of the mixed refrigerant is 0.3MPa.
The technical scheme of the invention at least comprises the following beneficial effects:
1. the invention adopts the novel mixed refrigerant to provide cold energy for each rectifying tower, and adopts the thermal coupling circulation process to supplement the refrigerant once, thereby meeting the whole process of krypton-xenon production without multiple supplementation;
2. The krypton-xenon production device of the invention firstly removes oxygen, simultaneously the tower top is rich in industrial oxygen, the tower bottom is deoxidized to produce crude krypton-xenon, the production of the industrial oxygen at the tower top can be regulated by variable load, and the sales requirement of the industrial oxygen in the market can be met;
3. the purity of the krypton-xenon product can reach more than 99.9998%, the dependence of the domestic electronic industry and the aerospace industry on imported high-purity krypton-xenon is solved, and sufficient raw materials are provided for the research of the domestic semiconductor industry, the electronic special gas industry and the aerospace industry, so that the development of economic and social benefits is promoted;
4. the invention has high integration of energy, specifically, the first mixed refrigerant and the second mixed refrigerant are respectively supplied to the condenser at the top of the pure krypton tower and the condenser at the top of the xenon tower for one time, so that the stable operation of the device can be satisfied all the time, and the whole production process does not need to be supplied again; after the mixed refrigerant III to the condenser at the top of the deoxidizing tower provide cold energy, the evaporated gas is reused by the main heat exchanger and the back cooler, so that the cold energy utilization rate is higher;
5. according to the invention, the purifier is arranged between the deoxidizing tower and the pure krypton tower, so that impurities in the krypton-xenon product are removed in the initial stage of rectification, the loads of the pure krypton tower, the crude xenon tower and the refined xenon tower are effectively reduced, and the investment cost of equipment is reduced;
6. The invention is provided with the recovery tower, all the discharged air of the krypton-xenon device is recovered, and after further rectification processing, useful krypton-xenon components are extracted to the crude xenon tower, so that the value of xenon products is further improved.
Drawings
FIG. 1 is a schematic diagram of a production system for producing a high purity krypton xenon product using a mixed refrigerant in accordance with the present invention;
FIG. 2 is a schematic diagram of the deoxidizing unit of the present invention
FIG. 3 is a schematic diagram of the structure of the krypton purification unit of the present invention;
FIG. 4 is a schematic diagram of the structure of the xenon purification unit of the present invention.
In the figure:
1. a main heat exchanger; 2. a deoxidizing tower; 3. an electric heater I; 4. a condenser at the top of the deoxidizing tower; 5. a first separator; 6. a purifier; 7. a pure krypton column; 8. a second electric heater; 9. a condenser at the top of the pure krypton column; 10. a second separator; 11. a crude xenon column; 12. a xenon column top condenser; 13. an electric heater III; 14. a pure xenon column; 15. an electric heater IV; 16. a recovery tower; 17. fifth electric heater; 18. a third separator; 19. an industrial oxygen storage tank; 20. a krypton vaporizer; 21. a xenon vaporizer; 22. a gas phase outlet at the top of the deoxidizing tower; 23. a second inlet of the deoxidizing tower; 24. a liquid phase outlet at the bottom of the deoxidizing tower; 25. a first inlet of a condenser at the top of the deoxidizing column; 26. a first outlet of the deoxidizing column top condenser; 27. an inlet of the separator I; 28. a separator gas phase outlet; 29. a second liquid phase outlet of the separator; 30. a first liquid phase outlet of the separator; 31. a first inlet for pure krypton; 32. a liquid phase outlet at the bottom of the pure krypton tower; 33. a gas phase outlet at the top of the pure krypton tower; 34. a third inlet of the condenser at the top of the pure krypton tower; 35. an evaporation gas outlet; 36. a krypton column top condenser second inlet; 37. a krypton column top condenser second outlet; 38. a fourth inlet of the krypton column condenser; 39. a first outlet of the krypton column top condenser; 40. a second inlet of the separator; 41. a separator two-gas phase outlet; 42. a second outlet of the separator; 43. a crude xenon column first inlet; 44. a liquid phase outlet at the bottom of the crude xenon column; 45. a gas phase outlet at the top of the crude xenon column; 46. a first inlet of a xenon tower condenser; 47. a first outlet of the xenon column condenser; 48. a crude xenon column second inlet; 49. a fourth inlet of the xenon tower condenser; 50. a crude xenon column second outlet; 51. a first inlet of the pure xenon tower; 52. a gas phase outlet at the top of the pure xenon column; 53. a second inlet of the xenon tower condenser; 54. a second outlet of the xenon tower condenser; 55. a second inlet of the pure xenon tower; 56. a third inlet of the crude xenon column; 57. a liquid phase outlet at the bottom of the pure xenon column; 58. a recovery column first inlet; 59. a gas phase outlet at the top of the recovery tower; 60. a third inlet of the xenon tower condenser; 61. a third outlet of the xenon tower condenser; 62. a third inlet of the separator; 63. a separator liquid phase outlet; 64. a recovery overhead vapor phase outlet; 65. a recovery column second inlet; 66. a liquid phase outlet at the bottom of the recovery tower; 67. a first regulating valve; 68. a fourth regulating valve; 69. a second regulating valve; 70. a third regulating valve; 71. an eleventh regulating valve; 72. a fifth regulating valve; 73. a ninth regulator valve; 74. a tenth regulating valve; 75. a seventh regulating valve; 76. a recooling device; 77. mixing a first refrigerant; 78. mixing a second refrigerant; 79. a primary heat exchanger first inlet; 80. a third inlet of the main heat exchanger; 81. a primary heat exchanger second inlet; 82. a primary heat exchanger first outlet; 83. a third outlet of the main heat exchanger; 84. a second outlet behind the primary heat exchanger; 85. a first tee; 86. a second tee; 87. a sixth regulating valve; 88. an eighth regulating valve; 89. a xenon tower condenser gas phase outlet; 90. a third tee; 91. a first inlet of a condenser at the top of the pure krypton column; 92. a second outlet of the separator; 93. an eleventh regulating valve; 94. a withdrawal port in the recovery tower; 95. a deoxygenated top condenser second inlet; 96. a deoxygenated top condenser second outlet; 97. mixing a third refrigerant; 98. a third inlet of the condenser at the top of the deoxidizing column; 99. a first inlet of the deoxidizing tower.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 4 of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which are obtained by a person skilled in the art based on the described embodiments of the invention, fall within the scope of protection of the invention.
Example 1
As shown in FIG. 1, a production system for producing a high-purity krypton-xenon product by using a mixed refrigerant comprises a high-purity krypton-xenon production device and a mixed refrigerant device for providing a cold source for the high-purity krypton-xenon production device. The high-purity krypton-xenon production device comprises a main heat exchanger 1 connected with an air source, a deoxidizing unit connected with an outlet of the main heat exchanger 1, a krypton production unit connected with the deoxidizing unit, a xenon production unit connected with a liquid outlet of the krypton production unit, and a recovery unit connected with the liquid outlet of the xenon production unit, wherein an outlet of the recovery unit is connected with the xenon production unit for recovering xenon. The mixed refrigerant device comprises a condenser for providing a cold source for the high-purity krypton-xenon production device, the mixed refrigerant is injected into the condenser, and comprises a mixed refrigerant I, a mixed refrigerant II and a mixed refrigerant III, wherein the mixed refrigerant I is liquid nitrogen, and the mixed refrigerant II is 80% CF 4 And 20% O 2 The third mixed refrigerant is CF 4 The mixed condensing agent provides a cold source for the deoxidizing unit, the krypton production unit and the xenon production unit respectively.
The deoxidizing unit comprises a deoxidizing tower 2 connected with the outlet of the main heat exchanger 1 through a pipeline, a purifier 6 connected with the liquid phase outlet 24 at the bottom of the deoxidizing tower through a pipeline, a first separator 5 connected with the gas phase outlet 22 at the top of the deoxidizing tower through a pipeline, a mixed refrigerant device connected with the first separator 5 and the gas phase outlet 22 at the top of the deoxidizing tower for providing a cold source, and a first liquid phase outlet 30 of the first separator connected with the second inlet 23 of the deoxidizing tower through a pipeline for refluxing condensed liquid.
The krypton production unit comprises a pure krypton column 7 connected to the outlet of the purifier 6 through a pipe, a second separator 10 connected to the gas phase outlet 33 at the top of the pure krypton column through a pipe, the liquid phase outlet 32 at the bottom of the pure krypton column is connected to the xenon production unit through a pipe, a mixed refrigerant device is connected to the second separator 10 and used for providing a cold source, and a first outlet 42 of the second separator is connected to the second inlet of the pure krypton column 7 through a pipe for refluxing condensed liquid.
The xenon production unit comprises a crude xenon tower 11 connected with a liquid phase outlet 32 at the bottom of the pure krypton tower through a pipeline, a pure xenon tower 14 connected with a second outlet 50 of the crude xenon tower through a pipeline, a gas phase outlet 45 at the top of the crude xenon tower and a gas phase outlet 52 at the top of the pure xenon tower are connected with a mixed refrigerant device through pipelines, the gas phase at the top of the crude xenon tower exchanges heat and then flows back fully, the purer xenon gas flows to an inlet of the pure xenon tower after rectifying the components, and the pure xenon product is obtained at the liquid phase outlet at the bottom of the pure xenon tower after the gas phase at the top of the pure xenon tower exchanges heat and then flows back fully.
The raw material gas is sequentially connected with a deoxidizing tower 2, a purifier 6, a pure krypton tower 7, a crude xenon tower 11, a pure xenon tower 14 and a recovery tower 16 after passing through the main heat exchanger 1. The mixed refrigerant cold supply system respectively provides energy for the main heat exchanger 1, the deoxidizing column top condenser 4, the pure krypton column top condenser 9, the xenon column top condenser 12 and the aftercooler 76. The bottom of the deoxidizing tower is provided with an electric heater I3, the bottom of the pure krypton tower is provided with an electric heater II 8, and a purifier 6 is arranged between the deoxidizing tower 2 and the pure krypton tower 7; the top of the deoxidizing tower 2 is provided with a first separator 5, one path of liquid in the first separator preferentially guarantees reflux, and the other path of liquid is rich in industrial oxygen; a first regulating valve 67 is arranged between the first outlet 82 of the raw material gas after exiting the main heat exchanger and the deoxidizing tower 2; a second regulating valve 69 is arranged between a second outlet 84 of the deoxidization tower top gas phase first tee joint 85 and the back cooler 76 after passing through the main heat exchanger; a third regulating valve 70 is arranged between the third outlet 83 of the evaporated nitrogen passing through the main heat exchanger and the aftercooler 76; the liquid phase outlet 24 at the bottom of the deoxidizing tower is connected with the purifier 6 through a fourth regulating valve 68; the raw gas is connected with a first inlet 79 of the main heat exchanger 1, a first outlet 82, a first regulating valve 67, a first inlet 99 of the deoxidizing tower 2, a gas phase outlet 22 at the top of the deoxidizing tower, a first tee joint 85, a first inlet 25 of a condenser 4 at the top of the deoxidizing tower, a first outlet 26 of a condenser 4 at the top of the deoxidizing tower, an inlet 27 of a separator, a first liquid phase outlet 30 of the separator and a second inlet 23 of the deoxidizing tower; the separator-second liquid phase outlet 29 is connected to the industrial oxygen tank 19 through an eleventh regulating valve 71; the deoxidizing column bottom liquid phase outlet 24 is connected with the pure krypton column first inlet 31 through a fourth regulating valve 68 and a purifier 6.
The top of the pure krypton tower 7 is provided with a second separator 10, one path of liquid in the second separator preferentially ensures reflux, and the other path of liquid produces a high-purity krypton product; the liquid phase outlet 32 at the bottom of the pure krypton tower is connected with the first inlet 43 of the crude xenon tower, after the crude xenon tower 11 is rectified, the gas phase outlet 45 of the crude xenon tower is connected with the first inlet 46 of the xenon tower condenser, after heat exchange, total reflux is carried out, after components are rectified, the purer xenon gas is connected with the inlet 55 of the pure xenon tower through the eleventh regulating valve 93; the pure xenon tower gas phase outlet 52 exchanges heat to the xenon tower condenser second inlet 53 and then is subjected to total reflux, and after rectification, a high-purity xenon product is obtained at the pure xenon tower bottom liquid phase outlet 57; the separator two gas phase outlet 41 is connected with a second tee 86 through a fifth regulating valve 72; the second outlet 92 of the second separator is connected with the krypton vaporizer 20 through a sixth regulating valve 87; the gas phase outlet 33 at the top of the pure krypton tower is connected with the first inlet 91 of the condenser at the top of the pure krypton tower, the first outlet 39 of the condenser at the top of the krypton tower, the second inlet 40 of the separator, the second gas phase outlet 41 of the separator, the second first outlet 42 of the separator and the fifth regulating valve 72 through the second tee joint 86; the pure krypton column bottom liquid phase outlet 32 is connected to a crude xenon column first inlet 43.
The liquid phase outlet 44 at the bottom of the crude xenon column is connected to the first inlet 58 of the recovery column, and the gas phase outlet 59 at the top of the recovery column is connected to the third inlet 60 of the xenon column condenser after heat exchange, and the third outlet 61 of the xenon column condenser is connected with the third first inlet 62 of the separator; the second outlet 50 of the crude xenon tower is connected with the first inlet 51 of the pure xenon tower through an eleventh regulating valve 93; the separator tri-gas vent is provided with a seventh regulating valve 75; the crude xenon column top gas phase outlet 45 is connected to a crude xenon column second inlet 48 through a xenon column condenser first inlet 46, a xenon column condenser first outlet 47; the second outlet 50 of the crude xenon tower is connected with the first inlet 51 of the pure xenon tower through an eleventh regulating valve 93; the crude xenon column bottom liquid phase outlet 44 is connected to the recovery column first inlet 58. The bottom of the crude xenon tower and the bottom of the pure xenon tower are respectively provided with an electric heater III 13 and an electric heater IV 15.
The gas phase outlet 52 at the top of the pure xenon tower is connected with the second inlet 55 of the pure xenon tower through the second inlet 53 of the xenon tower condenser and the second outlet 54 of the xenon tower condenser; the bottom liquid phase outlet 57 of the pure xenon column is connected with the xenon vaporizer 21 through an eighth regulating valve 88
The pure xenon bottom liquid phase outlet 57 is connected with the xenon vaporizer 21 through an eighth regulating valve 88; the gas phase outlet 35 of the krypton tower condenser is connected with the top condenser 4 of the deoxidizing tower through a ninth regulating valve 73; a tenth regulating valve 74 and a third tee 90 are respectively provided between the xenon column condenser gas phase outlet 89 and the krypton column top condenser second inlet 36.
The recovery unit comprises a recovery tower 46 connected with the liquid phase outlet 44 at the bottom of the crude xenon tower through a pipeline, a third separator 18 connected with the second inlet 65 of the recovery tower through a pipeline, and the gas phase outlet 59 at the top of the recovery tower is connected with the second inlet 65 of the recovery tower through a third inlet of the mixed refrigerant device, a third outlet of the mixed refrigerant device, a third inlet of the separator, and a liquid phase outlet 63 of the separator; the extraction outlet in the recovery tower 16 is connected with the third inlet of the crude xenon tower 11, and the third gas phase outlet of the separator is discharged to the atmosphere through a seventh regulating valve; the recovery column bottom liquid phase outlet 66 vents to atmosphere.
The recovery tower top gas phase outlet 59 is connected with the recovery tower second inlet 65 through the xenon tower condenser third inlet 60, the xenon tower condenser third outlet 61, the separator triple inlet 62 and the separator liquid phase outlet 63; the extraction port 94 in the recovery tower is connected with the third inlet 56 of the crude xenon tower, and the third gas phase outlet of the separator is discharged to the atmosphere through the seventh regulating valve 75; the recovery column bottom liquid phase outlet 66 vents to atmosphere.
The mixed refrigerant device comprises a deoxidizing column top condenser 4, a pure krypton column top condenser 9, a xenon column top condenser 12, a mixed refrigerant 77, a mixed refrigerant 78 and a mixed refrigerant 97, wherein the mixed refrigerant 77 is connected with a krypton column top condenser fourth inlet 38 through a pure krypton column top condenser third inlet 34, an evaporation gas outlet 35, a ninth regulating valve 73, a deoxidizing top condenser second inlet 95, a deoxidizing top condenser second outlet 96, and the mixed refrigerant 78 is connected with a deoxidizing column top condenser third inlet 98 through a krypton column top condenser second inlet 36, a krypton column top condenser second outlet 37, a xenon column condenser fourth inlet 49, a xenon column condenser gas phase outlet 89, a tenth regulating valve 74, a third tee 90 and the krypton column top condenser second inlet 36, the mixed refrigerant 97 is connected with a deoxidizing column top condenser top gas phase to a main heat exchanger third inlet 80, and a third regulating valve 70.
A production process for producing high-purity krypton-xenon commodity by adopting mixed refrigerant comprises the following steps:
step one, after heat exchange of the raw material gas through the main heat exchanger 1, the raw material gas enters the deoxidizing tower 2 through the first regulating valve 67, and is rectified through the first electric heater 3 of the tower kettle and the condenser 4 at the top of the deoxidizing tower, wherein the temperature of the raw material gas is 20-30 ℃, and the pressure is: 0.65Mpa, the flow is: 800Nm/h, gas phase fraction: 1, the content of krypton and xenon is 1000ppm and 20ppm respectively;
Step two, enabling gas phase after primary rectification purification of the raw material gas entering the deoxidizing tower 2 in the step one to enter a deoxidizing tower top condenser 4 and a main heat exchanger 1 respectively through a first tee joint 85, recycling part of cold energy through the main heat exchanger 1, a third regulating valve 70 to a back cooler 76, and enabling crude krypton-xenon liquid at the deoxidizing tower bottom to enter a purifier 6 through a fourth regulating valve 68; the temperature of the crude krypton-xenon liquid at the bottom of the deoxidizing tower is minus 129.5 ℃, and the mole fraction of krypton-xenon is 99.97%;
step three, in the step two, the gas phase enters the top condenser 4 of the deoxidizing tower through the first tee joint 85 and is liquefied and then enters the first separator 5, the liquid phase outlet 30 at the bottom of the first separator flows back to the second inlet 23 of the deoxidizing tower, and the liquid phase outlet 29 at the second separator flows to the industrial oxygen storage tank 19 through the eleventh regulating valve 71; the liquid phase temperature of the industrial oxygen is-164 ℃, and the molar purity is 99.97%;
step four, the crude krypton-xenon liquid in the deoxidizing tower kettle in the step two is connected with a purifier 6 through a fourth regulating valve 68, the gas phase of the outlet of the purifier is discharged into a pure krypton tower 7, the outlet temperature of the purifier is 30-35 ℃, and the mole fraction of the krypton-xenon is 99.995%;
step five, rectifying the raw material gas of the pure krypton tower 7 in the step four through a condenser 9 at the top of the pure krypton tower and a second electric heater 8, liquefying the gas phase of the pure krypton tower top through the condenser 9 at the top of the pure krypton tower for multiple times, returning the liquefied gas phase into the second separator 10, and a liquid phase outlet 42 at the bottom of the second separator back to the pure krypton tower 7, wherein a second liquid phase outlet 92 of the second separator is connected with a krypton vaporizer 20 through a fifth regulating valve 87, and the purity of the krypton gas at the inlet of the krypton vaporizer 20 is 99.9996%;
Step six, in the step five, the liquid phase outlet 32 at the bottom of the pure krypton tower is connected with the first inlet 43 of the crude xenon tower, and the xenon content of the liquid phase outlet 44 at the bottom of the pure krypton tower is 99.95%;
step seven, rectifying raw material gas of the crude xenon tower in the step six through a xenon tower condenser 12 and a heater III 13, liquefying a gas phase of the top of the crude xenon tower through the xenon tower condenser 12 after multiple times of gasification and liquefaction, refluxing the liquefied gas phase of the top of the crude xenon tower into the crude xenon tower 11, enabling a second outlet 50 of the crude xenon tower to enter a pure xenon tower 14 through an eleventh regulating valve 93, wherein the gas phase xenon content of the second outlet 50 of the crude xenon tower is 99.999 percent, and the temperature is-90 ℃;
step eight, in step seven, the liquid phase outlet 44 at the bottom of the crude xenon tower is connected with the first inlet 58 of the recovery tower, the xenon content of the liquid phase outlet 44 at the bottom of the crude xenon tower is 90 percent, and the temperature is-70 ℃;
step nine, rectifying the raw material gas of the pure xenon tower in step seven through a xenon tower condenser 12 and a heater IV 15, liquefying the gas phase of the top of the pure xenon tower through the xenon tower condenser 12 after multiple times of gasification and liquefaction, and refluxing the liquefied gas phase of the top of the pure xenon tower into the pure xenon tower 14, wherein a liquid phase outlet 57 of the bottom of the pure xenon tower is connected with a xenon gasifier 21 through an eighth regulating valve 88, the purity of xenon at the liquid phase outlet 57 of the bottom of the pure xenon tower is 99.9996%, and the temperature is-86 ℃;
step ten, rectifying the raw material gas of the recovery tower in step eight through a xenon tower condenser 12 and a heater five 17, liquefying the recovered tower top gas through partial liquefaction of the xenon tower condenser 12 for multiple times, refluxing the liquefied gas into a third separator 18, discharging the gas phase outlet 64 of the third separator to the atmosphere through a seventh regulating valve 75, and discharging the gas with the gas volume of 0.05-0.1 Nm 3 And/h, the temperature is-112 ℃ and the pressure is 0.6MPa;
reflux of the third liquid phase outlet 63 of the separator in the eleventh and tenth steps to the first inlet 65 of the recovery tower, removal of the crude xenon tower 11 by the extraction opening 94 in the recovery tower, discharge of the liquid phase outlet 66 at the bottom of the recovery tower to the atmosphere, and discharge of 0.04Nm 3 And/h, the temperature is-78 to-75 ℃, and the pressure is 0.6MPa;
step twelve, pumping air in the recovery tower to the third inlet 56 of the crude xenon tower, wherein the content of the pumped air xenon is 88%, and the temperature is-85 ℃;
thirteen, mixing the refrigerant III 97 to a top condenser 4 of the deoxidizing tower, wherein the gas phase at the top of the top condenser 4 of the deoxidizing tower is reheated by a main heat exchanger 1, and the temperature of the refrigerant III 97 is-181 ℃ and the pressure is 0.65MPa;
the gas reheated by the main heat exchanger in the fourteen and thirteenth steps is sent to a back cooler 76 through a third regulating valve 70 to continuously recover cold energy, the temperature of the reheated gas is-67 ℃, and the pressure is 0.68MPa;
fifteen, mixing the first refrigerant 77 to the condenser 9 at the top of the krypton tower, and liquefying and circulating the first refrigerant 77 at the temperature of minus 175 ℃ and the pressure of 0.38-0.4 MPa through a ninth regulating valve 73 and a condenser 4 at the top of the deoxidizing tower;
sixteenth, liquefying the mixed refrigerant II 78 to the krypton tower top condenser 9, then liquefying the mixed refrigerant II to the xenon tower top condenser 12, and enabling a gas phase outlet 89 of the xenon tower condenser to enter a second inlet 36 of the krypton tower top condenser through a tenth regulating valve 74 and a third tee 90, wherein the mixed refrigerant II 78 is circularly reciprocated, and the temperature of the mixed refrigerant II 78 is minus 108 ℃ and the pressure of the mixed refrigerant II is 0.28MPa.
Example 2
A production process for producing high-purity krypton-xenon commodity by adopting mixed refrigerant comprises the following steps:
step one, after heat exchange of the raw material gas through the main heat exchanger 1, the raw material gas enters the deoxidizing tower 2 through the first regulating valve 67, and is rectified through the first electric heater 3 of the tower kettle and the condenser 4 at the top of the deoxidizing tower, wherein the temperature of the raw material gas is 20-30 ℃, and the pressure is: 0.65Mpa, the flow is: 800Nm/h, gas phase fraction: 1, the contents of krypton and xenon are 1500ppm and 100ppm respectively;
step two, enabling gas phase after primary rectification purification of the raw material gas entering the deoxidizing tower 2 in the step one to enter a deoxidizing tower top condenser 4 and a main heat exchanger 1 respectively through a first tee joint 85, recycling part of cold energy through the main heat exchanger 1, a third regulating valve 70 to a back cooler 76, and enabling crude krypton-xenon liquid at the deoxidizing tower bottom to enter a purifier 6 through a fourth regulating valve 68; the temperature of the crude krypton-xenon liquid at the bottom of the deoxidizing tower is-129.3 ℃, and the mole fraction of the krypton-xenon is 99.98%;
step three, in the step two, the gas phase enters the top condenser 4 of the deoxidizing tower through the first tee joint 85 and is liquefied and then enters the first separator 5, the liquid phase outlet 30 at the bottom of the first separator flows back to the second inlet 23 of the deoxidizing tower, and the liquid phase outlet 29 at the second separator flows to the industrial oxygen storage tank 19 through the eleventh regulating valve 71; the liquid phase temperature of the industrial oxygen is-165 ℃ and the molar purity is 99.98 percent;
Step four, the crude krypton-xenon liquid in the deoxidizing tower kettle in the step two is connected with a purifier 6 through a fourth regulating valve 68, the gas phase of the outlet of the purifier is discharged into a pure krypton tower 7, the outlet temperature of the purifier is 30-35 ℃, and the mole fraction of the krypton-xenon is 99.997%;
step five, rectifying the raw material gas of the pure krypton tower 7 in the step four through a condenser 9 at the top of the pure krypton tower and a second electric heater 8, liquefying the gas phase of the pure krypton tower top through the condenser 9 at the top of the pure krypton tower for multiple times, returning the liquefied gas phase into the second separator 10, and a liquid phase outlet 42 at the bottom of the second separator back to the pure krypton tower 7, wherein a second liquid phase outlet 92 of the second separator is connected with a krypton vaporizer 20 through a fifth regulating valve 87, and the purity of the krypton gas at an inlet of the krypton vaporizer 20 is 99.9997%;
step six, in the step five, the liquid phase outlet 32 at the bottom of the pure krypton tower is connected with the first inlet 43 of the crude xenon tower, and the xenon content of the liquid phase outlet 44 at the bottom of the pure krypton tower is 99.97%;
step seven, rectifying raw material gas of the crude xenon tower in the step six through a xenon tower condenser 12 and a heater III 13, liquefying a gas phase of the top of the crude xenon tower through the xenon tower condenser 12 after multiple times of gasification and liquefaction, refluxing the liquefied gas phase of the top of the crude xenon tower into the crude xenon tower 11, enabling a second outlet 50 of the crude xenon tower to enter a pure xenon tower 14 through an eleventh regulating valve 93, wherein the content of the gas phase xenon gas at the second outlet 50 of the crude xenon tower is 99.9993 percent, and the temperature is-89.5 ℃;
Step eight, in step seven, the liquid phase outlet 44 at the bottom of the crude xenon tower is connected with the first inlet 58 of the recovery tower, the xenon content of the liquid phase outlet 44 at the bottom of the crude xenon tower is 95%, and the temperature is-69.5 ℃;
step nine, rectifying the raw material gas of the pure xenon tower in step seven through a xenon tower condenser 12 and a heater IV 15, liquefying the gas phase of the top of the pure xenon tower through the xenon tower condenser 12 after multiple times of gasification and liquefaction, and refluxing the liquefied gas phase of the top of the pure xenon tower into the pure xenon tower 14, wherein a liquid phase outlet 57 of the bottom of the pure xenon tower is connected with a xenon gasifier 21 through an eighth regulating valve 88, the purity of xenon at the liquid phase outlet 57 of the bottom of the pure xenon tower is 99.9997%, and the temperature is-85.5 ℃;
step ten, the raw material gas of the recovery tower in the step eight is rectified by a xenon tower condenser 12 and a heater five 17,after gasification and liquefaction for multiple times, the recovered tower top gas is partially liquefied by the xenon tower condenser 12 and then flows back to the third separator 18, the third gas phase outlet 64 of the separator is discharged to the atmosphere through the seventh regulating valve 75, and the discharge amount is 0.05-0.1 Nm 3 And/h, the temperature is-113 ℃, and the pressure is 0.6MPa;
reflux of the third liquid phase outlet 63 of the separator in the eleventh and tenth steps to the first inlet 65 of the recovery tower, removal of the crude xenon tower 11 by the extraction opening 94 in the recovery tower, discharge of the liquid phase outlet 66 at the bottom of the recovery tower to the atmosphere, and discharge of 0.06Nm 3 And/h, the temperature is-76 ℃ and the pressure is 0.6MPa;
Step twelve, pumping air in the recovery tower to a third inlet 56 of the crude xenon tower, wherein the content of the pumped air xenon is 89%, and the temperature is-84 ℃;
thirteen, mixing the refrigerant III 97 to a top condenser 4 of the deoxidizing tower, wherein the gas phase at the top of the top condenser 4 of the deoxidizing tower is reheated by a main heat exchanger 1, and the temperature of the mixed refrigerant III 97 is-182 ℃ and the pressure is 0.66MPa;
the gas reheated by the main heat exchanger in the fourteen and thirteenth steps is sent to a back cooler 76 through a third regulating valve 70 to continuously recover cold energy, the temperature of the reheated gas is minus 68 ℃, and the pressure is 0.69MPa;
fifteen, mixing the first refrigerant 77 to the krypton tower top condenser 9, and liquefying and circulating the mixed refrigerant 77 through a ninth regulating valve 73 and a deoxidizing tower top condenser 4, wherein the temperature of the mixed refrigerant 77 is-177 ℃ and the pressure is 0.39MPa;
sixteenth, liquefying the mixed refrigerant II 78 to the krypton tower top condenser 9, then liquefying the mixed refrigerant II to the xenon tower top condenser 12, and enabling a gas phase outlet 89 of the xenon tower condenser to enter a second inlet 36 of the krypton tower top condenser through a tenth regulating valve 74 and a third tee 90, wherein the mixed refrigerant II 78 is circularly reciprocated, and the temperature is minus 109 ℃ and the pressure is 0.29MPa.
Example 3
A production process for producing high-purity krypton-xenon commodity by adopting mixed refrigerant comprises the following steps:
Step one, after heat exchange of the raw material gas through the main heat exchanger 1, the raw material gas enters the deoxidizing tower 2 through the first regulating valve 67, and is rectified through the first electric heater 3 of the tower kettle and the condenser 4 at the top of the deoxidizing tower, wherein the temperature of the raw material gas is 20-30 ℃, and the pressure is: 0.65Mpa, the flow is: 800Nm/h, gas phase fraction: 1, the content of krypton and xenon is 2000ppm and 200ppm respectively;
step two, enabling gas phase after primary rectification purification of the raw material gas entering the deoxidizing tower 2 in the step one to enter a deoxidizing tower top condenser 4 and a main heat exchanger 1 respectively through a first tee joint 85, recycling part of cold energy through the main heat exchanger 1, a third regulating valve 70 to a back cooler 76, and enabling crude krypton-xenon liquid at the deoxidizing tower bottom to enter a purifier 6 through a fourth regulating valve 68; the temperature of the crude krypton-xenon liquid at the bottom of the deoxidizing tower is-129.3 ℃, and the mole fraction of the krypton-xenon is 99.99%;
step three, in the step two, the gas phase enters the top condenser 4 of the deoxidizing tower through the first tee joint 85 and is liquefied and then enters the first separator 5, the liquid phase outlet 30 at the bottom of the first separator flows back to the second inlet 23 of the deoxidizing tower, and the liquid phase outlet 29 at the second separator flows to the industrial oxygen storage tank 19 through the eleventh regulating valve 71; the liquid phase temperature of the industrial oxygen is-165 ℃ and the molar purity is 99.99 percent;
Step four, the crude krypton-xenon liquid in the deoxidizing tower kettle in the step two is connected with a purifier 6 through a fourth regulating valve 68, the gas phase of the outlet of the purifier enters a pure krypton tower 7, the outlet temperature of the purifier is 30-35 ℃, and the mole fraction of the krypton-xenon is 99.999%;
step five, rectifying the raw material gas of the pure krypton tower 7 in the step four through a condenser 9 at the top of the pure krypton tower and a second electric heater 8, liquefying the gas phase of the pure krypton tower top through the condenser 9 at the top of the pure krypton tower for multiple times, returning the liquefied gas phase into the second separator 10, and a liquid phase outlet 42 at the bottom of the second separator back to the pure krypton tower 7, wherein a second liquid phase outlet 92 of the second separator is connected with a krypton vaporizer 20 through a fifth regulating valve 87, and the purity of the krypton gas at the inlet of the krypton vaporizer 20 is 99.9998%;
step six, in the step five, the liquid phase outlet 32 at the bottom of the pure krypton tower is connected with the first inlet 43 of the crude xenon tower, and the xenon content of the liquid phase outlet 44 at the bottom of the pure krypton tower is 99.98%;
step seven, rectifying raw material gas of the crude xenon tower in the step six through a xenon tower condenser 12 and a heater III 13, liquefying a gas phase of the top of the crude xenon tower through the xenon tower condenser 12 after multiple times of gasification and liquefaction, and refluxing the liquefied gas phase of the top of the crude xenon tower into the crude xenon tower 11, wherein a second outlet 50 of the crude xenon tower enters the pure xenon tower 14 through an eleventh regulating valve 93, and the gas phase xenon content of the second outlet 50 of the crude xenon tower is 99.9995 percent, and the temperature is minus 89 ℃;
Step eight, in step seven, the liquid phase outlet 44 at the bottom of the crude xenon tower is connected with the first inlet 58 of the recovery tower, the xenon content of the liquid phase outlet 44 at the bottom of the crude xenon tower is 99.92%, and the temperature is-69 ℃;
step nine, rectifying the raw material gas of the pure xenon tower in step seven through a xenon tower condenser 12 and a heater IV 15, liquefying the gas phase of the top of the pure xenon tower through the xenon tower condenser 12 after multiple times of gasification and liquefaction, and refluxing the liquefied gas phase of the top of the pure xenon tower into the pure xenon tower 14, wherein a liquid phase outlet 57 at the bottom of the pure xenon tower is connected with a xenon gasifier 21 through an eighth regulating valve 88, the purity of xenon at the liquid phase outlet 57 at the bottom of the pure xenon tower is 99.9998%, and the temperature is-85 ℃;
step ten, rectifying the raw material gas of the recovery tower in step eight through a xenon tower condenser 12 and a heater five 17, liquefying the recovered tower top gas through partial liquefaction of the xenon tower condenser 12 for multiple times, refluxing the liquefied gas into a third separator 18, discharging the gas phase outlet 64 of the third separator to the atmosphere through a seventh regulating valve 75, and discharging the gas with the gas volume of 0.05-0.1 Nm 3 And/h, the temperature is-115 ℃ and the pressure is 0.6MPa;
reflux of the third liquid phase outlet 63 of the separator in the eleventh and tenth steps to the first inlet 65 of the recovery tower, removal of the crude xenon tower 11 by the extraction opening 94 in the recovery tower, discharge of the liquid phase outlet 66 at the bottom of the recovery tower to the atmosphere, and discharge of 0.1Nm 3 And/h, the temperature is-75 ℃ and the pressure is 0.6MPa;
Step twelve, pumping air in the recovery tower to a third inlet 56 of the crude xenon tower in the step ten, wherein the content of the pumped air xenon is 90%, and the temperature is-83 ℃;
thirteen, mixing the refrigerant III 97 to a top condenser 4 of the deoxidizing tower, wherein the gas phase at the top of the top condenser 4 of the deoxidizing tower is reheated by a main heat exchanger 1, and the temperature of the mixed refrigerant III 97 is minus 183 ℃ and the pressure is 0.68MPa;
the gas reheated by the main heat exchanger in the fourteen and thirteenth steps is sent to a back cooler 76 through a third regulating valve 70 to continuously recover cold energy, the temperature of the reheated gas is-70 ℃, and the pressure is 0.7MPa;
fifteen, mixing the first refrigerant 77 to the krypton tower top condenser 9, and liquefying and circulating the mixed refrigerant 77 through a ninth regulating valve 73 and a deoxidizing tower top condenser 4, wherein the temperature of the mixed refrigerant 77 is minus 178 ℃ and the pressure is 0.4Pa;
sixteenth, liquefying the mixed refrigerant II 78 to the krypton tower top condenser 9, then liquefying the mixed refrigerant II to the xenon tower top condenser 12, and enabling a gas phase outlet 89 of the xenon tower condenser to enter a second inlet 36 of the krypton tower top condenser through a tenth regulating valve 74 and a third tee 90, wherein the mixed refrigerant II 78 is circularly reciprocated, and the temperature of the mixed refrigerant II 78 is minus 110 ℃ and the pressure of the mixed refrigerant II is 0.3MPa.
The foregoing is a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention and are intended to be comprehended within the scope of the present invention.

Claims (7)

1. The production system for producing the high-purity krypton-xenon product by adopting the mixed refrigerant is characterized by comprising a high-purity krypton-xenon production device and a mixed refrigerant device for providing a cold source for the high-purity krypton-xenon production device;
the high-purity krypton-xenon production device comprises a main heat exchanger connected with an air source, a deoxidizing unit connected with an outlet of the main heat exchanger, a krypton production unit connected with the deoxidizing unit, a xenon production unit connected with a liquid outlet of the krypton production unit, and a recovery unit connected with the liquid outlet of the xenon production unit, wherein an outlet of the recovery unit is connected with the xenon production unit and used for recovering xenon;
the mixed refrigerant device comprises a condenser for providing a cold source for the high-purity krypton-xenon production device, wherein mixed refrigerant is injected into the condenser, the mixed refrigerant comprises a mixed refrigerant I, a mixed refrigerant II and a mixed refrigerant III, the mixed refrigerant I is liquid nitrogen, and the mixed refrigerant II is 80% CF 4 And 20% O 2 The third mixed refrigerant is CF 4 The mixed condensing agent provides a condensing source for the deoxidizing unit, the krypton production unit and the xenon production unit respectively.
2. The production system for producing a high-purity krypton-xenon product using a mixed refrigerant according to claim 1, wherein the deoxidizing unit comprises a deoxidizing column connected to an outlet of the main heat exchanger through a pipe, a purifier connected to a liquid phase outlet of a bottom of the deoxidizing column through a pipe, a first separator connected to a gas phase outlet of a top of the deoxidizing column through a pipe, and the mixed refrigerant device is connected to the first separator and the gas phase outlet of the top of the deoxidizing column for providing a cold source, and a first liquid phase outlet of the separator is connected to a second inlet of the deoxidizing column through a pipe for refluxing condensed liquid.
3. The production system for producing a high-purity krypton-xenon product by using a mixed refrigerant according to claim 1, wherein the krypton production unit comprises a pure krypton column connected to an outlet of the deoxidizing unit through a pipe, a second separator connected to a gas phase outlet of the top of the pure krypton column through a pipe, a liquid phase outlet of the bottom of the pure krypton column is connected to the xenon production unit through a pipe, the mixed refrigerant device is connected to the second separator and is used for providing a cold source, and a first outlet of the second separator is connected to a second inlet of the pure krypton column through a pipe and is used for refluxing condensed liquid.
4. The production system for producing high-purity krypton-xenon products by using a mixed refrigerant according to claim 1, wherein the xenon production unit comprises a crude xenon column connected with the krypton production unit through a pipeline, a pure xenon column connected with a second outlet of the crude xenon column through a pipeline, a gas phase outlet at the top of the crude xenon column and a gas phase outlet at the top of the pure xenon column are connected with the mixed refrigerant device through pipelines, the gas phase at the top of the crude xenon column exchanges heat and then flows back fully, after components are exchanged by rectification, relatively pure xenon gas flows to an inlet of the pure xenon column, and after the gas phase at the top of the pure xenon column exchanges heat and then flows back fully, and after rectification, the high-purity xenon products are obtained at a liquid phase outlet at the bottom of the pure xenon column.
5. The production system for producing high-purity krypton-xenon products by using a mixed refrigerant according to claim 1, wherein the recovery unit comprises a recovery tower connected with a liquid phase outlet at the bottom of the crude xenon tower through a pipeline, and a third separator connected with a second inlet of the recovery tower through a pipeline, and a gas phase outlet at the top of the recovery tower is connected with the second inlet of the recovery tower through a third inlet of the mixed refrigerant device, a third outlet of the mixed refrigerant device, a third inlet of the separator, and a liquid phase outlet of the separator; the extraction outlet in the recovery tower is connected with the third inlet of the crude xenon tower, and the third gas phase outlet of the separator is discharged to the atmosphere through a seventh regulating valve; the liquid phase outlet at the bottom of the recovery tower is discharged to the atmosphere.
6. The production system for producing high-purity krypton-xenon product by using mixed refrigerant according to claim 1, wherein the mixed refrigerant device comprises a deoxidizing column top condenser, a pure krypton column top condenser, a xenon column top condenser, a mixed refrigerant I, a mixed refrigerant II and a mixed refrigerant III, wherein the externally-supplemented mixed refrigerant I is connected with the krypton column condenser fourth inlet through the pure krypton column top condenser third inlet, an evaporation gas outlet, a ninth regulating valve, a deoxidizing top condenser second inlet, a deoxidizing top condenser second outlet, and the externally-supplemented mixed refrigerant II is connected with the krypton column condenser fourth inlet through the krypton column top condenser second inlet, the krypton column top condenser second outlet, the xenon column condenser fourth inlet, a xenon column condenser gas phase outlet, a tenth regulating valve, a third tee joint is connected with the krypton column top condenser second inlet, the externally-supplemented mixed refrigerant III is connected with the deoxidizing column top condenser third inlet, and the deoxidizing column top condenser top gas phase is connected with the main heat exchanger third inlet, and the third regulating valve is connected with the regenerator.
7. The production process for producing the high-purity krypton-xenon product by adopting the mixed refrigerant is characterized by comprising the following steps of:
step one, after heat exchange of a main heat exchanger, raw material gas enters a deoxidizing tower through a first regulating valve, and heat and cold rectification are respectively provided by a tower kettle electric heater I and a deoxidizing tower top condenser, wherein the temperature of the raw material gas is 20-30 ℃, the pressure is 0.65Mpa, the flow is 800Nm/h, the gas phase fraction is 1, and the krypton and xenon contents are 1000-2000 ppm and 20-200 ppm respectively;
step two, enabling the gas phase after primary rectification purification of the raw material liquid entering the deoxidizing tower in the step one to enter a condenser at the top of the deoxidizing tower and a main heat exchanger respectively through a first tee joint, recycling part of cold energy through the main heat exchanger, and then enabling the cold energy to enter a back cooler, and enabling crude krypton-xenon liquid at the bottom of the deoxidizing tower to enter a purifier; the temperature of the crude krypton-xenon liquid at the bottom of the deoxidizing tower is minus 129.2 to minus 129.5 ℃, and the mole fraction of the krypton-xenon is 99.97 to 99.99 percent;
step three, the gas phase in the step two enters a condenser at the top of the deoxidizing tower through a first tee joint to be liquefied and then enters a first separator, a liquid phase outlet at the bottom of the first separator flows back to a second inlet of the deoxidizing tower, and a second liquid phase outlet of the first separator flows to an industrial oxygen storage tank through an eleventh regulating valve; the liquid phase temperature of the industrial oxygen is-164 to-166 ℃, and the molar purity is not lower than 99.98%;
Step four, the crude krypton-xenon liquid in the deoxidizing tower kettle in the step two is connected with a purifier through a fourth regulating valve, and the gas phase of the outlet of the purifier is discharged into the pure krypton tower; the outlet temperature of the purifier is 30 to minus 35 ℃, and the mole fraction of krypton and xenon is 99.995 to 99.999 percent;
step five, rectifying the raw material gas of the pure krypton tower in the step four through a condenser at the top of the pure krypton tower and an electric heater II, liquefying the gas phase of the pure krypton tower top through the condenser at the top of the pure krypton tower for multiple times, returning the liquefied gas phase into the separator II, and returning the liquid phase outlet at the bottom of the separator II to the pure krypton tower, wherein the second liquid phase outlet of the separator II is connected with a krypton vaporizer through a fifth regulating valve, and the purity of the krypton gas at the inlet of the krypton vaporizer is 99.9998%;
step six, a liquid phase outlet at the bottom of the pure krypton tower in the step five is connected with a first inlet of a crude xenon tower;
step seven, rectifying the raw material gas of the crude xenon tower in the step six through a xenon tower condenser and a heater, liquefying the gas phase of the top of the crude xenon tower through the condenser at the top of the xenon tower after gasifying and liquefying for many times, and refluxing the gas phase into the crude xenon tower, wherein a second outlet of the crude xenon tower enters the pure xenon tower through an eleventh regulating valve;
step eight, a liquid phase outlet at the bottom of the crude xenon tower in the step seven is connected with a first inlet of a recovery tower, the xenon content at the liquid phase outlet at the bottom of the crude xenon tower is 90%, and the temperature is-70 ℃;
Step nine, rectifying the raw material gas of the pure xenon tower in the step seven through a xenon tower condenser and a heater, liquefying the gas phase at the top of the pure xenon tower through the xenon tower condenser after gasifying and liquefying for many times, and refluxing the gas phase into the pure xenon tower, wherein a liquid phase outlet at the bottom of the pure xenon tower is connected with a xenon gasifier through an eighth regulating valve;
step ten, rectifying the raw material gas of the recovery tower in the step eight through a xenon tower condenser and a heater, liquefying the raw material gas of the recovery tower through multiple times of gasification, and refluxing the liquefied gas of the recovery tower top into a separator III through the partial liquefaction of the xenon tower condenser, wherein the gas phase of the separator III is discharged to the atmosphere through a seventh regulating valve, and the discharge capacity is 0.03Nm 3 And/h, the temperature is-115 ℃ and the pressure is 0.6MPa;
step eleven, the liquid phase outlet of the separator in the step ten flows back into the recovery tower, the gas in the recovery tower is pumped to remove coarse xenon, the liquid phase outlet at the bottom of the recovery tower is discharged to the atmosphere, and the discharge amount is 0.04Nm 3 And/h, the temperature is-78 ℃ and the pressure is 0.6MPa;
step twelve, pumping air from the recovery tower to a third inlet of the crude xenon tower in the step ten, wherein the content of the pumped xenon is 89%, and the temperature is-85 ℃;
thirteenth step, the mixed refrigerant III reaches a top condenser of the deoxidization tower, the top gas phase of the top condenser of the deoxidization tower is reheated by a main heat exchanger, the temperature of the mixed refrigerant III is minus 183 ℃, and the pressure is 0.65MPa;
Fourteen, delivering the re-heated gas in the thirteenth step to a back cooler through a third regulating valve to continuously recover cold energy, wherein the temperature of the re-heated gas is-69 ℃ and the pressure is 0.7MPa;
fifteen, the mixed refrigerant I reaches the condenser at the top of the krypton tower, and the mixed refrigerant I is liquefied and circulated through a ninth regulating valve and the condenser at the top of the deoxidizing tower, wherein the temperature of the mixed refrigerant I is minus 178 ℃ and the pressure is 0.4MPa;
sixthly, liquefying the mixed refrigerant II to the condenser at the top of the krypton tower and then to the condenser at the top of the xenon tower, wherein a gas phase outlet of the condenser at the xenon tower enters a second inlet of the condenser at the top of the krypton tower through a tenth regulating valve and a third tee joint, and the mixed refrigerant II is circularly reciprocated, wherein the temperature of the mixed refrigerant II is minus 110 ℃, and the pressure is 0.3MPa.
CN202310488889.1A 2023-04-28 2023-04-28 Production system and process for producing high-purity krypton-xenon product by adopting mixed refrigerant Pending CN116518646A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117379973A (en) * 2023-12-11 2024-01-12 中船重工天禾船舶设备江苏有限公司 Refrigerant detects integrated recovery unit

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117379973A (en) * 2023-12-11 2024-01-12 中船重工天禾船舶设备江苏有限公司 Refrigerant detects integrated recovery unit
CN117379973B (en) * 2023-12-11 2024-03-29 中船重工天禾船舶设备江苏有限公司 Refrigerant detects integrated recovery unit

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