CN212390705U - Rare gas krypton-xenon refining and ultra-pure oxygen production device - Google Patents
Rare gas krypton-xenon refining and ultra-pure oxygen production device Download PDFInfo
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- CN212390705U CN212390705U CN202021412388.3U CN202021412388U CN212390705U CN 212390705 U CN212390705 U CN 212390705U CN 202021412388 U CN202021412388 U CN 202021412388U CN 212390705 U CN212390705 U CN 212390705U
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- 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
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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
- F25J3/04757—Producing pure krypton and/or xenon recovered from a crude krypton/xenon mixture using a hybrid system, e.g. using adsorption, permeation or catalytic reaction
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- 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
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
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- 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
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- 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
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- 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
- F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
- F25J2215/52—Oxygen production with multiple purity O2
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- 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
- F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
- F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2
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- 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
- F25J2220/00—Processes or apparatus involving steps for the removal of impurities
- F25J2220/50—Separating low boiling, i.e. more volatile components from oxygen, e.g. N2, Ar
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- 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
- F25J2220/00—Processes or apparatus involving steps for the removal of impurities
- F25J2220/52—Separating high boiling, i.e. less volatile components from oxygen, e.g. Kr, Xe, Hydrocarbons, Nitrous oxides, O3
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- 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
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- 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
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Abstract
The utility model belongs to a rare gas krypton-xenon refining and ultra-pure oxygen production device; the device comprises a liquid oxygen storage tank and a nitrogen circulating compressor, wherein the liquid oxygen storage tank is connected with a primary concentration tower through a liquid oxygen pump and a low-temperature adsorption tower; the liquid phase outlet at the bottom 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 is connected with a krypton-xenon separation tower for storing and separating krypton and xenon sequentially through a tube pass of a recooling device, a secondary concentration tower, a krypton-xenon deoxygenation tower and a gas heating device, 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 filling system through a second valve; the method has the advantages of simple structure, reasonable flow design, relatively low cost, safe operation, high yield, high purity of rare gas, economy, energy conservation, wide application range and capability of effectively classifying and recovering oxygen on the premise of effectively preparing krypton and xenon.
Description
Technical Field
The utility model belongs to the technical field of air cryogenic separation, specifically be a rare gas krypton xenon refines and super pure oxygen's apparatus for producing.
Background
Krypton and xenon are used as rare gases and widely applied to the fields of illumination, space satellites, medical industry and the like. Air is the main source of these rare gases, with 1.14ppm krypton and 0.086ppm xenon in the air, krypton and xenon being extracted mainly from the by-products of the air separation plant.
With the development of large-scale air separation plants, the extraction of rare gases from large-scale air separation plants has enormous economic value. There are generally two ways of conventional krypton-xenon extraction: external compression process air mainly for producing oxygen productsPerforming preconcentration of krypton and xenon by using liquid oxygen as a raw material; the other is an air separation device with a compression flow in a liquid oxygen pump, because a large amount of liquid oxygen is pumped out from a condensation evaporator, the krypton-xenon concentrate cannot be extracted from the liquid oxygen, and krypton and xenon preconcentration is carried out by taking oxygen-rich liquid air as a raw material. The liquid oxygen/oxygen-enriched liquid has an excessively high content of hydrocarbons (typically methane CH)4Meaning that no more than 0.5%) is extremely dangerous, and it is only possible to continue to increase the concentration of krypton and xenon in liquid oxygen after the pre-removal of hydrocarbons from the depleted krypton-xenon concentrate, and currently the common method is to remove methane by a palladium catalyst through a chemical reaction at a temperature of about 450 ℃, and to remove carbon dioxide and water by adsorption with a molecular sieve, and then to concentrate to separate krypton and xenon from oxygen, krypton and xenon. Because a small amount of oxygen partially separated in the refining process cannot be well recovered, the resource waste is caused.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the rare gas krypton-xenon refining and ultra-pure oxygen production device has the advantages of safe operation, high yield, high rare gas purity, economy, energy conservation, wide application range and capability of effectively classifying and recovering oxygen on the premise of effectively preparing krypton and xenon.
In order to achieve the above purpose, the utility model adopts the technical scheme that:
a rare gas krypton-xenon refining and ultra-pure oxygen production device and a nitrogen circulating compressor comprise a liquid oxygen storage tank and a nitrogen circulating compressor, wherein the liquid oxygen storage tank is connected with a primary concentration tower through a liquid oxygen pump and a low-temperature adsorption tower; the liquid phase outlet at the bottom 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 is connected with a krypton-xenon separation tower for storing and separating krypton and xenon sequentially through a tube pass of the recooling device, the secondary concentration tower, the krypton-xenon deoxygenation tower and the gas heating device, the bottom of the krypton-xenon separation tower is connected with the xenon filling system through a first valve, and the middle upper part of the krypton-xenon separation tower is connected with the krypton gas filling system through a second valve.
Preferably, the catalytic oxidation system comprises a high-pressure liquid oxygen pump, and the high-pressure liquid oxygen pump is sequentially connected with the water bath type vaporizer, the preheater, the catalytic oxidation device, the drying tower and the high-pressure throttle valve.
Preferably, a primary concentrated gas phase outlet is formed in the top of the primary concentrating tower, and the primary concentrated gas phase outlet is respectively communicated with a reflux opening in the middle upper part of the primary concentrating tower and the industrial oxygen storage tank through a tube pass of the first tower top condenser.
Preferably, the top of the secondary concentration tower is provided with a secondary concentrated gas phase outlet, and the secondary concentrated gas phase outlet is respectively communicated with a reflux port at the middle upper part of the secondary concentration tower and an ultra-pure oxygen storage tank through a tube pass of a second tower top condenser.
Preferably, the top of the krypton-xenon deoxygenation tower is provided with a krypton-xenon deoxygenation gas-phase outlet, and the krypton-xenon deoxygenation gas-phase outlet is respectively communicated with the inlet of the liquid-oxygen pump and the reflux opening at the middle upper part of the krypton-xenon deoxygenation tower through the tube side of the condenser at the third tower top.
Preferably, the top of the krypton-xenon separation tower is provided with a krypton-xenon separation gas-phase outlet, and the krypton-xenon separation gas-phase outlet is respectively communicated with the inlet of the liquid-oxygen pump and the reflux opening at the middle upper part of the krypton-xenon separation tower through the tube pass of the fourth tower top condenser.
Preferably, the gas heating device is an electric furnace.
Preferably, the outlet of the nitrogen circulating compressor is respectively connected with a first reboiler at the bottom of the primary concentration tower and a second reboiler at the bottom of the secondary concentration tower through the tube pass of the heat exchanger; the outlet of the first reboiler is connected with the inlet of the nitrogen circulating compressor through the shell pass of the first overhead condenser and the shell pass of the heat exchanger; an outlet of the second reboiler is connected with a first inlet of a buffer tank, and an outlet of the buffer tank is respectively connected with a shell pass of a recooler, a shell pass of a second overhead condenser, a shell pass of a third overhead condenser and a shell pass of a fourth overhead condenser; and a shell pass outlet of the recooling device, a shell pass outlet of the second tower top condenser, a shell pass outlet of the third tower top condenser and a shell pass outlet of the fourth tower top condenser are respectively connected with an inlet of the nitrogen circulating compressor through a shell pass of the heat exchanger.
Preferably, the second inlet of the buffer tank is connected with a liquid nitrogen storage tank through a liquid nitrogen pump.
The device for producing the rare gas krypton-xenon refined and ultrapure oxygen prepared according to the scheme has the characteristics that the industrial oxygen and the ultrapure oxygen can be prepared by fractional recovery while the high-purity krypton-xenon gas is refined by adopting the liquid oxygen containing poor krypton-xenon as a raw material; the light components in the liquid oxygen can be effectively removed by arranging the primary concentration tower, so that the light components and part of the liquid oxygen enter the industrial oxygen storage tank together to achieve the aim of dehydrogenation; furthermore, the secondary concentration tower is arranged to realize the separation of oxygen and heavy components such as krypton and xenon, so that conditions are created for the separation of krypton and xenon in the subsequent working section, and meanwhile, the recovery of ultra-pure oxygen can be realized; after catalytic oxidation the utility model discloses used secondary concentration tower, krypton-xenon deoxidation tower and the krypton-xenon separation tower of separation krypton-xenon, above-mentioned form has reduced the use quantity of distillation column, has reduced the acquisition cost of enterprise, especially the utility model provides a krypton-xenon separation tower that uses not only has realized the separation purification in the same rectifying column of high-purity krypton and xenon, still has the function of saving high-purity xenon, and xenon content is few in the actual operation process specifically, closes not only can prevent behind the first valve that a small amount of krypton-xenon mixed liquid in the gas phase gets into xenon and fills the dress system, can also make the liquid phase xenon after the rectification pile up at the bottom of krypton-xenon separation tower to realize filling the dress to high-purity liquid phase xenon; furthermore, the high-pressure throttle valve in the utility model is arranged after catalytic oxidation, which can increase the pressure of liquid phase, thus being beneficial to the generation of positive reaction, leading the combustion of hydrocarbon to be more sufficient and leading the device with less residual quantity to be safer; the utility model has the advantages of simple structure, reasonable flow design, relatively low cost, safe operation, high yield, high purity of rare gas, economic and energy-saving performance, wide application range and effective classified recovery of oxygen under the premise of effectively preparing krypton and xenon.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Referring to fig. 1: the utility model relates to a rare gas krypton-xenon refining and ultra-pure oxygen production device, which comprises a liquid oxygen storage tank 1 and a nitrogen circulating compressor 27, wherein the liquid oxygen storage tank 1 is connected with a primary concentration tower 4 through a liquid oxygen pump 2 and a low-temperature adsorption tower 3; the liquid phase outlet at the bottom of the primary concentration tower 4 is connected with a catalytic oxidation system with a high-pressure throttle valve 5 at the tail end; the high-pressure throttle valve 5 is connected with a krypton-xenon separation tower 10 for storing and separating krypton and xenon sequentially through a tube pass of a recooling device 6, a secondary concentration tower 7, a krypton-xenon deoxygenation tower 8 and a gas heating device 9, the bottom of the krypton-xenon separation tower 10 is connected with a xenon filling system 12 through a first valve 34, and the middle upper part of the krypton-xenon separation tower 10 is connected with the krypton filling system 11 through a second valve 35. The catalytic oxidation system comprises a high-pressure liquid oxygen pump 13, and the high-pressure liquid oxygen pump 13 is sequentially connected with a water bath type vaporizer 14, a preheater 15, a catalytic oxidation device 16, a drying tower 36 and a high-pressure throttle valve 5. The top of the primary concentration tower 4 is provided with a primary concentrated gas phase outlet, and the primary concentrated gas phase outlet is respectively communicated with a reflux port 18 at the middle upper part of the primary concentration tower 4 and an industrial oxygen storage tank 19 through a tube pass of a first tower top condenser 17. The top of the secondary concentration tower 7 is provided with a secondary concentrated gas phase outlet, and the secondary concentrated gas phase outlet is respectively communicated with a reflux opening 21 at the middle upper part of the secondary concentration tower 7 and an ultra-pure oxygen storage tank 22 through a tube pass of a second tower top condenser 20. The top of the krypton-xenon deoxygenation tower 8 is provided with a krypton-xenon deoxygenation gas-phase outlet which is respectively communicated with an inlet of the liquid-oxygen pump 2 and a reflux opening 24 at the middle upper part of the krypton-xenon deoxygenation tower 8 through a tube pass of a third tower top condenser 23. The top of the krypton-xenon separation tower 10 is provided with a krypton-xenon separation gas-phase outlet which is respectively communicated with an inlet of the liquid-oxygen pump 2 and a reflux opening 26 at the middle upper part of the krypton-xenon separation tower 10 through a tube pass of a fourth tower top condenser 25. The gas heating device 9 is an electric furnace. The outlet of the nitrogen circulating compressor 27 is connected with a first reboiler 29 at the bottom of the primary concentration tower 4 and a second reboiler 30 at the bottom of the secondary concentration tower 7 through the tube pass of the heat exchanger 28; the outlet of the first reboiler 29 is connected to the inlet of the nitrogen recycle compressor 27 through the shell side of the first overhead condenser 17 and the shell side of the heat exchanger 28; an outlet of the second reboiler 30 is connected with a first inlet of a buffer tank 31, and an outlet of the buffer tank 31 is respectively connected with a shell pass of the recooler 6, a shell pass of the second overhead condenser 20, a shell pass of the third overhead condenser 23 and a shell pass of the fourth overhead condenser 25; the shell pass outlet of the recooling device 6, the shell pass outlet of the second overhead condenser 20, the shell pass outlet of the third overhead condenser 23 and the shell pass outlet of the fourth overhead condenser 25 are respectively connected with the inlet of a nitrogen circulating compressor 27 through the shell pass of a heat exchanger 28. A second inlet of the buffer tank 31 is connected to a liquid nitrogen storage tank 33 via a liquid nitrogen pump 32.
A production process of a rare gas krypton-xenon refining and ultra-pure oxygen production device comprises the following steps:
step 1: the krypton-xenon-poor liquid oxygen in the liquid oxygen storage tank 1 enters a low-temperature adsorption tower 3 through a liquid oxygen pump 2, and N in the krypton-xenon-poor liquid oxygen is adsorbed by the low-temperature adsorption tower 32O and CO2Then enters a primary concentration tower 4; the main components and volume fractions of the krypton-xenon-poor liquid oxygen comprise: o is2≥99.6%、Kr+Xe≤1000ppm、CH4≤1000ppm、N2O10-20 ppm and CO2 10 to 50 ppm; the temperature of the krypton-xenon-poor liquid oxygen is as follows: -180 ℃ and at a pressure of: 0.25 MPa; the pressure in the low-temperature adsorption tower 3 is 0.25 MPa; the low-temperature adsorption tower 3 is internally provided with N for removing liquid oxygen2O and CO2The molecular sieve of (4);
step 2: after the liquid oxygen entering the primary concentration tower 4 is concentrated and rectified, the liquid phase sequentially enters a water bath type vaporizer 14, a preheater 15, a catalytic oxidation device 16 and a drying tower 36 through a tower bottom liquid phase outlet of the primary concentration tower 4 and a high-pressure liquid oxygen pump 13, is throttled by a high-pressure throttle valve 5 and then enters a tube pass of a recooling device 6 for cooling; the primary concentration tower 4 concentrates the poor krypton-xenon liquid in the poor krypton-xenon liquid oxygen and the main components thereofThe volume fraction includes: o is2≥99.5%，Kr+Xe≤2500ppm 、CH4Less than or equal to 2500ppm, pressure is: 0.25MPa, temperature: -180 ℃;
the high-pressure liquid oxygen pump 13 increases the liquid oxygen pressure to 5.4-5.6 MPa, so that the separation of hydrocarbon solids can be avoided; the liquid oxygen with increased pressure is gasified by water bath type vaporizer 14 and preheater 15 to raise temperature, and the hydrocarbon is oxidized to below 0.5ppm by oxygen under the action of catalyst by catalytic oxidation device 16 to reduce hydrocarbon explosion risk, and further, H generated after catalytic oxidation is removed by drying tower 362O and CO2(ii) a Reducing the fluid pressure to 0.6-1.0 MPa through throttling of a high-pressure throttle valve 5;
and step 3: the cooled liquid oxygen enters a secondary concentration tower 7 for secondary concentration and rectification, and the liquid phase after secondary concentration and rectification enters a krypton-xenon deoxygenation tower 8 through a liquid phase outlet at the bottom of the secondary concentration tower 7; the components and volume fractions of the liquid oxygen after re-concentration and rectification in the secondary concentration tower 7 include: o is2Not more than 87 percent, not less than 13 percent of Kr + Xe, 0.15MPa of pressure, temperature: -179 ℃;
and 4, step 4: the liquid phase entering the krypton-xenon deoxygenation tower 8 is rectified and deoxygenated in the krypton-xenon deoxygenation tower 8 to prepare krypton-xenon mixed liquid, and the krypton-xenon mixed liquid is heated into a gas phase by a gas heating device 9 and then enters a krypton-xenon separation tower 10; the krypton-xenon mixed liquid passing through the krypton-xenon deoxygenation tower 8 comprises the following components: kr + Xe is more than or equal to 99.9 percent, and the pressure is as follows: 0.14MPa, temperature: -149 deg.C; heating the krypton-xenon mixed solution to a gas phase by a gas heating device 9, wherein the temperature of the gas phase is-100 ℃;
and 5: the gas phase heated by the gas heating device 9 enters a krypton-xenon separation tower 10 for separation, and the liquid phase after separation enters a xenon filling system 12 through the tower bottom of the krypton-xenon separation tower 10; the gas phase in the middle of the krypton-xenon separation tower 10 enters a krypton filling system 11; o is used in the krypton-xenon separation column 102Kr and Xe are separated according to different boiling points, and the heavy component xenon is deposited at the bottom of a krypton-xenon separation tower 10 and filled through a xenon filling system 12; the light component comprises O2And Kr, O2O compared with Kr2The components are light components and are not mixed,O2and partial Kr is discharged through a top gas phase outlet, and the Kr with high purity in the middle of the Kr-Xe separation tower 10 enters a Kr charging system 11; the purity of xenon in the xenon filling system 12 is 99.999%, and the purity of krypton in the krypton filling system 11 is 99.999%;
step 6: after the liquid oxygen enters the primary concentration tower 4 in the step 2, the gas phase after concentration and rectification enters the tube pass of a first tower top condenser 17 to be condensed into a liquid phase, one part of the liquid oxygen enters the primary concentration tower 4 through a reflux opening 18 at the middle upper part of the primary concentration tower 4 to be continuously concentrated and rectified, and the other part of the liquid oxygen enters an industrial oxygen storage tank 19; the liquid phase entering the industrial oxygen storage tank 19 is industrial liquid oxygen with the purity of 99.5 percent;
and 7: after the cooled liquid oxygen enters the secondary concentration tower 7 for secondary concentration and rectification, the gas phase enters a tube pass of a second tower top condenser 20 to be condensed into a liquid phase, one part of the gas phase enters the secondary concentration tower 7 through a reflux opening 21 at the middle upper part of the secondary concentration tower 7 for continuous secondary concentration and rectification, and the other part of the gas phase enters an ultra-pure oxygen storage tank 22; the liquid phase entering the ultra-pure oxygen storage tank 22 is ultra-pure liquid oxygen with the purity of 99.9999 percent;
and 8: in the step 4, after the gas phase of the liquid phase rectified in the krypton-xenon deoxygenation tower 8 enters the tube side of a third tower top condenser 23 to be condensed into a liquid phase, one part of the liquid phase enters the krypton-xenon deoxygenation tower 8 through a reflux opening 24 at the middle upper part of the krypton-xenon deoxygenation tower 8, and the other part of the liquid phase enters the liquid oxygen pump 2 through an inlet of the liquid oxygen pump 2 to repeat the steps 1-5;
and step 9: in the step 5, after the gas phase of the liquid phase which is rectified and separated in the krypton-xenon separation tower 10 enters a tube pass of a fourth tower top condenser 25 to be condensed into a liquid phase, one part of the liquid phase enters the krypton-xenon separation tower 10 through a reflux opening 26 at the middle upper part of the krypton-xenon separation tower 10, and the other part of the liquid phase enters a liquid oxygen pump 2 through an inlet of the liquid oxygen pump 2 to repeat the steps 1-5;
step 10: in the operation process of the steps 1 to 9, the nitrogen circulating compressor 27 is always in an operation state, nitrogen in the nitrogen circulating compressor 27 is pressurized to 1.0-1.3 MPa and then exchanges heat through a tube pass of the heat exchanger 28, the nitrogen after heat exchange respectively enters the first reboiler 29 at the bottom of the primary concentration tower 4 and the second reboiler 30 at the bottom of the secondary concentration tower 7 to provide heat and is discharged in a liquid nitrogen form, the liquid nitrogen in the first reboiler 29 enters the nitrogen circulating compressor 27 through a shell pass of the first overhead condenser 17 and a shell pass of the heat exchanger 28 to be repeatedly compressed and used, the liquid nitrogen in the second reboiler 30 at the bottom of the secondary concentration tower 7 enters the buffer tank 31 to be mixed with the liquid nitrogen from the liquid nitrogen storage tank 33 and then respectively enters the shell pass of the cooler 6, the shell pass of the second overhead condenser 20, the shell pass of the third overhead condenser 23 and the shell pass of the fourth overhead condenser 25, for condensing the gas phase in the tube passes of the recooler 6, the second overhead condenser 20, the third overhead condenser 23 and the fourth overhead condenser 25; after condensation, the shell pass outlet of the cooler 6, the shell pass outlet of the second overhead condenser 20, the shell pass outlet of the third overhead condenser 23 and the shell pass outlet of the fourth overhead condenser 25 respectively enter the shell pass of the heat exchanger 28, and after heat exchange in the shell pass of the heat exchanger 28, the condensed liquid enters the nitrogen circulating compressor 27 from the inlet of the nitrogen circulating compressor 27 to complete circulation; the pressure at the outlet of the buffer tank 31 is as follows: 1.0 MPa.
The utility model adopts the poor krypton-xenon-containing liquid oxygen as the raw material, so that the industrial oxygen and the ultra-pure oxygen can be prepared by fractional recovery while the high-purity krypton-xenon gas is refined; the light components in the liquid oxygen can be effectively removed by arranging the primary concentration tower, so that the light components and part of the liquid oxygen enter the industrial oxygen storage tank together to achieve the aim of dehydrogenation; furthermore, the secondary concentration tower is arranged to realize the separation of oxygen and heavy components such as krypton and xenon, so that conditions are created for the separation of krypton and xenon in the subsequent working section, and meanwhile, the recovery of ultra-pure oxygen can be realized; after catalytic oxidation the utility model discloses used secondary concentration tower, krypton-xenon deoxidation tower and the krypton-xenon separation tower of separation krypton-xenon, above-mentioned form has reduced the use quantity of distillation column, has reduced the acquisition cost of enterprise, especially the utility model provides a krypton-xenon separation tower that uses not only has realized the separation purification in the same rectifying column of high-purity krypton gas and xenon, still has the function of saving high-purity xenon, and xenon content is few in the actual operation process specifically, closes first valve 34 after not only can prevent that a small amount of krypton-xenon mixed liquid in the gas phase from getting into xenon filling system 12, can also make the liquid phase xenon after the rectification pile up at the bottom of krypton-xenon separation tower 10 to realize filling the dress to high-purity liquid phase xenon; the krypton gas and oxygen in the utility model rise after rectification, the oxygen rising speed is high and at the upper part, the slow krypton gas rising speed is mainly enriched at the middle upper part of the krypton-xenon separation tower, and the high-purity krypton gas can rapidly enter the krypton gas filling system 11; the krypton-xenon filling system 11 in the utility model can be used for collecting high-purity krypton, and the mixed gas of low-purity krypton and oxygen is discharged from the top of the krypton-xenon separation tower and participates in circulation again; the method has the advantages of safe operation, high yield, high purity of rare gas and capability of effectively classifying and recycling oxygen on the premise of effectively preparing krypton-xenon.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention in its corresponding aspects.
Claims (9)
1. A rare gas krypton-xenon refining and ultra-pure oxygen production device comprises a liquid oxygen storage tank (1) and a nitrogen circulating compressor (27), and is characterized in that: the liquid oxygen storage tank (1) is connected with the primary concentration tower (4) through a liquid oxygen pump (2) and a low-temperature adsorption tower (3);
the liquid phase outlet at the bottom of the primary concentration tower (4) is connected with a catalytic oxidation system with a high-pressure throttle valve (5) at the tail end;
the high-pressure throttle valve (5) is connected with a krypton-xenon separation tower (10) for storing and separating krypton and xenon sequentially through a tube pass of a recooling device (6), a secondary concentration tower (7), a krypton-xenon deoxygenation tower (8) and a gas heating device (9), the bottom of the krypton-xenon separation tower (10) is connected with a xenon filling system (12) through a first valve (34), and the middle upper part of the krypton-xenon separation tower (10) is connected with the krypton filling system (11) through a second valve (35).
2. The apparatus for refining rare gas krypton-xenon and producing ultrapure oxygen according to claim 1, characterized in that: the catalytic oxidation system comprises a high-pressure liquid oxygen pump (13), and the high-pressure liquid oxygen pump (13) is sequentially connected with a water bath type vaporizer (14), a preheater (15), a catalytic oxidation device (16), a drying tower (36) and a high-pressure throttle valve (5).
3. The apparatus for refining rare gas krypton-xenon and producing ultrapure oxygen according to claim 1, characterized in that: the top of the primary concentration tower (4) is provided with a primary concentrated gas phase outlet which is respectively communicated with a reflux opening (18) at the middle upper part of the primary concentration tower (4) and an industrial oxygen storage tank (19) through a tube pass of a first tower top condenser (17).
4. The apparatus for refining rare gas krypton-xenon and producing ultrapure oxygen according to claim 1, characterized in that: and a secondary concentrated gas phase outlet is formed in the top of the secondary concentration tower (7), and is respectively communicated with a reflux opening (21) in the middle upper part of the secondary concentration tower (7) and an ultra-pure oxygen storage tank (22) through a tube pass of a second tower top condenser (20).
5. The apparatus for refining rare gas krypton-xenon and producing ultrapure oxygen according to claim 1, characterized in that: the top of the krypton-xenon deoxygenation tower (8) is provided with a krypton-xenon deoxygenation gas-phase outlet which is respectively communicated with an inlet of the liquid-oxygen pump (2) and a reflux opening (24) at the middle upper part of the krypton-xenon deoxygenation tower (8) through a tube pass of a third tower top condenser (23).
6. The apparatus for refining rare gas krypton-xenon and producing ultrapure oxygen according to claim 1, characterized in that: the top of the krypton-xenon separation tower (10) is provided with a krypton-xenon separation gas-phase outlet which is respectively communicated with an inlet of the liquid-oxygen pump (2) and a reflux opening (26) at the middle upper part of the krypton-xenon separation tower (10) through a tube pass of a fourth tower top condenser (25).
7. The apparatus for refining rare gas krypton-xenon and producing ultrapure oxygen according to claim 1, characterized in that: the gas heating device (9) is an electric furnace.
8. The apparatus for refining rare gas krypton-xenon and producing ultrapure oxygen according to claim 1, characterized in that: the outlet of the nitrogen circulating compressor (27) is respectively connected with a first reboiler (29) at the bottom of the primary concentration tower (4) and a second reboiler (30) at the bottom of the secondary concentration tower (7) through the tube side of a heat exchanger (28);
the outlet of the first reboiler (29) is connected with the inlet of the nitrogen circulating compressor (27) through the shell side of the first overhead condenser (17) and the shell side of the heat exchanger (28);
an outlet of the second reboiler (30) is connected with a first inlet of a buffer tank (31), and an outlet of the buffer tank (31) is respectively connected with a shell pass of a recooler (6), a shell pass of a second overhead condenser (20), a shell pass of a third overhead condenser (23) and a shell pass of a fourth overhead condenser (25);
and a shell pass outlet of the recooling device (6), a shell pass outlet of the second overhead condenser (20), a shell pass outlet of the third overhead condenser (23) and a shell pass outlet of the fourth overhead condenser (25) are respectively connected with an inlet of the nitrogen circulating compressor (27) through a shell pass of the heat exchanger (28).
9. The apparatus for refining rare gas krypton-xenon and producing ultrapure oxygen according to claim 8, wherein: and a second inlet of the buffer tank (31) is connected with a liquid nitrogen storage tank (33) through a liquid nitrogen pump (32).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111692838A (en) * | 2020-07-16 | 2020-09-22 | 河南心连心深冷能源股份有限公司 | Rare gas krypton-xenon refining and ultrapure oxygen production device and production process |
| CN115854653A (en) * | 2023-02-27 | 2023-03-28 | 河南心连心深冷能源股份有限公司 | A device and production process for producing krypton-depleted xenon and ultra-pure oxygen using the same heat pump |
-
2020
- 2020-07-16 CN CN202021412388.3U patent/CN212390705U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111692838A (en) * | 2020-07-16 | 2020-09-22 | 河南心连心深冷能源股份有限公司 | Rare gas krypton-xenon refining and ultrapure oxygen production device and production process |
| CN111692838B (en) * | 2020-07-16 | 2024-11-22 | 河南心连心深冷能源股份有限公司 | A production device and production process for refining rare gases krypton and xenon and ultrapure oxygen |
| CN115854653A (en) * | 2023-02-27 | 2023-03-28 | 河南心连心深冷能源股份有限公司 | A device and production process for producing krypton-depleted xenon and ultra-pure oxygen using the same heat pump |
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