CN108362074B - Method and device for extracting krypton and xenon from oversized air separation equipment - Google Patents
Method and device for extracting krypton and xenon from oversized air separation equipment Download PDFInfo
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- CN108362074B CN108362074B CN201810249809.6A CN201810249809A CN108362074B CN 108362074 B CN108362074 B CN 108362074B CN 201810249809 A CN201810249809 A CN 201810249809A CN 108362074 B CN108362074 B CN 108362074B
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- xenon
- krypton
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- liquid oxygen
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- 229910052743 krypton Inorganic materials 0.000 title claims abstract description 40
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052724 xenon Inorganic materials 0.000 title claims abstract description 40
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000926 separation method Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 18
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 70
- PDEXVOWZLSWEJB-UHFFFAOYSA-N krypton xenon Chemical compound [Kr].[Xe] PDEXVOWZLSWEJB-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000005406 washing Methods 0.000 claims abstract description 49
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000001301 oxygen Substances 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 86
- 229910052786 argon Inorganic materials 0.000 claims description 43
- 238000009833 condensation Methods 0.000 claims description 26
- 230000005494 condensation Effects 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 19
- 238000000746 purification Methods 0.000 claims description 15
- 230000002457 bidirectional effect Effects 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 239000012263 liquid product Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 15
- 238000007906 compression Methods 0.000 description 4
- 230000001174 ascending effect Effects 0.000 description 3
- 230000006835 compression Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- -1 carbon hydrocarbon compounds Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000004094 preconcentration Methods 0.000 description 1
Classifications
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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
- F25J3/04406—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 using a dual pressure main column system
- F25J3/04412—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 using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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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
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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
- F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
- F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
- F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
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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
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
- F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
- F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
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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
- F25J3/04763—Start-up or control of the process; Details of the apparatus used
- F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
- F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
- F25J3/04878—Side by side arrangement of multiple vessels in a main column system, wherein the vessels are normally mounted one upon the other or forming different sections of the same column
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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
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/34—Processes or apparatus using separation by rectification using a side column fed by a stream from the low pressure column
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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
- 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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- 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
- F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
- F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention discloses a method and a device for extracting krypton and xenon from oversized air separation equipment. And pressurizing liquid oxygen taken out from the bottom of the upper tower by a liquid oxygen lifting pump, then feeding the liquid oxygen into a poor krypton-xenon washing tower for rectification, then feeding the liquid oxygen into a main condensing evaporator for evaporation and concentration, and finally feeding the liquid oxygen into the poor krypton-xenon washing tower for one-stage or two-stage rectification to obtain liquid containing krypton and xenon. The heat source of the lean krypton-xenon concentration tower can adopt lower tower nitrogen or lower tower forward air, and the method and the device are suitable for 8-12 ten thousand Nm3/h grade super-large air separation equipment, and have the characteristics of good safety, high reliability, high extraction rate of krypton-xenon, stable extraction rate of oxygen products and the like.
Description
Technical Field
The invention relates to the technical field of air separation, in particular to a method and a device for extracting krypton and xenon from oversized air separation equipment.
Background
Krypton and xenon are widely used as rare gases in the fields of illumination, space satellite, medical industry and the like. The content of krypton in the air was 1.14ppm, the content of xenon was 0.086ppm, and krypton and xenon were mainly extracted from byproducts of the air separation apparatus. With the development of the air separation equipment towards 8-12 ten thousand Nm3/h grade oversized, the extraction of rare gas from the oversized air separation equipment has huge economic value.
At present, domestic krypton-xenon extraction equipment is mostly concentrated in space division equipment below the level of 6 ten thousand Nm 3/h. For a space division device below the 6 ten thousand Nm3/h level, the traditional extraction of krypton and xenon generally has 2 modes: an external compression flow air separation device mainly producing gas-oxygen products uses liquid oxygen as raw materials to pre-concentrate krypton and xenon; another is an air separation device of the compression flow in a liquid oxygen pump, since a large amount of liquid oxygen is pumped out from a condensation evaporator, it is impossible to extract krypton-xenon concentrate from the liquid oxygen, and krypton-xenon preconcentration is performed by taking the oxygen-enriched liquid air as a raw material.
For 8-12 ten thousand Nm3/h ultra-large air separation equipment, a liquid oxygen pump compression process is generally adopted, and because of the large size of the equipment, the process flow organization and the equipment arrangement mode are greatly different from those of the air separation equipment below 6 ten thousand Nm3/h level: on the basis of the conventional liquid oxygen internal compression process flow, an scheme suitable for oversized air separation equipment is adopted, wherein an upper tower is arranged in parallel with a lower tower, a main condensation evaporator is arranged on the lower tower, a liquid oxygen lifting pump is additionally arranged, and high-pressure liquid oxygen products are extracted from the bottom of the upper tower. According to the characteristics of the oversized air separation equipment, the original krypton-xenon extraction mode is not applicable any more. Therefore, a krypton and xenon extraction system suitable for 8 to 12 ten thousand Nm3/h ultra-large air separation equipment is required.
Disclosure of Invention
The invention aims at: the method and the device for extracting the krypton and the xenon from the oversized air separation equipment are provided, so that a krypton-xenon-lean washing tower is arranged at the upper part of a main condensation evaporator, liquid oxygen at the bottom of the upper tower is used as a raw material, the liquid oxygen amount of the krypton-xenon-lean washing tower is stable, the load of the main condensation evaporator is stable, and the krypton-xenon extraction rate is higher.
The aim of the invention is achieved by the following technical scheme:
an apparatus for extracting krypton and xenon from an oversized air separation plant, comprising: the device comprises a lower tower, an upper tower, a main condensation evaporator, a liquid oxygen lifting pump, a krypton-xenon-lean washing tower, a krypton-xenon-lean concentration tower and a krypton-xenon-lean evaporator, wherein the bottom of the lower tower is connected with a raw material air inlet pipe, the raw material air inlet pipe is provided with a branch and is connected with the inlet of the krypton-xenon-lean washing tower, the upper part of the lower tower is provided with the krypton-xenon-lean washing tower, the main condensation evaporator is arranged in the krypton-xenon-lean washing tower, the main condensation evaporator is communicated with the lower tower through a pipeline, the top of the krypton-xenon-lean washing tower and the top of the krypton-xenon-lean concentration tower are respectively communicated with the top of the krypton-xenon-lean washing tower through a pipeline, the outlet of the krypton-xenon-lean washing tower and the bottom of the lower tower are communicated with the upper condensation tower through an oxygen-rich liquid pipe, and the main condensation evaporator is provided with non-gas.
The invention discloses a device for extracting krypton and xenon from oversized air separation equipment, wherein a liquid oxygen product outlet pipe is arranged on a high-pressure liquid oxygen pump and is connected with a subcooler.
The invention relates to a device for extracting krypton and xenon from oversized air separation equipment, wherein the bottom of an upper tower is provided with a high-pressure liquid oxygen pump, the high-pressure liquid oxygen pump is connected with a high-pressure liquid oxygen outlet pipe, and the high-pressure liquid oxygen outlet pipe is connected with a heat exchanger.
The invention relates to a device for extracting krypton and xenon from oversized air separation equipment, which is characterized in that an argon purification system is arranged outside an upper tower, and comprises: the device comprises a crude argon tower and a crude argon condenser, wherein the upper tower is in bidirectional intercommunication through a pipeline of the crude argon tower, the top and the bottom of the crude argon condenser are both communicated with the upper tower through pipelines, the subcooler is connected with the crude argon condenser through a pipeline, and the crude argon condenser is provided with a crude argon outlet pipe.
The device for extracting krypton and xenon from oversized air separation equipment also comprises a second-stage krypton-xenon purification system, wherein the second-stage krypton-xenon purification system comprises: the device comprises a second-stage krypton-xenon-lean washing tower and a second-stage krypton-xenon-lean evaporator, wherein the top of the second-stage krypton-xenon-lean washing tower is connected with a krypton-xenon-lean concentration tower through a pipeline, a krypton-xenon-lean pipe is communicated with the top of the second-stage krypton-xenon-lean washing tower, an inlet of the second-stage krypton-xenon-lean evaporator is communicated with a raw material air inlet pipe, an outlet of the second-stage krypton-xenon-lean evaporator is connected with an oxygen-enriched liquid pipe, and the bottom of the second-stage krypton-xenon-lean washing tower is provided with a second-stage krypton-xenon-lean pipe.
A method for extracting krypton and xenon, comprising the steps of:
s1, rectifying raw material air A1 by a lower tower to obtain an oxygen-enriched liquid space;
s2, the oxygen-enriched liquid air is delivered to the top of the crude argon tower after decompression and throttling;
s3, rectifying the oxygen-enriched liquid space through an upper tower to obtain liquid oxygen with higher concentration of krypton and xenon;
s4, liquid oxygen firstly enters a lean krypton-xenon washing tower for rectification, and then enters a main condenser for evaporation;
s5, delivering the liquid oxygen evaporated by the main condenser into a krypton-xenon-lean concentration tower and a krypton-xenon-lean evaporator for further evaporation;
s6, obtaining a liquid product containing krypton and xenon at the product outlet ends of the krypton-xenon-lean concentration tower and the krypton-xenon-lean evaporator;
and S7, further processing the product obtained in the last step to the required concentration and state.
In the method for extracting krypton and xenon according to the present invention, the step S6 is followed by a second-stage purification step.
In the krypton and xenon extraction method, part of raw material air A1 is used as a heat source of a crude argon tower.
A method for extracting krypton and xenon features that most of the liquid oxygen in main condenser is returned to the bottom of upper tower, so maintaining a certain circulation rate of liquid oxygen in main condensing evaporator.
According to the technical scheme, the invention has the beneficial effects that:
1. the method is suitable for 8-12 ten thousand Nm3/h ultra-large air separation equipment with the grade of 8-12 ten thousand Nm3/h, and has good safety and high reliability.
2. The lean krypton-xenon washing tower is arranged at the upper part of the main condensation evaporator, and liquid oxygen at the bottom of the upper tower is used as a raw material, so that the liquid oxygen amount of the lean krypton-xenon washing tower is stable, the load of the main condensation evaporator is stable, and the extraction rate of krypton-xenon is higher.
3. The liquid oxygen is used as raw material to extract the poor krypton-xenon, only part of oxygen is taken away from the poor krypton-xenon product, and the extraction rate of the oxygen product is not influenced.
4. Most of the liquid oxygen of the main condensation evaporator flows back to the liquid oxygen pool at the bottom of the upper tower, so that the liquid oxygen of the main condensation evaporator maintains a certain circulation rate, the concentration of the carbon hydrocarbon compounds in the main condensation evaporator is kept within a safe range, and the safety of the main condensation evaporator is ensured.
5. The extra-large air separation equipment adopts liquid oxygen to extract krypton and xenon, the height of a cold box is reasonable, liquid air can smoothly enter a crude argon condenser, and the overall reliability of the air separation equipment is high.
Drawings
FIG. 1 is a schematic diagram of an apparatus for extracting krypton and xenon from an oversized air separation plant in accordance with the present invention;
FIG. 2 is a schematic diagram of a second embodiment of an apparatus for extracting krypton and xenon from an oversized air separation plant in accordance with the present invention.
Detailed Description
The invention will be further described with reference to specific examples and figures.
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Fig. 1 is a first embodiment of a method and apparatus for extracting krypton and xenon from an oversized air separation plant of the present invention, comprising: the bottom of the lower tower C1 is connected with a raw material air inlet pipe A1, the raw material air inlet pipe A1 is provided with a branch and is connected with an inlet of the poor krypton-xenon evaporator K3, the upper part of the lower tower C1 is provided with the poor krypton-xenon washing tower C4, the poor krypton-xenon washing tower C4 is internally provided with the main condensing evaporator K1, the main condensing evaporator K1 is communicated with the lower tower C1 through a pipeline, the top of the poor krypton-xenon washing tower C4 and the top of the poor krypton-xenon concentrating tower C5 are communicated with the bottom of the upper tower C2 after being converged through a pipeline, the top of the poor krypton-xenon washing tower C4 is respectively communicated with the top of the poor krypton-xenon concentrating tower C5 and the bottom of the upper tower C2 through pipelines, the bottom of the upper tower C2 is communicated with the top of a lean krypton-xenon washing tower C4 through a high-pressure liquid oxygen pump OP1, an outlet of the lean krypton-xenon evaporator K3 and the bottom of the lower tower C1 are communicated with the upper tower C2 after being converged through an oxygen-enriched liquid pipe A2, a non-condensable gas pipe A3 is arranged on the main condensation evaporator K1, a lean krypton-xenon pipe A4 is arranged at the bottom of the lean krypton-xenon evaporator K3, a liquid oxygen product pipe is also arranged on the high-pressure liquid oxygen pump OP1, the liquid oxygen product pipe is connected with a subcooler, the high-pressure liquid oxygen pump OP1 is arranged at the bottom of the upper tower C2, the high-pressure liquid oxygen pipe is connected with a heat exchanger, an argon purification system is arranged on the outer side of the upper tower C2, and the argon purification system comprises: the device comprises a crude argon column C3 and a crude argon condenser K2, wherein the upper column C2 is in bidirectional intercommunication with the crude argon column C3 through a pipeline, the top and the bottom of the crude argon condenser K2 are both communicated with the upper column C2 through pipelines, the subcooler is connected with the crude argon condenser K2 through a pipeline, and the crude argon condenser K2 is provided with a crude argon outlet pipe.
Fig. 2 is a second embodiment of an apparatus for extracting krypton and xenon from an oversized air separation plant according to the present invention, comprising: the bottom of the lower tower C1 is connected with a raw material air inlet pipe A1, the raw material air inlet pipe A1 is provided with a branch and is connected with an inlet of the poor krypton-xenon evaporator K3, the upper part of the lower tower C1 is provided with the poor krypton-xenon washing tower C4, the poor krypton-xenon washing tower C4 is internally provided with the main condensing evaporator K1, the main condensing evaporator K1 is communicated with the lower tower C1 through a pipeline, the top of the poor krypton-xenon washing tower C4 and the top of the poor krypton-xenon concentrating tower C5 are communicated with the bottom of the upper tower C2 after being converged through a pipeline, the top of the poor krypton-xenon washing tower C4 is respectively communicated with the top of the poor krypton-xenon concentrating tower C5 and the bottom of the upper tower C2 through pipelines, the bottom of the upper tower C2 is communicated with the top of a lean krypton-xenon washing tower C4 through a high-pressure liquid oxygen pump OP1, an outlet of the lean krypton-xenon evaporator K3 and the bottom of the lower tower C1 are communicated with the upper tower C2 after being converged through an oxygen-enriched liquid pipe A2, a non-condensable gas pipe A3 is arranged on the main condensation evaporator K1, a lean krypton-xenon pipe A4 is arranged at the bottom of the lean krypton-xenon evaporator K3, a liquid oxygen product pipe is also arranged on the high-pressure liquid oxygen pump OP1, the liquid oxygen product pipe is connected with a subcooler, the high-pressure liquid oxygen pump OP1 is arranged at the bottom of the upper tower C2, the high-pressure liquid oxygen pipe is connected with a heat exchanger, an argon purification system is arranged on the outer side of the upper tower C2, and the argon purification system comprises: the crude argon column C3 and the crude argon condenser K2, the upper column C2 is communicated with each other in a two-way through a pipeline crude argon column C3, the top and the bottom of the crude argon condenser K2 are communicated with the upper column C2 through pipelines, the subcooler is connected with the crude argon condenser K2 through a pipeline, the crude argon condenser K2 is provided with a crude argon outlet pipe, and the crude argon condenser K2 is also provided with a second-stage krypton-xenon purification system, and the second-stage krypton-xenon purification system comprises: the system comprises a secondary krypton-xenon-lean washing tower C6 and a secondary krypton-xenon-lean evaporator K4, wherein the top of the secondary krypton-xenon-lean washing tower C6 is connected with a krypton-xenon-lean concentration tower C5 through a pipeline, the krypton-xenon-lean pipe A4 is communicated with the top of the secondary krypton-xenon-lean washing tower C6, the inlet of the secondary krypton-xenon-lean evaporator K4 is communicated with a raw material air inlet pipe A1, the outlet of the secondary krypton-xenon-lean evaporator K4 is connected with an oxygen-enriched liquid pipe A2, and the bottom of the secondary krypton-xenon-lean washing tower C6 is provided with a secondary krypton-xenon-lean pipe A5.
A method for extracting krypton and xenon, comprising the steps of:
s1, rectifying raw material air A1 by a lower tower C1 to obtain oxygen-enriched liquid air;
s2, the oxygen-enriched liquid space is sent to the top of a crude argon column C3 after decompression and throttling;
s3, rectifying the oxygen-enriched liquid space through an upper tower C2 to obtain liquid oxygen with higher concentration of krypton and xenon;
s4, liquid oxygen firstly enters a lean krypton-xenon washing tower C4 for rectification, and then enters a main condenser K1 for evaporation;
s5, delivering the liquid oxygen evaporated by the main condenser K1 into a krypton-xenon-lean concentration tower C5 and a krypton-xenon-lean evaporator K3 for further evaporation;
s6, obtaining a liquid product containing krypton and xenon at the product outlet end of the krypton-xenon-lean concentration column C5 and the krypton-xenon-lean evaporator K3;
and S7, further processing the product obtained in the last step to the required concentration and state.
The step S6 is followed by a second purification process.
A portion of the feed air A1 serves as a heat source for the crude argon column C3.
Most of the oxygen-enriched liquid air of the main condenser K1 flows back to the bottom of the upper tower, so that the liquid oxygen of the main condensing evaporator maintains a certain circulation rate.
The working process of the invention is as follows: part of liquid oxygen from the bottom of the upper tower C2 is pressurized by a liquid oxygen lifting pump OP2, enters a lean krypton-xenon washing tower C4, is rectified with ascending gas from a main condensation evaporator K1, enters the main condensation evaporator K1, is evaporated and concentrated, enters a lean krypton-xenon concentration tower C5, is rectified again, enters a lean krypton-xenon evaporator K3, and is evaporated and concentrated again to obtain product liquid containing krypton and xenon. The gas evaporated by the main condensation evaporator K1 rises into the lean krypton-xenon washing tower C4, is rectified with liquid oxygen and then enters the upper tower C2. The gas evaporated by the krypton-xenon-lean evaporator K3 rises into the krypton-xenon-lean concentration column C5, is rectified with liquid oxygen, and then, merges with the gas from the krypton-xenon-lean washing column C4, and enters the upper column (C2). The heat source of the krypton-xenon-lean evaporator K3 may be lower column nitrogen or lower column forward flow air.
Example 2 differs from example 1 in the operation: the liquid oxygen from the main condensation evaporator K1 firstly enters a lean krypton-xenon concentration tower C5, is rectified with the ascending gas from the krypton-xenon evaporator K3, then enters the krypton-xenon evaporator K3, is evaporated and concentrated, then enters a secondary lean krypton-xenon concentration tower C6, is rectified with the ascending gas from the secondary krypton-xenon evaporator K4, then enters the secondary krypton-xenon evaporator K4, and is evaporated and concentrated again to obtain product liquid containing krypton and xenon. The gas evaporated by the second-stage lean krypton-xenon evaporator K4 rises into a second-stage lean krypton-xenon concentration tower C6, is rectified with liquid oxygen, and then enters a first-stage lean krypton-xenon concentration tower C5; the gas evaporated by the low-krypton xenon evaporator K3 rises into the low-krypton xenon concentration column C5, merges with the rising gas from the second low-krypton xenon concentration column C6, rectifies with liquid oxygen, merges with the rising gas from the low-krypton xenon washing column C4, and enters the upper column C2.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (5)
1. An apparatus for extracting krypton and xenon from an oversized air separation plant, comprising: the device comprises a lower tower, an upper tower, a main condensation evaporator, a liquid oxygen lift pump, a krypton-xenon-lean washing tower, a krypton-xenon-lean concentration tower and a krypton-xenon-lean evaporator, wherein the bottom of the lower tower is connected with a raw material air inlet pipe, the raw material air inlet pipe is provided with a branch and is connected with the inlet of the krypton-xenon-lean washing tower, the upper part of the lower tower is provided with the krypton-xenon-lean washing tower, the main condensation evaporator is arranged in the krypton-xenon-lean washing tower, the main condensation evaporator is communicated with the lower tower through a pipeline, the top of the krypton-xenon-lean washing tower and the top of the krypton-xenon-lean concentration tower are respectively communicated with the top of the krypton-xenon-lean washing tower through a pipeline, the outlet of the krypton-xenon-lean washing tower and the bottom of the lower tower are communicated with the upper condensation tower through an oxygen-rich liquid pipe, and the main condensation evaporator is provided with non-krypton-xenon-lean tube; the high-pressure liquid oxygen pump is also provided with a liquid oxygen product outlet pipe, and the liquid oxygen product outlet pipe is connected with the subcooler;
an argon purification system is arranged outside the upper tower, and the argon purification system comprises: the system comprises a crude argon tower and a crude argon condenser, wherein the upper tower is in bidirectional intercommunication through a pipeline of the crude argon tower, the top and the bottom of the crude argon condenser are both communicated with the upper tower through pipelines, the subcooler is connected with the crude argon condenser through a pipeline, and the crude argon condenser is provided with a crude argon outlet pipe;
there is also a second stage krypton-xenon purification system comprising: the device comprises a second-stage krypton-xenon-lean washing tower and a second-stage krypton-xenon-lean evaporator, wherein the top of the second-stage krypton-xenon-lean washing tower is connected with a krypton-xenon-lean concentration tower through a pipeline, a krypton-xenon-lean pipe is communicated with the top of the second-stage krypton-xenon-lean washing tower, an inlet of the second-stage krypton-xenon-lean evaporator is communicated with a raw material air inlet pipe, an outlet of the second-stage krypton-xenon-lean evaporator is connected with an oxygen-enriched liquid pipe, and the bottom of the second-stage krypton-xenon-lean washing tower is provided with a second-stage krypton-xenon-lean pipe; the bottom of the upper tower is provided with a high-pressure liquid oxygen pump, the high-pressure liquid oxygen pump is connected with a high-pressure liquid oxygen outlet pipe, and the high-pressure liquid oxygen outlet pipe is connected with the heat exchanger.
2. The method for extracting krypton and xenon by using the apparatus according to claim 1, comprising the steps of:
s1, rectifying raw material air by a lower tower to obtain oxygen-enriched liquid air;
s2, the oxygen-enriched liquid air is sent to a crude argon tower condenser after decompression and throttling;
s3, rectifying the oxygen-enriched liquid air in the upper tower to obtain liquid oxygen with higher concentration of krypton and xenon;
s4, liquid oxygen firstly enters a lean krypton-xenon washing tower C4 for rectification, and then enters a main condenser K1 for evaporation;
s5, delivering the liquid oxygen evaporated by the main condenser into a krypton-xenon-lean concentration tower and a krypton-xenon-lean evaporator for further evaporation;
s6, obtaining a liquid product containing krypton and xenon at the product outlet ends of the krypton-xenon-lean concentration tower and the krypton-xenon-lean evaporator;
and S7, further processing the product obtained in the last step to the required concentration and state.
3. The method for extracting krypton and xenon according to claim 2, wherein: the step S6 is followed by a second purification process.
4. A method of extracting krypton and xenon according to claim 3, wherein: the portion of the feed air serves as the heat source for the crude argon column.
5. The method for extracting krypton and xenon according to claim 4, wherein: most of the liquid oxygen of the main condenser is refluxed to the bottom of the upper tower, so that the liquid oxygen of the main condensing evaporator maintains a certain circulation rate.
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| CN114353434A (en) * | 2022-03-17 | 2022-04-15 | 杭州制氧机集团股份有限公司 | Device and method for concentrating krypton and xenon through low-temperature rectification |
| CN115839601B (en) * | 2023-02-27 | 2023-05-12 | 中科富海(杭州)气体工程科技有限公司 | Liquid space division and krypton-xenon pre-concentration integrated equipment |
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