EP1482266A1 - Procédé et dispositif pour la récupération de Krypton et/ou Xénon par séparation cryogénique d'air - Google Patents
Procédé et dispositif pour la récupération de Krypton et/ou Xénon par séparation cryogénique d'air Download PDFInfo
- Publication number
- EP1482266A1 EP1482266A1 EP20040011942 EP04011942A EP1482266A1 EP 1482266 A1 EP1482266 A1 EP 1482266A1 EP 20040011942 EP20040011942 EP 20040011942 EP 04011942 A EP04011942 A EP 04011942A EP 1482266 A1 EP1482266 A1 EP 1482266A1
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- EP
- European Patent Office
- Prior art keywords
- krypton
- xenon
- column
- liquid
- crude argon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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.
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
- 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
- F25J3/04084—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 nitrogen
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
- 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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- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
- F25J3/04218—Parallel arrangement of the main heat exchange line in cores having different functions, e.g. in low pressure and high pressure cores
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- 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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
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- 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
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- 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
- F25J3/0469—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 and an intermediate re-boiler/condenser
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
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- F25J3/04642—Recovering noble gases from air
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- 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
- F25J3/04703—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 being arranged in more than one vessel
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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
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- 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
- F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
- F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
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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
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- 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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- 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
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- 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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen
-
- 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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/58—Processes or apparatus involving steps for recycling of process streams the recycled stream being argon or crude argon
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2250/00—Details related to the use of reboiler-condensers
- F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2250/00—Details related to the use of reboiler-condensers
- F25J2250/04—Down-flowing type boiler-condenser, i.e. with evaporation of a falling liquid film
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2250/00—Details related to the use of reboiler-condensers
- F25J2250/10—Boiler-condenser with superposed stages
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2250/00—Details related to the use of reboiler-condensers
- F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
Definitions
- the invention relates to a method for obtaining krypton and / or xenon by Cryogenic decomposition of air according to the preamble of patent claim 1.
- the basics of cryogenic decomposition of air in general as well as the Structure of rectification systems for nitrogen-oxygen separation in particular are in the monograph "Tiefftemperaturtechnik” by Hausen / Linde (2nd edition, 1985) and in an essay by Latimer in Chemical Engineering Progress (Vol. 63, No.2, 1967, Page 35).
- the high pressure column is under operated at a higher pressure than the low pressure column; the two columns are standing preferably in heat exchange relationship with each other, for example via a Main condenser, in the top gas of the high-pressure column against evaporating Bottom fluid of the low pressure column is liquefied.
- the rectification system of Invention can be designed as a classic double column system, but also as Three or more column system.
- In addition to the columns for nitrogen-oxygen separation may be other devices for obtaining other air components, in particular of noble gases, for example an argon production.
- a method for obtaining krypton and / or xenon by Cryogenic separation of air and a corresponding device are off DE 10000017 A1.
- a krypton and xenon Tra fraction namely the bottom liquid, from the high-pressure column of the double column to the nitrogen-oxygen separation without concentration-changing measures in another Column, which serves for krypton-xenon recovery.
- the invention is based on the object, the krypton and xenon recovery on to improve and in particular to carry out in a particularly economical manner.
- This object is achieved in that the second feed air flow downstream its work-inducing relaxation into the krypton-xenon enrichment column is initiated.
- Krypton and xenon are introduced into the krypton-xenon concentrate. He surrenders a particularly high yield of krypton and / or xenon. It is the Investment needs relatively low, because no additional column for washing out Krypton and xenon are needed from the work-performing relaxed air, as is the case with EP 1308680 A1 (local Figure 4) is the case, but this air directly into the anyway existing krypton-xenon enrichment column is introduced, preferably having a bottom evaporator.
- the feed point of the air is preferably in lower portion of the krypton-xenon enrichment column, for example immediately above the swamp or one to five. preferably one to three floors above.
- the krypton-xenon enrichment column serves additionally for washing out krypton and xenon from the feed air, which works was relaxed.
- the condensate flows back into the first crude argon column and does not need in the second crude argon column, from in this Case the crude argon product is withdrawn. Corresponding the sales in the second crude argon column decreases. This can be done accordingly be executed cheaper.
- the invention also relates to a device for obtaining krypton and / or Xenon by cryogenic separation of air according to claims 7 and 8.
- compressed air flows in. It is divided into a first air flow (direct air) 102, a second air flow (turbine air) 103 and a third air flow (internal compression air) 104.
- the main heat exchanger has three parallel blocks 105a, 105b, 105c in the exemplary embodiment.
- the first air stream 102 is cooled in all three blocks 105a, 105b, 105c of the main heat exchanger to about dew point and introduced without further pressure-changing measures via line 1 in gaseous form in the high pressure column 2 of a rectification system for nitrogen-oxygen separation.
- the rectification system for nitrogen-oxygen separation also has a low-pressure column 3 and a main condenser 4, which in the example is designed as a combined falling-film and bath evaporator.
- Gaseous nitrogen 6 from the head of the high-pressure column is fed to the condensation space of the main condenser 4.
- the condensate 7 formed there is introduced into the high-pressure column and used there as reflux.
- Some theoretical plates deeper liquid nitrogen 106 is removed from the high pressure column 2 and branched at 107.
- a first branch stream of liquid nitrogen is recovered via line 114 as a liquid nitrogen product (LIN).
- Another branch stream 111 of the liquid nitrogen from the high-pressure column 2 is brought to a desired product pressure in a liquid state pump 112, vaporized in the main heat exchanger block 105a (pseudo-vaporized in the case of supercritical pressure) and warmed to about ambient temperature and via line 113 discharged as gaseous pressure product (PGAN).
- the third air stream 104 which has been brought to a correspondingly high pressure in a secondary compressor 115 with aftercooler 116, serves to vaporize the nitrogen which has been brought to liquid pressure.
- impure liquid nitrogen becomes some theoretical soils below of the head taken from the high pressure column 2, in the subcooling countercurrent 10th subcooled and via line 11 and throttle valve 12 of the low pressure column 3 at the top fed.
- the liquefied or supercritical cold as part of the internal compression High pressure air 117 is at least partially in liquid via valve 118 and line 44 Form throttled into the high-pressure column 2, and that at a first intermediate point some theoretical soils above the high pressure column bottoms. From a second Intermediate point, which in turn has some theoretical soil above this first Intermediate point is arranged, an oxygen-containing liquid 45 from the High pressure column deducted, which hardly ever volatile components like especially krypton and xenon.
- the in the subcooling countercurrent 10 cooled liquid is via line 46 and throttle valve 47 in the Low pressure column 3 fed.
- the oxygen-enriched bottoms liquid 13 of the high-pressure column 2 also becomes cooled in the subcooling countercurrent 10.
- the supercooled oxygen-enriched Liquid 14-15 is further cooled in a pure argon evaporator 63 and becomes finally to a part via line 16 and 16a in the evaporation space of a Rohargon top condenser 17 a Rohargonrektbericht 18/19 introduced.
- On another part 16b of the supercooled oxygen-containing liquid 16 is introduced into the Evaporation space of a top condenser 21 of a pure argon column 22 is fed.
- the crude argon top condenser 17 is designed as a circulation evaporator, that is the evaporation chamber contains a liquid bath into which a heat exchanger block at least partially, preferably completely submerged (not shown). Liquid is due to the thermosiphon effect at the bottom of the Sucked in evaporation passages. At the upper end of a mixture exits Steam and undiluted liquid, the latter in the liquid bath flowing back.
- the oxygen-enriched Fraction 16a partially evaporated; for example, 0.5 to 10 mol%, preferably 1 to 5 mol% of the introduced liquid 16a become liquid as rinsing liquid 26 from the Evaporating the Rohargon top condenser 17 subtracted.
- impure nitrogen 33 in gaseous form and oxygen 34 in liquid form at least partially as products or residual gas deducted.
- the gaseous impurity nitrogen 33 is in the subcooling countercurrent 10 and warmed in the main heat exchanger 105a / 105c.
- the liquid oxygen 34 is divided into two parts. A first part 35 is withdrawn as a liquid product (LOX), optionally after partial supercooling in the subcooling countercurrent 10 (not shown).
- the second part 41 of the liquid oxygen 34 from the bottom of the low-pressure column 3 is - similar to the liquid nitrogen 111 from the high pressure column - a Subjected to internal compression (internal compression) by in a pump 42 on brought the desired product pressure and via line 43 the Main heat exchanger (block 105a) flows in, where it evaporates (or - at supercritical product pressure - pseudo-evaporated) and at about ambient temperature is warmed up. Finally, it is sent via line 120 as a gaseous oxygen pressure product won. Evaporation and warming become indirect Heat exchange with the high pressure air stream 104 - 117 carried out.
- Another oxygen stream 93 is directly gaseous from the low pressure column. 3 withdrawn, warmed in the heat exchanger blocks 105a, 105b and finally withdrawn via line 94 as a non-pressurized gas product (GOX).
- GOX non-pressurized gas product
- the rising steam enriches to argon.
- a another portion 82 of the overhead gas 81 serves as a heating means for the bottom evaporator 27 of the krypton-xenon enrichment column 24, is in the Liquefaction space introduced and condensed there.
- the generated liquid 83 is charged as reflux liquid to the first crude argon column 18.
- the accumulating in the bottom of the second Rohargonkla 19 liquid 52 is by means of a pump 53 via line 54 to the head of the first crude argon column 18 promoted.
- Bottom liquid 55 of the first crude argon column 18 flows via a further pump 56 and line 57 back to the low pressure column 3.
- Gaseous remaining crude argon 58 from the liquefaction space of the condenser-evaporator 17 is further decomposed in the pure argon column 22, in particular of volatiles such as nitrogen released.
- Reinargon product (LAR) becomes withdrawn via the lines 59 and 60 in liquid form.
- Another part 61 of the Bottom liquid of the pure argon column 22 is in the above-mentioned pure argon evaporator 63 evaporated with connected separator 62 and 64 via line as ascending steam returned to the pure argon column 22.
- the top condenser 21 of the pure argon column is as already described by a supercooled liquid 16b cooled. From the evaporation room of the Top condenser 21, vapor 66 and remaining liquid 65 are withdrawn. The steam 66 is at a suitable intermediate point in the low pressure column. 3 fed. The virtually krypton and xenon-free liquid 65 is applied to the Krypton-xenon enrichment column 24 abandoned. In the liquefaction room of Top condenser 21 condenses overhead gas 67 of the pure argon column 22 partially. there generated reflux liquid 68 is applied to the pure argon column. residual steam 69 is blown off into the atmosphere.
- the second air stream 103 is in a turbine-driven booster 85 with Aftercooler 86 further compressed, in the main heat exchanger block 105 a to a Cooled intermediate temperature and relaxed work in an air turbine 87.
- the expanded air 88 is introduced via line 88 into the krypton-xenon enrichment column 24 blown.
- a krypton-xenon concentrate 30 in liquid form taken (crude Kr / Xe), for example, a krypton content of about 2400 ppm and a xenon content of about 200 ppm contains: Otherwise, there is the concentrate 30 mainly from oxygen and contains for example still about 10 to 40 mol% Nitrogen and hydrocarbons.
- the concentrate 30 may be in a liquid tank stored or directly to further processing to obtain pure krypton and / or xenon are supplied.
- Equalizing currents 96, 97 are provided.
- FIG. 1 also shows an additional column 89 to Obtaining Helium Neon Concentrate 90, 91 (crude HeNe) from not condensed nitrogen vapor 92, which is withdrawn from the main condenser 4.
- This helium-neon extraction is basically independent of the Krypton-xenon recovery according to the invention.
- compressed air flows in. It is divided into a first air flow (direct air) 102, a second air flow (turbine air) 103 and a third air flow (internal compression air) 104.
- the main heat exchanger has two parallel blocks 105a, 105b in the exemplary embodiment.
- the first air stream 102 is cooled in both blocks 105a and 105b of the main heat exchanger to about dew point and introduced without further pressure-changing measures via line 1 in gaseous form in the high pressure column 2 of a rectification system for nitrogen-oxygen separation.
- Another branch stream 111 of the liquid nitrogen from the top of the high-pressure column 2 (or main condenser 4) is brought to a desired product pressure in a liquid state pump 112, vaporized in the main heat exchanger block 105a (or pseudo-vaporized in the case of supercritical pressure) and warmed to about ambient temperature and discharged via line 113 as gaseous pressure product (PGAN).
- the third air stream 104 which has been brought to a correspondingly high pressure in a secondary compressor 115 with aftercooler 116, serves to vaporize the nitrogen which has been brought to liquid pressure.
- impure liquid nitrogen becomes some theoretical soils below of the head taken from the high pressure column 2, in the subcooling countercurrent 10th subcooled and via line 11 and throttle valve 12 of the low pressure column 3 at the top fed.
- the liquefied or supercritical cold as part of the internal compression High pressure air 117 is at least partially in liquid via valve 118 and line 44 Form throttled into the high-pressure column 2, namely at a "first intermediate point” some theoretical soils above the high pressure column bottoms. From a “second Intermediate point ", which in turn has some theoretical soil above this first Intermediate point is arranged, an oxygen-containing liquid 45 from the High pressure column deducted, which hardly ever volatile components like especially krypton and xenon.
- the in the subcooling countercurrent 10 cooled liquid 119 is partially via line 46 and throttle valve 47 in the Low pressure column 3 fed. Another part of the 20 supercooled oxygenated Liquid 119 is in the evaporation space of a top condenser 21 a Reinargonkla 22 fed.
- the oxygen-enriched bottoms liquid 13 of the high-pressure column 2 also becomes cooled in the subcooling countercurrent 10.
- the supercooled oxygen-enriched Liquid 14-15 is further cooled in a pure argon evaporator 63 and becomes finally via line 16 into the evaporation space of a crude argon top condenser 17 introduced the head condenser of a Rohargonrektbericht 18/19 represents.
- the oxygen-enriched fraction 16 is partially vaporized; for example, 0.5 to 10 mol%, preferably 1 to 5 mol% of the introduced liquid 16 become liquid as rinsing liquid 26 from the evaporation space of the crude argon top condenser 17 deducted. Due to this partial evaporation, the concentration of less volatile components, in particular of krypton and xenon, in the Increased liquid and reduced in the vapor (in each case in comparison to Composition of the oxygen-enriched fraction 16). The at the partial Evaporation generated steam is called gaseous stream 25 from the Evaporating the Rohargon top condenser 17 subtracted. remaining Liquid is discharged as "rinsing liquid" 26 from the liquid bath and the Krypton-xenon enrichment column 24 fed immediately above the bottom.
- the low pressure column 3 Of the low pressure column 3 are impure nitrogen 33 in gaseous form and oxygen 34 in liquid form at least partially as products or residual gas deducted.
- the gaseous impurity nitrogen 33 is released together with flash gas 110 the separator 109 in the subcooling countercurrent 10 and in the main heat exchanger 105a / 105b warmed up.
- the liquid oxygen 34 is divided into three parts divided up. A first and a second part are first together via line 35 and pump 36 promoted.
- the first part 37 flows to the evaporation space of the Main capacitor 4 and is partially evaporated there.
- the resulting vapor-liquid mixture 38 flows back to the bottom of the low-pressure column 3.
- the second part is withdrawn as a liquid product (LOX), after Partial subcooling in the subcooling countercurrent 10.
- the third part 41 of the liquid oxygen 34 from the bottom of the low-pressure column 3 is - Similar to the liquid nitrogen 111 from the high pressure column - an internal compression (Internal compression) by in a pump 42 to the desired Brought product pressure and via line 43 the main heat exchanger (block 105a) flows where it evaporates (or - in the case of supercritical product pressure - pseudo-evaporated) and warmed to about ambient temperature. In the end it is recovered via line 120 as a gaseous oxygen pressure product. Evaporation and warming are in indirect heat exchange with the High pressure air flow 104 - 117 performed.
- Internal compression Internal compression
- the rising steam enriches to argon.
- the top gas of the first crude argon column 18 flows via line 49 on to the bottom of the second crude argon column 19.
- the accumulating in the bottom of the second Rohargonkla 19 liquid 52 is by means of a pump 53 via line 54 to the head of the first crude argon column 18 promoted.
- Bottom liquid 55 of the first crude argon column 18 flows via a further pump 56 and line 57 back to the low pressure column 3.
- Gaseous crude argon 58 from the liquefaction space of the crude argon overhead condenser 17 is further decomposed in the pure argon column 22, in particular of volatiles such as nitrogen released.
- Reinargon product (LAR) becomes withdrawn via the lines 59 and 60 in liquid form.
- Another part 61 of the Bottom liquid of the pure argon column 22 is in the above-mentioned pure argon evaporator 63 evaporated with connected separator 62 and 64 via line as ascending steam returned to the pure argon column 22.
- the top condenser 21 of the pure argon column is as already described by a supercooled liquid 20 cooled. From the evaporation space of the top condenser 21, vapor 66 and remaining liquid 65 are withdrawn. The steam 66 is on suitable intermediate point fed into the low-pressure column 3. The - practical Krypton and xenon-free liquid 65 is applied to the krypton-xenon enrichment column 24 abandoned. In the liquefaction space of the top condenser 21 overhead gas 67 of the pure argon column 22 partially condenses. It generated Return liquid 68 is charged to the pure argon column. Residual steam 69 is in the atmosphere was blown off.
- the second air stream 103 is in a turbine-driven booster 85 with Aftercooler 86 further compressed, in the main heat exchanger block 105 a to a Cooled intermediate temperature and relaxed work in an air turbine 87.
- the expanded air 88 is introduced via line 88 into the krypton-xenon enrichment column 24 blown.
- the latter is in the embodiment of the low-pressure column 3 at a suitable intermediate point fed.
- a krypton-xenon concentrate 30 in liquid form taken (crude KrXe), for example, a krypton content of about 2400 ppm and a xenon content of about 200 ppm contains: Otherwise, there is the concentrate 30 mainly from oxygen and still contains about 10 mol% of nitrogen as well Hydrocarbons.
- the concentrate 30 may be stored in a liquid tank or directly to further processing to obtain pure krypton and / or xenon be supplied.
- FIG. 3 does not differ from FIG. 2 with regard to the sequence of the method steps.
- the arrangement of the krypton-xenon enrichment column 24 is different. While it is mounted in FIG. 2 as a separate container above the first crude argon column 18, it is located in FIG. 3 between the crude argon top condenser 17 and the mass transfer region of the second crude argon column 19.
- Krypton-xenon enrichment column 24 and second crude argon column 19 thus to some extent form one Double column with the second condenser-evaporator as "main condenser". Since the krypton-xenon enrichment column and the crude argon columns 18, 19 have a similar diameter, such an arrangement can be particularly favorable in terms of apparatus.
- the pure argon column 22 is arranged lower than in FIG. 2, so that the liquid 65 has to flow upwards.
- the evaporation space of the top condenser 21 of the pure argon column 22 is operated at a slightly higher pressure than in FIG. 2, so that the flushing liquid 65 is forced into the krypton-xenon enrichment column due to the corresponding pressure gradient.
- a corresponding pressure difference is maintained in the gas line 66 through the control flap 294.
- the pure argon column of Figure 5 is also lower than in Figure 2. However, no increased pressure in the evaporation space of the top condenser 21 is required because the rinsing liquid 465 is introduced from the top condenser 21 of the pure argon column 22 directly at an intermediate point 492 in the low pressure column 3, the lower than the capacitor 21 is located.
- the feed liquid 493 for the krypton-xenon enrichment column is branched off here already upstream of the top condenser 21 from the liquid 20, which was withdrawn via the lines 45 and 119 from the second intermediate point of the high-pressure column 2. Another part of this liquid 20 flows into the evaporation space of the top condenser 21 of the pure argon column 22.
- the invention may be used as the main capacitor instead of in the Drawings illustrated falling film evaporator 4 a combination of Falling film evaporator and circulation evaporator are used, the evaporation side connected in series.
- the invention may have a further advantage cause: That only a very small amount of low volatility Components of the air enters the low pressure column, the circulation pump 36 for the falling film evaporator can be saved.
- the fluid to be evaporated flows from above down through the evaporation chamber and is partially evaporated.
- a “Circulation evaporator” also called liquid bath evaporator
- the Heat exchanger block in a liquid bath of the fluid to be evaporated. This flows through the thermosiphon effect from bottom to top through the Evaporation passages and exits above as a two-phase mixture again.
- the Remaining liquid flows outside the heat exchanger block in the Liquid bath back. (In a circulation evaporator, the evaporation space both the evaporation passages and the outer space around the Include heat exchanger block.)
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- Mechanical Engineering (AREA)
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- Separation By Low-Temperature Treatments (AREA)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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DE2003134560 DE10334560A1 (de) | 2003-05-28 | 2003-07-29 | Verfahren und Vorrichtung zur Gewinnung von Krypton und/oder Xenon durch Tieftemperaturzerlegung von Luft |
EP20040011942 EP1482266B1 (fr) | 2003-05-28 | 2004-05-19 | Procédé et dispositif pour la récupération de Krypton et/ou Xénon par séparation cryogénique d'air |
Applications Claiming Priority (7)
Application Number | Priority Date | Filing Date | Title |
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DE10324542 | 2003-05-28 | ||
DE10324542 | 2003-05-28 | ||
DE10334560 | 2003-07-29 | ||
DE2003134560 DE10334560A1 (de) | 2003-05-28 | 2003-07-29 | Verfahren und Vorrichtung zur Gewinnung von Krypton und/oder Xenon durch Tieftemperaturzerlegung von Luft |
EP03022546 | 2003-10-02 | ||
EP03022546 | 2003-10-02 | ||
EP20040011942 EP1482266B1 (fr) | 2003-05-28 | 2004-05-19 | Procédé et dispositif pour la récupération de Krypton et/ou Xénon par séparation cryogénique d'air |
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EP1482266A1 true EP1482266A1 (fr) | 2004-12-01 |
EP1482266B1 EP1482266B1 (fr) | 2010-01-20 |
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EP2801777A1 (fr) | 2013-05-08 | 2014-11-12 | Linde Aktiengesellschaft | Installation de décomposition de l'air dotée d'un entraînement de compresseur principal |
DE102013017590A1 (de) | 2013-10-22 | 2014-01-02 | Linde Aktiengesellschaft | Verfahren zur Gewinnung eines Krypton und Xenon enthaltenden Fluids und hierfür eingerichtete Luftzerlegungsanlage |
EP2963367A1 (fr) | 2014-07-05 | 2016-01-06 | Linde Aktiengesellschaft | Procédé et dispositif cryogéniques de séparation d'air avec consommation d'énergie variable |
EP2963371B1 (fr) | 2014-07-05 | 2018-05-02 | Linde Aktiengesellschaft | Procede et dispositif de production d'un produit de gaz sous pression par decomposition a basse temperature d'air |
EP2963369B1 (fr) | 2014-07-05 | 2018-05-02 | Linde Aktiengesellschaft | Procede et dispositif cryogeniques de separation d'air |
PL2963370T3 (pl) | 2014-07-05 | 2018-11-30 | Linde Aktiengesellschaft | Sposób i urządzenie do kriogenicznego rozdziału powietrza |
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DE2605305A1 (de) * | 1976-02-11 | 1977-08-18 | Messer Griesheim Gmbh | Verfahren zur gewinnung von krypton und xenon |
EP1308680A1 (fr) * | 2001-10-31 | 2003-05-07 | Linde AG | Procédé et dispositif de production de krypton et/ou xénon par distillation cryogénique de l'air |
EP1376037A1 (fr) * | 2002-06-24 | 2004-01-02 | Linde Aktiengesellschaft | Procédé et dispositif de séparation d'air avec une colonne de mélange et récupération de krypton et xénon |
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2003
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DE2605305A1 (de) * | 1976-02-11 | 1977-08-18 | Messer Griesheim Gmbh | Verfahren zur gewinnung von krypton und xenon |
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EP2312248A1 (fr) | 2009-10-07 | 2011-04-20 | Linde Aktiengesellschaft | Procédé et dispositif de production d'oxygène sous pression et de crypton/xénon |
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RU2700970C2 (ru) * | 2014-10-16 | 2019-09-24 | Линде Акциенгезелльшафт | Способ варьируемого получения аргона путем низкотемпературного разложения |
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WO2016058666A1 (fr) * | 2014-10-16 | 2016-04-21 | Linde Aktiengesellschaft | Procédé et dispositif de récupération variable d'argon par fractionnement à basse température |
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CN108362074A (zh) * | 2018-03-26 | 2018-08-03 | 四川空分设备(集团)有限责任公司 | 一种从特大型空分设备中提取氪和氙的方法和装置 |
CN108413706A (zh) * | 2018-05-15 | 2018-08-17 | 瀚沫能源科技(上海)有限公司 | 一种氪氙浓缩和氖氦浓缩含循环氮气的整合装置及方法 |
CN108413706B (zh) * | 2018-05-15 | 2023-10-03 | 瀚沫能源科技(上海)有限公司 | 一种氪氙浓缩和氖氦浓缩含循环氮气的整合装置及方法 |
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CN115839601A (zh) * | 2023-02-27 | 2023-03-24 | 中科富海(杭州)气体工程科技有限公司 | 液体空分及氪氙预浓缩一体化设备 |
CN115839601B (zh) * | 2023-02-27 | 2023-05-12 | 中科富海(杭州)气体工程科技有限公司 | 液体空分及氪氙预浓缩一体化设备 |
Also Published As
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DE10334560A1 (de) | 2004-12-16 |
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