EP1231440A1 - Procédé et installation de séparation d'air par distillation cryogénique - Google Patents

Procédé et installation de séparation d'air par distillation cryogénique Download PDF

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Publication number
EP1231440A1
EP1231440A1 EP01129565A EP01129565A EP1231440A1 EP 1231440 A1 EP1231440 A1 EP 1231440A1 EP 01129565 A EP01129565 A EP 01129565A EP 01129565 A EP01129565 A EP 01129565A EP 1231440 A1 EP1231440 A1 EP 1231440A1
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EP
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Prior art keywords
column
liquid
product
pressure
air
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EP01129565A
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German (de)
English (en)
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EP1231440B1 (fr
Inventor
Theo Sentis
Jens Juckel
Thorsten Moeller
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Air Liquide AGS GmbH
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Messer AGS GmbH
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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
    • F25J3/04721—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
    • 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
    • F25J3/04436—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 at least a triple pressure main column system
    • F25J3/04448—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 at least a triple pressure main column system in a double column flowsheet with an intermediate pressure column
    • 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
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • 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.
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • 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
    • 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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/10—Mathematical formulae, modeling, plot or curves; Design methods

Definitions

  • the invention relates to a method and a device for cryogenic decomposition of air for the production of nitrogen, oxygen and argon, according to the features of the preamble of claims 1 and 14.
  • the products rectified from the air are at least partially withdrawn from the rectification system as liquids, conveyed to the desired final pressure by means of conveying devices, such as cryo pumps, and then in a countercurrent heat exchanger network connected to the rectification system Air evaporates to gaseous products, preferably to pressurized nitrogen or pressurized oxygen.
  • the air separation plants designed with an internal compression circuit have the fundamental disadvantage that, depending on the quantities of product withdrawn as a liquid from the rectification system, the process air used is partially liquefied, the amount of which reduces the amount of air rectified in the pressure column of the rectification system, which has the consequence that the separation effort and thus the structural effort in the rectification columns connected to the pressure column increase and / or the product yields and in particular the argon yield decrease.
  • the oxygen-enriched bottom liquid of the pressure column is expanded into an RL flash column equipped with or without rectification devices, a bottom evaporator and a top condenser, and the vapor produced in the expansion in the RL flash column is located between that of the pressure column and the rectified operating pressure of the low pressure column.
  • the RL flash column low-oxygen steam is additionally generated by bottom evaporation with gaseous nitrogen from the pressure column.
  • the bottom liquid formed is merely throttled to form a two-phase mixture, which is then further broken down in the low-pressure column.
  • the throttled bottom liquid or, alternatively, in a particularly advantageous embodiment of US Pat. No.
  • the achievable yield of additional Return is limited by the fact that only a relatively small proportion of the gaseous Compressed nitrogen from the pressure column for heating the bottom evaporator of the RL flash column can be used without the lift current to the lower sections of the low pressure column is lowered so much that the Nitrogen content in the argon side gas rises so much that the crude argon condenser can no longer be operated.
  • the invention is therefore based on the object of a method and a device to create the type mentioned, by means of which an inexpensive Oxygen and nitrogen production with high product yields, especially at connected argon rectification.
  • a heat exchanger network (all of the in the Coldbox involved in cooling the incoming and outgoing process streams Heat exchangers, such as high heat exchangers, subcoolers and LOX evaporators) Pre-cooled process air predominantly in a first partial flow vaporous process air directly and in a second partial flow to the pressure level throttled the pressure column as predominantly liquid process air with the from the Throttling resulting steam flow at least partially into the pressure column fed.
  • Heat exchangers such as high heat exchangers, subcoolers and LOX evaporators
  • the remaining portion of liquid process air not supplied to the pressure column is transferred to the Pressure level of the liquid air column throttled as a liquid and vapor Partial air flow into the liquid air column and as a liquid return to the low pressure column fed.
  • the nitrogen product present at the top of the pressure column with a Residual oxygen content of up to less than 1ppm is at least partially considered vapor and / or liquid product withdrawn from the rectification column.
  • the vaporous top product rectified in the pressure column is by means of the main condenser through indirect heat exchange with evaporating oxygen-rich liquid bottom fraction of the low pressure column at least partially condensed and the condensate obtained at least partially as a return of Pressure column fed.
  • the oxygen-rich liquid bottom product of the pressure column becomes at least partially as a cooling medium in the condenser of the crude argon column and / or as a return in the Low pressure column fed.
  • the media fed into the low pressure column are under a pressure of usually 1.1 to 1.6 bar by means of rectifiers in the form of differently arranged conventional floors and / or ordered Packs or packing in a nitrogen-rich vaporous overhead product and broken down into an oxygen-rich liquid sump product.
  • the bottom liquid evaporated at least partially by means of the main condenser rises in the low pressure column and is countercurrent with trickling liquid rectified.
  • the gaseous low-oxygen crude argon product present at the top of the crude argon column with a maximum of 6 vol .-% residual oxygen is by indirect Heat exchange with liquid process medium, such as with Bottom liquid of the pressure column, at least partly to liquid raw argon condensed and at least partially as a return of the crude argon column fed. At least part of the top product is either vaporized Product directly in front of the head or as a liquid product from the raw argon condenser deducted or possibly after further treatment steps, such as Heating up to ambient temperature of the gaseous crude argon product, Compression to approx.
  • the one with rectifiers in the form of differently arranged ordered packings and / or packing, top condenser and bottom evaporator Equipped pure argon column fed raw argon is under one Operating pressure from 1.1 to 5 bar to a large extent oxygen and Low nitrogen liquid sump product, part of which is a pure argon product less than 1 ppm residual oxygen content and residual nitrogen content from the Deducted pure argon column and the part remaining in the pure argon column Maintaining rectification in the bottom evaporator is evaporated to one rectified nitrogen-rich top product.
  • the sump liquid rectified in the pure argon column is removed using a Gaseous process medium operated bottom evaporator at least partially evaporates and the vaporous nitrogen-rich in the pure argon column Top product by means of sump liquid injected from the liquid air column condensed.
  • the non-condensable gaseous inert part of the nitrogen-rich top product the pure argon column is blown off into the system environment as a purge gas.
  • the one that occurs on the coolant side during operation of the crude argon condenser Steam is fed into the low pressure column.
  • liquid process air is under a pressure that is between the operating pressure of the Pressure and the low pressure column and which is when using liquid air Cooling medium at approx. 2.3 to 2.6 bar, by means of both the upper and arranged below the feed point, as conventional floors and / or orderly packs or packing formed rectifiers in one gaseous low-oxygen head product and in an oxygen-rich Swamp liquid disassembled.
  • the sump liquid rectified in the liquid air column is in one Bottom evaporator partially evaporated to below the feed point liquefied air to enable rectification and thereby the Oxygen content of the bottom liquid and thus the yield of the top product increase.
  • the latent heat of an is advantageous for heating the bottom evaporator predominantly gaseous process medium and / or the sensitive heat of one liquid extracted from the process.
  • bottom liquid finds a current decoupled from the process, such as for example bottom liquid of the pressure column, a vaporous side gas stream or top product stream of the pressure column and particularly preferably a vaporous one Side deduction of the raw argon column use, which individually or in combination a bottom evaporator of the liquid air column can be fed.
  • Feed material itself i.e. pressurized, cryogenic gaseous process air can be used by referring to the pressure levels of the Liquid air column is passed through the bottom evaporator of the liquid air column and there by releasing the sensitive heat contained in the gas stream generated for the liquid air column.
  • the Extracted partial flow of process air from the heat exchanger network which after the Throttling to the pressure level of the compressed air or liquid air column in predominantly is in liquid form, throttled and directly as predominantly liquid process air and completely fed into the pressure column and liquid from the pressure column
  • Side deductions as a coolant for the condenser and as a feed for the liquid air column and as a return for the low pressure column.
  • the entire is made of withdrawn from the heat exchanger network and predominantly after throttling liquid air flow in a operated at the operating pressure of the liquid air column Separation tank that connects directly to the liquid air column via a gas line connected, relaxed into it.
  • the separator container becomes the one at Throttling generated steam and part of the liquid air as feed streams in the liquid air column is fed in, another part of the liquid air is called Cooling medium passed to the condenser of the liquid air column and the remaining part the liquid air as the return liquid into both the low pressure and the Pressure column fed. Because the container is at a sufficient height in the Coldbox is arranged, it is possible to remove liquid from the separation tank solely by using the geodetic height difference in the pressure column feed. This arrangement has proven to be particularly advantageous if Larger quantities of process air are liquefied and / or with throttling high steam is to be expected.
  • the invention further relates to a device according to the features of Claims 14 to 20.
  • a rectifier that is not pretreated by rectification is used in the liquid air column
  • Liquid air flow used which has a higher nitrogen content than that previously according to US Pat. No. 5,715,706 has bottom liquid of the pressure column, whereby with the same oxygen content in the bottom liquid in the liquid air column and RL flash column a higher yield of nitrogen and the resultant additional column return, performance optimization of the liquid air column achieved becomes.
  • the invention can be used particularly advantageously when liquid products, preferably liquid oxygen or nitrogen, from the rectification columns of the Rectification system to be deducted to only liquid products generate or to counter the liquid products with compressed air evaporate (internal compression systems and liquid systems with integrated Air liquefier).
  • liquid products preferably liquid oxygen or nitrogen
  • cryogenic air which due to the throttling to the pressure level of the various rectification columns would be at least partially liquefied conventional process control as return liquid in the pressure or Low pressure column and would feed the reflux conditions in this Only slightly improve the columns.
  • the inventive pre-separation of the liquefied air in the Liquid air column creates a low-oxygen overhead product that is above the Feed point for the liquid air in the low pressure column as additional return can be fed, whereby the with the inventive method achievable argon yield improved by 5 to 10%.
  • Liquid air column is that in the low pressure column is a pure gaseous Nitrogen product can be generated without having to do so in the pressure column accordingly to have to produce low-oxygen washing liquid.
  • the operation of the top condenser with liquefied air ensures that the Operating pressure of the liquid air column only about 1 bar above that of the low pressure column , which means that the separation effort, i.e. the number of Separation stages reduced by up to 10 and / or the required return flow rate reduced and the nitrogen yield in the liquid air column is increased accordingly.
  • the pressure-reduced operation of the liquid air column advantageously results in a Variety of, optimally adapted to the specific rectification system Integration options for the liquid air column.
  • the heat extracted from the system process is extracted using the Bottom evaporator coupled into the liquid air column in such a way that the Oxygen concentration in the bottom liquid of the liquid air column between 45 and Is 70 percent.
  • the heat extracted from the system process is extracted using the Bottom evaporator coupled into the liquid air column in such a way that the Oxygen concentration in the bottom liquid of the liquid air column between 45 and Is 70 percent.
  • Another significant advantage of the invention is that a liquid Side draw or part of the bottom product of the liquid air column for cooling the Head capacitor of the pure argon column can be used. Because of the engagement of the side draw or bottom product of the liquid air column as a condensation medium in the pure argon column this can be the case with conventional process control used for this purpose liquid head product of the pressure column and instead used as additional return liquid in the low pressure column be, whereby the argon yield increases again and / or the Number of separation stages in the low pressure column can be reduced.
  • the liquefied All or part of the air is initially fed into the pressure column and out of the Pressure column in the form of liquid side deductions as an insert medium for the Liquid air column, as well as a condensation medium for the top condenser Liquid air column related and the remaining portion of the liquid air as Return liquid fed into the low pressure column.
  • a procedure in which the liquefied air precedes has proven particularly useful the relaxation and division into the pressure, low pressure and liquid air column passed through an evaporator arranged in the sump of the pressure column and there is pre-cooled by indirect heat exchange, which increases the irreversibility of the Reduce throttling process and by the incomplete theoretical Separating sump evaporator, the yield of top product in the Pressure column is increased.
  • the air separation according to the invention becomes the liquid air column of the rectification system at the greatest possible height in the Coldbox arranged separator tank upstream.
  • the cryogenic liquid air stream under pressure relaxes.
  • the one at the Steam generated in the separating tank is released with a Partial flow of the air liquefied during throttling into the downstream Liquid air column fed.
  • a rectification system shown schematically in Fig. 1 with a pressure and Low pressure column 1, 3 with common main condenser 2 existing Rectification column, which is connected to a crude argon and liquid air column 10, 17 is, the entire process air before it is fed into one of the entirety of all heat exchangers arranged in the cold box, such as, for example, main heat exchangers, Freezer and / or other separate heat exchanger existing Heat exchanger network to a slightly higher pressure level than that of the Pressure column 1, which usually moves between 4 and 6 bar, compresses and at the ambient temperature level of disruptive secondary components such as Steam and carbon dioxide, cleaned.
  • a partial flow of the pre-cleaned air its share of the total air from the amount of liquid or internally compressed depends on gaseous products before being fed into the Heat exchanger network at a pressure that varies according to the required Pressure level of the internally compressed product flows to be extracted from the system straightens and is usually between 10 and 80 bar, post-compressed.
  • the one on the Pressure level of the pressure column 1 available compressed and cleaned Process air is in the heat exchanger network, close to its dew point cooled and as a predominantly vaporous first partial stream 4 via a line 63 directly below rectification devices 47 in the by means of Main condenser 2 with the low pressure column 3 thermally coupled pressure column 1 fed.
  • the second partial flow 5 of the process air which is conveyed to the higher pressure level, becomes also cooled in the heat exchanger network and in a line 64 with throttle 45 relaxed to the pressure level of the pressure column and as a liquid partial air flow 5b together with that created during the relaxation in throttle 45 vaporous partial air flow 5c via a line 65 above the lower one Rectification devices 47 fed into the pressure column 1.
  • throttling becomes any suitable for reducing pressure Device, such as a fitting with moving parts, but also one simple cross-sectional tapering of the line.
  • the in the with Rectifying devices 47 in the form of differently arranged conventional floors and / or ordered packings or packing equipped pressure column 1 below the lower rectification devices 47
  • the predominantly vaporized process air 4 is fed in together with the lower area above the lower rectifying devices 47 of the pressure column 1 injected liquid partial air stream 5b and the vaporous partial air stream 5c in an oxygen-rich liquid bottom product 6 and into a low-oxygen vaporous nitrogen product 7 with a residual oxygen content of usually Disassembled 0.5 - 10 ppm.
  • Nitrogen product is partly over as vaporous pressure nitrogen product 7a a line 40 is drawn off and the product portion remaining in the pressure column 1 in the condenser 2 by means of indirect heat exchange with evaporating liquid bottom product 8 of the low pressure column 3 condensed. That way generated condensate is on a line 9 as the return liquid to the pressure and Low pressure column 1, 3 distributed or as a liquid nitrogen product 7b over a Line 41 withdrawn with a residual oxygen content of 0.5 to 10 ppm.
  • the through the condenser 2 to the operating pressure of the low pressure column 3 from usual 1.2 to 1.6 bar coupled operating pressure of pressure column 1 is between 4 and 6 bar.
  • the sump liquid 6 rectified in the pressure column 1 is replaced by a Throttle 48a equipped line 48 as a return to the low pressure column 3 and via a further line 49 provided with a throttle 49a as cooling liquid in the working at the same operating pressure as the low pressure column 3, in the As a rule, a top condenser 11 of the crude argon column 10 designed as a thermosiphon relaxed into it.
  • the in the rectifier 50 in the form of differently arranged conventional floors and / or ordered Packs or packing equipped low pressure column 3 supplied liquid and gaseous streams are evaporated in the swamp oxygen-rich liquid bottom product 8 at an operating pressure of usually 1.2 to 1.6 bar in a low-oxygen vaporous nitrogen product 12 with a residual oxygen content of 0.2 to 10 ppm and in the oxygen-rich liquid bottom product 8 with an oxygen content of at least 99.5% by volume disassembled.
  • the liquid oxygen product 8a rectified in the low pressure column 3 can be about a line 43 and the vapor present in the low pressure column 3 Oxygen product 8b via a line 42 from the low pressure column 3 for further Deducted use.
  • the one remaining in the low pressure column 3 Residual portion of bottom liquid 8 is used to maintain the rectification indirect heat exchange, usually as a thermosiphon, in special cases also evaporated as a downdraft evaporator, trained condenser 2.
  • From the Low pressure column 3 is in the middle column area, the so-called argon belly, a share of about 30% of the amount of steam rising from the condenser 2 corresponding argon-oxygen mixture 13 with an argon content of usually 8 to 12 vol .-% deducted and via a line 13a in the Raw argon column 10 fed.
  • the in the rectifier 51 in the form of differently arranged shelves and / or ordered packs or Packed crude argon column 10 fed gaseous argon-oxygen mixture is in an oxygen-rich liquid bottom product 15 and in rectified a low-oxygen vaporous crude argon product 14.
  • the Crude argon product 14 is a vaporous or liquid crude argon product 14a, b with a residual oxygen content of 0.2 to 5 vol .-% via a line 33a, 33b the crude argon column 10 deducted for further use.
  • a product vaporized crude argon stream drawn off in front of the crude argon column 10 is in the, usually designed as a thermosiphon capacitor 11 indirect heat exchange with evaporating cooling medium, usually Bottom liquid 6 of the pressure column 1, condensed and back into the Raw argon column 10 fed.
  • the condensation on the coolant side in the Condenser 11 generated steam is through a line 53 in the middle section the low pressure column 3 fed.
  • the one in the liquid air column 17 air streams 5d, e fed in are rectified by means of the rectifying devices 54 into a low-oxygen vaporous nitrogen product 18 with a Residual oxygen content from 0.5 to 10 ppm and into an oxygen-rich liquid Bottom product 19 rectified.
  • the liquid rectified in the liquid air column 17 Bottom product 19 has an oxygen content of 40 to 70% by volume.
  • the liquid partial air flow 5d fed into the liquid air column 17 becomes one predominantly at the level of its feed point from the liquid air column 17 again tapped and via a line 23 with a choke 55 in a top capacitor 22nd the liquid air column 17 fed.
  • the not in the head capacitor 22 of the Liquid air column 17 is fed in liquid air as liquid partial air flow 5f a line 16 by means of throttle 56 in the area of the upper rectification devices 50 of the low pressure column 3 relaxed.
  • the coolant-side operating pressure usually as a thermosiphon trained capacitor 22 is only slightly above the operating pressure of the Low pressure column 3, so that the resulting during the evaporation of the liquid air Steam can be fed into the low pressure column 3 via a line 25.
  • the liquid bath of the top condenser 22 is in a temperature range of air approx. 87 to 89 K, so that the liquid air column 17 at an operating pressure of 2.2 to 2.6 bar can be operated.
  • Nitrogen product 18 is a gaseous, low-oxygen head product 18 c from the Liquid air column 17 deducted and / or by indirect heat exchange in the Top condenser 22 condenses with liquid air which evaporates and partially fed back into the liquid air column 17 as the return liquid.
  • Condensate 18b a line 24 by means of throttle 57 as an additional return above the Rectification devices 50 fed into the low pressure column 3.
  • the portion not evaporated in a bottom evaporator 21 of the liquid air column 17 oxygen-rich liquid bottom product 19 is via a line 58 of the Low pressure column 3 supplied.
  • Figure 2 shows a rectification system, in which in the low pressure column 1 also a pure nitrogen product 12 with a residual oxygen content of 0.5 to 10 ppm is withdrawn, but in which the return liquid 18b required for this is withdrawn exclusively from the liquid air column 17.
  • Rectification system that cooled from the heat exchanger network under one Second air partial flow 5, which is at a pressure of 10 to 80 bar, is not as shown in FIG. 1 throttled to the pressure level of the pressure column, but before the pressure drop in the throttle 46a by means of a line 66 to the bottom evaporator 21 and through indirect heat exchange with evaporating bottom liquid pre-cooled and then passed via line 46 to the throttle 46a and on the Pressure level of the liquid air column 17 relaxed.
  • a partial flow of the liquefied air is released a side drain liquid air column 17 withdrawn again and as a cooling liquid for the condenser 22 and as a return liquid for the low pressure column 3 used.
  • FIG. 3 shows a rectification system according to the invention, in which in contrast to the rectification system shown in Figure 1, part of the bottom product 19 of the Liquid air column 17 via a line 59 as a cooling medium in a condenser 31 a pure argon column equipped with conventional rectifying devices 39 32 is fed, the coolant-side operating pressure of the usually as Thermosiphon trained pure argon condenser 31 only slightly above of the operating pressure of the low pressure column 3 is that that used evaporating bottom liquid 19 together with the steam flow from the Raw argon condenser 11 can be fed back into the low pressure column 3.
  • a liquid is introduced into the pure argon column 32 via the line 33b
  • Oxygen-free crude argon product 14b that is fed into a nitrogen and oxygen-free bottom product 34 and a nitrogen-rich top product 35 rectified becomes.
  • the top product 35 is in the form of a gaseous inert stream 38 via a Throttle 38a provided line 29 drawn off and blown into the environment.
  • Out the separating tank 27 is also at least one other part the liquid partial air stream 5d withdrawn via line 59 and into the Liquid air column 17 fed.
  • the withdrawal of cooling medium for the condenser 22 the liquid air column 17 and the return liquid 5f are carried out as already shown in FIG. 1 shown as a side vent from the liquid air column 17 could alternatively also directly done from the separator tank 27.
  • FIG. 4 shows a graphic representation of the irreversibilities in the crude argon column 10 for operation with and without side capacitor 11.
  • the ordinate individual floors and on the abscissa the exergy loss as a measure of the Irreversibility applied to every floor. It can be seen that the area under the curve for the exergy loss of the crude argon column 10 with side deduction clearly is smaller than the curve for a crude argon column 10 without a side draw.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
EP01129565A 2000-12-12 2001-12-12 Procédé et installation de séparation d'air par distillation cryogénique Expired - Lifetime EP1231440B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10061908A DE10061908A1 (de) 2000-12-12 2000-12-12 Verfahren und Vorrichtung zur Tieftemperaturzerlegung von Luft
DE10061908 2000-12-12

Publications (2)

Publication Number Publication Date
EP1231440A1 true EP1231440A1 (fr) 2002-08-14
EP1231440B1 EP1231440B1 (fr) 2007-07-18

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EP01129565A Expired - Lifetime EP1231440B1 (fr) 2000-12-12 2001-12-12 Procédé et installation de séparation d'air par distillation cryogénique

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EP (1) EP1231440B1 (fr)
AT (1) ATE367563T1 (fr)
DE (2) DE10061908A1 (fr)
PT (1) PT1231440E (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102008016355A1 (de) 2008-03-29 2009-10-01 Linde Ag Verfahren und Vorrichtung zur Tieftemperaturzerlegung von Luft
WO2024026165A1 (fr) * 2022-07-28 2024-02-01 Praxair Technology, Inc. Système et procédé de séparation d'air cryogénique utilisant quatre colonnes de distillation comprenant une colonne de pression intermédiaire
WO2024026168A1 (fr) * 2022-07-28 2024-02-01 Praxair Technology, Inc. Unité de séparation d'air et procédé de séparation cryogénique d'air à l'aide d'un système de colonne de distillation comprenant une colonne de cuve à pression intermédiaire
US11959701B2 (en) 2022-07-28 2024-04-16 Praxair Technology, Inc. Air separation unit and method for production of high purity nitrogen product using a distillation column system with an intermediate pressure kettle column

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5878310B2 (ja) * 2011-06-28 2016-03-08 大陽日酸株式会社 空気分離方法及び装置
EP2597409B1 (fr) * 2011-11-24 2015-01-14 L'AIR LIQUIDE, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Procédé et installation pour la séparation de l'air par distillation cryogénique
JP5655104B2 (ja) 2013-02-26 2015-01-14 大陽日酸株式会社 空気分離方法及び空気分離装置
CN114949897B (zh) * 2022-06-22 2023-06-27 安徽佳先功能助剂股份有限公司 一种尼龙酸二异丁酯的连续脱水蒸馏装置

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US4717409A (en) * 1985-05-17 1988-01-05 The Boc Group Plc Liquid vapor contact method and apparatus
EP0694744A1 (fr) * 1994-07-25 1996-01-31 The BOC Group plc Séparation de l'air
EP0752565A2 (fr) * 1995-07-06 1997-01-08 The BOC Group plc Production d'argon

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
US4717409A (en) * 1985-05-17 1988-01-05 The Boc Group Plc Liquid vapor contact method and apparatus
EP0694744A1 (fr) * 1994-07-25 1996-01-31 The BOC Group plc Séparation de l'air
EP0752565A2 (fr) * 1995-07-06 1997-01-08 The BOC Group plc Production d'argon

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102008016355A1 (de) 2008-03-29 2009-10-01 Linde Ag Verfahren und Vorrichtung zur Tieftemperaturzerlegung von Luft
WO2024026165A1 (fr) * 2022-07-28 2024-02-01 Praxair Technology, Inc. Système et procédé de séparation d'air cryogénique utilisant quatre colonnes de distillation comprenant une colonne de pression intermédiaire
WO2024026168A1 (fr) * 2022-07-28 2024-02-01 Praxair Technology, Inc. Unité de séparation d'air et procédé de séparation cryogénique d'air à l'aide d'un système de colonne de distillation comprenant une colonne de cuve à pression intermédiaire
US11959701B2 (en) 2022-07-28 2024-04-16 Praxair Technology, Inc. Air separation unit and method for production of high purity nitrogen product using a distillation column system with an intermediate pressure kettle column

Also Published As

Publication number Publication date
PT1231440E (pt) 2007-10-12
DE50112737D1 (de) 2007-08-30
EP1231440B1 (fr) 2007-07-18
DE10061908A1 (de) 2002-06-27
ATE367563T1 (de) 2007-08-15

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