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EP1403602A1 - Procédé et dispositif pour la production d'azote ultra pur - Google Patents

Procédé et dispositif pour la production d'azote ultra pur Download PDF

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Publication number
EP1403602A1
EP1403602A1 EP02023334A EP02023334A EP1403602A1 EP 1403602 A1 EP1403602 A1 EP 1403602A1 EP 02023334 A EP02023334 A EP 02023334A EP 02023334 A EP02023334 A EP 02023334A EP 1403602 A1 EP1403602 A1 EP 1403602A1
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EP
European Patent Office
Prior art keywords
pressure column
low
column
fraction
oxygen
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.)
Withdrawn
Application number
EP02023334A
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German (de)
English (en)
Inventor
Ralph Spöri
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linde GmbH
Original Assignee
Linde GmbH
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Filing date
Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Publication of EP1403602A1 publication Critical patent/EP1403602A1/fr
Withdrawn legal-status Critical Current

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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
    • F25J3/04151—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
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • F25J3/04212—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product and simultaneously condensing vapor from a column serving as reflux within the or another 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
    • F25J3/04006—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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)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
    • 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
    • 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
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
    • 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
    • F25J2200/20—Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • 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
    • F25J2200/32—Processes or apparatus using separation by rectification using a side column fed by a stream from the high 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
    • 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
    • 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
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • 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
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • 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
    • F25J2235/42—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being nitrogen
    • 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
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/42—One fluid being nitrogen

Definitions

  • the invention relates to a process for the production of high-purity nitrogen by low-temperature separation of air in a rectification column system which has a high-pressure column and a low-pressure column, in which process feed air is introduced into the high-pressure column, an oxygen-enriched fraction is removed from the high-pressure column and fed into the low-pressure column and a highly pure nitrogen fraction is removed from the low pressure column and discharged as a product.
  • a particularly high nitrogen purity is achieved with regard to more volatile impurities, in particular hydrogen, by withdrawing the nitrogen product from a number of trays (so-called barrier trays) below the top of the low-pressure column. The more volatile components are removed from the top of the low pressure column with a flushing stream.
  • the highly pure nitrogen product in the known processes still contains more volatile impurities such as hydrogen, which until now could only be reduced by appropriate measures in the pre-cleaning of air, which require a high level of equipment.
  • the invention is therefore based on the object of further increasing the purity of the highly pure nitrogen product and at the same time making do with a moderate outlay on equipment.
  • This object is achieved in that the oxygen-enriched fraction is subjected to a cleaning step to remove more volatile impurities before it is introduced into the low-pressure column.
  • the more volatile impurities accumulate not only in the upper region of the low pressure column, but also be entered with the oxygen-enriched fraction in the low pressure column, which is necessarily introduced below the removal of the nitrogen product.
  • this fraction of more volatile constituents is depleted from the air, their hydrogen content, for example, is surprisingly so high that it has an influence on the purity of the nitrogen product.
  • the targeted purification according to the invention of the oxygen-enriched fraction before it is introduced into the low-pressure column effectively prevents the entry of more volatile impurities into the low-pressure column below the removal of the highly pure nitrogen product.
  • the entire oxygen-enriched product of the high-pressure column can be moved into the low-pressure column without this reducing the product purity.
  • the air factor ratio between product and application quantity
  • the high purity nitrogen product can be kept clean even when there is an increased hydrogen concentration in the feed air.
  • oxygen-enriched A fraction that has a higher oxygen content than the atmospheric air is referred to here as “oxygen-enriched”. This can be, for example, 25 to 40 mol%, preferably 30 to 35 mol%.
  • Volatile impurities are understood to mean air components which have a lower boiling point than nitrogen, for example hydrogen, neon and / or helium.
  • any cleaning method can be used in the invention.
  • the oxygen-enriched fraction is introduced into a separation column in the cleaning step to remove more volatile impurities and is purified there by countercurrent mass transfer.
  • the separation column is preferably designed as an output column.
  • the oxygen-enriched fraction is introduced in liquid form into the upper region of the separation column.
  • Rising steam can be formed, for example, by a sump evaporator.
  • a gaseous fraction from the low pressure column is introduced as rising steam into the lower area of the separation column.
  • the cleaned oxygen-enriched fraction is removed from the lower area of the separation column and from there introduced into the low pressure column.
  • the separation column is operated, for example, at approximately the same pressure as the low-pressure column, so that the oxygen-enriched fraction flows into the low-pressure column without the aid of a pump or other conveying means.
  • the feed preferably takes place at the same point at which the gaseous fraction which rises in the separation column in countercurrent to the oxygen-enriched fraction is also removed from the low-pressure column.
  • the undesirable more volatile components are enriched in the top gas of the separation column.
  • the top gas With the top gas, they are removed from the upper area of the separation column. If the low-pressure column and the separation column are operated under a pressure which is higher than the atmospheric pressure, it is expedient to relax the top gas while performing work and thus to obtain cold for the process.
  • the top gas of the separation column can be condensed against an evaporating liquid intermediate fraction of the low-pressure column and can be used as a refrigerant for a further condenser-evaporator, for example a top condenser of the low-pressure column.
  • process cold can be obtained by other methods, for example by expanding residual gas from a top condenser of the low-pressure column or from the low-pressure column itself, or by means of an air turbine which blows into the high-pressure column. Any combination of such cold recovery methods is also possible. Direct blowing of air into the low pressure column should generally be avoided as this would in turn lead to contamination of the nitrogen product with more volatile impurities.
  • the highly pure nitrogen product is often required under superatmospheric pressure.
  • the high pressure column which is usually shared Condenser-evaporator, the main condenser, is in heat-exchanging connection with the low-pressure column, then there is a pressure of, for example, 6 to 20, preferably 7 to 16 bar.
  • gaseous top nitrogen is at least partially condensed from the low pressure column in the liquefaction chamber of the top condenser by indirect heat exchange with a cooling fraction evaporating in the evaporation chamber of the top condenser. At least a part of the liquid nitrogen generated is fed as a return to the low pressure column.
  • a flushing gas is preferably drawn off from the top condenser, with which also more volatile impurities escape.
  • the top condenser is preferably cooled with the bottom liquid of the low pressure column.
  • the scope of the plywood floors is, for example, one to ten, preferably three to five theoretical or practical floors.
  • the highly pure nitrogen fraction can be brought up to a higher pressure in the liquid state downstream of its removal, then evaporated in a product evaporator by indirect heat exchange and removed as a highly pure product.
  • the invention also relates to a device for obtaining high-purity nitrogen by low-temperature separation of air according to claims 9 to 15.
  • Compressed and cleaned feed air 1 is cooled in a main heat exchanger 2 and fed to a high-pressure column 4 under a pressure of 14 bar (3).
  • the rectification system also has a low-pressure column 5, which is operated at a pressure of 5 bar and is in heat-exchanging connection with the high-pressure column via a common condenser-evaporator (main condenser) 6.
  • a gaseous nitrogen fraction 7 from the top of the high-pressure column is liquefied in the main condenser 6 and, for the first part, is fed via lines 8 and 9 as a return to the high-pressure column.
  • a second part 10 is subcooled in a subcooling countercurrent 11 and led via line 12 to the top of the low pressure column 5.
  • the bottom liquid 13 is drawn off as an oxygen-enriched fraction from the high-pressure column and is also supercooled (11).
  • the supercooled oxygen-enriched fraction 14 is expanded in a throttle valve 15 to approximately the operating pressure of the low-pressure column 5 and, according to the invention, fed to a cleaning step for removing more volatile impurities, which in the example consists of a separation column 16 which is designed as an output column.
  • the oxygen-enriched fraction is fed to the top of the separation column 16 and there enters into countercurrent mass transfer with a gaseous fraction 17 from an intermediate point of the low-pressure column 5.
  • the cleaned oxygen-enriched fraction is removed from the bottom of the separation column 16 and flows via line 18 into the low-pressure column 5.
  • the feed can be like shown take place at the same point at which the gaseous fraction 17 is drawn off, or also offset by one or more theoretical or practical floors.
  • the gaseous nitrogen 23 condenses almost completely from the top of the low-pressure column 5; the condensate 24/25 is returned to the low pressure column.
  • a residual vapor which in particular contains more volatile impurities such as helium, neon and / or hydrogen, is removed as purge gas 26 from the fraction 19 condensed in the top condenser (as shown) or alternatively directly from the top condenser 22.
  • the residual steam 26 is blown off into the atmosphere or mixed with another residual stream, for example in line 38.
  • part of the liquid flowing down in the low-pressure column 5 is removed as a highly pure nitrogen fraction 28, in the liquid state under pressure (in the example 14 bar) brought (pump 29) and led via lines 30 and 31 through the subcooling countercurrent 11 to a product evaporator 32.
  • the nitrogen 33 evaporated under a pressure of 13.4 bar is warmed in the main heat exchanger 2 and finally discharged as a highly pure pressure product 34 (PGAN).
  • a part can be used as sealing gas [Sealgas].
  • the high purity nitrogen product can optionally be further compressed in the gaseous state.
  • the high purity pressurized nitrogen product 34 has a total contamination of 10 ppb (including carbon monoxide). If necessary, part of the gaseous nitrogen 7 can be warmed from the top of the pressure column in the main heat exchanger 2 and can be obtained as a further pressure product of lower purity (not shown).
  • the product evaporator 32 can be designed as a circulation evaporator (bath evaporator with thermosiphon effect) or as a falling film evaporator.
  • Liquid Expelled nitrogen 37 is optionally returned to the low pressure column 5.
  • a residual vapor which in particular contains more volatile impurities such as helium, neon and / or hydrogen, can also be removed from the product evaporator 32 (not shown).
  • a flushing liquid can be supplied via line 44. continuously or discontinuously removed and discarded in order to avoid the accumulation of less volatile components in the evaporation space of the top condenser 22.
  • part of the liquid, highly pure nitrogen fraction 28 can be obtained from the low pressure column as a liquid product.
  • the impure oxygen 38 which is produced by evaporation of the bottom liquid 19 of the low-pressure column 5 in the top condenser 22 of the low-pressure column, is heated in the heat exchangers 11 and 2 and removed as a by-product or residual gas (39). It can be used, for example, for the regeneration of a device for air purification (not shown).
  • cold is generated by work-relieving expansion 43 of the top gas 40-41-42 of the separation column 16.
  • the top gas 40 is previously warmed to an intermediate temperature in the supercooling counterflow 11 and in the main heat exchanger 2.
  • the throughput through the expansion machine can be adjusted by means of a bypass line 46, which contains an expansion valve.
  • the expansion turbine can be driven with the impure oxygen (residual gas) 38 from the evaporation space of the top condenser 22 of the low pressure column.
  • the mechanical energy obtained in the expansion machine 43 can be used, for example, for the post-compression of the pressurized nitrogen product evaporated in the product evaporator 32 or for increasing the pressure in the top gas of the separation column upstream of the expansion machine 43, preferably by direct mechanical coupling of the expansion machine 43 and a corresponding compressor.
  • the relaxation machine 43 can deliver the mechanical energy to a generator or to a dissipative brake.
  • the mass transfer elements in the low pressure column and in the high pressure column can be formed in the invention and in the exemplary embodiment by conventional mass transfer trays (for example sieve trays), packing (disordered packing) and / or ordered packing. Combinations of different types of elements in one column are also possible.
  • the top gas 40 of the separation column 16 is not introduced into the supercooling counterflow 11, but into an additional condenser-evaporator. There it is condensed in indirect heat exchange with an evaporating intermediate liquid from the low-pressure column and finally - in addition to the low-pressure column bottom liquid 19, 20 - introduced into the evaporation chamber of the top condenser.

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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)
EP02023334A 2002-09-28 2002-10-18 Procédé et dispositif pour la production d'azote ultra pur Withdrawn EP1403602A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10245379A DE10245379A1 (de) 2002-09-28 2002-09-28 Verfahren und Vorrichtung zur Gewinnung von hoch reinem Stickstoff
DE10245379 2002-09-28

Publications (1)

Publication Number Publication Date
EP1403602A1 true EP1403602A1 (fr) 2004-03-31

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP02023334A Withdrawn EP1403602A1 (fr) 2002-09-28 2002-10-18 Procédé et dispositif pour la production d'azote ultra pur

Country Status (2)

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EP (1) EP1403602A1 (fr)
DE (1) DE10245379A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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