EP0834711A2 - Procédé et dispositif pour la production d'azote à haute pureté - Google Patents

Procédé et dispositif pour la production d'azote à haute pureté Download PDF

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Publication number
EP0834711A2
EP0834711A2 EP97117183A EP97117183A EP0834711A2 EP 0834711 A2 EP0834711 A2 EP 0834711A2 EP 97117183 A EP97117183 A EP 97117183A EP 97117183 A EP97117183 A EP 97117183A EP 0834711 A2 EP0834711 A2 EP 0834711A2
Authority
EP
European Patent Office
Prior art keywords
column
nitrogen
pure nitrogen
pressure column
fraction
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Withdrawn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
EP97117183A
Other languages
German (de)
English (en)
Other versions
EP0834711A3 (fr
Inventor
Ralph Dipl.-Ing. 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
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Publication of EP0834711A2 publication Critical patent/EP0834711A2/fr
Publication of EP0834711A3 publication Critical patent/EP0834711A3/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Withdrawn legal-status Critical Current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
    • F25J3/04642—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
    • F25J3/04715—The auxiliary column system simultaneously produces 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
    • F25J2200/06—Processes or apparatus using separation by rectification in a dual pressure main column system in a classical double column flow-sheet, 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
    • 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
    • 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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2

Definitions

  • the invention relates to a method for obtaining high-purity nitrogen by Cryogenic air separation, in which cleaned and compressed air through Rectification in a column consisting of a pressure column and a low pressure column Double column is disassembled, with pressure column and low pressure column in Heat exchange relationship.
  • the process uses a nitrogen rich Fraction from the pressure column introduced into a pure nitrogen column, part of the Head fraction of the pure nitrogen column condensed by indirect heat exchange and at the head of the pure nitrogen column containing a more volatile components Fraction deducted.
  • EP-299364-B1 therefore proposed an additional pure nitrogen column to connect to the pressure column, which is used to discharge the more volatile Components.
  • the pure nitrogen column is designed as a reinforcement column, whose bottom liquid is returned to the pressure column.
  • the highly pure Nitrogen product is withdrawn from the pressure column. This method is suitable the enrichment of helium and neon in the nitrogen product compared to one to significantly reduce ordinary double-column processes.
  • the lowest possible content of volatile components in high-purity nitrogen also limited in this process by their concentration in the feed air.
  • This object is achieved in that at least one theoretical or practical bottom below the point where the nitrogen-rich fraction from the Pressure column is introduced into the pure nitrogen column, high purity nitrogen as a product is withdrawn from the pure nitrogen column.
  • the pure nitrogen column therefore has a stripping section, which is used for further depletion especially of helium, neon and optionally hydrogen.
  • This can basically have any number of theoretical floors; it can in principle, any low concentration of volatile components can be achieved, especially one that is below that of the feed air.
  • high purity nitrogen with a residual content of less than 1 ppb of more volatile impurities can be obtained.
  • the more volatile Shares, especially helium, neon and possibly hydrogen, are on the head deducted from the pure nitrogen column. The deduction can be made directly via the Mass transfer elements of the pure nitrogen column or at the liquefaction room of the Head capacitor of the pure nitrogen column can be arranged.
  • the pure nitrogen column has, for example, 3 to 10, preferably 5 to 8 theoretical plates.
  • the Pure nitrogen column for example 2 to 8, preferably 2 to 3 theoretical plates be provided.
  • the nitrogen-rich fraction is preferably gaseous in the pure nitrogen column introduced.
  • At least part of the bottom liquid of the pure nitrogen column evaporated by indirect heat exchange.
  • the swamp heater of the Pure nitrogen column can be felt or preferably latent by transfer Heat can be operated from any suitable heating medium.
  • air under pressure or the top fraction of a column are suitable for Separation of argon and nitrogen.
  • the method has at least one theoretical or practical bottom below where the nitrogen-rich fraction is removed, a nitrogen-rich liquid is taken and as a liquid product withdrawn and / or is given as a return to the low pressure column.
  • a nitrogen-rich liquid is taken and as a liquid product withdrawn and / or is given as a return to the low pressure column.
  • the Section in the pressure column between these two points is in itself from EP-299364-B1 known and has a higher reflux ratio than the one below Part of the pressure column. This will cause the rising gas to turn on in this section Depleted of carbon monoxide, so that the feed fraction for the pure nitrogen column and thus the product of the pressure column also has a particularly low content Have carbon monoxide.
  • the high-purity nitrogen can be liquid and / or gaseous from the pure nitrogen column deducted, a particularly low residual volatile However, components can be reached in liquid form when removed.
  • the head cooling of the pure nitrogen column can also be carried out by any suitable medium be made.
  • An oxygen-enriched fraction is preferably produced taken from the pressure column and in the indirect heat exchange, in which a part the top fraction of the pure nitrogen column condenses, at least partially evaporates.
  • one is connected to the low pressure column Pure oxygen column produces a highly pure oxygen product, the Bottom fraction of the pure oxygen column in the indirect heat exchange, in which a part of the top fraction of the pure nitrogen column condenses, at least partially is evaporated.
  • Both types of head cooling of the pure nitrogen column are in the EP-299364-B1 shown in detail.
  • the fraction from the pure nitrogen column containing the more volatile components can be introduced into a further separation device, which is used to extract helium and / or neon is used.
  • the pure nitrogen column of the invention particularly high proportion of the helium and / or neon contained in the air in the Head fraction smuggled, especially when others if necessary existing drains for volatile components (e.g. on Top condenser of the pressure column) also in the separator for the extraction of Helium and / or neon are led.
  • the particularly high purity of the Nitrogen product results in a high yield of helium and / or neon.
  • a conventional double column 1 for Air separation indicated consisting of a pressure column 2, a low pressure column 3 and a main capacitor (first KDV) 4. Air rising in the pressure column is enriched with nitrogen and volatile components.
  • Bottom liquid of the low pressure column 3 partially or completely condensed. This liquefaction is preferably carried out essentially completely, a small non-condensed portion removed via a drain line 8 and discarded or mixed with another residual stream (e.g. stream 12).
  • Another part 9 of the top gas 5 is introduced into a pure nitrogen column 10.
  • a pure nitrogen column 10 In the exemplary embodiment, there are 3 theoretical ones above the feed point Floors.
  • a second KDV 11 is arranged above it, in which the top fraction of the Pure nitrogen column 10 is condensed by indirect heat exchange. Of the fraction 12 remaining in gaseous form contains helium, neon and optionally hydrogen, which are kept away from the nitrogen product.
  • the insert fraction 9 for the pure nitrogen column contains a further 8 theoretical ones Floors.
  • the content of volatile components in the nitrogen-rich fraction 9 is still about 53 ppm, to about less than 0.1 ppm reduced.
  • Liquid high-purity nitrogen is the product 13 from the sump Pure nitrogen column 10 deducted.
  • the sump heater (third condenser evaporator) 14 of the pure nitrogen column is, for example, with a partial flow 15 of Operating air operated, which thus condenses at least partially.
  • the condensed Air 16 can then be fed into the pressure column 2.
  • Part of the liquid flowing down in the pure nitrogen column is at the level of Feeding the nitrogen-rich fraction 9 withdrawn via a line 17 and to Head of the pressure column 2 returned.
  • the one taken directly from the pressure column In the example nitrogen becomes 15 theoretical soils below the head removed (18) and fed to the low pressure column 3 as a return.
  • a part of Pressure column nitrogen 18 can also be obtained as a liquid product.
  • the The main component of the invention is high-purity oxygen.
  • an oxygen-rich fraction 20 removed, which is low in volatile components in an additional column 21 introduced, which is designed as a side column to the low pressure column 3 and at Demand can be designed as a raw argon column.
  • the additional column 21 becomes one more fraction 22 depleted in less volatile components and one Pure oxygen column 19 abandoned as a return.
  • the head cooling 11 of the pure nitrogen column 10, for example by evaporating relaxed sump liquid can be carried out from the pressure column (see Figure 3 from EP-299364-B1). With simultaneous pure oxygen production in one Pure oxygen column 19, however, it is favorable to the oxygen and Integrate nitrogen purification by the second condenser-evaporator 11 serves at the same time as a sump heater for the pure oxygen column 19. Details of the Purest oxygen production and its integration with the purest nitrogen production can be found in EP-299364-B1 (see in particular FIG. 4).

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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)
EP97117183A 1996-10-02 1997-10-02 Procédé et dispositif pour la production d'azote à haute pureté Withdrawn EP0834711A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19640711 1996-10-02
DE1996140711 DE19640711A1 (de) 1996-10-02 1996-10-02 Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff

Publications (2)

Publication Number Publication Date
EP0834711A2 true EP0834711A2 (fr) 1998-04-08
EP0834711A3 EP0834711A3 (fr) 1998-07-15

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP97117183A Withdrawn EP0834711A3 (fr) 1996-10-02 1997-10-02 Procédé et dispositif pour la production d'azote à haute pureté

Country Status (2)

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EP (1) EP0834711A3 (fr)
DE (1) DE19640711A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1001236A2 (fr) * 1998-11-11 2000-05-17 Linde Aktiengesellschaft Procédé de production d'azote à ultra haute pureté
US8661847B2 (en) 2008-08-11 2014-03-04 Robert Brockmann Production of a clean gas, in particular for testing a pressurized construction component for leaks

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19819263C2 (de) * 1998-04-30 2003-08-21 Linde Ag Verfahren und Vorrichtung zur Gewinnung von Druckstickstoff

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3079759A (en) * 1961-03-22 1963-03-05 Air Prod & Chem Separation of gaseous mixtures
EP0299364A2 (fr) * 1987-07-09 1989-01-18 Linde Aktiengesellschaft Procédé et dispositif de séparation de l'air par rectification
US5123947A (en) * 1991-01-03 1992-06-23 Air Products And Chemicals, Inc. Cryogenic process for the separation of air to produce ultra high purity nitrogen

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3079759A (en) * 1961-03-22 1963-03-05 Air Prod & Chem Separation of gaseous mixtures
EP0299364A2 (fr) * 1987-07-09 1989-01-18 Linde Aktiengesellschaft Procédé et dispositif de séparation de l'air par rectification
US5123947A (en) * 1991-01-03 1992-06-23 Air Products And Chemicals, Inc. Cryogenic process for the separation of air to produce ultra high purity nitrogen

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1001236A2 (fr) * 1998-11-11 2000-05-17 Linde Aktiengesellschaft Procédé de production d'azote à ultra haute pureté
EP1001236A3 (fr) * 1998-11-11 2000-11-08 Linde Aktiengesellschaft Procédé de production d'azote à ultra haute pureté
US6276172B1 (en) 1998-11-11 2001-08-21 Linde Aktiengesellschaft Process for producing ultrapure nitrogen
US8661847B2 (en) 2008-08-11 2014-03-04 Robert Brockmann Production of a clean gas, in particular for testing a pressurized construction component for leaks

Also Published As

Publication number Publication date
DE19640711A1 (de) 1998-04-09
EP0834711A3 (fr) 1998-07-15

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