EP1134524B1 - Procédé de production d'azote gazeux - Google Patents

Procédé de production d'azote gazeux Download PDF

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Publication number
EP1134524B1
EP1134524B1 EP01105925A EP01105925A EP1134524B1 EP 1134524 B1 EP1134524 B1 EP 1134524B1 EP 01105925 A EP01105925 A EP 01105925A EP 01105925 A EP01105925 A EP 01105925A EP 1134524 B1 EP1134524 B1 EP 1134524B1
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EP
European Patent Office
Prior art keywords
nitrogen
condenser
evaporator
oxygen
air
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.)
Expired - Lifetime
Application number
EP01105925A
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German (de)
English (en)
Other versions
EP1134524A2 (fr
EP1134524A3 (fr
Inventor
Dietrich Dipl.-Ing. Rottmann
Christian Dipl.-Ing. Kunz
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
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Publication of EP1134524A3 publication Critical patent/EP1134524A3/fr
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Publication of EP1134524B1 publication Critical patent/EP1134524B1/fr
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Classifications

    • 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
    • F25J3/044—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 single pressure main column system only
    • 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
    • F25J3/04248—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
    • F25J3/04321—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 of 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
    • 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
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams 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
    • 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

Definitions

  • the invention relates to a method according to the preamble of claim 1. It is used for the recovery of gaseous nitrogen by cryogenic separation of air in a distillation column system having a single column. Such a procedure is known from DE 196 23 310.
  • Single column methods are a common method of producing nitrogen. she have, in contrast to double column method, only one pressure column (the single column) on and no further column (low-pressure column) leading to the nitrogen-oxygen separation used and operated at a lower pressure than the pressure column. This does not exclude that the distillation column system beyond the single column addition Having columns, for example, to obtain particularly pure nitrogen or Oxygen.
  • distillation column system comprises the interconnected distillation columns, but not the heat exchangers or the machines like compressors or Expanders. In the simplest case, the distillation column system exclusively formed by the single column.
  • oxygen-enriched is meant here a mixture of air gases, the has a higher oxygen concentration than air, to practically pure Oxygen.
  • oxygen concentration preferably 25 to 90%, preferably 30 to 80%.
  • a method with a nitrogen cycle according to the preamble of claim 1 is from US 4,400,188. With nitrogen in over in a cycle compressor Column pressure was brought, a condenser evaporator is heated, which the Sump heating of the single column represents. Process refrigeration is by a common Residual gas turbine generated with gas from another condenser-evaporator, a head capacitor operated.
  • the invention is based on the object, a method of the type mentioned and to provide a corresponding device, the energy particularly favorable to operate.
  • This object is achieved in that a second oxygen-enriched gas taken from the evaporation space of the condenser-evaporator, performing work is relaxed and warmed in the main heat exchanger.
  • the total reflux liquid for the single column in the condenser-evaporator generated is the total reflux liquid for the single column in the condenser-evaporator generated. It is therefore generally only a single condenser-evaporator required.
  • Air compressors and cycle compressors can be formed by a single machine be, namely by a combi-machine, in which several pinions on a shaft some of which are air compressors and one or more Realize cycle compressor.
  • the cycle compressor can at least partially by a to the rest of the gas turbine coupled compressors are formed, wherein at least a part of the at work-performing expansion of the second oxygen-enriched gas generated mechanical energy to compress the first part and / or the second part the nitrogen-rich fraction is used.
  • the invention also relates to a device according to claim 5.
  • the top nitrogen 5 (the "nitrogen-rich fraction") from the single column 4 still contains 1 ppm to 1 ppb of oxygen and is in a subcooler 6 and (line 7) further in Main heat exchanger 2 warmed to about ambient temperature.
  • the warm one Head nitrogen 8 is fed to a cycle compressor 9, for example, two to has three stages. Behind each stage of the cycle compressor is a After- or intermediate cooling to remove the heat of compression, of which, however, in the schematic drawing, only the aftercooling 10 behind the Amplifier is shown.
  • a first part 12 of the compressed to a pressure of 9.5 bar Head nitrogen 11 is returned to the main heat exchanger 2, there to several Kelvin cooled above the column temperature and via line 13 the Liquefaction space of a condenser-evaporator 14 supplied.
  • the resulting nitrogen-rich liquid 15 is in the subcooler. 6 subcooled and via line 16 and throttle valve 17 to the head of the single column given up.
  • a portion 18 of the nitrogen-rich liquid 16 may be referred to as Liquid nitrogen product LIN are deducted.
  • the liquid production is in the Example about 0% of the air volume.
  • the liquid nitrogen from the Withdrawn from a single column, the head here as Flashgasabscheider between the Throttling valve 17 and the liquid product removal 18 is used.
  • a second part 19 of the compressed in the cycle compressor 9 head nitrogen 11 is called gaseous nitrogen product under pressure (DGAN) dissipated.
  • DGAN gaseous nitrogen product under pressure
  • a portion 20 of the pressurized nitrogen from an intermediate stage of the cycle compressor led out and at a pressure between the operating pressure of the single column 4 and the final pressure of the cycle compressor 9 as gaseous pressure nitrogen product (DGAN ').
  • DGAN gaseous pressure nitrogen product
  • the cycle compressor 9 serves at the same time as a product compressor.
  • the condenser-evaporator 14 is in the example of Figure 1 directly in the sump arranged the single column. On its evaporation side evaporates the oxygen-enriched bottoms liquid of the single column 4 below their operating pressure forming a vapor having an oxygen content of about 80%. While a first part of the vapor generated in the condenser-evaporator 14 in the single column. 4 rises ("first oxygen-enriched gas”), a second part 21 (“second oxygen-enriched gas”) oxygen-enriched gas ”) to the cold end of the main heat exchanger 2. After heating to an intermediate temperature, this fraction flows via line 22 to a residual gas turbine 23 and will work there from about 3 bar to about 1.5 bar relaxed.
  • the working expanded oxygen-enriched gas 24 becomes completely warmed up in the main heat exchanger 2 and via line 25 as impure Oxygen product UGOX delivered. It can not be used as a regeneration gas in the illustrated air purification and / or used as a gaseous by-product and / or released into the atmosphere.
  • the turbine 23 can via a Bypass 26 can be regulated. A small amount of liquid 27 becomes continuous or intermittently as rinsing liquid from the evaporation space of the condenser-evaporator 14 discharged.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Treating Waste Gases (AREA)

Claims (5)

  1. Procédé de production d'azote gazeux par séparation d'air à basse température dans un système de colonne de distillation, qui présente une colonne unique (4), où, dans le procédé
    l'air de charge (1) est comprimé dans un compresseur d'air, refroidi dans un échangeur de chaleur principal (2) et acheminé (3) à la colonne unique (4),
    une fraction riche en azote (5, 7, 8) est extraite du système de colonne de distillation et est comprimée pour fournir au moins une première partie dans un compresseur à circulation (9),
    la première partie (12, 13) de la fraction riche en azote (5, 7, 8) est amenée en aval du compresseur à circulation (9) à l'espace de liquéfaction d'un condenseur-évaporateur (14) et y est condensée à une pression qui est supérieure à la pression de fonctionnement de la colonne unique (4), du liquide riche en azote (15, 16) se formant alors,
    une fraction fluide enrichie en oxygène provenant du système de colonne de distillation est au moins partiellement évaporée dans l'espace d'évaporation du condenseur-évaporateur (14),
    à partir de la vapeur (232) formée dans l'espace d'évaporation du condenseur-évaporateur (14), un premier gaz enrichi en oxygène est formé, introduit dans la colonne unique (4) et y est utilisé en tant que vapeur montante, et
    une deuxième partie (19, 20) de la fraction riche en azote (5, 7, 8) est extraite au moins temporairement sous forme de produit d'azote gazeux,
    caractérisé en ce que
    un deuxième gaz enrichi en oxygène est extrait de l'espace d'évaporation du condenseur-évaporateur (14), est détendu en fournissant du travail (23) et est réchauffé dans l'échangeur de chaleur principal (2).
  2. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que tout le liquide de retour pour la colonne unique (4) est produit dans le condenseur-évaporateur (14).
  3. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le compresseur d'air et le compresseur à circulation (9) sont formés par une seule machine.
  4. procédé selon l'une quelconque des revendications précédentes, caractérisé en ce qu'au moins une partie de l'énergie mécanique produite lors de la détente fournissant du travail (23) du deuxième gaz enrichi en oxygène (21) est utilisée pour la compression de la première partie et/ou de la deuxième partie de la fraction riche en azote (5, 7, 8).
  5. Dispositif de production d'azote gazeux par séparation d'air à basse température comprenant un système de colonne de distillation, qui présente une colonne unique (4) et comprenant :
    un compresseur d'air,
    une conduite d'air de charge (1, 3) qui conduit du compresseur d'air à travers un échangeur de chaleur principal (2) dans la colonne unique (4),
    un compresseur à circulation (9) pour la compression de la première partie d'une fraction riche en azote (5, 7, 8) provenant du système de colonne de distillation,
    une conduite de circulation (12, 13) qui est guidée de la sortie du compresseur à circulation (9) jusqu'à l'espace de liquéfaction d'un condenseur-évaporateur (14),
    des moyens pour le transport d'une fraction fluide enrichie en oxygène provenant du système de colonne de distillation jusqu'à l'espace d'évaporation du condenseur-évaporateur (14),
    des moyens pour produire un premier gaz enrichi en oxygène provenant de la vapeur formée dans l'espace d'évaporation du condenseur-évaporateur (14) et pour son introduction dans la colonne unique (4) et comprenant
    une conduite de produit de gaz pour l'extraction d'une deuxième partie (19, 20) de la fraction riche en azote (5, 7, 8) sous forme de produit d'azote gazeux,
    caractérisé par
    une machine de détente (23) pour la détente produisant du travail d'un deuxième gaz enrichi en oxygène issu de l'espace d'évaporation du condenseur-évaporateur (14).
EP01105925A 2000-03-17 2001-03-09 Procédé de production d'azote gazeux Expired - Lifetime EP1134524B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10013074 2000-03-17
DE10013074A DE10013074A1 (de) 2000-03-17 2000-03-17 Verfahren zur Gewinnung von gasförmigem Stickstoff

Publications (3)

Publication Number Publication Date
EP1134524A2 EP1134524A2 (fr) 2001-09-19
EP1134524A3 EP1134524A3 (fr) 2002-01-09
EP1134524B1 true EP1134524B1 (fr) 2005-10-05

Family

ID=7635135

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01105925A Expired - Lifetime EP1134524B1 (fr) 2000-03-17 2001-03-09 Procédé de production d'azote gazeux

Country Status (4)

Country Link
US (1) US6470707B2 (fr)
EP (1) EP1134524B1 (fr)
AT (1) ATE306062T1 (fr)
DE (2) DE10013074A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10157544A1 (de) * 2001-11-23 2003-06-12 Messer Ags Gmbh Verfahren und Vorrichtung zur Erzeugung von Stickstoff aus Luft
US7864163B2 (en) 2006-09-06 2011-01-04 Apple Inc. Portable electronic device, method, and graphical user interface for displaying structured electronic documents
DE102007024168A1 (de) * 2007-05-24 2008-11-27 Linde Ag Verfahren und Vorrichtung zur Tieftemperatur-Luftzerlegung
DE102007051183A1 (de) * 2007-10-25 2009-04-30 Linde Aktiengesellschaft Verfahren zur Tieftemperatur-Luftzerlegung
DE102007051184A1 (de) * 2007-10-25 2009-04-30 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Tieftemperatur-Luftzerlegung
EP2236964B1 (fr) * 2009-03-24 2019-11-20 Linde AG Procédé et dispositif de séparation de l'air à basse température

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1392294A (en) * 1971-06-28 1975-04-30 British Oxygen Co Ltd Air separation
US4400188A (en) * 1981-10-27 1983-08-23 Air Products And Chemicals, Inc. Nitrogen generator cycle
DE19543395A1 (de) * 1995-11-21 1997-05-22 Linde Ag Doppelsäulenverfahren und -vorrichtung zur Tieftemperaturzerlegung von Luft
DE19623310A1 (de) * 1995-11-21 1996-11-07 Linde Ag Einzelsäulenverfahren und -vorrichtung zur Tieftemperaturzerlegung von Luft
EP0816784A1 (fr) * 1996-06-26 1998-01-07 Crio & Eng S.r.l. Dispositif pour le fractionnement d'air ou d'un mélange d'oxygène et d'azote pour la production d'oxygène et d'azote ou d'azote
FR2767317B1 (fr) * 1997-08-14 1999-09-10 Air Liquide Procede de conversion d'un debit contenant des hydrocarbures par oxydation partielle
GB9806293D0 (en) * 1998-03-24 1998-05-20 Boc Group Plc Separation of air
DE10013073A1 (de) * 2000-03-17 2000-10-19 Linde Ag Verfahren und Vorrichtung zur Tieftemperaturzerlegung von Luft

Also Published As

Publication number Publication date
DE10013074A1 (de) 2001-09-20
EP1134524A2 (fr) 2001-09-19
ATE306062T1 (de) 2005-10-15
EP1134524A3 (fr) 2002-01-09
DE50107586D1 (de) 2005-11-10
US6470707B2 (en) 2002-10-29
US20010052242A1 (en) 2001-12-20

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