EP1001236A3 - Verfahren zur Gewinnung von ultrareinem Stickstoff - Google Patents

Verfahren zur Gewinnung von ultrareinem Stickstoff Download PDF

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Publication number
EP1001236A3
EP1001236A3 EP99122146A EP99122146A EP1001236A3 EP 1001236 A3 EP1001236 A3 EP 1001236A3 EP 99122146 A EP99122146 A EP 99122146A EP 99122146 A EP99122146 A EP 99122146A EP 1001236 A3 EP1001236 A3 EP 1001236A3
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EP
European Patent Office
Prior art keywords
nitrogen
low pressure
pressure column
free
column
Prior art date
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Granted
Application number
EP99122146A
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English (en)
French (fr)
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EP1001236B1 (de
EP1001236A2 (de
Inventor
Dietrich Dipl.-Ing. Rottmann
Christian Dipl.-Ing. Kunz
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Linde GmbH
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Linde GmbH
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Publication of EP1001236A3 publication Critical patent/EP1001236A3/de
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Publication of EP1001236B1 publication Critical patent/EP1001236B1/de
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04151Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04218Parallel arrangement of the main heat exchange line in cores having different functions, e.g. in low pressure and high pressure cores
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04006Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078Providing 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
    • F25J3/04084Providing 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04151Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04193Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206Division 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
    • F25J3/04212Division 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284Generation 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
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    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333Generation 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
    • F25J3/04351Generation 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04Processes 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
    • F25J3/04436Processes 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
    • F25J3/04454Processes 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 a main column system not otherwise provided, e.g. serially coupling of columns or more than three pressure levels
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/02Processes 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
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    • F25J3/04763Start-up or control of the process; Details of the apparatus used
    • F25J3/04866Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04951Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network
    • F25J3/04963Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network and inter-connecting equipment within or downstream of the fractionation unit(s)
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/10Processes or apparatus using separation by rectification in a quadruple, or more, column or pressure system
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    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/50Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/72Refluxing the column with at least a part of the totally condensed overhead gas
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00Processes characterised by the type or other details of the feed stream
    • F25J2210/42Nitrogen
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/42Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00Processes or apparatus involving steps for the removal of impurities
    • F25J2220/42Separating low boiling, i.e. more volatile components from nitrogen, e.g. He, H2, Ne
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    • F25J2235/00Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
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    • F25J2250/00Details related to the use of reboiler-condensers
    • F25J2250/20Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
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    • F25J2270/00Refrigeration techniques used
    • F25J2270/42Quasi-closed internal or closed external nitrogen refrigeration cycle
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    • F25J2290/00Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/62Details of storing a fluid in a tank
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00Refrigeration
    • Y10S62/92Carbon monoxide

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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)
  • Arrangement Of Elements, Cooling, Sealing, Or The Like Of Lighting Devices (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

Die Erfindung betrifft ein Verfahren zur Gewinnung von ultrareinem Stickstoff durch Tieftemperaturzerlegung von Luft in einem Rektifiziersystem mit wenigstens einer Rektifiziersäule, wobei verdichtete und gereinigte Einsatzluft in eine Drucksäule geführt, aus der Drucksäule eine sauerstofffreie Druckstickstofffraktion gewonnen, in eine Niederdrucksäule geführt und in der Niederdrucksäule kohlenmonoxidfreier Niederdruckstickstoff als Kopfgas gewonnen wird.
Erfindungsgemäß wird die sauerstofffreie Druckstickstofffraktion (1) entweder aus einem oberen Bereich der Drucksäule flüssig entnommen oder aus einem Flüssigkeitstank (22) mit gespeichertem sauerstofffreiem Stickstoff bereitgestellt und die sauerstofffreie Druckstickstofffraktion (1) in die in ihrem Sumpf beheizte Niederdrucksäule (2) entspannt. Hierbei wird in der Niederdrucksäule (2) aufsteigender Dampf gebildet und mit Hilfe eines am Kopf der Niederdrucksäule (2) aufgegebenen Rücklaufes mit ultrareinem Stickstoff von Kohlenmonoxid befreit, am Kopf der Niederdrucksäule (2) als kohlenmonoxidfreies Kopfgas (5) abgezogen und nach einer Druckerhöhung (5) teilweise verflüssigt. Der verflüssigte Teil (17, 18) wird in eine in ihrem Sumpf beheizte He-Ne-H2-Säule (4) entspannt, aus der der ultrareine Stickstoff (19) flüssig entnommen wird.
EP99122146A 1998-11-11 1999-11-05 Verfahren zur Gewinnung von ultrareinem Stickstoff Expired - Lifetime EP1001236B1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE19852019 1998-11-11
DE19852019 1998-11-11
DE19924375 1999-05-27
DE19924375 1999-05-27

Publications (3)

Publication Number Publication Date
EP1001236A2 EP1001236A2 (de) 2000-05-17
EP1001236A3 true EP1001236A3 (de) 2000-11-08
EP1001236B1 EP1001236B1 (de) 2004-09-29

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EP99122146A Expired - Lifetime EP1001236B1 (de) 1998-11-11 1999-11-05 Verfahren zur Gewinnung von ultrareinem Stickstoff

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US (1) US6276172B1 (de)
EP (1) EP1001236B1 (de)
JP (1) JP2000180051A (de)
KR (1) KR20000035406A (de)
CN (1) CN1134640C (de)
AT (1) ATE278166T1 (de)
CA (1) CA2289173A1 (de)
DE (2) DE19929798A1 (de)
ES (1) ES2229608T3 (de)
SG (1) SG74755A1 (de)
TW (1) TW432191B (de)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10158327A1 (de) * 2001-11-28 2003-06-18 Linde Ag Verfahren und Vorrichtung zur Herstellung hoch reinen Stickstoffs aus weniger reinem Stickstoff
DE10205094A1 (de) * 2002-02-07 2003-08-21 Linde Ag Verfahren und Vorrichtung zur Erzeugung hoch reinen Stickstoffs
CN102959352B (zh) * 2009-07-24 2016-07-06 英国备选能源国际有限公司 二氧化碳和氢气的分离
CN102797974A (zh) * 2012-07-31 2012-11-28 张立永 氢脉
CN114165989A (zh) * 2021-11-22 2022-03-11 四川空分设备(集团)有限责任公司 制取中压氮气的装置及方法

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US4464188A (en) * 1983-09-27 1984-08-07 Air Products And Chemicals, Inc. Process and apparatus for the separation of air
US5167125A (en) * 1991-04-08 1992-12-01 Air Products And Chemicals, Inc. Recovery of dissolved light gases from a liquid stream
EP0569310A1 (de) * 1992-05-08 1993-11-10 Nippon Sanso Corporation Flüssiglufttrennungsapparat und Verfahren dafür
EP0834711A2 (de) * 1996-10-02 1998-04-08 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff
DE19806576A1 (de) * 1998-02-17 1998-08-06 Linde Ag Verfahren und Vorrichtung zur Gewinnung von CO-freiem Stickstoff

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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
US5170630A (en) * 1991-06-24 1992-12-15 The Boc Group, Inc. Process and apparatus for producing nitrogen of ultra-high purity
US5351492A (en) * 1992-09-23 1994-10-04 Air Products And Chemicals, Inc. Distillation strategies for the production of carbon monoxide-free nitrogen
FR2696821B1 (fr) * 1992-10-09 1994-11-10 Air Liquide Procédé et installation de production d'azote ultra-pur sous pression.
JP3447437B2 (ja) * 1995-07-26 2003-09-16 日本エア・リキード株式会社 高純度窒素ガス製造装置
US5906113A (en) * 1998-04-08 1999-05-25 Praxair Technology, Inc. Serial column cryogenic rectification system for producing high purity nitrogen

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4464188A (en) * 1983-09-27 1984-08-07 Air Products And Chemicals, Inc. Process and apparatus for the separation of air
US5167125A (en) * 1991-04-08 1992-12-01 Air Products And Chemicals, Inc. Recovery of dissolved light gases from a liquid stream
EP0569310A1 (de) * 1992-05-08 1993-11-10 Nippon Sanso Corporation Flüssiglufttrennungsapparat und Verfahren dafür
EP0834711A2 (de) * 1996-10-02 1998-04-08 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff
DE19806576A1 (de) * 1998-02-17 1998-08-06 Linde Ag Verfahren und Vorrichtung zur Gewinnung von CO-freiem Stickstoff

Also Published As

Publication number Publication date
EP1001236B1 (de) 2004-09-29
CA2289173A1 (en) 2000-05-11
CN1255619A (zh) 2000-06-07
KR20000035406A (ko) 2000-06-26
ES2229608T3 (es) 2005-04-16
EP1001236A2 (de) 2000-05-17
JP2000180051A (ja) 2000-06-30
US6276172B1 (en) 2001-08-21
SG74755A1 (en) 2000-08-22
DE59910646D1 (de) 2004-11-04
ATE278166T1 (de) 2004-10-15
DE19929798A1 (de) 2000-05-25
TW432191B (en) 2001-05-01
CN1134640C (zh) 2004-01-14

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