EP0834711A2 - Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff - Google Patents
Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff Download PDFInfo
- 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- Withdrawn
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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
- F25J3/04642—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
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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
- 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
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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
- 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)
Abstract
Description
Claims (9)
- Verfahren zur Gewinnung von hochreinem Stickstoff durch Tieftemperaturzerlegung von Luft, bei dem gereinigte und verdichtete Luft durch Rektifkation in einer aus einer Drucksäule (2) und einer Niederdrucksäule (3) bestehenden Doppelsäule (1) zerlegt wird, wobei Drucksäule (2) und Niederdrucksäule (3) in Wärmeaustauschbeziehung (4) stehen und wobei bei dem Verfahren eine stickstoffreiche Fraktion (9) aus der Drucksäule (2) in eine Reinstickstoffsäule (10) eingeführt, ein Teil der Kopffraktion der Reinstickstoffsäule durch indirekten Wärmeaustausch (11) kondensiert und am Kopf der Reinstickstoffsäule (10) eine leichterflüchtige Komponenten enthaltende Fraktion (12) abgezogen wird, dadurch gekennzeichnet, daß mindestens einen theoretischen oder praktischen Boden unterhalb der Stelle, an der die stickstoffreiche Fraktion (9) aus der Drucksäule (2) in die Reinstickstoffsäule (10) eingeführt wird, hochreiner Stickstoff (13) als Produkt aus der Reinstickstoffsäule (10) abgezogen wird.
- Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß mindestens ein Teil der Sumpfflüssigkeit der Reinstickstoffsäule durch indirekten Wärmeaustausch (14) verdampft wird.
- Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß mindestens einen theoretischen oder praktischen Boden unterhalb der Stelle, an der die stickstoffreiche Fraktion (5, 9) entnommen wird, eine stickstoffreiche Flüssigkeit (18) entnommen und als Flüssigprodukt abgezogen und/oder als Rücklauf auf die Niederdrucksäule (3) aufgegeben wird.
- Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß der hochreine Stickstoff (13) in flüssiger Form aus der Reinstickstoffsäule (10) abgezogen wird.
- Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß eine sauerstoffangereicherte Fraktion aus der Drucksäule (2) entnommen und bei dem indirekten Wärmeaustausch (11), bei dem ein Teil der Kopffraktion der Reinstickstoffsäule (10) kondensiert, mindestens teilweise verdampft wird.
- Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß in einer mit der Niederdrucksäule (3) verbundenen Reinsauerstoffsäule (19) ein hochreines Sauerstoffprodukt erzeugt wird, wobei die Sumpffraktion der Reinsauerstoffsäule bei dem indirekten Wärmeaustausch (11), bei dem ein Teil der Kopffraktion der Reinstickstoffsäule (10) kondensiert, mindestens teilweise verdampft wird.
- Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß die leichterflüchtige Komponenten enthaltende Fraktion (12) aus der Reinstickstoffsäule (10) in eine weitere Trenneinrichtung eingeleitet wird, die zur Gewinnung von Helium und/oder Neon dient.
- Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß ein Teil der in der Reinstickstoffsäule (10) herabfließenden Flüssigkeit an einer Zwischenstelle der Reinstickstoffsäule (10) abgezogen und in die Drucksäule (2) eingeleitet (17) wird.
- Vorrichtung zur Gewinnung von hochreinem Stickstoff durch Tieftemperaturzerlegung von Luft, mit einer Leitung für gereinigte und verdichtete Luft, die in eine aus einer Drucksäule (2) und einer Niederdrucksäule (3) bestehende Doppelsäule (1) führt, mit einem ersten Kondensator-Verdampfer (4), dessen Verflüssigungsseite mit der Drucksäule (2) und dessen Verdampfungsseite mit der Niederdrucksäule (3) in Strömungsverbindung stehen, mit einer Leitung (5, 9) für die Einführung einer stickstoffreichen Fraktion aus der Drucksäule (2) in eine Reinstickstoffsäule (10), mit einem zweiten Kondensator-Verdampfer (11), dessen Verflüssigungsseite mit dem Kopf der Reinstickstoffsäule (10) verbunden ist und mit einer am Kopf der Reinstickstoffsäule (10) angeordneten Restgasleitung (12) zum Abzug einer leichterflüchtige Komponenten enthaltende Fraktion, gekennzeichnet durch eine Produktleitung (13) für hochreinen Stickstoff, die mindestens einen theoretischen oder praktischen Boden unterhalb der Stelle, an der die Leitung (9) für die stickstoffreiche Fraktion aus der Drucksäule (2) in die Reinstickstoffsäule (10) mündet, mit der Reinstickstoffsäule (10) verbunden ist.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE1996140711 DE19640711A1 (de) | 1996-10-02 | 1996-10-02 | Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff |
DE19640711 | 1996-10-02 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0834711A2 true EP0834711A2 (de) | 1998-04-08 |
EP0834711A3 EP0834711A3 (de) | 1998-07-15 |
Family
ID=7807713
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP97117183A Withdrawn EP0834711A3 (de) | 1996-10-02 | 1997-10-02 | Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff |
Country Status (2)
Country | Link |
---|---|
EP (1) | EP0834711A3 (de) |
DE (1) | DE19640711A1 (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1001236A2 (de) * | 1998-11-11 | 2000-05-17 | Linde Aktiengesellschaft | Verfahren zur Gewinnung von ultrareinem Stickstoff |
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)
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)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3079759A (en) * | 1961-03-22 | 1963-03-05 | Air Prod & Chem | Separation of gaseous mixtures |
EP0299364A2 (de) * | 1987-07-09 | 1989-01-18 | Linde Aktiengesellschaft | Verfahren und Vorrichtung zur Luftzerlegung durch Rektifikation |
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 |
-
1996
- 1996-10-02 DE DE1996140711 patent/DE19640711A1/de not_active Withdrawn
-
1997
- 1997-10-02 EP EP97117183A patent/EP0834711A3/de not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3079759A (en) * | 1961-03-22 | 1963-03-05 | Air Prod & Chem | Separation of gaseous mixtures |
EP0299364A2 (de) * | 1987-07-09 | 1989-01-18 | Linde Aktiengesellschaft | Verfahren und Vorrichtung zur Luftzerlegung durch Rektifikation |
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)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1001236A2 (de) * | 1998-11-11 | 2000-05-17 | Linde Aktiengesellschaft | Verfahren zur Gewinnung von ultrareinem Stickstoff |
EP1001236A3 (de) * | 1998-11-11 | 2000-11-08 | Linde Aktiengesellschaft | Verfahren zur Gewinnung von ultrareinem Stickstoff |
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 |
---|---|
EP0834711A3 (de) | 1998-07-15 |
DE19640711A1 (de) | 1998-04-09 |
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