EP0775880A2 - Procédé et dispositif à double colonne pour la séparation cryogénique d'air - Google Patents

Procédé et dispositif à double colonne pour la séparation cryogénique d'air Download PDF

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Publication number
EP0775880A2
EP0775880A2 EP96117880A EP96117880A EP0775880A2 EP 0775880 A2 EP0775880 A2 EP 0775880A2 EP 96117880 A EP96117880 A EP 96117880A EP 96117880 A EP96117880 A EP 96117880A EP 0775880 A2 EP0775880 A2 EP 0775880A2
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EP
European Patent Office
Prior art keywords
column
low
pressure
separation
separation column
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Withdrawn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
EP96117880A
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German (de)
English (en)
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EP0775880A3 (fr
Inventor
Jürgen Dipl.-Phys. Voit
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Linde GmbH
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Linde GmbH
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Filing date
Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Publication of EP0775880A2 publication Critical patent/EP0775880A2/fr
Publication of EP0775880A3 publication Critical patent/EP0775880A3/fr
Withdrawn legal-status Critical Current

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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
    • F25J3/04248—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
    • F25J3/0429—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 feed air, e.g. used as waste or product air or expanded into an auxiliary 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
    • F25J3/04248—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
    • F25J3/0429—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 feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or 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
    • F25J3/04248—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
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/38—Processes or apparatus using separation by rectification using pre-separation or distributed distillation before a main column system, e.g. in a at least a double 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
    • F25J2200/76—Refluxing the column with condensed overhead gas being cycled in a quasi-closed loop refrigeration cycle

Definitions

  • the invention relates to a method for the low-temperature separation of air in a rectification column system, which has a pre-separation column and a low-pressure column, in which feed air is introduced into the pre-separation column, in which a nitrogen-enriched top fraction and an oxygen-enriched bottom fraction are generated in the pre-separation column, at least some of which oxygen-enriched bottoms fraction is introduced into the low-pressure column, and in which liquid oxygen and gaseous nitrogen are generated in the low-pressure column, that is to say a double-column system for extracting oxygen and / or nitrogen from air.
  • This is understood here to mean a process or a system which has at least two columns for nitrogen-oxygen separation. This includes systems in which the feed air is broken down into three or more columns and / or in which further columns are provided for the extraction of other air components such as noble gases, for example a crude argon column.
  • a double column process of the type mentioned above is known from DE-C-2854508.
  • return for the two columns is generated in a common condenser-evaporator, in which nitrogen-enriched overhead gas from the pre-separation column is liquefied against evaporating oxygen from the bottom of the low-pressure column.
  • This thermal coupling of the two columns requires that the pressure in the pre-separation column be so high that the condensation temperature of the nitrogen at the top of this column exceeds that of the oxygen in the bottom of the low pressure column. A corresponding amount of energy must therefore be put into the compression of the feed air.
  • the invention is therefore based on the object of specifying a method of the type mentioned at the outset which operates in an energetically particularly favorable manner.
  • This object is achieved in that the pressure in the pre-separation column is substantially equal to the pressure in the low pressure column.
  • the pressure difference between the two columns is less than about 0.5 bar, preferably less than about 0.1 bar. This is achieved, for example, in that at least one line connecting the two columns (for example the bottom liquid line from the pre-separation column into the Low pressure column) contains no pressure-changing devices such as expansion valves. The pressure difference due to the pressure loss along this line is thus fixed. It is much lower than in the conventional double-column method described above.
  • the low pressure column in the invention is preferably operated under the lowest possible pressure. This is determined by the fact that the top product of the low-pressure column can be removed from the process under essentially atmospheric pressure, if appropriate after passing through one or more heat exchangers; if this overhead product is used as regeneration gas in a cleaning device (e.g. a molecular sieve system), the pressure of the low pressure column must also enable it to operate.
  • the low pressure column pressure can be, for example, 1.2 to 1.5 bar, preferably 1.3 to 1.4 bar.
  • oxygen with a purity of, for example, 80 vol% to 99.9 vol% can be obtained.
  • pure nitrogen can also be produced.
  • Argon extraction is also possible if the low pressure column is followed by argon rectification in a known manner (see for example EP-B-377117).
  • other noble gases can be generated in the usual way.
  • the return for the columns is preferably generated in the process according to the invention in that at least a portion of the nitrogen-enriched top fraction from the pre-separation column is heated, compressed, liquefied by indirect heat exchange and returned to the rectification column system, in particular to the pre-separation column.
  • the compression of the nitrogen-enriched top fraction takes place, for example, at about ambient temperature and leads to a pressure of, for example, 2.8 to 6.0 bar, preferably 3.0 to 5.0 bar.
  • the amount of nitrogen recompressed in the circuit on the pre-separation column is - depending on the purity of the oxygen product - for example 3% to 30%, preferably 10 to 20% of the total amount of feed air (standard volume).
  • the indirect heat exchange for liquefying the nitrogen-enriched top fraction is preferably carried out against at least part of the oxygen-enriched bottom fraction, which evaporates in the process.
  • the circuit at the head of the pre-disassembly column thus also serves as a sump heater the pre-disassembly column.
  • the condenser-evaporator, in which the indirect heat exchange takes place, can be arranged inside or outside the pre-separation column.
  • reflux can be generated in the process according to the invention in that at least a portion of the gaseous nitrogen from the low pressure column is heated, compressed, liquefied by indirect heat exchange and returned to the rectification column system, in particular to the low pressure column.
  • the compression of the gaseous nitrogen takes place, for example, at approximately ambient temperature and leads to a pressure of, for example, 4.0 to 6.0 bar, preferably 4.5 to 5.0 bar.
  • the amount of nitrogen recompressed in the circuit on the low-pressure column is - depending on the purity of the oxygen product - for example 30% to 90%, preferably 40 to 80% of the total amount of feed air (standard volume).
  • the indirect heat exchange for liquefying the gaseous nitrogen is preferably carried out against at least part of the liquid oxygen from the low-pressure column, which evaporates in the process.
  • the circuit at the top of the low pressure column thus also serves to heat the bottom of the low pressure column.
  • the condenser-evaporator, in which the indirect heat exchange takes place, can be arranged inside or outside the low-pressure column.
  • Each of the two columns preferably has such a circuit, the entire amount of circuit being fed back into the corresponding column.
  • the liquefied top fraction from one column can be given in whole or in part as reflux to the other column.
  • the top fraction to be recompressed can be heated in a main heat exchanger against the feed air to be cooled.
  • the recompressed fraction is preferably also cooled again in this main heat exchanger before liquefaction.
  • Part of the feed air can be expanded while performing work, in order to gain cold to compensate for exchange and insulation losses and, if necessary, for product liquefaction. It is advantageous if the part of the feed air to be relaxed while working is recompressed upstream of the relaxing work. Energy gained during the work-relieving relaxation is preferably used for recompression of the part to be relieved of work the air used.
  • the expansion machine and post-compressor can be mechanically coupled for this purpose.
  • the invention also relates to a device for the low-temperature separation of air according to claims 9 to 13.
  • Feed air 1 is compressed in a main air compressor 2 to a pressure of, for example, 1.2 bar to 1.5 bar, preferably 1.3 bar to 1.4 bar, most preferably approximately 1.35 bar. At least some of the compressed feed air 3 flows via a line 4 to a main heat exchanger 5, is cooled there against product flows and is fed via lines 6 and 7 into a pre-separation column 10, the operating pressure of which is 1.1 to 1.4 bar, preferably 1, 15 to 1.35 bar, most preferably about 1.25 bar. Part of the cooled air can also be passed through line 8 through a heat exchanger 9.
  • nitrogen is obtained as the top gas and an oxygen-enriched liquid as the bottom fraction.
  • the nitrogen-enriched top fraction 11 is heated in the heat exchanger 9 and (line 12) further in the main heat exchanger 5 to about ambient temperature, in a first recompressor 13 to a pressure of 2.8 to 5 bar, preferably 2.9 to 4 bar, most preferably about 3 , 0 bar compressed, via line 14 back to the main heat exchanger 5 and from the cold end of it to a first condenser-evaporator 16 (15).
  • a first condenser-evaporator 16 15
  • the condensate is throttled - if necessary after subcooling in 9 - into the pre-separation column 10 (17, 18).
  • the amount of circulation passed through the recompressor 13 is 10% of the total feed air (standard volume).
  • the condenser-evaporator 16 can be arranged outside the sump of the pre-separation column 10, in a departure from the illustration.
  • the entire bottom liquid of the pre-separation column which is not evaporated in the first condenser-evaporator 16, flows via line 19 into a low-pressure column 20, preferably a few theoretical plates above the Swamp.
  • steam 21 can be fed into the low pressure column from the sump of the pre-separation column.
  • Part of the liquid 17 obtained in this first circuit can be introduced directly or - via line 22 as shown in the drawing - indirectly into the low-pressure column 20, which works under a pressure of 1.1 to 1.4 bar, preferably 1.15 to 1.25 bar, most preferably about 1.2 bar.
  • the feed point is below the head, but above that of the bottom fraction 19, 21.
  • gaseous nitrogen 23 is drawn off from the top of the low-pressure column 20, optionally warmed to approximately ambient temperature in a heat exchanger 24 and (line 25) further in the main heat exchanger 5, in a second recompressor 26 to a pressure of 4 to 6 bar, preferably 4.5 to 5.0 bar, most preferably compressed about 4.7 bar, back via line 27 to the main heat exchanger 5 and from its cold end to a second condenser-evaporator 29 (28).
  • a second condenser-evaporator 29 There it is at least partially, preferably completely or essentially completely, liquefied in indirect heat exchange with evaporating bottom liquid (oxygen) from the low-pressure column.
  • the condensate is throttled into the low-pressure column 20 (30, 31), if necessary after subcooling in 24. Part of the heated gaseous nitrogen can be removed as residual gas or product before or after the recompression (line 32). In the exemplary embodiment, the amount of circulation passed through the recompressor 26 is 74% of the total feed air (standard volume).
  • the condenser-evaporator 29 can be arranged outside the sump of the low-pressure column 20, in a departure from the illustration.
  • Gaseous product oxygen 34 with a purity of, for example, 80 to 99.9% by volume, preferably 90 to 99.5% by volume, is withdrawn via line 33 and likewise heated in the main heat exchanger 5. If necessary, the oxygen product or a part thereof can be removed in liquid form (line 35). To produce a high-pressure product, the liquid oxygen removed can be pressurized and evaporated (internal compression). If desired, a portion of the condensed nitrogen can be recovered upstream or downstream of valve 31 as a liquid product.
  • a portion 36 (for example 10 to 60 vol%, preferably 45 to 55 vol%, most preferably approximately 53 vol%) of the feed air is relaxed in a relaxation machine 40, and then above the remaining feed air 7, 8 into the pre-separation column 10 fed (41).
  • the air to be expanded to perform the work is previously compressed to a pressure of 1.5 to 4 bar, preferably 1.5 to 2.5 bar, most preferably approximately 1.9 bar, by means of a secondary compressor 38 driven by the expansion machine 40 and, if appropriate by an additional, externally driven compressor 37.
  • the compressed fluid is cooled in indirect heat exchange with cooling water, as indicated by the aftercoolers shown in the drawing.
  • intermediate cooling is preferably carried out between two stages.
  • the cleaning of the feed air is not shown in the drawing. It can be carried out by any of the known methods, for example in a switchable heat exchanger (Revex) or in one or more molecular sieve systems. In the latter case, it is possible to subject all of the feed air (line 3) to cleaning together.
  • Revex switchable heat exchanger
  • molecular sieve systems molecular sieve systems
  • the mass transfer elements in the pre-separation column are formed by still bottoms, those in the low pressure column by orderly packing.
  • conventional still bottoms, packing elements (unordered packing) and / or ordered packing can be used in each of the two columns in the invention. Combinations of different types of elements in one column are also possible. Because of the low pressure drop, ordered packings in all columns, especially in the low pressure column, are preferred. These further increase the energy-saving effect of the invention.

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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)
EP96117880A 1995-11-21 1996-11-07 Procédé et dispositif à double colonne pour la séparation cryogénique d'air Withdrawn EP0775880A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19543395A DE19543395A1 (de) 1995-11-21 1995-11-21 Doppelsäulenverfahren und -vorrichtung zur Tieftemperaturzerlegung von Luft
DE19543395 1995-11-21

Publications (2)

Publication Number Publication Date
EP0775880A2 true EP0775880A2 (fr) 1997-05-28
EP0775880A3 EP0775880A3 (fr) 1998-02-25

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Application Number Title Priority Date Filing Date
EP96117880A Withdrawn EP0775880A3 (fr) 1995-11-21 1996-11-07 Procédé et dispositif à double colonne pour la séparation cryogénique d'air

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US (1) US5813251A (fr)
EP (1) EP0775880A3 (fr)
DE (1) DE19543395A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10013075A1 (de) * 2000-03-17 2001-09-20 Linde Ag Verfahren zur Gewinnung von gasförmigem und flüssigem Stickstoff mit variablem Anteil des Flüssigprodukts
DE10013074A1 (de) * 2000-03-17 2001-09-20 Linde Ag Verfahren zur Gewinnung von gasförmigem Stickstoff
DE102007051184A1 (de) * 2007-10-25 2009-04-30 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Tieftemperatur-Luftzerlegung

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2854508C2 (de) 1978-12-16 1981-12-03 Linde Ag, 6200 Wiesbaden Verfahren und Vorrichtung zur Tieftemperaturzerlegung eines Gasgemisches
EP0377117B1 (fr) 1988-12-01 1992-03-25 Linde Aktiengesellschaft Procédé et dispositif de séparation de l'air

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1271419A (en) * 1969-08-16 1972-04-19 Bernard Ramsey Bligh Air distillation process
US4507134A (en) * 1983-06-02 1985-03-26 Kabushiki Kaisha Kobe Seiko Sho Air fractionation method
US4704148A (en) * 1986-08-20 1987-11-03 Air Products And Chemicals, Inc. Cycle to produce low purity oxygen
DE3817244A1 (de) * 1988-05-20 1989-11-23 Linde Ag Verfahren zur tieftemperaturzerlegung von luft
DE4030749A1 (de) * 1990-09-28 1992-04-02 Linde Ag Verfahren zur tieftemperaturzerlegung von luft
DE4406049A1 (de) * 1994-02-24 1995-09-07 Linde Ag Verfahren und Vorrichtung zur Gewinnung von reinem Argon
CA2142318A1 (fr) * 1994-02-24 1995-08-25 Horst Corduan Methode et appareil pour la recuperation d'argon pur

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2854508C2 (de) 1978-12-16 1981-12-03 Linde Ag, 6200 Wiesbaden Verfahren und Vorrichtung zur Tieftemperaturzerlegung eines Gasgemisches
EP0377117B1 (fr) 1988-12-01 1992-03-25 Linde Aktiengesellschaft Procédé et dispositif de séparation de l'air

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EP0775880A3 (fr) 1998-02-25
DE19543395A1 (de) 1997-05-22
US5813251A (en) 1998-09-29

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