US1880981A - Separation of oxygen, nitrogen, and argon from air - Google Patents

Separation of oxygen, nitrogen, and argon from air Download PDF

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Publication number
US1880981A
US1880981A US465772A US46577230A US1880981A US 1880981 A US1880981 A US 1880981A US 465772 A US465772 A US 465772A US 46577230 A US46577230 A US 46577230A US 1880981 A US1880981 A US 1880981A
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nitrogen
oxygen
argon
column
rectification
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US465772A
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Pollitzer Franz
Stark Stephan
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • F25J3/04715—The auxiliary column system simultaneously produces oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/08—Processes or apparatus using separation by rectification in a triple pressure main 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/923—Inert gas
    • Y10S62/924—Argon

Definitions

  • the invention relates to a process for obtaining oxygen and nitrogen by a two-stage rectification of liquid air with the simultaneous production of ⁇ argon in a third rectifying column.
  • the maj orportion of the nitrogen is first separated and the residue consisting principally of oxygen and argon is separated into pure oxygen and a mixture rich in argon by a further rectification.
  • the heat-interchange necessary for effecting the latter rectification is obtainedv by means of a cycle either of nitrogen, with indirect heating or cooling of the column, or of argon, with direct exchange.
  • the present invention makes possible a considerable simplification and reduction of expense in the production of argon in connection with the two-stage rectification of air.
  • nitrogen is obtained under a pressure which is sufficient to permit its condensation in the oxygen-rich liquid in the lower part of the argon rectification column.
  • a portion of the nitrogen is withdrawn from the first column in the gaseous state and utilized for heating and cooling the argon column. I-Iitherto this nitrogen, insofar as it was not returned in the liquid state to the first rectification column, was utilized for washing oxygen out of the nitrogen vapors in the second rectification column, and as much nitrogen as was available was used for this purpose in order to make the washing operation as complete as possible.
  • the withdrawal of nitrogen for use in the argon column has heretofore been considered to be incompatible with the obtaining of a high yield of oxygen or the production of a practically pure nitrogen.
  • l and 2 are 4the two rectifying columns of a two-stage rectifier, such as is commonly used for the production of oxygen and nitrogen.
  • 3 is the argon rectification column, the argon-oxygen mixture being introduced through pipe 4.
  • the pressure column l contains a sufficient number of plates that nitrogen containing 1% or less of oxygen is obtained at the upper end.
  • the second column is made so large that it has the effect of fifteen ideal rectification plates. In this way the nitrogen vapor may be purified to a content of oxygen of about 2%. ,0
  • argon column For heating the argon column a part. of the nitrogen is withdrawn in the gaseous state from the nitrogen condenser 5 or below it, at the pressure of about five atmospheres existing in column l and is liquefied in coil 6 of the argon vaporizer 7.y The liquid nitrogen is then expanded through valve 8 into condenser 9 as a cooling means for the condenser. The vaporized nitrogen leaving lat 10 can be conducted, together with the nitrogen leav-,BO ing the second column at 1l, to a counter current heat exchanger (not shown).
  • A-process for the production of argon, oxy- 15 gen and nitrogen by the low temperature rectification of air which comprises subjecting liquid air to two stages of rectification, operating the first stage to produce a fraction containing a high percentage of nitrogen, withdrawing only a portion of the oxygenargon mixture in liquid form from the second rectification stage at a point where the oxygen content of the liquid is about 90 to 98%, lntroducing said oxygen-argon mixture into the middle portion of a further rectification column, and subjecting said oxygen-argon mixture to further rectification, the mixture being heated by the liquefaction of a portion ofthe gaseous nitrogen fraction from the lirst stage and being cooled by the evaporation of the nitrogen thus liquefied, high percentage oxygen being obtained at the bottom of said further rectification column.
  • FRANZ POLLITZER STEPHAN STARK.

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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)

Description

'0a.4, 1932. F. POLLmER Em. `1,880,981
SEPARATION OF OXYGEN, NITROGEN, AND ARGON FROM AIR Filed July 3, 1930 Patented Oct. 4, A1932 isaiasi UNITED erlfiasl PATENT.; OFFICE FRANZ IPOLLITZER, F GROSSHESSELOHE, NEAR MUNICH, AND STEPHAN STARK,
' GRUNWALD, NEAR MUNICH, GERMANY SEPARATION 0F OXYGEN, NITRUGEN, AND AEGON FROM AIB Application filed July 3, 1930, Serial No. 465,772, and in Germany February 8, 1930.
The invention relates to a process for obtaining oxygen and nitrogen by a two-stage rectification of liquid air with the simultaneous production of` argon in a third rectifying column.
For the separation of argon from the air, the maj orportion of the nitrogen is first separated and the residue consisting principally of oxygen and argon is separated into pure oxygen and a mixture rich in argon by a further rectification. The heat-interchange necessary for effecting the latter rectification is obtainedv by means of a cycle either of nitrogen, with indirect heating or cooling of the column, or of argon, with direct exchange.
The present invention makes possible a considerable simplification and reduction of expense in the production of argon in connection with the two-stage rectification of air. In the first stage nitrogen is obtained under a pressure which is sufficient to permit its condensation in the oxygen-rich liquid in the lower part of the argon rectification column. In the process of the invention a portion of the nitrogen is withdrawn from the first column in the gaseous state and utilized for heating and cooling the argon column. I-Iitherto this nitrogen, insofar as it was not returned in the liquid state to the first rectification column, was utilized for washing oxygen out of the nitrogen vapors in the second rectification column, and as much nitrogen as was available was used for this purpose in order to make the washing operation as complete as possible. The withdrawal of nitrogen for use in the argon column has heretofore been considered to be incompatible with the obtaining of a high yield of oxygen or the production of a practically pure nitrogen.
In the process of the invention a part of the oxygen-rich mixture is reworked in the argon column. At the same time the first column is operated to produce a fraction containing a high percentage of nitrogen, and in lthe second column the rectification is improved by increasing the plate number or effeet.. It was found that the withdrawal of argon fromthesecond column promotes the separation of oxygen and nitrogen, and comensates the unfavorable effect of diminishing the amount of washing liquid.
By way of illustration, one method of carrying out the invention will be described with reference to the accompanying schematic drawing.
In the drawing, l and 2 are 4the two rectifying columns of a two-stage rectifier, such as is commonly used for the production of oxygen and nitrogen. 3 is the argon rectification column, the argon-oxygen mixture being introduced through pipe 4. The pressure column l contains a sufficient number of plates that nitrogen containing 1% or less of oxygen is obtained at the upper end. The second column is made so large that it has the effect of fifteen ideal rectification plates. In this way the nitrogen vapor may be purified to a content of oxygen of about 2%. ,0
For heating the argon column a part. of the nitrogen is withdrawn in the gaseous state from the nitrogen condenser 5 or below it, at the pressure of about five atmospheres existing in column l and is liquefied in coil 6 of the argon vaporizer 7.y The liquid nitrogen is then expanded through valve 8 into condenser 9 as a cooling means for the condenser. The vaporized nitrogen leaving lat 10 can be conducted, together with the nitrogen leav-,BO ing the second column at 1l, to a counter current heat exchanger (not shown).
In the method of operation herein described only a part of the oxygen obtained in column 2, for example one-half, is introduced into the argon rectifying column 3. If column 2 is operated to produce an oxygen of over 99% in purity, as is demanded by present industrial requirements, very little argon would be obtained by the further working of this oxygen. Therefore, in the process of the invention the oxygen to be treated in the argon column is withdrawn from a higher portion of column 2 where the oxygen content of the liquid is between 90 and 98%. g5 In the lower part of column 3 this oxygen is brought to the same or a higher purity as that produced in column 2. The lower parts of the two columns therefore operate in parallel with reference to the liquid. With this 100 method of operation it is possible to withdraw at 12 a substantial proportion of the argon content of the air, in the form of aV mixture containing 50% to 90% of ar on.
v A Thus the process of the invention aior s a.
simple method of simultaneously obtaining from the airy practically pure oxygen, nitrogen and argon.
In the same way the process is generally 1o applicable to the separatlon of ternag mixtures, where the ar on is represente by a gas of intermediate oiling point,
' We claim:
A-process for the production of argon, oxy- 15 gen and nitrogen by the low temperature rectification of air which comprises subjecting liquid air to two stages of rectification, operating the first stage to produce a fraction containing a high percentage of nitrogen, withdrawing only a portion of the oxygenargon mixture in liquid form from the second rectification stage at a point where the oxygen content of the liquid is about 90 to 98%, lntroducing said oxygen-argon mixture into the middle portion of a further rectification column, and subjecting said oxygen-argon mixture to further rectification, the mixture being heated by the liquefaction of a portion ofthe gaseous nitrogen fraction from the lirst stage and being cooled by the evaporation of the nitrogen thus liquefied, high percentage oxygen being obtained at the bottom of said further rectification column.
In testimony whereof, We ax our signatures.
FRANZ POLLITZER. STEPHAN STARK.
US465772A 1930-02-07 1930-07-03 Separation of oxygen, nitrogen, and argon from air Expired - Lifetime US1880981A (en)

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Cited By (34)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2424201A (en) * 1944-02-19 1947-07-15 Air Reduction Separation of the constituents of gaseous mixtures
US2480093A (en) * 1943-05-27 1949-08-23 Air Prod Inc Method of and apparatus for pumping liquid oxygen
US2519892A (en) * 1945-01-16 1950-08-22 Air Reduction Method of producing liquid oxygen
US2547177A (en) * 1948-11-02 1951-04-03 Linde Air Prod Co Process of and apparatus for separating ternary gas mixtures
US2552451A (en) * 1947-07-03 1951-05-08 Standard Oil Dev Co Fractionation of low molecular weight component mixtures
US2559132A (en) * 1948-02-12 1951-07-03 British Oxygen Co Ltd Fractional separation of air
US2597385A (en) * 1946-02-11 1952-05-20 Air Prod Inc Separation of gas mixtures
US2626510A (en) * 1947-06-18 1953-01-27 Air Prod Inc Air fractionating cycle and apparatus
US2650483A (en) * 1949-04-19 1953-09-01 British Oxygen Co Ltd Separation of air
US2700282A (en) * 1948-02-12 1955-01-25 British Oxygen Co Ltd Fractional separation of air
US2728205A (en) * 1949-06-20 1955-12-27 Linde Eismasch Ag Process of and apparatus for the production of argon
US2817216A (en) * 1952-08-12 1957-12-24 Air Liquide Process and apparatus for the separation, by rectification, of a gas mixture containing at least three components
US2824428A (en) * 1957-03-19 1958-02-25 Union Carbide Corp Process and apparatus for separating air
US2934908A (en) * 1954-08-16 1960-05-03 Union Carbide Corp High argon recovery using proper shelf-top pinch principle
US2982107A (en) * 1957-12-16 1961-05-02 Air Reduction Separation of the elements of air
US3214926A (en) * 1963-04-15 1965-11-02 Philips Corp Method of producing liquid oxygen and/or liquid nitrogen
US3264830A (en) * 1963-08-09 1966-08-09 Air Reduction Separation of the elements of air
US3363426A (en) * 1963-10-29 1968-01-16 Stoklosinski Roman Gas separation with particular reference to air separation
US3688513A (en) * 1969-05-06 1972-09-05 Martin Streich Production of nitrogen and argon-free oxygen
US3729943A (en) * 1969-05-05 1973-05-01 Georges Claude Process for separation of ternary gaseous mixtures by rectification
US4137056A (en) * 1974-04-26 1979-01-30 Golovko Georgy A Process for low-temperature separation of air
US4433990A (en) 1981-12-08 1984-02-28 Union Carbide Corporation Process to recover argon from oxygen-only air separation plant
EP0286314A1 (en) * 1987-04-07 1988-10-12 The BOC Group plc Air separation
US4838785A (en) * 1988-07-05 1989-06-13 Cameron Forge Company Walking beam furnace insulation
US4838913A (en) * 1988-02-10 1989-06-13 Union Carbide Corporation Double column air separation process with hybrid upper column
US5305611A (en) * 1992-10-23 1994-04-26 Praxair Technology, Inc. Cryogenic rectification system with thermally integrated argon column
US5778699A (en) * 1995-09-29 1998-07-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and installation for the production of argon by cryogenic distillation
EP1055891A1 (en) * 1999-05-25 2000-11-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Cryogenic distillation system for air separation
EP1055890A1 (en) * 1999-05-25 2000-11-29 L'air Liquide Société Anonyme pour l'étude et l'exploitation des procédés Georges Claude Cryogenic distillation system for air separation
EP1055892A1 (en) * 1999-05-25 2000-11-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Cryogenic distillation system for air separation
EP1055893A1 (en) * 1999-05-25 2000-11-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Cryogenic distillation system for air separation
JP2007192466A (en) * 2006-01-19 2007-08-02 Nippon Steel Corp Cryogenic air separation plant and its control method
CN114735666A (en) * 2022-06-09 2022-07-12 北京化工大学 Process for separating and refining rare gas
US11413569B2 (en) * 2018-08-23 2022-08-16 Koninklijke Philips N.V. Hybrid oxygen concentrator with oxygen side balancing

Cited By (41)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2480093A (en) * 1943-05-27 1949-08-23 Air Prod Inc Method of and apparatus for pumping liquid oxygen
US2424201A (en) * 1944-02-19 1947-07-15 Air Reduction Separation of the constituents of gaseous mixtures
US2519892A (en) * 1945-01-16 1950-08-22 Air Reduction Method of producing liquid oxygen
US2597385A (en) * 1946-02-11 1952-05-20 Air Prod Inc Separation of gas mixtures
US2626510A (en) * 1947-06-18 1953-01-27 Air Prod Inc Air fractionating cycle and apparatus
US2552451A (en) * 1947-07-03 1951-05-08 Standard Oil Dev Co Fractionation of low molecular weight component mixtures
US2559132A (en) * 1948-02-12 1951-07-03 British Oxygen Co Ltd Fractional separation of air
US2700282A (en) * 1948-02-12 1955-01-25 British Oxygen Co Ltd Fractional separation of air
US2547177A (en) * 1948-11-02 1951-04-03 Linde Air Prod Co Process of and apparatus for separating ternary gas mixtures
US2650483A (en) * 1949-04-19 1953-09-01 British Oxygen Co Ltd Separation of air
US2728205A (en) * 1949-06-20 1955-12-27 Linde Eismasch Ag Process of and apparatus for the production of argon
US2817216A (en) * 1952-08-12 1957-12-24 Air Liquide Process and apparatus for the separation, by rectification, of a gas mixture containing at least three components
US2934908A (en) * 1954-08-16 1960-05-03 Union Carbide Corp High argon recovery using proper shelf-top pinch principle
US2824428A (en) * 1957-03-19 1958-02-25 Union Carbide Corp Process and apparatus for separating air
US2982107A (en) * 1957-12-16 1961-05-02 Air Reduction Separation of the elements of air
US3214926A (en) * 1963-04-15 1965-11-02 Philips Corp Method of producing liquid oxygen and/or liquid nitrogen
US3264830A (en) * 1963-08-09 1966-08-09 Air Reduction Separation of the elements of air
US3363426A (en) * 1963-10-29 1968-01-16 Stoklosinski Roman Gas separation with particular reference to air separation
US3729943A (en) * 1969-05-05 1973-05-01 Georges Claude Process for separation of ternary gaseous mixtures by rectification
US3688513A (en) * 1969-05-06 1972-09-05 Martin Streich Production of nitrogen and argon-free oxygen
US4137056A (en) * 1974-04-26 1979-01-30 Golovko Georgy A Process for low-temperature separation of air
US4433990A (en) 1981-12-08 1984-02-28 Union Carbide Corporation Process to recover argon from oxygen-only air separation plant
EP0286314A1 (en) * 1987-04-07 1988-10-12 The BOC Group plc Air separation
US4883516A (en) * 1987-04-07 1989-11-28 The Boc Group, Inc. Air separation
US4838913A (en) * 1988-02-10 1989-06-13 Union Carbide Corporation Double column air separation process with hybrid upper column
US4838785A (en) * 1988-07-05 1989-06-13 Cameron Forge Company Walking beam furnace insulation
US5305611A (en) * 1992-10-23 1994-04-26 Praxair Technology, Inc. Cryogenic rectification system with thermally integrated argon column
US5778699A (en) * 1995-09-29 1998-07-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and installation for the production of argon by cryogenic distillation
EP1055893A1 (en) * 1999-05-25 2000-11-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Cryogenic distillation system for air separation
EP1055890A1 (en) * 1999-05-25 2000-11-29 L'air Liquide Société Anonyme pour l'étude et l'exploitation des procédés Georges Claude Cryogenic distillation system for air separation
EP1055892A1 (en) * 1999-05-25 2000-11-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Cryogenic distillation system for air separation
EP1055891A1 (en) * 1999-05-25 2000-11-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Cryogenic distillation system for air separation
JP2000356465A (en) * 1999-05-25 2000-12-26 L'air Liquide Low-temperature distillating system for separating air
US6202441B1 (en) 1999-05-25 2001-03-20 Air Liquide Process And Construction, Inc. Cryogenic distillation system for air separation
US6276170B1 (en) 1999-05-25 2001-08-21 Air Liquide Process And Construction Cryogenic distillation system for air separation
US6347534B1 (en) 1999-05-25 2002-02-19 Air Liquide Process And Construction Cryogenic distillation system for air separation
JP4540182B2 (en) * 1999-05-25 2010-09-08 レール・リキード−ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード Cryogenic distillation system for air separation
JP2007192466A (en) * 2006-01-19 2007-08-02 Nippon Steel Corp Cryogenic air separation plant and its control method
JP4551334B2 (en) * 2006-01-19 2010-09-29 新日本製鐵株式会社 Cryogenic air separation device and control method thereof
US11413569B2 (en) * 2018-08-23 2022-08-16 Koninklijke Philips N.V. Hybrid oxygen concentrator with oxygen side balancing
CN114735666A (en) * 2022-06-09 2022-07-12 北京化工大学 Process for separating and refining rare gas

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DE542400C (en) 1932-01-23
NL30531C (en)
GB358842A (en) 1931-10-15

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