US3751933A - Method of air separation into oxygen and argon - Google Patents

Method of air separation into oxygen and argon Download PDF

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Publication number
US3751933A
US3751933A US00162792A US3751933DA US3751933A US 3751933 A US3751933 A US 3751933A US 00162792 A US00162792 A US 00162792A US 3751933D A US3751933D A US 3751933DA US 3751933 A US3751933 A US 3751933A
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United States
Prior art keywords
oxygen
argon
column
liquid
fraction
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Expired - Lifetime
Application number
US00162792A
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English (en)
Inventor
S Misarenko
L Tsitrin
E Borzenko
G Golovko
V Boiko
V Malchenko
G Balabaev
B Tolstogo
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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
    • F25J3/04406—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 dual pressure main column system
    • F25J3/04412—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 dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of 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
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
    • 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
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/92—Details relating to the feed point
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen
    • 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

  • ABSTRACT A method of air separation into oxygen and argon in double rectification columns with the drawing off of liquid or gaseous oxygen and simultaneous obtaining of argon by withdrawing a fraction of raw argon from one of the plates. of the upper rectifying column, with a portion of the liquid oxygen flow being returned to said rectifying column onto a plate thereof that is located below the raw argon fraction withdrawal zone, whereby a forced circulation flow of liquid oxygen is created.
  • the present invention relates to methods of producing oxygen, and more particularly to methods of air separation into oxygen and argon.
  • the installation for carrying out said method besides a double rectification column with. a condenser, comprises heat-exchange equipment, throttle valves, acetylene adsorbers, recoolers and a rectifying column for raw argon.
  • the still liquor is directed through the acetylene adsorber, expander and recooler into the middle portion of the upper column. Nitrogen from the pockets of the lower column is directed through the recooler and ex pander valve to the upper plate of the upper column. From the upper column, below the still liquor inlet, a fraction is withdrawn to be rectified in the raw argon column, the fraction having the following composition: 9 I 1 vol. percent of argon, about 0.5 percent of nitrogen, the rest being oxygen. From the upper portion of the raw argon column gaseous raw argon is drawn off that has the following composition: 90 92 vol. percent of argon, -4 vol. percent of nitrogen and 5-4 vol. percent of oxygen.
  • the oxygen produced as a result of rectification whose purity is 99.2-99.5 vol. percent, is accumulated in the condenser and is drawn off from the column in a liquid or gaseous state or, else, in a-liquid and partially gaseous state.
  • the known method is disadvantageous in that the purity of oxygen thus produced is not adequately high for ensuring cutting of metal without burrs.
  • the coefficient of obtaining raw argon is not sufficiently high either.
  • the argon fraction being withdrawn contains nitrogen which sharply deteriorates the rectification process in the raw argon column and is responsible for considerable losses of argon in the course of its further purification.
  • An object of the present invention is to provide a method of air separation into oxygen and argon which would ensure the production of oxygen with a purity as high as 99.9 vol. percent.
  • Another object of the invention is to increase the amount of raw argon obtained and to decrease the content of nitrogen therein.
  • the essence of the present invention resides in that in a method of air separation into oxygen and argon in double rectification columns with the drawing off of liquid or gaseous oxygen and simultaneous production of argon by withdrawing a fraction of raw argon from one of the plates of the upper column, a portion of the liquid oxygen flow is returned to the rectifying column onto its plate that is located below the raw argon fraction withdrawal zone, whereby a forced circulation flow of liquid oxygen is created.
  • Highly pressurized air after the main heat exchanger (not shown) having a temperature of from l40 to 1 50 C and pressure of 180 to 200 gauge atm. is throttled by a throttle valve 2 along a pipeline 1 and directed 'Lto a lower column 3.
  • Air from the expander is also directed to the lower column 3 along a pipeline 4.
  • liquid nitrogen is collected, which through a recooler 6 and a throttle valve 7 is directed to an upper column 8.
  • the still liquor containing 36 to 40 vol. percent of oxygen from the still 9 of the lower column 3 through acetylene adsorbers l0 and a throttle valve 11 is supplied into the middle portion of the upper column 8.
  • Oxygen that has collected in a condenser 12 is drawn off in a liquid state through a recooler 13, and a portion of oxygen is drawn off in a gaseous state along a pipeline 14 through a heat exchanger (not shown).
  • an oxygen circulation flow is introduced by feeding a portion of liquid oxygen that has been withdrawn after the recooler 13 or before it by a pump 15 into the upper column 8 onto one of its plates located below the argon fraction withdrawal zone.
  • the introduction of the oxygen circulation flow results in an increase of oxygen concentration in the place of such introduction, better rectification conditions are created on the bottom plates of the upper rectifying column 8 and the concentration of oxygen in the liquid of the condenser 12 is increased to about 99.9 vol. percent.
  • the content of nitrogen is brought down to 0.1 vol. percent in the argon fraction withdrawn from the upper column 8 in the form of vapors along a pipeline 16; better conditions are created for rectification in a raw argon column 17, since the fraction composition then closer approximates a binary mixture, so that the yield of raw argon is increased and the quality thereof becomes higher.
  • the high-quality raw argon (97.5 to 98.0 vol. percent of argon, 0.2 to 0.5 vol. percent,"of nitrogen, the rest being oxygen) is withdrawn from the raw argon column 17 in a gaseous state along a pipeline l8, and the downflowing liquid phlegm is returned to the upper column 8 along a pipeline l9.
  • Condenser 20 of the raw argon column 17 is fed with the still liquor.
  • Nitrogen is removed from the upper column 8 along a pipeline 21 through the recoolers 6 and 13 and other rectifying column with the drawing off of liquid or gaseous oxygen; simultaneously withdrawing a fraction of raw argon from an upper section of said rectifying columnand returning a portion of the flow of liquid oxygen to the rectifying column at a point below the raw argon fraction withdrawal zone, a forced circulation flow of liquid oxygen being thus created.

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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)
US00162792A 1971-07-14 1971-07-15 Method of air separation into oxygen and argon Expired - Lifetime US3751933A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE2135235A DE2135235A1 (de) 1971-07-14 1971-07-14 Verfahren zur luftzerlegung unter gewinnung von sauerstoff und argon

Publications (1)

Publication Number Publication Date
US3751933A true US3751933A (en) 1973-08-14

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ID=5813683

Family Applications (1)

Application Number Title Priority Date Filing Date
US00162792A Expired - Lifetime US3751933A (en) 1971-07-14 1971-07-15 Method of air separation into oxygen and argon

Country Status (5)

Country Link
US (1) US3751933A (fr)
BE (1) BE770620A (fr)
DE (1) DE2135235A1 (fr)
FR (1) FR2150218A1 (fr)
NL (1) NL7109958A (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4137056A (en) * 1974-04-26 1979-01-30 Golovko Georgy A Process for low-temperature separation of air
US4615716A (en) * 1985-08-27 1986-10-07 Air Products And Chemicals, Inc. Process for producing ultra high purity oxygen
US4723975A (en) * 1985-05-17 1988-02-09 The Boc Group Plc Air separation method and apparatus
WO1988006705A1 (fr) * 1987-02-26 1988-09-07 Donald Erickson Pression accrue d'alimentation en oxygene tres pur a faible consommation d'energie
US4843828A (en) * 1985-10-04 1989-07-04 The Boc Group, Plc Liquid-vapor contact method and apparatus
US5078766A (en) * 1989-07-28 1992-01-07 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Equipment for air distillation to produce argon

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2547177A (en) * 1948-11-02 1951-04-03 Linde Air Prod Co Process of and apparatus for separating ternary gas mixtures
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
US3127260A (en) * 1964-03-31 Separation of air into nitrogen
US3596471A (en) * 1968-03-15 1971-08-03 Messer Griesheim Gmbh Process for recovering a mixture of krypton and xenon from air with argon stripper

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3127260A (en) * 1964-03-31 Separation of air into nitrogen
US2547177A (en) * 1948-11-02 1951-04-03 Linde Air Prod Co Process of and apparatus for separating ternary gas mixtures
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
US3596471A (en) * 1968-03-15 1971-08-03 Messer Griesheim Gmbh Process for recovering a mixture of krypton and xenon from air with argon stripper

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4137056A (en) * 1974-04-26 1979-01-30 Golovko Georgy A Process for low-temperature separation of air
US4781739A (en) * 1984-08-20 1988-11-01 Erickson Donald C Low energy high purity oxygen increased delivery pressure
US4723975A (en) * 1985-05-17 1988-02-09 The Boc Group Plc Air separation method and apparatus
US4615716A (en) * 1985-08-27 1986-10-07 Air Products And Chemicals, Inc. Process for producing ultra high purity oxygen
US4843828A (en) * 1985-10-04 1989-07-04 The Boc Group, Plc Liquid-vapor contact method and apparatus
WO1988006705A1 (fr) * 1987-02-26 1988-09-07 Donald Erickson Pression accrue d'alimentation en oxygene tres pur a faible consommation d'energie
US5078766A (en) * 1989-07-28 1992-01-07 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Equipment for air distillation to produce argon

Also Published As

Publication number Publication date
DE2135235A1 (de) 1973-08-16
FR2150218A1 (fr) 1973-04-06
BE770620A (fr) 1972-01-28
NL7109958A (fr) 1973-01-23

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