US2779174A - Low temperature separation of gaseous mixtures - Google Patents

Low temperature separation of gaseous mixtures Download PDF

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Publication number
US2779174A
US2779174A US465712A US46571254A US2779174A US 2779174 A US2779174 A US 2779174A US 465712 A US465712 A US 465712A US 46571254 A US46571254 A US 46571254A US 2779174 A US2779174 A US 2779174A
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column
pressure
oxygen
air
rectification
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US465712A
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English (en)
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Vesque Henri
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Air Liquide SA
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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
    • F25J3/04666—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
    • 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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04242—Cold end purification of the feed air
    • 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
    • F25J3/04406—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
    • F25J3/04684—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 and a bottom re-boiler
    • 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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04854—Safety aspects of operation
    • 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
    • F25J2200/52—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high pressure column of a double 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
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • 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
    • Y10S62/939—Partial feed stream expansion, air
    • Y10S62/94—High pressure column

Definitions

  • This fraction is generally a mixture made up essentially cause the argon, scarcely more volatile than the oxygen, 7
  • the invention embodies the following features. All air to be separated, compressed to a pressure greater than that of the high pressure column, and cooled by exchange with the products of its separation to a temperature appreciably higher than its temperature of liquefaction under the said pressure, is divided into two parts. One of these parts is introduced into the high pressure column withan expansion elfected, preferably with performance of external work, to the pressure of this column. The other part is cooled to the temperature of liquefaction, and partially liquefied by heat exchange pressure column.
  • the liquid thus obtained is used, after expansion, to cause by its vaporization, cooling by in direct contact with the upper part of the auxiliary column
  • the liquid from the coil at the bottom of the high pressure column may first be passed through a coil at the bottom .of the auxiliary column.
  • the gas resulting from this vaporization is introduced into the low pressure column.
  • a first heat exchanger z coole d by separated gases leaving in the neighbourhood of atmospheric pressure.
  • a first part representing approximately 70% of the'air to be separated is expanded by the turbine 4 to a pressure of approximately five atmospheres and enters'atgthis pressure, by the tube 5, intol the high pressure column 10, several trays above the-bottom;
  • the second part is cooled in a heat exchanger 3 to a temperature .of about -158 C., and enters by the tube '6' into'a'coil 7 located a-tthe lower part of the column 10.
  • The'column 10 is surmounted by a column 11 functioning in the neighbourhood of atmospheric pressure.
  • the two columns are thermically connectedby the vapourizer-condenser 9 forming a condenser at the top of the column 10 and a vapourizer at the base of the column 11.
  • the column 11 also receives, as will be explained later, the fraction of the air to be separated, not introduced into the high pressure column, and which is liquefied in the coil 7. This fraction having about 30% of the total of the air, enters the column 11 in a gaseous state by the tube 17.
  • This last fraction is introduced into the auxiliary column 21 near the base.
  • the column 21 functions at the same pressure as the column 11.
  • the column 21 is heated at the bottom on the one hand by a gaseous fraction having its origin in the column 11 (stream and on the other hand optionally by a coil 22 into which there passes the air liquefied previously in the coil 7 and having been preferably subjected to sub-cooling of several degrees in the exchanger 26 cooled by oxygen drawn from the column -11. After its passage into the coil 22, this air is expanded by the valve 23 to the pressure of the column 11.
  • the oxygen drawn in gaseous state from the column 11 is preferably used to cool, in the exchanger 26, the air under pressure of approximately 15 atmospheres which has been liquefied in the coil 7, and then is caused to leave by the conduit 32 after having been reheated in the exchanger 3 and 2 in counter-current with the 'entering air.
  • the exchanger 26 may be omitted and the oxygen (stream 19) carried directly from the column 11 to the exchanger 3.
  • the gaseous nitrogen leaving the top of the column 11 cools successively, in the exchanger 13 and 15, the liquid nitrogen and the liquid rich in oxygen, all having their origin in the col-umn 10, then leaves by the tube 31 after being reheated, as is the oxygen, in the exchangers 3 and 2.
  • the argon leaving the top of the column 21 by the tube 27 is equally reheated in the same exchangers and leaves by the tube 33.
  • oxygen usually contains hydrocarbon impurities
  • One set of filters 41, 42 is shown between the coil 7 and the heat exchanger 26.
  • Another set of filters 43, 44 is shown in the pipe line 8. Two filters are shown in each case so that one can be operated while the other is regenerated. These filters are preferably of the type in which the impurities are adsorbed on a solid adsorbent.
  • the comparison of the apparatus described above, with known apparatuses makes the following points clear.
  • the yield in argon separated is better.
  • the argon fraction is substantially pure.
  • the oxygen obtained is substantially pure.
  • the portion of the air to be separated which enters the high pressure column enters into it several trays above the bottom, this bottom being heated in indirect contact by condensation in the coil 7 of the other portion of the air.
  • the liquid leaving the column 10 by the tube 8 can thus have an amount of oxygen greater than its usual amount, for example, about 50%. Containing more oxygen, this liquid contains less nitrogen. The latter leaves then at the top of the high pressure column in greater quantity. As a result of this it is possible, even though only a part of the air is separated in the high pressure column, for substantially the same quantity of liquid nitrogen to leave the column as in the usual process where all the air enters the high pressure column.
  • the higher part of the low pressure column receiving then the same quantity of washing liquid at the same purity functions according to normal conditions and furnishes gaseous nitrogen of the usual purity.
  • the lower part of the low pressure column being heated by condensation of the same quantity of nitrogen, the yield at the base of this column is equally satisfactory.
  • the oxygen obtained will be all the more pure since almost the total amount of argon leaves the column 11 by the tube 20, the oxygen being entrained with the argon returning to the column 11 by the tube 25.
  • a process for the separation by liquefaction and rectification, of a gaseous mixture having three principal constituents utilizing a main column made up of two rectification zones in mutual heat exchange relationship and under different pressures, and an auxiliary column receiving a fraction having its origin in the lower pressure rectification zone and in which a part of the mixture to be separated previously compressed to a pressure higher than that of the higher pressure rectification zone is expanded to the higher pressure and introduced into the higher pressure zone, comprising liquefying another part of the compressed gaseous mixture by indirect heat exchange with a liquid from the higher pressure rectification zone, then utilizing said other part for cooling by indirect contact With the auxiliary column and introducing said other part into the lower pressure zone.

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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)
US465712A 1954-06-29 1954-10-29 Low temperature separation of gaseous mixtures Expired - Lifetime US2779174A (en)

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FR1108033T 1954-06-29

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BE (1) BE539332A (fr)
FR (1) FR1108033A (fr)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2850881A (en) * 1957-01-11 1958-09-09 Coyne Chemical Company Method and apparatus for purifying nitrous oxide
US2918802A (en) * 1956-09-27 1959-12-29 Air Liquide Process of separation of air into its elements
US3079759A (en) * 1961-03-22 1963-03-05 Air Prod & Chem Separation of gaseous mixtures
US3340697A (en) * 1964-05-06 1967-09-12 Hydrocarbon Research Inc Heat exchange of crude oxygen and expanded high pressure nitrogen
US3360944A (en) * 1966-04-05 1968-01-02 American Messer Corp Gas liquefaction with work expansion of major feed portion
US3535887A (en) * 1967-12-01 1970-10-27 Mc Donnell Douglas Corp High purity oxygen production from air by plural stage separation of plural streams of compressed air with utilization of recompressed overhead as a source of heat exchange
US3648471A (en) * 1969-02-14 1972-03-14 Genrikh Maxovich Basin Method of liberation of nitrogen and oxygen from air
US4137056A (en) * 1974-04-26 1979-01-30 Golovko Georgy A Process for low-temperature separation of air
US4410343A (en) * 1981-12-24 1983-10-18 Union Carbide Corporation Air boiling process to produce low purity oxygen
US4854954A (en) * 1988-05-17 1989-08-08 Erickson Donald C Rectifier liquid generated intermediate reflux for subambient cascades

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2209748A (en) * 1938-08-03 1940-07-30 Air Reduction Method of separating the constituents of gaseous mixtures
US2409458A (en) * 1943-04-27 1946-10-15 Air Reduction Separation of the constituents of gaseous mixtures
US2433536A (en) * 1945-07-06 1947-12-30 Air Reduction Method of separating the components of air
US2547177A (en) * 1948-11-02 1951-04-03 Linde Air Prod Co Process of and apparatus for separating ternary gas mixtures
US2626510A (en) * 1947-06-18 1953-01-27 Air Prod Inc Air fractionating cycle and apparatus

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2209748A (en) * 1938-08-03 1940-07-30 Air Reduction Method of separating the constituents of gaseous mixtures
US2409458A (en) * 1943-04-27 1946-10-15 Air Reduction Separation of the constituents of gaseous mixtures
US2433536A (en) * 1945-07-06 1947-12-30 Air Reduction Method of separating the components of air
US2626510A (en) * 1947-06-18 1953-01-27 Air Prod Inc Air fractionating cycle and apparatus
US2547177A (en) * 1948-11-02 1951-04-03 Linde Air Prod Co Process of and apparatus for separating ternary gas mixtures

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2918802A (en) * 1956-09-27 1959-12-29 Air Liquide Process of separation of air into its elements
US2850881A (en) * 1957-01-11 1958-09-09 Coyne Chemical Company Method and apparatus for purifying nitrous oxide
US3079759A (en) * 1961-03-22 1963-03-05 Air Prod & Chem Separation of gaseous mixtures
US3340697A (en) * 1964-05-06 1967-09-12 Hydrocarbon Research Inc Heat exchange of crude oxygen and expanded high pressure nitrogen
US3360944A (en) * 1966-04-05 1968-01-02 American Messer Corp Gas liquefaction with work expansion of major feed portion
US3535887A (en) * 1967-12-01 1970-10-27 Mc Donnell Douglas Corp High purity oxygen production from air by plural stage separation of plural streams of compressed air with utilization of recompressed overhead as a source of heat exchange
US3648471A (en) * 1969-02-14 1972-03-14 Genrikh Maxovich Basin Method of liberation of nitrogen and oxygen from air
US4137056A (en) * 1974-04-26 1979-01-30 Golovko Georgy A Process for low-temperature separation of air
US4410343A (en) * 1981-12-24 1983-10-18 Union Carbide Corporation Air boiling process to produce low purity oxygen
US4854954A (en) * 1988-05-17 1989-08-08 Erickson Donald C Rectifier liquid generated intermediate reflux for subambient cascades

Also Published As

Publication number Publication date
FR1108033A (fr) 1956-01-09
BE539332A (fr) 1900-01-01

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