US1968518A - Method and apparatus for liquefying and separating gaseous mixtures - Google Patents

Method and apparatus for liquefying and separating gaseous mixtures Download PDF

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Publication number
US1968518A
US1968518A US632479A US63247932A US1968518A US 1968518 A US1968518 A US 1968518A US 632479 A US632479 A US 632479A US 63247932 A US63247932 A US 63247932A US 1968518 A US1968518 A US 1968518A
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United States
Prior art keywords
cooling
conduit
column
mixture
chamber
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US632479A
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English (en)
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William W Fraser
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Linde Air Products Co
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Linde Air Products Co
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Priority to US632479A priority Critical patent/US1968518A/en
Priority to GB11971/33A priority patent/GB418673A/en
Priority to FR762175D priority patent/FR762175A/fr
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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
    • 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
    • Y10S62/902—Apparatus
    • Y10S62/909—Regeneration
    • 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
    • Y10S62/902—Apparatus
    • Y10S62/91—Expander

Definitions

  • This invention relates to a method and apparatus for liquei'ying and separating gaseous mixtures into their constituents. More particularly, it relates to a method and apparatus for liquel-i'ying air and separating-it into constituents in a manner which yields oxygen of relatively high degrees of purity.
  • the invention has for its object generally to provide an improved method for liquefying gases l and separating the same into constituents together with suitable apparatus for carrying out the same, whereby separated gas products of relatively high degrees of purity are obtainedwith a relatively small expenditure of energy. 18 More specifically, it is an object to provide an improved heat cycle for the operation of gas liquei'ying and rectifying apparatus, which permits starting of the apparatus and obtaining the desired gas products in substantial quantities in to relatively short periods of time, in a manner having relatively high overall thermal efliciencies.
  • the invention accordingly comprises the several steps and the relation of one or more of such steps with respect to each of the others, and the apparatus embodying features of construction, combinations of elements and arrangement of parts which are adapted to effect such steps, all as exemplified in the following detailed disclosure, and the scope of the application of which will be indicated in the claims.
  • Fig. l is a diagrammatic view of apparatus, mainly illustrated in section, which exemplifies suitable apparatus and means for carrying out a process in accordance with the invention
  • FIG. 2 and Fig. 3 are similar views showing modified forms of apparatus adapted for the practice of the invention, but in which the principle thereof is carried out with greater degrees of refinement than in the apparatus of Fig. 1.
  • the method and apparatus herein provided incorporate the principles of liquefaction of gases ll devised by Linde and employ the expansion of a gaseous mixture through an expansion valve into a suitable separating chamber, for example the receiving chamber of a rectifying column whereby there is obtained liquefaction of the gaseous mixture together with simultaneous separation of the same into constituents. It is also proposed to utilize the refrigerating effect produced by expanding the gaseous mixture in such a manner as to cause the same to do external work. This is commonly achieved by means of an expansion engine. In the method and apparatus of the present invention these two principles of refrigeration and liquefaction are advantageously combined, portions of the gaseous mixture to be treated being cooled simultaneously by the two expansion principles, after which they are introduced together into the rectifying column.
  • the heat exchangers which have heated portions of the gas mixture to be treated passing in countercurrent fashion in heat exchanging relation with the waste products.
  • the heat exchangers commonly employed comprise a chamber generally provided with baffles through which are passed tubes carrying the cooling medium, the product to be cooled passing about the bafiles and over the tubes in countercurrents; the relation in the exchangers, however, of the hot and cold mediums may be reversed.
  • uniformity is insured by effecting heat exchange in a plurality of stages which not only achieves uniform distribution of the temperature gradient, but also insures a uniform distribution of the pressure drop, whereby uniform activity at all points in the passage of the heat exchanging mediums is attained and the cooling effect of the cooling medium substantially completely utilized. It is hence important that where the cooling medium is initially under pressure, that thesame shall be properly expanded during its passage in order to utilize the cooling effect made possible by the remnant energy of the waste products initially under pressure. It is here .contemplated, though not necessary, that all waste products from the liquefying and rectifying apparatus shall be utilized in this manner.
  • 10 denotes a compressor which compresses the gaseous mixture to be treated to a relatively high pressure.
  • this initial pressure may be, for example, one hundred atmospheres; the air to be compressed is preferably initially purified and dehumidified by suitable means not here shown in the interests of clearness in the drawings, but are well known in the art.
  • the compressed gas is passed from the compressor 10 to a suitable cooling means 11, for example a coil or radiator exposed for cooling by the atmosphere. After traversing this coil, the mixture is passed to the inner conduit or coil 12 of a heat exchanger 13.
  • Conduit 14- here provides the exit from coil 12, and leads to a branch point 15, where the now cooled compressed medium is separated into two portions; one portion being led by way of the conduit 16 to an inner conduit or coil 17 of heat exchanger 18; the other portion being led by way of conduit 19 to an expansion engine 20.
  • the cooled portion of the compressed medium which leaves the heat exchanger 18 passes by way of the exit conduit 21 to a receiving chamber 22 of the high pressure column of a multi-column rectifying apparatus.
  • the conduit 21 is here indicated as including additional cooling means, in the form of a coil 23 disposed in the base of the column, by which the compressed medium is brought to the temperature not greatly different from that of liquefaction prior to its introduction and expansion into the receiving chamber 22.
  • the discharge from the coil 23 is through an expansion valve 24 and a distributing nozzle 25 disposed within the chamber.
  • the portion of the compressed medium which has been caused to expand in the expansion engine 20, when properly cooled, is also introduced into the receiving chamber 22 by means of a suitable distributing nozzle here shown at 26.
  • a suitable distributing nozzle here shown at 26.
  • the gas portions discharging into the chamber 22 from the nozzles 25 and 26 become converted into liquid and vapor, the liquid gravitating to the lower portion of the column where a pool of condensate collects and may submerge the coil 23.
  • This column is also shown as provided with suitable dephlegmating means, for example perforated partitions 27.
  • the column terminates in a condenser 28 which insures the backward return of condensate by the recondensation of vapors arising in the column.
  • the liquid withdrawn from the high pressure column is passed to the receiving chamber 30 of the low pressure column superposed above the high pressure column.
  • This is here achieved by providing a conduit 31 leading from the bottom of chamber 22 to a distributing nozzle 32 in the chamber 30.
  • the exit of fluid from the nozzle 32 is controlled by means of an expansion valve 33.
  • liquid condensate of the less volatile constituent collects in the chamber 22, for example as shown on the top dephlegmating tray of the group at 2'1, this may be likewise passed into the low pressure column by means of a conduit 34' having a distributing nozzle 35 in the chamber 30., and provided with a controlling valve 36.
  • This latter rectifying column subjects the gaseous mixture liquefied therein to further distillation and counter-current washing, whereby a gas product of still greater purity than had in the first column separates out.
  • the purified liquid product may be withdrawn from the lower end of chamber 30.
  • a liquid containing a very high percentage of oxygen collects about the condenser 28, which latter supplies the heat for distilling off a gas fraction, representing mainly nitrogen, from the low pressure column.
  • Substantially pure gaseous oxygen collects in the lower partof chamber 30 above the liquid and may be withdrawn from a point in suitable proximity to the pool of liquid that collects therein.
  • the cold uncondensed vapors are withdrawn from the top of the chamber 30 by way of the discharge conduit 40.
  • This conduit is arranged to supply the cooling medium to the exchanger 18, the entrance of the cooling medium being arranged to pass in countercurrent fashion over the coil 17 in the exchanger 18.
  • the cooled products which have now been partially warmed are passed by means of a conduit 41 into the exchanger 13, where they are passed in similar countercurrent fashion over the coil 12.
  • the passage of the cooling medium is preferably arranged to take place accompanied by expansion. This is accomplished by providing 'increasing volume accompanying the passage of the medium, and is here indicated by the tapershown on the exchangers 13 and 18.
  • the passage of the cooling medium is thus arranged to enter progressively a larger and larger space until the medium discharges at a pressure relatively close to atmospheric through a discharge passage 42.
  • the vapors and liquid introduced into the pressure chamber are subject to fractional distillation and countercurrent washing, whereby the more volatile constituents rise and are removed as vapors from the top of the chamber while the less volatile constituent is carried down and collects as a liquid in the bottom of the chamber. While the liquid which collects in the bottom of chamber 22 will have the amount of the less volatile constituent continually increased by the practice of fractional distillation, it is seen that withdrawals. from this chamber determine a certain maximum content thereof, the rate of withdrawal being here regulated by the valve 33, which also serves as an expansion valve for the introduction of fluid into the chamber 30 of the low pressure column.
  • the liquid thus passed from the high pressure column to the low pressure column is subject to further fractional distillation and countercurrent washing until a gas product of the-desired purity is attained.
  • the rate of distillation in the low pressure column is dependent upon the temperature difference between the liquid in chamber 30 and the condenser 28, which difference is determined by the respective pressure conditions, in the chamber 22 and 30.
  • the conditions in the former may be controlled in part by the rate at which the more volatile constituent is withdrawn from the interior of condenser 28, since this constituent comprises the fraction from which heat is extracted with greatest difiiculty. Means are accordingly provided to control such withdrawal.
  • this means comprises a conduit 43 leading from the condenser dome and arranged to discharge into the exchanger 18 at a point which is substantially at the temperature of this last withdrawn product and passes in countercurrent fashion about the coil 17.
  • the passage of this cold medium is thus parallel with that introduced by the conduit 43.
  • the refrigerating effect of this last withdrawn waste product is thus also utilized in the practice of the method of the present invention.
  • the compression is accomplished in a plurality of stages which are correlated with the stages of cooling arranged to utilize to the fullest practical extent the refrigerating effect of the waste products from the rectifying apparatus here employed.
  • a compressor is shown as accom-' plishing the first stage of compression, from which it discharges into an inner conduit or coil 51 of an exchanger 52 and then discharges into a conduit 53 leading to a second stage compressor 54, from which it passes into an inner conduit or coil 55 of an exchanger 56. From this second exchanger, a conduit 5'!
  • the conduit 69 leads by way of an expansion valve 70 to a distributing nozzle '71 in the chamber 66.
  • This chamber has a condenser '12 at its upper end and is arranged to collect condensate at its lower end.
  • the liquid collected is arranged to be withdrawn by means of a conduit 73.1eading from the bottom of chamber 66 and passing .into receiving chamber 74 of a low pressure column superposed above the high pressure column in the rectifying apparatus.
  • a conduit '75 is arranged to withdraw the waste products from the upper end of the rectifying apparatus, these products having first passed through the exchanger 68, are then introduced into the exchanger 63, where they pass in countercurrent fashion over the coil 62 and have exit by way of conduit 76. This latter conduit passes these products on to exchanger 56 where they pass in countercurrent fashion over the coil 55.
  • a conduit '77 is arranged to withdraw uncondensed products from the dome of the condenser '72. This conduit is arranged to join with a'conduit '78, which provides for the exit of the waste products from the heat exchanger 56. The commingled waste products from the conduits 77 and '78 are then passed preferably by means of an injector or other expansion device.
  • conduit 57 which leads to a branch point 58 where it is divided into parts, one 01' which is led by conduit 59 to expansion engine 60;
  • the first portion, expanded by the engine 60, is passed by conduit 64 to a distributing nozzle 65 into a receiving chamber 66 of the high pressure column of the rectifying apparatus, the same as shown in Fig. 2.
  • the other portion emerging from coil 62 is treated differently in this form of device from that shown in Fig. 2.
  • the exit conduit 81 of the coil 62 leads to another branch point 82, from which a conduit 83 leads a portion to a second expansion engine 84, while a conduit 85 leads the other portion to a pro-cooling means 86; thislatter may be in the form of a heat exchanger that supplies cooled medium by way of conduit 87 to expansion valve 88 and distributing nozzle 89 in the chamber 66.
  • the portion from the expansion engine 84 is preferably introduced in the chamber 66 by means of a distributing nozzle 90. It is contemplated, however, that such further expanded medium may be introduced at other points of the rectifying column, since this portion is mainly used to accelerate the initial obtaining of liquid in the rectifying apparatus.
  • the waste products are withdrawn from the rectifying apparatus through conduits and 77, as shown in Fig. 2 and a final cooling effect produced by expansion in the conduit 80, which supplies a cooling medium for the initial heat exchanger.
  • the rectifying apparatus here employed is shown in the form of a two-column apparatus which is a thoroughly practical form of device for the liquefaction and separation of air into constituents, and from which an oxygen product may be obtained from the low pressure column, which is of 98% or higher purity, it is evident that, by the use of three or more columns, substantially any desired degree of purity may be attained in the product desired. It will also be seen that by the use of such multi-column apparatus, the initial pressure at which the waste products having the refrigerating effect supplied to the exchangers is reduced. By the step of cooling ina plurality of stages, as here proposed, it is seen, moreover, that the low pressure waste products may be utilized to the fullest practical extent and thereby obtain the benefit of substantially their full refrigerating effect.
  • a multi-column rectifying apparatus having different pressures in the columns arranged for the distilling off of gas fractions, of a multi-stage compressing means arranged to compress the whole of the gas mixture to be separated in successive stages to a relatively high degree of compression, a plurality of interchangers arranged to receive and cool the compressed gas mixture as it passes from stage to stage whereby a succession of cooling stages is provided, conduit means for receiving said highly compressed gas mixture and dividing the same into two parts, an expansion engine for receiving and expanding one of said parts and passing the same to a high pressure column of said rectifying apparatus, an additional interchanger for receiving and cooling said second part of the highly compressed gas mixture, valved expansion means for discharging said second part into a column of said rectifying apparatus, conduit means for withdrawing a cold waste product from another column of said rectifying apparatus and passing the same through said interchangers, and means for further cooling said waste product by causing the same to expand progressively and do internal, work and utilizing said cooling effect in
  • the method of separating gaseous mixtures into constituents by liquefaction and rectification which comprises compressing the mixture to a relatively high pressure, cooling the compressed mixture to successively lower temperatures in a plurality of stages, dividing said mixture at a point intermediate said cooling stages into a plurality of portions, expanding, collecting and liquefying said portions, conjointly rectifying said liquefied portions successively in stages at high and low pressures, separating and withdrawing relatively uncondensable fractions from each of said high and low pressure rectifying stages, immediately thereafter effecting throttling expansion of the fraction separated from said high pressure stage to enhance the cooling effect, passing the fraction separated from the low pressure rectifying stage in heat exchanging relation with the compressed mixture in one of said cooling stages, admixing the throttled fraction with said low pressure fraction, and passing the resulting mixture in heat exchanging relation with the compressed mixture in another of said stages.
  • the method of separating gaseous mixtures into constituents by liquefaction and rectification which comprises compressing the mixture successively in stages to a relatively high pressure, initially cooling the compressed mixture in stages located between desired compression stages, dividing said mixture at the terminus of said initial cooling stages into a plurality of portions, finally cooling one of said portions in at least one additional cooling stage and then expanding the same by throttling expansion, engine expanding the remaining portion, collecting and liquefying said portions, conjointly rectifying said liquefied portions successively in stages at high and low pressures, separating and withdrawing relatively uncondensable fractions from each of said high and low pressure rectifying stages, immediately thereafter eilecting throttling expansion of the fraction separated from said high pressure stage to enhance the cooling effect, passing the fraction separated from the low pressure rectifying stage with progressive expansion in countercurrent heat exchanging relation with the compressed mixture in said initial and final cooling stages, and ap plying directly the cooling eifect of said throttled fraction to a predetermined initial cooling stage by admixing the same with said
  • the method of separating gaseous mixtures into constituents by liquefaction and rectification which comprises compressing the input gaseous mixture to a relatively high pressure, cooling such compressed mixture to successively lower temperatures in a plurality of stages, expanding, collecting and liquefying said cooled mixture, rectitying said liquefied mixture successively in stages at high and low pressures, separating and withdrawing relatively uncondensable fractions from each of said rectifying stages, immediately thereafter reducing the temperature and pressure of the fraction separated from the high pressure stage by throttling expansion, applying the low pressure fraction to accomplish at least a part of the cooling of the input compressed mixture, admixing said expanded fraction with said low pressure fraction at a point later in the outgoing direction than where said low pressure fraction is admitted to said cooling operation and where its temperature on expansion corresponds substantially with that of said low pressure fraction, and immediately using the resultant mixture in heat exchanging relation to accomplish a further part oi. said cooling of the input compressed mixture.

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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)
US632479A 1932-09-10 1932-09-10 Method and apparatus for liquefying and separating gaseous mixtures Expired - Lifetime US1968518A (en)

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US632479A US1968518A (en) 1932-09-10 1932-09-10 Method and apparatus for liquefying and separating gaseous mixtures
GB11971/33A GB418673A (en) 1932-09-10 1933-04-24 Improvements in or relating to methods of separating gas mixtures into constituents
FR762175D FR762175A (fr) 1932-09-10 1933-09-08 Procédé et dispositif pour la liquéfaction de mélanges gazeux et la séparation de leurs constituants

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2448491A (en) * 1944-11-06 1948-08-31 Little Inc A Air separating system and process
US2525660A (en) * 1944-09-04 1950-10-10 Arthur J Fausek Apparatus for separating the constituents of atmosphere
US2527301A (en) * 1943-08-04 1950-10-24 Arthur J Fausek Method of separating the constituents of gaseous mixtures
US2568223A (en) * 1944-10-20 1951-09-18 Baufre William Lane De Process and apparatus for extracting oxygen from atmospheric air
US2729953A (en) * 1946-10-09 1956-01-10 Air Prod Inc Air fractionating cycle and apparatus
US2804292A (en) * 1949-02-02 1957-08-27 Air Prod Inc Gas-liquid contact apparatus
US2991633A (en) * 1958-03-17 1961-07-11 Itt Joule-thomson effect cooling system
US2997854A (en) * 1957-08-16 1961-08-29 Air Prod Inc Method and apparatus for separating gaseous mixtures
US3091094A (en) * 1957-07-04 1963-05-28 Linde Eismasch Ag Process of and apparatus for separating gases with cold production by workproducing expansion of low-boiling product
US3091941A (en) * 1957-07-04 1963-06-04 Linde Eismasch Ag Process and apparatus for refrigeration by work-producing expansion
US3258930A (en) * 1961-02-23 1966-07-05 Linde Eismasch Ag Process and apparatus for separating gaseous mixtures by low-temperature rectification
US3631683A (en) * 1968-01-26 1972-01-04 Messer Griesheim Gmbh Rectification by precooling and dividing the feed gas into partial streams
US3656311A (en) * 1967-11-15 1972-04-18 Messer Griesheim Gmbh Rectification by dividing the feed gas into partial streams
US20140178270A1 (en) * 2010-07-29 2014-06-26 Precision Combustion, Inc. Sabatier process and apparatus for controlling exothermic reaction

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE884203C (de) * 1943-07-29 1953-07-23 Linde S Eismaschinen Akt Ges G Anordnung zur Gaszerlegung
US7810588B2 (en) 2007-02-23 2010-10-12 Baker Hughes Incorporated Multi-layer encapsulation of diamond grit for use in earth-boring bits
WO2011088353A1 (fr) * 2010-01-15 2011-07-21 Jaffrey Syed Kamal H Séparateur de gaz polyatomique

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2527301A (en) * 1943-08-04 1950-10-24 Arthur J Fausek Method of separating the constituents of gaseous mixtures
US2525660A (en) * 1944-09-04 1950-10-10 Arthur J Fausek Apparatus for separating the constituents of atmosphere
US2568223A (en) * 1944-10-20 1951-09-18 Baufre William Lane De Process and apparatus for extracting oxygen from atmospheric air
US2448491A (en) * 1944-11-06 1948-08-31 Little Inc A Air separating system and process
US2729953A (en) * 1946-10-09 1956-01-10 Air Prod Inc Air fractionating cycle and apparatus
US2804292A (en) * 1949-02-02 1957-08-27 Air Prod Inc Gas-liquid contact apparatus
US3091941A (en) * 1957-07-04 1963-06-04 Linde Eismasch Ag Process and apparatus for refrigeration by work-producing expansion
US3091094A (en) * 1957-07-04 1963-05-28 Linde Eismasch Ag Process of and apparatus for separating gases with cold production by workproducing expansion of low-boiling product
US2997854A (en) * 1957-08-16 1961-08-29 Air Prod Inc Method and apparatus for separating gaseous mixtures
US2991633A (en) * 1958-03-17 1961-07-11 Itt Joule-thomson effect cooling system
US3258930A (en) * 1961-02-23 1966-07-05 Linde Eismasch Ag Process and apparatus for separating gaseous mixtures by low-temperature rectification
US3656311A (en) * 1967-11-15 1972-04-18 Messer Griesheim Gmbh Rectification by dividing the feed gas into partial streams
US3631683A (en) * 1968-01-26 1972-01-04 Messer Griesheim Gmbh Rectification by precooling and dividing the feed gas into partial streams
US20140178270A1 (en) * 2010-07-29 2014-06-26 Precision Combustion, Inc. Sabatier process and apparatus for controlling exothermic reaction
US9446365B2 (en) * 2010-07-29 2016-09-20 Precision Combustion, Inc. Sabatier process and apparatus for controlling exothermic reaction

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GB418673A (en) 1934-10-24
FR762175A (fr) 1934-04-05

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