US2096694A - Process and apparatus for obtaining noble gases - Google Patents

Process and apparatus for obtaining noble gases Download PDF

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Publication number
US2096694A
US2096694A US26302A US2630235A US2096694A US 2096694 A US2096694 A US 2096694A US 26302 A US26302 A US 26302A US 2630235 A US2630235 A US 2630235A US 2096694 A US2096694 A US 2096694A
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liquid
still
column
vapor
oxygen
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US26302A
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English (en)
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Erb Karl
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IG Farbenindustrie AG
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IG Farbenindustrie AG
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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
    • F25J3/04745—Krypton and/or Xenon
    • 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

Definitions

  • the present invention relates to a process and apparatus for obtaining, particularly from air, the noble or inert gases having boiling points higher than that of oxygen.
  • Rectification is often applied in the separation of the inert gases having boiling points higher than that of oxygen, particularly of krypton, from air or other suitable starting mixtures containing oxygen.
  • liquid oxygen obtained for example by rectification of liquid air, or other liquefied starting mixture while said liquid flows as a continuous stream through a suitable evaporating device.
  • undesirable by efiects such as the crystallization of hydrocarbons, particularly of acetylene, may be avoided if the evaporation of the liquefied starting material is effected while the said liquid fiows as a continuous stream through a suitable evaporating device.
  • liquid oxygen obtained, for example, by the rectification o1 liquid air is evaporated in one or several elongated stills.
  • the stills, or evaporating devices used differ from the usual rectification column in that they have a very small cross-sectional area and are of a great length.
  • the still may be of any desired form, for example in the form of a coil or of several coils running in parallel or of a nest of tubes.
  • the vapor produced by this simple evaporation process necessarily contains a relatively large quantity of the inert gases.
  • theconcentration of inert gases and of hydrocarbons in the residual liquid may be considerably increased without endangering the work.
  • the residual liquid oxygen discharged from the still is of a relatively small volume as compared to the volume of the starting material and contains a high concentration of the inert gases as well as of hydrocarbons. This produces a substantial increase in the working safety.
  • the ratio of hydrocarbons to inert gases in the residual liquid increases whereas the ratio of hydrocarbons to inert gases in the vapor produced decreases.
  • the quantity of residual liquid discharged from the still must therefore be adjusted in such a manner that the quantity of hydrocarbons returned to the column will be maintained sufficiently small as to'be unobjectionable. If the quantity of residual liquid discharged is small, or in any case if it is desirable,-all, or part the desired purity.
  • the liquid being evaporated and the vapor produced may be made to circulate in the elongated still in counter-current, in continuous current or partially in counter-current and partially in continuouscurrent. Circulation of the liquid and vapor as a continuous current is desirable since high velocity of fiow in a still of small cross sectional area is possible. If the circulation is counter-current it is advantageous to gradually decrease the cross-sectional area of the still to correspond with the gradually decreasing total quantity of liquid and vapor flowing.
  • a liquid separator is mounted at the discharge end of the still in order to separate the liquid residue from the vapor produced.
  • FIGs. 1 and 2 diagrammatically illustrate two forms of the apparatus.
  • the apparatus comprises a rectification column I into which a stream of liquid air may be introduced through pipe 2 and vaporous air may be introduced through pipe 3. Both quantities of air, or at least one of them con- .tain the inert gases having higher boiling points than oxygen that are to be obtained.
  • the liquid passes down through the column I and then passes into the still 4 as a continuous stream.
  • the still 4 is, in comparison to the rectification column I, of very small cross-sectional area. In view of the fact that the flow of liquid and vapor produced in still 4 is counter-current, the crosssectional area of the still is progressively decreased to correspond roughly with the total quantity of liquid and vapor flowing through the still.
  • the still 4 is heated by means of tube 5 through which compressed air is passed.
  • This air is liquefied by the evaporation of the liquid in the still and is conducted through valve 6 and pipe 2 into the rectification column.
  • A. separator I is provided at the discharge end of still 4 to receive the discharge from the still and separate the vapor from the residual liquid. The separated vapor may be conducted back to the column by means of pipe 9 and valve 10.
  • the liquid residue obtained and which contains the inert gases of high boiling points as well as hydrocarbons and other impurities of high boiling points is withdrawn from separator 1 by means of the valve 8.
  • Still I4 differs from still 4 in that it provides two distillation stages, in the first of which the liquid and the vapor flow counter-current to each other and in the second stage of which the liquid and vapor flow in continuous current into separator 11. In the first stage the vapor produced flows directly back into the column whereas in the second stage the vapor is conducted into separator l1 wherein the vapor is separated from the residual liquid. The vapor is thereafter conducted back to the column I by means of pipe 18 and valve 13. The residual liquid is withdrawn from separator l1 by means of valve I9.
  • Compressed air for heating the liquid is supplied to tube l6 of still 14 through valve 15. As in still 4, this compressed air is liquefied by the evaporation of the liquidin the still and this liquefied air is then conducted through valve 6 and pipe 2 into the rectification column I.
  • Valves H and 12 are provided at the inlets of stills 4 and I4 respectively in order to control the flow of liquid to the stills. By operating stills 4 and I4 alternately the still out of operation may be cleaned of any separations before they become objectionable. Gas may be withdrawn from the separators 1 or l1 by means of valves 23 or 24 respectively.
  • the apparatus shownin Fig. 2 comprises a rectification column 25 into which the starting liquid is introduced through pipe 26.
  • the starting liquid may, for example be liquid oxygen containing krypton which is obtained from a two stage air-separating apparatus, not shown.
  • a still 21, of conventional construction may be arranged at the bottom of column 25 for forming a relatively small part of the vapor passed through column 25.
  • the still 21 is heated by means of compressed nitrogen supplied through pipe 3
  • the greater part of the evaporation of the liquid oxygen takes place in the still 28 which is shown in the form of an elongated coil.
  • a chamber33 surrounds still 28 and the compressed nitrogen is conducted from the coil 32 into the chamber 33.
  • the compressed nitrogen is liquefied by the evaporation of liquid oxygen in stills 21 and 28 and this liquefied nitrogen may be returned to said two-stage air-separating system by means ofvalve 34 and pipe 35.
  • the evaporating liquid and the vapor produced flow downwardly in still 28 in a continuous current.
  • Liquid is maintained in still 21 at a sufficient level to force evaporating liquid and vapor through still 28 into separator 30 and to reconduct separated vapor through valve 31 and pipe 29 into the column 25.
  • the residual liquid is withdrawn from separator 30 by means of valve 46.
  • a second rectification column 36 for further treatment. This may be done by closing or partially closing valve 31 and opening valve 38.
  • the rectification column 36 is provided with a still at its bottom. This still may be heated by means of compressed air which is supplied to the heating coil 39. This compressed air is liquefied by the evaporation of liquid in the still. This liquefied air may be supplied to the air-separating device described or it may be introduced as washing liquid in column 36 by means of pipe 40, as shown in the drawing.
  • Column 36 is provided with a condenser 4
  • Liquid nitrogen is withdrawn from the discharge pipe of chamber 33 through valve 42 and is conducted to the condenser 4
  • the process of obtaining noble gases having higher boiling points than oxygen which comprises supplying gaseous and liquefied mixtures containing oxygen and the said noble gases to a rectification column, passing the liquid obtained at the bottom of said column through an evaporating device as a continuous stream, vaporizing said liquid in said evaporating device, continuously passing the liquid and the produced vapors to a separator, separating vapor from the residual liquid,v returning the separated vapor to the rectification column and removing this liquid from the separator.
  • the process of obtaining noble gases having higher boiling points than oxygen which comprises supplying gaseous and liquefied mixtures containing oxygen and the said noble gases to a rectification column, passing the liquid obtained at the bottom of said column from said column through an evaporating device as a continuous stream, vaporizing said stream of liquid in said Liquid oxygen containing a large evaporating device, passing the oxygen. vapor counter-current to the stream of liquid to said column, Continuously passing the stream of liquid and accompanying vapors from saidevapo rating device to a separator, separating vapor from the residual liquid,- returning the separated vapor to the rectification column and removing this liquid from the separator.
  • the process of obtaining noble gases having higher boiling points than oxygen which comprises supplying gaseous and liquefied mixtures containing oxygen and the said noble gases to a rectification column,passing the liquid obtained at the bottom of said column from said column through an evaporating device as a continuous stream, vaporizing said liquid in said evaporating device, passing the oxygen vapor produced in the first stage of the evaporation counter-current to the stream of liquid to said column, passing the vapor produced in the next stage of the evaporation with the residual liquid as a continuous current to a separator, separating vapor from the residual liquid, returning the separated vapor to the column and removing this liquid from the.
  • An apparatus for obtaining noble gases from oxygen-containing gas mixtures which comprises a rectification column, an evaporating device of relatively small cross-sectional area and of a relatively great length connected at one end with the bottom of said rectification column, means for supplying a continuous stream of liquefied oxygen-containing gases to said evaporating device, means for heating said stream of liquid,

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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)
US26302A 1934-06-16 1935-06-12 Process and apparatus for obtaining noble gases Expired - Lifetime US2096694A (en)

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DE458371X 1934-06-16

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US (1) US2096694A (xx)
FR (1) FR791360A (xx)
GB (1) GB458371A (xx)
NL (1) NL43934C (xx)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3768270A (en) * 1970-11-27 1973-10-30 British Oxygen Co Ltd Air separation
US3779028A (en) * 1970-10-12 1973-12-18 British Oxygen Co Ltd Improved krypton xenon recovery method
US20060185389A1 (en) * 2005-02-18 2006-08-24 Weber Joseph A Cryogenic rectification system for neon production

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3779028A (en) * 1970-10-12 1973-12-18 British Oxygen Co Ltd Improved krypton xenon recovery method
US3768270A (en) * 1970-11-27 1973-10-30 British Oxygen Co Ltd Air separation
US20060185389A1 (en) * 2005-02-18 2006-08-24 Weber Joseph A Cryogenic rectification system for neon production
WO2006091363A3 (en) * 2005-02-18 2007-11-22 Praxair Technology Inc Cryogenic rectification system for neon production
US7299656B2 (en) * 2005-02-18 2007-11-27 Praxair Technology, Inc. Cryogenic rectification system for neon production

Also Published As

Publication number Publication date
FR791360A (fr) 1935-12-10
NL43934C (xx)
GB458371A (en) 1936-12-17

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