US2270880A - Separation of krypton and xenon from air - Google Patents

Separation of krypton and xenon from air Download PDF

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Publication number
US2270880A
US2270880A US260943A US26094339A US2270880A US 2270880 A US2270880 A US 2270880A US 260943 A US260943 A US 260943A US 26094339 A US26094339 A US 26094339A US 2270880 A US2270880 A US 2270880A
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United States
Prior art keywords
liquid
air
krypton
column
separator
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Expired - Lifetime
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US260943A
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English (en)
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Kahle Heinrich
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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
    • 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
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/40—Air or oxygen enriched air, i.e. generally less than 30mol% of O2
    • 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
    • Y10S62/925—Xenon or krypton

Definitions

  • the principal object of the present invention is to provide a simple method of operation which makes it possible, despite the presence of hydrocarbons, to carry the concentration of krypton so far in a single stage that the enriched washing liquid after removal of the hydrocarbons can be processed directly to substantially pure krypton in a single additional stage.
  • Another object of the present invention is to provide an improved apparatus for carrying out such process.
  • the main volume of the air from which the krypton lis to be separated is compressed to a y relatively low pressure by suitable means not shown and supplied through conduit I0 to a pair of regenerators 2a and 2b wherein it is cooled to approximately its dew point .temperature in the customary manner by contact with cold surfaces in the regenerators.
  • the air leaves the (Cl. Bil-122) regenerators 2a or 2b through conduit II and is hereupon introduced into the lower portion of column 3.
  • the cold air to be liquefied is conducted by conduit i4 to a coil I5 in liqueiler I3 from which conduits I6 and I6' conduct the liqueiled air to the upper portion of column 3.
  • the liqueiler I3 is refrigerated by a suitable low temperature medium lconducted therethrough.
  • a throttling or control valve I'I is interposed in the conduit I6 for reducing the pressure of and regulating the proportion of reilux liquid supplied to the column 3.
  • 'I'he column 3 is provided with suitable gas and liquid contact means such as trays I8 so that the air introduced through conduit II is effectively washed by the reux liquid. Liquid containing the krypton washed out of the air collects at the bottom of column 3 and is conducted therefrom by a yconduit I9 to the mid-portion of a rectumbler column 4, the flow being regulated by valve 20.
  • Column I is also provided with trays or perforated plates 2
  • an additional portionof liquid air is introduced at the top of column 4.
  • Such liquid is supplied by a branch 24 of conduit I6, the amount being controlled by valve 25 therein.
  • the cold air from which the krypton has been washed is conducted from the tops of both columns 3 and 4 by conduit 26 to the cold ends of all the regenerators, alternately Ia or Ib and alternately 2a or 2b wherein it deposits refrigeration and is warmed.
  • the air freevoi krypton leaves the warm ends of the regenerators through a conduit 21.
  • the sump 22 is connected by a conduit 28 to the upper end of an evaporator or vaporizer coil 23 in a vaporizer 30, the flow being controlled by a valve 3
  • AThe lower end of coil 29 is connected by conduit 32 to a gas and liquid separator 33 from the upper end of 'which the released gas flows to the lower portion of column 4 through conduit 34.
  • the relatively'pure krypton concentrate is withdrawn from the lower part of separator 33 through a conduii 35.
  • this amount for example 80 cubic meters per hour, are withdrawn and evaporated in the evaporator 30 to a residue of 15 cubicmeters per hour which is withdrawn at 35, and the thereby resultant vapors which are poor in krypton and hydrocarbons are led back from the separator 33 into the column t.
  • evaporator 29 have no blind angles and opportunities for the deposition of solidremoved components such as, for example, acetylene.
  • solidremoved components such as, for example, acetylene.
  • Athe liquid is evaporated in a simple tube 29 with continuous co-current downflow and the separation of the vapors is effected in a subsequent separator 33 of simple construction
  • through which the liquid is transferred from column 4 into auxiliary evaporator 29, and likewise the valve in conduit 35 through which the liquid is withdrawn from bons is transferred from one of the main rectification columns to the small after-evaporator 20 and separator 33, that is. to a portion of the apparatus which is of relatively very small dimension. This greatly increases the safety of the main rectification.
  • the most favorable ratio for the evaporation in the after-evaporator 29 lies between 4 andl l0, that is, the liquid withdrawn from column 4 is to be reduced in evaporator 29 to at least onequarter, and at the most to one-tenth, of its original volume.
  • Process for the production of krypton and xenon from air which comprises compressing and cooling air, compressing, cooling and liquefying a relatively small portion of air, washing said cooled air with a portion of the liquefied air to form a washing liquid containing krypton, rectifying said washing liquid with another portion of said liquefied air, withdrawing the rectified washing liquid at a relatively high rate, effecting rapid evaporation of a major portion of said withdrawn liquid under continuous downow, separating the vapors of said evaporation from the remainder of the withdrawn liquid, returning said vaporsto said rectication step to be rectified with additional portions of washing liquid, and withdrawing from said separation the remainder of the liquid containing a relatively high concentration of krypton.
  • Apparatus for separating krypton and xenon from air comprising means for cooling air compressed to a suitable pressure, means for such cooled air with liq'uidair, column means for rectifying the liquid product from said washing means with additional liquid air, a separate evaporator connected to receive rectied washing liquid from said rectier column, a separator for separating liquid and vapor discharged from said evaporator, passage means for returning vapor from said separator to said rectifying column and means for continually withdrawing liquid from said separator.
  • Apparatus for separating krypton and xenon from air comprising a pair of regenerators for alternately cooling air to be washed, a second pair of regenerators for alternately cooling a smaller volume of air, means for liquefying said smaller volume of air, means for washing said cooled air with a portion of said liqueiied air, column means for rectiiying a liquid withdrawn from said washing means with another portion of said liqueiied air, means for heating the lower portion of said rectiiier column, a separate vaporizer for rapidly but incompletely vaporizing liquid drawn from the lower'portion of said rectier, a separator for separating liquid and vapor discharged from said vaporizer, means for returning vapor from said separator to said rectier, and means for continuously withdrawing liquid from said separator.
  • Process for the production of krypton and xenon from air which comprises treating air at low temperatures to form a liquid containing said rare gases, subjecting such liquid to rectilication to form al rare gas containing concentrate, withdrawing said concentrate from said rectification stage at a relatively high rate, separately vaporizing a major portion of said concentrate during continuous co-current downiiow to a degree such that the ratio of evaporation between the volume of liquid before said evaporation and the volume of liquid remaining after said evaporation is between 4 and 10, separating the vapors produced from such remainder of liquid, returning such separated vapors to the rectifying stage, and withdrawing said remainder of liquid containing a relatively high concentration of said rare gases.
  • Process for the production of krypton and xenon from air which comprises treating air at low temperatures to form a liquid containing said rare gases, subjecting such liquid to rectiflcation to form a rare gas containing concentrate,
  • Apparatus for separating krypton and xenon from air comprising means for cooling air compressed to a suitable pressure, means for washing such cooled air with liquid air, column means for rectifying the liquid product ⁇ from said washing means with additional liquid air, a separate evaporator connected to receive rectified washing liquid from said rectifying column, said evaporator comprising a tubular heating surface having its outlet lower than its inlet and arranged so that the liquid and vapor flow therethrough is uninterruptedly downward, means for supplying a relatively high-temperature heating me dium so as to externally heat said evaporator, a separator connected to receive vapor and a remainder of liquid from the outlet of said evaporator for separating such liquid from the vapor produced, passage means for returning vapor from said separator to said rectifying column, and means for withdrawing liquid from said separator.
  • Apparatus' for separating krypton and xenon from air comprising means for cooling air compressed to a suitable pressure.
  • means for washing such cooled air with liquid air column means for rectifying the liquid product from said washing means with additional liquid air, said column having a liquid collecting space in the lower portion thereof, a separate evaporator connected to receive rectified washing liquid from said rectier column, a separator for separating liquid and vapor discharged from said evaporator, the combined volume of said separator and said evaporator being substantially less than the volume of the liquid holding space of said rectifying column, passage means for returning vapor from said separator to said rectifying column, and means for withdrawing liquid from said separator.

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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)
US260943A 1938-04-09 1939-03-10 Separation of krypton and xenon from air Expired - Lifetime US2270880A (en)

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DE2270880X 1938-04-09

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US2270880A true US2270880A (en) 1942-01-27

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US (1) US2270880A (fr)
BE (1) BE433522A (fr)
FR (1) FR852154A (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3191393A (en) * 1959-12-30 1965-06-29 Air Reduction Krypton-xenon separation from a gas mixture
US9601645B2 (en) * 2008-10-13 2017-03-21 Sunlink Corporation Solar array mounting system with universal clamp

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3191393A (en) * 1959-12-30 1965-06-29 Air Reduction Krypton-xenon separation from a gas mixture
US9601645B2 (en) * 2008-10-13 2017-03-21 Sunlink Corporation Solar array mounting system with universal clamp

Also Published As

Publication number Publication date
BE433522A (fr) 1900-01-01
FR852154A (fr) 1940-01-25

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