WO2016128111A1 - Procédé d'extraction d'hélium - Google Patents

Procédé d'extraction d'hélium Download PDF

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Publication number
WO2016128111A1
WO2016128111A1 PCT/EP2016/000131 EP2016000131W WO2016128111A1 WO 2016128111 A1 WO2016128111 A1 WO 2016128111A1 EP 2016000131 W EP2016000131 W EP 2016000131W WO 2016128111 A1 WO2016128111 A1 WO 2016128111A1
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WO
WIPO (PCT)
Prior art keywords
nitrogen
fraction
helium
rich fraction
rich
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2016/000131
Other languages
German (de)
English (en)
Inventor
Heinz Bauer
Martin Gwinner
Andreas Bub
Christoph HERTEL
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linde GmbH
Original Assignee
Linde GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Priority to AU2016218602A priority Critical patent/AU2016218602B2/en
Priority to CA2976341A priority patent/CA2976341C/fr
Priority to US15/549,854 priority patent/US20180023888A1/en
Publication of WO2016128111A1 publication Critical patent/WO2016128111A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/028—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 characterised by the separated product stream separation of noble gases
    • F25J3/029—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 characterised by the separated product stream separation of noble gases of helium
    • 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
    • F25J3/0204—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 characterised by the feed stream
    • F25J3/0209—Natural gas or substitute natural gas
    • 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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/0257—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 characterised by the separated product stream separation of nitrogen
    • 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
    • F25J2200/02—Processes or apparatus using separation by rectification in a single 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
    • F25J2200/40—Features relating to the provision of boil-up in the bottom of a 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • 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
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • 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
    • F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • 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
    • 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
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • 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
    • F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
    • 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
    • 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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/04—Recovery of liquid products
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/42—Separating low boiling, i.e. more volatile components from nitrogen, e.g. He, H2, Ne
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/42—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being nitrogen
    • 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
    • F25J2240/00—Processes or apparatus involving steps for expanding of process streams
    • F25J2240/02—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream
    • F25J2240/12—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream the fluid being nitrogen
    • 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
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/02—Internal refrigeration with liquid vaporising loop
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
    • 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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/34—Details about subcooling of liquids

Definitions

  • the invention relates to a method for obtaining a helium product fraction from a nitrogen and helium-containing feed fraction, wherein
  • Nitrogen and helium-containing feed fraction warmed, compressed and the partially condensed nitrogen and helium-containing
  • Feed fraction is mixed.
  • helium product fraction includes high purity helium whose
  • Concentration of impurities does not exceed a value of 100 vppm, preferably of 10 vppm.
  • nitrogen and helium-containing feed fraction is to be understood as meaning a fraction which contains 1 to 20 mol% of helium and 80 to 99 mol% of nitrogen. Furthermore, this feed fraction may contain 0.1 to 2 mol% of methane and traces of hydrogen, argon and / or other noble gases.
  • helium is commercially obtained almost exclusively from a mixture of volatile natural gas components, which typically contains, in addition to helium, methane and nitrogen as well as traces of hydrogen, argon and other noble gases. To freeze out unwanted contaminants in the
  • the concentration of these impurities in helium must not exceed a value of 100 vppm, preferably 10 vppm.
  • the actual helium liquefaction upstream helium purification usually consists of a combination of cryogenic - based on partial condensation - and adsorptive process with regeneration by pressure and / or temperature changes. Due to the comparatively high product value, the highest possible helium yield, preferably> 99%, is desirable. For this reason, the helium-rich fraction often goes through the cryogenic step
  • Nitrogen-rich stream which is at elevated pressure and containing helium, is separated by utilizing a pressure gradient into a helium-containing stream of medium pressure and a nitrogen-rich stream of low pressure. This separation takes place in a rectification column which has a reboiler and a condenser.
  • the object of the present invention is to provide a generic method for obtaining a helium product fraction which makes it possible to deliver at least a subset of the nitrogen-rich stream obtained during the separation at the same pressure as the helium-containing stream in order to produce the nitrogen atom. rich stream then, for example, to be able to perform a work-relaxation.
  • Fraction and a second nitrogen-rich fraction is carried out in a separation column to which the 1st nitrogen-rich fraction is fed as reflux,
  • Separation column is fed as stripping gas
  • At least a partial stream of the 2nd nitrogen-rich fraction is evaporated under a pressure of less than 5 bar against the partially to be condensed nitrogen and helium-containing feed fraction
  • a third nitrogen-rich fraction is withdrawn, the amount of stripping gas being adjusted so that the third nitrogen-rich fraction is at least 30% of that in the 1st nitrogen-rich fraction
  • the third nitrogen-rich fraction serves, at least in part, for the cooling of the nitrogen and helium-containing feed fraction which is to be partially condensed.
  • the third nitrogen-rich fraction is at least partially expanded work
  • the separation column is operated at a pressure of 7 to 20 bar, preferably from 10 to 15 bar
  • the third nitrogen-rich fraction at least 50th % of the nitrogen contained in the 1st nitrogen-rich fraction contains, - at least a partial stream of the 2nd nitrogen-rich fraction is evaporated under a pressure of less than 3 bar against the partially to be condensed nitrogen and helium-containing feed fraction, and / or the adsorptive cleaning process is a (V) PSA and / or TSA process.
  • a nitrogen and helium-containing feed fraction which originates for example from a natural gas decomposition process, first a catalytic methane oxidation A and then via line 2 a
  • Drying unit B supplied.
  • the separated in the drying unit B water is withdrawn via line 30.
  • Feed fraction usually a pressure between 10 and 40 bar, preferably between 15 and 25 bar, is fed via line 3 to the heat exchanger E1 and partially condensed in this against yet to be explained process streams. Via line 4, the partially condensed feed fraction becomes a
  • Separator D1 supplied and separated in this in a 1st helium-rich fraction 5 and a first nitrogen-rich fraction 8.
  • the helium-rich fraction 5 is fed after heating in the heat exchanger E1 an adsorptive purification process D. This is designed as (V) PSA and / or TSA process.
  • the helium-rich fraction obtained in it and drawn off via line 6 represents the helium product fraction, its concentration
  • Impurities do not exceed a value of 100 vppm, preferably 100 vppm.
  • this helium product fraction is fed to a liquefaction process, not shown in FIG.
  • the withdrawn from the adsorptive purification process D, helium-containing residual gas is fed via line 7 to a recompressor C, in this compressed to the pressure of the catalytic methane oxidation A feed fraction 1 and this mixed via line 32.
  • nitrogen-rich fraction 8 is expanded in the valve a and fed to the separation column T in the upper region as reflux.
  • the separation column T is preferably operated at a pressure between 7 and 20 bar, in particular between 10 and 15 bar. It is separated into a second helium-rich
  • the second helium-rich fraction 9 is in the heat exchanger E1 against the partially condensed
  • the oxygen contained in the air is used in the catalytic methane oxidation A as an oxidizing agent.
  • a partial stream of the second nitrogen-rich liquid fraction 1 1 is evaporated in the heat exchanger E1 and fed to the separation column T as stripping gas 12.
  • This stripping gas supply effects the separation process taking place in the separation column T and determines the helium content of the second helium-rich fraction 9.
  • At least one substream of the 2nd nitrogen-rich fraction 11 is evaporated under a pressure of less than 5 bar, preferably of less than 3 bar, in the heat exchanger E1 against the feed fraction 3 to be partially condensed.
  • Procedure serves to set the lowest possible temperature in the separator D1.
  • Circulating container D2 supplied. The deducted from this via line 14
  • Liquid fraction is fed under the aforementioned low pressure to the heat exchanger E1, in this at least partially evaporated and fed again to the circulation tank D2.
  • Feed fraction 3 warmed and then the above
  • Drying unit B which is usually an adsorptive
  • Drying process is, fed as a regeneration gas. Via line 16, this laden regeneration gas is withdrawn from the process.
  • the non-circulating tank D2 supplied partial stream 13 of the 2nd nitrogen-rich fraction 1 1 can be supercooled in the heat exchanger E1 and discharged via control valve d and line 17 as supercooled liquid.
  • liquefied nitrogen LIN
  • a partial flow of the liquid fraction 14 withdrawn from the circulation container D2 can be withdrawn in the manner described above via control valve d and line 17.
  • the cold required for the partial condensation of the feed fraction 3 can only by the heating of cold, gaseous decomposition products and the above-described evaporation from the circulation container D2
  • the amount of the stripping gas 12 fed to the separation column T is additionally selected so that a third nitrogen-rich fraction 20 can be withdrawn from the separation column T in the region of its sump, at least 30%, preferably at least 50% of that in FIG Nitrogen-rich fraction 8 contains nitrogen contained.
  • a third nitrogen-rich fraction 20 can be withdrawn from the separation column T in the region of its sump, at least 30%, preferably at least 50% of that in FIG Nitrogen-rich fraction 8 contains nitrogen contained.
  • Procedure can now be obtained in the separation column T, a further nitrogen-rich fraction at elevated pressure.
  • this further or third nitrogen-rich fraction can be compressed to a pressure which is 4 to 20 bar, preferably 5 to 15 bar, above the pressure of the column T.
  • the nitrogen-rich fraction 21 is cooled in the heat exchanger E1 and then expanded in the expansion device X work.
  • the expanded nitrogen-rich fraction 22 is then heated in the heat exchanger E1 against the partially to be condensed feed fraction 3 and the above-described nitrogen-rich fraction 15 admixed.
  • This work-in-progress relaxation X which increases the thermodynamic efficiency of the process, is optional, but allows or increases the amount of supercooled liquid (LIN) withdrawn via line 17.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Separation Of Gases By Adsorption (AREA)

Abstract

L'invention concerne un procédé d'extraction d'une fraction de produit d'hélium (6) à partir d'une fraction de charge (3) contenant de l'azote et de l'hélium. La fraction de charge (3) contenant de l'azote et de l'hélium est partiellement condensée (E1), séparée en une 1ère fraction riche en hélium (5) et une 1ère fraction riche en azote (8) et la première est repurifiée par adsorption. Selon l'invention, la séparation est effectuée dans une colonne de séparation (T) à laquelle sont acheminées la 1ère fraction riche en azote (8) sous forme de reflux et un courant partiel de la 2ème fraction riche en azote sous la forme de gaz de réextraction (12). Le volume de gaz de réextraction (12) est réglé de telle sorte qu'une 3ème fraction riche en azote (20), laquelle contient au moins 30 % de l'azote contenu dans la 1ère fraction riche en azote (8), peut être extraite dans la colonne de séparation (T).
PCT/EP2016/000131 2015-02-10 2016-01-26 Procédé d'extraction d'hélium Ceased WO2016128111A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
AU2016218602A AU2016218602B2 (en) 2015-02-10 2016-01-26 Method for recovering helium
CA2976341A CA2976341C (fr) 2015-02-10 2016-01-26 Procede d'extraction d'helium
US15/549,854 US20180023888A1 (en) 2015-02-10 2016-01-26 Method for recovering helium

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DE10007440A1 (de) * 2000-02-18 2001-08-23 Linde Ag Verfahren zum Abtrennen einer Helium-reichen Fraktion aus einem wenigstens Methan, Stickstoff und Helium enthaltenden Strom

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RU2015124169A (ru) 2017-01-10
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AU2016218602A1 (en) 2017-08-31
CA2976341A1 (fr) 2016-08-18
RU2689252C2 (ru) 2019-05-24
DE102015001664A1 (de) 2016-08-11
US20180023888A1 (en) 2018-01-25

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