WO2010060533A1 - Helium recovery - Google Patents

Helium recovery Download PDF

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Publication number
WO2010060533A1
WO2010060533A1 PCT/EP2009/007944 EP2009007944W WO2010060533A1 WO 2010060533 A1 WO2010060533 A1 WO 2010060533A1 EP 2009007944 W EP2009007944 W EP 2009007944W WO 2010060533 A1 WO2010060533 A1 WO 2010060533A1
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WIPO (PCT)
Prior art keywords
fraction
carbon dioxide
helium
separation
nitrogen
Prior art date
Application number
PCT/EP2009/007944
Other languages
German (de)
French (fr)
Inventor
Hans Schmidt
Martin Gwinner
Jürgen WITTE
Original Assignee
Linde Aktiengesellschaft
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Publication date
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Publication of WO2010060533A1 publication Critical patent/WO2010060533A1/en

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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
    • F25J3/0204—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
    • F25J3/0233—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 CnHm with 1 carbon atom or more
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
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    • 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
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    • 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
    • F25J3/0266—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 carbon dioxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/066—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/067—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of carbon dioxide
    • 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
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/0685—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of noble gases
    • F25J3/069—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation 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
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • 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
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    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/04—Mixing or blending of fluids with the feed stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J2215/02—Mixing or blending of fluids to yield a certain product
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    • 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
    • F25J2215/30—Helium
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J2230/32—Compression of the product stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J2230/80—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being carbon dioxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
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    • 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
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    • 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
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Definitions

  • the invention relates to a process for obtaining a helium-rich product fraction from a feed fraction comprising essentially carbon dioxide, helium, methane and higher hydrocarbons.
  • the outflowing gas mixture consists to a large extent of carbon dioxide.
  • the carbon dioxide content is usually between 70 and 98% by volume.
  • the gas mixture low proportions of methane - usually between 0.1 and 20% by volume - and heavier hydrocarbons and helium shares up to 1% by volume.
  • the gas mixtures of such sources have hitherto usually been used for the so-called Enhanced Oil Recovery (EOR).
  • EOR Enhanced Oil Recovery
  • helium-rich product fraction from the gas mixture, which allows an immediate feed into a helium liquefaction process with regard to the pressure and the trace components contained in it.
  • the helium-rich product fraction would therefore have to have a helium content of at least 50% by volume.
  • the fixed point of carbon dioxide is about -55 0 C, which is essentially independent of the respective pressure.
  • a coarse separation of the carbon dioxide from the gas mixture can take place by means of a low-temperature decomposition.
  • Further carbon dioxide separation can only take place by alternative methods, such as the so-called BCCK process with integrated methanol scrubbing or a pressure swing adsorption process.
  • BCCK process with integrated methanol scrubbing
  • a pressure swing adsorption process is comparatively expensive, while pressure swing adsorption processes can also be considered only to a limited extent due to the similar molecular sizes of carbon dioxide and methane.
  • Object of the present invention is to provide a generic method for obtaining a helium-rich product fraction, which solves this problem and avoids the aforementioned disadvantages.
  • a method for obtaining a helium-rich product fraction which comprises the following method steps:
  • the helium-rich product fraction has a helium content of at least
  • the carbon dioxide-rich residual fraction and the nitrogen-rich residual fraction are compressed together, wherein the compression is preferably carried out by means of at least one screw compressor, the carbon dioxide-rich residual fraction and / or the nitrogen-rich residual fraction of the feed fraction is mixed into the cryogenic carbon dioxide separation prior to their introduction,
  • cryogenic nitrogen separation is preceded by a carbon dioxide guard (protection) bed,
  • Separation column is integrated into the heat exchanger, and
  • the feed fraction containing essentially carbon dioxide, helium, methane and higher hydrocarbons a maximum carbon dioxide content of 98% by volume, a maximum methane content of 10% by volume and a
  • the feed fraction containing essentially carbon dioxide, helium, nitrogen, methane and higher hydrocarbons is fed via line 1 to an optionally provided drying unit A.
  • the separated in this from the feed fraction water is withdrawn via line 1 1 and, if necessary, subjected to a wastewater aftertreatment.
  • the thus freed from water feed fraction is withdrawn via line 2 from the drying unit A, partially condensed in the heat exchanger X, a relaxed a and a separating column B supplied.
  • a separation column B is to be provided if the method is to achieve the highest possible helium yield.
  • the reboiler - represented by the wiring 10 - advantageously integrated into the heat exchanger X.
  • only one separator can be provided. From the bottom of this separation column B, a liquid carbon dioxide-rich residual fraction, which will be discussed in more detail below, is withdrawn via line 8.
  • a carbon dioxide-depleted gas fraction is withdrawn via line 3, heated in the heat exchanger X and fed to an adsorption process C.
  • This serves for adsorptive separation of carbon dioxide and is preferably designed as a pressure swing adsorption process.
  • pressure swing adsorption processes allow depletion of carbon dioxide to a residual level of less than 5 ppm by volume.
  • the resulting in the adsorption process C carbon dioxide-rich residual fraction, which will be discussed in more detail below, is withdrawn via line 11.
  • the largely freed from carbon dioxide, helium-enriched fraction is withdrawn via line 4 from the adsorption process C and fed to an optionally provided carbon dioxide protection bed D for the further reduction of the carbon dioxide content. This serves to prevent possibly occurring carbon dioxide breakthroughs, which would lead to a relocation of the downstream cryogenic decomposition unit E by freezing carbon dioxide.
  • the helium-enriched fraction withdrawn from the carbon dioxide protection bed D is fed via line 5 to a cryogenic nitrogen separation unit E.
  • This consists of one or more separation columns which allow separation into a nitrogen- and methane-depleted fraction 6 and a nitrogen-rich residue fraction 12.
  • this separation unit E also serves for the rectificative separation of methane and higher hydrocarbons, which are withdrawn via the nitrogen-rich residual fraction 12.
  • the realized in the separation unit E cryogenic separation process must be designed such that the separation of nitrogen, methane and higher hydrocarbons so far that further processing of the helium-rich, nitrogen-depleted fraction in a downstream adsorption process is possible.
  • the nitrogen-depleted fraction withdrawn via line 6 is consequently freed from nitrogen and methane in an adsorption process F so far that the desired helium-rich product fraction from the adsorption process F via line 7 deducted and fed to a helium liquefaction process, not shown in the figure.
  • the aforementioned adsorption process F is preferably designed as a pressure swing adsorption process.
  • the withdrawn via line 13 nitrogen-rich residual fraction of the adsorption process F is preferably supplied together with the carbon dioxide-rich residual fraction from the adsorption process C a single or multi-stage designed compression unit G.
  • a compression to a pressure level which is an admixture of the two residual gas fractions via line 14 in the separation column B to be supplied
  • Feed fraction in line 2 allows.
  • the joint compression of the two aforementioned residual fractions in a compression unit G enables a reduction of investment and operating costs.
  • the withdrawn from the bottom of the separation column B liquid carbon dioxide-rich residual fraction is divided into two streams. Via line 8, a small partial flow to a pressure between 5 and 20 bar is relaxed b to ensure the refrigerant supply to the heat exchanger X. With this procedure, an additional refrigeration unit for this cryogenic separation is saved.
  • the warmed-up stream is compressed in a single-stage or multi-stage compressor unit V1.
  • the main stream of the withdrawn from the separation column B liquid carbon dioxide-rich residual fraction is fed via line 8 'the heat exchanger X and admixed after evaporation and heating to the compressed in the compressor unit V1 partial flow.
  • This mixture is compressed in a further single or multi-stage compressor unit V2 to the desired discharge pressure and discharged via line 9 from the process. With this procedure, a minimization of the total compressor capacity for this unit is achieved.
  • cryogenic nitrogen separation E resulting nitrogen-rich residual fraction is fed via line 12 of a single or multi-stage designed compressor unit H and after completion of compression via line 15 preferably the carbon dioxide-rich residual fraction in the line 9 admixed.
  • a partial flow of the compressed nitrogen-rich residual fraction can be introduced via the dashed line 16 for the purpose of supplying refrigeration to the cryogenic nitrogen. Separation E be recycled.
  • a separate refrigeration cycle for this separation unit E can be saved, resulting in a reduction of investment and operating costs.
  • FIG. 2 shows a possible embodiment of that shown in FIG.
  • Nitrogen separation unit E This consists essentially of a heat exchanger X 'and a separation column B'. Via line 5, the helium-enriched fraction is fed to the heat exchanger X 1 , partially condensed in this, then relaxed a and fed via line 5 'of the separation column B'. A partial stream of the helium-enriched fraction, after passing through the heat exchanger X ', is fed via line 5 "to the bottom heating of the separation column B 1 and then to the separation column B 1 itself.
  • the nitrogen-rich residual fraction is withdrawn via line 12 and fed to the one or more stages designed compressor unit H.
  • the compressed carbon dioxide-rich residual fraction is withdrawn via line 15.
  • Refrigeration supply of the nitrogen separation unit E are returned to the cryogenic nitrogen separation E.
  • the nitrogen-rich residual fraction 16 is cooled in the heat exchanger X 1 to an intermediate temperature.
  • a partial flow 16 'of the cooled residual fraction is expanded to the suction pressure of the compressor unit H, reheated in the heat exchanger X' and the nitrogen-rich residual fraction 12 admixed.
  • the remaining partial stream 16 is driven to the cold end of the heat exchanger X 'and likewise expanded to the suction pressure of the compressor unit H in order to provide the peak cooling for this cryogenic separation unit together with the expanded bottom product 12 of the separation column B' 16 "of the nitrogen-rich residual fraction reheated in the heat exchanger X 1 .
  • one of the two partial streams 16716 "described above can be dispensed with.
  • a fuel gas fraction can additionally be obtained.
  • the helium-enriched fraction in the heat exchanger X 1 is only condensed and then fed to a separator, not shown in the figure 2. From the bottom of this separator, a methane-rich liquid fraction is separated, expanded to the desired fuel gas pressure, warmed in the heat exchanger X 'and discharged as a fuel gas fraction. The withdrawn at the top of the separator, depleted of methane gas fraction is further cooled in the heat exchanger X 'and driven via line 5' in the separation column B '.
  • all the compressor units are designed as cost-effective screw compressor, but this only applies if the pressure conditions are favorable for the screw compressor.
  • the helium-rich product fraction 7 withdrawn from the adsorption process F can be fed directly to a helium liquefaction process without further processing. It is a helium recovery rate of up to 100% feasible, provided that the carbon dioxide separation takes place by means of a separation column B; In this case, the integration of the Aufkochers 10 in the heat exchanger X allows a particularly energy-saving process.

Abstract

The invention relates to a method for recovering a helium-rich product fraction from a feed fraction made up substantially of carbon dioxide, helium, methane and higher hydrocarbons, exhibiting the following process steps: a) removal of the carbon dioxide (B) from the feed fraction (1, 2); b) adsorptive separation (C) of the carbon dioxide depleted fraction (3) removed from the carbon dioxide removal (B) into a carbon dioxide rich residual fraction (11) and a helium enriched fraction (4, 5); c) cryogenic removal of nitrogen, methane and higher hydrocarbons (E) from the helium enriched fraction (4, 5); and d) adsorptive separation (F) of the nitrogen depleted fraction (6) removed from the cryogenic nitrogen removal (E) into a nitrogen rich residual fraction (13) and the helium rich product fraction (7).

Description

Beschreibung description
Helium-GewinnungHelium extraction
Die Erfindung betrifft ein Verfahren zum Gewinnen einer Helium-reichen Produktfraktion aus einer im Wesentlichen Kohlendioxid, Helium, Methan und höhere Kohlenwasserstoffe enthaltenden Einsatzfraktion.The invention relates to a process for obtaining a helium-rich product fraction from a feed fraction comprising essentially carbon dioxide, helium, methane and higher hydrocarbons.
Es existieren etliche Hochdruck-Gasguellen, bei denen das ausströmende Gasgemisch zu einem Großteil aus Kohlendioxid besteht. Der Kohlendioxid-Anteil beträgt üblicherweise zwischen 70 und 98 Vol-%. Darüber hinaus weist das Gasgemisch geringe Anteile an Methan - üblicherweise zwischen 0,1 und 20 Vol-% - und schwereren Kohlenwasserstoffen auf sowie Helium-Anteile bis zu 1 Vol-%. Die Gasgemische derartiger Quellen werden bisher üblicherweise für die sog. Enhanced OiI Recovery (EOR) verwendet.There are several high-pressure gas sources in which the outflowing gas mixture consists to a large extent of carbon dioxide. The carbon dioxide content is usually between 70 and 98% by volume. In addition, the gas mixture low proportions of methane - usually between 0.1 and 20% by volume - and heavier hydrocarbons and helium shares up to 1% by volume. The gas mixtures of such sources have hitherto usually been used for the so-called Enhanced Oil Recovery (EOR).
Da das Edelgas Helium jedoch zunehmend knapp wird, wird angedacht, derartigeHowever, as the noble gas helium is becoming increasingly scarce, is considered such
Quellen auch für die Gewinnung von Helium zu nutzen. Dazu wäre es erforderlich, aus dem Gasgemisch eine Helium-reiche Produktfraktion herzustellen, die im Hinblick auf den Druck sowie die in ihr enthaltenen Spurenkomponenten eine unmittelbare Zuführung in einen Helium-Verflüssigungsprozess ermöglicht. Die Helium-reiche Produktfraktion müsste daher einen Helium-Anteil von wenigstens 50 Vol-% aufweisen.To use sources for the extraction of helium. For this purpose, it would be necessary to produce a helium-rich product fraction from the gas mixture, which allows an immediate feed into a helium liquefaction process with regard to the pressure and the trace components contained in it. The helium-rich product fraction would therefore have to have a helium content of at least 50% by volume.
Der Festpunkt von Kohlendioxid liegt bei ca. -55 0C, wobei dieser im Wesentlichen unabhängig von dem jeweiligen Druck ist. Dies hat zur Folge, dass mittels einer Tieftemperaturzerlegung nur eine Grobabtrennung des Kohlendioxids aus dem Gasgemisch erfolgen kann. Eine weitere Kohlendioxid-Abtrennung kann ausschließlich durch alternative Verfahren, wie beispielsweise den sog. BCCK-Prozess mit integrierter Methanol-Wäsche oder einen Druckwechseladsorptionsprozess erfolgen. Das vorgenannte BCCK-Verfahren ist jedoch vergleichsweise aufwändig, während Druckwechseladsorptionsprozesse aufgrund der ähnlichen Molekülgrößen von Kohlendioxid und Methan ebenfalls nur begrenzt in Betracht gezogen werden können.The fixed point of carbon dioxide is about -55 0 C, which is essentially independent of the respective pressure. As a result, only a coarse separation of the carbon dioxide from the gas mixture can take place by means of a low-temperature decomposition. Further carbon dioxide separation can only take place by alternative methods, such as the so-called BCCK process with integrated methanol scrubbing or a pressure swing adsorption process. However, the aforementioned BCCK process is comparatively expensive, while pressure swing adsorption processes can also be considered only to a limited extent due to the similar molecular sizes of carbon dioxide and methane.
Bisher ist kein geeignetes Verfahren zum Gewinnen einer Helium-reichen Produktfraktion aus einer im Wesentlichen Kohlendioxid, Helium, Methan und höhere Kohlenwasserstoffe enthaltenden Einsatzfraktion bekannt, das eine Helium-Gewinnung mit hoher Ausbeute bei gleichzeitig geringem Energie-, Maschinen- und/oder Investitionskostenaufwand ermöglicht.So far, no suitable method for obtaining a helium-rich product fraction from a substantially carbon dioxide, helium, methane and higher Hydrocarbon-containing feed fraction known that allows helium recovery with high yield with low energy, machinery and / or investment cost.
Aufgabe der vorliegenden Erfindung ist es, ein gattungsgemäßes Verfahren zum Gewinnen einer Helium-reichen Produktfraktion anzugeben, das dieses Problem löst und die vorgenannten Nachteile vermeidet.Object of the present invention is to provide a generic method for obtaining a helium-rich product fraction, which solves this problem and avoids the aforementioned disadvantages.
Zur Lösung dieser Aufgabe wird ein Verfahren zum Gewinnen einer Helium-reichen Produktfraktion angegeben, das folgende Verfahrensschritte aufweist:To achieve this object, a method for obtaining a helium-rich product fraction is specified, which comprises the following method steps:
a) Abtrennung des Kohlendioxids aus der im Wesentlichen Kohlendioxid, Helium, Methan und höhere Kohlenwasserstoffe enthaltenden Einsatzfraktiona) separation of the carbon dioxide from the feed fraction containing essentially carbon dioxide, helium, methane and higher hydrocarbons
b) Adsorptive Auftrennung der aus der Kohlendioxid-Abtrennung abgezogenen Kohlendioxid-abgereicherten Fraktion in eine Kohlendioxid-reiche Restfraktion und eine Helium-angereicherte Fraktionb) Adsorptive separation of the deducted from the carbon dioxide separation carbon dioxide-depleted fraction into a carbon dioxide-rich residual fraction and a helium-enriched fraction
c) Kryogene Abtrennung von Stickstoff, Methan und höheren Kohlenwasserstoffen aus der Helium-angereicherten Fraktion undc) Cryogenic separation of nitrogen, methane and higher hydrocarbons from the helium-enriched fraction and
d) Adsorptive Auftrennung der aus der kryogenen Stickstoff-Abtrennung abgezogenen Stickstoff-abgereicherten Fraktion in eine Stickstoff-reiche Restfraktion und die Helium-reiche Produktfraktiond) Adsorptive separation of the withdrawn from the cryogenic nitrogen separation nitrogen-depleted fraction into a nitrogen-rich residual fraction and the helium-rich product fraction
Weitere vorteilhafte Ausgestaltungen des erfindungsgemäßen Verfahrens zum Gewinnen einer Helium-reichen Produktfraktion, die Gegenstände der abhängigen Patentansprüche darstellen, sind dadurch gekennzeichnet, dassFurther advantageous embodiments of the method according to the invention for obtaining a helium-rich product fraction, which constitute subject matters of the dependent claims, are characterized in that
- die Helium-reiche Produktfraktion einen Helium-Gehalt von wenigstens- The helium-rich product fraction has a helium content of at least
30 Vol-%, vorzugsweise von wenigstens 50 Vol-% aufweist,30 vol%, preferably of at least 50 vol%,
die Kohlendioxid-reiche Restfraktion und die Stickstoff-reiche Restfraktion gemeinsam verdichtet werden, wobei die Verdichtung vorzugsweise mittels wenigstens eines Schraubenverdichters erfolgt, die Kohlendioxid-reiche Restfraktion und/oder die Stickstoff-reiche Restfraktion der Einsatzfraktion vor deren Zuführung in die kryogene Kohlendioxid- Abtrennung zugemischt wird bzw. werden,the carbon dioxide-rich residual fraction and the nitrogen-rich residual fraction are compressed together, wherein the compression is preferably carried out by means of at least one screw compressor, the carbon dioxide-rich residual fraction and / or the nitrogen-rich residual fraction of the feed fraction is mixed into the cryogenic carbon dioxide separation prior to their introduction,
der kryogenen Stickstoff-Abtrennung ein Kohlendioxid-Guard(Schutz)-Bett vorgeschaltet ist,the cryogenic nitrogen separation is preceded by a carbon dioxide guard (protection) bed,
sofern die Einsatzfraktion in wenigstens einem Wärmetauscher abgekühlt und anschließend in einer Trennkolonne aufgetrennt wird, der Aufkocher derif the feed fraction is cooled in at least one heat exchanger and then separated in a separation column, the reboiler of
Trennkolonne in den Wärmetauscher integriert ist, undSeparation column is integrated into the heat exchanger, and
die im Wesentlichen Kohlendioxid, Helium, Methan und höhere Kohlenwasserstoffe enthaltende Einsatzfraktion einen Kohlendioxid-Anteil von maximal 98 Vol-%, einen Methan-Anteil von maximal 10 Vol-% und einenthe feed fraction containing essentially carbon dioxide, helium, methane and higher hydrocarbons a maximum carbon dioxide content of 98% by volume, a maximum methane content of 10% by volume and a
Helium-Anteil von maximal 2 Vol-% aufweist.Helium content of not more than 2% by volume.
Das erfindungsgemäße Verfahren zum Gewinnen einer Helium-reichen Produktfraktion sowie weitere Ausgestaltungen desselben seien nachfolgend anhand des in den Figuren 1 und 2 dargestellten Ausführungsbeispieles näher erläutert.The method according to the invention for obtaining a helium-rich product fraction and further embodiments thereof will be explained in more detail below with reference to the exemplary embodiment illustrated in FIGS. 1 and 2.
Wie anhand der Figur 1 dargestellt, wird über Leitung 1 die im Wesentlichen Kohlendioxid, Helium, Stickstoff, Methan und höhere Kohlenwasserstoffe enthaltende Einsatzfraktion einer optional vorzusehenden Trocknungs-Einheit A zugeführt. Das in dieser aus der Einsatzfraktion abgetrennte Wasser wird über Leitung 11 abgezogen und, sofern erforderlich, einer Abwasser-Nachbehandlung unterzogen.As shown with reference to FIG. 1, the feed fraction containing essentially carbon dioxide, helium, nitrogen, methane and higher hydrocarbons is fed via line 1 to an optionally provided drying unit A. The separated in this from the feed fraction water is withdrawn via line 1 1 and, if necessary, subjected to a wastewater aftertreatment.
Die derart von Wasser befreite Einsatzfraktion wird über Leitung 2 aus der Trocknungs- Einheit A abgezogen, im Wärmetauscher X partiell kondensiert, entspannt a und einer Trennkolonne B zugeführt. Eine derartige Trennkolonne B ist dann vorzusehen, wenn das Verfahren eine möglichst hohe Helium-Ausbeute erreichen soll. Hierbei ist der Aufkocher - dargestellt durch die Leitungsführung 10 - in vorteilhafter weise in den Wärmetauscher X integriert. Alternativ zu der in der Figur 1 gezeigten Trennkolonne B kann auch lediglich ein Abscheider vorgesehen werden. Aus dem Sumpf dieser Trennkolonne B wird über Leitung 8 eine flüssige Kohlendioxidreiche Restfraktion, auf die im Folgenden noch näher eingegangen werden wird, abgezogen.The thus freed from water feed fraction is withdrawn via line 2 from the drying unit A, partially condensed in the heat exchanger X, a relaxed a and a separating column B supplied. Such a separation column B is to be provided if the method is to achieve the highest possible helium yield. Here, the reboiler - represented by the wiring 10 - advantageously integrated into the heat exchanger X. As an alternative to the separation column B shown in FIG. 1, only one separator can be provided. From the bottom of this separation column B, a liquid carbon dioxide-rich residual fraction, which will be discussed in more detail below, is withdrawn via line 8.
Am Kopf der Trennkolonne B wird über Leitung 3 eine Kohlendioxid-abgereicherte Gasfraktion abgezogen, im Wärmetauscher X angewärmt und einem Adsorptions- Prozess C zugeführt. Dieser dient der adsorptiven Abtrennung von Kohlendioxid und ist vorzugsweise als Druckwechseladsorptionsprozess ausgelegt. Derartige Druckwechseladsorptionsprozesse erlauben eine Abreicherung von Kohlendioxid auf einen Restgehalt von weniger als 5 Vol-ppm. Die in dem Adsorptions-Prozess C anfallende Kohlendioxid-reiche Restfraktion, auf die im Folgenden noch näher eingegangen werden wird, wird über Leitung 11 abgezogen.At the top of the separation column B, a carbon dioxide-depleted gas fraction is withdrawn via line 3, heated in the heat exchanger X and fed to an adsorption process C. This serves for adsorptive separation of carbon dioxide and is preferably designed as a pressure swing adsorption process. Such pressure swing adsorption processes allow depletion of carbon dioxide to a residual level of less than 5 ppm by volume. The resulting in the adsorption process C carbon dioxide-rich residual fraction, which will be discussed in more detail below, is withdrawn via line 11.
Die von Kohlendioxid weitgehend befreite, Helium-angereicherte Fraktion wird über Leitung 4 aus dem Adsorptions-Prozess C abgezogen und einem optional vorzusehenden Kohlendioxid-Schutz-Bett D für die weitere Reduzierung des Kohlendioxid-Gehaltes zugeführt. Dies dient der Verhinderung eventuell auftretender Kohlendioxid-Durchbrüche, die zu einer Verlegung der nachgeschalteten kryogenen Zerlegungseinheit E durch ausfrierendes Kohlendioxid führen würden.The largely freed from carbon dioxide, helium-enriched fraction is withdrawn via line 4 from the adsorption process C and fed to an optionally provided carbon dioxide protection bed D for the further reduction of the carbon dioxide content. This serves to prevent possibly occurring carbon dioxide breakthroughs, which would lead to a relocation of the downstream cryogenic decomposition unit E by freezing carbon dioxide.
Die aus dem Kohlendioxid-Schutz-Bett D abgezogene, Helium-angereicherte Fraktion wird über Leitung 5 einer kryogenen Stickstoff-Abtrenneinheit E zugeführt. Diese besteht aus einer oder mehreren Trennkolonnen, die eine Auftrennung in eine Stickstoff- und Methan-abgereicherte Fraktion 6 und eine Stickstoff-reiche Restfraktion 12 ermöglichen. Neben Stickstoff dient diese Abtrenneinheit E auch der rektifikatorischen Abtrennung von Methan und höheren Kohlenwasserstoffen, die über die Stickstoff-reiche Restfraktion 12 abgezogen werden. Hierbei muss der in der Abtrenneinheit E realisierte Tieftemperaturtrennprozess derart ausgelegt sein, dass die Abtrennung von Stickstoff, Methan und höheren Kohlenwasserstoffen so weit erfolgt, dass eine Weiterverarbeitung der Helium-reichen, Stickstoff-abgereicherten Fraktion in einem nachgeschalteten Adsorptionsprozess möglich ist.The helium-enriched fraction withdrawn from the carbon dioxide protection bed D is fed via line 5 to a cryogenic nitrogen separation unit E. This consists of one or more separation columns which allow separation into a nitrogen- and methane-depleted fraction 6 and a nitrogen-rich residue fraction 12. In addition to nitrogen, this separation unit E also serves for the rectificative separation of methane and higher hydrocarbons, which are withdrawn via the nitrogen-rich residual fraction 12. Here, the realized in the separation unit E cryogenic separation process must be designed such that the separation of nitrogen, methane and higher hydrocarbons so far that further processing of the helium-rich, nitrogen-depleted fraction in a downstream adsorption process is possible.
Die über Leitung 6 abgezogene Stickstoff-abgereicherte Fraktion wird in einem Adsorptionsprozess F folglich soweit von Stickstoff und Methan befreit, dass aus dem Adsorptionsprozess F über Leitung 7 die gewünschte Helium-reiche Produktfraktion abgezogen und einem in der Figur nicht dargestellten Helium-Verflüssigungsprozess zugeführt werden kann.The nitrogen-depleted fraction withdrawn via line 6 is consequently freed from nitrogen and methane in an adsorption process F so far that the desired helium-rich product fraction from the adsorption process F via line 7 deducted and fed to a helium liquefaction process, not shown in the figure.
Auch der vorgenannte Adsorptionsprozess F ist vorzugsweise als Druckwechseladsorptionsprozess ausgelegt. Die über Leitung 13 abgezogene Stickstoff-reiche Restfraktion des Adsorptionsprozesses F wird vorzugsweise gemeinsam mit der Kohlendioxid-reichen Restfraktion aus dem Adsorptionsprozess C einer ein- oder mehrstufig ausgelegten Verdichtungseinheit G zugeführt. In dieser erfolgt eine Verdichtung auf ein Druckniveau, das eine Zumischung der beiden Restgasfraktionen über Leitung 14 in die der Trennkolonne B zuzuführendeAlso, the aforementioned adsorption process F is preferably designed as a pressure swing adsorption process. The withdrawn via line 13 nitrogen-rich residual fraction of the adsorption process F is preferably supplied together with the carbon dioxide-rich residual fraction from the adsorption process C a single or multi-stage designed compression unit G. In this, a compression to a pressure level, which is an admixture of the two residual gas fractions via line 14 in the separation column B to be supplied
Einsatzfraktion in der Leitung 2 ermöglicht. Die gemeinsame Verdichtung der beiden vorgenannten Restfraktionen in einer Verdichtungseinheit G ermöglicht eine Reduzierung der Investitions- und Betriebskosten.Feed fraction in line 2 allows. The joint compression of the two aforementioned residual fractions in a compression unit G enables a reduction of investment and operating costs.
Die aus dem Sumpf der Trennkolonne B abgezogene flüssige Kohlendioxid-reiche Restfraktion wird in zwei Ströme aufgeteilt. Über Leitung 8 wird ein geringer Teilstrom auf einen Druck zwischen 5 und 20 bar entspannt b, um die Kältemittelversorgung für den Wärmetauscher X zu gewährleisten. Mit dieser Vorgehensweise wird eine zusätzliche Kälteeinheit für diese kryogene Abtrennung eingespart. Der angewärmte Strom wird in einer ein- oder mehrstufig ausgebildeten Verdichtereinheit V1 komprimiert. Der Hauptstrom der aus der Trennkolonne B abgezogenen flüssigen Kohlendioxid-reichen Restfraktion wird über Leitung 8' dem Wärmetauscher X zugeführt und nach Verdampfung und Anwärmung dem in der Verdichtereinheit V1 verdichteten Teilstrom zugemischt. Diese Mischung wird in einer weiteren ein- oder mehrstufig ausgeführten Verdichtereinheit V2 auf den gewünschten Abgabedruck verdichtet und über Leitung 9 aus dem Prozess abgeführt. Mit dieser Verfahrensführung wird eine Minimierung der Gesamt-Verdichterleistung für diese Einheit erreicht.The withdrawn from the bottom of the separation column B liquid carbon dioxide-rich residual fraction is divided into two streams. Via line 8, a small partial flow to a pressure between 5 and 20 bar is relaxed b to ensure the refrigerant supply to the heat exchanger X. With this procedure, an additional refrigeration unit for this cryogenic separation is saved. The warmed-up stream is compressed in a single-stage or multi-stage compressor unit V1. The main stream of the withdrawn from the separation column B liquid carbon dioxide-rich residual fraction is fed via line 8 'the heat exchanger X and admixed after evaporation and heating to the compressed in the compressor unit V1 partial flow. This mixture is compressed in a further single or multi-stage compressor unit V2 to the desired discharge pressure and discharged via line 9 from the process. With this procedure, a minimization of the total compressor capacity for this unit is achieved.
Die bereits erwähnte, in der kryogenen Stickstoff-Abtrennung E anfallende Stickstoff- reiche Restfraktion wird über Leitung 12 einer ein- oder mehrstufig ausgelegten Verdichtereinheit H zugeführt und nach erfolgter Verdichtung über Leitung 15 vorzugsweise der Kohlendioxid-reichen Restfraktion in der Leitung 9 zugemischt. Ein Teilstrom der verdichteten Stickstoff-reichen Restfraktion kann über die gestrichelt gezeichnete Leitung 16 zum Zwecke der Kälteversorgung in die kryogene Stickstoff- Abtrennung E zurückgeführt werden. Damit kann ein eigener Kältekreislauf für diese Abtrenneinheit E eingespart werden, woraus eine Reduzierung von Investitions- und Betriebskosten resultiert.The already mentioned, in the cryogenic nitrogen separation E resulting nitrogen-rich residual fraction is fed via line 12 of a single or multi-stage designed compressor unit H and after completion of compression via line 15 preferably the carbon dioxide-rich residual fraction in the line 9 admixed. A partial flow of the compressed nitrogen-rich residual fraction can be introduced via the dashed line 16 for the purpose of supplying refrigeration to the cryogenic nitrogen. Separation E be recycled. Thus, a separate refrigeration cycle for this separation unit E can be saved, resulting in a reduction of investment and operating costs.
Die Figur 2 zeigt eine mögliche Ausführungsform der in der Figur 1 dargestelltenFIG. 2 shows a possible embodiment of that shown in FIG
Stickstoff-Abtrenneinheit E. Diese besteht im Wesentlichen aus einem Wärmetauscher X' sowie einer Trennkolonne B'. Über Leitung 5 wird die Helium-angereicherte Fraktion dem Wärmetauscher X1 zugeführt, in diesem partiell kondensiert, anschließend entspannt a und über Leitung 5' der Trennkolonne B' zugeführt. Ein Teilstrom der Helium-angereicherten Fraktion wird nach Durchgang durch den Wärmetauscher X' über Leitung 5" der Sumpfheizung der Trennkolonne B1 und anschließend der Trennkolonne B1 selbst zugeführt.Nitrogen separation unit E. This consists essentially of a heat exchanger X 'and a separation column B'. Via line 5, the helium-enriched fraction is fed to the heat exchanger X 1 , partially condensed in this, then relaxed a and fed via line 5 'of the separation column B'. A partial stream of the helium-enriched fraction, after passing through the heat exchanger X ', is fed via line 5 "to the bottom heating of the separation column B 1 and then to the separation column B 1 itself.
Am Kopf der Trennkolonne B' wird über Leitung 6 die Stickstoff- und Methan- abgereicherte Fraktion abgezogen und der anhand der Figur 1 beschriebenenAt the top of the separation column B ', the nitrogen- and methane-depleted fraction is withdrawn via line 6 and described with reference to FIG
Weiterbehandlung zugeführt. Aus dem Sumpf der Trennkolonne B' wird über Leitung 12 die Stickstoff-reiche Restfraktion abgezogen und der ein- oder mehrstufig ausgelegten Verdichtereinheit H zugeführt. Die verdichtete Kohlendioxid-reiche Restfraktion wird über Leitung 15 abgezogen. Wie bereits erwähnt, kann ein Teilstrom der verdichteten Stickstoff-reichen Restfraktion über Leitung 16 zum Zwecke derFurther treatment supplied. From the bottom of the separation column B ', the nitrogen-rich residual fraction is withdrawn via line 12 and fed to the one or more stages designed compressor unit H. The compressed carbon dioxide-rich residual fraction is withdrawn via line 15. As already mentioned, a partial flow of the compressed nitrogen-rich residual fraction via line 16 for the purpose of
Kälteversorgung der Stickstoff-Abtrenneinheit E in die kryogene Stickstoff-Abtrennung E zurückgeführt werden.Refrigeration supply of the nitrogen separation unit E are returned to the cryogenic nitrogen separation E.
In vorteilhafter Weise wird die Stickstoff-reiche Restfraktion 16 im Wärmetauscher X1 auf eine Zwischentemperatur abgekühlt. Ein Teilstrom 16' der abgekühlten Restfraktion wird auf den Saugdruck der Verdichtereinheit H entspannt, erneut im Wärmetauscher X' angewärmt und der Stickstoff-reichen Restfraktion 12 zugemischt. Der restliche Teilstrom 16" wird bis zum kalten Ende des Wärmetauschers X' gefahren und ebenfalls auf den Saugdruck der Verdichtereinheit H entspannt, um gemeinsam mit dem entspannten Sumpfprodukt 12 der Trennkolonne B' die Spitzenkälte für diese kryogene Abtrenneinheit bereitzustellen. Nacherfolgter Entspannung wird auch dieser Teilstrom 16" der Stickstoff-reichen Restfraktion wieder im Wärmetauscher X1 angewärmt. Sofern es der Kältebedarf der Stickstoff-Abtrenneinheit E erlaubt, kann auf einen der beiden vorbeschriebenen Teilströme 16716" verzichtet werden. Sofern die der Trennkolonne B1 über Leitung 5 zugeführte Helium-angereicherte Fraktion einen Methan-Gehalt von mehr als 0.5 Vol-% aufweist, kann zusätzlich eine Brenngasfraktion gewonnen werden. In diesem Falle wird die Helium-angereicherte Fraktion im Wärmetauscher X1 lediglich ankondensiert und anschließend einem in der Figur 2 nicht dargestellten Abscheider zugeführt. Aus dem Sumpf dieses Abscheiders wird eine Methan-reiche Flüssigfraktion abgetrennt, auf den gewünschten Brenngasdruck entspannt, im Wärmetauscher X' angewärmt und als Brenngasfraktion abgegeben. Die am Kopf des Abscheiders abgezogenen, an Methan abgereicherte Gasfraktion wird im Wärmetauscher X' weiter abgekühlt und über Leitung 5' in die Trennkolonne B' gefahren.Advantageously, the nitrogen-rich residual fraction 16 is cooled in the heat exchanger X 1 to an intermediate temperature. A partial flow 16 'of the cooled residual fraction is expanded to the suction pressure of the compressor unit H, reheated in the heat exchanger X' and the nitrogen-rich residual fraction 12 admixed. The remaining partial stream 16 "is driven to the cold end of the heat exchanger X 'and likewise expanded to the suction pressure of the compressor unit H in order to provide the peak cooling for this cryogenic separation unit together with the expanded bottom product 12 of the separation column B' 16 "of the nitrogen-rich residual fraction reheated in the heat exchanger X 1 . If the refrigeration requirement of nitrogen separation unit E permits, one of the two partial streams 16716 "described above can be dispensed with. If the helium-enriched fraction fed to the separation column B 1 via line 5 has a methane content of more than 0.5% by volume, a fuel gas fraction can additionally be obtained. In this case, the helium-enriched fraction in the heat exchanger X 1 is only condensed and then fed to a separator, not shown in the figure 2. From the bottom of this separator, a methane-rich liquid fraction is separated, expanded to the desired fuel gas pressure, warmed in the heat exchanger X 'and discharged as a fuel gas fraction. The withdrawn at the top of the separator, depleted of methane gas fraction is further cooled in the heat exchanger X 'and driven via line 5' in the separation column B '.
Vorzugsweise sind sämtliche Verdichtereinheiten als kostengünstige Schraubenverdichter ausgelegt, wobei dies jedoch nur dann gilt, wenn die Druckverhältnisse für die Schraubenverdichter günstig sind.Preferably, all the compressor units are designed as cost-effective screw compressor, but this only applies if the pressure conditions are favorable for the screw compressor.
Das erfindungsgemäße Verfahren zum Gewinnen einer Helium-reichen Produktfraktion weist gegenüber den zum Stand der Technik zählenden Verfahren eine Vielzahl von Vorteilen auf:The process according to the invention for obtaining a helium-rich product fraction has a large number of advantages over the processes belonging to the prior art:
- Niedrige Investitionskosten durch Integration der beiden Adsorptionsprozesse- Low investment costs through integration of the two adsorption processes
C/F und der kryogenen Stickstoff-Abtrenneinheit E mit der Recycle- Verdichtungseinheit G.C / F and the cryogenic nitrogen separation unit E with the recycle compression unit G.
Niedrige Investitions- und Betriebskosten durch Minimierung der Maschinenanzahl; des Weiteren können überwiegend vergleichsweise kostengünstige Schraubenverdichter zur Anwendung kommen.Low capital and operating costs by minimizing the number of machines; Furthermore, predominantly comparatively cost-effective screw compressors can be used.
Kein Fremdkältebedarf bzw. externer Kältekreislauf erforderlich, falls - wie vorstehend erläutert - die Kälteversorgung der Abtrenneinheit E in die Verdichtereinheit H integrierten ist.No external cold demand or external refrigeration cycle required if - as explained above - the cooling supply of the separation unit E is integrated into the compressor unit H.
Die aus dem Adsorptionsprozess F abgezogene Helium-reiche Produktfraktion 7 kann unmittelbar ohne weitere Bearbeitung einem Helium- Verflüssigungsprozess zugeführt werden. Es ist eine Helium-Gewinnungsrate von bis zu 100 % realisierbar, sofern die Kohlendioxid-Abtrennung mittels einer Trennkolonne B erfolgt; hierbei ermöglicht die Integration des Aufkochers 10 in den Wärmetauscher X ein besonders energiesparendes Verfahren. The helium-rich product fraction 7 withdrawn from the adsorption process F can be fed directly to a helium liquefaction process without further processing. It is a helium recovery rate of up to 100% feasible, provided that the carbon dioxide separation takes place by means of a separation column B; In this case, the integration of the Aufkochers 10 in the heat exchanger X allows a particularly energy-saving process.

Claims

Patentansprüche claims
1. Verfahren zum Gewinnen einer Helium-reichen Produktfraktion aus einer im Wesentlichen Kohlendioxid, Helium, Methan und höhere Kohlenwasserstoffe enthaltenden Einsatzfraktion, aufweisend folgende Verfahrensschritte:A process for recovering a helium-rich product fraction from a feed fraction containing essentially carbon dioxide, helium, methane and higher hydrocarbons, comprising the following process steps:
a) Abtrennung des Kohlendioxids (B) aus der Einsatzfraktion (1 , 2)a) Separation of the carbon dioxide (B) from the feed fraction (1, 2)
b) Adsorptive Auftrennung (C) der aus der Kohlendioxid-Abtrennung (B) abgezogenen Kohlendioxid-abgereicherten Fraktion (3) in eine Kohlendioxid- reiche Restfraktion (11) und eine Helium-angereicherte Fraktion (4, 5)b) adsorptive separation (C) of the carbon dioxide-depleted fraction (3) withdrawn from the carbon dioxide separation (B) into a carbon dioxide-rich residual fraction (11) and a helium-enriched fraction (4, 5)
c) Kryogene Abtrennung von Stickstoff, Methan und höheren Kohlenwasserstoffen (E) aus der Helium-angereicherten Fraktion (4, 5) undc) Cryogenic separation of nitrogen, methane and higher hydrocarbons (E) from the helium-enriched fraction (4, 5) and
d) Adsorptive Auftrennung (F) der aus der kryogenen Stickstoff-Abtrennung (E) abgezogenen Stickstoff-abgereicherten Fraktion (6) in eine Stickstoff-reiche Restfraktion (13) und die Helium-reiche Produktfraktion (7)d) Adsorptive separation (F) of the nitrogen-depleted fraction (6) withdrawn from the cryogenic nitrogen separation (E) into a nitrogen-rich residual fraction (13) and the helium-rich product fraction (7)
2. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, dass die Helium-reiche2. The method according to claim 1, characterized in that the helium-rich
Produktfraktion (7) einen Helium-Gehalt von wenigstens 30 Vol-%, vorzugsweise von wenigstens 50 Vol-% aufweist.Product fraction (7) has a helium content of at least 30% by volume, preferably of at least 50% by volume.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Kohlendioxid-reiche Restfraktion (1 1) und die Stickstoff-reiche Restfraktion (13) gemeinsam verdichtet werden (G), wobei die Verdichtung vorzugsweise mittels wenigstens eines Schraubenverdichters erfolgt.3. The method according to claim 1 or 2, characterized in that the carbon dioxide-rich residual fraction (1 1) and the nitrogen-rich residual fraction (13) are compressed together (G), wherein the compression is preferably carried out by means of at least one screw compressor.
4. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die Kohlendioxid-reiche Restfraktion (11) und/oder die4. The method according to any one of the preceding claims 1 to 3, characterized in that the carbon dioxide-rich residual fraction (11) and / or the
Stickstoff-reiche Restfraktion (13) der Einsatzfraktion (2) vor deren Zuführung in die kryogene Kohlendioxid-Abtrennung (B) zugemischt wird bzw. werden. Nitrogen-rich residual fraction (13) of the feed fraction (2) before being supplied into the cryogenic carbon dioxide separation (B) is or are mixed.
5. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 4, dadurch gekennzeichnet, dass der kryogenen Stickstoff-Abtrennung (E) ein Kohlendioxid- Guard(Schutz)-Bett (D) vorgeschaltet ist.5. The method according to any one of the preceding claims 1 to 4, characterized in that the cryogenic nitrogen separation (E) is preceded by a carbon dioxide guard (protection) -Bett (D).
6. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 5, wobei die6. The method according to any one of the preceding claims 1 to 5, wherein the
Einsatzfraktion (1 , 2) in wenigstens einem Wärmetauscher (X) abgekühlt und anschließend in einer Trennkolonne (B) aufgetrennt wird, dadurch gekennzeichnet, dass der Aufkocher (10) der Trennkolonne (B) in den Wärmetauscher (X) integriert ist.Feed fraction (1, 2) cooled in at least one heat exchanger (X) and then separated in a separation column (B), characterized in that the reboiler (10) of the separation column (B) in the heat exchanger (X) is integrated.
7. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 6, dadurch gekennzeichnet, dass die im Wesentlichen Kohlendioxid, Helium, Methan und höhere Kohlenwasserstoffe enthaltende Einsatzfraktion einen Kohlendioxid-Anteil von maximal 98 Vol-%, einen Methan-Anteil von maximal 10 Vol-% und einen Helium-Anteil von maximal 2 Vol-% aufweist. 7. The method according to any one of the preceding claims 1 to 6, characterized in that the substantially carbon dioxide, helium, methane and higher hydrocarbons containing feed fraction a carbon dioxide content of not more than 98% by volume, a methane content of not more than 10% by volume and a helium content of not more than 2% by volume.
PCT/EP2009/007944 2008-11-26 2009-11-05 Helium recovery WO2010060533A1 (en)

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