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AU2006212459B2 - Method for separating trace components from a stream that is rich in nitrogen - Google Patents
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AU2006212459B2 - Method for separating trace components from a stream that is rich in nitrogen - Google Patents

Method for separating trace components from a stream that is rich in nitrogen Download PDF

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AU2006212459B2
AU2006212459B2 AU2006212459A AU2006212459A AU2006212459B2 AU 2006212459 B2 AU2006212459 B2 AU 2006212459B2 AU 2006212459 A AU2006212459 A AU 2006212459A AU 2006212459 A AU2006212459 A AU 2006212459A AU 2006212459 B2 AU2006212459 B2 AU 2006212459B2
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fraction
nitrogen
helium
rich
pure
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AU2006212459A1 (en
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Nikos Larass
Hans Schmidt
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Linde GmbH
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Linde GmbH
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/04—Purification or separation of nitrogen
    • C01B21/0405—Purification or separation processes
    • 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
    • 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
    • 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
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0053—Hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0078—Noble gases
    • C01B2210/0079—Helium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0078—Noble gases
    • C01B2210/0081—Neon
    • 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
    • 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
    • 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
    • F25J2205/80—Processes or apparatus using other separation and/or other processing means using membrane, i.e. including a permeation 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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/30—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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/32—Neon
    • 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
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • 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
    • F25J2280/00—Control of the process or apparatus
    • F25J2280/02—Control in general, load changes, different modes ("runs"), measurements

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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)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Description

Translation from German of PCT Application PCT/EP2006/000949 Method for separating trace 5 components from a stream that is rich in nitrogen The invention relates to a method for separating hydrogen, helium and/or neon from a liquid fraction that 10 is rich in nitrogen and has a pressure of at least 10 bar. From DE-A 101 06 484 there is a method known for the simultaneous recovery of a pure helium and a pure nitrogen fraction from a feed stream that contains at 15 least methane, nitrogen and helium. The citation of DE-A 101 06 484 is intended to include the entire content of that document in the disclosure of this patent application. It has been found that the feed stream containing 20 methane, nitrogen and helium, which is fed to a process as described in DE-A 101 064 84 - has significantly higher concentrations of the trace components argon, neon and hydrogen than previously assumed. Therefore, if by means of a process as described in DE-A 25 101 06 484, a gaseous nitrogen product stream hereinafter referred to as GAN product or GAN product stream - is to be recovered, this leads to the hydrogen contained in the feed gas concentrating primarily in this GAN product stream. Typically, the same purity 2 specifications apply for the purities of the liquid nitrogen product stream - hereinafter referred to as LIN product - and the GAN product stream; these can in fact be met in the LIN product stream but not in the GAN 5 product stream. A delivery of the GAN product stream in accordance with specifications is thus no longer possible with a method as described in DE-A 101 06 484. As known from the figure as well as the associated figure description of DE-A 101 06 484, the separation of the LIN 10 product stream in a recovery plant for helium and nitrogen usually takes place in a nitrogen/methane separation column in which the liquid nitrogen stream is drawn off in the upper part of the column via a riser base; see the figure of DE-A 101 06 484, in particular 15 separation column T and draw-off line 26. As explained based on the figure from DE-A 101 06 484, up to now this liquid nitrogen stream has been expanded and separated in a separator D3 into a pure nitrogen fraction and a gas fraction rich in nitrogen. After removal from the 20 separator, the former is supplied for its intended use such as coolant for helium liquefaction - while the nitrogen-rich gas fraction drawn from the head of the separator is warmed and subsequently vented to the atmosphere. 25 All non-condensable components as well as the remaining helium in the overhead product of the nitrogen/methane separation column T are returned to the process in the case of DE-A 101 06 484 in order to increase the helium yield. Hydrogen usually concentrates in the liquid in the 30 upper part of the nitrogen/methane separation column T. It is therefore drawn off from the column T via the side 3SXA774.I arm 26 together with the LIN stream. If the hydrogen concentration in the feed stream is greater than 100 ppmv, this results in a significant increase of the hydrogen concentration in the LIN stream drawn off the 5 separation column T via line 26. However, this is non-critical if the expansion of the LIN stream takes place in an atmospheric tank success, since in this case the hydrogen contained goes nearly completely into the gas phase and is released to the atmosphere via the pressure control of the tank. However, the substream of the LIN stream which is to be used as a GAN product stream still contains all the hydrogen, which results in the 10 maximum permitted concentration of non-inert components, such as hydrogen, oxygen, carbon monoxide, etc being exceeded in the GAN product stream. It is generally not possible to market such a product stream. In one embodiment the invention provides a method for the recovery of a pure helium 15 fraction and a pure nitrogen fraction from a feed stream containing at least methane, nitrogen, helium and hydrogen, which process comprises partially condensing the feed stream and separating into a helium-rich gas fraction and an initial nitrogen-rich liquid fraction; 20 feeding the helium-rich gas fraction to a subsequent purification stage in which a pure helium fraction is recovered by an adsorptive, permeative and/or rectification process, in which the helium-depleted fraction produced in the purification stage is re-combined with the feed stream; -4 separating the nitrogen-rich liquid fraction into a helium-depleted gas fraction, which is also re-introduced to the feed stream, and a second nitrogen-rich liquid fraction; and 5 feeding at least one substream of the second nitrogen-rich liquid fraction to a rectification process for recovery of a pure nitrogen fraction, wherein a nitrogen-rich liquid fraction (29) drawn from the rectification process for recovering a pure nitrogen fraction (T) is at least partially expanded (e) and subjected to 10 phase separation (D), with the expansion (e) being performed at a pressure conducive to a separation of hydrogen, helium and/or neon to residual levels below 20 ppmv, and wherein the hydrogen-rich gas fraction (30) recovered in the phase separation (D) is mixed with the expanded (f) sump product (20') from the rectification process for recovering a pure nitrogen fraction (T) and the mixed fraction (20) thus obtained is warmed to provide 15 cooling. In accordance with the invention, from now on the liquid nitrogen stream will be expanded at a pressure which facilitates a separation of the undesired trace components. The actual separation of the undesired trace components hydrogen, helium and/or neon then takes 20 place in the associated phase separation. These can subsequently be mixed with the sump product of the separation column, warmed and vaporised and delivered as a fuel gas at the battery limit.
15W,4774.1 -5 Now the LIN (product) stream from the phase separation meets the specifications for a GAN product stream and can thus, after warming at the battery limit, can be delivered at the desired pressure as a GAN product which meets specifications. 5 The inventive method for separating hydrogen, helium and/or neon as well as further embodiments of the same are explained in more detail below based on the embodiment depicted in the figure. 10 The figure here shows an excerpt from the figure of DE-A 101 06 484. The figure depicts the rectification column T, to which a nitrogen-rich liquid fraction is fed via lines 18 and 19. This fraction is warmed in the heat exchanger E4, partially vaporising it before it is fed to the separation column T; the feed takes place preferably - as shown in 15 the figure - in the area of the sump of the rectification column T. The rectification column T can have a condenser in the head section which, for example, is designed as a separate heat exchanger E5 or a wound heat exchanger. Furthermore, as also depicted in the figure, a nitrogen- 6 rich gas fraction can be drawn off from the rectification column T via line 23, partially condensed in the heat exchanger E5 and returned to the rectification column T. The head section of the rectification column T serves 5 here as a separator for the separation of a nitrogen-rich liquid fraction from the gas fraction drawn from the head of the rectification column T via line 24. The withdrawal of the pure liquid nitrogen fraction from the rectification column T takes place via line 26, with 10 this fraction then being expanded in a separator D3 via the valve d. The pure nitrogen fraction recovered is then fed from the sump of the separator D3 via line 28 for its downstream intended use, such as a coolant for helium liquefaction and/or dispensed as a saleable LIN product. 15 The pure nitrogen fraction recovered in this manner has a purity greater than 99.99%. A nitrogen-rich gas fraction is drawn off from the head of the separator D3 via line 27, mixed with the gas fraction from line 24 and warmed in the heat exchanger E4 20 - it is thus part of the utilisation of cold in the heat exchanger E4 - and subsequently vented to the atmosphere via line 25 and/or returned to the process (not shown in the figure). A substream of the pure liquid nitrogen fraction 25 withdrawn via line 26 is then, in accordance with the invention, expanded in valve e to a pressure which facilitates separation of the undesired trace components, i.e. hydrogen, helium and/or neon, enables and consequently allows the delivery of a GAN product stream 30 at the required pressure at the battery limit. This expanded fraction is fed to a separator D via line 29.
-7 At the head of the separator D the aforementioned trace components are concentrated, drawn off via line 30 and mixed in line 20 with the sump product 20' of the column T, which is preferably expanded to fuel gas pressure by means of the regulating stop valve f. Not shown in the figure is a warming of this (mixture) fraction 20 which provides cooling. 5 An LIN product stream is drawn from the sump of separator D via line 31 and the level regulating valve h, which, after warming in the heat exchanger E4, can be delivered via line 32 as a gaseous pure nitrogen or GAN product stream. 10 Corresponding to a further advantageous embodiment of the inventive method, the hydrogen-rich gas fraction 30 recovered in the phase separation D is subjected to pressure control g. By this means, the hydrogen content in the LIN product stream drawn from the separator D via line 3 1 can be selectively regulated and/or set. 15 Throughout this specification and the claims which follow, unless the context requires otherwise, the word "comprise", and variations such as "comprises" and "comprising", will be understood to imply the inclusion of a stated integer or step or group of integers or steps but not the exclusion of any other integer or step or group of integers or steps. 20 The reference in this specification to any prior publication (or information derived from it), or to any matter which is known, is not, and should not be taken as an acknowledgment or admission or any form of suggestion that that prior publication (or information derived from it) or known matter forms part of the common general knowledge in the field of endeavour to which this specification relates.

Claims (2)

1. A method for the recovery of a pure helium fraction and a pure nitrogen fraction from a feed stream containing at least methane, nitrogen, helium and hydrogen, which 5 process comprises partially condensing the feed stream and separating into a helium-rich gas fraction and an initial nitrogen-rich liquid fraction; feeding the helium-rich gas fraction to a subsequent purification stage in which a pure helium fraction is recovered by an adsorptive, permeative and/or rectification process, in which the helium-depleted fraction produced in the purification stage is re-combined 10 with the feed stream; separating the nitrogen-rich liquid fraction into a helium-depleted gas fraction, which is also re-introduced to the feed stream, and a second nitrogen-rich liquid fraction; and feeding at least one substream of the second nitrogen-rich liquid fraction to a 15 rectification process for recovery of a pure nitrogen fraction, wherein a nitrogen-rich liquid fraction (29) drawn from the rectification process for recovering a pure nitrogen fraction (T) is at least partially expanded (e) and subjected to phase separation (D), with the expansion (e) being performed at a pressure conducive to a separation of hydrogen, helium and/or neon to residual levels below 20 ppmv, and wherein 20 the hydrogen-rich gas fraction (30) recovered in the phase separation (D) is mixed with the expanded (f) sump product (20') from the rectification process for recovering a pure nitrogen fraction (T) and the mixed fraction (20) thus obtained is warmed to provide cooling.
150.,774.l1 -9 2. A method according to claim 1, wherein the nitrogen-rich liquid fraction (31) recovered in the phase separation (D) is vaporised (E4) to provide cooling. 3. A method according to claim I or claim 2, wherein the nitrogen-rich liquid fraction 5 (3 1) recovered in the phase separation (D) is delivered as a gaseous pure nitrogen product. 4. A method according to any one of the preceding claims, wherein the mixed fraction (20) is delivered as a fuel gas. 10 5. A method according to any one of the preceding claims wherein the hydrogen-rich gas fraction (30) recovered in the phase separation (D) is subjected to pressure control (g). 6. A method according to claim 1, substantially as hereinbefore described.
AU2006212459A 2005-02-11 2006-02-03 Method for separating trace components from a stream that is rich in nitrogen Ceased AU2006212459B2 (en)

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US10215488B2 (en) * 2016-02-11 2019-02-26 Air Products And Chemicals, Inc. Treatment of nitrogen-rich natural gas streams
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