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'US 2009001 cu») United States cz) Patent Application Publication co) Pub. No.: US 2009/0013718 Al oy os) om an @ (66) Schmidt METHOD FOR THE SIMULTANEOUS: RECOVERY OF A PURE HELIUM AND PURE NITROGEN FRACTION Inventor, (or sal CComespondenee Address CROWELL & MORING LLP INTELLECTUAL PROPERTY GROUP. P.O. BOX 14300 WASHINGTON, DC 20044-4300 (US) Assignee: LINDE AKTIENGESELLSCHAFT, ‘Wiesbaden (DE) Appl. No, 110817,369 PCT Filed Feb. 28, 2006 PCT No, PCTEPOGOISI8 §371 (0,0), (2),(4)Date Sep. 18,2008, SA STI (43) Pub, Date Jan. 15, 2009 G0) Foreign Application Priority Data Mar 4,2005 (DE) 10 2008 010054. Publication Classification G1) Ine F254 302 Cor 21704 (2006.01), (2006.01), (2) Us.CL 621639; 428/285 on ABSTRACT A process for simultaneous recovery ofa pure helium and a pure nitrogen fraction from a feed stream containing atleast ‘ethane, nitrogen and helium, i disclosed. The fox stream is partially condensed and separated into heliumerich gas fraction anda niteogen- and methane-rich liquid fraction. The heliun-rich gas fraction is conveyed to a purification stage in whieh a pure helium Traction is recovered by adsorption, permeation andor rectification, At least one partial stream of the nitrogen and methane-rich liquid fraction is taken to & retification process for recovery of a pure nitrogen fraction. Patent Application Publication Jan. 15, 2009 US 2009/0013718 AI 4" a Fig. US 2009/0013718 Al METHOD FOR THE SIMULTANEOUS. RECOVERY OF A PURE HELIUM AND PURE ‘NITROGEN FRACTION 10001] This application claims the priority of International Application No. PCT'EP2006001818, filed Feb. 28, 2006, ‘and Gennan Patent Document No. 10 2008 010 054.6, fled Mat. 4, 2005, the disclosures of which aro expressly incorpo- rated By reference herein, BACKGROUND AND SUMMARY OF THE INVENTION 10002] The invention elates to a process forthe simulta- neous recovery ofa pure helium and pure nitrogen fraction froma feed stream containing at lest melbane, nitrogen and helium. [0003] Helium is normally recovered in large quantities from natural gas or ffom natural gas factions such as ‘acerte for example in what age known as LNG baseload plants from a gas mixture consisting then essentially of ‘ethane, nitrogen and hydrogen. gas mixture ofthis Kind, shih is drawn oft from a medium-pressure separator before the LNG storage tank, has for example, the following typical ‘composition: 60% methane (CH,), 38% nitrogen (N,) and 5°% helium (He). 10004) Saaler amounts of helium cam also be separated and recovered from air in eryogenc air fractionation plantsby cans of what ie known is ow-temperatre ie fractionation. 10005] For storage and transport particularly ever longer distances the helium recovered is sonal lguelied. This procedure in addition to the smaller storage or tank volume euired for the elium, asthe advantage tht at the eonsum- ssi in addition tothe helium itself its coldness andlor its Tow temperature can be used as well 10006) 1th helium is recovered by using low-temperature ‘echinology the obvious thing is o separate the nitrogen con- tained i the ra gas atleast vo Fiquely it partially and to use itasreffigerant for pre-cooling in te helium liquefaction 10007} Liquid nitrogen is frequently generated by means of a separate cryogenic ar fractionation plant for useas a refrig= ‘rant in helium liquefaction. The distdvantage of eryogenic ‘extricton of nitrogen from airs that thes to he fractionated in adsorbers has to be freed from components which are troublesome in eryogenicairfactionation, such as steam or ‘carbon dioxide, before itis conveyed to eryogenie air frac 10008] From German patent application 101 06 484 @ _generie process isknown for the simultaneous extraction of a Pure helium and a pure nitrogen fraction froma feed stream ‘containing at least methane, nitrogen and helium. In this process, the fed steam i initially partially condensed and Separated into a heliumrich gas fraction and frst nitrogen- rich liguid fraction, While the helivin-tich pas Traction is taken to a post-purfication stage, in which a pure helium fraction is recovered by an adsorption, permeation andor rectification process, the first nitrogen-rich igui fraction is separated into a helium-deplted gas fraction which i like- ‘wise again retumed to the feed stream and into a second nitegen-rich lguid fraction, This latter is then conveyed to @ reclification process to recover purenitiogen fraction Refer ‘nparticular to theonly drawing from DE-A 101 06484, With Jan. 15, 2009 the citation of DE-A 101 06 484, its content is hereby incor porated by reference herein into the present patent applica- ‘ie, [0009] Disadvantapeous in the procedure described in DE-A 101 06 484 is that it requires « comparatively lange expenditure for equipment; for example, for the eoluma \whieh serves to recover the pure nitrogen fraction atleast wo separators are located upstream. Furthermore the control bility of the separation column is limited sinee only one feed stream s brought to the column. In addition, the refrigeration performance of the process isnot used optimally in thecental hat exchanger. [0010] ‘The object ofthe present invention isto specify & szencric process for the simultancous recovery of @ pure hoelium and a pure nitrogen fraction from a feed steam con- ‘wining atleast methane, nitrogen and helium whieh avoids the aforementioned disadvantages, [0011] To achieve this objective a generic process is pro- posed in whieh [0012] the feed stream is partially condense andl separated into a heliumrieh gos fraction an nitrogen- and methne- ch Mid fraction, [0013] the hetium-rich pas faction is conveyed to a purifl- ‘ation stage in which s pure helm fraction is obtained by an adsorption, permeation andor rectification proces, and [0014] atleast a partial stream ofthe nitrogen and meth- fne-rich liquid fraction is conveyed toa rectification process to recover a pure nitrogen faction, [0015] In contrast othe process described in DE-A 101 06 484, the second separator can now bedispensed with in aceor- ‘dance with the invention sine the Figuid fraction obsained ia the parial condensation is taken atleast panally det to the Fctfiation process to reeaver the pure nitrogen fraction, [0016] Further developing the process in accordance with the iaventon, sts provided that least partial steam ofthe nitrogen-rich liquid fraction is expand, heated and eon- ‘dense countercurrent tthe feed steam tobe condensed an {ollowing re-compression, admixed tothe feed stream prior to condensing the latter 0017] This recirculation of atleast a partial steam of the niteogen-rich guid fraction results ina higher specifi elig- craton performance, The result of this is that the volume recitculated into the feed steam is reduced and consequently the eireulaton compressor, if needed, can havea lower shalt output. [0018] | Anaddtitionat advantageous embodiment ofthe pro- ‘ess in accordance with the invention is characterized in that at east one paral steam ofthe niteogen-rich liquid faction is expanded, heated aa taken to the rectification process to recover the pure nitrogen fraction through its reboier. 0019} By means of tis process, compared with the pro- ‘ess deseribed in DE-A 101 06 484, optimized contro is achieved of the product specifications of the column for the recovery ofthe pure nitrogen fraction. [0020] Furthermore, the pure nitrogen faction obtained in the rectification process for recovery of the pure nitrogen is preferably supercooled in aeordance witha further advan {Bonus embodiment ofthe process, [0021] This embodiment makes particular sense when this pure trogen faction isto be ced toa storage presse — {or example for stomge in an atmospheric nitrogen tank — since the nitrogen Hash gas losses can be drastically reduced US 2009/0013718 Al by means of the aforementioned procedre. As a con quence, the product volume of the liguid nitrogen is, increased 10022] |The process in accordance with the invention and ditional embodiments are explained in what follows using the embodiments shown i the drawing, BRIEF DESCRIPTION OF THE DRAWING 10023] The FIGURE illustrates an embodiment of the present invention, DETAILED DESCRIPTION OF THE DRAWING 10024} The feed stream containing atleast methane, nitto- ten and helium is taken va Fine Ito heat exchanger F, which Js preferably configured asa plate heat exchanger, and parr tally condensed therein. Notshown ia the drawing sa sinigle- ‘or multiple-stage compression of this feed stream: in this respec, reference is made to the corresponding explanations jn DE-A 101 06 484, in particular the drawing and the description ofthe dawing. The feed stream Tis ata pressure bperween 15 and 30 bar following compression, 10025] Also not shown in the drawing is an open expander

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