• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
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    • 专利摘要:
    Abstract Process for obtaining a pure helium fraction A process is described for obtaining a pure helium fraction from a starting fraction comprising at least helium, methane and nitrogen. According to the invention, a) the starting fraction (1) is subjected to an N2/CH4 removal (A), b) the fraction (2) which comprises essentially helium and nitrogen and is obtained in the N2/CH4 removal (A) is compressed (B), 10 c) the compressed fraction (3) is subjected to an N2 removal (D), and d) the helium-rich fraction (6) obtained in the N2 removal (D) is subjected to an adsorptive purification process (E) in which the pure helium fraction (7) is obtained. (This refers to Figure 2)
    公开号:AU2013200075A1
    申请号:U2013200075
    申请日:2013-01-04
    公开日:2013-07-18
    发明作者:Heinz Bauer；Andreas Bub；Martin Gwinner；Said Al Rabadi
    申请人:Linde GmbH；
    IPC主号:F25J3-00
    专利说明:
    - 1 AUSTRALIA PATENTS ACT 1990 COMPLETE SPECIFICATION FOR A STANDARD PATENT ORIGINAL Name of Applicant: Linde Aktiengesellschaft Actual Inventors: Heinz Bauer and Martin Gwinner and Andreas Bub and Said Al Rabadi Address for Service is: SHELSTON IP 60 Margaret Street Telephone No: (02) 9777 1111 SYDNEY NSW 2000 Facsimile No. (02) 9241 4666 CCN: 3710000352 Attorney Code: SW Invention Title: Process for obtaining a pure helium fraction The following statement is a full description of this invention, including the best method of performing it known to me/us: File: 77456AUPOO 2 Description Process for obtaining a pure helium fraction The invention relates to a process for obtaining a pure helium fraction from a starting fraction comprising at least helium, methane and nitrogen. 5 Helium is commercially obtained virtually exclusively from a mixture of volatile natural gas components, this mixture comprising, as well as helium, typically methane and nitrogen, and traces of hydrogen, argon and other noble gases. Helium collects with other gases in underground structures of sufficient gas-tightness. In the course of 10 production of mineral oil, helium is made available as a component of the gas which accompanies the mineral oil, or in the course of production of natural gas. It is theoretically possible to obtain helium from the atmosphere, but this is uneconomic due to low concentrations. 15 In order to avoid unwanted freezing during a helium liquefaction process, the concentration of impurities in the helium stream to be liquefied must not exceed a value of 1000 ppmv, preferably 10 ppmv. For this reason, the helium liquefaction process is connected downstream of a helium purification process. The latter consists typically of a combination of cryogenic processes, generally based on partial condensation, and 20 adsorptive processes, the regeneration in the case of the latter being possible through pressure and/or temperature swing. In many cases, it is advantageous to design the helium purification process such that, as well as the purified helium, nitrogen of technical grade purity - wherein the sum of 25 impurities is less than 100 ppmv, preferably less than 10 ppmv - can be obtained. In order to be able to release nitrogen in the desired purity, however, an N 2
    /CH
    4 separation additionally has to be provided. In general, only a portion, typically 5 to 70%, preferably 10 to 50%, of the nitrogen present in the mixture to be purified is brought to 30 high purity. The remaining nitrogen is released to the atmosphere together with methane as a low-pressure gas, either directly or after an oxidation step, preferably implemented in a flare or an incinerator. If the methane content in this N 2
    /CH
    4 fraction 3 is at least 10% by volume, it can also be released as fuel gas and/or be supplied to a methane recovery. The working example shown in Figure 1 illustrates a generic process for obtaining a 5 pure helium fraction from a starting fraction comprising at least helium, methane and nitrogen. In this process, the starting fraction 100 is first subjected to a compression A' to a pressure between 20 and 40 bar. The compressed starting fraction 101 is then, 10 provided that it comprises hydrogen, subjected to a preferably catalytic hydrogen removal B'. The starting fraction 102 thus prepurified is then supplied to a cryogenic nitrogen removal C'. From this, an N 2
    /CH
    4 -rich fraction is drawn off via line 106 and is subjected to a cryogenic N 2
    /CH
    4 removal E'. From this, an N 2
    /CH
    4 -rich fraction is drawn off via line 107 and a nitrogen fraction via line 108, the latter generally having a sum of 15 impurities of less 100 ppmv, preferably less than 10 ppmv. The helium-rich fraction 103 obtained in the cryogenic nitrogen removal C' is subjected to an adsorptive purifying process D'. This process may be a TSA process, a PSA process, a VPSA process or a combination of the aforementioned processes. Via line 20 104, the pure helium fraction obtained therein is drawn off and supplied to the further use thereof, for example a liquefaction. The residual gas fraction 105 obtained in the adsorption process D' can be added to the starting fraction 100. It is an object of a preferred embodiment of the present invention to specify a generic 25 process for obtaining a pure helium fraction which has lower capital and operating costs. Any discussion of the prior art throughout the specification should in no way be considered as an admission that such prior art is widely known or forms part of 30 common general knowledge in the field. It is an object of the present invention to overcome or ameliorate at least one of the disadvantages of the prior art, or to provide a useful alternative.
    4 To address this problem, a process is proposed for obtaining a pure helium fraction from a starting fraction comprising at least helium, methane and nitrogen, wherein a) the starting fraction is subjected to an N 2
    /CH
    4 removal, b) the fraction which comprises essentially helium and nitrogen and is obtained in the 5 N 2
    /CH
    4 removal is compressed, c) the compressed fraction is subjected to an N 2 removal, and d) the helium-rich fraction obtained in the N 2 removal is subjected to an adsorptive purification in which the pure helium fraction is obtained. 10 Unless the context clearly requires otherwise, throughout the description and the claims, the words "comprise", "comprising", and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is to say, in the sense of "including, but not limited to". 15 Further advantageous configurations of the process according to the invention for obtaining a pure helium fraction, which are the subject matter of the dependent claims, are characterized in that - the compressed fraction is subjected to an H 2 removal prior to supply to the N 2 20 removal, - the fraction which comprises essentially helium and nitrogen and is obtained in the N 2
    /CH
    4 removal is compressed to a pressure between 15 and 35 bar, preferably between 20 and 25 bar, 25 - the adsorptive purifying process is designed as a TSA, PSA or VPSA process, - the N 2
    /CH
    4 removal is implemented by means of a wash, to which liquefied nitrogen which is obtained in the N 2 removal is preferably supplied as reflux, 30 and/or - the wash is preferably operated at a pressure of 1.2 to 5 bar, preferably of 1.5 to 2 bar. 35 5 The process according to the invention for obtaining a pure helium fraction is explained in detail hereinafter with reference to the working example shown in Figure 2. The starting fraction 1 comprising at least helium, methane and nitrogen is, in 5 accordance with the invention, first subjected to an N 2
    /CH
    4 removal A. The N 2
    /CH
    4 -rich fraction obtained is drawn off via line 10. The N 2
    /CH
    4 removal A is preferably implemented by means of a wash or by a wash column. This is supplied with the starting fraction 1 at the bottom. Liquefied nitrogen (9) which is obtained in the N 2 removal (D) yet to be described is preferably applied as reflux to the top of the wash 10 column. The wash column is preferably operated at a pressure of 1.2 to 5 bar, especially of 1.5 to 2 bar. In addition, the wash column is operated at a temperature corresponding to the boiling temperature of nitrogen within the pressure range specified (-195 to -185'C). 15 The fraction 2 which comprises essentially helium and nitrogen and is obtained in the
    N
    2
    /CH
    4 removal A is subsequently supplied to a compression unit B. Compression is effected therein to a pressure between 15 and 35 bar, preferably between 20 and 25 bar. 20 If the starting fraction 1 or 2 comprises hydrogen, a preferably catalytic hydrogen removal unit C to which the compressed fraction 3 is supplied should be provided. The fraction 4 treated in the hydrogen removal unit C is then subjected to a preferably cryogenic nitrogen removal D. From this, a nitrogen-rich fraction is drawn off via line 5 and optionally supplied to the further use thereof, for example in helium precooling prior 25 to liquefaction and in employment in the radiation shield of liquid helium tanks. The helium-rich fraction 6 obtained in the nitrogen removal D is subjected to an adsorptive purifying process E, from which the pure helium fraction obtained is drawn off via line 7. In the case of the inventive process regime too, the residual gas fraction 8 30 obtained in the adsorptive purifying process E can be supplied to the starting fraction, in which case, however, it is now supplied to the fraction 2 which has already been substantially freed of methane and nitrogen. In contrast to the procedure described with reference to Figure 1, in the case of the 35 process according to the invention, a pure helium fraction is obtained by purifying the 6 starting fraction, prior to the compression thereof, to very substantially free it of methane, any further high boilers present and a majority of the nitrogen, typically 10 to 90%, preferably 30 to 80%. Only the remaining fraction comprising essentially helium and nitrogen is compressed to 15 to 35 bar, preferably 20 to 25 bar. In this case, a 5 methane content of the compressed fraction of < 100 ppmv, preferably < 10 ppmv, is established. The early removal of the N 2
    /CH
    4 fraction reduces the burden on the downstream process steps. Even though two independent (cryogenic) removal steps are now 10 required, the capital and operating costs are lowered. Moreover, the further removal of combustible components considerably lowers the safety requirements (for example explosion protection) in the downstream process steps. The nitrogen obtained in the N 2 removal (D) fulfils the typical purity demands - this 15 means that the sum of impurities is 5100 ppmv, preferably 10 ppmv - which are made on liquefied nitrogen which finds use in a helium plant. The liquefied nitrogen may find use, for example, in helium precooling prior to liquefaction and in employment in radiation shields of liquid helium tanks.
    权利要求:
    Claims (11)
    [1] 1. A process for obtaining a pure helium fraction from a starting fraction comprising at least helium, methane and nitrogen, wherein a) the starting fraction is subjected to an N 2 /CH 4 removal, 5 b) the fraction which comprises essentially helium and nitrogen and is obtained in the N 2 /CH 4 removal is compressed, c) the compressed fraction is subjected to an N 2 removal, and d) the helium-rich fraction obtained in the N 2 removal is subjected to an adsorptive purification process in which the pure helium fraction is obtained. 10
    [2] 2. A process according to Claim 1, wherein the compressed fraction is subjected to an H 2 removal prior to supply to the N 2 removal.
    [3] 3. A process according to Claim 1 or claim 2, wherein the fraction which comprises 15 essentially helium and nitrogen and is obtained in the N 2 /CH 4 removal is compressed to a pressure between 15 and 35 bar.
    [4] 4. A process according to claim 3 wherein the fraction which comprises essentially helium and nitrogen and is obtained in the N 2 /CH 4 removal is compressed to a 20 pressure between 20 and 25 bar.
    [5] 5. A process according to any one of the preceding Claims 1 to 4, wherein the adsorptive purifying process is designed as a TSA, PSA or VPSA process. 25
    [6] 6. A process according to any one of the preceding Claims 1 to 5, wherein the N 2 /CH 4 removal is implemented by means of a wash, to which liquefied nitrogen which is obtained in the N 2 removal is preferably supplied as reflux.
    [7] 7. A process according to Claim 6, wherein the wash is operated at a pressure of 30 1.2 to 5 bar.
    [8] 8. A process according to Claim 7, wherein the wash is operated at a pressure of 1.5 to 2 bar. 8
    [9] 9. A pure helium fraction obtained by the process according to any one of claims 1 to 8.
    [10] 10. A process for obtaining a pure helium fraction from a starting fraction 5 substantially as herein described with reference to any one of the embodiments of the invention illustrated in the accompanying drawings and/or examples.
    [11] 11. A pure helium fraction obtained by the process substantially as herein before described with reference to any one of the embodiments of the invention 10 illustrated in the accompanying drawings and/or examples.
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    同族专利:
    公开号 | 公开日
    RU2573083C2|2016-01-20|
    RU2012157331A|2014-07-10|
    DE102012000147A1|2013-07-11|
    AU2013200075B2|2018-01-04|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO2016174317A1|2015-04-30|2016-11-03|L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude|Production of helium from a gas stream containing hydrogen|US4238211A|1978-11-20|1980-12-09|Helix Technology Corporation|Method of employing a first contaminant to prevent freeze-out of a second contaminant during cryogenic processing of a gaseous stream|
    DE10106484A1|2001-02-13|2002-08-14|Linde Ag|Simultaneous recovery of helium and nitrogen pure fractions from process stream containing methane, nitrogen and helium, involves partially condensing process stream, and further processing|
    US7201019B2|2004-11-19|2007-04-10|Praxair Technology, Inc.|Light gas component separation from a carbon dioxide mixture|
    DE102005010053A1|2005-03-04|2006-09-07|Linde Ag|Helium recovery in LNG plants|
    DE102005010054A1|2005-03-04|2006-09-07|Linde Ag|Process for simultaneously recovering a helium and a nitrogen pure fraction|US10962283B2|2018-09-13|2021-03-30|Air Products And Chemicals, Inc.|Helium extraction from natural gas|
    法律状态:
    2018-05-10| FGA| Letters patent sealed or granted (standard patent)|
    优先权:
    申请号 | 申请日 | 专利标题
    DE102012000147.9||2012-01-05||
    DE102012000147A|DE102012000147A1|2012-01-05|2012-01-05|Method for obtaining a helium pure fraction|
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