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DE3668157D1 - Hybrid-membran/kryogenverfahren zur reinigung von wasserstoff. - Google Patents

Hybrid-membran/kryogenverfahren zur reinigung von wasserstoff.

Info

Publication number
DE3668157D1
DE3668157D1 DE8686111372T DE3668157T DE3668157D1 DE 3668157 D1 DE3668157 D1 DE 3668157D1 DE 8686111372 T DE8686111372 T DE 8686111372T DE 3668157 T DE3668157 T DE 3668157T DE 3668157 D1 DE3668157 D1 DE 3668157D1
Authority
DE
Germany
Prior art keywords
hybrid membrane
purifying hydrogen
cryogenic process
cryogenic
purifying
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
DE8686111372T
Other languages
English (en)
Inventor
Jeffrey Alan Hopkins
Stephen Paul Dimartino
David Michael Nicholas
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Products and Chemicals Inc
Original Assignee
Air Products and Chemicals Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=25084775&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=DE3668157(D1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Air Products and Chemicals Inc filed Critical Air Products and Chemicals Inc
Application granted granted Critical
Publication of DE3668157D1 publication Critical patent/DE3668157D1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • 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
    • F25J3/0219—Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/501—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/506—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification at low temperatures
    • 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
    • F25J3/0252—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 hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/046—Purification by cryogenic separation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C01B2203/047—Composition of the impurity the impurity being carbon monoxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C01B2203/048—Composition of the impurity the impurity being an organic compound
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C01B2203/0495—Composition of the impurity the impurity being water
    • 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
    • F25J2205/80—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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/04—Mixing or blending of fluids with the feed 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/12—Refinery or petrochemical off-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
    • 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
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/931—Recovery of hydrogen

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Hydrogen, Water And Hydrids (AREA)
DE8686111372T 1985-08-23 1986-08-18 Hybrid-membran/kryogenverfahren zur reinigung von wasserstoff. Expired - Lifetime DE3668157D1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US06/769,204 US4654047A (en) 1985-08-23 1985-08-23 Hybrid membrane/cryogenic process for hydrogen purification

Publications (1)

Publication Number Publication Date
DE3668157D1 true DE3668157D1 (de) 1990-02-15

Family

ID=25084775

Family Applications (1)

Application Number Title Priority Date Filing Date
DE8686111372T Expired - Lifetime DE3668157D1 (de) 1985-08-23 1986-08-18 Hybrid-membran/kryogenverfahren zur reinigung von wasserstoff.

Country Status (5)

Country Link
US (1) US4654047A (de)
EP (1) EP0213525B1 (de)
JP (1) JPS6249927A (de)
CA (1) CA1272119C (de)
DE (1) DE3668157D1 (de)

Families Citing this family (44)

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US4749393A (en) * 1987-09-18 1988-06-07 Air Products And Chemicals, Inc. Process for the recovery of hydrogen/heavy hydrocarbons from hydrogen-lean feed gases
US4960579A (en) * 1988-04-01 1990-10-02 Union Carbide Corporation Membrane process and system for nitrogen production
JPH0635170Y2 (ja) * 1988-07-28 1994-09-14 三菱重工業株式会社 壜検査装置
FR2636341A1 (fr) * 1988-09-12 1990-03-16 Air Liquide Procede et installation de recuperation des hydrocarbures les plus lourds d'un melange gazeux
FR2636250B1 (fr) * 1988-09-12 1992-01-17 Air Liquide Procede et installation de recuperation d'hydrogene et de monoxyde de carbone
FR2636249B1 (fr) * 1988-09-12 1992-05-15 Air Liquide Procede et installation de recuperation d'hydrogene
US4957513A (en) * 1989-05-10 1990-09-18 Raytheon Company Method of purifying a mixed H2 /H2 Se vapor stream
US4934148A (en) * 1989-05-12 1990-06-19 Union Carbide Corporation Dry, high purity nitrogen production process and system
US5116396A (en) * 1989-05-12 1992-05-26 Union Carbide Industrial Gases Technology Corporation Hybrid prepurifier for cryogenic air separation plants
US4941893B1 (en) * 1989-09-19 1996-07-30 Advanced Silicon Materials Inc Gas separation by semi-permeable membranes
US4952219A (en) * 1989-09-29 1990-08-28 Air Products And Chemicals, Inc. Membrane drying of gas feeds to low temperature units
US4936887A (en) * 1989-11-02 1990-06-26 Phillips Petroleum Company Distillation plus membrane processing of gas streams
US5082481A (en) * 1990-04-10 1992-01-21 Lummus Crest, Inc. Membrane separation process for cracked gases
US5006132A (en) * 1990-06-12 1991-04-09 Air Products And Chemicals, Inc. Membrane processed purified pipeline gas
US5077029A (en) * 1990-07-23 1991-12-31 Union Carbide Industrial Gases Technology Corporation Membrane/deoxo control method and system
US5071451A (en) * 1990-12-28 1991-12-10 Membrane Technology & Research, Inc. Membrane process and apparatus for removing vapors from gas streams
US5147550A (en) * 1990-12-28 1992-09-15 Membrane Technology And Research, Inc. Membrane process and apparatus for removing a component from a fluid stream
US5100446A (en) * 1991-01-07 1992-03-31 Union Carbide Industrial Gases Technology Corporation Crude neon production system
US5352272A (en) * 1991-01-30 1994-10-04 The Dow Chemical Company Gas separations utilizing glassy polymer membranes at sub-ambient temperatures
US5837032A (en) * 1991-01-30 1998-11-17 The Cynara Company Gas separations utilizing glassy polymer membranes at sub-ambient temperatures
US5129921A (en) * 1991-05-30 1992-07-14 Membrane Technology & Research, Inc. Membrane gas separation process and apparatus
GB2274253B (en) * 1993-01-14 1997-04-16 Boc Group Plc Gas separation apparatus
IL106909A0 (en) * 1993-09-05 1993-12-28 Rotem Ind Ltd Method for improving the efficiency of cryogenic-membrane separation hybrids
US5452581A (en) * 1994-04-01 1995-09-26 Dinh; Cong X. Olefin recovery method
US5634354A (en) * 1996-05-08 1997-06-03 Air Products And Chemicals, Inc. Olefin recovery from olefin-hydrogen mixtures
US5955044A (en) * 1997-09-30 1999-09-21 Johnson Matthey Inc. Method and apparatus for making ultra-pure hydrogen
US6179900B1 (en) * 1997-10-09 2001-01-30 Gkss Forschungszentrum Geesthacht Gmbh Process for the separation/recovery of gases
WO1999067587A1 (en) * 1998-06-25 1999-12-29 Process Systems International, Inc. Cryogenic and membrane synthesis gas production
FR2780391B1 (fr) * 1998-06-26 2000-10-20 Air Liquide Procede de production de monoxyde de carbone
US6161397A (en) * 1998-08-12 2000-12-19 Air Products And Chemicals, Inc. Integrated cryogenic and non-cryogenic gas mixture separation
US6475655B1 (en) * 1999-06-23 2002-11-05 Daihatsu Motor Co., Ltd. Fuel cell system with hydrogen gas separation
JP2001062240A (ja) * 1999-08-27 2001-03-13 Air Liquide Japan Ltd 混合ガスの濃度調整方法および濃度調整装置
CA2469153C (en) * 2001-12-18 2008-03-04 Fluor Corporation Combined recovery of hydrogen and hydrocarbon liquids from hydrogen-containing gases
JP5102932B2 (ja) * 2004-01-29 2012-12-19 Ｊｘ日鉱日石エネルギー株式会社 高純度水素製造方法
JP5406441B2 (ja) * 2007-09-07 2014-02-05 日本エア・リキード株式会社 ガス成分および凝縮性成分の製造方法および製造装置
JP2009061420A (ja) * 2007-09-07 2009-03-26 Air Liquide Japan Ltd ガス成分および凝縮性成分の製造方法および製造システム
US20090165646A1 (en) * 2007-12-31 2009-07-02 Sarang Gadre Effluent gas recovery process for silicon production
US20100037655A1 (en) * 2008-08-13 2010-02-18 Air Liquide Process And Construction Inc. Hydrogen Recovery From A Mixture Of Hydrogen and Hydrocarbons At Low Pressure And Of Low Hydrogen Content
US8187361B2 (en) * 2009-07-02 2012-05-29 America Air Liquide, Inc. Effluent gas recovery system in polysilicon and silane plants
US8495882B2 (en) * 2009-08-10 2013-07-30 General Electric Company Syngas cleanup section with carbon capture and hydrogen-selective membrane
DE102010047543A1 (de) * 2010-10-05 2012-04-05 Linde Ag Abtrennen von Wasserstoff
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WO2020059301A1 (ja) * 2018-09-20 2020-03-26 パナソニックＩｐマネジメント株式会社 水素純化器およびその運転方法
CN115999328B (zh) * 2021-10-22 2025-03-28 中国石油化工股份有限公司 膜分离结合精馏制备乙烯的方法和系统

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Also Published As

Publication number Publication date
EP0213525A1 (de) 1987-03-11
JPS6249927A (ja) 1987-03-04
EP0213525B1 (de) 1990-01-10
CA1272119A (en) 1990-07-31
US4654047A (en) 1987-03-31
CA1272119C (en) 1990-07-31

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