WO1999042773A1 - Purification de l'air avec des regenerateurs et lit adsorbant pour l'eau - Google Patents

Purification de l'air avec des regenerateurs et lit adsorbant pour l'eau Download PDF

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Publication number
WO1999042773A1
WO1999042773A1 PCT/EP1999/001127 EP9901127W WO9942773A1 WO 1999042773 A1 WO1999042773 A1 WO 1999042773A1 EP 9901127 W EP9901127 W EP 9901127W WO 9942773 A1 WO9942773 A1 WO 9942773A1
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WO
WIPO (PCT)
Prior art keywords
regenerators
air
low
water
temperature
Prior art date
Application number
PCT/EP1999/001127
Other languages
German (de)
English (en)
Inventor
Wilhelm Rohde
Original Assignee
Linde Aktiengesellschaft
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
Priority claimed from DE19807225A external-priority patent/DE19807225A1/de
Application filed by Linde Aktiengesellschaft filed Critical Linde Aktiengesellschaft
Priority to AU29277/99A priority Critical patent/AU2927799A/en
Publication of WO1999042773A1 publication Critical patent/WO1999042773A1/fr

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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
    • F25J3/04—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 for air
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04163—Hot end purification of the feed air
    • F25J3/04169—Hot end purification of the feed air by adsorption of the impurities
    • 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
    • B01D53/02—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 adsorption, e.g. preparative gas chromatography
    • B01D53/04—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 adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • 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
    • B01D53/26—Drying gases or vapours
    • B01D53/261—Drying gases or vapours by adsorption
    • 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
    • F25J3/04—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 for air
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04163—Hot end purification of the feed air
    • 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
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40001—Methods relating to additional, e.g. intermediate, treatment of process gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
    • B01D2259/40086—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by using a purge gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/416—Further details for adsorption processes and devices involving cryogenic temperature treatment
    • 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
    • F25J2205/24—Processes or apparatus using other separation and/or other processing means using regenerators, cold accumulators or reversible heat exchangers
    • 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
    • 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 method for the low-temperature decomposition of air, in which in at least one switchable pair of regenerators a partial stream or the entire air stream to be split is cooled by heat exchange with a part of the decomposition products, contaminants condensing out, after which the cleaned air stream is fed to the low-temperature drop.
  • the invention further relates to a device for performing the method according to the invention.
  • cryogenic air separation - hereinafter referred to as low-temperature separation - the air is first cooled to approximately cooling water temperature and then to approx. 15 ° C, then adsorptively dried and freed of carbon dioxide - preferably using a moister sieve - and then in plate heat exchangers cooled to liquefaction temperature against escaping products and residual gas (s).
  • the plate heat exchangers used for this can only be manufactured up to a certain size; If the air volume is large enough, several heat exchangers must be connected in parallel.
  • regenerators came for the heat exchange between air and waste products for use. These were preferably arranged in pairs.
  • the air cools down on the heat storage mass of the regenerator, the disruptive components to be removed, such as water and carbon dioxide, being eliminated liquid or solid.
  • the storage mass of the regenerator slowly warms up.
  • the decomposition products from the cryogenic air separation are warmed up and carry the previously separated air contaminants out of the regenerator.
  • the decomposition products release their cold to the storage mass of the regenerator.
  • the regenerators are switched over at periodic intervals, so that the air flows in through the regenerator previously cooled with decomposition products and the decomposition products through the one previously operated with decomposition air
  • regenerators with tube spirals for pure oxygen consisted of quartzite stones, for oxygen of lower purity from so-called aluminum trays; these are spirally wound, corrugated aluminum strips.
  • Regenerators with quartzite filling and pipe spirals have a not insignificant empty volume, which is why the compressed air stored in them is partially lost with every switching operation, which leads to a deterioration in the yield.
  • DE 27 34 934 A1 discloses a method and a device for the low-temperature separation of air, wherein in at least one switchable pair of regenerators, part of the air to be separated is cooled by heat exchange with a part of the separation products, while the rest of the air to be decomposed is purified by adsorption and cooled in a heat exchanger by heat exchange with another part of the decomposition products. Then both air flows are fed to the cryogenic decomposition. It can thus be implemented a procedure in which only that portion of the air to be broken down is adsorptively freed of water and carbon dioxide, which is used for heating the z. B. 100,000 Nm 3 / h of product oxygen is required.
  • a disadvantage of the method and the device according to DE 27 34 934 A1 is that a large heat storage capacity must be available for the condensation of water. On the one hand, this requirement causes higher investment costs and, on the other hand, leads to higher air switching losses being accepted, in particular because of the larger regenerator volume have to. This has a not inconsiderable impact on the energy consumption of the cutting plant.
  • the object of the present invention is to provide a method and a device for the low-temperature separation of air which, compared to the known methods and devices for low-temperature separation of air, enable a reduction in costs and energy.
  • water is separated off from the air flow passed through the pair of regenerators before the further contaminants, such as e.g. B. carbon dioxide, by means of adsorption.
  • the device according to the invention is therefore characterized in that the regenerators have an adsorption bed arranged in their inlet region.
  • the heat exchange of the air flow conducted through the regenerators takes place exclusively against an impure nitrogen flow from the low-temperature separation. Because of this procedure, the regenerators used can be comparatively simple; at least the provision of tube bundles in the storage mass of the regenerators can be dispensed with.
  • the method according to the invention for the low-temperature decomposition of air is proposed that a partial flow of the air to be separated, which is not fed to the regenerators, is freed of impurities by means of adsorption and then cooled in indirect heat exchange with a decomposition product to be heated.
  • At least 50 to 85% of the amount of air supplied to the cryogenic decomposition is passed through the regenerators. Since - as already mentioned at the beginning - for the production of 100,000 Nm 3 / h of product oxygen, almost 500,000 NnrvVh of air have to be fed to the low-temperature decomposition, and 400,000 Nm 3 / h of residual gas - i.e. impure nitrogen - are generated, this has
  • a further advantageous embodiment of the method according to the invention for the low-temperature separation of air is characterized in that the adsorptive separation of water from the air flow led through the regenerators is integrated into the regenerators.
  • the regenerators can be preceded by a separate adsorber in which the adsorptive separation of water takes place.
  • the adsorbent layer required for the adsorptive separation of the water is advantageously integrated into the regenerator itself, preferably in its inlet area.
  • the method according to the invention for the low-temperature decomposition of air is proposed that the regeneration of the adsorption agent loaded with water takes place by rinsing the adsorption agent.
  • an impure nitrogen stream from the low-temperature decomposition is preferably used as the purge gas.
  • a so-called heatless regeneration of the adsorbent layer can be achieved with the purge gas quantity passed through the regenerator for the purpose of regeneration.
  • the amount of purge gas - ie the amount of impure nitrogen - is approximately equal to the amount of air to be cooled in the regenerators, it is sufficient if a relatively short adsorbent layer, e.g. B. an aluminum layer is provided, by means of which the air is cooled, for example, to a dew point of 5 ° C. This ensures that no drop-shaped water forms on the trays or beds of the regenerators. If the aforementioned heatless regeneration is also implemented, this leads to the regenerators being even more compact, since no heating surfaces and heat capacities for water condensation and re-evaporation have to be provided.
  • a relatively short adsorbent layer e.g. B. an aluminum layer
  • the device according to the invention for performing the method according to the invention is characterized in that the regenerators have an adsorption bed arranged in the inlet region.
  • this consists of a water-adsorbing adsorbent. Depending on the choice of the adsorbent used, it can - apart from water - remove other components from the air flow to be separated.
  • regenerators contain steel trays and / or a steel bed as a heat-storing material. These steel trays or steel fillings - those instead of aluminum trays or quartzite stones
  • the steel or aluminum trays have a width of 30 to 500 mm.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

L'invention concerne un procédé pour la séparation à basse température de l'air, selon lequel un flux partiel ou bien le flux d'air entier à séparer est refroidi dans au moins une paire de régénérateurs réversibles, par échange de chaleur avec une partie des produits de séparation, les impuretés étant éliminées par condensation. Le flux d'air ainsi purifié est ensuite soumis à une séparation à basse température. L'invention concerne également un dispositif permettant la mise en oeuvre de ce procédé, comportant au moins une paire de régénérateurs réversibles et dans lequel la conduite d'admission d'air est reliée aux régénérateurs. De l'eau est séparée, par adsorption, du flux d'air acheminé à travers la paire de régénérateurs, avant l'élimination par condensation des impuretés, et l'échange thermique du flux d'air acheminé à travers les régénérateurs s'effectue exclusivement à l'encontre d'un flux azoté impur issu de la séparation à basse température. Le flux partiel du flux d'air à séparer, qui n'est pas acheminé aux régénérateurs, est libéré des impuretés par adsorption et est ensuite refroidi au cours d'un échange thermique indirect avec au moins un produit de séparation à réchauffer. De préférence, au moins 50 à 85 % de l'air soumis à la séparation à basse température est acheminé à travers les régénérateurs.
PCT/EP1999/001127 1998-02-20 1999-02-22 Purification de l'air avec des regenerateurs et lit adsorbant pour l'eau WO1999042773A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU29277/99A AU2927799A (en) 1998-02-20 1999-02-22 Air purification with regenerators and adsorption bed for water

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE19807225A DE19807225A1 (de) 1998-02-20 1998-02-20 Verfahren und Vorrichtung zur Tieftemperaturzerlegung von Luft
DE19807225.2 1998-02-20
EP98109037.6 1998-05-18
EP98109037A EP0947788A1 (fr) 1998-02-20 1998-05-18 Purification d'air par échangeurs de chaleur réversibles et lit adsorbant pour l'eau

Publications (1)

Publication Number Publication Date
WO1999042773A1 true WO1999042773A1 (fr) 1999-08-26

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PCT/EP1999/001127 WO1999042773A1 (fr) 1998-02-20 1999-02-22 Purification de l'air avec des regenerateurs et lit adsorbant pour l'eau

Country Status (2)

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AU (1) AU2927799A (fr)
WO (1) WO1999042773A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2949553A1 (fr) * 2009-09-02 2011-03-04 Air Liquide Procede de production d'au moins un gaz pauvre en co2 et d'un ou plusieurs fluides riches en co2
EP3118557A2 (fr) 2015-07-16 2017-01-18 Linde Aktiengesellschaft Accumulateur de froid a lit fixe et procede de stockage d'energie thermique

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3214926A (en) * 1963-04-15 1965-11-02 Philips Corp Method of producing liquid oxygen and/or liquid nitrogen
US3508412A (en) * 1966-08-12 1970-04-28 Mc Donnell Douglas Corp Production of nitrogen by air separation
DE2734934A1 (de) * 1977-08-03 1979-02-08 Linde Ag Verfahren und vorrichtung zur tieftemperaturzerlegung von luft
US4224045A (en) * 1978-08-23 1980-09-23 Union Carbide Corporation Cryogenic system for producing low-purity oxygen
US4367082A (en) * 1980-06-14 1983-01-04 Kabushiki Kaisha Kobe Seiko Sho Air separating system
US4400188A (en) * 1981-10-27 1983-08-23 Air Products And Chemicals, Inc. Nitrogen generator cycle
EP0537597A1 (fr) * 1991-10-07 1993-04-21 Praxair Technology, Inc. Procédé d'adsorption à pression alternée à basses températures avec réfrigération
EP0765681A2 (fr) * 1995-09-26 1997-04-02 Praxair Technology, Inc. Prépurificateur d'air pour adsorption à pression alternée
US5802872A (en) * 1997-07-30 1998-09-08 Praxair Technology, Inc. Cryogenic air separation with combined prepurifier and regenerators

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3214926A (en) * 1963-04-15 1965-11-02 Philips Corp Method of producing liquid oxygen and/or liquid nitrogen
US3508412A (en) * 1966-08-12 1970-04-28 Mc Donnell Douglas Corp Production of nitrogen by air separation
DE2734934A1 (de) * 1977-08-03 1979-02-08 Linde Ag Verfahren und vorrichtung zur tieftemperaturzerlegung von luft
US4224045A (en) * 1978-08-23 1980-09-23 Union Carbide Corporation Cryogenic system for producing low-purity oxygen
US4367082A (en) * 1980-06-14 1983-01-04 Kabushiki Kaisha Kobe Seiko Sho Air separating system
US4400188A (en) * 1981-10-27 1983-08-23 Air Products And Chemicals, Inc. Nitrogen generator cycle
EP0537597A1 (fr) * 1991-10-07 1993-04-21 Praxair Technology, Inc. Procédé d'adsorption à pression alternée à basses températures avec réfrigération
EP0765681A2 (fr) * 1995-09-26 1997-04-02 Praxair Technology, Inc. Prépurificateur d'air pour adsorption à pression alternée
US5802872A (en) * 1997-07-30 1998-09-08 Praxair Technology, Inc. Cryogenic air separation with combined prepurifier and regenerators

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2949553A1 (fr) * 2009-09-02 2011-03-04 Air Liquide Procede de production d'au moins un gaz pauvre en co2 et d'un ou plusieurs fluides riches en co2
WO2011027079A1 (fr) * 2009-09-02 2011-03-10 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procédé de production d'au moins un gaz pauvre en co2 et d'au moins un fluide riche en co2
EP3118557A2 (fr) 2015-07-16 2017-01-18 Linde Aktiengesellschaft Accumulateur de froid a lit fixe et procede de stockage d'energie thermique
DE102015009256A1 (de) 2015-07-16 2017-01-19 Linde Aktiengesellschaft Festbettkältespeicher und Verfahren zur Speicherung von thermischer Energie

Also Published As

Publication number Publication date
AU2927799A (en) 1999-09-06

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