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WO1999042773A1 - Air purification with regenerators and adsorption bed for water - Google Patents

Air purification with regenerators and adsorption bed for water 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
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.)
Ceased
Application number
PCT/EP1999/001127
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German (de)
French (fr)
Inventor
Wilhelm Rohde
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Linde GmbH
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Linde GmbH
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Filing date
Publication date
Priority claimed from DE19807225A external-priority patent/DE19807225A1/en
Application filed by Linde GmbH filed Critical Linde GmbH
Priority to AU29277/99A priority Critical patent/AU2927799A/en
Publication of WO1999042773A1 publication Critical patent/WO1999042773A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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

The invention relates to a method for the low-temperature separation of air, according to which a partial stream or the entire air stream to be separated is cooled in at least one reversible regenerator pair by heat exchange with part of the separation products and impurities are condensated out. The air stream purified in this manner is then subjected to low-temperature separation. The invention also relates to a device for carrying out this method, comprising at least one reversible regenerator pair, in which the air inlet line is joined to the regenerators. According to the invention water is separated from the air stream fed through the regenerator pair in an adsorptive manner before the impurities are condensated out, and the heat exchange of the air stream fed through the regenerators is carried out exclusively in exchange for an impure nitrogen stream from the low-temperature separation. That partial stream of the air stream to be separated which is not fed to the regenerators is freed of impurities in an adsorptive manner and then cooled in an indirect heat exchange with at least one separation product to be pre-heated. Preferably at least 50 to 85 % of the air subjected to low-temperature separation is fed through the regenerators.

Description

Beschreibung description

LUFTREINIGUNG MIT REGENERATOREN UND ADSORPTIVBETT FÜR WASSERAIR PURIFICATION WITH REGENERATORS AND ADSORPTIVE BED FOR WATER

Die Erfindung betrifft ein Verfahren zur Tieftemperaturzerlegung von Luft, bei dem in mindestens einem umschaltbaren Regeneratorenpaar ein Teilstrom oder der gesamte zu zerlegende Luftstrom durch Wärmetausch mit einem Teil der Zerlegungsprodukte gekühlt wird, wobei Verunreinigungen auskondensieren, wonach der so gereinigte Luftstrom der Tieftemperaturzeriegung zugeführt wird.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.

Ferner betrifft die Erfindung eine Vorrichtung zum Durchführen des erfindungsgemäßen Verfahrens.The invention further relates to a device for performing the method according to the invention.

Bei der kryogenen Luftzerlegung - im folgenden Tieftemperaturzerlegung genannt - wird die Luft nach der Verdichtung zunächst auf annähernd Kühlwassertemperatur und dann bis auf ca. 15°C abgekühlt, anschließend adsorptiv getrocknet und von Kohlendioxid befreit - vorzugsweise mittels eines Moisiebes - und sodann in Platten- wärmetauschem gegen ausströmende Produkte und Restgas(e) auf Verflüssigungstemperatur abgekühlt. Die hierzu verwendeten Plattenwärmetauscher können jedoch nur bis zu einer bestimmten Größe gefertigt werden; bei entsprechend großen Luftmengen sind daher mehrere Wärmetauscher parallel zu schalten.In 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). However, 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.

Bereits in den Anfängen der kryogenen Luftzerlegung, als die Sauerstoffproduktion einer Anlage etwa bei 2000 Nm3/h bis 6000 Nm3/h lag - was in der damaligen Zeit als Großanlage bezeichnet wurde - , kamen für den Wärmetausch zwischen Luft und Zeriegungsprodukte sog. Regeneratoren zum Einsatz. Diese waren vorzugsweise jeweils paarweise angeordnet. In einem Regenerator kühlt sich die Luft an der Wärmespeichermasse des Regenerators ab, wobei die störenden und zu entfernenden Bestandteile, wie Wasser und Kohlendioxid, flüssig bzw. fest ausgeschieden werden. Die Speichermasse des Regenerators wärmt sich dabei langsam an.In the very beginning of cryogenic air separation, when the oxygen production of a plant was around 2000 Nm 3 / h to 6000 Nm 3 / h - which was then called a large plant - so-called regenerators came for the heat exchange between air and waste products for use. These were preferably arranged in pairs. In a regenerator, 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.

In dem zweiten Regenerator des Regeneratorenpaares werden die Zeriegungsprodukte aus der kryogenen Luftzerlegung angewärmt und tragen dabei die vorher ausgeschiedenen Verunreinigungen der Luft wieder aus dem Regenerator heraus. Dabei geben die Zerlegungsprodukte ihre Kälte an die Speichermasse des Regenerators ab. In periodischen Abständen werden die Regeneratoren umgeschaltet, so daß die Luft durch den zuvor mit Zerlegungsprodukten gekühlten Regenerator einströmt und die Zerlegungsprodukte durch den vorher mit Zerlegungsluft betriebenenIn the second regenerator of the pair of regenerators, 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

Regenerator ausströmen. Hierbei ist anzumerken, daß die Produkte bei derartigen Luftzerlegungsanlagen vorwiegend Sauerstoff mit unterschiedlicher Reinheit und unreiner Stickstoff waren.Flush out the regenerator. It should be noted here that the products in such air separation plants were predominantly oxygen with different purities and impure nitrogen.

War Sauerstoff mit geringer Reinheit gewünscht, so wurde dieser in einemIf oxygen with low purity was desired, it was combined in one

Regeneratorenpaar Luft/Sauerstoff und der unreine Stickstoff in einem zweiten Regeneratorenpaar Luft/unreiner Stickstoff abgekühlt bzw. angewärmt. War Sauerstoff mit höheren Reinheit gefragt, so wurden in die Speichermassen der Regeneratoren Rohrbündel, durch welche der Sauerstoff konstant abgezogen werden konnte, eingebettet.Air / oxygen regenerator pair and the impure nitrogen cooled or warmed in a second air / impure nitrogen regenerator pair. If higher purity oxygen was required, tube bundles through which the oxygen could be drawn off constantly were embedded in the storage masses of the regenerators.

Durch den indirekten Wärmetausch zwischen der zu zerlegenden Luft und dem unreinen Stickstoff sowie Sauerstoff entstanden große Temperaturdifferenzen zwischen einströmender Luft und ausströmenden Produkten; dies galt insbesondere für den ausströmenden Sauerstoff. Die dadurch entstandenen Kälteverluste konnten nur durch die Vergrößerung der Luftmenge, die in sog. Expansionsturbinen entspannt wurde, kompensiert werden. Diese großen Turbinenluftmengen, die direkt in die Niederdruckkolonne eingeblasen wurden, hatten aber auch eine nicht unbedeutende Verschlechterung der Ausbeute und damit einen erhöhten Energiebedarf zur Folge.The indirect heat exchange between the air to be separated and the impure nitrogen and oxygen created large temperature differences between the inflowing air and the outflowing products; this was especially true for the outflowing oxygen. The resulting cold losses could only be compensated for by increasing the amount of air that was expanded in so-called expansion turbines. However, these large amounts of turbine air, which were blown directly into the low-pressure column, also resulted in a not insignificant deterioration in the yield and thus an increased energy requirement.

Die bereits erwähnten Wärmespeichermassen in den Regeneratoren mit Rohrspiralen für reinen Sauerstoff bestanden aus Quarzit-Steinen, für Sauerstoff geringerer Reinheit aus sog. Aluminium-Horden; dies sind spiralförmig aufgewickelte, geriffelte Aluminiumbänder. Regeneratoren mit Quarzitfüllung und Rohrspiralen haben ein nicht unbedeutendes Leervolumen, weshalb die in ihnen gespeicherte Druckluft bei jedem Schal-vorgang teilweise verloren geht, was zu einer Verschlechterung der Ausbeute führt.The heat storage masses already mentioned in the 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.

In den 60er Jahren begänne Platten-Wärmetauscher und damit auch die sog. REVEX-Wärmetauscher (Reversing-Heat-Exchanger) die Regeneratoren zu verdrängen. Auch die Entwicklung von Molekularsieben, mittels derer Wasser und Kohlendioxid bei Umgebungstemperatur aus der Luft entfernt werden kann, trug dazu bei, daß die Regeneratoren verdrängt wurden. Zudem wurde zunehmend auch der in der Tieftemperaturzerlegung gewonnene Stickstoff neben dem Sauerstoff als Produkt angesehen. Eine Produktmenge Sauerstoff plus Stickstoff ist in sog. REVEX-Anlagen nur bis 50 % und bei der Verwendung von Regeneratoren nur bis ca. 45 % der eingesetzten Luftmenge realisierbar.In the 1960s, plate heat exchangers and thus also the so-called REVEX heat exchangers (reversing heat exchangers) began to regenerate oust. The development of molecular sieves, by means of which water and carbon dioxide can be removed from the air at ambient temperature, also contributed to the displacement of the regenerators. In addition, the nitrogen obtained in the low-temperature decomposition was increasingly viewed as a product alongside oxygen. A product quantity of oxygen plus nitrogen can only be realized in so-called REVEX systems up to 50% and when using regenerators only up to approx. 45% of the air quantity used.

Bei großen Sauerstoffmengen, wie z. B. 100.000 Nm3/h Sauerstoff, müssen annäh- ernd 500.000 Nm3/h Luft der Tieftemperaturzerlegung zugeführt werden. Davon sind 400.000 Nm3/h Restgas, also unreiner Stickstoff, der nicht getrocknet werden muß und zudem Kohlendioxid enthalten darf. Es ist deshalb nicht notwendig, die gesamte zu zerlegende Luft in entsprechenden (Molsieb)Adsorberstationen zu trocken und von Kohlendioxid zu befreien. Dies würde zudem eine beträchtliche Anzahl von der Adsorberstation nachgeschalteten, parallel angeordneten Plattenwärmetauschem erfordern.With large amounts of oxygen, such as. B. 100,000 Nm 3 / h oxygen, approximately 500,000 Nm 3 / h air must be fed to the low-temperature decomposition. Of this, 400,000 Nm 3 / h are residual gas, i.e. impure nitrogen, which does not have to be dried and which may also contain carbon dioxide. It is therefore not necessary to dry all of the air to be separated in appropriate (molecular sieve) adsorber stations and to remove carbon dioxide. This would also require a considerable number of plate heat exchangers connected in parallel from the adsorber station.

Zur Lösung dieses Problems ist aus der DE 27 34 934 A1 ein Verfahren sowie eine Vorrichtung zur Tieftemperaturzerlegung von Luft bekannt, wobei in mindestens einem umschaltbaren Regeneratorenpaar ein Teil der zu zerlegenden Luft durch Wärmetausch mit einem Teil der Zerlegungsprodukte gekühlt wird, während der restliche Teil der zu zerlegenden Luft durch Adsorption gereinigt und in einem Wärmetauscher durch Wärmetausch mit einem anderen Teil der Zerlegungsprodukte gekühlt wird. Anschließend werden beide Luftströme der Tieftemperaturzerlegung zugeführt. Es kann somit eine Verfahrensweise realisiert werden, bei der nur derjenige Anteil der zu zerlegenden Luft adsorptiv von Wasser und Kohlendioxid befreit wird, der für die Anwärmung der z. B. 100.000 Nm3/h Produktsauerstoff erforderlich ist.To solve this problem, 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.

Nachteilig bei dem Verfahren sowie der Vorrichtung gemäß der DE 27 34 934 A1 ist jedoch, daß für die Kondensation von Wasser eine große Wärmespeicherkapazität vorhanden sein muß. Diese Forderung verursacht einerseits höhere Investitionskosten und führt andererseits dazu, daß insbesondere wegen des größeren Regeneratorvolumens auch höhere Luftschaltverluste in Kauf genommen werden müssen. Dies beeinflußt den Energiebedarf der Zerlegungsanlage nicht unbeträchtlich.A disadvantage of the method and the device according to DE 27 34 934 A1, however, 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.

Aufgabe der vorliegenden Erfindung ist es, ein Verfahren sowie eine Vorrichtung zur Tieftemperaturzerlegung von Luft anzugeben, das bzw. die gegenüber den bekannten Verfahren und Vorrichtungen zur Tieftemperaturzerlegung von Luft eine Kosten- und Energiereduzierung ermöglicht.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.

Dies wird entsprechend dem erfindungsgemäßen Verfahren dadurch erreicht, daß die Abtrennung von Wasser aus dem durch das Regeneratorenpaar geführten Luftstrom vor dem Auskondensieren der Verunreinigungen adsorptiv und der Wärmetausch des durch die Regeneratoren geführten Luftstromes ausschließlich gegen einen unreinen Stickstoffstrom aus der Tieftemperaturzerlegung erfolgt.This is achieved in accordance with the method according to the invention in that the separation of water from the air flow conducted through the regenerator pair takes place adsorptively before the contaminants are condensed out and the heat exchange of the air flow guided through the regenerators takes place exclusively against an impure nitrogen flow from the low-temperature decomposition.

Erfindungsgemäß erfolgt die Abtrennung von Wasser aus dem durch das Regeneratorenpaar geführten Luftstrom vor dem Auskondensieren der weiteren Verunreinigungen, wie z. B. Kohlendioxid, mittels Adsorption. Die erfindungsgemäße Vorrichtung ist deshalb dadurch gekennzeichnet, daß die Regeneratoren ein in ihrem Einlaßbereich angeordnetes Adsorptionsbett aufweisen.According to the invention, 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.

Bei dem erfindungsgemäßen Verfahren erfolgt der Wärmetausch des durch die Regeneratoren geführten Luftstromes ausschließlich gegen einen unreinen Stickstoffstrom aus der Tieftemperaturzerlegung. Aufgrund dieser Verfahrensweise können die verwendeten Regeneratoren vergleichsweise einfach aufgebaut sein; zumindest kann auf das Vorsehen von Rohrbündeln in der Speichermasse der Regeneratoren verzichtet werden.In the method according to the invention, 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.

Das erfindungsgemäße Verfahren zur Tieftemperaturzerlegung von Luft weiterbildend wird vorgeschlagen, daß ein Teilstrom der zu zerlegenden Luft, der nicht den Regeneratoren zugeführt wird, mittels der Adsorption von Verunreinigungen befreit und anschließend im indirekten Wärmetausch mit einem anzuwärmenden Zerlegungsprodukt abgekühlt wird. ' 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. '

Diese Verfahrensweise macht es erforderlich, daß parallel zu den erwähnten Regeneratoren Adsorber, die geeignete Adsorptionsmittel enthalten, angeordnet werden. In diesen Adsorbern erfolgt ein Trocknen und Entfernen von Verunreinigen aus den Teilluftstrom, der anschließend vor seiner Zuführung in die Tieftemperaturzerlegung, vorzugsweise gegen den Produktsauerstoff, der dadurch angewärmt wird, abgekühlt wird.This procedure requires that adsorbers containing suitable adsorbents be arranged in parallel with the regenerators mentioned become. In these adsorbers, impurities are dried and removed from the partial air stream, which is then cooled before being fed into the low-temperature decomposition, preferably against the product oxygen, which is thereby heated.

Vorzugsweise werden wenigstens 50 bis 85 % der der Tieftemperaturzerlegung zugeführten Luftmenge durch die Regeneratoren geleitet. Da - wie eingangs bereits erwähnt - für die Produktion von 100.000 Nm3/h Produktsauerstoff annähernd 500.000 NnrvVh Luft der Tieftemperaturzerlegung zugeführt werden müssen, und dabei 400.000 Nm3/h Restgas - also unreiner Stickstoff entstehen -, hat diesePreferably 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

Verfahrensweise den Vorteil, daß das gesamte Restgas für die Abkühlung des zu zerlegenden Luftstromes verwendet wird. Durch die Adsorber wird im wesentlichen nur derjenige Teilstrom der zu zerlegenden Luft geführt, der für die Anwärmung der Produktsauerstoffmenge und des Regeneriergases für die Adsorber benötigt wird.Procedure the advantage that the entire residual gas is used for cooling the air stream to be broken down. Essentially only the partial flow of the air to be separated that is required for heating the product oxygen quantity and the regeneration gas for the adsorbers is passed through the adsorbers.

Eine weitere vorteilhafte Ausgestaltung des erfindungsgemäßen Verfahrens zur Tieftemperaturzerlegung von Luft ist dadurch gekennzeichnet, daß die adsorptive Abtrennung von Wasser aus dem durch die Regeneratoren geführten Luftstrom in die Regeneratoren integriert ist.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.

Prinzipiell kann den Regeneratoren ein separater Adsorber, in dem die adsorptive Abtrennung von Wasser erfolgt, vorgeschaltet werden. In vorteilhafter Weise wird jedoch die für die adsorptive Abtrennung des Wassers benötigte Adsorptionsmittelschicht in den Regenerator selbst, vorzugsweise in dessen Einlaßbereich integriert. Mittels dieser Ausgestaltung der Erfindung kann die für die Entfernung von Wasser benötigte Menge an Adsoφtionsmittel extrem klein gehalten werden, da sie nur für die kurze Luftperiode der Regeneratoren ausgelegt werden muß.In principle, the regenerators can be preceded by a separate adsorber in which the adsorptive separation of water takes place. However, the adsorbent layer required for the adsorptive separation of the water is advantageously integrated into the regenerator itself, preferably in its inlet area. By means of this embodiment of the invention, the amount of adsorbent required for the removal of water can be kept extremely small, since it only has to be designed for the short air period of the regenerators.

Das erfindungsgemäße Verfahren zur Tieftemperaturzerlegung von Luft weiterbildend wird vorgeschlagen, daß die Regenerierung des mit Wasser beladenen Adsoφtions- mittels durch Spülen des Adsoφtionsmittels erfolgt. Hierbei wird als Spülgas vorzugsweise ein unreiner Stickstoffstrom aus der Tieftemperaturzeriung verwendet. Mit der zum Zwecke der Regenerierung durch den Regenerator geführten Spülgasmenge läßt sich eine sog. Heatless-Regenerierung der Adsorptionsmittelschicht realisieren.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. In this case, 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.

Ist die Spülgasmenge - also die Menge an unreinem Stickstoff - annähernd gleich der in den Regeneratoren abzukühlenden Luftmenge, so ist es ausreichend, wenn im Einlaßbereich der Regeneratoren eine relativ kurze Adsorptionsmittelschicht, z. B. eine Alugelschicht, vorgesehen wird, mittels derer die Luft bspw. auf einen Taupunkt von 5°C abgekühlt wird. Dadurch wird gewährleistet, daß sich kein tropfförmiges Wasser auf den Horden oder Schüttungen der Regeneratoren bildet. Wird des weiteren die erwähnte Heatless-Regenerierung realisiert, führt dies dazu, daß die Regeneratoren noch kompakter bauen, da keine Heizflächen und Wärmekapazitäten für Wasserkondensation und Wiederverdampfung vorgesehen werden müssen.If 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.

Wie bereits erwähnt, zeichnet sich die erfindungsgemäße Vorrichtung zum Durchführen des erfindungsgemäßen Verfahrens dadurch aus, daß die Regeneratoren ein im Einlaßbereich angeordnetes Adsorptionsbett aufweisen. Dieses besteht entsprechend einer vorteilhaften Ausgestaltung der erfindungsgemäßen Vorrichtung aus einem Wasser-adsorbierenden Adsorptionsmittel. Entsprechend der Wahl des verwendeten Adsorptionsmittels kann dieses - neben Wasser - weitere Komponenten aus dem zu zerlegenden Luftstrom entfernen.As already mentioned, 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. According to an advantageous embodiment of the device according to the invention, 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.

Es wird weiterhin vorgeschlagen, daß die Regeneratoren Stahlhorden und/oder eine Stahlschüttung als wärmespeicherndes Material enthalten. Diese Stahlhorden bzw. Stahlschüttungen - die anstelle von Aluminium-Horden oder Quarzit-SteinenIt is further proposed that the 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

Verwendung finden - führen zu wesentlich kompakteren Regeneratoren und damit zu geringeren Schaltverlusten. Zudem ist Stahl preiswerter als Aluminium. Prinzipiell können jedoch auch Aluminiumhorden und/oder Aluminiumschüttungen als wärmespeicherndes Material verwendet werden.Find use - lead to much more compact regenerators and thus lower switching losses. In addition, steel is cheaper than aluminum. In principle, however, aluminum trays and / or aluminum fillings can also be used as the heat-storing material.

Die erfindungsgemäße Vorrichtung weiterbildend wird vorgeschlagen, daß die Stahloder Aluminiumhorden eine Breite von 30 bis 500 mm aufweisen. Further developing the device according to the invention it is proposed that the steel or aluminum trays have a width of 30 to 500 mm.

Claims

Patentansprüche claims 1. Verfahren zur Tieftemperaturzeriegung von Luft, bei dem in mindestens einem umschaltbaren Regeneratorenpaar ein Teilstrom oder der gesamte zu zerlegende Luftstrom durch Wärmetausch mit einem Teil der Zerlegungsprodukte gekühlt wird, wobei Verunreinigungen auskondensieren, wonach der so gereinigte1. A process for the low-temperature extraction of air, in which, in at least one switchable pair of regenerators, a partial stream or the entire air stream to be separated is cooled by heat exchange with a part of the decomposition products, with contaminants condensing out, after which the cleaned one Luftstrom der Tieftemperaturzeriegung zugeführt wird, dadurch gekennzeichnet, daß die Abtrennung von Wasser aus dem durch das Regeneratorenpaar geführten Luftstrom vor dem Auskondensieren der Verunreinigungen adsoφtiv und der Wärmetausch des durch die Regeneratoren geführten Luftstromes ausschließlich gegen einen unreinen Stickstoff ström aus der Tieftemperaturzeriegung erfolgt.Air flow of the low-temperature reduction is supplied, characterized in that the separation of water from the air flow guided by the regenerator pair before the condensation of the contaminants is adsorbent and the heat exchange of the air flow guided by the regenerators takes place exclusively against an impure nitrogen flow from the low-temperature reduction. 2. Verfahren zur Tieftemperaturzeriegung von Luft nach Anspruch 1 , dadurch gekennzeichnet, daß ein Teilstrom der zu zerlegende Luft, der nicht den2. A method for the low-temperature decomposition of air according to claim 1, characterized in that a partial flow of the air to be separated, which is not the Regeneratoren zugeführt wird, adsorptiv von Verunreinigungen befreit und anschließend im indirekten Wärmetausch mit wenigstens einem anzuwärmenden Zerlegungsprodukt abgekühlt wird.Regenerators is supplied, adsorptively freed of impurities and then cooled in indirect heat exchange with at least one decomposition product to be heated. 3. Verfahren zur Tieftemperaturzeriegung von Luft nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß wenigstens 50 bis 85 % der der Tieftemperaturzeriegung zugeführten Luftmenge durch die Regeneratoren geführt wird.3. A method for low-temperature reduction of air according to claim 1 or 2, characterized in that at least 50 to 85% of the amount of air supplied to the low-temperature reduction is passed through the regenerators. 4. Verfahren zur Tieftemperaturzeriegung von Luft nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß die adsoφtive Abtrennung von Wasser aus dem durch die Regeneratoren geführten Luftstromes in die Regeneratoren integriert ist.4. A method for low-temperature extraction of air according to one of the preceding claims, characterized in that the adsoφtive separation of water from the air flow guided by the regenerators is integrated into the regenerators. 5. Verfahren zur Tieftemperaturzeriegung von Luft nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß die Regenerierung des mit Wasser beladenen Adsorptionsmittels durch Spülen des Adsorptionsmittels erfolgt. 5. A process for the low-temperature extraction of air according to one of the preceding claims, characterized in that the regeneration of the adsorbent loaded with water is carried out by flushing the adsorbent. 6. Verfahren zur Tieftemperaturzeriegung von Luft nach Anspruch 5, dadurch gekennzeichnet, daß als Spülgas ein unreiner Stickstoffstrom aus der Tieftemperaturzeriegung verwendet wird.6. A process for the low-temperature reduction of air according to claim 5, characterized in that an impure nitrogen stream from the low-temperature reduction is used as the purge gas. 7. Vorrichtung zum Durchführen des Verfahrens nach einem der vorhergehenden Ansprüche mit mindestens einem umschaltbaren Regeneratorenpaar, bei der die Lufteintrittsleitung mit den Regeneratoren verbunden ist, dadurch gekennzeichnet, daß die Regeneratoren ein im Einlaßbereich angeordnetes Adsorptionsbett aufweisen.7. Device for performing the method according to one of the preceding claims with at least one switchable pair of regenerators, in which the air inlet line is connected to the regenerators, characterized in that the regenerators have an adsorption bed arranged in the inlet region. 8. Vorrichtung nach Anspruch 7, dadurch gekennzeichnet, daß das Adsorptionsbett aus einem Wasser-adsorbierenden Adsorptionsmittel besteht.8. The device according to claim 7, characterized in that the adsorption bed consists of a water-adsorbing adsorbent. 9. Vorrichtung nach Anspruch 7 oder 8, dadurch gekennzeichnet, daß die Regeneratoren Stahlhorden und/oder eine Stahlschüttung als wärmespeicherndes Material enthalten.9. Apparatus according to claim 7 or 8, characterized in that the regenerators contain steel trays and / or a steel bed as a heat-storing material. 10. Vorrichtung nach Anspruch 7 oder 8, dadurch gekennzeichnet, daß die Regen- eratoren Aluminiumhorden und/oder eine Aluminiumschüttung als wärmespeicherndes Material enthalten.10. The device according to claim 7 or 8, characterized in that the regenerators contain aluminum trays and / or an aluminum fill as heat-storing material. 11. Vorrichtung nach Anspruch 9 oder 10, dadurch gekennzeichnet, daß die Stahloder Aluminiumhorden eine Breite von 30 bis 500 mm aufweisen.11. The device according to claim 9 or 10, characterized in that the steel or aluminum trays have a width of 30 to 500 mm. 12. Vorrichtung nach einem der Ansprüche 7 bis 11 , dadurch gekennzeichnet, daß zusätzlich zu dem mindestens einen umschaltbaren Regeneratorenpaar mindestens ein umschaltbares Adsorbeφaar und ein Wärmetauscher angeordnet sind und eine Zweigleitung der Lufteintrittsleitung über die Adsorber mit dem Wärmetauscher verbunden ist. 12. The device according to one of claims 7 to 11, characterized in that in addition to the at least one switchable pair of regenerators at least one switchable Adsorbeφaar and a heat exchanger are arranged and a branch line of the air inlet line via the adsorber is connected to the heat exchanger.
PCT/EP1999/001127 1998-02-20 1999-02-22 Air purification with regenerators and adsorption bed for water Ceased WO1999042773A1 (en)

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