EP1094286B1 - Process and device for cryogenic air separation - Google Patents

Process and device for cryogenic air separation Download PDF

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Publication number
EP1094286B1
EP1094286B1 EP00119941A EP00119941A EP1094286B1 EP 1094286 B1 EP1094286 B1 EP 1094286B1 EP 00119941 A EP00119941 A EP 00119941A EP 00119941 A EP00119941 A EP 00119941A EP 1094286 B1 EP1094286 B1 EP 1094286B1
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Prior art keywords
pressure column
section
condenser
evaporator
low
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German (de)
French (fr)
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EP1094286A1 (en
Inventor
Gerhard Dipl.-Ing. Pompl
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Linde GmbH
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Linde GmbH
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Priority claimed from DE19950570A external-priority patent/DE19950570A1/en
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    • 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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • F25J3/04878—Side by side arrangement of multiple vessels in a main column system, wherein the vessels are normally mounted one upon the other or forming different sections of the same column
    • 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
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
    • 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
    • F25J3/04406—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 using a dual pressure main column system
    • F25J3/04412—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 using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • 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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • F25J3/04884—Arrangement of reboiler-condensers
    • 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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04896—Details of columns, e.g. internals, inlet/outlet devices
    • 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
    • F25J5/002—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger
    • F25J5/005—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger in a reboiler-condenser, e.g. within a column
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/42—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being nitrogen
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/04—Down-flowing type boiler-condenser, i.e. with evaporation of a falling liquid film
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/10—Boiler-condenser with superposed stages
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams

Definitions

  • the invention relates to a method for the low temperature decomposition of air with the Features of the preamble of claim 1.
  • the rectification system of the invention can be used as a classic two column system be formed, but also as a three or more column system. It may be in addition to the columns for nitrogen-oxygen separation further devices for Production of other air components, in particular of noble gases, for example, an argon recovery.
  • a designed as a condenser-evaporator heat exchanger has evaporation and Liquefaction passages on. In the evaporation passages becomes a liquid evaporated. They are in heat exchange contact with the liquefaction passages, in which a gaseous fraction in indirect heat exchange with the evaporating Liquid condenses. Details about evaporation processes are for example the monograph "Evaporation and its technical applications" by Billet (1981) refer to.
  • a condenser-evaporator can consist of one or more Heat exchanger blocks be constructed.
  • a condenser-evaporator system points one or more condenser evaporators.
  • falling film evaporator as a condenser-evaporator in Air separation plants used, as for example in EP 681153 A or EP 410832 A is shown.
  • the evaporates to Liquid enters the top of the evaporation passages and flows as a relatively thin film on the walls, separating the evaporation and liquefaction passages, down.
  • This evaporator type has a particularly low pressure loss in the Evaporation passages and is therefore energetically generally cheaper than a Circulation evaporator.
  • the invention is therefore based on the object, a method of the initially mentioned type and to provide a corresponding device that economically and Operationally are particularly favorable to operate and in particular a have particularly low energy consumption.
  • non-evaporated liquid (second oxygen-rich liquid) is indeed as in the conventional falling film evaporation of a Supplied conveyor, such as a pump; this transports the Liquid, however, not back to the entry of the evaporation passages of the same Falling film evaporator, but on a second section of the condenser-evaporator system.
  • the first section needs only a relatively small Part, for example, 30 to 50%, preferably 38 to 42%, of the total Evaporating power of the condenser-evaporator system to take.
  • the oxygen product is preferably in the inventive method subtracted from the second section of the condenser-evaporator system, either as a gas or as a liquid.
  • a gaseous pressure oxygen product can be obtained by oxygenated liquid in the liquid state to an elevated pressure brought and then evaporated against air or nitrogen (so-called Internal compression).
  • the first portion of the condenser-evaporator system of the invention may be arranged within the low-pressure column or in a separate container.
  • the method and the corresponding apparatus according to the invention can be used for each Type of nitrogen-oxygen separation can be used, especially independently from the product purities in the heads and swamps of the columns.
  • the vapor that enters the evaporation passages of the second section of the Condenser-evaporator system is generated, preferably not withdrawn exclusively or mainly as a gaseous oxygen product, but at least half initiated in the low-pressure column and there as used ascending steam. If the entire oxygen product is liquid won and / or internally compressed, can also the whole in the second section of the condenser-evaporator system generated gas in the low-pressure column to be led back.
  • a third oxygen-rich liquid remains in the second section of the condenser-evaporator system as non-vaporized part of the second oxygen-rich Liquid. It preferably collects in the liquid bath of or one Circulation evaporator. It is preferably used in the process according to the invention at least partially into the low pressure column and / or to the evaporation passages the first section of the condenser-evaporator system liquid returned. This return can be conveniently shared with the above mentioned return of steam are carried out in the low-pressure column, by a corresponding line at the level of the liquid of the bath is arranged. This will simultaneously the liquid level in the circulation evaporator regulated, without additional control or regulating devices would be required.
  • the second section is partially formed as a second falling-film evaporator
  • the already existing conveyor between the first and second section additionally for the generation of a liquid circulation at the second falling film evaporator can be used.
  • the liquefaction passages of the condenser-evaporator system are preferably so connected to the two columns, as in claim 4 is described. This can be dispensed with pumps at these points, and although even if pressure column and low pressure column arranged side by side are. (In this case, it is favorable if the first section of the condenser-evaporator system below the lowest floor of the low pressure column and the second section of the condenser-evaporator system above the top Bottom of the pressure column are arranged.)
  • the trained as a falling film evaporator first section is preferably so dimensioned that in him the amount of nitrogen-rich liquid through Condensation of a nitrogen-rich gas fraction is generated from the pressure column, the is required as reflux in the low-pressure column (plus, where appropriate, as pressureless liquid product withdrawn amount).
  • the rest of the Heat transfer (50 to 70%, preferably 58 to 62%) is in the second section performed the condenser-evaporator system, in such a way that there generates at least the amount of liquid required as reflux in the pressure column becomes.
  • the heating surface of the heating surface it may in some cases be more favorable, in the first section a larger proportion of nitrogen-rich To condense fraction as described above, according to the heating surface of second section (usually at the head of the pressure column) to the first section (in the Usually in the bottom of the low-pressure column to relocate. In this case, part of the first nitrogen-rich liquid formed in the first section as reflux is abandoned on the pressure column. For this purpose, if necessary, the use of a Liquid pump required.
  • the nitrogen-rich gas fraction is generally the head nitrogen of the Pressure column formed.
  • the first section of the condenser-evaporator system is preferred designed exclusively as a falling film evaporator.
  • He can dimension particularly well as a single, relatively compact block be realized, or in the form of several (for example four) particularly low Blocks arranged side by side.
  • An arrangement immediately in the Swamp of the low-pressure column is also favorable for a low overall height of the plant and their insulation (coldbox).
  • the second section of the condenser-evaporator system can be replaced by at least two evaporation side serially connected sections is formed, the first as a falling film evaporator and the second is designed as a circulation evaporator.
  • the Liquid that realized the evaporation passages of the falling film evaporator Escapes portion is, for example, in the liquid bath of or one introduced as a circulation evaporator realized section.
  • the falling film evaporator-circulation evaporator combination can, for example, with continuous Be equipped liquefaction passages, as in EP 795349 A in detail is described.
  • the liquid from the bath of the Circulating evaporator in the low-pressure column or the exit of the Evaporation passages of the first section of the condenser-evaporator system recycled and to increase the amount of liquid in the as a falling film evaporator trained section of the second section are used.
  • the invention also relates to a device for the cryogenic separation of air according to claim 9. Particularly advantageous embodiments of the device are described in the claims 10 to 13.
  • gaseous feed air 1 which has been previously compressed, cleaned and cooled to about the dew point (not shown), is fed to the pressure column 2 immediately above the sump.
  • the pressure column 2 is part of a rectification system, which also has a low pressure column 3 and a main condenser in the form of a condenser-evaporator system 101, 102, 103.
  • the air is decomposed in the pressure column 2 into top nitrogen and into an oxygen-enriched liquid. The latter is not deducted in the special embodiment, as usual at the bottom, but some theoretical or practical floors higher on line 5.
  • the oxygen-enriched liquid 5 is via a line, not shown at an intermediate point in the low pressure column 3 throttled.
  • the low-pressure column 3 one or more are in the upper area Nitrogen products withdrawn (not shown). Below the bottom Rectification section becomes oxygen in the purity required for the product won. This flows as the first oxygen-rich liquid from the bottom or packing section of the low-pressure column 3 and is in a Collecting device 7 collected. The first oxygen-rich liquid continues to flow to the upper end of the first section 101 of the condenser-evaporator system and is introduced into its evaporation passages. The first section 101 is as Falling film evaporator formed. There, about 28 to 30% of the first evaporate oxygen-rich liquid 7 in indirect heat exchange with a first part 8 the nitrogen-rich gas fraction 4 from the head of the pressure column 2. This condenses the nitrogen-rich gas 8 to a first nitrogen-rich liquid 9.
  • the vapor 11 in the first section 101 of the condenser-evaporator system is generated, flows back to the lowest rectification section of the low-pressure column and participates in the countercurrent mass transfer within this column.
  • the liquid remaining portion 12 forms a second oxygen-rich liquid. This is about Withdrawn line 13 and by means of a pump 14 to the second section of the Condenser evaporator led by a combination of another Falling film evaporator 102 and a circulation evaporator 103 is formed, as in EP 795349 A is described in detail.
  • the second oxygen-rich liquid flows into the evaporation passages of the further falling film evaporator 102 down and evaporates there to about 40%.
  • the resulting steam 15 is completely via line 16 in the low pressure column. 3 returned, since in the example no oxygen as gaseous product directly from the rectification system is discharged.
  • the line 16 is used for the same time Keeping constant the liquid level in the liquid bath 18, by excess Liquid together with the steam generated in the second section 102, 103 for Low pressure column 3 is guided.
  • the liquefaction passages of the further falling film evaporator 102 and the Circulating evaporator 103 are executed continuously. You will be of a second Part 22 of the nitrogen-rich gas fraction 4 from the pressure column 2 acted upon. Of the Nitrogen initially flows through the falling film evaporator 102 and then through the circulation evaporator 103 and condenses at least partially, preferably practically complete. The resulting second nitrogen-rich liquid 23 is completely abandoned as reflux to the pressure column 2.
  • Figure 2 shows in detail the connection between the conduit 16 and the outer space around the two condenser-evaporators 102, 103, which form the second section of the condenser-evaporator system.
  • the dimensions of the line are designed essentially according to the amount of gas to be transported. It is arranged so that liquid from the liquid bath of the circulation evaporator 103 can overflow and flow back as a film 26 at the bottom of the line 16 in the low pressure column 3 and in the liquid sump below the first falling film evaporator 101. As a result, the liquid level of the liquid bath of the circulation evaporator 103 is kept at a constant level without special control measures.
  • FIG. 3 differs from FIG. 1 by an additional line 301 via which a Part of the first nitrogen-rich liquid 9 as reflux to the pressure column. 2 can be abandoned.
  • a liquid pump 302 for overcoming the static level between the first section 101 of the condenser-evaporator system and upper Area of the pressure column 2 necessary.
  • the entire Heating surface of the portion 102 are integrated into the first section 101, so that the second section of the condenser-evaporator system only one Circulation evaporator 103 exists.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The cyrogenic separation of air with a rectifier system for separating nitrogen and oxygen incorporates a pressure column (2), a low pressure column (3) and a condenser-evaporator system (101,102,103) for heating the low pressure column. The condenser-evaporator system has a first and second section. The first section has a pipe for introducing compacted and pre-cleaned circulating air (1) into the pressure column; A first oxygen-rich liquid (6) is conveyed to, and returned from, the evaporation passages. The second section conveys a second oxygen-rich liquid (12,13) from the evaporation passages

Description

Die Erfindung betrifft ein Verfahren zur Tieftemperaturzerlegung von Luft mit den Merkmalen des Oberbegriffs des Patentanspruchs 1.The invention relates to a method for the low temperature decomposition of air with the Features of the preamble of claim 1.

Die Grundlagen der Tieftemperaturzerlegung von Luft im allgemeinen sowie der Aufbau von Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung mit zwei oder mehr Säulen im speziellen sind in der Monographie "Tieftemperaturtechnik" von Hausen/Linde (2. Auflage, 1985) oder aus einem Aufsatz von Latimer in Chemical Engineering Progress (Vol. 63, No.2, 1967, Seite 35) bekannt Die Drucksäule und Niederdrucksäule eines Zweisäulensyslems stehen in Regelfall über ein Kondensator-Verdampfer-System (Hauptkondensator) in Wärmeaustauschbeziehung, in dem Kopfgas der Drucksäule gegen verdampfende Sumpfflüssigkeit der Mitteldrucksäule verflüssigt wird.The basics of cryogenic decomposition of air in general as well as the Construction of rectification system for nitrogen-oxygen separation with two or more Columns in particular are in the monograph "cryogenic technology" of Hausen / Linde (2nd edition, 1985) or from an article by Latimer in Chemical Engineering Progress (Vol. 63, No.2, 1967, page 35) known the pressure column and Low-pressure column of a Zeiläulensyslems are usually on a condenser-evaporator system (Main condenser) in heat exchange relationship, in which Top gas of the pressure column against vaporizing bottom liquid of the medium-pressure column is liquefied.

Das Rektifiziersystem der Erfindung kann als klassisches Zweisäulensystem ausgebildet sein, aber auch als Drei- oder Mehrsäulensystem. Es kann zusätzlich zu den Kolonnen zur Stickstoff-Sauerstoff-Trennung weitere Vorrichtungen zur Gewinnung anderer Luftkomponenten, insbesondere von Edelgasen aufweisen, beispielsweise eine Argongewinnung.The rectification system of the invention can be used as a classic two column system be formed, but also as a three or more column system. It may be in addition to the columns for nitrogen-oxygen separation further devices for Production of other air components, in particular of noble gases, for example, an argon recovery.

Ein als Kondensator-Verdampfer ausgebildeter Wärmetauscher weist Verdampfungs-und Verflüssigungspassagen auf. In den Verdampfungspassagen wird eine Flüssigkeit verdampft. Sie stehen in Wärmeaustauschkontakt mit den Verflüssigungspassagen, in denen eine gasförmige Fraktion in indirektem Wärmeaustausch mit der verdampfenden Flüssigkeit kondensiert. Einzelheiten über Verdampfungsvorgänge sind beispielsweise der Monographie "Verdampfung und ihre technischen Anwendungen" von Billet (1981) zu entnehmen. Ein Kondensator-Verdampfer kann aus einem oder mehreren Wärmetauscherblöcken aufgebaut sein. Ein Kondensator-Verdampfer-System weist einen oder mehrere Kondensator-Verdampfer auf.A designed as a condenser-evaporator heat exchanger has evaporation and Liquefaction passages on. In the evaporation passages becomes a liquid evaporated. They are in heat exchange contact with the liquefaction passages, in which a gaseous fraction in indirect heat exchange with the evaporating Liquid condenses. Details about evaporation processes are for example the monograph "Evaporation and its technical applications" by Billet (1981) refer to. A condenser-evaporator can consist of one or more Heat exchanger blocks be constructed. A condenser-evaporator system points one or more condenser evaporators.

Jahrzehntelang wurden in der Tieftemperaturluftzerlegung praktisch ausschließlich Umlaufverdampfer als Kondensator-Verdampfer eingesetzt. Bei diesem Typ ist ein Wärmetauscherblock in einem Bad der zu verdampfenden Flüssigkeit angeordnet Die Verdampfungspassagen sind oben und unten offen. Flüssigkeit aus dem Bad wird von dem bei der Verdampfung entstehenden Gas nach oben mitgerissen (Thermosiphon-Effekt) und fließt in das Flüssigkeitsbad zurück. Hierdurch ist ein natürlicher Flüssigkeitsumlauf allein durch den Verdampfungsvorgang und ohne Zufuhr mechanischer Energie gegeben.For decades, almost exclusively in the cryogenic air separation Circulating evaporator used as a condenser-evaporator. In this type is a Heat exchanger block arranged in a bath of liquid to be evaporated The Evaporation passages are open at the top and bottom. Liquid from the bath is from entrained upwards in the evaporation of the gas (thermosiphon effect) and flows back into the liquid bath. This is a natural one Liquid circulation solely by the evaporation process and without supply given mechanical energy.

Seit einiger Zeit werden auch Fallfilmverdampfer als Kondensator-Verdampfer in Luftzerlegungsanlagen eingesetzt, wie es beispielsweise in EP 681153 A oder EP 410832 A dargestellt ist. Bei diesem Typ von Verdampfer tritt die zu verdampfende Flüssigkeit oben in die Verdampfungspassagen ein und strömt als relativ dünner Film an den Wänden, die Verdampfungs- und Verflüssigungspassagen trennen, nach unten. Dieser Verdampfertyp weist einen besonders niedrigen Druckverlust in den Verdampfungspassagen auf und ist daher energetisch im allgemeinen günstiger als ein Umlaufverdampfer.For some time, falling film evaporator as a condenser-evaporator in Air separation plants used, as for example in EP 681153 A or EP 410832 A is shown. In this type of evaporator, the evaporates to Liquid enters the top of the evaporation passages and flows as a relatively thin film on the walls, separating the evaporation and liquefaction passages, down. This evaporator type has a particularly low pressure loss in the Evaporation passages and is therefore energetically generally cheaper than a Circulation evaporator.

Allerdings muß bei der Verdampfung einer sauerstoffreichen Flüssigkeit eine totale Verdampfung verhindert werden, die ein Trockenlaufen der Verdampfungspassagen zur Folge hätte. Dazu wird in der Regel aus den Verdampfungspassagen austretende Flüssigkeit mittels einer Pumpe wieder an den Eintritt der Verdampfungspassagen zurückgeführt. Diese Maßnahme wirkt einerseits der energiesparenden Wirkung des Fallfilmverdampfers entgegen; zum anderen werden unerwünschte schwererflüchtige Bestandteile in der Flüssigkeit angereichert.However, in the evaporation of an oxygen-rich liquid must be a total Evaporation can be prevented, which causes dry running of the evaporation passages would result. This is usually exiting from the evaporation passages Liquid by means of a pump back to the entrance of the evaporation passages recycled. On the one hand, this measure has the effect of saving energy Falling film evaporator against; on the other hand are unwanted volatile people Ingredients enriched in the liquid.

Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren der eingangs genannten Art und eine entsprechende Vorrichtung anzugeben, die wirtschaftlich und betriebstechnisch besonders günstig zu betreiben sind und insbesondere einen besonders niedrigen Energieverbrauch aufweisen.The invention is therefore based on the object, a method of the initially mentioned type and to provide a corresponding device that economically and Operationally are particularly favorable to operate and in particular a have particularly low energy consumption.

Diese Aufgabe wird durch die Merkmale des kennzeichnenden Teils des Patentanspruchs 1 gelöst. Die in dem Fallfilmverdampfer (erster Abschnitt des Kondensator-Verdampfer-Systems) nicht verdampfte Flüssigkeit (zweite sauerstoffreiche Flüssigkeit) wird zwar wie bei der üblichen Fallfilmverdampfung einer Fördereinrichtung zugeführt, beispielsweise einer Pumpe; diese transportiert die Flüssigkeit jedoch nicht zurück zum Eintritt der Verdampfungspassagen desselben Fallfilmverdampfers, sondern auf einen zweiten Abschnitt des Kondensator-Verdampfer-Systems. Dadurch braucht der erste Abschnitt nur einen relativ geringen Teil, beispielsweise 30 bis 50 %, vorzugsweise 38 bis 42 %, der gesamten Verdampfungsleistung des Kondensator-Verdampfer-Systems zu übernehmen. Entsprechend groß ist der natürliche Flüssiganteil am Austritt der Verdampfungspassagen des Fallfilmverdampfers. Auf einen künstlichen Flüssigkeitsumlauf kann somit ganz oder weitgehend verzichtet werden. Die Fördereinrichtung läßt die zunächst nicht verdampfte Flüssigkeit weiter zu einem zweiten Abschnitt des Kondensator-Verdampfer-Systems strömen. Dieser ist ganz oder teilweise als Umlaufverdampfer ausgebildet. Dort stellt sich das Problem der Notwendigkeit eines künstlichen Flüssigkeitsumlaufs daher nicht oder nur in geringerem Umfang.This object is achieved by the features of the characterizing part of Patent claim 1 solved. The in the falling film evaporator (first section of the Condenser-evaporator system) non-evaporated liquid (second oxygen-rich liquid) is indeed as in the conventional falling film evaporation of a Supplied conveyor, such as a pump; this transports the Liquid, however, not back to the entry of the evaporation passages of the same Falling film evaporator, but on a second section of the condenser-evaporator system. As a result, the first section needs only a relatively small Part, for example, 30 to 50%, preferably 38 to 42%, of the total Evaporating power of the condenser-evaporator system to take. The natural liquid content at the outlet of the Evaporation passages of the falling film evaporator. On an artificial Liquid circulation can thus be completely or largely dispensed with. The Conveyor allows the initially unevaporated liquid continues to one second section of the condenser-evaporator system. This one is whole or partially designed as a circulation evaporator. There is the problem of Necessity of an artificial fluid circulation therefore not or only in to a lesser extent.

Im Rahmen der Erfindung hat sich herausgestellt, daß sich mit Hilfe der erfindungsgemäßen Maßnahmen die Pumpenmenge auf etwa 30 % reduzieren läßt. Der energetische Effekt der verringerten Pumpenleistung ist dabei nicht auf die Einsparung an Antriebsenergie beschränkt; der Vorteil beruht vielmehr zu einem größeren Teil aus dem verminderten Wärmeeintrag, der sich durch die geringere Fördermenge an zweiter sauerstoffreicher Flüssigkeit ergibt.In the context of the invention has been found that with the help of measures according to the invention can reduce the pump quantity to about 30%. The energetic effect of the reduced pump power is not on the Savings limited to drive energy; the advantage is rather based on one larger part of the reduced heat input, which is due to the lower Flow rate results in the second oxygen-rich liquid.

Das Sauerstoffprodukt wird bei dem erfindungsgemäßen Verfahren vorzugsweise aus dem zweiten Abschnitt des Kondensator-Verdampfer-Systems abgezogen, entweder als Gas oder als Flüssigkeit. Im letzteren Fall kann gegebenenfalls neben einem Flüssigsauerstoffprodukt ein gasförmiges Drucksauerstoffprodukt gewonnen werden, indem sauerstoffreiche Flüssigkeit in flüssigem Zustand auf einen erhöhten Druck gebracht und anschließend gegen Luft oder Stickstoff verdampft wird (sogenannte Innenverdichtung).The oxygen product is preferably in the inventive method subtracted from the second section of the condenser-evaporator system, either as a gas or as a liquid. In the latter case, where appropriate, in addition to a Liquid oxygen product a gaseous pressure oxygen product can be obtained by oxygenated liquid in the liquid state to an elevated pressure brought and then evaporated against air or nitrogen (so-called Internal compression).

Der erste Abschnitt des Kondensator-Verdampfer-Systems der Erfindung kann innerhalb der Niederdrucksäule oder in einem separaten Behälter angeordnet sein.The first portion of the condenser-evaporator system of the invention may be arranged within the low-pressure column or in a separate container.

Das erfindungsgemäße Verfahren und die entsprechende Vorrichtung können zu jeder Art von Stickstoff-Sauerstoff-Trennung eingesetzt werden, insbesondere unabhängig von den Produktreinheiten in den Köpfen und Sümpfen der Säulen. The method and the corresponding apparatus according to the invention can be used for each Type of nitrogen-oxygen separation can be used, especially independently from the product purities in the heads and swamps of the columns.

Der Dampf, der in den Verdampfungspassagen des zweiten Abschnitts des Kondensator-Verdampfer-Systems erzeugt wird, wird vorzugsweise nicht ausschließlich oder hauptsächlich als gasförmiges Sauerstoffprodukt abgezogen, sondern mindestens zur Hälfte in die Niederdrucksäule eingeleitet und dort als aufsteigender Dampf eingesetzt. Falls das gesamte Sauerstoffprodukt flüssig gewonnen und/oder innenverdichtet wird, kann auch das gesamte im zweiten Abschnitt des Kondensator-Verdampfer-Systems erzeugte Gas in die Niederdrucksäule zurückgeführt werden.The vapor that enters the evaporation passages of the second section of the Condenser-evaporator system is generated, preferably not withdrawn exclusively or mainly as a gaseous oxygen product, but at least half initiated in the low-pressure column and there as used ascending steam. If the entire oxygen product is liquid won and / or internally compressed, can also the whole in the second section of the condenser-evaporator system generated gas in the low-pressure column to be led back.

Eine dritte sauerstoffreiche Flüssigkeit verbleibt im zweiten Abschnitt des Kondensator-Verdampfer-Systems als nicht verdampfter Teil der zweiten sauerstoffreichen Flüssigkeit. Sie sammelt sich vorzugsweise im Flüssigkeitsbad des oder eines Umlaufverdampfers. Sie wird bei dem erfindungsgemäßen Verfahren vorzugsweise mindestens teilweise in die Niederdrucksäule und/oder zu den Verdampfungspassagen des ersten Abschnitts des Kondensator-Verdampfer-Systems Flüssigkeit zurückgeleitet. Diese Rückleitung kann auf günstige Weise gemeinsam mit der oben erwähnten Rückführung von Dampf in die Niederdrucksäule durchgeführt werden, indem eine entsprechende Leitung auf Höhe des Flüssigkeitsspiegels des Bads angeordnet ist. Hiermit wird gleichzeitig der Flüssigkeitsstand im Umlaufverdampfer geregelt, ohne daß zusätzliche Stell- oder Regeleinrichtungen erforderlich wären.A third oxygen-rich liquid remains in the second section of the condenser-evaporator system as non-vaporized part of the second oxygen-rich Liquid. It preferably collects in the liquid bath of or one Circulation evaporator. It is preferably used in the process according to the invention at least partially into the low pressure column and / or to the evaporation passages the first section of the condenser-evaporator system liquid returned. This return can be conveniently shared with the above mentioned return of steam are carried out in the low-pressure column, by a corresponding line at the level of the liquid of the bath is arranged. This will simultaneously the liquid level in the circulation evaporator regulated, without additional control or regulating devices would be required.

Wenn der zweite Abschnitt teilweise als zweiter Fallfilmverdampfer ausgebildet ist, kann außerdem die ohnehin vorhandene Fördereinrichtung zwischen erstem und zweitem Abschnitt zusätzlich für die Erzeugung eines Flüssigkeitsumlaufs an dem zweiten Fallfilmverdampfer genutzt werden.If the second section is partially formed as a second falling-film evaporator, In addition, the already existing conveyor between the first and second section additionally for the generation of a liquid circulation at the second falling film evaporator can be used.

Die Verflüssigungspassagen des Kondensator-Verdampfer-Systems sind vorzugsweise so mit den beiden Säulen verbunden, wie es in Patentanspruch 4 beschrieben ist. Dadurch kann an diesen Stellen auf Pumpen verzichtet werden, und zwar auch dann, wenn Drucksäule und Niederdrucksäule nebeneinander angeordnet sind. (In diesem Fall ist es günstig, wenn der erste Abschnitt des Kondensator-Verdampfer-Systems unterhalb des untersten Bodens der Niederdrucksäule und der zweite Abschnitt des Kondensator-Verdampfer-Systems oberhalb des obersten Bodens der Drucksäule angeordnet sind.) The liquefaction passages of the condenser-evaporator system are preferably so connected to the two columns, as in claim 4 is described. This can be dispensed with pumps at these points, and although even if pressure column and low pressure column arranged side by side are. (In this case, it is favorable if the first section of the condenser-evaporator system below the lowest floor of the low pressure column and the second section of the condenser-evaporator system above the top Bottom of the pressure column are arranged.)

Der als Fallfilmverdampfer ausgebildete erste Abschnitt wird dabei vorzugsweise so dimensioniert, daß in ihm diejenige Menge an stickstoffreicher Flüssigkeit durch Kondensation einer stickstoffreichen Gasfraktion aus der Drucksäule erzeugt wird, die als Rücklauf in der Niederdrucksäule benötigt wird (plus gegebenenfalls die als druckloses Flüssigprodukt abgezogenen Menge). Dies stellt beispielsweise einen Anteil 30 bis 50 %, vorzugsweise 38 bis 42 % an der gesamten Wärmeübertragungsleistung des Kondensator-Verdampfer-Systems dar. Der Rest der Wärmeübertragung (50 bis 70 %, vorzugsweise 58 bis 62 %) wird im zweiten Abschnitt des Kondensator-Verdampfer-Systems durchgeführt, und zwar so, daß dort mindestens die als Rücklauf in der Drucksäule benötigte Flüssigkeitsmenge erzeugt wird.The trained as a falling film evaporator first section is preferably so dimensioned that in him the amount of nitrogen-rich liquid through Condensation of a nitrogen-rich gas fraction is generated from the pressure column, the is required as reflux in the low-pressure column (plus, where appropriate, as pressureless liquid product withdrawn amount). This represents, for example, one Share 30 to 50%, preferably 38 to 42% of the total Heat transfer performance of the condenser-evaporator system. The rest of the Heat transfer (50 to 70%, preferably 58 to 62%) is in the second section performed the condenser-evaporator system, in such a way that there generates at least the amount of liquid required as reflux in the pressure column becomes.

Aus Gründen der räumlichen Aufteilung der Heizfläche kann es in manchen Fällen günstiger sein, in dem ersten Abschnitt einen größeren Anteil der stickstoffreichen Fraktion zu kondensieren als oben beschrieben, um entsprechend Heizfläche vom zweiten Abschnitt (in der Regel am Kopf der Drucksäule) zum ersten Abschnitt (in der Regel im Sumpf der Niederdrucksäule zu verlagern. In diesem Fall wird ein Teil der ersten stickstoffreichen Flüssigkeit, die im ersten Abschnitt gebildet wird, als Rücklauf auf die Drucksäule aufgegeben wird. Hierfür ist gegebenenfalls der Einsatz einer Flüssigpumpe erforderlich.For reasons of spatial distribution of the heating surface, it may in some cases be more favorable, in the first section a larger proportion of nitrogen-rich To condense fraction as described above, according to the heating surface of second section (usually at the head of the pressure column) to the first section (in the Usually in the bottom of the low-pressure column to relocate. In this case, part of the first nitrogen-rich liquid formed in the first section as reflux is abandoned on the pressure column. For this purpose, if necessary, the use of a Liquid pump required.

Die stickstoffreiche Gasfraktion wird im allgemeinen durch Kopfstickstoff der Drucksäule gebildet.The nitrogen-rich gas fraction is generally the head nitrogen of the Pressure column formed.

Der erste Abschnitt des Kondensator-Verdampfer-Systems ist vorzugsweise ausschließlich als Fallfilmverdampfer ausgebildet. Mit Hilfe der oben geschilderten Dimensionierung kann er besonders günstig als einzelner, relativ kompakter Block realisiert werden, oder in Form von mehreren (zum Beispiel vier) besonders niedrigen Blöcken, die nebeneinander angeordnet werden. Eine Anordnung unmittelbar im Sumpf der Niederdrucksäule ist ebenfalls günstig für eine niedrige Bauhöhe der Anlage und ihrer Isolierung (Coldbox).The first section of the condenser-evaporator system is preferred designed exclusively as a falling film evaporator. With the help of the above He can dimension particularly well as a single, relatively compact block be realized, or in the form of several (for example four) particularly low Blocks arranged side by side. An arrangement immediately in the Swamp of the low-pressure column is also favorable for a low overall height of the plant and their insulation (coldbox).

Der zweite Abschnitt des Kondensator-Verdampfer-Systems kann durch mindestens zwei verdampfungsseitig seriell verbundene Teilabschnitte gebildet wird, deren erster als Fallfilmverdampfer und deren zweiter als Umlaufverdampfer ausgebildet ist. Die Flüssigkeit, die den Verdampfungspassagen des als Fallfilmverdampfer realisierten Teilabschnitts entströmt, wird dabei zum Beispiel in das Flüssigkeitsbad des oder eines als Umlaufverdampfer verwirklichten Teilabschnitts eingeleitet. Die Fallfilmverdampfer-Umlaufverdampfer-Kombination kann beispielsweise mit durchgehenden Verflüssigungspassagen ausgestattet sein, wie es in EP 795349 A im einzelnen beschrieben ist. In diesem Fall kann die Flüssigkeit aus dem Bad des Umlaufverdampfers in die Niederdrucksäule oder zum Austritt der Verdampfungspassagen des ersten Abschnitts des Kondensator-Verdampfer-Systems zurückgeführt und zur Erhöhung der Flüssigkeitsmenge in dem als Fallfilmverdampfer ausgebildeten Teilabschnitt des zweiten Abschnitts genutzt werden.The second section of the condenser-evaporator system can be replaced by at least two evaporation side serially connected sections is formed, the first as a falling film evaporator and the second is designed as a circulation evaporator. The Liquid that realized the evaporation passages of the falling film evaporator Escapes portion is, for example, in the liquid bath of or one introduced as a circulation evaporator realized section. The falling film evaporator-circulation evaporator combination can, for example, with continuous Be equipped liquefaction passages, as in EP 795349 A in detail is described. In this case, the liquid from the bath of the Circulating evaporator in the low-pressure column or the exit of the Evaporation passages of the first section of the condenser-evaporator system recycled and to increase the amount of liquid in the as a falling film evaporator trained section of the second section are used.

Die Erfindung betrifft außerdem eine Vorrichtung zur Tieftemperaturzerlegung von Luft gemäß Patentanspruch 9. Besonders vorteilhafte Ausgestaltungen der Vorrichtung sind in den Patentansprüchen 10 bis 13 beschrieben.The invention also relates to a device for the cryogenic separation of air according to claim 9. Particularly advantageous embodiments of the device are described in the claims 10 to 13.

Die Erfindung sowie weitere Einzelheiten der Erfindung werden im folgenden anhand zweier in den Zeichnungen schematisch dargestellten Ausführungsbeispiele zur Gewinnung gasförmigen Drucksauerstoffs näher erläutert.The invention and further details of the invention are described below two in the drawings schematically illustrated embodiments of Recovery of gaseous pressure oxygen explained in more detail.

Gemäß Figur 1 wird gasförmige Einsatzluft 1, die zuvor verdichtet, gereinigt und auf etwa Taupunkt abgekühlt wurde (nicht dargestellt), der Drucksäule 2 unmittelbar oberhalb des Sumpfs zugeleitet. Die Drucksäule 2 ist Teil eines Rektifiziersystems, das außerdem eine Niederdrucksäule 3 und einen Hauptkondensator in Form eines Kondensator-Verdampfer-Systems 101, 102, 103 aufweist. Die Luft wird in der Drucksäule 2 in Kopfstickstoff und in eine sauerstoffangereicherte Flüssigkeit zerlegt. Letztere wird bei dem speziellen Ausführungsbeispiel nicht wie sonst üblich am Sumpf, sondern einige theoretische beziehungsweise praktische Böden höher über Leitung 5 abgezogen. (Einzelheiten über diese Verfahrensweise, die zum Zurückhalten von schwererflüchtigen Bestandteilen dient, sind der älteren deutschen Patentanmeldung 19835474 beziehungsweise den zu dieser Anmeldung korrespondierenden Anmeldungen in weiteren Ländern zu entnehmen.) Die sauerstoffangereicherte Flüssigkeit 5 wird über eine nicht dargestellte Leitung an einer Zwischenstelle in die Niederdrucksäule 3 eingedrosselt. According to FIG. 1 , gaseous feed air 1, which has been previously compressed, cleaned and cooled to about the dew point (not shown), is fed to the pressure column 2 immediately above the sump. The pressure column 2 is part of a rectification system, which also has a low pressure column 3 and a main condenser in the form of a condenser-evaporator system 101, 102, 103. The air is decomposed in the pressure column 2 into top nitrogen and into an oxygen-enriched liquid. The latter is not deducted in the special embodiment, as usual at the bottom, but some theoretical or practical floors higher on line 5. (Details of this procedure, which serves to retain less volatile constituents, can be found in the older German patent application 19835474 or the applications corresponding to this application in other countries.) The oxygen-enriched liquid 5 is via a line, not shown at an intermediate point in the low pressure column 3 throttled.

In der Niederdrucksäule 3 werden im oberen Bereich ein oder mehrere Stickstoffprodukte abgezogen (nicht dargestellt). Unterhalb des untersten Rektifizierabschnitts wird Sauerstoff in der für das Produkt benötigten Reinheit gewonnen. Dieser fließt als erste sauerstoffreiche Flüssigkeit vom untersten Boden beziehungsweise Packungsabschnitt der Niederdrucksäule 3 ab und wird in einer Sammeleinrichtung 7 gesammelt. Die erste sauerstoffreiche Flüssigkeit strömt weiter zum oberen Ende des ersten Abschnitts 101 des Kondensator-Verdampfer-Systems und wird in dessen Verdampfungspassagen eingeleitet. Der erste Abschnitt 101 ist als Fallfilmverdampfer ausgebildet. Dort verdampfen etwa 28 bis 30 % der ersten sauerstoffreichen Flüssigkeit 7 in indirektem Wärmeaustausch mit einem ersten Teil 8 der stickstoffreichen Gasfraktion 4 vom Kopf der Drucksäule 2. Dabei kondensiert das stickstoffreiche Gas 8 zu einer ersten stickstoffreichen Flüssigkeit 9. Diese wird in einem Drosselventil 10 entspannt und vollständig als Rücklauf auf den Kopf der Niederdrucksäule 3 aufgegeben. Da bei dem Beispiel kein flüssiges Stickstoffprodukt erzeugt wird, ist der Fallfilmverdampfer 101 so dimensioniert, daß in ihm genau diejenige Menge an stickstoffreichem Gas 8 kondensiert, die als Rücklaufflüssigkeit für die Niederdrucksäule benötigt wird.In the low-pressure column 3, one or more are in the upper area Nitrogen products withdrawn (not shown). Below the bottom Rectification section becomes oxygen in the purity required for the product won. This flows as the first oxygen-rich liquid from the bottom or packing section of the low-pressure column 3 and is in a Collecting device 7 collected. The first oxygen-rich liquid continues to flow to the upper end of the first section 101 of the condenser-evaporator system and is introduced into its evaporation passages. The first section 101 is as Falling film evaporator formed. There, about 28 to 30% of the first evaporate oxygen-rich liquid 7 in indirect heat exchange with a first part 8 the nitrogen-rich gas fraction 4 from the head of the pressure column 2. This condenses the nitrogen-rich gas 8 to a first nitrogen-rich liquid 9. This is in a throttle valve 10 is relaxed and completely as return to the head of the Low pressure column 3 abandoned. Because in the example no liquid nitrogen product is generated, the falling film evaporator 101 is dimensioned so that in him exactly condenses the amount of nitrogen-rich gas 8, which is used as reflux liquid for the low pressure column is needed.

Der Dampf 11, der im ersten Abschnitt 101 des Kondensator-Verdampfer-Systems erzeugt wird, strömt zum untersten Rektifizierabschnitt der Niederdrucksäule zurück und nimmt an dem Gegenstrom-Stoffaustausch innerhalb dieser Säule teil. Der flüssig verbleibende Anteil 12 bildet eine zweite sauerstoffreiche Flüssigkeit. Diese wird über Leitung 13 abgezogen und mittels einer Pumpe 14 zu dem zweiten Abschnitt des Kondensator-Verdampfers geführt, der durch eine Kombination aus einem weiteren Fallfilmverdampfer 102 und einem Umlaufverdampfer 103 gebildet wird, wie sie in EP 795349 A im einzelnen beschrieben ist.The vapor 11 in the first section 101 of the condenser-evaporator system is generated, flows back to the lowest rectification section of the low-pressure column and participates in the countercurrent mass transfer within this column. The liquid remaining portion 12 forms a second oxygen-rich liquid. This is about Withdrawn line 13 and by means of a pump 14 to the second section of the Condenser evaporator led by a combination of another Falling film evaporator 102 and a circulation evaporator 103 is formed, as in EP 795349 A is described in detail.

Die zweite sauerstoffreiche Flüssigkeit strömt in den Verdampfungspassagen des weiteren Fallfilmverdampfers 102 nach unten und verdampft dort zu etwa 40 %. Der entstandene Dampf 15 wird vollständig über Leitung 16 in die Niederdrucksäule 3 zurückgeleitet, da in dem Beispiel kein Sauerstoff als gasförmiges Produkt direkt aus dem Rektifiziersystem abgeführt wird. Die Leitung 16 dient gleichzeitig zum Konstanthalten des Flüssigkeitsspiegels im Flüssigkeitsbad 18, indem überschüssige Flüssigkeit gemeinsam mit dem im zweiten Abschnitt 102, 103 erzeugten Dampf zur Niederdrucksäule 3 geführt wird. (Diese Funktion wird anhand der Detailzeichnung von Figur 2 unten näher erläutert.) Die verbleibende Flüssigkeit 17 aus dem Teilabschnitt 102 fließt in das Flüssigkeitsbad 18 des Umlaufverdampfers 103 und bildet zusammen mit der im Umlaufverdampfer umgeworfenen Flüssigkeit 19 eine dritte sauerstoffreiche Flüssigkeit. Diese wird als Sauerstoffprodukt gewonnen, indem sie zum Teil über Leitung 20 abgezogen, mittels einer Pumpe 21 innenverdichtet, auf die bekannte Weise unter erhöhtem Druck verdampft und schließlich als gasförmiges Druckprodukt herausgeführt wird. Falls als Wärmeträger für die Verdampfung des Produktsauerstoffs ein Teil der Einsatzluft eingesetzt wird, kann der dabei verflüssigte Luftstrom 24 an einer Zwischenstelle in die Drucksäule 2 eingeführt werden. Alternativ oder zusätzlich ist es möglich, einen auf über Drucksäulendruck gebrachten Stickstoffstrom gegen den verdampfenden Produktsauerstoff zu kondensieren (Stickstoffkreislauf, nicht dargestellt).The second oxygen-rich liquid flows into the evaporation passages of the further falling film evaporator 102 down and evaporates there to about 40%. Of the resulting steam 15 is completely via line 16 in the low pressure column. 3 returned, since in the example no oxygen as gaseous product directly from the rectification system is discharged. The line 16 is used for the same time Keeping constant the liquid level in the liquid bath 18, by excess Liquid together with the steam generated in the second section 102, 103 for Low pressure column 3 is guided. (This function is based on the detail drawing of Figure 2 explains in more detail below.) The remaining liquid 17 from the section 102 flows into the liquid bath 18 of the circulation evaporator 103 and forms together with the overturned in the circulation evaporator liquid 19, a third oxygen-rich Liquid. This is obtained as an oxygen product by partly over Deducted line 20, internally compressed by a pump 21, the well-known Evaporated under increased pressure and finally as a gaseous pressure product is led out. If used as a heat transfer medium for the evaporation of the product oxygen Part of the feed air is used, the thereby liquefied air flow 24 at an intermediate point are introduced into the pressure column 2. Alternatively or in addition It is possible, a brought about pressure column pressure nitrogen flow against the evaporating product oxygen to condense (nitrogen cycle, not ) Shown.

Die Verflüssigungspassagen des weiteren Fallfilmverdampfers 102 und des Umlaufverdampfers 103 sind durchgehend ausgeführt. Sie werden von einem zweiten Teil 22 der stickstoffreichen Gasfraktion 4 aus der Drucksäule 2 beaufschlagt. Der Stickstoff strömt zunächst durch den Fallfilmverdampfer 102 und anschließend durch den Umlaufverdampfer 103 und kondensiert mindestens teilweise, vorzugsweise praktisch vollständig. Die dabei entstandene zweite stickstoffreiche Flüssigkeit 23 wird vollständig als Rücklauf auf die Drucksäule 2 aufgegeben.The liquefaction passages of the further falling film evaporator 102 and the Circulating evaporator 103 are executed continuously. You will be of a second Part 22 of the nitrogen-rich gas fraction 4 from the pressure column 2 acted upon. Of the Nitrogen initially flows through the falling film evaporator 102 and then through the circulation evaporator 103 and condenses at least partially, preferably practically complete. The resulting second nitrogen-rich liquid 23 is completely abandoned as reflux to the pressure column 2.

Figur 2 zeigt im Detail die Verbindung zwischen der Leitung 16 und dem Außenraum um die beiden Kondensator-Verdampfer 102, 103, die den zweiten Abschnitt des Kondensator-Verdampfer-Systems bilden. Die Dimensionen der Leitung werden im wesentlichen nach der zu transportierenden Gasmenge ausgelegt. Sie wird so angeordnet, daß Flüssigkeit aus dem Flüssigkeitsbad des Umlaufverdampfers 103 überlaufen und als Film 26 an der Unterseite der Leitung 16 in die Niederdrucksäule 3 beziehungsweise in den Flüssigkeitssumpf unterhalb des ersten Fallfilmverdampfers 101 zurückfließen kann. Hierdurch wird der Flüssigkeitsspiegel des Flüssigkeitsbads des Umlaufverdampfers 103 ohne spezielle Regelmaßnahmen auf konstanter Höhe gehalten. Figure 2 shows in detail the connection between the conduit 16 and the outer space around the two condenser-evaporators 102, 103, which form the second section of the condenser-evaporator system. The dimensions of the line are designed essentially according to the amount of gas to be transported. It is arranged so that liquid from the liquid bath of the circulation evaporator 103 can overflow and flow back as a film 26 at the bottom of the line 16 in the low pressure column 3 and in the liquid sump below the first falling film evaporator 101. As a result, the liquid level of the liquid bath of the circulation evaporator 103 is kept at a constant level without special control measures.

Figur 3 unterscheidet sich von Figur 1 durch eine zusätzliche Leitung 301, über die ein Teil der ersten stickstoffreichen Flüssigkeit 9 als Rücklauf auf die Drucksäule 2 aufgegeben werden kann. Bei der dargestellten Anordnung von Säulen und Kondensatoren ist eine Flüssigpumpe 302 zur Überwindung der statischen Höhe zwischen erstem Abschnitt 101 des Kondensator-Verdampfer-Systems und oberem Bereich der Drucksäule 2 notwendig. Mit Hilfe dieser Überleitung von Flüssigkeit in die Drucksäule kann bei der Variante von Figur 3 gegenüber Figur 1 mehr Heizfläche in den ersten Abschnitt 101 verlegt werden, der hier als Sumpfverdampfer der Niederdrucksäule 3 ausgebildet ist. Entsprechend weniger Heizfläche (und damit weniger Volumen) wird für den zweiten Abschnitt 102, 103 benötigt, in dem Beispiel am Kopf der Drucksäule 2. Hierdurch kann die räumliche Aufteilung des Kondensator-Verdampfer-Systems optimiert werden. Der Vorteil dieser Optimierung ist in vielen Fällen höher als der Aufwand für die zusätzliche Leitung 301 und die Flüssigpumpe 302.FIG. 3 differs from FIG. 1 by an additional line 301 via which a Part of the first nitrogen-rich liquid 9 as reflux to the pressure column. 2 can be abandoned. In the illustrated arrangement of columns and Capacitors is a liquid pump 302 for overcoming the static level between the first section 101 of the condenser-evaporator system and upper Area of the pressure column 2 necessary. With the help of this transfer of liquid into the Pressure column can in the variant of Figure 3 over Figure 1 more heating surface in be laid the first section 101, here as the bottom evaporator of Low pressure column 3 is formed. Correspondingly less heating surface (and thus less volume) is needed for the second section 102, 103, in the example on Head of the pressure column 2. This allows the spatial distribution of the condenser-evaporator system be optimized. The benefit of this optimization is in many Cases higher than the cost of the additional line 301 and the liquid pump 302nd

In einem extremen Beispiel (in der Zeichnung nicht dargestellt), kann die gesamte Heizfläche des Teilabschnitts 102 in den ersten Abschnitt 101 integriert werden, so daß der zweite Abschnitt des Kondensator-Verdampfer-Systems nur noch aus einem Umlaufverdampfer 103 besteht.In an extreme example (not shown in the drawing), the entire Heating surface of the portion 102 are integrated into the first section 101, so that the second section of the condenser-evaporator system only one Circulation evaporator 103 exists.

Claims (13)

  1. Process for the low-temperature fractionation of air, in which compressed and pre-purified feed air (1) is introduced into a rectification system for nitrogen/oxygen separation, which includes
    a pressure column (2),
    a low-pressure column (3), and
    a condenser-evaporator system (101, 102, 103) for heating the low-pressure column (3),
    wherein
    the condenser-evaporator system has a first section (101), which is designed as a falling-film evaporator,
    a first oxygen-rich liquid (6) from the low-pressure column (3) is introduced into the evaporation passages of the falling-film evaporator (101), where it is partially evaporated, with an oxygen-rich vapour (11) and a second oxygen-rich liquid (12) being formed, and
       wherein
    the oxygen-rich vapour (11) is at least partially passed back into the low-pressure column (3),
    characterized in that the condenser-evaporator system includes a second section (102, 103) which is at least partially designed as a forced-circulation evaporator (103), and in that the second oxygen-rich liquid (12, 13) is at least partially passed, by means of a delivery device (14) to the evaporation passages of the second section (102, 103) of the condenser-evaporator system.
  2. Process according to Claim 1, characterized in that at least half of the vapour produced in the evaporation passages of the second section of the condenser-evaporator system is introduced (16) into the low-pressure column (3).
  3. Process according to Claim 1 or 2, characterized in that a third oxygen-rich liquid (18), which is formed from that part of the second oxygen-rich liquid (12, 13) which has not evaporated in the second section (102, 103) of the condenser-evaporator system, is at least partially passed back (16) into the low-pressure column (3) and/or to the evaporation passages of the first section (101) of the condenser-evaporator system.
  4. Process according to any of Claims 1 to 3, characterized in that
    a nitrogen-rich gas fraction (4) is produced in the upper region of the pressure column (2),
    a first part (8) of the nitrogen-rich gas fraction (4) is introduced into the liquefaction passages of the first section (101) of the condenser-evaporator system, where it is at least partially condensed, with a first nitrogen-rich liquid (9) being formed,
    a second part (22) of the nitrogen-rich gas fraction (4) is introduced into the liquefaction passages of the second section (102, 103) of the condenser-evaporator system, where it is at least partially condensed, with a second nitrogen-rich liquid (23) being formed,
    the first nitrogen-rich liquid (9) is at least partially expanded (10) and added as reflux to the low-pressure column (3) and,
    the second nitrogen-rich liquid (23) is at least partially added as reflux to the pressure column (2).
  5. Process according to Claim 4, characterized in that part of the first nitrogen-rich liquid (9) is added (301, 302) as reflux to the pressure column (2).
  6. Process according to any of Claims 1 to 5, characterized in that pressure column (2) and low-pressure column (3) are arranged next to one another, with the first section (101) of the condenser-evaporator system being arranged beneath the bottom plate or the bottom packing section of the low-pressure column (3) and/or the second section of the condenser-evaporator system being arranged above the top plate or the top packing section of the pressure column (2).
  7. Process according to any of Claims 1 to 6, characterized in that the first section (101) of the condenser-evaporator system is designed exclusively as a falling-film evaporator.
  8. Process according to any of Claims 1 to 7, characterized in that the second section of the condenser-evaporator system is formed by at least two subsections which are connected in series on the evaporation side and at least one of which is designed as a falling-film evaporator (102) and at least one of which is designed as a forced-circulation evaporator (103).
  9. Apparatus for the low-temperature fractionation of air having a rectification system for nitrogen/oxygen separation, which includes
    a pressure column (2),
    a low-pressure column (3), and
    a condenser-evaporator system (101, 102, 103) for heating the low-pressure column (3),
    wherein
    the condenser-evaporator system has a first section (101), which is designed as a falling-film evaporator,
    and having
    a feed air line (1) for introducing compressed and pre-purified feed air (1) into the pressure column (2),
    means for feeding a first oxygen-rich liquid (6) out of the low-pressure column (3) into the evaporation passages of the falling-film evaporator (101), and
    means for returning oxygen-rich vapour (11) from the evaporation passages of the falling-film evaporator (101) into the low-pressure column (3),
    characterized in that the condenser-evaporator system includes a second section (102, 103) which is at least partially designed as a forced-circulation evaporator (103), and the apparatus includes means for introducing a second oxygen-rich liquid (12, 13) from the evaporation passages of the falling-film evaporator (101) to the evaporation passages of the second section (102, 103) of the condenser-evaporator system, which comprise a delivery device (14).
  10. Apparatus according to Claim 9, characterized in that pressure column (2) and low-pressure column (3) are arranged next to one another, with the first section (101) of the condenser-evaporator system being arranged beneath the bottom plate or the bottom packing section of the low-pressure column (3) and/or the second section of the condenser-evaporator system being arranged above the top plate or the top packing section of the pressure column (2).
  11. Apparatus according to Claim 9 or 10, characterized in that the first section (101) of the condenser-evaporator system is designed exclusively as a falling-film evaporator.
  12. Apparatus according to any of Claims 9 to 11, characterized in that the second section of the condenser-evaporator system is formed by at least two subsections which are connected in series on the evaporation side and the first of which is designed as a falling-film evaporator (102) and the second of which is designed as a forced-circulation evaporator (103).
  13. Apparatus according to any of Claims 9 to 11, characterized in that the outlet (9) of the liquefaction passages of the first section (101) of the condenser-evaporator system is connected, via a liquid line (301) and if appropriate via a liquid pump (302), to the pressure column (2).
EP00119941A 1999-10-20 2000-09-13 Process and device for cryogenic air separation Revoked EP1094286B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP00119941A EP1094286B1 (en) 1999-10-20 2000-09-13 Process and device for cryogenic air separation

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE19950570 1999-10-20
DE19950570A DE19950570A1 (en) 1999-10-20 1999-10-20 Low temperature decomposition of air comprises using rectification system consisting of condenser-vaporizer system, pressure column and low pressure column
EP00102564 2000-02-07
EP00102564 2000-02-07
EP00119941A EP1094286B1 (en) 1999-10-20 2000-09-13 Process and device for cryogenic air separation

Publications (2)

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EP1094286A1 EP1094286A1 (en) 2001-04-25
EP1094286B1 true EP1094286B1 (en) 2005-06-15

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DE (1) DE50010552D1 (en)
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Publication number Priority date Publication date Assignee Title
DE10113790A1 (en) 2001-03-21 2002-09-26 Linde Ag Three-column system for low-temperature air separation
EP3910274A1 (en) * 2020-05-13 2021-11-17 Linde GmbH Method for the low-temperature decomposition of air and air separation plant

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DE2402246A1 (en) * 1974-01-18 1975-07-31 Linde Ag PROCESS FOR THE RECOVERY OF OXYGEN OF MEDIUM PURITY
FR2650379B1 (en) * 1989-07-28 1991-10-18 Air Liquide VAPORIZATION-CONDENSATION APPARATUS FOR DOUBLE AIR DISTILLATION COLUMN, AND AIR DISTILLATION INSTALLATION COMPRISING SUCH AN APPARATUS
GB9016766D0 (en) * 1990-07-31 1990-09-12 Boc Group Plc Boiling liquefied gas
DE19605500C1 (en) * 1996-02-14 1997-04-17 Linde Ag Liquid oxygen generator process assembly
US5775129A (en) * 1997-03-13 1998-07-07 The Boc Group, Inc. Heat exchanger
US5761927A (en) * 1997-04-29 1998-06-09 Air Products And Chemicals, Inc. Process to produce nitrogen using a double column and three reboiler/condensers

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ATE298070T1 (en) 2005-07-15
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EP1094286A1 (en) 2001-04-25

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