EP3327393A1 - Procédé et dispositif de production d'un flux de produit d'oxygène ultrapur par cryogénie de séparation d'air - Google Patents

Procédé et dispositif de production d'un flux de produit d'oxygène ultrapur par cryogénie de séparation d'air Download PDF

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EP3327393A1
EP3327393A1 EP16020468.1A EP16020468A EP3327393A1 EP 3327393 A1 EP3327393 A1 EP 3327393A1 EP 16020468 A EP16020468 A EP 16020468A EP 3327393 A1 EP3327393 A1 EP 3327393A1
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Prior art keywords
column
pure oxygen
mass transfer
oxygen
transfer section
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EP16020468.1A
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German (de)
English (en)
Inventor
Dimitri GOLUBEV
Stefan Dowy
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Linde GmbH
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Linde GmbH
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Priority to EP16020468.1A priority Critical patent/EP3327393A1/fr
Priority to DE102017010786.6A priority patent/DE102017010786A1/de
Publication of EP3327393A1 publication Critical patent/EP3327393A1/fr
Withdrawn legal-status Critical Current

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    • 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
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • F25J3/04715—The auxiliary column system simultaneously produces oxygen
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    • 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
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Definitions

  • the invention relates to a method for obtaining a high-purity oxygen product stream by cryogenic separation of air according to the preamble of patent claim 1.
  • the distillation column system for nitrogen-oxygen separation can be designed as a two-column system (for example as a classic Linde double column system), or as a three or more column system.
  • Fig.2 from US 4977746 a method of the type mentioned above with a classic double column, a classic crude argon column and a pure oxygen column is known, which is connected to the crude argon column.
  • a high purity oxygen product stream can be recovered that is largely free of less volatile components.
  • no oxygen-free crude argon can be obtained in this system, but the simple crude argon column is too short.
  • an oxygen content in the percentage range at the top of the crude argon column can be achieved here;
  • the crude argon column then required two pumps, one from the intermediate point of the crude argon column to the top of the pure oxygen column and one from the bottom of the crude argon column to the low pressure column.
  • the invention is therefore based on the object of obtaining both a high-purity oxygen product stream and oxygen-free crude argon without the need for a particularly complex apparatus.
  • the argon transition stream (the "Argon-enriched stream”) is not introduced as usual in the crude argon column, but in the pure oxygen column, at an intermediate point.
  • the upper mass transfer section of the pure oxygen column above the intermediate point also serves for the removal of methane and less volatile components and the argon-oxygen separation.
  • the feed gas for the crude argon column comes from the top of the pure oxygen column and is already enriched in argon (from 11.3% to 15.3% argon, for example).
  • the crude argon column for the production of oxygen-free Rohargon can be made correspondingly smaller and one-piece.
  • oxygen-free is meant here an oxygen content of less than 10 ppm, preferably less than 1 ppm.
  • methane-free oxygen fraction is simultaneously obtained, which is fed to the pure oxygen mass transfer section of the pure oxygen column, from the bottom of which the high-purity oxygen product stream is withdrawn.
  • This oxygen fraction is referred to below as methane-free.
  • methane-free is meant here a methane content which is below 0.1 ppm, for example below 10 ppb, preferably below 1 ppm.
  • the pure oxygen column can consist of two containers which have the pure oxygen mass transfer section or the upper mass transfer section for hydrocarbon removal.
  • the pure oxygen column is realized as a continuous container, in which the ascending gas is passed without pipelines at the intermediate point. In this way, the Verrohrungsaufwand can be reduced.
  • the upper mass transfer section of the pure oxygen column can be formed by structured packing (also referred to as "ordered packing” in German) and the pure oxygen mass transfer section by conventional rectification trays. In this way, the two corresponding column sections may have the same or similar diameter despite different throughput.
  • a packing density of 350 to 750 m 2 / m 3 is used in the upper mass transfer section.
  • the rectification soils are preferably realized by sieve trays.
  • both the upper mass transfer section of the pure oxygen column and the pure oxygen mass transfer section are formed by structured packing.
  • the packing is then preferably designed as a copper packing, ie the sheets from which the packing is made have a copper content of at least 95 mol%, in particular of at least 99%.
  • the packing density in the pure oxygen mass transfer section (7) of the pure oxygen column (5) is more than 1000 m 2 / m 3 and that in the upper mass transfer section (6) of the pure oxygen column (5) is less than 800 m 2 / m 3 ,
  • the invention also relates to a device according to claim 12.
  • the device according to the invention can be supplemented by device features which correspond to the characteristics of individual, several or all dependent method claims.
  • This double column here forms the distillation column system for nitrogen-oxygen separation. It is classically designed with high-pressure column 1 under a main condenser 2, which is located at the lower end of a low-pressure column 3.
  • a gaseous intermediate fraction from the low-pressure column forms the argon-enriched stream 4 from the distillation column system for nitrogen-oxygen separation and is fed to the pure oxygen column 5 at an intermediate point.
  • the inflowing gas flows into the upper mass transfer section 6 of the pure oxygen column 5, where it is depleted of oxygen and methane.
  • the upper mass transfer section 6 thus simultaneously forms the first section of the argon-oxygen separation which otherwise takes place in the following crude argon column 10. This is applied in the sump with the head gas 9 of the pure oxygen column.
  • the crude argon column 10 has a top condenser 11 in which the overhead gas of the crude argon column is completely liquefied except for the crude argon product stream 12.
  • the raw argon product gas 12 is further processed here in a classical pure argon column 13 with removal of the residual nitrogen.
  • a high purity argon product HLAR is withdrawn via line 14 from the bottom of the pure argon column 13.
  • the bottom liquid 15 of the crude argon column is introduced by means of a pump 16 into the pure oxygen column 5, namely at two different locations.
  • a first part 17 is led to the head of the pure oxygen column 5 and there introduced as reflux liquid to the upper mass transfer section 5;
  • a second part 18 of the bottom liquid 15 of the crude argon column 10 is used as a methane-free liquid oxygen fraction and applied to the top of a pure oxygen mass transfer section 7 of the pure oxygen column 5, which is located below the intermediate point is located at which the argon-enriched stream 4 is introduced from the low-pressure column 3.
  • This liquid forms the reflux in the pure oxygen mass transfer section 7.
  • both mass transfer sections 6, 7 of the pure oxygen column 5 are formed by structured packing, the lower mass transfer section 7 having two packing beds, the upper mass transfer section 6 of a.
  • the upper mass transfer section 6 is operated with a lower packing density (specific surface area) than that under 7.
  • the packing density is, for example, 500 m 2 / m 3 in the upper mass transfer section 6 and 1200 m 2 / m 3 in the lower mass transfer section 7.
  • a "similar column diameter is understood here to mean a difference in column diameters of less than 40%. in which the liquid oxygen or the high purity oxygen product stream are only byproducts of relatively small amount (for example, in a system with internally compressed oxygen as the main product), the difference in the column diameters can also be higher.
  • the top condenser 11 of the crude argon column is conventionally cooled by means of oxygen-enriched bottom liquid 22, 23, 24 from the high-pressure column 1 or the subcooling countercurrent 19.
  • the heating of the sump evaporator 8 of the pure argon column is carried out with a partial flow 25 of the cold feed air 26 under high-pressure column pressure.
  • Atmospheric air AIR is drawn in via a line 27 and a filter 28 from a main air compressor and brought there to a pressure of about 6 bar.
  • the compressed air is cooled in a pre-cooler, which is formed here by a direct contact cooler, and cleaned in a cleaning device, which is formed by a pair of switchable molecular sieve adsorber.
  • the purified high-pressure air 32 is introduced into a main heat exchanger 33 and cooled there to about dew point.
  • the cold feed air 26 flows in gaseous form into the high-pressure column 1 via line 77.
  • a part 25 is used in this embodiment for heating the sump of the pure oxygen column 5.
  • the liquid air 34 from the sump evaporator 8 is introduced via line 35 into the evaporation space of the top condenser 36 of the pure argon column 13.
  • a first part 37 of the top gas of the high-pressure column is liquefied in the main condenser 2.
  • This liquid nitrogen obtained is partly used as reflux in the high pressure column 1, partially withdrawn via line 39, cooled in the subcooling countercurrent 19 and withdrawn via lines 40 and 41 as a high purity liquid nitrogen product HLIN.
  • the remainder 42 of the overhead gas is warmed in the main heat exchanger 33 and fed via line 43 for use as a sealing gas (seal gas).
  • stream 43 may be withdrawn as part of stream 50 from an intermediate location of the high pressure column and warmed in the main heat exchanger.
  • the oxygen-enriched bottom liquid 22, 23 is used in a conventional manner for heating and cooling the pure argon column 13 and for cooling the crude argon column 10. Steam 44 and liquids 45/46 from the respective capacitors are introduced separately into the low-pressure column 3.
  • a somewhat less pure nitrogen liquid 47 having, for example, 1 ppm oxygen content is withdrawn from an intermediate point of the high-pressure column and, after supercooling 19, fed via line 48/49 as reflux liquid to the top of the low-pressure column 3.
  • a gaseous nitrogen stream 50 is withdrawn and fed into a nitrogen cycle consisting of a feed gas compressor 51 with aftercooler 52, a cycle compressor 53 with aftercooler 54, two serial turbine-driven booster 55, 56, with aftercoolers 57, 58, two nitrogen turbines 59, 60, a separator 61 and the left part of the main heat exchanger 33 shown in the drawing consists.
  • the invention works in principle, regardless of the specific design of the high-pressure column - for example, with or without pure nitrogen section - and regardless of the nitrogen cycle and in particular its entry and exit points to the high-pressure column.
  • Liquid generated in the nitrogen cycle is fed on the one hand via line 62 into the high-pressure column, on the other hand via lines 63, 49 into the low-pressure column 3.
  • Gaseous nitrogen 64 from the top of the low-pressure column 3 is heated in the supercooling countercurrent 19 and further (line 65) in the main heat exchanger 33 to about ambient temperature.
  • a first portion 66 of the warm impure nitrogen may be introduced via the feed gas compressor 51 into the circuit; another part 67 serves as a cooling gas for an evaporative cooler 72 for cooling cooling water 73.
  • the gaseous oxygen product 68 from the low-pressure column 3 is mixed here with the residual gas 69 from an intermediate point of the low-pressure column 3.
  • the mixture 70 is warmed in the main heat exchanger and finally used as regeneration gas 71 or blown off into the atmosphere ATM.
  • FIG. 2 is different from this FIG. 1 in that the low-pressure column 3 has an additional mass transfer section between the residual gas outlet 69 and the liquid feed 45.
  • the liquid air 34/235 from the liquefaction space of the bottom evaporator 8 of the pure oxygen column 5 is introduced here into the intermediate point which is thus created.
  • the required process and liquefaction refrigerants are not generated in a nitrogen cycle, but by the work-performing expansion of part of the feed air in one or more turbines.
  • the main products are in this process Oxygen products and not nitrogen products as in the other embodiments, each having a nitrogen cycle.
  • the cold generated thereby is registered for the most part by a liquid air stream 301 in the distillation column system, which is introduced into the high-pressure column 1.
  • a part 302 is removed immediately, cooled in the subcooling countercurrent 319 and introduced via line 303 together with the liquid air 34/235 from the evaporator 8 in the low pressure column.
  • FIG. 4 is again largely identical to FIG. 1 ; However, the sump evaporator 8 of the pure oxygen column 5 is not cooled here with air, but with a portion 451 of the gaseous nitrogen stream 450 from the high-pressure column. The liquid nitrogen 452 obtained in this process is fed via lines 453, 449 into the low-pressure column.
  • FIG. 5 In the lower mass transfer section 507 of the pure oxygen column 5, conventional rectification trays, for example sieve trays, are used, whereas in the embodiments described so far only structured packings were used. In this way, the different load in the upper 6 and lower mass transfer section 507 can be compensated.
  • the packing density in the upper mass transfer section 6 is 500 m 2 / m 3 . Otherwise it is different FIG. 5 not from FIG. 1 ,

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EP16020468.1A 2016-11-25 2016-11-25 Procédé et dispositif de production d'un flux de produit d'oxygène ultrapur par cryogénie de séparation d'air Withdrawn EP3327393A1 (fr)

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EP16020468.1A EP3327393A1 (fr) 2016-11-25 2016-11-25 Procédé et dispositif de production d'un flux de produit d'oxygène ultrapur par cryogénie de séparation d'air
DE102017010786.6A DE102017010786A1 (de) 2016-11-25 2017-11-22 Verfahren und Vorrichtung zur Gewinnung eines Hochreinsauerstoffproduktstroms durch Tieftemperaturzerlegung von Luft

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Publication number Priority date Publication date Assignee Title
WO2021078405A1 (fr) * 2019-10-23 2021-04-29 Linde Gmbh Procédé et système pour la séparation d'air à basse température
WO2021204424A3 (fr) * 2020-04-09 2021-12-02 Linde Gmbh Procédé de séparation d'air à basse température, installation de séparation d'air et ensemble composé d'au moins deux installations de séparation d'air
WO2023030679A1 (fr) * 2021-09-01 2023-03-09 Linde Gmbh Procédé de séparation à basse température de l'air et station de séparation d'air
WO2024052279A1 (fr) * 2022-09-06 2024-03-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Unité de séparation d'air et procédé de séparation d'air

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US4977746A (en) 1989-01-20 1990-12-18 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and plant for separating air and producing ultra-pure oxygen
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US4977746A (en) 1989-01-20 1990-12-18 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and plant for separating air and producing ultra-pure oxygen
EP0467395A1 (fr) * 1990-07-20 1992-01-22 Praxair Technology, Inc. Densité variable d'un garnissage profilé d'un système de destillation cryogénique
DE10152356A1 (de) * 2001-10-24 2002-12-12 Linde Ag Verfahren und Vorrichtung zur Gewinnung von Argon und hoch reinem Sauerstoff durch Tieftemperatur-Zerlegung
EP3067649A1 (fr) * 2015-03-13 2016-09-14 Linde Aktiengesellschaft Système de colonnes de distillation et procédé de production d'oxygène par séparation cryogénique de l'air

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021078405A1 (fr) * 2019-10-23 2021-04-29 Linde Gmbh Procédé et système pour la séparation d'air à basse température
WO2021204424A3 (fr) * 2020-04-09 2021-12-02 Linde Gmbh Procédé de séparation d'air à basse température, installation de séparation d'air et ensemble composé d'au moins deux installations de séparation d'air
WO2023030679A1 (fr) * 2021-09-01 2023-03-09 Linde Gmbh Procédé de séparation à basse température de l'air et station de séparation d'air
WO2024052279A1 (fr) * 2022-09-06 2024-03-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Unité de séparation d'air et procédé de séparation d'air

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