EP2381197B1 - Verfahren und Gerät zur Stickstoffherstellung durch Tieftemperaturdestillation von Luft - Google Patents

Verfahren und Gerät zur Stickstoffherstellung durch Tieftemperaturdestillation von Luft Download PDF

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Publication number
EP2381197B1
EP2381197B1 EP11160944.2A EP11160944A EP2381197B1 EP 2381197 B1 EP2381197 B1 EP 2381197B1 EP 11160944 A EP11160944 A EP 11160944A EP 2381197 B1 EP2381197 B1 EP 2381197B1
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EP
European Patent Office
Prior art keywords
column
air
flow rate
nitrogen
carbon monoxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Not-in-force
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EP11160944.2A
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English (en)
French (fr)
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EP2381197A1 (de
Inventor
Patrick Le Bot
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Publication of EP2381197A1 publication Critical patent/EP2381197A1/de
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/044—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 single pressure main column system only
    • 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • 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
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04793—Rectification, e.g. columns; Reboiler-condenser
    • 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
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/0655—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of hydrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/44—Separating high boiling, i.e. less volatile components from nitrogen, e.g. CO, Ar, O2, hydrocarbons

Definitions

  • the present invention relates to a method and apparatus for producing nitrogen by cryogenic distillation.
  • the pharmacy industry is a potential market for nitrogen sales.
  • the CO content in the nitrogen produced is about 80% of the CO content in the air supplying the simple column.
  • An object of the invention is to allow the production of very low carbon monoxide nitrogen by cryogenic distillation of air even when the air supplying the column is occasionally polluted with carbon monoxide.
  • a method for producing nitrogen by cryogenic distillation of air in which air containing carbon monoxide is sent to a cryogenic distillation column, a nitrogen flow D is withdrawn at the top of the distillation column, with a CO content lower than a fixed value S1, and a cryogenic liquid flow rich in nitrogen from an external source is sent to the top of the column, the flow of cryogenic liquid sent to the column being less than a value V if the CO content in the air does not exceed a previously defined threshold (SO), characterized in that: the flow of cryogenic liquid sent to the column is greater than a value V if the carbon monoxide content of the air exceeds this previously defined threshold (S0).
  • SO previously defined threshold
  • an apparatus for producing nitrogen by cryogenic distillation comprising a cryogenic distillation column, a pipe for sending air containing carbon monoxide to the column, a pipe for withdrawing a carbon dioxide. product rich in nitrogen from the column, a pipe for sending liquid nitrogen from an external source, for example a storage, to the column characterized in that it comprises means for regulating the flow of liquid nitrogen sent to the column according to the carbon monoxide content of the air, means for measuring the carbon monoxide content of the air or the nitrogen-rich product and means for increasing the flow of liquid nitrogen sent to the column if the content exceeds a threshold.
  • the proposed invention makes it possible to significantly increase the limit concentration of CO in the air beyond which it is no longer possible to produce sufficiently pure nitrogen gas from the air separation apparatus.
  • An air flow 1 purified in CO 2 and in moisture but containing carbon monoxide is cooled in a heat exchanger 2. Its carbon monoxide content is measured by an analyzer 3 upstream of the distillation column 5.
  • the air separates into a nitrogen-rich overhead gas and an oxygen enriched tank liquid.
  • the tank liquid 17 is expanded by a valve 18 and sent to the head condenser 9 in a known manner.
  • the vaporized liquid 21 is heated in the exchanger 2.
  • a gaseous product rich in nitrogen 29 is withdrawn at the top of the column, heated in the exchanger 2 and sent to a customer. Its carbon monoxide content is measured by an analyzer 23 and must not exceed a threshold S1, for example 5 ppm.
  • the cold behavior of the apparatus is ensured by sending liquid nitrogen from a storage 7 which constitutes a source external to the air separation apparatus.
  • the flow rate V of this liquid is substantially constant as long as the carbon monoxide content of the air does not exceed a threshold S0.
  • the pipe 19 of liquid nitrogen is connected to the top of the column 5 through a valve 11. An oxygen-enriched liquid can be withdrawn from the column 5 through a pipe 13.
  • the molar amount V of liquid nitrogen sent to the column 5 by the pipe 19 corresponds to at most about 5% of the molar flow rate of nitrogen produced, possibly at most 3% of the molar flow rate of nitrogen produced, that is to say the amount required to hold the apparatus cold in the absence of an expansion turbine or other means for producing cold.
  • the quantity V is therefore substantially constant.
  • the CO content of this nitrogen flow rate V is less than 5 ppm, since the liquid stored in this external storage 7 may possibly serve as a backup, after vaporization, in the event of an inadvertent stoppage or not, of the unit of nitrogen production. All the liquid withdrawn in the tank is sent via line 17 to the condenser 9.
  • the analyzer 3 sends a signal to the FIC 12 to change the flow rate sent by the pipe 19 so as to increase the amount of liquid nitrogen arriving in the column so that the flow exceeds the value V.
  • the limit CO content in the air can rise to 6.5 ppm without the carbon monoxide content in the atmosphere. produced nitrogen exceeds 5 ppm, required by standards.
  • the limit content of CO in air 1 is 9.5 ppm without the carbon monoxide content in the nitrogen product 19 exceeds 5 ppm, required by the standards.
  • an additional flow of oxygen-enriched liquid 13 is withdrawn from the tank of the column 5 by means of a valve 15 and a pipe when the carbon monoxide content of the air exceeds the threshold S 0 and when the liquid nitrogen arrives through line 19.
  • This purge rate is substantially the same, on a molar basis, as the additional flow rate sent into the column through line 19, and is removed from the production unit. It can possibly be stored in a dedicated tank, or released to the atmosphere after spraying.
  • the ratio between the cryogenic liquid flow rate sent to the column and the carbon monoxide content of the air can be constant. Otherwise, the cryogenic liquid flow rate to the column may be set to one or more values, the value being a function of whether the carbon monoxide content of the air is in one or more range (s) predefined (s). Thus the flow can be 10%, if the content is between 5 and 6.5 ppm and 40% if the content is between 6.5 and 9.5 ppm.

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

Claims (10)

  1. Verfahren zur Herstellung von Stickstoff durch TieftemperaturDestillation von Luft, wobei kohlenmonoxidhaltige Luft an eine Tieftemperatur-Destillationskolonne geleitet wird, eine Menge D Stickstoff am Kopf der Destillationskolonne (5) abgezogen wird, mit einem CO-Gehalt, der geringer als ein festgelegter Wert S1 ist, und eine Menge stickstoffreicher kryogener Flüssigkeit, die aus einer externen Quelle (7) stammt, in den Kopf der Kolonne geleitet wird, wobei die Menge kryogener Flüssigkeit, die an die Kolonne geleitet wird, kleiner als ein Wert V ist, wenn der CO-Gehalt in der Luft einen zuvor definierten Schwellwert (S0) nicht überschreitet, dadurch gekennzeichnet, dass die Menge kryogener Flüssigkeit, die an die Kolonne geleitet wird, größer als der Wert V ist, wenn der Kohlenmonoxid-Gehalt der Luft diesen zuvor definierten Schwellwert (S0) überschreitet.
  2. Verfahren nach Anspruch 1, wobei die Menge Luft, die an die Destillationskolonne (5) geleitet wird, reduziert ist, wenn der Kohlenmonoxid-Gehalt der Luft den zuvor definierten Schwellwert überschreitet.
  3. Verfahren nach einem der vorhergehenden Ansprüche, wobei, wenn der Kohlenmonoxid-Gehalt der Luft unterhalb des gegebenen Schwellwerts liegt, die Molmenge kryogener Flüssigkeit, die an die Kolonne (5) geleitet wird, höchstens gleich 5% der Molmenge gasförmigen Stickstoffs D ist, die aus der Kolonne abgezogen wird.
  4. Verfahren nach einem der vorhergehenden Ansprüche, wobei eine Ablassmenge mit Sauerstoff angereicherter Flüssigkeit hergestellt wird, dadurch gekennzeichnet, dass die mit Sauerstoff angereicherte Menge kryogener Flüssigkeit, die hergestellt wird, im Wesentlichen konstant ist, wenn die Menge kryogener Flüssigkeit, die an die Kolonne (5) geleitet wird, kleiner als ein Wert V ist, und erhöht ist, wenn die Menge kryogener Flüssigkeit, die an die Kolonne geleitet wird, größer als der Wert V ist.
  5. Verfahren nach Anspruch 4, wobei die Erhöhung der mit Sauerstoff angereicherten Molmenge, die abgezogen wird, im Wesentlichen gleich der Erhöhung der Molmenge kryogener Flüssigkeit ist, die an die Kolonne (5) geleitet wird.
  6. Verfahren nach einem der vorhergehenden Ansprüche, wobei das Verhältnis zwischen der Menge kryogener Flüssigkeit, die an die Kolonne (5) geleitet wird, und dem Kohlenmonoxidgehalt der Luft konstant ist.
  7. Verfahren nach einem der Ansprüche 1 bis 6, wobei die Menge kryogener Flüssigkeit, die an die Kolonne (5) geleitet wird, einen oder mehrere gegebene(n) Wert(e) hat, wenn sich der Kohlenmonoxidgehalt der Luft in einem oder mehreren vordefinierten Bereich(en) befindet.
  8. Verfahren nach einem der vorhergehenden Ansprüche, wobei die Menge kryogener Flüssigkeit gemäß dem Kohlenmonoxidgehalt der Luft geregelt wird.
  9. Verfahren nach einem der vorhergehenden Ansprüche, wobei die Menge kryogener Flüssigkeit gemäß dem Kohlenmonoxidgehalt des hergestellten Stickstoffs geregelt wird.
  10. Vorrichtung zur Herstellung von Stickstoff durch Tieftemperaturdestillation, umfassend eine Tieftemperatur-Destillationskolonne (5), eine Leitung, um kohlenmonoxidhaltige Luft an die Kolonne zu leiten, eine Leitung, um ein stickstoffreiches Produkt aus der Kolonne abzuziehen, eine Leitung, um flüssigen Stickstoff aus einer externen Quelle (7), zum Beispiel einem Lager, an die Kolonne zu leiten, dadurch gekennzeichnet, dass sie Mittel zum Regeln der Menge flüssigen Stickstoffs, die an die Kolonne geleitet wird, in Abhängigkeit von dem Kohlenmonoxidgehalt der Luft, Mittel zum Messen des Kohlenmonoxidgehalts der Luft oder des stickstoffreichen Produkts und Mittel zum Erhöhen der Menge flüssigen Stickstoffs, die an die Kolonne geleitet wird, wenn der Gehalt einen Schwellwert überschreitet, umfasst.
EP11160944.2A 2010-04-22 2011-04-04 Verfahren und Gerät zur Stickstoffherstellung durch Tieftemperaturdestillation von Luft Not-in-force EP2381197B1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR1053075A FR2959297B1 (fr) 2010-04-22 2010-04-22 Procede et appareil de production d'azote par distillation cryogenique d'air

Publications (2)

Publication Number Publication Date
EP2381197A1 EP2381197A1 (de) 2011-10-26
EP2381197B1 true EP2381197B1 (de) 2013-09-18

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EP11160944.2A Not-in-force EP2381197B1 (de) 2010-04-22 2011-04-04 Verfahren und Gerät zur Stickstoffherstellung durch Tieftemperaturdestillation von Luft

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Country Link
US (1) US9476640B2 (de)
EP (1) EP2381197B1 (de)
JP (1) JP5788206B2 (de)
CN (1) CN102235802B (de)
AU (1) AU2011201849B2 (de)
BR (1) BRPI1101677A2 (de)
CA (1) CA2736371A1 (de)
ES (1) ES2436079T3 (de)
FR (1) FR2959297B1 (de)

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* Cited by examiner, † Cited by third party
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CN104048478B (zh) * 2014-06-23 2016-03-30 浙江大川空分设备有限公司 高提取率和低能耗污氮气提纯氮气的设备及其提取方法

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WO1984003554A1 (en) * 1983-03-08 1984-09-13 Daido Oxygen Apparatus for producing high-purity nitrogen gas
US4784677A (en) * 1987-07-16 1988-11-15 The Boc Group, Inc. Process and apparatus for controlling argon column feedstreams
JPH01269892A (ja) * 1988-04-20 1989-10-27 Hitachi Ltd 高純度窒素を採取する空気分離装置
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FR2903483B1 (fr) * 2006-07-04 2014-07-04 Air Liquide Procede et appareil de separation d'air par distillation cryogenique
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Also Published As

Publication number Publication date
CA2736371A1 (en) 2011-10-22
FR2959297B1 (fr) 2012-04-27
JP5788206B2 (ja) 2015-09-30
AU2011201849A1 (en) 2011-11-10
US9476640B2 (en) 2016-10-25
ES2436079T3 (es) 2013-12-26
CN102235802B (zh) 2015-03-04
EP2381197A1 (de) 2011-10-26
US20110259047A1 (en) 2011-10-27
CN102235802A (zh) 2011-11-09
AU2011201849B2 (en) 2014-06-12
BRPI1101677A2 (pt) 2012-10-16
FR2959297A1 (fr) 2011-10-28
JP2011242122A (ja) 2011-12-01

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