EP2381197B1 - Procédé et appareil de production d'azote par distillation cryogénique d'air - Google Patents

Procédé et appareil de production d'azote par distillation cryogénique d'air 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
Authority
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
Application number
EP11160944.2A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP2381197A1 (fr
Inventor
Patrick Le Bot
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
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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Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP2381197A1 publication Critical patent/EP2381197A1/fr
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Publication of EP2381197B1 publication Critical patent/EP2381197B1/fr
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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
    • F25J3/044—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)
EP11160944.2A 2010-04-22 2011-04-04 Procédé et appareil de production d'azote par distillation cryogénique d'air Not-in-force EP2381197B1 (fr)

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 (fr) 2011-10-26
EP2381197B1 true EP2381197B1 (fr) 2013-09-18

Family

ID=43446359

Family Applications (1)

Application Number Title Priority Date Filing Date
EP11160944.2A Not-in-force EP2381197B1 (fr) 2010-04-22 2011-04-04 Procédé et appareil de production d'azote par distillation cryogénique d'air

Country Status (9)

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

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Family Cites Families (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3619377A (en) * 1969-08-04 1971-11-09 Phillips Petroleum Co Control of composition of overhead vaporous product in a partially condensing fractionation column
DE3486017T3 (de) * 1983-03-08 1999-03-04 Daidousanso Co. Ltd., Osaka Sehr reiner Stickstoffgaserzeugungsapparat.
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
GB8828133D0 (en) 1988-12-02 1989-01-05 Boc Group Plc Air separation
JPH051882A (ja) * 1991-06-25 1993-01-08 Hitachi Ltd 超高純度窒素製造装置
FR2694383B1 (fr) * 1992-07-29 1994-09-16 Air Liquide Production et installation de production d'azote gazeux à plusieurs puretés différentes.
JP2838623B2 (ja) 1992-08-06 1998-12-16 日本エア・リキード株式会社 超高純度窒素製造方法及びその装置
US5351492A (en) * 1992-09-23 1994-10-04 Air Products And Chemicals, Inc. Distillation strategies for the production of carbon monoxide-free nitrogen
FR2697620B1 (fr) * 1992-10-30 1994-12-23 Air Liquide Procédé et installation de production d'azote gazeux à débit variable.
US5589151A (en) * 1993-12-31 1996-12-31 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process for the preparation of high-purity liquid nitrogen
US5511380A (en) * 1994-09-12 1996-04-30 Liquid Air Engineering Corporation High purity nitrogen production and installation
US5983667A (en) * 1997-10-31 1999-11-16 Praxair Technology, Inc. Cryogenic system for producing ultra-high purity nitrogen
US6006546A (en) * 1998-04-29 1999-12-28 Air Products And Chemicals, Inc. Nitrogen purity control in the air separation unit of an IGCC power generation system
JPH11325720A (ja) * 1998-05-14 1999-11-26 Daido Hoxan Inc 超高純度窒素ガス製造方法およびそれに用いる装置
FR2903483B1 (fr) * 2006-07-04 2014-07-04 Air Liquide Procede et appareil de separation d'air par distillation cryogenique
FR2910602B1 (fr) * 2006-12-21 2012-12-14 Air Liquide Procede et appareil de separation d'un melange comprenant au moins de l'hydrogene, de l'azote et du monoxyde de carbone par distillation cryogenique
JP5001882B2 (ja) 2008-03-10 2012-08-15 日新製鋼株式会社 導電性に優れたばね用鋼板の製造方法

Also Published As

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

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