EP1001236B1 - Procédé de production d'azote à ultra haute pureté - Google Patents

Procédé de production d'azote à ultra haute pureté Download PDF

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Publication number
EP1001236B1
EP1001236B1 EP99122146A EP99122146A EP1001236B1 EP 1001236 B1 EP1001236 B1 EP 1001236B1 EP 99122146 A EP99122146 A EP 99122146A EP 99122146 A EP99122146 A EP 99122146A EP 1001236 B1 EP1001236 B1 EP 1001236B1
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Prior art keywords
column
nitrogen
free
low
pressure column
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EP99122146A
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German (de)
English (en)
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EP1001236A3 (fr
EP1001236A2 (fr
Inventor
Dietrich Dipl.-Ing. Rottmann
Christian Dipl.-Ing. Kunz
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Linde GmbH
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Linde GmbH
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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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04218—Parallel arrangement of the main heat exchange line in cores having different functions, e.g. in low pressure and high pressure cores
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    • 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
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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
    • F25J3/04084—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 nitrogen
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    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
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    • F25J3/04436—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 at least a triple pressure main column system
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    • 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
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    • F25J3/04963—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network and inter-connecting equipment within or downstream of the fractionation unit(s)
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    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
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    • F25J2210/42—Nitrogen
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    • 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
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    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/62—Details of storing a fluid in a tank
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/92—Carbon monoxide

Definitions

  • the invention relates to a method and an apparatus for the extraction of ultra-pure nitrogen by cryogenic decomposition of an oxygen-free Pressure nitrogen fraction.
  • the object of the invention is therefore to avoid this disadvantage and Reduce energy consumption.
  • Another object of the invention is to provide a method that either with a liquid pressure nitrogen fraction directly from the pressure column or is operated from a tank with liquid pressure column nitrogen.
  • the ultrapure nitrogen is obtained in liquid form and is easier to transport in this form and therefore easier to distribute to customers become.
  • the process can also be used universally. Because it can with Connection to an air separation plant (with or without liquid nitrogen tank) or only on a liquid nitrogen tank (with spatial separation from the air separation plant) be used. On an air separation plant with a liquid nitrogen tank also the ultra pure liquid nitrogen can be obtained without the Air separation plant is in operation.
  • the carbon monoxide-free top gas upstream of its compression (9) and a top gas of the He-Ne-H 2 column can be combined to form a cold gas stream which is free of carbon monoxide.
  • the gas stream formed during the evaporation of the liquid refrigerant and a top gas of the He-Ne-H 2 column can be combined to form a cold gas stream.
  • the cold gas stream is advantageously heated in a heat exchanger, compressed and cooled again in countercurrent in the same heat exchanger and then partly in the low-pressure column and partly in the He-Ne-H 2 column for heating the sump used and liquefied except for gaseous residual streams.
  • the streams liquefied during the heating of the He-Ne-H 2 column and the low-pressure column can be fed back to the He-Ne-H 2 column.
  • the streams liquefied during the heating of the He-Ne-H 2 column and the low-pressure column in the evaporator / condenser of the low-pressure column can liquefy the carbon monoxide-free overhead gas of the low-pressure column except for a residual stream and are at least partially fed as reflux to the He-Ne-H 2 column.
  • the disadvantage of an additional investment for the condenser / evaporator is then offset by the advantage, which should not be underestimated, that in the event of air leakage during the compression of the carbon monoxide-free gas stream, the ultra-pure liquid nitrogen cannot be contaminated.
  • Ultrapure nitrogen can be drawn off in liquid form from the He-Ne-H 2 column and can be obtained partly as the reflux of the low-pressure column and partly as a liquid ultrapure nitrogen product.
  • the ultra pure liquid nitrogen product can be fed to a product tank.
  • the ultra pure liquid nitrogen product can be pressurized with a pump, under Use of the cold content in the production of oxygen-free Compressed nitrogen fraction evaporates, warmed up and as a gaseous pressure product Use are fed.
  • the process for producing ultra pure Liquid nitrogen product also made and ultra-pure nitrogen gas product thereby making good use of the coldness of the original liquid product become.
  • Figure 1 shows a method according to the first variant of the invention with provision of oxygen-free nitrogen for the process from a liquid nitrogen tank.
  • Figure 2 shows a method according to the first variant of the invention with provision of oxygen-free nitrogen for the process from a pressure column Rectification system.
  • Figure 3 shows a method as in Figure 1, but with an additional Evaporator / condenser, that is, according to the second variant of the invention.
  • FIG. 4 shows a method as in FIG. 2 with an additional evaporator / condenser, thus also according to the second variant of the invention.
  • Figure 5 shows a method as in Figure 2 for the case of retrofitting a Rectification system with the method according to the first variant of the invention.
  • FIG. 1 shows schematically an embodiment of the method according to the invention for the production of ultra-pure nitrogen. Except for a residual content in the range of a few mol-ppm of oxygen-free liquid pressurized nitrogen fraction 1, the pressure is released into a heated low-pressure column 2, which is operated at a pressure between 4.5 and 5.5 bar. In the low-pressure column 2, rising steam is released from the He-Ne-H 2 column 4 of carbon monoxide and thus also of impurities boiling heavier than carbon monoxide, such as argon and the residual oxygen content, depending on the purity requirement, by means of ultrapure nitrogen 3 which is applied at the top as a return line exempted a few mol-ppb.
  • the carbon monoxide-free head gas 5 and a head gas 6 of the He-Ne-H 2 column are combined to form a carbon monoxide-free cold gas stream 7, heated in a heat exchanger 8 and cooled again after compression 9 in the same heat exchanger 8.
  • the cooled gas stream 10 is used to a part 11 in the low pressure column 2 and to another part 12 in the He-Ne-H 2 column 4 for heating 13, 14 of the sump and liquefied except for gaseous residual streams 15, 16.
  • the liquefied streams 17, 18 are fed to the He-Ne-H 2 column 4 as a return.
  • the as Insert used liquid pressure nitrogen fraction 1 over a liquid tank 22 a booster pump 23 removed and a heat exchanger 24 in the low pressure column 2 out.
  • the ultra-pure Liquid nitrogen product 20 supercooled and then without gaseous Relaxation losses in the product tank 21 relaxed. Because of the hypothermia of the Liquid nitrogen product 20, the product tank 21 can be operated as pressureless Liquid tank to be run.
  • FIG. 2 schematically shows the production of the ultra-pure liquid nitrogen product 20 as in FIG. 1.
  • the liquid nitrogen fraction 1 used as the insert is different from in the embodiment according to FIG. 1 of a pressure column 25 of a rectification system removed and passed through a heat exchanger 24 into the low pressure column 2.
  • the ultra pure liquid nitrogen product 20 is pressurized by a pump 26 in counterflow to the liquid nitrogen fraction 1 via the heat exchanger 24 passed and using the cold content in a condenser 27 and in one Heat exchanger 28 in the extraction of the oxygen-free pressure nitrogen fraction used, evaporated, warmed and as a gaseous ultra-pure printed product 29 fed for further use.
  • FIG. 3 schematically shows an embodiment of the method according to the invention using a condenser / evaporator 30.
  • the carbon monoxide-free top gas 5 of the low-pressure column 2 (against one by combining the liquefied streams 17, 18 formed liquid refrigerant 31, which evaporates here) liquefied in the condenser / evaporator 30 except for a gaseous residual stream 32 and used in the He-Ne-H 2 column 4 as the return 33.
  • a gas stream 5 ′ formed during the evaporation of the liquid refrigerant and the top gas 6 of the He-Ne-H 2 column 4 are combined to form the cold carbon monoxide-free gas stream 7.
  • Figure 4 shows schematically an embodiment of the method according to the invention in FIG. 2, but carried out with the condenser / evaporator 30 as in FIG. 3.
  • FIG. 5 shows schematically that the inventive method on a existing rectification system can be used.
  • the rectification system Condenser 27 added and the heat exchanger 8 receives two additional Passages for the use of the cold of the ultra-pure nitrogen 20 'to be heated the cooling and liquefaction of a partial flow 34 of the air 35 for the Rectification system.
  • the ultra-pure heated in the heat exchanger 8 Nitrogen is used as a gaseous ultrapure printed product 29 for further use fed.
  • a common feature of the design of the method according to the invention according to Figures 1 to 5 is that all residual gas flows (15, 16, 36 in Figure 1, 2, 5 and 15, 16, 32, 36 in Figure 3, 4) to a cold residual gas stream 37 summarized heated in the heat exchanger 8 and as an impure gas 38 to the Atmosphere.
  • m 3 means: m 3 in the normal state at 0 ° C and 1.0133 bar; ie 1m 3 corresponds to 1.25 kg.

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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)
  • Removal Of Specific Substances (AREA)
  • Arrangement Of Elements, Cooling, Sealing, Or The Like Of Lighting Devices (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Claims (8)

  1. Procédé en vue de l'obtention d'azote ultrapur par fractionnement à basse température d'une fraction d'azote sous pression exempte d'oxygène, lors duquel la fraction d'azote sous pression exempte d'oxygène (1) est prélevée soit à l'état fluide hors d'un domaine supérieur d'une colonne sous pression en vue du fractionnement d'air à basse température, soit hors d'un réservoir de fluide (22) avec de l'azote emmagasiné exempt d'oxygène et est détendue dans une colonne basse pression (2) chauffée (13) dans son puits, une vapeur montante se formant dans la colonne basse pression et étant débarrassée du monoxyde de carbone à l'aide d'un reflux (3) chargé au niveau de la tête de la colonne basse pression avec de l'azote ultrapur et étant évacuée au niveau de la tête de la colonne basse pression en tant que gaz de tête exempt de monoxyde de carbone (5, 7) et
    soit du gaz de tête exempt de monoxyde de carbone (5, 7) de la colonne basse pression étant partiellement liquéfié (13, 14) après une augmentation de pression (9) et la partie liquéfiée (17, 18) étant détendue dans une colonne He-Ne-H2 (4), chauffée (14) dans son puits, de laquelle l'azote ultrapur (19, 20) est prélevé à l'état fluide,
    soit du gaz de tête exempt de monoxyde de carbone (5) de la colonne basse pression étant partiellement liquéfié dans un condenseur-évaporateur (30) contre un réfrigérant fluide (31) qui est en l'occurrence vaporisé, et un courant gazeux (5', 7) se formant lors de l'évaporation (30) du réfrigérant fluide, étant partiellement liquéfié (13, 14) après une augmentation de pression (9) et la partie liquéfiée (17, 18, 31) étant acheminée en tant que réfrigérant (31) au condenseur-évaporateur (30), le gaz de tête exempt de monoxyde de carbone (5) de la colonne basse pression étant liquéfié jusqu'à un courant résiduel restant sous forme gazeuse (32) dans le condenseur/évaporateur (30) de la colonne basse pression et étant acheminé au moins partiellement en tant que reflux (33) à une colonne He-Ne-H2 (4), hors de laquelle l'azote ultrapur (19, 20) est prélevé à l'état fluide.
  2. Procédé selon la revendication 1, caractérisé en ce que le gaz de tête exempt de monoxyde de carbone (5), en amont de sa compression (9), et un gaz de tête (6) de la colonne He-Ne-H2 (4) sont combinés pour former un courant gazeux froid (7) qui est exempt de monoxyde de carbone.
  3. Procédé selon la revendication 1, caractérisé en ce que le courant gazeux (5') se formant lors de l'évaporation (30) du réfrigérant fluide et un gaz de tête (6) de la colonne He-Ne-H2 (4) sont combinés pour former un courant gazeux froid (7).
  4. Procédé selon la revendication 2 ou 3, caractérisé en ce que le courant gazeux froid (7, 10) est échauffé dans un échangeur thermique (8), est comprimé (9) et est à nouveau refroidi en contre-courant dans le même échangeur thermique (8) et est ensuite utilisé, pour une partie (12), dans la colonne basse pression (2) et, pour une autre partie (11), dans la colonne He-Ne-H2 (4), en vue de l'échauffement du puits (13, 14) et est liquéfié, en l'occurrence, à l'exception de courants résiduels subsistant à l'état gazeux (15, 16).
  5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu'une partie de l'azote ultrapur (19) prélevé à l'état fluide hors de la colonne He-Ne-H2 est utilisée en tant que reflux (3) de la colonne basse pression (2).
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que le produit d'azote liquéfié ultrapur (19, 20) est acheminé à une citerne de produit (21).
  7. Procédé selon la revendication 6, caractérisé en ce que le produit d'azote liquéfié ultrapur est mis sous pression à l'aide d'une pompe, est vaporisé par utilisation du contenant réfrigérant obtenu lors de l'obtention de la fraction d'azote sous pression exempte d'oxygène, est échauffé et est acheminé en tant que produit gazeux sous pression à une application.
  8. Dispositif en vue de l'obtention d'azote ultrapur par fractionnement à basse température d'une fraction d'azote sous pression exempte d'oxygène, ayant des moyens en vue de l'acheminement d'une fraction d'azote sous pression exempte d'oxygène, provenant d'un domaine supérieur d'une colonne sous pression en vue du fractionnement d'air à basse température ou provenant d'un réservoir de fluide avec de l'azote emmagasiné exempt d'oxygène dans une colonne basse pression, chauffée dans son puits, ayant des moyens en vue de la charge d'azote ultrapur en tant que reflux au niveau de la tête de la colonne basse pression, ayant des moyens en vue de l'évacuation de gaz de tête exempt de monoxyde de carbone hors de la tête de la colonne basse pression,
    soit les moyens en vue de l'évacuation dé gaz de tête exempt de monoxyde de carbone étant reliés aux moyens en vue de l'augmentation de pression (9) et en vue de la liquéfaction partielle subséquente (13, 14) du gaz de tête exempt de monoxyde de carbone, et le dispositif présentant des moyens en vue de l'introduction de la partie liquéfiée du gaz de tête exempt de monoxyde de carbone dans une colonne He-Ne-H2, chauffée dans son puits, et des moyens en vue du prélèvement de l'azote ultrapur à l'état fluide hors de la colonne He-Ne-H2,
    soit les moyens en vue de l'évacuation de gaz de tête exempt de monoxyde de carbone étant reliés à un condenseur/évaporateur (30) en vue de la liquéfaction partielle du gaz de tête exempt de monoxyde de carbone dans l'optique de la production d'un fluide contre un réfrigérant fluide (31) s'évaporant pour former un courant gazeux (5', 7), et le dispositif présentant des moyens en vue de l'augmentation de pression (9) et en vue de la liquéfaction partielle subséquente (13, 14) du courant gazeux (5', 7), des moyens en vue de l'introduction de la partie liquéfiée (17, 18, 31) du courant gazeux en tant que réfrigérant (31) dans le condenseur/évaporateur (30), des moyens en vue de l'introduction de fluide produit dans le condenseur/évaporateur (30) de la colonne basse pression en tant que reflux (33) dans une colonne He-Ne-H2 (4) et des moyens en vue du prélèvement de l'azote ultrapur (19, 20) à l'état fluide hors de la colonne He-Ne-H2.
EP99122146A 1998-11-11 1999-11-05 Procédé de production d'azote à ultra haute pureté Expired - Lifetime EP1001236B1 (fr)

Applications Claiming Priority (4)

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DE19852019 1998-11-11
DE19852019 1998-11-11
DE19924375 1999-05-27
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EP (1) EP1001236B1 (fr)
JP (1) JP2000180051A (fr)
KR (1) KR20000035406A (fr)
CN (1) CN1134640C (fr)
AT (1) ATE278166T1 (fr)
CA (1) CA2289173A1 (fr)
DE (2) DE19929798A1 (fr)
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DE10158327A1 (de) * 2001-11-28 2003-06-18 Linde Ag Verfahren und Vorrichtung zur Herstellung hoch reinen Stickstoffs aus weniger reinem Stickstoff
DE10205094A1 (de) * 2002-02-07 2003-08-21 Linde Ag Verfahren und Vorrichtung zur Erzeugung hoch reinen Stickstoffs
US9163188B2 (en) * 2009-07-24 2015-10-20 Bp Alternative Energy International Limited Separation of carbon dioxide and hydrogen
CN102797974A (zh) * 2012-07-31 2012-11-28 张立永 氢脉
CN114165989A (zh) * 2021-11-22 2022-03-11 四川空分设备(集团)有限责任公司 制取中压氮气的装置及方法

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US4464188A (en) * 1983-09-27 1984-08-07 Air Products And Chemicals, Inc. Process and apparatus for the separation of air
US5123947A (en) * 1991-01-03 1992-06-23 Air Products And Chemicals, Inc. Cryogenic process for the separation of air to produce ultra high purity nitrogen
US5167125A (en) * 1991-04-08 1992-12-01 Air Products And Chemicals, Inc. Recovery of dissolved light gases from a liquid stream
US5170630A (en) * 1991-06-24 1992-12-15 The Boc Group, Inc. Process and apparatus for producing nitrogen of ultra-high purity
JP3306517B2 (ja) * 1992-05-08 2002-07-24 日本酸素株式会社 空気液化分離装置及び方法
US5351492A (en) * 1992-09-23 1994-10-04 Air Products And Chemicals, Inc. Distillation strategies for the production of carbon monoxide-free nitrogen
FR2696821B1 (fr) * 1992-10-09 1994-11-10 Air Liquide Procédé et installation de production d'azote ultra-pur sous pression.
JP3447437B2 (ja) * 1995-07-26 2003-09-16 日本エア・リキード株式会社 高純度窒素ガス製造装置
DE19640711A1 (de) * 1996-10-02 1998-04-09 Linde Ag Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff
DE19806576A1 (de) * 1998-02-17 1998-08-06 Linde Ag Verfahren und Vorrichtung zur Gewinnung von CO-freiem Stickstoff
US5906113A (en) * 1998-04-08 1999-05-25 Praxair Technology, Inc. Serial column cryogenic rectification system for producing high purity nitrogen

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SG74755A1 (en) 2000-08-22
CN1255619A (zh) 2000-06-07
ATE278166T1 (de) 2004-10-15
CN1134640C (zh) 2004-01-14
ES2229608T3 (es) 2005-04-16
DE59910646D1 (de) 2004-11-04
DE19929798A1 (de) 2000-05-25
TW432191B (en) 2001-05-01
US6276172B1 (en) 2001-08-21
CA2289173A1 (fr) 2000-05-11
KR20000035406A (ko) 2000-06-26
EP1001236A3 (fr) 2000-11-08
JP2000180051A (ja) 2000-06-30
EP1001236A2 (fr) 2000-05-17

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