EP0610972B1 - Process for preparing nitrogen - Google Patents

Process for preparing nitrogen Download PDF

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Publication number
EP0610972B1
EP0610972B1 EP94106964A EP94106964A EP0610972B1 EP 0610972 B1 EP0610972 B1 EP 0610972B1 EP 94106964 A EP94106964 A EP 94106964A EP 94106964 A EP94106964 A EP 94106964A EP 0610972 B1 EP0610972 B1 EP 0610972B1
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EP
European Patent Office
Prior art keywords
column
nitrogen
fraction
mixture
turbine
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.)
Expired - Lifetime
Application number
EP94106964A
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German (de)
French (fr)
Other versions
EP0610972A3 (en
EP0610972A2 (en
Inventor
Sophie Gastinne
François Venet
Bao Ha
Naohiko Yamashita
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.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Liquid Air Engineering Corp Canada
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Teisan KK
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Application filed by Liquid Air Engineering Corp Canada, Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude, Teisan KK filed Critical Liquid Air Engineering Corp Canada
Publication of EP0610972A2 publication Critical patent/EP0610972A2/en
Publication of EP0610972A3 publication Critical patent/EP0610972A3/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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
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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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
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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
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    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
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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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    • F25J3/04351—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
    • F25J3/04357—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 and comprising a gas work expansion loop
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    • 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
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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
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    • 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
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
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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
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    • 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
    • F25J3/04472—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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages
    • F25J3/04496—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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for compensating variable air feed or variable product demand by alternating between periods of liquid storage and liquid assist
    • F25J3/04503—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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for compensating variable air feed or variable product demand by alternating between periods of liquid storage and liquid assist by exchanging "cold" between at least two different cryogenic liquids, e.g. independently from the main heat exchange line of the air fractionation and/or by using external alternating storage systems
    • F25J3/04509—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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for compensating variable air feed or variable product demand by alternating between periods of liquid storage and liquid assist by exchanging "cold" between at least two different cryogenic liquids, e.g. independently from the main heat exchange line of the air fractionation and/or by using external alternating storage systems within the cold part of the air fractionation, i.e. exchanging "cold" within the fractionation and/or main heat exchange line
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
    • F25J2200/00—Processes or apparatus using separation by rectification
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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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/52—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high pressure column of a double pressure main column system
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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
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    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
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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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
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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
    • 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
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    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/42—Separating low boiling, i.e. more volatile components from nitrogen, e.g. He, H2, Ne
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    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/40—Processes or apparatus involving steps for recycling of process streams the recycled stream being air
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    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
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    • 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
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    • Y10S62/00—Refrigeration
    • Y10S62/901—Single column
    • 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
    • Y10S62/912—External refrigeration system
    • Y10S62/913—Liquified gas
    • 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
    • Y10S62/939—Partial feed stream expansion, air

Definitions

  • the present invention relates to a process for the production of nitrogen gas under low or medium pressure, from a mixture to be treated containing mainly nitrogen and oxygen, such as air, in a distillation column. .
  • the subject of the present invention is a method as defined above, allowing both a good nitrogen extraction yield and a resistance to cold of the device by expansion in a turbine of a gas poor in oxygen.
  • the method of the present invention is characterized in that it comprises the step of extracting from the top of the column the vaporized part of step g) as waste gas and of joining it to the expanded mixture in the front turbine to send it to the exchanger and in that only a second non-expanded fraction of the mixture is distilled in the column.
  • the production of cold can also be ensured by expansion of a fraction of the recycled nitrogen, at a pressure less than or equal to the low pressure, then reheated and recompressed.
  • a condensed part of the cycle gas can be diverted to a buffer capacity, with sampling and reintroduction into the column in the event of an increase in the nitrogen production rate, while a part of the stream of liquid rich in oxygen is sent to a buffer capacity to be reinjected into the column head condenser, in the event of a reduction in the production of nitrogen gas, which makes it possible to replenish the stock of liquid nitrogen under pressure.
  • the two cold productions are combined by expansion of the recycling gas.
  • this stream 1 is cooled to an intermediate temperature represented by level 2a. Then this gas stream is expanded at low pressure of the order of 3 to 5 bar abs. in the turbine 3, while part of the non-turbinated gas stream continues to cool with the products of the distillation and is introduced into the distillation column 4, at an intermediate level between two distillation stages, the upper one, 4a , and the other lower, 4b.
  • a liquid fraction enriched in oxygen 7 is collected, which is extracted from the column, expanded in valve 8 and finally introduced into the condenser of column 4, essentially consisting of an exchanger. 5 for the condensation of all or part of the gaseous fraction available at the head of column 4.
  • This oxygen-enriched fraction is extracted from the abovementioned condenser, in the form of a stream 9, which is mixed with part of the turbinated gaseous stream 112, reheated in exchanger 2, and finally used or evacuated at the outlet of exchanger 2.
  • a part condensed in exchanger 5 provides part of the reflux of the distillation. Part can be extracted in liquid form via line 12. Another part is extracted in gaseous form via line 11. The corresponding stream is heated in the exchanger 2, to obtain a stream of nitrogen at the outlet of the latter.
  • relatively pure gas under low pressure part of which (X and / or Y) constitutes the production of the separation unit.
  • This stream 14 is firstly cooled in the exchanger 2, at least partly condensed at the bottom of the column 4, in the exchanger 6, in exchange for heat with the oxygen-rich fraction, during vaporization. Then the stream 20 of condensed nitrogen is expanded in valve 17 and introduced at the head of column 4.
  • the distillation column 4 works under a relatively low pressure, between 3 and 5 bar abs. for example.
  • the stream of recycled nitrogen can be extracted by a line 20a towards a buffer capacity 20c and returned by the line 20b to the column 4, downstream of the valve 17.
  • the rich fraction in oxygen 7 can be extracted from the installation by a bypass duct 7a towards the buffer capacity 7c and returned by the duct 7b to the column 4 downstream of the valve 8.
  • the two rocker-type versions described in Figures 1 and 2 have the advantage of having a production of gaseous nitrogen which can range from 50 to 150% of nominal production.

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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)

Description

La présente invention concerne un procédé de production d'azote gazeux sous basse ou moyenne pression, à partir d'un mélange à traiter contenant principalement de l'azote et de l'oxygène, tel que de l'air, dans une colonne de distillation.The present invention relates to a process for the production of nitrogen gas under low or medium pressure, from a mixture to be treated containing mainly nitrogen and oxygen, such as air, in a distillation column. .

Pour produire de l'azote à partir d'air atmosphérique par exemple, US-A-4.662.917 décrit un procédé consistant à :

  • a) comprimer le mélange à traiter à une pression au moins égale à la pression de fonctionnement de ladite colonne, de l'ordre de 3 à 5 bar ;
  • b) refroidir le mélange comprimé dans un échangeur et détendre une première fraction dudit mélange refroidi dans une turbine pour produire le froid nécessaire au procédé et réaliser la distillation du mélange dans la colonne pour obtenir, dans la partie haute de la colonne, une fraction enrichie en azote qui est ensuite réchauffé ;
  • c) extraire une partie de la fraction enrichie en azote réchauffée en tant que produit ;
  • d) comprimer une partie restante de la fraction enrichie en azote réchauffé et ensuite la refroidir;
  • e) recycler une partie de ladite partie restante de la fraction enrichie en azote dans l'échangeur-vaporiseur situé dans le bas de ladite colonne, dans lequel cette partie se condense sous forme d'un liquide riche en azote et fournit la chaleur nécessaire pour la vaporisation dans la colonne ;
  • f) introduire une partie du liquide riche en azote condensé dans l'étape e) ci-dessus dans la partie supérieure de la colonne en tant que liquide de reflux additionnel ;
  • g) extraire une fraction enrichie en oxygène sous forme liquide, de la partie inférieure de la colonne et détendre au moins une partie de ladite fraction à une pression inférieure à la pression de la colonne et vaporiser cette partie par transfert de chaleur avec la fraction enrichie en azote qui se condense dans la partie supérieure de la colonne.
To produce nitrogen from atmospheric air, for example, US-A-4,662,917 describes a process consisting in:
  • a) compressing the mixture to be treated at a pressure at least equal to the operating pressure of said column, of the order of 3 to 5 bar;
  • b) cooling the compressed mixture in an exchanger and expanding a first fraction of said cooled mixture in a turbine to produce the cold necessary for the process and distilling the mixture in the column to obtain, in the upper part of the column, an enriched fraction nitrogen which is then reheated;
  • c) extracting part of the fraction enriched in heated nitrogen as a product;
  • d) compressing a remaining part of the fraction enriched in heated nitrogen and then cooling it;
  • e) recycling part of said remaining part of the nitrogen-enriched fraction in the exchanger-vaporizer located at the bottom of said column, in which this part condenses in the form of a liquid rich in nitrogen and provides the heat necessary for vaporization in the column;
  • f) introducing part of the liquid rich in nitrogen condensed in step e) above into the upper part of the column as additional reflux liquid;
  • g) extracting an oxygen-enriched fraction in liquid form from the lower part of the column and expanding at least part of said fraction to a pressure below the column pressure and vaporizing this part by heat transfer with the enriched fraction nitrogen which condenses at the top of the column.

La présente invention a pour objet un procédé tel que défini précédemment, permettant tout à la fois un bon rendement d'extraction en azote et une tenue en froid de l'appareil par détente dans une turbine d'un gaz pauvre en oxygène.The subject of the present invention is a method as defined above, allowing both a good nitrogen extraction yield and a resistance to cold of the device by expansion in a turbine of a gas poor in oxygen.

Le procédé de la présente invention est caractérisé en ce qu'il comprend l'étape d'extraire du sommet de la colonne la partie vaporisée de l'étape g) en tant que gaz résiduaire et de la réunir au mélange détendu dans la turbine avant de l'envoyer à l'échangeur et en ce que seule une deuxième fraction non détendue du mélange est distillée dans la colonne.The method of the present invention is characterized in that it comprises the step of extracting from the top of the column the vaporized part of step g) as waste gas and of joining it to the expanded mixture in the front turbine to send it to the exchanger and in that only a second non-expanded fraction of the mixture is distilled in the column.

Selon la présente invention, la production de froid nécessaire au procédé est assurée, au moins partiellement :

  • par détente d'au moins un flux gazeux frigorigène qui est le mélange à traiter, qui est détendu à la pression du résiduaire, et mélangé avec celui-ci.
According to the present invention, the production of cold necessary for the process is ensured, at least partially:
  • by expansion of at least one refrigerant gas flow which is the mixture to be treated, which is expanded to the pressure of the waste, and mixed with the latter.

La production de froid peut également être assurée par détente d'une fraction de l'azote recyclé, à une pression inférieure ou égale à la basse pression, puis réchauffé et recomprimé.The production of cold can also be ensured by expansion of a fraction of the recycled nitrogen, at a pressure less than or equal to the low pressure, then reheated and recompressed.

Une partie condensée du gaz de cycle peut être dérivée vers une capacité tampon, avec prélèvement et réintroduction dans la colonne en cas d'accroissement du débit de production d'azote, tandis qu'une partie du courant de liquide riche en oxygène est envoyée vers une capacité tampon pour être réinjectée dans le condenseur de tête de colonne, en cas de réduction de la production d'azote gazeux, ce qui permet de reconstituer le stock d'azote liquide sous pression.A condensed part of the cycle gas can be diverted to a buffer capacity, with sampling and reintroduction into the column in the event of an increase in the nitrogen production rate, while a part of the stream of liquid rich in oxygen is sent to a buffer capacity to be reinjected into the column head condenser, in the event of a reduction in the production of nitrogen gas, which makes it possible to replenish the stock of liquid nitrogen under pressure.

Dans une réalisation particulière, on associe les deux productions de froid par détente du gaz de recyclage.In a particular embodiment, the two cold productions are combined by expansion of the recycling gas.

La présente invention est maintenant décrite par référence aux dessins annexés, dont les figures 1 et 2 représentent les différents modes d'exécution du procédé selon l'invention.The present invention is now described with reference to the accompanying drawings, in which Figures 1 and 2 show the different modes of carrying out the method according to the invention.

Conformément à la figure 1, un courant de gaz 1, par exemple de l'air, est comprimé (de manière non représentée), à une pression supérieure à la basse pression de la colonne de distillation 4, définie ci-après, et épuré de manière traditionnelle.In accordance with FIG. 1, a stream of gas 1, for example air, is compressed (not shown), at a pressure higher than the low pressure of the distillation column 4, defined below, and purified in the traditional way.

Dans l'échangeur de chaleur 2, ce courant 1 est refroidi jusqu'à une température intermédiaire représentée par le niveau 2a. Puis ce courant gazeux est détendu à la basse pression de l'ordre de 3 à 5 bar abs. dans la turbine 3, tandis qu'une partie du courant gazeux non turbinée continue son refroidissement avec les produits de la distillation et est introduite dans la colonne de distillation 4, à un niveau intermédiaire entre deux étages de distillation, l'un supérieur, 4a, et l'autre inférieur, 4b.In the heat exchanger 2, this stream 1 is cooled to an intermediate temperature represented by level 2a. Then this gas stream is expanded at low pressure of the order of 3 to 5 bar abs. in the turbine 3, while part of the non-turbinated gas stream continues to cool with the products of the distillation and is introduced into the distillation column 4, at an intermediate level between two distillation stages, the upper one, 4a , and the other lower, 4b.

A la partie inférieure de la colonne 4, on recueille une fraction liquide enrichie en oxygène 7, laquelle est extraite de la colonne, détendue dans la vanne 8 et finalement introduite dans le condenseur de la colonne 4, constitué pour l'essentiel par un échangeur 5 pour la condensation de tout ou partie de la fraction gazeuse disponible en tête de la colonne 4. Cette fraction enrichie en oxygène est extraite du condenseur précité, sous la forme d'un courant 9, lequel est mélangé avec une partie du courant gazeux turbiné 112, réchauffé dans l'échangeur 2, et finalement utilisé ou évacué à la sortie de l'échangeur 2.At the bottom of column 4, a liquid fraction enriched in oxygen 7 is collected, which is extracted from the column, expanded in valve 8 and finally introduced into the condenser of column 4, essentially consisting of an exchanger. 5 for the condensation of all or part of the gaseous fraction available at the head of column 4. This oxygen-enriched fraction is extracted from the abovementioned condenser, in the form of a stream 9, which is mixed with part of the turbinated gaseous stream 112, reheated in exchanger 2, and finally used or evacuated at the outlet of exchanger 2.

Quant à la fraction enrichie en azote disponible en tête de la colonne 4, une partie condensée dans l'échangeur 5 assure une partie du reflux de la distillation. Une partie peut être extraite sous forme liquide par le conduit 12. Une autre partie est extraite sous forme gazeuse par le conduit 11. Le courant correspondant est réchauffé dans l'échangeur 2, pour obtenir à la sortie de ce dernier un courant d'azote gazeux relativement pur, sous la basse pression, dont une partie (X et/ou Y) constitue la production de l'unité de séparation.As for the fraction enriched in nitrogen available at the top of column 4, a part condensed in exchanger 5 provides part of the reflux of the distillation. Part can be extracted in liquid form via line 12. Another part is extracted in gaseous form via line 11. The corresponding stream is heated in the exchanger 2, to obtain a stream of nitrogen at the outlet of the latter. relatively pure gas under low pressure, part of which (X and / or Y) constitutes the production of the separation unit.

Une autre partie comprimée en 13 de ce courant 11, sous la forme du flux 14, est recyclée dans l'unité de séparation. Ce courant 14 est tout d'abord refroidi dans l'échangeur 2, au moins en partie condensé au pied de la colonne 4, dans l'échangeur 6, en échange de chaleur avec la fraction riche en oxygène, en cours de vaporisation. Puis le courant 20 d'azote condensé est détendu dans la vanne 17 et introduit en tête de la colonne 4.Another part compressed at 13 of this stream 11, in the form of the stream 14, is recycled to the separation unit. This stream 14 is firstly cooled in the exchanger 2, at least partly condensed at the bottom of the column 4, in the exchanger 6, in exchange for heat with the oxygen-rich fraction, during vaporization. Then the stream 20 of condensed nitrogen is expanded in valve 17 and introduced at the head of column 4.

Selon ce premier mode d'exécution, la colonne de distillation 4 travaille sous une pression relativement basse, comprise entre 3 et 5 bar abs. par exemple.According to this first embodiment, the distillation column 4 works under a relatively low pressure, between 3 and 5 bar abs. for example.

Pour le reste, il est possible de stocker les fractions liquides disponibles dans l'installation, pendant des périodes de production relativement faible, et de restituer ces fractions liquides à l'installation pendant les périodes de production importante.For the rest, it is possible to store the liquid fractions available in the installation, during periods of relatively low production, and to return these liquid fractions to the installation during periods of high production.

A cette fin, le courant d'azote recyclé peut être extrait par un conduit 20a vers une capacité tampon 20c et restituée par le conduit 20b à la colonne 4, en aval de la vanne 17. De la même manière, la fraction riche en oxygène 7 peut être extraite de l'installation par un conduit de dérivation 7a vers la capacité tampon 7c et restituée par le conduit 7b à la colonne 4 en aval de la vanne 8.To this end, the stream of recycled nitrogen can be extracted by a line 20a towards a buffer capacity 20c and returned by the line 20b to the column 4, downstream of the valve 17. In the same way, the rich fraction in oxygen 7 can be extracted from the installation by a bypass duct 7a towards the buffer capacity 7c and returned by the duct 7b to the column 4 downstream of the valve 8.

Le mode d'exécution de la figure 2 diffère de celui représenté à la figure 1 par les caractéristiques suivantes :

  • une première partie, 1a, de l'air comprimé 1 est refroidie dans l'échangeur 2 puis introduite en 121 dans la colonne 4 ;
  • l'autre partie, 1b, de l'air comprimé 1 est dérivée avant son passage dans l'échangeur 2 pour être admise dans la partie compresseur 50 d'un ensemble turbine 3-booster 50, refroidie jusqu'à température ambiante dans l'échangeur 51 et ensuite introduite dans l'échangeur 2 pour être extraite à une température intermédiaire, détendue en 112 dans la turbine 3 et réunie avec la fraction 9 riche en oxygène et vaporisée dans le condenseur 5.
The embodiment of Figure 2 differs from that shown in Figure 1 by the following features:
  • a first part, 1a, of the compressed air 1 is cooled in the exchanger 2 then introduced at 121 into the column 4;
  • the other part, 1b, of the compressed air 1 is diverted before it passes through the exchanger 2 to be admitted into the compressor part 50 of a turbine 3-booster 50 assembly, cooled to ambient temperature in the exchanger 51 and then introduced into exchanger 2 to be extracted at an intermediate temperature, expanded at 112 in turbine 3 and combined with fraction 9 rich in oxygen and vaporized in condenser 5.

Les deux versions type bascule décrites dans les figures 1 et 2 présentent l'avantage de pouvoir disposer d'une production en azote gazeux pouvant aller de 50 à 150 % de la production nominale.The two rocker-type versions described in Figures 1 and 2 have the advantage of having a production of gaseous nitrogen which can range from 50 to 150% of nominal production.

Claims (6)

  1. Process for producing gaseous nitrogen from a mixture to be treated in a distillation column (4), the said mixture comprising more particularly nitrogen and oxygen, the said process consisting of :
    a) compressing the mixture to be treated to a pressure at least equal to the operating pressure of the said column, of the order of 3 to 5 bar;
    b) cooling the compressed mixture in an exchanger (2) and expanding a first fraction of the said cooled mixture in a turbine (3) to produce the cooling necessary for the process and then distilling the mixture in the column to obtain, in the upper part of the column, a fraction enriched in nitrogen which is then reheated;
    c) withdrawing part of the fraction enriched in reheated nitrogen as a product;
    d) compressing a remaining part of the fraction enriched in reheated nitrogen and then cooling it;
    e) recycling part of the said remaining part of the fraction enriched in nitrogen in the exchanger-vaporizer (6) situated at the bottom of the said column, in which this part condenses in the form of a liquid rich in nitrogen and provides the heat necessary for vaporization in the column;
    f) introducing part of the liquid rich in nitrogen condensed in stage e) above in the upper part of the column as additional reflux liquid;
    g) extracting a fraction enriched in oxygen in liquid form, from the lower part of the column and expanding at least part of the said fraction to a pressure less than the column pressure and vaporizing this part by heat transfer with the fraction enriched in nitrogen which condenses in the upper part of the column; and characterized in that it comprises the stage of :
    h) extracting from the top of the column (4) the said vaporized part from stage g) as a residual gas and reuniting it with the mixture expanded in the turbine (3) and conveying it to the exchanger (2) and in that only a non-expanded second fraction of the mixture is distilled in the column.
  2. Process according to claim 1, characterized in that the nitrogen withdrawn as a product is in gaseous and/or liquid form.
  3. Process according to one of claims 1 and 2, consisting of recompressing a first fraction of the said compressed mixture in a compressor (50) driven by the turbine (3), and cooling the said recompressed first fraction and expanding it in the said turbine (3).
  4. Process according to one of claims 1 to 3, wherein the first fraction of the mixture is expanded in the turbine (3) to a pressure close to atmospheric pressure.
  5. Process according to one of claims 1 to 4, wherein a condensed part (20a) of the fraction enriched in nitrogen from stage e) is diverted to a buffer vessel (20c) when the production of gaseous nitrogen is reduced.
  6. Process according to claim 5, wherein part of the fraction enriched in oxygen from stage g) is diverted to a buffer vessel (7c) when the production of gaseous nitrogen is at a maximum.
EP94106964A 1989-08-18 1990-08-13 Process for preparing nitrogen Expired - Lifetime EP0610972B1 (en)

Applications Claiming Priority (3)

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FR8911009A FR2651035A1 (en) 1989-08-18 1989-08-18 PROCESS FOR THE PRODUCTION OF NITROGEN BY DISTILLATION
FR8911009 1989-08-18
EP90402289A EP0413631B1 (en) 1989-08-18 1990-08-13 Nitrogen production process

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EP0610972A3 (en) 1994-09-28
US5373699A (en) 1994-12-20
DE69030327T2 (en) 1997-10-30
CA2023503A1 (en) 1991-02-19
EP0413631B1 (en) 1994-12-28
JP3162361B2 (en) 2001-04-25
FR2651035A1 (en) 1991-02-22
DE69015504T2 (en) 1995-06-01
EP0413631A1 (en) 1991-02-20
FR2651035B1 (en) 1994-12-23
DE69015504D1 (en) 1995-02-09
CA2023503C (en) 2000-06-27
JPH03186183A (en) 1991-08-14
DE69030327D1 (en) 1997-04-30
US5325674A (en) 1994-07-05
EP0610972A2 (en) 1994-08-17

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