EP0413631B1 - Procédé de production d'azote - Google Patents
Procédé de production d'azote Download PDFInfo
- Publication number
- EP0413631B1 EP0413631B1 EP90402289A EP90402289A EP0413631B1 EP 0413631 B1 EP0413631 B1 EP 0413631B1 EP 90402289 A EP90402289 A EP 90402289A EP 90402289 A EP90402289 A EP 90402289A EP 0413631 B1 EP0413631 B1 EP 0413631B1
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- EP
- European Patent Office
- Prior art keywords
- column
- nitrogen
- pressure stage
- fraction
- mixture
- 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.)
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims description 54
- 229910052757 nitrogen Inorganic materials 0.000 title claims description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000000203 mixture Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 4
- 230000008016 vaporization Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000003303 reheating Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 101100536354 Drosophila melanogaster tant gene Proteins 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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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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- 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
- F25J3/04284—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
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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
- F25J3/04284—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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- 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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- F25J3/04—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
- F25J3/04333—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
- 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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- 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
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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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04333—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
- 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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- 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
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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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- 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
- F25J3/04406—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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- 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
- F25J3/04472—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
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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
- 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
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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
- 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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- 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
- 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
- F25J2200/54—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
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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
- 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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
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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
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S62/00—Refrigeration
- Y10S62/901—Single column
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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
- 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
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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
- 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 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 production of cold necessary for the process is possibly ensured by expansion of at least one refrigerant gas flow, which may be the mixture to be treated, which is expanded at the low pressure of the column, and injected into the column.
- at least one refrigerant gas flow which may be the mixture to be treated, which is expanded at the low pressure of the column, and injected into the column.
- this current is cooled to an intermediate temperature represented by the level (2a). Then, a first part of this gas stream is expanded at low pressure of the order of 3 to 5 bar abs. in the turbine (3), then introduced into the distillation column (4).
- a second and last part continues to cool in the exchanger (2) until total or partial liquefaction (111) is expanded in the valve (112) and is introduced into the column (4) at an intermediate level, above the point of introduction of the expanded gas stream.
- the distillation column (4) can therefore be divided into 3 zones, respectively from top to bottom (4a), (4b), (4c).
- a part condensed in the exchanger (5) ensures part of the reflux of the distillation.
- a part can be extracted in liquid form by a pipe.
- a part is extracted, in gaseous form through the conduit (11).
- the corresponding current is heated if necessary, in a first exchanger, then in the exchanger (2), to obtain at the outlet of the latter a stream of relatively pure nitrogen 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), condensed at least in part at the bottom of the column (155), in the exchanger (166), by heat exchange with the fraction rich in relatively heavy nitrogen during vaporization, at the bottom of the column (155). Then the current (14) optionally passes through an impurity trap such as CO of the cold adsorption type (167) shown in dotted lines, expanded in a valve (168), and introduced into the column (155) at an intermediate level.
- an impurity trap such as CO of the cold adsorption type (167) shown in dotted lines, expanded in a valve (168), and introduced into the column (155) at an intermediate level.
- the relatively light fraction available at the head of this same column (155) is almost entirely condensed in the exchanger (6) existing at the foot of the column (4), in exchange for heat with the oxygen-rich fraction being vaporization, available at the bottom of the column (4).
- the non-condensed fraction available at the outlet of the exchanger (6) is mixed with the waste gas (9) after expansion.
- the relatively heavy fraction at the bottom of the column (155) is discharged through the conduit (18), in gaseous form, --- heated in the exchanger (2), and discharged in the heated state of the installation.
- a relatively heavy fraction available in liquid form at the bottom of the second stage (155) is drawn off into a stream (177) which is expanded in the valve (169) and introduced at the head of the first distillation stage (4).
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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 séparer, tel que de l'air, contenant principalement de l'azote et de l'oxygène.
Pour produire de l'azote gazeux à partir d'air atmosphérique par exemple, US-A-4662917 décrit un procédé consistant à : - a) comprimer le mélange à traiter à une pression au moins égale à la pression de fonctionnement de l'étage basse pression (4) de ladite colonne, de l'ordre de 3 à 5 bars,
- b) refroidir le mélange comprimé, puis réaliser ensuite la distillation du mélange dans la colonne et obtenir, dans la partie basse de la colonne, une fraction enrichie en oxygène et, dans la partie haute de la colonne, une fraction enrichie en azote,
- c) extraire au moins une partie de la fraction enrichie en azote en tant que produit, et
- d) comprimer la partie restante de la fraction enrichie en azote.
- Selon la présente invention, un procédé de production comprend les caractéristiques (a) à (d) ci-dessus. Or, la colonne de distillation de la présente invention comprend un étage basse pression et un étage moyenne pression. Le procédé de la présente invention est caractérisé en ce qu'il comprend les étapes de :
- e) recycler au moins une partie de ladite partie restante de la fraction enrichie en azote dans l'échangeur (166) de la cuve de l'étage moyenne pression (155) de ladite colonne, dans lequel cette partie se condense sous forme d'un liquide riche en azote,
- f) détendre et introduire au moins une partie du liquide riche en azote condensé dans l'étape (e) ci-dessus à un niveau intermédiaire de l'étage moyenne pression (155) de la colonne en tant que liquide de reflux,
- g) extraire une fraction enrichie en oxygène sous forme liquide, de la partie inférieure de l'étage basse pression (4) de la colonne et détendre au moins une partie de ladite fraction à une pression inférieure à la pression de l'étage basse pression (4) 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 et
- h) extraire et réchauffer un flux de production relativement lourd de l'étage moyenne pression (155).
- 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 au froid de l'appareil par détente dans une turbine d'un gaz pauvre en oxygène.
- Selon la présente invention, la production de froid nécessaire au procédé est éventuellement assurée par détente d'au moins un flux gazeux frigorigène, pouvant être le mélange à traiter, qui est détendu à la basse pression de la colonne, et injecté dans la colonne.
- La présente invention est maintenant décrite par référence au dessin annexe, qui représente un mode d'exécution du procédé selon l'invention.
- Tout d'abord, la distillation fractionnée est effectuée en deux étages, à savoir :
- un premier étage à température relativement basse, fonctionnant sous une pression relativement basse, comprise entre 3 et 5 bars,
- et un second étage (155) à température relativement haute, fonctionnant sous une pression relativement haute, comprise entre 6 et 12 bars.
- On comprime (de manière non représentée), à une pression supérieure à la basse pression de la colonne de distillation (4), définie ci-après, un courant de gaz, par exemple d'air préalablement épuré de manière traditionnelle.
- Dans l'échangeur de chaleur (2), ce courant est refroidi jusqu'à une température intermédiaire représentée par le niveau (2a). Puis, une première partie de ce courant gazeux est détendue à la basse pression de l'ordre de 3 à 5 bars abs. dans la turbine (3), puis introduite dans la colonne de distillation (4).
- Une seconde et dernière partie poursuit son refroidissement dans l'échangeur (2) jusqu'à liquéfaction totale ou partielle (111) est détendue dans la vanne (112) et est introduite dans la colonne (4) à un niveau intermédiaire, au-dessus du point d'introduction du courant gazeux détendu.
- La colonne de distillation (4) peut donc être divisée en 3 zones, respectivement de haut en bas (4a), (4b), (4c).
- 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 une conduite. Une partie est extraite, sous forme gazeuse par le conduit (11).
- Le courant correspondant est réchauffé le cas échéant, dans un premier échangeur, puis 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.
- 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), condensé au moins en partie au pied de la colonne (155), dans l'échangeur (166), par échange de chaleur avec la fraction riche en azote relativement lourde en cours de vaporisation, au pied de la colonne (155). Puis le courant (14) passe éventuellement dans un piège à impuretés -telle CO- du type à adsorption froide (167) représentée en pointillé, détendu dans une vanne (168), et introduit dans la colonne (155) à un niveau intermédiaire. La fraction relativement légère disponible en tête de cette même colonne (155) est en quasi-totalité condensée dans l'échangeur (6) existant au pied de la colonne (4), en échange de chaleur avec la fraction riche en oxygène en cours de vaporisation, disponible au pied de la colonne (4). La fraction non condensée disponible en sortie de l'échangeur (6) est mélangée au gaz résiduaire (9) après détente.
- La fraction relativement lourde au pied de la colonne (155) est évacuée par le conduit (18), sous forme gazeuse,---réchauffée dans l'échangeur (2), et évacuée à l'état réchauffé de l'installation. Une fraction relativement lourde disponible sous forme liquide au pied du deuxième étage (155) est soutirée en un courant (177) qui est détendu dans la vanne (169) et introduit en tête du premier étage (4) de distillation.
Claims (4)
- Procédé de production d'azote gazeux à partir d'un mélange à traiter dans une colonne de distillation ayant un étage basse pression (4) et un étage moyenne pression (155), ledit mélange comportant notamment de l'azote et de l'oxygène, ledit procédé consistant à :a) comprimer le mélange à traiter à une pression au moins égale à la pression de fonctionnement de l'étage basse pression (4) de ladite colonne, de l'ordre de 3 à 5 bars,b) refroidir le mélange comprimé, puis réaliser ensuite la distillation du mélange dans la colonne et obtenir, dans partie basse de la colonne, une fraction enrichie en oxygène et, dans la partie haute de la colonne, une fraction enrichie en azote,c) extraire au moins une partie de la fraction enrichie en azote en tant que produit,d) comprimer la partie restante de la fraction enrichie en azote,e) recycler au moins une partie de ladite partie restante de la fraction enrichie en azote dans l'échangeur (166) de la cuve de l'étage moyenne pression (155) de ladite colonne, dans lequel cette partie se condense sous forme d'un liquide riche en azote,f) détendre et introduire au moins une partie du liquide riche en azote condensé dans l'étape (e) ci-dessus à un niveau intermédiaire de l'étage moyenne pression (155) de la colonne en tant que liquide de reflux,g) extraire une fraction enrichie en oxygène sous forme liquide, de la partie inférieure de l'étage basse pression (4) de la colonne et détendre au moins une partie de ladite fraction à une pression inférieure à la pression de l'étage basse pression (4) 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 eth) extraire et réchauffer un flux de production relativement lourd de l'étage moyenne pression (155).
- Procédé selon la revendication 1, caractérisé en ce que la tenue en froid de l'appareil est assurée par détente adiabatique (polytropique) d'un ou plusieurs flux gazeux frigorigènes, dont l'un au moins est le mélange à traiter.
- Procédé selon la revendication 2, caractérisé en ce que le flux gazeux frigorigène est au moins une partie du mélange à traiter (1), détendu (3) avant son introduction dans l'étage basse pression.
- Procédé selon une des revendications précédentes caractérisé en ce que l'azote condensé en échange de chaleur avec la fraction en cuve de l'étage moyenne pression (155) passe dans un piège à impuretés (167) avant d'être introduit dans la colonne au niveau intermédiaire.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP94106964A EP0610972B1 (fr) | 1989-08-18 | 1990-08-13 | Procédé de production d'azote |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8911009 | 1989-08-18 | ||
FR8911009A FR2651035A1 (fr) | 1989-08-18 | 1989-08-18 | Procede de production d'azote par distillation |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP94106964.3 Division-Into | 1990-08-13 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0413631A1 EP0413631A1 (fr) | 1991-02-20 |
EP0413631B1 true EP0413631B1 (fr) | 1994-12-28 |
Family
ID=9384790
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP90402289A Expired - Lifetime EP0413631B1 (fr) | 1989-08-18 | 1990-08-13 | Procédé de production d'azote |
EP94106964A Expired - Lifetime EP0610972B1 (fr) | 1989-08-18 | 1990-08-13 | Procédé de production d'azote |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP94106964A Expired - Lifetime EP0610972B1 (fr) | 1989-08-18 | 1990-08-13 | Procédé de production d'azote |
Country Status (6)
Country | Link |
---|---|
US (2) | US5325674A (fr) |
EP (2) | EP0413631B1 (fr) |
JP (1) | JP3162361B2 (fr) |
CA (1) | CA2023503C (fr) |
DE (2) | DE69030327T2 (fr) |
FR (1) | FR2651035A1 (fr) |
Families Citing this family (21)
Publication number | Priority date | Publication date | Assignee | Title |
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US5251450A (en) * | 1992-08-28 | 1993-10-12 | Air Products And Chemicals, Inc. | Efficient single column air separation cycle and its integration with gas turbines |
FR2697325B1 (fr) * | 1992-10-27 | 1994-12-23 | Air Liquide | Procédé et installation de production d'azote et d'oxygène. |
FR2700205B1 (fr) * | 1993-01-05 | 1995-02-10 | Air Liquide | Procédé et installation de production d'au moins un produit gazeux sous pression et d'au moins un liquide par distillation d'air. |
US5303556A (en) * | 1993-01-21 | 1994-04-19 | Praxair Technology, Inc. | Single column cryogenic rectification system for producing nitrogen gas at elevated pressure and high purity |
US5511380A (en) | 1994-09-12 | 1996-04-30 | Liquid Air Engineering Corporation | High purity nitrogen production and installation |
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 |
DE19537910A1 (de) * | 1995-10-11 | 1997-04-17 | Linde Ag | Doppelsäulenverfahren und -vorrichtung zur Tieftemperaturzerlegung von Luft |
US5832748A (en) * | 1996-03-19 | 1998-11-10 | Praxair Technology, Inc. | Single column cryogenic rectification system for lower purity oxygen production |
US5682762A (en) * | 1996-10-01 | 1997-11-04 | Air Products And Chemicals, Inc. | Process to produce high pressure nitrogen using a high pressure column and one or more lower pressure columns |
US5794458A (en) * | 1997-01-30 | 1998-08-18 | The Boc Group, Inc. | Method and apparatus for producing gaseous oxygen |
US5868006A (en) * | 1997-10-31 | 1999-02-09 | The Boc Group, Inc. | Air separation method and apparatus for producing nitrogen |
US5934106A (en) * | 1998-01-27 | 1999-08-10 | The Boc Group, Inc. | Apparatus and method for producing nitrogen |
DE19843629A1 (de) | 1998-09-23 | 2000-03-30 | Linde Ag | Verfahren und Verflüssiger zur Erzeugung von flüssiger Luft |
US6279345B1 (en) | 2000-05-18 | 2001-08-28 | Praxair Technology, Inc. | Cryogenic air separation system with split kettle recycle |
GB0119500D0 (en) * | 2001-08-09 | 2001-10-03 | Boc Group Inc | Nitrogen generation |
US7114352B2 (en) * | 2003-12-24 | 2006-10-03 | Praxair Technology, Inc. | Cryogenic air separation system for producing elevated pressure nitrogen |
US20050247005A1 (en) * | 2004-04-01 | 2005-11-10 | Chris Mroz | Rigid ribbon having overall sinusoidal-like waveform shape |
US8753440B2 (en) * | 2011-03-11 | 2014-06-17 | General Electric Company | System and method for cooling a solvent for gas treatment |
JP6900230B2 (ja) | 2017-04-19 | 2021-07-07 | レール・リキード−ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード | 純度の異なる窒素を製造するための窒素製造システムおよびその窒素製造方法 |
US11686528B2 (en) | 2019-04-23 | 2023-06-27 | Chart Energy & Chemicals, Inc. | Single column nitrogen rejection unit with side draw heat pump reflux system and method |
WO2021242308A1 (fr) * | 2020-05-26 | 2021-12-02 | Praxair Technology, Inc. | Améliorations apportées à une unité de séparation d'air cryogénique à double colonne produisant de l'azote |
Citations (1)
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US4662917A (en) * | 1986-05-30 | 1987-05-05 | Air Products And Chemicals, Inc. | Process for the separation of air |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5231839B1 (fr) * | 1966-03-11 | 1977-08-17 | ||
FR2461906A1 (fr) * | 1979-07-20 | 1981-02-06 | Air Liquide | Procede et installation cryogeniques de separation d'air avec production d'oxygene sous haute pression |
US4594085A (en) * | 1984-11-15 | 1986-06-10 | Union Carbide Corporation | Hybrid nitrogen generator with auxiliary reboiler drive |
JPS61190277A (ja) * | 1985-02-16 | 1986-08-23 | 大同酸素株式会社 | 高純度窒素および酸素ガス製造装置 |
US4662918A (en) * | 1986-05-30 | 1987-05-05 | Air Products And Chemicals, Inc. | Air separation process |
US4662916A (en) * | 1986-05-30 | 1987-05-05 | Air Products And Chemicals, Inc. | Process for the separation of air |
US4834785A (en) * | 1988-06-20 | 1989-05-30 | Air Products And Chemicals, Inc. | Cryogenic nitrogen generator with nitrogen expander |
GB8820582D0 (en) * | 1988-08-31 | 1988-09-28 | Boc Group Plc | Air separation |
US4947649A (en) * | 1989-04-13 | 1990-08-14 | Air Products And Chemicals, Inc. | Cryogenic process for producing low-purity oxygen |
-
1989
- 1989-08-18 FR FR8911009A patent/FR2651035A1/fr active Granted
-
1990
- 1990-08-13 EP EP90402289A patent/EP0413631B1/fr not_active Expired - Lifetime
- 1990-08-13 DE DE69030327T patent/DE69030327T2/de not_active Expired - Fee Related
- 1990-08-13 EP EP94106964A patent/EP0610972B1/fr not_active Expired - Lifetime
- 1990-08-13 DE DE69015504T patent/DE69015504T2/de not_active Expired - Fee Related
- 1990-08-16 JP JP21507890A patent/JP3162361B2/ja not_active Expired - Fee Related
- 1990-08-17 CA CA002023503A patent/CA2023503C/fr not_active Expired - Fee Related
-
1992
- 1992-02-18 US US07/843,940 patent/US5325674A/en not_active Expired - Fee Related
-
1993
- 1993-10-08 US US08/133,292 patent/US5373699A/en not_active Expired - Lifetime
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4662917A (en) * | 1986-05-30 | 1987-05-05 | Air Products And Chemicals, Inc. | Process for the separation of air |
Also Published As
Publication number | Publication date |
---|---|
FR2651035B1 (fr) | 1994-12-23 |
DE69015504D1 (de) | 1995-02-09 |
EP0413631A1 (fr) | 1991-02-20 |
EP0610972A3 (en) | 1994-09-28 |
US5325674A (en) | 1994-07-05 |
DE69030327T2 (de) | 1997-10-30 |
FR2651035A1 (fr) | 1991-02-22 |
CA2023503A1 (fr) | 1991-02-19 |
JPH03186183A (ja) | 1991-08-14 |
EP0610972B1 (fr) | 1997-03-26 |
EP0610972A2 (fr) | 1994-08-17 |
CA2023503C (fr) | 2000-06-27 |
US5373699A (en) | 1994-12-20 |
DE69030327D1 (de) | 1997-04-30 |
DE69015504T2 (de) | 1995-06-01 |
JP3162361B2 (ja) | 2001-04-25 |
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