EP0531182B1 - Process and plant for distilling air and application in the feeding of gas to steel plants - Google Patents
Process and plant for distilling air and application in the feeding of gas to steel plants Download PDFInfo
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- EP0531182B1 EP0531182B1 EP92402246A EP92402246A EP0531182B1 EP 0531182 B1 EP0531182 B1 EP 0531182B1 EP 92402246 A EP92402246 A EP 92402246A EP 92402246 A EP92402246 A EP 92402246A EP 0531182 B1 EP0531182 B1 EP 0531182B1
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- liquid
- oxygen
- auxiliary gas
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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
- F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
- F25J3/04527—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general
- F25J3/04551—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the metal production
- F25J3/04557—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the metal production for pig iron or steel making, e.g. blast furnace, Corex
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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
- F25J3/04006—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
- F25J3/0409—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 oxygen
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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
- F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low pressure 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
- F25J3/0446—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 heat generated by mixing two different phases
- F25J3/04466—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 heat generated by mixing two different phases for producing oxygen as a mixing column overhead gas by mixing gaseous air feed and liquid oxygen
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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
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
- F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
- F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
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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
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
- F25J2200/06—Processes or apparatus using separation by rectification in a dual pressure main column system in a classical double column flow-sheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure 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
- F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
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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
- F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
- F25J2200/94—Details relating to the withdrawal point
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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
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
- F25J2215/52—Oxygen production with multiple purity O2
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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
- F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
- F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen
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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
- F25J2250/00—Details related to the use of reboiler-condensers
- F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
- F25J2250/40—One fluid being air
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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
- F25J2250/00—Details related to the use of reboiler-condensers
- F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
- F25J2250/50—One fluid being oxygen
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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
- Y10S62/915—Combustion
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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 an air distillation method as defined in the preambles of claims 1 and 2 and an air distillation installation according to the preambles of claims 10 and 11.
- Such a method and such an installation are known. for example, from document FR-A-2 169 561.
- FR-A-2.169.561 describes a process for the distillation of air in which a mixing column is supplied with a flow of liquid oxygen, coming from a double column and by part of the supply air of the double column.
- This mixing column operates at a pressure substantially the same as that of the medium pressure column of the double column.
- Certain industrial applications require significant quantities of impure oxygen under various pressures: gasification of coal, gasification of petroleum residues, direct reduction-smelting of iron ore, injection of coals into blast furnaces, metallurgy of non-ferrous metals, etc.
- the object of the invention is to satisfy such needs economically, that is to say to allow, with a relatively low investment and energy consumption, the production of impure oxygen at a selected purity and pressure. at will and, if necessary, the production of practically pure oxygen.
- the subject of the invention is a process for the distillation of air by means of a double distillation column coupled to a mixing column, as defined either in claim 1 or in claim 2.
- Said liquid can be the bottom liquid of the low pressure column, in particular oxygen practically without nitrogen, or else it can be drawn off a few trays above the bottom of the low pressure column.
- the invention also relates to an air distillation installation intended for the implementation of the process defined above, of the type described either in claim 10 or in claim 11.
- the invention also relates to the application of the process defined above to supplying gas to a steelworks, said impure oxygen being produced under the pressure of the blast furnace and being sent to the latter.
- said liquid is oxygen practically without nitrogen
- said oxygen is sent practically without nitrogen to the converters of the steelworks.
- FIGS. 1 to 3 schematically represent three embodiments of the air distillation installation according to the invention.
- the air distillation installation shown in FIG. 1 is intended to produce impure oxygen, for example having a purity of 80 to 97% and preferably 85 to 95%, under a determined pressure P clearly different from 6 x 105 Pa abs., Per example under 2 to 5 x 105 Pa or advantageously under a pressure higher by at least 2 x 105 Pa and being able to go up to approximately 30 x 105 Pa, preferably between 8 x 105 Pa and 15 x 105 Pa.
- Installation essentially comprises a heat exchange line 1, a double distillation column 2 itself comprising a medium pressure column 3, a low pressure column 4 and a main condenser-vaporizer 5, and a mixing column 6. Columns 3 and 4 typically operate at approximately 6 x 105 Pa and approximately 1 x 105 Pa, respectively.
- a mixing column is a column which has the same structure as a distillation column but which is used to mix in a manner close to reversibility a relatively volatile gas, introduced at its base, and a less volatile liquid, introduced at its top.
- Such a mixture produces refrigerating energy and therefore makes it possible to reduce the energy consumption linked to distillation.
- this mixture is used, moreover, to directly produce impure oxygen under pressure P, as will be described below.
- the air to be separated by distillation, compressed to 6 x 105 Pa and suitably purified, is conveyed to the base of the medium pressure column 3 by a pipe 7. Most of this air is cooled in the exchange line 1 and introduced at the base of the medium pressure column 3, and the rest, boosted at 8 then cooled, is expanded at low pressure in a turbine 9 coupled to the booster 8, then blown at an intermediate point of the low pressure column 4. From “rich liquid” (oxygen-enriched air), taken from the tank of column 3 is, after expansion in an expansion valve 10, introduced into column 4, approximately at the point of air blowing.
- Liquid oxygen is withdrawn from the tank of column 4, carried by a pump 13 at a pressure P1, slightly higher than the pressure P above to take account of losses load (P1-P less than 1 x 105 Pa), and introduced at the top of column 6.
- P1 is therefore advantageously between 8 x 105 Pa and 30 x 105 Pa, preferably between 8 x 105 Pa and 16 x 105 Pa.
- Auxiliary air, compressed at the same pressure P1 by an auxiliary compressor 14 and cooled in the exchange line 1, is introduced at the base of the mixing column 6.
- FIG. 1 also shows auxiliary heat exchangers 19, 20, 21 ensuring the recovery of the cold available in the fluids circulating in the installation.
- the pressure P of the impure oxygen produced can be chosen as desired.
- the adjustment of the double column makes it possible to obtain various degrees of purity for this gas.
- Another way of determining this degree of purity consists, as shown in FIG. 2, of choosing the level of sampling, in the low pressure column 4, of the liquid feeding the column 6, for example by leaving a few trays of distillation between the point and the column 4 tank.
- the installation can produce, simultaneously with the impure oxygen of column 6, oxygen at a different purity and at a pressure, in particular oxygen roughly pure, by drawing off at the bottom of column 4.
- This oxygen can be supplied in gaseous form, via a line 22 crossing the exchange line 1, under the low pressure of the low pressure column 4 or under pressure, in particular by pumping the liquid at 23 before it warms up in the exchange line; it can also be liquefied and sent to storage 24.
- FIG. 3 differs from that of FIG. 2 in that it also comprises a column 25 for producing impure argon coupled, in a conventional manner, to the low pressure column 4.
- the fact that the impure oxygen is produced not by the low pressure column 4 but by the mixing column 6 makes it possible to produce impure oxygen containing very little argon, which leaves the possibility of producing, in addition to argon, provided of course that the liquid oxygen withdrawn and pumped at 13 has sufficient purity, in particular at least equal to 98%.
- the air auxiliary to the pressure P1 may be suitably purified atmospheric air, but also come from an annex process comprising an air compressor. It may for example be air taken from the inlet of a gas turbine and the pressure of which may be adjusted by means of a booster or an expansion turbine. More generally, it is possible to use, to feed the base of the mixing column 6, a mixture of air gases less rich in oxygen than the liquid taken from the lower part of the low pressure column, in particular impure nitrogen originating possibly from the installation itself.
- the invention makes it possible to simultaneously produce, under particularly economical investment and energy consumption conditions, pure or nearly pure oxygen, impure oxygen and argon.
- the oxygen produced by column 4 is practically devoid of nitrogen and can therefore be used in the converters of a steelworks.
- the installation in the form of FIG. 2, thus makes it possible to supply both these converters with pure oxygen and the blast furnace of the steelworks with impure oxygen at the pressure of the blast furnace; in its form in FIG. 3, the installation can also supply the steelworks with argon.
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Description
La présente invention est relative à un procédé de distillation d'air tel que défini dans les préambules des revendications 1 et 2 et une installation de distillation d'air selon les préambules des revendications 10 et 11. Un tel procédé et une telle installation sont connus par exemple, du document FR-A-2 169 561.The present invention relates to an air distillation method as defined in the preambles of
FR-A-2.169.561 décrit un procédé de distillation d'air dans lequel une colonne de mélange est alimentée par un débit d'oxygène liquide, provenant d'une double colonne et par une partie de l'air d'alimentation de la double colonne. Cette colonne de mélange opère à une pression substantiellement la même que celle de la colonne moyenne pression de la double colonne.FR-A-2.169.561 describes a process for the distillation of air in which a mixing column is supplied with a flow of liquid oxygen, coming from a double column and by part of the supply air of the double column. This mixing column operates at a pressure substantially the same as that of the medium pressure column of the double column.
Certaines applications industrielles nécessitent des quantités importantes d'oxygène impur sous diverses pressions : gazéification du charbon, gazéification de résidus pétroliers, réduction-fusion directe du minerai de fer, injection de charbons dans les hauts fourneaux, métallurgie des métaux non ferreux, etc.Certain industrial applications require significant quantities of impure oxygen under various pressures: gasification of coal, gasification of petroleum residues, direct reduction-smelting of iron ore, injection of coals into blast furnaces, metallurgy of non-ferrous metals, etc.
Par ailleurs, certains contextes industriels nécessitent la fourniture simultanée, en grandes quantités, d'oxygène pratiquement pur et d'oxygène impur sous des pressions différentes. C'est notamment le cas des aciéries comportant des convertisseurs à l'oxygène et dans lesquelles le haut fourneau est alimenté en oxygène ou en air enrichi en oxygène.In addition, certain industrial contexts require the simultaneous supply, in large quantities, of practically pure oxygen and impure oxygen under different pressures. This is particularly the case for steelworks with oxygen converters and in which the blast furnace is supplied with oxygen or oxygen-enriched air.
L'invention a pour but de satisfaire de tels besoins de façon économique, c'est-à-dire de permettre, avec un investissement et une consommation d'énergie relativement faibles, la production d'oxygène impur à une pureté et une pression choisies à volonté et, si nécessaire, la production d'oxygène pratiquement pur.The object of the invention is to satisfy such needs economically, that is to say to allow, with a relatively low investment and energy consumption, the production of impure oxygen at a selected purity and pressure. at will and, if necessary, the production of practically pure oxygen.
A cet effet, l'invention a pour objet un procédé de distillation d'air au moyen d'une double colonne de distillation couplée à une colonne de mélange, tel que défini soit dans la revendication 1, soit dans la revendication 2.To this end, the subject of the invention is a process for the distillation of air by means of a double distillation column coupled to a mixing column, as defined either in claim 1 or in
Ledit liquide peut être le liquide de cuve de la colonne basse pression, notamment de l'oxygène pratiquement sans azote, ou bien être soutiré quelques plateaux au-dessus de la cuve de la colonne basse pression.Said liquid can be the bottom liquid of the low pressure column, in particular oxygen practically without nitrogen, or else it can be drawn off a few trays above the bottom of the low pressure column.
Dans le cadre d'un tel procédé, on peut en outre produire de l'argon au moyen d'une colonne de distillation additionnelle de production d'argon impur couplée à la colonne basse pression.In the context of such a process, it is also possible to produce argon by means of an additional distillation column for producing impure argon coupled to the low pressure column.
L'invention a également pour objet une installation de distillation d'air destinée à la mise en oeuvre du procédé défini ci-dessus, du type décrit soit dans la revendication 10, soit dans la revendication 11.The invention also relates to an air distillation installation intended for the implementation of the process defined above, of the type described either in
L'invention a encore pour objet l'application du procédé défini plus haut à l'alimentation en gaz d'une aciérie, ledit oxygène impur étant produit sous la pression du haut fourneau et étant envoyé à ce dernier.The invention also relates to the application of the process defined above to supplying gas to a steelworks, said impure oxygen being produced under the pressure of the blast furnace and being sent to the latter.
Lorsque ledit liquide est de l'oxygène pratiquement sans azote, de façon avantageuse, on envoie ledit oxygène pratiquement sans azote aux convertisseurs de l'aciérie.When said liquid is oxygen practically without nitrogen, advantageously, said oxygen is sent practically without nitrogen to the converters of the steelworks.
Des exemples de mise en oeuvre de l'invention vont maintenant être décrits en regard des dessins annexés, sur lesquels les figures 1 à 3 représentent schématiquement trois modes de réalisation de l'installation de distillation d'air conforme à l'invention.Examples of implementation of the invention will now be described with reference to the accompanying drawings, in which FIGS. 1 to 3 schematically represent three embodiments of the air distillation installation according to the invention.
L'installation de distillation d'air représentée à la figure 1 est destinée à produire de l'oxygène impur, par exemple ayant une pureté de 80 à 97 % et de préférence de 85 à 95 %, sous une pression déterminée P nettement différente de 6 x 10⁵ Pa abs., par exemple sous 2 à 5 x 10⁵ Pa ou avantageusement sous une pression supérieure d'au moins 2 x 10⁵ Pa et pouvant aller jusqu'à 30 x 10⁵ Pa environ, de préférence entre 8 x 10⁵ Pa et 15 x 10⁵ Pa. L'installation comprend essentiellement une ligne d'échange thermique 1, une double colonne de distillation 2 comprenant elle-même une colonne moyenne pression 3, une colonne basse pression 4 et un condenseur-vaporiseur principal 5, et une colonne de mélange 6. Les colonnes 3 et 4 fonctionnent typiquement sous environ 6 x 10⁵ Pa et environ 1 x 10⁵ Pa, respectivement.The air distillation installation shown in FIG. 1 is intended to produce impure oxygen, for example having a purity of 80 to 97% and preferably 85 to 95%, under a determined pressure P clearly different from 6 x 10⁵ Pa abs., Per example under 2 to 5 x 10⁵ Pa or advantageously under a pressure higher by at least 2 x 10⁵ Pa and being able to go up to approximately 30 x 10⁵ Pa, preferably between 8 x 10⁵ Pa and 15 x 10⁵ Pa. Installation essentially comprises a heat exchange line 1, a
Comme expliqué en détail dans le document US-A-4.022.030, une colonne de mélange est une colonne qui a la même structure qu'une colonne de distillation mais qui est utilisée pour mélanger de façon proche de la réversibilité un gaz relativement volatil, introduit à sa base, et un liquide moins volatil, introduit à son sommet.As explained in detail in document US-A-4,022,030, a mixing column is a column which has the same structure as a distillation column but which is used to mix in a manner close to reversibility a relatively volatile gas, introduced at its base, and a less volatile liquid, introduced at its top.
Un tel mélange produit de l'énergie frigorifique et permet donc de réduire la consommation d'énergie liée à la distillation. Dans le cas présent, ce mélange est mis à profit, en outre, pour produire directement de l'oxygène impur sous la pression P, comme cela sera décrit ci-dessous.Such a mixture produces refrigerating energy and therefore makes it possible to reduce the energy consumption linked to distillation. In the present case, this mixture is used, moreover, to directly produce impure oxygen under pressure P, as will be described below.
L'air à séparer par distillation, comprimé à 6 x 10⁵ Pa et convenablement épuré, est acheminé vers la base de la colonne moyenne pression 3 par une conduite 7. La majeure partie de cet air est refroidie dans la ligne d'échange 1 et introduite à la base de la colonne moyenne pression 3, et le reste, surpressé en 8 puis refroidi, est détendu à la basse pression dans une turbine 9 couplée au surpresseur 8, puis insufflé en un point intermédiaire de la colonne basse pression 4. Du "liquide riche" (air enrichi en oxygène), prélevé en cuve de la colonne 3 est, après détente dans une vanne de détente 10, introduit dans la colonne 4, à peu près au point d'insufflation de l'air. Du "liquide pauvre" (azote impur) prélevé en un point intermédiaire 11 de la colonne 3 est, après détente dans une vanne de détente 12, introduit au sommet de la colonne 4, constituant le gaz résiduaire de l'installation, et l'azote gazeux pur sous la moyenne pression produit en tête de la colonne 3, sont réchauffés dans la ligne d'échange 1 et évacués de l'installation. Ces gaz sont indiqués respectivement par NI et NG sur la figure 1.The air to be separated by distillation, compressed to 6 x 10⁵ Pa and suitably purified, is conveyed to the base of the
De l'oxygène liquide, plus ou moins pur suivant le réglage de la double colonne 2, est soutiré en cuve de la colonne 4, porté par une pompe 13 à une pression P1, légèrement supérieure à la pression P précitée pour tenir compte des pertes de charge (P1-P inférieur à 1 x 10⁵ Pa), et introduit au sommet de la colonne 6. P1 est donc avantageusement comprise entre 8 x 10⁵ Pa et 30 x 10⁵ Pa, de préférence entre 8 x 10⁵ Pa et 16 x 10⁵ Pa. De l'air auxiliaire, comprimé à la même pression P1 par un compresseur auxiliaire 14 et refroidi dans la ligne d'échange 1, est introduit à la base de la colonne de mélange 6. De cette dernière sont soutirés trois courants de fluide : à sa base, du liquide voisin du liquide riche et réuni à ce dernier via une conduite 15 munie d'une vanne de détente 15A ; en un point intermédiaire, un mélange essentiellement constitué d'oxygène et d'azote, qui est renvoyé en un point intermédiaire de la colonne basse pression 4 via une conduite 16 munie d'une vanne de détente 17 ; et à son sommet de l'oxygène impur qui, après réchauffement dans la ligne d'échange thermique, est évacué, sensiblement à la pression P, de l'installation via une conduite 18 en tant que gaz de production 0I.Liquid oxygen, more or less pure depending on the setting of the
On a également représenté sur la figure 1 des échangeurs de chaleur auxiliaires 19, 20, 21 assurant la récupération du froid disponible dans les fluides en circulation dans l'installation.FIG. 1 also shows
Comme on le comprend, grâce à la présence d'un circuit séparé pour l'air auxiliaire alimentant la colonne 6, on peut choisir à volonté la pression P de l'oxygène impur produit. De plus, comme indiqué plus haut, le réglage de la double colonne permet d'obtenir divers degrés de pureté pour ce gaz.As will be understood, thanks to the presence of a separate circuit for the auxiliary
Une autre manière de déterminer ce degré de pureté consiste, comme représenté à la figure 2, à choisir le niveau de prélèvement, dans la colonne basse pression 4, du liquide alimentant la colonne 6, par exemple en laissant quelques plateaux de distillation entre le point de prélèvement et la cuve de la colonne 4.Another way of determining this degree of purity consists, as shown in FIG. 2, of choosing the level of sampling, in the low pressure column 4, of the liquid feeding the
Comme on l'a également représenté sur la figure 2, l'installation peut produire, simultanément à l'oxygène impur de la colonne 6, de l'oxygène à une pureté et à une pression différentes, notamment de l'oxygène à peu près pur, par soutirage au bas de la colonne 4. Cet oxygène peut être fourni sous forme gazeuse, via une conduite 22 traversant la ligne d'échange 1, sous la basse pression de la colonne basse pression 4 ou sous pression, notamment par pompage du liquide en 23 avant son réchauffement dans la ligne d'échange ; il peut aussi être liquéfié et envoyé dans un stockage 24.As also shown in FIG. 2, the installation can produce, simultaneously with the impure oxygen of
L'installation de la figure 3 diffère de celle de la figure 2 par le fait qu'elle comprend en outre une colonne 25 de production d'argon impur couplée, de façon classique, à la colonne basse pression 4.The installation of FIG. 3 differs from that of FIG. 2 in that it also comprises a
En effet, le fait que l'oxygène impur soit produit non pas par la colonne basse pression 4 mais par la colonne de mélange 6 permet de produire de l'oxygène impur contenant très peu d'argon, ce qui laisse la possibilité de produire, en plus de l'argon, à condition bien entendu que l'oxygène liquide soutiré et pompé en 13 ait une pureté suffisante, notamment au moins égale à 98 %.Indeed, the fact that the impure oxygen is produced not by the low pressure column 4 but by the
L'air auxiliaire à la pression P1 peut être de l'air atmosphérique convenablement épuré, mais également provenir d'un procédé annexe comprenant un compresseur d'air. Il peut par exemple s'agir d'air prélevé à l'entrée d'une turbine à gaz et dont la pression est éventuellement ajustée au moyen d'un surpresseur ou d'une turbine de détente. Plus généralement, on peut utiliser pour alimenter la base de la colonne de mélange 6, un mélange de gaz de l'air moins riche en oxygène que le liquide prélevé dans la partie inférieure de la colonne basse pression, notamment de l'azote impur provenant éventuellement de l'installation elle-même.The air auxiliary to the pressure P1 may be suitably purified atmospheric air, but also come from an annex process comprising an air compressor. It may for example be air taken from the inlet of a gas turbine and the pressure of which may be adjusted by means of a booster or an expansion turbine. More generally, it is possible to use, to feed the base of the
Ainsi, l'invention permet de produire simultanément, dans des conditions particulièrement économiques d'investissement et de consommation d'énergie, de l'oxygène pur ou à peu près pur, de l'oxygène impur et de l'argon.Thus, the invention makes it possible to simultaneously produce, under particularly economical investment and energy consumption conditions, pure or nearly pure oxygen, impure oxygen and argon.
Il est à noter que l'oxygène produit par la colonne 4 est pratiquement dépourvu d'azote et peut donc être utilisé dans les convertisseurs d'une aciérie. L'installation, sous la forme de la figure 2, permet ainsi d'alimenter à la fois ces convertisseurs en oxygène pur et le haut fourneau de l'aciérie en oxygène impur à la pression du haut fourneau ; sous sa forme de la figure 3, l'installation peut alimenter en outre l'aciérie en argon.It should be noted that the oxygen produced by column 4 is practically devoid of nitrogen and can therefore be used in the converters of a steelworks. The installation, in the form of FIG. 2, thus makes it possible to supply both these converters with pure oxygen and the blast furnace of the steelworks with impure oxygen at the pressure of the blast furnace; in its form in FIG. 3, the installation can also supply the steelworks with argon.
Claims (17)
- Process for the distillation of air by means of a double distillation column (2) coupled to a mixing column (6), wherein the mixing column is supplied at the vessel with an auxiliary gas consisting of a mixture of air gases and at the head with a liquid richer in oxygen than the auxiliary gas, withdrawn from the lower part of the low pressure column (4), and impure oxygen constituting a production gas is withdrawn from the head of the mixing column (6), characterized in that the auxiliary gas and liquid supplying the mixing column (6) are compressed essentially to the same first pressure (P₁) greater than that of the medium pressure column (3).
- Process for the distillation of air by means of an installation comprising a double distillation column (2) coupled with a mixing column (6), wherein the mixing column is supplied at the vessel with an auxiliary gas consisting of a mixture of air gases and at the head with a liquid richer in oxygen than the auxiliary gas, withdrawn from the lower part of the low pressure column (4), and impure oxygen constituting a production gas is withdrawn from the head of the mixing column (6), characterized in that the auxiliary gas comes from a source other than the said installation and that the auxiliary gas and the liquid supplying the mixing column (6) are compressed essentially to the same first pressure (P₁) less than that of the medium pressure column (3).
- Process according to either of claims 1 or 2, characterized in that the liquid is the liquid in the vessel of the low pressure column (4).
- Process according to claim 3, characterized in that the liquid is oxygen practically without nitrogen.
- Process according to any one of claims 1 to 4, characterized in that the said liquid is withdrawn several plates above the vessel of the low pressure column (4).
- Process according to any one of claims 1 to 5, characterized in that oxygen is withdrawn from the vessel of the low pressure column (4) to constitute a second production gas.
- Process according to any one of claims 1 to 6, characterized in that argon is also produced by means of an additional distillation column for producing impure argon (25) coupled to the low pressure column (4).
- Process according to claim 1, or one of claims 3 to 7, dependent on claim 1, characterized in that the first pressure (P₁) is greater by at least 2 x 10⁵ Pa than the pressure in the medium pressure column.
- Process according to claim 8, characterized in that the first pressure lies between 8 x 10⁵ Pa and 16 x 10⁵ Pa.
- Installation for the distillation of air of the type comprising a double distillation column (2), a mixing column (6), a heat exchange line (1), a source of auxiliary gas consisting of a mixture of air gases, means for introducing the auxiliary gas at the base of the mixing column (6), means for withdrawing a liquid richer in oxygen than the auxiliary gas from the lower part of the low pressure column (4), means (13) for pumping this liquid and for introducing it at the top of the mixing column, and means for withdrawing impure oxygen from the head of the mixing column as the production gas of the installation, means (14) for compressing the auxiliary gas to a given pressure (P₁) different from that of the medium pressure column (3), a means for pumping (13) and carrying the liquid at the said given pressure, characterized in that passages for this compressed auxiliary gas are provided in the heat exchange line (1) and in that the said given pressure (P₁) is greater than that of the medium pressure column.
- Installation for the distillation of air of the type comprising a double distillation column (2), a mixing column (6), a heat exchange line (1), a source of air to be distilled, a source of auxiliary gas consisting of a mixture of air gases, means for introducing the auxiliary gas at the base of the mixing column (6), means for withdrawing a liquid richer in oxygen than the auxiliary gas from the lower part of the low pressure column (4), means (13) for pumping this liquid and for introducing it at the top of the mixing column, and means for withdrawing impure oxygen from the head of the mixing column as the production gas of the installation, characterized in that the said sources are separate and that it comprises means (14) in a separate circuit for compressing the auxiliary gas in a separate circuit at a given pressure (P₁) less than that of the medium pressure column (3), and passages for this compressed auxiliary gas provided in the heat exchange line (1) and in that the means of pumping (13) carries the liquid at the said given pressure (P₁).
- Installation according to claim 10 or 11, characterized in that the said liquid is withdrawn from the vessel of the low pressure column (4).
- Installation according to claim 10 or 11, characterized in that the said liquid is withdrawn several plates above the vessel of low pressure column (4).
- Installation according to any one of claims 10 to 13, characterized in that it comprises means for withdrawing oxygen from the vessel of the low pressure column (4) as a second production gas of the installation.
- Installation according to any one of claims 10 to 14, characterized in that it comprises a column for producing impure argon (25) coupled to the low pressure column (4).
- Application of a process according to any one of claims 1 to 9, to the gas supply of a steel works comprising a blast furnace, impure oxygen being produced at the pressure of the blast furnace and being conveyed to the latter.
- Application according to claim 16, characterized in that, the process being according to claim 4, oxygen is conveyed practically without nitrogen to converters of the steel works.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9110035A FR2680114B1 (en) | 1991-08-07 | 1991-08-07 | METHOD AND INSTALLATION FOR AIR DISTILLATION, AND APPLICATION TO THE GAS SUPPLY OF A STEEL. |
FR9110035 | 1991-08-07 |
Publications (3)
Publication Number | Publication Date |
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EP0531182A1 EP0531182A1 (en) | 1993-03-10 |
EP0531182B1 true EP0531182B1 (en) | 1996-02-21 |
EP0531182B2 EP0531182B2 (en) | 2000-12-27 |
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ID=9415988
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP92402246A Expired - Lifetime EP0531182B2 (en) | 1991-08-07 | 1992-08-06 | Process and plant for distilling air and application in the feeding of gas to steel plants |
Country Status (9)
Country | Link |
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US (1) | US5291737A (en) |
EP (1) | EP0531182B2 (en) |
CN (1) | CN1062656C (en) |
AU (1) | AU655485B2 (en) |
BR (1) | BR9203049A (en) |
CA (1) | CA2075420C (en) |
DE (1) | DE69208412T3 (en) |
ES (1) | ES2083709T5 (en) |
FR (1) | FR2680114B1 (en) |
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FR2731781B1 (en) * | 1995-03-15 | 1997-05-23 | Air Liquide | METHOD AND APPARATUS FOR VAPORIZING LIQUID FLOW |
US5582036A (en) * | 1995-08-30 | 1996-12-10 | Praxair Technology, Inc. | Cryogenic air separation blast furnace system |
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FR2753638B1 (en) * | 1996-09-25 | 1998-10-30 | PROCESS FOR SUPPLYING A GAS CONSUMER UNIT | |
FR2774159B1 (en) * | 1998-01-23 | 2000-03-17 | Air Liquide | COMBINED INSTALLATION OF AN OVEN AND AN AIR DISTILLATION APPARATUS AND METHOD OF IMPLEMENTING IT |
FR2774157B1 (en) * | 1998-01-23 | 2000-05-05 | Air Liquide | COMBINED INSTALLATION OF AN OVEN AND AN AIR DISTILLATION APPARATUS AND METHOD OF IMPLEMENTING IT |
FR2776057B1 (en) * | 1998-03-11 | 2000-06-23 | Air Liquide | METHOD AND PLANT FOR AIR SEPARATION BY CRYOGENIC DISTILLATION |
US5865041A (en) * | 1998-05-01 | 1999-02-02 | Air Products And Chemicals, Inc. | Distillation process using a mixing column to produce at least two oxygen-rich gaseous streams having different oxygen purities |
FR2782787B1 (en) * | 1998-08-28 | 2000-09-29 | Air Liquide | PROCESS AND PLANT FOR PRODUCING IMPURED OXYGEN BY AIR DISTILLATION |
FR2789162B1 (en) * | 1999-02-01 | 2001-11-09 | Air Liquide | PROCESS FOR SEPARATING AIR BY CRYOGENIC DISTILLATION |
FR2801963B1 (en) * | 1999-12-02 | 2002-03-29 | Air Liquide | METHOD AND PLANT FOR AIR SEPARATION BY CRYOGENIC DISTILLATION |
FR2795496B1 (en) * | 1999-06-22 | 2001-08-03 | Air Liquide | APPARATUS AND METHOD FOR SEPARATING AIR BY CRYOGENIC DISTILLATION |
FR2814178B1 (en) * | 2000-09-18 | 2002-10-18 | Air Liquide | SUPPLY OF OXYGEN-ENRICHED AIR TO A NON-FERROUS METAL PRODUCTION UNIT |
DE60024634T2 (en) * | 2000-10-30 | 2006-08-03 | L'Air Liquide, S.A. a Directoire et Conseil de Surveillance pour l'Etude et l'Exploitation des Procédés Georges Claude | Method and apparatus for cryogenic air separation integrated with associated method |
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EP1387136A1 (en) * | 2002-08-02 | 2004-02-04 | Linde AG | Process and device for producing impure oxygen by cryogenic air distillation |
FR2861841B1 (en) * | 2003-11-04 | 2006-06-30 | Air Liquide | METHOD AND APPARATUS FOR AIR SEPARATION BY CRYOGENIC DISTILLATION |
FR2862128B1 (en) * | 2003-11-10 | 2006-01-06 | Air Liquide | PROCESS AND INSTALLATION FOR SUPPLYING HIGH-PURITY OXYGEN BY CRYOGENIC AIR DISTILLATION |
FR2862004B3 (en) * | 2003-11-10 | 2005-12-23 | Air Liquide | METHOD AND INSTALLATION FOR ENRICHING A GASEOUS FLOW IN ONE OF ITS CONSTITUENTS |
FR2866900B1 (en) | 2004-02-27 | 2006-05-26 | Air Liquide | METHOD FOR RENOVATING A COMBINED INSTALLATION OF A HIGH STOVE AND A GAS SEPARATION UNIT OF THE AIR |
EP1666824A1 (en) * | 2004-12-03 | 2006-06-07 | Linde Aktiengesellschaft | Process and device for the recovery of Argon by cryogenic separation of air |
FR2895068B1 (en) * | 2005-12-15 | 2014-01-31 | Air Liquide | AIR SEPARATION METHOD BY CRYOGENIC DISTILLATION |
FR2898134B1 (en) | 2006-03-03 | 2008-04-11 | Air Liquide | METHOD FOR INTEGRATING A HIGH-FURNACE AND A GAS SEPARATION UNIT OF THE AIR |
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CN111271940A (en) * | 2020-01-19 | 2020-06-12 | 浙江智海化工设备工程有限公司 | Novel oxygen-enriched production method |
CN115885146A (en) * | 2020-07-22 | 2023-03-31 | 乔治洛德方法研究和开发液化空气有限公司 | Argon enhancement method and apparatus |
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US4595405A (en) * | 1984-12-21 | 1986-06-17 | Air Products And Chemicals, Inc. | Process for the generation of gaseous and/or liquid nitrogen |
DE3722746A1 (en) * | 1987-07-09 | 1989-01-19 | Linde Ag | METHOD AND DEVICE FOR AIR DISASSEMBLY BY RECTIFICATION |
FR2655137B1 (en) * | 1989-11-28 | 1992-10-16 | Air Liquide | AIR DISTILLATION PROCESS AND INSTALLATION WITH ARGON PRODUCTION. |
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-
1991
- 1991-08-07 FR FR9110035A patent/FR2680114B1/en not_active Expired - Fee Related
-
1992
- 1992-07-31 US US07/923,336 patent/US5291737A/en not_active Expired - Lifetime
- 1992-08-05 AU AU20798/92A patent/AU655485B2/en not_active Ceased
- 1992-08-06 EP EP92402246A patent/EP0531182B2/en not_active Expired - Lifetime
- 1992-08-06 DE DE69208412T patent/DE69208412T3/en not_active Expired - Fee Related
- 1992-08-06 ES ES92402246T patent/ES2083709T5/en not_active Expired - Lifetime
- 1992-08-06 BR BR929203049A patent/BR9203049A/en not_active IP Right Cessation
- 1992-08-06 CA CA002075420A patent/CA2075420C/en not_active Expired - Fee Related
- 1992-08-07 CN CN92110647A patent/CN1062656C/en not_active Expired - Fee Related
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EP0531182B2 (en) | 2000-12-27 |
CN1062656C (en) | 2001-02-28 |
FR2680114B1 (en) | 1994-08-05 |
AU655485B2 (en) | 1994-12-22 |
US5291737A (en) | 1994-03-08 |
DE69208412T3 (en) | 2001-08-23 |
CA2075420C (en) | 2003-05-13 |
DE69208412T2 (en) | 1996-07-04 |
ES2083709T3 (en) | 1996-04-16 |
CN1071000A (en) | 1993-04-14 |
AU2079892A (en) | 1993-02-11 |
CA2075420A1 (en) | 1993-02-08 |
ES2083709T5 (en) | 2001-03-16 |
EP0531182A1 (en) | 1993-03-10 |
DE69208412D1 (en) | 1996-03-28 |
FR2680114A1 (en) | 1993-02-12 |
BR9203049A (en) | 1993-05-04 |
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