CA2782958A1 - Process and unit for the separation of air by cryogenic distillation - Google Patents
Process and unit for the separation of air by cryogenic distillation Download PDFInfo
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- CA2782958A1 CA2782958A1 CA2782958A CA2782958A CA2782958A1 CA 2782958 A1 CA2782958 A1 CA 2782958A1 CA 2782958 A CA2782958 A CA 2782958A CA 2782958 A CA2782958 A CA 2782958A CA 2782958 A1 CA2782958 A1 CA 2782958A1
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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
- F25J3/04436—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using at least a triple pressure main column system
- F25J3/04454—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using at least a triple pressure main column system a main column system not otherwise provided, e.g. serially coupling of columns or more than three pressure levels
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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
- F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
- F25J3/04066—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams 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
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04163—Hot end purification of the feed air
- F25J3/04169—Hot end purification of the feed air by adsorption of the impurities
- F25J3/04181—Regenerating the adsorbents
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
- F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
- F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
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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
- F25J3/04309—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 nitrogen
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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
- F25J3/04412—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 in a classical double column flowsheet, 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
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/04—Mixing or blending of fluids with the feed stream
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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
- F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
- F25J2230/42—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being nitrogen
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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
- F25J2240/00—Processes or apparatus involving steps for expanding of process streams
- F25J2240/40—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval
- F25J2240/46—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval 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
- 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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- 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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream 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
- F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
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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
Abstract
Un appareil de séparation d'air comprend une colonne moyenne pression (39), une colonne basse pression (41), une enceinte (141), un échangeur (13), un condenseur de cuve (25) de la colonne basse pression et un condenseur (15) placé dans l'enceinte, une conduite pour envoyer de l'air comprimé, épuré et refroidi de l'échangeur à la colonne moyenne pression, une conduite pour envoyer un gaz calorigène au condenseur placé dans l'enceinte, une conduite pour envoyer un gaz enrichi en azote de la colonne moyenne pression au condenseur de la colonne basse pression, une conduite pour envoyer un débit enrichi en oxygène de la cuve de la colonne moyenne pression à la colonne basse pression, une conduite pour envoyer du liquide riche en oxygène de la cuve de la colonne basse pression à l'enceinte, une conduite pour soutirer de l'enceinte un fluide plus riche en oxygène que celui envoyé à l'enceinte, une conduite pour renvoyer un gaz de l'enceinte à la colonne basse pression, une conduite pour soutirer un gaz en tête de la colonne basse pression caractérisé en ce qu'il comprend un moyen de détente (51) pour détendre le liquide riche en oxygène en aval de la cuve de la colonne basse pression et en amont de l'enceinte et un compresseur (21) pour comprimer le gaz de l'enceinte en aval de l'enceinte et en amont de la colonne basse pression.An air separation apparatus comprises a medium pressure column (39), a low pressure column (41), an enclosure (141), an exchanger (13), a bottom condenser (25) of the low pressure column and a condenser (15) placed in the enclosure, a pipe for sending compressed, purified and cooled air from the exchanger to the medium pressure column, a pipe for sending a circulating gas to the condenser placed in the enclosure, a pipe to send a gas enriched in nitrogen from the medium pressure column to the condenser of the low pressure column, a pipe for sending a flow enriched in oxygen from the bottom of the medium pressure column to the low pressure column, a pipe for sending rich liquid in oxygen from the bottom of the low pressure column to the enclosure, a pipe for withdrawing from the enclosure a fluid richer in oxygen than that sent to the enclosure, a pipe for returning a gas from the enclosure to the column low pressure, a pipe for sout flow a gas at the top of the low pressure column characterized in that it comprises an expansion means (51) for expanding the oxygen-rich liquid downstream of the bottom of the low pressure column and upstream of the enclosure and a compressor (21) for compressing the gas from the enclosure downstream from the enclosure and upstream from the low pressure column.
Description
Procédé et appareil de séparation d'air par distillation cryogénique La présente invention est relative à un procédé et à un appareil de séparation d'air par distillation cryogénique.
Il est connu de séparer l'air dans un appareil comprenant une colonne moyenne pression et deux colonnes basse pression opérant à la même pression, une des colonnes basse pression étant alimentée en tête par le liquide de cuve de l'autre et chaque colonne basse pression ayant un io condenseur de cuve.
Un but de l'invention est de réduire l'énergie de séparation pour produire de l'oxygène impur, en particulier dans le cas où il n'y a pas de co-production d'azote.
Un autre but de l'invention est de réduire le coût d'au moins certains éléments de l'appareil.
Tous les pourcentages relatifs à des puretés sont des pourcentages molaires.
L'invention implique l'utilisation d'un compresseur froid pour comprimer un gaz riche en oxygène, provenant d'une enceinte opérant à une pression en dessous de celle de la colonne basse pression, le gaz étant destiné à la cuve d'une colonne basse pression. Ceci permet de découpler la pression en cuve de colonne moyenne pression avec le haut de la colonne basse pression.
L'invention est particulièrement intéressante pour le cas où de l'air se condense partiellement dans le condenseur de l'enceinte opérant à plus basse pression que la colonne basse pression.
Selon un objet de l'invention, il est prévu un procédé de séparation d'air par distillation cryogénique dans lequel :
i) un débit d'air comprimé et épuré est refroidi dans un échangeur et envoyé à une colonne opérant à une moyenne pression ii) le débit d'air se sépare en un débit enrichi en azote et un débit enrichi en oxygène iii) une partie du débit enrichi en azote est envoyé à une colonne basse pression Method and apparatus for separating air by cryogenic distillation The present invention relates to a method and apparatus for air separation by cryogenic distillation.
It is known to separate the air in a device comprising a column medium pressure and two low pressure columns operating at the same pressure, one of the low pressure columns being fed at the head by the vessel liquid of the other and each low pressure column having a tank condenser.
An object of the invention is to reduce the separation energy to produce impure oxygen, especially in the case where there is no co-production nitrogen.
Another object of the invention is to reduce the cost of at least some elements of the device.
All percentages for purities are percentages molars.
The invention involves the use of a cold compressor to compress a gas rich in oxygen, coming from an enclosure operating at a pressure in below that of the low pressure column, the gas being intended for the tank a low pressure column. This allows to decouple the tank pressure of medium pressure column with the top of the low pressure column.
The invention is particularly interesting for the case where air is partially condensed in the condenser of the speaker operating at lower pressure than the low pressure column.
According to one object of the invention, there is provided an air separation method by cryogenic distillation in which:
i) a flow of compressed and purified air is cooled in an exchanger and sent to a column operating at a moderate pressure ii) the airflow separates into a nitrogen-enriched flow and a flow rate enriched with oxygen iii) part of the nitrogen-enriched flow is sent to a column low pressure
2 iv) au moins une partie du débit enrichi en oxygène est envoyée à la colonne basse pression v) un débit riche en azote est soutiré de la tête de la colonne basse pression vi) un débit riche en oxygène est soutiré de la cuve de la colonne basse pression et envoyé à une enceinte contenant au moins un condenseur-vaporiseur vii) un débit gazeux provenant de l'enceinte en est soutiré renvoyé à la première colonne basse pression, de préférence en cuve viii) une partie du débit enrichi en azote de l'étape ii) se condense au moins partiellement dans un condenseur alimenté par un liquide de cuve de la colonne basse pression et est envoyé à la colonne moyenne pression et/ou la colonne basse pression ix) un débit de gaz calorigène, éventuellement au moins une partie de l'air comprimé, épuré et refroidi dans l'échangeur de l'étape i), se condense au moins partiellement dans le condenseur vaporiseur de l'enceinte x) on soutire un fluide plus riche en oxygène de l'enceinte que le débit soutiré en cuve de la colonne basse pression caractérisé en ce que l'on détend le débit riche en oxygène soutiré de la cuve de la colonne basse pression en amont de l'enceinte et on pressurise le débit gazeux de l'enceinte en amont de la première colonne basse pression.
De préférence :
- on comprime le débit gazeux provenant de l'enceinte dans un compresseur ayant une température d'entrée inférieure à -50 C, de préférence aucun étape de chauffage a lieu entre l'enceinte et le compresseur ;
- on détend le débit riche en oxygène soutiré de la colonne basse pression à une pression au plus 1 bar en dessous de la pression en cuve de la colonne basse pression, de préférence au plus 0,5 bar, voire au plus 0,2 bar en dessous de cette pression et/ou on comprime le débit gazeux provenant de l'enceinte pour augmenter sa pression d'au plus 1 bar, de préférence au plus 0,5 bar, voire au plus 0,2 bar en amont de la colonne basse pression , - l'enceinte ne contient pas de moyen d'échange de masse, voire ne contient ni garnissages ni plateaux de distillation , 2 (iv) at least part of the oxygen enriched flow is sent to the low pressure column (v) a nitrogen-rich flow is withdrawn from the head of the lower column pressure vi) a flow rich in oxygen is withdrawn from the tank of the column low pressure and sent to an enclosure containing at least one condenser-vaporizer (vii) a gas flow from the enclosure is withdrawn and returned to the first low pressure column, preferably in the tank viii) a portion of the nitrogen enriched flow of step ii) condenses to less partially in a condenser fed by a liquid tank of the low pressure column and is sent to the medium pressure column and / or the low pressure column (ix) a flow of caloric gas, possibly at least a part of compressed air, purified and cooled in the exchanger of step i), condenses at less partially in the evaporator condenser of the enclosure x) a fluid richer in oxygen from the enclosure is withdrawn than the flow rate withdrawn in vat from the low pressure column characterized in that the oxygen-rich flow rate withdrawn from the tank of the low pressure column upstream of the enclosure and pressurize the gaseous flow of the enclosure upstream of the first low pressure column.
Preferably:
the gas flow from the enclosure is compressed in a compressor having an inlet temperature lower than -50 C, preferably no heating step takes place between the enclosure and the compressor;
the oxygen-rich flow rate withdrawn from the lower column is expanded pressure at a pressure not exceeding 1 bar below the tank pressure of the low pressure column, preferably at most 0.5 bar, or at most 0.2 bar below this pressure and / or compressing the gas flow from the enclosure to increase its pressure by at most 1 bar, preferably at most 0.5 bar, or at most 0.2 bar upstream of the low pressure column, - the enclosure does not contain any means of mass exchange, or even contains neither garnishes nor distillation trays,
3 - l'enceinte constitue une deuxième colonne basse pression et contient des moyens d'échange de masse, tels que des garnissages ou des plateaux de distillation, placés au moins au-dessus du condenseur.
Selon un autre objet de l'invention, il est prévu un appareil de séparation d'air comprenant une colonne moyenne pression, une colonne basse pression, une enceinte, un échangeur, un condenseur de cuve de la colonne basse pression et un condenseur placé dans l'enceinte, une conduite pour envoyer de l'air comprimé, épuré et refroidi de l'échangeur à la colonne moyenne pression, une conduite pour envoyer un gaz calorigène au condenseur placé
io dans l'enceinte, une conduite pour envoyer un gaz enrichi en azote de la colonne moyenne pression au condenseur de la colonne basse pression, une conduite pour envoyer un débit enrichi en oxygène de la cuve de la colonne moyenne pression à la colonne basse pression, une conduite pour envoyer du liquide riche en oxygène de la cuve de la colonne basse pression à l'enceinte, une conduite pour soutirer de l'enceinte un fluide plus riche en oxygène que celui envoyé à l'enceinte, une conduite pour renvoyer un gaz de l'enceinte à
la colonne basse pression, une conduite pour soutirer un gaz en tête de la colonne basse pression caractérisé en ce qu'il comprend un moyen de détente pour détendre le liquide riche en oxygène en aval de la cuve de la colonne basse pression et en amont de l'enceinte et un compresseur pour comprimer le gaz de l'enceinte en aval de l'enceinte et en amont de la colonne basse pression.
Eventuellement :
- l'enceinte comprend des moyens d'échange de matière au-dessus du condenseur;
- l'enceinte ne comprend aucun moyen d'échange de matière au-dessus du condenseur;
- l'appareil comprend une turbine et une conduite pour envoyer un gaz riche en azote de la colonne moyenne pression à la turbine ;
- l'appareil comprend une pompe pour pressuriser un débit d'oxygène liquide provenant de la colonne basse pression et/ou de l'enceinte en amont de l'échangeur. 3 - the enclosure constitutes a second column low pressure and contains mass exchange means, such as packings or trays of distillation, placed at least above the condenser.
According to another object of the invention, there is provided a separation apparatus of air comprising a medium pressure column, a low pressure column, an enclosure, an exchanger, a bottom column condenser pressure and a condenser placed in the enclosure, a pipe to send Compressed, purified and cooled air from the exchanger to the middle column pressure, a pipe to send a caloric gas to the condenser placed in the enclosure, a pipe for sending a nitrogen-enriched gas from the medium pressure column at the condenser of the low pressure column, a driving to send an oxygen-enriched flow of the column vessel medium pressure at the low pressure column, a pipe to send oxygen rich liquid from the tank of the low pressure column to the enclosure, a pipe for withdrawing from the enclosure a fluid richer in oxygen than the one sent to the enclosure, a pipe to return a gas from the enclosure to the low pressure column, a pipe to draw a gas at the head of the low pressure column characterized in that it comprises a means of relaxation to relax the oxygen-rich liquid downstream of the column vessel low pressure and upstream of the enclosure and a compressor to compress the gas from the enclosure downstream of the enclosure and upstream of the lower column pressure.
Eventually :
the enclosure includes means for exchanging material over the condenser;
- the enclosure does not include any means of exchange of material above the condenser;
the apparatus comprises a turbine and a pipe for sending a gas rich in nitrogen from the medium pressure column to the turbine;
- the device includes a pump to pressurize a flow of oxygen liquid from the low pressure column and / or the chamber upstream of the exchanger.
4 L'invention sera décrite en plus de détail en se référant aux figures, qui représentent des appareils selon l'invention.
Dans la Figure 1, l'air 1 est comprimé entre 3 et 5 bars dans un compresseur 3, épuré dans une unité d'épuration 5 et divisé en deux. Une partie 9 se refroidit dans l'échangeur 13 et est envoyée au condenseur de cuve d'une enceinte 141 où elle se condense partiellement avant être envoyé à la colonne moyenne pression 39 d'une double colonne.
La double colonne comprend la colonne moyenne pression 39 et une colonne basse pression 41 qui la surmonte, le lien thermique entre les deux io colonnes étant assuré par un condenseur 25 dans la cuve de la colonne basse pression 41.
L'autre partie de l'air 7 est comprimé dans un compresseur 11, refroidi dans l'échangeur 13 et utilisé pour vaporiser de l'oxygène liquide sous pression. Comme l'oxygène est vaporisé à une basse pression la vaporisation 15 a lieu dans un vaporiseur extérieur 27, distinct de l'échangeur 13. L'air liquéfié
ainsi formé est envoyé à la colonne moyenne pression 39 après détente dans une vanne 19. L'air liquide peut également être envoyé à la colonne basse pression.
Un liquide enrichi en oxygène 17 est soutiré en cuve de la colonne moyenne pression 39, refroidi dans l'échangeur 43, détendu dans une vanne et envoyé à la colonne basse pression 41. Un liquide 49 ayant substantiellement la composition de l'air est soutiré à un niveau intermédiaire de la colonne moyenne pression 39, refroidi dans l'échangeur 43, détendu dans une vanne et envoyé à la colonne basse pression 41. Un liquide enrichi en azote 47 est soutiré en tête de la colonne moyenne pression 39, refroidi dans l'échangeur 43, détendu dans une vanne et envoyé en tête de la colonne basse pression 41.
Un gaz 45 riche en azote est soutiré en tête de la colonne basse pression, chauffé dans l'échangeur 43 et ensuite dans l'échangeur 13. Une partie de ce gaz peut être comprimé dans le compresseur 35 pour former le débit 37 qui participe à la régénération de l'unité d'épuration 5.
Un débit d'azote moyenne pression 33 est soutiré en tête de la colonne moyenne pression 39, chauffé dans l'échangeur 13, détendu dans la turbine 23 et de nouveau chauffé dans l'échangeur 13 avant de servir à la régénération de l'unité d'épuration 5.
Un débit riche en oxygène 53 contenant entre 45 et 75 % d'oxygène est soutiré de la cuve de la colonne basse pression 41, détendu dans une vanne 4 The invention will be described in more detail with reference to the figures, which represent apparatus according to the invention.
In Figure 1, air 1 is compressed between 3 and 5 bar in a compressor 3, purified in a purification unit 5 and divided into two. A
part 9 cools in the exchanger 13 and is sent to the tank condenser of a chamber 141 where it partially condenses before being sent to the medium pressure column 39 of a double column.
The double column comprises the medium pressure column 39 and a low pressure column 41 which overcomes it, the thermal link between the two columns being provided by a condenser 25 in the bottom column of the column pressure 41.
The other part of the air 7 is compressed in a compressor 11, cooled in the exchanger 13 and used to vaporize liquid oxygen under pressure. As oxygen is vaporized at low pressure the vaporization 15 takes place in an external vaporizer 27, separate from the exchanger 13. The air liquefied thus formed is sent to the medium pressure column 39 after relaxation in a valve 19. The liquid air can also be sent to the lower column pressure.
An oxygen-enriched liquid 17 is withdrawn in the bottom of the column medium pressure 39, cooled in the exchanger 43, expanded in a valve and sent to the low pressure column 41. A liquid 49 having substantially the composition of the air is drawn off at an intermediate level of the column medium pressure 39, cooled in the exchanger 43, expanded in a valve and sent to the low pressure column 41. A nitrogen-enriched liquid 47 is withdrawn at the top of the medium pressure column 39, cooled in the exchanger 43, relaxed in a valve and sent to the top of the lower column pressure 41.
A gas 45 rich in nitrogen is withdrawn at the top of the column pressure, heated in the exchanger 43 and then in the exchanger 13.
part of this gas can be compressed in the compressor 35 to form the flow 37 which participates in the regeneration of the purification unit 5.
A medium pressure nitrogen flow 33 is withdrawn at the top of the column medium pressure 39, heated in the exchanger 13, expanded in the turbine 23 and again heated in the exchanger 13 before being used for regeneration of the purification unit 5.
A flow rich in oxygen 53 containing between 45 and 75% of oxygen is withdrawn from the tank of the low pressure column 41, expanded in a valve
5 51 et envoyé en tête de l'enceinte 141 qui dans cette variante est une colonne de distillation avec un condenseur de cuve 15. Au-dessus du condenseur se trouvent des moyens d'échange de chaleur et de masse 143, par exemple des garnissages, structurés ou pas, ou des plateaux. La vanne 51 ne fait baisser la pression du liquide que de 0.15 bar environ Le liquide 53 est séparé dans l'enceinte pour former un liquide plus riche en oxygène 29 en cuve. C'est ce liquide 29 qui est envoyé au vaporiseur 27 après pressurisation dans la pompe 63. Un liquide de purge 61 est soutiré du vaporiseur 27. Alternativement un gaz riche en oxygène peut être soutiré de l'enceinte 141.
Un gaz de tête 145 est soutiré de l'enceinte, comprimé à la température de soutirage dans un compresseur 21 qui fait augmenter sa pression d'au plus 0.15.bars. Le gaz produit est réinjecté dans la cuve de la colonne basse pression à la pression de sortie du compresseur 21.
Avec un écart de température dans l'échangeur 13 de 2 C au bout chaud, on obtient un gain d'environ 2.5% par rapport au même schéma sans le compresseur froid en cuve de la colonne basse pression L'appareil de la figure 2 diffère de celui de la figure 1 en ce que l'enceinte 141 ne contient pas de garnissages ou de plateaux. Il y a aussi la condensation partielle ascendante dans le vaporiseur 15. Ainsi la différence de composition entre le liquide 53 envoyé à l'enceinte et le liquide 29 soutiré
de l'enceinte est très réduite même si le liquide 29 est tout de même plus riche en oxygène que le liquide 53. Le gaz 145 est le gaz produit par vaporisation partielle du liquide 53 dans l'enceinte 141 par échange de chaleur avec l'air 9.
Si on serre l'écart de température au bout chaud de l'échangeur 13 à
2 C, on a un gain d'environ 1.5% par rapport au même schéma sans compresseur froid en cuve BP.
On obtient une énergie très légèrement meilleure celui du procédé de WO-A-2007/129152 avec l'échangeur serré à 2 C au bout chaud. Même si 51 and sent to the top of the enclosure 141 which in this variant is a column of distillation with a tank condenser 15. Above the condenser is find means of heat exchange and mass 143, for example packings, structured or not, or trays. The valve 51 does not lower the liquid pressure only about 0.15 bar The liquid 53 is separated in the chamber to form a richer liquid in oxygen 29 in the tank. It is this liquid 29 which is sent to the vaporizer 27 after pressurization in the pump 63. A purge liquid 61 is withdrawn from the vaporizer 27. Alternatively a gas rich in oxygen can be withdrawn from the enclosure 141.
A top gas 145 is withdrawn from the chamber, compressed at room temperature in a compressor 21 which increases its pressure by at most 0.15.bars. The product gas is reinjected into the bottom column pressure at the outlet pressure of the compressor 21.
With a temperature difference in the exchanger 13 from 2 C to the end warm, we obtain a gain of about 2.5% compared to the same scheme without the cold compressor in tank of low pressure column The apparatus of Figure 2 differs from that of Figure 1 in that enclosure 141 does not contain packings or trays. There is also the partial condensation upward in the vaporizer 15. So the difference of composition between the liquid 53 sent to the chamber and the liquid 29 withdrawn of the enclosure is very small even if the liquid 29 is still richer in oxygen as the liquid 53. The gas 145 is the gas produced by vaporization partial of the liquid 53 in the chamber 141 by heat exchange with the air 9.
If we close the temperature difference at the hot end of the exchanger 13 to 2 C, we have a gain of about 1.5% compared to the same scheme without cold compressor in tank BP.
A slightly better energy is obtained than that of the process of WO-A-2007/129152 with the exchanger tight 2 C hot end. Even if
6 dans les deux procédés, on utilise un compresseur froid, dans la variante de l'invention la puissance du compresseur froid est 10 fois plus petite que dans la variante de l'art antérieur et la turbine azote 2 fois plus petite. On constate aussi que le taux de compression dans la variante selon l'invention est très faible et qu'une technologie proche d'un ventilateur doit suffire pour le compresseur 21 : ces éléments permettent de dire que le compresseur froid 21 et la turbine 23 seront moins coûteux que dans le procédé de l'art antérieur.
La compression cryogénique d'un fluide relativement riche en oxygène ne doit pas poser de problème de sécurité.
Le concept de compression de la partie vapeur dans la colonne basse pression peut être étendu au cas des schémas avec trois condenseurs dans la colonne basse pression, avec un ou deux compresseurs froid à placer entre les trois condenseurs de la colonne basse pression. 6 in both processes, a cold compressor is used, in the variant of the invention the power of the cold compressor is 10 times smaller than in the variant of the prior art and the nitrogen turbine 2 times smaller. We finds also that the compression ratio in the variant according to the invention is very low and that a technology close to a fan should suffice for the compressor 21: these elements make it possible to say that the cold compressor 21 and the turbine 23 will be less expensive than in the method of the prior art.
Cryogenic compression of a relatively oxygen-rich fluid must not pose a security problem.
The concept of compression of the steam part in the lower column pressure can be extended to the case of diagrams with three condensers in the low pressure column, with one or two cold compressors to be placed between three condensers of the low pressure column.
Claims (10)
i) un débit d'air comprimé et épuré est refroidi dans un échangeur (13) et envoyé à une colonne (39) opérant à une moyenne pression ii) le débit d'air se sépare en un débit enrichi en azote et un débit enrichi en oxygène iii) une partie du débit enrichi en azote est envoyé à une colonne basse pression (41) iv) au moins une partie du débit enrichi en oxygène est envoyée à
la colonne basse pression v) un débit riche en azote est soutiré de la tête de la colonne basse pression vi) un débit riche en oxygène est soutiré de la cuve de la colonne basse pression et envoyé à une enceinte (141) contenant au moins un condenseur-vaporiseur (15) vii) un débit gazeux provenant de l'enceinte en est soutiré renvoyé à
la colonne basse pression, de préférence en cuve, viii) une partie du débit enrichi en azote de l'étape ii) se condense au moins partiellement dans un condenseur (25) alimenté par du liquide provenant de la colonne basse pression et est envoyé à la colonne moyenne pression et/ou la colonne basse pression ix) un débit de gaz calorigène, éventuellement au moins une partie de l'air comprimé, épuré et refroidi dans l'échangeur de l'étape i), se condense au moins partiellement dans le condenseur vaporiseur de l'enceinte x) on soutire un fluide plus riche en oxygène de l'enceinte que le débit soutiré en cuve de la colonne basse pression xi) caractérisé en ce que l'on détend le débit riche en oxygène soutiré de la cuve de la colonne basse pression en amont de l'enceinte et on pressurise le débit gazeux de l'enceinte en amont de la première colonne basse pression. A process for separating air by cryogenic distillation in which:
i) a flow of compressed and purified air is cooled in a heat exchanger (13) and sent to a column (39) operating at medium pressure ii) the airflow separates into a nitrogen-enriched flow and a flow rate enriched with oxygen iii) part of the nitrogen-enriched flow is sent to a column low pressure (41) (iv) at least part of the oxygen-enriched flow is sent to the low pressure column (v) a nitrogen-rich flow is withdrawn from the head of the lower column pressure vi) a flow rich in oxygen is withdrawn from the tank of the column low pressure and sent to an enclosure (141) containing at least one condenser-vaporizer (15) (vii) a gas flow from the enclosure is withdrawn and returned to the low pressure column, preferably in the tank, viii) a portion of the nitrogen enriched flow of step ii) condenses to least partially in a condenser (25) supplied with liquid from of the low pressure column and is sent to the medium pressure column and / or the low pressure column (ix) a flow of caloric gas, possibly at least a part compressed air, purified and cooled in the exchanger of step i), condenses at least partially in the vaporizer condenser of the enclosure x) a fluid richer in oxygen from the enclosure is withdrawn than the flow withdrawn in tank of the low pressure column xi) characterized in that the oxygen-rich flow is expanded withdrawn from the tank of the low pressure column upstream of the enclosure and pressurizes the gaseous flow of the chamber upstream of the first column low pressure.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0958880A FR2953915B1 (en) | 2009-12-11 | 2009-12-11 | METHOD AND APPARATUS FOR AIR SEPARATION BY CRYOGENIC DISTILLATION |
| FR0958880 | 2009-12-11 | ||
| PCT/FR2010/052099 WO2011070257A1 (en) | 2009-12-11 | 2010-10-05 | Process and unit for the separation of air by cryogenic distillation |
Publications (1)
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| CA2782958A1 true CA2782958A1 (en) | 2011-06-16 |
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| CA2782958A Abandoned CA2782958A1 (en) | 2009-12-11 | 2010-10-05 | Process and unit for the separation of air by cryogenic distillation |
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| US (1) | US20120285197A1 (en) |
| EP (1) | EP2510294B1 (en) |
| JP (1) | JP5694363B2 (en) |
| CN (1) | CN102652247B (en) |
| AU (1) | AU2010329766B2 (en) |
| CA (1) | CA2782958A1 (en) |
| ES (1) | ES2486260T3 (en) |
| FR (1) | FR2953915B1 (en) |
| WO (1) | WO2011070257A1 (en) |
| ZA (1) | ZA201203625B (en) |
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| FR2990500A1 (en) * | 2012-05-11 | 2013-11-15 | Air Liquide | METHOD AND APPARATUS FOR AIR SEPARATION BY CRYOGENIC DISTILLATION |
| GB201409669D0 (en) | 2014-05-30 | 2014-07-16 | Highview Entpr Ltd | Improvements in air purification units |
| EP3026380A1 (en) * | 2014-11-27 | 2016-06-01 | Linde Aktiengesellschaft | Method and device for discharging heavier than air volatile components from an air separation facility |
| EP3290843A3 (en) * | 2016-07-12 | 2018-06-13 | Linde Aktiengesellschaft | Method and device for extracting pressurised nitrogen and pressurised nitrogen by cryogenic decomposition of air |
| CN106440660A (en) * | 2016-10-10 | 2017-02-22 | 浙江海天气体有限公司 | Air separation device with high-pressure heat exchange and oxygen supply |
| FR3074274B1 (en) * | 2017-11-29 | 2020-01-31 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | METHOD AND APPARATUS FOR AIR SEPARATION BY CRYOGENIC DISTILLATION |
| FR3090082B1 (en) * | 2018-12-13 | 2021-01-29 | Air Liquide | Apparatus for separating or liquefying a gas operating at cryogenic temperatures. |
| WO2020124427A1 (en) * | 2018-12-19 | 2020-06-25 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method for starting up a cryogenic air separation unit and associated air separation unit |
| FR3090831B1 (en) * | 2018-12-21 | 2022-06-03 | L´Air Liquide Sa Pour L’Etude Et L’Exploitation Des Procedes Georges Claude | Cryogenic distillation air separation apparatus and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4617036A (en) * | 1985-10-29 | 1986-10-14 | Air Products And Chemicals, Inc. | Tonnage nitrogen air separation with side reboiler condenser |
| CN1025067C (en) * | 1989-02-23 | 1994-06-15 | 琳德股份公司 | Process and method of seperating air by rectification |
| DE4126945A1 (en) * | 1991-08-14 | 1993-02-18 | Linde Ag | METHOD FOR AIR DISASSEMBLY BY RECTIFICATION |
| JP2966999B2 (en) * | 1992-04-13 | 1999-10-25 | 日本エア・リキード株式会社 | Ultra high purity nitrogen / oxygen production equipment |
| DE19537913A1 (en) * | 1995-10-11 | 1997-04-17 | Linde Ag | Triple column process for the low temperature separation of air |
| EP0793069A1 (en) * | 1996-03-01 | 1997-09-03 | Air Products And Chemicals, Inc. | Dual purity oxygen generator with reboiler compressor |
| US5664438A (en) * | 1996-08-13 | 1997-09-09 | Praxair Technology, Inc. | Cryogenic side column rectification system for producing low purity oxygen and high purity nitrogen |
| GB9711258D0 (en) * | 1997-05-30 | 1997-07-30 | Boc Group Plc | Air separation |
| US5934104A (en) * | 1998-06-02 | 1999-08-10 | Air Products And Chemicals, Inc. | Multiple column nitrogen generators with oxygen coproduction |
| JP2003014373A (en) * | 2001-07-02 | 2003-01-15 | Hitachi Ltd | Air separator apparatus |
| FR2844039B1 (en) * | 2002-09-04 | 2005-04-29 | Air Liquide | PROCESS AND PLANT FOR PRODUCING OXYGEN AND RARE GASES BY CRYOGENIC AIR DISTILLATION |
| US6622520B1 (en) * | 2002-12-11 | 2003-09-23 | Praxair Technology, Inc. | Cryogenic rectification system for producing low purity oxygen using shelf vapor turboexpansion |
| JP4230213B2 (en) * | 2002-12-24 | 2009-02-25 | 大陽日酸株式会社 | Air liquefaction separation apparatus and method |
| FR2854683B1 (en) * | 2003-05-05 | 2006-09-29 | Air Liquide | METHOD AND INSTALLATION FOR PRODUCING PRESSURIZED AIR GASES BY AIR CRYOGENIC DISTILLATION |
| US20070251267A1 (en) | 2006-04-26 | 2007-11-01 | Bao Ha | Cryogenic Air Separation Process |
| US20090241595A1 (en) * | 2008-03-27 | 2009-10-01 | Praxair Technology, Inc. | Distillation method and apparatus |
| WO2009136077A2 (en) * | 2008-04-22 | 2009-11-12 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and apparatus for separating air by cryogenic distillation |
| FR2930327A1 (en) * | 2008-04-22 | 2009-10-23 | Air Liquide | Air separating method for carbon oxycombustion frame, involves sending oxygen and nitrogen enrich liquids, and reheating nitrogen rich flow from low pressure columns and oxygen rich flow in exchange line |
-
2009
- 2009-12-11 FR FR0958880A patent/FR2953915B1/en not_active Expired - Fee Related
-
2010
- 2010-10-05 AU AU2010329766A patent/AU2010329766B2/en not_active Ceased
- 2010-10-05 WO PCT/FR2010/052099 patent/WO2011070257A1/en active Application Filing
- 2010-10-05 EP EP10776785.7A patent/EP2510294B1/en not_active Not-in-force
- 2010-10-05 JP JP2012542592A patent/JP5694363B2/en not_active Expired - Fee Related
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- 2010-10-05 US US13/515,059 patent/US20120285197A1/en not_active Abandoned
- 2010-10-05 CA CA2782958A patent/CA2782958A1/en not_active Abandoned
- 2010-10-05 CN CN201080055693.4A patent/CN102652247B/en not_active Expired - Fee Related
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2012
- 2012-05-17 ZA ZA2012/03625A patent/ZA201203625B/en unknown
Also Published As
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| AU2010329766B2 (en) | 2014-06-12 |
| FR2953915B1 (en) | 2011-12-02 |
| ZA201203625B (en) | 2013-01-30 |
| ES2486260T3 (en) | 2014-08-18 |
| JP5694363B2 (en) | 2015-04-01 |
| US20120285197A1 (en) | 2012-11-15 |
| EP2510294A1 (en) | 2012-10-17 |
| WO2011070257A1 (en) | 2011-06-16 |
| JP2013513775A (en) | 2013-04-22 |
| FR2953915A1 (en) | 2011-06-17 |
| CN102652247B (en) | 2014-09-24 |
| CN102652247A (en) | 2012-08-29 |
| AU2010329766A1 (en) | 2012-07-05 |
| EP2510294B1 (en) | 2014-04-30 |
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| FZDE | Discontinued |
Effective date: 20161005 |