EP3604994B1 - Method and device for producing argon by cryogenic distillation of air - Google Patents
Method and device for producing argon by cryogenic distillation of air Download PDFInfo
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- EP3604994B1 EP3604994B1 EP19187493.2A EP19187493A EP3604994B1 EP 3604994 B1 EP3604994 B1 EP 3604994B1 EP 19187493 A EP19187493 A EP 19187493A EP 3604994 B1 EP3604994 B1 EP 3604994B1
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 title claims description 80
- 229910052786 argon Inorganic materials 0.000 title claims description 40
- 238000000034 method Methods 0.000 title claims description 9
- 238000004821 distillation Methods 0.000 title claims description 7
- 238000003860 storage Methods 0.000 claims description 94
- 239000007788 liquid Substances 0.000 claims description 75
- 238000000926 separation method Methods 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000006735 deficit Effects 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 208000031968 Cadaver Diseases 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04763—Start-up or control of the process; Details of the apparatus used
- F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
- F25J3/04793—Rectification, e.g. columns; Reboiler-condenser
- F25J3/048—Argon recovery
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- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—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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- 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
- F25J3/04072—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 argon or argon enriched stream
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- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
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- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
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- F25J3/04812—Different modes, i.e. "runs" of operation
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Definitions
- the present invention relates to a process and to an apparatus for producing argon by cryogenic distillation of a gas from air.
- Air separation units comprising an argon separation column generally have multiple operating points and a certain operating range.
- the problem to be solved is to find a solution making it possible to keep the L / V ratios constant during changes of rate of the argon column so as to be able to increase the rate of change of rate, while maintaining efficiencies close to the nominal case.
- the invention consists in installing intermediate capacities at the outlet of the distributors which are filled with the excess liquid during the drop in load and used during the rise in load because without these capacities, the column would be in deficit of liquid and therefore of reflux .
- the notable advantage of this invention makes it possible to modify the load of the production of argon on the rise as well as on the descent as quickly as the productions of oxygen and nitrogen and to achieve expected speeds of up to 5. % / min or possibly more depending on the size of the device and the volumes to be involved.
- JPH11270965 describes a method and an apparatus for carrying out this method according to the preambles of claims 1 and 5 respectively.
- the Figure 1 shows an apparatus for producing argon by cryogenic distillation according to the invention.
- the apparatus comprises a system of columns for separating the cooled and purified air consisting of a double column comprising a medium pressure column and a low pressure column superimposed and thermally connected together.
- the low pressure column produces a gas enriched in argon ORG comprising at least 10 mol%; argon.
- ORG gas is sent to the bottom of an argon K separation column.
- the K argon separation column comprises eight layers of mass and heat transfer elements, which are structured packings 1, 2, 3, 4, 5, 6, 7, 8, (the layers also being called sections ), but the number of coats may be higher or lower depending on the purity required.
- the column also includes an overhead condenser C which receives oxygen enriched liquid from the column system, more specifically from the bottom of the medium pressure column. The liquid vaporizes there and the LRV formed vapor is sent to the column system.
- the ENT tank liquid from column K is pressurized by a pump P10 and sent to the column system through a valve V1.
- Condenser C receives an oxygen-enriched liquid from a medium pressure column of a double air separation column, forming part of the cooling system. columns. This oxygen-enriched liquid called rich liquid vaporizes at least partially in the condenser C to form an LRV gas.
- the liquid argon produced is returned in part to column K by valve V3 and is partially extracted by valve V2 as product ARG, when column K is in operation.
- a structure S formed by at least two stacked storages is a structure S formed by at least two stacked storages.
- six storages S1, S2, S3, S4, S5, S6 are stacked, so that the tank of an upper storage is the ceiling of the lower storage.
- the storages can nevertheless be independent of each other in order to be able to separate them and use them in another device.
- This structure is arranged parallel to the column and is supported by support means M, independent of the column K, fixed to the ground T.
- liquid is withdrawn at at least one intermediate level from column K and sent to at least one of the storages S1, S2, S3, S4, S5, S6.
- liquid 9 can be sent from a level below layer 8 and above layer 7 via valve V4 to storage S6 and / or liquid 13 can be sent from a level below layer 7 and above layer 6 through open valve V6 to storage S5 and / or liquid 17 can be sent through open valve V8 from below layer 6 and above layer 5 to storage S4 and / or liquid 21 can be sent through the open valve V10 from below the layer 5 and above layer 4 to storage S3 and / or liquid 25 can be sent through the open valve V12 from below layer 4 and above layer 3 to storage S2 and / or liquid 29 can be sent through the open valve V14 from below layer 3 and above layer 2 to the lower storage S1.
- the drop in load is detected by measuring the flow rate of LRV vaporized liquid sent from condenser C to the column system. If this drops below the first threshold, the sending of liquid to at least one storage is triggered and stops when the required level in the storage is reached.
- a second step if the column load is above a second threshold, greater than the first threshold, liquid is withdrawn from storage S6 and sent through valve V5 to an intermediate level between layers 7 and 6 and / or liquid is withdrawn from storage S5 and sent through valve V7 to an intermediate level between layers 6 and 5 and / or liquid is withdrawn from storage S4 and sent through valve V9 to an intermediate level between layers 5 and 4 and / or liquid is withdrawn from storage S3 and sent by valve V11 to an intermediate level between layers 4 and 3 and / or liquid is withdrawn from storage S2 and sent by valve V13 to an intermediate level between the layers 3 and 2 and / or liquid is withdrawn from storage S1 and sent through valve V15 to an intermediate level between layers 2 and 1.
- a reduced capacity could possibly be added at the top of the column to compensate for the liquid reflux in deficit during the drop in charge due to the excess liquid stored in the condenser C relative to the gas charge.
- storages S1, S2, S3, S4, S5, S6 will be filled when the load drops by section number N by a level control whose setpoint will be a ramp according to the flow rate of vaporized liquid LRV and a time delay.
- These same storages will be emptied into the lower section N-1 by a level control whose setpoint will be a ramp according to the flow rate of vaporized liquid LRV and a time delay.
- the storage vessel will be located at a level so that the liquid sent from column K to storage does not need to be pressurized to reach storage. Likewise, the storage liquid flows naturally to column K.
- the storages S1 to S6 are placed in a dedicated cold box containing no distillation column.
- the bottom liquid pump P10 of the argon separation column K can be placed directly below the lowest storage S1.
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Description
La présente invention est relative à un procédé et à un appareil de production d'argon par distillation cryogénique d'un gaz de l'air.The present invention relates to a process and to an apparatus for producing argon by cryogenic distillation of a gas from air.
Les unités de séparation d'air comprenant une colonne de séparation d'argon ont généralement plusieurs points de fonctionnement et une certaine plage de fonctionnement.Air separation units comprising an argon separation column generally have multiple operating points and a certain operating range.
Il est courant de passer d'un point de fonctionnement à un autre à des vitesses d'environ 0,5%/min sans ajout d'équipements supplémentaires. Le problème à résoudre est de trouver une solution permettant de conserver les rapports L/V constants pendant les changements de marche de la colonne argon de façon à pouvoir augmenter la vitesse de changement de marche, tout en maintenant des rendements proches du cas nominal.It is common to switch from one operating point to another at speeds of around 0.5% / min without adding additional equipment. The problem to be solved is to find a solution making it possible to keep the L / V ratios constant during changes of rate of the argon column so as to be able to increase the rate of change of rate, while maintaining efficiencies close to the nominal case.
L'invention consiste à installer des capacités intermédiaires à la sortie des distributeurs qui sont remplies par le liquide excédentaire pendant la baisse de charge et utilisées lors de la remontée en charge car sans ces capacités, la colonne serait en déficit de liquide et donc de reflux.The invention consists in installing intermediate capacities at the outlet of the distributors which are filled with the excess liquid during the drop in load and used during the rise in load because without these capacities, the column would be in deficit of liquid and therefore of reflux .
L'avantage notable de cette invention permet de modifier la charge de la production d'argon à la montée comme à la descente aussi vite que les productions d'oxygène et d'azote et d'atteindre des vitesses escomptées pouvant aller jusqu'à 5 %/min ou éventuellement au-delà en fonction de la taille de l'appareil et des volumes à mettre en jeu.The notable advantage of this invention makes it possible to modify the load of the production of argon on the rise as well as on the descent as quickly as the productions of oxygen and nitrogen and to achieve expected speeds of up to 5. % / min or possibly more depending on the size of the device and the volumes to be involved.
Il est connu de « Start-up storage means for off-spec argon in an air separation unit », Research Disclosures, mai 2000, de stocker un liquide provenant d'une colonne de séparation d'air dans un stockage lors de l'arrêt de la colonne et de le renvoyer à la colonne au redémarrage.It is known from “Start-up storage means for off-spec argon in an air separation unit”, Research Disclosures, May 2000, to store a liquid coming from an air separation column in a storage during shutdown. of the column and send it back to the column on restart.
JPH11270965 décrit un procédé et un appareil de mise en œuvre de ce procédé selon les préambules des revendications 1 et 5 respectivement.JPH11270965 describes a method and an apparatus for carrying out this method according to the preambles of
Selon un objet de cette invention, il est prévu un procédé selon la revendication 1.According to an object of this invention, there is provided a method according to
De préférence :
- aucun élément permettant l'échange de masse et de chaleur n'est disposé entre le deuxième et troisième niveaux.
- des débits d'au moins trois niveaux intermédiaires différents sont stockés chacun dans un stockage respectif lors de la première marche et aucun liquide n'est envoyé du stockage à la colonne et lors de la deuxième marche, un liquide est envoyé de chacun des au moins trois stockages à un niveau de la colonne inférieur à celui auquel le liquide était soutiré de la colonne.
- la colonne de séparation d'argon comprend un condenseur de tête alimenté en liquide par un liquide provenant du système de colonne, le liquide vaporisé dans le condenseur de tête étant renvoyé au système de colonnes selon les deux marches, et dans lequel on détecte si le seuil de charge de la colonne est dépassé en mesurant le débit de liquide vaporisé envoyé vers le système de colonnes.
- no element allowing the exchange of mass and heat is arranged between the second and third levels.
- flow rates of at least three different intermediate levels are each stored in a respective storage during the first run and no liquid is sent from the storage to the column and during the second run liquid is sent from each of the at least three storages at a column level lower than that at which the liquid was withdrawn from the column.
- the argon separation column comprises an overhead condenser supplied with liquid by a liquid coming from the column system, the liquid vaporized in the overhead condenser being returned to the column system according to the two steps, and in which it is detected whether the The column load threshold is exceeded by measuring the flow rate of vaporized liquid sent to the column system.
Selon un autre objet de l'invention, il est prévu un appareil selon la revendication 5.
De préférence :
- les au moins deux stockages sont constitué par deux réservoirs dans une virole commune, de préférence ne contenant que des stockages, le fond d'un stockage constituant de préférence le plafond du stockage inférieur.
- le plafond d'un stockage inférieur constitue la cuve d'un stockage immédiatement au-dessus du stockage inférieur
- l'appareil comprend des moyens de soutien pour les au moins deux stockages reliés directement au sol.
- l'appareil ne comprend aucun moyen de pressurisation du liquide à envoyer du niveau intermédiaire de la colonne vers le stockage et aucun moyen de pressurisation du liquide à envoyer du stockage vers la colonne, l'élévation du stockage étant choisie en fonction du point de soutirage et du point de renvoi du liquide.
- les au moins deux stockages sont reliés l'une à l'autre pour former une structure posée sur le sol.
- les au moins deux, de préférence au moins quatre, stockages forment un corps allongé dont la longueur est égale à au moins la moitié de la longueur de la colonne de séparation d'argon.
- au moins un des stockages et au moins une conduite, voire les deux, reliée(s) au stockage, sont disposés de sorte que le liquide passe de la colonne au stockage et/ou vice versa, sans utiliser une pompe.
- l'appareil ne comprend pas de pompe pour transporter de liquide de la colonne aux stockages et/ou des stockages à la colonne.
- les stockages sont disposés dans une boîte froide dédiée.
- les stockages sont disposés dans une boîte froide avec la colonne de séparation d'argon.
- la pompe de liquide de cuve de la colonne de séparation d'argon est disposée directement en dessous du stockage le plus bas.
Preferably:
- the at least two storages consist of two reservoirs in a common shell, preferably containing only storages, the bottom of a repository preferably constituting the ceiling of the lower storage.
- the ceiling of a lower storage constitutes the vessel of a storage immediately above the lower storage
- the apparatus comprises support means for the at least two storages connected directly to the ground.
- the apparatus does not include any means for pressurizing the liquid to be sent from the intermediate level of the column to the storage and no means for pressurizing the liquid to be sent from the storage to the column, the storage elevation being chosen as a function of the draw-off point and the point of return of the liquid.
- the at least two storages are connected to one another to form a structure placed on the ground.
- the at least two, preferably at least four, storages form an elongate body the length of which is at least half the length of the argon separation column.
- at least one of the storages and at least one pipe, or even both, connected to the storage, are arranged so that the liquid passes from the column to the storage and / or vice versa, without using a pump.
- the apparatus does not include a pump for transporting liquid from the column to the storages and / or from the storages to the column.
- the storages are placed in a dedicated cold box.
- the storages are placed in a cold box with the argon separation column.
- the bottom liquid pump of the argon separation column is placed directly below the lowest storage.
L'invention sera décrite en plus de détail en se référant à la figure.The invention will be described in more detail with reference to the figure.
La
L'appareil comprend un système de colonnes pour séparer l'air refroidi et épuré constitué par une double colonne comprenant une colonne moyenne pression et une colonne basse pression superposées et thermiquement reliées entre elles. La colonne basse pression produit un gaz enrichi en argon ORG comprenant au moins 10% mol ; d'argon. Le gaz ORG est envoyé en cuve d'une colonne de séparation d'argon K.The apparatus comprises a system of columns for separating the cooled and purified air consisting of a double column comprising a medium pressure column and a low pressure column superimposed and thermally connected together. The low pressure column produces a gas enriched in argon ORG comprising at least 10 mol%; argon. ORG gas is sent to the bottom of an argon K separation column.
La colonne de séparation d'argon K comprend huit couches d'éléments de transfert de masse et de chaleur, qui sont des garnissages structurés 1, 2, 3, 4, 5, 6, 7, 8, (les couches étant appelés aussi tronçons), mais le nombre de couches peut être supérieur ou inférieur en fonction de la pureté requise. La colonne comprend également un condenseur de tête C qui reçoit du liquide enrichi en oxygène du système de colonnes, plus spécifiquement de la cuve de la colonne moyenne pression. Le liquide s'y vaporise et la vapeur formée LRV est envoyée au système de colonnes.The K argon separation column comprises eight layers of mass and heat transfer elements, which are structured
Le liquide de cuve ORL de la colonne K est pressurisé par une pompe P10 et envoyé au système de colonnes à travers une vanne V1.The ENT tank liquid from column K is pressurized by a pump P10 and sent to the column system through a valve V1.
De l'argon gazeux en tête de la colonne K se condense dans le condenseur C. Le condenseur C reçoit un liquide enrichi en oxygène provenant d'une colonne moyenne pression d'une double colonne de séparation d'air, faisant partie du système de colonnes. Ce liquide enrichi en oxygène appelé liquide riche se vaporise au moins partiellement dans le condenseur C pour former un gaz LRV.Argon gas at the top of column K condenses in condenser C. Condenser C receives an oxygen-enriched liquid from a medium pressure column of a double air separation column, forming part of the cooling system. columns. This oxygen-enriched liquid called rich liquid vaporizes at least partially in the condenser C to form an LRV gas.
L'argon liquide produit est renvoyé en partie à la colonne K par la vanne V3 et est extrait en partie par la vanne V2 comme produit ARG, quand la colonne K est en fonctionnement.The liquid argon produced is returned in part to column K by valve V3 and is partially extracted by valve V2 as product ARG, when column K is in operation.
A côté de la colonne se trouve une structure S constituée par au moins deux stockages empilés. Dans la figure, six stockages S1, S2, S3, S4, S5, S6 sont empilés, de sorte que la cuve d'un stockage supérieur est le plafond du stockage inférieur.Next to the column is a structure S formed by at least two stacked storages. In the figure, six storages S1, S2, S3, S4, S5, S6 are stacked, so that the tank of an upper storage is the ceiling of the lower storage.
Les stockages peuvent néanmoins être indépendants les uns des autres afin de pouvoir les séparer et les utiliser dans un autre appareil.The storages can nevertheless be independent of each other in order to be able to separate them and use them in another device.
Mais il est préférable de construire une tour avec une virole unique contenant une multiplicité de compartiments, formés par des partitions P. Chacun compartiment sert comme stockage de liquide.But it is better to build a tower with a single ferrule containing a multiplicity of compartments, formed by partitions P. Each compartment serves as a liquid storage.
Cette structure est disposée parallèlement de la colonne et est soutenue par des moyens de soutien M, indépendant de la colonne K, fixés au sol T.This structure is arranged parallel to the column and is supported by support means M, independent of the column K, fixed to the ground T.
Quand la charge de la colonne K est au-dessus d'un premier seuil et en dessous d'un deuxième seuil, aucun débit de liquide n'est envoyé de la colonne K vers les stockages S1, S2, S3, S4, S5, S6 et aucun débit de liquide n'est envoyé des stockages vers la colonne K.When the charge of column K is above a first threshold and below a second threshold, no liquid flow is sent from column K to the storages S1, S2, S3, S4, S5, S6 and no liquid flow is sent from the storages to the K column.
Dans une première marche, quand la charge de la colonne est en dessous d'un premier seuil, du liquide est soutiré à au moins un niveau intermédiaire de la colonne K et envoyé vers au moins un des stockages S1, S2, S3, S4, S5, S6. Par exemple du liquide 9 peut être envoyé d'un niveau en dessous de la couche 8 et au-dessus de la couche 7 par la vanne V4 vers le stockage S6 et/ou du liquide 13 peut être envoyé d'un niveau en dessous de la couche 7 et au-dessus de la couche 6 par la vanne ouverte V6 vers le stockage S5 et/ou du liquide 17 peut être envoyé par la vanne ouverte V8 d'en dessous de la couche 6 et au-dessus de la couche 5 vers le stockage S4 et/ou du liquide 21 peut être envoyé par la vanne ouverte V10 d'en dessous de la couche 5 et au-dessus de la couche 4 vers le stockage S3 et/ou du liquide 25 peut être envoyé par la vanne ouverte V12 d'en dessous de la couche 4 et au-dessus de la couche 3 vers le stockage S2 et/ou du liquide 29 peut être envoyé par la vanne ouverte V14 d'en dessous de la couche 3 et au-dessus de la couche 2 vers le stockage inférieur S1.In a first step, when the column charge is below a first threshold, liquid is withdrawn at at least one intermediate level from column K and sent to at least one of the storages S1, S2, S3, S4, S5, S6. For example, liquid 9 can be sent from a level below
Evidemment le nombre de stockages peut être inférieur ou supérieur à 6.Obviously the number of storages can be lower or higher than 6.
La baisse de la charge est détectée en mesurant le débit de liquide vaporisé LRV envoyé du condenseur C vers le système de colonnes. Si celui-ci passe en dessous du premier seuil, l'envoi de liquide vers au moins un stockage est déclenché et s'arrête quand le niveau requis dans le stockage est atteint.The drop in load is detected by measuring the flow rate of LRV vaporized liquid sent from condenser C to the column system. If this drops below the first threshold, the sending of liquid to at least one storage is triggered and stops when the required level in the storage is reached.
Dans une deuxième marche, si la charge de la colonne est au-dessus d'un deuxième seuil, supérieur au premier seuil, du liquide est soutiré du stockage S6 et envoyé par la vanne V5 vers un niveau intermédiaire entre les couches 7 et 6 et/ou du liquide est soutiré du stockage S5 et envoyé par la vanne V7 vers un niveau intermédiaire entre les couches 6 et 5 et/ou du liquide est soutiré du stockage S4 et envoyé par la vanne V9 vers un niveau intermédiaire entre les couches 5 et 4 et/ou du liquide est soutiré du stockage S3 et envoyé par la vanne V11 vers un niveau intermédiaire entre les couches 4 et 3 et/ou du liquide est soutiré du stockage S2 et envoyé par la vanne V13 vers un niveau intermédiaire entre les couches 3 et 2 et/ou du liquide est soutiré du stockage S1 et envoyé par la vanne V15 vers un niveau intermédiaire entre les couches 2 et 1.In a second step, if the column load is above a second threshold, greater than the first threshold, liquid is withdrawn from storage S6 and sent through valve V5 to an intermediate level between
Lors de la première marche, aucun liquide n'est soutiré d'un stockage vers la colonne K et lors de la deuxième marche, aucun liquide n'est envoyé de la colonne vers un stockage.During the first run, no liquid is withdrawn from storage to column K and during the second run, no liquid is sent from the column to storage.
Quand la charge est réduite, lors de la première marche, la surface d'échange du condenseur C devant être réduite, de l'argon liquide est stockée dans le condenseur C lui-même à cet effet. Ce liquide sera déstocké lors de la remontée en charge et réalisera la fonction de capacité tampon.When the load is reduced, during the first operation, the exchange surface of the condenser C having to be reduced, liquid argon is stored in the condenser C itself for this purpose. This liquid will be removed from storage when the load is raised and will perform the buffer capacity function.
Une capacité réduite pourra éventuellement être ajoutée en haut de la colonne pour compenser le reflux liquide en déficit pendant la baisse de charge du fait de l'excédent de liquide stocké dans le condenseur C par rapport à la charge gaz.A reduced capacity could possibly be added at the top of the column to compensate for the liquid reflux in deficit during the drop in charge due to the excess liquid stored in the condenser C relative to the gas charge.
Pour les autres tronçons, des stockages S1, S2, S3, S4, S5, S6 seront remplis lors de la baisse de charge par le tronçon numéro N par un contrôle de niveau dont la consigne sera une rampe en fonction du débit de liquide vaporisé LRV et d'une temporisation. Ces mêmes stockages seront vidés dans le tronçon inférieur N-1 par un contrôle de niveau dont la consigne sera une rampe en fonction du débit de liquide vaporisé LRV et d'une temporisation.For the other sections, storages S1, S2, S3, S4, S5, S6 will be filled when the load drops by section number N by a level control whose setpoint will be a ramp according to the flow rate of vaporized liquid LRV and a time delay. These same storages will be emptied into the lower section N-1 by a level control whose setpoint will be a ramp according to the flow rate of vaporized liquid LRV and a time delay.
La cuve du stockage sera située à un niveau de sorte que le liquide envoyé de la colonne K vers le stockage n'ait pas besoin d'être pressurisé pour arriver au stockage. De même le liquide du stockage s'écoule naturellement vers la colonne K.The storage vessel will be located at a level so that the liquid sent from column K to storage does not need to be pressurized to reach storage. Likewise, the storage liquid flows naturally to column K.
La disposition de ces stockages incluant également une ligne d'équilibrage de pression sera faite en les ajustant les uns au-dessus des autres pour que leur élévation permette un bon fonctionnement hydraulique et ne nécessite pas un supportage exceptionnel au niveau de la colonne. Le soutien de la structure peut être fait par une tuyauterie verticale avec des fonds intermédiaires reposant au sol T.The arrangement of these storages also including a pressure balancing line will be made by adjusting them one above the other so that their elevation allows good hydraulic operation and does not require exceptional support at the column level. The support of the structure can be done by vertical piping with intermediate funds resting on the ground T.
Les stockages S1 à S6 sont disposés dans une boîte froide dédiée ne contenant pas de colonne de distillation.The storages S1 to S6 are placed in a dedicated cold box containing no distillation column.
Mais ils peuvent être disposés dans une boîte froide avec la colonne de séparation d'argon ou une autre colonne de distillation.But they can be arranged in a cold box with the argon separation column or other distillation column.
La pompe P10 de liquide de cuve de la colonne de séparation d'argon K peut être disposée directement en dessous du stockage le plus bas S1.The bottom liquid pump P10 of the argon separation column K can be placed directly below the lowest storage S1.
Claims (15)
- Method for producing argon by cryogenic distillation wherein an argon-enriched gas (ORG) produced by air separation in a system of columns is sent to an argon separation column (K), an argon-rich flow (ARG) is drawn off at the top of the column and an oxygen-rich liquid (ORL) is drawn off at the tank of the column and sent back to the system of columns wherein:i) during a first step, if, preferably only if, the load of the column (K) is below a first threshold, liquid is drawn off from the column at a first intermediate level of the column and stored in a first storage facility (S1, S2, S3, S4, S5, S6), with no liquid being sent from the first storage facility to the column and liquid is drawn off from the column (K) at a third intermediate level of the column and stored in a second storage facility (S1, S2, S3, S4, S5), with no liquid being sent from the second storage facility to the column,ii) during a second step, if, preferably only if, the load of the column is above a second threshold, greater than the first threshold, no liquid is sent from the column to the first storage facility, liquid is sent from the first storage facility to the column at a second intermediate level of the column, the second level being located below the first level, no liquid is sent from the column to the second storage facility, liquid is sent from the second storage facility to the column at a fourth intermediate level of the column, the fourth level being located below the third level and the third level not being located above the second level characterised in that the second level is separated from the first level by at least one layer of elements (2, 3, 4, 5, 6, 7) allowing for the exchange of mass and heat and the fourth level is separated from the third level by at least one layer of elements (2, 3, 4, 5, 6) allowing for the exchange of mass and heat.
- Method according to claim 1, wherein no element allowing for the exchange of mass and heat is disposed between the second and third levels.
- Method according to one of claims 1 and 2, wherein flows of at least three different intermediate levels are each stored in a respective storage facility (S1, S2, S3, S4, S5, S6) during the first step and no liquid is sent from the storage facility to the column and during the second step, a liquid is sent from each one of the at least three storage facilities to a level of the column (K) less than that at which the liquid was drawn off from the column.
- Method according to one of the preceding claims, wherein the argon separation column comprises a top condenser (C) supplied with liquid by a liquid coming from the system of columns, the liquid vaporised in the top condenser (LRV) being sent back to the system of columns according to the two steps, and wherein it is detected if the load threshold of the column is exceeded by measuring the flow of vaporised liquid sent to the system of columns.
- Device for producing argon by cryogenic distillation of air in a system of columns, for the implementation of a method according to one of the preceding claims, comprising an argon separation column (K), means for sending a gas containing argon and oxygen (ORG) to the column, means for extracting an argon-enriched fluid (ARG) at the top of the column, means for extracting an oxygen-enriched liquid (ORL) at the tank of the column and at least one first and one second storage facilities (S1, S2, S3, S4, S5, S6), disposed one above the other, the first storage facility being connected to a first intermediate level of the argon separation column by a duct and to a second intermediate level of the argon separation column below the first level by a duct, the second storage facility being connected to a third intermediate level of the argon separation column by a duct and to a fourth intermediate level of the argon separation column below the third level by a duct, the third level not being located above the second level characterised in that the device comprises at least one layer of elements allowing for the exchange of mass and heat (2, 3, 4, 5, 6, 7) and separating the second level of the column from the first level and at least one layer of elements allowing for the exchange of mass and heat (2, 3, 4, 5, 6) and separating the third level of the column from the fourth level, and characterised in that the two storage facilities are contiguous.
- Device according to claim 5, wherein the at least two storage facilities (S1, S2, S3, S4, S5, S6) are formed by two reservoirs in a common ferrule, more preferably containing only storage facilities, the bottom (P) of a storage facility more preferably constituting the ceiling of the lower storage facility.
- Device according to one of claims 5 or 6 comprising means of support (M) for the at least two storage facilities (S1, S2, S3, S4, S5, S6) connected directly to the ground (T).
- Device according to one of claims 5 to 7 comprising no means of pressurising the liquid to be sent from the intermediate level of the column (K) to the storage facility (S1, S2, S3, S4, S5, S6) and no means of pressurising the liquid to be sent from the storage facility to the column, the elevation of the storage facility being chosen according to the drawing off point and the point for sending the liquid back.
- Device according to one of claims 5 to 8, wherein the at least two storage facilities (S1, S2, S3, S4, S5, S6) are connected to one another to form a structure (S) placed on the ground.
- Device according to one of claims 5 to 9, wherein the at least two, more preferably at least four, storage facilities (S1, S2, S3, S4, S5, S6) form an elongated body (S) of which the length is equal to at least half of the length of the argon separation column.
- Device according to one of claims 5 to 10, wherein at least one of the storage facilities (S1, S2, S3, S4, S5, S6) and at least one duct, or even both, connected to the storage facility, are disposed such that the liquid passes from the column (K) to the storage facility and/or vice versa, without using a pump.
- Device according to one of claims 5 to 11 not comprising any pump to transport liquid from the column to the storage facilities and/or from the storage facilities to the column.
- Device according to one of claims 5 to 12, wherein the storage facilities (S1, S2, S3, S4, S5, S6) are disposed in a dedicated cold box.
- Device according to one of claims 5 to 12, wherein the storage facilities (S1, S2, S3, S4, S5, S6) are arranged in a cold box with the argon separation column (K).
- Device according to one of claims 5 to 14 comprising a pump (P10) comprising tank liquid of the argon separation column (K), the pump being disposed directly below the lowest storage facility (S1).
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FR1857220A FR3084736B1 (en) | 2018-08-01 | 2018-08-01 | METHOD AND APPARATUS FOR PRODUCTION OF ARGON BY CRYOGENIC AIR DISTILLATION |
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FR3110686B1 (en) | 2020-05-19 | 2023-06-09 | Air Liquide | A method of supplying oxygen and/or nitrogen as well as argon to a geographical area |
FR3123421B1 (en) | 2021-05-27 | 2023-07-14 | Air Liquide | Argon purification system by cryogenic distillation |
FR3137747B1 (en) * | 2022-07-05 | 2024-07-12 | Air Liquide | Process for regulating an air separation device by cryogenic distillation |
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US3878689A (en) * | 1970-07-27 | 1975-04-22 | Carl A Grenci | Liquefaction of natural gas by liquid nitrogen in a dual-compartmented dewar |
US4695303A (en) * | 1986-07-08 | 1987-09-22 | Mcdermott International, Inc. | Method for recovery of natural gas liquids |
FR2716816B1 (en) * | 1994-03-02 | 1996-05-03 | Air Liquide | Method for restarting an auxiliary argon / oxygen separation column by distillation, and corresponding installation. |
JPH1054656A (en) * | 1996-08-12 | 1998-02-24 | Nippon Sanso Kk | Air liquefying and separating device and method thereof |
JP3609009B2 (en) * | 1997-01-14 | 2005-01-12 | エア・ウォーター株式会社 | Air separation device |
JP4104726B2 (en) * | 1998-03-20 | 2008-06-18 | 大陽日酸株式会社 | Operation method of air liquefaction separator |
DE10158330A1 (en) * | 2001-11-28 | 2003-06-18 | Linde Ag | Method and device for producing a high-purity cryogenic liquid product from a less pure cryogenic feed liquid |
FR2903483B1 (en) * | 2006-07-04 | 2014-07-04 | Air Liquide | METHOD AND APPARATUS FOR AIR SEPARATION BY CRYOGENIC DISTILLATION |
EP2591301B1 (en) * | 2010-07-05 | 2020-09-02 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Apparatus and process for separating air by cryogenic distillation |
EP3175191A1 (en) * | 2014-07-31 | 2017-06-07 | Linde Aktiengesellschaft | Production of an air product in an air separation plant with cold storage unit |
-
2018
- 2018-08-01 FR FR1857220A patent/FR3084736B1/en not_active Expired - Fee Related
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2019
- 2019-07-22 EP EP19187493.2A patent/EP3604994B1/en active Active
- 2019-07-31 CN CN201910698523.0A patent/CN110793271B/en active Active
- 2019-07-31 US US16/527,467 patent/US11441840B2/en active Active
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EP3604994A1 (en) | 2020-02-05 |
FR3084736A1 (en) | 2020-02-07 |
CN110793271A (en) | 2020-02-14 |
US11441840B2 (en) | 2022-09-13 |
FR3084736B1 (en) | 2022-04-15 |
CN110793271B (en) | 2022-07-22 |
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