EP1175587B1 - Method and installation for producing argon by means of cryogenic distillation - Google Patents

Method and installation for producing argon by means of cryogenic distillation Download PDF

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Publication number
EP1175587B1
EP1175587B1 EP00915223A EP00915223A EP1175587B1 EP 1175587 B1 EP1175587 B1 EP 1175587B1 EP 00915223 A EP00915223 A EP 00915223A EP 00915223 A EP00915223 A EP 00915223A EP 1175587 B1 EP1175587 B1 EP 1175587B1
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Prior art keywords
column
argon
gas
sending
rich
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German (de)
French (fr)
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EP1175587A1 (en
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Bernard Saulnier
Jean-Pierre Gourbier
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Air Liquide SA
LAir Liquide SA a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude
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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
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04951—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network
    • F25J3/04963—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network and inter-connecting equipment within or downstream of the fractionation unit(s)
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04703—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 being arranged in more than one vessel
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/02—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams using a pump in general or hydrostatic pressure increase
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/923—Inert gas
    • Y10S62/924—Argon

Definitions

  • the present invention relates to a method and an installation of argon production by cryogenic distillation in accordance to the preambles of claims 1 and 6 respectively.
  • Such a method and such an installation are known to EP-A-0 786 633.
  • a flow enriched with argon is withdrawn from the column low pressure of a double column of air separation and sent down of a first column in order to lower as much as necessary the quantity of oxygen contained in the oxygen produced.
  • EP-A-0786633, J06-109361, EP-A-0669509, EP-A-0669508 and EP-A-558620 to send it in a second column called denitration column including a section of exhaustion intended to eliminate the nitrogen of the argon produced in tank, a section rectification method for removing argon from the residual nitrogen withdrawn at the head, a tank reboiler and a condenser at the head.
  • US-A-5133790 describes a system in which one installs sufficiently distillation trays in the low pressure column, above the point taking the feed from the first column, to lower the nitrogen content in such proportions that the argon produced has a 'commercial' argon, usually 1 ppm.
  • the denitration column can be deleted. It is then useful to have some trays of distillation above the draw point of the argon-rich fluid from the first column and provide a purge at the top of the first column so to eliminate a part of the introduced nitrogen.
  • the content of argon nitrogen produced can be about three times lower than that of feeding the column.
  • the disadvantage of this method is that it is essential to control the operation of the low pressure column so that never the nitrogen content at the point of withdrawal of the feed intended for the first column exceeds the allowable quantity, unless the column contains enough trays to dispose at the nominal point of a sufficient margin vis-à-vis this limit.
  • the flow sent at the head of the second column may be a gas or a liquid.
  • the caloric gas is a fraction of the gas enriched in argon that feeds the first column.
  • the first column is in two sections, one section being fed by the gas enriched in argon and the other having the head condenser.
  • the first column is fed from the column low pressure of a double column.
  • a top gas of the second column is sent either at the head of the first column is the condenser head of the first column.
  • the argon-rich fluid sent to the top of the second column can to be a gas or a liquid.
  • it comprises means for sending a part of the argon-enriched gas to the reboiler as a caloric gas.
  • the first column is constructed in two sections.
  • the installation comprises means for sending a head gas of the second column either at the head of the first column is at the head condenser of the first column.
  • an air flow 100 is sent to a double column conventional air separation comprising a medium pressure column 200 thermally connected to a low pressure column 300.
  • An argon-enriched flow rate containing 7% argon, a few ppm of nitrogen and oxygen taken from the low pressure column 300 is sent in the tank of the first section 7 of the first column 1.
  • a liquid flow 6 is returned from the vat from the first column column to the low column pressure.
  • the first section 7 containing structured packings of the type Cross corrugated is used to separate the flow enriched in argon.
  • a top gas 9 of the first section is sent to the tank of the second section 11 and a tank liquid of the second section is sent to the head of the first section 7 to serve as reflux.
  • the top gas of the first column (mixture column) is condensed at least partially in a head condenser 15 'against the rich liquid from the tank of the medium pressure column or other fluid.
  • a purge 13 of non-condensed argon rich gas can be removed. Like her can not be rich in nitrogen for temperature reasons, argon loss will be proportional to the amount of nitrogen introduced in the first section 7.
  • a argon-rich liquid flow containing argon and at most 1000ppm of nitrogen and 1000ppm of oxygen is withdrawn some trays theoretical below the top condenser, for example, three trays theoretical below.
  • the liquid 15 is sent to the top of the second column 2 in which is enriched in argon.
  • the nitrogen-enriched overhead gas 17 is returned at the second section 11 of the first column.
  • Part of the argon-enriched gas is used to heat the reboiler 19 of column 2 and the flow thus condensed is mixed with the liquid of tank 6 of the first section and returned to the low pressure column 300. All fluid hot enough for its condensation or cooling to produce at a higher temperature than the column liquid of column 2 can used for reboiling.
  • a liquid 21 or a gas rich in argon 23 is withdrawn in the tank of the second column 2.
  • the argon-enriched gas may come at least partially from a device other than the double column 200, 300. For example it can be transported by truck or pipeline from a more distant aircraft.
  • columns 200,300 and 7 are identical to those of Figure 1. By cons instead of returning the leading gas from the second column 2 directly to the top of column 11 it is better to send this flow directly to the head condenser 15 'above this column 11.
  • the overhead gas from column 11 is withdrawn from it, mixed with the overhead gas from column 2 and sent to the capacity 18 which contains the condenser 15 '.
  • the gas mixture condenses to less partially in this condenser before being returned in form liquid at the top of the column 11.
  • This system avoids the complexity of creating a supplementary feeding in the first column 11 without affecting significantly argon production.
  • This way of implementing the invention is particularly beneficial when the argon condenser and its capacity are separated from the first column.
  • the process does not use catalysis to purify argon.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The invention relates to a method for separating gas that is enriched with argon, whereby the gas is purified in oxygen in a first column (1) and a flow (15) that is collected from the head of the first column is dispatched to an exhaustion column (2). The product (21) is drawn out in a vessel pertaining to said exhaustion column.

Description

La présente invention concerne un procédé et une installation de production d'argon par distillation cryogénique conformément aux préambules des revendications 1 et 6 respectivement. Un tel procédé et une telle installation sont connus du document EP-A-0 786 633.The present invention relates to a method and an installation of argon production by cryogenic distillation in accordance to the preambles of claims 1 and 6 respectively. Such a method and such an installation are known to EP-A-0 786 633.

Habituellement, un débit enrichi en argon est soutiré de la colonne basse pression d'une double colonne de séparation d'air et envoyé en bas d'une première colonne afin d'abaisser autant que nécessaire la quantité d'oxygène contenu dans l'oxygène produit.Usually, a flow enriched with argon is withdrawn from the column low pressure of a double column of air separation and sent down of a first column in order to lower as much as necessary the quantity of oxygen contained in the oxygen produced.

Dans le procédé classique l'argon produit par cette première colonne est soutiré en tête et contient l'essentiel de l'azote introduit dans l'alimentation.In the conventional process the argon produced by this first column is taken off the top and contains most of the nitrogen introduced into the diet.

Il est alors d'usage comme on voit dans EP-A-0786633, J06-109361, EP-A-0669509, EP-A-0669508 et EP-A-558620 de l'envoyer dans une deuxième colonne dite colonne de déazotation comportant un tronçon d'épuisement destiné à éliminer l'azote de l'argon produit en cuve, un tronçon de rectification destiné à éliminer l'argon de l'azote résiduaire soutiré en tête, un rebouilleur de cuve et un condenseur en tête.It is then customary as can be seen in EP-A-0786633, J06-109361, EP-A-0669509, EP-A-0669508 and EP-A-558620 to send it in a second column called denitration column including a section of exhaustion intended to eliminate the nitrogen of the argon produced in tank, a section rectification method for removing argon from the residual nitrogen withdrawn at the head, a tank reboiler and a condenser at the head.

US-A- 5133790 décrit un système dans lequel on installe suffisamment de plateaux de distillation dans la colonne basse pression, au-dessus du point de prélèvement de l'alimentation de la première colonne, pour abaisser la teneur en azote dans des proportions telles que l'argon produit a une teneur en argon 'commerciale', généralement 1 ppm. Ainsi la colonne de déazotation peut être supprimée. Il est alors utile de disposer quelques plateaux de distillation au-dessus du point de soutirage du fluide riche en argon de la première colonne et de prévoir une purge en tête de la première colonne afin d'éliminer une partie de l'azote introduit. Dans ces conditions, la teneur en azote de l'argon produit peut être environ trois fois inférieure à celle de l'alimentation de la colonne.US-A-5133790 describes a system in which one installs sufficiently distillation trays in the low pressure column, above the point taking the feed from the first column, to lower the nitrogen content in such proportions that the argon produced has a 'commercial' argon, usually 1 ppm. Thus the denitration column can be deleted. It is then useful to have some trays of distillation above the draw point of the argon-rich fluid from the first column and provide a purge at the top of the first column so to eliminate a part of the introduced nitrogen. In these circumstances, the content of argon nitrogen produced can be about three times lower than that of feeding the column.

L'inconvénient de ce procédé est qu'il est indispensable de contrôler le fonctionnement de la colonne basse pression de façon à ce que jamais la teneur en azote au point de soutirage de l'alimentation destinée à la première colonne n'excède la quantité admissible, à moins que la colonne ne comporte assez de plateaux pour disposer au point nominal d'une marge suffisante vis-à-vis de cette limite.The disadvantage of this method is that it is essential to control the operation of the low pressure column so that never the nitrogen content at the point of withdrawal of the feed intended for the first column exceeds the allowable quantity, unless the column contains enough trays to dispose at the nominal point of a sufficient margin vis-à-vis this limit.

US-A-4977746 et US-A-4824453 divulguent un procédé de production d'argon et d'oxygène ultra pur dans lequel un liquide prélevé à un niveau intermédiaire de la colonne de production d'argon alimente la tête d'une colonne d'épuisement à la cuve de laquelle se forme l'oxygène ultra pur.

  • Selon un objet de l'invention, il est prévu un procédé de séparation selon la revendication 1.
US-A-4977746 and US-A-4824453 disclose a method for producing argon and ultra pure oxygen in which a liquid taken at an intermediate level of the argon production column feeds the head of a column of exhaustion in the tank from which ultra pure oxygen is formed.
  • According to one object of the invention, there is provided a separation method according to claim 1.

Le débit envoyé en tête de la deuxième colonne peut être un gaz ou un liquide.The flow sent at the head of the second column may be a gas or a liquid.

De préférence, le gaz calorigène est une fraction du gaz enrichi en argon qui alimente la première colonne.Preferably, the caloric gas is a fraction of the gas enriched in argon that feeds the first column.

Dans certains cas, la première colonne est en deux sections, une section étant alimentée par le gaz enrichi en argon et l'autre ayant le condenseur de tête.In some cases, the first column is in two sections, one section being fed by the gas enriched in argon and the other having the head condenser.

Normalement, la première colonne est alimentée à partir de la colonne basse pression d'une double colonne.Normally, the first column is fed from the column low pressure of a double column.

De préférence, un gaz de tête de la deuxième colonne est envoyé soit en tête de la première colonne soit au condenseur de tête de la première colonne.Preferably, a top gas of the second column is sent either at the head of the first column is the condenser head of the first column.

Selon un autre objet de l'invention, il est prévu une installation selon la revendication 6.According to another object of the invention, an installation according to the claim 6.

Le fluide riche en argon envoyé en tête de la deuxième colonne peut être un gaz ou un liquide.The argon-rich fluid sent to the top of the second column can to be a gas or a liquid.

De préférence elle comprend des moyens pour envoyer une partie du gaz enrichi en argon au rebouilleur de cuve comme gaz calorigène.Preferably it comprises means for sending a part of the argon-enriched gas to the reboiler as a caloric gas.

Eventuellement, la première colonne est construite en deux sections.Optionally, the first column is constructed in two sections.

De préférence, l'installation comprend des moyens pour envoyer un gaz de tête de la deuxième colonne soit à la tête de la première colonne soit au condenseur de tête de la première colonne.Preferably, the installation comprises means for sending a head gas of the second column either at the head of the first column is at the head condenser of the first column.

L'invention sera maintenant décrite en plus de détail en se référant aux figures 1 et 2 qui représentent des installations selon l'invention. The invention will now be described in more detail with reference to the Figures 1 and 2 which show facilities according to the invention.

Dans la figure 1, un débit d'air 100 est envoyé à une double colonne classique de séparation d'air comprenant une colonne moyenne pression 200 reliée thermiquement à une colonne basse pression 300. In FIG. 1, an air flow 100 is sent to a double column conventional air separation comprising a medium pressure column 200 thermally connected to a low pressure column 300.

Une partie des détails de cette colonne a été omise pour faciliter la présentation de l'invention.Some of the details in this column have been omitted to facilitate the presentation of the invention.

Un débit 5 enrichi en argon contenant 7% d'argon, quelques ppm d'azote et de l'oxygène prélevé dans la colonne basse pression 300 est envoyé en cuve du premier tronçon 7 de la première colonne 1.Un débit liquide 6 est renvoyé de la cuve de la colonne première colonne à la colonne basse pression.An argon-enriched flow rate containing 7% argon, a few ppm of nitrogen and oxygen taken from the low pressure column 300 is sent in the tank of the first section 7 of the first column 1. A liquid flow 6 is returned from the vat from the first column column to the low column pressure.

Le premier tronçon 7 contenant des garnissages structurés du type ondulé croisé sert à séparer le débit enrichi en argon.The first section 7 containing structured packings of the type Cross corrugated is used to separate the flow enriched in argon.

Un gaz de tête 9 du premier tronçon est envoyé en cuve du deuxième tronçon 11 et un liquide de cuve du deuxième tronçon est envoyé en tête du premier tronçon 7 pour servir de reflux.A top gas 9 of the first section is sent to the tank of the second section 11 and a tank liquid of the second section is sent to the head of the first section 7 to serve as reflux.

Le gaz de tête de la première colonne (colonne de mixture) est condensé au moins partiellement dans un condenseur de tête 15' contre du liquide riche de la cuve de la colonne moyenne pression ou un autre fluide. Une purge 13 de gaz riche en argon non-condensé peut être enlevée. Comme elle ne peut être riche en azote pour des raisons de température, la perte en argon sera proportionnelle à la quantité d'azote introduite dans le premier tronçon 7.The top gas of the first column (mixture column) is condensed at least partially in a head condenser 15 'against the rich liquid from the tank of the medium pressure column or other fluid. A purge 13 of non-condensed argon rich gas can be removed. Like her can not be rich in nitrogen for temperature reasons, argon loss will be proportional to the amount of nitrogen introduced in the first section 7.

Néanmoins, celle-ci pourra être cinq à dix fois supérieure à la teneur admissible dans le cas de US-A-5133790, pour une perte inférieure à 5%.Nevertheless, it may be five to ten times higher than the in the case of US-A-5133790, for a loss of less than 5%.

Un débit liquide riche en argon 15 contenant de l'argon et au plus 1000ppm d'azote et 1000ppm d'oxygène est soutiré quelques plateaux théoriques en dessous du condenseur de tête, par exemple, trois plateaux théorique en dessous.A argon-rich liquid flow containing argon and at most 1000ppm of nitrogen and 1000ppm of oxygen is withdrawn some trays theoretical below the top condenser, for example, three trays theoretical below.

Le liquide 15 est envoyé en tête de la deuxième colonne 2 dans laquelle elle s'enrichit en argon. Le gaz de tête 17 enrichi en azote est renvoyé au deuxième tronçon 11 de la première colonne. De préférence, il n'y a aucun moyen de séparation ni rebouilleur au-dessus du point d'introduction du liquide 15 et aucun condenseur de tête de la deuxième colonne 2.The liquid 15 is sent to the top of the second column 2 in which is enriched in argon. The nitrogen-enriched overhead gas 17 is returned at the second section 11 of the first column. Preferably, there is no separation medium or reboiler above the point of introduction of the liquid 15 and no overhead condenser of the second column 2.

Une partie du gaz enrichi en argon sert à chauffer le rebouilleur de cuve 19 de la colonne 2 et le débit ainsi condensé est mélangé avec le liquide de cuve 6 du premier tronçon et renvoyé à la colonne basse pression 300. Tout fluide suffisamment chaud pour que sa condensation ou son refroidissement se produise à une température supérieure au liquide de cuve de la colonne 2 peut servir au rebouillage.Part of the argon-enriched gas is used to heat the reboiler 19 of column 2 and the flow thus condensed is mixed with the liquid of tank 6 of the first section and returned to the low pressure column 300. All fluid hot enough for its condensation or cooling to produce at a higher temperature than the column liquid of column 2 can used for reboiling.

Un liquide 21 ou un gaz riche en argon 23 est soutiré en cuve de la deuxième colonne 2.A liquid 21 or a gas rich in argon 23 is withdrawn in the tank of the second column 2.

Le gaz enrichi en argon peut provenir au moins partiellement d'un appareil autre que la double colonne 200, 300. Par exemple il peut être transporté par camion ou par gazoduc depuis un appareil plus lointain.The argon-enriched gas may come at least partially from a device other than the double column 200, 300. For example it can be transported by truck or pipeline from a more distant aircraft.

Dans la deuxième figure, les colonnes 200,300 et 7 sont identiques à celles de la figure 1. Par contre au lieu de renvoyer le gaz de tête de la deuxième colonne 2 directement à la tête de la colonne 11, il est préférable d'envoyer ce débit directement au condenseur de tête 15' au-dessus de cette colonne 11. Dans le cas de la Figure 2, le gaz de tête de la colonne 11 est soutiré de celle-ci, mélangé avec le gaz de tête de la colonne 2 et envoyé à la capacité 18 qui contient le condenseur 15'. Le mélange de gaz se condense au moins partiellement dans ce condenseur avant d'être renvoyé sous forme liquide à la tête de la colonne 11.In the second figure, columns 200,300 and 7 are identical to those of Figure 1. By cons instead of returning the leading gas from the second column 2 directly to the top of column 11 it is better to send this flow directly to the head condenser 15 'above this column 11. In the case of Figure 2, the overhead gas from column 11 is withdrawn from it, mixed with the overhead gas from column 2 and sent to the capacity 18 which contains the condenser 15 '. The gas mixture condenses to less partially in this condenser before being returned in form liquid at the top of the column 11.

Ce système permet d'éviter la complexité consistant à créer une alimentation supplémentaire dans la première colonne 11, sans affecter de façon significative la production d'argon. Cette façon de mettre en oeuvre l'invention est particulièrement profitable quand le condenseur d'argon et sa capacité sont séparés de la première colonne.This system avoids the complexity of creating a supplementary feeding in the first column 11 without affecting significantly argon production. This way of implementing the invention is particularly beneficial when the argon condenser and its capacity are separated from the first column.

De préférence, le procédé n'utilise pas de catalyse pour épurer l'argon.Preferably, the process does not use catalysis to purify argon.

Claims (10)

  1. Process for separating an argon-enriched gas by cryogenic distillation, comprising the following steps:
    the step of sending an oxygen-containing, argon-enriched gas stream (5) to a first column (1);
    the step of separating the gas by distillation in the first column into an oxygen-enriched liquid and an argon-enriched gas;
    the step of at least partially condensing the argon-rich gas in an overhead condenser (15) of the first column in order to form reflux;
    the step of removing another argon-rich stream (15) containing at most 1000 ppm oxygen from the first column and of sending it to a second column (2);
    the step of warming the bottom of the second column by means of a warming gas; and
    the step of withdrawing, as final product, an argon-rich fluid (21, 23) from the lower portion of the second column, characterized in that the other argon-rich stream contains at most 1000 ppm nitrogen and is sent to the top of the second column.
  2. Process according to Claim 1, in which the warming gas is a fraction of the argon-enriched gas (5) which feeds the first column.
  3. Process according to Claim 1 or 2, in which the first column (1) is in two sections, one section (7) being fed with the argon-enriched gas and the other (11) having the overhead condenser.
  4. Process according to Claim 1, 2 or 3, in which the first column is fed from the low-pressure column (300) of a double column.
  5. Process according to one of the preceding claims, in which an overhead gas (17) of the second column (2) is sent either to the top of the first column or to the overhead condenser (15') of the first column.
  6. Plant for separating an argon-enriched gas by cryogenic distillation, comprising:
    a first column (1) having an overhead condenser (15');
    a second column (2) having a bottom reboiler (19);
    means for sending an argon-enriched gas to a first level of the first column;
    means for withdrawing an argon-rich fluid at a second level of the first column;
    means for sending the argon-rich fluid to the second column;
    means for sending a warming gas (5) to the bottom reboiler;
    means for withdrawing an argon-rich final product (21, 23) from the bottom of the second column,
    and in which, between the first and second levels, there are at least 100 theoretical trays characterized in that, it comprises means for sending the argon-rich fluid to the top of the second column.
  7. Plant according to Claim 6 or 7, comprising means for sending a portion of the argon-enriched gas (5) to the bottom reboiler (19) as warming gas.
  8. Plant according to Claim 6 or 7, in which the first column is constructed in two sections.
  9. Plant according to one of Claims 6 to 8, comprising means for sending an overhead gas (17) from the second column (2) either to the top of the first column (1) or to the overhead condenser (15') of the first column.
  10. Plant according to one of Claims 6 to 9, in which the second column (2) has no overhead condenser.
EP00915223A 1999-03-29 2000-03-27 Method and installation for producing argon by means of cryogenic distillation Expired - Lifetime EP1175587B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9903870 1999-03-29
FR9903870A FR2791762B1 (en) 1999-03-29 1999-03-29 PROCESS AND PLANT FOR THE PRODUCTION OF ARGON BY CRYOGENIC DISTILLATION
PCT/FR2000/000763 WO2000058675A1 (en) 1999-03-29 2000-03-27 Method and installation for producing argon by means of cryogenic distillation

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EP1175587B1 true EP1175587B1 (en) 2005-02-16

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EP2026024A1 (en) 2007-07-30 2009-02-18 Linde Aktiengesellschaft Process and device for producing argon by cryogenic separation of air
DE102007035619A1 (en) 2007-07-30 2009-02-05 Linde Ag Process and apparatus for recovering argon by cryogenic separation of air
US20100024478A1 (en) * 2008-07-29 2010-02-04 Horst Corduan Process and device for recovering argon by low-temperature separation of air
US8899075B2 (en) 2010-11-18 2014-12-02 Praxair Technology, Inc. Air separation method and apparatus
US10126280B2 (en) 2014-10-17 2018-11-13 The Trustees of Princeton University, Office of Technology and Trademark Licensing Device and method for testing underground argon

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DE821654C (en) * 1950-10-07 1951-11-19 Adolf Messer G M B H Process for the production of pure argon
DE930033C (en) * 1953-04-12 1956-03-08 Adolf Messer G M B H Process for producing argon
US5076823A (en) * 1990-03-20 1991-12-31 Air Products And Chemicals, Inc. Process for cryogenic air separation
US5133790A (en) * 1991-06-24 1992-07-28 Union Carbide Industrial Gases Technology Corporation Cryogenic rectification method for producing refined argon
US5207066A (en) * 1991-10-22 1993-05-04 Bova Vitaly I Method of air separation
CA2142318A1 (en) * 1994-02-24 1995-08-25 Horst Corduan Process and apparatus for recovery of pure argon
US5440884A (en) * 1994-07-14 1995-08-15 Praxair Technology, Inc. Cryogenic air separation system with liquid air stripping
WO1997001068A1 (en) * 1995-06-20 1997-01-09 Nippon Sanso Corporation Method and apparatus for separating argon
GB9605171D0 (en) * 1996-03-12 1996-05-15 Boc Group Plc Air separation
JP2002511136A (en) * 1998-04-21 2002-04-09 レール・リキード・ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード Air rectification process and plant with production of argon
US5970743A (en) * 1998-06-10 1999-10-26 Air Products And Chemicals, Inc. Production of argon from a cryogenic air separation process

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EP1175587A1 (en) 2002-01-30
US6574988B1 (en) 2003-06-10
WO2000058675A1 (en) 2000-10-05
FR2791762A1 (en) 2000-10-06
DE60018176D1 (en) 2005-03-24
DE60018176T2 (en) 2006-03-23
AU3660800A (en) 2000-10-16

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