EP0904518B1 - Procede de mise en marche d'une installation de separation de l'air a basse temperature et installation de separation de l'air a basse temperature - Google Patents

Procede de mise en marche d'une installation de separation de l'air a basse temperature et installation de separation de l'air a basse temperature Download PDF

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Publication number
EP0904518B1
EP0904518B1 EP97921813A EP97921813A EP0904518B1 EP 0904518 B1 EP0904518 B1 EP 0904518B1 EP 97921813 A EP97921813 A EP 97921813A EP 97921813 A EP97921813 A EP 97921813A EP 0904518 B1 EP0904518 B1 EP 0904518B1
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Prior art keywords
liquid
distillation column
column
process according
installation
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German (de)
English (en)
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EP0904518A1 (fr
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Georg Demski
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Linde GmbH
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Linde GmbH
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04472—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages
    • F25J3/04478—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for controlling purposes, e.g. start-up or back-up procedures
    • 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
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
    • 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
    • F25J3/04812—Different modes, i.e. "runs" of operation
    • F25J3/04824—Stopping of the process, e.g. defrosting or deriming; Back-up procedures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • 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
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • 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
    • 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
    • F25J2250/42—One fluid being nitrogen
    • 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
    • F25J2280/00—Control of the process or apparatus
    • F25J2280/10—Control for or during start-up and cooling down of the installation
    • 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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/62—Details of storing a fluid in a tank

Definitions

  • the invention relates to a method for starting up a plant for the low-temperature separation of a gas mixture, in particular air, which has at least one distillation column in which a more volatile fraction, in particular nitrogen, is produced and at least one source for cryogenic liquid, the method at least temporarily cryogenic liquid from this source is introduced into an upper region of the distillation column, this introduction of liquid starting at a time t 0 .
  • the process was developed as part of the production of nitrogen from air; however, the invention is also applicable to any other method for separation by distillation of a gas mixture at a temperature below the ambient temperature applicable. It mainly relates to restarting a system a business interruption, especially in the event that the pillar is still open low temperature, but is also due to the start of a warm system applicable.
  • the invention has for its object a particularly economical working Method and a corresponding device to specify a particular enable favorable start-up, in particular high purity in the more volatile product when restarting after business interruptions.
  • This object is achieved in that no air or essentially no air is introduced into the distillation column between the time t 0 and a later time t 1 > t 0 .
  • the air feed is opened, preferably carefully, that is, the amount of air fed in is regulated and slowly increased from zero to the normal value. It preferably rises strictly monotonously until it has reached this normal value.
  • the time t 1 can either be predetermined or determined by the fact that the liquid falling into the column has reached a certain lower column section, for example the sump, or that the liquid level in the sump of the column has reached a certain minimum height. In practice, it is sufficient if a reasonable time interval t 1 - t 0 (for example 3 to 10 minutes) is determined when the column is started up and this is used for later cases when the system is started up.
  • the Mass transfer elements in the column (floors, packing and / or ordered Packs) at least partially wetted and, if necessary, liquid distributors replenished.
  • the air is later admitted to the distillation column rectification in the entire column or in most of it immediately insert, and the more volatile fraction, which is obtained in the upper part of the column has the desired product purity.
  • the pressure in the distillation column is, for example, 3 to 15 bar, preferably 6 up to 9 bar.
  • the distillation column is designed for a nominal product quantity of the more volatile fraction. In the process, between the time t 0 and a later time t 1 > t 0 cryogenic liquid can be introduced into the distillation column in an amount which is less than the nominal product amount of the more volatile fraction.
  • the amount of liquid initially fed in is, for example, less than the nominal product amount. It can also be greater than or equal to the nominal product quantity, if this accelerates the wetting of the mass transfer elements.
  • the amount of liquid added preferably remains constant in the time interval from t 0 to t 1 and is subsequently reduced, for example to zero.
  • the column is therefore driven in particular even after the start of the air supply (time t 1 ) with total or almost total return, i.e. at least 90 mol% of the rising steam is condensed at the top of the column and at most 10 mol%, preferably at most 5 mol %, most preferably a maximum of 1 mol% of the vapor rising in the column as a volatile fraction.
  • the corresponding product line remains completely closed until time t 2 (for example 4 to 15 minutes after the start time t 0 ).
  • the time t 2 can be, for example, only about 3 to 20 minutes after the start time t 0 .
  • the amount of air supplied reaches its normal value; the removal of the more volatile fraction is increased to the nominal product quantity up to a time t 4 ⁇ t 3 .
  • the times t 3 and t 4 are, for example, 12 to 25 minutes after the start time t 0 .
  • the invention equally relates to single methods Distillation column and those with other columns. Often contains the volatile fraction from the top of the distillation column Very low boiling point contaminants. in the case of nitrogen, this can Helium, neon and / or hydrogen. That is why it is particularly high Purity requirements favorable if the more volatile fraction in the stationary Operation is initiated in a pure column, the pure column being a high purity product is removed.
  • the removal point of the high-purity product is preferably located below the introduction of the more volatile fraction. In such a process prevents the start-up method according to the invention in particular that the clean column due to less volatile components (in the case of nitrogen extraction: oxygen) is contaminated.
  • the upper region of the distillation column and the lower region of the are preferably Pure column via a condenser-evaporator in a heat-exchanging connection.
  • Such a double column is known per se from DE 4432137 A1.
  • the source of cryogenic liquid can be formed by a reservoir that is formed by is filled outside the system.
  • This reservoir can, for example, as Liquid tank to be formed, from which also in excess of the nominal product quantity additional requirements or in the event of an interruption to the plant Liquid is removed and counteracted in an external evaporator, for example Ambient air is evaporated.
  • the source of cryogenic liquid can be through a reservoir be formed, which is filled by a fluid obtained within the system. The amount of liquid consumed during start-up is then in the stationary Operation again generated and introduced into the reservoir.
  • the system has a pure column, it is particularly advantageous if that Reservoir is filled with a liquid from the pure column. This is in particular the bottom liquid of the pure column is suitable.
  • the bottom of the pure column can itself as Act as reservoir for the cryogenic liquid.
  • the reservoir is preferably through the evaporation space of the condenser-evaporator educated.
  • the condenser-evaporator can be in the bottom of the Pure column (see DE 4432137 A1) or be arranged outside the pure column. in the In the first case, the evaporation space is identical to the bottom of the column, in the second In this case, it is formed by its own container.
  • a liquid fraction from an external Source is introduced into the distillation column, as is known from DE 2417766 A is known.
  • all or substantially all Cold process requirements are covered by liquid feed, none of which Process streams is relaxed while working and the system does not generate any refrigeration Has relaxation machine (for example turbine).
  • you can this liquid fraction and the cryogenic liquid that is used when starting. be identical, i.e. come from the same reservoir.
  • One of these two reservoirs, or preferably a third can be used for emergency supply or for additional production through external evaporation be used.
  • External evaporation can, for example, by indirect Heat exchange with atmospheric air or water or with any other known method.
  • the regulation of the amount introduced to compensate for cold losses liquid fraction preferably takes place depending on the liquid level in the Bottom of the distillation column. In principle, the regulation is also dependent on other liquid levels in the system possible.
  • the method has at least a first and a second source of cryogenic liquid, cryogenic liquid from both sources being introduced into the distillation column at least at times, and the liquid from the second source from at least one theoretical base below the liquid the first source is fed.
  • the feeding of both liquids preferably begins approximately simultaneously, namely at time t 0 .
  • the simultaneous feeding of liquid at several points enables wetting of the mass transfer elements to be carried out more quickly; the air supply (time t 1 ) can start earlier, the starting process is further shortened.
  • This effect can be further enhanced by feeding liquid at three or more points on the column, for example in a packed column at each liquid distributor.
  • the different feeds can be carried out, for example, at the top and at two thirds of the column height (from below), at the top of the column and at half the column height or - in the case of three sources - at the top, at two thirds and at a third of the column height .
  • the feed quantities depend in each case on the number of theoretical plates located between the feed point and the feed point underneath or the column bottom;
  • the main criterion is the adequate wetting of the mass transfer elements that can be achieved as quickly as possible.
  • Wetting of the mass transfer elements can also be achieved if the two liquids applied in different places are the same Have composition; preferably have the liquids from the two However, sources differ in composition, particularly close to the equilibrium concentration in the distillation column in stationary operation liquid flowing down at the respective feed point. In this way can make a certain adjustment to the Concentration curve during the stationary operation of the distillation column be made. The starting process is further shortened.
  • the invention also relates to a plant for the low-temperature separation of air according to claims 15 to 17.
  • Atmospheric air is drawn in at 1, in the air compressor 2 to a pressure of over 3 bar, preferably 6.5 to 9.5 bar compressed and in one or more Cleaning stages 3, 4 of water, carbon dioxide and possibly of Free carbon monoxide and / or hydrogen by indirect heat exchange 5 cooled and via line 6 into a distillation column 7 operated as a pressure column fed.
  • the top gas 8 from the distillation column 7 is partly (9) in Condenser-evaporator 11 at least partially liquefied, the condensate 12 is given as a return to the distillation column 7 and not condensed Shares, mainly helium and neon, with a purge stream via line 13 subtracted from.
  • the gas in line 13 can for example be discarded or with a residual gas fraction are mixed. It is preferably continuously fed into the Pure column 14 described below passed by line 13 includes a valve and after this valve opens into line 10 downstream of the Dross valve there (in the drawing not shown).
  • the part of the top gas which is not introduced into the condenser-evaporator 11 Distillation column is removed as volatile fraction 10 and over a Throttle valve fed into a pure column (helium-neon discharge column) 14.
  • the Feed point is at the middle level of the pure column 14, in the lower Area of high purity nitrogen.
  • This high purity product is preferably in Vapor form taken directly above the bottom of the pure column (line 15).
  • the pure product nitrogen is used in 5 against air to be broken down to about Ambient temperature warmed up and drawn off via the product line 20.
  • the bottom of the helium-neon discharge column 14 is through the condenser-evaporator 11 heated, which also serves to form a return for the pressure column 7.
  • the head capacitor 16 of the helium-neon discharge column becomes more relaxed Bottom liquid 17 operated from the pressure column 7.
  • the against the condensing Head fraction of the helium-neon discharge column evaporated fraction is piped 19 deducted.
  • the residual gas 19 can, optionally together with an or several flushing streams, warmed against air to be separated and then for example as a regeneration gas in one or more purification stages 3, 4 be used. Parts not liquefied in the top condenser 16, in particular Helium and neon, possibly also hydrogen, leave the plant with the Purge stream 18.
  • a liquid fraction 24 for example Liquid nitrogen of ordinary purity
  • This liquid is supplied from outside the system and stored in a liquid tank.
  • This liquid tank is preferably independent of an emergency supply tank, its content to cover additional product needs or for emergency care in the Can be vaporized externally in the event of a business interruption.
  • the feed 24 preferably occurs at an intermediate point, that is, at least one theoretical floor below the head of the column.
  • the amount of imported here Liquid is, for example, a liquid level controller in the sump Distillation column 7 or depending on the liquid level in one of the Capacitors 11 or 16 set.
  • the product line 20 can alternatively or additionally externally via line 21 evaporated product fed from the emergency supply tank, not shown become.
  • To supply liquid from the emergency supply tank to start up the system can use a line from the emergency supply tank to the upper area of the Distillation column 7 may be provided.
  • the emergency supply tank can be removed from the system and / or filled from an external source. In the latter case it is Emergency supply system independent of the operation of the columns.
  • the two columns 7 and 14 can be arranged inside a vacuum insulation be, which also encloses a liquid tank, preferably the one in which the liquid fraction is stored, which is fed at 24. Details of this Arrangement can be found in EP 538857 A1.
  • the valve 23 When restarting after the interruption of operation, the valve 23 is partially or completely opened at the start time t 0 , while the air feed line 6 remains closed.
  • the liquid from the bottom of the pure column 14 flows via line 22 into the top of the distillation column 7.
  • the mass transfer elements trays, packing and / or ordered packing
  • the liquid distributors in the column 7 are gradually wetted or filled.
  • the line 6 is opened and air flows into the distillation column 7 in a quantity which slowly increases to the stationary value.
  • the gas introduced is partially or preferably completely condensed in the condenser-evaporator 11, as a result of which additional return liquid is produced.
  • the valve 23 is slowly closed, so that the amount of liquid flowing over 22 slowly decreases until it has dropped to zero at a time t 2 .
  • the liquid supply above 22 may remain open at most as long as the pressure at the top of the distillation column 7 is lower than the pressure in the bottom of the pure column 14 plus the hydrostatic pressure of the liquid. Otherwise, overhead gas would be pressed from the distillation column 7 into the pure column 14 via line 22 and contaminate it with oxygen. This can be ensured either by monitoring the corresponding pressure difference or by specifying a fixed point in time t 2 based on previously determined empirical values.
  • the entire process of restarting is preferably carried out automatically.

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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

L'installation comprend au moins une colonne de distillation (7) dans laquelle une fraction très volatile (10), notamment de l'azote, est générée, ainsi qu'au moins une source de liquide réfrigéré. Lorsque l'installation est mise en marche après une interruption de service, le liquide (22) réfrigéré au moins temporairement est conduit à partir d'un certain moment t0 de cette source à une zone supérieure de la colonne de distillation (7). Entre le moment de démarrage t0 et un moment ultérieur t1⊃t0, aucun air (6) n'est introduit dans la colonne de distillation (7).

Claims (17)

  1. Procédé de mise en marche d'une installation pour la séparation à basse température d'un mélange gazeux, en particulier d'air, qui présente au moins une colonne de distillation (7), dans laquelle est produite une fraction aisément volatile (10), en particulier de l'azote, et au moins une source pour liquide à basse température, dans lequel, dans le procédé, au moins momentanément, un liquide (22) à basse température issu de cette source est introduit dans une zone supérieure de la colonne de distillation (7), cette introduction du liquide commençant au moment t0, caractérisé en ce que, entre le moment t0 et un moment ultérieur t1 > t0, il n'est pas ou sensiblement pas envoyé de mélange gazeux (6) dans la colonne de distillation (7).
  2. Procédé selon la revendication 1, caractérisé en ce que la colonne de distillation (7) est dimensionnée pour une quantité de produit nominale de la fraction aisément volatile (10) et en ce que, entre le moment t0 et un moment ultérieur t1 > t0, il est introduit dans la colonne de distillation un liquide à basse température (22) en une quantité qui est plus faible que la quantité de produit nominale de la fraction aisément volatile (10).
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce qu'entre le moment t0 et un moment encore plus éloigné t2 > t1, on ne prélève pas ou sensiblement pas de fraction aisément volatile (10) de la colonne de distillation (7).
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que la fraction aisément volatile (10) est envoyée dans une colonne d'épuration (14) d'où est prélevé un produit très pur (15).
  5. Procédé selon la revendication 4, caractérisé en ce que la zone supérieure de la colonne de distillation (7) et la zone inférieure de la colonne d'épuration (14) sont en liaison d'échange de chaleur par le biais d'un condenseur-évaporateur (11).
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que la source pour liquide à basse température est formée par un réservoir qui est rempli à partir de l'extérieur de l'installation.
  7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que la source pour liquide à basse température est formée par un réservoir qui est rempli par un fluide obtenu à l'intérieur de l'installation.
  8. Procédé selon la revendication 7 ou selon l'une quelconque des revendications 4 ou 5, caractérisé en ce que le réservoir est rempli d'un liquide venant de la colonne d'épuration (14).
  9. Procédé selon les revendications 5 et 7, caractérisé en ce que le réservoir est formé par l'espace d'évaporation du condensateur-évaporateur (11).
  10. Procédé selon l'une quelconque des revendications 1 à 9, caractérisé en ce que, au cours de l'exploitation stationnaire de l'installation pour compenser les pertes de froid, une fraction liquide (24) est envoyée d'une source externe dans la colonne de distillation (7).
  11. Procédé selon la revendication 10, caractérisé en ce que la quantité de la fraction liquide (24) alimentée dans la colonne de distillation (7) est réglée en fonction du niveau du liquide dans le bas de la colonne de distillation (7).
  12. Procédé selon l'une quelconque des revendications 1 à 11, caractérisé par au moins une première source et une seconde source pour liquide à basse température, dans lequel le liquide à basse température, au moins momentanément, provenant des deux sources est introduit simultanément dans la colonne de distillation (7), et le liquide (24) provenant de la seconde source est alimenté à au moins un fond théorique en dessous du liquide (22) provenant de la première source.
  13. Procédé selon la revendication 12, caractérisé en ce que les liquides provenant des deux sources ont une composition différente.
  14. Procédé selon la revendication 13, caractérisé en ce que les compositions des deux liquides se situent tout près des concentrations à l'équilibre du liquide qui descend dans la colonne de distillation (7) en exploitation stationnaire, au point d'alimentation respectif.
  15. Installation pour la séparation à basse température d'un mélange gazeux, en particulier d'air, comprenant au moins une colonne de distillation (7) pour produire une fraction aisément volatile (10), en particulier de l'azote, une conduite d'alimentation (1, 6) qui conduit dans la zone inférieure de la colonne de distillation (7), une conduite de liquide (22) qui conduit dans la zone supérieure de la colonne de distillation (7), et des moyens de commande qui se présentent sous une forme telle que, au début de la mise en marche de l'installation, la conduite de liquide (22) soit ouverte et la conduite d'alimentation (1, 6) soit totalement ou sensiblement totalement fermée.
  16. Installation selon la revendication 15 comprenant une conduite de gaz (10) qui conduit de la zone supérieure de la colonne de distillation (7) dans une colonne d'épuration (14) et présente une soupape d'étranglement, une conduite de produit pur (15) qui est reliée à la zone inférieure de la colonne d'épuration (14), et une conduite de liquide (22) bloquable (23) par le biais de laquelle on peut établir une communication d'écoulement entre la zone inférieure de la colonne d'épuration (14) et la zone supérieure de la première colonne de distillation (7).
  17. Installation selon la revendication 15 comprenant une conduite de gaz (10) qui conduit de la zone supérieure de la première colonne de distillation (7) dans une colonne d'épuration (14) et présente une soupape d'étranglement, une conduite de produit pur (15) qui est reliée à la zone inférieure de la colonne d'épuration (14), un condenseur-évaporateur (11), dont l'espace d'évaporation est en communication d'écoulement côté liquide et côté gaz avec la zone inférieure de la colonne d'épuration (14), et une conduite de liquide (22) bloquable (23) par le biais de laquelle on peut établir une communication d'écoulement entre l'espace d'évaporation du condenseur-évaporateur (11) et la zone supérieure de la première colonne de distillation (7).
EP97921813A 1996-04-30 1997-04-28 Procede de mise en marche d'une installation de separation de l'air a basse temperature et installation de separation de l'air a basse temperature Expired - Lifetime EP0904518B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19617377 1996-04-30
DE19617377A DE19617377A1 (de) 1996-04-30 1996-04-30 Verfahren zum Wiederanfahren einer Anlage zur Tieftemperaturzerlegung von Luft und Anlage zur Tieftemperaturzerlegung von Luft
PCT/EP1997/002188 WO1997041400A1 (fr) 1996-04-30 1997-04-28 Procede de mise en marche d'une installation de decomposition de l'air a basse temperature et installation de decomposition de l'air a basse temperature

Publications (2)

Publication Number Publication Date
EP0904518A1 EP0904518A1 (fr) 1999-03-31
EP0904518B1 true EP0904518B1 (fr) 2001-12-19

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EP97921813A Expired - Lifetime EP0904518B1 (fr) 1996-04-30 1997-04-28 Procede de mise en marche d'une installation de separation de l'air a basse temperature et installation de separation de l'air a basse temperature

Country Status (5)

Country Link
EP (1) EP0904518B1 (fr)
DE (2) DE19617377A1 (fr)
ES (1) ES2170951T3 (fr)
PT (1) PT904518E (fr)
WO (1) WO1997041400A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2774752B1 (fr) * 1998-02-06 2000-06-16 Air Liquide Installation de distillation d'air et boite froide correspondante

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1463075A (en) * 1973-04-13 1977-02-02 Cryoplants Ltd Air separation
DE3732363A1 (de) * 1987-09-25 1989-04-06 Linde Ag Verfahren und vorrichtung zum wiederanfahren einer gaszerlegungsanlage
FR2660741A1 (fr) * 1990-04-10 1991-10-11 Air Liquide Procede et installation de production d'azote gazeux, et systeme de fourniture d'azote correspondant.

Also Published As

Publication number Publication date
WO1997041400A1 (fr) 1997-11-06
DE19617377A1 (de) 1997-11-06
DE59705898D1 (de) 2002-01-31
PT904518E (pt) 2002-05-31
ES2170951T3 (es) 2002-08-16
EP0904518A1 (fr) 1999-03-31

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