WO2008084167A2 - Procede et appareil de separation d'un melange gazeux par distillation cryogenique - Google Patents

Procede et appareil de separation d'un melange gazeux par distillation cryogenique Download PDF

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Publication number
WO2008084167A2
WO2008084167A2 PCT/FR2007/052552 FR2007052552W WO2008084167A2 WO 2008084167 A2 WO2008084167 A2 WO 2008084167A2 FR 2007052552 W FR2007052552 W FR 2007052552W WO 2008084167 A2 WO2008084167 A2 WO 2008084167A2
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Prior art keywords
capacity
column
liquid
sent
pressurization
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PCT/FR2007/052552
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English (en)
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WO2008084167A3 (fr
Inventor
Hervé Le Bihan
Jean-Marc Peyron
Original Assignee
L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude
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Application filed by L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude filed Critical L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude
Priority to EP07871966.3A priority Critical patent/EP2104825B1/fr
Priority to US12/520,112 priority patent/US8713964B2/en
Priority to CN2007800474576A priority patent/CN101595356B/zh
Publication of WO2008084167A2 publication Critical patent/WO2008084167A2/fr
Publication of WO2008084167A3 publication Critical patent/WO2008084167A3/fr
Priority to US14/200,049 priority patent/US9546815B2/en

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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
    • F25J3/04812—Different modes, i.e. "runs" of operation
    • F25J3/04836—Variable air feed, i.e. "load" or product demand during specified periods, e.g. during periods with high respectively low power costs
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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
    • F25J3/0204—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 characterised by the feed 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
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    • 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
    • F25J3/0228—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 characterised by the separated product stream
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    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
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    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04163—Hot end purification of the feed air
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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
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • 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
    • F25J3/04763—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
    • F25J3/04775—Air purification and pre-cooling
    • 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
    • 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
    • F25J3/0483—Rapid load change of the air fractionation unit
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • F25J2205/72—Pressurising or depressurising the adsorption 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/40—Processes or apparatus involving steps for recycling of process streams the recycled stream being air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/40—One fluid being air
    • 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
    • F25J2280/02—Control in general, load changes, different modes ("runs"), measurements
    • 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 present invention relates to a method and apparatus for separating a gas mixture by cryogenic distillation, in particular to a method and apparatus for separating air by cryogenic distillation.
  • the two bottles of the gas mixture purifications for a cryogenic separation apparatus operate cyclically between adsorption phases at high pressure and regeneration at low pressure.
  • the transition between regeneration and adsorption therefore requires a pressurization of the bottle with the supply gas of the cold box.
  • This additional flow must be provided by the main air compressor for the air separation units. This therefore requires sizing this compressor for the nominal flow rate increased by this rate of pressurization bottles.
  • the pressurization of the bottles is to the detriment of the supply flow of the cold box without major problem of stability for the columns.
  • the device according to the present invention can compensate for the lack of flow injected to the columns without specification of additional flow on the main air compressor. This allows a reduction in the price of the machine, greater flexibility and better energy optimization of the machine.
  • the system consists of a cryogenic liquid capacity with a bottom tank vaporizer.
  • a capacity is an enclosure containing no tray or lining.
  • a cryogenic liquid is a liquid at a temperature below 200K.
  • an apparatus for the cryogenic distillation of a gaseous mixture comprising a purification apparatus for purifying the gaseous mixture in a multi-bottle system of adsorbent, operating in a cycle comprising a phase of pressurization, a column system, a capacity, means for sending a cryogenic liquid to the capacity only outside a pressurization phase, preferably any pressurization phase, means for sending vaporized liquid of the capacity to a column of the system only during at least part of the period in which one of the bottles is in the pressurization phase, a vaporizer in the capacity to vaporize the contained liquid, means for sending a caloric gas to the vaporizer and means for drawing off liquid of the capacity.
  • cryogenic liquid consists of a part of the liquefied gas mixture and / or the heat-exchange gas is constituted by a part of the gaseous mixture;
  • the apparatus comprises means for sending the liquefied caloric gas into the vaporizer to the capacity;
  • a liquid of the capacity is sent to one (the) column of the column system.
  • a process for the cryogenic distillation of a gaseous mixture in an apparatus according to one of the apparatus claims in which only during at least part of the period in which one of the bottles is in the pressurization phase, a gas is sent from the capacity to a column of the column system and only outside one, preferably, any pressurization period, the liquid capacity is filled.
  • the gaseous mixture is air
  • the column system comprises at least one double column with a medium pressure column and a low pressure column thermally connected to each other and in which during at least a portion of the period in which one of the bottles is in the pressurization phase, air is sent from the capacity to the medium pressure column;
  • a gas of the capacity is sent to a column of the column system only during the period in which one of the bottles is in a pressurization phase;
  • the maximum pressure of the capacity is between 15 and 40 bar, preferably between 20 and 30 bar and / or the minimum pressure is between 4 and 10 bar.
  • the air separation apparatus comprises a conventional double column composed of three columns, a medium pressure column MP and a low pressure column LP, both being thermally connected to each other by a reboiler R1, and an argon column AR.
  • the reflux lines between the two columns are well known in the art and will not be described or illustrated.
  • the apparatus also includes a capacitor 15, a phase separator 17, and a main exchange line 5.
  • the subcoolers have not been illustrated.
  • the apparatus produces a high oxygen flow rate and a nitrogen rich flow rate from the low pressure column, one and / or the other being able to serve as final product in liquid and / or gaseous form.
  • Clean air 1 in a purifying unit A comprising adsorbent bottles was compressed at a pressure slightly higher than that of the medium pressure column MP.
  • Part 5 at the pressure slightly higher than that of the medium pressure column MP cools in the exchange line E01 and is sent in gaseous form to the medium pressure column MP.
  • Part 7 is overpressed in a BAC booster at an intermediate pressure and then supercharged again in a booster D01C driven by the turbine D01.
  • the flow 7 is thus at a high pressure, is cooled and sent to the hot end of the exchange line E01 where it cools partially before being divided into two fractions 11, 16 permanently or even three fractions 4, 11, 16 just before and / or during the filling phase.
  • Fraction 11 is expanded in the turbine D01 to provide the vast majority of the frigories required for the apparatus. Relaxed at the average pressure, the fraction 11 joins the fraction 5 to form the flow 13 which is sent to the medium pressure column MP.
  • Fraction 16 continues cooling in the exchange line E01 to the cold end, possibly supplying frigories for the vaporization of a liquid produced by the double column (not shown). Outside the filling phase of the capacity, all the liquefied air thus formed is sent through the valve V21 to the medium pressure column as flow 21. Obviously the flow 13 can be divided and sent to the two columns.
  • the capacity contains liquefied air at a high pressure (for example 25 bar abs) at its boiling point.
  • a high pressure for example 25 bar abs
  • the circuit 2 is opened by opening the valve V2 to supply the medium pressure column MP with gaseous air to compensate for the reduction in the flow rate. Feeding the columns as part of the flow is required for bottle pressurization.
  • the pressure in the capacity decreases with vaporization of liquid, the necessary heat being provided by the subcooling of all available liquid in the capacity.
  • the pressure of the capacity decreases to the pressure of the medium pressure column MP.
  • the amount of liquid vaporized and supplied to the medium pressure column corresponds to the amount of gas required to pressurize the purification bottle.
  • the remaining liquid is at the boiling point at the pressure of the medium pressure column MP.
  • valves V19, V29 are closed and the capacity
  • a purge circuit 3 ensures the permanent deconcentration of impurities from the capacity through the valve V3 which sends the purge to the rich tank liquid from the medium pressure column MP.
  • the filling of the capacity 15 is carried out, one takes warmer air 16 at the inlet of a turbine D01 at a pressure greater than the final high pressure of the capacity and it is condensed in the capacity 15, thanks to the tank vaporizer R2, the liquid of the capacity being colder than the air at the inlet of the turbine D01. This makes it possible to increase the pressure to 25 bar and to fill the capacity with liquid.
  • the system stops naturally when the temperature of the liquid of the capacity 15 is close to the temperature at the inlet of the turbine D01.
  • a small amount of liquid air (circuit 4) is produced by liquefying air in the vaporizer R2.
  • This liquid is then sent to a phase separator 17 and the liquid is sent via the pipe 29 through the valve V29 at the top of the capacity 15 to complete the level of the capacity, this liquid coming from the vaporizer R2 being colder than the liquid in the capacity.
  • the tank vaporizer R2 will ensure the equilibrium temperature of this liquid.
  • the valve V2 A purge circuit 3 ensures permanent deconcentration of the impurities of the capacity through the valve V3 which sends the purge to the rich tank liquid from the medium pressure column MP. This rich liquid is then vaporized in the head condenser of the AR argon column.
  • This filling phase can be done by filling directly with high-pressure liquid air 16,19 from the cold end of the main heat exchanger E01 as illustrated, or by taking an intermediate point fluid in the main exchanger in order to have the right equilibrium temperature of the final pressure of the capacity, either undercooled (it will then be heated by a tank exchanger as described above).
  • This device can also be applied to the cold distillation separation of mixture boxes having as main components of hydrogen and carbon monoxide. To compensate for reductions in carbon monoxide content during purification reversals, it is possible to destock carbon monoxide flow towards the suction of the carbon monoxide compressor or destock the flow of synthesis gas to stabilize the gas supplies. of the carbon monoxide and methane separation column. As the capacity remains inside the cold box, the risk of spreading liquid carbon monoxide is eliminated.
  • the invention can be applied to any cryogenic cold box preceded by a treatment to stabilize any cold flow fed or produced by the cryogenic columns.

Abstract

Un appareil de distillation cryogénique d un mélange gazeux (1) comprend un appareil d'épuration (A) pour épurer le mélange gazeux dans un système à plusieurs bouteilles d'adsorbant, un système de colonnes (MP,LP,AR), une capacité (15), des moyens pour envoyer un liquide cryogénique (19,V19,29,V29) à la capacité, des moyens pour envoyer du liquide vaporisé (2,V2) de la capacité à une colonne (MP) du système, un vaporiseur (R2) dans la capacité pour vaporiser le liquide contenu, des moyens pour envoyer un gaz calorigène (4) au vaporiseur et des moyens pour soutirer du liquide (3) de la capacité.

Description

Procédé et appareil de séparation d'un mélange gazeux par distillation cryogénique
La présente invention est relative à un procédé et appareil de séparation d'un mélange gazeux par distillation cryogénique, en particulier à un procédé et appareil de séparation d'air par distillation cryogénique.
Les deux bouteilles des épurations du mélange gazeux destiné à un appareil de séparation cryogénique fonctionnent de façon cyclique entre phases adsorption en haute pression et régénération en basse pression. La transition entre régénération et adsorption nécessite donc une pressurisation de la bouteille avec du gaz d'alimentation de la boîte froide. Ce supplément de débit doit être fourni par le compresseur d'air principal pour les unités de séparation d'air. Ceci oblige donc à dimensionner ce compresseur pour le débit nominal augmenté de ce débit de pressurisation des bouteilles. Pour les unités de séparation d'air sans production d'argon, on peut accepter que la pressurisation des bouteilles se fasse au détriment du débit d'alimentation de la boîte froide sans gros problème de stabilité pour les colonnes.
Pour les unités de séparation avec production d'argon, la perturbation de débit est trop sévère pour ne pas spécifier le compresseur sans ce débit additionnel.
Il est connu de compenser la réduction du débit d'air, en régulant les débits de liquide de reflux (US-A-6073463).
Le dispositif selon la présente invention peut compenser le manque de débit injecté vers les colonnes sans spécification de débit additionnel sur le compresseur d'air principal. Ceci permet une diminution du prix de la machine, une plus grande flexibilité et une meilleure optimisation énergétique de la machine.
Le système se compose d'une capacité de liquide cryogénique avec un vaporiseur de fond de cuve.
Une capacité est une enceinte ne contenant aucun plateau ou garnissage.
Un liquide cryogénique est un liquide à une température inférieure à 200K. Selon un objet de l'invention, il est prévu un appareil de distillation cryogénique d'un mélange gazeux comprenant un appareil d'épuration pour épurer le mélange gazeux dans un système à plusieurs bouteilles d'adsorbant, opérant selon un cycle comprenant une phase de pressurisation, un système de colonnes, une capacité, des moyens pour envoyer un liquide cryogénique à la capacité uniquement en dehors d'une phase de pressurisation, de préférence de toute phase de pressurisation, des moyens pour envoyer du liquide vaporisé de la capacité à une colonne du système uniquement pendant au moins une partie de la période dans laquelle l'une des bouteilles est en phase de pressurisation, un vaporiseur dans la capacité pour vaporiser le liquide contenu, des moyens pour envoyer un gaz calorigène au vaporiseur et des moyens pour soutirer du liquide de la capacité.
Selon d'autres aspects de l'invention :
- le liquide cryogénique est constitué par une partie du mélange gazeux liquéfié et/ou le gaz calorigène est constitué par une partie du mélange gazeux ;
- l'appareil comprend des moyens pour envoyer le gaz calorigène liquéfié dans le vaporiseur à la capacité ;
- on envoie un liquide de la capacité à une (la) colonne du système de colonnes. Selon un autre objet de l'invention, il est prévu un procédé de distillation cryogénique d'un mélange gazeux dans un appareil selon une des revendications d'appareil dans lequel uniquement pendant au moins une partie de la période dans laquelle l'une des bouteilles est en phase de pressurisation, on envoie un gaz de la capacité à une colonne du système de colonnes et uniquement en dehors d'une, de préférence, de toute, période de pressurisation, on remplit la capacité de liquide.
Selon d'autres caractéristiques de l'invention :
- en dehors d'une période de pressurisation, on condense au moins une partie du mélange gazeux dans un vaporiseur de cuve de la capacité et éventuellement on envoie le mélange gazeux liquéfié à la capacité ;
- le mélange gazeux est de l'air ;
- le système de colonnes comprend au moins une double colonne avec une colonne moyenne pression et une colonne basse pression reliées thermiquement entre elles et dans lequel pendant au moins une partie de la période dans laquelle l'une des bouteilles est en phase de pressurisation, on envoie de l'air de la capacité à la colonne moyenne pression ;
- on envoie de l'air de la capacité à la colonne moyenne pression, jusqu'à ce que la pression de la capacité atteigne la pression de la colonne moyenne pression ;
- on envoie un gaz de la capacité à une colonne du système de colonnes uniquement pendant la période dans laquelle l'une des bouteilles est en phase de pressurisation ;
- la pression maximale de la capacité est d'entre 15 et 40 bars , de préférence entre 20 et 30 bars et/ou la pression minimale est entre 4 et 10 bars.
L'invention sera décrite en plus de détail en se référant à la figure qui illustre un appareil de séparation d'air selon l'invention.
L'appareil de séparation d'air comprend une double colonne classique composée de trois colonnes, une colonne moyenne pression MP et une colonne basse pression BP, les deux étant reliés thermiquement entre elles par un rebouilleur R1 , et une colonne argon AR. Les conduites de reflux entre les deux colonnes sont bien connues dans l'art et ne seront ni décrites ni illustrées.
L'appareil comprend également une capacité 15, un séparateur de phases 17 et une ligne d'échange principale 5. Les sous-refroidisseurs n'ont pas été illustrés.
L'appareil produit de la colonne basse pression un débit riche en oxygène et un débit riche en azote, l'un et/ou l'autre pouvant servir de produit final sous forme liquide et/ou gazeuse.
De l'air 1 épuré dans une unité d'épuration A comprenant des bouteilles d'adsorbant a été comprimé à une pression légèrement supérieure à celle de la colonne moyenne pression MP.
Cet air est divisé en deux parties 5,7. La partie 5 à la pression légèrement supérieure à celle de la colonne moyenne pression MP se refroidit dans la ligne d'échange E01 et est envoyé sous forme gazeuse vers la colonne moyenne pression MP.
La partie 7 est surpressée dans un surpresseur BAC à une pression intermédiaire et ensuite surpressée de nouveau dans un surpresseur D01C entraîné par la turbine D01. Le débit 7 se retrouve ainsi à une haute pression, est refroidi et envoyé au bout chaud de la ligne d'échange E01 où il se refroidit partiellement avant être divisé en deux fractions 11 ,16 en permanence voire trois fractions 4,11 ,16 juste avant et/ou pendant la phase de remplissage. La fraction 11 est détendue dans la turbine D01 pour fournir la grande majorité des frigories nécessaires à l'appareil. Détendue à la moyenne pression, la fraction 11 rejoint la fraction 5 pour former le débit 13 qui est envoyé à la colonne moyenne pression MP.
La fraction 16 poursuit son refroidissement dans la ligne d'échange E01 jusqu'au bout froid, fournissant éventuellement des frigories pour la vaporisation d'un liquide produit par la double colonne (non-illustré). En dehors de la phase de remplissage de la capacité, tout l'air liquéfié ainsi formé est envoyé à travers la vanne V21 à la colonne moyenne pression comme débit 21. Evidemment le débit 13 peut être divisé et envoyé aux deux colonnes.
Il y a au moins deux phases de fonctionnement dans le procédé selon l'invention :
Selon une première phase, la capacité 15 contient de l'air liquéfié à une pression élevée (par exemple 25 bar abs) à sa température d'ébullition. Quand la pressurisation des bouteilles de l'appareil d'épuration A commence, pour durer ensuite environ 6 minutes, on ouvre le circuit 2 en ouvrant la vanne V2 pour alimenter la colonne moyenne pression MP en air gazeux pour compenser la réduction du débit d'alimentation des colonnes comme une partie du débit est requise pour la pressurisation des bouteilles. La pression dans la capacité 15 diminue avec vaporisation de liquide, la chaleur nécessaire étant fournie par le sous-refroidissement de la totalité du liquide disponible dans la capacité. La pression de la capacité 15 diminue jusqu'à la pression de la colonne moyenne pression MP. La quantité de liquide vaporisée et fournie à la colonne moyenne pression correspond à la quantité de gaz nécessaire pour pressuriser la bouteille d'épuration. Au final, le liquide restant est à la température d'ébullition à la pression de la colonne moyenne pression MP. Pendant cette phase, les vannes V19, V29 sont fermées et la capacité
15 n'est pas alimentée en air.
Un circuit de purge 3 assure la déconcentration permanente des impuretés de la capacité à travers la vanne V3 qui envoie la purge vers le liquide riche de cuve provenant de la colonne moyenne pression MP. Selon une deuxième phase, pendant la régénération des bouteilles (qui dure environ 140 minutes) : on effectue le remplissage de la capacité 15, on prend de l'air plus chaud 16 à l'entrée d'une turbine D01 à une pression supérieure à la pression haute finale de la capacité et on le condense dans la capacité 15, grâce au vaporiseur de cuve R2, le liquide de la capacité étant plus froid que l'air à l'entrée de la turbine D01. Cela permet de monter en pression la capacité à 25 bar et de la remplir la capacité 15 de liquide. Le système s'arrête naturellement quand la température du liquide de la capacité 15 est proche de la température à l'entrée de la turbine D01. Un petit appoint d'air liquide (circuit 4) est produit en liquéfiant de l'air dans le vaporiseur R2. Ce liquide est ensuite envoyé à un séparateur de phases 17 et le liquide est envoyé par la conduite 29 à travers la vanne V29 en tête de la capacité 15 pour compléter le niveau de la capacité, ce liquide provenant du vaporiseur R2 étant plus froid que le liquide dans la capacité. Le vaporiseur de cuve R2 assurera la mise à la température d'équilibre de ce liquide. Pendant cette phase, la vanne V2 Un circuit de purge 3 assure la déconcentration permanente des impuretés de la capacité à travers la vanne V3 qui envoie la purge vers le liquide riche de cuve provenant de la colonne moyenne pression MP. Ce liquide riche est ensuite vaporisé dans le condenseur de tête de la colonne argon AR. Cette phase de remplissage peut se faire en remplissant directement avec de l'air liquide haute pression 16,19 venant du bout froid de l'échangeur principal E01 comme illustré, soit en prenant un fluide à point intermédiaire dans l'échangeur principal afin d'avoir la bonne température d'équilibre de la pression finale de la capacité, soit sous refroidi (il sera alors réchauffé par un échangeur de cuve comme décrit précédemment).
Ce dispositif peut être appliqué également sur les boîtes froides de séparation par distillation de mélange ayant pour composants principaux de l'hydrogène et du monoxyde de carbone. Pour compenser les baisses de teneur de monoxyde de carbone lors des inversions d'épuration, on peut déstocker du débit de monoxyde de carbone vers l'aspiration du compresseur de monoxyde de carbone ou déstocker le débit de gaz de synthèse pour stabiliser les alimentations en gaz de la colonne de séparation de monoxyde de carbone et de méthane. Comme la capacité reste à l'intérieur de la boîte froide, le risque d'épandage de monoxyde de carbone liquide est supprimé.
De manière générale, l'invention peut être appliquée sur toute boîte froide cryogénique précédée d'une épuration pour stabiliser un quelconque débit froid alimentant ou produit par les colonnes cryogéniques.

Claims

REVENDICATIONS
1. Appareil de distillation cryogénique d'un mélange gazeux (1 ) comprenant un appareil d'épuration (A) pour épurer le mélange gazeux dans un système à plusieurs bouteilles d'adsorbant opérant selon un cycle comprenant une phase de pressurisation, un système de colonnes (MP1LP1AR), une capacité (15), des moyens pour envoyer un liquide cryogénique (19,V19,29,V29) à la capacité uniquement en dehors d'une phase de pressurisation, des moyens pour envoyer du liquide vaporisé (2,V2) de la capacité à une colonne (MP) du système uniquement pendant au moins une partie de la période dans laquelle l'une des bouteilles est en phase de pressurisation, un vaporiseur (R2) dans la capacité pour vaporiser le liquide contenu, des moyens pour envoyer un gaz calorigène (4) au vaporiseur et des moyens pour soutirer du liquide (3) de la capacité.
2. Appareil selon la revendication 1 dans lequel le liquide cryogénique est constitué par une partie du mélange gazeux liquéfié et/ou le gaz calorigène est constitué par une partie du mélange gazeux.
3. Appareil selon la revendication 1 ou 2 comprenant des moyens
(29,V29) pour envoyer le gaz calorigène liquéfié dans le vaporiseur à la capacité.
4. Appareil selon l'une des revendications précédentes dans lequel on envoie un liquide de la capacité à une (la) colonne (AR) du système de colonnes.
5. Procédé de distillation cryogénique d'un mélange gazeux dans un appareil selon l'une des revendications précédentes dans lequel uniquement pendant au moins une partie de la période dans laquelle l'une des bouteilles de l'unité d'épuration (A) est en phase de pressurisation, on envoie un gaz (2) d'une capacité (15) à une colonne (MP) du système de colonnes et uniquement en dehors d'une période de pressurisation, on remplit la capacité de liquide.
6. Procédé selon la revendication 5 dans lequel, en dehors d'une période de pressurisation, on condense au moins une partie du mélange gazeux dans un vaporiseur de cuve (R2) de la capacité et éventuellement on envoie le mélange gazeux liquéfié à la capacité.
7. Procédé selon l'une des revendications 5 ou 6 dans lequel le mélange gazeux est de l'air.
8. Procédé selon la revendication 7 dans lequel le système de colonnes comprend au moins une double colonne avec une colonne moyenne pression (MP) et une colonne basse pression (BP) reliées thermiquement entre elles et dans lequel pendant au moins une partie de la période dans laquelle l'une des bouteilles est en phase de pressurisation, on envoie de l'air de la capacité (15) à la colonne moyenne pression (MP).
9. Procédé selon la revendication 8 dans lequel on envoie de l'air de la capacité(15) à la colonne moyenne pression (MP), jusqu'à ce que la pression de la capacité atteigne substantiellement la pression de la colonne moyenne pression.
10. Procédé selon l'une des revendications 5 à 9 dans lequel on envoie un gaz de la capacité (15) à une colonne (MP) du système de colonnes uniquement pendant la période dans laquelle l'une des bouteilles est en phase de pressurisation.
PCT/FR2007/052552 2006-12-22 2007-12-18 Procede et appareil de separation d'un melange gazeux par distillation cryogenique WO2008084167A2 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP07871966.3A EP2104825B1 (fr) 2006-12-22 2007-12-18 Procede et appareil de separation d'un melange gazeux par distillation cryogenique
US12/520,112 US8713964B2 (en) 2006-12-22 2007-12-18 Method and device for separating a gas mixture by cryogenic distillation
CN2007800474576A CN101595356B (zh) 2006-12-22 2007-12-18 通过低温蒸馏分离气体混合物的方法和装置
US14/200,049 US9546815B2 (en) 2006-12-22 2014-03-07 Method and device for separating a gas mixture by cryogenic distillation

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FR0655924A FR2910604B1 (fr) 2006-12-22 2006-12-22 Procede et appareil de separation d'un melange gazeux par distillation cryogenique
FR0655924 2006-12-22

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US14/200,049 Division US9546815B2 (en) 2006-12-22 2014-03-07 Method and device for separating a gas mixture by cryogenic distillation

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US11097221B2 (en) 2018-10-05 2021-08-24 8 Rivers Capital, Llc Direct gas capture systems and methods of use thereof
KR20220005074A (ko) 2019-05-03 2022-01-12 8 리버스 캐피탈, 엘엘씨 탄소 포집을 위한 시스템 및 방법
JP2022546399A (ja) 2019-08-26 2022-11-04 ８ リバーズ キャピタル，エルエルシー オキシ燃料燃焼プロセスにおける火炎制御

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CN101595356A (zh) 2009-12-02
US20100011811A1 (en) 2010-01-21
US8713964B2 (en) 2014-05-06
EP2104825B1 (fr) 2018-08-15
US9546815B2 (en) 2017-01-17
CN101595356B (zh) 2012-11-28
FR2910604A1 (fr) 2008-06-27
FR2910604B1 (fr) 2012-10-26
EP2104825A2 (fr) 2009-09-30
WO2008084167A3 (fr) 2009-05-22

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