EP2591301A2 - Apparatus and process for separating air by cryogenic distillation - Google Patents

Apparatus and process for separating air by cryogenic distillation

Info

Publication number
EP2591301A2
EP2591301A2 EP11728894.4A EP11728894A EP2591301A2 EP 2591301 A2 EP2591301 A2 EP 2591301A2 EP 11728894 A EP11728894 A EP 11728894A EP 2591301 A2 EP2591301 A2 EP 2591301A2
Authority
EP
European Patent Office
Prior art keywords
flow
oxygen
liquid
rich
storage
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP11728894.4A
Other languages
German (de)
French (fr)
Other versions
EP2591301B1 (en
Inventor
Benoît DAVIDIAN
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP2591301A2 publication Critical patent/EP2591301A2/en
Application granted granted Critical
Publication of EP2591301B1 publication Critical patent/EP2591301B1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • F25J3/0204—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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—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
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low 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
    • F25J3/04406—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
    • F25J3/04763—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
    • 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
    • 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
    • F25J3/04854—Safety aspects of operation
    • F25J3/0486—Safety aspects of operation of vaporisers for oxygen enriched liquids, e.g. purging of liquids
    • 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
    • F25J2215/02—Mixing or blending of fluids to yield a certain product
    • 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
    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F25J2215/54—Oxygen production with multiple pressure O2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/50—One fluid being oxygen
    • 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 an apparatus and method for air separation by cryogenic distillation.
  • a purge liquid is sent to a storage, and a portion of storage liquid is sent into an exchanger to be mixed with oxygen gas.
  • the storage is also powered by liquid transported by a truck, so it is a liquid oxygen injection with a supplement of external liquid, thereby vaporizing the purge with heated oxygen gas.
  • a storage is supplied by a purge flow from the tank of the low pressure column in the event of reduction of the production of the column system, a storage flow is withdrawn from the storage which is vaporized in a emergency vaporizer.
  • the purge can compensate the evaporation losses in the storage and the excess is vaporized in the system of the emergency vaporization (without recovery of frigories in the cold box).
  • it is intended to send a purge flow to a storage of liquid oxygen, possibly using a pump depending on its pressure.
  • a flow of oxygen-rich liquid having a nominal flow rate is withdrawn from the low-pressure column, vaporized in a main evaporator to form a gaseous product, and an oxygen-rich liquid purge flow rate of not more than 2% of nominal output flow of the oxygen-rich flow of the vaporizer,
  • the oxygen-rich liquid purge flow rate of the low pressure column vessel or the vaporizer is sent into the storage system permanently or episodically, outside the stopping and starting periods of the column system.
  • the flow rate having a nominal flow rate is a flow rate of gas withdrawn from the low pressure column and the purge flow rate constitutes the only oxygen-rich flow rate withdrawn from the column system.
  • the storage is filled with liquid from a tank of at least one column of the column system.
  • a flow of oxygen rich gas having a nominal flow rate is withdrawn from the low pressure column in order to form a gaseous product, and an oxygen-rich liquid purge flow rate is drawn off in the bottom of the low pressure column, the purge flow being richer; in oxygen and heavy impurities that the flow having the nominal flow and constituting at most 2% of the nominal rate of production of oxygen-rich flow.
  • a flow of oxygen rich liquid having a nominal flow rate is withdrawn from the low pressure column, it is vaporized in a main vaporizer to form a gaseous product and an oxygen-rich liquid purge flow rate is drawn up constituting at most 2% of the flow rate; nominal flow rate of the oxygen-rich flow of the vaporizer.
  • the delivery of the product from the storage to the shaker vaporizer is only triggered if the customer's needs increase or if the production is reduced. column system.
  • the emergency vaporizer has a vaporization function of the overflow in the storage.
  • an apparatus for separating air by cryogenic distillation comprising a system of columns comprising a medium pressure column and a low pressure column, a storage, a backup vaporizer and either
  • a main vaporizer means for withdrawing from the low pressure column a flow of oxygen-rich liquid having a nominal flow rate and sending it to the main vaporizer, means for withdrawing a gaseous product formed by vaporization of the liquid flow, means for withdrawing an oxygen-rich liquid purge flow rate constituting not more than 2% of the nominal flow rate for producing the oxygen-rich flow rate of the vaporizer,
  • sensing and control means for detecting the liquid level in the storage and for triggering, if the level exceeds a threshold corresponding to the maximum capacity, withdrawing a liquid flow of the storage constituting at most 2% of the nominal flow rate of production of the flow rich in oxygen and the sending of this flow rate to the backup vaporizer to constitute a part of the gaseous product, these detection and control means being able to detect if the level of liquid in the storage is below the threshold and, in this case, triggering the sending of the liquid purge flow to the storage and the prevention of sending the liquid from the storage to the emergency vaporizer except in the case reducing the production of the column system or increasing the need of a customer for the gaseous product.
  • the device does not include a means of spraying purge liquid apart from the emergency vaporizer.
  • the apparatus comprises means for withdrawing from the low pressure column a flow of oxygen-rich gas having a nominal flow rate to form a gaseous product and means for withdrawing an oxygen-rich liquid purge flow rate in the bottom of the low pressure column; , the purge flow rate being richer in oxygen and heavy impurities than the flow rate having the nominal flow rate and constituting not more than 2% of the nominal rate of production of the oxygen-rich flow.
  • the device includes
  • a main vaporizer means for extracting from the low pressure column a flow of oxygen-rich liquid having a nominal flow rate and sending it to the main vaporizer, means for withdrawing a gaseous product formed by vaporization of the liquid flow rate and means for withdrawing an oxygen-rich liquid purge flow rate constituting not more than 2% of the nominal output flow rate of the oxygen-rich flow of the vaporizer.
  • the transfer pump may also be that used for the transfer of liquid oxygen production, if any.
  • the storage of liquid oxygen is filled with oxygen of "commercial industrial” quality which is therefore “pure” (99.5 mol%).
  • oxygen of "commercial industrial” quality which is therefore “pure” (99.5 mol%).
  • Sending a purge liquid with a mean purity lower than that of the storage liquid will slightly reduce the purity of liquid contained in the storage, which will nonetheless be at a higher average content than the customer demand.
  • a flow rich in oxygen, gaseous or liquid, contains at least 75 mol%. oxygen.
  • a flow of compressed and purified air 1 is cooled in a heat exchanger 3 and divided into three.
  • a flow 7 is withdrawn from the exchanger at an intermediate level, expanded in a turbine 9 and sent to a low pressure column 13 of a double column in gaseous form.
  • Another flow 5 after being supercharged in the compressor A liquefies in the exchanger 3, is expanded in a valve 1 1 and sent to the medium pressure column 13.
  • a third flow B sent directly into the medium pressure column.
  • Flow rates enriched with nitrogen and oxygen are sent from the medium pressure column to the low pressure column in a known manner.
  • the liquid oxygen accumulates around the reboiler 17.
  • a flow of liquid oxygen 19 containing less than 98% of oxygen is withdrawn from the tank of the low pressure column 15 and pressurized by a pump 23 up to 2 bars, alternatively the compression can be hydrostatic.
  • Part of the oxygen at this pressure is sent to a vaporizer 24 where it vaporizes by heat exchange with a portion of the supply air (5 or B) which is then sent to the column.
  • This vaporized flow rate constitutes the gaseous production of the column system in normal operation and is produced with a nominal flow rate.
  • a purge flow 121 containing impurities is withdrawn from the vaporizer
  • This flow rate is purer in oxygen than the flow rate 19.
  • the vaporized oxygen continues to heat up in the exchanger 3 as the flow rate 27 of low pressure oxygen.
  • the rest of the oxygen is pressurized to a pressure of 10 bar in a pump 25 and vaporizes in the exchanger 3 as flow 29.
  • all the oxygen can be vaporized to the lower pressure and the flow 29 does not exist.
  • a first conduit connects the vaporizer 24 with the storage 31 to bring the purge liquid 121 permanently or episodically, unless the column system does not work.
  • the storage 31 supplies a backup vaporizer 37 with liquid oxygen 35.
  • the purge liquid can be sent episodically, that is to say that the liquid is withdrawn from the vaporizer periodically, in a cycle, in order to have quantities of liquid allowing a correct analysis.
  • Oxygen is vaporized in the emergency vaporizer 37 in large quantities, when the customer's needs are particularly high or when the air separation device does not operate at full speed, in case of failure, for example.
  • an oxygen-rich liquid flow constituting less than 2% of the nominal oxygen gas flow rate 19 and preferably about 1% of the nominal flow is sent to the storage.
  • This liquid flow rate is sent to the backup vaporizer only if the level in the storage exceeds a threshold, this threshold being ordinarily that of the maximum capacity of the storage 31.
  • this flow sent to the backup vaporizer constitutes the overflow of the storage 31.
  • the vaporized oxygen is sent to the customer.
  • the storage 31 is filled by sending the liquid 121 there.
  • the liquid in the storage comes from a tanker 61 or from the apparatus itself by the flow 21, which can be diverted to storage punctually.
  • the liquid in the storage from the truck has a purity of 99.5 mol%.
  • the liquid 121 may be purer, as pure or less pure than the liquid from the tanker truck.61.
  • liquids accumulated in the bottom of the low pressure and / or medium pressure column in the lines 21 and 51 will obviously have a purity lower than that of the liquid from the truck 61 or that of the liquid 121. In some cases, the customer can withstand a short-term reduction of purity of the vaporized liquid in the backup vaporizer.
  • a valve 41 makes it possible to regulate the flow rates of these accumulated liquids sent to the storage 31.
  • a flow of compressed and purified air 1 is cooled in a heat exchanger 3 and divided into two.
  • a flow 7 is withdrawn from the exchanger at an intermediate level, expanded in a turbine 9 and sent to a low pressure column 13 of a double column in gaseous form.
  • Another flow 5 is cooled in the heat exchanger 3, and sent to the medium pressure column 13.
  • Flow rates enriched with nitrogen and oxygen are sent from the medium pressure column to the low pressure column in a known manner.
  • the liquid oxygen accumulates around the reboiler 17.
  • a flow of gaseous oxygen 19 containing 98% of oxygen is withdrawn from the tank of the low pressure column 15 and is heated in the exchanger 3 as flow 27 low pressure oxygen before undergoing a possible compression.
  • a purge flow 21 containing impurities is withdrawn from the tank of the column 15 continuously to avoid the accumulation of impurities in the bottom of the column. This liquid withdrawal is the only oxygen-rich withdrawal of the column system.
  • a first conduit connects the LP column vessel with the storage 31 to bring the purge liquid 21 continuously (either continuously or in regular batches), unless the column system does not work.
  • the storage 31 supplies a backup vaporizer 37 with liquid oxygen 35.
  • Oxygen is vaporized in the emergency vaporizer 37 in large quantities, when the customer's needs are particularly high or when the air separation device does not operate at full speed, in case of failure, for example.
  • an oxygen-rich liquid flow constituting less than 2% of the nominal oxygen gas flow rate 19 and preferably about 1% of the nominal flow is sent to the storage.
  • This liquid flow rate is sent to the backup vaporizer if the level in the storage exceeds a threshold, this threshold being ordinarily that of the maximum capacity of the storage 31.
  • this flow sent to the backup vaporizer constitutes the overflow of the storage 31.
  • Vaporized oxygen is sent to the customer
  • the storage 31 is filled by sending the liquid 21. In normal operation therefore, the storage liquid is not sent to the backup vaporizer, if the maximum level is not reached.
  • the triggering of the sending of the storage to the backup vaporizer may be necessary, in the event of a reduction in the production of the column system or an increase in the customer's needs.
  • the purge flow 21 has a higher oxygen molar purity than the flow rate 19.
  • liquid in the storage comes from a tank truck 61 or the device itself by a liquid flow drawn off punctually (not shown), which can be sent to storage.
  • the liquid in the storage from the truck has a purity of 99.5 mol%.
  • a pump may be needed to send the purge liquid 21 to the storage.
  • the purge flow 21 may be purer, as pure or less pure than the liquid supplying the storage from the tanker 61 for example.
  • the liquid from the storage 31 can be vaporized in a backup vaporizer 37 and sent to a customer in case of failure of the distillation apparatus and / or if production of the distillation apparatus is insufficient to supply the customer.

Abstract

In a process for delivering pressurized gas from an apparatus for separating air by cryogenic distillation, a stream of oxygen-rich liquid or gas (19) having a nominal flow rate is withdrawn from a low-pressure column, an oxygen-rich liquid purge stream (21,121) is withdrawn as bottoms from the low-pressure column and the oxygen-rich liquid purge stream is sent to a storage tank (31), in the event of a reduction in the production by the column system or an increase in the demand by a customer, a back-up stream is withdrawn from the storage tank (31) and vaporized in a back-up reboiler (37) and only if the liquid level in the storage tank exceeds a given threshold, a liquid stream is withdrawn from the storage tank constituting at most 2% of the nominal production output of the oxygen-rich stream and is sent to the back-up reboiler.

Description

Appareil et procédé de séparation d'air par distillation cryogénique  Apparatus and method for separating air by cryogenic distillation
La présente invention est relative à un appareil et à un procédé de séparation d'air par distillation cryogénique. The present invention relates to an apparatus and method for air separation by cryogenic distillation.
Dans ces appareils, il est nécessaire de prélever un débit de purge en permanence des vaporiseurs extérieurs servant à vaporiser de l'oxygène liquide à basse pression et/ou des vaporiseurs à l'intérieur des colonnes, pour éviter un accumulation potentiellement dangereuse d'impuretés. Ces débits de purge sont soutirés substantiellement en permanence par exemple de la cuve d'une colonne basse pression produisant seulement de l'oxygène gazeux soutiré directement de cette colonne, pour éviter l'accumulation des impuretés.  In these devices, it is necessary to draw a continuous purge flow of external vaporizers for vaporizing low pressure liquid oxygen and / or vaporizers inside the columns, to avoid a potentially dangerous accumulation of impurities. . These purge flow rates are withdrawn substantially continuously for example from the tank of a low pressure column producing only gaseous oxygen withdrawn directly from this column, to avoid the accumulation of impurities.
La purge des liquides cryogéniques de la boite froide sont en général envoyés vers un dispositif spécifique pour les vaporiser :  Purge of cryogenic liquids from the cold box is usually sent to a specific device to vaporize them:
• fosse à cailloux pour les très petites tailles de générateurs  • pebble pit for very small generators
• enceinte atmosphérique qui recueille les liquides, qui vont ensuite se vaporiser lentement  • atmospheric enclosure that collects liquids, which will then vaporize slowly
• évaporateur (utilisant un chauffage et une ventilation)  • evaporator (using heating and ventilation)
Dans EP-A-0605262, un liquide de purge est envoyé dans un stockage, et une partie de liquide du stockage est envoyé dans un échangeur pour être mélangé avec de l'oxygène gazeux. Le stockage est également alimenté par du liquide transporté par un camion : il s'agit donc d'une injection d'oxygène liquide avec un appoint de liquide extérieur, permettant ainsi de vaporiser la purge avec l'oxygène gazeux réchauffé.  In EP-A-0605262, a purge liquid is sent to a storage, and a portion of storage liquid is sent into an exchanger to be mixed with oxygen gas. The storage is also powered by liquid transported by a truck, so it is a liquid oxygen injection with a supplement of external liquid, thereby vaporizing the purge with heated oxygen gas.
Dans EP-A-1202012, on alimente un stockage par un débit de purge provenant de la cuve de la colonne basse pression en cas de réduction de la production du système de colonnes, on soutire du stockage un débit de secours qui est vaporisé dans un vaporiseur de secours.  In EP-A-1202012, a storage is supplied by a purge flow from the tank of the low pressure column in the event of reduction of the production of the column system, a storage flow is withdrawn from the storage which is vaporized in a emergency vaporizer.
Selon l'invention, la purge peut compenser les pertes d'évaporation dans le stockage et l'excès est vaporisé dans le système de la vaporisation de secours (sans récupération des frigories dans la boite froide). Selon l'invention, il est prévu d'envoyer un débit de purge vers un stockage d'oxygène liquide, éventuellement à l'aide d'une pompe en fonction de sa pression. According to the invention, the purge can compensate the evaporation losses in the storage and the excess is vaporized in the system of the emergency vaporization (without recovery of frigories in the cold box). According to the invention, it is intended to send a purge flow to a storage of liquid oxygen, possibly using a pump depending on its pressure.
Selon un objet de l'invention, il est prévu un procédé de séparation d'air par distillation cryogénique pour fournir un produit gazeux, éventuellement sous pression, dans lequel  According to one object of the invention, there is provided a method of air separation by cryogenic distillation to provide a gaseous product, possibly under pressure, in which
a) on envoie de l'air refroidi, épuré et comprimé dans un système de colonnes comprenant une colonne moyenne pression et une colonne basse pression (15)  a) cooling, purified and compressed air is supplied to a column system comprising a medium pressure column and a low pressure column (15)
b) i) on soutire de la colonne basse pression un débit de gaz riche en oxygène ayant un débit nominal pour former un produit gazeux et on soutire un débit de purge liquide riche en oxygène en cuve de la colonne basse pression, le débit de purge étant plus riche en oxygène et en impuretés lourdes que le débit ayant le débit nominal et constituant au plus 2% du débit nominal de production du débit riche en oxygène ou  b) i) a flow of oxygen-rich gas having a nominal flow rate is withdrawn from the low-pressure column to form a gaseous product and an oxygen-rich liquid purge flow rate is withdrawn in the bottom of the low-pressure column, the purge flow rate being richer in oxygen and heavy impurities than the flow rate having the nominal flow rate and constituting not more than 2% of the nominal oxygen-rich flow rate or
ii) on soutire de la colonne basse pression un débit de liquide riche en oxygène ayant un débit nominal, on le vaporise dans un vaporiseur principal pour former un produit gazeux et on soutire un débit de purge liquide riche en oxygène constituant au plus 2% du débit nominal de production du débit riche en oxygène du vaporiseur,  ii) a flow of oxygen-rich liquid having a nominal flow rate is withdrawn from the low-pressure column, vaporized in a main evaporator to form a gaseous product, and an oxygen-rich liquid purge flow rate of not more than 2% of nominal output flow of the oxygen-rich flow of the vaporizer,
c) on envoie le débit de purge liquide riche en oxygène dans un stockage,  c) the oxygen-rich liquid purge flow is sent to a storage,
d) si le niveau de liquide dans le stockage dépasse un seuil correspondant à la capacité maximale du stockage, on soutire un débit liquide du stockage constituant au plus 2% du débit nominal de production du débit riche en oxygène et on l'envoie au vaporiseur de secours pour constituer une partie du produit gazeux, et  d) if the liquid level in the storage exceeds a threshold corresponding to the maximum storage capacity, a liquid flow from the storage constituting not more than 2% of the nominal output flow rate of the oxygen-rich flow is withdrawn and sent to the vaporizer relief to form part of the gaseous product, and
e) si le niveau de liquide dans le stockage est en dessous du seuil, on envoie le débit de purge liquide au stockage mais on n'envoie du liquide du stockage au vaporiseur de secours qu'en cas de réduction de production du système de colonnes ou d'augmentation du besoin d'un client pour le produit gazeux. Selon d'autres objets facultatifs : e) if the liquid level in the storage is below the threshold, the liquid purge flow is sent to the storage but the liquid is sent from the storage to the backup vaporizer only in the case of a reduction in the production of the column system or increasing a customer's need for the gaseous product. According to other optional objects:
- on envoie le débit de purge liquide riche en oxygène de la cuve de la colonne basse pression ou du vaporiseur dans le stockage en permanence ou épisodiquement, en dehors de périodes d'arrêt et de démarrage du système de colonnes.  the oxygen-rich liquid purge flow rate of the low pressure column vessel or the vaporizer is sent into the storage system permanently or episodically, outside the stopping and starting periods of the column system.
- lors d'un arrêt du système de colonne, le débit de purge n'est pas envoyé au stockage  - when stopping the column system, the purge flow is not sent to the storage
- le débit ayant un débit nominal est un débit de gaz soutiré de la colonne basse pression et le débit de purge constitue le seul débit riche en oxygène soutiré du système de colonnes.  the flow rate having a nominal flow rate is a flow rate of gas withdrawn from the low pressure column and the purge flow rate constitutes the only oxygen-rich flow rate withdrawn from the column system.
- lors d'un arrêt du système de colonnes, on remplit le stockage au moyen de liquide provenant d'une cuve d'au moins une colonne du système de colonnes.  - When stopping the column system, the storage is filled with liquid from a tank of at least one column of the column system.
- on soutire de la colonne basse pression un débit de gaz riche en oxygène ayant un débit nominal pour former un produit gazeux et on soutire un débit de purge liquide riche en oxygène en cuve de la colonne basse pression, le débit de purge étant plus riche en oxygène et en impuretés lourdes que le débit ayant le débit nom inal et constituant au plus 2% du débit nom inal de production du débit riche en oxygène.  a flow of oxygen rich gas having a nominal flow rate is withdrawn from the low pressure column in order to form a gaseous product, and an oxygen-rich liquid purge flow rate is drawn off in the bottom of the low pressure column, the purge flow being richer; in oxygen and heavy impurities that the flow having the nominal flow and constituting at most 2% of the nominal rate of production of oxygen-rich flow.
- on soutire de la colonne basse pression un débit de liquide riche en oxygène ayant un débit nominal , on le vaporise dans un vaporiseur principal pour former un produit gazeux et on soutire un débit de purge liquide riche en oxygène constituant au plus 2% du débit nominal de production du débit riche en oxygène du vaporiseur.  a flow of oxygen rich liquid having a nominal flow rate is withdrawn from the low pressure column, it is vaporized in a main vaporizer to form a gaseous product and an oxygen-rich liquid purge flow rate is drawn up constituting at most 2% of the flow rate; nominal flow rate of the oxygen-rich flow of the vaporizer.
- l'envoi de liquide du stockage vers la vaporiseur de secours est toujours déclenché si le seuil dans le stockage est dépassé  - the sending of liquid from the storage to the backup vaporizer is always triggered if the threshold in the storage is exceeded
- si le seu il dans le stockage n'est pas atteint, l'envoi de l iqu ide du stockage vers le vaporiseur de secou rs est u niquement déclenché en cas d'augmentation des besoins du client ou en cas de réduction de production du système de colonnes.  - If only the storage is not reached, the delivery of the product from the storage to the shaker vaporizer is only triggered if the customer's needs increase or if the production is reduced. column system.
Ainsi le vaporiseur de secours a une fonction de vaporisation du trop- plein dans le stockage.  Thus, the emergency vaporizer has a vaporization function of the overflow in the storage.
Selon un autre objet de l'invention, il est prévu un appareil de séparation d'air par distillation cryogénique comprenant un système de colonnes comprenant une colonne moyenne pression et une colonne basse pression, un stockage, un vaporiseur de secours et soit According to another object of the invention, there is provided an apparatus for separating air by cryogenic distillation comprising a system of columns comprising a medium pressure column and a low pressure column, a storage, a backup vaporizer and either
i) des moyens pour soutirer de la colonne basse pression un débit de gaz riche en oxygène ayant un débit nominal pour former un produit gazeux et des moyens pour soutirer un débit de purge liquide riche en oxygène en cuve de la colonne basse pression, le débit de purge étant plus riche en oxygène et en impuretés lourdes que le débit ayant le débit nominal et constituant au plus 2% du débit nominal de production du débit riche en oxygène ou  i) means for withdrawing from the low pressure column a flow of oxygen-rich gas having a nominal flow rate to form a gaseous product and means for withdrawing an oxygen-rich liquid purge flow rate in the bottom of the low-pressure column, the flow rate purge being richer in oxygen and heavy impurities than the flow rate having the nominal flow and constituting at most 2% of the nominal flow rate of production of oxygen-rich flow or
ii) un vaporiseur principal, des moyens pour soutirer de la colonne basse pression un débit de liquide riche en oxygène ayant un débit nominal et de l'envoyer au vaporiseur principal, des moyens pour soutirer un produit gazeux formé par vaporisation du débit de liquide, des moyens pour soutirer un débit de purge liquide riche en oxygène constituant au plus 2% du débit nom inal de production du débit riche en oxygène du vaporiseur,  ii) a main vaporizer, means for withdrawing from the low pressure column a flow of oxygen-rich liquid having a nominal flow rate and sending it to the main vaporizer, means for withdrawing a gaseous product formed by vaporization of the liquid flow, means for withdrawing an oxygen-rich liquid purge flow rate constituting not more than 2% of the nominal flow rate for producing the oxygen-rich flow rate of the vaporizer,
et des moyens pour envoyer le débit de purge liquide riche en oxygène au stockage, des moyens de détection et de commande pour détecter le niveau de liquide dans le stockage et pour déclencher, si le niveau dépasse un seuil correspondant à la capacité maximale, le soutirage un débit liquide du stockage constituant au pl us 2% d u débit nom inal de production du débit riche en oxygène et l'envoi de ce débit au vaporiseur de secours pour constituer une partie du produit gazeux, ces moyens de détection et de commande pouvant détecter si le n iveau de liquide dans le stockage est en dessous du seuil et, pour déclencher dans ce cas, l'envoi du débit de purge liquide au stockage et l'empêchement de l'envoi du liquide du stockage au vaporiseur de secours sauf cas de réduction de production du système de colonnes ou d'augmentation du besoin d'un client pour le produit gazeux.  and means for sending the oxygen-rich liquid purge flow to the storage, sensing and control means for detecting the liquid level in the storage and for triggering, if the level exceeds a threshold corresponding to the maximum capacity, withdrawing a liquid flow of the storage constituting at most 2% of the nominal flow rate of production of the flow rich in oxygen and the sending of this flow rate to the backup vaporizer to constitute a part of the gaseous product, these detection and control means being able to detect if the level of liquid in the storage is below the threshold and, in this case, triggering the sending of the liquid purge flow to the storage and the prevention of sending the liquid from the storage to the emergency vaporizer except in the case reducing the production of the column system or increasing the need of a customer for the gaseous product.
Selon d'autres objets facultatifs :  According to other optional objects:
- l'appareil ne comprend pas de moyen de vaporisation de liquide de purge à part le vaporiseur de secours.  - The device does not include a means of spraying purge liquid apart from the emergency vaporizer.
- l'appareil comprend des moyens pour soutirer de la colonne basse pression un débit de gaz riche en oxygène ayant un débit nominal pour former un produit gazeux et des moyens pour soutirer un débit de purge liquide riche en oxygène en cuve de la colonne basse pression, le débit de purge étant plus riche en oxygène et en impuretés lourdes que le débit ayant le débit nominal et constituant au plus 2% du débit nominal de production du débit riche en oxygène. the apparatus comprises means for withdrawing from the low pressure column a flow of oxygen-rich gas having a nominal flow rate to form a gaseous product and means for withdrawing an oxygen-rich liquid purge flow rate in the bottom of the low pressure column; , the purge flow rate being richer in oxygen and heavy impurities than the flow rate having the nominal flow rate and constituting not more than 2% of the nominal rate of production of the oxygen-rich flow.
- l'appareil comprend  - the device includes
- un vaporiseur principal, des moyens pour soutirer de la colonne basse pression un débit de liquide riche en oxygène ayant un débit nominal et de l'envoyer au vaporiseur principal, des moyens pour soutirer un produit gazeux formé par vaporisation du débit de liquide et des moyens pour soutirer un débit de purge liquide riche en oxygène constituant au plus 2% du débit nominal de production du débit riche en oxygène du vaporiseur.  a main vaporizer, means for extracting from the low pressure column a flow of oxygen-rich liquid having a nominal flow rate and sending it to the main vaporizer, means for withdrawing a gaseous product formed by vaporization of the liquid flow rate and means for withdrawing an oxygen-rich liquid purge flow rate constituting not more than 2% of the nominal output flow rate of the oxygen-rich flow of the vaporizer.
- des moyens pour alimenter le stockage par un liquide d'une source extérieure.  means for supplying the storage with a liquid from an external source.
- des moyens pour envoyer un liquide de cuve de la colonne basse pression au stockage.  means for sending a bottom liquid from the low pressure column to storage.
- des moyens pour envoyer un liquide de cuve de la colonne moyenne pression au stockage.  means for sending a tank liquid from the medium-pressure column to storage.
On notera que la pompe de transfert peut être aussi celle qui est utilisée pour le transfert de la production d'oxygène liquide, le cas échéant.  It should be noted that the transfer pump may also be that used for the transfer of liquid oxygen production, if any.
Le stockage d'oxygène liquide est rempli avec de l'oxygène de qualité « industriel marchand » qui est donc « pur » (99.5% mol.). Pour alimenter le client lorsque l'appareil de séparation d'air ne fonctionne pas, il est prévu de vaporiser du liquide provenant de ce stockage dans un vaporiseur de secours. L'envoi d'un liquide de purge avec une pureté moyenne inférieure à celle du liquide du stockage va réduire légèrement la pureté de liquide contenu dans le stockage, qui sera néanmoins à une teneur moyenne supérieure à la demande client.  The storage of liquid oxygen is filled with oxygen of "commercial industrial" quality which is therefore "pure" (99.5 mol%). To feed the customer when the air separation device is not working, it is expected to vaporize liquid from this storage in a backup vaporizer. Sending a purge liquid with a mean purity lower than that of the storage liquid will slightly reduce the purity of liquid contained in the storage, which will nonetheless be at a higher average content than the customer demand.
Un débit riche en oxygène, gazeux ou liquide, contient au moins 75% mol. d'oxygène.  A flow rich in oxygen, gaseous or liquid, contains at least 75 mol%. oxygen.
L'invention sera décrite en plus de détail en se référant aux figures qui illustrent des appareils selon l'invention.  The invention will be described in more detail with reference to the figures which illustrate apparatus according to the invention.
Dans la Figure 1 , un débit d'air comprimé et épuré 1 est refroidi dans un échangeur de chaleur 3 et divisé en trois. Un débit 7 est soutiré de l'échangeur à un niveau intermédiaire, détendu dans une turbine 9 et envoyé à une colonne basse pression 13 d'une double colonne sous forme gazeuse. Un autre débit 5, après avoir été surpressé dans le compresseur A se liquéfie dans l'échangeur de chaleur 3, est détendu dans une vanne 1 1 et envoyé à la colonne moyenne pression 13. Un troisième débit B en envoyé directement dans la colonne moyenne pression. In Figure 1, a flow of compressed and purified air 1 is cooled in a heat exchanger 3 and divided into three. A flow 7 is withdrawn from the exchanger at an intermediate level, expanded in a turbine 9 and sent to a low pressure column 13 of a double column in gaseous form. Another flow 5, after being supercharged in the compressor A liquefies in the exchanger 3, is expanded in a valve 1 1 and sent to the medium pressure column 13. A third flow B sent directly into the medium pressure column.
Des débits enrichis en azote et en oxygène sont envoyés de la colonne moyenne pression à la colonne basse pression de manière connue. En cuve de la colonne basse pression 15, l'oxygène liquide s'accumule autour du rebouilleur 17. Un débit d'oxygène liquide 19 contenant moins de 98% d'oxygène est soutiré de la cuve de la colonne basse pression 15 et pressurisé par une pompe 23 jusqu'à 2 bars, alternativement la compression peut être hydrostatique. Une partie de l'oxygène à cette pression est envoyée à un vaporiseur 24 où elle se vaporise par échange de chaleur avec une partie de l'air d'alimentation (5 ou B) qui est ensuite envoyé à la colonne. Ce débit vaporisé constitue la production gazeuse du système de colonnes en fonctionnement normal et est produit avec un débit nominal .  Flow rates enriched with nitrogen and oxygen are sent from the medium pressure column to the low pressure column in a known manner. In the tank of the low pressure column 15, the liquid oxygen accumulates around the reboiler 17. A flow of liquid oxygen 19 containing less than 98% of oxygen is withdrawn from the tank of the low pressure column 15 and pressurized by a pump 23 up to 2 bars, alternatively the compression can be hydrostatic. Part of the oxygen at this pressure is sent to a vaporizer 24 where it vaporizes by heat exchange with a portion of the supply air (5 or B) which is then sent to the column. This vaporized flow rate constitutes the gaseous production of the column system in normal operation and is produced with a nominal flow rate.
Un débit de purge 121 contenant des impuretés est soutiré du vaporiseur A purge flow 121 containing impurities is withdrawn from the vaporizer
24 en permanence, sauf si le système de colonnes ne fonctionne pas. Ce débit est plus pur en oxygène que le débit 19. L'oxygène vaporisé poursuit son réchauffement dans l'échangeur 3 comme débit 27 d'oxygène basse pression. 24 permanently, unless the column system is not working. This flow rate is purer in oxygen than the flow rate 19. The vaporized oxygen continues to heat up in the exchanger 3 as the flow rate 27 of low pressure oxygen.
Le reste de l'oxygène est pressurisé jusqu'à une pression de 10 bars dans une pompe 25 et se vaporise dans l'échangeur 3 comme débit 29. Alternativement tout l'oxygène peut être vaporisé jusqu'à la pression plus basse et le débit 29 n'existe pas.  The rest of the oxygen is pressurized to a pressure of 10 bar in a pump 25 and vaporizes in the exchanger 3 as flow 29. Alternatively all the oxygen can be vaporized to the lower pressure and the flow 29 does not exist.
Une première conduite relie le vaporiseur 24 avec le stockage 31 pour y amener le liquide de purge 121 en permanence ou épisodiquement, sauf si le système de colonnes ne fonctionne pas. Le stockage 31 alimente un vaporiseur de secours 37 avec de l'oxygène liquide 35. L'envoi de liquide de purge peut être épisod iq ue, c'est-à-dire que le liquide est soutiré du vaporiseur périodiquement, selon un cycle, afin d'avoir des quantités de liquide permettant une analyse correcte.  A first conduit connects the vaporizer 24 with the storage 31 to bring the purge liquid 121 permanently or episodically, unless the column system does not work. The storage 31 supplies a backup vaporizer 37 with liquid oxygen 35. The purge liquid can be sent episodically, that is to say that the liquid is withdrawn from the vaporizer periodically, in a cycle, in order to have quantities of liquid allowing a correct analysis.
L'oxygène est vaporisé dans le vaporiseur de secours 37 en grande quantité, quand les besoins du client sont particulièrement élevés ou quand l'appareil de séparation d'air ne fonctionne pas à plein régime, en cas de panne par exemple. Par contre pendant les périodes où les besoins du client ne sont pas particulièrement élevés et l'appareil de séparation d'air fonctionne normalement, un débit liquide riche en oxygène constituant moins de 2% du débit nominal d'oxygène gazeux 19 et de préférence environ 1 % du débit nominal est envoyé vers le stockage. Ce débit liquide est envoyé au vaporiseur de secours uniquement si le niveau dans le stockage dépasse un seuil, ce seuil étant ordinairement celui de la capacité maximale du stockage 31 . Ainsi ce débit envoyé au vaporiseur de secours constitue le trop-plein du stockage 31 . L'oxygène vaporisé est envoyé au client. Oxygen is vaporized in the emergency vaporizer 37 in large quantities, when the customer's needs are particularly high or when the air separation device does not operate at full speed, in case of failure, for example. On the other hand, during periods when the customer's needs are not particularly high and the air separation apparatus is operating normally, an oxygen-rich liquid flow constituting less than 2% of the nominal oxygen gas flow rate 19 and preferably about 1% of the nominal flow is sent to the storage. This liquid flow rate is sent to the backup vaporizer only if the level in the storage exceeds a threshold, this threshold being ordinarily that of the maximum capacity of the storage 31. Thus this flow sent to the backup vaporizer constitutes the overflow of the storage 31. The vaporized oxygen is sent to the customer.
Ceci permet de récupérer les molécules de la purge dans le liquide 121 , et donc de réduire la production totale de l'appareil (gain d'énergie de 1 % à 2% environ maximum.)  This makes it possible to recover the molecules of the purge in the liquid 121, and thus to reduce the total production of the apparatus (energy gain from 1% to about 2% maximum.)
Si le niveau du stockage 31 est en dessous du seuil, en particulier quand le stockage n'est pas plein, on remplit le stockage 31 en y envoyant le liquide 121 .  If the level of the storage 31 is below the threshold, in particular when the storage is not full, the storage 31 is filled by sending the liquid 121 there.
La plupart du liquide dans le stockage provient d'un camion-citerne 61 ou de l'appareil lui-même par le débit 21 , qui peut être détourné vers le stockage ponctuellement. Le liquide dans le stockage provenant du camion a une pureté de 99,5% mol . Le liquide 121 peut être plus pur, aussi pur ou moins pur que le liquide provenant du camion-citerne.61 .  Most of the liquid in the storage comes from a tanker 61 or from the apparatus itself by the flow 21, which can be diverted to storage punctually. The liquid in the storage from the truck has a purity of 99.5 mol%. The liquid 121 may be purer, as pure or less pure than the liquid from the tanker truck.61.
L'envoi de ce liquide pur 121 au stockage 31 par la conduite 33 ne risque pas de perturber la pureté du liquide dans le stockage.  The sending of this pure liquid 121 to the storage 31 by the pipe 33 does not risk to disturb the purity of the liquid in the storage.
Par contre, il peut être envisagé d'envoyer également au stockage en cas d'arrêt de la colonne, les liquides accumulés en cuve de la colonne basse pression et/ou moyenne pression dans les conduites 21 et 51 . Ces liquides auront évidemment une pureté inférieure à celle du liquide provenant du camion 61 ou celle du liquide 121 . Dans certains cas, le client peut supporter à court terme une réduction de pureté du liquide vaporisé dans le vaporiseur de secours. Une vanne 41 permet de régler les débits de ces liquides accumulés envoyés au stockage 31 .  On the other hand, it may be envisaged also to send to the storage, in the event of the column being stopped, the liquids accumulated in the bottom of the low pressure and / or medium pressure column in the lines 21 and 51. These liquids will obviously have a purity lower than that of the liquid from the truck 61 or that of the liquid 121. In some cases, the customer can withstand a short-term reduction of purity of the vaporized liquid in the backup vaporizer. A valve 41 makes it possible to regulate the flow rates of these accumulated liquids sent to the storage 31.
Dans la Figure 2, un débit d'air comprimé et épuré 1 est refroidi dans un échangeur de chaleur 3 et divisé en deux. Un débit 7 est soutiré de l'échangeur à un niveau intermédiaire, détendu dans une turbine 9 et envoyé à une colonne basse pression 13 d'une double colonne sous forme gazeuse. Un autre débit 5 se refroidit dans l'échangeur de chaleur 3, et envoyé à la colonne moyenne pression 13. In Figure 2, a flow of compressed and purified air 1 is cooled in a heat exchanger 3 and divided into two. A flow 7 is withdrawn from the exchanger at an intermediate level, expanded in a turbine 9 and sent to a low pressure column 13 of a double column in gaseous form. Another flow 5 is cooled in the heat exchanger 3, and sent to the medium pressure column 13.
Des débits enrichis en azote et en oxygène sont envoyés de la colonne moyenne pression à la colonne basse pression de manière connue. En cuve de la colonne basse pression 15, l'oxygène liquide s'accumule autour du rebouilleur 17. Un débit d'oxygène gazeux 19 contenant 98% d'oxygène est soutiré de la cuve de la colonne basse pression 15 et se réchauffe dans l'échangeur 3 comme débit 27 d'oxygène basse pression avant de subir une éventuelle compression . Un débit de purge 21 contenant des impuretés est soutiré de la cuve de la colonne 15 en permanence pour éviter l'accumulation d'impuretés en cuve de colonne. Ce soutirage liquide constitue le seul soutirage riche en oxygène du système de colonne. Une première conduite relie la cuve de colonne BP avec le stockage 31 pour y amener le liquide de purge 21 en permanence (soit en continu, soit par batch réguliers), sauf si le système de colonnes ne fonctionne pas. Le stockage 31 alimente un vaporiseur de secours 37 avec de l'oxygène liquide 35.  Flow rates enriched with nitrogen and oxygen are sent from the medium pressure column to the low pressure column in a known manner. In the tank of the low pressure column 15, the liquid oxygen accumulates around the reboiler 17. A flow of gaseous oxygen 19 containing 98% of oxygen is withdrawn from the tank of the low pressure column 15 and is heated in the exchanger 3 as flow 27 low pressure oxygen before undergoing a possible compression. A purge flow 21 containing impurities is withdrawn from the tank of the column 15 continuously to avoid the accumulation of impurities in the bottom of the column. This liquid withdrawal is the only oxygen-rich withdrawal of the column system. A first conduit connects the LP column vessel with the storage 31 to bring the purge liquid 21 continuously (either continuously or in regular batches), unless the column system does not work. The storage 31 supplies a backup vaporizer 37 with liquid oxygen 35.
L'oxygène est vaporisé dans le vaporiseur de secours 37 en grande quantité, quand les besoins du client sont particulièrement élevés ou quand l'appareil de séparation d'air ne fonctionne pas à plein régime, en cas de panne par exemple.  Oxygen is vaporized in the emergency vaporizer 37 in large quantities, when the customer's needs are particularly high or when the air separation device does not operate at full speed, in case of failure, for example.
Par contre, pendant les périodes où les besoins du client ne sont pas particulièrement élevés et l'appareil de séparation d'air fonctionne normalement, un débit liquide riche en oxygène constituant moins de 2% du débit nominal d'oxygène gazeux 19 et de préférence environ 1 % du débit nominal est envoyé vers le stockage. Ce débit liquide est envoyé au vaporiseur de secours si le niveau dans le stockage dépasse un seuil, ce seuil étant ordinairement celu i de la capacité maximale du stockage 31 . Ainsi ce débit envoyé au vaporiseur de secours constitue le trop-plein du stockage 31 . L'oxygène vaporisé est envoyé au client  On the other hand, during periods when the customer's needs are not particularly high and the air separation apparatus is operating normally, an oxygen-rich liquid flow constituting less than 2% of the nominal oxygen gas flow rate 19 and preferably about 1% of the nominal flow is sent to the storage. This liquid flow rate is sent to the backup vaporizer if the level in the storage exceeds a threshold, this threshold being ordinarily that of the maximum capacity of the storage 31. Thus this flow sent to the backup vaporizer constitutes the overflow of the storage 31. Vaporized oxygen is sent to the customer
Ceci permet de récupérer les molécules de la purge dans le liquide 21 , et donc de réduire la production totale de l'appareil (gain d'énergie de 1 % à 2% environ maximum).  This makes it possible to recover the molecules of the purge in the liquid 21, and thus to reduce the total production of the apparatus (energy gain from 1% to about 2% maximum).
Si le niveau du stockage 31 est en dessous du seuil, en particulier quand le stockage n'est pas plein, on remplit le stockage 31 en y envoyant le liquide 21 . En fonctionnement normal donc, le liquide du stockage n'est pas envoyé au vaporiseur de secours, si le niveau maximal n'est pas atteint. Or le déclenchement de l'envoi du stockage vers le vaporiseur de secours peut être nécessaire, en cas de réduction de production du système de colonnes ou augmentation des besoins du client. If the level of the storage 31 is below the threshold, in particular when the storage is not full, the storage 31 is filled by sending the liquid 21. In normal operation therefore, the storage liquid is not sent to the backup vaporizer, if the maximum level is not reached. However, the triggering of the sending of the storage to the backup vaporizer may be necessary, in the event of a reduction in the production of the column system or an increase in the customer's needs.
Le débit de purge 21 a une pureté molaire en oxygène supérieur à celle du débit 19.  The purge flow 21 has a higher oxygen molar purity than the flow rate 19.
La plupart du liquide dans le stockage provient d'un camion-citerne 61 ou de l'appareil lui-même par un débit liquide soutiré ponctuellement (non-illustré), qui peut être envoyé vers le stockage. Le liquide dans le stockage provenant du camion a une pureté de 99,5% mol. Une pompe sera peut-être nécessaire pour envoyer le liquide de purge 21 vers le stockage.  Most of the liquid in the storage comes from a tank truck 61 or the device itself by a liquid flow drawn off punctually (not shown), which can be sent to storage. The liquid in the storage from the truck has a purity of 99.5 mol%. A pump may be needed to send the purge liquid 21 to the storage.
Le débit de purge 21 peut être plus pur, aussi pur ou moins pur que le liquide alimentant le stockage provenant du camion-citerne 61 par exemple.  The purge flow 21 may be purer, as pure or less pure than the liquid supplying the storage from the tanker 61 for example.
Le liquide du stockage 31 peut être vaporisé dans un vaporiseur de secours 37 et envoyé à un client en cas de panne de l'appareil de distillation et/ou si la production de l'appareil de distillation est insuffisante pour fournir le client.  The liquid from the storage 31 can be vaporized in a backup vaporizer 37 and sent to a customer in case of failure of the distillation apparatus and / or if production of the distillation apparatus is insufficient to supply the customer.
Pour le cas où le système de colonnes s'arrêterait, il peut être envisagé d'envoyer également au stockage 31 des liquides accumulés dans les cuves de colonnes lors de l'arrêt. Dans le cas de la Figure 2, il s'agit d'une colonne basse pression et d'une colonne moyenne pression mais il sera aisément compris que l'invention s'applique au cas où les liquides accumulés envoyés au stockage peuvent provenir d'une colonne argon, une colonne à pression intermédiaire ou une colonne de mélange. Ce soutirage d'un liquide accumulé en cours d'arrêt d'une colonne argon, une colonne à pression intermédiaire ou une colonne de mélange s'applique également au cas de la Figure 1 .  For the case where the column system would stop, it can be envisaged to also send to the storage 31 of the liquids accumulated in the column tanks during the shutdown. In the case of Figure 2, it is a low pressure column and a medium pressure column but it will be easily understood that the invention applies to the case where accumulated liquids sent to storage can come from an argon column, an intermediate pressure column or a mixing column. This withdrawal of a liquid accumulated while stopping an argon column, an intermediate pressure column or a mixing column also applies to the case of FIG.
Dans le cas où ces liquides impurs sont envoyés des cuves de colonnes jusqu'au stockage pendant l'arrêt d'une colonne, il est nécessaire parfois de régler l'envoi de liquide dans le stockage en fonction du niveau de liquide dans le stockage. Un tel réglage n'est pas nécessaire pour le cas où les liquides envoyés au stockage sont uniquement des liquides de purge permanents très purs. L'essentiel est de régler l'envoi de liquide de purge très purs (ou éventuellement d'un mélange de liquide de purge très purs et liquides accumulés moins pur) de sorte que le liquide envoyé au vaporiseur de secours ait une pureté au-dessus d'un seuil acceptable pour le client. In the case where these impure liquids are sent from the column tanks to storage during the shutdown of a column, it is sometimes necessary to adjust the delivery of liquid in the storage depending on the level of liquid in the storage. Such an adjustment is not necessary for the case where the liquids sent to the storage are only very pure permanent purge liquids. The main thing is to regulate the sending of very pure purge liquid (or possibly a mixture of pure purge liquid and liquid accumulated less pure) so that the liquid sent to the emergency vaporizer has a purity above a threshold acceptable to the client.

Claims

REVENDICATIONS
1 . Procédé de séparation d'air par distillation cryogénique pour fournir un produit gazeux, éventuellement sous pression, dans lequel 1. Process for the separation of air by cryogenic distillation to provide a gaseous product, possibly under pressure, in which
a) on envoie de l'air refroidi, épuré et comprimé dans un système de colonnes comprenant une colonne moyenne pression (13) et une colonne basse pression (15)  a) cooling, purified and compressed air is supplied to a column system comprising a medium pressure column (13) and a low pressure column (15)
b) i) on soutire de la colonne basse pression un débit de gaz riche en oxygène (19) ayant un débit nominal pour former un produit gazeux et on soutire un débit de purge liquide (21 ) riche en oxygène en cuve de la colonne basse pression, le débit de purge étant plus riche en oxygène et en impuretés lourdes que le débit ayant le débit nominal et constituant au plus 2% du débit nominal de production du débit riche en oxygène ou  b) i) withdrawing from the low pressure column a flow of oxygen-rich gas (19) having a nominal flow rate to form a gaseous product and withdrawing an oxygen-rich liquid purge flow (21) in the bottom column of the column pressure, the purge flow being richer in oxygen and heavy impurities than the flow rate having the nominal flow and constituting at most 2% of the nominal flow rate of production of oxygen-rich flow or
ii) on soutire de la colonne basse pression un débit de liquide riche en oxygène (19) ayant un débit nominal, on le vaporise dans un vaporiseur principal (24) pour former un produit gazeux et on soutire un débit de purge liquide riche en oxygène (121 ) constituant au plus 2% du débit nominal de production du débit riche en oxygène du vaporiseur,  ii) a flow of oxygen-rich liquid (19) having a nominal flow rate is withdrawn from the low-pressure column, vaporized in a main evaporator (24) to form a gaseous product and an oxygen-rich liquid purge flow is withdrawn; (121) constituting not more than 2% of the rated flow rate of the oxygen-rich flow of the vaporizer,
c) on envoie le débit de purge liquide riche en oxygène (21 , 121 ) dans un stockage (31 ),  c) the oxygen-rich liquid purge flow (21, 121) is sent to a storage (31),
d) si le niveau de liquide dans le stockage dépasse un seuil correspondant à la capacité maximale du stockage, on soutire un débit liquide du stockage constituant au plus 2% du débit nominal de production du débit riche en oxygène et on l'envoie au vaporiseur de secours pour constituer une partie du produit gazeux et  d) if the liquid level in the storage exceeds a threshold corresponding to the maximum storage capacity, a liquid flow from the storage constituting not more than 2% of the nominal output flow rate of the oxygen-rich flow is withdrawn and sent to the vaporizer relief to form part of the gaseous product and
e) si le niveau de liquide dans le stockage est en dessous du seuil, on envoie le débit de purge liquide au stockage mais on n'envoie du liquide du stockage au vaporiseur de secours qu'en cas de réduction de production du système de colonnes ou d'augmentation du besoin d'un client pour le produit gazeux.  e) if the liquid level in the storage is below the threshold, the liquid purge flow is sent to the storage but the liquid is sent from the storage to the backup vaporizer only in the case of a reduction in the production of the column system or increasing a customer's need for the gaseous product.
2. Procédé selon la revendication 1 dans lequel on envoie le débit de purge liquide riche en oxygène de la cuve de la colonne basse pression (15) ou du vaporiseur (24) dans le stockage en permanence ou épisodiquement, en dehors de périodes d'arrêt et de démarrage du système de colonnes. 2. Process according to claim 1, in which the oxygen-rich liquid purge flow rate from the tank of the low-pressure column (15) or the vaporizer (24) is sent into the storage system permanently or episodically, outside periods of time. Stopping and starting the column system.
3. Procédé selon la revendication 1 ou 2 dans lequel lors d'un arrêt du système de colonne, le débit de purge n'est pas envoyé au stockage. 3. Method according to claim 1 or 2 wherein during a judgment of the column system, the purge flow is not sent to the storage.
4. Procédé selon l'une des revendications précédentes dans lequel le débit ayant un débit nominal est un débit de gaz soutiré de la colonne basse pression (15) et le débit de purge constitue le seul débit riche en oxygène soutiré du système de colonnes. 4. Method according to one of the preceding claims wherein the flow rate having a nominal flow rate is a flow of gas withdrawn from the low pressure column (15) and the purge flow is the only oxygen-rich flow withdrawn from the column system.
5. Procédé selon l'une des revendications précédentes dans lequel lors d'un arrêt du système de colonnes, on remplit le stockage (31 ) au moyen de liquide provenant d'une cuve d'au moins une colonne (13, 15) du système de colonnes. 5. Method according to one of the preceding claims wherein during a judgment of the column system, filling the storage (31) with liquid from a tank of at least one column (13, 15) of the column system.
6. Procédé selon l'une des revendications précédentes dans lequel on soutire de la colonne basse pression un débit de gaz riche en oxygène (19) ayant un débit nominal pour former un produit gazeux et on soutire un débit de purge liquide (21 ) riche en oxygène en cuve de la colonne basse pression, le débit de purge étant plus riche en oxygène et en impuretés lourdes que le débit ayant le débit nominal et constituant au plus 2% du débit nominal de production du débit riche en oxygène. 6. Method according to one of the preceding claims wherein is withdrawn from the low pressure column a flow of oxygen-rich gas (19) having a nominal flow rate to form a gaseous product and a rich liquid purge flow (21) is withdrawn tank oxygen in the low pressure column, the purge flow being richer in oxygen and heavy impurities than the flow rate having the nominal flow and constituting at most 2% of the nominal rate of production of oxygen-rich flow.
7. Procédé selon l'une des revendications 1 à 5 dans lequel on soutire de la colonne basse pression un débit de liquide riche en oxygène (19) ayant un débit nominal, on le vaporise dans un vaporiseur principal (24) pour former un produit gazeux et on soutire un débit de purge liquide riche en oxygène (121 ) constituant au plus 2% du débit nominal de production du débit riche en oxygène du vaporiseur. 7. Method according to one of claims 1 to 5 wherein is withdrawn from the low pressure column a flow of oxygen-rich liquid (19) having a nominal flow, it is vaporized in a main vaporizer (24) to form a product gaseous and an oxygen-rich liquid purge flow (121) is withdrawn constituting at most 2% of the nominal flow rate for producing the oxygen-rich flow rate of the vaporizer.
8. Appareil de séparation d'air par distillation cryogénique comprenant un système de colonnes comprenant une colonne moyenne pression (13) et une colonne basse pression (15), un stockage (31 ), un vaporiseur de secours (37), et soit i) des moyens pour soutirer de la colonne basse pression un débit de gaz riche en oxygène (19) ayant un débit nominal pour former un produit gazeux et des moyens pour soutirer un débit de purge liquide (21 ) riche en oxygène en cuve de la colonne basse pression, le débit de purge étant plus riche en oxygène et en impuretés lourdes que le débit ayant le débit nominal et constituant au pl us 2% d u débit nom inal de production du débit riche en oxygène ou A cryogenic distillation air separation apparatus comprising a column system comprising a medium pressure column (13) and a low pressure column (15), a storage (31), a backup vaporizer (37), and either i) means for withdrawing from the low pressure column a flow of oxygen-rich gas (19) having a nominal flow rate to form a gaseous product and means for withdrawing an oxygen-rich liquid purge flow (21) in the tank of the low pressure column, the purge flow being richer in oxygen and heavy impurities than the flow rate having the nominal flow and constituting at most 2% of the nominal flow rate of production of oxygen-rich flow or
ii) un vaporiseur principal (24), des moyens pour soutirer de la colonne basse pression un débit de liquide riche en oxygène (19) ayant un débit nominal et de l'envoyer au vaporiseur principal, des moyens pour soutirer un produit gazeux formé par vaporisation du débit de liquide, des moyens pour soutirer un débit de purge liquide riche en oxygène (1 21 ) constituant au plus 2% du débit nominal de production du débit riche en oxygène du vaporiseur,  ii) a main vaporizer (24), means for withdrawing from the low pressure column a flow of oxygen-rich liquid (19) having a nominal flow rate and sending it to the main vaporizer, means for withdrawing a gaseous product formed by vaporization of the liquid flow, means for withdrawing an oxygen-rich liquid purge flow (1 21) constituting at most 2% of the nominal flow rate for producing the oxygen-rich flow of the vaporizer,
et des moyens pour envoyer le débit de purge liquide riche en oxygène (21 , 121 ) au stockage (31 ), des moyens de détection et de commande pour détecter le n iveau de liqu ide dans le stockage et pour déclencher, un iquement si le niveau dépasse un seuil correspondant à la capacité maximale du stockage, le soutirage un débit liquide du stockage constituant au plus 2% du débit nominal de production du débit riche en oxygène et l'envoi de ce débit au vaporiseur de secours pour constituer une partie du produit gazeux, ces moyens de détection et de commande pouvant détecter si le niveau de liquide dans le stockage est en dessous du seuil et, pour déclencher dans ce cas, l'envoi du débit de purge l iqu ide au stockage et l'empêchement de l'envoi du liquide du stockage au vaporiseur de secours sauf cas de réduction de production du système de colonnes ou d'augmentation du besoin d'un client pour le produit gazeux. and means for sending the oxygen-rich liquid purge flow (21, 121) to the storage (31), sensing and control means for detecting the liquor level in the storage and for triggering, only if the level exceeds a threshold corresponding to the maximum capacity of the storage, the withdrawal a liquid flow from the storage constituting not more than 2% of the nominal rate of production of oxygen-rich flow and the sending of this flow to the backup vaporizer to form part of the gaseous product, these detection and control means being able to detect if the liquid level in the storage is below the threshold and, to trigger in this case, the sending of the purge flow rate to the storage and the prevention of sending the liquid from the storage to the backup vaporizer except in the case of reducing the production of the column system or increasing the need of a customer for the gaseous product.
9. Appareil selon la revendication 8 ne comprenant pas de moyen de vaporisation de liquide de purge à part le vaporiseur de secours (37). 9. Apparatus according to claim 8 not including purge liquid vaporization means apart from the emergency vaporizer (37).
10. Appareil selon la revendication 8 ou 9 comprenant des moyens pour soutirer de la colonne basse pression un débit de gaz riche en oxygène (19) ayant un débit nominal pour former un produit gazeux et des moyens pour soutirer un débit de purge liquide (21 ) riche en oxygène en cuve de la colonne basse pression, le débit de purge étant plus riche en oxygène et en impuretés lourdes que le débit ayant le débit nominal et constituant au plus 2% du débit nominal de production du débit riche en oxygène. An apparatus according to claim 8 or 9 including means for withdrawing from the low pressure column a flow of oxygen-rich gas (19) having a nominal flow rate to form a gaseous product and means for drawing a liquid purge flow rate (21). ) rich in oxygen in the tank of the low pressure column, the purge flow being richer in oxygen and impurities heavy than the flow rate having the nominal flow rate and constituting not more than 2% of the nominal output flow of the oxygen-rich flow.
1 1 . Appareil selon la revendication 8 ou 9 comprenant un vaporiseur principal (24), des moyens pour soutirer de la colonne basse pression un débit de liquide riche en oxygène (19) ayant un débit nominal et de l'envoyer au vaporiseur principal, des moyens pour soutirer un produit gazeux formé par vaporisation du débit de liquide et des moyens pour soutirer un débit de purge l iquide riche en oxygène (121 ) constituant au plus 2% du débit nominal de production du débit riche en oxygène du vaporiseur. 1 1. Apparatus according to claim 8 or 9 comprising a main vaporizer (24), means for withdrawing a flow of oxygen-rich liquid (19) from the low pressure column having a nominal flow rate and sending it to the main vaporizer, means for withdrawing a gaseous product formed by vaporization of the liquid flow and means for withdrawing a purge flow oxygen-rich liquid (121) constituting at most 2% of the nominal rate of production of oxygen-rich flow of the vaporizer.
12. Appareil selon l'une des revendications 8 à 1 1 comprenant des moyens pour alimenter le stockage par un liquide d'une source extérieure. 12. Apparatus according to one of claims 8 to 11 comprising means for supplying the storage with a liquid from an external source.
13. Appareil selon l'une des revendications 8 à 12 comprenant des moyens pour envoyer un liquide de cuve de la colonne basse pression au stockage. 13. Apparatus according to one of claims 8 to 12 comprising means for sending a liquid tank from the low pressure column storage.
14. Appareil selon l'une des revendications 8 à 13 comprenant des moyens pour envoyer un liquide de cuve de la colonne moyenne pression au stockage. 14. Apparatus according to one of claims 8 to 13 comprising means for sending a liquid tank from the medium pressure column storage.
EP11728894.4A 2010-07-05 2011-07-05 Apparatus and process for separating air by cryogenic distillation Active EP2591301B1 (en)

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PL2986924T3 (en) * 2013-04-18 2017-12-29 Linde Aktiengesellschaft Retrofit device for the cryogenic separation of air, retrofit installation and method for retrofitting a low-temperature air separator facility
FR3084736B1 (en) * 2018-08-01 2022-04-15 Air Liquide METHOD AND APPARATUS FOR PRODUCTION OF ARGON BY CRYOGENIC AIR DISTILLATION
DE102019000335A1 (en) 2019-01-18 2020-07-23 Linde Aktiengesellschaft Process for providing air products and air separation plant
FR3095153B1 (en) * 2019-04-18 2021-11-26 Air Liquide France Ind Process for supplying cryogenic fluid to a machining machine

Family Cites Families (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2125949B (en) * 1982-08-24 1985-09-11 Air Prod & Chem Plant for producing gaseous oxygen
DE3913880A1 (en) * 1989-04-27 1990-10-31 Linde Ag METHOD AND DEVICE FOR DEEP TEMPERATURE DISPOSAL OF AIR
FR2652887B1 (en) * 1989-10-09 1993-12-24 Air Liquide PROCESS AND PLANT FOR THE PRODUCTION OF VARIABLE FLOW GAS OXYGEN BY AIR DISTILLATION.
FR2699992B1 (en) * 1992-12-30 1995-02-10 Air Liquide Process and installation for producing gaseous oxygen under pressure.
FR2706195B1 (en) * 1993-06-07 1995-07-28 Air Liquide Method and unit for supplying pressurized gas to an installation consuming an air component.
EP0793069A1 (en) * 1996-03-01 1997-09-03 Air Products And Chemicals, Inc. Dual purity oxygen generator with reboiler compressor
FR2751737B1 (en) * 1996-07-25 1998-09-11 Air Liquide METHOD AND INSTALLATION FOR PRODUCING A VARIABLE FLOW AIR GAS
JPH10132458A (en) * 1996-10-28 1998-05-22 Nippon Sanso Kk Method and equipment for producing oxygen gas
US5907959A (en) * 1998-01-22 1999-06-01 Air Products And Chemicals, Inc. Air separation process using warm and cold expanders
DK1051588T3 (en) * 1998-01-30 2002-07-01 Linde Ag Process and device for evaporating liquid oxygen
US6345517B1 (en) * 1998-02-04 2002-02-12 Texaco Inc. Combined cryogenic air separation with integrated gasifier
US6272884B1 (en) * 1998-04-08 2001-08-14 Praxair Technology, Inc. Rapid restart system for cryogenic air separation plant
DE19852020A1 (en) * 1998-08-06 2000-02-10 Linde Ag Method and device for the low-temperature separation of air
US6182471B1 (en) * 1999-06-28 2001-02-06 Praxair Technology, Inc. Cryogenic rectification system for producing oxygen product at a non-constant rate
US6357258B1 (en) * 2000-09-08 2002-03-19 Praxair Technology, Inc. Cryogenic air separation system with integrated booster and multicomponent refrigeration compression
EP1202012B1 (en) * 2000-10-30 2005-12-07 L'AIR LIQUIDE, Société Anonyme à Directoire et Conseil de Surveillance pour l'Etude et l'Exploitation des Process and installation for cryogenic air separation integrated with an associated process
FR2853407B1 (en) * 2003-04-02 2012-12-14 Air Liquide METHOD AND INSTALLATION FOR SUPPLYING GAS UNDER PRESSURE
FR2872262B1 (en) * 2004-06-29 2010-11-26 Air Liquide METHOD AND INSTALLATION FOR PROVIDING SUPPORT OF A PRESSURIZED GAS
US7409835B2 (en) * 2004-07-14 2008-08-12 Air Liquide Process & Construction, Inc. Backup system and method for production of pressurized gas
AU2005225027A1 (en) 2005-07-21 2007-02-08 L'air Liquide Societe Anonyme Pour L'etude Et L"Exploitation Des Procedes Georges Claude Process and apparatus for the separation of air by cryogenic distillation
US20110214453A1 (en) 2008-08-14 2011-09-08 Linde Aktiengesellschaft Process and device for cryogenic air fractionation

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WO2012004241A3 (en) 2013-11-28
EP2591301B1 (en) 2020-09-02
US20130098106A1 (en) 2013-04-25
ES2820436T3 (en) 2021-04-21
WO2012004242A3 (en) 2013-11-28
US9581386B2 (en) 2017-02-28
WO2012004241A2 (en) 2012-01-12
CN103282733A (en) 2013-09-04
EP2591300A2 (en) 2013-05-15
CN103282733B (en) 2015-11-25
CN103282732B (en) 2016-08-03
WO2012004242A2 (en) 2012-01-12

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