EP0768502A1 - Verfahren und Vorrichtung zur Verflüssigung und Behandlung von Erdgas - Google Patents

Verfahren und Vorrichtung zur Verflüssigung und Behandlung von Erdgas Download PDF

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Publication number
EP0768502A1
EP0768502A1 EP96402006A EP96402006A EP0768502A1 EP 0768502 A1 EP0768502 A1 EP 0768502A1 EP 96402006 A EP96402006 A EP 96402006A EP 96402006 A EP96402006 A EP 96402006A EP 0768502 A1 EP0768502 A1 EP 0768502A1
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EP
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Prior art keywords
refrigeration
gas
exchanger
liquid
fraction
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EP96402006A
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English (en)
French (fr)
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EP0768502B1 (de
Inventor
Pierre Capron
Alexandre Rojey
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IFP Energies Nouvelles IFPEN
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IFP Energies Nouvelles IFPEN
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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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0279—Compression of refrigerant or internal recycle fluid, e.g. kind of compressor, accumulator, suction drum etc.
    • F25J1/0292—Refrigerant compression by cold or cryogenic suction of the refrigerant 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0022—Hydrocarbons, e.g. natural 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/0035—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by gas expansion with extraction of work
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/004—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by flash gas recovery
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/0042—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by liquid expansion with extraction of work
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0047—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle
    • F25J1/0052—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle by vaporising a liquid refrigerant 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0047—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle
    • F25J1/0052—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle by vaporising a liquid refrigerant stream
    • F25J1/0055—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle by vaporising a liquid refrigerant stream originating from an incorporated cascade
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0211—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle
    • F25J1/0212—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle as a single flow MCR cycle
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0211—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle
    • F25J1/0214—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle as a dual level refrigeration cascade with at least one MCR cycle
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0211—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle
    • F25J1/0219—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle in combination with an internal quasi-closed refrigeration loop, e.g. using a deep flash recycle loop
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0257—Construction and layout of liquefaction equipments, e.g. valves, machines
    • F25J1/0262—Details of the cold heat exchange system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • F25J5/002—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger
    • F25J5/007—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger combined with mass exchange, i.e. in a so-called dephlegmator
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/80—Processes or apparatus using separation by rectification using integrated mass and heat exchange, i.e. non-adiabatic rectification in a reflux exchanger or dephlegmator
    • 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
    • F25J2205/50—Processes or apparatus using other separation and/or other processing means using absorption, i.e. with selective solvents or lean oil, heavier CnHm and including generally a regeneration step for the solvent or lean oil
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/60—Separating impurities from natural gas, e.g. mercury, cyclic hydrocarbons
    • F25J2220/64—Separating heavy hydrocarbons, e.g. NGL, LPG, C4+ hydrocarbons or heavy condensates in general
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/60—Separating impurities from natural gas, e.g. mercury, cyclic hydrocarbons
    • F25J2220/68—Separating water or hydrates
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/60—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being hydrocarbons or a mixture of hydrocarbons
    • 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
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass 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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/44—Particular materials used, e.g. copper, steel or alloys thereof or surface treatments used, e.g. enhanced surface

Definitions

  • the present invention relates to a process for liquefying and fractionating a fluid or a gaseous mixture formed at least in part from hydrocarbons, in particular a natural gas.
  • Natural gas is commonly produced at sites far from places of use and it is common to liquefy it in order to transport it over long distances by LNG carrier or to store it in liquid form.
  • the method according to the invention makes it possible to increase the production yield of separate constituents, for example C3 + hydrocarbons.
  • the ascending gas phase is contacted, for example, with a descending liquid hydrocarbon fraction.
  • the refrigeration operated during the pre-refrigeration stage can be ensured by an heat exchange at least partly continuous and countercurrent over at least part of the zone where the phases are brought into contact.
  • At least two liquid fractions having different compositions at different levels are taken, for example.
  • the pre-refrigeration step and the final liquefaction step are carried out by means of two different refrigeration cycles, each of the cycles operating with its own refrigerant mixture, the refrigerant mixture used during the final liquefaction step being, for example, partially condensed during the pre-refrigeration step.
  • the pre-refrigeration step and the final liquefaction step are refrigerated by means of a single refrigeration cycle operating with a refrigerant mixture.
  • the pre-cooling step is carried out in the presence of a solvent.
  • the solvent is for example injected into the gas.
  • the method according to the invention applies particularly well to the liquefaction of a natural gas, or also to obtain a refrigerant mixture ensuring liquefaction of a natural gas obtained at least in part by vaporization of at least one liquid fraction of a mixture of hydrocarbons resulting from the implementation of the process according to the invention.
  • the present invention also relates to an installation for the liquefaction of a fluid such as a gas formed at least in part from a mixture of hydrocarbons.
  • the fluid to be treated for example natural gas
  • the fluid to be treated is liquefied.
  • the refrigeration device comprises at least one means for withdrawing said liquid hydrocarbon fractions.
  • the installation comprises, for example, means for stabilizing said liquid hydrocarbon fractions, said stabilization means being connected to said withdrawal means.
  • the pre-refrigeration device may include at least one injection means, allowing the injection of a fluid other than gas.
  • the fluid can be a solvent sent into the gas to treat it, the solvent can also be chosen to be used as a separating agent.
  • the pre-refrigeration device comprises, for example, a vertical plate exchanger in which contact is made between the fluid or gas to be treated in ascending circulation and a liquid fraction descending by gravity.
  • the installation may include a pre-refrigeration device comprising a brazed aluminum plate exchanger and a final liquefaction device comprising a stainless steel plate exchanger.
  • FIG. 1 The schematic diagram of a process used in the prior art for liquefying a natural gas is briefly recalled in FIG. 1.
  • the liquefaction process includes a pre-refrigeration cycle which partially condenses the heaviest hydrocarbons contained in natural gas and in the mixture used in the main refrigeration cycle. These two cycles use a mixture of fluid as a refrigerant which, when vaporized, liquefies natural gas under pressure. After vaporization, the mixture is compressed, condensed by exchanging heat with the ambient medium, such as water or air available and recycled.
  • the two-phase mixture is introduced into a separation unit from which there emerge on the one hand a gaseous fraction depleted in heavy hydrocarbons, that is to say essentially composed of methane and / or nitrogen and on the other hand one or more liquid sections of higher molecular weight. These liquid sections or fractions can be made as narrow as necessary by passing them through a series of fractionation columns.
  • the gaseous fraction is sent to a final refrigeration stage to be liquefied.
  • the principle implemented in the invention described below consists in carrying out the pre-refrigeration of a natural gas by simultaneously causing the condensation of a liquid fraction of hydrocarbons and the contacting preferably against the current of the liquid fractions of hydrocarbons with gas.
  • condensation of the hydrocarbons and their contacting, preferably against the current with the gas, are advantageously carried out during an indirect heat exchange operation.
  • FIG. 2A The principle of the process is illustrated in FIG. 2A and applied by way of example to a natural gas containing hydrocarbons other than methane and in particular C 3 + hydrocarbons.
  • the gas to be treated is introduced into an enclosure EC1, such as a heat exchanger, through the conduit 2 located in its lower part.
  • Refrigeration of natural gas causes condensation of heavy hydrocarbons contained in the gas.
  • the condensed hydrocarbon liquid phase (s) descend into the exchanger by gravity, against the flow of the treated gas which progressively becomes depleted in propane, butane and heavy hydrocarbons due to the exchange of material.
  • the condensed hydrocarbon liquid phase is enriched progressively with heavier constituents.
  • the gas phase rich in methane and depleted in propane, butane and heavy hydrocarbons is evacuated through a pipe 5 at the head of the exchanger, and sent to a second refrigeration step or final liquefaction step shown diagrammatically in FIG. 2A by the reference L2.
  • the temperature variation or the temperature gradient caused in the exchanger are for example chosen according to the nature of the gas and, the quantity of condensed hydrocarbons, such as LPG and gasoline, to be recovered.
  • the reduction in temperature of the gas to be treated is preferably carried out in order to obtain a temperature gradient over the whole of the exchanger.
  • the two refrigeration steps are carried out by means of two independent refrigeration cycles.
  • the final liquefaction stage is carried out, for example as follows: the natural gas which leaves the exchanger EC1 via the conduit 5 is sent to the exchanger E2 in which it is liquefied and then to the exchanger E3 in which it is sub-cooled. It emerges from the exchanger E3 through the conduit 50 and it is expanded through the expansion valve V100 to form the LNG produced. Refrigeration in exchangers E2 and E3 is ensured, for example, by means of a refrigerant mixture which is compressed by means of compressor K2, cooled by means of water or cooling air in exchangers C2 and C3.
  • the refrigerant mixture is sent to the exchanger EC 1 through the line 100 and comes out partially condensed through the line 101.
  • the liquid and vapor phases are separated in the phase separator S100.
  • the liquid refrigerant mixture from the separator S100 is sent through the conduit 102 into the exchanger E2 in which it is sub-cooled, and expanded through the expansion valve V300.
  • the vapor refrigerant mixture from the separator S100 is sent via the pipe 103 in the exchanger E2 in which it is liquefied.
  • the liquid refrigerant mixture thus obtained is sent through the conduit 104 from the exchanger E2 to the exchanger E3 in which it is sub-cooled before being expanded through the expansion valve V200 and re-sent, after expansion, by the conduit 105 in the exchanger E3. Its at least partial vaporization in the exchanger E3 ensures the sub-cooling of the LNG before expansion and the sub-cooling of the refrigerant mixture.
  • the refrigeration cycle used during the pre-cooling step can implement different arrangements while remaining within the scope of the invention.
  • FIG. 2B shows a first example of an arrangement where the refrigerant mixture used during the pre-cooling step is condensed using water or cooling air in the exchanger C1.
  • the liquid refrigerant mixture thus obtained is sent via line 3 to the exchanger EC 1 in which it is sub-cooled. It is expanded at lower and lower pressure levels through the expansion valves V12, V11 and V10, the steam fractions obtained after each spraying being sent to the compressor K1 by the conduits 40, 41 and 42.
  • the compressor K1 is cooled by the exchanger C20 using water or cooling air. This arrangement makes it possible to reduce the compression power required, the maximum compression ratio of the compressor K1 applying only to the mixture fraction which provides refrigeration in the lowest temperature zone in the exchanger EC 1 .
  • the exchanger EC 1 comprises at least one means of recovery, for example a plate 7 delimiting, for example, two zones Z 1 and Z 2 .
  • This plateau communicates with the natural gas flow circuit (s) in each of the zones and with an evacuation duct 8 for the hydrocarbon fraction separated and recovered at the level of the plateau 7.
  • This hydrocarbon fraction enriched in propane and butane corresponds to the hydrocarbons which have condensed in zone Z2.
  • the liquid hydrocarbon phase not recovered at the level of the plate 7 is redistributed in the zone Z1 in order to flow downwardly towards the bottom of the exchanger.
  • the latter is for example provided with a conduit 9 located in its lower part to evacuate the gasoline fraction.
  • the exchanger can be equipped with several recovery trays distributed according, for example, to the nature of the cuts or hydrocarbons to be recovered, their volatility and / or the temperature prevailing at different places in the exchanger.
  • liquid hydrocarbon phases thus recovered are stabilized according to the methods described in FIGS. 4A, 4B and 4C.
  • a first embodiment not shown consists in using a means of heating the liquid volume collected at the bottom, for example an integrated reboiler B1 not shown in the figures in the lower part of the exchanger.
  • a means of heating the liquid volume collected at the bottom for example an integrated reboiler B1 not shown in the figures in the lower part of the exchanger.
  • the evacuation duct 8 communicating with the recovery plate 7 for the condensed LPGs of FIG. 3 is connected to a device 10 allowing their stabilization.
  • the additional stabilization process consists in sending, into the stabilization device 10, the fraction of condensate comprising methane and ethane in small quantity and formed mainly by an LPG fraction, recovered at the level of the plate 7.
  • the gaseous fraction rich in methane and ethane produced during stabilization is discharged through a conduit 11 and recycled to the exchanger EC 1 at the level of the plate 7 to be recovered and mixed with the gas to be treated.
  • the stabilized LPG fraction is removed at the bottom of the stabilization device at the reboiler 13 via a conduit 12.
  • Such a procedure advantageously makes it possible to stabilize the fraction rich in LPG before its recovery by the producer and thus to increase the production yield of methane and ethane.
  • FIG. 4B the installation described in FIG. 4A incorporates a second stabilization device 14, for the gasoline discharged through the conduit 9.
  • the operating diagram is identical to that described in relation to FIG. 4A, the condensate discharged through the conduit 9 comprising mainly gasoline is sent to the stabilization device 14.
  • the stabilized gasoline essentially composed of the C 5 + fraction, is evacuated through line 16 at the reboiler 17.
  • the gaseous fraction composed essentially of methane, ethane, propane and butane is evacuated from the device by line 15 to be recycled and remixed with the gas to be treated arriving through line 2.
  • FIG. 4C differs from that of FIG. 4A by the addition of two expansion valves V 1 and V 2 located respectively on the evacuation conduits 8 and 9.
  • the gas fractions from the stabilization devices 10 and 14 are recompressed through means such as compressors K 1 and K 2 before being returned by a pipe 16 to the gas to be treated at the pipe 2.
  • the stabilization of the various fractions advantageously makes it possible to increase the production yield of recoverable compounds such as the LPG fraction and the gasoline and on the other hand to be able to use them as constituents of a refrigerant fluid in the liquefaction process.
  • Natural gas is cooled to -15 ° C in the exchanger E1. It is then sent to the exchanger EC 1 through the conduit 3 'from which it emerges through the conduit 101 at -55 ° C. A liquid fraction is drawn off at the bottom through line 6 and an intermediate fraction richer in LPG is drawn off at -45 ° C through the line.
  • the top gas as well as the two withdrawn liquid fractions, have the following compositions (in molar%): Head gas Bottom liquid Intermediate sample liquid Methane 89.30 26.33 39.36 Nitrogen 4.32 0.36 0.51 Ethane 4.96 9.39 16.65 Propane 1.24 12.09 21.74 Isobutane 0.10 6.07 8.14 n-butane 0.06 15.28 13.20 Isopentane / 12.58 0.37 n-pentane / 10.30 / C 6 + / 7.60 /
  • the content of heavy hydrocarbons entrained in the gas would be much higher than in the process according to the invention.
  • the isopentane content would be of the order of 100 ppm instead of around 1 ppm with the method according to the invention. Similar differences are observed for the other heavy constituents contained in the gas.
  • the refrigeration of the first and second liquefaction stages of natural gas can be carried out independently or dependent on the examples given below by way of illustration only in FIGS. 5A, 5B and 5C.
  • FIG. 5A shows an alternative implementation of the method described above in FIG. 2A comprising an intermediate separation step and for which the two process refrigeration steps are carried out with independent refrigerant mixtures.
  • the gas is pre-refrigerated in the exchanger EC 1 and that of the final liquefaction stage producing liquefied natural gas (or LNG) with the same mixture of refrigerants .
  • the refrigerant mixture circulating in the cycle (K1, C1) is sent to a separator F in which it is separated into a vapor fraction containing the light fractions of the mixture and into a liquid fraction containing the heavy fractions.
  • the heavy fractions, condensed by refrigeration using for example water or cooling air, are discharged at the bottom of the separator F and sent by the conduits 51 and 3 to the exchanger EC 1 , to form a first refrigerant, after passing, for example, through the exchanger E1.
  • this first fluid ensures the precooling of the gas according to the method described for example in FIG. 2A in order to obtain at the head of the exchanger a gas purified mainly of heavy hydrocarbons and rich in methane . This gas is then sent to the final liquefaction stage.
  • the light fractions, coming from the separator F through the conduit 52 and forming a second refrigerant fluid are sent via the conduit 100 into the exchanger EC 1 .
  • This second fluid is at least partially condensed in the exchanger by heat exchange with the first fluid consisting of the heavy fractions previously described.
  • This second fluid is then sent via line 101 to the final liquefaction stage to obtain Liquefied Natural Gas (or LNG).
  • the second fluid is sent through line 4 "of the exchanger E2 of the final liquefaction cycle to line 4, to be mixed with the first fluid before being returned to the cycle (K1, C1) via line 4 ', after passing through the exchanger EC1.
  • FIG. 5C describes another embodiment according to the invention in which the gas pre-refrigeration is ensured at least in part by recycling a fraction of the gas purified from the heavy constituents, as well as by a first refrigerant mixture as described in Figure 2A.
  • the gas purified from heavy fractions is sent via line 5 to the final liquefaction stage L2 where it is first of all expanded in a turbine T1 according to a process for example described in detail in application FR 94 / 02 024 from the requestor before being sent to a separator F2.
  • the vapor fraction obtained is sent via a pipe 53 to a pipe 54 for introduction into the exchanger EC 1 .
  • the liquid fraction issuing from the bottom of the separator F2 via the conduit 56 is expanded in one or more turbines T6 before being sent to a second separator F3.
  • the LNG produced is obtained which is sent through the conduit 57, and a vapor fraction evacuated through the conduit 55 to a compression device K4. This recompressed steam fraction is then sent to line 53 to be mixed with the first fraction.
  • the mixture of the two fractions is then introduced at the head of the exchanger EC 1 through the conduit 54. It emerges at the bottom of the exchanger EC1, after having warmed up and thus having provided part of the pre-refrigeration of natural gas. It is sent through line 57, for example, in exchanger E1 where it is used as a refrigeration agent, and sent from this exchanger through line 59 to compressor K3 before being cooled in a condenser. At the outlet of the condenser, it is sent through the conduit 58 to be recycled with the gas to be treated.
  • the sealing of the refrigeration circuits is found to be imperfect, for example when the compression devices used are not completely sealed. It then becomes necessary to compensate for these losses of mixture, for example by making a refilling of refrigerant mixture.
  • this top-up is carried out using at least part of the fractioned and recovered hydrocarbon cuts according to the process described in FIG. 3, for example.
  • the natural gas is dehydrated at the same time as its fractionation.
  • the device of FIG. 2A is provided with at least one insertion conduit 20 preferably situated at the level of the head of the exchanger.
  • the condensed hydrocarbon liquid phase is enriched progressively with heavier constituents as it descends and the condensed aqueous phase rich in solvent at the top of the exchanger becomes depleted in solvent by contact with the gas.
  • the aqueous phase is discharged through line 7 and the liquid hydrocarbon phase through line 9.
  • the solvent vaporized and entrained in the gas phase makes it possible to avoid the problems of hydrate formation linked to cooling.
  • a solvent at least partially miscible with water is used.
  • it has a boiling point lower than that of water or forms with water an azeotrope whose boiling point is lower than that of water so as to be able to be entrained by the non-condensed gas. .
  • This solvent is for example an alcohol and preferably methanol. It can also be chosen from the following solvents: methylpropylether, ethylpropylether, dipropylether, methyltertiobutylether, dimethoxymethane, dimethoxyethane, ethanol, methoxyethanol, propanol or else be chosen from different classes of solvents such as for example amines or ketones or a mixture formed from one or more of these products.
  • the amount of solvent to be injected is usually adjusted according to the temperature, pressure and / or composition of the gas in order to avoid the formation of hydrates and the formation of ice crystals due to the presence of water. .
  • the ratio in moles of the flow rate of solvent to the flow rate of the treated gas is between 1/1000 and 1/10.
  • the treatment process is optimized by adapting the quantity of solvent injected as a function of a parameter relating to the gas, for example its temperature and / or its variation in temperature and / or its composition and / or its pressure and / or operating conditions. For this, account is taken, for example, of the temperature values and / or of the temperature gradient measured by the temperature sensors located at the level of the exchanger.
  • account is also taken of the operations then carried out on the treated gas coming from the enclosure.
  • the gas By counter-current circulation, the gas entrains the solvent contained in the liquid phases which descend by gravity. These liquid phases are collected at the bottom, substantially purified of solvent.
  • the solvent injected at the head is therefore mainly discharged into the gas phase leaving at the head. The quantity of solvent injected can thus be adjusted in order to obtain the level of concentration in this gas phase required to avoid the formation of hydrates, taking into account the conditions of temperature and pressure.
  • the solvent injected at the head is not necessarily pure and can be, for example, mixed with water, provided however that the concentration of solvent in aqueous phase makes it possible to avoid the formation of hydrates.
  • the injection of a solvent through line 20 also makes it possible to eliminate constituents other than water. It is possible, for example, to remove undesirable aromatic hydrocarbons capable of crystallizing by sending a solvent which selectively eliminates them.
  • the solvent can in this case be for example a polar solvent such as for example an ether. an alcohol, or a ketone.
  • FIG. 6B describes an embodiment allowing the injection of a separation agent, for example a solvent, through line 20.
  • a separation agent for example a solvent
  • the gas is initially refrigerated in an exchanger E1 before being sent to the exchanger EC1.
  • the conduit 20 for injecting the separating agent is located in the figure at the head of the exchanger but can also, without departing from the scope of the invention, be positioned at any level of the exchanger EC1.
  • FIGS. 6C and 6D describe two other embodiments of the method according to the invention where the refrigeration at least in one stage of the liquefaction cycle is carried out using a refrigerating agent obtained by implementing at least two stages of the method according to the invention.
  • FIG. 6C describes a first example of implementation of the method according to the invention during which the natural gas is refrigerated by means of two independent refrigeration cycles.
  • the refrigerant mixture used during the second refrigeration stage consists of methane, ethane, propane and nitrogen and sent under pressure in vapor phase via line 100 in the exchanger EC1 where it is cooled and partially condensed .
  • the liquid phase thus obtained descends by gravity and is simultaneously contacted against the current by the gaseous phase which circulates in an ascending direction.
  • a first liquid fraction enriched in propane is collected via the line 206. This liquid fraction is then refrigerated in the exchanger EC1 and sent through the conduit 204 in the exchanger E2 where it is cooled, expanded and vaporized to provide the required refrigeration in the exchanger E2.
  • a vapor fraction enriched in methane and nitrogen is collected via line 205 which is then sent to the exchanger E2 in which it is liquefied by forming a second liquid fraction.
  • This second liquid fraction is sub-cooled in the exchanger E3, expanded and vaporized to provide the required refrigeration in the exchanger E3.
  • the natural gas arriving through line 2 is cooled during a first step in the exchanger EC1. At the end of this first refrigeration step, a first liquid fraction is evacuated through line 8.
  • the gaseous fraction produced during this first step and leaving the exchanger EC1 by the conduit 5 is sent to the exchangers E2 and E3. It comes out liquefied from the exchanger E3 by the conduit 50 and after expansion through the valve V100, forms the LNG produced.
  • Refrigeration during the first stage is ensured for example by a refrigeration cycle operating with a mixture of fluids similar to that described in FIG. 2B.
  • FIG. 6D schematizes an example of implementation according to the invention where the refrigeration of natural gas is ensured by a single refrigeration cycle.
  • the refrigerant mixture consisting of methane, ethane, propane, butane, pentane and nitrogen is sent under pressure in the vapor phase to the condenser C1 from which it emerges partially condensed.
  • the two phases thus produced are separated in the separator S200.
  • the liquid fraction from the bottom of the separator is then sent via line 3 into the exchanger EC1 where it is sub-cooled, then expanded and vaporized to provide the required refrigeration in the exchanger EC1.
  • the vapor fraction from the head of separator S200 is sent via line 207 to the exchanger EC1.
  • a vapor fraction enriched in methane and nitrogen is collected which is sent to the exchanger E2 in which it is liquefied. It is then sub-cooled in the exchanger E3, then expanded and vaporized to produce the refrigeration required in the exchanger E3.
  • the exchanger EC 1 is for example a tube and shell type exchanger such as that which is shown diagrammatically in FIG. 7.
  • the gas to be treated arriving via the conduit 2 circulates in an ascending direction inside vertical tubes 30.
  • These tubes are preferably provided with a lining, for example a structured lining making it possible to improve the contact between the gas which goes up and the liquid fractions go down.
  • the treated gas is evacuated at the head via line 5.
  • the solvent introduced by the conduit 20 (FIG. 6A) is sent into the various tubes 30 by a supply ramp 31 and a distribution plate 32.
  • the liquid hydrocarbon phase stabilized by heating using a reboiler B 2 located in the lower part of the exchanger EC 1 , for example, is discharged under level control, via line 9, and the aqueous phase is evacuated under level control via line 6.
  • Refrigeration is ensured by a heat transfer fluid introduced into the exchanger through the pipe 33 and evacuated after heat exchange through the pipe 34.
  • the exchanger EC 1 is a plate exchanger, for example of brazed aluminum, such as that which is shown diagrammatically in FIG. 8.
  • Such an exchanger is constituted by an assembly of flat plates 35 between which there are corrugated intermediate plates 36 which make it possible to mechanically maintain the assembly and to improve the heat transfer.
  • These plates delimit channels 37 in which the fluids participating during the heat exchange process circulate.
  • the gas to be treated introduced into the exchanger through the conduit 2 circulates in the channels 37 in an upward direction while being cooled progressively by the heat transfer fluid.
  • the corrugated intermediate plates 36 playing the role of a structured lining, promote contact between the rising gas and the falling liquid fractions.
  • the solvent sent through line 20 in the case of simultaneous dehydration and fractionation processes, is distributed uniformly above the channels 37 in which the gas to be treated circulates.
  • the refrigeration fluid is introduced into the exchanger at its upper part through the conduit 38 which arrives substantially perpendicular to the plane of the section shown in FIG. 8 in a channel supply enclosure not shown in the figure. It is evacuated after heat exchange by the conduit 39 which emerges perpendicular to the plane of the section shown in FIG. 8, the conduit being connected to a channel evacuation enclosure not shown in the figure.
  • the supply and evacuation chambers are devices known to those skilled in the art allowing the passage of the fluids circulating in each of the channels in the evacuation conduit and conversely for distributing the fluid coming from a conduit in the different channels .
  • the liquid hydrocarbon phase is removed under level control (LC, V) via line 9 and the aqueous phase is removed under level control via line 6.
  • plate heat exchangers can also be used, for example stainless steel plate heat exchangers welded together, either edge to edge, or over their entire surface by a diffusion welding technique.
  • FIG. 9 shows diagrammatically an exemplary embodiment of a plate making it possible to sample phases according to their nature according to a method described in FIG. 3, for example.
  • the plate 7 includes chimneys 40 allowing the gas to rise towards the upper part of the exchanger.
  • the liquid phase which is collected on this tray can be evacuated through line 8 with a controlled flow rate, but can also flow by overflow towards the lower part of the exchanger. It is thus possible to collect only a fraction of the liquid phase arriving from the upper part of the exchanger.
  • liquid phases for example a liquid hydrocarbon phase and an aqueous phase
  • aqueous phase which is heavier tends to accumulate at the bottom of the tray and it is possible to evacuate it for example through perforations 41 arranged in the tray.
  • the liquefaction installation may include different plate exchangers.

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US11408676B2 (en) 2015-07-08 2022-08-09 Chart Energy & Chemicals, Inc. Mixed refrigerant system and method

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JPH09113129A (ja) 1997-05-02
DE69618736D1 (de) 2002-03-14
US5718126A (en) 1998-02-17
DE69618736T2 (de) 2002-09-05
KR100441039B1 (ko) 2004-10-02
ES2171630T3 (es) 2002-09-16
JP3988840B2 (ja) 2007-10-10
EP0768502B1 (de) 2002-01-23
KR970021263A (ko) 1997-05-28
FR2739916A1 (fr) 1997-04-18
FR2739916B1 (fr) 1997-11-21
SA96170420B1 (ar) 2006-04-22

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