EP1639062B1 - Method and plant for simultaneous production of a natural gas for liquefaction and a liquid cut from natural gas - Google Patents
Method and plant for simultaneous production of a natural gas for liquefaction and a liquid cut from natural gas Download PDFInfo
- Publication number
- EP1639062B1 EP1639062B1 EP04767210A EP04767210A EP1639062B1 EP 1639062 B1 EP1639062 B1 EP 1639062B1 EP 04767210 A EP04767210 A EP 04767210A EP 04767210 A EP04767210 A EP 04767210A EP 1639062 B1 EP1639062 B1 EP 1639062B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- natural gas
- column
- pretreated
- stream
- liquefiable
- 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.)
- Expired - Lifetime
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 344
- 239000003345 natural gas Substances 0.000 title claims abstract description 141
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000007788 liquid Substances 0.000 title claims description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 48
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 43
- 238000004821 distillation Methods 0.000 claims abstract description 35
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000011084 recovery Methods 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 239000004215 Carbon black (E152) Substances 0.000 claims description 7
- 230000006835 compression Effects 0.000 claims description 7
- 238000007906 compression Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 5
- 239000003949 liquefied natural gas Substances 0.000 description 33
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 25
- 239000003507 refrigerant Substances 0.000 description 18
- 230000004907 flux Effects 0.000 description 15
- 238000009434 installation Methods 0.000 description 14
- 239000001294 propane Substances 0.000 description 12
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 8
- 238000000605 extraction Methods 0.000 description 8
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 7
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 6
- -1 C 5 hydrocarbons Chemical class 0.000 description 5
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000001282 iso-butane Substances 0.000 description 4
- 235000013847 iso-butane Nutrition 0.000 description 4
- 229940035415 isobutane Drugs 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000012808 vapor phase Substances 0.000 description 4
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 description 1
- 238000012550 audit Methods 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000009975 flexible effect Effects 0.000 description 1
- 230000001965 increasing effect Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- GJVFBWCTGUSGDD-UHFFFAOYSA-L pentamethonium bromide Chemical compound [Br-].[Br-].C[N+](C)(C)CCCCC[N+](C)(C)C GJVFBWCTGUSGDD-UHFFFAOYSA-L 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007430 reference method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000005514 two-phase flow Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- 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
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/0238—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of CnHm with 2 carbon atoms or more
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
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- 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
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- 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
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- F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
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- 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
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- F25J1/0057—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 after expansion of the liquid refrigerant stream with extraction of work
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- 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
- F25J1/0215—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 with one SCR cycle
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- F25J1/0229—Integration with a unit for using hydrocarbons, e.g. consuming hydrocarbons as feed stock
- F25J1/0231—Integration with a unit for using hydrocarbons, e.g. consuming hydrocarbons as feed stock for the working-up of the hydrocarbon feed, e.g. reinjection of heavier hydrocarbons into the liquefied gas
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- F25J1/0235—Heat exchange integration
- F25J1/0237—Heat exchange integration integrating refrigeration provided for liquefaction and purification/treatment of the gas to be liquefied, e.g. heavy hydrocarbon removal from natural gas
- F25J1/0239—Purification or treatment step being integrated between two refrigeration cycles of a refrigeration cascade, i.e. first cycle providing feed gas cooling and second cycle providing overhead gas cooling
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- F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
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- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- 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
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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
- F25J2240/00—Processes or apparatus involving steps for expanding of process streams
- F25J2240/02—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream
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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
- 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
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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
- F25J2270/00—Refrigeration techniques used
- F25J2270/12—External refrigeration with liquid vaporising loop
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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
- F25J2270/00—Refrigeration techniques used
- F25J2270/60—Closed external refrigeration cycle with single component refrigerant [SCR], e.g. C1-, C2- or C3-hydrocarbons
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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
- F25J2270/00—Refrigeration techniques used
- F25J2270/66—Closed external refrigeration cycle with multi component refrigerant [MCR], e.g. mixture of hydrocarbons
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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
- F25J2280/00—Control of the process or apparatus
- F25J2280/02—Control in general, load changes, different modes ("runs"), measurements
Definitions
- the process of the present invention is applicable to production facilities, from a natural gas extracted from the subsoil, of liquefied natural gas (which will be referred to as "LNG”) as the main product and a cut.
- LNG liquefied natural gas
- NNL natural gas liquids
- NGL is understood to mean C 2 + to C 3 + hydrocarbons that can be extracted from natural gas.
- these NGLs may comprise ethane, propane, butane, and C 5 + hydrocarbons.
- LNG produced after extraction of NGLs has a reduced heating value compared to LNG produced without extraction of NGLs.
- Known natural gas liquefaction plants comprise successively a liquefied gas production unit, a liquefaction unit itself and an LNG denitrogenation unit.
- the unit for producing a gas capable of being liquefied necessarily comprises means for removing heavy hydrocarbons C 6 + which can crystallize during liquefaction.
- Such a process has a thermodynamic efficiency optimized for the production of a natural gas at ambient temperature and for the extraction of NGL.
- the main purpose of the invention is to overcome this disadvantage, that is to say to have a simultaneous production process of LNG and a cut of NGL, more economical and more flexible than existing methods.
- the plant shown in the Figure relates to the simultaneous production, from a source 11 of decarbonated, desulphurized and dry starting natural gas, of LNG 13 as the main product and a section of NGL 15 as a by-product.
- This installation comprises a C 6 + heavy hydrocarbon removal unit 17, a NGL recovery unit 19, and a liquefaction unit 21.
- the unit 17 for removing heavy hydrocarbons successively comprises, downstream of the source 11, first, second and third refrigerants 25, 27, 29, and a first distillation column, or auxiliary distillation column 31 equipped with a head condenser.
- This condenser comprises, between the head of the first column 31 and a first separator tank 33, a fourth refrigerant 35 on the one hand, and a reflux pump 37 on the other hand.
- the NGL recovery unit 19 comprises first, second, and third heat exchangers 41, 43, 45, a second separator tank 47, a second distillation column, or main distillation column 49, a first turbine 51 coupled to a first compressor 53, a second compressor 55 driven by an external power source 56, a fifth refrigerant 57 and a pump 59 for extracting NGLs.
- Unit 21 for liquefying natural gas comprises fourth and fifth heat exchangers 65, 67 cooled by a refrigerating cycle 69.
- This cycle 69 comprises a three-stage compressor 73A, 73B, 73C, provided with first and second intermediate refrigerants 75A and 75B and an outlet refrigerant 75C, four refrigerants 77A-77D in series, a third separator tank 79, and first and second hydraulic turbines 81 and 83.
- the initial molar composition of the decarbonated, desulfurized and dry starting natural gas stream 101 comprises 3.90% nitrogen, 87.03% methane, 5.50% ethane, 2.00% propane, 0, 34% iso butane, 0.54% n-butane, 0.18% iso pentane, 0.15% n-pentane, 0.31% C 6 hydrocarbons, 0.03% d C 7 hydrocarbons and 0.02% C 8 hydrocarbons.
- This gas 101 is successively cooled in the first, second and third refrigerants 25, 27, 29 to form the cooled starting natural gas 103.
- This gas 103 is then introduced into the distillation column 31.
- This column 31 produces at the bottom a section 105 of heavy hydrocarbons C 6 + .
- This cup 105 is expanded in an expansion valve 106 to produce a relaxed heavy hydrocarbon stream 107, which is introduced into the second distillation column 49 at a lower N1 level.
- the first column 31 produces a stream 109 of pretreated gas at the head.
- This stream 109 is cooled and partially condensed in the fourth refrigerant 35, and then introduced into the first separator tank 33, where separation takes place between a gas phase constituting the pre-treated natural gas 111 and a liquid phase constituting a reflux liquid. 112, which is refluxed in the purification column by the reflux pump 37.
- the molar composition of the pretreated gas stream 111 comprises 3.9783% nitrogen, 88.2036% methane, 5.3622% ethane, 1.7550% propane, 0.2488% iso butane, 0.3465% n-butane, 0.0616% iso pentane, 0.0384% n-pentane, 0.0057% C 6 hydrocarbons.
- the pre-treated natural gas stream 111 is then split into a feed stream 113 of the LNG recovery unit 19 and a feed stream 115 of the gas liquefaction unit 21.
- the distribution between these two currents is chosen by the control of two respective control valves 114 and 116.
- the stream 113 introduced into the recovery unit 19 is cooled in the second heat exchanger 43 to give a two-phase flow 117 of cooled pre-treated natural gas.
- This stream 117 is introduced into the second separator tank 47, which produces a vapor stream 119 and a liquid stream 121.
- the liquid stream 121 is expanded in an expansion valve 123 and then introduced into the column 49 at a level N2 higher than the N1 level.
- the vapor stream 119 is separated into a majority fraction 125 and a minor fraction 127.
- the major fraction 125 is expanded in the turbine 51 to give a relaxed main fraction 129, which is introduced at a level N3 greater than the level N2 in the column 49.
- the minor fraction 127 is cooled in the third heat exchanger 45, expanded in an expansion valve 131 and then introduced at an upper N4 level of the distillation column 49.
- the N4 level is higher than the N3 level.
- Column 49 is also equipped with an intermediate reboiler 141.
- a reboiler stream 143 is extracted from this column at a level N1a less than N2 and greater than N1. This stream is warmed in the second heat exchanger 43 and reintroduced into the second column 49 at a level b N1 between the level N1 and the level N1.
- the section 15 of NGL is extracted from the bottom of the distillation column 49 by the pump 59.
- a bottom reboiler 145 is mounted on the column 49 to adjust the molar ratio of the hydrocarbons to C 1 relative to the hydrocarbons in question.
- this cut of NGL comprises 0.3688% of methane, 36.8810% of ethane, 33.8344% of propane, 6.157% of iso-butane, 9.9267% of n-butane, 3, 3354% of iso pentane, 2.7808% of n-pentane, 5.7498% of C 6 hydrocarbons, 0.5564% of C 7 hydrocarbons, 0.3710% of C 8 hydrocarbons.
- the respective extraction rates of ethane, propane, and C 4 + hydrocarbons are 36.15%, 91.21%, and 99.3%.
- the recovery rate of ethane is greater than 30%.
- the recovery rate of propane is greater than 80% and is preferably greater than 90%.
- the recovery rate of C 4 + hydrocarbons is greater than 90% and is preferably greater than 95%.
- a stream 151 of purified natural gas is extracted at the top of the column 49. This stream 151 is heated successively in the heat exchanger 45, in the heat exchanger 43 and then in the heat exchanger 41. note that no external cold source is required for the operation of the LNG recovery unit 19.
- the heated gas stream 153 from the exchanger 41 is then compressed successively in the first compressor 51 and then in the second compressor 55 to produce a gas stream 155 at the liquefaction pressure.
- This stream 155 is cooled in the fifth refrigerant 57 and then in the first heat exchanger 41 to give a stream 157 of purified cooled gas.
- the stream 157 is mixed with the feed stream 115 of the gas liquefaction unit, extracted from the C 6 + heavy hydrocarbon removal unit 17.
- This stream 157 and this stream 115 have substantially equal temperatures and pressures and form the stream 161 of natural gas capable of being liquefied.
- the molar composition of this stream 161 of natural gas capable of being liquefied comprises 4.1221% nitrogen, 91.9686% methane, 3.7118% ethane, 0.1858% propane, 0.0063% d iso butane, 0.0051% n-butane and 0.0003% C 5 + hydrocarbons.
- the flow 161 of natural gas that can be liquefied is then successively cooled in the fourth and fifth heat exchangers 65, 67 to produce the LNG stream 13.
- This LNG stream 13 is then denitrogenized in a unit 165.
- Refrigeration in the fourth and fifth heat exchangers 65, 67 is provided by a coolant stream 201.
- This stream 201 partially liquefied in the fourth refrigerant 77D, is introduced into the separator tank 71 and separated into a vapor phase 201 and a liquid phase 203.
- the vapor phase 203 is liquefied in the heat exchanger 65 to provide a liquid stream which is then subcooled in the fifth heat exchanger 67 to provide a subcooled liquid stream 207.
- This subcooled liquid flow 207 is expanded in the first hydraulic turbine 81, then in an expansion valve 208, to give a first refrigeration flow 209.
- This flow 209 vaporizes in the heat exchanger 67 and allows the liquid to be liquefied. gas 161.
- the liquid phase 205 is sub-cooled in the exchanger 65 to give a subcooled flow which, in turn, is expanded in the second hydraulic turbine 83 and then in an expansion valve 210, to give a second refrigerant stream 211
- the streams 209 and 211 are mixed to give a combined stream 213 which is vaporized in the exchanger 65. This vaporization cools the stream 161 and condenses the vapor phase 203 of the refrigerant mixture stream 201.
- the mixture stream 213 is then compressed in the compressor 77, whose characteristics are given in the table below, to obtain a compressed mixture stream 215.
- Compressor 73A 73B 73C Suction temperature (° C) - 37.44 34 34 Discharge temperature (° C) 67.25 68.70 68.15 Suction pressure (Bar) 3.65 18.30 29.70 Discharge pressure (Bar) 18.70 30.00 47.61 Polytropic yield (%) 82 82 82 Power (KW) 74109 24396 21882
- This stream of compressed mixture 215 is then successively cooled in the four refrigerants in series 81 to form the stream 201.
- the first, second, third and fourth refrigerants 25, 27, 29, 35 for cooling the starting natural gas on the one hand, and the four refrigerants 77A to 77D for cooling the mixing flow 201 on the other hand, use the same propane refrigeration cycle (not shown).
- This cycle comprises the following four vaporization stages: 6.7 ° C. and 7.92 bars, 0 ° C. and 4.76 bars, -20 ° C. and 2.44 bars, -36 ° C. and 1.30 bars.
- the pressure of the distillation column 31 is preferably between 45 and 65 bar.
- the pressure in the second column is greater than 35 bar.
- the purified gas stream 157 and the feed stream of the gas liquefying unit 115 are produced at a pressure greater than 55 bar.
- This method thus makes it possible to achieve energy savings as shown in the table below, where the powers consumed in a reference installation without an auxiliary column 31 and in an installation according to the invention are compared.
- the starting natural gas stream 101 is directly fed into the LNG extraction unit 19 and the refrigerants 25, 27, 29 and 35 that use the propane cycle are also used to pre-cool the gas flow at the liquefaction pressure 155, unlike the installation according to the invention where the exchanger 41 is used to perform this pre-cooling.
- Reference method Process according to the invention Compressor 73 of mixed refrigerant (KW) 119460 120387 Compressor (not shown) of refrigerant propane (KW) 69700 72174 Compressor 55 of treated gas (KW) 20650 14964 Total (KW) 209810 207525
- the installation according to the invention makes it possible simultaneously to produce LNG 13 and a cut of LGN 15 with a saving of 2285 kW compared to the reference installation.
- the entire stream of pre-treated natural gas 111 leaving the unit 17 for removing heavy hydrocarbons is directed directly to the liquefaction unit 21 by the 115.
- the LNG produced then has a relatively high calorific value.
- the NGL recovery unit 19 is then started gradually, without affecting the productivity of the liquefaction unit 21.
- the heating value of the LNG produced is then adjusted by the relative flow rates of the feed streams 113 of the recovery unit. of LNG and 115 of the gas liquefaction unit.
- the LNG recovery unit may comprise a third distillation column mounted downstream of the second distillation column and operating at a lower or higher pressure than this second column.
- This third column enriches NGLs in a particular component such as propane.
- An example of such a unit is described in EP-A-0 535 752.
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Abstract
Description
La présente invention est relative à un procédé de production simultanée d'un gaz naturel apte à être liquéfié et d'une coupe de liquides de gaz naturel (LGN) à partir d'un gaz naturel de départ comprenant de l'azote, du méthane, des hydrocarbures en C2 à C5, et des hydrocarbures lourds en C6 +, du type comprenant les étapes suivantes :
- (a) on pré-traite ledit gaz naturel de départ pour obtenir un gaz naturel pré-traité ;
- (b) on refroidit le gaz naturel pré-traité issu de l'étape (a) jusqu'à une température voisine de son point de rosée ;
- (c) on détend le gaz naturel pré-traité refroidi issu de l'étape (b) et on introduit le gaz naturel détendu dans une unité de récupération des LGN comprenant au moins une colonne de distillation principale, de façon à produire, d'une part, en tête de colonne, un gaz naturel purifié et d'autre part, ladite coupe de LGN ; et
- (d) on forme ledit gaz naturel apte à être liquéfié à partir du gaz naturel purifié issu de l'étape (c).
- (a) pre-treating said starting natural gas to obtain a pre-treated natural gas;
- (b) cooling the pre-treated natural gas from step (a) to a temperature close to its dew point;
- (c) the cooled pre-treated natural gas from step (b) is expanded and the expanded natural gas is introduced into an NGL recovery unit comprising at least one main distillation column, so as to produce one part, at the top of the column, a purified natural gas and secondly, said cut of NGL; and
- (d) forming said natural gas capable of being liquefied from the purified natural gas from step (c).
Le procédé de la présente invention s'applique aux installations de production, à partir d'un gaz naturel extrait du sous-sol, de gaz naturel liquéfié (que l'on désignera par « GNL ») comme produit principal et d'une coupe de liquides du gaz naturel (que l'on désignera par « LGN ») comme produit secondaire.The process of the present invention is applicable to production facilities, from a natural gas extracted from the subsoil, of liquefied natural gas (which will be referred to as "LNG") as the main product and a cut. natural gas liquids (referred to as "NGL") as a by-product.
Dans la présente invention, on entend par LGN des hydrocarbures en C2 + à C3 + qui peuvent être extraits du gaz naturel. A titre d'exemple, ces LGN peuvent comprendre de l'éthane, du propane, du butane, et des hydrocarbures en C5 +.In the present invention, NGL is understood to mean C 2 + to C 3 + hydrocarbons that can be extracted from natural gas. By way of example, these NGLs may comprise ethane, propane, butane, and C 5 + hydrocarbons.
Le GNL produit après extraction des LGN possède un pouvoir calorifique réduit par rapport à un GNL produit sans extraction des LGN.LNG produced after extraction of NGLs has a reduced heating value compared to LNG produced without extraction of NGLs.
Des installations de liquéfaction de gaz naturel connues comportent successivement une unité de production d'un gaz apte à être liquéfié, une unité de liquéfaction proprement dite et une unité de déazotation du GNL. L'unité de production d'un gaz apte à être liquéfié comprend nécessairement des moyens d'élimination des hydrocarbures lourds en C6 + qui peuvent cristalliser lors de la liquéfaction.Known natural gas liquefaction plants comprise successively a liquefied gas production unit, a liquefaction unit itself and an LNG denitrogenation unit. The unit for producing a gas capable of being liquefied necessarily comprises means for removing heavy hydrocarbons C 6 + which can crystallize during liquefaction.
Pour produire simultanément du gaz naturel apte à être liquéfié, et des LGN, on peut par exemple utiliser un procédé du type précité, tel que celui décrit dans la demande FR -A- 2 817 766.In order simultaneously to produce liquefied natural gas and NGLs, it is possible, for example, to use a process of the aforementioned type, such as that described in application FR-A-2,817,766.
Un tel procédé possède un rendement thermodynamique optimisé pour la production d'un gaz naturel à température ambiante et pour l'extraction de LGN.Such a process has a thermodynamic efficiency optimized for the production of a natural gas at ambient temperature and for the extraction of NGL.
Par suite, ce procédé ne donne pas entière satisfaction dans le cas où le gaz naturel obtenu doit être liquéfié. En effet, la dépense énergétique nécessaire pour la liquéfaction du gaz naturel obtenu est relativement élevée.As a result, this process is not entirely satisfactory in the case where the natural gas obtained must be liquefied. Indeed, the energy expenditure required for the liquefaction of the natural gas obtained is relatively high.
L'invention a pour but principal de remédier à cet inconvénient, c'est-à-dire de disposer d'un procédé de production simultanée de GNL et d'une coupe de LGN, plus économique et plus souple que les procédés existants.The main purpose of the invention is to overcome this disadvantage, that is to say to have a simultaneous production process of LNG and a cut of NGL, more economical and more flexible than existing methods.
A cet effet, l'invention a pour objet un procédé du type précité, caractérisé en ce l'étape (a) comprend les sous-étapes suivantes :
- (a1) on refroidit le gaz naturel de départ jusqu'à une température voisine de son point de rosée ;
- (a2) on introduit ledit gaz naturel de départ refroidi issu de l'étape (a1) dans une colonne de distillation auxiliaire qui produit en tête ledit gaz naturel pré-traité, lequel gaz naturel pré-traité ne contient pratiquement plus d'hydrocarbures en C6 +, cette première cotonne de distillation auxiliaire produisant en outre une coupe d'hydrocarbures lourds essentiellement en C6 +.
- (a1) cooling the starting natural gas to a temperature close to its dew point;
- (a2) introducing said cooled starting natural gas from step (a1) into an auxiliary distillation column which produces at its head said pre-treated natural gas, which pre-treated natural gas contains practically no more hydrocarbons in C 6 + , this first auxiliary distillation cotonne further producing a heavy hydrocarbon fraction essentially C 6 + .
Le procédé suivant l'invention peut comporter une ou plusieurs des caractéristiques suivantes, prises isolément ou suivant toutes les combinaisons possibles :
- l'étape (d) comprend les sous-étapes suivantes :
- (d1) on comprime à une pression de liquéfaction le gaz naturel purifié extrait de la tête de ladite colonne principale dans au moins un premier compresseur;
- (d2) on refroidit le gaz naturel purifié comprimé issu de l'étape (d1), par échange de chaleur avec ledit gaz naturel purifié extrait de la tête de la colonne principale, dans un premier échangeur de chaleur, pour produire le gaz naturel apte à être liquéfié ;
- l'étape (b) comprend la sous-étape suivante :
- (b1) on refroidit le gaz naturel pré-traité issu de l'étape (a) par échange de chaleur avec le gaz naturel purifié extrait de la deuxième colonne principale dans un deuxième échangeur de chaleur ;
- l'étape (c) comprend les sous-étapes-suivantes :
- (c1) on introduit le gaz naturel pré-traité refroidi issu de l'étape (b) dans un ballon séparateur pour obtenir un flux liquide et un flux gazeux ;
- (c2) on détend le flux gazeux issu de (c1) dans une turbine accouplée au premier compresseur ;
- (c3) on introduit le flux issu de l'étape (c2) dans la colonne principale à un niveau N3 intermédiaire ;
- (c4) on détend le flux liquide issu de l'étape (c1) et on introduit ce flux liquide détendu dans la colonne principale à un niveau N2 inférieur au niveau N3 ;
- dans l'étape (d1), on comprime le gaz naturel purifié comprimé en sortie du premier compresseur dans un deuxième compresseur alimenté par une source d'énergie externe pour atteindre ladite pression de liquéfaction ;
- la pression de la colonne de distillation principale est supérieure à 35 bars ;
- le gaz naturel apte à être liquéfié comprend en outre une partie du gaz naturel pré-traité directement issu de l'étape (a) ;
- le procédé comprend une phase de démarrage dans laquelle le gaz naturel apte à être liquéfié est constitué majoritairement ou totalement par le gaz naturel pré-traité directement issu de l'étape (a), ledit gaz naturel apte à être liquéfié étant relativement enrichi en hydrocarbures de C2 à C5, et le procédé comprend une phase ultérieure de production dans laquelle la partie de gaz naturel pré-traité directement issu de l'étape (a) dans le gaz naturel apte à être liquéfié est ajustée en fonction de la teneur en hydrocarbures de C2 à C5 désirée dans le gaz naturel apte à être liquéfié ; et
- un liquide produit par la colonne auxiliaire est détendu et introduit dans la colonne principale.
- step (d) comprises the following substeps:
- (d1) the purified natural gas extracted from the head of said main column is compressed at a liquefaction pressure in at least a first compressor;
- (d2) the purified compressed natural gas resulting from step (d1) is cooled by heat exchange with said purified natural gas extracted from the head of the main column, in a first heat exchanger, for producing the natural gas suitable for liquefying;
- step (b) comprises the following substep:
- (b1) cooling the pre-treated natural gas from step (a) by heat exchange with the purified natural gas extracted from the second main column in a second heat exchanger;
- step (c) comprises the following sub-steps:
- (c1) the cooled pre-treated natural gas from step (b) is introduced into a separator flask to obtain a liquid flow and a gas flow;
- (c2) the gas stream from (c1) is expanded in a turbine coupled to the first compressor;
- (c3) introducing the stream from step (c2) into the main column at an intermediate N3 level;
- (c4) the liquid stream resulting from step (c1) is expanded and this expanded liquid stream is introduced into the main column at a level N2 lower than the level N3;
- in step (d1), the purified compressed natural gas at the outlet of the first compressor is compressed in a second compressor supplied by an external energy source to reach said liquefaction pressure;
- the pressure of the main distillation column is greater than 35 bars;
- the liquefied natural gas further comprises a portion of the pre-treated natural gas directly from step (a);
- the method comprises a start-up phase in which the liquefied natural gas consists predominantly or totally of the pre-treated natural gas directly from step (a), said liquefied natural gas being relatively enriched in hydrocarbons; from C 2 to C 5 , and the process comprises a subsequent production stage in which the portion of pre-treated natural gas directly from step (a) in the liquefied natural gas is adjusted according to the content in hydrocarbons of C 2 to C 5 desired in the natural gas capable of being liquefied; and
- a liquid produced by the auxiliary column is expanded and introduced into the main column.
L'invention a en outre pour objet une installation de production simultanée d'un gaz naturel apte à être liquéfié et d'une coupe de liquides de gaz naturel (LGN) à partir d'un gaz naturel de départ comprenant de l'azote, du méthane, des hydrocarbures en C2 à C5, et des hydrocarbures lourds en C6 + du type comprenant :
- (a) une unité de pré-traitement dudit gaz naturel de départ pour obtenir un gaz naturel pré-traité ;
- (b) des moyens de refroidissement du gaz naturel pré-traité jusqu'à une température voisine de son point de rosée ;
- (c) une unité de récupération des LGN comprenant des moyens de détente du gaz naturel pré-traité refroidi et comprenant au moins une colonne principale de distillation qui produit, d'une part, en tête de colonne, un gaz naturel purifié et d'autre part ladite coupe de LGN ; et
- (d) des moyens d'amenée du gaz naturel purifié issu de l'étape (c) dans une conduite de gaz naturel apte à être liquéfié ;
- (a1) des moyens de refroidissement du gaz naturel de départ jusqu'à une température voisine de son point de rosée ;
- (a2) une colonne de distillation auxiliaire du gaz naturel de départ refroidi qui produit en tête ledit gaz naturel pré-traité, lequel ne contient pratiquement plus d'hydrocarbures en C6 +, cette colonne auxiliaire produisant en outre une coupe d'hydrocarbures lourds essentiellement en C6 +.
- (a) a pre-treatment unit of said starting natural gas to obtain a pre-treated natural gas;
- (b) means for cooling the pretreated natural gas to a temperature close to its dew point;
- (c) an NGL recovery unit comprising means for expanding the cooled pre-treated natural gas and comprising at least one main distillation column which produces, on the one hand, at the top of the column, a purified natural gas and on the other hand, said cut of NGL; and
- (d) means for supplying purified natural gas from step (c) into a liquefied natural gas line;
- (a1) means for cooling the starting natural gas to a temperature close to its dew point;
- (a2) an auxiliary distillation column of the cooled starting natural gas which produces said pre-treated natural gas at the top, which contains substantially no more C 6 + hydrocarbons, this auxiliary column also producing a heavy hydrocarbon fraction essentially in C 6 + .
L'installation suivant l'invention peut comporter ou plusieurs des caractéristiques suivantes, prises isolément ou suivant toutes les combinaisons possibles :
- les moyens de formation du gaz naturel apte à être liquéfié comprennent :
- (d1) des moyens de compression du gaz naturel purifié extrait de la tête de la colonne principale à une pression de liquéfaction, comportant au moins un premier compresseur ;
- (d2) un premier échangeur de chaleur qui met le gaz naturel purifié comprimé issu desdits moyens de compression en relation d'échange thermique avec ledit gaz naturel purifié extrait de la tête de la colonne principale, ledit gaz naturel purifié comprimé étant refroidi dans ce premier échangeur pour produire le gaz naturel apte à être liquéfié ;
- les moyens de refroidissement du gaz naturel pré-traité comprennent un deuxième échangeur de chaleur qui met ce gaz en relation d'échange thermique avec ledit gaz naturel purifié extrait de la colonne principale ;
- l'unité de récupération des LNG comprend :
- (c1) un ballon séparateur du gaz naturel pré-traité refroidi qui produit un flux liquide et un flux gazeux ;
- (c2) une première turbine de détente dudit flux gazeux accouplée audit premier compresseur ;
- (c3) des moyens d'introduction du flux gazeux détendu dans la colonne principale à un niveau intermédiaire N3 ;
- (c4) des moyens de détente dudit flux liquide et des moyens d'introduction du flux liquide détendu dans la colonne principale à un niveau N2 inférieur à N3 ;
- les moyens de compression du gaz naturel purifié extrait de la tête de la colonne principale comprennent en outre un deuxième compresseur entraîné par une source d'énergie externe et destiné à augmenter la pression du gaz naturel purifié comprimé jusqu'à la pression de liquéfaction ; et
- les moyens de formation du gaz naturel purifié comprennent des moyens d'introduction sélective d'une partie réglable du gaz naturel pré-traité directement issu de l'unité de pré-traitement dans une conduite de gaz naturel apte à être liquéfié.
- the means for forming liquefied natural gas comprise:
- (d1) compression means purified natural gas extracted from the head of the main column at a liquefaction pressure, comprising at least a first compressor;
- (d2) a first heat exchanger which supplies the purified compressed natural gas from said compression means in heat exchange relation with said purified natural gas extracted from the head of the main column, said purified compressed natural gas being cooled in this first exchanger to produce liquefied natural gas;
- the cooling means of the pre-treated natural gas comprise a second heat exchanger which puts this gas in heat exchange relationship with said purified natural gas extracted from the main column;
- the LNG recovery unit includes:
- (c1) a cooled pretreated natural gas separator flask which produces a liquid stream and a gas stream;
- (c2) a first expansion turbine of said gas flow coupled to said first compressor;
- (c3) means for introducing the gas stream expanded in the main column to an intermediate level N3;
- (c4) means for expanding said liquid stream and means for introducing the expanded liquid stream into the main column at a level N2 less than N3;
- the compression means purified natural gas extracted from the head of the main column further comprises a second compressor driven by an external energy source and intended to increase the pressure of compressed purified natural gas to the liquefaction pressure; and
- the means for forming purified natural gas comprise means for selectively introducing an adjustable portion of the pre-treated natural gas directly from the pre-treatment unit into a line of natural gas capable of being liquefied.
Un exemple de mise en oeuvre de l'invention va maintenant être décrit en regard de la Figure unique annexée, qui représente un schéma synoptique fonctionnel d'une.installation selon l'invention.An exemplary implementation of the invention will now be described with reference to the appended single figure, which represents a functional block diagram of an installation according to the invention.
L'installation représentée sur la Figure est relative à la production simultanée, à partir d'une source 11 de gaz naturel de départ décarbonaté, désulfuré et sec, de GNL 13 comme produit principal et d'une coupe de LGN 15 comme produit secondaire. Cette installation comprend une unité 17 d'élimination des hydrocarbures lourds en C6 +, une unité 19 de récupération des LGN, et une unité 21 de liquéfaction.The plant shown in the Figure relates to the simultaneous production, from a
Dans ce qui suit, on désignera par une même référence un flux de liquide et la conduite qui le véhicule, et les pressions considérées sont des pressions absolues.In what follows, will be designated by the same reference a liquid flow and the pipe that conveys it, and the pressures considered are absolute pressures.
L'unité 17 d'élimination des hydrocarbures lourds comprend successivement, en aval de la source 11, des premier, deuxième et troisième réfrigérants 25, 27, 29, et une première colonne de distillation, ou colonne de distillation auxiliaire 31 équipée d'un condenseur de tête. Ce condenseur comprend, entre la tête de la première colonne 31 et un premier ballon séparateur 33, un quatrième réfrigérant 35 d'une part, et une pompe de reflux 37 d'autre part.The
L'unité 19 de récupération des LGN comprend des premier, deuxième, et troisième échangeurs de chaleur 41, 43, 45, un deuxième ballon séparateur 47, une deuxième colonne de distillation, ou colonne de distillation principale 49, une première turbine 51 accouplée à un premier compresseur 53, un deuxième compresseur 55 entraîné par une source d'énergie externe 56, un cinquième réfrigérant 57 et une pompe 59 d'extraction des LGN.The
L'unité 21 de liquéfaction de gaz naturel comprend des quatrième et cinquième échangeurs de chaleur 65, 67 refroidis par un cycle frigorifique 69.
Ce cycle 69 comprend un compresseur 73 à trois étages 73A, 73B, 73C, muni de premier et second réfrigérants intermédiaires 75A et 75B et d'un réfrigérant de sortie 75C, quatre réfrigérants 77A à 77D en série, un troisième ballon séparateur 79 et des première et seconde turbines hydrauliques 81 et 83.This
Un exemple de mise en oeuvre du procédé selon l'invention va maintenant être décrit.An exemplary implementation of the method according to the invention will now be described.
La composition molaire initiale du flux 101 de gaz naturel de départ décarbonaté, désulfuré et sec comprend 3,90% d'azote, 87,03% de méthane, 5,50% d'éthane, 2,00% de propane, 0,34% d'iso butane, 0,54% de n-butane, 0,18 % d'iso pentane, 0,15% de n-pentane, 0,31% d'hydrocarbures en C6, 0,03% d'hydrocarbures en C7 et 0,02% d'hydrocarbures en C8.The initial molar composition of the decarbonated, desulfurized and dry starting
Ce gaz 101 est successivement refroidi dans les premier, deuxième et troisième réfrigérants 25, 27, 29 pour former le gaz naturel de départ refroidi 103. Ce gaz 103 est ensuite introduit dans la colonne de distillation 31.This
Cette colonne 31 produit en pied une coupe 105 d'hydrocarbures lourds en C6 +. Cette coupe 105 est détendue dans une vanne de détente 106 pour produire un flux 107 d'hydrocarbures lourds détendu, qui est introduit dans la deuxième colonne de distillation 49 à un niveau N1 inférieur.This
Par ailleurs, la première colonne 31 produit en tête un flux 109 de gaz pré-traité. Ce flux 109 est refroidi et partiellement condensé dans le quatrième réfrigérant 35, puis introduit dans le premier ballon séparateur 33, où s'effectue la séparation entre une phase gazeuse constituant le gaz naturel pré-traité 111 et une phase liquide constituant un liquide de reflux 112, lequel est retourné en reflux dans la colonne de purification par la pompe de reflux 37.Moreover, the
La composition molaire du flux de gaz prétraité 111 comprend 3,9783% d'azote, 88.2036% de méthane, 5.3622% d'éthane, 1.7550% de propane, 0.2488% d'iso butane, 0.3465% de n-butane, 0.0616 % d'iso pentane, 0.0384% de n-pentane, 0,0057% d'hydrocarbures en C6.The molar composition of the pretreated
Dans ce flux 111, les hydrocarbures en C6 + sont sensiblement éliminés.In this
Le flux de gaz naturel pré-traité 111 est ensuite partagé en un courant 113 d'alimentation de l'unité 19 de récupération de LNG et un courant 115 d'alimentation de l'unité 21 de liquéfaction de gaz. La répartition entre ces deux courants est choisie par la commande de deux vannes de réglage respectives 114 et 116.The pre-treated
Le courant 113 introduit dans l'unité 19 de récupération est refroidi dans le deuxième échangeur de chaleur 43 pour donner un flux diphasique 117 de gaz naturel pré-traité refroidi. Ce flux 117 est introduit dans le deuxième ballon séparateur 47, qui produit un flux de vapeur 119 et un flux de liquide 121. Le flux de liquide 121 est détendu dans une vanne de détente 123, puis introduit dans la colonne 49 à un niveau N2 supérieur au niveau N1.The
Le flux de vapeur 119 est séparé en une fraction majoritaire 125 et une fraction minoritaire 127.The
La fraction majoritaire 125 est détendue dans la turbine 51 pour donner une fraction principale détendue 129, qui est introduite à un niveau N3 supérieur au niveau N2 dans la colonne 49.The
La fraction minoritaire 127 est refroidie dans le troisième échangeur de chaleur 45, détendue dans une vanne de détente 131 puis introduite à un niveau N4 supérieur de la colonne de distillation 49. Le niveau N4 est supérieur au niveau N3.The
La colonne 49 est par ailleurs équipée d'un rebouilleur intermédiaire 141. Un courant de rebouilleur 143 est extrait de cette colonne à un niveau N1a inférieur à N2 et supérieur à N1. Ce courant est réchauffé dans le deuxième échangeur de chaleur 43 et réintroduit dans la deuxième colonne 49 à un niveau N1b compris entre le niveau N1a et le niveau N1.
La coupe 15 de LGN est extraite de la cuve de la colonne de distillation 49 par la pompe 59. En outre, un rebouilleur de cuve 145 est monté sur la colonne 49 pour ajuster le rapport molaire des hydrocarbures en C1 par rapport aux hydrocarbures en C2 de la coupe de LGN 15. Ce rapport est préférentiellement inférieur à 0,02.The
Ainsi, cette coupe de LGN 15 comprend 0,3688% de méthane, 36,8810% d'éthane, 33,8344% de propane, 6,1957% d'iso butane, 9,9267% de n-butane, 3,3354% d'iso pentane, 2,7808% de n-pentane, 5,7498% d'hydrocarbures en C6, 0,5564% d'hydrocarbures en C7, 0,3710% d'hydrocarbures en C8.Thus, this cut of NGL comprises 0.3688% of methane, 36.8810% of ethane, 33.8344% of propane, 6.157% of iso-butane, 9.9267% of n-butane, 3, 3354% of iso pentane, 2.7808% of n-pentane, 5.7498% of C 6 hydrocarbons, 0.5564% of C 7 hydrocarbons, 0.3710% of C 8 hydrocarbons.
Les taux d'extraction respectifs de l'éthane, du propane, et des hydrocarbures en C4 + sont 36,15%, 91,21%, et 99,3%. Ainsi, par le procédé selon l'invention, le taux de récupération d'éthane est supérieur à 30%. Le taux de récupération de propane est supérieur à 80% et est préférentiellement supérieur à 90%. Le taux de récupération des hydrocarbures en C4 + est supérieur à 90% et est préférentiellement supérieur à 95%.The respective extraction rates of ethane, propane, and C 4 + hydrocarbons are 36.15%, 91.21%, and 99.3%. Thus, by the method according to the invention, the recovery rate of ethane is greater than 30%. The recovery rate of propane is greater than 80% and is preferably greater than 90%. The recovery rate of C 4 + hydrocarbons is greater than 90% and is preferably greater than 95%.
Un flux 151 de gaz naturel purifié est extrait en tête de la colonne 49. Ce flux 151 est réchauffé successivement dans l'échangeur de chaleur 45, dans l'échangeur de chaleur 43 puis dans l'échangeur de chaleur 41. On remarque qu'aucune source de froid extérieure n'est nécessaire pour le fonctionnement de l'unité 19 de récupération des LNG.A
Le flux gazeux réchauffé 153 issu de l'échangeur 41 est alors comprimé successivement dans le premier compresseur 51 puis dans le deuxième compresseur 55 pour produire un flux gazeux 155, à la pression de liquéfaction.The
Ce flux 155 est refroidi dans le cinquième réfrigérant 57 puis dans le premier échangeur de chaleur 41 pour donner un flux 157 de gaz purifié refroidi. Le flux 157 est mélangé au courant d'alimentation 115 de l'unité de liquéfaction de gaz, extrait de l'unité 17 d'élimination des hydrocarbures en lourds en C6 +. Ce flux 157 et ce courant 115 ont des températures et des pressions sensiblement égales et forment le flux 161 de gaz naturel apte à être à liquéfier.This
La composition molaire de ce flux 161 de gaz naturel apte à être liquéfié comprend 4,1221% d'azote, 91,9686% de méthane, 3,7118% d'éthane, 0,1858% de propane, 0,0063% d'iso butane, 0,0051% de n-butane et 0,0003% d'hydrocarbures en C5 +.The molar composition of this
Le flux 161 de gaz naturel apte à être liquéfié est ensuite refroidi successivement dans les quatrième et cinquième échangeurs de chaleur 65, 67 pour produire le flux de GNL 13. Ce flux de GNL 13 subit ensuite une déazotation dans une unité 165.The
La réfrigération dans les quatrième et cinquième échangeurs de chaleur 65, 67 est fournie par un flux 201 de mélange réfrigérant. Ce flux 201, partiellement liquéfié dans le quatrième réfrigérant 77D, est introduit dans le ballon séparateur 71 et séparé en une phase vapeur 201 et une phase liquide 203.Refrigeration in the fourth and
Les compositions molaires de ce flux 201 et des phases liquide et vapeur 203 et 205 sont les suivantes :
La phase vapeur 203 est liquéfiée dans l'échangeur de chaleur 65 pour donner un flux liquide qui est ensuite sous-refroidi dans le cinquième échangeur de chaleur 67 pour donner un flux liquide 207 sous-refroidi.The
Ce flux liquide sous-refroidi 207 est détendu dans la première turbine hydraulique 81, puis dans une vanne de détente 208, pour donner un premier flux de réfrigération 209. Ce flux 209 se vaporise dans l'échangeur de chaleur 67 et permet de liquéfier le gaz 161.This subcooled
La phase liquide 205 est sous-refroidie dans l'échangeur 65 pour donner un flux sous-refroidi qui, à son tour, est détendu dans la deuxième turbine hydraulique 83 puis dans une vanne de détente 210, pour donner un second flux de réfrigérant 211. Les flux 209 et 211 sont mélangés pour donner un flux combiné 213 qui est vaporisé dans l'échangeur 65. Cette vaporisation refroidit le flux 161 et condense la phase vapeur 203 du flux de mélange réfrigérant 201. Le flux de mélange 213 est ensuite comprimé dans le compresseur 77, dont les caractéristiques sont données dans le tableau ci-dessous, pour obtenir un flux de mélange 215 comprimé.
Ce flux de mélange comprimé 215 est alors successivement refroidi dans les quatre réfrigérants en série 81 pour former le flux 201.This stream of
Les premier, deuxième, troisième et quatrième réfrigérants 25, 27, 29, 35 de refroidissement du gaz naturel de départ d'une part, et les quatre réfrigérants 77A à 77D de refroidissement du flux de mélange 201 d'autre part, utilisent le même cycle frigorifique au propane (non représenté). Ce cycle comporte les quatre étages de vaporisation suivants : 6,7°C et 7,92 bars, 0°C et 4,76 bars, -20°C et 2,44 bars, -36°C et 1,30 bar.The first, second, third and
A titre d'exemple, une modélisation des températures, pressions et débits de l'installation en fonctionnement représentée sur la Figure est donnée dans le tableau ci-dessous.
Comme illustré dans cet exemple, la pression de la colonne de distillation 31 est préférentiellement comprise entre 45 et 65 bars. Préférentiellement, la pression dans la seconde colonne est supérieure à 35 bars.As illustrated in this example, the pressure of the
Il est ainsi possible d'optimiser le fonctionnement de chacune des colonnes pour favoriser d'une part, l'extraction d'hydrocarbures en C6 + dans la colonne 31 et d'autre part, l'extraction d'éthane et de propane dans la colonne 49.It is thus possible to optimize the operation of each of the columns to favor, on the one hand, the extraction of C 6 + hydrocarbons in
Par ailleurs, le flux de gaz purifié 157 et le courant d'alimentation de l'unité de liquéfaction de gaz 115 sont produits à une pression supérieure à 55 bars.On the other hand, the purified
Ce procédé permet ainsi de réaliser des gains d'énergie comme illustré dans le tableau ci-dessous, où les puissances consommées dans une installation de référence dépourvue de colonne auxiliaire 31 et dans une installation selon l'invention sont comparées.This method thus makes it possible to achieve energy savings as shown in the table below, where the powers consumed in a reference installation without an
Plus précisément, dans l'installation de référence, le flux de gaz naturel de départ 101 est directement amené dans l'unité 19 d'extraction des LNG et les réfrigérants 25, 27, 29 et 35 qui utilisent le cycle au propane servent également à pré-refroidir le flux gazeux à la pression de liquéfaction 155, contrairement à l'installation selon l'invention où l'échangeur 41 est utilisé pour effectuer ce pré-refroidissement.
Ainsi, l'installation selon l'invention permet de produire simultanément du GNL 13 et une coupe de LGN 15 avec une économie de 2285 kW par rapport à l'installation de référence.Thus, the installation according to the invention makes it possible simultaneously to produce
Par ailleurs, lors du démarrage de l'installation selon l'invention, la totalité du flux de gaz naturel pré-traité 111 sortant de l'unité 17 d'élimination des hydrocarbures lourds est dirigée directement vers l'unité de liquéfaction 21 par le courant d'alimentation 115. Le GNL produit possède alors un pouvoir calorifique relativement élevé. L'unité 19 de récupération des LGN est ensuite démarrée progressivement, sans affecter la productivité de l'unité de liquéfaction 21. Le pouvoir calorifique du GNL produit est ensuite ajusté par les débits relatifs des courants d'alimentation 113 de l'unité de récupération de LNG et 115 de l'unité de liquéfaction de gaz.Furthermore, when starting up the installation according to the invention, the entire stream of pre-treated
De même, en cas d'incident dans l'unité 19 de récupération de LNG, la totalité du flux de gaz naturel pré-traité 111 sortant de l'unité d'élimination des hydrocarbures lourds 17 est dirigée directement vers l'unité de liquéfaction 21 par le courant d'alimentation 115.Similarly, in the event of an incident in the
En variante, l'unité de récupération de LNG peut comprendre une troisième colonne de distillation montée en aval de la deuxième colon ne de distillation et qui fonctionne à une pression inférieure ou supérieure à cette deuxième colonne. Cette troisième colonne permet d'enrichir les LGN en un composant particulier comme le propane. Un exemple d'une telle unité est décrit dans EP-A-0 535 752.Alternatively, the LNG recovery unit may comprise a third distillation column mounted downstream of the second distillation column and operating at a lower or higher pressure than this second column. This third column enriches NGLs in a particular component such as propane. An example of such a unit is described in EP-A-0 535 752.
Grâce à l'invention qui vient d'être décrite, il est possible de disposer d'une installation qui produit simultanément du GNL et des LGN de manière économique et flexible en disposant de taux élevés d'extraction pour les hydrocarbures en C2 à C5. La consommation d'énergie est significativement réduite, de manière surprenante, par l'insertion d'une colonne de distillation auxiliaire en amont de l'unité de récupération des LNG et par l'introduction dans cette unité de la fraction de tête de cette colonne.Thanks to the invention that has just been described, it is possible to have a facility that simultaneously produces LNG and NGLs economically and flexibly by having high extraction rates for hydrocarbons C 2 to C 5 . The energy consumption is significantly reduced, surprisingly, by the insertion of an auxiliary distillation column upstream of the LNG recovery unit and the introduction into this unit of the top fraction of this column. .
La productivité d'une telle installation est accrue par la possibilité de diriger au moins une partie de cette fraction de tête directement vers l'unité de liquéfaction, notamment lors des phases de démarrage de l'installation ou en cas de panne dans l'unité de récupération de LNGThe productivity of such an installation is increased by the possibility of directing at least a portion of this head fraction directly to the liquefaction unit, in particular during the start-up phases of the installation or in case of failure in the unit. LNG recovery
Par ailleurs, cette installation permet de produire des GNL dont on peut ajuster le pouvoir calorifique.Moreover, this installation makes it possible to produce LNG with which the calorific value can be adjusted.
Claims (13)
- Process for the simultaneous production of a liquefiable natural gas (161) and a natural gas liquids (NGL) cut (15) from a starting natural gas (101) containing nitrogen, methane, C2 to C5 hydrocarbons and C6 + heavy hydrocarbons;
of the type comprising the following steps:(a) the said starting natural gas (101) is pretreated in order to obtain a pretreated natural gas (111);(b) the pretreated natural gas (111) resulting from step (a) is cooled down to a temperature close to its dew point;(c) the cooled pretreated natural gas (117) resulting from step (b) is expanded and the expanded natural gas (121, 127,129) is introduced into an NGL recovery unit (19) comprising at least one main distillation column (49) so as to produce, on the one hand, as column top product, a purified natural gas (151) and, on the other hand, the said NGL cut (15); and(d) the said liquefiable natural gas (161) is formed from the purified natural gas (151) resulting from step (c);characterized in that step (a) comprises the following substeps:(a1) the starting natural gas (101) is cooled down to a temperature close to its dew point;(a2) the said cooled starting natural gas (103) resulting from step (a1) is introduced into an auxiliary distillation column (31) equipped with an overhead condenser (32) that produces a reflux, the auxiliary distillation column (31) operating at a pressure between 45 and 65 bar and producing, as top product, the said pretreated natural gas (111), which pretreated natural gas (111) no longer contains practically any C6 + hydrocarbons, this auxiliary distillation column (31) furthermore producing a cut (105) of essentially C6 + heavy hydrocarbons;in that step (c) comprises the following substeps:(c1) the cooled pretreated natural gas (117) resulting from step (b) is introduced into a separator tank (47) in order to obtain a liquid stream (121) and a gas stream (125);(c2) the gas stream (125) resulting from step (c1) is expanded in a turbine (51) coupled to a first compressor (53);(c3) the stream (129) resulting from step (c2) is introduced into the main column (49) at an intermediate level N3;(c4) the liquid stream (121) resulting from step (c1) is expanded and this expanded liquid stream (121) is introduced into the main column (49) at a level N2 below the level N3;and in that the liquefiable natural gas (161) furthermore includes a portion (115) of the pretreated natural gas (111) coming directly from step (a). - Process according to Claim 1, characterized in that step (d) comprises the following substeps:(d1) the purified natural gas (151) extracted from the top of the said main column (49) is compressed at a liquefaction pressure in at least a first compressor (53);(d2) the compressed purified natural gas (155) resulting from step (d1) is cooled, by heat exchange with the said purified natural gas (151) extracted from the top of the main column (49), in a first heat exchanger (41) in order to produce the liquefiable natural gas (161).
- Process according to Claim 2, characterized in that step (b) comprises the following substep:(b1) the pretreated natural gas (113) resulting from step (a) is cooled by heat exchange with the purified natural gas (151) extracted from the second main column (49) in a second heat exchanger (43).
- Process according to Claim 2 or 3, characterized in that, in step (d1), the compressed purified natural gas (153) output by the first compressor (53) is compressed in a second compressor (55) supplied by an external energy source (56) in order to reach the said liquefaction pressure.
- Process according to any one of Claims 1 to 4, characterized in that the pressure of the main distillation column (49) is greater than 35 bar.
- Process according to any one of Claims 1 to 5, characterized in that it includes a start-up phase in which the liquefiable natural gas (161) consists mostly or completely of the pretreated natural gas (111) coming directly from step (a), the said liquefiable natural gas (161) being relatively enriched with C2 to C5 hydrocarbons, and in that the process includes a subsequent production phase in which the portion (115) of pretreated natural gas (111) coming directly from step (a) in the liquefiable natural gas (161) is adjusted according to the desired C2 to C5 hydrocarbon content in the liquefiable natural gas (161).
- Process according to any one of the preceding claims, characterized in that a liquid (105) produced by the auxiliary column (31) is expanded and introduced into the main column (49).
- Process according to any one of the preceding claims, characterized in that the auxiliary distillation column (31) is designed to extract approximately 98 mol% of C6 + hydrocarbons present in the starting natural gas (101).
- Process according to any one of the preceding claims, characterized in that the molar content of C6 + hydrocarbons in the pretreated natural gas (111) is approximately equal to 57 ppm.
- Plant for the simultaneous production of a liquefiable natural gas (161) and a natural gas liquids (NGL) cut (15) from a starting natural gas (101) containing nitrogen, methane, C2 to C5 hydrocarbons and C6 + heavy hydrocarbons, of the type comprising:(a) a unit (17) for pretreatment of the said starting natural gas (11) in order to obtain a pretreated natural gas (111);(b) means (43) for cooling the pretreated natural gas (111) down to a temperature close to its dew point;(c) a unit (19) for recovering the NGLs, comprising means (51, 123, 131) for expanding the cooled pretreated natural gas (117) and comprising at least one main distillation column (49) which produces, on the one hand, as column top product, a purified natural gas (151) and, on the other hand, the said NGL cut (15); and(d) means (53, 55, 41) for forming the liquefiable natural gas from the purified natural gas (151) resulting from step (c);characterized in that the pretreatment unit (17) comprises:(a1) means (25, 27, 29) for cooling the starting natural gas (101) down to a temperature close to its dew point;(a2) an auxiliary distillation column (31) for distilling the cooled starting natural gas (103), which auxiliary column is equipped with an overhead condenser (32) producing a reflux, the auxiliary distillation column (31) operating at a pressure between 45 and 65 bar and producing, as top product, the said pretreated natural gas (111), which no longer contains practically any C6 + hydrocarbons, this auxiliary column furthermore producing a cut (105) of essentially C6 + heavy hydrocarbons;in that the unit (19) for recovering the NGLs comprises:(c1) a separator tank (47) for separating the cooled pretreated natural gas (117), which tank produces a liquid stream (121) and a gas stream (119);(c2) a first expansion turbine (51) for expanding the said gas stream, the said turbine being coupled to a first compressor (53);(c3) means for introducing the expanded gas stream (129) into the main column (49) at an intermediate level N3;(c4) means (123) for expanding the said liquid stream (121) and means for introducing the expanded liquid stream into the main column (49) at a level N2 below N3;and in that the means for forming the liquefiable natural gas (161) comprise means for selectively introducing an adjustable portion (115) of the pretreated natural gas (111) coming directly from the pretreatment unit (17) into a liquefiable natural gas line (161).
- Plant according to Claim 10, characterized in that the means (53, 55, 41) for forming the liquefiable natural gas (161) comprise:(d1) means (53, 55) for compressing the purified natural gas (151) extracted from the top of the main column (49) at a liquefaction pressure, comprising at least the first compressor (53); and(d2) a first heat exchanger (41) which brings the compressed purified natural gas (155) coming from the said compression means (53, 55) into heat-exchange relationship with the said purified natural gas (151) extracted from the top of the main column (49), the said compressed purified natural gas (155) being cooled in this first exchanger (41) in order to produce the liquefiable natural gas (161).
- Plant according to Claim 11, characterized in that the means (43) for cooling the pretreated natural gas (111) comprise a second heat exchanger (43) which brings this gas (111) into heat-exchange relationship with the said purified natural gas (151) extracted from the main column (49).
- Plant according to Claim 11 or 12, characterized in that the means (53, 55) for compressing the purified natural gas (151) extracted from the top of the main column (49) furthermore comprise a second compressor (55) driven by an external energy source and intended to increase the pressure of the compressed purified natural gas (155) up to the liquefaction pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL04767210T PL1639062T3 (en) | 2003-06-02 | 2004-05-28 | Method and plant for simultaneous production of a natural gas for liquefaction and a liquid cut from natural gas |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0306632A FR2855526B1 (en) | 2003-06-02 | 2003-06-02 | METHOD AND INSTALLATION FOR THE SIMULTANEOUS PRODUCTION OF A NATURAL GAS THAT CAN BE LIQUEFIED AND A CUTTING OF NATURAL GAS LIQUIDS |
| PCT/FR2004/001334 WO2004108865A2 (en) | 2003-06-02 | 2004-05-28 | Method and plant for simultaneous production of a natural gas for liquefaction and a liquid cut from natural gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1639062A2 EP1639062A2 (en) | 2006-03-29 |
| EP1639062B1 true EP1639062B1 (en) | 2007-05-02 |
Family
ID=33427602
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP04767210A Expired - Lifetime EP1639062B1 (en) | 2003-06-02 | 2004-05-28 | Method and plant for simultaneous production of a natural gas for liquefaction and a liquid cut from natural gas |
Country Status (16)
| Country | Link |
|---|---|
| US (1) | US7237407B2 (en) |
| EP (1) | EP1639062B1 (en) |
| JP (1) | JP4669473B2 (en) |
| KR (1) | KR101062153B1 (en) |
| CN (1) | CN100588702C (en) |
| AT (1) | ATE361352T1 (en) |
| CA (1) | CA2527381C (en) |
| CY (1) | CY1106780T1 (en) |
| DE (1) | DE602004006266T2 (en) |
| ES (1) | ES2286670T3 (en) |
| FR (1) | FR2855526B1 (en) |
| MX (1) | MXPA05012952A (en) |
| PL (1) | PL1639062T3 (en) |
| PT (1) | PT1639062E (en) |
| TW (1) | TWI352614B (en) |
| WO (1) | WO2004108865A2 (en) |
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| US7946127B2 (en) | 2007-02-21 | 2011-05-24 | Honeywell International Inc. | Apparatus and method for optimizing a liquefied natural gas facility |
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| FR2914990B1 (en) * | 2007-04-13 | 2010-02-26 | Air Liquide | METHOD FOR COLDING A CRYOGENIC EXCHANGE LINE |
| EP1988494A1 (en) * | 2007-04-30 | 2008-11-05 | Honeywell International Inc. | System and method for coordination and optimization of liquefied natural gas (LNG) processes |
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-
2003
- 2003-06-02 FR FR0306632A patent/FR2855526B1/en not_active Expired - Fee Related
-
2004
- 2004-05-28 PL PL04767210T patent/PL1639062T3/en unknown
- 2004-05-28 MX MXPA05012952A patent/MXPA05012952A/en active IP Right Grant
- 2004-05-28 EP EP04767210A patent/EP1639062B1/en not_active Expired - Lifetime
- 2004-05-28 CN CN200480018355A patent/CN100588702C/en not_active Expired - Lifetime
- 2004-05-28 ES ES04767210T patent/ES2286670T3/en not_active Expired - Lifetime
- 2004-05-28 AT AT04767210T patent/ATE361352T1/en not_active IP Right Cessation
- 2004-05-28 CA CA2527381A patent/CA2527381C/en not_active Expired - Lifetime
- 2004-05-28 DE DE602004006266T patent/DE602004006266T2/en not_active Expired - Lifetime
- 2004-05-28 WO PCT/FR2004/001334 patent/WO2004108865A2/en active IP Right Grant
- 2004-05-28 KR KR1020057022877A patent/KR101062153B1/en not_active Expired - Lifetime
- 2004-05-28 PT PT04767210T patent/PT1639062E/en unknown
- 2004-05-28 JP JP2006508346A patent/JP4669473B2/en not_active Expired - Lifetime
- 2004-06-01 TW TW093115702A patent/TWI352614B/en not_active IP Right Cessation
- 2004-06-02 US US10/860,689 patent/US7237407B2/en active Active
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2007
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Also Published As
| Publication number | Publication date |
|---|---|
| FR2855526A1 (en) | 2004-12-03 |
| JP4669473B2 (en) | 2011-04-13 |
| US7237407B2 (en) | 2007-07-03 |
| ATE361352T1 (en) | 2007-05-15 |
| JP2007526924A (en) | 2007-09-20 |
| TW200503815A (en) | 2005-02-01 |
| WO2004108865A3 (en) | 2005-02-17 |
| DE602004006266T2 (en) | 2008-01-10 |
| CY1106780T1 (en) | 2012-05-23 |
| CA2527381C (en) | 2012-03-13 |
| PT1639062E (en) | 2007-08-09 |
| WO2004108865A2 (en) | 2004-12-16 |
| CN1813046A (en) | 2006-08-02 |
| DE602004006266D1 (en) | 2007-06-14 |
| FR2855526B1 (en) | 2007-01-26 |
| ES2286670T3 (en) | 2007-12-01 |
| CN100588702C (en) | 2010-02-10 |
| KR101062153B1 (en) | 2011-09-05 |
| CA2527381A1 (en) | 2004-12-16 |
| PL1639062T3 (en) | 2007-11-30 |
| KR20060021869A (en) | 2006-03-08 |
| MXPA05012952A (en) | 2006-02-28 |
| TWI352614B (en) | 2011-11-21 |
| US20040244415A1 (en) | 2004-12-09 |
| EP1639062A2 (en) | 2006-03-29 |
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