EP2433075A2 - Procédé et appareil pour séparer des hydrocarbures et de l'azote - Google Patents
Procédé et appareil pour séparer des hydrocarbures et de l'azoteInfo
- Publication number
- EP2433075A2 EP2433075A2 EP10755496A EP10755496A EP2433075A2 EP 2433075 A2 EP2433075 A2 EP 2433075A2 EP 10755496 A EP10755496 A EP 10755496A EP 10755496 A EP10755496 A EP 10755496A EP 2433075 A2 EP2433075 A2 EP 2433075A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- stream
- fractionation
- nitrogen
- process according
- fractionator
- 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.)
- Withdrawn
Links
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 89
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 55
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000000926 separation method Methods 0.000 title claims abstract description 30
- 238000005194 fractionation Methods 0.000 claims abstract description 91
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 238000010992 reflux Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 38
- 238000003303 reheating Methods 0.000 claims description 5
- 239000003345 natural gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 13
- 239000012263 liquid product Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 description 26
- 238000009833 condensation Methods 0.000 description 9
- 230000005494 condensation Effects 0.000 description 9
- 239000008246 gaseous mixture Substances 0.000 description 9
- 238000005057 refrigeration Methods 0.000 description 9
- 238000009835 boiling Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000001419 dependent effect Effects 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
- F25J3/0209—Natural gas or substitute 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
- 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
- F25J3/0233—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 1 carbon atom or more
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—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
- F25J3/0257—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 nitrogen
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
- F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
- F25J3/0635—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of CnHm with 1 carbon atom or more
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
- F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
- F25J3/066—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of nitrogen
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
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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
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
- F25J2200/06—Processes or apparatus using separation by rectification in a dual pressure main column system in a classical double column flow-sheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead gas
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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
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/78—Refluxing the column with a liquid stream originating from an upstream or downstream fractionator column
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/06—Splitting of the feed stream, e.g. for treating or cooling in different ways
-
- 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
- F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
- F25J2235/60—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being (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
- F25J2270/00—Refrigeration techniques used
- F25J2270/02—Internal refrigeration with liquid vaporising loop
Definitions
- This invention relates to processes and apparatus for the low temperature separation of nitrogen from a gaseous mixture comprising nitrogen gas and hydrocarbons. Such mixtures occur naturally in geological formations and can also result from nitrogen injection as a method of improving oil or gas production. Nitrogen separation may be required as part of an overall processing of gaseous hydrocarbons to meet sales specifications, such as maximum inert content or minimum calorific value.
- Low temperature fractionation presents an energy efficient method for the separation of nitrogen from gaseous hydrocarbon streams, in particular gaseous hydrocarbon streams wherein the hydrocarbons comprise predominantly methane, such as natural gas.
- Separated nitrogen streams of high purity can be produced, thereby maximising hydrocarbon recovery and, where the nitrogen stream is vented to atmosphere, minimising environmental impact.
- a double column arrangement (such as disclosed in US 7,127,915) similar to that used in air separation is conventional and is often the most economical choice considering both capital cost and energy consumption.
- the columns are typically configured in a stacked arrangement, with the upper fractionation column operating at low pressure, just above atmospheric, and the lower fractionation column operating at high pressure, typically at approximately 27 bar (2700 kPa).
- a feed gas (01) is cooled and at least partially condensed in heat exchanger (02).
- the partially condensed feed (03) is expanded across valve (06) to form a two-phase feed (07) which is fed to a high pressure column (08).
- the high pressure column (08) separates the two-phase feed (07) into a nitrogen rich overhead vapour fraction (19) and a hydrocarbon rich liquid fraction (09).
- the hydrocarbon rich liquid fraction (09) from the high pressure column (08) is sub- cooled in heat exchanger (10) to form stream (12) which is expanded across valve (13) to form a further two-phase feed stream (14) which is fed to an intermediate stage of a low pressure column (15).
- the overhead vapour (19) from the high pressure column (08) is fully condensed in heat exchange with boiling liquid at the bottom of the low pressure column (15) in reboil heat exchanger (04).
- the liquid may either be piped from the bottom tray or packed section, or the reboil heat exchanger (04) may be submerged in the liquid in the sump of the low pressure column (15).
- the fully condensed overhead stream (20) is split. A portion is passed as reflux (22) to the high pressure column (08) and a portion (23) is sub-cooled in heat exchangers (10) and (24) to form stream (25) which is expanded across valve (26) and passes as reflux (27) to the low pressure column (15).
- a nitrogen vapour stream (28) with low methane content from the low pressure column (15) is rewarmed in heat exchanger (24) to provide refrigeration for sub-cooling of the nitrogen rich reflux stream and is further rewarmed in heat exchangers (10) and (02).
- the purity of the hydrocarbon product (31) from the bottom of the low pressure fractionation column (15) is ensured by provision of sufficient reboil in heat exchange with the overhead vapour from the high pressure column (08) in the reboil heat exchanger (04).
- Purity of the nitrogen product from the low pressure fractionation column overhead (28) is ensured by conditioning the feed streams to the column and, in particular, providing sufficient flow of nitrogen rich reflux (27).
- the pressure drop between high pressure fractionation column (08) and low pressure fractionation column (15) provides the required refrigeration by Joule-Thomson expansion. High purity nitrogen and hydrocarbon streams are withdrawn from the top and bottom of the low pressure fractionation column (15) respectively.
- options to increase the available reflux include:
- Process selection will be dependent on considerations such as plant capacity, feed gas nitrogen content and variability and feed and product gas pressure.
- Use of an upstream 'pre-separation' system is efficient in producing product gas at elevated pressure, hence reducing product gas compression power requirements and may also be preferred when the gaseous feed comprises contaminants such as carbon dioxide and heavy hydrocarbons, which are tolerated at higher levels in the pre-separation system.
- Inclusion of either a pre-separation system or a nitrogen recycle system does however introduce additional equipment items.
- the present invention provides an alternative double column system for the separation of nitrogen from a gaseous mixture comprising nitrogen gas and hydrocarbons which uses improved heat integration to maximise the nitrogen reflux stream and to optimise the feed conditions to the low pressure fractionation column.
- This provides additional flexibility to process gases having low nitrogen content, for example less than 35 mol%, and potentially as low as 20 mol% without recourse to the use of additional equipment for pre-separation or nitrogen recycling as described above.
- the invention is also useful for the separation of gases having nitrogen content above 35 mol%, with improved separation efficiency being observed in comparison with conventional separation techniques.
- the present invention provides a process for the separation of nitrogen from a gaseous feed comprising a mixture of hydrocarbons and nitrogen gas, the process comprising the steps of:
- step (i) cooling and at least partially condensing the gaseous feed; (ii) feeding the cooled and at least partially condensed feed from step (i) to a first fractionation to produce an overhead vapour stream having an enriched nitrogen content and a condensed product having a reduced nitrogen content which is subjected to a second fractionation, which comprises reboil, at a lower pressure than the first fractionation;
- step (iv) sub-cooling the condensed product of the first fractionation and dividing the resulting sub-cooled product into at least two streams: a first stream being expanded and fed to the second fractionation, and a second stream being expanded and reheated in heat exchange with the separated vapour stream from step (iii) before being fed to the second fractionation; (v) removing a hydrocarbon product stream low in nitrogen from the second fractionation; and (vi) removing a nitrogen rich stream from the second fractionation.
- steps (iii) and (iv) enables separation of feed streams with lower nitrogen content than is feasible with prior art processes, such as the conventional double column arrangement described above.
- partial condensation of the overhead vapour stream from the first fractionation allows the separated vapour stream from step (iii) to be efficiently condensed in heat exchange with reheat of the second stream of the condensed product in step (iv) to provide reflux to the second fractionation.
- the reheated second stream has an increased vapour fraction and its introduction into the second fractionation provides an increased quantity of stripping vapour to the second fractionation.
- the effect of these steps is to provide improved separation, even for feed compositions comprising less than 35 mol% nitrogen, for example 20 to 35 mol%, while maintaining the overall energy efficiency of the separation process.
- partial condensation of the overhead stream from the first fractionation allows the first fractionation and the second fractionation steps to be 'decoupled' as there is no physical requirement for the second fractionator to be elevated above the first fractionator.
- the hydrocarbons in the gaseous feed comprise or consist of methane.
- the gaseous feed may comprise or consist of natural gas.
- the gaseous feed comprises less than 40 mol% nitrogen, less than 35 mol% nitrogen, or iess than 30 mol% nitrogen.
- the gaseous feed comprises at least 20 mol% nitrogen.
- the gaseous feed may further comprise other inert gases, such as helium. If required, the gaseous feed may be subjected to one or more pre-treatment procedures to remove impurities and/or unwanted components which could solidify in either of the fractionations.
- the gaseous feed is cooled and partially condensed prior to the first fractionation.
- heat exchange during cooling of the gaseous feed may be used to provide reboil to the second fractionation.
- cooling of the gaseous feed may be obtained by heat exchange with the hydrocarbon product low in nitrogen from the second fractionation and/or the nitrogen rich stream from the second fractionation.
- the hydrocarbon product low in nitrogen from the second fractionation is pumped to elevated pressure and evaporated to provide cooling to the gaseous feed.
- the gaseous feed may also be split into at least two streams, each of which may be independently processed according to any of the steps described above before being directed to the first fractionation.
- at least one of the at least two streams is used to provide reboil to the second fractionation energy efficiently via heat exchange, that stream is preferably fed to an intermediate stage of the first fractionation.
- at least one of the at least two streams is not used to provide reboil to the second fractionation, that stream is preferably fed below the bottom stage of the first fractionation to provide stripping vapour.
- the first fractionation is at a pressure of 5 to 30 bar (0.5 to 3.0 MPa).
- reboil in the second fractionation may be provided by heat exchange with the overhead vapour stream from the first fractionation during the partial condensation thereof, thereby reducing energy consumption.
- the first stream may comprise between 10% and 50% of the sub cooled product.
- the first stream is expanded to form a two-phase feed, prior to being fed to the second fractionation.
- the second stream is preferably expanded to form a two-phase feed before being reheated via heat exchange with the separated vapour stream from step (iii). If required, further reheating of the second stream, after expansion thereof, may be effected by heat exchange with the condensed product from the first fractionation and/or the overhead vapour stream from the first fractionation.
- the first stream is fed to the second fractionation at a higher stage than the second stream.
- the hydrocarbon product stream low in nitrogen from the second fractionation is preferably removed from the second fractionation as a liquid stream.
- the nitrogen rich stream from the second fractionation may be reheated by heat exchange with the overhead vapour stream from the first fractionation during partial condensation thereof and/or by heat exchange with the separated vapour stream in step (iii) during condensation thereof.
- the residual nitrogen content of the hydrocarbon product and the residual hydrocarbon content of the nitrogen rich stream obtained from the second fractionation are dependent on the composition of the feed gas.
- the process of the present invention typically provides a hydrocarbon product comprising 2 mol% or less residual nitrogen content, and possibly a hydrocarbon product comprising less than 1 mol% residual nitrogen can be obtained.
- the process may be operated with a more relaxed specification so as to obtain a hydrocarbon product having, for example, up to 10 mol% residual nitrogen content.
- the present invention also provides an apparatus for the separation of nitrogen from a gaseous feed comprising a mixture of hydrocarbons, the apparatus comprising of:
- step (iii) means for conveying the cooled and at least partially condensed feed from step (i) to the first fractionator;
- (viii) means for expanding a first stream prior to entry into the second fractionator, and means for expanding and heating prior to entry into the second fractionator;
- (x) means for conveying a nitrogen rich stream from the second fractionator.
- the first and second fractionators may be in a stacked configuration, with the second fractionator positioned above the first fractionator.
- the overall height of the apparatus may be reduced by arranging the first and second fractionators in a non-stacked configuration.
- the second fractionator comprises a reboil heat exchanger.
- Suitable means for expanding the streams include liquid and two-phase expansion turbines.
- Figure 1 shows a conventional stacked double column apparatus for the separation of nitrogen from a gaseous mixture comprising nitrogen gas and hydrocarbons, as described above.
- Figure 2 shows a stacked double column apparatus in accordance with the present invention.
- Figure 3 shows an uncoupled double column apparatus also in accordance with the present invention
- FIG 4 also shows an uncoupled double column apparatus in accordance with the present invention.
- a high pressure column (08) and a low pressure column (15) are provided in a stacked arrangement, with the high pressure column (08) positioned below the low pressure column (15).
- a feed gas (01) is cooled and at least partially condensed in a heat exchanger (02) and is expanded across valve (06) to form two-phase feed (07) to the bottom of the high pressure column (08).
- the high pressure column (08) separates the two-phase feed (07) into a nitrogen rich overhead vapour fraction (19) and a hydrocarbon rich liquid fraction (09)
- the hydrocarbon rich liquid fraction (09) from the high pressure column (08) is sub- cooled in heat exchanger (10) and the resulting stream (12) is split into two portions.
- One portion is expanded across valve (13) to form a two-phase feed stream (14) which is fed to an intermediate stage of the low pressure column (15).
- the other portion is expanded across valve (16) and is reheated at low pressure to form a two-phase feed stream (18), which has a higher vapour fraction and is fed to a lower stage of the low pressure column (15) than feed stream (14).
- the overhead vapour (19) from the high pressure column (08) is partially condensed in heat exchange with boiling liquid at the bottom of the low pressure column (15) in a reboil heat exchanger (04).
- the boiling liquid may either be piped to the reboil heat exchanger (04) from a bottom tray or packed section of the low pressure column (15), or the reboil heat exchanger (04) may be submerged in the liquid in the sump of the low pressure column (15).
- the partially condensed overhead stream (20) is separated into a liquid stream (22) and a separated vapour stream (23) in a phase separator (21).
- the liquid stream (22) is passed as reflux to the high pressure column (08).
- the separated vapour stream (23) is fully condensed and sub-cooled in heat exchangers (10) and (24) to form stream (25) which is expanded across valve (26) and is passed as reflux (27) to the low pressure column (15).
- a hydrocarbon product (31) with low nitrogen content from the low pressure column (15) is pumped to an elevated pressure by a pump (32), dependent on the composition and pressure of the feed gas (01), and the resulting stream (33) is evaporated and reheated in heat exchangers (10) and (02) to form a gaseous product (35).
- Evaporation and reheating of the hydrocarbon stream (33) in heat exchanger (02) preferably provides at least a portion of, and more preferably the majority of, the refrigeration required for cooling and condensation of the feed gas (01).
- a nitrogen vapour stream (28) with low hydrocarbon content from the low pressure column (15) is preferably reheated in heat exchanger (24) to provide further refrigeration for sub-cooling of the separated vapour stream (23) and is preferably further reheated in heat exchangers (10) and (02).
- a high pressure column (08) and a low pressure column (15) are provided in an uncoupled arrangement.
- a feed gas (01) is cooled and at least partially condensed in a heat exchanger (02) and is then sub-cooled in heat exchange with boiling liquid at the bottom of the low pressure column (15) in a reboil heat exchanger (04).
- the boiling liquid may either be piped to the reboil heat exchanger (04) from a bottom tray or packed section of the low pressure column (15), or the reboil heat exchanger (04) may be submerged in the liquid in the sump of the low pressure column (15).
- the cooled and at least partially condensed feed gas (05) is expanded across valve (06) to form two-phase feed (07) to the bottom of the high pressure column (08).
- the hydrocarbon rich liquid fraction (09) from the high pressure column (08) is sub- cooled in heat exchangers (10) and (11) and the resulting stream (12) is split into two portions.
- One portion is expanded across a valve (13) to form a two-phase feed stream (14) to an intermediate stage of the low pressure column (15).
- the other portion is expanded across a valve (16) and is reheated at low pressure to form a two-phase feed stream (18), which has a higher vapour fraction and is fed to a lower stage of the low pressure column (15) than feed stream (14).
- the overhead vapour (19) from the high pressure column (08) is partially condensed in heat exchanger (10).
- the partially condensed overhead stream (20) is separated into a liquid stream (22) and a separated vapour stream (23) in a phase separator (21).
- the liquid stream (22) is passed as reflux to the high pressure column (08).
- the separated vapour stream (23) is fully condensed and sub-cooled in heat exchangers (11) and (24) to form stream (25) which is expanded across a valve (26) and is passed as reflux (27) to the low pressure column (15).
- a hydrocarbon product (31) with low nitrogen content, from the low pressure column (15), is pumped to an elevated pressure by a pump (32), dependent on the composition and pressure of the feed gas (01), and the resulting stream (33) is evaporated and reheated in heat exchanger (02) to form a gaseous product (34).
- Evaporation and reheating of the hydrocarbon stream (33) in the heat exchanger (02) preferably provides at least a portion of, and more preferably the majority of, the refrigeration required for cooling and condensation of the feed gas (01).
- a nitrogen vapour stream (28) with low hydrocarbon content from the low pressure column (15) is preferably reheated in heat exchanger (24) to provide further refrigeration for sub-cooling of the separated vapour stream (23) and is preferably further reheated in heat exchangers (10) and (02).
- a high pressure column (08) and a low pressure column (15) are provided in an uncoupled arrangement, and multiple feeds are provided to the high pressure column.
- a feed gas (01) is cooled and at least partially condensed in a heat exchanger (02) and is split with a portion being expanded across valve (36) to form a two-phase feed (37) which is fed to the bottom of high pressure column (08).
- the remaining portion of the feed gas (01) is further cooled in a heat exchanger (35) to form a stream (03) which is then sub- cooled in heat exchange with boiling liquid at the bottom of the low pressure column (15) in a reboil heat exchanger (04).
- the boiling liquid may either be piped to reboil heat exchanger (04) from a bottom tray or packed section of the low pressure column (15), or the reboil heat exchanger (04) may be submerged in the liquid in the sump of the low pressure column (15).
- the cooled and at least partially condensed feed gas (05) is expanded across valve (06) to form feed stream (07) which is fed to an intermediate stage of high pressure column (08).
- the hydrocarbon rich liquid fraction (09) from the high pressure column (08) is sub- cooled in heat exchangers (10) and (11) and the resulting stream (12) is split into two portions.
- One portion is expanded across valve (13) to form a two-phase feed stream (14) which is fed to an intermediate stage of a low pressure column (15).
- the other portion is expanded across valve (16) and is reheated at low pressure to form a two- phase feed stream (18) which has a higher vapour fraction and is fed to a lower stage of the low pressure column (15) than feed stream (14).
- the overhead vapour (19) from the high pressure column is partially condensed in a heat exchanger (10).
- the partially condensed overhead stream (20) is separated into a liquid stream (22) and a separated vapour portion (23) in a phase separator (21).
- the liquid stream (22) passes as reflux to the high pressure column (08).
- the separated vapour stream (23) is fully condensed and subcooled in heat exchangers (11) and (24) to form a stream (25) which is expanded across valve (26) and is passed as reflux (27) to the low pressure column (15).
- a hydrocarbon product (31) with low nitrogen content, from the low pressure column (15), is pumped to an elevated pressure by pump (32), dependent on the composition and pressure of feed gas (01), and the resulting stream (33) is evaporated and reheated in heat exchangers (35) and (02) to form a gaseous product (34).
- Evaporation and reheating of the hydrocarbon stream (33) in the heat exchangers (35) and (02) preferably provides at least a portion of, and more preferably the majority of, the refrigeration required for cooling and condensation of the feed gas (01).
- a nitrogen vapour stream (28) with low hydrocarbon content from the low pressure column (15) is preferably reheated in heat exchanger (24) to provide further refrigeration for sub-cooling of the separated vapour stream (23) and is preferably further reheated in heat exchangers (11), (10), (35) and (02).
- Table 1 shows typical operating parameters for the conventional double column apparatus shown in Figure 1 when used to separate a gaseous mixture consisting of 40 mol% nitrogen gas and 60 mol% methane. It will be observed that, based on 6 theoretical separation stages in the high pressure column (08) and 6 theoretical separation stages in the low pressure column (15), the conventional double column apparatus is able to separate such a mixture to obtain a nitrogen product stream (Stream 30) having a residual methane content of 0.8 moi% when producing a methane product stream (Stream 35) having a residual nitrogen content of 2.0 mol%.
- Table 2 shows typical operating parameters for the conventional double column apparatus shown in Figure 1 when used to separate a gaseous mixture consisting of 30 mol% nitrogen gas and 70 mol% methane. It will be observed that, based on the same number of theoretical separation stages in columns (08) and (15) as per Comparative Example 1 , and producing a methane product stream (Stream 35) having a residual nitrogen content of 2.0 mol%, hydrocarbon recovery in the conventional double column apparatus is reduced, with the residual methane content of the nitrogen product stream (Stream 30) increasing to 11.1mol%.
- Table 3 shows typical operating parameters for the process of the invention using the apparatus shown in Figure 2, when used to separate a gaseous mixture consisting of 40 mof% nitrogen gas and 60 mol% methane. With this gaseous mixture, the first stream accounts for 33% by molar flow of the sub cooied product. It will be observed that, based on the same number of theoretical separation stages in columns (08) and (15) as per Comparative Example 1 , the process of the invention is able to separate such a mixture to obtain a nitrogen product stream (Stream 30) having an improved residual methane content of 0.4 mol% when producing a methane product stream (Stream 35) having a residual nitrogen content of 2.0 mol%.
- Table 4 shows typical operating parameters for the process of the invention using the apparatus shown in Figure 2, when used to separate a gaseous mixture consisting of 30 mol% nitrogen gas and 70 mol% methane.
- the process and apparatus of the invention is able to maintain good separation efficiency even when the nitrogen content of the gaseous feed is below 35 moi%.
- the first stream accounts for 25% by molar flow of the sub cooled product.
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
L'invention concerne un procédé et un appareil pour séparer l'azote contenu dans une charge d'alimentation gazeuse comprenant un mélange d'hydrocarbures et d'azote gazeux. Le procédé selon l'invention comprend les étapes qui consistent : (i) à refroidir et condenser au moins partiellement la charge d'alimentation gazeuse; (ii) à introduire la charge d'alimentation refroidie et au moins partiellement condensée au cours de l'étape (i) dans une première tour de fractionnement pour produire un courant de vapeur de tête à teneur élevée en azote et un condensat à teneur réduite en azote qui subit un deuxième fractionnement lequel consiste notamment à réaliser une nouvelle ébullition à une pression inférieure à celle régnant dans la première tour de fractionnement; (iii) à condenser au moins partiellement le courant de vapeur de tête, et à procéder à une séparation pour obtenir un courant liquide lequel est utilisé pour obtenir un reflux dans la première tour de fractionnement, et un courant de vapeur séparé qui est condensé pour obtenir un reflux dans la deuxième tour de fractionnement; et (iv) à procéder au sous-refroidissement du condensat du premier fractionnement et à diviser le produit sous-refroidi résultant en au moins deux courants : un premier courant qui subit une expansion et qui est introduit dans la deuxième tour de fractionnement, et un deuxième courant qui subit une expansion, est réchauffé par échange thermique avec le courant de vapeur séparé issu de l'étape (ii) avant d'être introduit dans la deuxième tour de fractionnement; (v) à supprimer un courant de produits hydrocarbures à faible teneur en azote se trouvant dans la deuxième tour de fractionnement; et (iv) à supprimer un courant riche en azote se trouvant dans la deuxième tour de fractionnement.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0905124A GB2455462B (en) | 2009-03-25 | 2009-03-25 | Process and apparatus for separation of hydrocarbons and nitrogen |
| PCT/GB2010/050488 WO2010109228A2 (fr) | 2009-03-25 | 2010-03-23 | Procédé et appareil pour séparer des hydrocarbures et de l'azote |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP2433075A2 true EP2433075A2 (fr) | 2012-03-28 |
Family
ID=40640137
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP10755496A Withdrawn EP2433075A2 (fr) | 2009-03-25 | 2010-03-23 | Procédé et appareil pour séparer des hydrocarbures et de l'azote |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US20120090355A1 (fr) |
| EP (1) | EP2433075A2 (fr) |
| GB (1) | GB2455462B (fr) |
| WO (1) | WO2010109228A2 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110131964A (zh) * | 2019-05-21 | 2019-08-16 | 中石化炼化工程(集团)股份有限公司 | 一种化学链空气分离方法及其系统 |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102008056191A1 (de) * | 2008-11-06 | 2010-05-12 | Linde Ag | Verfahren zum Abtrennen von Stickstoff |
| DE102009038458A1 (de) * | 2009-08-21 | 2011-02-24 | Linde Ag | Verfahren zum Abtrennen von Stickstoff aus Erdgas |
| US9726426B2 (en) | 2012-07-11 | 2017-08-08 | Butts Properties, Ltd. | System and method for removing excess nitrogen from gas subcooled expander operations |
| FR3012211B1 (fr) * | 2013-10-18 | 2018-11-02 | L'air Liquide,Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Procede de deazotation du gaz naturel avec ou sans recuperation d'helium |
| JP2017523179A (ja) * | 2014-07-29 | 2017-08-17 | リンデ アクティエンゲゼルシャフト | 炭化水素流からメタンを回収するための方法およびシステム |
| DE102015004120A1 (de) * | 2015-03-31 | 2016-10-06 | Linde Aktiengesellschaft | Verfahren zum Abtrennen von Stickstoff aus einer Kohlenwasserstoff-reichen Fraktion |
| FR3039080B1 (fr) * | 2015-07-23 | 2019-05-17 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Methode de purification d'un gaz riche en hydrocarbures |
| US10520250B2 (en) | 2017-02-15 | 2019-12-31 | Butts Properties, Ltd. | System and method for separating natural gas liquid and nitrogen from natural gas streams |
| FR3075940B1 (fr) * | 2017-12-21 | 2020-05-22 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Procede de liquefaction d'un courant de gaz naturel contenant de l'azote |
| FR3075939B1 (fr) * | 2017-12-21 | 2020-06-19 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Procede de production d'azote pur a partir d'un courant de gaz naturel contenant de l'azote |
| US12504227B2 (en) | 2018-08-27 | 2025-12-23 | Bcck Holding Company | System and method for natural gas liquid production with flexible ethane recovery or rejection |
| US11015865B2 (en) | 2018-08-27 | 2021-05-25 | Bcck Holding Company | System and method for natural gas liquid production with flexible ethane recovery or rejection |
| US11674749B2 (en) * | 2020-03-13 | 2023-06-13 | Air Products And Chemicals, Inc. | LNG production with nitrogen removal |
| FR3121743B1 (fr) * | 2021-04-09 | 2023-04-21 | Air Liquide | Procédé et appareil de séparation d’un mélange contenant au moins de l’azote et du méthane |
| US11635255B1 (en) | 2022-04-08 | 2023-04-25 | Axip Energy Services, Lp | Liquid or supercritical carbon dioxide capture from exhaust gas |
| EP4703662A1 (fr) | 2024-09-02 | 2026-03-04 | Linde GmbH | Procédé pour obtenir une fraction riche en hélium |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4664686A (en) * | 1986-02-07 | 1987-05-12 | Union Carbide Corporation | Process to separate nitrogen and methane |
Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3210951A (en) * | 1960-08-25 | 1965-10-12 | Air Prod & Chem | Method for low temperature separation of gaseous mixtures |
| DE1601257B1 (de) * | 1968-01-26 | 1970-10-01 | Messer Griesheim Gmbh | Verfahren zur Tieftemperatur-Rektifikation eines Gasgemisches |
| DE2110417A1 (de) * | 1971-03-04 | 1972-09-21 | Linde Ag | Verfahren zum Verfluessigen und Unterkuehlen von Erdgas |
| US4415345A (en) * | 1982-03-26 | 1983-11-15 | Union Carbide Corporation | Process to separate nitrogen from natural gas |
| US4878932A (en) * | 1989-03-21 | 1989-11-07 | Union Carbide Corporation | Cryogenic rectification process for separating nitrogen and methane |
| US4936888A (en) * | 1989-12-21 | 1990-06-26 | Phillips Petroleum Company | Nitrogen rejection unit |
| GB2298034B (en) * | 1995-02-10 | 1998-06-24 | Air Prod & Chem | Dual column process to remove nitrogen from natural gas |
| US5771714A (en) * | 1997-08-01 | 1998-06-30 | Praxair Technology, Inc. | Cryogenic rectification system for producing higher purity helium |
| FR2802825B1 (fr) * | 1999-12-23 | 2002-05-03 | Air Liquide | Appareil de separation par distillation et procede de nettoyage d'un vaporisateur-condenseur de l'appareil |
| GB0000327D0 (en) * | 2000-01-07 | 2000-03-01 | Costain Oil Gas & Process Limi | Hydrocarbon separation process and apparatus |
| FR2826969B1 (fr) * | 2001-07-04 | 2006-12-15 | Technip Cie | Procede de liquefaction et de deazotation de gaz naturel, installation de mise en oeuvre, et gaz obtenus par cette separation |
| GB0220791D0 (en) | 2002-09-06 | 2002-10-16 | Boc Group Plc | Nitrogen rejection method and apparatus |
-
2009
- 2009-03-25 GB GB0905124A patent/GB2455462B/en active Active
-
2010
- 2010-03-23 EP EP10755496A patent/EP2433075A2/fr not_active Withdrawn
- 2010-03-23 US US13/259,355 patent/US20120090355A1/en not_active Abandoned
- 2010-03-23 WO PCT/GB2010/050488 patent/WO2010109228A2/fr not_active Ceased
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4664686A (en) * | 1986-02-07 | 1987-05-12 | Union Carbide Corporation | Process to separate nitrogen and methane |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110131964A (zh) * | 2019-05-21 | 2019-08-16 | 中石化炼化工程(集团)股份有限公司 | 一种化学链空气分离方法及其系统 |
Also Published As
| Publication number | Publication date |
|---|---|
| GB2455462A (en) | 2009-06-17 |
| US20120090355A1 (en) | 2012-04-19 |
| WO2010109228A2 (fr) | 2010-09-30 |
| GB0905124D0 (en) | 2009-05-06 |
| WO2010109228A3 (fr) | 2013-04-04 |
| GB2455462B (en) | 2010-01-06 |
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