EP2507567A2 - Procédé et appareil d'extraction d'azote présent dans du gnl - Google Patents

Procédé et appareil d'extraction d'azote présent dans du gnl

Info

Publication number
EP2507567A2
EP2507567A2 EP10787542A EP10787542A EP2507567A2 EP 2507567 A2 EP2507567 A2 EP 2507567A2 EP 10787542 A EP10787542 A EP 10787542A EP 10787542 A EP10787542 A EP 10787542A EP 2507567 A2 EP2507567 A2 EP 2507567A2
Authority
EP
European Patent Office
Prior art keywords
stream
fractionation column
nitrogen
feed
overhead
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP10787542A
Other languages
German (de)
English (en)
Other versions
EP2507567B1 (fr
Inventor
Adrian Finn
Grant Johnson
Terence Tomlinson
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Costain Oil Gas and Process Ltd
Original Assignee
Costain Oil Gas and Process Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Costain Oil Gas and Process Ltd filed Critical Costain Oil Gas and Process Ltd
Publication of EP2507567A2 publication Critical patent/EP2507567A2/fr
Application granted granted Critical
Publication of EP2507567B1 publication Critical patent/EP2507567B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—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
    • F25J3/0204—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
    • F25J3/0257—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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/40—Features relating to the provision of boil-up in the bottom of a 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the 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
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • 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
    • F25J2200/76—Refluxing the column with condensed overhead gas being cycled in a quasi-closed loop refrigeration cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/04—Recovery of liquid products
    • 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
    • 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
    • F25J2240/30—Dynamic liquid or hydraulic expansion with extraction of work, e.g. single phase or two-phase turbine
    • 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 separation of nitrogen from liquefied natural gas (LNG) - mixtures comprising nitrogen gas and low-boiling hydrocarbons, such as methane, ethane, propane and butane.
  • LNG liquefied natural gas
  • Nitrogen is found in many natural gas reservoirs, sometimes at relatively high levels, for example greater than around 5 mol%, which can necessitate removal to meet specifications for use as fuel, but often at lower levels not requiring removal. As high quality gas fields are depleted, natural gas increasingly needs to be sourced from lower quality gas fields, containing higher levels of contaminants such as nitrogen.
  • Fractionation systems used for the separation of nitrogen from liquefied natural gas typically incorporate a reboiler to produce stripping vapour, required to reduce the nitrogen level in the LNG product to less than 1 mol%.
  • An example of a conventional apparatus for separation of nitrogen from LNG is shown in Figure 1.
  • a nitrogen-containing LNG feed stream (101 ) already sub-cooled at elevated pressure is further cooled in a reboil heat exchange system (102).
  • the resultant stream (103) is expanded in a hydraulic expansion turbine (104) to give a two-phase stream (105), which is fed to a fractionation column (106).
  • Liquid (140) from the bottom tray (or packed section) of the fractionation column is partially vaporised in the reboil heat exchange system (102), to produce stripping vapour (141 ) which is fed to the fractionation column, and thereby also providing refrigeration to further sub-cool the feed stream (101 ).
  • a LNG stream (107) having low nitrogen content is withdrawn from the bottom of the fractionation column, and is reduced in pressure across a valve (108) to give a two- phase stream (109).
  • the two-phase stream (109) is then passed to a vapour-liquid separator (1 1 1 ) to separate a flash gas stream (1 10) and a low pressure LNG stream (1 12) for storage.
  • the flash gas stream (1 10) is passed to a compressor (134), and a resulting compressed stream (135) is cooled by a heat exchanger (136) to give a fuel gas stream (137).
  • An overhead vapour stream (1 13) rich in nitrogen, but with significant methane content, is withdrawn from the top of the fractionation column (106).
  • the nitrogen vapour overhead from the fractionation column generally comprises significant amounts of methane as the column incorporates no rectification section.
  • the methane-containing overhead vapour is typically used as fuel gas for power generation or to drive compression equipment.
  • restrictions exist as to the nitrogen content of fuel gas which may be used in gas turbines, particularly those derived from aero engines, which can typically burn gases comprising up to 10 mol%, or up to 15 mol% nitrogen, and sometimes as high as 20 mol% nitrogen.
  • the methane-containing overhead vapour from the fractionation column is sometimes used as part of a refrigeration cycle in processes that require methane as a refrigerant. It would be preferable if the methane content of the fractionation overhead vapour could be substantially eliminated.
  • the process and apparatus of the present invention avoids the necessity for a nitrogen rejection unit by producing an overhead vapour stream from the LNG fractionation that has a suitable composition (i.e. substantially devoid of hydrocarbons) for venting to the atmosphere.
  • the recycled portion may be used as a nitrogen-rich reflux stream, which nitrogen-rich reflux stream may be efficiently cooled by heat exchange with one or more streams withdrawn from the fractionation, particularly against evaporating methane rich liquid streams.
  • thermodynamic losses are reduced and process efficiency is increased, leading to greater LNG production with lower power consumption, as well as improved separation in the fractionation system.
  • the process of this invention also avoids the operating complexity of a separate nitrogen rejection unit and is robust to changes in feed composition.
  • step (iii) dividing the overhead vapour stream from step (ii) into at least first and second overhead streams;
  • step (iv) compressing, cooling and at least partially condensing at least the first overhead stream from step (iii);
  • step (v) expanding the stream from step (iv) and passing the expanded stream to the fractionation column as reflux, wherein cooling in step (iv) is provided, at least in part, by heat exchange with one or more streams from the fractionation column.
  • the process of the present invention adds a rectification section to the fractionation column, which enables an overhead stream to be obtained from the fractionation column that is substantially devoid of hydrocarbons.
  • the process of the present invention is capable of producing an overhead stream from the fractionation column that comprises less than 2 mol% methane, less than 1 mol% methane, less than 0.5 mol% methane, and potentially as low as 0.1 mol% methane.
  • the heat integration of the process is improved, thereby reducing energy demands.
  • the proportion of the overhead vapour stream from step (ii) that is recycled to the column as reflux in steps (iii) to (v) is preferably in the range of from 20 to 80 mol% of the total overhead vapour stream, more preferably 30 to 70 mol%, and most preferably 40 to 60 mol% of the total overhead vapour stream from the fractionation column.
  • the exact amount of reflux depends on the nitrogen content of the feed and overhead stream purity.
  • the expression “one or more streams from the fractionation column” refers to any liquid or gas from the fractionation column that can be used as a source of refrigeration to cool a compressed overhead stream from step (iv).
  • the expression may refer to overhead vapour withdrawn from the top of the fractionation column.
  • the expression may also refer to the liquid stream withdrawn from the bottom of the fractionation column.
  • the expression may further refer to a side stream obtained from an intermediate stage of the column.
  • the expression may refer to liquid and/or vapour within the column where one or more heat exchange steps takes place within the column.
  • the LNG feed may consist of, or consist substantially of, methane.
  • the feed may also comprise small amounts of other hydrocarbons such as, for example, ethane, propane, butane and/or heavier hydrocarbons.
  • the hydrocarbons in the LNG feed usually comprise greater than 80 mol% methane, more typically greater than 85 mol% methane, and potentially up to near 100% methane.
  • the balance of the LNG feed may comprise ethane, propane, butane and/or heavier hydrocarbons.
  • the total content of ethane and/or propane and/or heavier hydrocarbons in the LNG feed is less than 20 mol%, more preferably less than 10 mol%, and most preferably less than 5 mol%.
  • the total content of propane and/or heavier hydrocarbons in the LNG feed is preferably less than 10 mol%, more preferably less than 5 mol%, and most preferably less than 2 mol%.
  • the total content of hydrocarbons heavier than propane in the LNG feed is preferably less than 5 mol%, more preferably less than 2 mol% and most preferably less than 1 mol%.
  • the process of the present invention may be used in particular for the separation of nitrogen from LNG feeds that comprise up to 40 mol% nitrogen.
  • the feed may comprise up to 30 mol% nitrogen, up to 20 mol% nitrogen or up to 15 mol% nitrogen.
  • the feed comprises at least 1 mol% nitrogen, for example at least 2 mol% nitrogen, possibly 5 mol% nitrogen, or at least 10 mol% nitrogen.
  • the present invention is particularly applicable to the separation of nitrogen from feeds that comprise or consist of liquefied natural gas.
  • the fractionation column is typically operated in a pressure range of from 100 to 500 kPa, more preferably 100 to 300 kPa, and most preferably 120 to 200 kPa.
  • suitable operating pressures for the fractionation column include 130 kPa, 140 kPa, 150 kPa, 160 kPa, 170 kPa, 180 kPa and 190 kPa.
  • the operating temperature of the fractionation column is dependent on the operating pressure, but the overhead temperature is generally in the range -175 °C to -190 °C and the bottom liquid temperature is generally in the range -135 °C to -160°C.
  • an overhead vapour stream having an enriched nitrogen content is one that comprises a higher mole fraction of nitrogen than that of the feed.
  • a liquid stream having reduced nitrogen content is one that comprises a lower mole fraction of nitrogen than that of the feed.
  • the feed is supplied to the fractionation column at or around the operating temperature and pressure of the column. Suitable operating temperatures and pressures for the fractionation column are discussed above. In most cases, the LNG feed will be supplied at a pressure significantly higher than the operating pressure of the fractionation column.
  • a liquefied natural gas feed would typically have a pressure in the range of from 3,000 to 10,000 kPa. In most cases it is therefore necessary to expand the cooled feed to column pressure.
  • the feed may be expanded to column pressure across an expansion valve or by way of an expansion turbine. Expansion turbines have the benefit of extracting work from the process under near-isentropic conditions and reducing the amount of upstream cooling of the feed LNG that is necessary, and thus providing a reduction in energy requirements in upstream liquefaction plant.
  • the cooled and expanded feed is preferably supplied to the fractionation column as a two-phase vapour-liquid mixture. More preferably, the two-phase mixture has a vapour fraction of from 1 to 40 mol%, more preferably 2 to 20 mol%, and most preferably from 3 to 10 mol%, for example 5 to 8 mol%.
  • cooling in step (iv) is provided, at least in part, by heat exchange with at least a portion of the overhead vapour stream withdrawn from the fractionation column.
  • cooling in step (iv) is provided, at least in part, by heat exchange with at least a portion of the liquid product stream withdrawn from the fractionation column.
  • the portion of the liquid product stream passed in heat exchange with the compressed first overhead vapour stream in step (iv) may optionally be expanded first, in order to provide further cooling.
  • Heat to the fractionation column is preferably provided, at least in part by a reboiler. Heated vapour from the reboiler is fed back to the fractionation column to strip nitrogen from the descending LNG in the column.
  • cooling in step (iv) may be provided, at least in part, by heat exchange with a stream from the fractionation column in the reboiler.
  • the type of reboiler that may be used is not limited, and a person of skill in the art can select suitable reboiler systems.
  • thermosyphon, forced-circulation, and kettle reboilers may be used in the process of the invention.
  • the fractionation column may comprise an internal reboiler, located within the column, or an external reboiler located outside the fractionation column.
  • the reboiler is preferably immersed in boiling liquid at the bottom of the fractionation column.
  • a liquid stream is withdrawn from the column and fed to the reboiler to produce a heated vapour stream, which is returned to the column as stripping vapour.
  • the bulk of the condensing duty required to cool and at least partially condense the compressed overhead stream from step (iv) is provided by heat exchange with one or more evaporating methane-rich liquids, which may be selected from the liquid product stream withdrawn from the fractionation column and/or boiling liquid at the bottom of the fractionation column and/or a liquid side-stream that is withdrawn from the column and fed to a column-side reboiler.
  • further cooling of the first overhead stream from step (iii) may be provided by heat exchange with the LNG feed.
  • heat exchange with a liquid stream from the fractionation column in the reboiler may be used to provide cooling of the feed in step (i).
  • the reflux feed is fed to the top stage of the fractionation column in step (v) to provide rectification of the column vapour, and thereby improve separation, reducing methane content of the column overhead vapour.
  • the reflux stream is expanded before being fed to the fractionation column, for example using an expansion valve or an expansion turbine.
  • the liquid stream withdrawn from the fractionation column in step (ii) is preferably expanded to form a two-phase vapour-liquid stream. As noted above, this expanded stream, or a portion thereof, may be used to provide cooling in step (iv).
  • the two-phase stream is then passed to a vapour-liquid separator to separate a low pressure liquid hydrocarbon stream substantially free of nitrogen, and a hydrocarbon vapour stream.
  • the hydrocarbon vapour stream contains less than about 15 mol% nitrogen, and more preferably less than about 10 mol% nitrogen.
  • the hydrocarbon vapour stream may advantageously be compressed and cooled to form a fuel gas product. Alternatively, this stream may be used as part of a refrigeration cycle.
  • an apparatus for the separation of nitrogen from a feed comprising liquefied natural gas and nitrogen comprising:
  • step (iii) means for conveying the cooled and expanded feed from step (i) to the fractionation column;
  • one or more heat exchangers for cooling and at least partially condensing the compressed stream from step (v) in heat exchange with one or more streams from the fractionation column;
  • the apparatus of the invention comprises a heat exchanger for cooling and condensing at least one stream from step (v) in heat exchange with at least a portion of the overhead vapour stream withdrawn from the column.
  • the apparatus of the invention comprises a heat exchanger for cooling and condensing at least one stream from step (v) in heat exchange with at least a portion of the condensed stream withdrawn from the column.
  • the apparatus may further comprise an expander to expand the condensed stream withdrawn from the column, or a portion thereof, before heat exchange with the at least one stream from step (v).
  • the fractionation column may comprise one or more reboilers, which may be internal or external to the column.
  • the type of reboiler that may be used is not particularly limited, and thermosiphon, forced-circulation, and kettle reboilers are examples of reboiler types that are compatible with the apparatus of the invention.
  • the reboiler may be a heat exchanger as specified in step (vi) which is operable to provide cooling and condensing to the at least one stream from step (v) via heat exchange with a stream from the fractionation column.
  • the reboiler is operable to provide cooling to the feed via heat exchange with a stream from the fractionation column.
  • the apparatus of the invention preferably comprises means for expanding the bottom liquid stream from step (ii), at least a portion of which may be passed to a heat exchanger in step (vi) as described above, a vapour-liquid separator, and means for conveying the expanded stream to the vapour-liquid separator to separate a liquid stream and a vapour stream.
  • the apparatus may further comprise means for compressing and cooling a vapour stream withdrawn from the vapour-liquid separator.
  • Suitable means for expanding the stream from step (vi) and optionally the bottom liquid stream from step (ii) include expansion valves and expansion turbines.
  • Suitable operating parameters for the process of the present invention are disclosed in detail above. It is to be understood that the apparatus of the invention is operable in accordance with parameters discussed above in connection with the process of the invention. Furthermore, preferred operating parameters for the process of the invention are also preferred operating parameters for the apparatus of the invention.
  • Figure 1 shows a conventional fractionation apparatus for the separation of nitrogen from a gaseous mixture comprising nitrogen gas and hydrocarbons, as described above;
  • Figure 2 shows a fractionation apparatus in accordance with the present invention.
  • FIG. 3 shows another embodiment of a fractionation apparatus in accordance with the present invention.
  • a liquid stream (240) is removed from the bottom tray (or packed section) of the fractionation column below the two-phase feed stream (205) and is partially vaporised to produce stripping vapour (241 ) in reboil heat exchange system (202), providing refrigeration to further sub-cool the feed stream (201 ) and condense nitrogen rich reflux stream (223).
  • Nitrogen rich overhead vapour (213) is removed from the fractionation column (206) and passed to a heat exchange system (214) where it is warmed to a suitable temperature (215) for atmospheric venting (217) downstream of a pressure control valve (216).
  • a portion (218) of the nitrogen rich overhead vapour (213) from the fractionation column is compressed in a compression system (219) to give a compressed stream (220).
  • Compression system (219) includes inter-stage cooling which is not shown.
  • the compressed stream (220) is then cooled (typically in heat exchange against air or water) in a cooler (221 ) to give a high pressure nitrogen rich stream (222).
  • the high pressure nitrogen rich stream (222) is further cooled in heat exchange systems (214) and (202) to give a liquid stream (224) which is further sub-cooled in the heat exchange system (214) to provide a sub-cooled liquid stream (225).
  • the sub-cooled liquid stream (225) is let down to fractionation column pressure across a valve (226) to give a two phase stream (227) which is supplied as reflux to the fractionation column (206).
  • the two-phase stream (209) is then passed to a vapour-liquid separator (21 1 ) and a flash gas stream (210) and a low pressure LNG product stream (212) for storage are obtained.
  • the flash gas stream (210) is compressed using a compressor (234), giving a stream (235), which is cooled (typically in heat exchange against air or water) in a cooler (236) to give a fuel gas stream (237).
  • the necessary refrigeration to cool and sub-cool the nitrogen rich reflux stream (222) to form the stream (225) is provided by heat exchange with the overhead vapour (213) from the fractionation column (206) and the liquid stream (240) that is fed to the reboil heat exchange system (202).
  • FIG. 3 differs from that of Figure 2 by way of the heat exchange systems that are employed to provide the reflux stream to the fractionation column (306).
  • a sub-cooled liquid feed stream (301 ) comprising LNG and nitrogen is further cooled in a reboil heat exchange system (302), to give a stream (303).
  • Stream (303) is expanded in hydraulic expansion turbine (304) to give a two- phase stream (305) which is fed to the fractionation column (306).
  • a liquid stream (340) is removed from the bottom tray (or packed section) of the fractionation column (306) below the two-phase feed stream (305) and is partially vaporised to produce stripping vapour (341 ) in the reboil heat exchange system (302), which provides refrigeration to further sub-cool the feed stream (301 ).
  • Nitrogen rich overhead vapour (313) from the fractionation column (206) passes to a heat exchange system (314) where it is warmed to a suitable temperature (315) for atmospheric venting (317) downstream of pressure control valve (316).
  • a portion (318) of the nitrogen rich overhead vapour (313) from the fractionation column is compressed in a compression system (319) to give a compressed stream (320).
  • the compression system (319) includes inter-stage cooling which is not shown.
  • the compressed stream (320) is then cooled (typically in heat exchange against air or water) in a cooler (321 ) to give a high pressure nitrogen rich stream (322).
  • the high pressure nitrogen rich stream (322) is further cooled and sub-cooled in the heat exchange system (314) to provide a sub-cooled liquid stream (325).
  • the sub-cooled liquid stream (325) is let down to fractionation column pressure across a valve (326) to give a two phase stream (327) which is supplied as reflux to the fractionation column (206).
  • a LNG stream (307), with low nitrogen content, is removed from the fractionation column (306).
  • a portion (328) of the stream (307) is let down to just above storage pressure across a valve (330) to produce a two-phase stream (331 ), which is vaporised to provide refrigeration in the heat exchange system (314).
  • a remaining portion (329) of the stream (307) is let down to storage pressure across a valve (308) to give a two-phase stream (333).
  • the stream (332) resulting from vaporisation of the stream (331 ) in the heat exchange system (314) is combined with the stream (333) to give a two-phase stream (309).
  • the two-phase stream (309) is then passed to a vapour-liquid separator (31 1 ) to separate a flash gas stream (310) and a low pressure LNG product stream (312) for storage.
  • the flash gas stream (310) is compressed by means of a compressor (334), giving a stream (335), which is cooled (typically in heat exchange against air or water) in a cooler (336) to give a fuel gas stream (337).
  • Table 1 shows operating data for the separation of nitrogen from a LNG feed comprising 10 mol% nitrogen, 85 mol% methane, 4 mol% ethane and 1 mol% propane, at a mass flow rate of 200,000 kg/h, according to the prior art separation system described in Figure 1.
  • Table 2 shows corresponding operating data for the separation of nitrogen from the LNG feed used in Example 1 , at a mass flow rate of 200,000 kg/h, according to the process of the invention as described in Figure 2.
  • Vapour Fraction (molar) 0.039 Vapour Liquid 1.000 0.000 1.000
  • the improved separation obtained by the process of the present invention can be attributed to the provision of the low temperature nitrogen rich reflux stream (227), which is obtained at -191.6 °C and supplied to the column at a temperature 25 °C below the feed (205) to the column.
  • the rectification of column vapour provided by this nitrogen rich reflux stream allows the temperature differential between the overhead vapour stream (213) and the liquid hydrocarbon stream (207) to be increased to 35.3 °C, and the temperature differential between the nitrogen rich overhead vapour stream (213) and the feed (205) to the column to be increased to 23.3 °C, reflective of the increased purity of the nitrogen rich overhead vapour stream (213).
  • Example 1 in contrast, where no nitrogen rich reflux stream is provided, the temperature differential between the column overhead vapour stream (213) and the liquid hydrocarbon stream (207) is only 10.3 °C, and the temperature differential between the column overhead vapour stream (213) and the feed (205) to the column is negligible at 0.3 °C, reflective of much poorer separation.
  • Table 3 shows corresponding corresponding operating data for the separation of nitrogen from the LNG feed used in Example 1 , at a mass flow rate of 200,000 kg/h, according to the process of the invention as described in Figure 3.
  • Vapour Fraction (molar) 0.076 Vapour Liquid 1.000 0.000 1.000 1.000
  • Vapour Fraction (molar) 0.024 Vapour Liquid 0.500 Vapour Liquid 1.000
  • the process of the present invention shown in Figure 3 also gives rise to an nitrogen rich overhead vapour stream (313) which comprises 99.5 mol% of nitrogen, and only 0.5 mol% methane (in comparison with 63 mol% nitrogen and 37 mol% methane in the overhead stream (313) in Example 1 ).
  • the improved separation obtained by the process is attributable to rectification of the column vapour by the low temperature nitrogen rich reflux stream (327), which is obtained at -191.6 °C and supplied to the column at a temperature 24.2 °C below the feed (205) to the column.
  • This in turn means that the temperature differential between the nitrogen rich overhead vapour stream (313) and the liquid hydrocarbon stream (307) is increased to 33.6 °C, and the temperature differential between the nitrogen rich overhead vapour stream (313) and the feed (205) to the column is increased to 23.5 °C, reflecting the increased purity of the nitrogen rich overhead vapour stream.
  • the LNG feed used in the process of the present invention may undergo additional separation and/or conditioning.
  • additional processes include one or more of the following: ⁇ Separation of vapour formed on expansion of the LNG feed stream.
  • the separated vapour may, in a preferred example, then be introduced as a separate feed to the fractionation column, and more preferably to the fractionation column above the main feed; ⁇ Heating a portion of the LNG feed stream and introducing it as a separate feed to the fractionation column, preferably above the main feed.
  • the portion of the stream is preferably heated by way of a well integrated heat exchange operation; • Cooling a portion of the LNG feed stream and introducing it as a separate feed to the fractionation column, preferably above the main feed.
  • the portion of the stream is preferably heated by way of a well integrated heat exchange operation.
  • the fractionation column may additionally comprise or incorporate a side condenser system.
  • a vapour side draw is taken from an intermediate point, preferably above the main LNG feed to the fractionation column.
  • the vapour side draw is warmed in a heat exchange operation; compressed and cooled; condensed primarily against an evaporating liquid stream rich in methane and sub-cooled against cold vapour in a heat exchange operation; expanded to the fractionation column pressure; and returned to the fractionation column as an intermediate two phase feed.
  • vapour side draw comprises a mixture of methane and nitrogen
  • it can be condensed against methane rich liquid streams at a lower pressure than can the overhead stream from the fractionation column, which is purer in nitrogen.
  • compression power requirements overall can be reduced.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
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  • 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 des procédés et des appareils permettant d'extraire de l'azote présent dans des alimentations en gaz naturel liquéfié. Les procédés comprennent les étapes consistant : (i) à refroidir l'alimentation et faire passer l'alimentation dans une colonne de fractionnement ; (ii) à retirer de la colonne de fractionnement un courant de vapeur de tête ayant une teneur en azote enrichie, et un courant de liquide ayant une teneur en azote réduite ; (iii) à diviser le courant de vapeur de tête provenant de l'étape (ii) en au moins des premier et second courants de tête ; (iv) à comprimer, refroidir et au moins partiellement condenser au moins le premier courant de tête provenant de l'étape (iii) ; et (v) à détendre le courant provenant de l'étape (iv) et faire passer le courant détendu dans la colonne de fractionnement en tant que reflux. Un refroidissement est prévu à l'étape (iv), au moins en partie, par échange de chaleur avec un ou plusieurs courants provenant de la colonne de fractionnement.
EP10787542.9A 2009-11-30 2010-11-30 Procédé et appareil d'extraction d'azote présent dans du gnl Active EP2507567B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0920947A GB2462555B (en) 2009-11-30 2009-11-30 Process and apparatus for separation of Nitrogen from LNG
PCT/GB2010/051997 WO2011064605A2 (fr) 2009-11-30 2010-11-30 Procédé et appareil d'extraction d'azote présent dans du gnl

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EP2507567A2 true EP2507567A2 (fr) 2012-10-10
EP2507567B1 EP2507567B1 (fr) 2020-06-24

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AU (3) AU2010322827A1 (fr)
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Publication number Publication date
AU2010322827A1 (en) 2012-06-21
AU2016244250A1 (en) 2016-11-03
GB2462555A (en) 2010-02-17
EP2507567B1 (fr) 2020-06-24
US20120285196A1 (en) 2012-11-15
GB0920947D0 (en) 2010-01-13
AU2018204827A1 (en) 2018-07-19
WO2011064605A2 (fr) 2011-06-03
GB2462555B (en) 2011-04-13
WO2011064605A3 (fr) 2013-04-04

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