US3596472A - Process for liquefying natural gas containing nitrogen - Google Patents

Process for liquefying natural gas containing nitrogen Download PDF

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US3596472A
US3596472A US784124A US3596472DA US3596472A US 3596472 A US3596472 A US 3596472A US 784124 A US784124 A US 784124A US 3596472D A US3596472D A US 3596472DA US 3596472 A US3596472 A US 3596472A
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natural gas
nitrogen
circuit
rectifying zone
expanded
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Martin Streich
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Messer Griesheim GmbH
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Messer Griesheim GmbH
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0211—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
    • F25J1/0217—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 at least a three level refrigeration cascade with at least one MCR cycle
    • F25J1/0218—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 at least a three level refrigeration cascade with at least one MCR cycle with one or more SCR cycles, e.g. with a C3 pre-cooling cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0022—Hydrocarbons, e.g. natural gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/004—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by flash gas recovery
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/0045—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 vaporising a liquid return stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0047—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle
    • F25J1/0052—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle by vaporising a liquid refrigerant stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/006—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the refrigerant fluid used
    • F25J1/007—Primary atmospheric gases, mixtures thereof
    • F25J1/0072—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
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    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0211—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle
    • F25J1/0214—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle as a dual level refrigeration cascade with at least one MCR cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0211—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle
    • F25J1/0219—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle in combination with an internal quasi-closed refrigeration loop, e.g. using a deep flash recycle loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • 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
    • F25J2200/50—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
    • F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/94—Details relating to the withdrawal point
    • 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
    • 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
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/60—Closed external refrigeration cycle with single component refrigerant [SCR], e.g. C1-, C2- or C3-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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/34—Details about subcooling of liquids
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/927—Natural gas from nitrogen

Definitions

  • the liquefied gas is distilled into three fractions: nitrogen, a mixture of nitrogen and methane, and liquid natural gas subatantially free of nitrogen.
  • the mllxture of nitrogen and methane provides the refrigerant in a third and coldest open circuit of the cascade system to subceol the liquid natural gas to storage temperature.
  • This.invention relates to a process for the liquefaction of natural gas containing nitrogen. in countercurrent heat exchangers by means of closed circuits of multicomponent refrigerant mixtures, arranged in cascade manner.
  • Dutch patent 108,678 discloses that natural gas can be cooled this way down to its storage temperature, approximately -l60 C.
  • natural gas having an appreciable content of nitrogen is cooled, liquefied and subcooled in countercurrent heat exchangers which include closed circuits of multicomponent refrigerant mixtures, arranged in cascade manner, each circuit going through only one pressure stage.
  • the lower-boiling inert components, particularly nitrogen are removed therefrom by distillation in a column.
  • an at least partially gaseous mixture of methane and nitrogen is withdrawn from the column, liquefied by heat exchange with the multicomponent refrigerant mixture of the colder closed circuit in the cascadesystem, subcooled against itself in expanded condition, and finally expanded; this expanded stream then subcools the liquefied natural gas and is desirably also used to cool the vapor in the top portion ofthe column.
  • the gaseous mixture of the added and coldest refrigeration circuit in the cascade system can be used for the generation of heat and energy. Inasmuch as this added circuit is an open circuit, no compressor is needed and thereby-investment and operating costs are reduced.
  • the multicomponent refrigerant mixture of the colder closed circuit is first cooled in the sump of the nitrogen distillation column. Then, it is expanded and used to subcool the liquefied natural gas to a temperature of about l40 C. If desired, before expanding the refrigerant mixture of the colder closed circuit, it may be further cooled by passage through a coil in the middle portion of the distillation column. l-Urthermore, the nitrogen withdrawn from the top of the column and the vent gas from the liquid natural gas storage tank can be utilized as sources of refrigeration in the heat exchangers used to liquefy and sub cool the liquefied natural gas.
  • each of the multicomponent refrigerant mixtures in the closed circuits is advantageous to expand to a pressure between about 3 and 5 atmospheres ab solute instead of atmospheric pressure since, in this way, the pressure drop in the circuit is smaller, i.e.. energy is saved and less heat exchanger surface is needed.
  • Natural gas with an appreciable content of nitrogen is supplied through line 1 at high pressure and approximately ambient temperature to heat exchangers 2 and 3 wherein it is cooled and liquefied. Thence, the liquefied natural gas flows through first sump coil 5 to heat the liquid in the sump of nitrogen distillation column 6, and thereby to be further cooled. it is then expanded through expansion valve '7 and discharged into column 6.
  • Column 6 operates at a pressure of 14 atmospheres absolute. Therein, the natural gas is separated into three fractions. Substantially nitrogen-free, liquid natural gas is withdrawn from the sump of column 6. Substantially pure nitrogen is withdrawn from the top of column ti.
  • a mixed methane and nitrogen fraction is withdrawn, its volume and composition being controlled so as to cool the liquid methane to a storage temperature of --l60 C.
  • the nitrogen-free liquid natural gas is withdrawn from the sump of column 6 through line 8 and fiows through the two heat exchangers t and 9 where it is subcooled to 160 C. Thereafter, the liquid natural gas is expanded and discharged into a storage tank.
  • the first and warmer closed circuit supplies practically all the refrigeration needed between ambient temperature and approximately 75 C. in this circuit, the refrigerant mixture of methane, ethane, propane and butane is completely liquefied at ambient temperature when compressed to 42 atmospheres absolute.
  • This mixture is compressed to 42 atmospheres absolute by compressor 10, is completely liquefied in cooler 11 by means of cooling water, and flows through line 12 into heat exchanger 2 wherein it is subcooled against itself after having been expanded.
  • this refrigerant mixture trans fers its refrigeration to the natural gas and the refrigerant mixture of the second and colder closed circuit passing through heat exchanger 2.
  • Line 14 returns the refrigerant of the first circuit from heat exchanger 2 to compressor 10 and thus closes the circuit.
  • the multicomponent refrigerant mixture of the second and colder closed circuit flows through line 15 and heat exchangers 2 and 3 whereby it is cooled and liquefied.
  • This liquid then flows through second sump coil 16 in column s and through heat exchanger 4.
  • the thus subcooled liquid is expanded in expansion valve 17 and passed through line to which extends successively through heat exchangers t, 3 and 2, whereby the mixture is warmed to ambient temperature.
  • Line 118 returns the warmed mixture to compressor 119 where it is again compressed and, after flowing through water cooler 20, passes through line 15.
  • the refrigerant mixture of the second circuit can transfer practically no refrigeration below C. to the natural gas. it is possible, but thermodynamically not favorable, to extend the operation of this second circuit over an even greater temperature range.
  • the second circuit is followed by a third circuit in the cascade arrangement.
  • This third circuit which is open operates with a mixture of nitrogen and methane to supply the natural gas with refrigeration between 145 C. and C., needed for subcooling.
  • the methane and nitrogen mixture for this added circuit is withdrawn from the middle portion of column ti, liquefied against the expanded, evaporating refrigerant mixture of the second circuit and, after expansion, vaporized by heat exchange with the natural gas.
  • refrigeration is essentially supplied by a three-circuit cascade system with the following characteristics:
  • a gaseous mixture of methane and nitrogen is withdrawn from column 6 through line 21 and liquefied in heat exchanger 4 with refrigeration from the second circuit.
  • the liquid then flows through heat exchanger 9 where it is subcooled, and through expansion valve 22 where it is expanded to 3.8 atmospheres absolute.
  • This expanded stream gives up a part of its refrigeration in cooling coil 23 of column 6 in order to produce reflux.
  • This stream passes through line 24 back to heat exchanger 9 where it gives up the greater part of its refrigeration to subcool the liquid natural gas to -l60 C. it then continues to flow through heat exchangers 4, 3 and 2. whereby it is heated to ambient temperature and subsequently utilized for the generation of heat and energy.
  • the process of this invention permits an advantageous combination of nitrogen removal from the natural gas, which is highly desirable, and a third circuit in a cascade system. It would be thennodynamically unfavorable to extend the temperature ranges of the first two closed circuits too much. This is avoided by the present invention without necessitating an extra compressor and its control and regulating devices for an additional refrigeration circuit.
  • a process for liquefying natural gas containing nitrogen and supplied at high pressure which comprises cooling and liquefying said natural gas by countercurrent heat exchange with two closed refrigeration circuits in cascade arrangement,
  • each of said closed circuits having a multicomponent refrigerant mixture which undergoes a single expansion, expanding the liquefied natural gas and discharging it into a rectifying zone maintained at an intermediate pressure.
  • withdrawing an at least partially gaseous mixture of nitrogen and methane from the middle portion of said rectifying zone to provide the refrigerant mixture for a third and coldest open circuit in said cascade arrangement withdrawing liquefied natural gas substantially free of nitrogen from the bottom of said rectifying zone and subcooling it to storage temperature by countercurrent heat exchange with said open circuit.
  • each of the two multicomponent refrigerant mixtures is expanded to a pressure higher than 2 atmospheres atmospheres absolute.
  • each of the two multicomponent refrigerant mixtures is made up of components of the natural gas containing nitrogen.

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US784124A 1967-12-20 1968-12-16 Process for liquefying natural gas containing nitrogen Expired - Lifetime US3596472A (en)

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DE19671551611 DE1551611C3 (de) 1967-12-20 1967-12-20 Verfahren zum Verflüssigen von Erdgas

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US3818714A (en) * 1971-03-04 1974-06-25 Linde Ag Process for the liquefaction and subcooling of natural gas
US3914949A (en) * 1971-02-19 1975-10-28 Chicago Bridge & Iron Co Method and apparatus for liquefying gases
US3964891A (en) * 1972-09-01 1976-06-22 Heinrich Krieger Process and arrangement for cooling fluids
US3970441A (en) * 1973-07-17 1976-07-20 Linde Aktiengesellschaft Cascaded refrigeration cycles for liquefying low-boiling gaseous mixtures
US4112700A (en) * 1974-08-09 1978-09-12 Linde Aktiengesellschaft Liquefaction of natural gas
US4312652A (en) * 1978-10-09 1982-01-26 Linde Aktiengesellschaft Separation system
US4456460A (en) * 1982-03-10 1984-06-26 Flexivol, Inc. Process for recovering ethane, propane and heavier hydrocarbons from a natural gas stream
US4597788A (en) * 1982-03-10 1986-07-01 Flexivol, Inc. Process for recovering ethane, propane and heavier hydrocarbons from a natural gas stream
US4732583A (en) * 1984-12-03 1988-03-22 Phillips Petroleum Company Gas separation
US4738699A (en) * 1982-03-10 1988-04-19 Flexivol, Inc. Process for recovering ethane, propane and heavier hydrocarbons from a natural gas stream
US4746342A (en) * 1985-11-27 1988-05-24 Phillips Petroleum Company Recovery of NGL's and rejection of N2 from natural gas
US4767428A (en) * 1982-03-10 1988-08-30 Flexivol, Inc. Nitrogen removal system
US4948404A (en) * 1989-08-03 1990-08-14 Phillips Petroleum Company Liquid nitrogen by-product production in an NGL plant
US5390499A (en) * 1993-10-27 1995-02-21 Liquid Carbonic Corporation Process to increase natural gas methane content
WO1995031679A1 (en) * 1994-05-13 1995-11-23 Ppg Industries, Inc. Liquefaction of chlorine or other substances
US6016665A (en) * 1997-06-20 2000-01-25 Exxon Production Research Company Cascade refrigeration process for liquefaction of natural gas
US6070429A (en) * 1999-03-30 2000-06-06 Phillips Petroleum Company Nitrogen rejection system for liquified natural gas
US6199403B1 (en) 1998-02-09 2001-03-13 Exxonmobil Upstream Research Company Process for separating a multi-component pressurizied feed stream using distillation
US6223557B1 (en) 1998-10-22 2001-05-01 Exxonmobil Upstream Research Company Process for removing a volatile component from natural gas
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US20050279133A1 (en) * 2004-06-16 2005-12-22 Eaton Anthony P Semi-closed loop LNG process
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US20080264076A1 (en) * 2007-04-25 2008-10-30 Black & Veatch Corporation System and method for recovering and liquefying boil-off gas
US20090205367A1 (en) * 2008-02-15 2009-08-20 Price Brian C Combined synthesis gas separation and LNG production method and system
WO2009103715A2 (en) * 2008-02-20 2009-08-27 Shell Internationale Research Maatschappij B.V. Method and apparatus for cooling and separating a hydrocarbon stream
US8671699B2 (en) 2005-05-19 2014-03-18 Black & Veatch Holding Company Method and system for vaporizing liquefied natural gas with optional co-production of electricity
US9003829B2 (en) * 2010-05-12 2015-04-14 Linde Aktiengesellschaft Nitrogen removal from natural gas
US20150246859A1 (en) * 2014-02-28 2015-09-03 Fluor Technologies Corporation Configurations and Methods for Nitrogen Rejection, LNG and NGL Production from High Nitrogen Feed Gases
WO2015196295A1 (en) * 2014-06-27 2015-12-30 Rtj Technologies Inc. Method and arrangement for producing liquefied methane gas (lmg) from various gas sources
US20150377551A1 (en) * 2014-06-30 2015-12-31 Black & Veatch Corporation Process and system for removing nitrogen from lng
US9574822B2 (en) 2014-03-17 2017-02-21 Black & Veatch Corporation Liquefied natural gas facility employing an optimized mixed refrigerant system
US9777960B2 (en) 2010-12-01 2017-10-03 Black & Veatch Holding Company NGL recovery from natural gas using a mixed refrigerant
US20180149424A1 (en) * 2013-01-24 2018-05-31 Russell H. Oelfke Liquefied Natural Gas Production
US10113127B2 (en) * 2010-04-16 2018-10-30 Black & Veatch Holding Company Process for separating nitrogen from a natural gas stream with nitrogen stripping in the production of liquefied natural gas
US10139157B2 (en) 2012-02-22 2018-11-27 Black & Veatch Holding Company NGL recovery from natural gas using a mixed refrigerant
US10393430B2 (en) 2015-09-11 2019-08-27 Rtj Technologies Inc. Method and system to control the methane mass flow rate for the production of liquefied methane gas (LMG)
US10436505B2 (en) 2014-02-17 2019-10-08 Black & Veatch Holding Company LNG recovery from syngas using a mixed refrigerant
US10563913B2 (en) 2013-11-15 2020-02-18 Black & Veatch Holding Company Systems and methods for hydrocarbon refrigeration with a mixed refrigerant cycle

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GB8418840D0 (en) * 1984-07-24 1984-08-30 Boc Group Plc Gas refrigeration
AUPM485694A0 (en) * 1994-04-05 1994-04-28 Bhp Petroleum Pty. Ltd. Liquefaction process
FR2743140B1 (fr) * 1995-12-28 1998-01-23 Inst Francais Du Petrole Procede et dispositif de liquefaction en deux etapes d'un melange gazeux tel qu'un gaz naturel
DE19716415C1 (de) * 1997-04-18 1998-10-22 Linde Ag Verfahren zum Verflüssigen eines Kohlenwasserstoff-reichen Stromes
FR2778232B1 (fr) * 1998-04-29 2000-06-02 Inst Francais Du Petrole Procede et dispositif de liquefaction d'un gaz naturel sans separation de phases sur les melanges refrigerants
MY117548A (en) * 1998-12-18 2004-07-31 Exxon Production Research Co Dual multi-component refrigeration cycles for liquefaction of natural gas
US8020406B2 (en) 2007-11-05 2011-09-20 David Vandor Method and system for the small-scale production of liquified natural gas (LNG) from low-pressure gas
GB2469077A (en) * 2009-03-31 2010-10-06 Dps Bristol Process for the offshore liquefaction of a natural gas feed
EP2641042A1 (en) * 2010-11-16 2013-09-25 Praxair Technology, Inc. System and method for cryogenic cooling of a process stream with enhanced recovery of refrigeration
DE102011010633A1 (de) * 2011-02-08 2012-08-09 Linde Ag Verfahren zum Abkühlen eines ein- oder mehrkomponentigen Stromes
US10935312B2 (en) * 2018-08-02 2021-03-02 Air Products And Chemicals, Inc. Balancing power in split mixed refrigerant liquefaction system
CN109631492A (zh) * 2018-12-13 2019-04-16 西安石油大学 一种采用混合冷剂级联的天然气液化装置及方法

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Cited By (61)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3914949A (en) * 1971-02-19 1975-10-28 Chicago Bridge & Iron Co Method and apparatus for liquefying gases
US3818714A (en) * 1971-03-04 1974-06-25 Linde Ag Process for the liquefaction and subcooling of natural gas
US3964891A (en) * 1972-09-01 1976-06-22 Heinrich Krieger Process and arrangement for cooling fluids
US3970441A (en) * 1973-07-17 1976-07-20 Linde Aktiengesellschaft Cascaded refrigeration cycles for liquefying low-boiling gaseous mixtures
US4112700A (en) * 1974-08-09 1978-09-12 Linde Aktiengesellschaft Liquefaction of natural gas
US4312652A (en) * 1978-10-09 1982-01-26 Linde Aktiengesellschaft Separation system
US4456460A (en) * 1982-03-10 1984-06-26 Flexivol, Inc. Process for recovering ethane, propane and heavier hydrocarbons from a natural gas stream
US4597788A (en) * 1982-03-10 1986-07-01 Flexivol, Inc. Process for recovering ethane, propane and heavier hydrocarbons from a natural gas stream
US4738699A (en) * 1982-03-10 1988-04-19 Flexivol, Inc. Process for recovering ethane, propane and heavier hydrocarbons from a natural gas stream
US4767428A (en) * 1982-03-10 1988-08-30 Flexivol, Inc. Nitrogen removal system
US4732583A (en) * 1984-12-03 1988-03-22 Phillips Petroleum Company Gas separation
US4746342A (en) * 1985-11-27 1988-05-24 Phillips Petroleum Company Recovery of NGL's and rejection of N2 from natural gas
US4948404A (en) * 1989-08-03 1990-08-14 Phillips Petroleum Company Liquid nitrogen by-product production in an NGL plant
US5390499A (en) * 1993-10-27 1995-02-21 Liquid Carbonic Corporation Process to increase natural gas methane content
WO1995012100A1 (en) * 1993-10-27 1995-05-04 Liquid Carbonic Corporation Process to increase natural gas methane content
US5490390A (en) * 1994-05-13 1996-02-13 Ppg Industries, Inc. Liquefaction of chlorine or other substances
WO1995031679A1 (en) * 1994-05-13 1995-11-23 Ppg Industries, Inc. Liquefaction of chlorine or other substances
US6016665A (en) * 1997-06-20 2000-01-25 Exxon Production Research Company Cascade refrigeration process for liquefaction of natural gas
US6199403B1 (en) 1998-02-09 2001-03-13 Exxonmobil Upstream Research Company Process for separating a multi-component pressurizied feed stream using distillation
US6223557B1 (en) 1998-10-22 2001-05-01 Exxonmobil Upstream Research Company Process for removing a volatile component from natural gas
US6070429A (en) * 1999-03-30 2000-06-06 Phillips Petroleum Company Nitrogen rejection system for liquified natural gas
WO2002088612A1 (de) * 2001-05-02 2002-11-07 Linde Aktiengesellschaft Verfahren zum abtrennen von stickstoff aus einer stickstoff-enthaltenden, kohlenwasserstoff-reichen fraktion
AU2002319155B2 (en) * 2001-05-02 2007-03-29 Linde Antiengesellschaft Method for separating nitrogen out of a hydrocarbon-rich fraction that contains nitrogen
WO2006009610A3 (en) * 2004-06-16 2006-02-23 Conocophillips Co Semi-closed loop lng process
US20080256976A1 (en) * 2004-06-16 2008-10-23 Conocophillips Company Semi-closed loop lng process
US20050279133A1 (en) * 2004-06-16 2005-12-22 Eaton Anthony P Semi-closed loop LNG process
US9651300B2 (en) 2004-06-16 2017-05-16 Conocophillips Company Semi-closed loop LNG process
EA013234B1 (ru) * 2004-06-16 2010-04-30 Конокофиллипс Компани Полузакрытый способ получения сжиженного природного газа
US7866184B2 (en) 2004-06-16 2011-01-11 Conocophillips Company Semi-closed loop LNG process
WO2006094969A1 (en) * 2005-03-09 2006-09-14 Shell Internationale Research Maatschappij B.V. Method for the liquefaction of a hydrocarbon-rich stream
US20080173043A1 (en) * 2005-03-09 2008-07-24 Sander Kaart Method For the Liquefaction of a Hydrocarbon-Rich Stream
AU2006222005B2 (en) * 2005-03-09 2009-06-18 Shell Internationale Research Maatschappij B.V. Method for the liquefaction of a hydrocarbon-rich stream
US8671699B2 (en) 2005-05-19 2014-03-18 Black & Veatch Holding Company Method and system for vaporizing liquefied natural gas with optional co-production of electricity
US8650906B2 (en) 2007-04-25 2014-02-18 Black & Veatch Corporation System and method for recovering and liquefying boil-off gas
US20080264076A1 (en) * 2007-04-25 2008-10-30 Black & Veatch Corporation System and method for recovering and liquefying boil-off gas
US20090205367A1 (en) * 2008-02-15 2009-08-20 Price Brian C Combined synthesis gas separation and LNG production method and system
US9243842B2 (en) 2008-02-15 2016-01-26 Black & Veatch Corporation Combined synthesis gas separation and LNG production method and system
WO2009103715A2 (en) * 2008-02-20 2009-08-27 Shell Internationale Research Maatschappij B.V. Method and apparatus for cooling and separating a hydrocarbon stream
WO2009103715A3 (en) * 2008-02-20 2014-10-02 Shell Internationale Research Maatschappij B.V. Method and apparatus for cooling and separating a hydrocarbon stream
US20100307193A1 (en) * 2008-02-20 2010-12-09 Marco Dick Jager Method and apparatus for cooling and separating a hydrocarbon stream
US10113127B2 (en) * 2010-04-16 2018-10-30 Black & Veatch Holding Company Process for separating nitrogen from a natural gas stream with nitrogen stripping in the production of liquefied natural gas
US9003829B2 (en) * 2010-05-12 2015-04-14 Linde Aktiengesellschaft Nitrogen removal from natural gas
AU2011201487B2 (en) * 2010-05-12 2016-03-03 Linde Aktiengesellschaft Nitrogen removal from natural gas
US9777960B2 (en) 2010-12-01 2017-10-03 Black & Veatch Holding Company NGL recovery from natural gas using a mixed refrigerant
US10139157B2 (en) 2012-02-22 2018-11-27 Black & Veatch Holding Company NGL recovery from natural gas using a mixed refrigerant
US20180149424A1 (en) * 2013-01-24 2018-05-31 Russell H. Oelfke Liquefied Natural Gas Production
US10563913B2 (en) 2013-11-15 2020-02-18 Black & Veatch Holding Company Systems and methods for hydrocarbon refrigeration with a mixed refrigerant cycle
US10436505B2 (en) 2014-02-17 2019-10-08 Black & Veatch Holding Company LNG recovery from syngas using a mixed refrigerant
US9487458B2 (en) * 2014-02-28 2016-11-08 Fluor Corporation Configurations and methods for nitrogen rejection, LNG and NGL production from high nitrogen feed gases
US20170023293A1 (en) * 2014-02-28 2017-01-26 Fluor Technologies Corporation Configurations and methods for nitrogen rejection, lng and ngl production from high nitrogen feed gases
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US20150246859A1 (en) * 2014-02-28 2015-09-03 Fluor Technologies Corporation Configurations and Methods for Nitrogen Rejection, LNG and NGL Production from High Nitrogen Feed Gases
US9574822B2 (en) 2014-03-17 2017-02-21 Black & Veatch Corporation Liquefied natural gas facility employing an optimized mixed refrigerant system
US20170102182A1 (en) * 2014-06-27 2017-04-13 Rtj Technologies Inc. Method and arrangement for producing liquefied methane gas (lmg) from various gas sources
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US10240863B2 (en) * 2014-06-27 2019-03-26 Rtj Technologies Inc. Method and arrangement for producing liquefied methane gas (LMG) from various gas sources
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US20150377551A1 (en) * 2014-06-30 2015-12-31 Black & Veatch Corporation Process and system for removing nitrogen from lng
US10443930B2 (en) * 2014-06-30 2019-10-15 Black & Veatch Holding Company Process and system for removing nitrogen from LNG
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US10393430B2 (en) 2015-09-11 2019-08-27 Rtj Technologies Inc. Method and system to control the methane mass flow rate for the production of liquefied methane gas (LMG)

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GB1181049A (en) 1970-02-11
GB1208196A (en) 1970-10-07
SU476766A3 (ru) 1975-07-05
FR1596088A (nl) 1970-06-15
NL6818394A (nl) 1969-06-24
NL160078C (nl) 1979-09-17
DE1551611A1 (de) 1970-04-16
DE1551611B2 (de) 1975-08-21
NL160078B (nl) 1979-04-17

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