US3797261A - Single-stage fractionation of natural gas containing nitrogen - Google Patents

Single-stage fractionation of natural gas containing nitrogen Download PDF

Info

Publication number
US3797261A
US3797261A US00142299A US3797261DA US3797261A US 3797261 A US3797261 A US 3797261A US 00142299 A US00142299 A US 00142299A US 3797261D A US3797261D A US 3797261DA US 3797261 A US3797261 A US 3797261A
Authority
US
United States
Prior art keywords
nitrogen
natural gas
fraction
distillation zone
stages
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US00142299A
Other languages
English (en)
Inventor
F Juncker
J Kranz
M Streich
H Tanz
G Vollrath
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.)
Linde GmbH
Original Assignee
Linde GmbH
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 Linde GmbH filed Critical Linde GmbH
Application granted granted Critical
Publication of US3797261A publication Critical patent/US3797261A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

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
    • F25J3/028—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 noble gases
    • F25J3/029—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 noble gases of helium
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/04—Purification; Separation; Use of additives by distillation
    • 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
    • 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
    • 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
    • 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
    • F25J2240/12—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream the fluid being 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/02—Internal 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
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
    • F25J2270/06—Internal refrigeration with work-producing gas expansion loop with multiple gas expansion loops
    • 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
    • F25J2270/60—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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/66—Closed external refrigeration cycle with multi component refrigerant [MCR], e.g. mixture of hydrocarbons
    • 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

  • ABSTRACT Separation of natural gas containing nitrogen into a low-nitrogen fraction and a high-nitrogen fraction is achieved in a single distillation column in which reflux is provided by expanding the high-nitrogen fraction with the performance of work and using the resulting refrigeration to condense vapor in the upper section of the column while additional reflux is provided by vaporizing a recycle medium in heat exchange relation with vapor in the column.
  • Incoming natural gas is passed in heat exchange relation with liquid in the column bottom, further cooled and expanded into the middle section of the column.
  • a helium-rich fraction may be separated from the high-nitrogen fraction.
  • This invention relates to a process for separating natural gas containing nitrogen into a low-nitrogen and a high-nitrogen fraction by low-temperature distillation in a single column.
  • natural gas contains different percentages of nitrogen, carbon dioxide, and heavy hydrocarbons. If the contents of noncombustible components are substantial, it becomes necessary or expedient to separate the noncombustible components prior to transportation or utilization.
  • the customary method for removal of nitrogen is the distillation of natural gas at low temperatures. However, this method is subject to difficulties due to the carbon dioxide in the natural gas.
  • Carbon dioxide has a triple point of "566C and a very low solubility at low temperatures. Therefore, depending on the method, the carbon dioxide may become solid at low temperatures. In known processes, carbon dioxide is therefore separated before the natural gas enters the low-temperature plant. This separation is costly since, for instance, special carbon dioxide adsorbers with regeneration facilities must be provided, and additional energy is required.
  • the reflux required for the distillation is produced'by work-performing expansion of at least the greater part of the high-nitrogen fraction and using the refrigeration produced by this expansion and by vaporization of a recycle medium to condense vapor in the column.
  • the pressure for this process is between IO and 35 ata (atmospheres absolute? and a pressure of approximately 28 ata is preferred. Methane is a preferred recycle medium.
  • the process becomes particularly favorable if the high-nitrogen fraction is expanded in several stages with inter-stage heating.
  • the natural gas entering the plant at high pressure is utilized to heat the column sump before it is expanded into the middle section of the distillation column.
  • the natural gas is also brought into heat exchange relation with vapor in the lower section of the column before being expanded into the column; thus, the reflux,
  • the process of the invention is very well suited for recovering a helium-rich fraction from natural gas containing a worthwhile percentage, say over 0.1 percent, of helium.
  • the head product of the distillation which contains helium, is enriched in two nitrogen condensing stages; in the first stage fractional condensation is carried out by heat exchange with highnitrogen fraction boiling at high pressure, and in the second stage with cold gaseous high-nitrogen fraction at approximately atmospheric pressure from the workperforming expansion of the high-nitrogen fraction. Refrigeration for the second stage can also be supplied by nitrogen evaporating at low pressure. If necessary, the low-nitrogen liquid fraction from the sump of the distillation column may be pumped to higher pressure before being vaporized and heated to ambient temperature.
  • FIG. 1 is a flow diagram of an embodiment of the invention utilizing two-stage expansion of the highnitrogen fraction
  • FIG. 2 is similar to FIG. 1 with additional features for helium recovery.
  • natural gas enters the low-temperature plant through line 1 after removal of moisture in a drier (not shown).
  • the natural gas contains about 43% by volume of nitrogen and 56% by volume of methane, the remainder consisting of heavy hydrocarbons 0.4%m helium 0.4% and carbon dioxide 0.2%.
  • the gas pressure is 55 ata.
  • the natural gas is cooled by counter-current flow to the separation fractions. Then it flows through vaporizer 3 in the bottom of distillation column 4 and thus .it provides part of the vapor upflow required in column 4.
  • the natural gas is then further cooled by flowing through subcooler 5 and coil .6 in. the lower section of column 4 where it produces more vapor upflow and thus improves the rectification conditions. Finally, the subcooled natural gas is expanded through expansion valve 7 into the middle section of column 4 to a pressure of 28 ata.
  • distillation column 4 the natural gas is separated into a high-nitrogen mixture at the head of column 4 and a low-nitrogen mixture at the bottom of column 4.
  • the high-nitrogen mixture is withdrawn in gaseous state through line 8, somewhat heated in heat exchanger 9, and! expanded in workperforming turbine 10 to a medium pressure of about 6 ata. Then it is reheated in heat exchanger 11 against condensing vapors of the high-nitrogen mixture, further expanded in turbine 12 to about atmospheric pressure and once again heated in heat exchanger 13 against condensing vapors of the high-nitrogen mixture. After further heating in heat exchangers 9, 5, and 2, the high-nitrogen fraction is finally available at the plant outlet at ambient temperature.
  • Liquid high-nitrogen mixture from the column head can be expanded through line 14 into storage vessel 15 where it is separated into a liquid and a gaseous phase.
  • the gaseous phase is withdrawn through line 18 and fed through valve 19 into the discharge line of turbine 10.
  • the liquid phase is Withdrawn through line 16 and expanded through expansion valve 17 into the discharge line of turbine 12. This is necessary only in case of a sudden need for refrigeration in column 4, for instance in case of a sudden rise in pressure in column 4.
  • the liquid from storage vessel 15 will then supply the necessary additional refrigeration.
  • the low-nitrogen mixture is withdrawn from the sump of column 4 through line 20, pressurized by pump 21 to the inlet pressure of 55 ata of the natural gas and heated in heat exchanger 2 to ambient temperature.
  • the refrigeration supplied by expansion of the gas in turbines l0, 12 is not enough to produce sufficient reflux for the complete fractionation of the natural gas. Therefore, a recycle medium is provided to improve the reflux conditions.
  • the preferred recycle medium or gas is methane; however a mixture of nitrogen and light hydrocarbons may also be used.
  • the recycle gas is compressed froin a'pr'e'sgur'bfabom 2 ata t o apressii re which is higher than the pressure of distillation column Since, in the present example, the recycle medium is also to take refrigeration from the returning lownitrogen fraction in line 20, it is compressed to 55 ata.
  • the recycle gas After flowing through after-cooler 23, it is cooled in heat exchanger 2 against itself and the returning fractions. Then, in heat exchanger 24, the recycle gas heats the liquid in the column sump, and in heat exchangers 5 and 9 it is subcooled. After expansion to 2 ata in expansion valve 25, it evaporates in heat exchanger 236, at least to a great extent. Consequently, with heat exchanger 26, the recycle medium also produces reflux in column 4. In heat exchangers 9, 5 and 2, the recycle gas is reheated to approximately ambient temperature. Since expansion of the high-nitrogen fraction in workperforming turbines 10 and 12 supplies a lot of refrigeration, the recycle gas may be discharged from the lowtemperature plant at a relatively low temperature. In compressor 22, the recycle gas may then be compressed cold, i.e., with less energy consumption. Preferably, the recycle gas is fed into compressor 22 at a temperature of about 35C since, at that temperature, it is not necessary to use special materials for compressor 22.
  • FIG. 2 illustrates the process with the additional recovery of helium.
  • Identical plant components have been marked with identical reference numerals from FIG. 1 and the process will be described only insofar as it differs from the process shown in FIG. 1.
  • the head of distillation column 4 is provided with an additional condenser 27 where the highnitrogen vapor mixture rising from heat exchanger 11 is extensively liquefied.
  • the gas withdrawn above condenser 27 through line 28 already contains 5 to 10 percent by volume of helium.
  • this vapor mixture is further concentrated by partial condensation to 80 to 90 percent by volume of helium.
  • the helium vapor concentrate is withdrawn through line 30, while the nitrogen condensate is returned to column 4 by line 32.
  • the concentration of helium is accomplished in two stages.
  • the refrigeration for first-stage condenser 27 is supplied by evaporating the high-nitrogen liquid mixture which is withdrawn from column 4 through line 14, expanded to 24 ata in expansion valve 31 and discharged into condenser 27.
  • the resulting high-nitrogen vapor mixture is then conducted through turbines l0 and 12 as already described for FIG. 1.
  • the refrigeration for the concentration second-stage heat exchanger 29 is supplied by the cold high-nitrogen vapor mixture from turbine 12, which is subsequently heated to ambient temperature as described for FIG. 1.
  • the refrigeration for the second concentration stage may also be supplied by high-nitrogen liquid mixture evaporating at low pressure.
  • Heat exchangers 24, 3, 6, 26, 13 and 11 may also be located outside column 4 as plate heat exchangers.
  • the process of this invention avoids very low temperatures for the natural gas and for the low-nitrogen product fraction. Furthermore, the natural gas evaporates at high pressure. Thus, it is possible to tolerate higher percentages of heavy hydrocarbons in the natural gas without entailing deposits and plugging. Conditions are similar where carbon dioxide is concerned. The carbon dioxide passes through the plant without being deposited anywhere. The costly pre-puriflcation of the natural gas is thus avoided.
  • a process for the separation of natural gas containing nitrogen into a low-nitrogen fraction and a highnitrogen fraction in a single distillation Zone which comprises expanding at least the greater part of said high-nitrogen fraction with the performance of work, using the resulting refrigeration to condense vapor of the upper section of said distillation zone to provide reflux in said distillation zone, and providing additional reflux below the aforesaid reflux by vaporizing a closed recycle liquefied gas in indirect heat exchange relation with vapor of said distillation zone after said recycle gas has been passed in indirect heat exchange relation with liquid while the said liquid is at the bottom of said distillation zone.
US00142299A 1970-05-12 1971-05-11 Single-stage fractionation of natural gas containing nitrogen Expired - Lifetime US3797261A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE2022954A DE2022954C3 (de) 1970-05-12 1970-05-12 Verfahren zur Zerlegung von stickstoffhaltigem Erdgas

Publications (1)

Publication Number Publication Date
US3797261A true US3797261A (en) 1974-03-19

Family

ID=5770782

Family Applications (1)

Application Number Title Priority Date Filing Date
US00142299A Expired - Lifetime US3797261A (en) 1970-05-12 1971-05-11 Single-stage fractionation of natural gas containing nitrogen

Country Status (3)

Country Link
US (1) US3797261A (ja)
JP (1) JPS4926682B1 (ja)
DE (1) DE2022954C3 (ja)

Cited By (36)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4017283A (en) * 1971-11-17 1977-04-12 Sulzer Brothers Limited Method and plant for making up nitrogen vaporization losses in nitrogen-containing liquified natural gas carrying tankers
US4251249A (en) * 1977-01-19 1981-02-17 The Randall Corporation Low temperature process for separating propane and heavier hydrocarbons from a natural gas stream
US4400188A (en) * 1981-10-27 1983-08-23 Air Products And Chemicals, Inc. Nitrogen generator cycle
US4411677A (en) * 1982-05-10 1983-10-25 Air Products And Chemicals, Inc. Nitrogen rejection from natural gas
EP0131128A1 (en) * 1983-06-01 1985-01-16 Air Products And Chemicals, Inc. Nitrogen rejection from natural gas integrated with NGL recovery
US4592767A (en) * 1985-05-29 1986-06-03 Union Carbide Corporation Process for separating methane and nitrogen
US4662919A (en) * 1986-02-20 1987-05-05 Air Products And Chemicals, Inc. Nitrogen rejection fractionation system for variable nitrogen content natural gas
US4680041A (en) * 1985-12-30 1987-07-14 Phillips Petroleum Company Method for cooling normally gaseous material
US4732598A (en) * 1986-11-10 1988-03-22 Air Products And Chemicals, Inc. Dephlegmator process for nitrogen rejection from natural gas
US5041149A (en) * 1990-10-18 1991-08-20 Union Carbide Industrial Gases Technology Corporation Separation of nitrogen and methane with residue turboexpansion
US5329775A (en) * 1992-12-04 1994-07-19 Praxair Technology, Inc. Cryogenic helium production system
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
US20040182109A1 (en) * 2002-11-19 2004-09-23 Oakey John Douglas Nitrogen rejection method and apparatus
US20110226012A1 (en) * 2009-02-17 2011-09-22 S.M.E. Products Lp Hydrocarbon Gas Processing
US20110226011A1 (en) * 2010-03-31 2011-09-22 S.M.E. Products Lp Hydrocarbon Gas Processing
US20110226014A1 (en) * 2010-03-31 2011-09-22 S.M.E. Products Lp Hydrocarbon Gas Processing
US20110226013A1 (en) * 2010-03-31 2011-09-22 S.M.E. Products Lp Hydrocarbon Gas Processing
US20110232328A1 (en) * 2010-03-31 2011-09-29 S.M.E. Products Lp Hydrocarbon Gas Processing
US20140318177A1 (en) * 2011-10-06 2014-10-30 Rustam H. Sethna Integration of a liquefied natural gas liquefier with the production of liquefied natural gas
US9021831B2 (en) 2009-02-17 2015-05-05 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9080811B2 (en) 2009-02-17 2015-07-14 Ortloff Engineers, Ltd Hydrocarbon gas processing
US9637428B2 (en) 2013-09-11 2017-05-02 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9783470B2 (en) 2013-09-11 2017-10-10 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9790147B2 (en) 2013-09-11 2017-10-17 Ortloff Engineers, Ltd. Hydrocarbon processing
US9933207B2 (en) 2009-02-17 2018-04-03 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9939195B2 (en) 2009-02-17 2018-04-10 Ortloff Engineers, Ltd. Hydrocarbon gas processing including a single equipment item processing assembly
US9939196B2 (en) 2009-02-17 2018-04-10 Ortloff Engineers, Ltd. Hydrocarbon gas processing including a single equipment item processing assembly
US20180274854A1 (en) * 2015-12-18 2018-09-27 Bechtel Hydrocarbon Technology Solution, Inc. Systems and Methods for Recovering Desired Light Hydrocarbons from Refinery Waste Gas Using a Back-End Turboexpander
US10215488B2 (en) 2016-02-11 2019-02-26 Air Products And Chemicals, Inc. Treatment of nitrogen-rich natural gas streams
US10533794B2 (en) 2016-08-26 2020-01-14 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US10551119B2 (en) 2016-08-26 2020-02-04 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US10551118B2 (en) 2016-08-26 2020-02-04 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US11428465B2 (en) 2017-06-01 2022-08-30 Uop Llc Hydrocarbon gas processing
US11543180B2 (en) 2017-06-01 2023-01-03 Uop Llc Hydrocarbon gas processing
US11686528B2 (en) 2019-04-23 2023-06-27 Chart Energy & Chemicals, Inc. Single column nitrogen rejection unit with side draw heat pump reflux system and method

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2772896B1 (fr) * 1997-12-22 2000-01-28 Inst Francais Du Petrole Procede de liquefaction d'un gaz notamment un gaz naturel ou air comportant une purge a moyenne pression et son application
US11221176B2 (en) * 2018-08-14 2022-01-11 Air Products And Chemicals, Inc. Natural gas liquefaction with integrated nitrogen removal

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2583090A (en) * 1950-12-29 1952-01-22 Elliott Co Separation of natural gas mixtures
US2658360A (en) * 1946-05-08 1953-11-10 Chemical Foundation Inc Transportation of natural gas
US2677945A (en) * 1948-01-21 1954-05-11 Chemical Foundation Inc Transportation of natural gas
US2713781A (en) * 1953-10-26 1955-07-26 Mississippi River Fuel Corp Variable reversible rectification process
US2823523A (en) * 1956-03-26 1958-02-18 Inst Gas Technology Separation of nitrogen from methane
US3420068A (en) * 1966-09-13 1969-01-07 Air Liquide Process for the production of a fluid rich in methane from liquefied natural gas under a low initial pressure
US3507127A (en) * 1967-12-26 1970-04-21 Phillips Petroleum Co Purification of nitrogen which contains methane
US3512368A (en) * 1968-01-02 1970-05-19 Phillips Petroleum Co Helium and nitrogen containing fuel product recovery
US3607733A (en) * 1969-04-25 1971-09-21 Phillips Petroleum Co Controlled evaporation in heat exchange zones

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2658360A (en) * 1946-05-08 1953-11-10 Chemical Foundation Inc Transportation of natural gas
US2677945A (en) * 1948-01-21 1954-05-11 Chemical Foundation Inc Transportation of natural gas
US2583090A (en) * 1950-12-29 1952-01-22 Elliott Co Separation of natural gas mixtures
US2713781A (en) * 1953-10-26 1955-07-26 Mississippi River Fuel Corp Variable reversible rectification process
US2823523A (en) * 1956-03-26 1958-02-18 Inst Gas Technology Separation of nitrogen from methane
US3420068A (en) * 1966-09-13 1969-01-07 Air Liquide Process for the production of a fluid rich in methane from liquefied natural gas under a low initial pressure
US3507127A (en) * 1967-12-26 1970-04-21 Phillips Petroleum Co Purification of nitrogen which contains methane
US3512368A (en) * 1968-01-02 1970-05-19 Phillips Petroleum Co Helium and nitrogen containing fuel product recovery
US3607733A (en) * 1969-04-25 1971-09-21 Phillips Petroleum Co Controlled evaporation in heat exchange zones

Cited By (51)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4017283A (en) * 1971-11-17 1977-04-12 Sulzer Brothers Limited Method and plant for making up nitrogen vaporization losses in nitrogen-containing liquified natural gas carrying tankers
US4251249A (en) * 1977-01-19 1981-02-17 The Randall Corporation Low temperature process for separating propane and heavier hydrocarbons from a natural gas stream
US4400188A (en) * 1981-10-27 1983-08-23 Air Products And Chemicals, Inc. Nitrogen generator cycle
US4411677A (en) * 1982-05-10 1983-10-25 Air Products And Chemicals, Inc. Nitrogen rejection from natural gas
EP0094062A2 (en) * 1982-05-10 1983-11-16 Air Products And Chemicals, Inc. Nitrogen rejection from natural gas
EP0094062A3 (en) * 1982-05-10 1985-01-30 Air Products And Chemicals, Inc. Nitrogen rejection from natural gas
EP0131128A1 (en) * 1983-06-01 1985-01-16 Air Products And Chemicals, Inc. Nitrogen rejection from natural gas integrated with NGL recovery
US4504295A (en) * 1983-06-01 1985-03-12 Air Products And Chemicals, Inc. Nitrogen rejection from natural gas integrated with NGL recovery
US4592767A (en) * 1985-05-29 1986-06-03 Union Carbide Corporation Process for separating methane and nitrogen
US4680041A (en) * 1985-12-30 1987-07-14 Phillips Petroleum Company Method for cooling normally gaseous material
US4662919A (en) * 1986-02-20 1987-05-05 Air Products And Chemicals, Inc. Nitrogen rejection fractionation system for variable nitrogen content natural gas
US4732598A (en) * 1986-11-10 1988-03-22 Air Products And Chemicals, Inc. Dephlegmator process for nitrogen rejection from natural gas
US5041149A (en) * 1990-10-18 1991-08-20 Union Carbide Industrial Gases Technology Corporation Separation of nitrogen and methane with residue turboexpansion
US5329775A (en) * 1992-12-04 1994-07-19 Praxair Technology, Inc. Cryogenic helium production system
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
US20040182109A1 (en) * 2002-11-19 2004-09-23 Oakey John Douglas Nitrogen rejection method and apparatus
US7059152B2 (en) * 2002-11-19 2006-06-13 The Boc Group Plc Nitrogen rejection method and apparatus
US9052137B2 (en) * 2009-02-17 2015-06-09 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US20110226012A1 (en) * 2009-02-17 2011-09-22 S.M.E. Products Lp Hydrocarbon Gas Processing
US9939196B2 (en) 2009-02-17 2018-04-10 Ortloff Engineers, Ltd. Hydrocarbon gas processing including a single equipment item processing assembly
US9939195B2 (en) 2009-02-17 2018-04-10 Ortloff Engineers, Ltd. Hydrocarbon gas processing including a single equipment item processing assembly
US9933207B2 (en) 2009-02-17 2018-04-03 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9080811B2 (en) 2009-02-17 2015-07-14 Ortloff Engineers, Ltd Hydrocarbon gas processing
US9021831B2 (en) 2009-02-17 2015-05-05 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9057558B2 (en) * 2010-03-31 2015-06-16 Ortloff Engineers, Ltd. Hydrocarbon gas processing including a single equipment item processing assembly
US20110232328A1 (en) * 2010-03-31 2011-09-29 S.M.E. Products Lp Hydrocarbon Gas Processing
US20110226011A1 (en) * 2010-03-31 2011-09-22 S.M.E. Products Lp Hydrocarbon Gas Processing
US9068774B2 (en) * 2010-03-31 2015-06-30 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9074814B2 (en) * 2010-03-31 2015-07-07 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9052136B2 (en) * 2010-03-31 2015-06-09 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US20110226014A1 (en) * 2010-03-31 2011-09-22 S.M.E. Products Lp Hydrocarbon Gas Processing
US20110226013A1 (en) * 2010-03-31 2011-09-22 S.M.E. Products Lp Hydrocarbon Gas Processing
US20140318177A1 (en) * 2011-10-06 2014-10-30 Rustam H. Sethna Integration of a liquefied natural gas liquefier with the production of liquefied natural gas
US9790147B2 (en) 2013-09-11 2017-10-17 Ortloff Engineers, Ltd. Hydrocarbon processing
US9927171B2 (en) 2013-09-11 2018-03-27 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US10227273B2 (en) 2013-09-11 2019-03-12 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9783470B2 (en) 2013-09-11 2017-10-10 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US9637428B2 (en) 2013-09-11 2017-05-02 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US10793492B2 (en) 2013-09-11 2020-10-06 Ortloff Engineers, Ltd. Hydrocarbon processing
US20180274854A1 (en) * 2015-12-18 2018-09-27 Bechtel Hydrocarbon Technology Solution, Inc. Systems and Methods for Recovering Desired Light Hydrocarbons from Refinery Waste Gas Using a Back-End Turboexpander
AU2015417433B2 (en) * 2015-12-18 2019-08-22 Bechtel Hydrocarbon Technology Solutions, Inc. Systems and methods for recovering desired light hydrocarbons from refinery waste gas using a back-end turboexpander
RU2703249C1 (ru) * 2015-12-18 2019-10-15 Бектел Гидрокарбон Текнолоджи Солушенз, Инк. Системы и способы для извлечения целевых легких углеводородов из газообразных отходов рафинирования с использованием турбодетандера в оконечной части систем
CN108883342A (zh) * 2015-12-18 2018-11-23 贝克特尔碳氢技术解决方案股份有限公司 用于使用后端透平膨胀机从炼油厂废气回收期望的轻质烃的系统和方法
US10215488B2 (en) 2016-02-11 2019-02-26 Air Products And Chemicals, Inc. Treatment of nitrogen-rich natural gas streams
US10533794B2 (en) 2016-08-26 2020-01-14 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US10551119B2 (en) 2016-08-26 2020-02-04 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US10551118B2 (en) 2016-08-26 2020-02-04 Ortloff Engineers, Ltd. Hydrocarbon gas processing
US11428465B2 (en) 2017-06-01 2022-08-30 Uop Llc Hydrocarbon gas processing
US11543180B2 (en) 2017-06-01 2023-01-03 Uop Llc Hydrocarbon gas processing
US11686528B2 (en) 2019-04-23 2023-06-27 Chart Energy & Chemicals, Inc. Single column nitrogen rejection unit with side draw heat pump reflux system and method

Also Published As

Publication number Publication date
DE2022954A1 (de) 1971-12-02
DE2022954C3 (de) 1978-05-18
DE2022954B2 (de) 1977-09-01
JPS4926682B1 (ja) 1974-07-11

Similar Documents

Publication Publication Date Title
US3797261A (en) Single-stage fractionation of natural gas containing nitrogen
US3347055A (en) Method for recuperating refrigeration
RU2215952C2 (ru) Способ разделения потока многокомпонентного исходного материала под давлением путем использования дистилляции
US3780534A (en) Liquefaction of natural gas with product used as absorber purge
RU2224961C2 (ru) Способ удаления летучих компонентов из природного газа
US3818714A (en) Process for the liquefaction and subcooling of natural gas
JP5015674B2 (ja) 空気分離プロセスにおけるｌｎｇベース液化装置の能力増強システム
RU2355960C1 (ru) Двухступенчатый отвод азота из сжиженного природного газа
US3210951A (en) Method for low temperature separation of gaseous mixtures
US4372764A (en) Method of producing gaseous oxygen and a cryogenic plant in which said method can be performed
US4715873A (en) Liquefied gases using an air recycle liquefier
US3886758A (en) Processes for the production of nitrogen and oxygen
US3721099A (en) Fractional condensation of natural gas
US3401531A (en) Heat exchange of compressed nitrogen and liquid oxygen in ammonia synthesis feed gas production
US5509271A (en) Process and installation for the separation of a gaseous mixture
JPH06117753A (ja) 空気の高圧低温蒸留方法
US5735142A (en) Process and installation for producing high pressure oxygen
US4331461A (en) Cryogenic separation of lean and rich gas streams
US5428962A (en) Process and installation for the production of at least one gaseous product under pressure and at least one liquid by distillation of air
US7464568B2 (en) Cryogenic distillation method and system for air separation
US5412953A (en) Process and installation for the production of gaseous oxygen and/or gaseous nitrogen under pressure by distillation of air
US4586942A (en) Process and plant for the cooling of a fluid and in particular the liquefaction of natural gas
US4704147A (en) Dual air pressure cycle to produce low purity oxygen
CN106595221A (zh) 制氧系统和制氧方法
KR20000052974A (ko) 압축 질소를 생성시키는 방법 및 장치