US2567461A - Separation of gaseous mixtures at low temperatures - Google Patents

Separation of gaseous mixtures at low temperatures Download PDF

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Publication number
US2567461A
US2567461A US7747A US774748A US2567461A US 2567461 A US2567461 A US 2567461A US 7747 A US7747 A US 7747A US 774748 A US774748 A US 774748A US 2567461 A US2567461 A US 2567461A
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Prior art keywords
refrigerant
pressure
column
ethylene
fractionating
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Expired - Lifetime
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US7747A
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English (en)
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Aicher Alfred August
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PETROCARBON Ltd
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PETROCARBON Ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—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
    • F25J3/0242—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 3 carbon atoms 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
    • F25J3/0219—Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
    • 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
    • F25J3/0238—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of CnHm with 2 carbon atoms or more
    • 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
    • F25J2200/80—Processes or apparatus using separation by rectification using integrated mass and heat exchange, i.e. non-adiabatic rectification in a reflux exchanger or dephlegmator
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/12—Refinery or petrochemical off-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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/62—Ethane or ethylene
    • 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
    • F25J2270/88—Quasi-closed internal refrigeration or heat pump cycle, if not otherwise provided
    • 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
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration

Definitions

  • This invention relates to the separation of gases by fractionation at low temperatures and more particularly to the supply of cold for the process.
  • the object of the invention is to provide an improved process and apparatus for the supply of cold for the separation of gases by fractionation at low temperatures, especially in such cases in which one or several refrigerants are used and in which different portions of these refrigerants are allowed to evaporate under different pres- :ures and at correspondingly different temperaures.
  • a known method of separating gaseous mixtures is first to cool and partially condense the mixtures and thereafter to pass the mixtures or portions thereof through fractionating towers or columns, each of which is equipped with a condenser at the top and a re-boiler at the bottom.
  • the temperature in the condenser is lower than that in the re-boiler of the same column and heat is extracted from the condenser and supplied to the re-boiler.
  • the extraction of heat at a low temperature requires a source of refrigeration. This source of refrigeration is frequently provided in the form of a separate refrigerating cycle circulating a known refrigerant.
  • the other part of the refrigerant, which is not evaporated at the intermediate pressure, is expanded to a lower pressure and there made to evaporate, thus performing a duty at a lower temperature, whereupon it is returned through suitable heat exchangers to the suction of a compressor.
  • the invention consists in a process for the separation of gaseous mixtures by fractionation at low temperatures in which cold vapour of a refrigerant which has been condensed at an elevated pressure and expanded to a lower pressure fit which is preferably also higher than 1 atmosphere and which has performed a refrigerating duty by evaporating at this pressure is at least in part reliquefied in the re-boiler of a fractionating column and in which the liquid so formed is thereupon expanded to a still lower pressure and made to perform a further refrigerating duty by evaporating at said still lower presssure.
  • the invention also consists in a process in accordance with the preceding paragraph in which the reliquefied refrigerant, after expansion to the said still lower pressure, is mixed with a portion of the same refrigerant which has been expanded from the intermediate pressure to the same said still lower pressure without having as yet performed a refrigerating duty.
  • the invention also consists in a process in accordance with the next but one preceding paragraph in which the reliquefled refrigerant, after expansion to the said still lower pressure, is mixed with a portion of the same refrigerant which has been expanded directly to this pressure from the initial elevated pressure at which it was liquefied.
  • the invention also consists in a process in accordance with any of the preceding three paragraphs in which the said still lower pressure is not below 1 atmosphere.
  • the invention also consists in a process in accordance with any of the preceding four paragraphs applied to the removal of ethylene or ethane or both from a mixture of hydrocarbon gases containing the same.
  • the accompanying diagrammatic drawing represents an apparatus or plant, which may be used according to one form of the present invention.
  • the mixture which contains hydrogen, methane, ethylene, ethane, propylene, propane, butylene, butane and butadiene, is compressed to a pressure between 4 and 10 atmospheres and cooled and partially condensed in thermal contact with several refrigerants.
  • the methane has been removed in a fractionating tower, the remaining liquid, now containing ethylene, ethane, propylene, propane, butylene, butane and butadiene, is treated for the removal of ethylene and ethane, both s'i'ibstantially pure, in the manner indicated below.
  • the remaining liquid referred to above is fed at intermediate point a to the suction side of a fractionating'column a which operates at 4 atm. pressure, and is here separated into a gaseous overhead containing substantially only ethylene and ethane, and a liquid residue containing all components with boiling points higher than that of ethane.
  • the gaseous overhead leaves at the top of the column and is thereupon condensed in a system of tubes b in the re-boiler of a second column c, expanded in a valve d to approximately 1.5 atm. abs. and fed into the middle point e of the second column c. From this column c, gaseous ethylene is taken as overhead at the top and gaseous ethane as residue from the lower end of the column.
  • the refrigerant which is ethylene
  • the refrigerant which is ethylene
  • a low pressure compressor e and from 4 to 13 atm. in a high pressure compressor 1' It is then pre-cocled in a heat exchanger g with cold ethylene gas returning partly at 4 and partly at 1 atm. pressure.
  • the pro-cooled compressed ethylene is liquefied in a condenser h in thermal contact with evaporating liquid ammonia from a separate refrigerating cycle.
  • the liquid ethylene then separates into two streams.
  • One stream passes through a sub-cooler 1' and expansion valve 7' to a vessel k which is at 4 atm. pressure; the other stream passes through another sub-cooler l and expansion valve m to a vessel n which is at approximately 1 atm. pressure.
  • the liquid ethylene from the vessel n, a part of which has entered from the expansion valve m, and another part after being reliquefled has entered through the expansion valve 1' is evaporated in a reflux condener s of the second fractionating column 0, whence the vapours return to the vessel n and are passed back to the suction side of the low pressure compressor e through the sub-cooler l and heat exchanger g.
  • the bottom t of column a is heated by the reboiler t to the temperature required to boil off the ethylene and ethane while leaving higher boiling components to be withdrawn as residue from the bottom of the tower.
  • three pressures are employed in the process: an elevated pressure, an intermediate pressure and a low pressure. It is not essential for the intermediate pressure to be higher than 1 atmosphere, though it is preferred to operate the plant so that the pressure is never at any point below 1 atmosphere in order to avoid any possibility of air leaking into the plant. Not the whole of the portion of the refrigerant which is evaporated at the intermediate pressure is returned to the suction or to the intermediate stage of the compressor, but instead a part or the whole of this vapour is condensed in thermal contact with the liquid boiling in the re-boiler of a fractionating tower, the temperature of which is lower than the condensing temperature of the refrigerant at the obtaining pressure.
  • liquid refrigerant which has now persuitable heat exchangers to the suction of the compressor.
  • the reliquefled refrigerant on being expanded from the intermediate to the'lower pressure, mixes with another portion of the same refrigerant which has been expanded from the intermediate to the lower pressure without having performed a duty at this intermediate pressure and without having been reliquefled.
  • the reliqueiled refrigerant. after being expanded from the intermediate to the lower pressure may be mixed with a portion of the same refrigerant which has been expanded directly from the initial higher pressure.
  • process of supp ying cold and heat to said condensers and reboilers which comprises passing a compressed and cooled refrigerant liquid in a closed circuit through a reflux condenser of one fractionating column whereby the refrigerant liquid is evaporated and cold supplied to the condenser, passing at least part of the resulting refrigerant vapor through the reboiler of a succeeding fractionating column whereby the refrigerant vapor is condensed and heat is supplied to the reboiler, expanding the thus reliquefled refrigerant to a lower pressure and passing it through the reflux condenser of said succeeding fractionating column, whereby the reliquefled refrigerant is evaporated and cold is supplied to the reflux condenser of said succeeding column.
  • the process of supplying heat and cold to said reboiler and reflux condensers which comprises compressing and liquefying ethylene, passing the liquid ethylene through the reflux condenser of said first column to provide cooling therefor, whereby the liquid ethylene becomes at least partly vaporized, passing at least part of the vaporized ethylene through the reboiler of said second column to supply heat thereto, whereby at least part of the ethylene becomes condensed, reducing the pressure on the so-liquefled ethylene and passing it through the reflux condenser of said second column to supply cooling thereto, and then passing the so-vaporized ethylene back to the compression step of the process.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US7747A 1947-02-19 1948-02-12 Separation of gaseous mixtures at low temperatures Expired - Lifetime US2567461A (en)

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GB4811/47A GB632438A (en) 1947-02-19 1947-02-19 Improvements in and relating to the separation of gaseous mixtures at low temperatures

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BE (1) BE480496A (US07122603-20061017-C00294.png)
FR (1) FR961430A (US07122603-20061017-C00294.png)
GB (1) GB632438A (US07122603-20061017-C00294.png)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2700282A (en) * 1948-02-12 1955-01-25 British Oxygen Co Ltd Fractional separation of air
US2765637A (en) * 1950-10-30 1956-10-09 Air Liquide Frigorific separation process of gas mixture by liquefying and rectifying
US2824433A (en) * 1952-02-29 1958-02-25 Philips Corp Method of separating gas-mixtures in a rectifying column
US3002358A (en) * 1960-08-01 1961-10-03 Shell Oil Co Propylene distillation
US3119677A (en) * 1961-01-16 1964-01-28 Phillips Petroleum Co Separation of gases
US3509728A (en) * 1966-02-22 1970-05-05 Petrocarbon Dev Ltd Low temperature separation of gases utilizing two distillation columns having a common condenser-evaporator
US3581510A (en) * 1968-07-08 1971-06-01 Phillips Petroleum Co Gas liquefaction by refrigeration with parallel expansion of the refrigerant
USRE29914E (en) * 1965-03-31 1979-02-20 Compagnie Francaise D'etudes Et De Construction Technip Method and apparatus for the cooling and low temperature liquefaction of gaseous mixtures
US4218229A (en) * 1977-08-06 1980-08-19 Linde Aktiengesellschaft Separation of ethylene-containing hydrocarbon mixtures by low temperature rectification

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1529625A (en) * 1923-06-15 1925-03-10 Carbide & Carbon Chem Corp Process of recovering helium
US1843043A (en) * 1924-02-13 1932-01-26 Patart Georges Leon Emile Process for the separation of the several components of gaseous mixtures
US2057804A (en) * 1934-05-09 1936-10-20 Lee S Twomey Method of separating the constituents of air
US2146197A (en) * 1936-03-14 1939-02-07 Lee S Twomey Method of and apparatus for separating mixed gases and vapors
US2424201A (en) * 1944-02-19 1947-07-15 Air Reduction Separation of the constituents of gaseous mixtures

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1529625A (en) * 1923-06-15 1925-03-10 Carbide & Carbon Chem Corp Process of recovering helium
US1843043A (en) * 1924-02-13 1932-01-26 Patart Georges Leon Emile Process for the separation of the several components of gaseous mixtures
US2057804A (en) * 1934-05-09 1936-10-20 Lee S Twomey Method of separating the constituents of air
US2146197A (en) * 1936-03-14 1939-02-07 Lee S Twomey Method of and apparatus for separating mixed gases and vapors
US2424201A (en) * 1944-02-19 1947-07-15 Air Reduction Separation of the constituents of gaseous mixtures

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2700282A (en) * 1948-02-12 1955-01-25 British Oxygen Co Ltd Fractional separation of air
US2765637A (en) * 1950-10-30 1956-10-09 Air Liquide Frigorific separation process of gas mixture by liquefying and rectifying
US2824433A (en) * 1952-02-29 1958-02-25 Philips Corp Method of separating gas-mixtures in a rectifying column
US3002358A (en) * 1960-08-01 1961-10-03 Shell Oil Co Propylene distillation
US3119677A (en) * 1961-01-16 1964-01-28 Phillips Petroleum Co Separation of gases
USRE29914E (en) * 1965-03-31 1979-02-20 Compagnie Francaise D'etudes Et De Construction Technip Method and apparatus for the cooling and low temperature liquefaction of gaseous mixtures
US3509728A (en) * 1966-02-22 1970-05-05 Petrocarbon Dev Ltd Low temperature separation of gases utilizing two distillation columns having a common condenser-evaporator
US3581510A (en) * 1968-07-08 1971-06-01 Phillips Petroleum Co Gas liquefaction by refrigeration with parallel expansion of the refrigerant
US4218229A (en) * 1977-08-06 1980-08-19 Linde Aktiengesellschaft Separation of ethylene-containing hydrocarbon mixtures by low temperature rectification

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BE480496A (US07122603-20061017-C00294.png)
FR961430A (US07122603-20061017-C00294.png) 1950-05-11
GB632438A (en) 1949-11-28

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