US3436925A - Rectification of liquefied coke oven gas portion by contact between liquefied and revaporized portions thereof - Google Patents

Rectification of liquefied coke oven gas portion by contact between liquefied and revaporized portions thereof Download PDF

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US3436925A
US3436925A US579338A US3436925DA US3436925A US 3436925 A US3436925 A US 3436925A US 579338 A US579338 A US 579338A US 3436925D A US3436925D A US 3436925DA US 3436925 A US3436925 A US 3436925A
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mixture
liquid
liquefied
rectification
coke oven
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US579338A
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English (en)
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Fritz Jakob
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Linde GmbH
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Linde GmbH
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification 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
    • 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
    • F25J3/0233—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
    • F25J3/0276—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 H2/N2 mixtures, i.e. of ammonia synthesis 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
    • F25J2200/02—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
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • 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
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • 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
    • F25J2210/14—Coke-ovens 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
    • F25J2215/20—Ammonia synthesis gas, e.g. H2/N2 mixture
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/02—Internal refrigeration with liquid vaporising loop

Definitions

  • An object of this invention is to provide an improved process for the rectification of a mixture having a wide boiling point distribution.
  • a more particular object is to provide an improved process for the rectification of a mixture, wherein said mixture is fed as liquid to the top of the rectification column.
  • a further object includes the aforementioned objects as applied to low temperature processes wherein refrigeration energy is consequential, and in particular to the production of enriched hydrogen gas from coke oven gas, and also to the production of ethylene.
  • This invention is particularly beneficial for the treatment of feed streams wherein about 30 to 80, of preferably 50 to 70 mol percent of the feed has an average boiling point of about at least 15 (1., preferably at least 30 C. higher than 70 to 20, preferably 50 to 30 mol percent of the feed. Furthermore, it is to be noted that the process of this invention is even more important for cryogenic processes wherein at least 30 mol percent, preferably at least 50 mol percent of the feed has a boiling point below about 40 0, preferably below about C.
  • the portion of the liquid feed that is vaporized and passed as vapor to the bottom of the rectification column it is preferred that at least 20 percent, more preferably at least 30 percent of the liquid feed be so utilized.
  • the liquid which is in equilibrium with the introduced vapor at the foot of the rectification column and is collected in the sump, is so rich in high-boiling component that it represents an acceptable product, un less, of course, it is necessary to produce a highly pure product.
  • That portion of the mixture which is to be vaporized and introduced into the rectification column is advantageously formed from the stream which is richest in the high-boiling mixture component, or in the high-boiling group of mixture components, in order to obtain the high-boiling component which is the purest possible for this particular case.
  • one portion of this mixture when producing methane from a liquid mixture as obtained during the cooling of coke oven gas, one portion of this mixture can be vaporized in heat exchange with coke oven gas. It is furthermore possible, when producing methane from coke oven gas, to adrnix the low-boiling components exiting at the head of the rectification column directly to the cold residual gas.
  • the attached drawing is a schematic representation of a preferred embodiment of this invention, illustrating that section of a coke oven gas separating plant important for the production of methane from coke oven gas, and for the purpose of producing a hydrogen-nitrogen mixture for the ammonia synthesis.
  • the precooled coke oven gas is fed to the plant via conduit 1 and is further cooled in heat exchangers 2 and 3.
  • a part of the coke oven gas condenses, namely practically all of CH CO, and N
  • This condensate is separated in the liquid-vapor separator 4 from the remaining coke oven gas and fed, in two portions via different paths, to the rectification column 5.
  • One portion about 80 to 30%, is fed directly via conduit 6 to rectification column 5 where it is employed as reflux.
  • the other portion is conducted, by conduit 7, to heat exchanger 3, evaporated therein, and subsequently introduced into column 5 at the foot thereof.
  • the liquid, at the vapor feed point, is very substantially enriched in methane, owing to the favorable boiling relationships of CH on the one hand, and CO+N2, on the other hand; consequently, this liquid can be withdrawn directly as a product from the bottom of column. 5 through conduit 8.
  • the process of this invention can, in such a case, yield methane ot a 95 purity.
  • the product is then vaporized in the heat exchanger 2 at a relatively high temperature (the boiling temperature of the moderately pure methane); thus, it transfers its refrigeration values at this relatively high temperature.
  • the condensate separated in the liquid-vapor separator must be formed at a lower temperature in the heat exchanger 3.
  • one portion of the condensate is additionally vaporized in the heat exchanger 3. Since the condensate still contains substantial proportions of CO and N its median boiling temperature is considerably lower than the boiling temperature of the sump liquid, or of the product. Consequently, the vaporization of a portion of the condensate in the heat exchanger 3, yields refrigeration ot a lower temperature.
  • the resultant mixture of these residual gases is warmed in the heat exchangers 3 and 2.
  • the hydrogen-nitrogen mixture coming from the nitrogen iwashing stage is likewise conducted through these heat exchangers, via conduit 10.
  • a typical analysis of coke oven gas in conduit 1 which can be treated by this invention is Component: Vol. percent range H 50-57 N 6l2 CO 5-7 CH 22-25 C l-L, 12 C H 0.7-2 C H 30.6 CGHG 0. -1 CO 2-5
  • teachings of this invention can also be particularly advantageously employed in the production of ethylene where the boiling relationships between ethylene, on the one hand, and methane, on the other hand, are likewise favorable for the production of a moderately pure product.
  • ethylene and methane have normal boiling points of ll9 C. and l61 C., respectively, thereby giving a mixture of such liquefied gases a boiling point separation of 42 C.
  • a feed mixture comprising 45% ethylene and 55% methane is treated so as to vaporize 54% thereof, thereof, with the residual 46% being employed as reflux.
  • the resultant bottoms product contains ethylene, and in the resultant overhead gas, ethylene is lost to an extent of only about 12%.
  • a process as gaseous stream is coke oven gas.
  • a process as defined by claim 1 further comprising the step of passing said overhead vapor from the rectification column also in indirect heat exchange relationship with said gaseous stream.
  • a process as defined by claim 1, wvherein 30-80 mol percent of said liquid phase mixture has an average boiling point of about at least C. higher than 70-20 mol percent of said liquid phase mixture, and at least mol percent of said liquid phase mixture has a boiling point below about C.
US579338A 1965-09-21 1966-09-14 Rectification of liquefied coke oven gas portion by contact between liquefied and revaporized portions thereof Expired - Lifetime US3436925A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0137744A2 (de) * 1983-09-20 1985-04-17 Costain Petrocarbon Limited Trennung von Kohlenwasserstoffgemischen
US4690702A (en) * 1984-09-28 1987-09-01 Compagnie Francaise D'etudes Et De Construction "Technip" Method and apparatus for cryogenic fractionation of a gaseous feed
US5737940A (en) * 1996-06-07 1998-04-14 Yao; Jame Aromatics and/or heavies removal from a methane-based feed by condensation and stripping

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2071763A (en) * 1930-03-10 1937-02-23 Union Carbide & Carbon Corp Process for the separation of gas mixtures
US2559132A (en) * 1948-02-12 1951-07-03 British Oxygen Co Ltd Fractional separation of air
US2664719A (en) * 1950-07-05 1954-01-05 Union Carbide & Carbon Corp Process and apparatus for separating gas mixtures
US2743590A (en) * 1952-11-29 1956-05-01 Air Liquide Method for the fractionation of gas mixtures
US2817216A (en) * 1952-08-12 1957-12-24 Air Liquide Process and apparatus for the separation, by rectification, of a gas mixture containing at least three components
US2997854A (en) * 1957-08-16 1961-08-29 Air Prod Inc Method and apparatus for separating gaseous mixtures
US3209548A (en) * 1962-02-27 1965-10-05 Air Liquide Process for the manufacture of oxygen-enriched air
US3264831A (en) * 1962-01-12 1966-08-09 Linde Ag Method and apparatus for the separation of gas mixtures

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2071763A (en) * 1930-03-10 1937-02-23 Union Carbide & Carbon Corp Process for the separation of gas mixtures
US2559132A (en) * 1948-02-12 1951-07-03 British Oxygen Co Ltd Fractional separation of air
US2664719A (en) * 1950-07-05 1954-01-05 Union Carbide & Carbon Corp Process and apparatus for separating gas mixtures
US2817216A (en) * 1952-08-12 1957-12-24 Air Liquide Process and apparatus for the separation, by rectification, of a gas mixture containing at least three components
US2743590A (en) * 1952-11-29 1956-05-01 Air Liquide Method for the fractionation of gas mixtures
US2997854A (en) * 1957-08-16 1961-08-29 Air Prod Inc Method and apparatus for separating gaseous mixtures
US3264831A (en) * 1962-01-12 1966-08-09 Linde Ag Method and apparatus for the separation of gas mixtures
US3209548A (en) * 1962-02-27 1965-10-05 Air Liquide Process for the manufacture of oxygen-enriched air

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0137744A2 (de) * 1983-09-20 1985-04-17 Costain Petrocarbon Limited Trennung von Kohlenwasserstoffgemischen
EP0137744A3 (en) * 1983-09-20 1986-05-28 Costain Petrocarbon Limited Separation of hydrocarbon mixtures
US4690702A (en) * 1984-09-28 1987-09-01 Compagnie Francaise D'etudes Et De Construction "Technip" Method and apparatus for cryogenic fractionation of a gaseous feed
US5737940A (en) * 1996-06-07 1998-04-14 Yao; Jame Aromatics and/or heavies removal from a methane-based feed by condensation and stripping

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DE1519598A1 (de) 1970-02-26

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