US2962867A - Process for decomposing hydrogencontaining gas mixtures - Google Patents

Process for decomposing hydrogencontaining gas mixtures Download PDF

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US2962867A
US2962867A US676112A US67611257A US2962867A US 2962867 A US2962867 A US 2962867A US 676112 A US676112 A US 676112A US 67611257 A US67611257 A US 67611257A US 2962867 A US2962867 A US 2962867A
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nitrogen
air
gas
washing
decomposition
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Seidel Max
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Linde GmbH
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Gesellschaft fuer Lindes Eismaschinen AG
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/02—Preparation of nitrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/025—Preparation or purification of gas mixtures for ammonia synthesis
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/506—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification at low temperatures
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
    • C10K1/16—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with non-aqueous liquids
    • C10K1/165—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with non-aqueous liquids at temperatures below zero degrees Celsius
    • 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
    • F25J3/0276—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
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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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    • 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
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    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/0423—Subcooling of liquid process streams
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    • 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
    • F25J3/04—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 for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
    • 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
    • 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
    • F25J3/04—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 for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low pressure column
    • 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
    • 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
    • F25J3/04—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 for air
    • F25J3/04406—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 for air using a dual pressure main column system
    • F25J3/04412—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 for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure 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
    • F25J3/04—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 for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04563—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating
    • F25J3/04587—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating for the NH3 synthesis, e.g. for adjusting the H2/N2 ratio
    • 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
    • F25J3/04—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 for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04612—Heat exchange integration with process streams, e.g. from the air gas consuming unit
    • 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
    • F25J3/04—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 for air
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/0489—Modularity and arrangement of parts of the air fractionation unit, in particular of the cold box, e.g. pre-fabrication, assembling and erection, dimensions, horizontal layout "plot"
    • 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
    • F25J2205/24—Processes or apparatus using other separation and/or other processing means using regenerators, cold accumulators or reversible heat exchangers
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/42—One fluid being nitrogen
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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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/52—One fluid being oxygen enriched compared to air, e.g. "crude oxygen"
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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
    • F25J2260/00—Coupling of processes or apparatus to other units; Integrated schemes
    • F25J2260/02—Integration in an installation for exchanging heat, e.g. for waste heat recovery
    • 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
    • Y10S62/931—Recovery of hydrogen
    • Y10S62/934—From nitrogen

Definitions

  • Nitrogen compressed at room temperature to high pressure, for example 180 atmospheres, is cooled by counter-current contact with cold decomposition products and is then expanded and liquefied. A part is expanded only to the washing pressure, the other part, used as refrigerant, to a lower pressure. A closed nitrogen refrigerating cycle has also been used already. It is disadvantageous that large quantities of nitrogen must be compressed to high pressure.
  • the procedure according to the present invention does not possess the described disadvantages.
  • the invention refers to a procedure for the decomposition of hydrogencontaining gas mixtures, particularly coke over gas, in which the difiicultly condensible components of the gas mixture are washed out with liquid nitrogen, won by an air decomposition procedure in which this nitrogen is produced from gaseous nitrogen compressed at room temperature to high pressure, cooled in counter-current with itself and with components of the gas mixture.
  • the characterizing feature of the invention consists in that the cooled nitrogen is liquefied at least partly by indirect heat exchange with cold air that is to be decomposed.
  • any desired amounts of air can be decomposed in the air decomposition installation, although the air and gas mixture decomposition installations are functionally connected with each other.
  • the air decomposition installation can therefore be dimensioned for large amounts of air; it can be equipped with expansion turbines which may be inserted with good economy only in cases of large outputs.
  • Into the air decomposition installation flows the same quantity of air, by weight, as decomposition products flow out.
  • the pressure under which the air is rectified is independent of the washing pressure; therefore it is not necessary to compress the entire quantity of air to be decomposed to the washing pressure. There is no free, open connection between the air and the gas mixture decomposition installation.
  • the air decomposition installation serves as source of cold whereby the coldness of cold air to be decomposed is withdrawn. It is however not withdrawn from cold oxygen and also not from cold nitrogen. The cold economy of the cold exchangers in the air decomposition installation is therefore always balanced.
  • a part of the cold air to be decomposed can be blown directly into the upper column, which is under approximately atmospheric pressure.
  • the procedure according to the invention use is made of this mode of action in two difierent ways.
  • the cooled nitrogen intended for the washing is liquefied at least partly by indirect heat exchange with liquid air enriched with oxygen whereby a part of this enriched liquid air is evaporated.
  • the liquid gas mixture can then be decomposed in the upper column into pure nitrogen and pure oxygen.
  • the cooled nitrogen is liquefied at least partly by indirect heat exchange with gaseous air cooled to condensation temperature and subsequently to be expanded, for example in a turbine, to approximately condensation temperature, whereupon it is led directly into the upper column.
  • the hydrogen-nitrogen mixture formed in the washing process usually does not yet have the desired composition. It is already known to add liquid nitrogen. It is however more advantageous to make the amount of washing nitrogen only so small that the mixtures are sufficiently purified, and if necessary to add any nitrogen still required for the desired hydrogen-nitrogen ratio only to the mixture formed by the washing after it is again heated.
  • liquid nitrogen must be evaporated in indirect heat exchange with the washed gas mixture under a pressure which lies below the Washing pressure. Only in this Way can a temperature be achieved which is sufliciently low to completely condense the nitrogen remaining in the hydrogen.
  • the required liquid nitrogen is withdrawn from the washing nitrogen and evaporated in indirect heat exchange with the gas mixture to be purified, under negative pressure.
  • a device for carrying out the procedure according to the invention consists in its main parts of a coke over gas producer and an air decomposition installation. Both installations have their own insulating envelopes and are connected with each other through two insulated lines. The one line serves for cold gaseous washing nitrogen, the other serves for at least partially liquefied washing nitrogen. The cold losses would however be somewhat less if both installations were insulated in common. But separate insulations have the advantage that no explosive gas mixtures can form in the insulating envelopes even when, for example, a flange or packing box becomes leaky. For the same reason it is also more expedient to introduce washing nitrogen into the air decomposition installation, instead of charging liquid or cold gaseous air into the coke oven gas installation.
  • the washing nitrogen can be liquefied by heat exchange with liquid air
  • there is an evaporating condensor arranged in the air decomposition installation which on the exaporator side, has liquid air enriched with oxygen flowing through it, which flows from the foot of the lower column to the upper column of a double rectification column.
  • a heat exchanger is arranged in the air decomposition installation, for washing nitrogen on the one hand and gaseous cold air on the other hand, which is subsequently expanded in an expansion turbine and then blown into the upper column of a double rectification column.
  • Fig. 1 shows a suitable combination of a gas decomposition installation for the preparation of a hydrogennitrogen mixture with an air decomposition installation with a counter-current pipe system as heat exchanger and with a rectification column, in front of which is connected an expansion machine.
  • the air decomposition installation consists of the compressor 11, the heat exchanger 12, the expansion machine 13, the liquefier 14, the pressure column 15, the upper column 16, the air entrance line 1, the exit line for pure nitrogen 2 and the exit line for oxygen 3.
  • the gas decomposition installation consists of the higher pressure nitrogen compressor 21, the heat exchangers 22 and 23, the washing column 24, the heat exchanger 25, the residual gas evaporator 27, the crude gas entrance line 5, the nitrogen exit line 6, the residual gas exit line 7 and the expansion valves 8.
  • Both installations are connected through the heat exchanger 31, which in this case is an evaporator condensor.
  • the air for the air decomposition installation is com pressed by the compressor 11 to for example 26 atmospheres absolute pressure, cooled in the heat exchanger 12 and then divided into two streams.
  • the one stream is liquefied in the liquefier 14, and then expanded into the pressure column 15.
  • the other stream is expanded in the expansion machine 13, yielding work, and then likewise led into the pressure column 15.
  • the oxygenenrichecl liquid collecting at the foot of the pressure column 15 is expanded and then led through the heat exchanger 31, where it evaporates partially. On the basis of this evaporation so much heat is withdrawn from the compressed and cooled washing nitrogen flowing in from the gas decomposition installation in an indirect heat exchange, that it is liquefied. From the heat exchanger 31 the oxygen enriched liquid-vapor mixture arrives in the upper column 16.
  • the crude gas entering at 5 under a suitable pressure of for example 15 atmospheres absolute pressure arrives through the heat exchanger 25 and the residual gas evaporator 27 at the bottom of the Washing column 24, in which the liquid nitrogen runs down and washes out the contaminations.
  • the pure gas leaving at the head of the washing column 24 gives up its coldness in the heat exchanger 25 to the crude gas and the heat exchanger 23 to a part of the high pressure nitrogen and leaves the installation at 6.
  • Nitrogen, possibly still lacking for the desired mixture composition can be added to the line 6 directly through a line from the high pressure nitrogen compressor 21.
  • the residual gas becomes heated in the heat exchanger 22 in counter current to the other part of the high pressure nitrogen and leaves at 7.
  • Figure 2 represents a gas decomposition installation for the production of gas having a high hydrogen content.
  • the additional coldness to be produced in this installation is withdrawn from a Linde-Frankl air decomposition installation by means of heat exchange through regenerators. 7
  • the air decomposition installation consists of the compressor 11, the regenerators 17 and 18, the pressure column 15, the upper column 16, the expansion turbine 13, the pipe coils 19, the air entrance line 1, the exit line for pure nitrogen 2, the exit line for oxygen 3, and the exit line for impure nitrogen 4.
  • the gas decomposition consists of the high pressure nitrogen compressor 21, the heat exchangers 22 and 23, the washing column 24, and the heat exchangers 25 and 26, the residual gas evaporator 27, the nitrogen vacuum evaporator 23, the vacuum pump 29, the crude gas entrance line 5, the hydrogen exit line 9 and the residual gas exit line 7.
  • the two installations are connected with each other by the heat exchanger 32.
  • the air for the air decomposition installation is compressed by the compressor 11, formed as a turbocompressor, to for example 5.6 atmospheres absolute pressure, cooled oflf in the regenerators 17 and 18, and for the most part led to the pressure column 15.
  • a small part of the compressed air is withdrawn from the iddle of the regenerators 17 and led to the expansion turbine 13.
  • a part of the compressed air, completely cooled down in the regenerators 17 and 18, is slightly heated again in the heat exchanger 32 by liquefying compressed washing nitrogen from the gas decomposition installation and led together with the part of the compressed air withdrawn from the middle of the regenerators 17 to the expansion turbine 13, expanded so as to yield work, and then led into the upper column 16.
  • the pure nitrogen is drawn from the head of the upper column 16 through the pipe coils 19 to the regenerators 17 and the line 2, entirely or in part by the high pressure nitrogen compressor 21.
  • the impure nitrogen is withdrawn through a so-called Lachmann tap between the head of the upper column 16 and the inlet point of the liquid crude oxygen from the foot of the pressure column 15, heated by the regenerators 17 and leaves the installation at 4.
  • the oxygen from the upper column 16 leaves the installation through the regenerators 18 at 3.
  • the crude gas entering at 5 with a suitable pressure of for example 30 atmospheres absolute pressure arrives through the heat exchangers 25 and 26 and the residual gas evaporator 27 into the washing column 24, in which the contaminations are washed out by downwardly flowing liquid nitrogen.
  • the nitrogen is compressed in the high pressure nitrogen compressor 21 to for example atmospheres absolute pressure, cooled in the heat exchangers 22 and 23 and thereafter liquefied in the heat exchanger 32 according to the invention in indirect heat exchange with compressed air.
  • the one part is led after corresponding expansion into the upper part of the wash ing column 24.
  • the other part is expanded, if necessary with supercooling, for example by hydrogen being withdrawn, into the nitrogen vacuum evaporator 28 arranged above the washing column 24.
  • the nitrogen evaporated under vacuum is drawn through the heat exchanger 23 by the vacuum pump 29.
  • the vacuum pump 29 Through the evaporation of the nitrogen under vacuum so much coldness is produced at sufiiciently low temperature, that almost all the nitr geu-down to a slight residue of for example 2%is condensed out of the hydrogen-nitrogen mixture coming from the washing column 24 and pure or almost pure hydrogen leaves the gas decomposition installation at 9, after it has given up its coldness in the heat exchanger 25 to a part of the crude gas.
  • the liquefied residual gas is withdrawn from the lower part of the washing column 24, evaporated in the residual gas evaporator 27 by cooling crude gas and leaves the installation at 7, after its cold ness has been exchanged partly in the heat exchanger 26 with the crude gas and partly in the heat exchanger 22 with the high pressure nitrogen.
  • Process for the decomposition of a hydrogen-containing gas mixture involving washing at least one ditficultly condensible component out of said gas mixture by contacting it with liquid nitrogen which comprises simultaneously operating a gas decomposing plant operating upon said gas mixture and an air decomposing plant, withdrawing nitrogen from said air decomposing plant, compressing the nitrogen to the pressure required for said washing operation, precooling the compressed nitrogen by indirect heat exchange with at least one fraction of said hydrogen-containing gas mixture in said gas decomposing plant, further cooling and at least partially liquifying said precooled nitrogen by indirect heat exchange in said airdecomposing plant and returning the resulting liquefied nitrogen to said gas decomposing plant and using it therein as the washing liquid.
  • Apparatus for the decomposition of a hydrogen containing gas mixture consisting of a gas decomposition plant comprising a liquid nitrogen washer for said gas mixture and a heat-exchanger for cooling nitrogen, an air separation plant, and a condensor for liquefying the washing nitrogen which is cooled in said heat-exchanger of the gas decomposition plant by heat-exchange with a fraction withdrawn from said gas decomposition plant, said condensor being situated in said air separation plant and two connecting lines between said two plants, one connecting said heat-exchanger of said gas decomposition plant with said condensor and the other connecting said condensor with said nitrogen washer in the gas decomposition plant.
  • Apparatus as claimed in claim 6 comprising an expansion machine and a connecting line for passing a gaseous fraction withdrawn from said air separation plant and warmed in said condensor to said expansion machine.

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US676112A 1956-09-20 1957-08-05 Process for decomposing hydrogencontaining gas mixtures Expired - Lifetime US2962867A (en)

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DEG20593A DE1023061B (de) 1956-09-20 1956-09-20 Verfahren zur Zerlegung von Wasserstoff enthaltenden Gasgemischen, insbesondere Koksofengas, und Vorrichtung zur Durchfuehrung des Verfahrens

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3089311A (en) * 1959-12-21 1963-05-14 Linde Eismasch Ag Regenerative heat-transfer process
US3092283A (en) * 1960-07-29 1963-06-04 Sulzer Ag Means for insulating elements of a low temperature unit
US3251189A (en) * 1960-04-14 1966-05-17 Linde Eismaschinen Ag Gas separation process and apparatus
US3327487A (en) * 1963-03-21 1967-06-27 Ernst karwat
US3401531A (en) * 1965-05-19 1968-09-17 Linde Ag Heat exchange of compressed nitrogen and liquid oxygen in ammonia synthesis feed gas production
US3421333A (en) * 1964-08-28 1969-01-14 Linde Ag Thawing technique for a single air separation plant
US3426543A (en) * 1963-06-19 1969-02-11 Linde Ag Combining pure liquid and vapor nitrogen streams from air separation for crude hydrogen gas washing
US3596470A (en) * 1965-05-18 1971-08-03 Linde Ag Process and apparatus for the low-temperature separation of a hydrogen-rich gas mixture

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1354380A (en) * 1914-01-07 1920-09-28 Godfrey L Cabot Apparatus for producing liquid oxygen
US1723425A (en) * 1924-11-06 1929-08-06 Ammonia Soc Process of separating hydrogen from gaseous mixtures
US1843043A (en) * 1924-02-13 1932-01-26 Patart Georges Leon Emile Process for the separation of the several components of gaseous mixtures
US2417279A (en) * 1944-07-22 1947-03-11 Air Reduction Separation of the constituents of gaseous mixtures
US2785548A (en) * 1954-05-26 1957-03-19 Linde Eismasch Ag Process for the production of liquid oxygen by separation from air

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1354380A (en) * 1914-01-07 1920-09-28 Godfrey L Cabot Apparatus for producing liquid oxygen
US1843043A (en) * 1924-02-13 1932-01-26 Patart Georges Leon Emile Process for the separation of the several components of gaseous mixtures
US1723425A (en) * 1924-11-06 1929-08-06 Ammonia Soc Process of separating hydrogen from gaseous mixtures
US2417279A (en) * 1944-07-22 1947-03-11 Air Reduction Separation of the constituents of gaseous mixtures
US2785548A (en) * 1954-05-26 1957-03-19 Linde Eismasch Ag Process for the production of liquid oxygen by separation from air

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3089311A (en) * 1959-12-21 1963-05-14 Linde Eismasch Ag Regenerative heat-transfer process
US3251189A (en) * 1960-04-14 1966-05-17 Linde Eismaschinen Ag Gas separation process and apparatus
US3092283A (en) * 1960-07-29 1963-06-04 Sulzer Ag Means for insulating elements of a low temperature unit
US3327487A (en) * 1963-03-21 1967-06-27 Ernst karwat
US3426543A (en) * 1963-06-19 1969-02-11 Linde Ag Combining pure liquid and vapor nitrogen streams from air separation for crude hydrogen gas washing
US3421333A (en) * 1964-08-28 1969-01-14 Linde Ag Thawing technique for a single air separation plant
US3596470A (en) * 1965-05-18 1971-08-03 Linde Ag Process and apparatus for the low-temperature separation of a hydrogen-rich gas mixture
US3401531A (en) * 1965-05-19 1968-09-17 Linde Ag Heat exchange of compressed nitrogen and liquid oxygen in ammonia synthesis feed gas production

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BE560978A (en))
DE1023061B (de) 1958-01-23

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