EP1134525A1 - Procédé de production d'azote liquide et gazeux avec une quantité variable de liquide - Google Patents

Procédé de production d'azote liquide et gazeux avec une quantité variable de liquide Download PDF

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Publication number
EP1134525A1
EP1134525A1 EP01106637A EP01106637A EP1134525A1 EP 1134525 A1 EP1134525 A1 EP 1134525A1 EP 01106637 A EP01106637 A EP 01106637A EP 01106637 A EP01106637 A EP 01106637A EP 1134525 A1 EP1134525 A1 EP 1134525A1
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EP
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Prior art keywords
column
oxygen
nitrogen
liquid
condenser
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Granted
Application number
EP01106637A
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German (de)
English (en)
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EP1134525B1 (fr
Inventor
Dietrich Dipl.-Ing. Rottmann
Christian Dipl.-Ing. Kunz
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Linde GmbH
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Linde GmbH
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04854—Safety aspects of operation
    • F25J3/0486—Safety aspects of operation of vaporisers for oxygen enriched liquids, e.g. purging of liquids
    • 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
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/04018—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of main feed air
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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
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    • F25J3/0403—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of nitrogen
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    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
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    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
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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
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    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • F25J3/04212—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product and simultaneously condensing vapor from a column serving as reflux within the or another column
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    • F25J3/04357—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen and comprising a gas work expansion loop
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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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    • F25J2220/42—Separating low boiling, i.e. more volatile components from nitrogen, e.g. He, H2, Ne
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/50—Separating low boiling, i.e. more volatile components from oxygen, e.g. N2, Ar
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/52—Separating high boiling, i.e. less volatile components from oxygen, e.g. Kr, Xe, Hydrocarbons, Nitrous oxides, O3
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/42—Processes or apparatus involving steps for increasing the pressure of gaseous process streams 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen
    • 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
    • F25J2240/40—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval
    • F25J2240/46—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval the fluid being oxygen
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream 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
    • 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
    • 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
    • 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
    • F25J2250/50—One fluid being oxygen

Definitions

  • the invention relates to a method according to the preamble of claim 1. It serves for the production of gaseous and liquid nitrogen with a variable proportion of Liquid product through low temperature separation of air in one Distillation column system that has a single column.
  • Single column processes are a common method of producing nitrogen. she unlike double-column processes, only have one pressure column (the single column) on and no other column (low pressure column) for nitrogen-oxygen separation used and operated under lower pressure than the pressure column. This does not rule out that the distillation column system extends beyond the individual column Has columns, for example for the production of particularly pure nitrogen or Oxygen.
  • distillation column system comprises the interconnected distillation columns, but not the heat exchangers or the machines such as compressors or Relaxation machines.
  • the distillation column system formed exclusively by the single column.
  • Oxygen enriched is understood here to mean a mixture of air gases that has a higher oxygen concentration than air, up to practically pure Oxygen. In practice, for example, there are fractions with a Oxygen content of 25 to 90%, preferably 30 to 80%. (All percentages refer here and below to the molar amount, unless otherwise is specified.)
  • the liquid fraction (molar ratio between liquid and gaseous product nitrogen) can be variable. At different times So there can be different steady-state operating conditions, including one different proportions of the nitrogen product are obtained in liquid form, in extreme cases this proportion can also be zero.
  • the process can then be between two Border cases are moved back and forth, the maximum gas production (MaxGAN case) with minimal liquid content and maximum liquid production (MaxLIN case) with maximum liquid content and minimum gas content (possibly exclusively liquid nitrogen production). Any value of the Liquid fraction can be set between the two limits for minimum and maximum liquid content.
  • a nitrogen cycle process according to the preamble of claim 1 known from US 4400188. With nitrogen in a circuit compressor on over Column pressure has been brought up, a condenser evaporator is heated, which is the Represents sump heating of the single column. Process cold is a common Residual gas turbine generated using gas from another condenser-evaporator, a top capacitor is operated. Such nitrogen cycle processes are energetically cheaper than single column processes without bottom heating. Because of the Circulation can also be a liquid nitrogen product in this process variable quantity are generated, even if this is not in the publication itself is described. However, one would come across in such a method Difficulties if you wanted to vary the liquid product content.
  • the invention has for its object a method of the type mentioned and to specify a corresponding device in which in addition to the gaseous Nitrogen product a variable amount of liquid product with relatively little effort can be won.
  • the liquid product can go directly to the liquefaction chamber of the condenser-evaporator be removed. However, it is preferably first relaxed and thereby separating flash gas.
  • the phase separation can for example carried out in the single column or in a separate separator become.
  • the second oxygen-enriched gas that for work relaxation is provided, is preferably like the first oxygen-enriched gas from the generated steam formed in the condenser-evaporator.
  • the two For example, oxygen-enriched gases have the same composition.
  • the entry pressure of work-related relaxation is not - as is the case with Residual gas turbines common - at the single column or top condenser pressure bound, but preferably to the evaporation pressure in the condenser-evaporator. Therefore, the turbine inlet pressure may increase as the Liquid product proportion increase analogously to the evaporation pressure.
  • the second oxygen-enriched gas generates the additional cold that is required for the increased product liquefaction is necessary. Also the increase in the amount of residual gas increases cold production.
  • the liquid product content can be, for example, 0 to 20%, preferably 0 to 16% of the total nitrogen product, with a total product amount Nitrogen, for example 75 to 0%, preferably 75 to 25% of the amount of air.
  • the Operating pressure in the bottom of the single column is, for example, 3 to 8 bar, preferably 3 to 5 bar.
  • the pressure difference between the evaporation side of the The condenser-evaporator and the lower section of the column is, for example, 0 up to 5 bar, preferably 0 to 3 bar.
  • the second oxygen-enriched gas ultimately comes from the single column a corresponding pressure increasing step is required, which in the invention is preferably carried out in the liquid state, for example by means of a Liquid pump.
  • a Liquid pump for example, an oxygen-enriched liquid from the single column withdrawn and brought to an increased pressure in the liquid state, the second oxygen-enriched gas resulting from the increased pressure oxygen-containing liquid is generated.
  • the oxygen-enriched liquid forms downstream of the Pressure increase the oxygenated liquid fraction contained in the Evaporation chamber of the condenser-evaporator is introduced.
  • the oxygen-enriched liquid is caused, for example, by the bottom liquid Single column formed and by means of a pump to at least the increased pressure brought under which the evaporation chamber of the condenser-evaporator is.
  • the first and second oxygen-enriched gas i.e. the rising steam for the The single column and the fraction that has to be relieved of work become immediate here generated by evaporation of the liquid fraction from the single column.
  • the distillation column system has one in addition to the single column Pure oxygen column on.
  • the oxygen-enriched liquid from the single column is applied to the pure oxygen column downstream of the pressure increase.
  • the lower area of the pure oxygen column is an oxygen-rich fraction deducted gaseous and / or liquid product and / or intermediate.
  • the liquid oxygen-enriched fraction, which the evaporation space of the Condenser-evaporator is also supplied comes from the lower area the pure oxygen column.
  • the steam generated in the condenser evaporator is in the introduced at the bottom of the pure oxygen column and there as rising steam used.
  • the top gas of the pure oxygen column serves as a first part Working gas of relaxation work ("second oxygen enriched Gas ”) and a second part - after a corresponding pressure reduction - as rising steam in the single column (“first oxygen-enriched gas”). Because of the higher oxygen concentration on the evaporation side of the In this variant, the condenser-evaporator has a higher circuit pressure than in embodiments where the evaporator side of the condenser-evaporator sump liquid is applied to the single column.
  • Mass transfer section - here called pure oxygen column - arranged under the increased pressure is operated.
  • the increased pressure brought liquid from the single column further oxygen enriched and depleted of more volatile components.
  • Liquid and / or Steam from the bottom of the pure oxygen column can be used directly as an oxygen product deducted and / or fed to a further step.
  • the condenser-evaporator is in this embodiment of the invention preferably arranged directly in the bottom of the pure oxygen column, but it can also be housed in a separate container.
  • the pure oxygen column is preferably designed as a pure stripping column and contains, for example, 30 to 50 preferably 35 to 45 theoretical plates.
  • the oxygen-rich fraction can be further purified in the distillation column system by adding an extra column to remove more volatile Impurities is supplied, from the upper area of a pure oxygen product is subtracted.
  • the oxygen-rich fraction is preferably from the bottom of the Pure oxygen column or from the evaporation chamber of the condenser-evaporator deducted.
  • the rising steam becomes less volatile in the additional column Free components that are depleted in the pure oxygen product (e.g. less than 100 ppm, preferably less than 10 ppm Impurities with a higher boiling point than oxygen; there may be residual levels up to about 1 ppb can be achieved). Residual liquid from the additional column can enter the Pure oxygen column or the condenser-evaporator can be returned.
  • the Additional column is preferably designed and contains as a pure reinforcing column for example 10 to 40, preferably 10 to 30 theoretical plates.
  • Return liquid for the additional column is preferably in a top condenser generated in which a second oxygen-enriched liquid fraction from the lower Area of the single column is at least partially evaporated.
  • the second oxygen-enriched liquid fraction can, for example, together with that on the Pure oxygen column applied oxygen-enriched liquid from the Single column can be removed and brought to increased pressure.
  • Air compressors and circuit compressors can be formed by a single machine be, namely by a combination machine, in which several pinions on a shaft sit, some of which are the air compressor and one or more of which Realize cycle compressors.
  • the circuit compressor can be at least partially connected to the residual gas turbine Coupled compressor are formed, with at least a portion of the generated work-relieving relaxation of the second oxygen-enriched gas mechanical energy to compress the first part and / or the second part the nitrogen-rich fraction is used.
  • the distillation column system has a pure nitrogen column, one Nitrogen fraction from the upper area of the single column in liquid state on the Pure nitrogen column is abandoned and from the bottom of the Pure nitrogen column a pure nitrogen product is withdrawn.
  • the pure nitrogen column serves to remove volatile impurities from the nitrogen, especially helium, neon and hydrogen.
  • the bottom product of the Pure nitrogen column is practically free of helium, neon and hydrogen (for example less than 10 ppb, preferably less than 5 ppb of more volatile than nitrogen Impurities) and can be removed in gas or liquid form.
  • the Pure nitrogen column is preferably operated as a pure stripping column (stripping column) and contains, for example, 10 to 20, preferably 10 to 15 theoretical plates.
  • the nitrogen cycle (first part of the nitrogen-rich fraction from the Distillation column system) can either use very pure gas from the lower range the pure nitrogen column or with head gas of the single column. Likewise it is possible to produce gaseous pressure product (second part of the nitrogen-rich fraction the distillation system) helium and neon free from the pure nitrogen column and / or something to be deducted less from the head of the single column.
  • the pure nitrogen column preferably has a bottom evaporator, the Nitrogen fraction taken from the single column in gaseous form and up before its task the pure nitrogen column is liquefied in the sump evaporator. Through this The procedure is no further heating medium for the operation of the pure nitrogen column required.
  • the operating pressure of the pure nitrogen column is slightly lower (for example by 0.5 to 1.0 bar) as the pressure at the top of the single column. The one in the Bottom evaporator liquefied fraction is placed on the pure nitrogen column before the task relaxed at their operating pressure.
  • the invention also relates to a device according to claim 12.
  • compressed and cleaned feed air is introduced via a line 1, which is under a pressure of approximately 3.5 bar.
  • Air compressor and air purification - for example using a molecular sieve - are not shown in the drawing.
  • the air is cooled in a main heat exchanger 2 to approximately dew point and fed via line 3 to a single column 4 at an intermediate point.
  • the intermediate point is, for example, 5 to 20 theoretical or practical trays above the bottom of the column 4.
  • the operating pressure at the bottom of the individual column is 3.0 bar in the example.
  • the top nitrogen 5 (the "nitrogen-rich fraction") from the single column 4 still contains 1 ppm to 1 ppb oxygen and is in a subcooler 6 and (line 7) further in Main heat exchanger 2 warmed to about ambient temperature.
  • the warm one Top nitrogen 8 is fed to a circuit compressor 9, for example two to has three levels. There is one behind each stage of the circuit compressor Aftercooling or intermediate cooling to remove the compression heat, of which, however, only the aftercooling 10 behind the in the schematic drawing Power stage is shown.
  • a first part 12 of the compressed to a pressure of 9.5 bar Top nitrogen 11 is returned to the main heat exchanger 2, there to several Kelvin cooled above the column temperature and the line 13 Liquefaction chamber of a condenser-evaporator 14 supplied.
  • the nitrogen-rich liquid 15 thus formed is in the subcooler 6 supercooled and via line 16 and throttle valve 17 to the top of the single column given up.
  • a portion 18 of the nitrogen-rich liquid 16 can be as Liquid nitrogen product LIN are withdrawn.
  • the liquid production is in the Example about 0% of the air volume.
  • the liquid nitrogen from the Single column deducted, the head here as a flash gas separator between the Throttle valve 17 and the liquid product removal 18 is used.
  • a second part 19 of the top nitrogen 11 compressed in the circuit compressor 9 is called gaseous nitrogen product removed under pressure (DGAN).
  • DGAN gaseous nitrogen product removed under pressure
  • a portion 20 of the pressurized nitrogen from an intermediate stage of the cycle compressor led out and at a pressure between the operating pressure of the individual column 4 and the final pressure of the circuit compressor 9 as a gaseous pressure nitrogen product (DGAN ').
  • the circuit compressor 9 serves in both cases at the same time as a product compressor.
  • the condenser-evaporator 14 is in the example of FIG. 1 directly in the sump the single column.
  • first oxygen-enriched gas oxygen-enriched gas
  • second oxygen-enriched gas led to the cold end of the main heat exchanger 2.
  • this fraction flows via line 22 to a residual gas turbine 23 and becomes work-performing from about 3 bar to about 1.5 bar relaxed.
  • the turbine 23 can have a Bypass 26 can be regulated. A small amount of liquid 27 becomes continuous or intermittently as rinsing liquid from the evaporation chamber of the condenser-evaporator 14 dissipated.
  • the method according to FIG. 1 differs from the prior art according to US 4400188 by the type of refrigeration. This is done here by work Relaxation of an oxygen-enriched gas 21 from the evaporation space of the condenser-evaporator 14 accomplished. This measure does indeed Simplification of the equipment, since only a single condenser-evaporator for Operation of the single column 4 is required, but this alone can not be the perform the desired simple variation of the liquid product portion, as is the case with the Embodiments of Figures 2 to 10 is the case.
  • the condenser-evaporator 214 is arranged in a separate container outside the individual column 4. In the present case, this is not only an apparatus detail, but also enables the pressure in the evaporation space of the condenser-evaporator 214 to be decoupled from the operating pressure of the individual column 4.
  • the bottom liquid (the "liquid oxygen-enriched fraction") 228 is pumped up here by a pump 229 brought a pressure of 4 to 8 bar and introduced under this increased pressure or possibly after a slight throttling 230 via line 231 into the evaporation space of the condenser-evaporator 214.
  • the steam 232 which is drawn off from the condenser-evaporator 214 under this pressure, flows back to the first column ("first oxygen-enriched gas") 233 with throttling 234 to the single column 4.
  • first oxygen-enriched gas first oxygen-enriched gas
  • second oxygen-enriched gas second oxygen-enriched gas
  • the advantage of decoupling the condenser-evaporator from the operating pressure The column does not exhaust itself in a somewhat greater cooling capacity of the turbine 23 is a consequence of the higher entry pressure. Rather, the measure can Liquid production (here: exclusively liquid nitrogen 18) with relatively simple Averages can be varied in a range from about 0 to 4.3% of the quantity of feed air. Switching between the operating cases works as follows: To For example, to achieve maximum liquid production, the levy is first applied gaseous nitrogen (via line 19 and / or line 20) is reduced, the Circuit compressor unchanged with constant throughput and constant final pressure continues to run, as well as the air compressor not shown in the drawings.
  • the maximum compressed gas production with one Liquid production of, for example, 0% of the amount of feed air to be achieved do exactly the opposite.
  • the condenser-evaporator 214 will then operated on the evaporation side at a pressure which is about 0.2 bar higher than the pressure at the bottom of the single column; in extreme cases, the two pressures can also be the same his. This procedure nevertheless results in an energy saving of approximately 30% against a standard nitrogen generator.
  • the (not shown) Air compressor and the cycle compressor 9 are preferably in the invention a combined machine and with a common drive Mistake.
  • the characteristic curve of the apparatus can be fully automatically between the above mentioned extreme operating cases and every intermediate case back and forth be brought here without the compression machines (air compressors and Circuit compressor) must be readjusted. Just have to be adjusted the residual gas turbine and the amount of gaseous product nitrogen.
  • FIGS. 3 to 8 show how the method according to the invention relates to a Obtaining pure oxygen, high-purity oxygen and / or high-purity Nitrogen can expand.
  • FIG. 3 largely corresponds to FIG. 2.
  • the method and the device from FIG. 3 additionally have a pure nitrogen column 335 with a bottom evaporator 336.
  • Top nitrogen 337 from the individual column 4 (operating pressure here: about 3 bar at the top) is at least partially condensed in the bottom evaporator 336 and fed via line 338 after throttling 339 to about 2.5 bar to the top of the pure nitrogen column 335.
  • Highly volatile components, in particular helium, neon and hydrogen, are stripped off from the liquid flowing down in the column 335 and are stripped off with a purge gas 340.
  • Highly pure nitrogen is obtained in the sump, which still contains about 0.1 ppm of impurities. It forms a first part of the liquid nitrogen product 318.
  • the rest is drawn off via line 342, forms the "nitrogen-rich fraction" and is fed to the circuit compressor 9.
  • the nitrogen-rich liquid 316 generated in the condenser-evaporator 214 is partly fed via line 343 to the top of the pure nitrogen column 335. This amount of liquid nitrogen at the top of the pure nitrogen column 335 corresponds exactly to the LIN product amount 318.
  • the amount 388 is evaporated against itself in the bottom evaporator 336.
  • the circuit compressor 9 is not fed directly with gas from the pure nitrogen column 335, but rather from the top gas 442 of the individual column 4, which here forms the “nitrogen-rich fraction”.
  • the pressure nitrogen product 19, 20 still contains volatile impurities such as helium and neon.
  • the top nitrogen which serves as an insert for the pure nitrogen column 335 and as a heating medium for its bottom evaporator 435, is also circulated and branched upstream of the condenser-evaporator 214 via line 437.
  • the pure nitrogen column 335 can therefore be operated under a higher pressure than the individual column, for example at 8 bar.
  • a further gaseous pressure nitrogen product 444, 445 (UPDGAN) with particularly high purity can be obtained at the bottom of the pure nitrogen column 335.
  • a residual fraction 446 is drawn off from the top of the pure nitrogen column 335 and, for example, heated together with the exhaust gas from the turbine 23 in the main heat exchanger 2.
  • the method and the plant of FIG. 5 serve to obtain additional oxygen with a purity of 99.5 to 99.9999%, preferably 99.5 to 99.9%, which is argon-free (1 ppm argon or less).
  • a mass transfer section around the circumference of 30 to 60 theoretical or practical trays is arranged above the condenser evaporator 514 known from FIGS. 2 to 4, which forms a pure oxygen column 546.
  • the bottom liquid of the individual column 4 is not led directly to the condenser-evaporator 514, but is applied to the top of the pure oxygen column 546. As it flows through this column, it continues to accumulate oxygen.
  • the "liquid oxygen-enriched fraction" is formed here by the bottom liquid of the pure oxygen column 546.
  • the top gas 532 of the pure oxygen column 546 from FIG. 5 forms a first part the "first oxygen-enriched gas” 533 and to a second part the “second oxygen-enriched gas "521.
  • the two fractions are like the ones above described embodiments of the single column or work-related relaxation 23 supplied.
  • an additional column 649 is also provided, which serves to separate less volatile components such as hydrocarbons, krypton and / or xenon from the gaseous bottom product 650 of the pure oxygen column 546. It is operated under the same pressure as the pure oxygen column 546 and has a top condenser 651, which is cooled with a part 652 of the bottom liquid 628 of the individual column 4 which is pressurized in the pump 629. The resulting steam 653 is mixed with the exhaust gas from the turbine 23. Flushing can also be carried out here via line 654. The bottom liquid 655 of the additional column 649 is returned to the bottom of the pure oxygen column 546.
  • High-purity oxygen with a total content of 1 ppm of residual impurities is obtained at the top of the additional column 649. It is delivered to a first part 647, 648 as a gaseous and to a second part 656 as a liquid high-purity product.
  • FIG. 7 shows how the gaseous high-purity oxygen can be released by means of internal compression at a pressure which is higher than the operating pressure of the additional column 649 and is, for example, approximately 8 bar.
  • the entire high-purity product is drawn off in liquid form via line 756 and brought to the increased pressure in a pump 757.
  • At least a part 758 is evaporated under this pressure in the main heat exchanger 2 and removed at 759 as a high-purity pressurized oxygen product.
  • a second turbine 961 in which a part 960 of the cycle nitrogen compressed in the cycle compressor is expanded while performing work. This is shown by way of example in FIG. 9 , which otherwise corresponds to FIG. 2. This part is removed from the main heat exchanger at an intermediate temperature which is equal to the inlet temperature of the first turbine 23 or higher or lower.
  • the expanded nitrogen 962 is fed back into the circuit.
  • FIG. 10 While in the previous exemplary embodiments the residual gas turbine 23 is coupled to a generator or to another braking device for dissipating mechanical energy, in FIG. 10 it drives a booster 1063 directly, which is connected upstream of the externally driven circuit compressor and does some of the compression work without it to consume energy brought in from outside.
  • Figure 10 is otherwise identical to Figure 2. Depending on the size of the system, it may be useful to use such a turbine booster for each of the design variants described.
  • FIG. 10 also shows the optional removal of a nitrogen product 1064 under the outlet pressure of the booster 1063.
  • An essential aspect of the invention consists in a flexible operation of the plant with regard to the liquid product portion.
  • the diagram of FIG. 11 serves to illustrate these possibilities of running the process of FIG. 2 with different or varying product specifications, namely - in the example shown here - with constant operation of the air compressor (9,400 Nm 3 / h at 3.4 bar outlet pressure) and of the circulation compressor 9 (15,200 Nm 3 / h at 9.5 bar outlet pressure).
  • the diagram shows the increase in the amount of liquid product (below the curve) from just above zero (left) to 400 Nm 3 / h.
  • the pressure in the condenser-evaporator and the turbine flow increase, while the oxygen concentration in the condenser and the amount of gaseous product nitrogen decrease.
  • the operating pressure of the column inside the column remains constant.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
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  • Separation By Low-Temperature Treatments (AREA)
  • Treating Waste Gases (AREA)
EP01106637A 2000-03-17 2001-03-16 Procédé de production d'azote liquide et gazeux avec une quantité variable de liquide Expired - Lifetime EP1134525B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE10013075A DE10013075A1 (de) 2000-03-17 2000-03-17 Verfahren zur Gewinnung von gasförmigem und flüssigem Stickstoff mit variablem Anteil des Flüssigprodukts
DE10013075 2000-03-17
EP01105924 2001-03-09
EP01105924 2001-03-09

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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007031759A1 (de) 2007-07-07 2009-01-08 Linde Ag Verfahren und Vorrichtung zur Erzeugung von gasförmigem Druckprodukt durch Tieftemperaturzerlegung von Luft
DE102007031765A1 (de) 2007-07-07 2009-01-08 Linde Ag Verfahren zur Tieftemperaturzerlegung von Luft
DE102009034979A1 (de) 2009-04-28 2010-11-04 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von gasförmigem Drucksauerstoff
EP2312248A1 (fr) 2009-10-07 2011-04-20 Linde Aktiengesellschaft Procédé et dispositif de production d'oxygène sous pression et de crypton/xénon
EP2458311A1 (fr) 2010-11-25 2012-05-30 Linde Aktiengesellschaft Procédé et dispositif de production d'un produit d'impression gazeux par décomposition à basse température d'air
DE102010052544A1 (de) 2010-11-25 2012-05-31 Linde Ag Verfahren zur Gewinnung eines gasförmigen Druckprodukts durch Tieftemperaturzerlegung von Luft
EP2520886A1 (fr) 2011-05-05 2012-11-07 Linde AG Procédé et dispositif de production d'un produit comprimé à oxygène gazeux par décomposition à basse température d'air
EP2568242A1 (fr) 2011-09-08 2013-03-13 Linde Aktiengesellschaft Procédé et dispositif destinés à la production d'acier
EP2600090A1 (fr) 2011-12-01 2013-06-05 Linde Aktiengesellschaft Procédé et dispositif destinés à la production d'oxygène sous pression par décomposition à basse température de l'air
DE102011121314A1 (de) 2011-12-16 2013-06-20 Linde Aktiengesellschaft Verfahren zur Erzeugung eines gasförmigen Sauerstoff-Druckprodukts durch Tieftemperaturzerlegung von Luft
DE102013017590A1 (de) 2013-10-22 2014-01-02 Linde Aktiengesellschaft Verfahren zur Gewinnung eines Krypton und Xenon enthaltenden Fluids und hierfür eingerichtete Luftzerlegungsanlage
DE102012017488A1 (de) 2012-09-04 2014-03-06 Linde Aktiengesellschaft Verfahren zur Erstellung einer Luftzerlegungsanlage, Luftzerlegungsanlage und zugehöriges Betriebsverfahren
EP2784420A1 (fr) 2013-03-26 2014-10-01 Linde Aktiengesellschaft Procédé de séparation de l'air et installation de séparation de l'air
WO2014154339A2 (fr) 2013-03-26 2014-10-02 Linde Aktiengesellschaft Procédé de séparation d'air et installation de séparation d'air
EP2801777A1 (fr) 2013-05-08 2014-11-12 Linde Aktiengesellschaft Installation de décomposition de l'air dotée d'un entraînement de compresseur principal
EP2963371A1 (fr) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Procede et dispositif de production d'un produit de gaz sous pression par decomposition a basse temperature d'air
EP2963367A1 (fr) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Procédé et dispositif cryogéniques de séparation d'air avec consommation d'énergie variable
EP2963370A1 (fr) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Procede et dispositif cryogeniques de separation d'air
EP2963369A1 (fr) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Procede et dispositif cryogeniques de separation d'air
CN114183997A (zh) * 2021-11-22 2022-03-15 四川空分设备(集团)有限责任公司 一种制取低压氮气的装置及方法

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US20060260327A1 (en) * 2005-05-18 2006-11-23 Shoji Kanamori Apparatus and method for rapidly freezing small objects
DE102007024168A1 (de) * 2007-05-24 2008-11-27 Linde Ag Verfahren und Vorrichtung zur Tieftemperatur-Luftzerlegung
DE102007051184A1 (de) * 2007-10-25 2009-04-30 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Tieftemperatur-Luftzerlegung
DE102007051183A1 (de) * 2007-10-25 2009-04-30 Linde Aktiengesellschaft Verfahren zur Tieftemperatur-Luftzerlegung
WO2014154361A2 (fr) * 2013-03-28 2014-10-02 Linde Aktiengesellschaft Procédé et dispositif permettant de produire avec une consommation d'énergie variable de l'oxygène sous pression sous forme gazeuse
DE202015004181U1 (de) 2015-06-12 2015-07-09 Linde Aktiengesellschaft Luftzerlegungsanlage und Steuereinrichtung für Luftzerlegungsanlage
CN112805524B (zh) * 2018-10-23 2022-12-06 林德有限责任公司 用于低温分离空气的方法和设备
WO2021204418A1 (fr) * 2020-04-09 2021-10-14 Linde Gmbh Procédé de production d'un produit d'azote gazeux et liquide au moyen d'une séparation à basse température de l'air, et système de séparation d'air
CN114165988B (zh) * 2021-11-22 2023-01-31 四川空分设备(集团)有限责任公司 低压氮制取装置及方法
JP7379764B1 (ja) * 2022-08-09 2023-11-15 レール・リキード－ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード 空気分離装置および空気分離方法

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DE10013073A1 (de) * 2000-03-17 2000-10-19 Linde Ag Verfahren und Vorrichtung zur Tieftemperaturzerlegung von Luft

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DE102007031759A1 (de) 2007-07-07 2009-01-08 Linde Ag Verfahren und Vorrichtung zur Erzeugung von gasförmigem Druckprodukt durch Tieftemperaturzerlegung von Luft
DE102007031765A1 (de) 2007-07-07 2009-01-08 Linde Ag Verfahren zur Tieftemperaturzerlegung von Luft
EP2015012A2 (fr) 2007-07-07 2009-01-14 Linde Aktiengesellschaft Procédé pour la séparation cryogénique d'air
EP2015013A2 (fr) 2007-07-07 2009-01-14 Linde Aktiengesellschaft Procédé et dispositif de production d'un gaz sous pression par séparation cryogénique d'air
DE102009034979A1 (de) 2009-04-28 2010-11-04 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von gasförmigem Drucksauerstoff
EP2312248A1 (fr) 2009-10-07 2011-04-20 Linde Aktiengesellschaft Procédé et dispositif de production d'oxygène sous pression et de crypton/xénon
EP2458311A1 (fr) 2010-11-25 2012-05-30 Linde Aktiengesellschaft Procédé et dispositif de production d'un produit d'impression gazeux par décomposition à basse température d'air
DE102010052545A1 (de) 2010-11-25 2012-05-31 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung eines gasförmigen Druckprodukts durch Tieftemperaturzerlegung von Luft
DE102010052544A1 (de) 2010-11-25 2012-05-31 Linde Ag Verfahren zur Gewinnung eines gasförmigen Druckprodukts durch Tieftemperaturzerlegung von Luft
EP2466236A1 (fr) 2010-11-25 2012-06-20 Linde Aktiengesellschaft Procédé de production d'un produit d'impression gazeux par décomposition à basse température de l'air
EP2520886A1 (fr) 2011-05-05 2012-11-07 Linde AG Procédé et dispositif de production d'un produit comprimé à oxygène gazeux par décomposition à basse température d'air
DE102011112909A1 (de) 2011-09-08 2013-03-14 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von Stahl
EP2568242A1 (fr) 2011-09-08 2013-03-13 Linde Aktiengesellschaft Procédé et dispositif destinés à la production d'acier
EP2600090A1 (fr) 2011-12-01 2013-06-05 Linde Aktiengesellschaft Procédé et dispositif destinés à la production d'oxygène sous pression par décomposition à basse température de l'air
DE102011121314A1 (de) 2011-12-16 2013-06-20 Linde Aktiengesellschaft Verfahren zur Erzeugung eines gasförmigen Sauerstoff-Druckprodukts durch Tieftemperaturzerlegung von Luft
DE102012017488A1 (de) 2012-09-04 2014-03-06 Linde Aktiengesellschaft Verfahren zur Erstellung einer Luftzerlegungsanlage, Luftzerlegungsanlage und zugehöriges Betriebsverfahren
EP2784420A1 (fr) 2013-03-26 2014-10-01 Linde Aktiengesellschaft Procédé de séparation de l'air et installation de séparation de l'air
WO2014154339A2 (fr) 2013-03-26 2014-10-02 Linde Aktiengesellschaft Procédé de séparation d'air et installation de séparation d'air
EP2801777A1 (fr) 2013-05-08 2014-11-12 Linde Aktiengesellschaft Installation de décomposition de l'air dotée d'un entraînement de compresseur principal
DE102013017590A1 (de) 2013-10-22 2014-01-02 Linde Aktiengesellschaft Verfahren zur Gewinnung eines Krypton und Xenon enthaltenden Fluids und hierfür eingerichtete Luftzerlegungsanlage
EP2963371A1 (fr) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Procede et dispositif de production d'un produit de gaz sous pression par decomposition a basse temperature d'air
EP2963367A1 (fr) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Procédé et dispositif cryogéniques de séparation d'air avec consommation d'énergie variable
EP2963370A1 (fr) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Procede et dispositif cryogeniques de separation d'air
EP2963369A1 (fr) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Procede et dispositif cryogeniques de separation d'air
WO2016005031A1 (fr) 2014-07-05 2016-01-14 Linde Aktiengesellschaft Procédé et dispositif de fractionnement de l'air à basse température à consommation d'énergie variable
CN114183997A (zh) * 2021-11-22 2022-03-15 四川空分设备(集团)有限责任公司 一种制取低压氮气的装置及方法

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EP1134525B1 (fr) 2010-09-15
US20010054298A1 (en) 2001-12-27
DE50115625D1 (de) 2010-10-28
ATE481607T1 (de) 2010-10-15
DE10013075A1 (de) 2001-09-20

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