EP1134525B1 - 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
EP1134525B1
EP1134525B1 EP01106637A EP01106637A EP1134525B1 EP 1134525 B1 EP1134525 B1 EP 1134525B1 EP 01106637 A EP01106637 A EP 01106637A EP 01106637 A EP01106637 A EP 01106637A EP 1134525 B1 EP1134525 B1 EP 1134525B1
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Prior art keywords
column
oxygen
nitrogen
liquid
condenser
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Expired - Lifetime
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EP01106637A
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German (de)
English (en)
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EP1134525A1 (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
    • 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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    • 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 is for the recovery of gaseous and liquid nitrogen with variable proportion of the liquid product by cryogenic separation of air in a distillation column system having a single column.
  • Single column methods are a common method of producing nitrogen. In contrast to double column methods, they have only one pressure column (the single column) and no further column (low pressure column) which is used for nitrogen-oxygen separation and operated at a lower pressure than the pressure column. This does not preclude the distillation column system from having additional columns beyond the single column, for example for obtaining 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 expansion machines.
  • the distillation column system is formed exclusively by the single column.
  • oxygen-enriched is meant here a mixture of air gases having a higher oxygen concentration than air, up to practically pure oxygen.
  • fractions having an oxygen content of 25 to 90%, preferably 30 to 80% are fractions having an oxygen content of 25 to 90%, preferably 30 to 80%. (All percentages here and below refer to the molar amount, unless stated otherwise.)
  • the method serves for the simultaneous production of gaseous and liquid product nitrogen, wherein the liquid fraction (molar ratio between liquid and gaseous product nitrogen) may be variable. At different times, therefore, different stationary operating states can prevail, for which a different proportion of the nitrogen product is obtained in liquid form, in extreme cases, this proportion can also be zero.
  • the process can then be moved back and forth between two borderline cases, the maximum gas production (MaxGAN case) with minimal liquid content and the maximum liquid production (MaxLIN case) with maximum liquid content and minimal gas content (possibly only liquid production of nitrogen). In this case, any desired value of the liquid fraction, which lies between the two limit values for minimum and maximum liquid content, can also be set.
  • a method with a nitrogen cycle according to the preamble of claim 1 is US 4400188 known.
  • nitrogen which was brought in a cycle compressor on column pressure, a condenser-evaporator is heated, which is the sump heating of the single column.
  • Process refrigeration is produced by a conventional residual gas turbine, which is operated with gas from another condenser-evaporator, a top condenser.
  • Such nitrogen cycle processes are energetically more favorable than single column processes without sump heating. Because of the cycle, even in this process, a liquid nitrogen product can in principle be generated in a variable amount, even if this is not described in the document itself. However, difficulties would arise in such a process if one wanted to vary the proportion of liquid product.
  • the invention has for its object to provide a method of the type mentioned above and a corresponding device in which in addition to the gaseous nitrogen product, a variable amount of liquid product can be obtained with relatively little effort.
  • This object is achieved in that a portion of the nitrogen-rich liquid from the condenser-evaporator is at least temporarily withdrawn as a liquid product, the evaporation space of the condenser-evaporator is operated under a pressure which is higher than the operating pressure of the single column and a second oxygen-enriched gas is taken from one of the columns of the distillation column system and / or from the evaporation space of the condenser-evaporator, work-expanded and heated in the main heat exchanger.
  • the liquid product can be taken directly from the liquefaction space of the condenser-evaporator. Preferably, however, it is first relaxed and thereby resulting flash gas separated.
  • the phase separation can be carried out, for example, in the single column or in a separate separator.
  • the operating pressures of the condenser-evaporator and the single column are decoupled.
  • the pressure on the liquefaction side of the condenser-evaporator nitrogen cycle
  • the pressure on the evaporation side-irrespective of the operating pressure of the single column- can be adjusted to the lower oxygen concentration at the same evaporation temperature without having to readjust any compression machines.
  • the second oxygen-enriched gas which is intended for work-performing expansion, is preferably generated, like the first oxygen-enriched gas, from the vapor formed in the condenser-evaporator.
  • the two oxygen-enriched gases have the same composition.
  • the inlet pressure of the work-performing expansion is not bound to the single-column or top-condenser pressure, as is usual with residual gas turbines, but preferably to the evaporation pressure in the condenser-evaporator. Therefore, the inlet pressure of the turbine may increase in line with an increase in the proportion of liquid product analogous to the evaporation pressure.
  • the correspondingly increased enthalpy difference in the work-performing expansion of the second oxygen-enriched gas produces the additional cold that is necessary for the increased product liquefaction.
  • the increase in the amount of residual gas also increases the production of refrigerants.
  • the liquid product content may for example be 0 to 20%, preferably 0 to 16% of the total nitrogen product, with a total product amount of nitrogen of 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 condenser-evaporator and the lower portion of the column is for example 0 to 5 bar, preferably 0 to 3 bar.
  • the second oxygen-enriched gas Since the second oxygen-enriched gas must ultimately come from the single column, it needs a corresponding pressure increasing step, which is preferably carried out in the liquid state in the invention, for example by means of a liquid pump.
  • a pressure increasing step which is preferably carried out in the liquid state in the invention, for example by means of a liquid pump.
  • an oxygen-enriched liquid is withdrawn from the single column and brought to an elevated pressure in the liquid state, wherein the second oxygen-enriched gas is generated from the resulting under elevated pressure oxygen-enriched liquid.
  • the oxygen-enriched liquid downstream of the pressure increase forms the oxygen-enriched liquid fraction which is introduced into the evaporation space of the condenser-evaporator.
  • the oxygen-enriched liquid is formed for example by the bottom liquid of the single column and brought by means of a pump to at least the increased pressure, below which the evaporation space of the condenser-evaporator.
  • the first and the second oxygen-enriched gas, ie the rising vapor for the single column and the work-performing relaxing fraction, are here produced directly by evaporation of the liquid fraction from the single column.
  • the distillation column system has, in addition to the single column, a pure oxygen column.
  • the oxygen-enriched liquid from the single column is fed to the pure oxygen column downstream of the pressure increase.
  • an oxygen-rich fraction is withdrawn as gaseous and / or liquid product and / or intermediate.
  • the liquid oxygen-enriched fraction, the evaporation space of the Condenser evaporator is also derived from the lower part of the pure oxygen column.
  • the vapor generated in the condenser-evaporator is introduced into the lower part of the pure oxygen column and used there as rising steam.
  • the head gas of the pure oxygen column serves as a working gas of the working expansion ("second oxygen-enriched gas”) and to a second part - after 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 condenser-evaporator prevails in this variant, a higher circuit pressure than in embodiments in which the evaporation side of the condenser-evaporator is subjected to bottom liquid of the single column.
  • the liquid brought to the elevated pressure from the single column is further enriched in oxygen and depleted in more volatile components.
  • Liquid and / or vapor from the bottom of the pure oxygen column can be withdrawn directly as an oxygen product and / or fed to a further working step.
  • the condenser-evaporator is preferably arranged directly in the bottom of the pure oxygen column in this embodiment of the invention, but it can also be accommodated 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 feeding it to an auxiliary column for removal of low volatility impurities from the top of which a pure oxygen product is withdrawn.
  • the oxygen-rich fraction is preferably withdrawn from the bottom of the pure oxygen column or from the evaporation space of the condenser-evaporator.
  • the rising vapor in the additional column is freed of less volatile components which are depleted in the pure oxygen product (for example less than 100 ppm, preferably less than 10 ppm of higher boiling point impurities than oxygen; about 1 ppb can be achieved). Residual liquid from the additional column can be returned to the pure oxygen column or the condenser-evaporator.
  • the additional column is preferably designed as a pure reinforcing column and contains, for example, 10 to 40, preferably 10 to 30 theoretical plates.
  • Return liquid for the additional column is preferably produced in a top condenser, in which a second oxygen-enriched liquid fraction from the lower region of the single column is at least partially evaporated.
  • the second oxygen-enriched liquid fraction can be withdrawn from the single column together with the oxygen-enriched liquid applied to the pure oxygen column and brought to elevated pressure.
  • the entire reflux liquid for the single column and optionally the pure oxygen column is produced in the condenser-evaporator. It is therefore generally only a single condenser-evaporator required in the case of an additional column two.
  • Air compressor and cycle compressor can be formed by a single machine, namely by a combi-machine, in which several pinions sit on a shaft, some of which implement the air compressor and one or more of the cycle compressor.
  • the cyclic compressor may be at least partially formed by a compressor coupled to the residual gas turbine, wherein at least a portion of the mechanical energy generated during work expansion of the second oxygen-enriched gas is used to compress the first part and / or the second part of the nitrogen-rich fraction.
  • the distillation column system has a pure nitrogen column, wherein a nitrogen fraction from the upper region of the single column in the liquid state is applied to the pure nitrogen column and a pure nitrogen product is withdrawn from the lower region of the pure nitrogen column.
  • the pure nitrogen column serves to deplete volatile nitrogen impurities, in particular helium, neon and hydrogen.
  • the bottoms product of the pure nitrogen column is virtually free of helium, neon and hydrogen (eg less than 10 ppb, preferably less than 5 ppb of impurities more volatile than nitrogen) and can be withdrawn 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 be operated either with very pure gas from the lower region of the pure nitrogen column or with head gas of the single column. It is also possible gaseous pressure product (second part of the nitrogen-rich fraction from the distillation system) helium and neon-free from the pure nitrogen column and / or slightly less purely deducted from the head of the single column.
  • the pure nitrogen column preferably has a bottom evaporator, wherein the nitrogen fraction is removed in gaseous form from the single column and liquefied prior to its task on the pure nitrogen column in the bottom evaporator.
  • the operating pressure of the pure nitrogen column is slightly lower (for example by 0.5 to 1.0 bar) than the pressure at the top of the single column. The liquefied in the bottom evaporator fraction is relaxed before the task on the pure nitrogen column to its operating pressure.
  • the invention also relates to a device according to claim 12.
  • FIG. 1 In the process of FIG. 1 is introduced via a line 1 compressed and purified feed air, which is under a pressure of about 3.5 bar.
  • Air compressor and air purification - for example by means of a molecular sieve - are not shown in the drawing.
  • the air is cooled in a main heat exchanger 2 to about dew point and fed via line 3 of a single column 4 at an intermediate point.
  • the intermediate point is, for example, 5 to 20 theoretical plates or practically above the bottom of the column 4.
  • the operating pressure at the bottom of the single 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 heated in a subcooler 6 and (line 7) further in the main heat exchanger 2 to about ambient temperature.
  • the warm head nitrogen 8 is fed to a cycle compressor 9, which has, for example, two to three stages. Behind each stage of the cycle compressor is a subsequent or intermediate cooling to remove the heat of compression, of which, however, only the aftercooling 10 is shown behind the final stage in the schematic drawing.
  • 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, cooled there to several Kelvin above the column temperature and fed via line 13 to the liquefaction space of a condenser-evaporator 14.
  • the nitrogen-rich liquid 15 formed in the process is subcooled in the subcooler 6 and fed via line 16 and throttle valve 17 to the top of the single column.
  • a portion 18 of the nitrogen-rich liquid 16 may be withdrawn as liquid nitrogen product LIN.
  • the liquid production in the example is about 0% of the amount of air.
  • the liquid nitrogen is withdrawn from the single column, the head serves here as a flash gas between the throttle valve 17 and the liquid product removal 18.
  • a second part 19 of the compressed in the cycle compressor 9 head nitrogen 11 is discharged as a gaseous nitrogen product under pressure (DGAN).
  • DGAN gaseous nitrogen product under pressure
  • a portion 20 of the pressurized nitrogen can be led out of an intermediate stage of the cycle compressor and recovered at a pressure between the operating pressure of the individual column 4 and the final pressure of the cycle compressor 9 as gaseous pressure nitrogen product (DGAN ').
  • DGAN ' gaseous pressure nitrogen product
  • the cycle compressor 9 serves as a product compressor at the same time.
  • the condenser-evaporator 14 is in the example of FIG. 1 arranged directly in the bottom of the single column. On its evaporation side, the oxygen-enriched bottoms liquid of the single column 4 evaporates below its operating pressure to form a vapor having an oxygen content of about 80%. While a first part of the vapor generated in the condenser-evaporator 14 rises in the single column 4 ("first oxygen-enriched gas”), a second part 21 (“second oxygen-enriched gas”) is led to the cold end of the main heat exchanger 2. After warming to an intermediate temperature, this fraction flows via line 22 to a residual gas turbine 23 and is there to perform work from about 3 bar to about 1.5 bar relaxed.
  • the work expanded oxygen-enriched gas 24 is completely warmed in the main heat exchanger 2 and discharged via line 25 as impure oxygen product UGOX. It can be used as a regeneration gas in the air purification, not shown, and / or as a gaseous by-product and / or released into the atmosphere.
  • the turbine 23 can be regulated via a bypass 26. A small amount of liquid 27 is discharged continuously or intermittently as rinsing liquid from the evaporation space of the condenser-evaporator 14.
  • the method according to FIG. 1 differs from the prior art according to US 4400188 by the way of cooling. This is accomplished here by working expansion of an oxygen-enriched gas 21 from the evaporation space of the condenser-evaporator 14. Although this measure causes a simplification of the apparatus, since only a single condenser-evaporator for the operation of the single column 4 is required, but this alone can not perform the desired simple variation of the liquid product content, as in the embodiments of the FIGS. 2 to 10 the case is.
  • the condenser-evaporator 214 is arranged in a separate container outside the single column 4. In the present case, this not only represents an apparatus-specific detail, but also enables the decoupling of the pressure in the evaporation space of the condenser-evaporator 214 from the operating pressure of the single column 4.
  • the bottoms liquid (the "liquid oxygen-enriched fraction") 228 is here by means of a pump 229 brought a pressure of 4 to 8 bar and introduced under this increased pressure or optionally after slight throttling 230 via line 231 in the evaporation space of the condenser-evaporator 214.
  • first oxygen-enriched gas a first portion
  • second oxygen-enriched gas a second oxygen-enriched gas
  • the procedure is reversed exactly the reverse.
  • the condenser-evaporator 214 is then driven on the evaporation side with a pressure which is about 0.2 bar higher than the pressure at the bottom of the single column; the two pressures can be the same in extreme cases.
  • the air compressor (not shown) and the cycle compressor 9 are preferably combined in the invention in a combination machine and provided with a common drive.
  • the characteristic curve of the apparatus can be moved back and forth fully automatically between the abovementioned extreme operating cases and any intervening case, without the compaction machines (air compressor and cycle compressor) having to be readjusted. Only the residual gas turbines and the amount of gaseous product nitrogen need to be adjusted.
  • FIGS. 3 to 8 show how the inventive method can be extended to a recovery of pure oxygen, high purity oxygen and / or high purity nitrogen.
  • FIG. 3 corresponds largely FIG. 2 , The method and the device of FIG. 3 However, they additionally have a pure nitrogen column 335 with bottom evaporator 336. Head 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 head of the pure nitrogen column 335. From the liquid flowing down in the column 335, more volatile components, in particular helium, neon and hydrogen are stripped off, which are withdrawn with a purge gas 340. In the swamp falls to highly pure nitrogen, which still contains about 0.1 ppm of impurities. It forms the liquid nitrogen product 318 to a first part.
  • Head 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 head of the pure nitrogen column 335.
  • the remainder is withdrawn via line 342, forms the "nitrogen-rich fraction" and is fed to the cycle compressor 9.
  • the nitrogen-rich liquid 316 produced in the condenser-evaporator 214 is partially fed to the top of the pure nitrogen column 335 via line 343. This amount of liquid nitrogen at the top of the pure nitrogen column 335 corresponds exactly to the amount of LIN product 318.
  • the amount 388 is evaporated in the bottom evaporator 336 against itself.
  • the cycle compressor 9 is different from FIG. 3 not directly fed with gas from the pure nitrogen column 335, but from the head gas 442 of the single column 4, which here forms the "nitrogen-rich fraction".
  • the pressurized nitrogen product 19, 20 still contains volatile contaminants such as helium and neon.
  • the overhead nitrogen which serves as an insert for the pure nitrogen column 335 and as a heating means for the bottom evaporator 435, is recirculated and branched off upstream of the condenser-evaporator 214 via line 437.
  • the pure nitrogen column 335 can therefore be operated at a higher pressure than the single column, for example at 8 bar.
  • a further gaseous compressed nitrogen product 444, 445 (UPDGAN) with particularly high purity can be obtained at the bottom of the pure nitrogen column 335. From the top of the pure nitrogen column 335, a residual fraction 446 is withdrawn and, for example, warmed together with the exhaust gas of the turbine 23 in the main heat exchanger 2.
  • the procedure and the plant of FIG. 5 serve to obtain additional oxygen of purity of 99.5 to 99.9999%, preferably 99.5 to 99.9%, which is argon-free (1 ppm argon or less).
  • This is above the from the FIGS. 2 to 4 known capacitor evaporator 514 a mass transfer section arranged around the periphery of 30 to 60 theoretical or practical trays, which forms a pure oxygen column 546.
  • the bottom liquid 528 of the single column 4 is not led directly to the condenser-evaporator 514, but fed to the head 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 of FIG. 5 forms to a first part of the "first oxygen-enriched gas” 533 and a second part of the "second oxygen-enriched gas” 521.
  • the two fractions are supplied as in the embodiments described above, the single column or the work-performing expansion 23.
  • a gaseous oxygen product GOX is withdrawn via the lines 547 and 548, which is purer than the first oxygen-enriched gas fraction 532.
  • an additional column 649 which serves for the separation of 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 sump liquid 628 of the single column 4 pressurized in the pump 629. Resulting steam 653 is added to the exhaust gas of the turbine 23. Via line 654 can also be made here a purge. The bottom liquid 655 of the additional column 649 is returned to the bottom of the pure oxygen column 546. At the top of the additional column 649, highly pure oxygen with a total content of 1 ppm of residual impurities accumulates. It is delivered to a first part 647, 648 as gaseous and to a second part 656 as liquid high purity product.
  • FIG. 7 shows how the gaseous high purity oxygen can be discharged by means of internal compression under a pressure which is higher than the operating pressure of the additional column 649 and is for example about 8 bar.
  • the entire high purity product is withdrawn via line 756 liquid, brought in a pump 757 to the elevated pressure. At least a portion 758 is vaporized under this pressure in the main heat exchanger 2 and discharged at 759 as a high purity pressure oxygen product.
  • FIG. 8 are the pure nitrogen column 335 from FIG. 3 and the two columns 546 and 649 of FIG. 6 realized together, so that nitrogen and oxygen can be obtained simultaneously as high purity products UPDGAN, UPGOX.
  • a second turbine 961 in which a part 960 of the circulating nitrogen compressed in the cycle compressor is expanded to perform work. This is in FIG. 9 exemplified, the otherwise FIG. 2 equivalent. This part is discharged at an intermediate temperature from the main heat exchanger, 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 circulation.
  • the residual gas turbine 23 is coupled to a generator or to another braking device for dissipating mechanical energy, it drives in FIG. 10 directly to a booster 1063, which is upstream of the externally driven cycle compressor and this part of the compression work decreases, without consuming externally introduced energy.
  • FIG. 10 is otherwise with FIG. 2 identical. Depending on the size of the system, it may be useful in each of the described embodiments to use such a turbine booster. In FIG. 10 In addition, the optional removal of a 1064 nitrogen product at the exit pressure of booster 1063 is shown.
  • An essential aspect of the invention consists in a flexible operation of the plant with regard to the liquid product content.
  • the diagram of FIG. 11 serves to illustrate these possibilities, the process of FIG. 2 to drive with different or varying product specifications, and indeed - in this one Example shown - at constant operation of the air compressor (9,400 Nm 3 / h at 3.4 bar outlet pressure) and the cycle compressor 9 (15,200 Nm 3 / h at 9.5 bar outlet pressure).
  • the diagram shows the increase of the liquid product quantity (under 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 within the column remains constant.

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Claims (12)

  1. Procédé de production d'azote gazeux ou liquide à une proportion variable de produit liquide, par décomposition d'air à basse température dans un système à colonne de distillation qui présente une seule colonne (4), tandis que dans le procédé :
    - de l'air d'alimentation (1) est comprimé dans un compresseur d'air, est refroidi dans un échangeur de chaleur principal (2) et est apporté (3) à la colonne unique (4),
    - une fraction (5, 7, 8) riche en azote dont au moins une première partie étant comprimée dans un compresseur de circuit (9, 1063) est extraite du système de colonne de distillation,
    - la première partie (12, 13) de la fraction (5, 7, 8) riche en azote est apportée en aval du compresseur de circuit (1063, 9) à la chambre de liquéfaction d'un évaporateur-condenseur (214) pour y être condensée sous une pression supérieure à la pression de travail de la colonne unique (4), ce qui produit du liquide (15, 16) riche en azote,
    - au moins une partie d'une fraction liquide (228, 231) riche en oxygène provenant du système de colonne de distillation est évaporée dans la chambre d'évaporation de l'évaporateur-condenseur (214),
    - un premier gaz (234, 533) riche en oxygène est produit à partir de la vapeur (232) produite dans la chambre d'évaporation de l'évaporateur-condenseur (214), est introduit dans la colonne unique (4) et y est utilisé comme vapeur montante et
    - une deuxième partie (19, 20, 1064) de la fraction (5, 7, 8) riche en azote est extraite au moins une partie du temps sous la forme d'un produit gazeux d'azote,
    caractérisé en ce que
    - une partie (18) du liquide (15, 16) riche en azote est extraite de l'évaporateur-condenseur (214) au moins une partie du temps sous la forme d'un produit liquide,
    - la chambre d'évaporation de l'évaporateur-condenseur (214) est conduite au moins une partie du temps sous une pression supérieure à la pression de travail de la colonne unique (4) et
    - un deuxième gaz (221, 521) enrichi en oxygène est prélevé de l'une (546) des colonnes du système de distillation et/ou de la chambre d'évaporation de l'évaporateur-condenseur (214), est détendue (23) en produisant du travail et est chauffée dans l'échangeur de chaleur principal (2).
  2. Procédé selon la revendication 1, caractérisé en ce qu'un liquide (228, 528) enrichi en azote est extrait de la colonne unique (4) et est amené (229) à l'état liquide à une pression plus élevée, le deuxième gaz (232, 221, 521) enrichi en oxygène étant produit à partir du liquide (231) ainsi obtenu, enrichi en oxygène et placé sous pression plus élevée.
  3. Procédé selon la revendication 2, caractérisé en ce que le liquide (231) enrichi en oxygène forme en aval de l'augmentation de pression (229) la fraction liquide enrichie en oxygène qui est introduite dans la chambre d'évaporation de l'évaporateur-condenseur (214).
  4. Procédé selon la revendication 2, caractérisé en ce que le système de colonne de distillation présente une colonne (546) à oxygène pur, le liquide (231) enrichi en oxygène étant délivré en aval de l'augmentation de pression (229) dans la colonne (546) à oxygène pur et une fraction (547) riche en oxygène est extraite de la partie inférieure de la colonne (546) à oxygène pur, la fraction liquide enrichie en oxygène qui est apportée dans la chambre d'évaporation de l'évaporateur-condenseur (514) provenant de la partie inférieure de la colonne (546) à oxygène pur, la vapeur produite dans l'évaporateur-condenseur (514) étant introduite dans la partie inférieure de la colonne (546) à oxygène pur pour y être utilisée comme vapeur montante.
  5. Procédé selon la revendication 4, caractérisé en ce que le système de colonne de distillation présente une colonne supplémentaire (649) qui sert à éliminer les impuretés moins volatiles, la fraction (650) enrichie en oxygène provenant de la colonne (546) à oxygène pur étant introduite dans la colonne supplémentaire (649) et un produit d'oxygène pur (647, 656, 756, 758, 759) étant extrait de la partie supérieure de la colonne supplémentaire (649).
  6. Procédé selon la revendication 5, caractérisé en ce que la colonne supplémentaire (649) présente un condenseur de tête (651) dans lequel une deuxième fraction liquide (652) enrichie en oxygène provenant de la partie inférieure de la colonne unique (4) est évaporée au moins en partie.
  7. Procédé selon l'une des revendications précédentes, caractérisé en ce que la totalité du liquide renvoyé dans la colonne unique (4) et éventuellement dans la colonne (546) à oxygène pur est produit dans l'évaporateur-condenseur (14, 514).
  8. Procédé selon l'une des revendications précédentes, caractérisé en ce que le compresseur d'air et le compresseur de circuit (9) sont constitués d'une seule machine.
  9. Procédé selon l'une des revendications précédentes, caractérisé en ce qu'au moins une partie de l'énergie mécanique produite lors de la détente (23) avec production de travail du deuxième gaz (221, 521) enrichi en oxygène est utilisée pour comprimer (1063) la première partie et/ou la deuxième partie de la fraction (5, 7, 8) riche en azote.
  10. Procédé selon l'une des revendications précédentes, caractérisé en ce que le système de colonne de distillation présente une colonne (335) à azote pur, une fraction d'azote (338, 437) provenant de la partie supérieure de la colonne unique (4) étant délivrée à l'état liquide dans la colonne (335) à azote pur et un produit d'azote pur (318, 444, 445) étant extrait de la partie inférieure de la colonne (335) à azote pur.
  11. Procédé selon la revendication 10, caractérisé en ce que la colonne (335) à azote pur présente un évaporateur de pied (336, 435), la fraction d'azote (337, 437) étant prélevée à l'état gazeux de la colonne unique (4) et étant liquéfiée avant d'être délivrée (338, 339) dans l'évaporateur de pied (336, 435) de la colonne (335) à azote pur.
  12. Dispositif de production d'azote gazeux et d'azote liquide avec une fraction variable de produit liquide, par décomposition d'air à basse température dans un système de colonnes de distillation qui contiennent une colonne (4), et présentant :
    - un compresseur d'air,
    - un conduit d'alimentation (1, 3) qui relie le compresseur d'air à la colonne (4) par l'intermédiaire d'un échangeur de chaleur principal (2),
    - un compresseur de circuit (9, 1063) qui comprime la première partie d'une fraction (5, 7, 8) riche en azote provenant du système de colonnes de distillation,
    - un conduit de circuit (12, 13) qui relie la sortie du compresseur de circuit (1063, 9) à la chambre de liquéfaction d'un évaporateur-condenseur (14),
    - des moyens (228, 231) qui amènent une fraction liquide enrichie en oxygène provenant du système de colonnes de distillation à la chambre d'évaporation de l'évaporateur-condenseur (14),
    - des moyens de production d'un gaz (233, 533) enrichi en oxygène provenant de la vapeur (232) formée dans la chambre d'évaporation de l'évaporateur-condenseur (14) et pour l'introduire dans la colonne (4) et
    - un conduit de produit gazeux qui extrait une deuxième partie (19, 20, 1064) de la fraction (5, 7, 8) riche en azote comme produit gazeux d'azote,
    caractérisé par
    - un conduit de produit liquide (15, 16) relié à la chambre de liquéfaction de l'évaporateur-condenseur (14),
    - l'agencement de l'évaporateur-condenseur (14) à l'intérieur d'un récipient séparé de la colonne (4) et
    - une machine de détente (23) qui détend avec production de travail un deuxième gaz (221, 521) enrichi en oxygène provenant de l'une des colonnes (546) du système de distillation et/ou de la chambre d'évaporation de l'évaporateur-condenseur (14).
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
DE10013075 2000-03-17
DE10013075A DE10013075A1 (de) 2000-03-17 2000-03-17 Verfahren zur Gewinnung von gasförmigem und flüssigem Stickstoff mit variablem Anteil des Flüssigprodukts
EP01105924 2001-03-09
EP01105924 2001-03-09

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US6477860B2 (en) 2002-11-12
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ATE481607T1 (de) 2010-10-15
DE10013075A1 (de) 2001-09-20
US20010054298A1 (en) 2001-12-27

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