WO2022174976A1 - Providing a nitrogen product - Google Patents
Providing a nitrogen product Download PDFInfo
- Publication number
- WO2022174976A1 WO2022174976A1 PCT/EP2022/025017 EP2022025017W WO2022174976A1 WO 2022174976 A1 WO2022174976 A1 WO 2022174976A1 EP 2022025017 W EP2022025017 W EP 2022025017W WO 2022174976 A1 WO2022174976 A1 WO 2022174976A1
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- WO
- WIPO (PCT)
- Prior art keywords
- low
- argon
- air separation
- pressure column
- column
- Prior art date
Links
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 76
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 266
- 229910052786 argon Inorganic materials 0.000 claims abstract description 133
- 238000000926 separation method Methods 0.000 claims abstract description 105
- 239000012530 fluid Substances 0.000 claims abstract description 48
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000001301 oxygen Substances 0.000 claims abstract description 47
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 47
- 239000007789 gas Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000011084 recovery Methods 0.000 claims description 7
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 claims description 5
- 230000007257 malfunction Effects 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 description 23
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000000605 extraction Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
Classifications
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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
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
- F25J3/04715—The auxiliary column system simultaneously produces oxygen
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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
- F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
- 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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- 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
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04163—Hot end purification of the feed air
- F25J3/04169—Hot end purification of the feed air by adsorption of the impurities
- F25J3/04175—Hot end purification of the feed air by adsorption of the impurities at a pressure of substantially more than the highest pressure column
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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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
- F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
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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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
- F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
- F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
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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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
- F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
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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
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
- F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
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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
- F25J3/04793—Rectification, e.g. columns; Reboiler-condenser
- F25J3/048—Argon recovery
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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
- F25J3/04812—Different modes, i.e. "runs" of operation
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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
- F25J3/04812—Different modes, i.e. "runs" of operation
- F25J3/04818—Start-up of the process
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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
- F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
- F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
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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
- F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
- F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
- F25J3/04878—Side by side arrangement of multiple vessels in a main column system, wherein the vessels are normally mounted one upon the other or forming different sections of the same column
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- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
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- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
- F25J2200/06—Processes or apparatus using separation by rectification in a dual pressure main column system in a classical double column flow-sheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
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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
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
- F25J2215/52—Oxygen production with multiple purity O2
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- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
- F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2
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- 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
- F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen
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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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/58—Processes or apparatus involving steps for recycling of process streams the recycled stream being argon or crude argon
Definitions
- the invention relates to an air separation plant and an air separation process for providing a nitrogen product.
- Air separation plants of the classic type have rectification column systems which can be designed, for example, as two-column systems, in particular as double-column systems, but also as three-column or multi-column systems.
- rectification columns for obtaining nitrogen and/or oxygen in the liquid and/or gaseous state ie rectification columns for nitrogen-oxygen separation, rectification columns for obtaining further air components, in particular inert gases, can be provided.
- the rectification columns of the rectification column systems mentioned are operated at pressures in different pressure ranges.
- Known double column systems have a so-called high-pressure column (also referred to as a pressure column, medium-pressure column or lower column) and a so-called low-pressure column (upper column).
- the high-pressure column is typically operated at a pressure in a pressure range of 4 to 7 bar, in particular approx. 5.3 bar, while the low-pressure column is operated at a pressure in a pressure range of typically 1 to 2 bar, in particular approx. 1.4 bar. In certain cases, higher pressures can also be used in both rectification columns.
- the pressures specified here and below in the respective pressure ranges are, in particular, absolute pressures (bar (abs.), bara) at the top of the columns specified in each case.
- a conventionally designed air separation plant with a corresponding double column system is typically designed to provide a gaseous nitrogen product with 100 ppb to 1 ppm oxygen content and more than 10 ppm argon content.
- compressed nitrogen with significantly less than 4 ppm argon is increasingly required.
- Various measures can be taken for this purpose, for example increasing the number of plates for the rectification.
- Corresponding plants are typically equipped with an argon rectification, which traditionally includes a raw and a pure argon column. Further refinements are explained below.
- JP H05 1883 A A method is known from JP H05 1883 A, in which a bypass line is used between an extraction line from a low-pressure column, which opens into a crude argon column, and the low-pressure column.
- the bypass line can be used until a start-up operation is complete.
- Further methods are known from JP 2 906010 B2, DE 10 2016 011084 A1, JP H10 82582 A, US Pat. No. 6,138,474 A and US 2017/299262 A1.
- the object of the present invention is to remedy this deficiency and to improve the provision of gaseous nitrogen products, in particular for the applications mentioned.
- Air separation plants with double-column systems and so-called crude and possibly pure argon columns are typically used to obtain argon.
- An example is illustrated by Häring (see above) in Figure 2.3A and described from page 26 in the section "Rectification in the Low-pressure, Crude and Pure Argon Column” and from page 29 in the section "Cryogenic Production of Pure Argon".
- a pure argon column can also be dispensed with for argon recovery if the relevant rectification columns are adapted accordingly.
- Pure argon can, for example, be withdrawn from the crude argon column or a comparable rectification column further below than the fluid conventionally transferred to the pure argon column, with a section arranged above the withdrawal point being used for nitrogen separation.
- fluid is removed from the low-pressure column somewhat below the so-called argon maximum, at which approximately 10% argon is typically reached in the low-pressure column, as is known in principle.
- Further separating apparatus can be connected between the low-pressure column and a crude argon column, for example a column section in which the fluid drawn off from the low-pressure column is sent in the opposite direction to bottom liquid from the crude argon column.
- An argon sluice column is a rectification column for argon-oxygen separation, which is not used to obtain an argon product, but only to remove argon from the air to be separated in the high-pressure column and low-pressure column. Its circuit differs only slightly from that of a classic crude argon column, but it contains significantly fewer theoretical plates, namely less than 40, in particular between 15 and 30.
- An argon sluice column is fed with fluid from the low-pressure column, as is also used in conventional argon extraction .
- a fluid is removed from the low-pressure column that is enriched in argon both compared to the bottom liquid and compared to the top gas of the low-pressure column, and this fluid is fed to one or more separation apparatuses.
- the low-pressure column is provided with a side offtake which is connected to one or more further separating devices.
- Liquids and gases can be rich or poor in one or more components, where "rich” means a content of at least 50%, 75%, 90%, 95%, 99%, 99.5%, 99, 9% or 99.99% and “poor” can stand for a content of at most 50%, 25%, 10%, 5%, 1%, 0.1% or 0.01% on a mole, weight or volume basis .
- the term "predominantly” can in particular correspond to the definition of "rich”.
- Liquids and gases can also be enriched or depleted in one or more components, these terms referring to a content in a starting liquid or a starting gas from which the liquid or gas was obtained.
- the liquid or the gas is "enriched” in particular when this or this is at least 1.1 times 1.5 times, 2 times, 5 times, 10 times, 100 times or 1,000 times the content, and in particular "depleted” if this or this is at most 0.9 times, 0.5 times the content , 0.1 times, 0.01 times or 0.001 times the content of a corresponding component based on the starting liquid or the starting gas. If, for example, “oxygen” or “nitrogen” is mentioned here, this also includes a liquid or a gas that is rich in oxygen or nitrogen, but does not necessarily have to consist exclusively of them.
- the present invention proposes temporarily discharging at least part of the fluid taken from the low-pressure column and normally transferred to the argon production or the argon discharge from the air separation plant without subjecting it to further rectification.
- the fluid can, for example, be fed to a residual gas from the top of the low-pressure column.
- the present invention proposes an air separation plant for fier ein a gaseous nitrogen product by low-temperature separation of air, the air separation plant having a rectification column system with a floor pressure column, a low-pressure column and at least one other Has rectification column.
- the high-pressure column and the low-pressure column can be provided in particular in the form of a known double column.
- the air separation plant is set up to provide the gaseous nitrogen product using a top gas formed in the low-pressure column, and to heat this in a materially unchanged composition compared to a material composition on which it was formed in the low-pressure column and in particular to compress it externally.
- the air separation unit is configured to form an oxygen and argon rich and nitrogen lean fluid in the low pressure column and to exhaust at least a portion of the oxygen and argon rich and nitrogen lean fluid from the low pressure column.
- the air separation plant is also set up, in a first operating mode, to subject at least part of the oxygen- and argon-rich and nitrogen-poor fluid discharged from the low-pressure column to a low-temperature separation using the at least one further rectification column mentioned, and in a second operating mode at least discharge part of the fluid rich in oxygen and argon and poor in nitrogen, discharged from the low-pressure column, from the air separation unit without subjecting it to cryogenic separation and without subjecting it to further rectification.
- the fluid rich in oxygen and argon and low in nitrogen is discharged from the low-pressure column
- the measures proposed according to the invention can in particular shorten the start-up time up to the production of gaseous nitrogen, in particular with the specifications mentioned initially and below Removal of argon and stable operation of the low-pressure column can be achieved through a concentration profile similar to that in the design case.
- the at least one further rectification column is provided within the scope of the present invention in particular in an argon recovery unit with a crude argon column.
- the fluid rich in oxygen and argon and low in nitrogen is separated into an argon-enriched gas (so-called crude argon) and an argon-depleted liquid.
- the argon-enriched gas typically comprises about 1 ppm oxygen and 0.5% nitrogen.
- About a third of the argon-enriched gas is removed from the top of the crude argon column and transferred to the pure argon column, if present.
- the argon-depleted liquid is typically returned to the low pressure column.
- a pure argon column is used, if present in a corresponding configuration, mainly to the in the argon-enriched gas from the Distill residual nitrogen contained in the crude argon column.
- argon with a residual content of typically about 1 ppm nitrogen and 1 ppm oxygen can be drawn off from the bottom of the pure argon column and, optionally after further processing, discharged as a product from the plant.
- a rectification column corresponding to a crude argon column can be operated as mentioned at the outset.
- the crude argon column is provided with a top condenser which condenses part of the argon-enriched gas rising in the crude argon column and thus provides a liquid reflux.
- the top condenser of the crude argon column is cooled, for example, with expanded, oxygen-enriched fluid from the bottom of the high-pressure column. For this purpose, this is fed into an evaporation space of the top condenser, which is separate from the column interior of the crude argon column.
- the pure argon column can have a comparable design.
- the present invention is particularly useful in reducing the time to on-spec gaseous nitrogen product.
- the air separation plant provided according to the invention is set up to carry out the second operating mode after the air separation plant has been started up and before the first operating mode.
- the air separation plant can also be set up to carry out the second operating mode instead of the first operating mode in the event of a malfunction or a break in operation of the argon recovery unit.
- the air separation plant can be set up to carry out the second operating mode until at least one parameter which characterizes a low-temperature separation in the low-pressure column corresponds to a specification.
- This parameter, which characterizes the low-temperature separation in the low-pressure column can in particular be a purity of the gaseous nitrogen product.
- the start-up time can in particular 0.5 to 1 days can be reduced.
- the parameter indicates stable operation in the low-pressure column and after a correspondingly stable operating state has been reached, the argon rectification can slowly be put into operation.
- the argon recovery unit is not in operation in the second operating mode or is fed with a smaller amount of the oxygen- and argon-rich and nitrogen-poor fluid from the low-pressure column than in the first operating mode, and that at the beginning of the first mode of operation the argon recovery unit is started up or is in operation or is fed with a larger amount of the fluid rich in oxygen and argon and lean in nitrogen than in the second.
- the air separation plant can be used in particular to form the gaseous nitrogen product as pure (ultra) nitrogen with an argon content of less than 4 ppm,
- the measures according to the invention can also be advantageous in an air separation plant set up to provide a nitrogen product of lower purity.
- the air separation plant can be set up in particular to convert the fluid rich in oxygen and argon and low in nitrogen, which is taken from the low-pressure column and subjected to the low-temperature separation using the at least one further rectification column and discharged from the air separation plant in the second operating mode, into of the low pressure column containing 70 to 95 mole percent oxygen, 5 to 30 mole percent argon and less than 300 ppm nitrogen.
- this can have, for example, 86 to 92 mole percent oxygen and 8 to 14 mole percent argon, in another specific example about 88 mole percent oxygen and about 12 mole percent argon and about 250 ppm nitrogen.
- a bypass line can be provided, the air separation plant can include a control device, and the control device can be set up to carry out a volume measurement and to open and close the bypass line by controlling a valve arranged in the bypass line.
- control device can be set up to monitor one or more components of the air separation plant and to switch from the first to the second operating mode on the basis of a result of the monitoring.
- efficiency or performance of the separation in a crude argon column and/or the efficiency of an argon transfer pump that conveys the bottom liquid of the crude argon column can be monitored and reacted accordingly, with the advantages mentioned.
- the air separation plant can be set up in particular to discharge the fluid rich in oxygen and argon and low in nitrogen from the low-pressure column at different removal points in the first and the second operating mode. Such an embodiment is also included in the wording that "fluid is discharged from the low-pressure column".
- a process for the production of a gaseous nitrogen product by cryogenic separation of air in which an air separation plant is used which has a rectification column system with a high-pressure column, a low-pressure column and at least one further rectification column, is also the subject of the invention, wherein the gaseous nitrogen product is produced using a top gas formed in the low-pressure column is provided, in the low-pressure column a fluid rich in oxygen and argon and poor in nitrogen is formed and at least part of the fluid rich in oxygen and argon and poor in nitrogen is discharged from the low-pressure column, and in a first operating mode at least a part the oxygen- and argon-rich and nitrogen-poor fluid discharged from the low-pressure column to a low-temperature separation using the at least one further rectification column and a further rectification is subjected to ication.
- the method is characterized in that in a second operating mode at least part of the oxygen and argon rich and Nitrogen-poor fluid discharged from the low-pressure column is discharged from the air separation unit without being subjected to cryogenic separation.
- FIG. 1 shows an air separation plant according to an embodiment of the invention in a simplified, schematic representation.
- Air separation plants of the type shown are often described elsewhere, for example in Fl.-W. Häring (ed.), Industrial Gases Processing, Wiley-VCH,
- FIG. 1 an air separation plant according to one embodiment of the invention is illustrated in a simplified, schematic representation and denoted by 100.
- the air separation plant 100 has a rectification column system 10 with a high-pressure column 11 , a low-pressure column 12 , a crude argon column 13 , a pure argon column 14 and a further separation apparatus 15 .
- the high-pressure column 11 is connected in a known manner to the low-pressure column 12 via a main condenser 15 in a heat-exchanging manner.
- the further separator 15 has two separate separating sections 15a, 15b.
- atmospheric air is sucked in and compressed by means of a main air compressor 1 or one or more corresponding compressor stages via a filter that is not designated separately. Compression takes place to a pressure in a pressure range that is above a pressure range in which the high-pressure column 11 is operated.
- the correspondingly treated feed air is divided, also in a manner known per se, into partial flows which are cooled in the illustrated manner in a main heat exchanger 4, in booster or turbine arrangements 5, 6 compressed or expanded and fed into the high-pressure column 11 or discharged as so-called excess air.
- Liquid taken from the high-pressure column 11 is fed after cooling in a sub-cooling countercurrent 7 into the low-pressure column 12, which is also fed with bottom liquid from the high-pressure column 11, which was previously passed through top condensers of the crude and pure argon columns 13, 14, among other things.
- Bottom liquid A from the low-pressure column 12 is pressurized in liquid form by means of an internal compression pump 8 and, after evaporation or pseudo-evaporation, is made available as an internally compressed oxygen product.
- Top gas B drawn off from the top of the low-pressure column 12 is compressed externally in a compressor 9 after heating in the subcooling countercurrent flow 7 and in the main heat exchanger 4 .
- Impure nitrogen C is removed from the low-pressure column 12 via a side offtake, also heated in the subcooling countercurrent 7 and in the main heat exchanger 4 and used, for example, as regeneration gas in the pre-cleaning unit 2 .
- Fluid D rich in oxygen and argon and poor in nitrogen is taken from the low pressure column 12 .
- the fluid D is fed into the separating section 15a of the further separating apparatus 15 and sent there towards the crude argon column 13 with the bottom liquid E conveyed by a pump 16 .
- Liquid F from a lower region of the separation section 15a of the further separation apparatus 15, which is depleted in argon compared to the fluid D, is fed back into the low-pressure column 12.
- pure oxygen G is obtained from further bottom liquid of the crude argon column 13 using a bottom evaporator 17 fed with feed air.
- Top gas Fl of the separating section 15a of the further separating apparatus 15 is transferred to the crude argon column 13, which is coupled in a known manner to the pure argon column 14 and is operated in a corresponding manner, whereby pure argon I can be removed from the pure argon column 14.
- At least part of the fluid D rich in oxygen and argon and low in nitrogen can be fed to the impure nitrogen C via a bypass 20 without decomposition in the rectification columns 13 to 15.
- Other fluid connections are indicated at 21-23
- bypass 20 in the air separation plant 100 formed in the low-pressure column 11 and discharged from this fluid D, which is rich in oxygen and argon and low in nitrogen in a first operating mode at least partially a low-temperature separation using the raw and pure argon column 13, 14 and, in a second mode of operation, are at least partially discharged from the air separation plant 100 without subjecting it to cryogenic separation.
- Corresponding operating modes can be set in particular according to a control device 50, which open or close the bypass 20 or prevent or enable a feed into the separating section 15a.
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Abstract
The invention relates to an air separation system (100) for producing a gaseous nitrogen product by means of a low-temperature air separation, having a rectification column system (10) with a high-pressure column (11), a low-pressure column (12), and at least one additional rectification column (13, 14), wherein the air separation system (100) is designed to provide the gaseous nitrogen product using a head gas formed in the low-pressure column (12); the air separation system (100) is designed to form a fluid which is enriched with oxygen and argon and is depleted of nitrogen in the low-pressure column (11) and discharge at least one part of the fluid which is enriched with oxygen and argon and is depleted of nitrogen out of the low-pressure column (12); and the air separation system (100) is designed to subject at least one part of the fluid which is enriched with oxygen and argon and is depleted of nitrogen and which is discharged from the low-pressure column (12) to a low-temperature separation, thereby using the at least one additional rectification column (13, 14), in a first operating mode. According to the invention, the air separation system (100) is designed to discharge at least one part of the fluid which is enriched with oxygen and argon and is depleted of nitrogen and which is discharged from the low-pressure column (12) out of the air separation system (100) without subjecting said part to the low-temperature separation or to an additional rectification process in a second operating mode. The invention likewise relates to a corresponding method.
Description
Beschreibung description
Bereitsteiluna eines Stickstoffprodukts Provision of a nitrogen product
Die Erfindung betrifft eine Luftzerlegungsanlage und ein Luftzerlegungsverfahren zur Bereitstellung eines Stickstoffprodukts. The invention relates to an air separation plant and an air separation process for providing a nitrogen product.
Technischer Hintergrund Technical background
Die Herstellung von Luftprodukten in flüssigem oder gasförmigem Zustand durch Tieftemperaturzerlegung von Luft in Luftzerlegungsanlagen ist bekannt und beispielsweise bei H.-W. Häring (Hrsg.), Industrial Gases Processing, Wiley-VCH, 2006, insbesondere Abschnitt 2.2.5, "Cryogenic Rectification", beschrieben. The production of air products in a liquid or gaseous state by low-temperature separation of air in air separation plants is known and is described, for example, by H.-W. Häring (ed.), Industrial Gases Processing, Wiley-VCH, 2006, in particular Section 2.2.5, "Cryogenic Rectification".
Luftzerlegungsanlagen klassischer Art weisen Rektifikationskolonnensysteme auf, die beispielsweise als Zweikolonnensysteme, insbesondere als Doppelkolonnensysteme, aber auch als Drei- oder Mehrkolonnensysteme ausgebildet sein können. Neben Rektifikationskolonnen zur Gewinnung von Stickstoff und/oder Sauerstoff in flüssigem und/oder gasförmigem Zustand, also Rektifikationskolonnen zur Stickstoff-Sauerstoff- Trennung, können Rektifikationskolonnen zur Gewinnung weiterer Luftkomponenten, insbesondere von Edelgasen, vorgesehen sein. Air separation plants of the classic type have rectification column systems which can be designed, for example, as two-column systems, in particular as double-column systems, but also as three-column or multi-column systems. In addition to rectification columns for obtaining nitrogen and/or oxygen in the liquid and/or gaseous state, ie rectification columns for nitrogen-oxygen separation, rectification columns for obtaining further air components, in particular inert gases, can be provided.
Die Rektifikationskolonnen der genannten Rektifikationskolonnensysteme werden auf Drücken in unterschiedlichen Druckbereichen betrieben. Bekannte Doppelkolonnensysteme weisen eine sogenannte Hochdruckkolonne (auch als Druckkolonne, Mitteldruckkolonne oder untere Kolonne bezeichnet) und eine sogenannte Niederdruckkolonne (obere Kolonne) auf. Die Hochdruckkolonne wird typischerweise auf einem Druck in einem Druckbereich von 4 bis 7 bar, insbesondere ca. 5,3 bar, betrieben, die Niederdruckkolonne dagegen auf einem Druck in einem Druckbereich von typischerweise 1 bis 2 bar, insbesondere ca. 1 ,4 bar. In bestimmten Fällen können in beiden Rektifikationskolonnen auch höhere Drücke eingesetzt werden. Bei den hier und nachfolgend angegebenen Drücken in den jeweiligen Druckbereichen handelt es sich insbesondere um Absolutdrücke (bar (abs.), bara) am Kopf der jeweils angegebenen Kolonnen.
Eine in üblicher Weise ausgestaltete Luftzerlegungsanlage mit einem entsprechenden Doppelkolonnensystem ist typischerweise für zur Bereitstellung eines gasförmigen Stickstoffprodukts mit 100 ppb bis 1 ppm Sauerstoffgehalt und mehr als 10 ppm Argongehalt ausgebildet. Insbesondere im Bereich der Halbleiterfertigung wird jedoch zunehmend Druckstickstoff mit deutlich weniger als 4 ppm Argon benötigt. Zu diesem Zweck können unterschiedliche Maßnahmen ergriffen werden, beispielsweise die Erhöhung der Trennstufenzahl für die Rektifikation. The rectification columns of the rectification column systems mentioned are operated at pressures in different pressure ranges. Known double column systems have a so-called high-pressure column (also referred to as a pressure column, medium-pressure column or lower column) and a so-called low-pressure column (upper column). The high-pressure column is typically operated at a pressure in a pressure range of 4 to 7 bar, in particular approx. 5.3 bar, while the low-pressure column is operated at a pressure in a pressure range of typically 1 to 2 bar, in particular approx. 1.4 bar. In certain cases, higher pressures can also be used in both rectification columns. The pressures specified here and below in the respective pressure ranges are, in particular, absolute pressures (bar (abs.), bara) at the top of the columns specified in each case. A conventionally designed air separation plant with a corresponding double column system is typically designed to provide a gaseous nitrogen product with 100 ppb to 1 ppm oxygen content and more than 10 ppm argon content. In particular in the area of semiconductor production, however, compressed nitrogen with significantly less than 4 ppm argon is increasingly required. Various measures can be taken for this purpose, for example increasing the number of plates for the rectification.
Entsprechende Anlagen sind typischerweise mit einer Argonrektifikation ausgestattet, die klassischerweise eine Roh- und eine Reinargonkolonne umfasst. Weitere Ausgestaltungen sind unten erläutert. Corresponding plants are typically equipped with an argon rectification, which traditionally includes a raw and a pure argon column. Further refinements are explained below.
Beim Anfahren einer entsprechenden Anlage aus dem warmen oder kalten Zustand ist die Zeit, die bis zum Erreichen einer entsprechenden Reinheit des gasförmigen Stickstoffprodukts verstreicht, ausgesprochen hoch. Die Erreichung einer ausreichenden Reinheit des gasförmigen Stickstoffprodukts hängt, wie auch weiter unten erläutert, von der ausreichenden Entfernung von Argon aus der Niederdruckkolonne ab. Diese wiederum richtet sich nach der Zeit, die bis zur vollen Funktion der Argonrektifikation verstreicht. Letztere ist deutlich höher als die bis zur Erreichung der Funktion der Stickstoff-Sauerstoff-Trennung. Es können sich insgesamt Zeiten bis zur Erreichung einer spezifikationsgerechten Reinheit des gasförmigen Stickstoffprodukts von mehr als 3,5 Tagen ergeben. When starting up a corresponding plant from the warm or cold state, the time that elapses before the gaseous nitrogen product achieves a corresponding purity is extremely high. Achieving sufficient purity of the gaseous nitrogen product depends on sufficient removal of argon from the low pressure column, as also explained below. This in turn depends on the time that elapses until the argon rectification is fully functional. The latter is significantly higher than that required to achieve the nitrogen-oxygen separation function. Total times to achieve on-spec gaseous nitrogen product purity can be in excess of 3.5 days.
Aus der JP H05 1883 A ist ein Verfahren bekannt, bei dem eine Bypassleitung zwischen einer Entnahmeleitung aus einer Niederdruckkolonne, die in eine Rohargonkolonne mündet, und der Niederdruckkolonne verwendet wird. Die Bypassleitung kann verwendet werden, bis ein Anfahrbetrieb abgeschlossen ist. Weitere Verfahren sind aus der JP 2 906010 B2, der DE 10 2016 011084A1 , der JP H10 82582 A, der US 6 138474 A und der US 2017/299262 A1 bekannt. A method is known from JP H05 1883 A, in which a bypass line is used between an extraction line from a low-pressure column, which opens into a crude argon column, and the low-pressure column. The bypass line can be used until a start-up operation is complete. Further methods are known from JP 2 906010 B2, DE 10 2016 011084 A1, JP H10 82582 A, US Pat. No. 6,138,474 A and US 2017/299262 A1.
Die vorliegende Erfindung stellt sich die Aufgabe, diesen Mangel zu beheben und die Bereitstellung von gasförmigen Stickstoffprodukten, insbesondere für die genannten Anwendungen, zu verbessern. The object of the present invention is to remedy this deficiency and to improve the provision of gaseous nitrogen products, in particular for the applications mentioned.
Offenbarung der Erfindung
Vor diesem Hintergrund wird eine Luftzerlegungsanlage zur Bereitstellung eines Stickstoffprodukts mit den Merkmalen des Anspruchs 1 vorgeschlagen. Ein Verfahren mit den Merkmalen des Anspruchs 12 ist ebenfalls Gegenstand der Erfindung. Ausgestaltungen der Erfindung sind Gegenstand der Unteransprüche und der nachfolgenden Beschreibung. Disclosure of Invention Against this background, an air separation plant for providing a nitrogen product with the features of claim 1 is proposed. A method with the features of claim 12 is also the subject of the invention. Refinements of the invention are the subject matter of the dependent claims and the following description.
Nachfolgend werden zunächst einige bei der Beschreibung der vorliegenden Erfindung und ihrer Vorteile verwendete Begriffe sowie der zugrunde liegende technische Hintergrund näher erläutert. Some of the terms used in the description of the present invention and its advantages, as well as the underlying technical background, are explained in more detail below.
Die in einer Luftzerlegungsanlage eingesetzten Vorrichtungen sind in der zitierten Fachliteratur, beispielsweise bei Häring (s.o.) in Abschnitt 2.2.5.6, "Apparatus", beschrieben. Sofern die nachfolgenden Definitionen nicht hiervon abweichen, wird daher zum Sprachgebrauch, der im Rahmen der vorliegenden Anmeldung verwendet wird, ausdrücklich auf die zitierte Fachliteratur verwiesen. The devices used in an air separation plant are described in the specialist literature cited, for example in Häring (see above) in Section 2.2.5.6, "Apparatus". Unless the following definitions deviate from this, reference is therefore expressly made to the technical literature cited for the language used in the context of the present application.
Zur Argongewinnung werden typischerweise Luftzerlegungsanlagen mit Doppelkolonnensystemen und sogenannten Roh- und ggf. Reinargonkolonnen eingesetzt. Ein Beispiel ist bei Häring (s.o.) in Figur 2.3A veranschaulicht und ab Seite 26 im Abschnitt "Rectification in the Low-pressure, Crude and Pure Argon Column" sowie ab Seite 29 im Abschnitt "Cryogenic Production of Pure Argon" beschrieben. Grundsätzlich kann zur Argongewinnung auch auf eine Reinargonkolonne verzichtet werden, wenn die betreffenden Rektifikationskolonnen entsprechend angepasst werden. Reinargon kann beispielsweise aus der Rohargonkolonne bzw. einer vergleichbaren Rektifikationskolonne weiter unterhalb als das herkömmlicherweise in die Reinargonkolonne überführte Fluid abgezogen werden, wobei ein oberhalb der Entnahmestelle angeordneter Abschnitt zur Stickstoffabtrennung dient. Air separation plants with double-column systems and so-called crude and possibly pure argon columns are typically used to obtain argon. An example is illustrated by Häring (see above) in Figure 2.3A and described from page 26 in the section "Rectification in the Low-pressure, Crude and Pure Argon Column" and from page 29 in the section "Cryogenic Production of Pure Argon". In principle, a pure argon column can also be dispensed with for argon recovery if the relevant rectification columns are adapted accordingly. Pure argon can, for example, be withdrawn from the crude argon column or a comparable rectification column further below than the fluid conventionally transferred to the pure argon column, with a section arranged above the withdrawal point being used for nitrogen separation.
Zur Argongewinnung wird der Niederdruckkolonne Fluid etwas unterhalb des sogenannten Argonmaximums, an dem in der Niederdruckkolonne typischerweise etwa 10% Argon erreicht werden, entnommen, wie grundsätzlich bekannt. Auf die Erläuterungen zu Figur 2.4 in Häring (s.o.) wird verwiesen.
Zwischen die Niederdruckkolonne und eine Rohargonkolonne können weitere Trennapparate geschaltet werden, beispielsweise ein Kolonnenabschnitt, in dem das aus der Niederdruckkolonne abgezogene Fluid Sumpfflüssigkeit aus der Rohargonkolonne entgegengeschickt wird. To obtain argon, fluid is removed from the low-pressure column somewhat below the so-called argon maximum, at which approximately 10% argon is typically reached in the low-pressure column, as is known in principle. Reference is made to the explanations for Figure 2.4 in Häring (see above). Further separating apparatus can be connected between the low-pressure column and a crude argon column, for example a column section in which the fluid drawn off from the low-pressure column is sent in the opposite direction to bottom liquid from the crude argon column.
Statt einer Gewinnung von Argon kann in bekannten Anlagen auch lediglich eine Argonausschleusung unter Verwendung einer Argonauschleuskolonne erfolgen. Bei einer Argonauschleuskolonne handelt es sich um eine Rektifikationskolonne zur Argon- Sauerstoff-Trennung, die nicht zur Gewinnung eines Argonprodukts, sondern lediglich zur Ausschleusung von Argon der in Hochdrucksäule und Niederdrucksäule zu zerlegenden Luft dient. Ihre Schaltung unterscheidet sich nur wenig von der einer klassischen Rohargonsäule, allerdings enthält sie deutlich weniger theoretische Böden, nämlich weniger als 40, insbesondere zwischen 15 und 30. Eine Argonauschleuskolonne wird mit Fluid aus der Niederdruckkolonne gespeist, wie es auch in einer herkömmlichen Argongewinnung eingesetzt wird. Instead of obtaining argon, in known plants it is also possible to simply remove argon using an argon removal column. An argon sluice column is a rectification column for argon-oxygen separation, which is not used to obtain an argon product, but only to remove argon from the air to be separated in the high-pressure column and low-pressure column. Its circuit differs only slightly from that of a classic crude argon column, but it contains significantly fewer theoretical plates, namely less than 40, in particular between 15 and 30. An argon sluice column is fed with fluid from the low-pressure column, as is also used in conventional argon extraction .
In den beiden Fällen, der Argongewinnung und der reinen Argonausschleusung, wird also der Niederdruckkolonne ein Fluid entnommen, das sowohl gegenüber der Sumpfflüssigkeit als auch gegenüber dem Kopfgas der Niederdruckkolonne an Argon angereichert ist, und dieses Fluid wird einem oder mehreren Trennapparaten zugeführt. Entsprechend ist die Niederdruckkolonne mit einem Seitenabzug versehen, der mit einem oder mehreren weiteren Trennapparaten verbunden ist. In both cases, argon production and pure argon discharge, a fluid is removed from the low-pressure column that is enriched in argon both compared to the bottom liquid and compared to the top gas of the low-pressure column, and this fluid is fed to one or more separation apparatuses. Correspondingly, the low-pressure column is provided with a side offtake which is connected to one or more further separating devices.
Flüssigkeiten und Gase können im hier verwendeten Sprachgebrauch reich oder arm an einer oder an mehreren Komponenten sein, wobei "reich" für einen Gehalt von wenigstens 50%, 75%, 90%, 95%, 99%, 99,5%, 99,9% oder 99,99% und "arm" für einen Gehalt von höchstens 50%, 25%, 10%, 5%, 1%, 0,1% oder 0,01% auf Mol-, Gewichts- oder Volumenbasis stehen kann. Der Begriff "überwiegend" kann insbesondere der Definition von "reich" entsprechen. Liquids and gases, as used herein, can be rich or poor in one or more components, where "rich" means a content of at least 50%, 75%, 90%, 95%, 99%, 99.5%, 99, 9% or 99.99% and "poor" can stand for a content of at most 50%, 25%, 10%, 5%, 1%, 0.1% or 0.01% on a mole, weight or volume basis . The term "predominantly" can in particular correspond to the definition of "rich".
Flüssigkeiten und Gase können ferner angereichert oder abgereichert an einer oder mehreren Komponenten sein, wobei sich diese Begriffe auf einen Gehalt in einer Ausgangsflüssigkeit oder einem Ausgangsgas beziehen, aus der oder dem die Flüssigkeit oder das Gas gewonnen wurde. Die Flüssigkeit oder das Gas ist insbesondere dann "angereichert", wenn diese oder dieses zumindest den 1 ,1 -fachen,
1 ,5-fachen, 2-fachen, 5-fachen, 10-fachen 100-fachen oder 1.000-fachen Gehalt, und insbesondere dann "abgereichert", wenn diese oder dieses höchstens den 0,9-fachen, 0, 5-fachen, 0,1 -fachen, 0,01 -fachen oder 0,001 -fachen Gehalt einer entsprechenden Komponente, bezogen auf die Ausgangsflüssigkeit oder das Ausgangsgas, enthält. Ist hier beispielsweise von "Sauerstoff" oder "Stickstoff" die Rede, sei hierunter auch eine Flüssigkeit oder ein Gas verstanden, der reich an Sauerstoff oder Stickstoff ist, jedoch nicht notwendigerweise ausschließlich hieraus bestehen muss. Liquids and gases can also be enriched or depleted in one or more components, these terms referring to a content in a starting liquid or a starting gas from which the liquid or gas was obtained. The liquid or the gas is "enriched" in particular when this or this is at least 1.1 times 1.5 times, 2 times, 5 times, 10 times, 100 times or 1,000 times the content, and in particular "depleted" if this or this is at most 0.9 times, 0.5 times the content , 0.1 times, 0.01 times or 0.001 times the content of a corresponding component based on the starting liquid or the starting gas. If, for example, "oxygen" or "nitrogen" is mentioned here, this also includes a liquid or a gas that is rich in oxygen or nitrogen, but does not necessarily have to consist exclusively of them.
Merkmale und Vorteile der Erfindung Features and advantages of the invention
Wird aus der Niederdruckkolonne eines Doppelkolonnensystems kein an Argon angereichertes Fluid entnommen, verschiebt sich die Trennung zwischen Sauerstoff und Argon nach oben. Entsprechendes ist der Fall, wenn beispielsweise eine Argongewinnung nach dem Flochfahren einer entsprechenden Anlage noch nicht voll im Betrieb ist. An der Entnahmestelle für gasförmigen Stickstoff aus der Niederdruckkolonne liegt daher in solchen Fällen (noch) keine ausreichende Reinheit vor. Erst wenn auch Argongewinnung vollständig in Betrieb ist, verschiebt sich die Trennung von Sauerstoff und Argon in der Niederdruckkolonne nach unten, so dass die spezifikationsgerechte Gewinnung von gasförmigem Stickstoff, insbesondere in der eingangs erwähnten Reinheit, möglich ist. Wie erwähnt, wird hierdurch die Zeit, bis gasförmiger Stickstoff in der gewünschten Reinheit zur Verfügung gestellt werden kann, deutlich verlängert. Entsprechendes gilt auch, wenn anstelle einer Argongewinnung eine Argonausschleusung in der erläuterten Weise erfolgt. If no argon-enriched fluid is taken from the low-pressure column of a double-column system, the separation between oxygen and argon shifts upwards. The same is the case if, for example, argon production is not yet fully operational after a corresponding plant has been shut down. In such cases, there is not (yet) sufficient purity at the removal point for gaseous nitrogen from the low-pressure column. Only when argon production is also fully operational does the separation of oxygen and argon in the low-pressure column shift downwards, so that gaseous nitrogen can be produced on specification, particularly in the purity mentioned at the outset. As mentioned, the time before gaseous nitrogen can be made available in the desired purity is significantly lengthened as a result. The same also applies if, instead of argon extraction, argon is discharged in the manner explained.
Die vorliegende Erfindung schlägt vor diesem Flintergrund eine zeitweise Ausleitung zumindest eines Teils des aus der Niederdruckkolonne entnommenen und normalerweise in die Argongewinnung oder die Argonausschleusung überführten Fluids aus der Luftzerlegungsanlage vor, ohne dass dieses einer weiteren Rektifikation unterworfen wird. Das Fluid kann dabei beispielsweise einem Restgas vom Kopf der Niederdruckkolonne zugespeist werden. Against this background, the present invention proposes temporarily discharging at least part of the fluid taken from the low-pressure column and normally transferred to the argon production or the argon discharge from the air separation plant without subjecting it to further rectification. The fluid can, for example, be fed to a residual gas from the top of the low-pressure column.
Insgesamt schlägt die vorliegende Erfindung eine Luftzerlegungsanlage zur Fierstellung eines gasförmigen Stickstoffprodukts durch Tieftemperaturzerlegung von Luft vor, wobei die Luftzerlegungsanlage ein Rektifikationskolonnensystem mit einer Flochdruckkolonne, einer Niederdruckkolonne und zumindest einer weiteren
Rektifikationskolonne aufweist. Die Hochdruckkolonne und die Niederdruckkolonne können insbesondere in Form einer bekannten Doppelkolonne bereitgestellt sein. Overall, the present invention proposes an air separation plant for fierstellung a gaseous nitrogen product by low-temperature separation of air, the air separation plant having a rectification column system with a floor pressure column, a low-pressure column and at least one other Has rectification column. The high-pressure column and the low-pressure column can be provided in particular in the form of a known double column.
Die Luftzerlegungsanlage ist dafür eingerichtet, das gasförmige Stickstoffprodukt unter Verwendung eines in der Niederdruckkolonne gebildeten Kopfgases bereitzustellen, und dieses insbesondere in stofflich unveränderter Zusammensetzung gegenüber einer stofflichen Zusammensetzung, auf der es in der Niederdruckkolonne gebildet wird, zu erwärmen und insbesondere extern zu verdichten. The air separation plant is set up to provide the gaseous nitrogen product using a top gas formed in the low-pressure column, and to heat this in a materially unchanged composition compared to a material composition on which it was formed in the low-pressure column and in particular to compress it externally.
Die Luftzerlegungsanlage ist dafür eingerichtet, in der Niederdruckkolonne ein an Sauerstoff und Argon reiches und an Stickstoff armes Fluid zu bilden und zumindest einen Teil des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids aus der Niederdruckkolonne auszuleiten. Die Luftzerlegungsanlage ist ferner dafür eingerichtet, in einem ersten Betriebsmodus zumindest einen Teil des an Sauerstoff und Argon reichen und an Stickstoff armen, aus der Niederdruckkolonne ausgeleiteten Fluids einer Tieftemperaturtrennung unter Verwendung der erwähnten, zumindest einen weiteren Rektifikationskolonne zu unterwerfen, und in einem zweiten Betriebsmodus zumindest einen Teil des an Sauerstoff und Argon reichen und an Stickstoff armen, aus der Niederdruckkolonne ausgeleiteten Fluids aus der Luftzerlegungsanlage auszuleiten, ohne dieses der Tieftemperaturtrennung zu unterwerfen und ohne dieses einer weiteren Rektifikation zu unterwerfen. The air separation unit is configured to form an oxygen and argon rich and nitrogen lean fluid in the low pressure column and to exhaust at least a portion of the oxygen and argon rich and nitrogen lean fluid from the low pressure column. The air separation plant is also set up, in a first operating mode, to subject at least part of the oxygen- and argon-rich and nitrogen-poor fluid discharged from the low-pressure column to a low-temperature separation using the at least one further rectification column mentioned, and in a second operating mode at least discharge part of the fluid rich in oxygen and argon and poor in nitrogen, discharged from the low-pressure column, from the air separation unit without subjecting it to cryogenic separation and without subjecting it to further rectification.
Ist hier davon die Rede, dass das an Sauerstoff und Argon reiche und an Stickstoff armen Fluid "aus der Niederdruckkolonne ausgeleitet wird", soll dies explizit nicht auf eine einzige Entnahmestelle beschränkt sein. Es können auch mehrere Entnahmestellen vorgesehen sein, die auch durch Trennböden voneinander getrennt sein können. Die Entnahme - immer jedoch als an Sauerstoff und Argon reiches und an Stickstoff armes Fluid, insbesondere mit den weiter unten angegeben konkreten Gehalten - kann auch in dem ersten und zweiten Betriebsmodus an unterschiedlichen Stellen aus der Niederdruckkolonne ausgeleitet werden. If it is mentioned here that the fluid rich in oxygen and argon and low in nitrogen is "discharged from the low-pressure column", this should explicitly not be limited to a single extraction point. Several removal points can also be provided, which can also be separated from one another by separating floors. The withdrawal-always as a fluid rich in oxygen and argon and low in nitrogen, in particular with the concrete contents specified below-can also be discharged from the low-pressure column at different points in the first and second operating mode.
Durch die erfindungsgemäß vorgeschlagenen Maßnahmen kann insbesondere eine Verkürzung der Anfahrzeit bis zur Herstellung von gasförmigem Stickstoff, insbesondere mit den eingangs und nachfolgend erwähnten Spezifikationen, durch
Entfernung von Argon und ein stabiler Betrieb der Niederdruckkolonne durch ein ähnliches Konzentrationsprofil wie im Auslegungsfall erreicht werden. The measures proposed according to the invention can in particular shorten the start-up time up to the production of gaseous nitrogen, in particular with the specifications mentioned initially and below Removal of argon and stable operation of the low-pressure column can be achieved through a concentration profile similar to that in the design case.
Es ergibt sich ferner eine Verbesserung des Anlagenbetriebs, beispielsweise bei Ausfall des Argonsystems, insbesondere einer Transferpumpe, die eine Sumpfflüssigkeit der Rohargonkolonne zurück in die Niederdruckkolonne oder eine andere Trenneinheit fördert, da durch den Einsatz der Erfindung das Konzentrationsprofil in der Niederdruckkolonne stabil gehalten werden kann. Eine entsprechende Argonentfernung ist in den letzteren Fällen auch bei Unterschreitung der Rohargonleistung für Anlagen, die zur Bereitstellung von Stickstoff normaler Reinheitsgrade eingerichtet sind, vorteilhaft. There is also an improvement in plant operation, for example if the argon system fails, in particular a transfer pump that pumps a bottom liquid from the crude argon column back into the low-pressure column or another separation unit, since the use of the invention allows the concentration profile in the low-pressure column to be kept stable. A corresponding removal of argon is advantageous in the latter cases, even if the crude argon output for plants that are set up to provide nitrogen of normal degrees of purity is not reached.
In einem Fall, in dem kein Argon bereitgestellt werden soll bzw. ein Argonsystem nicht in Betrieb ist, ergibt sich eine Verbesserung der Effizienz um mehrere Prozent. Im Rahmen der vorliegenden Erfindung reduziert sich die Gefahr eines Stickstoffdurchbruchs zur Rohargonsäule, falls vorhanden. In a case where no argon is to be provided or an argon system is not in operation, there is an improvement in efficiency of several percent. Within the scope of the present invention, the risk of nitrogen breakthrough to the crude argon column, if any, is reduced.
Bei Anlagen zur Bereitstellung von hochreinem Stickstoff ist der sich durch die Erfindung ergebende Verlust von Sauerstoff vernachlässigbar, da in diesen Anlagen in der Regel Niederdrucksauerstoff entlüftet wird. In plants for the provision of high-purity nitrogen, the loss of oxygen resulting from the invention is negligible, since low-pressure oxygen is generally vented in these plants.
Wie mehrfach erwähnt, ist die zumindest eine weitere Rektifikationskolonne im Rahmen der vorliegenden Erfindung insbesondere in einer Argongewinnungseinheit mit einer Rohargonkolonne bereitgestellt. As mentioned several times, the at least one further rectification column is provided within the scope of the present invention in particular in an argon recovery unit with a crude argon column.
In der Rohargonkolonne erfolgt eine Trennung des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids in ein an Argon angereichertes Gas (sogenanntes Rohargon) und eine an Argon abgereicherte Flüssigkeit. Das an Argon angereicherte Gas umfasst typischerweise etwa 1 ppm Sauerstoff und 0,5% Stickstoff. Etwa ein Drittel des an Argon angereicherten Gases wird der Rohargonkolonne am Kopf entnommen und in die Reinargonkolonne, falls vorhanden, überführt. Die an Argon abgereicherte Flüssigkeit wird typischerweise in die Niederdruckkolonne zurückgeleitet. In the crude argon column, the fluid rich in oxygen and argon and low in nitrogen is separated into an argon-enriched gas (so-called crude argon) and an argon-depleted liquid. The argon-enriched gas typically comprises about 1 ppm oxygen and 0.5% nitrogen. About a third of the argon-enriched gas is removed from the top of the crude argon column and transferred to the pure argon column, if present. The argon-depleted liquid is typically returned to the low pressure column.
Eine Reinargonkolonne dient, falls in einer entsprechenden Ausgestaltung vorhanden, hauptsächlich dazu, den in dem an Argon angereicherten Gas aus der
Rohargonkolonne enthaltenen Reststickstoff abzudestillieren. Aus dem Sumpf der Reinargonkolonne kann auf diese Weise Argon mit einem Restgehalt von typischerweise etwa 1 ppm Stickstoff und 1 ppm Sauerstoff abgezogen und, ggf. nach weiterer Aufbereitung, als Produkt aus der Anlage ausgeleitet werden. Falls eine Reinargonkolonne nicht vorhanden ist, aber dennoch Reinargon gewonnen werden soll, kann eine an sich einer Rohargonkolonne entsprechende Rektifikationskolonne wie eingangs erwähnt betrieben werden. A pure argon column is used, if present in a corresponding configuration, mainly to the in the argon-enriched gas from the Distill residual nitrogen contained in the crude argon column. In this way, argon with a residual content of typically about 1 ppm nitrogen and 1 ppm oxygen can be drawn off from the bottom of the pure argon column and, optionally after further processing, discharged as a product from the plant. If there is no pure argon column, but pure argon is still to be obtained, a rectification column corresponding to a crude argon column can be operated as mentioned at the outset.
Die Rohargonkolonne ist mit einem Kopfkondensator versehen, der einen Teil des in der Rohargonkolonne aufsteigenden an Argon angereicherten Gases kondensiert und damit einen flüssigen Rücklauf bereitstellt. Bei bekannten Luftzerlegungsanlagen wird der Kopfkondensator der Rohargonkolonne beispielsweise mit entspanntem, sauerstoffangereichertem Fluid aus dem Sumpf der Hochdruckkolonne gekühlt. Hierzu wird dieses in einen Verdampfungsraum des Kopfkondensators eingespeist, der vom Säuleninnenraum der Rohargonkolonne getrennt ist. Die Reinargonkolonne kann grundsätzlich vergleichbar ausgebildet sein. The crude argon column is provided with a top condenser which condenses part of the argon-enriched gas rising in the crude argon column and thus provides a liquid reflux. In known air separation plants, the top condenser of the crude argon column is cooled, for example, with expanded, oxygen-enriched fluid from the bottom of the high-pressure column. For this purpose, this is fed into an evaporation space of the top condenser, which is separate from the column interior of the crude argon column. In principle, the pure argon column can have a comparable design.
Wie erwähnt, eignet sich die vorliegende Erfindung insbesondere dazu, die Zeit bis zur Bereitstellung eines spezifikationsgerechten gasförmigen Stickstoffprodukts zu verkürzen. In diesem Fall ist die erfindungsgemäß bereitgestellte Luftzerlegungsanlage gemäß einer entsprechenden Ausführungsform der Erfindung dafür eingerichtet, den zweiten Betriebsmodus nach einem Anfahren der Luftzerlegungsanlage und vor dem ersten Betriebsmodus durchzuführen. As noted, the present invention is particularly useful in reducing the time to on-spec gaseous nitrogen product. In this case, according to a corresponding embodiment of the invention, the air separation plant provided according to the invention is set up to carry out the second operating mode after the air separation plant has been started up and before the first operating mode.
In einer weiteren Ausgestaltung kann die Luftzerlegungsanlage jedoch auch dafür eingerichtet sein, den zweiten Betriebsmodus bei einer Betriebsstörung oder Betriebspause der Argongewinnungseinheit statt des ersten Betriebsmodus durchzuführen. Auf die obigen Erläuterungen wird verwiesen. In a further embodiment, however, the air separation plant can also be set up to carry out the second operating mode instead of the first operating mode in the event of a malfunction or a break in operation of the argon recovery unit. Reference is made to the above explanations.
In sämtlichen Ausgestaltungen kann die Luftzerlegungsanlage dafür eingerichtet sein, den zweiten Betriebsmodus so lange durchzuführen, bis wenigstens eine Kenngröße, die eine Tieftemperaturtrennung in der Niederdruckkolonne kennzeichnet, einer Vorgabe entspricht. Bei dieser Kenngröße, die die Tieftemperaturtrennung in der Niederdruckkolonne kennzeichnet, kann es sich insbesondere um eine Reinheit des gasförmigen Stickstoffprodukts handeln. Die Anfahrzeit kann dabei insbesondere um
0,5 bis 1 Tage reduziert werden. Die Kenngröße lässt auf einen stabilen Betrieb in der Niederdruckkolonne schließen und nach Erreichen eines entsprechenden stabilen Betriebszustands kann die Argonrektifikation langsam in Betrieb gesetzt werden. In all of the configurations, the air separation plant can be set up to carry out the second operating mode until at least one parameter which characterizes a low-temperature separation in the low-pressure column corresponds to a specification. This parameter, which characterizes the low-temperature separation in the low-pressure column, can in particular be a purity of the gaseous nitrogen product. The start-up time can in particular 0.5 to 1 days can be reduced. The parameter indicates stable operation in the low-pressure column and after a correspondingly stable operating state has been reached, the argon rectification can slowly be put into operation.
Mit anderen Worten kann in einer Ausgestaltung der Erfindung vorgesehen sein, dass die Argongewinnungseinheit in dem zweiten Betriebsmodus nicht in Betrieb ist oder mit einer geringeren Menge des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids aus der Niederdruckkolonne gespeist wird als in dem ersten Betriebsmodus, und dass zu Beginn des ersten Betriebsmodus die Argongewinnungseinheit in Betrieb gesetzt wird oder in Betrieb ist bzw. mit einer größeren Menge des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids gespeist wird als in dem zweiten. In other words, in one embodiment of the invention it can be provided that the argon recovery unit is not in operation in the second operating mode or is fed with a smaller amount of the oxygen- and argon-rich and nitrogen-poor fluid from the low-pressure column than in the first operating mode, and that at the beginning of the first mode of operation the argon recovery unit is started up or is in operation or is fed with a larger amount of the fluid rich in oxygen and argon and lean in nitrogen than in the second.
Die Luftzerlegungsanlage kann insbesondere zur Bildung des gasförmigen Stickstoffprodukts als Rein(st)stickstoff mit einem Argongehalt von weniger als 4 ppm,The air separation plant can be used in particular to form the gaseous nitrogen product as pure (ultra) nitrogen with an argon content of less than 4 ppm,
3 ppm, 2 ppm oder 1 ppm und mit einem Sauerstoffgehalt von 0.2 ppb oder weniger und bis zu 1 ppm eingerichtet sein. Wie erwähnt, ergibt sich insbesondere in diesem Fall der besondere Vorteil der Verringerung der Anfahrzeit. In einer anderen Alternative, wie ebenfalls erwähnt, können die erfindungsgemäßen Maßnahmen aber auch bei einer zur Bereitstellung eines Stickstoffprodukts geringerer Reinheit eingerichteten Luftzerlegungsanlage vorteilhaft sein. 3 ppm, 2 ppm or 1 ppm and with an oxygen content of 0.2 ppb or less and up to 1 ppm. As mentioned, in this case in particular there is the particular advantage of reducing the start-up time. In another alternative, as also mentioned, the measures according to the invention can also be advantageous in an air separation plant set up to provide a nitrogen product of lower purity.
In sämtlichen Fällen kann die Luftzerlegungsanlage insbesondere dafür eingerichtet sein, das an Sauerstoff und Argon reiche und an Stickstoff arme Fluid, das der Niederdruckkolonne entnommen und der Tieftemperaturtrennung unter Verwendung der zumindest einen weiteren Rektifikationskolonne unterworfen und in dem zweiten Betriebsmodus aus der Luftzerlegungsanlage ausgeleitet wird, in der Niederdruckkolonne mit einem Gehalt von 70 bis 95 Molprozent Sauerstoff, 5 bis 30 Molprozent Argon und weniger als 300 ppm Stickstoff zu bilden. In einem Beispiel kann dieses beispielsweise 86 bis 92 Molprozent Sauerstoff und 8 bis 14 Molprozent Argon aufweisen, in einem weiteren konkreten Beispiel ca. 88 Molprozent Sauerstoff und ca. 12 Molprozent Argon sowie ca. 250 ppm Stickstoff. In all cases, the air separation plant can be set up in particular to convert the fluid rich in oxygen and argon and low in nitrogen, which is taken from the low-pressure column and subjected to the low-temperature separation using the at least one further rectification column and discharged from the air separation plant in the second operating mode, into of the low pressure column containing 70 to 95 mole percent oxygen, 5 to 30 mole percent argon and less than 300 ppm nitrogen. In one example, this can have, for example, 86 to 92 mole percent oxygen and 8 to 14 mole percent argon, in another specific example about 88 mole percent oxygen and about 12 mole percent argon and about 250 ppm nitrogen.
In einer Luftzerlegungsanlage gemäß einer Ausgestaltung der Erfindung kann für die Ausleitung zumindest eines Teils des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids aus der Luftzerlegungsanlage in dem zweiten Betriebsmodus
eine Bypassleitung bereitgestellt sein, die Luftzerlegungsanlage kann eine Steuereinrichtung umfassen, und die Steuereinrichtung kann zur Durchführung einer Mengenmessung und zum Öffnen und Schließen der Bypassleitung durch Ansteuern eines in der Bypassleitung angeordneten Ventils eingerichtet sein. In an air separation plant according to one embodiment of the invention, at least part of the fluid rich in oxygen and argon and low in nitrogen can be used for discharging from the air separation plant in the second operating mode a bypass line can be provided, the air separation plant can include a control device, and the control device can be set up to carry out a volume measurement and to open and close the bypass line by controlling a valve arranged in the bypass line.
Die Steuereinrichtung kann insbesondere dazu eingerichtet sein, eine oder mehrere Komponenten der Luftzerlegungsanlage zu überwachen und auf Grundlage eines Ergebnisses der Überwachung von dem ersten in den zweiten Betriebsmodus umzuschalten. Hierbei kann insbesondere eine Leistungsfähigkeit bzw. Performance der Trennung in einer Rohargonkolonne und/oder eine Leistungsfähigkeit einer Argontransferpumpe, die Sumpfflüssigkeit der Rohargonkolonne fördert, überwacht und entsprechend, mit den genannten Vorteilen, reagiert werden. In particular, the control device can be set up to monitor one or more components of the air separation plant and to switch from the first to the second operating mode on the basis of a result of the monitoring. In particular, the efficiency or performance of the separation in a crude argon column and/or the efficiency of an argon transfer pump that conveys the bottom liquid of the crude argon column can be monitored and reacted accordingly, with the advantages mentioned.
Die Luftzerlegungsanlage kann insbesondere dafür eingerichtet sein, das an Sauerstoff und Argon reiche und an Stickstoff arme Fluid in dem ersten und dem zweiten Betriebsmodus an unterschiedlichen Entnahmestellen aus der Niederdruckkolonne auszuleiten. Auch eine derartige Ausgestaltung ist von der Formulierung umfasst, dass jeweils "Fluid aus der Niederdruckkolonne ausgeleitet" wird. The air separation plant can be set up in particular to discharge the fluid rich in oxygen and argon and low in nitrogen from the low-pressure column at different removal points in the first and the second operating mode. Such an embodiment is also included in the wording that "fluid is discharged from the low-pressure column".
Ein Verfahren zur Herstellung eines gasförmigen Stickstoffprodukts durch Tieftemperaturzerlegung von Luft, bei dem eine Luftzerlegungsanlage verwendet wird, die ein Rektifikationskolonnensystem mit einer Hochdruckkolonne, einer Niederdruckkolonne und zumindest einer weiteren Rektifikationskolonne aufweist, ist ebenfalls Gegenstand der Erfindung, wobei das gasförmige Stickstoffprodukt unter Verwendung eines in der Niederdruckkolonne gebildeten Kopfgases bereitgestellt wird, in der Niederdruckkolonne ein an Sauerstoff und Argon reiches und an Stickstoff armes Fluid gebildet und zumindest einen Teil des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids aus der Niederdruckkolonne ausgeleitet wird, und in einem ersten Betriebsmodus zumindest ein Teil des an Sauerstoff und Argon reichen und an Stickstoff armen, aus der Niederdruckkolonne ausgeleiteten Fluids einer Tieftemperaturtrennung unter Verwendung der zumindest einen weiteren Rektifikationskolonne und einer weiteren Rektifikation unterworfen wird. A process for the production of a gaseous nitrogen product by cryogenic separation of air, in which an air separation plant is used which has a rectification column system with a high-pressure column, a low-pressure column and at least one further rectification column, is also the subject of the invention, wherein the gaseous nitrogen product is produced using a top gas formed in the low-pressure column is provided, in the low-pressure column a fluid rich in oxygen and argon and poor in nitrogen is formed and at least part of the fluid rich in oxygen and argon and poor in nitrogen is discharged from the low-pressure column, and in a first operating mode at least a part the oxygen- and argon-rich and nitrogen-poor fluid discharged from the low-pressure column to a low-temperature separation using the at least one further rectification column and a further rectification is subjected to ication.
Das Verfahren zeichnet sich erfindungsgemäß dadurch aus, dass in einem zweiten Betriebsmodus zumindest ein Teil des an Sauerstoff und Argon reichen und an
Stickstoff armen, aus der Niederdruckkolonne ausgeleiteten Fluids aus der Luftzerlegungsanlage ausgeleitet wird, ohne dass dieses der Tieftemperaturtrennung unterworfen wird. According to the invention, the method is characterized in that in a second operating mode at least part of the oxygen and argon rich and Nitrogen-poor fluid discharged from the low-pressure column is discharged from the air separation unit without being subjected to cryogenic separation.
In dem Verfahren wird insbesondere eine Luftzerlegungsanlage verwendet, wie sie vorstehend in unterschiedlichen Ausgestaltungen erläutert wurde. Verfahrensschritte des erfindungsgemäßen Verfahrens ergeben sich dabei durch die entsprechen Ausgestaltungen, wobei stets dann, wenn zuvor davon die Rede ist, dass eine Luftzerlegungsanlage für einen bestimmten Betrieb "eingerichtet" ist, ein entsprechender Verfahrensschritt realisiert wird. In the method, in particular, an air separation plant is used, as has been explained above in different configurations. Method steps of the method according to the invention result from the corresponding configurations, with a corresponding method step always being implemented when it is previously said that an air separation plant is “set up” for a specific operation.
Die Erfindung wird nachfolgend unter Bezugnahme auf die beigefügten Zeichnungen näher erläutert, die die bevorzugten Ausgestaltungen der vorliegenden Erfindung veranschaulichen. The invention will be explained in more detail below with reference to the accompanying drawings, which illustrate the preferred embodiments of the present invention.
Kurze Beschreibung der Zeichnungen Brief description of the drawings
Figur 1 zeigt eine Luftzerlegungsanlage gemäß einer Ausführungsform der Erfindung in vereinfachter, schematischer Darstellung. FIG. 1 shows an air separation plant according to an embodiment of the invention in a simplified, schematic representation.
Nachfolgend beziehen sich Erläuterungen bzgl. bestimmter Verfahrensschritte auch auf entsprechende Vorrichtungen bzw. Komponenten von Anlagen und umgekehrt. Auf eine wiederholte Erläuterung wird der Übersichtlichkeit halber verzichtet. In the following, explanations regarding certain method steps also relate to corresponding devices or components of plants and vice versa. A repeated explanation is omitted for the sake of clarity.
Luftzerlegungsanlagen der gezeigten Art sind vielfach an anderer Stelle beschrieben, beispielsweise bei Fl.-W. Häring (Hrsg.), Industrial Gases Processing, Wiley-VCH,Air separation plants of the type shown are often described elsewhere, for example in Fl.-W. Häring (ed.), Industrial Gases Processing, Wiley-VCH,
2006, insbesondere Abschnitt 2.2.5, "Cryogenic Rectification". Für detaillierte Erläuterungen zu Aufbau und Funktionsweise sei daher auf entsprechende Fachliteratur verwiesen. Eine Luftzerlegungsanlage zum Einsatz der vorliegenden Erfindung kann auf unterschiedlichste Weise ausgebildet sein. 2006, particularly Section 2.2.5, "Cryogenic Rectification". For detailed explanations of the structure and function, please refer to the relevant specialist literature. An air separation plant for the use of the present invention can be designed in the most varied of ways.
In Figur 1 ist eine Luftzerlegungsanlage gemäß einer Ausführungsform der Erfindung in vereinfachter, schematischer Darstellung veranschaulicht und mit 100 bezeichnet.
Die Luftzerlegungsanlage 100 weist ein Rektifikationskolonnensystem 10 mit einer Hochdruckkolonne 11 , einer Niederdruckkolonne 12, einer Rohargonkolonne 13, einer Reinargonkolonne 14 und einem weiteren Trennapparat 15 auf. Die Hochdruckkolonne 11 ist in bekannter Weise mit der Niederdruckkolonne 12 über einen Hauptkondensator 15 wärmetauschend verbunden. Der weitere T rennapparat 15 weist zwei voneinander getrennte Trennabschnitte 15a, 15b auf. In FIG. 1, an air separation plant according to one embodiment of the invention is illustrated in a simplified, schematic representation and denoted by 100. The air separation plant 100 has a rectification column system 10 with a high-pressure column 11 , a low-pressure column 12 , a crude argon column 13 , a pure argon column 14 and a further separation apparatus 15 . The high-pressure column 11 is connected in a known manner to the low-pressure column 12 via a main condenser 15 in a heat-exchanging manner. The further separator 15 has two separate separating sections 15a, 15b.
In der Luftzerlegungsanlage 100 wird atmosphärische Luft mittels eines Hauptluftverdichters 1 oder einer oder mehrerer entsprechender Verdichterstufen über ein nicht gesondert bezeichnetes Filter angesaugt und verdichtet. Die Verdichtung erfolgt auf einen Druck in einem Druckbereich, der oberhalb eines Druckbereichs liegt, in dem die Hochdruckkolonne 11 betrieben wird. In the air separation plant 100, atmospheric air is sucked in and compressed by means of a main air compressor 1 or one or more corresponding compressor stages via a filter that is not designated separately. Compression takes place to a pressure in a pressure range that is above a pressure range in which the high-pressure column 11 is operated.
Nach dem Durchlaufen einer Vorreinigungseinheit 2, die in bekannter Weise ausgebildet sein können, wird die entsprechend behandelte Einsatzluft in ebenfalls an sich bekannter Weise in Teilströme aufgeteilt, die in der veranschaulichten Weise in einem Hauptwärmetauscher 4 abgekühlt, in Booster- bzw. Turbinenanordnungen 5, 6 verdichtet bzw. entspannt und in die Hochdruckkolonne 11 eingespeist bzw. als sogenannte Überschussluft ausgeleitet werden. Aus der Hochdruckkolonne 11 entnommene Flüssigkeit wird nach Abkühlung in einem Unterkühlungsgegenströmer 7 in die Niederdruckkolonne 12 eingespeist, die ferner mit Sumpfflüssigkeit der Hochdruckkolonne 11 gespeist wird, welche zuvor unter anderem durch Kopfkondensatoren der Roh- und Reinargonkolonne 13, 14 geführt wurde. After passing through a pre-cleaning unit 2, which can be designed in a known manner, the correspondingly treated feed air is divided, also in a manner known per se, into partial flows which are cooled in the illustrated manner in a main heat exchanger 4, in booster or turbine arrangements 5, 6 compressed or expanded and fed into the high-pressure column 11 or discharged as so-called excess air. Liquid taken from the high-pressure column 11 is fed after cooling in a sub-cooling countercurrent 7 into the low-pressure column 12, which is also fed with bottom liquid from the high-pressure column 11, which was previously passed through top condensers of the crude and pure argon columns 13, 14, among other things.
Sumpfflüssigkeit A aus der Niederdruckkolonne 12 wird mittels einer Innenverdichtungspumpe 8 flüssig auf Druck gebracht und nach Verdampfung oder Pseudoverdampfung als innenverdichtetes Sauerstoffprodukt bereitgestellt. Vom Kopf der Niederdruckkolonne 12 abgezogenes Kopfgas B wird nach Erwärmung in dem Unterkühlungsgegenströmer 7 und in dem Hauptwärmetauscher 4 extern in einem Verdichter 9 verdichtet. Über einen Seitenabzug wird Unreinstickstoff C aus der Niederdruckkolonne 12 entnommen, ebenfalls in dem Unterkühlungsgegenströmer 7 und in dem Hauptwärmetauscher 4 erwärmt, und beispielsweise als Regeneriergas in der Vorreinigungseinheit 2 verwendet.
An Sauerstoff und Argon reiches und an Stickstoff armes Fluid D wird der Niederdruckkolonne 12 entnommen. In einem Argogewinnungsmodus, zuvor als erster Betriebsmodus bezeichnet, wird das Fluid D in den Trennabschnitt 15a des weiteren Trennapparats 15 eingespeist, und dort mit einer Pumpe 16 geförderter Sumpfflüssigkeit E der Rohargonkolonne 13 entgegengeschickt. Flüssigkeit F aus einem unteren Bereich des Trennabschnitt 15a des weiteren Trennapparats 15, die gegenüber dem Fluid D an Argon abgereichert ist, wird in die Niederdruckkolonne 12 zurückgespeist. Im Trennabschnitt 15b des weiteren Trennapparats 14 wird unter Verwendung eines mit Einsatzluft gespeisten Sumpfverdampfers 17 aus weiterer Sumpfflüssigkeit der Rohargonkolonne 13 Reinsauerstoff G gewonnen. Bottom liquid A from the low-pressure column 12 is pressurized in liquid form by means of an internal compression pump 8 and, after evaporation or pseudo-evaporation, is made available as an internally compressed oxygen product. Top gas B drawn off from the top of the low-pressure column 12 is compressed externally in a compressor 9 after heating in the subcooling countercurrent flow 7 and in the main heat exchanger 4 . Impure nitrogen C is removed from the low-pressure column 12 via a side offtake, also heated in the subcooling countercurrent 7 and in the main heat exchanger 4 and used, for example, as regeneration gas in the pre-cleaning unit 2 . Fluid D rich in oxygen and argon and poor in nitrogen is taken from the low pressure column 12 . In an argon extraction mode, previously referred to as the first operating mode, the fluid D is fed into the separating section 15a of the further separating apparatus 15 and sent there towards the crude argon column 13 with the bottom liquid E conveyed by a pump 16 . Liquid F from a lower region of the separation section 15a of the further separation apparatus 15, which is depleted in argon compared to the fluid D, is fed back into the low-pressure column 12. In the separating section 15b of the further separating apparatus 14, pure oxygen G is obtained from further bottom liquid of the crude argon column 13 using a bottom evaporator 17 fed with feed air.
Kopfgas Fl des Trennabschnitts 15a des weiteren Trennapparats 15 wird in die Rohargonkolonne 13 überführt, die in bekannter Weise mit der Reinargonkolonne 14 gekoppelt ist und in entsprechender Weise betrieben wird, wodurch der Reinargonkolonne 14 Reinargon I entnommen werden kann. Top gas Fl of the separating section 15a of the further separating apparatus 15 is transferred to the crude argon column 13, which is coupled in a known manner to the pure argon column 14 and is operated in a corresponding manner, whereby pure argon I can be removed from the pure argon column 14.
Über einen ein Bypass 20 kann bei Bedarf und in bestimmten Betriebsmodi, insbesondere dem zuvor erwähnten zweiten Betriebsmodus, zumindest ein Teil des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids D ohne Zerlegung in den Rektifikationskolonnen 13 bis 15 dem Unreinstickstoff C zugespeist werden. Weitere Fluidverbindungen sind mit 21 bis 23 angegeben If necessary and in certain operating modes, in particular the aforementioned second operating mode, at least part of the fluid D rich in oxygen and argon and low in nitrogen can be fed to the impure nitrogen C via a bypass 20 without decomposition in the rectification columns 13 to 15. Other fluid connections are indicated at 21-23
Durch die Bereitstellung des Bypasses 20 kann in der Luftzerlegungsanlage 100 das in der Niederdruckkolonne 11 gebildete und aus dieser ausgeleitete Fluid D, das an Sauerstoff und Argon reich und an Stickstoff arm ist, in einem ersten Betriebsmodus zumindest zum Teil einer Tieftemperaturtrennung unter Verwendung der Roh- und Reinargonkolonnne 13, 14 unterworfen werden und in einem zweiten Betriebsmodus zumindest zum Teil aus der Luftzerlegungsanlage 100 ausgeleitet werden, ohne es der Tieftemperaturtrennung zu unterwerfen. By providing the bypass 20 in the air separation plant 100 formed in the low-pressure column 11 and discharged from this fluid D, which is rich in oxygen and argon and low in nitrogen, in a first operating mode at least partially a low-temperature separation using the raw and pure argon column 13, 14 and, in a second mode of operation, are at least partially discharged from the air separation plant 100 without subjecting it to cryogenic separation.
Entsprechende Betriebsmodi können insbesondere nach Maßgabe einer Steuereinrichtung 50 eingestellt werden, die den Bypass 20 öffnen oder schließen bzw. eine Einspeisung in den Trennabschnitt 15a unterbinden oder ermöglichen.
Corresponding operating modes can be set in particular according to a control device 50, which open or close the bypass 20 or prevent or enable a feed into the separating section 15a.
Claims
1. Luftzerlegungsanlage (100) zur Herstellung eines gasförmigen Stickstoffprodukts durch Tieftemperaturzerlegung von Luft, die ein Rektifikationskolonnensystem (10) mit einer Hochdruckkolonne (11), einer Niederdruckkolonne (12) und zumindest einer weiteren Rektifikationskolonne (13, 14) aufweist, wobei 1. Air separation plant (100) for producing a gaseous nitrogen product by low-temperature separation of air, which has a rectification column system (10) with a high-pressure column (11), a low-pressure column (12) and at least one further rectification column (13, 14), wherein
- die Luftzerlegungsanlage (100) dafür eingerichtet ist, das gasförmige Stickstoffprodukt unter Verwendung eines in der Niederdruckkolonne (12) gebildeten Kopfgases bereitzustellen, - the air separation plant (100) is set up to provide the gaseous nitrogen product using an overhead gas formed in the low-pressure column (12),
- die Luftzerlegungsanlage (100) dafür eingerichtet ist, in der Niederdruckkolonne (11) ein an Sauerstoff und Argon reiches und an Stickstoff armes Fluid zu bilden und zumindest einen Teil des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids aus der Niederdruckkolonne (12) auszuleiten, und - the air separation plant (100) is set up to form a fluid rich in oxygen and argon and poor in nitrogen in the low-pressure column (11) and at least part of the fluid rich in oxygen and argon and poor in nitrogen from the low-pressure column (12) to discharge, and
- die Luftzerlegungsanlage (100) dafür eingerichtet ist, in einem ersten Betriebsmodus zumindest einen Teil des an Sauerstoff und Argon reichen und an Stickstoff armen, aus der Niederdruckkolonne (12) ausgeleiteten Fluids einer Tieftemperaturtrennung unter Verwendung der zumindest einen weiteren Rektifikationskolonne (13, 14) zu unterwerfen, dadurch gekennzeichnet, dass - the air separation plant (100) is set up for, in a first operating mode, at least part of the fluid rich in oxygen and argon and low in nitrogen, discharged from the low-pressure column (12), to a low-temperature separation using the at least one further rectification column (13, 14) to submit, characterized in that
- die Luftzerlegungsanlage (100) dafür eingerichtet ist, in einem zweiten Betriebsmodus zumindest einen Teil des an Sauerstoff und Argon reichen und an Stickstoff armen, aus der Niederdruckkolonne (12) ausgeleiteten Fluids aus der Luftzerlegungsanlage (100) auszuleiten, ohne dieses der Tieftemperaturtrennung zu unterwerfen und ohne dieses einer weiteren Rektifikation zu unterwerfen. - the air separation plant (100) is set up to, in a second operating mode, discharge at least part of the fluid rich in oxygen and argon and low in nitrogen from the low-pressure column (12) from the air separation plant (100) without subjecting it to low-temperature separation and without subjecting it to further rectification.
2. Luftzerlegungsanlage (100) nach Anspruch 1 , bei der die zumindest eine weitere Rektifikationskolonne (13, 14) in einer Argongewinnungseinheit mit einer Rohargonkolonne (13) bereitgestellt ist.
2. Air separation plant (100) according to claim 1, wherein the at least one further rectification column (13, 14) is provided in an argon recovery unit with a crude argon column (13).
3. Luftzerlegungsanlage (100) nach Anspruch 1 oder 2, die dafür eingerichtet ist, den zweiten Betriebsmodus nach einem Anfahren der Luftzerlegungsanlage (100) und vor dem ersten Betriebsmodus durchzuführen. 3. Air separation plant (100) according to claim 1 or 2, which is set up to carry out the second operating mode after a start-up of the air separation plant (100) and before the first operating mode.
4. Luftzerlegungsanlage (100) nach Anspruch 2, die dafür eingerichtet ist, den zweiten Betriebsmodus bei einer Betriebsstörung oder Betriebspause der Argongewinnungseinheit statt des ersten Betriebsmodus durchzuführen. 4. Air separation plant (100) according to claim 2, which is set up to carry out the second operating mode instead of the first operating mode in the event of a malfunction or a break in operation of the argon recovery unit.
5. Luftzerlegungsanlage (100) nach Anspruch 3 oder Anspruch 4, die dafür eingerichtet ist, den zweiten Betriebsmodus so lange durchzuführen, bis wenigstens eine Kenngröße, die eine Tieftemperaturtrennung in der Niederdruckkolonne (11) kennzeichnet, einer Vorgabe entspricht. 5. Air separation plant (100) according to claim 3 or claim 4, which is set up to carry out the second operating mode until at least one parameter which characterizes a low-temperature separation in the low-pressure column (11) corresponds to a specification.
6. Luftzerlegungsanlage (100) nach Anspruch 5, wobei die Kenngröße, die die Tieftemperaturtrennung in der Niederdruckkolonne (11) kennzeichnet, eine Reinheit des gasförmigen Stickstoffprodukts ist. The air separation plant (100) of claim 5, wherein the parameter characterizing cryogenic separation in the low pressure column (11) is a purity of the gaseous nitrogen product.
7. Luftzerlegungsanlage (100) nach einem der vorstehenden Ansprüche, die zur Bildung des gasförmigen Stickstoffprodukts als Reinstickstoff mit einem Argongehalt von weniger als 4 ppm, 3 ppm, 2 ppm oder 1 ppm und mit einem Sauerstoffgehalt von 0.2 ppb bis 1 ppm eingerichtet ist. 7. Air separation plant (100) according to any one of the preceding claims, which is set up to form the gaseous nitrogen product as pure nitrogen with an argon content of less than 4 ppm, 3 ppm, 2 ppm or 1 ppm and with an oxygen content of 0.2 ppb to 1 ppm.
8. Luftzerlegungsanlage (100), nach einem der vorstehenden Ansprüche, die dafür eingerichtet ist, das an Sauerstoff und Argon reiche und an Stickstoff arme Fluid in der Niederdruckkolonne (12) mit einem Gehalt von 70 bis 95 Molprozent Sauerstoff, 5 bis 30 Molprozent Argon und weniger als 300 ppm Stickstoff zu bilden. 8. An air separation unit (100) according to any one of the preceding claims, which is arranged to contain the oxygen- and argon-rich and nitrogen-poor fluid in the low pressure column (12) with a content of 70 to 95 mole percent oxygen, 5 to 30 mole percent argon and form less than 300 ppm nitrogen.
9. Luftzerlegungsanlage (100) nach einem der vorstehenden Ansprüche, die eine Steuereinrichtung (50) zum Umschalten zwischen dem ersten und dem zweiten Betriebsmodus umfasst. 9. Air separation plant (100) according to any one of the preceding claims, which comprises a control device (50) for switching between the first and the second operating mode.
10. Luftzerlegungsanlage (100) nach Anspruch 9, bei dem für die die Ausleitung zumindest eines Teils des an Sauerstoff und Argon reichen und an Stickstoff
armen Fluids aus der Luftzerlegungsanlage (100) in dem zweiten Betriebsmodus eine Bypassleitung (20) bereitgestellt ist und bei dem die Steuereinrichtung zum Öffnen und Schließen der Bypassleitung durch Ansteuern eines in der Bypassleitung (20) angeordneten Ventils eingerichtet ist. 10. Air separation plant (100) according to claim 9, wherein for the discharge of at least a portion of the rich in oxygen and argon and in nitrogen poor fluid from the air separation plant (100) in the second operating mode a bypass line (20) is provided and in which the control device for opening and closing the bypass line by controlling a valve arranged in the bypass line (20) is set up.
11 . Luftzerlegungsanlage (100) nach Anspruch 10, bei dem die Steuereinrichtung (50) eingerichtet ist, eine oder mehrere Komponenten der Luftzerlegungsanlage (100) zu überwachen und auf Grundlage eines Ergebnisses der Überwachung von dem ersten in den zweiten Betriebsmodus umzuschalten. 11 . Air separation plant (100) according to Claim 10, in which the control device (50) is set up to monitor one or more components of the air separation plant (100) and to switch from the first to the second operating mode on the basis of a result of the monitoring.
12. Luftzerlegungsanlage (100) nach einem der vorstehenden Ansprüche, die dafür eingerichtet ist, das an Sauerstoff und Argon reiche und an Stickstoff arme Fluid in dem ersten und dem zweiten Betriebsmodus an unterschiedlichen Entnahmestellen aus der Niederdruckkolonne (12) auszuleiten. 12. Air separation plant (100) according to any one of the preceding claims, which is set up to discharge the fluid rich in oxygen and argon and low in nitrogen in the first and the second operating mode at different removal points from the low-pressure column (12).
13. Verfahren zur Herstellung eines gasförmigen Stickstoffprodukts durch Tieftemperaturzerlegung von Luft, bei dem eine Luftzerlegungsanlage (100) verwendet wird, die ein Rektifikationskolonnensystem (10) mit einer Flochdruckkolonne (11), einer Niederdruckkolonne (12) und zumindest einer weiteren Rektifikationskolonne (13, 14) aufweist, wobei 13. A process for producing a gaseous nitrogen product by low-temperature separation of air, in which an air separation plant (100) is used which has a rectification column system (10) with a flat pressure column (11), a low-pressure column (12) and at least one further rectification column (13, 14 ) has, where
- das gasförmige Stickstoffprodukt unter Verwendung eines in der Niederdruckkolonne (12) gebildeten Kopfgases bereitgestellt wird, - the gaseous nitrogen product is provided using an overhead gas formed in the low-pressure column (12),
- in der Niederdruckkolonne (11) ein an Sauerstoff und Argon reiches und an Stickstoff armes Fluid gebildet und zumindest einen Teil des an Sauerstoff und Argon reichen und an Stickstoff armen Fluids aus der Niederdruckkolonne (12) ausgeleitet wird, und - A fluid rich in oxygen and argon and poor in nitrogen is formed in the low-pressure column (11) and at least part of the fluid rich in oxygen and argon and poor in nitrogen is discharged from the low-pressure column (12), and
- in einem ersten Betriebsmodus zumindest ein Teil des an Sauerstoff und Argon reichen und an Stickstoff armen, aus der Niederdruckkolonne (12) ausgeleiteten Fluids einer Tieftemperaturtrennung unter Verwendung der zumindest einen weiteren Rektifikationskolonne (13, 14) unterworfen wird, dadurch gekennzeichnet, dass
- in einem zweiten Betriebsmodus zumindest ein Teil des an Sauerstoff und Argon reichen und an Stickstoff armen, aus der Niederdruckkolonne (12) ausgeleiteten Fluids aus der Luftzerlegungsanlage (100) ausgeleitet wird, ohne dass dieses der Tieftemperaturtrennung und ohne dass dieses einer weiteren Rektifikation unterworfen wird. - in a first operating mode, at least part of the fluid that is rich in oxygen and argon and low in nitrogen and discharged from the low-pressure column (12) is subjected to a low-temperature separation using the at least one further rectification column (13, 14), characterized in that - in a second operating mode, at least part of the fluid rich in oxygen and argon and low in nitrogen and discharged from the low-pressure column (12) is discharged from the air separation plant (100) without being subjected to low-temperature separation and without being subjected to further rectification .
14. Verfahren nach Anspruch 13, bei dem eine Luftzerlegungsanlage (100) nach einem der Ansprüche 1 bis 12 verwendet wird.
14. The method according to claim 13, wherein an air separation plant (100) according to any one of claims 1 to 12 is used.
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2022
- 2022-01-19 WO PCT/EP2022/025017 patent/WO2022174976A1/en active Application Filing
- 2022-02-10 TW TW111104876A patent/TW202234006A/en unknown
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH051883A (en) | 1991-06-24 | 1993-01-08 | Hitachi Ltd | Air separation device |
JPH06281323A (en) * | 1993-03-26 | 1994-10-07 | Nippon Steel Corp | Ar recovery device and recovery method |
JP2906010B2 (en) | 1993-03-26 | 1999-06-14 | 新日本製鐵株式会社 | Ar recovery device and recovery method |
JPH1082582A (en) | 1996-09-06 | 1998-03-31 | Nippon Sanso Kk | Air liquefaction separation device and start-up method thereof |
US6138474A (en) | 1999-01-29 | 2000-10-31 | Air Products And Chemicals, Inc. | Argon production control through argon inventory manipulation |
US20170299262A1 (en) | 2014-10-16 | 2017-10-19 | Linde Aktiengesellschaft | Method and device for variably obtaining argon by means of low-temperature separation |
DE102016011084A1 (en) | 2016-09-13 | 2018-03-15 | Linde Aktiengesellschaft | A method and apparatus for recovering a high purity oxygen product stream by cryogenic separation of air |
Non-Patent Citations (1)
Title |
---|
H.-W. HÄRING: "Industrial Gases Processing", 2006, WILEY-VCH |
Also Published As
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TW202234006A (en) | 2022-09-01 |
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