EP4567360A2 - Verfahren zur herstellung von hochreinem sauerstoff und lufttrennvorrichtung zur herstellung von hochreinem sauerstoff - Google Patents

Verfahren zur herstellung von hochreinem sauerstoff und lufttrennvorrichtung zur herstellung von hochreinem sauerstoff Download PDF

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Publication number
EP4567360A2
EP4567360A2 EP24217636.0A EP24217636A EP4567360A2 EP 4567360 A2 EP4567360 A2 EP 4567360A2 EP 24217636 A EP24217636 A EP 24217636A EP 4567360 A2 EP4567360 A2 EP 4567360A2
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EP
European Patent Office
Prior art keywords
nitrogen
oxygen
rectification column
gas
condenser
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP24217636.0A
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English (en)
French (fr)
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EP4567360A3 (de
Inventor
Kenji Hirose
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP4567360A2 publication Critical patent/EP4567360A2/de
Publication of EP4567360A3 publication Critical patent/EP4567360A3/de
Pending legal-status Critical Current

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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
    • F25J3/04309—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 nitrogen
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F25J3/04054—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams of air
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    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
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    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
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    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04236—Integration of different exchangers in a single core, so-called integrated cores
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    • 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
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • F25J3/0426—The cryogenic component does not participate in the fractionation
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    • 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
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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
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    • F25J3/04321—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 oxygen
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/50—Oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/50—Separating low boiling, i.e. more volatile components from oxygen, e.g. N2, Ar
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/42—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/10—Boiler-condenser with superposed stages
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams

Definitions

  • the present invention relates to a high-purity oxygen production method and an air separation apparatus for producing high-purity oxygen.
  • cryogenic air separation As high-purity oxygen production methods in which components having a higher boiling point or a lower boiling point than oxygen are controlled to the order of ppm or less, there are known methods that employ cryogenic air separation.
  • One such production method that can be cited is a method in which an oxygen-containing liquid or gas is discharged from a cryogenic air separation apparatus, and high-purity oxygen is rectified (see, for example, WO2018/219685 A1 ).
  • a process liquid such as an oxygen-enriched liquid is used as the heat medium, as in WO2018/219685 , since the sensible heat of the process liquid is used to provide the latent heat of vaporisation of the liquefied oxygen, a large molar flow rate is required, while at the same time the amount of heat supplied is limited by process balance constraints, and as a result there is a problem in that the amount of high-purity oxygen that can be recovered remains small.
  • the present disclosure provides a high-purity oxygen production method and an air separation apparatus for producing high-purity oxygen, with which energy consumption is reduced even while a process gas is used as a heat medium for liquefied oxygen, so as to avoid high-purity oxygen production capacity constraints.
  • US 2023/0038170 relates to a process for oxygen production at 99.8% content whereas the present invention allows oxygen to be produced with ppm order impurities.
  • the liquid fed to the oxygen column comes from the liquid sump at the bottom of the column fed by the feed air, where hydrocarbons from feed air are accumulated.
  • the feed (oxygen containing stream) to the pure oxygen column is comes from a section where hydrocarbons (eg. methane) have been removed.
  • the difference between the boiling point of oxygen and the ⁇ T of the heat exchanger determine the saturation temperature and pressure of the condensable gas. Principally, the lower the saturation pressure, the less energy is needed for reboil.
  • the present invention uses oxygen-enriched gas for oxygen reboil, where the saturation pressure can be lower than pure nitrogen.
  • the method comprises:
  • the oxygen-containing fluid may be a liquid or a gas-liquid mixture.
  • the nitrogen gas in the vapour stream is caused to exchange heat with the oxygen-enriched liquid in the nitrogen condenser, thereby vaporising the oxygen-enriched liquid to generate oxygen-enriched gas.
  • the oxygen-enriched gas which is utilised as a heat medium for the oxygen evaporator, has a pressure and composition sufficient to vaporise the rectified liquefied oxygen in the bottom portion of the high-purity oxygen rectification column using latent heat.
  • oxygen-enriched gas containing a large amount of oxygen can vaporise liquefied oxygen at a lower pressure than air or nitrogen, liquefied oxygen can be vaporised at the supply pressure from the nitrogen evaporator without the use of a com pressor.
  • the oxygen-containing gas condensed (re-liquefied) in the oxygen evaporator may be re-supplied to the nitrogen condenser.
  • recondensed oxygen enriched liquid obtained by condensing the oxygen enriched gas in the oxygen evaporator is re-supplied to a refrigerant side of the nitrogen condenser and vaporised through heat exchange with the vapour stream (nitrogen gas).
  • the recondensed oxygen enriched liquid may be delivered to the nitrogen condenser by means of a head pressure utilizing a height difference between the oxygen evaporator and the nitrogen condenser.
  • delivery may be effected using a pump.
  • the nitrogen rectification column may include a rectification portion for separating high boiling-point components (for example, methane) from the oxygen contained in the supplied feed air, and for discharging an oxygen-containing liquid from an upper stage thereof.
  • high boiling-point components for example, methane
  • the oxygen-containing liquid serving as the feedstock for the high-purity oxygen is obtained by discharging some reflux liquid from above the feed air introduction portion of the nitrogen rectification column as the oxygen-containing liquid, the reflux liquid containing sufficient oxygen to serve as a feedstock for the high-purity oxygen while having high boiling-point components removed sufficiently.
  • a rectification portion is disposed midway between the feed air introduction portion and the oxygen-containing liquid discharge portion, and is configured such that high boiling-point components removed from the feed air are transferred into the liquefied oxygen by gas-liquid contact and are concentrated in the lower portion of the rectification column.
  • the rectification portion may consist of rectification plates, structured packing, or random packing.
  • a high-purity oxygen production method includes:
  • a fourth high-purity oxygen production method includes:
  • the first, second, third and fourth high-purity oxygen production methods may include a waste gas extraction step in which gas discharged from the top portion of the high-purity oxygen rectification column is passed through the main heat exchanger and is extracted as waste gas.
  • High-purity oxygen is oxygen having a concentration of at least 99.99% mol. According to the present invention, there is provided an air separation apparatus for producing high purity oxygen, comprising:
  • the air separation apparatus may comprise:
  • a fourth air separation apparatus may comprise:
  • the air separation apparatus may comprise:
  • the air separation apparatus may include:
  • Energy consumption can be reduced even while using a process gas as a heat medium for liquefied oxygen, so as to avoid high-purity oxygen production capacity constraints.
  • the first air separation apparatus A1 according to a comparative example will be described with reference to Figure 1 .
  • the first air separation apparatus A1 comprises a main heat exchanger 1, a nitrogen rectification column 2, a nitrogen condenser 3, an expansion turbine 92, a high-purity oxygen rectification column 5, and an oxygen evaporator 6.
  • the main heat exchanger 1 cools feed air introduced from a hot end and discharges the same from a cold end.
  • the cooled feed air is introduced into the nitrogen rectification column 2 via a feed air pipeline L1.
  • the nitrogen rectification column 2 comprises a bottom portion 21, a rectification portion 22, and a top portion 23.
  • the feed air pipeline L1 is connected to the bottom portion 21.
  • Oxygen-enriched liquid that collects in the bottom portion 21 is sent to a refrigerant phase 31 of the nitrogen condenser 3 via an oxygen-enriched liquid pipeline L21.
  • the nitrogen condenser 3 is provided above the top portion 23.
  • a portion of nitrogen gas (vapour stream) discharged from the top 23 of the nitrogen rectification column 2 is introduced into the nitrogen condenser 3 via a reflux pipeline L231, and is cooled (condensed) through heat exchange with the oxygen-enriched liquid to form liquefied nitrogen.
  • the liquefied nitrogen is returned to the top portion 23 of the nitrogen rectification column 2 as reflux liquid.
  • An oxygen-containing fluid is discharged from between intermediate portions 221, 222 of the rectification portion 22 of the nitrogen rectification column 2 via the oxygen-containing fluid pipeline L221 and is introduced into a top portion 53 of the high-purity oxygen rectification column 5.
  • Nitrogen gas discharged from the top portion 23 of the nitrogen rectification column 2 is sent via a product nitrogen gas extraction pipeline L23 to the main heat exchanger 1 and is extracted as product nitrogen gas.
  • Oxygen-enriched gas (oxygen-enriched liquid vapour) discharged from a top portion 31 of the nitrogen condenser 3 is introduced via a waste gas extraction pipeline L31 into the cold end of the main heat exchanger 1, is discharged from an intermediate part thereof, is then expanded and cooled in the expansion turbine 92, and is again sent to the main heat exchanger 1 and is extracted as waste gas.
  • a portion of the oxygen-enriched gas (oxygen-enriched liquid vapour) discharged from the top portion (refrigerant phase) 31 of the nitrogen condenser 3 is sent as a heat medium via a heat medium pipeline L311 to the oxygen evaporator 6, is re-liquefied, and is returned again to the top portion (refrigerant phase) 31 of the nitrogen condenser 3.
  • the re-liquefied oxygen-enriched gas is supplied as a recycled oxygen-enriched liquid to the nitrogen condenser 3, as a refrigerant.
  • the high-purity oxygen rectification column 5 includes a bottom portion 51, a rectification portion 52, and a top portion 53.
  • Oxygen-containing liquid is introduced into the top portion 53 of the high-purity oxygen rectification column 5 and is rectified in the rectification portion 52, and liquefied oxygen collects in the bottom portion 51.
  • the oxygen evaporator 6 is provided in the bottom portion 51 of the high-purity oxygen rectification column 5. Liquid oxygen is converted into a vapour stream (oxygen gas) by the heat medium nitrogen gas in the oxygen evaporator 6, heat and material are exchanged in the rectification portion 52, and high-purity oxygen accumulates in the bottom portion 51. Gas discharged from the top portion 53 of the high-purity oxygen rectification column 5 passes through a pipeline L53 to merge with the waste gas extraction pipeline L31, is sent to the main heat exchanger 1, and is extracted as waste gas.
  • the second air separation apparatus A2 according to the comparative example will be described with reference to Figure 2 .
  • the same reference numerals as those in Figure 1 have the same functions, and therefore descriptions thereof may be omitted.
  • the second air separation apparatus A2 comprises the main heat exchanger 1, the nitrogen rectification column 2, a first nitrogen condenser 3, a second nitrogen condenser 4, a compressor 91, the expansion turbine 92, the high-purity oxygen rectification column 5, and the oxygen evaporator 6. Aspects of the configuration that differ from embodiment 1 will mainly be described.
  • the first nitrogen condenser 3 is disposed above the nitrogen rectification column 2, and the second nitrogen condenser 4 is disposed above the first nitrogen condenser 3.
  • Some nitrogen gas (vapour stream) discharged from the top portion 23 of the nitrogen rectification column 2 is introduced into the first nitrogen condenser 3 via a first reflux pipeline L231, and is cooled (condensed) through heat exchange with the oxygen-enriched liquid to form liquefied nitrogen.
  • the liquefied nitrogen is returned to the top portion 23 of the nitrogen rectification column 2 as reflux liquid.
  • Some nitrogen gas (vapour stream) discharged from the top portion 23 of the nitrogen rectification column 2 is introduced into the second nitrogen condenser 4 via a second reflux pipeline L232, and is cooled (condensed) through heat exchange with the oxygen-enriched liquid to form liquefied nitrogen.
  • the liquefied nitrogen is returned to the top portion 23 of the nitrogen rectification column 2 as reflux liquid.
  • An oxygen-enriched liquid pipeline L211 is a pipeline through which oxygen-enriched liquid discharged from the bottom portion 21 of the nitrogen rectification column 2 is passed partially through the main heat exchanger 1 and is then introduced into the second nitrogen condenser 4.
  • the oxygen-enriched liquid from the second nitrogen condenser 4 is sent as a refrigerant to the first nitrogen condenser 3.
  • the compressor 91 compresses gas discharged from a top portion 41 of the second nitrogen condenser 4.
  • a recycled gas pipeline L41 is a pipeline through which gas is discharged from the top portion 41 of the second nitrogen condenser 4, is compressed by the compressor 91, is passed through the main heat exchanger 1, and is then introduced as recycled gas into the rectification portion 22 of the nitrogen rectification column 2.
  • the third air separation apparatus A3 comprises the main heat exchanger 1, a first nitrogen rectification column 2, a second nitrogen rectification column 7, the first nitrogen condenser 3, the second nitrogen condenser 4, the compressor 91, the expansion turbine 92, the high-purity oxygen rectification column 5, and the oxygen evaporator 6. Aspects of the configuration that differ from Figure 2 will mainly be described.
  • Oxygen-enriched gas (vapour) generated in the first nitrogen condenser 3 and oxygen-enriched liquid discharged from the bottom portion 21 of the first nitrogen rectification column 2 are introduced into the second nitrogen rectification column 7.
  • An oxygen-enriched liquid pipeline L212 is a pipeline through which oxygen-enriched liquid discharged from the bottom portion 21 of the first nitrogen rectification column 2 is introduced into the main heat exchanger 1, is discharged from an intermediate stage thereof, and is then introduced between intermediate stages 721 and 722 of the rectification portion of the second nitrogen rectification column 7.
  • An oxygen-containing liquid pipeline L723 is a pipeline that introduces oxygen-containing fluid discharged from between intermediate stages 722, 723 of the rectification portion of the second nitrogen rectification column 7 into the top portion 53 of the high-purity oxygen rectification column 5.
  • the position at which the oxygen-containing fluid is discharged into the oxygen-containing fluid pipeline L723 is above the position at which the oxygen-enriched liquid from the oxygen-enriched liquid pipeline L212 is introduced.
  • a heat medium pipeline L711 is a pipeline through which gas (oxygen-enriched gas) discharged from below the lower-stage rectification portion 721 of the second nitrogen rectification column 7 is sent as a heat medium to the oxygen evaporator 6, is re-liquefied, and is sent as a refrigerant phase 41 to the second nitrogen condenser 4 via pipeline L61.
  • a recycled gas pipeline L722 is a pipeline through which gas is discharged from between the intermediate stages 721 and 722 of the rectification portion of the second nitrogen rectification column 7, is compressed by the compressor 91, is passed through a portion of the main heat exchanger 1, and is then introduced as recycled gas into the rectification portion 22 of the first nitrogen rectification column 2.
  • a waste gas extraction pipeline L411 is a pipeline through which gas discharged from the top portion 41 of the second nitrogen condenser 4 is passed partially through the main heat exchanger 1, is then sent to the expansion turbine 92 to be expanded and cooled, is again passed through the main heat exchanger 1, and is extracted as waste gas, after mixing with top gas from the oxygen rectification column.
  • a vapour stream pipeline L731 is a pipeline through which a vapour stream that is discharged from a top portion 73 of the second nitrogen rectification column 7 and is sent to the second nitrogen condenser 4 and is returned in liquid form in part to the top portion 73 of the second nitrogen rectification column 7.
  • a pipeline L732 branches off from the liquid stream pipeline L731 downstream of the second nitrogen condenser 4 and feeds into the top portion 23 of the first nitrogen rectification column 2.
  • a liquid transfer pump P1 is provided in the pipeline L732.
  • the fourth air separation apparatus A4 will be described with reference to Figure 4 .
  • the same reference numerals as those in figures 2 and 3 have the same functions, and therefore descriptions thereof may be omitted.
  • the fourth air separation apparatus A4 comprises the main heat exchanger 1, the first nitrogen rectification column 2, the second nitrogen rectification column 7, the first nitrogen condenser 3, the second nitrogen condenser 4, the compressor 911, the expansion turbine 921, the high-purity oxygen rectification column 5, and the oxygen evaporator 6. Aspects of the configuration that differ from figure 3 will mainly be described.
  • the compressor 911 compresses a portion of the feed air.
  • the expansion turbine 921 expands compressed air that has been compressed by the compressor 911, introduced into the main heat exchanger 1, and discharged from an intermediate part thereof.
  • a feed air branch pipeline L11 is a pipeline that branches off from the feed air pipeline L1 upstream of the main heat exchanger 1, sends a portion of the feed air to the compressor 911 that compresses the feed air, sends the feed air compressed by the compressor 911 to the main heat exchanger 1 and discharges the same from an intermediate part thereof to the expansion turbine 921 that expands the feed air, and then sends the feed air to the rectification portion of the second nitrogen rectification column 7.
  • a low-pressure nitrogen gas extraction pipeline L732 is a pipeline through which gas discharged from the top portion 73 of the second nitrogen rectification column 7 is extracted as low-pressure nitrogen gas.
  • a waste gas extraction pipeline L412 is a pipeline through which gas discharged from the top portion 41 of the second nitrogen condenser 4 is extracted as waste gas.
  • the pipeline L53 merges with the waste gas extraction pipeline L412.
  • coldness required for the heat balance is obtained by using the expansion turbine 921 to expand either a portion of the feed air or product nitrogen gas discharged from the first nitrogen rectification column 2 to the pressure of the second nitrogen rectification column 7.
  • Motive power obtained by the expansion turbine 921 may be applied to the motive power of the compressor 911 that compresses the feed air. It should be noted that the same applies to figures 2 and 3 .
  • Nitrogen gas (330 Nm 3 /h, 9.7 barA), liquefied nitrogen (48 Nm3/h, 9.7 barA), oxygen-enriched liquid (552 Nm 3 /h, oxygen 35.3%) were discharged from the first nitrogen rectification column 2.
  • the liquefied nitrogen and oxygen-enriched liquid were introduced into the second nitrogen rectification column 7.
  • Low-pressure nitrogen gas (311 Nm3/h, 4.3 barA), oxygen-containing liquid (73 Nm3/h, 20.0 % O2), oxygen enriched gas (54Nm3/h, 4.3 barA, 36.3% O2), low-pressure oxygen enriched liquid (232 Nm3/h, 75.5% O2) were discharged from the second nitrogen rectification column 7.
  • the oxygen enriched gas was used as the heat medium in the oxygen evaporator 6, and was introduced to the second nitrogen condenser 4 as a coolant.
  • the low-pressure oxygen enriched liquid was introduced to the second nitrogen condenser 4 as a coolant.
  • the oxygen-containing liquid was introduced to the oxygen rectification column.
  • the oxygen rectification column 5 was operated at 1.5 barA, and high-purity oxygen (10.8 Nm 3 /h, 100%) collected in the bottom portion 51.
  • the heat medium used in the oxygen evaporator 6 in the present example has a higher oxygen concentration than the feed air, thus allowing condensation to occur at a lower pressure such as 4.3 barA for the oxygen enriched gas instead of 9.9 barA for the feed air, and as a result reducing the compression energy required for the heat medium.
  • the amount of feed air that can be supplied to the first nitrogen rectification column 2 can be increased, also making it possible to improve the nitrogen gas recovery.
  • methane is distributed to the oxygen stream in the comparative example process because there is no mechanism to separate methane from oxygen, and the methane concentration in oxygen will be more than 4.8 ppm when 11 Nm3/h of oxygen is produced from 1000 Nm3/h of feed air.
  • the oxygen-containing liquid supplied to the oxygen rectification column is derived from the methane-free reflux fluid above the location where the methane-containing fluid is supplied, so that an oxygen product with a methane content of less than 1 ppm can be produced.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)
EP24217636.0A 2023-12-06 2024-12-05 Verfahren zur herstellung von hochreinem sauerstoff und lufttrennvorrichtung zur herstellung von hochreinem sauerstoff Pending EP4567360A3 (de)

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TW202538219A (zh) 2025-10-01
EP4567360A3 (de) 2025-09-17
CN120101420A (zh) 2025-06-06
US20250189218A1 (en) 2025-06-12
JP7505702B1 (ja) 2024-06-25
KR20250087458A (ko) 2025-06-16

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