EP2312247A1 - Procédé et dispositif de production d'azote liquide par décomposition de l'air à basse température - Google Patents

Procédé et dispositif de production d'azote liquide par décomposition de l'air à basse température Download PDF

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Publication number
EP2312247A1
EP2312247A1 EP10013337A EP10013337A EP2312247A1 EP 2312247 A1 EP2312247 A1 EP 2312247A1 EP 10013337 A EP10013337 A EP 10013337A EP 10013337 A EP10013337 A EP 10013337A EP 2312247 A1 EP2312247 A1 EP 2312247A1
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Prior art keywords
pressure column
pressure
low
nitrogen
top condenser
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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.)
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EP10013337A
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German (de)
English (en)
Inventor
Alexander Alekseev
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Linde GmbH
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Linde GmbH
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Priority to EP10013337A priority Critical patent/EP2312247A1/fr
Publication of EP2312247A1 publication Critical patent/EP2312247A1/fr
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04151Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04193Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/042Division of the main heat exchange line in consecutive sections having different functions having an intermediate feed connection
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04151Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/0423Subcooling of liquid process streams
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04278Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using external refrigeration units, e.g. closed mechanical or regenerative refrigeration units
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284Generation 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
    • F25J3/0429Generation 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
    • F25J3/04296Claude expansion, i.e. expanded into the main or high pressure column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04339Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of air
    • F25J3/04345Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of air and comprising a gas work expansion loop
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04406Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04424Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system without thermally coupled high and low pressure columns, i.e. a so-called split columns
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/20Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/02Internal refrigeration with liquid vaporising loop
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/90External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration

Definitions

  • the invention relates to a method according to the preamble of patent claim 1.
  • the "first pressure”, in which the feed air is cleaned for example, 5 to 12 bar, preferably 5.5 to 7.0 bar. He is about equal to the operating pressure of the high pressure column or is slightly above.
  • the "second pressure" is well above the first pressure. It is for example at least 50 bar, in particular 50 to 80 bar, preferably 55 to 70 bar.
  • the "main heat exchanger” may be formed of one or more parallel and / or serially connected heat exchanger sections, for example one or more plate heat exchanger blocks.
  • distillation column system for nitrogen-oxygen separation has exactly two distillation columns, namely a high-pressure column and a low-pressure column (30). Other distillation columns for nitrogen-oxygen separation do not exist in the system. Further distillation columns for other separation tasks, for example for the noble gas production can be provided in principle. Preferably, however, the invention relates to methods and devices which have no further separation columns apart from the high-pressure column and the low-pressure column.
  • the "nitrogen-oxygen separation distillation column system” also includes a single high-pressure column top condenser for liquefying overhead gas of the high-pressure column, which is designed as a condenser-evaporator and has a liquefaction space and a single evaporation space.
  • the high-pressure column head condenser has only a single evaporation space, that is, all parts of the evaporation space are in communication with each other.
  • the high-pressure column top condenser does not use multiple cooling media operated different composition, but preferably only with a single cooling medium.
  • the high-pressure column top condenser also has only a single liquefaction space, in which at least part of the top gas of the high-pressure column becomes liquefied.
  • the "choke flow” is cooled in the main heat exchanger by indirect heat exchange and liquefied or - at supercritical pressure - pseudo-liquefied.
  • the relaxation of the inductor current prior to its introduction into the denitration system for nitrogen-oxygen separation is usually carried out in a throttle valve; Alternatively, a work-performing relaxation can be made in a liquid turbine. In the relaxation of the inductor current creates a two-phase mixture, which consists predominantly of liquid.
  • the invention is therefore based on the object to provide a method of the type mentioned above and a corresponding device, which have a very low energy consumption. In this case, the expenditure on equipment should be kept within limits.
  • the high-pressure column top condenser is not cooled with a throttled air flow, but with bottom liquid from the high-pressure column.
  • the invention has the advantage that a fraction having a constant composition (and thus a constant boiling temperature) is used on the evaporation side of the high-pressure column top condenser. Especially with changing load (underload / overload), this results in a particularly stable operation of the columns. Even if the composition of the fractions in the columns changes during a load change, the head temperature of the high-pressure column remains constant and the operating pressures of the columns need not be readjusted.
  • liquid air from the reactor flow (about 21 mol% oxygen content) boils at a lower temperature than the bottom liquid of the high-pressure column (minimum 32 mol%, usually 36 to 40 mol% oxygen content), so that the operating pressure of the high-pressure column at the Invention are kept relatively low and the process works energetically particularly favorable.
  • the relaxed throttle flow can be fed directly or indirectly into the evaporation chamber of the high-pressure column top condenser.
  • the refrigerant flow is introduced immediately downstream of the expansion of the throttle flow directly into the evaporation space of the high-pressure column top condenser.
  • the refrigerant flow can be formed by the entire throttle flow or by a part which is branched off immediately after the relaxation.
  • the phase separation is carried out at an intermediate point of the high-pressure column.
  • the inductor current (or a part thereof) at an intermediate point in the High pressure column introduced and the refrigerant flow from a arranged at this intermediate point collecting device for liquid (for example cup) again taken.
  • the intermediate point is, for example, immediately above the sixth to twelfth, preferably the eighth to the eleventh theoretical bottom from below with a total circumference of, for example 40 to 90, preferably 40 to 60 theoretical plates in the high pressure column (depending on the desired product purity).
  • the cold required for the product liquefaction is generated in a two-turbine air cycle, as described in claim 4.
  • the two expansion machines are usually formed by expansion turbines. They preferably have the same inlet pressure (at the level of the intermediate pressure or above) and / or the same outlet pressure (at the level of the first pressure).
  • the mechanical energy generated in the expansion machines is transmitted by mechanical coupling to two serial booster in which a portion of the air from the intermediate pressure to the high pressure is further compressed, as is the subject of claim 5.
  • the high pressure stream can then be used as a throttle current; alternatively or additionally, the two turbine streams are formed by the high-pressure stream; In this case, the refrigeration and thus the liquid production can be further increased, without having to be supplied with energy from the outside.
  • the entire cold used in the high-pressure column top condenser is provided by the refrigerant flow.
  • the refrigerant flow formed from the throttle flow thus represents the some feed stream for the evaporation space of the high-pressure column top condenser.
  • the vapor generated in the evaporation chamber of the high-pressure column head condenser can be introduced into the low-pressure column, in particular at its bottom. He serves there as ascending steam, preferably it forms the entire rising in the low pressure column steam.
  • neither the high-pressure column nor the low-pressure column have a reboiler for producing ascending vapor from liquid of the corresponding column.
  • At least part of the liquid obtained in the liquefaction space of the high-pressure column overhead condenser can be introduced into the low-pressure column and further separated there.
  • a liquid crude oxygen stream from the bottom of the high-pressure column is preferably introduced into the low-pressure column.
  • a decomposition air flow which is formed by another part of the purified feed air, is introduced in a gaseous state into the high-pressure column, in particular at its bottom.
  • the decomposition airflow may be formed by a portion of the two turbine streams downstream of the work-performing expansion.
  • At least 50 mol%, especially 50 to 60 mol%, of the total amount of feed air introduced into the nitrogen-oxygen separation distillation column system is introduced in the liquid state distillation column system for nitrogen-oxygen separation ,
  • the invention also relates to a process for the recovery of liquid nitrogen by cryogenic air separation according to claim 14.
  • FIG. 1 is divided by three dashed rectangles into the process parts pretreatment of air, refrigeration system and distillation column system for nitrogen-oxygen separation (from left to right).
  • the incoming air 1 is fed via a filter 2 to a main air compressor 3 and there compressed to a first pressure of 5.5 to 7.0 bar and cooled in a pre-cooler 4 back to about ambient temperature, for example by indirect heat exchange in a heat exchanger or through direct heat exchange in a direct contact cooler.
  • the precooled air is purified under the first pressure in a purifier 5 containing molecular sieve adsorber.
  • the purified air 6 (AIR) is supplied to the refrigeration system, which serves to cool the feed air and to generate liquefaction refrigeration.
  • the purified feed air 6 is first at least partially mixed with a recycle stream 7 to a circulation stream 8.
  • the circulation stream 8 is further compressed in a cycle compressor 9 with aftercooler 10 to an intermediate pressure of 30 to 40 bar.
  • the entire intermediate compressed air 11 is further compressed in two serially connected after-compressors 12, 14 to a high pressure of at least 50 bar, in particular between 50 and 80 bar, preferably to 55 to 70 bar.
  • the after-compressors 12, 14 are each followed by an after-cooler 13, 15.
  • the high-pressure air 16 is divided into two partial streams 17, 18.
  • the first partial flow 17 includes a throttle flow and a first turbine flow, which enter together in the warm end of a main heat exchanger 19 and are cooled to a first intermediate temperature which is between ambient temperature and dew point of the air. At this intermediate temperature, the first turbine stream 20 is branched off from the first partial stream. The remainder is further cooled to the cold end in the main heat exchanger and pseudo-liquefied and forms the inductor 21, which comprises slightly more than half of the total amount of air 1.
  • the first Turbine stream 20 is in a first (cold) turbine 22 working to relax to about the first pressure and to a temperature which is a few degrees above the tau.
  • the expanded first turbine stream 23 is completely or substantially completely gaseous and forms a gaseous decomposition air stream 24 to a first part.
  • the remainder 25 is supplied to the cold end of the main heat exchanger 19 and reheated to approximately ambient temperature.
  • the second partial flow of the high-pressure air 16 forms a second turbine stream 18. This is expanded from about ambient temperature and the high pressure in a second (warm) turbine 26 work, also about the first pressure.
  • the relaxed second turbine stream 27 re-enters the main heat exchanger 19 at a second intermediate temperature where it is combined with the part 25 of the expanded first substream 23 to form the recycle stream 7 and recycled to the cycle compressor 9.
  • the operating pressure of the high-pressure column 28 is between 5.5 and 7.0 bar.
  • the decomposition air stream 24 is fed in gaseous form directly at the bottom of the high-pressure column 28.
  • the throttle flow 21 is expanded in a throttle valve 32 to a pressure of below 4 bar and completely introduced as a refrigerant flow 33 in the evaporation chamber of the high-pressure column top condenser.
  • the head gas 34 of the high-pressure column 28 consists of virtually pure nitrogen and is led to a first part 35 (in a molar amount which is slightly less than half of the incoming air quantity 1) in the liquefaction space of the high-pressure column top condenser 29 and there substantially completely liquefied.
  • Liquid 36 produced in the high-pressure column overhead condenser is fed to a first part 37 as reflux to the high-pressure column 28.
  • the remainder 38 is cooled after cooling in a subcooling countercurrent 39 and fed via a throttle valve 40 as reflux to the low pressure column 30, which is operated at a pressure below 4 bar.
  • the accumulating in the bottom of the high pressure column 28 liquid is as a liquid crude oxygen stream 41 on the Subcooling countercurrent 39 and a throttle valve 42 is fed into the evaporation space of the low-pressure column top condenser 31.
  • the refrigerant flow 33 is almost completely evaporated in the high-pressure column top condenser, only a relatively small amount, required for rinsing and regulating, is removed in liquid form.
  • the vapor 43 generated in the evaporation space of the high-pressure column overhead condenser 29 is introduced directly into the bottom region of the low-pressure column 30.
  • the liquid remaining fraction 44 from the evaporation space of the high-pressure column top condenser 29 is guided via a throttle valve 45 into the evaporation space of the low-pressure column top condenser 31.
  • the oxygen-enriched liquid 80 which accumulates in the bottom of the low-pressure column 30, is also introduced into the evaporation space of the low-pressure column top condenser 31 after being supercooled in the subcooling countercurrent 39 and throttling.
  • the top nitrogen 46 of the low-pressure column 30 is guided into the liquefaction space of the low-pressure column top condenser 31 and is substantially completely liquefied there.
  • the liquid obtained in the sump of the high-pressure column 28 is fed as liquid crude oxygen stream 41 via the subcooling countercurrent 39 and a throttle valve 42 into the evaporation chamber of the low-pressure column top condenser 31, which is under a pressure of 1.4 to 1.6 bar.
  • the cold gas from the low pressure column top condenser 31 is first passed through the subcooling countercurrent 39 thereby cooling the liquids. Thereafter, it flows via lines 56 and 57 to the main heat exchanger and cools the warm air streams there. Via line 62 and the low-pressure column top condenser 31 is flushed by a small amount of liquid (purge) is removed.
  • the residual gas 57/58 (Waste / Reg gas) is discharged in hot directly (60) or indirectly (61) after use as a regeneration gas 59 in the cleaning device 5 in the environment (amb).
  • the liquid 47 from the liquefaction space of the low-pressure column top condenser 31 is returned to a first part 48 as reflux to the first Low pressure column 30 abandoned.
  • the residue 49, 51 is available at a pressure of more than 3 bar as a liquid nitrogen product (LlN to storage) and is stored in a liquid tank, not shown.
  • By throttling 53 a small subset 52 it is possible to subcool the liquid nitrogen 49, 51 in a nitrogen subcooler 50.
  • the thereby evaporated nitrogen 54 is mixed with the residual gas 56 from the low-pressure column top condenser 31 (Waste).
  • a small amount of the top gas 35 of the high-pressure column 28 can be obtained as compressed nitrogen product 63, 64 in gaseous form.
  • This fraction (PGAN) from the high-pressure column 28 is also passed through the main heat exchanger 19 and helps to cool the warm air streams.
  • the throttling flow 21 in the throttle valve 232 is initially only expanded up to the operating pressure of the high-pressure column 28 and fed to it at an intermediate point. In the high pressure column, a phase separation takes place. At least a portion of the liquid portion of the expanded throttle flow is then introduced as refrigerant stream 270, 233 into the evaporation space of the high-pressure column top condenser after corresponding further throttling 271. The gaseous portion of the throttle flow 21 is thus available as ascending vapor in the high-pressure column 28.
  • FIGS. 3 to 7 various circuits of the refrigeration system are shown, each with in the FIGS. 1 and 2 described distillation column systems can be combined.
  • FIG. 3 represents only an enlarged detail of FIG. 1
  • This variant has the advantage that the warm turbine 26 is relaxed by a particularly high pressure (the high pressure under which the throttle flow 21 is also located) and correspondingly higher temperature. Pre-cooling of the second turbine stream 18 in the main heat exchanger 19 is not required in this case. It takes no line from the main heat exchanger 19 to the hot turbine 26, the heat exchanger is simple and inexpensive to manufacture.
  • the inlet pressure of the second (warm) turbine 26 is lower and is at the level of the intermediate pressure.
  • the second turbine stream 518 is already branched off upstream of the two secondary compressors 12, 14 from the circulating stream 11 compressed to the intermediate pressure, precooled in the main heat exchanger 19 and finally fed to the turbine 26.
  • the main heat exchanger 19 is additionally cooled by a refrigerator 666.
  • a chiller can also in the variant of FIG. 4 be supplemented.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
EP10013337A 2009-10-09 2010-10-05 Procédé et dispositif de production d'azote liquide par décomposition de l'air à basse température Withdrawn EP2312247A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP10013337A EP2312247A1 (fr) 2009-10-09 2010-10-05 Procédé et dispositif de production d'azote liquide par décomposition de l'air à basse température

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EP09012802 2009-10-09
EP10013337A EP2312247A1 (fr) 2009-10-09 2010-10-05 Procédé et dispositif de production d'azote liquide par décomposition de l'air à basse température

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US (1) US20110083469A1 (fr)
EP (1) EP2312247A1 (fr)
CN (1) CN102042742A (fr)
BR (1) BRPI1003929A2 (fr)
MX (1) MX2010011008A (fr)
RU (1) RU2540032C2 (fr)

Cited By (2)

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DE102013019504A1 (de) 2013-11-21 2015-05-21 Linde Aktiengesellschaft Verfahren zur Gewinnung eines flüssigen Stickstoffprodukts durch Tieftemperaturzerlegung von Luft und Luftzerlegungsanlage
EP3290843A3 (fr) * 2016-07-12 2018-06-13 Linde Aktiengesellschaft Procédé et dispositif destiné à fabriquer de l'azote pressurisé et liquide par décomposition à basse température de l'air

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CN104048478B (zh) * 2014-06-23 2016-03-30 浙江大川空分设备有限公司 高提取率和低能耗污氮气提纯氮气的设备及其提取方法
EP2963371B1 (fr) * 2014-07-05 2018-05-02 Linde Aktiengesellschaft Procede et dispositif de production d'un produit de gaz sous pression par decomposition a basse temperature d'air
CN109028759A (zh) * 2018-07-12 2018-12-18 北京拓首能源科技股份有限公司 一种利用液化天然气冷能的冷媒循环系统

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DE1145649B (de) * 1959-11-17 1963-03-21 Linde Eismasch Ag Verfahren zur Tieftemperaturgaszerlegung mit grossem Kaeltebedarf
US4448595A (en) * 1982-12-02 1984-05-15 Union Carbide Corporation Split column multiple condenser-reboiler air separation process
US4715873A (en) * 1986-04-24 1987-12-29 Air Products And Chemicals, Inc. Liquefied gases using an air recycle liquefier
EP0316768A2 (fr) 1987-11-13 1989-05-24 Linde Aktiengesellschaft Procédé de séparation d'air par rectification à basse température
US5144808A (en) * 1991-02-12 1992-09-08 Liquid Air Engineering Corporation Cryogenic air separation process and apparatus
US5660059A (en) 1995-07-06 1997-08-26 The Boc Group Plc Air separation
US5906113A (en) * 1998-04-08 1999-05-25 Praxair Technology, Inc. Serial column cryogenic rectification system for producing high purity nitrogen
US6499312B1 (en) 2001-12-04 2002-12-31 Praxair Technology, Inc. Cryogenic rectification system for producing high purity nitrogen
DE102004046344A1 (de) 2004-09-24 2006-03-30 Linde Ag Verfahren und Vorrichtung zur Tieftemperatur-Zerlegung von Luft
WO2009095188A2 (fr) * 2008-01-28 2009-08-06 Linde Aktiengesellschaft Procédé et dispositif de séparation de l'air à basse température

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013019504A1 (de) 2013-11-21 2015-05-21 Linde Aktiengesellschaft Verfahren zur Gewinnung eines flüssigen Stickstoffprodukts durch Tieftemperaturzerlegung von Luft und Luftzerlegungsanlage
EP3290843A3 (fr) * 2016-07-12 2018-06-13 Linde Aktiengesellschaft Procédé et dispositif destiné à fabriquer de l'azote pressurisé et liquide par décomposition à basse température de l'air

Also Published As

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BRPI1003929A2 (pt) 2013-02-13
RU2010141520A (ru) 2012-04-20
RU2540032C2 (ru) 2015-01-27
MX2010011008A (es) 2011-04-20
US20110083469A1 (en) 2011-04-14
CN102042742A (zh) 2011-05-04

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