EP3133361A1 - Systeme de colonnes de distillation et installation de production d'oxygene par separation cryogenique de l'air - Google Patents

Systeme de colonnes de distillation et installation de production d'oxygene par separation cryogenique de l'air Download PDF

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Publication number
EP3133361A1
EP3133361A1 EP16001736.4A EP16001736A EP3133361A1 EP 3133361 A1 EP3133361 A1 EP 3133361A1 EP 16001736 A EP16001736 A EP 16001736A EP 3133361 A1 EP3133361 A1 EP 3133361A1
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Prior art keywords
column
mass transfer
argon
condenser
space
Prior art date
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Granted
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EP16001736.4A
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German (de)
English (en)
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EP3133361B1 (fr
Inventor
Dimitri Goloubev
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Linde GmbH
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Linde GmbH
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Publication of EP3133361A1 publication Critical patent/EP3133361A1/fr
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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
    • 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
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    • 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
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
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    • F25J3/0228—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 characterised by the separated product stream
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    • F25J3/04084—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 nitrogen
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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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    • F25J3/04703—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser being arranged in more than one vessel
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Definitions

  • the invention relates to a distillation column system for the production of oxygen by cryogenic separation of air according to the preamble of patent claim 1.
  • the distillation column system of the invention can basically be designed as a classic two-column system with high-pressure column and low-pressure column. In addition to the two separation columns for nitrogen-oxygen separation, it can have other devices for obtaining other air components, in particular noble gases, for example krypton-xenon recovery.
  • the main capacitor is formed in the invention as a condenser-evaporator.
  • condenser-evaporator refers to a heat exchanger in which a first condensing fluid stream undergoes indirect heat exchange with a second evaporating fluid stream.
  • Each condenser-evaporator has a liquefaction space and an evaporation space, which consist of liquefaction passages or evaporation passages. In the liquefaction space, the condensation (liquefaction) of the first fluid flow is performed, in the evaporation space the evaporation of the second fluid flow. Evaporation and liquefaction space are formed by groups of passages that are in heat exchange relationship with each other.
  • argon discharge column here refers to an argon-oxygen separation column which serves not to extract a pure argon product but to remove argon from the air, which is separated into high-pressure column and low-pressure column.
  • Their circuit differs only slightly from that of a classical crude argon column, which generally has 70 to 180 theoretical plates; however, it contains significantly less theoretical plates, namely less than 40, in particular between 15 and 35.
  • the bottom portion of an argon discharge column is connected to an intermediate point of the low pressure column, and the argon discharge column is usually cooled by a top condenser and relaxed bottoms liquid on its evaporation side the high-pressure column is introduced; an argon discharge column generally has no bottom evaporator.
  • argon column is used here as a generic term for argon discharge columns, full-quality crude argon columns and all transitions in between.
  • the distillation column system of an air separation plant is arranged in one or more cold boxes.
  • a "cold box” is here understood to mean an insulating casing which comprises a heat-insulated interior completely with outer walls; in the interior to be isolated plant parts are arranged, for example, one or more separation columns and / or heat exchangers.
  • the insulating effect can be effected by appropriate design of the outer walls and / or by the filling of the gap between system parts and outer walls with an insulating material. In the latter variant, a powdery material such as perlite is preferably used.
  • Both the distillation column system for nitrogen-oxygen separation of a cryogenic air separation plant and the main heat exchanger and other cold plant parts must be enclosed by one or more cold boxes.
  • the outer dimensions of the coldbox usually determine the transport dimensions of the package in prefabricated systems.
  • a "main heat exchanger” serves to cool feed air in indirect heat exchange with recycle streams from the distillation column system. It may be formed from a single or multiple parallel and / or serially connected heat exchanger sections, for example one or more plate heat exchanger blocks. Separate heat exchangers which specifically serve to vaporize or pseudo-evaporate a single liquid or supercritical fluid without heating and / or vaporization of another fluid, do not belong to the main heat exchanger. Such a separate heat exchanger can be formed for example by a secondary condenser or by a separate heat exchanger for the evaporation or pseudo-evaporation of a liquid stream under elevated pressure.
  • some air separation plants include, in addition to the main heat exchanger, a secondary condenser or a high pressure exchanger for vaporization or pseudo-vaporization of liquid pressurized product against a high pressure air stream formed by a portion of the feed air.
  • top, bottom, above, bottom, aboveve, bottom, aboveve, below, “above”, “below”, verticalically”, “horizontally”, etc. refer here to the spatial orientation of the apparatuses in normal operation.
  • a distillation column system of the type mentioned is out US 5235816 known. Such systems are prefabricated regularly as far as possible during production, the prefabricated parts are transported to the site and finally connected there. Depending on the size of the system, for example, the entire double column can be transported with its coldbox. If the size of the system no longer allows this, the double column - if necessary in two parts - is transported without coldbox and piping. An additional column such as the argon column causes additional effort with its own coldbox. This column is brought separately to the site and connected there with relatively great effort on site with the rest of the system. In order to avoid an additional cryogenic pump, this column is placed (in its own cold box) on an elaborate frame. Among other things, this frame causes increased footprint for the entire plant ("plant footprint").
  • an argon column is disclosed, which is installed in the low-pressure column and whose top condenser is arranged outside the low-pressure column.
  • the invention has for its object to make a distillation column system of the type mentioned as compact as possible to simplify its structure and to find a particularly reliable control method.
  • the argon column overhead condenser is placed inside the low pressure column.
  • the argon discharge column head condenser is designed as a forced-flow (once-through) evaporator; at its upper end, the evaporation space is connected to the interior of the low-pressure column, so that the gas generated there can flow into the upper mass transfer region.
  • the argon column head condenser need not be arranged centrally above the argon column (if the argon column is completely or partially installed in the low pressure column), but the entire cross section of the low pressure column can be used.
  • a liquid flow is forced through its own pressure through the evaporation space where it partially evaporates.
  • This pressure is generated for example by a liquid column in the supply line to the evaporation chamber.
  • the height of this liquid column corresponds to the pressure loss in the evaporation chamber.
  • the gas-liquid mixture emerging from the evaporation space is passed on directly to the next process step after phases and in particular is not introduced into a liquid bath of the condenser-evaporator, from which the liquid remaining portion would be sucked in again ("once through").
  • a liquid is partially evaporated.
  • the effluent two-phase mixture is preferably introduced into a liquid distributor at the top of the central mass transfer region.
  • the vaporized portion flows upward in the upper mass transfer region, the liquid remaining portion forms at least part of the return for at least a portion of the central mass transfer region, which in particular forms the argon portion of the low pressure column.
  • the forced-flow evaporator could be operated exclusively with the crude oxygen from the high-pressure column, as in conventional argon processes.
  • it has proved to be more favorable to pressurize the evaporation space of the argon column overhead condenser with a liquid which originates from the upper mass transfer region of the low-pressure column.
  • the liquid collector below the upper mass transfer region is connected to means for introducing liquid from the liquid collector via the inlet into the evaporation space of the argon column overhead condenser.
  • Liquid draining from the upper mass transfer section is combined in the liquid receiver and, for example, introduced via a line into the evaporation chamber of the argon column overhead condenser.
  • the liquid thus serves to cool the head of the argon column. It is oxygen-rich than the crude oxygen from the high-pressure column and thus allows a lower temperature difference and correspondingly lower thermodynamic losses in the argon column overhead condenser.
  • control method 3 the two-phase mixture is introduced from the evaporation space of the argon condenser in a container which acts as a phase separator and liquid buffer.
  • the deposited in the container liquid is passed into the underlying liquid distributor.
  • the amount of liquid is controlled by means of a fixed aperture or corresponding hole in the bottom of the container or by means of a control valve in the liquid line.
  • Gas is withdrawn from the tank via a gas line. It contains a control valve, via which the pressure in the evaporation space is adjusted, thus the temperature difference in the argon condenser and thus its achievement.
  • top condenser is as conventional bath evaporator formed and arranged to a first part in the low pressure column.
  • another container for the second part of the top condenser is used here.
  • the argon condenser is designed to produce all the reflux for the argon column. There is therefore no further argon condenser which would be arranged outside the low-pressure column.
  • the argon column is designed as Argonausschleuskla.
  • an argon product may also be formed as a crude argon column, at the head of which an oxygen-depleted or oxygen-free crude argon product is recovered.
  • the crude argon product is either removed or fed to further workup in a pure argon column.
  • the argon column or a part of it is arranged within the low-pressure column, in the middle mass transfer area.
  • this is designed as a partition wall section, that is, it contains a vertical partition which separates the argon section of the low pressure column ("first mass transfer space") from the argon column (“second mass transfer space”).
  • the first mass transfer space is open at the top to the top mass transfer area and down to the bottom mass transfer area. "This means that ascending gas can flow down into the first mass transfer space without significant obstruction and flow up out of the first mass transfer space.
  • the second mass transfer space is gas-tight at the top towards the upper mass transfer area.
  • the gas flowing in from below from the lower mass transfer region is therefore not reintroduced into the low pressure column after rectification in the second mass transfer space (in the argon column) but is continued via one or more special gas lines and / or introduced into the liquefaction space of the argon column overhead condenser.
  • the argon column also has a separate crude argon column, which is outside the low pressure column.
  • the second mass transfer space is open at the bottom to the lower mass transfer region.
  • the rising gas from the lower mass transfer area thus flows into the second mass transfer and is there subjected to an argon-oxygen separation.
  • the second mass transfer space is closed down to the lower mass transfer area, so that a different concentration can prevail in the lower area of the second mass transfer space than at the upper end of the lower mass transfer area.
  • the rectificatively seen "upper" part of an argon column can be installed in the partition section, while the rest of the argon column, which is connected at the lower end to the low-pressure column, is realized separately.
  • argon column For a full argon production, a separate crude argon column can be added.
  • the argon column then consists of the combination of crude argon column and second mass transfer space, wherein the second mass transfer space can be rectificatively connected to the upper or the lower end of the crude argon column.
  • the head of the argon column is in fluid communication with the liquefaction space of the argon column overhead condenser.
  • the argon column is formed exclusively by a separate crude argon column. This is then connected in a conventional manner, in that the head of the argon column is in flow connection with the liquefaction space of the argon column overhead condenser and the bottom of the argon column is in fluid communication with an intermediate region of the low pressure column, in particular with the area between the middle and lower mass transfer region.
  • a crude oxygen line for the introduction of raw oxygen from the bottom of the high-pressure column is provided in the upper mass transfer region of the low-pressure column;
  • the raw oxygen can be fed directly into the liquid receiver before the evaporation chamber.
  • this - customary - introduction of bottom liquid from the high-pressure column into the low-pressure column is not conducted via the argon column overhead condenser, but directly into the upper mass transfer region.
  • the liquid which is introduced into the evaporation space of the argon column overhead condenser is thus more oxygen-rich than in the conventional method, because here the liquid collected under the upper section is used.
  • the distillation column system includes a bypass line for introducing liquid from the liquid receiver located below the top mass transfer section into the liquid distributor at the top of the lower mass transfer section, with a control valve disposed in the bypass line.
  • this bypass line can be controlled outside the invention, the performance of the argon column head capacitor.
  • the control valve is opened, a small amount of nitrogen-richer fluid flows directly into the manifold, bypassing the central mass transfer section.
  • the nitrogen content in the liquefaction space of the argon overhead condenser increases, the average condensation temperature decreases and the capacity of the condenser is reduced by reducing the driving temperature difference (control method 1).
  • the conversion in the crude argon column could also be regulated by means of a valve in the gas stream upstream of the crude argon condenser.
  • a gas supply line for the introduction of gas from the argon column is used in the liquefaction space of the argon column overhead condenser, which contains a control valve.
  • the gas supply line immediately downstream of the control valve may be connected to a starting line, which is designed for the controlled discharge of gas from the low-pressure column.
  • the start-up line is connected to the gas supply line outside the container wall and is only used when the system is cold-running. It complies with a control valve, which is closed in stationary operation. When starting up, care must be taken to ensure that the mass transfer chambers are cooled uniformly on both sides of the partition wall. Large temperature differences between these two sections should be avoided in order to minimize the stress on the partition caused by thermally induced stresses.
  • the startup line either goes outdoors or is integrated into a non-nitrogen line in front of the main heat exchanger. Depending on the temperature to the right and left of the partition, the control valve is opened more or less when starting.
  • the starting line is integrated directly into the gas supply line after the control valve for the argon column overhead condenser - ie outside the column.
  • This starting technique can be used not only in the invention, but in principle at the dividing wall column section with overlying capacitor.
  • the invention also relates to a plant for the production of oxygen by cryogenic separation of air according to claims 8 to 12 with a main air compressor, an air pre-cooling unit, an air purification unit and a main heat exchanger and with two of the above-described distillation column systems, both receiving feed air from the common main heat exchanger.
  • At least a portion of the feed air for both distillation column systems can be cooled together in the main heat exchanger and withdrawn from the main heat exchanger in a total compressed air line.
  • the total compressed air line is then branched into the first compressed air sub-flow line to the first distillation column system and the second compressed air sub-flow line to the second distillation column system.
  • the two compressed air partial flow lines are connected directly to the main heat exchanger.
  • a system according to the invention has a high-pressure exchanger in addition to the main heat exchanger, then this is likewise used for both distillation column systems, ie the high-pressure cold air from the high-pressure exchanger is distributed to the two distillation column systems and the product stream intended for the high-pressure exchanger becomes liquid from both distillation columns -Systems removed, merged and sent to the high pressure exchanger.
  • the main heat exchanger usually consists anyway of several parallel blocks. Then it is advisable to divide the blocks into two symmetrical groups in order to better control the main heat exchanger.
  • the air to be separated in the first distillation column system and the corresponding stream of impure nitrogen are passed out of the same distillation column system.
  • the second group the respective streams flow to and from the second distillation column system. The remaining streams (product or turbine streams) are distributed evenly over the blocks of both groups.
  • the apparatuses upstream and downstream of the two distillation column systems may in particular be formed by a single pre-cooling, a single air purification and / or a single main heat exchanger.
  • the first distillation column system and the second distillation column system have the same size and in particular high-pressure column, low pressure column and argon column are the same size.
  • a “same size” is understood here that the corresponding column heights and diameters not more than 10%, in particular not more than 5% diverge.
  • the comparison relates in pairs to the corresponding sections of the first and second high-pressure columns, the first and the second low-pressure columns and the argon columns.
  • the two distillation column systems can each be housed in a separate coldbox.
  • the first and second distillation column systems are arranged in a common coldbox.
  • the two distillation column systems are operated independently.
  • the warm parts of the plant and the main heat exchanger and optionally a high-pressure exchanger are shared, for example.
  • each of the two distillation column systems has its own main heat exchanger and optionally its own high pressure heat exchanger.
  • both distillation column systems each have a separate subcooling countercurrent which is operable independently of the subcooling countercurrent of the other distillation column system, and in particular is not connected to piping to or from the other distillation column system.
  • the invention also relates to a method for recovering oxygen by cryogenic decomposition of air according to claims 13 to 15.
  • the method according to the invention can be supplemented by method features which correspond to the characteristics of individual, several or all dependent device claims.
  • FIG. 1 is to see a plant with a single distillation column system.
  • the construction of the low-pressure column of this distillation column system is described in detail in FIG FIG. 6 (some of the below-mentioned reference numerals are given only there).
  • the distillation column system of the embodiment of the FIG. 1 has a high pressure column 101, a low pressure column 102, a main condenser 103 and an argon column 152.
  • the main capacitor 103 is formed in the example by a three-stage cascade evaporator, so a multi-level pocket evaporator.
  • the Pair of columns 101/102 is arranged in the form of a double column.
  • the argon column 152 is arranged in a central mass transfer region 130 of the low-pressure column 102.
  • the argon column overhead condenser 155 sits in the interior of the low-pressure column 102 above the central mass transfer area 130.
  • the low-pressure column 102 also has an upper mass transfer area 131 and a lower mass transfer area 132 (see in particular FIG. 6 ).
  • the system shown has an atmospheric air inlet filter 302, a main air compressor 303, an air pre-cooling unit 304, an air cleaning unit 305 (typically formed by a pair of molecular sieve adsorbers), a Booster Air Compressor 306 with aftercooler 307, and a main heat exchanger 308.
  • the main heat exchanger 308 is housed in its own cold box, which is separated from the cold box by the distillation column system. A total compressed air flow 100 from the cold end of the main heat exchanger 308 is introduced into the high pressure column 101.
  • the air recompressed in the final compressor 306 to its final pressure is liquefied in the main heat exchanger 308 (or, if its pressure is supercritical, pseudo-liquefied) and fed via lines 311/111 to the distillation column system.
  • a nitrogen gas stream 104, 114 from the high-pressure column 101 is introduced into the liquefaction space of the main condenser 103.
  • liquid nitrogen 115 is generated therefrom, which is passed to at least a first part as a first liquid nitrogen stream 105 to the first high-pressure column 101.
  • a liquid oxygen stream 106 from the low-pressure column 102 flows from the lower end of the lowermost mass transfer layer 107 of the low-pressure column 102 and is thereby introduced into the evaporation space of the main condenser 103.
  • gaseous oxygen is formed in the evaporation space of the main condenser 103. It is introduced at least to a first part in the first low-pressure column 102 by flowing from below into the bottom mass transfer layer 107 of the low-pressure column 102; if necessary, a second part can be obtained directly as gaseous oxygen product and heated in the main heat exchanger 308 (not realized in this embodiment).
  • the reflux liquid 109 for the low pressure column 102 is formed by a nitrogen-enriched liquid 120 which is withdrawn at the high pressure column 101 from an intermediate point (or alternatively directly from the top) and cooled in a subcooling countercurrent 123. From the top of the low-pressure column 102, impure nitrogen 110 is withdrawn and fed as residual gas through the subcooling countercurrent 123 and via the line 32 to the main heat exchanger 308.
  • an oxygen-enriched bottoms liquid stream 151 is withdrawn and cooled in the subcooling countercurrent 123.
  • the entire cooled bottoms liquid 153 is fed to the upper mass transfer region of the low pressure column 102. It flows into the bottom section of the upper mass transfer zone together with the return liquid from above.
  • the effluent from this section liquid is collected by a liquid collector 133 and introduced into the evaporation space of the argon column overhead condenser 155.
  • the argon column overhead condenser 155 is embodied here according to the invention as a forced-flow evaporator.
  • the fraction evaporated in the top condenser 155 flows back into the top mass transfer region 131 and the liquid remaining fraction 157 is fed into the central mass transfer region 130 of the low-pressure column 102.
  • the argon-enriched "product" 163 of the argon column is removed in gaseous form from the argon column 152 or its top condenser 155 and passed via line 164 through a separate passage group through the main heat exchanger 308.
  • the argon-enriched fraction 163 could be mixed with the impure nitrogen and the mixture passed through the main heat exchanger.
  • the liquid air 111 from the main heat exchanger is supplied via the line 111 to the high-pressure column 101 at an intermediate point. At least a portion 127 is removed again immediately and introduced through the subcooler 123 and via the line 128 in the upper mass transfer region of the low-pressure column 102, above the feed of the sump fraction 153. Via line 129 is also gaseous air from a Einblaseturbine 137 in the low-pressure column 102, at the same level as the crude oxygen 153.
  • liquid oxygen 141 is withdrawn from the evaporation space of the main condenser 103 and fed via line 14 at least partially to an internal compression.
  • the liquid oxygen 14 is pumped by a pump 15 to a high product pressure, vaporized under this high product pressure in the main heat exchanger 308 or (if its pressure is supercritical) pseudo-evaporated, warmed to about ambient temperature and finally withdrawn as gaseous pressure oxygen product GOXIC.
  • pressurized nitrogen is withdrawn directly from the top of the high-pressure column 101 (lines 104, 142), passed via line 42 to the main heat exchanger 308, warmed there and finally recovered as gaseous pressure nitrogen product MPGAN. Part of it can be used as sealing gas (seal gas).
  • a portion 143 of the liquid nitrogen produced in the main condenser 103 is supplied via line 43 to an internal compression (pump 16) and recovered as gaseous high pressure nitrogen product GANIC.
  • the plant can also supply liquid products LOX, LIN.
  • the mass transfer elements in the low-pressure column 102 are formed exclusively by ordered packing.
  • the oxygen section 107 of the low-pressure column 102 is provided with an ordered packing having a specific surface area of 750 m 2 / m 3 or alternatively 1200 m 2 / m 3 , in the remaining sections the packing has a specific surface area of 750 or 500 m 2 / m 3 on.
  • the low-pressure column 102 may have a nitrogen section above the mass transfer areas shown in the drawing; this can then also be equipped with a particularly dense packing (for example with a specific surface area of 1200 m 2 / m 3 for the purpose of reducing the height of the column).
  • the argon column 152 in the exemplary embodiment contains exclusively pack with a specific surface area of 1200 m 2 / m 3 or alternatively 750 m 2 / m 3 .
  • the mass transfer elements exclusively by ordered packing with a specific surface area of 1200 m 2 / m 3 or 750 m 2 / m 3 educated.
  • at least a portion of the mass transfer elements in the high pressure column 101 could be formed by conventional distillation trays, for example through sieve trays.
  • the system of FIG. 1 is designed as a two-turbine method with a medium-pressure turbine 138 and an injection turbine 137.
  • FIG. 2 is different from this FIG. 1 in that it is designed as a single-turbine system. It has only one injection turbine but no mid-pressure turbine.
  • FIG. 3 is almost identical to FIG. 2 but has a pressure nitrogen turbine 337 instead of the injection turbine. It is operated with a part 342 of the pressurized nitrogen 142, which is withdrawn in gaseous form from the top of the high-pressure column 101.
  • the turbine stream 442 is withdrawn from an intermediate point of the high-pressure column 101 and expanded work in a non-nitrogen nitrogen turbine 437.
  • FIG. 5 a plant with two distillation column systems is shown, which is designed according to the invention.
  • the first distillation column system of the embodiment of the FIG. 5 has a first high-pressure column 101, a first low-pressure column 102, a first main capacitor 103 and a first argon column 152.
  • a second high pressure column 201, a second low pressure column 202, a second main condenser 203 and a second argon column 252 belong to the second distillation column system of Figs FIG. 1 illustrated plant.
  • Both main capacitors 103, 203 are formed in the example by a three-stage cascade evaporator.
  • the pairs of columns 101/102, 201/202 are arranged in the form of two double columns.
  • the argon columns 152/252 are arranged in a central mass transfer region of the low-pressure columns 102, 202.
  • the argon column overhead condensers 155, 255 are located in the interior of the respective low-pressure column 102, 202 above the central mass transfer region 113, 213 and are formed according to the invention as a forced-flow evaporator.
  • the low-pressure columns 102, 202 also each have an upper mass transfer region above the argon column overhead condenser 155, 255 and a lower mass transfer region below the argon column 152/252 or the middle mass transfer region 113, 213, respectively.
  • the arrangement of the mass transfer areas in the low-pressure columns is in particular made FIG. 6 seen.
  • Each of the two distillation column systems is independently regulated.
  • the pressure in the low-pressure columns for example, can be set and controlled separately. Through this decoupling, the overall control effort is made easier and any manufacturing tolerances in both double columns can be better compensated.
  • the system shown has an atmospheric air inlet filter 302, a main air compressor 303, an air pre-cooling unit 304, an air cleaning unit 305 (typically formed by a pair of molecular sieve adsorbers), a Booster Air Compressor 306 with aftercooler 307, and a main heat exchanger 308.
  • the main heat exchanger 308 is housed in its own coldbox, which is separate from the coldbox (s) around the distillation column systems.
  • a total compressed air flow 99 from the cold end of the main heat exchanger 308 is branched into a first compressed air partial flow 100 and a second compressed air partial flow 200.
  • the first compressed air sub-stream 100 is introduced into the first high-pressure column 101, the second compressed air sub-stream 200 into the second high-pressure column 201.
  • the air recompressed in the secondary compressor 306 to its final pressure is liquefied in the main heat exchanger 308 (or, if its pressure is supercritical, pseudo-liquefied) and fed via line 311 to the distillation column systems where it is branched into the streams 111 and 112.
  • a first nitrogen gas stream 104, 114 from the first high-pressure column 101 is introduced into the liquefaction space of the first main condenser 103.
  • liquid nitrogen 115 becomes generated, which is passed to at least a first part as a first liquid nitrogen stream 105 to the first high-pressure column 101.
  • a second nitrogen gas stream 204, 214 from the second high-pressure column 201 is introduced into the liquefaction space of the second main condenser 203.
  • liquid nitrogen 215 is generated, which is conducted to at least a first part as a second liquid nitrogen flow 205 to the second high-pressure column 201.
  • a first liquid oxygen stream from the first low-pressure column 102 flows from the lower end of the lowermost mass transfer layer 107 of the first low-pressure column 102 and is thereby introduced into the evaporation space of the first main capacitor 103.
  • gaseous oxygen is formed in the evaporation space of the first main capacitor 103. It is introduced at least to a first part as the first oxygen gas stream in the first low-pressure column 102 by flowing from below into the bottom mass transfer layer 107 of the first low-pressure column 102; if necessary, a second part can be obtained directly as a gaseous oxygen product and heated in the main heat exchanger 308.
  • a second liquid oxygen stream from the second low-pressure column 202 flows from the lower end of the lowermost mass transfer layer 207 of the second low-pressure column 202 and is thereby introduced into the evaporation space of the second main condenser 203.
  • gaseous oxygen is formed in the evaporation space of the second main capacitor 203. It is introduced at least to a first part as a second oxygen gas stream in the second low-pressure column 202 by flowing from below into the bottom mass transfer layer 207 of the second low-pressure column 202; a second part can be obtained directly as a gaseous oxygen product if necessary and heated in the main heat exchanger 308 (not shown).
  • the reflux liquids 109, 209 for the two low-pressure columns 102, 202 are each formed by a nitrogen-enriched liquid 120, 220 withdrawn at both high-pressure columns 101, 201 from an intermediate point (or alternatively directly from the head) and cooled in subcooling countercurrents 123, 223 becomes. From the top of both low-pressure columns 102, 202, impure nitrogen 110, 210 is withdrawn and as residual gas through a respective subcooling countercurrent 123, 223 and guided via the common line 32 to the main heat exchanger 308.
  • an oxygen-enriched bottoms liquid stream 151, 251 is drawn off and cooled in the respective subcooling countercurrent 123, 223.
  • all of the cooled bottom liquid 153, 253 is fed to the top mass transfer region of the low pressure columns 102, 202. It flows into the bottom section of the upper mass transfer zone together with the return liquid from above.
  • the effluent from this section liquid is collected by a liquid collector 133, 233 and introduced into the evaporation space of the argon column overhead condenser 155, 255.
  • the argon column overhead condenser 155, 255 is embodied here according to the invention as a forced-flow evaporator.
  • the argon-enriched "product" 163, 263 of the argon column is removed in gaseous form from the argon column 152, 252 or its top condenser 155, 255 and passed via line 164 through a separate passage group through the main heat exchanger 308.
  • the argon-enriched fractions 163, 263 could be mixed with the impure nitrogen 110, 210 and the mixture passed through the main heat exchanger.
  • the liquid or supercritical air 311 from the main heat exchanger is fed via the lines 111, 211 to the high-pressure columns 101, 201 at an intermediate point. At least a portion 127, 227 is removed immediately and introduced through the subcooler 123, 323 and via the line 128, 228 in the upper mass transfer region of the low-pressure columns 102, 202, above the feed of the sump fraction 153, 253. Via line 129, 229, further, gaseous air from an injection turbine 137 is introduced into the low-pressure columns 102, 202 at the same height as the raw oxygen 153, 253.
  • liquid oxygen 141, 241 is withdrawn from the evaporation spaces of the main condensers 103, 203, combined and fed via line 14 at least partially to an internal compression.
  • the liquid oxygen 14 is pumped by a pump 15 to a high product pressure, vaporized under this high product pressure in the main heat exchanger 308 or (if its pressure is supercritical) pseudo-evaporated, warmed to about ambient temperature and finally withdrawn as gaseous pressure oxygen product GOXIC.
  • pressurized nitrogen is withdrawn directly from the head of the high-pressure columns 101, 201 (lines 104, 142 and 204, 242), together via line 42 to the main heat exchanger 308, where it is heated and finally recovered as gaseous compressed nitrogen product MPGAN. Part of it can be used as sealing gas (seal gas).
  • sealing gas sealing gas
  • a part 143, 243 of the liquid nitrogen produced in the main condensers 103, 203 is supplied via line 43 to an internal compression (pump 16) and recovered as gaseous high-pressure nitrogen product GANIC.
  • the plant can also supply liquid products LOX, LIN. These can be removed separately from each distillation column system as shown.
  • the mass transfer elements in the two low-pressure columns 102, 202 are formed exclusively by ordered packing.
  • the oxygen sections 107, 207 of the two low-pressure columns 102, 202 are provided with an ordered packing having a specific surface area of 750 m 2 / m 3 or alternatively 1200 m 2 / m 3 , in the remaining sections the packing has a specific surface of 750 or 500 m 2 / m 3 on.
  • the two low pressure columns 102, 202 may have a nitrogen section above the mass transfer areas shown in the drawing; this can then also be equipped with a particularly dense packing (for example with a specific surface area of 1200 m 2 / m 3 for the purpose of reducing the height of the column).
  • the argon columns 152, 252 contain in the embodiment only pack with a specific surface area of 1200 m 2 / m 3 or alternatively 750 m 2 / m 3 .
  • the mass transfer elements are formed exclusively by ordered packing with a specific surface area of 1200 m 2 / m 3 or 750 m 2 / m 3 .
  • at least a portion of the mass transfer elements could be formed in one or both high pressure columns 101, 201 by conventional distillation trays, for example through sieve trays.
  • FIG. 5 is analogous to FIG. 1 is formed as a two-turbine method with a medium-pressure turbine 138 and an injection turbine 137.
  • FIG. 5 which has two distillation column systems, including the turbine configurations of Figures 2 . 3 or 4 be used
  • Each of the two distillation column systems is independently regulated.
  • the pressure in the low-pressure columns for example, can be set and controlled separately. Through this decoupling, the overall control effort is made easier and any manufacturing tolerances in both double columns can be better compensated.
  • FIG. 6 only a section of the double column 101, 102 is shown, which extends from the upper end of the high-pressure column 101 to the second packing layer of the upper mass transfer region 131 of the low-pressure column and contains in particular the argon column 152 and the argon column overhead condenser 155.
  • the embodiment of the FIG. 6 be used in other two-column systems, for example, those with arrangement of the low-pressure column next to the high-pressure column and / or arrangement of the main capacitor outside the low-pressure column.
  • liquid oxygen is evaporated, which runs out of the lower mass transfer region 132 or from the bath 65 in FIG Sump of the low pressure column is sucked; in countercurrent thereto, gaseous nitrogen is vaporized from the top of the high-pressure column 101. (The nitrogen pipes are in FIG. 6 not shown.)
  • the liquid collectors and distributors are in FIG. 6 not shown except for the collector 133 between the upper mass transfer region 131 and the argon column overhead condenser 155, the two liquid distributors 44, 420 at the head of the first and second mass transfer chambers 134, 135 and the liquid distributor 45 at the top of the lower mass transfer section 132.
  • the rest is FIG. 6 very schematic and usually not to scale.
  • the middle mass transfer region 130 of the low-pressure column is subdivided in a first gas-tight manner into a first mass transfer space 134 and a second mass transfer space 135 by a vertical planar partition wall 136.
  • the first mass transfer space 134 is open at the top to the upper mass transfer area 131 and down to the lower mass transfer area 132, that is gas from the lower mass transfer area 132 can flow into the first mass transfer space 134 of the central mass transfer area 131, and gas from the first mass transfer space 134 can be upwardly in drain off the upper mass transfer area of the low pressure column.
  • the first mass transfer space 134 fulfills the function of the argon section of the low-pressure column, that is to say the mass transfer area which, in a conventional plant, is located directly above the argon transition via which an argon-containing fraction would be passed to an external crude argon column or argon column.
  • the second mass transfer space 135 forming the argon column 152 is also open at the bottom to the bottom mass transfer area 132; Ascending gas flows from the lower mass transfer region 132 of the low-pressure column into the second mass transfer space 135. At its upper side, however, the second mass transfer space 135 is closed gas-tight to the upper mass transfer area 131.
  • the conclusion upwards is effected by a horizontal plate 36, which - except for the performed lines 37, 37, 41 - is gas-tight.
  • the argon column overhead condenser 155 which is designed as a condenser-evaporator, is located here according to the invention as a forced-flow evaporator.
  • the liquefaction space of the argon column overhead condenser 155 is in fluid communication with the head of the argon column 152 via the gas conduit 37 and the liquid conduits 62, 41.
  • overhead gas of the argon column 152 flows via the gas line 37 from the upper end of the second mass transfer space 135 into the liquefaction space and is at least partially liquefied there.
  • the liquid thus produced is withdrawn via line 62, returned via the line 41 into the second mass transfer space 135 and distributed by means of a liquid distributor 420 as reflux liquid of the argon column over the cross section of the second mass transfer space 135.
  • the gaseous remaining portion 163 is withdrawn from the container of the low-pressure column 102 and further as in the FIGS. 1 to 5 shown treated.
  • the effluent from the two mass transfer chambers 134, 135 of the central mass transfer region 130 liquid is collected in a liquid collector, not shown.
  • the liquid continues to flow to the liquid distributor 45, which distributes it over the entire column cross-section and gives up on the lower mass transfer region 132.
  • the crude oxygen 153 from the bottom of the high-pressure column 101 is - similar to in FIG. 1 - Introduced between two packing sections of the upper mass transfer region 131. At the same point, an air flow 129 is introduced, which has previously been expanded to approximately low-pressure column pressure to perform work (see injection turbines 137 in the FIGS. 1 . 2 and 5 ).
  • a two-phase mixture exits via line 73.
  • the liquid portion L flows into the liquid distributor 44 at the top of the first mass transfer space 134.
  • the vaporized portion V flows back up into the upper mass transfer portion 131.
  • the control of the argon column head capacitor 155 is carried out in the embodiment of FIG. 6 with a control method 1, for which a bypass line 49/50 and a control valve 48 are needed. Thereby, the performance of the argon column overhead condenser 155 is controlled.
  • a small amount of relatively nitrogen-rich liquid flows into the manifold 45 and increases the nitrogen content in the vapor rising from the lower section 132 and thus also in the entire argon column 152 and further in the liquefaction space of the argon column overhead condenser 155 arranged valve a controlled reduction of the power of the capacitor.
  • the relatively nitrogen-rich liquid comes in the embodiment of the collector 133 at the lower end of the upper mass transfer area 131st
  • the control valve 48 is closed in stationary operation, or it flows only a very small amount of liquid. In the event of deviations from stationary operation, for example during a load change, less than 5% of the total liquid 71/49 flows out of the liquid collector 133 via the bypass line, in any case less than 15%.
  • control methods may be used, one of which will be described in more detail below.
  • FIG. 7 shows an alternative control method 2 with a control valve 700 in the gas supply line 37 to the liquefaction space of the argon column overhead condenser 155.
  • the condensation pressure can be adjusted with appropriate condensation temperature. This directly influences the driving temperature difference in the condenser 155 and correspondingly also the condenser performance or the conversion in the argon column 152.
  • a rule method 3 is in FIG. 12 shown.
  • the two-phase mixture from the evaporation space of the argon condenser 155 is introduced into an additional container 1250.
  • the gaseous portion V is returned to the low-pressure column so that it is available as ascending vapor in the upper mass transfer section 131.
  • the liquid portion L is introduced via line 1254 into the liquid distributor 44 at the top of the first mass transfer space 134 (the argon portion).
  • a control valve 1252 By means of a control valve 1252, the pressure in the evaporation space of the argon capacitor 155 and thus its performance can be adjusted.
  • the liquid line 1254 may also include a control valve.
  • the liquid flow is controlled by a fixed orifice, for example in the form of an opening in the bottom of the container 1250. This must be dimensioned so that the liquid level in the container will move within the upper and lower container limits depending on the pressure in the container.
  • FIG. 9 based on FIG. 2 but has a complete argon recovery, in which the oxygen content in the overhead product 963 of the argon column is reduced to, for example, 0.1 to 100 ppm.
  • the largely oxygen-free Argon gas 963 is then fed to a pure argon column in which an argon nitrogen separation is performed.
  • the few theoretical plates in the partition section 135 are not sufficient. Therefore, a crude argon column 900 of almost usual length is used, and the second mass transfer space 135 in the partition wall portion of the low pressure column 102 is used as the top mass transfer region of the crude argon rectification.
  • the second mass transfer space 135 must be sealed gas-tight on its underside, for example by a semicircular plate Below this plate argon-containing gas 901 is withdrawn from the low pressure column 102 and fed to the bottom of the crude argon column 900.
  • the bottom liquid 902 of the crude argon column 900 is returned in the opposite direction to the same location of the low-pressure column 102.
  • the top of the crude argon column is in fluid communication with the lower end of the second mass transfer space 135 via conduits 903 (for gas) and 904 (for liquid). Its upper end is as shown in Figs FIGS. 1 to 7 known to be connected to argon column overhead condenser 155.
  • the second mass transfer space 135 is open at the bottom and is analogous to the FIGS. 1 to 5 operated. However, its head is not directly connected to the argon top condenser 155, but via lines 905 and 906 to the bottom of the crude argon column 900.
  • the top of the crude argon column is in fluid communication with the liquefaction space of the argon column top condenser via lines 907 and 908.
  • FIG. 11 shows an embodiment without partition wall section in the low pressure column.
  • the argon column here consists exclusively of the separate Rohargonklave 900 whose head analogous to FIG. 10 is connected to the argon column overhead condenser 155 (907, 908).
  • the sump of the crude argon column 900 of FIG. 11 is analogous to FIG. 9 connected to a corresponding intermediate point of the low-pressure column 102 (901, 902).

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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)
EP16001736.4A 2015-08-20 2016-08-04 Systeme de colonnes de distillation et installation de production d'oxygene par separation cryogenique de l'air Active EP3133361B1 (fr)

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US10578356B2 (en) 2017-08-25 2020-03-03 Praxair Technology, Inc. Annular divided wall column for an air separation unit having a ring shaped support grid
US10684071B2 (en) 2017-08-25 2020-06-16 Praxair Technology, Inc. Annular divided wall column for an air separation unit
EP3998447A4 (fr) * 2019-07-10 2023-04-12 Taiyo Nippon Sanso Corporation Dispositif et procédé de séparation d'air
US20220196325A1 (en) * 2020-12-17 2022-06-23 L'air Liquide, Societe Anonyme Pour L'etude Et L?Exploitation Des Procedes Georges Claude Method and apparatus for improving start-up for an air separation apparatus
US11512897B2 (en) * 2021-01-14 2022-11-29 Air Products And Chemicals, Inc. Fluid recovery process and apparatus
EP4230936A1 (fr) * 2022-02-17 2023-08-23 Linde GmbH Système de rectification cryogénique de l'air, unité de commande, unité de séparation de l'air et procédé de séparation cryogénique de l'air

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CN106468498B (zh) 2020-09-22
US10845118B2 (en) 2020-11-24
EP3133361B1 (fr) 2018-06-13
US20170051971A1 (en) 2017-02-23
PL3133361T3 (pl) 2018-11-30

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