EP0229803B1 - Verfahren und vorrichtung für luftdestillation - Google Patents

Verfahren und vorrichtung für luftdestillation Download PDF

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Publication number
EP0229803B1
EP0229803B1 EP86904215A EP86904215A EP0229803B1 EP 0229803 B1 EP0229803 B1 EP 0229803B1 EP 86904215 A EP86904215 A EP 86904215A EP 86904215 A EP86904215 A EP 86904215A EP 0229803 B1 EP0229803 B1 EP 0229803B1
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EP
European Patent Office
Prior art keywords
column
section
argon
liquid
low pressure
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.)
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EP86904215A
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English (en)
French (fr)
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EP0229803A1 (de
Inventor
Jean-Renaud Brugerolle
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Application filed by LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority to AT86904215T priority Critical patent/ATE50857T1/de
Publication of EP0229803A1 publication Critical patent/EP0229803A1/de
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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
    • F25J3/04333—Generation 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
    • F25J3/04351—Generation 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 nitrogen
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    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J3/00—Removing solid residues from passages or chambers beyond the fire, e.g. from flues by soot blowers
    • F23J3/02—Cleaning furnace tubes; Cleaning flues or chimneys
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
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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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    • 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
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    • 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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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
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    • F25J3/04321—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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    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
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    • F25J3/04654—Producing crude argon in a crude argon column
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    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/52—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen enriched compared to air ("crude oxygen")
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/923—Inert gas
    • Y10S62/924—Argon

Definitions

  • the present invention relates to the air distillation technique by means of an installation provided with an argon production column.
  • air distillation installations provided with an argon production column generally comprise a double column consisting of a medium pressure distillation column operating at about 6 bars, of a low distillation column pressure operating slightly above atmospheric pressure, and a condenser-vaporizer.
  • the air is sent, after purification and cooling, to the tank of the medium pressure column.
  • the “rich liquid (oxygen-enriched air) collected in the bottom of the medium pressure column is sent to the feed at an intermediate point in the low pressure column, while part of the“ poor liquid ”, consisting almost entirely of nitrogen, collected at the head of the medium pressure column is sent to reflux at the head of the low pressure column.
  • the low-pressure column is connected to the argon production column by a pipe called “argon tapping and a return pipe for liquid less rich in argon.
  • the low pressure column is generally provided in the tank with gaseous oxygen and liquid oxygen withdrawal pipes, and the medium pressure column is generally provided at the head with gaseous nitrogen and liquid nitrogen withdrawal pipes.
  • the vapor at the top of the low pressure column (“impure nitrogen”) consists of nitrogen containing up to a few% of oxygen and is generally discharged into the atmosphere.
  • FR-A-2 550 325 proposes a solution to limit this drawback. This solution has the advantage of being simple, but its effectiveness is limited.
  • distillation of a given air flow is capable of supplying approximately 21% of this oxygen flow and, under certain conditions, this quantity of oxygen is in excess of actual needs, while other productions , including argon, are sought after.
  • the object of the invention is to make it possible in all cases to optimize the excess oxygen in order to increase the desired productions, in particular that of argon.
  • the subject of the invention is a process for the distillation of air by means of an installation comprising a main distillation apparatus associated with an argon production column by an argon tapping pipe, this process being such that defined in claim 1.
  • the invention also relates to an installation intended for the implementation of such a method.
  • This installation is as defined in claim 13.
  • a “column” or “section of a column is a material and heat exchange apparatus having the structure of a distillation column, that is to say comprising a packing or a certain number of trays of the type used in distillation.
  • Figure 1 illustrates by a diagram how a conventional air distillation installation, shown in more detail in the other figures, is modified according to the invention.
  • At least two sections of mixing column K1 and K2 are added to the conventional installation, operating under two pressures P1 and P2 which, as will be seen below, may or may not be equal.
  • the K1 section is supplied at its base with nitrogen gas which can contain up to a few % of oxygen but practically devoid of argon (that is to say containing less than 1% of argon, and preferably less than 0.05% of argon), while the section K2 is supplied at its summit by liquid oxygen practically devoid of argon (with the same meaning as above) and nitrogen.
  • the head vapor of the section K1 is sent to the base of the section K2, and the tank liquid of the latter is sent in reflux to the top of the section K1.
  • lean liquid LP1 consisting of nitrogen containing up to a few% of oxygen, is drawn off and impure oxygen, that is to say containing, is drawn off at the top of the section K2. up to about 15% nitrogen, and preferably about 5-10% nitrogen.
  • At least one intermediate withdrawal is carried out between the base of the section K1 and the top of the section K2, to constitute a residual gas from the installation composed of an oxygen-nitrogen mixture at approximately 10 to 30% d oxygen, and therefore having a composition close to that of air but devoid of argon.
  • the intermediate racking is carried out between the sections K1 and K2. It can be constituted by overhead steam from section K1, which directly supplies the residual gas R.
  • tank liquid LR1 from section K2, this liquid being made up of a mixture oxygen-nitrogen with a content of approximately 40 to 75% of oxygen; this liquid is then sent to the head of a third section of mixing column K3, operating under a pressure P3 and supplied at its base, like the section K1, with nitrogen gas which is possibly impure but practically without argon.
  • the residual gas R1 is then drawn off at the head of the section K3, while the tank liquid of this section constitutes lean liquid LP2 consisting, like the liquid LP1, of nitrogen containing up to a few% of oxygen.
  • the LP1 and LP2 liquids are sent back to the installation to improve the distillation; the impure gaseous oxygen withdrawn at the head of the section K2 can constitute a production gas, or be purified to produce pure gaseous oxygen, as will be seen below.
  • the source of the liquid oxygen and of the nitrogen gas stream (s) will appear in the following description.
  • the diagram in FIG. 1 ensures a remixing of liquid oxygen and nitrogen gas, both almost free of argon, under conditions close to reversibility, which corresponds to recovery of energy.
  • This energy manifests itself in the form of a heat pump type refrigeration transfer between the liquid oxygen and the lean liquid LP1-LP2 and can be used to increase the production of the installation other than oxygen, namely nitrogen gas under pressure, liquid productions and especially argon, as will appear in the following description. It is noted that the above technical effect would also be obtained by supplying the top of the section K2 with liquid oxygen containing up to a few% of nitrogen as an impurity.
  • FIGS 2 to 9 show several examples of implementation of the basic principle illustrated in Figure 1 with double column air distillation plants.
  • the air distillation installation shown in FIG. 2 is intended to produce, on the one hand, impure oxygen containing approximately 5 to 10% nitrogen, on the other hand, argon, and optionally nitrogen. It essentially comprises a double column 1, an argon production column 2, a remixing column 3 and a remixing minaret 4.
  • the double column 1 comprises, in a conventional manner, a lower column 5 operating under a medium pressure MP of the order of 6 bar absolute, an upper column 6 operating under a low pressure BP slightly above atmospheric pressure, and a vaporizer- condenser 7 which puts in heat exchange relation the tank liquid (practically pure liquid oxygen) of the low pressure column with the overhead vapor (practically pure nitrogen) of the medium pressure column.
  • the air to be treated, compressed to 6 bars, purified and cooled near its dew point, is injected at the bottom of the medium pressure column.
  • the tank liquid in this column rich in oxygen (rich liquid LR at about 40% oxygen) contains almost all of the oxygen and argon in the incoming air; it is expanded and injected at 8 at an intermediate location of the low pressure column, while liquid from the top of column 5 (liquid poor in oxygen, LP), is expanded and injected at 9 at the top of the low pressure column.
  • a pipe 10 for argon tapping sends a gas almost free of nitrogen to column 2, and a pipe 11 brings the tank liquid from the latter, slightly less rich in argon, at about near the same level in the low pressure column.
  • the impure argon (argon mixture) is extracted from the top of column 2 and is then purified in a conventional manner.
  • the impure oxygen thus produced contains practically only nitrogen as an impurity.
  • the remixing minaret 4 constitutes the section of mixing column K3 in FIG. 1. Its base communicates directly with the top of the low pressure column 6. It is therefore supplied at its base with impure nitrogen (nitrogen containing up to to a few% of oxygen). At its summit, this minaret is supplied with 13 by the rich liquid LR1 coming from column 3 and suitably expanded.
  • the relatively reversible remixing of the impure nitrogen and the rich liquid LR1 produces an additional quantity of poor liquid LP2, consisting of nitrogen containing up to a few% of oxygen, which falls into column 6 and increases the reflux there.
  • the waste gas R1 devoid of argon and whose composition is close to that of air is evacuated.
  • part of the rich liquid LR or LR1 can be expanded and vaporized in a condenser at the head of column 2, then returned to column 6 near level 8. Furthermore, as shown, part of the vapor from the top of column 6 can be withdrawn, for example to produce by distillation in an auxiliary column section (not shown) pure nitrogen under low pressure.
  • liquid is taken from the low pressure column, a few trays above the argon tapping 10, and sent to the head of an auxiliary low pressure column 14; the latter is supplied at its base with impure oxygen from the mixing column 3, expanded at low pressure in a turbine 15.
  • the bottom liquid of the column 14 is impure oxygen without argon, that the is added upstream of the pump 12 to the pure liquid oxygen withdrawn from the low pressure column. All the argon contained in the liquid injected at the top of the column 14 leaves with the overhead vapor of this column and is returned to the low pressure column 6, at about the same level as the withdrawal of said liquid.
  • the column 3 operates in the vicinity of the low pressure and directly receives at the head liquid oxygen coming from the tank of the column 6.
  • the turbine 15 of FIG. 3 is eliminated and the columns 3 and 14 are combined in a single ferrule 16.
  • the tank of column 3 is supplied with nitrogen obtained by expansion in a turbine 17 of medium pressure nitrogen. As shown, medium pressure nitrogen expanded in the turbine 17 and then in an expansion valve 17A can also be blown at the head of the column 6.
  • FIG. 5 shows another means of supplying low pressure nitrogen at the base of column 3: the upper part of column 6 is split by an auxiliary column 18 operating at a somewhat higher pressure, for example 1.8 bar against 1.4 bar for column 6.
  • Part of the treated air flow is diverted and expanded to 1.8 bar in a turbine 19.
  • Part of the turbinated flow is sent to the base of column 18, which receives at the head, like column 6, lean liquid at the correct pressure.
  • the rest of the turbined air is expanded to 1.4 bar in an expansion valve 20 and blown into column 6, as is the tank liquid in column 18. It is impure nitrogen, containing up to at a few% of oxygen and practically no argon, withdrawn at the head of column 18, which is used to feed the base of column 3.
  • Figure 6 illustrates a variant of Figure 5 which eliminates the pump (not shown) for raising the liquid LP1.
  • the section K1 is transferred above the column 18, in the same shell as the latter, and the liquid LR1 is shared between the top of the minaret 4 and that of the section K1.
  • a second waste gas R is then produced at the head of the section K1, as indicated in phantom in FIG. 6.
  • the residual gas R1 leaves the minaret 4 at a pressure of the order of 1.3 bar, sufficient for it to be used for the regeneration of the adsorption bottles (not shown) serving purifying the incoming air.
  • This is advantageous but results in a relatively high operating pressure, which is costly in terms of compression energy of the incoming air.
  • the rolling of air in the valve 20 corresponds to a loss of energy.
  • FIG. 7 takes up the principle of FIG. 5 but makes it possible to avoid any rolling of air and to lower the operating pressure: the column 18 is transferred under the column 3, in the same shell; it is supplied at the head by the lean liquid falling from the section K1 and by an addition of lean liquid LP drawn off at the top of the column 5 and expanded in a valve 21, and in the tank by all of the air expanded to 1.8 bar in the turbine 19. Since this flow rate provides an impure nitrogen flow rate at the head of the column 18 greater than that necessary for the operation of the column 3, it is possible to draw from it an additional residual gas R, under approximately 1 , 6 bar, which can be used for the regeneration of the aforementioned adsorption bottles. The gas R1 leaving the minaret 4 is no longer used for this regeneration and need only be at a pressure slightly higher than atmospheric pressure, to overcome the pressure losses of the heat exchange line used for cooling incoming air. The system operating pressure is thus lowered.
  • FIG. 7 shows the source and the use of the two types of rich liquid: (a) rich liquid with argon, originating on the one hand from the tank of the medium pressure column 5, on the other hand from the tank of the column 18. These two flows are combined and serve both to reflux into the low pressure column 6 and to supply the head condenser 2A of the column 2, in a conventional manner; and (b) rich liquid LR1 without argon, taken between the sections K1 and K2 of column 3 and sent to the head of minaret 4. Furthermore, by comparing this FIG. 7 with FIG. 1, it can be seen that one performs between the sections K1 and K2 the two withdrawals indicated in FIG. 1, namely a direct withdrawal of waste gas R and a withdrawal of liquid LR1 which, after mixing with nitrogen, also supplies waste gas R1, but at a pressure different.
  • FIG. 7 also shows pipes for drawing off gaseous oxygen or low pressure liquid from column 6 and nitrogen gas or medium pressure liquid from column 5.
  • FIG. 8 Another possibility to avoid any loss of energy by air rolling is illustrated by the installation of FIG. 8.
  • the double column 5,6 surmounted by the minaret 4 constituting the section K3 of FIG. 1
  • the turbined air in the turbine 19 is expanded to 1.3 bar and blown into column 6.
  • two auxiliary columns are used: on the one hand, a column 3A, operating at 1.4 bar, which joins the column 14 for purifying oxygen and, under it, the section K2 of FIG. 1, and on the other hand a column 3B, operating at 1.5 bar, which joins the section K1 of FIG. 1 and, under this one, a splitting 6A of the upper part of the low pressure column 6.
  • the section K2 is supplied at the head with liquid oxygen withdrawn from the tank of column 6 and, in the tank, by gas G withdrawn at the head of column 3B, that is to say at the head of the section K1.
  • Rich liquid without argon LR1 withdrawn from the bottom of column 3A, is sent under reflux both at the top of column 3B and minaret 4.
  • Poor liquid is sent under reflux both at the top of column 6 and of section 6A, while the liquid rich with argon coming from the tank of column 5 is, in part, injected both into column 6 and into section 6A, and, for another part, vaporized in the condenser of head 2A of column 2 then injected into the tank of section 6A.
  • the very rich liquid collected at the bottom of the latter is in turn injected into column 6.
  • FIG. 8 Pressure drop considerations show that the arrangement of FIG. 8 is particularly suitable in the case where at least column 2 is fitted with packings. Furthermore, it is understood that the installation of FIG. 8 could also operate by replacing the air trigger with a nitrogen trigger.
  • FIG. 9 shows another installation in which the sections K1 and K3 both operate at the pressure of the low pressure column 6 and are combined.
  • the double column is surmounted by a remixing column 3B supplied at the head with liquid oxygen originating from the tank of column 6 and into the tank by the impure nitrogen at the top of this same column 6.
  • the tank liquid from column 3B is refluxed into column 6, and impure oxygen is drawn off at the top from column 3B.
  • the residual gas R is drawn off between the sections K2 on the one hand, K1-K3 on the other hand.
  • the invention is compatible not only with double column installations, but also with any type of air distillation installation comprising means for producing argon.
  • An example of such a simple column installation is illustrated in FIG. 10, which is a more complete diagram than FIGS. 2 to 9.
  • the air, compressed and purified, is cooled and partially liquefied in a heat exchange line 20.
  • the majority of the air flow is expanded to 1.5 bar in a turbine 21 (Claude cycle), then injected into the simple distillation column 1A connected to column 2 for the production of argon.
  • the liquefied air, expanded in a valve 22, is injected into the same column. This produces oxygen in the tank and nitrogen at the top.
  • This latter gas after heating in the exchange line 20, is partially compressed to 6 bars by a compressor 23, cooled and passes through a coil 24 provided in the tank of column 1A, where it condenses by vaporizing the liquid oxygen, then it is partially expanded in a valve 25 and sent under reflux to the top of the column 1A.
  • the rest of the condensed nitrogen is expanded in a valve 26, vaporized in the condenser at the head of column 2 then sent to the tank of the mixing column 3, bringing together the sections K1 and K2, which operates at 2 to 3 bars.
  • the liquid oxygen produced in the tank of column 1A is at least partly brought by pump to the pressure of column 3 and injected at the top of the latter.
  • the impure gaseous oxygen withdrawn at the head of column 3 is condensed in a second coil 27 in the tank of column 1A, expanded in a valve 28 and injected into this same column 1A.
  • the section K3 located above the column 1A is supplied at the top by the rich liquid LR1 drawn off between the sections K1 and K2 and expanded at low pressure, and in the tank by the nitrogen at the top of the column 1A.
  • This section K3 produces in the tank lean liquid LP2 which, like the lean liquid LP1 coming from the tank of column 3, is sent under reflux at the top of column 1A; it produces the waste gas R1 at the head, which is heated in the exchange line 20 before being evacuated or, if the pressure is sufficient, used to regenerate the bottles of adsorbent used to purify the incoming air .
  • the installation can also produce liquid oxygen, drawn off from the bottom of column 1A, gaseous oxygen, also drawn off from the bottom of this column and heated in the exchange line 20, and nitrogen gas, drawn off at the top of the same column and, after heating, discharged upstream of the compressor 23.
  • nitrogen can also be taken at 6 bars downstream of the compressor 23.

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Claims (18)

1. Verfahren zur Destillation von Luft mit Hilfe einer Anlage, die eine Hauptdestillationsapparatur (1 ; 1,18 ; 1,6A ; 1A) umfaßt, die mit einer Argon-Gewinnungskolonne (2) durch eine Argon-Anbohrleitung (10) verbunden ist, welches Verfahren folgende Schritte umfaßt :
- des Basis eines ersten Mischkolonnenabschnitts (K1) wird gasförmiger Stickstoff zugeführt, der gegebenenfalls verunreinigt, aber praktisch frei von Argon ist, und der Spitze eines zweiten Mischkolonnenabschnitts (K2) wird flüssiger Sauerstoff zugeführt, der gegebenenfalls verunreinigt, aber praktisch frei von Argon ist ;
- der Basis des zweiten Abschnitts (K2) wird mindestens ein Teil des Dampfs vom Kopf des ersten Abschnitts zugeführt, und der Spitze des ersten Abschnitts (K1) wird ein Teil der an der Basis des zweiten Abschnitts erzeugten Flüssigkeit zugeführt ;
- von dem zweiten Abschnitt (K2) wird an dessen Kopf verunreinigter Sauerstoff abgezogen, der höchsten einige Prozent Stickstoff enthält ;
- von dem ersten Abschnitt (K1) wird an dessen Basis arme Flüssigkeit (LP1) abgezogen, die aus Stickstoff besteht, der höchstens einige Prozent Sauerstoff enthält, und diese arme Flüssigkeit wird im Rücklauf in die Hauptdestillationsapparatur (1 ; 1,18 ; 1,6A ; 1A) geführt ; und
- zwischen den beiden Mischkolonnenabschnitten (K1, K2) wird ein Teil der an der Basis des zweiten Abschnitts (K2) produzierten Flüssigkeit (LR1) abgezogen, und diese Flüssigkeit wird mit dem gasförmigen Stickstoff, der gegebenenfalls verunreinigt, aber praktisch frei von Argon ist, rückvermischt in einem dritten Mischkolonnenabschnitt (K3), wobei der Dampf vom Kopf dieses dritten Mischkolonnenabschnitts Restgas (R1) darstellt, das aus einem Gemisch von Stickstoff und Sauerstoff gebildet ist, das ungefähr 10 bis 30 % Sauerstoff enthält, während die an der Basis des dritten Abschnitts erzeugte Flüssigkeit (LP2) zusätzliche arme Rückflußflüssigkeit für die Hauptdestillationsapparatur (1 ; 1,18 ; 1,6A ; 1A) darstellt, welche Flüssigkeit aus Stickstoff besteht, der höchstens einige Prozent Sauerstoff enthält.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der genannte verunreinigte Sauerstoff weniger als 15 % Stickstoff enthält.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß zwischen den beiden ersten Abschnitten (K1, K2) ein Teil des Dampfs (R) vom Kopf des ersten Abschnitts abgezogen wird, welche Entnahme ein Restgas (R) aus einem Gemisch von Stickstoff und Sauerstoff mit ungefähr 10 bis 30 % Sauerstoff darstellt.
4. Verfahren nach einem der Ansprüche 1 bis 3, bei welchem die Hauptdestillationsapparatur eine Doppelkolonne (1) umfaßt, die ihrerseits eine Mitteldruckkolonne (5) umfaßt, welche unter verhältnismäßig hohem Druck arbeitet, und eine Niederdruckkolonne (6), welche unter verhältnismäßig niedrigem Druck arbeitet und mit der Argon-Gewinnungskolonne (2) durch die genannte Argon-Anbohrleitung (10) verbunden ist, dadurch gekennzeichnet, daß man den ersten und den zweiten Mischkolonnenabschnitt (K1, K2) bei Mitteldruck arbeiten läßt, indem der erste Abschnitt (K1) mit dem aus der Mitteldruckkolonne (5) abgezogenen Stickstoff und der zweite Abschnitt (K2) mit dem vom Sumpf der Niederdruckkolonne (6) abgezogenen und auf den gleichen Druck gebrachten flüssigen Sauerstoff gespeist wird.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß der verunreinigte Sauerstoff durch Verdampfen von flüssigem Sauerstoff aus der Hauptdestillationsapparatur (1A) kondensiert wird, und daß die gewonnene Flüssigkeit im Rückfluß in diese Apparatur in einer Höhe eingeleitet wird, die über der Höhe der Argon-Anbohrleitung (10) liegt.
6. Verfahren nach einem der Ansprüche 1 bis 4, worin die Hauptdestillationsapparatur eine Doppelkolonne (1) umfaßt, die ihrerseits eine Mitteldruckkolonne (5) umfaßt, welche unter einem verhältnismäßig hohen Druck arbeitet, und eine Niederdruckkolonne (6), welche unter einem verhältnismäßig niedrigen Druck arbeitet und mit der Argon-Gewinnungskolonne (2) durch die genannte Argon-Anbohrleitung (10) verbunden ist, dadurch gekennzeichnet, daß der verunreinigte Sauerstoff in einer Niederdruck-Hilfskolonne (14) destilliert wird, die mit Flüssigkeit gespeist wird, die der Niederdruckkolonne (6) oberhalb der Argon-Anbohrleitung entnommen ist, und daß der Dampf vom Kopf dieser Niederdruck-Hilfskolonne (14) in ungefähr der gleichen Höhe in die Niederdruckkolonne (6) geleitet wird, während seine Sumpf-Flüssigkeit im Rücklauf in den zweiten Mischkolonnenabschnitt (K2) geleitet wird.
7. Verfahren nach einem der Ansprüche 1 bis 6, bei welchem die Hauptdestillationsapparatur eine Doppelkolonne (1) umfaßt, die ihrerseits eine Mitteldruckkolonne (5) umfaßt, welche unter verhältnismäßig hohem Druck arbeitet, und eine Niederdruckkolonne (6), welche unter verhältnismäßig niedrigem Druck arbeitet und mit der Argon-Gewinnungskolonne (2) durch die genannte Argon-Anbohrleitung (10) verbunden ist, dadurch gekennzeichnet, daß in einer Turbine (17) ein Teil des Dampfs vom Kopf der Mitteldruckkolonne (5) entspannt wird.
8. Verfahren nach Anspruch 7, dadurch gekennzeichnet, daß man den ersten Mischkolonnenabschnitt (K1) und den zweiten Mischkolonnenabschnitt (K2) unter ein und demselben Druck nahe dem Niederdruck arbeiten läßt, indem der erste Abschnitt (K1) mit dem von der Mitteldruckkolonne abgezogenen und in der genannten Turbine (17) entspannten Stickstoff gespeist wird und indem der zweite Abschnitt (K2) unmittelbar mit flüssigen Sauerstoff gespeist wird, der dem Sumpf der Niederdruckkolonne (6) entnommen ist.
9. Verfahren nach einem der Ansprüche 1 bis 3, bei welchem die Hauptdestillationsapparatur (1,18) eine Doppelkolonne umfaßt, die ihrerseits eine Mittaidruckkoionne (5), welche unter verhältnismäßig hohem Druck arbeitet, und eine Niederdruckkolonne (6) umfaßt, welche unter verhältnismäßig niedrigem Druck arbeitet und mit der Argon-Gewinnungskolonne (2) durch die genannte Argon-Anbohrleitung verbunden ist, dadurch gekennzeichnet, daß man den ersten Mischkolonnenabschnitt (K1) und den zweiten Mischkolonne-. nabschnitt (K2) unter einem etwas über dem Niederdruck liegenden Rezyklierungsdruck arbeiten läßt, daß man einen Teil der behandelten Luft in einer Turbine (19) auf diesen Rezyklierungsdruck entspannt, daß man mindestens einen Teil der aus der Turbine heraustretenden Luft destilliert (in 18), wobei die arme Flüssigkeit als Rücklauf benutzt wird, und daß man den aus dieser Destillation sich ergebenden verunreinigten Stickstoff in den ersten Mischkolonnenabschnitt (K1) einführt.
10. Verfahren nach Anspruch 9, dadurch gekennzeichnet, daß die aus der Turbine heraustretende überschüssige Luft nach dem Entspannen in einem Ventil (20) in die Niederdruckkolonne (6) eingeblasen wird.
11. Verfahren nach Anspruch 9, dadurch gekennzeichnet, daß die Gesamtmenge der aus der Turbine austretenden Luft destilliert wird, wobei als Rücklauf die an der Basis des ersten Mischkolonnenabschnitts (K1) erzeugte arme Flüssigkeit verwendet wird, daß in die Mischkolonne an ihrer Basis der aus dieser Destillation sich ergebende verunreinigte Stickstoff eingeführt wird, und daß Restgas (R) zwischen den beiden Mischkolonnenabschnitten (K1, K2) entnommen wird.
12. Verfahren nach einem der Ansprüche 1 bis 11, dadurch gekennzeichnet, daß das Restgas (R, R1) zur Regenerierung von Adsorptionsflaschen verwendet wird, die zur Reinigung der eintretenden Luft dienen.
13. Anlage zur Destillation von Luft, umfassend :
- eine Hauptdestillationsapparatur (1 ; 1,18; 1,6A; 1A), die mit einer Argon-Gewinnungskolonne (2) durch eine Argon-Anbohrleitung (10) verbunden ist ;
- einen ersten Mischkolonnenabschnitt (K1) und eine Einrichtung zum Zuführen von gegebenenfalls verunreinigtem, aber praktisch argonfreiem, gasförmigem Stickstoff in die Basis dieses Abschnitts ;
- einen zweiten Mischkolonnenabschnitt (K2) und eine Einrichtung zum Zuführen von gegebenenfalls verunreinigtem, aber praktisch argonfreiem flüssigen Sauerstoff ;
- eine Einrichtung zum Zuführen von mindestens einem Teil des Dampfs von dem Kopf des ersten Abschnitts in die Basis des zweiten Abschnitts (K2) und einem Teil der an der Basis des zweiten Abschnitts erzeugten Flüssigkeit in die Spitze des ersten Abschnitts (K1) ;
- eine Einrichtung zum Zuführen der an der .Basis des ersten Abschnitts erzeugten Flüssigkeit (LP1) im Rückfluß in die Hauptdestillationsapparatur (1 ; 1,18 ; 1,6A; 1 A) ;
- eine Einrichtung zum Wegführen des am Kopf des zweiten Abschnitts (K2) vorliegenden Dampfs aus diesem Abschnitt ;
- eine Einrichtung zum intermediären Abziehen von Flüssigkeit zwischen der Basis des ersten Abschnitts (K1) und der Spitze des zweiten Abschnitts (K2) ; und
- einen dritten Mischkolonnenabschnitt (K3), eine Einrichtung zum Zuführen von gegebenenfalls verunreinigtem, aber praktisch argonfreiem, gasförmigem Stickstoff in die Basis dieses Abschnitts und zum Zuführen von durch die genannte Einrichtung zum intermediären Abziehen abgezogener Flüssigkeit (LR1) an die Spitze dieses Abschnitts, sowie eine Einrichtung zum Abziehen eines Restgases der Anlage (R1) vom Kopf dieses dritten Abschnitts.
14. Anlage nach Anspruch 13, dadurch gekennzeichnet, daß sie eine Einrichtung zum Abziehen von ein Restgas (R) der Anlage darstellendem Dampf zwischen der Basis des ersten Abschnitts (K1) und der Spitze des zweiten Abschnitts (K2) aufweist.
15. Anlage nach Anspruch 13 oder 14 des Typs, bei welchem die Hauptdestillationsapparatur (1) eine Doppelkolonne umfaßt, die ihrerseits eine unter verhältnismäßig hohem Druck arbeitende Mitteldruckkolonne (5) und eine unter verhältnismäßig niedrigem Druck arbeitende, durch die genannte Argon-Anbohrleitung (10) mit der Argon-Gewinnungskolonne (2) verbundene Nieder- . druckkolonne (6) aufweist, dadurch gekennzeichnet, daß sie einen Hilfskolonnenabschnitt (14) aufweist, dem an seiner Spitze Flüssigkeit zugeführt wird, die in der Niederdruckkolonne (6) oberhalb der Argon-Anbohrleitung (10) entnommen worden ist, eine Einrichtung zum Einleiten des Dampfs vom Kopf dieses Hilfsabschnitts in die Niederdruckkolonne in ungefähr der gleichen Höhe, wobei dem Hilfsabschnitt (14) an seiner Basis der Dampf vom Kopf des zweiten Mischkolonnenabschnitts (K2) zugeführt wird, während die Trogflüssigkeit dieses Hilfsabschnitts im Rücklauf in den Kopf des zweiten Mischkolonnenabschnitts eingeleitet wird.
16. Anlage nach einem der Ansprüche 13 bis 15 des Typs, bei dem die Hauptdestillationsapparatur (1) eine Doppelkolonne umfaßt, die ihrerseits eine unter einem verhältnismäßig hohen Druck arbeitende Mitteldruckkolonne (5) und eine unter einem verhältnismäßig niedrigen Druck arbeitende und durch die genannte Argon-Anbohrleitung (10) mit der Argon-Gewinnungskolonne (2) verbundene Niederdruckkolonne (6) aufweist, dadurch gekennzeichnet, daß sie eine Entspannungsturbine (17) für den Dampf vom Kopf der Mitteldruckkolonne (5) aufweist.
17. Anlage nach einem der Ansprüche 13 bis 16 des Typs, bei dem die Hauptdestillationsapparatur (1,18) eine Doppelkolonne (1) umfaßt, die ihrerseits eine unter verhältnismäßig hohem Druck arbeitende Mitteldruckkolonne (5) und eine unter verhältnismäßig niedrigem Druck arbeitende und durch die genannte Argon-Anbohrleitung (10) mit der Argon-Gewinnungskolonne (2) verbundene Niederdruckkolonne (6) aufweist, dadurch gekennzeichnet, daß sie eine Entspannungsturbine (19) für einen Teil der eintretenden Luft aufweist und einen zweiten Hilfskolonnenabschnitt (18), der unter einem etwas über dem Niederdruck liegenden Druck arbeitet und am Kopf verunreinigten Stickstoff erzeugt, der der Basis des ersten Mischkolonnenabschnitts (K1) zugeführt wird.
EP86904215A 1985-07-15 1986-07-09 Verfahren und vorrichtung für luftdestillation Expired - Lifetime EP0229803B1 (de)

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FR8510796 1985-07-15
FR8510796A FR2584803B1 (fr) 1985-07-15 1985-07-15 Procede et installation de distillation d'air

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EP0229803B1 true EP0229803B1 (de) 1990-03-07

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EP (1) EP0229803B1 (de)
JP (1) JPH0731004B2 (de)
KR (1) KR880700215A (de)
AU (1) AU584229B2 (de)
BR (1) BR8606791A (de)
CA (1) CA1310579C (de)
DE (1) DE3669392D1 (de)
DK (1) DK130687D0 (de)
ES (1) ES2000213A6 (de)
FI (1) FI871121A (de)
FR (1) FR2584803B1 (de)
IN (1) IN167585B (de)
NZ (1) NZ216821A (de)
PT (1) PT82966B (de)
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Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8620754D0 (en) * 1986-08-28 1986-10-08 Boc Group Plc Air separation
DE3871220D1 (de) * 1987-04-07 1992-06-25 Boc Group Plc Lufttrennung.
GB8806478D0 (en) * 1988-03-18 1988-04-20 Boc Group Plc Air separation
DE3913880A1 (de) * 1989-04-27 1990-10-31 Linde Ag Verfahren und vorrichtung zur tieftemperaturzerlegung von luft
US5133790A (en) * 1991-06-24 1992-07-28 Union Carbide Industrial Gases Technology Corporation Cryogenic rectification method for producing refined argon
US5309719A (en) * 1993-02-16 1994-05-10 Air Products And Chemicals, Inc. Process to produce a krypton/xenon enriched stream from a cryogenic nitrogen generator
US5490391A (en) * 1994-08-25 1996-02-13 The Boc Group, Inc. Method and apparatus for producing oxygen
FR2778233B1 (fr) * 1998-04-30 2000-06-02 Air Liquide Installation de distillation d'air et boite froide correspondante
FR2789162B1 (fr) * 1999-02-01 2001-11-09 Air Liquide Procede de separation d'air par distillation cryogenique
FR2801963B1 (fr) 1999-12-02 2002-03-29 Air Liquide Procede et installation de separation d'air par distillation cryogenique
ATE342478T1 (de) * 1999-04-05 2006-11-15 Air Liquide Vorrichtung mit variabler auslastung und entsprechendes verfahren zur trennung eines einsatzgemisches
DE10139097A1 (de) * 2001-08-09 2003-02-20 Linde Ag Verfahren und Vorrichtung zur Erzeugung von Sauerstoff durch Tieftemperatur-Zerlegung von Luft
ES2278703T5 (es) † 2001-12-04 2010-03-17 Air Products And Chemicals, Inc. Proceso y aparato para la separacion criogenica de aire.
EP1387136A1 (de) * 2002-08-02 2004-02-04 Linde AG Verfahren und Vorrichtung zur Erzeugung von unreinem Sauerstoff durch Tieftemperaturzerlegung von Luft
FR2854232A1 (fr) * 2003-04-23 2004-10-29 Air Liquide Procede de distillation d'air pour produire de l'argon
DE102012021694A1 (de) 2012-11-02 2014-05-08 Linde Aktiengesellschaft Verfahren zur Tieftemperaturzerlegung von Luft in einer Luftzerlegungsanlage und Luftzerlegungsanlage
BR112015009379A2 (pt) * 2012-11-02 2017-07-04 Linde Ag processo para separação de baixa temperatura de ar em uma usina de separação de ar e usina de separação de ar
AU2018269511A1 (en) 2017-05-16 2019-11-28 Terrence J. Ebert Apparatus and process for liquefying gases
FR3074274B1 (fr) 2017-11-29 2020-01-31 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et appareil de separation d'air par distillation cryogenique
US20220126263A1 (en) 2019-02-25 2022-04-28 L'air Liquide, Société Anonyme Pour L'etude Et L'exploitation Des Precédés Georges Claude Matrix integrating at least one heat exchange function and one distillation function
FR3093172B1 (fr) 2019-02-25 2021-01-22 L´Air Liquide Sa Pour L’Etude Et L’Exploitation Des Procedes Georges Claude Appareil d’échange de chaleur et de matière
FR3110686B1 (fr) 2020-05-19 2023-06-09 Air Liquide Procédé de fourniture d’oxygène et/ou d’azote ainsi que d’argon à une zone géographique
US20240035743A1 (en) * 2022-08-01 2024-02-01 Air Products And Chemicals, Inc. Process and apparatus for recovery of at least nitrogen and argon

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2280383A (en) * 1939-09-08 1942-04-21 Baufre William Lane De Method and apparatus for extracting an auxiliary product of rectification
US2547177A (en) * 1948-11-02 1951-04-03 Linde Air Prod Co Process of and apparatus for separating ternary gas mixtures
US4022030A (en) * 1971-02-01 1977-05-10 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Thermal cycle for the compression of a fluid by the expansion of another fluid
US4137056A (en) * 1974-04-26 1979-01-30 Golovko Georgy A Process for low-temperature separation of air
US4433989A (en) * 1982-09-13 1984-02-28 Erickson Donald C Air separation with medium pressure enrichment
FR2550325A1 (fr) * 1983-08-05 1985-02-08 Air Liquide Procede et installation de distillation d'air au moyen d'une double colonne
US4533375A (en) * 1983-08-12 1985-08-06 Erickson Donald C Cryogenic air separation with cold argon recycle

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PT82966B (pt) 1992-08-31
DE3669392D1 (de) 1990-04-12
FI871121A0 (fi) 1987-03-13
AU584229B2 (en) 1989-05-18
ZA865185B (en) 1987-03-25
DK130687A (da) 1987-03-13
FR2584803B1 (fr) 1991-10-18
EP0229803A1 (de) 1987-07-29
WO1987000609A1 (fr) 1987-01-29
FI871121A (fi) 1987-03-13
PT82966A (fr) 1986-08-01
AU6129086A (en) 1987-02-10
ES2000213A6 (es) 1988-01-16
DK130687D0 (da) 1987-03-13
JPH0731004B2 (ja) 1995-04-10
IN167585B (de) 1990-11-17
US4818262A (en) 1989-04-04
CA1310579C (fr) 1992-11-24
BR8606791A (pt) 1987-10-13
JPS63500329A (ja) 1988-02-04
FR2584803A1 (fr) 1987-01-16
KR880700215A (ko) 1988-02-20
NZ216821A (en) 1988-01-08

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