WO2022028732A1 - Procédé et installation pour effectuer un processus industriel - Google Patents

Procédé et installation pour effectuer un processus industriel Download PDF

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Publication number
WO2022028732A1
WO2022028732A1 PCT/EP2021/025248 EP2021025248W WO2022028732A1 WO 2022028732 A1 WO2022028732 A1 WO 2022028732A1 EP 2021025248 W EP2021025248 W EP 2021025248W WO 2022028732 A1 WO2022028732 A1 WO 2022028732A1
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WIPO (PCT)
Prior art keywords
rectification
subjected
argon
impure argon
heat exchange
Prior art date
Application number
PCT/EP2021/025248
Other languages
German (de)
English (en)
Inventor
Dirk Schwenk
Dimitri GOLUBEV
Original Assignee
Linde Gmbh
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Publication date
Application filed by Linde Gmbh filed Critical Linde Gmbh
Priority to EP21739562.3A priority Critical patent/EP4189311B1/fr
Publication of WO2022028732A1 publication Critical patent/WO2022028732A1/fr

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Classifications

    • 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
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/40—Features relating to the provision of boil-up in the bottom of a column
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/58—Argon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • 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
    • F25J2260/00—Coupling of processes or apparatus to other units; Integrated schemes
    • F25J2260/58—Integration in an installation using argon
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/02—Internal refrigeration with liquid vaporising loop
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/88—Quasi-closed internal refrigeration or heat pump cycle, if not otherwise provided
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop

Definitions

  • the present invention relates to a method for carrying out an industrial process and a corresponding system according to the respective preambles of the independent patent claims.
  • Pure argon is required for various purposes, for example the semiconductor industry. Pure argon is used in particular to provide inert gas atmospheres, especially in cases where nitrogen proves to be too reactive. For example, nitrogen can lead to the undesirable formation of metal nitrides in sputtering processes.
  • the present invention is not restricted by the specific use of argon, but can be used in a large number of industrial processes, for example also in the field of melting metallurgy or as an inert gas or flushing gas for heat treatment.
  • the pure argon is, in particular, so-called argon 6.0 with a purity of at least 99.9999%.
  • Such pure argon typically contains less than 0.5 ppm nitrogen, 0.5 ppm oxygen, 0.5 ppm water, 0.1 ppm hydrocarbons, 0.1 ppm carbon monoxide, 0.1 ppm carbon dioxide and 0.5 ppm hydrogen as secondary components .
  • argon is mentioned in general below, this also includes, in addition to pure argon, mixtures that are rich in argon but also have corresponding secondary components, as long as the argon content is more than 50%, 75%, 80%, 90%, 95 %, 99%, 99.9%, 99.99%, 99.999%. All percentages refer here in particular to mole percent or volume percent.
  • Argon can be produced as an air product in a liquid or gaseous state by low-temperature separation of air in an air separation plant and subsequent purification, as for example at H.-W. Häring (ed.), Industrial Gases Processing, Wiley-VCH, 2006, in particular Section 2.2.5, "Cryogenic Rectification”. Production can take place on site, i.e. at the point of consumption, for example in a semiconductor factory, or it can be transported in a suitable form to the place of consumption.
  • DE 10 2018006 002 B3 therefore proposes a method for recycling argon from an industrial process, in which the argon previously used in the industrial process is processed using low-temperature separation.
  • a further embodiment of a corresponding method is disclosed in US Pat. No. 5,706,674 A.
  • FR 1 478 995 A relates to the separation of components of a gas mixture such as air by rectification and in particular to a process for separating nitrogen and oxygen in a single rectification column, the refrigerant of which consists in part of compressed liquefied air.
  • a method for recovering and purifying argon is known from EP 0 761 596 A1, in which the energy consumption is said to be low due to simple steps.
  • This method includes: a first step of reacting impure argon gas with hydrogen gas so that oxygen contained in the impure argon gas is converted into water, thereby substantially removing oxygen from the impure argon gas; a second step of introducing the impure argon gas into an adsorption device, the adsorption device being caused to adsorb water and carbon dioxide contained in the impure argon gas, thereby substantially removing the water and carbon dioxide from the impure argon gas; and a third step in which the impure argon gas is subjected to low-temperature liquefaction and the liquefied argon is introduced into a rectifier, the rectifier being caused to remove low-boiling point impurity components and high-boiling point impurity components contained in the impure argon gas , to be removed by purification and separation,
  • a stream containing at least 93 mol % oxygen is fed from an adsorptive air separation plant to a purification device which comprises a heat exchanger and a cryogenic distillation column, and the stream is cooled in the heat exchanger and separated in the cryogenic distillation column.
  • the present invention sets itself the task of improving the processing of argon from corresponding industrial processes.
  • the present invention solves this problem by a method for carrying out an industrial process and a corresponding system according to the respective preambles of the independent patent claims.
  • Configurations are the subject matter of the dependent patent claims and the following description, with explanations relating to the method and its configurations applying in the same way to a corresponding system and its configurations.
  • a “condenser evaporator” refers to a heat exchanger in which a first, condensing fluid stream enters into indirect heat exchange with a second, evaporating fluid stream.
  • Each condenser evaporator has a condensing space and an evaporating space.
  • Condensation and evaporation chambers have liquefaction and evaporation passages. The condensation (liquefaction) of the first fluid stream is carried out in the liquefaction chamber, and the evaporation of the second fluid stream is carried out in the evaporation chamber.
  • the evaporating and condensing spaces are formed by groups of passages which are in heat exchange relationship with each other.
  • the main condenser which connects a high-pressure column and a low-pressure column of an air separation plant in a heat-exchanging manner, is designed as a condenser evaporator.
  • the main condenser can be designed in particular as a single-stage or multi-stage bath evaporator, in particular as a cascade evaporator (as described, for example, in EP 1 287302 B1), or else as a falling film evaporator.
  • the main condenser can be formed by a single heat exchanger block or by several heat exchanger blocks arranged in a common pressure vessel.
  • Corresponding condenser evaporators can also be used within the scope of the present invention, in particular as top condensers.
  • a liquid or two-phase stream is pushed through the evaporation space by its own pressure and partially evaporated there.
  • 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) or by throttling the liquid flow to a lower pressure level.
  • Liquids and gases can be rich or poor in one or more components, where "rich” means a content of at least 50%, 75%, 90%, 95%, 99%, 99.5%, 99, 9% or 99.99% and “poor” can stand for a content of at most 50%, 25%, 10%, 5%, 1%, 0.1% or 0.01% on a mole, weight or volume basis .
  • the term "predominantly” may correspond to the definition of "rich”.
  • Liquids and gases can also be enriched or depleted in one or more components, these terms referring to a content in a starting liquid or a starting gas from which the liquid or gas was obtained.
  • the liquid or the gas is "enriched” if this or this at least 1.1 times, 1.5 times, 2 times, 5 times, 10 times, 100 times or 1,000 times the content, and ""depleted” if it contains at most 0.9, 0.5, 0.1, 0.01 or 0.001 times the content of a corresponding component, based on the starting liquid or the starting gas. If, for example, “oxygen” or “nitrogen” is mentioned here, this also includes a liquid or a gas that is rich in oxygen or nitrogen, but does not necessarily have to consist exclusively of them.
  • pressure level and "temperature level” to characterize pressures and temperatures, which is intended to express the fact that corresponding pressures and temperatures in a corresponding system do not have to be used in the form of exact pressure or temperature values in order to to realize the inventive concept.
  • pressures and temperatures typically vary within certain ranges, for example, ⁇ 1%, 5%, or 10% about an average value.
  • Corresponding pressure levels and temperature levels can be in disjoint areas or in areas that overlap one another. In particular, for example, pressure levels include unavoidable or expected pressure losses. The same applies to temperature levels.
  • the pressure levels given here in bar are absolute pressures.
  • impure argon is carried out from a process step of the type explained above and that Impure argon or a portion thereof is subjected to processing to obtain pure argon.
  • the pure argon or a part thereof is finally returned to the process step, with the processing comprising compression, heat exchange and rectification in a rectification column which has a bottom evaporator and a top condenser.
  • the pure argon is obtained as the bottom product of the rectification column, more volatile components, but in particular not less volatile components, being separated from the impure argon in the rectification column to obtain the pure argon.
  • the rectification column is, in particular, a single rectification column that is not coupled in series with other rectification columns, with “serial coupling” being understood to mean that a fluid that is obtained by separation in a first rectification column is fed into a further rectification column .
  • the present process differs from that disclosed in US Pat. No. 5,706,674 by using a single rectification column.
  • the impure argon can generally be oxygen-free or essentially oxygen-free impure argon, but also impure argon containing oxygen to a certain extent.
  • the oxygen can be catalytically converted with hydrogen to form water, with the water then being separated from the impure argon.
  • the impure argon discharged from the process step, or a portion thereof, is subjected to compression, heat exchange with other streams explained below with cooling, and at least partial condensation in the bottom evaporator to obtain an impure argon condensate.
  • a first part of the impure argon condensate is fed into the rectification column in condensed form and a second part is subjected to evaporation in the top condenser.
  • the vaporized second portion of the impure argon condensate or a portion thereof is fed back to the rectification as a circulating stream.
  • the use of the circulating stream enables a significant reduction in the achievable residual levels of carbon monoxide.
  • the present invention proposes that the recycle stream is subjected to at least a part of the compression together with the impure argon discharged from the process step or the part thereof subjected to compression.
  • a combination with the impure argon from the process step can take place upstream or in the compressor that is used in this compression, the latter for example by feeding between different compressor stages of a multi-stage compressor or a screw compressor.
  • the present invention makes it possible to dispense with a separate compressor and thus creates a low-maintenance and cost-effective method.
  • impure argon can contain oxygen.
  • the impure argon can be subjected to a catalytic conversion of at least part of the oxygen with hydrogen to form water of a type known in principle (so-called “DeOxo”) and then at least part of the processing.
  • the water can be separated off at least in part, in particular by condensing out, if necessary, with a remainder of the impure argon being able to be subjected at least in part to the treatment.
  • this remaining residue can be subjected to an adsorptive process before the actual treatment to remove unwanted components that interfere with the treatment (above all CO2), in particular a thermal swing adsorption using molecular sieves.
  • an adsorptive process before the actual treatment to remove unwanted components that interfere with the treatment (above all CO2), in particular a thermal swing adsorption using molecular sieves.
  • residual amounts of water that have not been separated can be removed. If no separate removal of water, for example by condensation, is carried out after the catalytic conversion, the entire mixture obtained in the catalytic conversion can also be subjected to the adsorptive process.
  • the pure argon is provided using a bottom product formed in the rectification, the bottom product formed in the rectification or a part thereof being subjected to heat exchange with the previously explained impure argon fed in and in particular also the circulating stream combined therewith.
  • the bottom product formed in the rectification or the part thereof which is subjected to heat exchange with heating is subjected to evaporation in the top condenser after removal and before heating.
  • the vaporization of the condensed impure argon used as the circulating flow can also take place in the heat exchanger block.
  • the bottom product formed in the rectification or the part thereof which is subjected to the heat exchange with heating can, after removal from the rectification column and before evaporation in the top condenser, be throttled in particular to a pressure level which is based on a target temperature (of the bottom product or of said portion) after evaporation in the top condenser.
  • This configuration serves in particular to maintain the pressure in the rectification column, specifically by appropriately adjusting the overheating of the argon product (to be evaporated in the top condenser) at the outlet of the top condenser.
  • the pressure is determined in particular by means of a corresponding TIC control (which adjusts a corresponding valve and records the temperature of the evaporated fluid).
  • the pressure in the column depends on the selected temperature difference for the particular design of the top condenser. Furthermore, heat exchange can be performed before and after evaporation in the top condenser. In other words, a condensed stream of material fed to the top condenser can be subjected to a heat exchange in a corresponding heat exchanger (subcooler) with an evaporated stream of material drawn off from the top condenser, i.e. a heat exchange of the same fluid “with itself” takes place.
  • the top condenser can be designed as a bath evaporator, the bottom product formed in the rectification or the part thereof which is subjected to evaporation in the top condenser being fed into a liquid bath of the top condenser. In this case, the evaporation takes place in a liquid bath in which a heat exchanger block is arranged at least partially submerged.
  • the top condenser can also be designed as a forced-feed condenser evaporator, the bottom product formed in the rectification or the part thereof which is subjected to evaporation in the head condenser being forced through passages in the head condenser without being fed into a liquid bath.
  • a top gas formed in the rectification can be condensed in particular in the top condenser and then returned to a first portion as reflux in the rectification and a second portion subjected to heat exchange with heating and removed from the process (as residual gas).
  • the condensation in the top condenser can in particular also take place in corresponding (separate) passages of the heat exchanger block mentioned, which is designed, for example, as a forced-guide condenser evaporator.
  • the treatment mentioned several times can in particular include adsorptive purification to remove moisture and carbon dioxide, in particular temperature swing adsorption, with the second portion of the top gas formed in the rectification, which is subjected to the heat exchange with heating and is carried out from the process, after heating and before its removal from the process, can be used in part or in full as regeneration gas in adsorptive purification.
  • heating can also take place.
  • the circulating stream can be combined with the impure argon discharged from the process step or with the part thereof subjected to compression upstream of the compression or in the compression.
  • this circulatory flow can be throttled in particular to an inlet pressure of the compressor used, in the latter case, which can include in particular the feed between different compressor stages or via an intermediate feed in a screw compressor, a corresponding throttling can be dispensed with.
  • the rectification column used in the context of the present invention has, in particular, two separating sections arranged one above the other, the first part of the impure argon condensate, which is fed into the rectification column in condensed form, being fed into the rectification column between the separating sections.
  • the recycle stream is formed in an amount which is 25 to 75% of an amount of the impure argon discharged from the process step or the part thereof subjected to compression.
  • the amount can also be 40 to 60% or about 50%, for example.
  • compression can be carried out at a pressure level of 4 to 6 bar
  • the rectification column can be operated at a pressure level of 2.5 to 5 bar
  • the top condenser can be operated at an evaporation pressure level of 1.1 to 3 bar
  • Evaporation rooms are operated.
  • Specific examples are about 5.0 bar for the compression pressure level, about 3.5 bar for the rectification column, and about 1.3 and 2.2 bar (for the recycle stream and the argon product or the bottom product of the rectification column) for the head condenser or its evaporation space.
  • the process can also be carried out at pressures which are reduced or increased in relation to the values mentioned, for example a pressure of from 9 to 15 bar in the rectification. The other pressures are adjusted accordingly.
  • the pure argon or the part thereof that is fed back to the process step can be compressed from the evaporation pressure level to a suitable pressure level, for example a pressure level of about 12 bar.
  • the heat exchange envisaged within the scope of the present invention can also be carried out with the evaporation of liquid nitrogen, which in this way leads to increased cooling and compensates for cold losses in the system.
  • the heat exchange can be performed using a single heat exchanger or using multiple heat exchangers thermally coupled, as discussed.
  • the impure argon processed within the scope of the present invention can in particular contain 90 to 99.5% argon and otherwise 0.1 to 9% nitrogen, 100 to 2000 ppm carbon monoxide, 500 to 5000 ppm hydrogen and/or 10 to 800 ppm carbon dioxide .
  • the impure argon processed in the context of the present invention contains 99% argon and otherwise 0.5% nitrogen, 1000 ppm carbon monoxide, 2500 ppm hydrogen and 50 ppm carbon dioxide and is at a rate of 100 to 500 standard cubic meters per hour, for example 100 up to 500 standard cubic meters per hour.
  • the impure argon can in principle be oxygen-free or essentially oxygen-free, but it can also, for example, as mentioned, have an oxygen content of 100 to 1000 ppm.
  • the impure argon contains about 500 ppm oxygen. This oxygen can be at least partially removed by the catalytic reaction with hydrogen.
  • the pure argon provided within the scope of the present invention can in particular contain more than 99.999% argon and otherwise 0.001 to 0.1 ppm carbon monoxide, 0.009 to 0.9 ppm oxygen and less than 10 ppb nitrogen. In a specific example, it contains less than 0.1 ppm carbon monoxide, 0.5 ppm oxygen and less than 10 ppb nitrogen and is provided at a rate of 200 to 300 standard cubic meters per hour, for example 280 standard cubic meters per hour.
  • the system has means that are set up to carry out a method according to one of the configurations explained.
  • FIG. 1 illustrates a method according to one embodiment of the invention in a simplified, schematic representation.
  • FIG. 2 illustrates a method according to an embodiment of the invention in a simplified, schematic representation.
  • FIG. 3 illustrates a method according to an embodiment of the invention in a simplified, schematic representation.
  • FIGS. 1, 2 and 3 methods for carrying out an industrial process denoted overall by 100, 200 and 300 according to embodiments of the invention are illustrated in a simplified, schematic representation.
  • impure argon in the form of a stream A is carried out from a process step 10 of the type explained above.
  • the impure argon, i.e. material flow A is subjected to processing, generally designated 20, to obtain pure argon in the form of material flow B, with the pure argon or part thereof, ie material flow B or part thereof, being fed back to process step 10 , as shown in Figures 1 and 2 not separately.
  • FIGS. 1 and 2 (methods 100 and 200) on the one hand and FIG. 3 (method 300) on the other hand arise in the processing of the impure argon, ie the material flow A, as explained below.
  • the different processing shown in FIG. 3 (method 300) compared to FIG. 2 (method 200) can also be used in the method illustrated in FIG. 1 (method 100).
  • the processing 20 includes a compression 21 with after-cooling not specifically designated (the latter only in the methods 100 and 200 according to FIGS. 1 and 2), a heat exchange 22 between the material flows explained below, in particular in a common heat exchanger or in several thermally coupled heat exchangers , and a rectification 23 in a rectification column, which is again designated separately as 24 and has a bottom evaporator 25 and a top condenser 26 .
  • a top condenser 26 is used, which is arranged in a liquid bath 26a into which the bottom liquid of the rectification column 24 is fed
  • a forced-flow Condenser evaporator used ie the bottom liquid of the rectification column 24 is forced out there through the top condenser 26 and does not get into a corresponding liquid bath.
  • the running from the process step 10 impure argon or a part thereof, ie the stream A, the compression 21, with cooling the heat exchange 22, and subjected to at least partial condensation in the bottom evaporator 25 to obtain an impure argon condensate in the form of a stream C.
  • the impure argon condensate, i.e. stream C is fed into the rectification column 24 in a first condensed form in the form of a stream D and in a second part in the form of a stream E of evaporation in the (each with expansion via valves not provided with separate reference numbers).
  • Top condenser 26 subjected.
  • the vaporized second portion of the impure argon condensate or a portion thereof is fed back to the rectification 23 in the form of a stream F as a circulating stream.
  • the circulating flow, ie the material flow F is subjected to at least a part of the compression 21 together with the impure argon carried out from the process step 10 or the part thereof subjected to the compression 21, ie the material flow A.
  • the material flow F is combined upstream of the compression 21 with the impure argon carried out from the process step 10 or with the part thereof subjected to the compression 21, ie the material flow A.
  • the rectification column 24 has two separating sections 29 arranged one above the other, the first part of the impure argon condensate, which is fed into the rectification column 24 in condensed form, ie the stream D, being fed into the rectification column 24 between the separating sections 29 .
  • the pure argon, i.e. stream B, is provided in the form of a stream G using a bottom product formed in rectification 23, with the bottom product formed in rectification 23 or a part thereof, i.e. stream G, being subjected to heat exchange 22 while being heated . Furthermore, the bottom product formed in rectification 23 or the part thereof that is subjected to heat exchange 22 with heating, i.e. material flow G, is subjected to evaporation in top condenser 26 after removal and before heating, and in the example shown before and after the Evaporation in the top condenser 26 subject to a mutual heat exchange 28, ie a corresponding heat exchange 28 "against itself".
  • the method 100 according to Figure 1 differs on the one hand from the methods 200 and 300 according to Figures 2 and 3 on the other hand with regard to the separation 10, in particular in the design of the top condenser 26.
  • the bottom product After removal and before evaporation in the head condenser 26, the bottom product, which is evaporated there, can be throttled by means of a valve 26b (correspondingly designated only in Figure 3) to a pressure level that is based on a target temperature after evaporation in the head condenser 26 is set.
  • this configuration serves in particular to maintain the pressure in the rectification column 24.
  • the pressure can be adjusted in particular by means of a corresponding TIC control (which adjusts the valve 26b and records the temperature of the evaporated fluid, i.e. the material flow E after the evaporation).
  • Corresponding measures are optional, but can nonetheless be used in all configurations of the present invention.
  • the heat exchange 22 is typically not carried out in the embodiment according to FIG. It is also optional in the other configurations.
  • a top gas formed in rectification 23 is condensed in a first proportion in top condenser 26 and returned to rectification 23 in the form of a stream H as reflux, while a second proportion in the form of a stream K is subjected to heat exchange 22 with heating and from the Executed method and, for example, ultimately released to the environment (atmosphere ATM).
  • treatment 20 includes adsorptive purification 27, to which material flow A or a material flow formed from it is subjected before it is cooled by heat exchanger 22, material flow K being partially used as regeneration gas in the adsorptive after heating in heat exchanger 22 Cleaning 27 is used, especially after further heating in a heater not designated separately.
  • FIGS. 1 and 2 relate to the processing of oxygen-free or essentially oxygen-free impure argon
  • FIG. 3 method 300
  • He can do that Substance stream A together with the circuit stream F after the compression, in particular without subsequent post-cooling to provide the required heat of reaction, are subjected to a catalytic conversion 30 of oxygen with hydrogen to form water. If the hydrogen content of the impure argon is not sufficient, external hydrogen can be added, as illustrated in the form of a dashed H2 material flow. After the catalytic conversion 30, cooling 31 can be carried out in a water separator 32 for the condensative removal of water H2O. Residual water can be removed in the adsorptive cleaning 27.
  • the pure argon or the part thereof that is fed back to the process step 10 is subjected to a suitable compression 30 in all illustrated embodiments.
  • the heat exchange 22 is also carried out with the evaporation of liquid nitrogen LIN, which is provided in the form of a stream L and can then be used, like the stream K, as regeneration gas.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

La présente invention concerne un procédé pour effectuer un processus industriel (100), où de l'argon impur est déversé à partir d'une étape de traitement (10), où l'argon impur ou une partie de celui-ci est traité (20) de manière à obtenir de l'argon pur, et où l'argon pur ou une partie de celui-ci est renvoyé à l'étape de traitement (10). Le traitement (20) comprend une compression (21), un échange thermique (22) et une rectification (23) dans une colonne de rectification (24), colonne ayant un rebouilleur (25) et un condenseur de tête (26), l'argon impur déversé depuis l'étape de traitement (10), ou une partie de celui-ci, est soumis à la compression (21), à l'échange thermique (22) avec refroidissement, et à au moins une condensation partielle dans le rebouilleur (25) pour obtenir un condensat d'argon impur, une première partie du condensat d'argon impur étant introduite dans la colonne de rectification (24) sous une forme condensée, et une seconde partie du condensat d'argon impur étant soumise à une évaporation dans le condenseur de tête (26), et la seconde partie évaporée du condensat d'argon impur, ou une partie de celle-ci, étant renvoyée à la rectification (23) en tant que courant de circulation. Il est prévu dans la portée de l'invention que le courant de circulation soit au moins en partie soumis à la compression (21) conjointement avec l'argon impur déversé depuis l'étape de traitement (10) ou conjointement avec la partie de celui-ci qui a été soumise à la compression (21). L'argon pur est fourni en utilisant un produit de fond qui est formé lors de la rectification (23). Après l'élimination et avant le chauffage, le produit de fond qui est formé lors de la rectification (23) ou une partie de celui-ci est soumis à un chauffage lors de l'échange thermique (22), et le produit de fond formé lors de la rectification (23) ou une partie de celui-ci qui a été soumis à un chauffage lors de l'échange thermique (22) est soumis à une évaporation dans le condenseur de tête (26). La présente invention porte également sur une installation correspondante.
PCT/EP2021/025248 2020-08-03 2021-07-07 Procédé et installation pour effectuer un processus industriel WO2022028732A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1478995A (fr) 1965-05-07 1967-04-28 Fleur Corp Procédé de séparation des éléments d'un mélange de gaz
EP0761596A1 (fr) 1995-09-05 1997-03-12 Teisan Kabushiki Kaisha Procédé et dispositif pour la purification d'argon
US5706674A (en) 1997-01-17 1998-01-13 Air Products And Chemicals, Inc. Argon recovery from silicon crystal furnace
EP1287302B1 (fr) 2000-05-31 2005-09-21 Linde AG Condenseur a bain a plusieurs etages
FR3020668A3 (fr) 2015-04-27 2015-11-06 Air Liquide Procede de purification d'oxygene basse purete provenant d'un appareil de separation par adsorption
DE102018006002B3 (de) 2018-07-28 2019-11-07 Messer Group Gmbh Verfahren zum Wiederverwerten von Argon

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1478995A (fr) 1965-05-07 1967-04-28 Fleur Corp Procédé de séparation des éléments d'un mélange de gaz
EP0761596A1 (fr) 1995-09-05 1997-03-12 Teisan Kabushiki Kaisha Procédé et dispositif pour la purification d'argon
US5706674A (en) 1997-01-17 1998-01-13 Air Products And Chemicals, Inc. Argon recovery from silicon crystal furnace
EP1287302B1 (fr) 2000-05-31 2005-09-21 Linde AG Condenseur a bain a plusieurs etages
FR3020668A3 (fr) 2015-04-27 2015-11-06 Air Liquide Procede de purification d'oxygene basse purete provenant d'un appareil de separation par adsorption
DE102018006002B3 (de) 2018-07-28 2019-11-07 Messer Group Gmbh Verfahren zum Wiederverwerten von Argon

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
"Industrial Gases Processing", 2006, WILEY-VCH
"The recovery and recycling of high purity argon in the semiconductor industry", AICHE NATIONAL MEETING, 6 March 1988 (1988-03-06), pages 1 - 19
O'BRIEN J V ET AL: "The recovery and recycling of high purity argon in the semiconductor industry", AICHE NATIONAL MEETING,, 6 March 1988 (1988-03-06), pages 1 - 19, XP002957420 *

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