EP1605198A2 - Verfahren zur Herstellung von flüssigem Carbondioxide, und Benutzung zur Herstellung von superkritischem Carbondioxide - Google Patents

Verfahren zur Herstellung von flüssigem Carbondioxide, und Benutzung zur Herstellung von superkritischem Carbondioxide Download PDF

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Publication number
EP1605198A2
EP1605198A2 EP05300449A EP05300449A EP1605198A2 EP 1605198 A2 EP1605198 A2 EP 1605198A2 EP 05300449 A EP05300449 A EP 05300449A EP 05300449 A EP05300449 A EP 05300449A EP 1605198 A2 EP1605198 A2 EP 1605198A2
Authority
EP
European Patent Office
Prior art keywords
carbon dioxide
process according
container
temperature
application
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.)
Withdrawn
Application number
EP05300449A
Other languages
English (en)
French (fr)
Other versions
EP1605198A3 (de
Inventor
Vincent Boisdon
Harald Winter
Christophe Magneney
Olivier Deretz
Dominique Bras
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
LAir Liquide SA a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude, LAir Liquide SA a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude filed Critical LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Publication of EP1605198A2 publication Critical patent/EP1605198A2/de
Publication of EP1605198A3 publication Critical patent/EP1605198A3/de
Withdrawn legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C7/00—Methods or apparatus for discharging liquefied, solidified, or compressed gases from pressure vessels, not covered by another subclass
    • F17C7/02—Discharging liquefied gases
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C13/00—Details of vessels or of the filling or discharging of vessels
    • F17C13/02—Special adaptations of indicating, measuring, or monitoring equipment
    • F17C13/025—Special adaptations of indicating, measuring, or monitoring equipment having the pressure as the parameter
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C9/00—Methods or apparatus for discharging liquefied or solidified gases from vessels not under pressure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2221/00—Handled fluid, in particular type of fluid
    • F17C2221/01—Pure fluids
    • F17C2221/013—Carbon dioxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
    • F17C2223/01—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the phase
    • F17C2223/0146—Two-phase
    • F17C2223/0153—Liquefied gas, e.g. LPG, GPL
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
    • F17C2223/03—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the pressure level
    • F17C2223/036—Very high pressure (>80 bar)
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2225/00—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel
    • F17C2225/01—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel characterised by the phase
    • F17C2225/0107—Single phase
    • F17C2225/0115—Single phase dense or supercritical, i.e. at high pressure and high density
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2225/00—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel
    • F17C2225/04—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel characterised by other properties of handled fluid after transfer
    • F17C2225/042—Localisation of the filling point
    • F17C2225/046—Localisation of the filling point in the liquid
    • F17C2225/047—Localisation of the filling point in the liquid with a dip tube
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
    • F17C2227/03—Heat exchange with the fluid
    • F17C2227/0337—Heat exchange with the fluid by cooling
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
    • F17C2250/06—Controlling or regulating of parameters as output values
    • F17C2250/0605—Parameters
    • F17C2250/0626—Pressure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
    • F17C2250/06—Controlling or regulating of parameters as output values
    • F17C2250/0605—Parameters
    • F17C2250/0631—Temperature

Definitions

  • the present invention relates to a process for producing dioxide of free-standing liquid carbon, under stabilized pressure, at a point of application one end of a power line. It also concerns a using said process to produce supercritical carbon dioxide.
  • the invention finds a particularly advantageous application in the field of preparative chromatography by supercritical extraction of active ingredients in fine chemicals and pharmaceuticals, as well as in the field of the preparation of wafers of semiconductor components.
  • the technologies implemented up to now consist in taking CO 2 carbon dioxide in the gas phase of a CO 2 storage tank, the interest being to avoid taking directly the non-volatile impurities contained in the CO 2 storage tank. liquid phase.
  • the gaseous CO 2 is then liquefied by compression and then fed to the chromatography apparatus.
  • this technology does not guarantee satisfactory thermodynamic conditions at the point of application and can cause malfunctions of the high pressure pump of the chromatography apparatus.
  • the sampling in the gas phase leads to an accumulation of non-volatile organic compounds in the storage tank, which are not easy to eliminate by cleaning operations which are complex and expensive.
  • this method obliges the CO 2 supplier to fill the tank at the customer site, his limit of liability then stopping at the CO 2 at the outlet of the delivery truck's delivery flange. The carbon dioxide supplier can not then meet the commitment request in terms of quality up to the point of application.
  • the technical problem to be solved by the object of this invention is to provide a method of producing carbon dioxide liquid, under stabilized pressure, at a point of application at a end of a power line, which would satisfy the thermodynamic and purity requirements mentioned above, and this to the point of application, that is to say, in the example of preparative chromatography, at the inlet of the high pressure pump carbon dioxide in the supercritical phase.
  • the container from which the dioxide originates carbon to be delivered contains carbon dioxide with the same pressure than that of the carbon dioxide that will be delivered to the point application.
  • This pressure within the container is kept constant by temperature control.
  • This type of container is usually a bottle of carbon dioxide whose temperature is controlled by its storage in a thermostated room.
  • the liquid carbon dioxide taken from the thermostatic container is cooled in the supply line so that its pressure remains constant and identical to that of the CO 2 in the container, which is also that of CO 2 at the point of application.
  • the choice of the cooling temperature value is such that at the point of application, this temperature is below the boiling point of the carbon dioxide at the application pressure.
  • the conditions of stability of the pressure of carbon dioxide in the supply line are made due to the control of the temperature of the storage container, upstream of the line.
  • the elimination of the risk of presence of bubbles upstream of the high pressure pump is obtained by controlling the temperature of the carbon dioxide, generally by cooling. Indeed, this control makes it possible to place the thermodynamic point of CO 2 outside the boiling curve, in the liquid phase of carbon dioxide. For example, a cooling around -5 ° C for a pressure between 60 and 70.10 5 Pa (60 and 70 bar) ensures this absence of bubbles.
  • the CO 2 removal in the storage container is such that the CO 2 is directly taken from the liquid phase.
  • the removal of gaseous CO 2 in the gaseous atmosphere of the bottle, for example, and its compression at a pressure of the order of 80 ⁇ 10 5 Pa (80 bar) and a non-controlled temperature as in the prior art can lead to a feed of the high pressure pump of the chromatograph with a pressurized gas that is not compatible with the suction conditions of the pump, the sizing of the cooler is not sufficient to ensure the liquefaction of the supercharged gas.
  • the removal of the liquid phase also avoids any risk accumulation of non-volatile compounds in conditioned storage, which ensures a stability in the time of the purity of the product and the state packaging.
  • an advantageous arrangement of the method according to the invention is that carbon dioxide is circulated in the line suction supply from the point of application.
  • FIG. 1 is a diagram of an installation implementing the process for the preparation of carbon dioxide according to the invention.
  • FIG. 2 is a liquid-vapor equilibrium diagram of the carbon.
  • FIG. 1 shows an installation intended to supply, from at least one container 10, free liquid carbon dioxide and under a stabilized pressure at an application point 21 at one end of a feed line.
  • a high pressure pump 3 Downstream of this application point 21 is a high pressure pump 3 provided, for example, to bring the CO 2 from the liquid phase to a supercritical phase in an application to an extraction chromatograph of active principles.
  • the containers used may be storage tanks of type packaged such as frames, bottles, etc., or in bulk tank, isolated or not with vacuum or polyurethane insulation.
  • the corresponding container is fed and put into pressure by means of compression of the liquid carbon dioxide.
  • the containers are generally delivered at an ambient temperature of about 20 ° C. and at a pressure of 60 to 70 ⁇ 10 5 Pa (60 to 70 bars) corresponding to the equilibrium between the liquid CO 2 and the gaseous CO 2 (FIG. 2). at this temperature. Beyond 70.10 5 Pa (70 bar), a pressure switch, not shown, triggers the shutdown of the heating system of the container 10 for security purposes.
  • pressurization control and stabilization means are provided: they consist of means for controlling the temperature of the carbon dioxide in the container 10.
  • said temperature control means are constituted by a convector 11 placed in a thermostatically controlled box 12. The convector 11 is regulated from a pressure sensor 22 located on the line 20 of food.
  • the liquid carbon dioxide is taken from the liquid phase of the container 10 and introduced into the feed line via a dip tube 13.
  • the liquid carbon dioxide from the container 10 is cooled, while maintaining its pressure at the value of the pressure in the container 10 at a temperature such that at point 21 the liquid CO 2 temperature is lower at the boiling temperature of the carbon dioxide at this pressure ( Figure 2), this to prevent any formation of bubbles.
  • this cooling is carried out in a coil 23 placed in a bath 24 at a controlled temperature.
  • cooling is effected to a temperature of -5 ° C, for example, or any other temperature thermodynamically placing the CO 2 inside the liquid phase in the boiling diagram.
  • the choice of the cooling temperature must take into account the heat losses that may occur between the location of the coil 23 and the point 21 of application. The further the cooling means will be away from the point of application, the more liquid carbon dioxide will have to be cooled to a lower temperature.
  • the circulation of carbon dioxide in the supply line 20 is suctioned from point 21 application. This avoids any introduction of impurities into the line.
  • the liquid carbon dioxide is subjected to purification operations, in particular filtration using for example porous membranes 25, ceramic or sintered glass, whose cutoff threshold is between 0.1 and 5 microns.
  • the liquid CO 2 is dried by absorption using zeolites 26, for example.

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Non-Alcoholic Beverages (AREA)
EP05300449A 2004-06-11 2005-06-03 Verfahren zur Herstellung von flüssigem Carbondioxide, und Benutzung zur Herstellung von superkritischem Carbondioxide Withdrawn EP1605198A3 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0406335A FR2871549B1 (fr) 2004-06-11 2004-06-11 Procede de production de gaz carbonique liquide et application a la production de gaz carbonique supercritique
FR0406335 2004-06-11

Publications (2)

Publication Number Publication Date
EP1605198A2 true EP1605198A2 (de) 2005-12-14
EP1605198A3 EP1605198A3 (de) 2008-01-23

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP05300449A Withdrawn EP1605198A3 (de) 2004-06-11 2005-06-03 Verfahren zur Herstellung von flüssigem Carbondioxide, und Benutzung zur Herstellung von superkritischem Carbondioxide

Country Status (2)

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EP (1) EP1605198A3 (de)
FR (1) FR2871549B1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN120650626A (zh) * 2025-06-27 2025-09-16 上海宇肇管道工程建设有限公司 气体自动充装装置及其控制方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4751822A (en) 1986-02-07 1988-06-21 Carboxyque Francaise Process and plant for supplying carbon dioxide under high pressure
FR2781037A1 (fr) 1998-07-10 2000-01-14 Messer France Installation de regulation fonctionnelle d'une unite de stockage-distribution de dioxyde de carbone

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE495795C (de) * 1928-05-05 1930-04-12 Pierre Polard Verfahren zum Foerdern fluessiger Gase durch einen Pumpvorgang
US3282305A (en) * 1964-02-20 1966-11-01 Gen Dynamics Corp Cylinder filling apparatus
DE3300297C2 (de) * 1983-01-07 1986-07-10 Danfoss A/S, Nordborg Vorrichtung zum Fördern von Flüssiggas
US5850876A (en) * 1990-01-08 1998-12-22 Pyrozone Pty. Ltd. Apparatus and system for the storage and supply of liquid CO2 at low pressure for extinguishing of fires
US5193991A (en) * 1991-03-01 1993-03-16 Suprex Corporation Liquefied carbon dioxide pump
US5761911A (en) * 1996-11-25 1998-06-09 American Air Liquide Inc. System and method for controlled delivery of liquified gases
DE10205130A1 (de) * 2002-02-07 2003-08-28 Air Liquide Gmbh Verfahren zum unterbrechungsfreien Bereitstellen von flüssigem, unterkühltem Kohlendioxid bei konstantem Druck oberhalb von 40 bar sowie Versorgungssystem

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4751822A (en) 1986-02-07 1988-06-21 Carboxyque Francaise Process and plant for supplying carbon dioxide under high pressure
FR2781037A1 (fr) 1998-07-10 2000-01-14 Messer France Installation de regulation fonctionnelle d'une unite de stockage-distribution de dioxyde de carbone

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN120650626A (zh) * 2025-06-27 2025-09-16 上海宇肇管道工程建设有限公司 气体自动充装装置及其控制方法

Also Published As

Publication number Publication date
FR2871549B1 (fr) 2006-08-04
FR2871549A1 (fr) 2005-12-16
EP1605198A3 (de) 2008-01-23

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