EP1547637A2 - Dynamic conditioning of gaseous mixtures at high pressures, preferably of mixtures N2O/O2 - Google Patents

Dynamic conditioning of gaseous mixtures at high pressures, preferably of mixtures N2O/O2 Download PDF

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Publication number
EP1547637A2
EP1547637A2 EP20040300773 EP04300773A EP1547637A2 EP 1547637 A2 EP1547637 A2 EP 1547637A2 EP 20040300773 EP20040300773 EP 20040300773 EP 04300773 A EP04300773 A EP 04300773A EP 1547637 A2 EP1547637 A2 EP 1547637A2
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EP
European Patent Office
Prior art keywords
compound
pressure
gaseous
bar
content
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Granted
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EP20040300773
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German (de)
French (fr)
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EP1547637A3 (en
EP1547637B1 (en
Inventor
François Simondet
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Air Liquide Sante International SA
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Publication of EP1547637A3 publication Critical patent/EP1547637A3/en
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Publication of EP1547637B1 publication Critical patent/EP1547637B1/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/10—Mixing gases with gases
    • B01F23/19—Mixing systems, i.e. flow charts or diagrams; Arrangements, e.g. comprising controlling means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/80—Forming a predetermined ratio of the substances to be mixed
    • B01F35/88—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise
    • 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
    • F17C2221/03—Mixtures
    • 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
    • F17C2223/0107—Single phase
    • F17C2223/0123—Single phase gaseous, e.g. CNG, GNC
    • 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
    • F17C2223/033—Small pressure, e.g. for liquefied gas
    • 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
    • F17C2223/035—High pressure (>10 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
    • F17C2225/0123—Single phase gaseous, e.g. CNG, GNC
    • 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
    • F17C2225/03—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel characterised by the pressure level
    • F17C2225/036—Very high pressure, i.e. above 80 bars
    • 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
    • F17C2265/00—Effects achieved by gas storage or gas handling
    • F17C2265/02—Mixing fluids
    • F17C2265/025—Mixing fluids different fluids
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/0318—Processes

Definitions

  • the present invention relates to a dynamic process for conditioning gas mixtures, in particular O 2 / N 2 O mixtures containing a proportion of N 2 O greater than or equal to 30% by volume for a pressure of at least 170 bars.
  • the so-called gravimetric conditioning method is generally used to condition gaseous mixtures based on liquefied gases, such as N 2 O or CO 2 , or mixtures of air gases, such as O 2 , N 2 , Ar or He .
  • this method of manufacture has the drawbacks of leading to a high rate of manufacturing waste, after analytical control, an unproductive manufacturing method because the containers must be filled to the unit, a cycle of packaging rolling penalizing times production, and at a high cost of analytical control.
  • the quantities of gas introduced are therefore controlled by measuring the pressure and gas temperature.
  • the determination of gas contents is based on two instruments which add up their measurement inaccuracies.
  • the location of the points measuring system on the packaging plant does not allow direct access to physical quantities sought, namely temperature and pressure are usually measured on the conditioning ramp by a temperature sensor or a sensor of pressure.
  • the values thus measured are only approximations but not effective measurements of the temperature or pressure inside the containers conditioning.
  • the dynamic gas mixing method makes it possible to overcome some of these problems and disadvantages.
  • This method described, in particular by the document EP-A-1174178 consists in filling the bottles with the gas mixture in its final composition expected from the beginning to the end of the filling sequence.
  • the mixture is made in upstream of the conditioning ramp in a very low mixing chamber dimension where are introduced continuously the various gaseous constituents entering the composition of the final mixture.
  • the quantities introduced for each gas are controlled by a flow meter mass installed on each line of gas used in the composition of the mixture to be produced.
  • a set of several control valves makes it possible to control the flow of gas through the action of an automatic control system. Counting the masses by mass flow meter makes it possible to overcome the uncertainties of measurements and the hazards of realization related to the inaccuracies on the quantities mentioned above.
  • Conditioning with a dynamic mixer is however accompanied in in some cases, a relaxation of the gas downstream of the mixing chamber and a lowering of the temperature of the gases below the temperature of demixing or demixing, which can be explained by the fact that the line downstream of the chamber is at the same pressure as the containers brought back to atmospheric pressure.
  • the gas circulation is then two-phase in the packaging ramps to the bottles.
  • the mixture is thus always maintained in the gaseous state, the homogeneity of the mixture is kept and the differences in levels are sufficiently low to control all the bottles by analysis of a single bottle taken from the ramp of conditioning.
  • the final pressure is limited by the pressurization of N 2 O at around 170 bars.
  • the N 2 O must then be heated to rise to higher pressures and this then generates its passage to the supercritical state.
  • the reheating temperature is also limited by the decomposition temperature of N 2 O and this, especially as some metals of the packaging device and the bottle, such as silver, platinum, cobalt, copper and nickel oxides, are catalysts of the reaction.
  • the problem to be solved is therefore to improve the packaging process with dynamic mixer, in particular the method described in document EP-A-1174178, so as to be able to produce dynamic packaging of gaseous mixtures at pressures greater than 170 bar, in particular N 2 O / O 2 medical gas mixtures whose N 2 O content is greater than or equal to 30% by volume.
  • the invention also relates to a method for packaging gas containers, in which a gas mixture containing a first and a second gaseous compound is produced and introduced into a plurality of packaging containers, said gaseous mixture being produced by use of a manufacturing method according to the invention, preferably the gaseous mixture consists of oxygen and nitrous oxide (N 2 O).
  • the first step of carrying out premixing with a dynamic mixer makes it possible to obtain an O 2 / N 2 O premix with an accuracy of ⁇ 0.5%.
  • the dilution by pressure rise makes it possible to obtain a precise O 2 / N 2 O mixture at a high pressure, that is to say up to 250 to 300 bar or more, preferably by monitoring the temperature / pressure pair by means of one or more pressure and temperature sensors, the precision resulting from the use of a mass flowmeter.
  • control of the introduction of oxygen, during the dilution stage with pressure can be carried out by mass counting at the mass flow meter, which ensures the realization of a very precise mixture at high pressure.
  • the homogenization of the mixture during the second preparation stage is generally correctly; nevertheless, it can be accelerated, if necessary, by a packaging cycle after filling and / or using a dip tube which allows to introduce the oxygen at the bottom of each container during filling.
  • the advantages of the method for producing the O 2 / N 2 O mixture include an accuracy and homogeneity of the gaseous compositions produced; a final pressure of the mixture which is no longer limited by the conditioning method; or a lack of demixing at low temperatures for full bottles.
  • the method of preparation is not limited to the case of O 2 / N 2 O mixtures. It may be generalized to other gases or mixtures containing one or more gases, such as CO 2 , N 2 O, O 2 , N 2 , Hey ...

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)
  • Treating Waste Gases (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Accessories For Mixers (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Silicon Compounds (AREA)

Abstract

Method for preparing gas mixtures (A) of at least two components, i.e. oxygen, nitrogen, helium, carbon dioxide, nitrous oxide and carbon monoxide, in desired proportions. Method for preparing gas mixtures (A) of at least two components, i.e. oxygen, nitrogen, helium, carbon dioxide, nitrous oxide and carbon monoxide, in desired proportions comprises: (a) dynamic premixing, in predetermined proportions, of the components to form a premix at pressure, P1, not over 200 bar, containing an intermediate content (Ti) of second component that is greater than its final content (Tf); (b) increasing the pressure of the premix by adding more first component; and (c) stopping the addition when the mixture reaches a second pressure P2 that is above P1 and greater than 170 bar, and has content of second component Tf. An independent claim is also included for a process for filling gas containers with (A) produced by the new method.

Description

La présente invention concerne un procédé de conditionnement en dynamique des mélanges gazeux, en particulier de mélanges O2/N2O contenant une proportion de N2O supérieure ou égale à 30 % en volume pour à une pression d'au moins 170 bars.The present invention relates to a dynamic process for conditioning gas mixtures, in particular O 2 / N 2 O mixtures containing a proportion of N 2 O greater than or equal to 30% by volume for a pressure of at least 170 bars.

Actuellement, il existe plusieurs méthodes de conditionnement de mélanges gazeux dans des récipients sous pression, telles des bouteilles de gaz.Currently, there are several methods of conditioning gas mixtures in pressure vessels, such as gas cylinders.

Ainsi, la méthode de conditionnement dite gravimétrique est généralement utilisée pour conditionner des mélanges gazeux à base de gaz liquéfiés, tels N2O ou CO2, ou des mélanges de gaz de l'air, tels O2, N2, Ar ou He. Cependant, cette méthode de fabrication présente les inconvénients de conduire à un taux important de rebut de fabrication, après contrôle analytique, un mode de fabrication peu productif car les récipients doivent être remplis à l'unité, un cycle de roulage des emballages pénalisant les temps de production, et à un coût de contrôle analytique élevé.Thus, the so-called gravimetric conditioning method is generally used to condition gaseous mixtures based on liquefied gases, such as N 2 O or CO 2 , or mixtures of air gases, such as O 2 , N 2 , Ar or He . However, this method of manufacture has the drawbacks of leading to a high rate of manufacturing waste, after analytical control, an unproductive manufacturing method because the containers must be filled to the unit, a cycle of packaging rolling penalizing times production, and at a high cost of analytical control.

Par ailleurs, on connaít aussi la méthode de conditionnement séquentiel gravimétrique et pression/température. Toutefois, avec cette méthode, les mélanges réalisés dans les différentes bouteilles d'une même rampe de production présentent souvent des écarts de composition finale. Pour éviter cela, il convient de respecter des temps de stabilisation et de mise en équilibre des pressions qui pénalisent la productivité globale.Moreover, the sequential conditioning method is also known. gravimetric and pressure / temperature. However, with this method, mixtures made in the different bottles of the same production ramp often have final composition differences. To avoid this, it is necessary to respect stabilizing and balancing pressures that penalize overall productivity.

Dans le cas d'autres méthodes classiques de conditionnement des mélanges, les quantités de gaz introduites sont donc contrôlées par mesure de la pression et de la température des gaz. Or, la détermination des teneurs de gaz est basée sur deux instruments de mesure qui additionnent leurs imprécisions de mesure. De plus, l'emplacement des points de mesure sur l'installation de conditionnement ne permet pas d'accéder directement aux grandeurs physiques recherchées, à savoir la température et la pression sont généralement mesurées sur la rampe de conditionnement par une sonde de température ou un capteur de pression. Cependant, les valeurs ainsi mesurées ne sont que des approximations mais pas des mesures effectives de la température ou de la pression régnant à l'intérieur les récipients de conditionnement. In the case of other conventional methods of mixing mixtures, the quantities of gas introduced are therefore controlled by measuring the pressure and gas temperature. However, the determination of gas contents is based on two instruments which add up their measurement inaccuracies. In addition, the location of the points measuring system on the packaging plant does not allow direct access to physical quantities sought, namely temperature and pressure are usually measured on the conditioning ramp by a temperature sensor or a sensor of pressure. However, the values thus measured are only approximations but not effective measurements of the temperature or pressure inside the containers conditioning.

La méthode de mélange des gaz en dynamique permet de palier une partie de ces problèmes et inconvénients. Cette méthode décrite, notamment par le document EP-A-1174178, consiste à remplir les bouteilles avec le mélange gazeux dans sa composition finale attendue du début jusqu'à la fin de la séquence de remplissage. Le mélange est réalisé en amont de la rampe de conditionnement dans une chambre de mélange de très faible dimension où sont introduits en continu les différents constituants gazeux entrant dans la composition du mélange final.The dynamic gas mixing method makes it possible to overcome some of these problems and disadvantages. This method described, in particular by the document EP-A-1174178, consists in filling the bottles with the gas mixture in its final composition expected from the beginning to the end of the filling sequence. The mixture is made in upstream of the conditioning ramp in a very low mixing chamber dimension where are introduced continuously the various gaseous constituents entering the composition of the final mixture.

Les quantités introduites pour chaque gaz sont contrôlées par un débitmètre massique installé sur chaque ligne de gaz entrant dans la composition du mélange à réaliser. Par ailleurs, un ensemble de plusieurs vannes de régulation permet de contrôler le débit des gaz grâce à l'action d'un système de régulation automatique. Le comptage des masses par débitmètre massique permet de s'affranchir des incertitudes de mesures et des aléas de réalisation liés aux imprécisions sur les quantités évoqués ci-avant.The quantities introduced for each gas are controlled by a flow meter mass installed on each line of gas used in the composition of the mixture to be produced. In addition, a set of several control valves makes it possible to control the flow of gas through the action of an automatic control system. Counting the masses by mass flow meter makes it possible to overcome the uncertainties of measurements and the hazards of realization related to the inaccuracies on the quantities mentioned above.

Le conditionnement avec un mélangeur dynamique s'accompagne cependant dans certains cas, d'une détente du gaz en aval de la chambre de mélange et d'un abaissement de la température des gaz en-dessous de la température de démélange ou de démixtion, ce qui s'explique par le fait que la ligne en aval de la chambre est à la même pression que les récipients ramenés à la pression atmosphérique. La circulation des gaz est alors diphasique dans les rampes de conditionnement vers les bouteilles.Conditioning with a dynamic mixer is however accompanied in in some cases, a relaxation of the gas downstream of the mixing chamber and a lowering of the temperature of the gases below the temperature of demixing or demixing, which can be explained by the fact that the line downstream of the chamber is at the same pressure as the containers brought back to atmospheric pressure. The gas circulation is then two-phase in the packaging ramps to the bottles.

Or, étant donné que les phases liquide et gazeuse se déplacent à des vitesses d'écoulement différentes, le remplissage des bouteilles n'est plus homogène et on peut constater des écarts de teneurs finales dans des bouteilles conditionnées sur la même rampe, lors d'une même fabrication. Ces disparités peuvent s'expliquer par des écoulements préférentiels dans les tuyauteries des rampes de remplissage des emballages.However, since the liquid and gaseous phases move at speeds flow, the filling of the bottles is no longer homogeneous and can be to notice differences in final contents in bottles conditioned on the same ramp, during the same production. These disparities can be explained by flows preferential in the pipe filling ramps packaging.

Pour résoudre ce problème de démélange, il a été proposé par le document EP-A-1174178 de maintenir la température du mélange au-dessus de celle de démélange en utilisant, pour ce faire, un dispositif parfaitement régulé de réchauffage des gaz en sortie de la chambre de mélange dynamique, durant le cycle de remplissage.To solve this problem of demixing, it has been proposed by EP-A-1174178 to keep the temperature of the mixture above that of the demix using, for this purpose, a perfectly regulated device for reheating the gases at the outlet of the dynamic mixing chamber, during the filling cycle.

Le mélange étant ainsi toujours maintenu à l'état gazeux, l'homogénéité du mélange est conservée et les écarts de teneurs sont suffisamment faibles pour permettre de contrôler l'ensemble des bouteilles par analyse d'une seule bouteille prélevée sur la rampe de conditionnement.The mixture is thus always maintained in the gaseous state, the homogeneity of the mixture is kept and the differences in levels are sufficiently low to control all the bottles by analysis of a single bottle taken from the ramp of conditioning.

Toutefois, en pratique, il est apparu parfois une limitation dans la réalisation du conditionnement de certains mélanges gazeux, en particulier ceux du type O2/N2O dont la teneur en N2O est supérieure ou égale à 30% en volume pour des pressions supérieures à 170 bars.However, in practice, there has sometimes been a limitation in carrying out the conditioning of certain gaseous mixtures, in particular those of the O 2 / N 2 O type, the N 2 O content of which is greater than or equal to 30% by volume for pressures above 170 bar.

En effet, pour ce type de mélanges, la pression finale est limitée par la mise en pression du N2O aux environs de 170 bars. Le N2O doit alors être chauffé pour monter à des pressions supérieures et ce qui engendre alors son passage à l'état supercritique.Indeed, for this type of mixtures, the final pressure is limited by the pressurization of N 2 O at around 170 bars. The N 2 O must then be heated to rise to higher pressures and this then generates its passage to the supercritical state.

Or, la température de réchauffage est aussi limitée par la température de décomposition du N2O et ce, d'autant plus que certains métaux du dispositif de conditionnement et de la bouteille, tels l'argent, le platine, le cobalt, le cuivre et les oxydes de nickel, sont des catalyseurs de la réaction.However, the reheating temperature is also limited by the decomposition temperature of N 2 O and this, especially as some metals of the packaging device and the bottle, such as silver, platinum, cobalt, copper and nickel oxides, are catalysts of the reaction.

Le conditionnement en dynamique de certains mélanges gazeux est donc limité, en général, à une pression voisine de 170 bars.The dynamic conditioning of certain gas mixtures is therefore limited, in in general, at a pressure close to 170 bars.

Le problème à résoudre est donc d'améliorer le procédé de conditionnement avec mélangeur dynamique, notamment le procédé décrit par le document EP-A-1174178, de manière à pouvoir réaliser des conditionnements en dynamique de mélanges gazeux à des pressions supérieures à 170 bars, en particulier des mélanges de gaz médicaux de type N2O/O2 dont la teneur en N2O est supérieure ou égale à 30% en volume.The problem to be solved is therefore to improve the packaging process with dynamic mixer, in particular the method described in document EP-A-1174178, so as to be able to produce dynamic packaging of gaseous mixtures at pressures greater than 170 bar, in particular N 2 O / O 2 medical gas mixtures whose N 2 O content is greater than or equal to 30% by volume.

La solution de l'invention est alors un procédé de fabrication d'un mélange gazeux contenant au moins un premier composé et au moins un deuxième composé dans des proportions désirées, lesdits premier et deuxième composés étant choisis dans le groupe formé par O2, N2, He, CO2, N2O et CO, dans lequel :

  • (a) on réalise un pré-mélange en dynamique de proportions déterminées desdits premier et deuxième composés pour obtenir un pré-mélange gazeux à une première pression (P1) inférieure ou égale à 200 bars et contenant une teneur intermédiaire (Ti) dudit deuxième composé supérieure à la teneur finale (Tf) dudit deuxième composé dans la composition finale souhaitée,
  • (b) on augmente la pression du pré-mélange gazeux obtenu à l'étape (a) par introduction du premier composé de manière à réaliser concomitamment une dilution du deuxième composé avec ledit premier composé,
  • (c) on stoppe l'étape (b), lorsque le mélange gazeux atteint la deuxième pression (P2) souhaitée, avec P2 > P1 et P2 > 170 bars, et contient une teneur finale (Tf) souhaitée en le deuxième composé.
    • The solution of the invention is then a process for manufacturing a gaseous mixture containing at least a first compound and at least a second compound in desired proportions, said first and second compounds being chosen from the group formed by O 2 , N 2 , He, CO 2 , N 2 O and CO, wherein:
  • (a) dynamic pre-mixing of determined proportions of said first and second compounds to obtain a gaseous premix at a first pressure (P1) less than or equal to 200 bar and containing an intermediate content (Ti) of said second compound greater than the final content (Tf) of said second compound in the desired final composition,
  • (b) increasing the pressure of the gaseous premix obtained in step (a) by introducing the first compound so as to concomitantly carry out a dilution of the second compound with said first compound,
  • (c) stopping step (b), when the gaseous mixture reaches the desired second pressure (P2), with P2> P1 and P2> 170 bar, and contains a final content (Tf) desired in the second compound.

    • Selon le cas, le procédé de l'invention peut comprendre l'une ou plusieurs des caractéristiques techniques suivantes :

    • la première pression (P1) est comprise entre 100 et 200 bars, de préférence inférieure ou égale à 170 bars.
    • la deuxième pression (P2) est supérieure à 200 bars, de préférence supérieure à 250 bars, de préférence encore supérieure ou égale à 300 bars.
    • le premier composé est de l'oxygène et le deuxième composé est du protoxyde d'azote (N2O), et on réalise, à l'étape (a), un pré-mélange O2/N2O. La teneur en le premier composé est supérieure ou égale à 30 %, de préférence entre 30 et 60 % et/ou la teneur en le deuxième composé est supérieure ou égale à 35 %, de préférence d'au moins 40 %.
    • le premier composé est de l'oxygène et le deuxième composé est du dioxyde de carbone (CO2), et on réalise, à l'étape (a), un pré-mélange O2/CO2. La teneur en le deuxième composé est comprise entre 1 et 10% en volume, de préférence entre 3 et 7%.
    • à l'étape (a), le pré-mélange gazeux est introduit dans un ou plusieurs récipients de conditionnement, en particulier des bouteilles de gaz sous pression.
    • à l'étape (a), le pré-mélange gazeux est réalisé au moyen d'un mélangeur en dynamique.
    • à l'étape (b), on augmente progressivement la pression du pré-mélange gazeux jusqu'à la deuxième pression (P2) et on diminue concomitamment la proportion du deuxième composé dans le mélange depuis la teneur intermédiaire (Ti) jusqu'à la teneur finale (Tf) souhaitée dudit deuxième composé dans le mélange final désiré. Pour atteindre une valeur finale (Tf) précise souhaitée, on peut utiliser un débitmètre massique.
    • le mélange gazeux souhaité est constitué de 50% en volume d'oxygène en tant que premier composé et de 50% en volume de protoxyde d'azote (N2O) en tant que deuxième composé.
    Depending on the case, the method of the invention may comprise one or more of the following technical characteristics:
    • the first pressure (P1) is between 100 and 200 bar, preferably less than or equal to 170 bar.
    • the second pressure (P2) is greater than 200 bar, preferably greater than 250 bar, more preferably greater than or equal to 300 bar.
    • the first compound is oxygen and the second compound is nitrous oxide (N 2 O), and in step (a), an O 2 / N 2 O premix is carried out. the first compound is greater than or equal to 30%, preferably 30 to 60% and / or the content of the second compound is greater than or equal to 35%, preferably at least 40%.
    • the first compound is oxygen and the second compound is carbon dioxide (CO 2 ), and in step (a), an O 2 / CO 2 premix is produced. The content of the second compound is between 1 and 10% by volume, preferably between 3 and 7%.
    • in step (a), the gaseous premix is introduced into one or more conditioning containers, in particular pressurized gas cylinders.
    • in step (a), the gaseous premix is produced by means of a dynamic mixer.
    • in step (b), the pressure of the gaseous premix is gradually increased to the second pressure (P2) and the proportion of the second compound in the mixture from the intermediate content (Ti) to the final desired content (Tf) of said second compound in the desired final mixture. To reach a desired final value (Tf), a mass flow meter can be used.
    • the desired gas mixture consists of 50% by volume of oxygen as the first compound and 50% by volume of nitrous oxide (N 2 O) as the second compound.

    L'invention porte aussi sur un procédé de conditionnement de récipients de gaz, dans lequel on réalise et on introduit un mélange gazeux contenant un premier et un deuxième composés gazeux dans plusieurs récipients de conditionnement, ledit mélange gazeux étant réalisé par mise en oeuvre d'un procédé de fabrication selon l'invention, de préférence le mélange gazeux est constitué d'oxygène et de protoxyde d'azote (N2O).The invention also relates to a method for packaging gas containers, in which a gas mixture containing a first and a second gaseous compound is produced and introduced into a plurality of packaging containers, said gaseous mixture being produced by use of a manufacturing method according to the invention, preferably the gaseous mixture consists of oxygen and nitrous oxide (N 2 O).

    La présente invention va maintenant être décrite plus en détail à l'aide d'un exemple de réalisation donné illustratif, à savoir la fabrication d'un mélange gazeux O2/N20 contenant plus de 30% d'oxygène en volume (mélange 50% O2 + 50% N2O) à une pression de plus de 200 bars.The present invention will now be described in more detail with the aid of an exemplary illustrative embodiment, namely the manufacture of an O 2 / N 2 gas mixture containing more than 30% oxygen by volume (mixture 50% O 2 + 50% N 2 O) at a pressure of more than 200 bar.

    La réalisation du mélange gazeux selon l'invention se fait en deux étapes principales, à savoir :

    • d'abord la réalisation d'un pré-mélange O2/N2O au moyen d'un mélangeur dynamique de manière à obtenir pré-mélange O2/N2O à une pression entre 100 et 200 bars à une teneur initiale Ti en N2O supérieure (Ti = 60% en volume par exemple) à la teneur finale Tf (Tf = 50% en volume en N2O), le pré-mélange O2/N2O étant introduit dans les récipients de conditionnement d'une chaíne de remplissage, telles que des bouteilles de gaz,
    • puis une mise en pression du pré-mélange, c'est-à-dire une augmentation progressive de la pression au-delà de 200 bars, par dilution avec de l'O2 gazeux jusqu'à obtenir la pression finale souhaitée, par exemple une pression de 250 bars à 300 bars, ou plus.
    The gaseous mixture according to the invention is produced in two main stages, namely:
    • firstly the production of an O 2 / N 2 O premix by means of a dynamic mixer so as to obtain premix O 2 / N 2 O at a pressure between 100 and 200 bar at an initial content Ti in upper N 2 O (Ti = 60% by volume for example) at the final content Tf (Tf = 50% by volume in N 2 O), the O 2 / N 2 O premix being introduced into the packaging containers of a filling chain, such as gas bottles,
    • then pressurizing the premix, that is to say gradually increasing the pressure above 200 bars, by dilution with O 2 gas until the desired final pressure, for example a pressure of 250 bar at 300 bar, or more.

    La première étape de réalisation du pré-mélange avec un mélangeur dynamique permet d'obtenir un pré-mélange O2/N2O avec une précision de ± 0,5 %.The first step of carrying out premixing with a dynamic mixer makes it possible to obtain an O 2 / N 2 O premix with an accuracy of ± 0.5%.

    Ensuite, la dilution par montée en pression permet l'obtention d'un mélange O2/N2O précis à une pression élevée, c'est-à-dire jusqu'à 250 à 300 bars ou plus, de préférence en surveillant le couple température/pression au moyen d'un ou plusieurs capteurs de pression et de température, la précision résultant de l'utilisation d'un débitmètre massique.Then, the dilution by pressure rise makes it possible to obtain a precise O 2 / N 2 O mixture at a high pressure, that is to say up to 250 to 300 bar or more, preferably by monitoring the temperature / pressure pair by means of one or more pressure and temperature sensors, the precision resulting from the use of a mass flowmeter.

    Le contrôle de l'introduction de l'oxygène, lors de l'étape de dilution avec montée en pression, peut être effectué par un comptage massique au débitmètre de masse, ce qui assure la réalisation d'un mélange très précis à pression élevée. The control of the introduction of oxygen, during the dilution stage with pressure, can be carried out by mass counting at the mass flow meter, which ensures the realization of a very precise mixture at high pressure.

    L'homogénéisation du mélange pendant la seconde étape de préparation se fait généralement correctement ; néanmoins, elle peut être accélérée, en cas de besoin, par un cycle de roulage des emballages après remplissage et/ou par l'utilisation d'un tube plongeur qui permet d'introduire l'oxygène au fond de chaque récipient pendant le remplissage.The homogenization of the mixture during the second preparation stage is generally correctly; nevertheless, it can be accelerated, if necessary, by a packaging cycle after filling and / or using a dip tube which allows to introduce the oxygen at the bottom of each container during filling.

    Les avantages de la méthode de réalisation du mélange O2/N2O sont notamment une exactitude et une homogénéité des compositions gazeuses fabriquées ; une pression finale du mélange qui n'est plus limitée par la méthode de conditionnement ; ou une absence de démixtion aux basses températures pour les bouteilles pleines.The advantages of the method for producing the O 2 / N 2 O mixture include an accuracy and homogeneity of the gaseous compositions produced; a final pressure of the mixture which is no longer limited by the conditioning method; or a lack of demixing at low temperatures for full bottles.

    Ceci permet dans pour la plupart des pays européens ou tempérés, un stockage à l'extérieur des bouteilles et leur transport sans précaution particulière et ce, même en hiver.This allows in most European or temperate countries the outside of the bottles and their transport without any particular precautions, even in winter.

    En outre, la quantité stockée pour une même taille de bouteille est beaucoup plus importante, ce qui se traduit par une plus grande autonomie pour un même volume.In addition, the quantity stored for the same bottle size is much more important, which translates into greater autonomy for the same volume.

    La méthode de préparation n'est pas limitée au cas des mélanges O2/N2O. Elle peut se généraliser à d'autres gaz ou mélanges contenant un ou plusieurs gaz, comme CO2, N2O, O2, N2, He ...The method of preparation is not limited to the case of O 2 / N 2 O mixtures. It may be generalized to other gases or mixtures containing one or more gases, such as CO 2 , N 2 O, O 2 , N 2 , Hey ...

    Claims (11)

    Procédé de fabrication d'un mélange gazeux contenant au moins un premier composé et au moins un deuxième composé dans des proportions désirées, lesdits premier et deuxième composés étant choisis dans le groupe formé par O2, N2, He, CO2, N2O et CO, dans lequel : (a) on réalise un pré-mélange en dynamique de proportions déterminées desdits premier et deuxième composés pour obtenir un pré-mélange gazeux à une première pression (P1) inférieure ou égale à 200 bars et contenant une teneur intermédiaire (Ti) dudit deuxième composé supérieure à la teneur finale (Tf) dudit deuxième composé dans la composition finale souhaitée, (b) on augmente la pression du pré-mélange gazeux obtenu à l'étape (a) par introduction du premier composé de manière à réaliser concomitamment une dilution du deuxième composé avec ledit premier composé, (c) on stoppe l'étape (b), lorsque le mélange gazeux atteint la deuxième pression (P2) souhaitée, avec P2 > P1 et P2 > 170 bars, et contient une teneur finale (Tf) souhaitée en le deuxième composé. A process for producing a gaseous mixture containing at least a first compound and at least a second compound in desired proportions, said first and second compounds being selected from the group consisting of O 2 , N 2 , He, CO 2 , N 2 O and CO, wherein: (a) dynamic pre-mixing of determined proportions of said first and second compounds to obtain a gaseous premix at a first pressure (P1) less than or equal to 200 bar and containing an intermediate content (Ti) of said second compound greater than the final content (Tf) of said second compound in the desired final composition, (b) increasing the pressure of the gaseous premix obtained in step (a) by introducing the first compound so as to concomitantly carry out a dilution of the second compound with said first compound, (c) stopping step (b), when the gaseous mixture reaches the desired second pressure (P2), with P2> P1 and P2> 170 bar, and contains a final content (Tf) desired in the second compound. Procédé selon la revendication 1, caractérisé en ce que la première pression (P1) est comprise entre 100 et 200 bars, de préférence inférieure ou égale à 170 bars.Process according to claim 1, characterized in that the first pressure (P1) is between 100 and 200 bar, preferably less than or equal to 170 bar. Procédé selon l'une des revendications 1 ou 2, caractérisé en ce que la deuxième pression (P2) est supérieure à 200 bars, de préférence supérieure à 250 bars, de préférence encore supérieure ou égale à 300 bars.Process according to one of claims 1 or 2, characterized in that the second pressure (P2) is greater than 200 bar, preferably greater than 250 bar, more preferably greater than or equal to 300 bar. Procédé selon l'une des revendications 1 ou 3, caractérisé en ce que le premier composé est de l'oxygène et le deuxième composé est du protoxyde d'azote (N2O), et on réalise, à l'étape (a), un pré-mélange O2/N2O.Process according to one of claims 1 or 3, characterized in that the first compound is oxygen and the second compound is nitrous oxide (N 2 O), and in step (a) , an O 2 / N 2 O premix. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que la teneur en le premier composé est supérieure ou égale à 30 %, de préférence entre 30 et 60 % et/ou la teneur en le deuxième composé est supérieure ou égale à 35 %, de préférence d'au moins 40 % en volume. Process according to one of Claims 1 to 4, characterized in that the content of the first compound is greater than or equal to 30%, preferably 30 to 60% and / or the content of the second compound is greater than or equal to 35%, preferably at least 40% by volume. Procédé selon l'une des revendications 1 ou 3, caractérisé en ce que le premier composé est de l'oxygène et le deuxième composé est du dioxyde de carbone (CO2), et on réalise, à l'étape (a), un pré-mélange O2/CO2, de préférence la teneur en le deuxième composé est comprise entre 1 et 10%, préférentiellement entre 3 et 7% en volume.Process according to one of claims 1 or 3, characterized in that the first compound is oxygen and the second compound is carbon dioxide (CO 2 ), and in step (a) a pre-mixing O 2 / CO 2 , preferably the content of the second compound is between 1 and 10%, preferably between 3 and 7% by volume. Procédé selon l'une des revendications 1 à 6, caractérisé en ce qu'à l'étape (a), le pré-mélange gazeux est introduit dans un ou plusieurs récipients de conditionnement, en particulier des bouteilles de gaz sous pression.Process according to one of Claims 1 to 6, characterized in that in step (a), the gaseous premix is introduced into one or more conditioning containers, in particular pressurized gas bottles. Procédé selon l'une des revendications 1 à 7, caractérisé en ce qu'à l'étape (a), le pré-mélange gazeux est réalisé au moyen d'un mélangeur en dynamique.Process according to one of Claims 1 to 7, characterized in that in step (a) the gaseous premix is produced by means of a dynamic mixer. Procédé selon l'une des revendications 1 à 8, caractérisé en ce qu'à l'étape (b), on augmente progressivement la pression du pré-mélange gazeux jusqu'à la deuxième pression (P2) et on diminue concomitamment la proportion du deuxième composé dans le mélange depuis la teneur intermédiaire (Ti) jusqu'à la teneur finale (Tf) souhaitée dudit deuxième composé dans le mélange final désiré.Process according to one of Claims 1 to 8, characterized in that in step (b) the pressure of the gaseous premix is gradually increased to the second pressure (P2) and the proportion of the second compound in the mixture from the intermediate content (Ti) to the desired final content (Tf) of said second compound in the desired final mixture. Procédé selon l'une des revendications 1 à 5 et 7 à 9, caractérisé en ce que le mélange gazeux souhaité est constitué de 50% en volume d'oxygène en tant que premier composé et de 50% en volume de protoxyde d'azote (N2O) en tant que deuxième composé.Process according to one of Claims 1 to 5 and 7 to 9, characterized in that the desired gaseous mixture consists of 50% by volume of oxygen as the first compound and 50% by volume of nitrous oxide ( N 2 O) as the second compound. Procédé de conditionnement de récipients de gaz, dans lequel on réalise et on introduit un mélange gazeux contenant un premier et un deuxième composés gazeux dans plusieurs récipients de conditionnement, ledit mélange gazeux étant réalisé par mise en oeuvre d'un procédé de fabrication selon l'une des revendications 1 à 10, de préférence le mélange gazeux est constitué d'oxygène et de protoxyde d'azote (N2O).Process for the conditioning of gas containers, in which a gas mixture containing a first and a second gaseous compound is produced and introduced into a plurality of packaging containers, said gaseous mixture being produced using a manufacturing method according to the invention. one of claims 1 to 10, preferably the gaseous mixture consists of oxygen and nitrous oxide (N 2 O).
    EP20040300773 2003-12-17 2004-11-09 Dynamic conditioning of gaseous mixtures at high pressures, preferably of mixtures N2O/O2 Not-in-force EP1547637B1 (en)

    Applications Claiming Priority (2)

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    FR0351093 2003-12-17
    FR0351093A FR2863912B1 (en) 2003-12-17 2003-12-17 DYNAMIC CONDITIONING OF HIGH-PRESSURE GASEOUS MIXTURES, PARTICULARLY OF N2O / O2 MIXTURE

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    EP1547637A2 true EP1547637A2 (en) 2005-06-29
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    EP (1) EP1547637B1 (en)
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    FR2976259B1 (en) 2011-06-09 2013-07-05 Air Liquide PROCESS FOR CONDITIONING A NO / N2 GAS MIXTURE

    Citations (2)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    US4718462A (en) * 1980-01-18 1988-01-12 Fix R Method and apparatus for forming gaseous mixtures
    EP1174178A1 (en) * 2000-07-18 2002-01-23 Air Liquide Santé (International) Process and plant for dynamic gas conditioning, in particular for medical use

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    DE19651994A1 (en) * 1996-12-13 1998-06-18 Basf Ag Process for the production of self-separating, compact or cellular moldings, optionally containing reinforcing agents, from polyisocyanate polyaddition products and internal mold release agents therefor

    Patent Citations (2)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    US4718462A (en) * 1980-01-18 1988-01-12 Fix R Method and apparatus for forming gaseous mixtures
    EP1174178A1 (en) * 2000-07-18 2002-01-23 Air Liquide Santé (International) Process and plant for dynamic gas conditioning, in particular for medical use

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    EP1547637A3 (en) 2005-07-13
    ATE349270T1 (en) 2007-01-15
    ES2279318T3 (en) 2007-08-16
    DE602004003890D1 (en) 2007-02-08
    US7267143B2 (en) 2007-09-11
    DE602004003890T2 (en) 2007-10-31
    FR2863912A1 (en) 2005-06-24
    EP1547637B1 (en) 2006-12-27
    US20050155643A1 (en) 2005-07-21

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