WO2023094781A1 - Positive-pressure multiway inerting device - Google Patents

Positive-pressure multiway inerting device Download PDF

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Publication number
WO2023094781A1
WO2023094781A1 PCT/FR2022/052180 FR2022052180W WO2023094781A1 WO 2023094781 A1 WO2023094781 A1 WO 2023094781A1 FR 2022052180 W FR2022052180 W FR 2022052180W WO 2023094781 A1 WO2023094781 A1 WO 2023094781A1
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WO
WIPO (PCT)
Prior art keywords
ramp
gas
vacuum
stainless steel
valve
Prior art date
Application number
PCT/FR2022/052180
Other languages
French (fr)
Inventor
Frédéric LEGROS
Original Assignee
Universite Du Mans
Centre National De La Recherche Scientifique
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 Universite Du Mans, Centre National De La Recherche Scientifique filed Critical Universite Du Mans
Priority to EP22840235.0A priority Critical patent/EP4436704A1/en
Publication of WO2023094781A1 publication Critical patent/WO2023094781A1/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/02—Feed or outlet devices therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest

Definitions

  • the present invention belongs to the field of laboratory equipment, in particular in a chemical and/or biology laboratory.
  • Inerting devices also called vacuum ramps, are widely used in chemistry and biology laboratories. In particular, they make it possible to manipulate and synthesize air-sensitive samples.
  • a vacuum manifold typically includes dual tubing - one for vacuum and one for inert gas. The vacuum is created by a mechanical pump.
  • a cold trap containing, for example, liquid nitrogen is placed between this pump and the main part of the vacuum ramp. This trap is used to collect most of the gases and liquids that evaporate during the experiment, in order to prevent organic or corrosive compounds from damaging the mechanical pump.
  • vacuum ramps have numerous drawbacks. They are made of glass, therefore very fragile and can cause injuries to users when they break. They are not very modular, in particular from the point of view of the fittings and valves, and by the fact that the vacuum ramp is made up of a single piece of glass. They require the use of grease at the fittings which can contribute to the contamination of the samples and the fouling of the ramp. Finally, it is not possible to use oxygen as a gas in such vacuum ramps.
  • the present invention relates to a vacuum ramp device for the synthesis and / or manipulation of air-sensitive components
  • a vacuum ramp device for the synthesis and / or manipulation of air-sensitive components
  • a vacuum ramp device for the synthesis and / or manipulation of air-sensitive components
  • a vacuum source preferably a pump vacuum
  • a second gas manifold intended to be connected to a source of gas
  • the latter being at least three-way arranged so as to alternately connect the first vacuum manifold or the second gas manifold overpressure to a container
  • the second gas ramp is capable of withstanding an overpressure of between 0.10 and 0.40 bar
  • the first vacuum ramp is made of stainless steel and/or polytetrafluoroethylene
  • the second gas train is made of stainless steel and/or polytetrafluoroethylene.
  • the second gas ramp is capable of withstanding a constant and/or variable overpressure, preferably constant at 0.15 bar.
  • the first vacuum ramp and the second gas ramp are made of stainless steel.
  • the first vacuum ramp and the second gas ramp are made of polytetrafluoroethylene.
  • the first vacuum ramp is made of stainless steel and the second gas ramp is made of polytetrafluoroethylene.
  • the first vacuum ramp is made of polytetrafluoroethylene and the second gas ramp is made of stainless steel.
  • the second gas ramp is connected at its outlet to a pressure relief valve.
  • the gas source is chosen from: argon, nitrogen, helium, hydrogen, ethylene, oxygen or a mixture of these.
  • the tap is made of stainless steel with at least one seat made of polytetrafluoroethylene.
  • the invention also relates to a system comprising the device according to the invention, according to which it comprises a vacuum source, a gas source and a pressure relief valve.
  • the invention also relates to a method for implementing the device according to the invention, comprising: a first vacuum step consisting in expelling any air included in the first vacuum ramp, using a suitable means, such as a vacuum pump; a second step of pressurizing the second gas ramp using a source of gas, such as argon, nitrogen, helium, hydrogen, ethylene , oxygen or a mixture thereof; a third step consisting in closing each tap comprising a valve, connecting the two ramps to at least one container, so as to position the valve in the closed position; a fourth step consisting in opening the valve of the tap in the so-called “vacuum” position capable of creating a vacuum in the container; a fifth step consisting in turning this same valve of the tap into a so-called “gas” position capable of filling the gas container included in the second gas manifold.
  • steps 3 to 5 are repeated per cycle in succession at least twice, preferably three times to perform inerting in the container.
  • the pressurization leads to a suppression, preferably constant at 0.15 bar.
  • the fourth step comprises a step of heating the container to evacuate the residual water.
  • the invention relates to a device for handling air-sensitive components comprising a vacuum ramp and at least one gas ramp adapted to the overpressure condition, in particular a laboratory device suitable in particular for use in a experimental setup in chemistry laboratory.
  • the invention also relates to a system comprising such a device as well as to a process for the synthesis and/or manipulation of an air-sensitive component implementing such a device.
  • This inerting device has the advantage of being hermetic to air and water in order to carry out chemical reactions under these particular conditions.
  • the double vacuum ramp is a glass device frequently used in chemical laboratories, in particular in experimental assemblies for the manipulation and/or synthesis of compounds sensitive to the air, resulting in the need to control the atmosphere in contact with them.
  • This double vacuum ramp is formed of a vacuum ramp and another ramp placed under inert gas, for example using nitrogen or argon.
  • the vacuum is created by a mechanical pump and a cold trap generally arranged between the pump and the vacuum ramp. This trap serves to collect most of the gases and liquids that evaporate during the experiment.
  • the double ramp has an oil column at the outlet of the inert gas ramp, commonly called a "bubbler", making it possible to visually control the flow of inert gas.
  • a preliminary step consists in lubricating all of the fittings which are made of frosted glass to increase, among other things, the tightness of the fittings, then involving a cleaning step with, for example, acetone or petroleum ether.
  • These fat additions can be sources of pollution during synthesis or during the handling of components.
  • the implementation of this device has a significant set of drawbacks which are very often formulated and known as being the rules to be observed for its proper use of preliminary steps or precautions to be taken.
  • the major drawback of this device is its great fragility, making it difficult to use and maintain. Indeed, parts or even the whole of this device is very brittle. The risk of injury with broken glass for the user is therefore significant during its use and maintenance. In addition, cleaning or deslagging all the parts of this device sometimes proves impossible due to the fragility of the overall structure. Thus, after several uses, many traces of pollutant within this device are easily identifiable.
  • the object of the invention is to remedy all of these aforementioned drawbacks.
  • the aim of the invention is to provide a synthesis and/or manipulation device offering a more secure implementation due to a greatly improved robustness.
  • this device makes it possible to obtain guaranteed reaction products without pollution inherent in the use of the latter, while limiting gas consumption as much as possible.
  • this device also has the advantage of increasing the gas distribution rate from the overpressure ramp in a container connected to this ramp, saving time.
  • a first aspect of the invention proposes a vacuum ramp device for the synthesis and/or manipulation of air-sensitive components comprising at least a first vacuum ramp vacuum intended to be connected to a vacuum source, preferably a vacuum pump, and a second gas manifold intended to be connected to a gas source, and at least one three-way valve arranged so as to alternately connect the first vacuum ramp to the second overpressure gas ramp and to a container.
  • This second ramp is able to withstand an overpressure of between 0 and 0.40 bar, preferably between 0.10 and 0.40 bar, preferably between 0.10 and 0.35 bar.
  • the first vacuum ramp is made of stainless steel and/or polytetrafluoroethylene
  • the second gas ramp is made of stainless steel and/or polytetrafluoroethylene.
  • the use of stainless steel or polytetrafluoroethylene makes the ramps less fragile compared to conventional glass ramps.
  • a more robust inerting device has several advantages: it requires fewer repairs, replacement or precautions when using it, it also avoids injuries to users that can be caused when a ramp breaks during handling.
  • the inerting device according to the invention is more modular and easier to use than a conventional glass ramp. It is thus possible to use standardized connectors ensuring simple connectivity with various external elements (tanks, taps, etc.).
  • the ramps of the device can also be in several portions that can be assembled or disassembled easily. The device can thus adopt a wide variety of configurations. The maintenance or replacement of the various elements is also facilitated.
  • the inerting device according to the invention does not require the lubrication or cleaning of the connections, thus limiting the pollution of the device, in particular the contamination of the reagents present in the containers connected to the device and the fouling of the ramps. Finally, it is possible to use oxygen as a gas in the inerting device of the invention due to the absence of grease.
  • the second ramp is able to withstand an overpressure at a constant pressure and/or at a variable pressure, preferably constant at 0.15 bar.
  • the first ramp is made of stainless steel (or stainless steel) and the second ramp is made of polytetrafluoroethylene (PTFE).
  • PTFE polytetrafluoroethylene
  • first vacuum ramp and the second gas ramp are made of stainless steel. According to another embodiment, the first vacuum ramp and the second gas ramp are made of polytetrafluoroethylene.
  • the first vacuum ramp is made of polytetrafluoroethylene and the second gas ramp is made of stainless steel.
  • the second gas ramp is connected at its outlet to a pressure relief valve.
  • a pressure relief valve is a non-return valve.
  • This non-return valve prevents any entry of external gas and does not generate the inconvenience of oil return unlike the bubbler.
  • the non-return valve prevents any entry of external gas, therefore it prevents excessive consumption of gas from the gas source. Thanks to the absence of a bubbler, the inerting device according to the invention is perfectly suited to a wider range of processes such as for example the catalysis and the synthesis of materials reactive with oxygen.
  • the gas source is chosen from: argon (Ar), nitrogen (N2), helium (He), hydrogen (H2), ethylene ( C2H4), oxygen (O2) or a mixture of these.
  • the gas may be an inert gas or a gas of the combustible type.
  • the device comprises at least one four-way valve arranged so as to alternately connect the first vacuum ramp to the second overpressure gas ramp, to a third gas ramp and to a container.
  • the valve is made of stainless steel with at least one seat made of polytetrafluoroethylene.
  • the present invention also relates to a system comprising the device as described above.
  • This system includes a vacuum source (preferably a vacuum pump), a gas source and a pressure relief valve.
  • a vacuum source preferably a vacuum pump
  • a gas source preferably a gas source
  • a pressure relief valve preferably a pressure relief valve
  • the system also includes at least one pressure gauge connected to the first vacuum ramp.
  • the invention also relates to a method for implementing the device as described above, comprising: a first vacuum step consisting in expelling any air included in the first vacuum ramp , using a suitable means, such as a vacuum pump; a second step of pressurizing the second gas ramp using a source of gas, such as argon, nitrogen, helium, hydrogen, ethylene or oxygen or a mixture thereof; a third step consisting in closing each tap comprising a valve, connecting the two ramps to at least one container, so as to position the valve in the closed position; a fourth step consisting in opening the valve in the so-called “empty” position capable of creating a vacuum in the chosen container; and a fifth step consisting in turning this same valve into a so-called “gas” position capable of filling the gas container included in the second gas ramp.
  • a suitable means such as a vacuum pump
  • a source of gas such as argon, nitrogen, helium, hydrogen, ethylene or oxygen or a mixture thereof
  • a third step consisting in
  • steps 3 to 5 are repeated per cycle in succession at least twice, preferably three times to perform inerting in the container.
  • Figure 1 shows a general diagram of a double vacuum ramp of the prior art.
  • Figure 2 shows a diagram of the device proposed according to a first embodiment of the invention.
  • Figure 3 shows a side view of the device of Figure 2.
  • Figure 4 shows an exploded view of the device of Figure 2.
  • FIG. 1 shows a system 1 of the prior art considered classic, having a double glass ramp 3 comprising a valve thus connecting the double ramp 3 to a container 7.
  • This system 1 comprises a gas source 9 connected to one ramp and a vacuum source 11 connected to the other ramp.
  • the vacuum source 11 is preferably a vacuum pump.
  • This system 1 comprises two traps, a first trap 13 is connected to the gas ramp and a second trap 15 is arranged between the gas ramp and the vacuum pump 11.
  • This system requires each use to properly grease all the fittings of ground glass and clean them with, for example, dichloromethane. The purpose of lubrication is, moreover, to seal the ground glass fittings.
  • This fat is a pollution source which is known in practice and which is frequently found in the reaction products. There are also identity tables listing all the types of fats used allowing their identification in the reaction products (Example: “NMR chemical Schifts of trace Impurities” article Organometallics 2010,29, 2176-2179.)
  • the device 2 of the invention as shown in Figures 2 to 4 comprises a double ramp.
  • a first so-called vacuum ramp 4 is dedicated to vacuum and a second so-called gas ramp 6 is dedicated to containing a gas, preferably an inert gas.
  • This first vacuum ramp 4 is connected to a vacuum source, that is to say a means for performing the vacuum correctly.
  • the vacuum is formed using a vane pump or either using a dry pump or any type of pump that can reach the desired value.
  • This first vacuum ramp 4 is able to withstand a negative pressure, preferably at a pressure of 5*10 -3 bar, preferably at a pressure of 5*10 -3 mbar.
  • this first vacuum ramp 4 is wholly or partly made of stainless steel (also called stainless steel)
  • the first vacuum ramp 4 may comprise polytetrafluoroethylene (PTFE also called Teflon - registered trademark).
  • the second gas ramp 6 as shown is connected to a gas source, to an overpressure valve (not visible) and to a manometer 8.
  • the pressure inside this second gas ramp 6 can vary from 0 to 0.40 bar, preferably the pressure inside this second gas manifold 6 will remain constant (i.e. stable) at a pressure between 0 and 0.35 bar, preferably at 0.15 bar.
  • the overpressure valve present in the device 2 opens in order to evacuate the effective overpressure in the second gas train 6.
  • the overpressure can be controlled but also untimely during the implementation of the device 2, for example, following a release of gas from a handling container.
  • this second gas rail 6 is wholly or partly made of stainless steel. According to another embodiment, the second gas rail 6 is made of polytetrafluoroethylene.
  • the first and second ramps are made of 316L stainless steel, but other materials, such as polytetrafluoroethylene, can be considered for the use of corrosive gas where the quality of stainless steel would not be sufficient.
  • the first ramp is made of stainless steel and the second ramp is made of polytetrafluoroethylene.
  • the first ramp is made of polytetrafluoroethylene and the second ramp is made of stainless steel.
  • the first and second ramps are made of polytetrafluoroethylene.
  • the choice of the gas source can be indifferently a neutral gas (argon, helium and nitrogen), or any combustible type gas (hydrogen, ethylene, oxygen) falling within the technical characteristics of 316L stainless steel. .
  • the gas can be pure or be a mixture of several gases. Depending on the type of assembly desired by the user, the choice of gas may differ.
  • This device 2 is suitable for a large panel of gases because it has a safety of use unequaled in the prior art. Indeed, the absence of pollutant, for example of grease type, in the device 2 allows the use of gas such as pure oxygen without risk of explosion. In fact, oxygen pure being flammable in contact with grease, the use of this gas is impossible in conventional Schlenk lines requiring lubrication of the connections.
  • the first vacuum ramp 4 and the second gas ramp 6 are connected to at least one container by at least one valve 10 to a three-way valve 12 as shown in Figure 3 for choosing the vacuum, the gas or a closed position.
  • valve 10 may be made of stainless steel and preferably with a seat of polytetrafluoroethylene or entirely of polytetrafluoroethylene
  • first vacuum ramp 4, second gas ramp 6 and valve 10 can be made of stainless steel or polytetrafluoroethylene.
  • the device 2 comprises a plurality of valves 10 three-way 12. More generally, the plurality of valves 10 allows to increase the number of containers (not shown ) connected to the device 2 in order to increase the number of possible reactions in parallel using this device 2 and thus save time.
  • the valves 10 are arranged so as to alternately connect the first vacuum ramp 4 or the second gas ramp 6 under overpressure to the plurality of containers using a connection means 14 connected to the corresponding valve 10.
  • This connection means 14 has the advantage of being capable of forming a hermetic atmosphere between the exterior of the device 2 and the container, that is to say that no gas exit or entry from outside the device 2 can enter the container.
  • valve 10 three-way 12 advantageously facilitates the connection of the first ramp or the second ramp to the container.
  • the valve 10 may be four-way.
  • the valve will include a handle, valve or any other similar means making it possible to clearly identify whether the valve is in the closed or open position for each of the ramps, in particular with each of the two ramps.
  • the device in addition to a first vacuum ramp 4 and a second gas ramp 6, the device may comprise a third ramp, for example a gas ramp. Consequently, it will be noted that the device will therefore have at least one four-way valve 10 in order to be able to connect the three ramps to the container.
  • At least one additional pressure gauge can be added using standardized fittings to the ramps, such as a vacuum gauge, which has the advantage for the invention of being a means of measurement of the residual gas pressure in a vacuum tube for example.
  • the three-way valves 10 are in the closed position. Then initially, open, towards the container, the tap valve 10 to the empty position, that is to say open for the first vacuum ramp 4, then the tap valve 10 is closed and the latter is reopened on the gas position, that is to say in the open position for the second gas ramp 6. It is thus possible to repeat the operation several times in order to obtain a desired inerting.
  • the device 2 advantageously has a plurality of connectors, preferably standardized stainless steel connectors.
  • the entire device 2 is removable, thus facilitating washing in its entirety and the replacement of parts forming the device 2.
  • the device 2 comprises at least: A fluted end piece 16 in stainless steel for a hose, an adapter fitting 18 (ISO-KF16), a collar 20 (ISO-DN16) , a seal 22, a second gas ramp 6, a pressure gauge 8 in stainless steel, a union tee 24 in stainless steel, an elbow 26 in stainless steel, a 3-way stainless steel PTFE ball valve 10, a bent tube 28, a first vacuum ramp 4,
  • the connection means 14 is a stainless steel 30 (ISO-316) hose connector, a ring centering ring with filter 32 in stainless steel (ISO-KF16), a centering ring 34 in stainless steel (ISO-DN16), a pressure relief valve 25 with spring rated at 0.35 bar, a shutter 36 in stainless steel (ISO -DN16).
  • rods, elbows, tubes or fittings can have any cross-sectional shape, such as, for example, but not limited to, round, square, elliptical.
  • the device 2 can be integrated into a general gas distribution network as well as into several hoods in series.
  • the use of the device 2 is easy, its method of use comprises a sequence of steps, as described below: a first vacuum step consisting in expelling any air included in the first vacuum ramp 4, using a suitable means, such as a vacuum pump; a second step of pressurizing the second gas ramp 6 using a source of gas, such as argon, nitrogen, helium, oxygen, hydrogen, ethylene, or a mixture of gases; a third step consisting in closing each tap 10 comprising a valve, connecting the two ramps (4, 6) to at least one container, so as to position the valve in the closed position; a fourth step consisting in opening the valve of the tap 10 in the so-called “vacuum” position capable of creating a vacuum in the container; a fifth step consisting in turning this same valve of the tap 10 into a so-called "gas” position capable of filling the gas container included in the second gas ramp 6.
  • a first vacuum step consisting in expelling any air included in the first vacuum ramp 4, using a suitable means, such as a vacuum pump
  • the second pressurizing step is carried out until the pressure in the second gas ramp is between 0 and 0.35 bar.
  • the overpressure to be reached remains constant at 0.15 bar.
  • steps 3 to 5 are repeated per cycle in succession at least three times to perform inerting in the container.
  • step 4 may include a step of heating the container in order to vaporize traces of water in the latter and evacuate them through the vacuum ramp.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The present invention relates to a vacuum manifold device (2) for the synthesis and/or handling of air-sensitive compounds, the device comprising at least one first vacuum line (4) which is intended to be connected to a vacuum source and a second gas line (6) which is intended to be connected to a gas source, and at least one stopcock (10), said stopcock being at least a three-way stopcock arranged so as to connect either the first vacuum line (4) or the second gas line (6), which is at a positive pressure, to a container, the second gas line (6) being capable of withstanding a positive pressure of between 0.10 and 0.40 bar. In particular, said device is intended for use in the chemistry laboratory and the first vacuum line (4) is made of stainless steel and/or of polytetrafluoroethylene, and the second gas line (6) is made of stainless steel and/or of polytetrafluoroethylene.

Description

DISPOSITIF D’INERTAGE MULTI- VOIES EN SURPRESSION MULTI-WAY OVERPRESSURE INERTATION DEVICE
DOMAINE DE L’INVENTION FIELD OF THE INVENTION
[0001] La présente invention appartient au domaine du matériel de laboratoire, notamment en laboratoire de chimie et/ou de biologie. The present invention belongs to the field of laboratory equipment, in particular in a chemical and/or biology laboratory.
ÉTAT DE LA TECHNIQUE STATE OF THE ART
[0002] Les dispositifs d’inertage, aussi appelés rampes à vide, sont très utilisés dans les laboratoires de chimie et de biologie. Ils permettent notamment de manipuler et de synthétiser des échantillons sensibles à l’air. Une rampe à vide comprend typiquement une double tubulure - une pour le vide et une pour le gaz inerte. Le vide est créé par une pompe mécanique. Un piège à froid contenant par exemple de l’azote liquide est placé entre cette pompe et la partie principale de la rampe à vide. Ce piège sert à recueillir la plupart des gaz et des liquides qui s’évaporent au cours de l'expérience, afin d'empêcher des composés organiques ou corrosifs d’endommager la pompe mécanique. [0002] Inerting devices, also called vacuum ramps, are widely used in chemistry and biology laboratories. In particular, they make it possible to manipulate and synthesize air-sensitive samples. A vacuum manifold typically includes dual tubing - one for vacuum and one for inert gas. The vacuum is created by a mechanical pump. A cold trap containing, for example, liquid nitrogen is placed between this pump and the main part of the vacuum ramp. This trap is used to collect most of the gases and liquids that evaporate during the experiment, in order to prevent organic or corrosive compounds from damaging the mechanical pump.
[0003] Malheureusement, ces rampes à vide présentent de nombreux inconvénients. Elles sont en verre, donc très fragiles et peuvent occasionner des blessures aux utilisateurs lorsqu’elles se cassent. Elles sont peu modulables, notamment du point de vue des raccords et robinets, et par le fait que la rampe à vide est constituée d’une pièce en verre unique. Elles nécessitent l’utilisation de graisse au niveau des raccords ce qui peut contribuer à la contamination des échantillons et à l’encrassement de la rampe. Enfin, il n’est pas possible d’utiliser de l’oxygène comme gaz dans de telles rampes à vide. [0003] Unfortunately, these vacuum ramps have numerous drawbacks. They are made of glass, therefore very fragile and can cause injuries to users when they break. They are not very modular, in particular from the point of view of the fittings and valves, and by the fact that the vacuum ramp is made up of a single piece of glass. They require the use of grease at the fittings which can contribute to the contamination of the samples and the fouling of the ramp. Finally, it is not possible to use oxygen as a gas in such vacuum ramps.
[0004] La demande de brevet américaine US 2018/0156344, sans pour autant divulguer une double rampe, divulgue un dispositif permettant d’évacuer l’air d’un élément et de le remplacer par un gaz inerte. L’utilisation de ce dispositif nécessite plusieurs étapes de manipulations de vannes entre différentes sources de gaz ce qui complexifie sa mise en œuvre. [0005] Il existe donc un besoin pour des dispositifs d’inertage multi- voies en surpression plus robustes, modulables, ne nécessitant pas de graisse, pouvant être utilisés lors de manipulations faisant intervenir de l’oxygène, et permettant un démontage aisé. [0004] American patent application US 2018/0156344, without disclosing a double ramp, discloses a device for evacuating air from an element and replacing it with an inert gas. The use of this device requires several valve manipulation steps between different gas sources, which complicates its implementation. [0005] There is therefore a need for multi-way overpressure inerting devices that are more robust, modular, do not require grease, can be used during manipulations involving oxygen, and allow easy dismantling.
RÉSUMÉ SUMMARY
[0006] La présente invention concerne un dispositif de rampe à vide pour la synthèse et/ou la manipulation de composants sensibles à l’air comprenant au moins une première rampe à vide destinée à être connectée à une source de vide, de préférence une pompe à vide, et une seconde rampe à gaz destinée à être connectée à une source de gaz, et au moins un robinet, ce dernier étant au moins à trois voies disposé de sorte à connecter alternativement la première rampe à vide ou la seconde rampe à gaz en surpression à un contenant, caractérisé en ce que la seconde rampe à gaz est apte à résister à une surpression comprise entre 0,10 et 0,40 bar, la première rampe à vide est en acier inoxydable et/ou en polytétrafluoroéthylène, et la seconde rampe à gaz est en acier inoxydable et/ou en polytétrafluoroéthylène. Selon un mode de réalisation, la seconde rampe à gaz est apte à résister à une surpression constante et/ou variable, de préférence constante à 0,15 bar. Selon un mode de réalisation, la première rampe à vide et la seconde rampe à gaz sont en acier inoxydable. Selon un mode de réalisation, la première rampe à vide et la seconde rampe à gaz sont en polytétrafluoroéthylène. Selon un mode de réalisation, la première rampe à vide est en acier inoxydable et la seconde rampe à gaz est en polytétrafluoroéthylène. Selon un mode de réalisation, la première rampe à vide est en polytétrafluoroéthylène et la seconde rampe à gaz est en acier inoxydable. Selon un mode de réalisation, la seconde rampe à gaz est connectée à sa sortie à une soupape de surpression. Selon un mode de réalisation, la source de gaz est choisie parmi : de l’argon, de l’azote, de l’hélium, de l’hydrogène, de l’éthylène, de l’oxygène ou un mélange de ces derniers. Selon un mode de réalisation, le robinet est en acier inoxydable avec au moins un siège en polytétrafluoroéthylène. The present invention relates to a vacuum ramp device for the synthesis and / or manipulation of air-sensitive components comprising at least a first vacuum ramp intended to be connected to a vacuum source, preferably a pump vacuum, and a second gas manifold intended to be connected to a source of gas, and at least one tap, the latter being at least three-way arranged so as to alternately connect the first vacuum manifold or the second gas manifold overpressure to a container, characterized in that the second gas ramp is capable of withstanding an overpressure of between 0.10 and 0.40 bar, the first vacuum ramp is made of stainless steel and/or polytetrafluoroethylene, and the second gas train is made of stainless steel and/or polytetrafluoroethylene. According to one embodiment, the second gas ramp is capable of withstanding a constant and/or variable overpressure, preferably constant at 0.15 bar. According to one embodiment, the first vacuum ramp and the second gas ramp are made of stainless steel. According to one embodiment, the first vacuum ramp and the second gas ramp are made of polytetrafluoroethylene. According to one embodiment, the first vacuum ramp is made of stainless steel and the second gas ramp is made of polytetrafluoroethylene. According to one embodiment, the first vacuum ramp is made of polytetrafluoroethylene and the second gas ramp is made of stainless steel. According to one embodiment, the second gas ramp is connected at its outlet to a pressure relief valve. According to one embodiment, the gas source is chosen from: argon, nitrogen, helium, hydrogen, ethylene, oxygen or a mixture of these. According to one embodiment, the tap is made of stainless steel with at least one seat made of polytetrafluoroethylene.
[0007] L’invention concerne également un système comportant le dispositif selon l’invention, selon lequel il comprend une source de vide, une source de gaz et une soupape de surpression. [0008] L’invention concerne également un procédé de mise en œuvre du dispositif selon l’invention, comprenant : une première étape de mise sous vide consistant à chasser tout air compris dans la première rampe à vide, à l’aide d’un moyen approprié, tel qu’une pompe à vide ; une deuxième étape de mise en pression de la seconde rampe à gaz à l’aide d’une source de gaz, tel que de l’argon, de l’azote, de l’hélium, de l’hydrogène, de l’éthylène, de l’oxygène ou un mélange de ces derniers ; une troisième étape consistant à fermer chaque robinet comportant une vanne, reliant les deux rampes à au moins un contenant, de sorte à positionner la vanne en position fermée ; une quatrième étape consistant à ouvrir la vanne du robinet en position dite « vide » apte à effectuer le vide dans le contenant ; une cinquième étape consistant à tourner cette même vanne du robinet dans une position dite « gaz » apte à remplir le contenant du gaz compris dans la seconde rampe à gaz. The invention also relates to a system comprising the device according to the invention, according to which it comprises a vacuum source, a gas source and a pressure relief valve. The invention also relates to a method for implementing the device according to the invention, comprising: a first vacuum step consisting in expelling any air included in the first vacuum ramp, using a suitable means, such as a vacuum pump; a second step of pressurizing the second gas ramp using a source of gas, such as argon, nitrogen, helium, hydrogen, ethylene , oxygen or a mixture thereof; a third step consisting in closing each tap comprising a valve, connecting the two ramps to at least one container, so as to position the valve in the closed position; a fourth step consisting in opening the valve of the tap in the so-called “vacuum” position capable of creating a vacuum in the container; a fifth step consisting in turning this same valve of the tap into a so-called “gas” position capable of filling the gas container included in the second gas manifold.
[0009] Selon un mode de réalisation, les étapes 3 à 5 sont répétées par cycle à la suite au moins deux fois, de préférence trois fois pour effectuer un inertage dans le contenant. Selon un mode de réalisation, la mise en pression amène à une suppression, de préférence constante à 0, 15 bar. Selon un mode de réalisation, la quatrième étape comprend une étape de chauffage du contenant pour évacuer l’eau résiduelle. According to one embodiment, steps 3 to 5 are repeated per cycle in succession at least twice, preferably three times to perform inerting in the container. According to one embodiment, the pressurization leads to a suppression, preferably constant at 0.15 bar. According to one embodiment, the fourth step comprises a step of heating the container to evacuate the residual water.
DESCRIPTION DÉTAILLÉE DETAILED DESCRIPTION
[0010] L’invention concerne un dispositif pour manipuler des composants sensibles à l’air comportant une rampe à vide et au moins une rampe pour gaz adaptée à la condition de surpression, en particulier un dispositif de laboratoire convenant notamment à une utilisation dans un montage expérimental en laboratoire de chimie. L’invention est aussi relative à un système comprenant un tel dispositif ainsi qu’à un procédé de synthèse et/ou de manipulation de composant sensible à l’air mettant en œuvre un tel dispositif. [0011] Ce dispositif d’inertage a l’avantage d’être hermétique à l’air et à l’eau afin de réaliser des réactions chimiques sous ces conditions particulières. Dans l’art antérieur, il est connu la double rampe à vide, appelée Schlenk line en anglais, est un appareil en verre fréquemment utilisé dans les laboratoires de chimie, notamment dans les montages expérimentaux de manipulations et/ou de synthèse de composés sensibles à l’air, entrainant la nécessité de contrôler l’atmosphère en contact avec ces derniers. Cette double rampe à vide est formée d’une rampe mise sous vide et d’une autre rampe mise sous gaz inerte, par exemple à l’aide d’azote ou d’argon. Le vide est créé par une pompe mécanique et un piège à froid généralement disposé entre la pompe et la rampe à vide. Ce piège sert à recueillir la plupart des gaz et des liquides qui s'évaporent au cours de l'expérience. La double rampe présente en sortie de rampe à gaz inerte une colonne à huile, appelée communément « bulleur » permettant de contrôler visuellement le débit de gaz inerte. The invention relates to a device for handling air-sensitive components comprising a vacuum ramp and at least one gas ramp adapted to the overpressure condition, in particular a laboratory device suitable in particular for use in a experimental setup in chemistry laboratory. The invention also relates to a system comprising such a device as well as to a process for the synthesis and/or manipulation of an air-sensitive component implementing such a device. This inerting device has the advantage of being hermetic to air and water in order to carry out chemical reactions under these particular conditions. In the prior art, it is known that the double vacuum ramp, called Schlenk line in English, is a glass device frequently used in chemical laboratories, in particular in experimental assemblies for the manipulation and/or synthesis of compounds sensitive to the air, resulting in the need to control the atmosphere in contact with them. This double vacuum ramp is formed of a vacuum ramp and another ramp placed under inert gas, for example using nitrogen or argon. The vacuum is created by a mechanical pump and a cold trap generally arranged between the pump and the vacuum ramp. This trap serves to collect most of the gases and liquids that evaporate during the experiment. The double ramp has an oil column at the outlet of the inert gas ramp, commonly called a "bubbler", making it possible to visually control the flow of inert gas.
[0012] Avant l’utilisation du dispositif, une étape préliminaire consiste à graisser l’ensemble des raccords qui sont en verre dépoli pour augmenter, entre-autres, l’étanchéité des raccords, impliquant ensuite une étape de nettoyage avec, par exemple de l’acétone ou de l’éther de pétrole. Ces ajouts de graisse peuvent être sources de pollution lors de la synthèse ou lors de la manipulation de composants. [0012] Before using the device, a preliminary step consists in lubricating all of the fittings which are made of frosted glass to increase, among other things, the tightness of the fittings, then involving a cleaning step with, for example, acetone or petroleum ether. These fat additions can be sources of pollution during synthesis or during the handling of components.
[0013] D’autre part, la mise en route du dispositif nécessite plusieurs opérations successives, notamment destinées à purger l’air présent dans la double rampe à l’aide de gaz inerte, ces opérations sont consommatrices de gaz inerte et donc onéreuses. De plus, ces opérations répétées présentent un risque important d’entrée accidentelle d’huile provenant du bulleur dans la double rampe, cette huile étant elle aussi une source de pollution pouvant entraver la qualité des produits de synthèse contenus dans les ballons reliés à la rampe. [0013] On the other hand, starting up the device requires several successive operations, in particular intended to purge the air present in the double ramp using inert gas, these operations consuming inert gas and therefore expensive. In addition, these repeated operations present a significant risk of accidental entry of oil from the bubbler into the double ramp, this oil also being a source of pollution that can hinder the quality of the synthetic products contained in the balloons connected to the ramp. .
[0014] Ainsi, la mise en œuvre de ce dispositif présente un ensemble important d’inconvénients qui sont bien souvent formulés et connus comme étant les règles à respecter pour son bon usage d’étapes préliminaires ou de précautions à user. Cependant, l’inconvénient majeur de ce dispositif est sa grande fragilité, rendant difficile son utilisation et son entretien. En effet, des parties voire l’ensemble de cet appareil est très cassant. Le risque de blessure avec du verre brisé pour l’utilisateur est donc important lors de son usage et de son entretien. En outre, le nettoyage ou décrassage de l’ensemble des parties de ce dispositif s’avère parfois impossible du fait de la fragilité de la structure d’ensemble. Ainsi, après plusieurs utilisations, de nombreuses traces de polluant au sein de cet appareil sont facilement identifiables. [0014] Thus, the implementation of this device has a significant set of drawbacks which are very often formulated and known as being the rules to be observed for its proper use of preliminary steps or precautions to be taken. However, the major drawback of this device is its great fragility, making it difficult to use and maintain. Indeed, parts or even the whole of this device is very brittle. The risk of injury with broken glass for the user is therefore significant during its use and maintenance. In addition, cleaning or deslagging all the parts of this device sometimes proves impossible due to the fragility of the overall structure. Thus, after several uses, many traces of pollutant within this device are easily identifiable.
[0015] D’autre part, à la suite d’une casse, la réparation de ce dispositif n’est pas aisée voire impossible car la structure initiale est trop fragile pour autoriser toute modification structurelle. [0015] On the other hand, following a breakage, the repair of this device is not easy or even impossible because the initial structure is too fragile to allow any structural modification.
[0016] La demande de brevet américaine US 2018/0156344 Al, sans pour autant divulguer une double rampe, divulgue un dispositif permettant d’évacuer l’air d’un élément et de le remplacer par un gaz inerte. L’utilisation de ce dispositif nécessite plusieurs étapes de manipulations de vannes entre différentes sources de gaz ce qui complexifie sa mise en œuvre. [0016] American patent application US 2018/0156344 Al, without disclosing a double ramp, discloses a device for evacuating air from an element and replacing it with an inert gas. The use of this device requires several stages of manipulation of valves between different gas sources, which complicates its implementation.
[0017] L’invention a pour objet de remédier à l’ensemble de ces inconvénients susmentionnés. En particulier, l’invention a pour but de fournir un dispositif de synthèse et/ou de manipulation offrant une mise en œuvre plus sécurisée du fait d’une robustesse grandement améliorée. De plus, ce dispositif permet d’obtenir des produits de réaction garantis sans pollution inhérente à l’usage de ce dernier, tout en limitant au maximum la consommation de gaz. De plus, ce dispositif présente en outre comme avantage d’augmenter le débit de distribution de gaz issu de la rampe en surpression dans un contenant connecté à cette rampe, faisant gagner du temps. The object of the invention is to remedy all of these aforementioned drawbacks. In particular, the aim of the invention is to provide a synthesis and/or manipulation device offering a more secure implementation due to a greatly improved robustness. In addition, this device makes it possible to obtain guaranteed reaction products without pollution inherent in the use of the latter, while limiting gas consumption as much as possible. In addition, this device also has the advantage of increasing the gas distribution rate from the overpressure ramp in a container connected to this ramp, saving time.
[0018] Pour atteindre au moins l’un de ces buts, un premier aspect de l’invention propose un dispositif de rampe à vide pour la synthèse et/ou la manipulation de composants sensibles à l’air comprenant au moins une première rampe à vide destinée à être connectée à une source de vide, de préférence une pompe à vide, et une seconde rampe à gaz destinée à être connectée à une source de gaz, et au moins un robinet à trois voies disposé de sorte à connecter alternativement la première rampe à vide à la seconde rampe à gaz en surpression et à un contenant. Cette seconde rampe est apte à résister à une surpression comprise entre 0 et 0,40 bar, de préférence entre 0,10 et 0,40 bar, de préférence entre 0,10 et 0,35 bar. La première rampe à vide est en acier inoxydable et/ou en polytétrafluoroéthylène, et la seconde rampe à gaz est en acier inoxydable et/ou en polytétrafluoroéthylène. [0018] To achieve at least one of these goals, a first aspect of the invention proposes a vacuum ramp device for the synthesis and/or manipulation of air-sensitive components comprising at least a first vacuum ramp vacuum intended to be connected to a vacuum source, preferably a vacuum pump, and a second gas manifold intended to be connected to a gas source, and at least one three-way valve arranged so as to alternately connect the first vacuum ramp to the second overpressure gas ramp and to a container. This second ramp is able to withstand an overpressure of between 0 and 0.40 bar, preferably between 0.10 and 0.40 bar, preferably between 0.10 and 0.35 bar. The first vacuum ramp is made of stainless steel and/or polytetrafluoroethylene, and the second gas ramp is made of stainless steel and/or polytetrafluoroethylene.
[0019] Avantageusement, l’utilisation de l’acier inoxydable ou du polytétrafluoroéthylène rend les rampes moins fragiles comparées aux rampes classiques en verre. Un dispositif d’inertage plus robuste présente plusieurs avantages : il nécessite moins de réparation, remplacement ou de précautions à l’utilisation, il permet aussi d’éviter des blessures chez les utilisateurs qui peuvent être occasionnées lorsqu’une rampe casse pendant une manipulation. De plus, le dispositif d’inertage selon l’invention est plus modulable et facile d’utilisation qu’une rampe classique en verre. Il est ainsi possible d’utiliser des raccords normalisés assurant une connectivité simple avec divers éléments externes (ballons, robinets...). Les rampes du dispositif peuvent aussi se présenter en plusieurs portions pouvant être assemblées ou démontées facilement. Le dispositif peut ainsi adopter une grande variété de configurations. L’entretien ou le remplacement des différents éléments s’en trouve également facilité. Ce n’est pas le cas de rampes classiques qui sont construites comme une pièce unique. Le dispositif d’inertage selon l’invention ne nécessite pas le graissage ou le nettoyage des connexions limitant ainsi la pollution du dispositif, notamment la contamination des réactifs présents dans les contenants raccordés au dispositif et l’encrassement des rampes. Enfin, il est possible d’utiliser de l’oxygène comme gaz dans le dispositif d’inertage de l’invention du fait de l’absence de graisse. [0019] Advantageously, the use of stainless steel or polytetrafluoroethylene makes the ramps less fragile compared to conventional glass ramps. A more robust inerting device has several advantages: it requires fewer repairs, replacement or precautions when using it, it also avoids injuries to users that can be caused when a ramp breaks during handling. In addition, the inerting device according to the invention is more modular and easier to use than a conventional glass ramp. It is thus possible to use standardized connectors ensuring simple connectivity with various external elements (tanks, taps, etc.). The ramps of the device can also be in several portions that can be assembled or disassembled easily. The device can thus adopt a wide variety of configurations. The maintenance or replacement of the various elements is also facilitated. This is not the case with classic ramps which are built as a single piece. The inerting device according to the invention does not require the lubrication or cleaning of the connections, thus limiting the pollution of the device, in particular the contamination of the reagents present in the containers connected to the device and the fouling of the ramps. Finally, it is possible to use oxygen as a gas in the inerting device of the invention due to the absence of grease.
[0020] Selon un mode de réalisation, la seconde rampe est apte à résister à une surpression à une pression constante et/ou à une pression variable, de préférence constante à 0,15 bar. [0020]According to one embodiment, the second ramp is able to withstand an overpressure at a constant pressure and/or at a variable pressure, preferably constant at 0.15 bar.
[0021] Selon un mode de réalisation préféré de l’invention, la première rampe est en acier inoxydable (ou inox) et la seconde rampe en polytétrafluoroéthylène (PTFE). According to a preferred embodiment of the invention, the first ramp is made of stainless steel (or stainless steel) and the second ramp is made of polytetrafluoroethylene (PTFE).
[0022] Selon un autre mode de réalisation, la première rampe à vide et la seconde rampe à gaz sont en acier inoxydable. [0023] Selon un autre mode de réalisation, la première rampe à vide et la seconde rampe à gaz sont en polytétrafluoroéthylène. According to another embodiment, the first vacuum ramp and the second gas ramp are made of stainless steel. According to another embodiment, the first vacuum ramp and the second gas ramp are made of polytetrafluoroethylene.
[0024] Selon un autre mode de réalisation, la première rampe à vide est en polytétrafluoroéthylène et la seconde rampe à gaz est en acier inoxydable. [0024] According to another embodiment, the first vacuum ramp is made of polytetrafluoroethylene and the second gas ramp is made of stainless steel.
[0025] Selon une autre caractéristique de l’invention, la seconde rampe à gaz est connectée à sa sortie à une soupape de surpression. Avantageusement, cela permet de s’affranchir des bulleurs comparé aux rampes à vides (ou Schlenk lines) conventionnelles. L’inconvénient du bulleur est qu’un retour d’huile ou entrée d’un gaz externe (non souhaitée) est possible lorsque la pression dans la rampe à gaz est négative. La soupape de surpression est un clapet anti-retour. Ce clapet anti-retour permet d’éviter toute entrée de gaz externe et ne génère pas l’inconvénient du retour d’huile contrairement au bulleur. De plus, le clapet anti-retour évitant toute entrée de gaz externe, il permet par conséquent d’éviter une consommation excessive de gaz provenant de la source de gaz. Grâce à l’absence de bulleur, le dispositif d’inertage selon l’invention est parfaitement adapté à une plus large gamme de procédés tels que par exemple la catalyse et la synthèse de matériaux réactifs à l’oxygène. [0025] According to another characteristic of the invention, the second gas ramp is connected at its outlet to a pressure relief valve. Advantageously, this eliminates bubblers compared to conventional vacuum lines (or Schlenk lines). The disadvantage of the bubbler is that an oil return or entry of an external gas (undesired) is possible when the pressure in the gas ramp is negative. The pressure relief valve is a non-return valve. This non-return valve prevents any entry of external gas and does not generate the inconvenience of oil return unlike the bubbler. In addition, the non-return valve prevents any entry of external gas, therefore it prevents excessive consumption of gas from the gas source. Thanks to the absence of a bubbler, the inerting device according to the invention is perfectly suited to a wider range of processes such as for example the catalysis and the synthesis of materials reactive with oxygen.
[0026] Avantageusement, la source de gaz est choisie parmi : de l’argon (Ar), de l’azote (N2), de l’hélium (He), de l’hydrogène (H2), de l’éthylène (C2H4), de l’oxygène (O2) ou un mélange de ces derniers. De façon avantageuse, le gaz pourra être un gaz neutre ou un gaz du type combustible. Advantageously, the gas source is chosen from: argon (Ar), nitrogen (N2), helium (He), hydrogen (H2), ethylene ( C2H4), oxygen (O2) or a mixture of these. Advantageously, the gas may be an inert gas or a gas of the combustible type.
[0027] Selon une caractéristique possible, le dispositif comprend au moins un robinet à quatre voies disposé de sorte à connecter alternativement la première rampe à vide à la seconde rampe à gaz en surpression, à une troisième rampe à gaz et à un contenant. [0027] According to one possible feature, the device comprises at least one four-way valve arranged so as to alternately connect the first vacuum ramp to the second overpressure gas ramp, to a third gas ramp and to a container.
[0028] Préférentiellement, le robinet est en acier inoxydable avec au moins un siège en polytétrafluoroéthylène. [0028] Preferably, the valve is made of stainless steel with at least one seat made of polytetrafluoroethylene.
[0029] Selon un deuxième aspect, la présente invention a également trait à un système comportant le dispositif tel que décrit ci-dessus. Ce système comprend une source de vide (de préférence une pompe à vide), une source de gaz et une soupape de surpression. [0030] Avantageusement, le système comprend au moins également un manomètre connecté à la première rampe à vide. According to a second aspect, the present invention also relates to a system comprising the device as described above. This system includes a vacuum source (preferably a vacuum pump), a gas source and a pressure relief valve. [0030] Advantageously, the system also includes at least one pressure gauge connected to the first vacuum ramp.
[0031] Selon un troisième aspect, l’invention porte également sur un procédé de mise en œuvre du dispositif tel que décrit ci-dessus, comprenant : une première étape de mise sous vide consistant à chasser tout air compris dans la première rampe à vide, à l’aide d’un moyen approprié, tel qu’une pompe à vide; une deuxième étape de mise en pression de la seconde rampe à gaz à l’aide d’une source de gaz, tel que de l’argon, de l’azote, de l’hélium, de l’hydrogène, de l’éthylène ou de l’oxygène ou un mélange de ces derniers ; une troisième étape consistant à fermer chaque robinet comportant une vanne, reliant les deux rampes à au moins un contenant, de sorte à positionner la vanne en position fermée ; une quatrième étape consistant à ouvrir la vanne en position dite « vide » apte à effectuer le vide dans le contenant choisi ; et une cinquième étape consistant à tourner cette même vanne dans une position dite « gaz » apte à remplir le contenant du gaz compris dans la seconde rampe à gaz. [0031] According to a third aspect, the invention also relates to a method for implementing the device as described above, comprising: a first vacuum step consisting in expelling any air included in the first vacuum ramp , using a suitable means, such as a vacuum pump; a second step of pressurizing the second gas ramp using a source of gas, such as argon, nitrogen, helium, hydrogen, ethylene or oxygen or a mixture thereof; a third step consisting in closing each tap comprising a valve, connecting the two ramps to at least one container, so as to position the valve in the closed position; a fourth step consisting in opening the valve in the so-called “empty” position capable of creating a vacuum in the chosen container; and a fifth step consisting in turning this same valve into a so-called “gas” position capable of filling the gas container included in the second gas ramp.
[0032] Avantageusement, les étapes 3 à 5 sont répétées par cycle à la suite au moins deux fois, de préférence trois fois pour effectuer un inertage dans le contenant. Advantageously, steps 3 to 5 are repeated per cycle in succession at least twice, preferably three times to perform inerting in the container.
BRÈVE DESCRIPTION DES FIGURES BRIEF DESCRIPTION OF FIGURES
[0033] Afin d’expliquer l’invention, sans limiter l’invention de quelque manière que ce soit, des exemples de modes de réalisation préférés sont fournis ci-dessous, en faisant référence aux figures suivantes : In order to explain the invention, without limiting the invention in any way, examples of preferred embodiments are provided below, with reference to the following figures:
[0034] La figure 1 représente un schéma général d’une double rampe à vide de l’art antérieur. [0034] Figure 1 shows a general diagram of a double vacuum ramp of the prior art.
[0035] La figure 2 représente un schéma du dispositif proposé selon un premier mode de réalisation de l’invention. [0036] La figure 3 représente une vue de profil du dispositif de la figure 2. Figure 2 shows a diagram of the device proposed according to a first embodiment of the invention. [0036] Figure 3 shows a side view of the device of Figure 2.
[0037] La figure 4 représente une vue éclatée du dispositif de la figure 2. [0037] Figure 4 shows an exploded view of the device of Figure 2.
MODES DE RÉALISATION ILLUSTRATIFS DE L'INVENTION ILLUSTRATIVE EMBODIMENTS OF THE INVENTION
[0038] La figure 1 représente un système 1 de l’art antérieur considéré comme classique, présentant une double rampe en verre 3 comportant un robinet connectant ainsi la double rampe 3 à un contenant 7. Ce système 1 comprend une source de gaz 9 connectée à une rampe et une source de vide 11 connectée à l’autre rampe. La source de vide 11 est de préférence une pompe à vide. Ce système 1 comprend deux pièges, un premier piège 13 est connecté à la rampe à gaz et un second piège 15 est disposé entre la rampe à gaz et la pompe à vide 11. Ce système nécessite à chaque utilisation de graisser correctement tous les raccords de verre dépoli et de les nettoyer avec par exemple, du dichlorométhane. Le graissage a pour objectif, en outre, de rendre étanche les raccords de verre dépoli. Cette graisse est une source de pollution qui est dans la pratique connue et qui est fréquemment retrouvée dans les produits de réaction. Il existe d’ailleurs des tableaux d’identité répertoriant tous les types de graisses employées permettant leur identification dans les produits de réaction (Exemple : « NMR chemical Schifts of trace Impurities » article Organometallics 2010,29, 2176-2179.) [0038] Figure 1 shows a system 1 of the prior art considered classic, having a double glass ramp 3 comprising a valve thus connecting the double ramp 3 to a container 7. This system 1 comprises a gas source 9 connected to one ramp and a vacuum source 11 connected to the other ramp. The vacuum source 11 is preferably a vacuum pump. This system 1 comprises two traps, a first trap 13 is connected to the gas ramp and a second trap 15 is arranged between the gas ramp and the vacuum pump 11. This system requires each use to properly grease all the fittings of ground glass and clean them with, for example, dichloromethane. The purpose of lubrication is, moreover, to seal the ground glass fittings. This fat is a pollution source which is known in practice and which is frequently found in the reaction products. There are also identity tables listing all the types of fats used allowing their identification in the reaction products (Example: “NMR chemical Schifts of trace Impurities” article Organometallics 2010,29, 2176-2179.)
[0039] Le dispositif 2 de l’invention tel que représenté sur les figures 2 à 4 comporte une double rampe. Une première rampe dite à vide 4 est dédiée au vide et une seconde rampe dite à gaz 6 est dédiée à contenir un gaz, de préférence un gaz inerte. The device 2 of the invention as shown in Figures 2 to 4 comprises a double ramp. A first so-called vacuum ramp 4 is dedicated to vacuum and a second so-called gas ramp 6 is dedicated to containing a gas, preferably an inert gas.
[0040] Cette première rampe à vide 4 est connectée à une source de vide, c’est-à-dire un moyen permettant d’effectuer correctement le vide. Le vide est constitué à l’aide d’une pompe à palettes ou indifféremment à l’aide d’une pompe sèche ou tout type de pompe pouvant atteindre la valeur recherchée. Cette première rampe à vide 4 est apte à résister à une pression négative, de préférence à une pression de 5*10-3 bar, de préférence à une pression de 5*10-3 mbar. This first vacuum ramp 4 is connected to a vacuum source, that is to say a means for performing the vacuum correctly. The vacuum is formed using a vane pump or either using a dry pump or any type of pump that can reach the desired value. This first vacuum ramp 4 is able to withstand a negative pressure, preferably at a pressure of 5*10 -3 bar, preferably at a pressure of 5*10 -3 mbar.
[0041] Selon un mode de réalisation préféré, cette première rampe à vide 4 est tout ou en partie constituée en acier inoxydable (aussi appelé inox) Selon un autre mode de réalisation, la première rampe à vide 4 pourra comporter du polytétrafluoroéthylène (PTFE aussi appelé téflon - marque déposée). According to a preferred embodiment, this first vacuum ramp 4 is wholly or partly made of stainless steel (also called stainless steel) According to another mode of realization, the first vacuum ramp 4 may comprise polytetrafluoroethylene (PTFE also called Teflon - registered trademark).
[0042] La seconde rampe à gaz 6 tel que représentée est connectée à une source de gaz, à une soupape de surpression (non visible) et à un manomètre 8. La pression à l’intérieur de cette seconde rampe à gaz 6 peut varier de 0 à 0,40 bar, de préférence la pression à l’intérieur de cette seconde rampe à gaz 6 restera constante (i.e. stable) à une pression comprise entre 0 et 0,35 bar, de préférence à 0,15 bar. A noter qu’ au-delà des 0,35 bar, la soupape de surpression présente dans le dispositif 2 s’ouvre afin d’évacuer la surpression effective dans la seconde rampe à gaz 6. La surpression peut être contrôlée mais également intempestive lors de la mise en œuvre du dispositif 2, par exemple, à la suite d’un dégagement gazeux provenant d’un contenant de manipulation. The second gas ramp 6 as shown is connected to a gas source, to an overpressure valve (not visible) and to a manometer 8. The pressure inside this second gas ramp 6 can vary from 0 to 0.40 bar, preferably the pressure inside this second gas manifold 6 will remain constant (i.e. stable) at a pressure between 0 and 0.35 bar, preferably at 0.15 bar. It should be noted that beyond 0.35 bar, the overpressure valve present in the device 2 opens in order to evacuate the effective overpressure in the second gas train 6. The overpressure can be controlled but also untimely during the implementation of the device 2, for example, following a release of gas from a handling container.
[0043] Selon un mode de réalisation préféré, cette seconde rampe à gaz 6 est tout ou en partie constituée en acier inoxydable. Selon un autre mode de réalisation, la seconde rampe à gaz 6 est en polytétrafluoroéthylène. According to a preferred embodiment, this second gas rail 6 is wholly or partly made of stainless steel. According to another embodiment, the second gas rail 6 is made of polytetrafluoroethylene.
[0044] Préférentiellement, les première et seconde rampes sont en inox 316L, mais d’autres matériaux, tels que le polytétrafluoroéthylène, peuvent être envisagés pour l’utilisation de gaz corrosif où la qualité de l’acier inoxydable ne serait pas suffisante. Par exemple, la première rampe est en acier inoxydable et la seconde rampe est en polytétrafluoroéthylène. Dans un autre exemple, la première rampe est en polytétrafluoroéthylène et la seconde rampe est en acier inoxydable. Dans un autre exemple encore, les première et seconde rampes sont en polytétrafluoroéthylène. Preferably, the first and second ramps are made of 316L stainless steel, but other materials, such as polytetrafluoroethylene, can be considered for the use of corrosive gas where the quality of stainless steel would not be sufficient. For example, the first ramp is made of stainless steel and the second ramp is made of polytetrafluoroethylene. In another example, the first ramp is made of polytetrafluoroethylene and the second ramp is made of stainless steel. In yet another example, the first and second ramps are made of polytetrafluoroethylene.
[0045] De façon avantageuse, le choix de la source de gaz pourra être indifféremment un gaz neutre (argon, hélium et azote), ou tout gaz type combustible (hydrogène, éthylène, oxygène) rentrant dans les caractéristiques techniques de l’INOX 316L. Le gaz peut être pur ou être un mélange de plusieurs gaz. Selon le type de montage souhaité par l’utilisateur, le choix du gaz pourra différer. Ce dispositif 2 est adapté pour un panel de gaz important car il présente une sécurité d’usage inégalée dans l’art antérieur. En effet, l’absence de polluant, par exemple de type graisse, dans le dispositif 2 autorise l’utilisation de gaz tel que de l’oxygène pur sans risque d’explosion. En effet, l’oxygène pur étant inflammable en contact de la graisse, l’utilisation de ce gaz est impossible dans les Schlenk lines conventionnelles nécessitant un graissage des connections. [0045] Advantageously, the choice of the gas source can be indifferently a neutral gas (argon, helium and nitrogen), or any combustible type gas (hydrogen, ethylene, oxygen) falling within the technical characteristics of 316L stainless steel. . The gas can be pure or be a mixture of several gases. Depending on the type of assembly desired by the user, the choice of gas may differ. This device 2 is suitable for a large panel of gases because it has a safety of use unequaled in the prior art. Indeed, the absence of pollutant, for example of grease type, in the device 2 allows the use of gas such as pure oxygen without risk of explosion. In fact, oxygen pure being flammable in contact with grease, the use of this gas is impossible in conventional Schlenk lines requiring lubrication of the connections.
[0046] En cas d’utilisation de gaz corrosif, des joints adaptés de type polytétrafluoroéthylène devront être utilisés. [0046] If corrosive gas is used, suitable seals of the polytetrafluoroethylene type must be used.
[0047] La première rampe à vide 4 et la seconde rampe à gaz 6 sont reliées à au moins un contenant par au moins un robinet 10 à une vanne trois voies 12 tel que représenté sur la figure 3 permettant de choisir le vide, le gaz ou une position fermée. The first vacuum ramp 4 and the second gas ramp 6 are connected to at least one container by at least one valve 10 to a three-way valve 12 as shown in Figure 3 for choosing the vacuum, the gas or a closed position.
[0048] Selon le mode de réalisation, le robinet 10 pourra être en acier inoxydable et de préférence avec un siège en polytétrafluoroéthylène ou entièrement en polytétrafluoroéthylène Depending on the embodiment, the valve 10 may be made of stainless steel and preferably with a seat of polytetrafluoroethylene or entirely of polytetrafluoroethylene
[0049] Ainsi, l’ensemble du dispositif (première rampe à vide 4, seconde rampe à gaz 6 et robinet 10) peut être en acier inoxydable ou en polytétrafluoroéthylène. Thus, the entire device (first vacuum ramp 4, second gas ramp 6 and valve 10) can be made of stainless steel or polytetrafluoroethylene.
[0050] Selon ce mode de réalisation préféré représenté sur les figures 2 à 4, le dispositif 2 comprend une pluralité de robinets 10 à trois voies 12. Plus généralement, la pluralité de robinets 10 permet d’augmenter le nombre de contenants (non représentés) connectés au dispositif 2 afin d’augmenter le nombre de réactions possibles en parallèle à l’aide de ce dispositif 2 et ainsi gagner du temps. According to this preferred embodiment shown in Figures 2 to 4, the device 2 comprises a plurality of valves 10 three-way 12. More generally, the plurality of valves 10 allows to increase the number of containers (not shown ) connected to the device 2 in order to increase the number of possible reactions in parallel using this device 2 and thus save time.
[0051] Les robinets 10 sont disposés de sorte à connecter alternativement la première rampe à vide 4 ou la seconde rampe à gaz 6 en surpression à la pluralité de contenant à l’aide d’un moyen de connexion 14 relié au robinet 10 correspondant. Ce moyen de connexion 14 a l’avantage d’être apte à former une atmosphère hermétique entre l’extérieur du dispositif 2 et le contenant, c’est-à-dire qu’aucune sortie ou entrée de gaz de l’extérieur du dispositif 2 peut entrer dans le contenant. The valves 10 are arranged so as to alternately connect the first vacuum ramp 4 or the second gas ramp 6 under overpressure to the plurality of containers using a connection means 14 connected to the corresponding valve 10. This connection means 14 has the advantage of being capable of forming a hermetic atmosphere between the exterior of the device 2 and the container, that is to say that no gas exit or entry from outside the device 2 can enter the container.
[0052] Ce robinet 10 à trois voies 12 permet avantageusement de faciliter la connexion de la première rampe ou de la seconde rampe au contenant. Dans un autre mode de réalisation, le robinet 10 pourra être à quatre voies. Selon différentes variantes de réalisation, le robinet comprendra une manette, vanne ou tout autre moyen similaire permettant d’identifier clairement si le robinet est en position fermée ou ouverte pour chacune des rampes, en particulier avec chacune des deux rampes. This valve 10 three-way 12 advantageously facilitates the connection of the first ramp or the second ramp to the container. In another embodiment, the valve 10 may be four-way. According to different embodiments, the valve will include a handle, valve or any other similar means making it possible to clearly identify whether the valve is in the closed or open position for each of the ramps, in particular with each of the two ramps.
[0053] Selon un autre mode de réalisation (non représenté), en plus d’une première rampe à vide 4 et d’une seconde rampe à gaz 6 le dispositif pourra comprendre une troisième rampe, par exemple une rampe à gaz. En conséquence, on notera que le dispositif disposera donc d’au moins un robinet 10 à quatre voies afin d’être apte à connecter les trois rampes au contenant. According to another embodiment (not shown), in addition to a first vacuum ramp 4 and a second gas ramp 6, the device may comprise a third ramp, for example a gas ramp. Consequently, it will be noted that the device will therefore have at least one four-way valve 10 in order to be able to connect the three ramps to the container.
[0054] Selon un autre mode de réalisation encore, au moins un manomètre complémentaire pourra être ajouté à l’aide de raccords normalisés aux rampes, tel qu’un vacuomètre, qui a l’avantage pour l’invention d’être un moyen de mesure de la pression de gaz résiduel dans un tube à vide par exemple. [0054]According to yet another embodiment, at least one additional pressure gauge can be added using standardized fittings to the ramps, such as a vacuum gauge, which has the advantage for the invention of being a means of measurement of the residual gas pressure in a vacuum tube for example.
[0055] En condition normale d’utilisation, les robinets 10 trois voies sont en position fermée. Puis dans un premier temps, en ouvre, vers le contenant, la vanne du robinet 10 sur la position vide c’est-à-dire ouverte pour la première rampe à vide 4 puis on ferme la vanne du robinet 10 et on réouvre cette dernière sur la position gaz, c’est-à-dire en position ouverte pour seconde la rampe à gaz 6. On peut ainsi répéter plusieurs fois l’opération afin d’obtenir un inertage souhaité. In normal conditions of use, the three-way valves 10 are in the closed position. Then initially, open, towards the container, the tap valve 10 to the empty position, that is to say open for the first vacuum ramp 4, then the tap valve 10 is closed and the latter is reopened on the gas position, that is to say in the open position for the second gas ramp 6. It is thus possible to repeat the operation several times in order to obtain a desired inerting.
[0056] Tel que représenté sur la figure 4, le dispositif 2 présente avantageusement une pluralité de raccords, de préférence, des raccords normalisés en acier inoxydable. Ainsi l’ensemble du dispositif 2 est démontable facilitant ainsi le lavage dans son intégralité et le remplacement de parties formant le dispositif 2. As shown in Figure 4, the device 2 advantageously has a plurality of connectors, preferably standardized stainless steel connectors. Thus the entire device 2 is removable, thus facilitating washing in its entirety and the replacement of parts forming the device 2.
[0057] Dans le but de détailler le mode de réalisation préféré, sans limiter l’invention de quelque manière que ce soit, la liste des éléments de raccords utilisés est fournie ci- dessous, en faisant référence à la figure 4. [0057] For the purpose of detailing the preferred embodiment, without limiting the invention in any way whatsoever, the list of connector elements used is provided below, with reference to Figure 4.
[0058] Ainsi, selon le mode de réalisation de la figure 4, le dispositif 2 comprend au moins : Un embout cannelé 16 en acier inoxydable pour flexible, un raccord adaptateur 18 (ISO-KF16), un collier 20 (ISO-DN16), un joint 22, un seconde rampe à gaz 6, un manomètre 8 en acier inoxydable, un té d’union 24 en acier inoxydable, un coude 26 en acier inoxydable, un robinet vanne à boisseau 10 en PTFE acier inoxydable 3 voies, un tube cintré 28, une première rampe à vide 4, le moyen de connexion 14 est un connecteur pour flexible en acier inoxydable 30 (ISO-316) , un anneau de centrage avec filtre 32 en acier inoxydable (ISO-KF16), un anneau de centrage 34 en acier inoxydable (ISO-DN16), un clapet de surpression 25 avec ressort taré à 0,35 bar, un obturateur 36 en acier inoxydable (ISO-DN16). Thus, according to the embodiment of Figure 4, the device 2 comprises at least: A fluted end piece 16 in stainless steel for a hose, an adapter fitting 18 (ISO-KF16), a collar 20 (ISO-DN16) , a seal 22, a second gas ramp 6, a pressure gauge 8 in stainless steel, a union tee 24 in stainless steel, an elbow 26 in stainless steel, a 3-way stainless steel PTFE ball valve 10, a bent tube 28, a first vacuum ramp 4, the connection means 14 is a stainless steel 30 (ISO-316) hose connector, a ring centering ring with filter 32 in stainless steel (ISO-KF16), a centering ring 34 in stainless steel (ISO-DN16), a pressure relief valve 25 with spring rated at 0.35 bar, a shutter 36 in stainless steel (ISO -DN16).
[0059] A la lecture des figures, on notera que plusieurs de ces éléments précités sont présents en plusieurs exemplaires afin de répondre au montage du mode de réalisation prévu. Certains modes de réalisation privilégieront l’utilisation d’une partie des éléments précités mais ne comprendront pas l’ensemble des raccords présents dans le mode de réalisation préféré décrit ci-dessus. On reading the figures, it will be noted that several of these aforementioned elements are present in several copies in order to respond to the assembly of the planned embodiment. Some embodiments will favor the use of some of the aforementioned elements but will not include all of the connectors present in the preferred embodiment described above.
[0060] Pour éviter toute incertitude, il convient de mentionner que les tiges, coudes, tubes ou raccords peuvent avoir une forme en coupe transversale quelconque, comme par exemple, sans s’y limiter, ronde, carrée, elliptique. [0060] For the avoidance of doubt, it should be mentioned that the rods, elbows, tubes or fittings can have any cross-sectional shape, such as, for example, but not limited to, round, square, elliptical.
[0061] Le dispositif 2 peut être intégré à un réseau de distribution générale de gaz ainsi que sur plusieurs hottes en séries. The device 2 can be integrated into a general gas distribution network as well as into several hoods in series.
[0062] L’utilisation du dispositif 2 est aisée, son procédé d’utilisation comprend un enchaînement d’étapes, telles que décrites ci-dessous : une première étape de mise sous vide consistant à chasser tout air compris dans la première rampe à vide 4, à l’aide d’un moyen approprié, tel qu’une pompe à vide ; une deuxième étape de mise en pression de la seconde rampe à gaz 6 à l’aide d’une source de gaz, telle que de l’argon, de l’azote, de l’hélium, de l’oxygène, de l’hydrogène, de l’éthylène, ou un mélange de gaz ; une troisième étape consistant à fermer chaque robinet 10 comportant une vanne, reliant les deux rampes (4, 6) à au moins un contenant, de sorte à positionner la vanne en position fermée ; une quatrième étape consistant à ouvrir la vanne du robinet 10 en position dite « vide » apte à effectuer le vide dans le contenant ; une cinquième étape consistant à tourner cette même vanne du robinet 10 dans une position dite « gaz » apte à remplir le contenant du gaz compris dans la seconde rampe à gaz 6. [0062] The use of the device 2 is easy, its method of use comprises a sequence of steps, as described below: a first vacuum step consisting in expelling any air included in the first vacuum ramp 4, using a suitable means, such as a vacuum pump; a second step of pressurizing the second gas ramp 6 using a source of gas, such as argon, nitrogen, helium, oxygen, hydrogen, ethylene, or a mixture of gases; a third step consisting in closing each tap 10 comprising a valve, connecting the two ramps (4, 6) to at least one container, so as to position the valve in the closed position; a fourth step consisting in opening the valve of the tap 10 in the so-called “vacuum” position capable of creating a vacuum in the container; a fifth step consisting in turning this same valve of the tap 10 into a so-called "gas" position capable of filling the gas container included in the second gas ramp 6.
[0059] La deuxième étape de mise en pression est effectuée jusqu’à ce que la pression dans la seconde rampe de gaz soit comprise entre 0 et 0,35 bar. De préférence, la surpression à atteindre reste constante à 0,15 bar. The second pressurizing step is carried out until the pressure in the second gas ramp is between 0 and 0.35 bar. Preferably, the overpressure to be reached remains constant at 0.15 bar.
[0063] On notera qu’ avantageusement le marquage des vannes permettra d’effectuer les étapes 3 à 5 sans risque de confusion. [0063] It will be noted that advantageously the marking of the valves will make it possible to carry out steps 3 to 5 without risk of confusion.
[0064] Avantageusement, les étapes 3 à 5 sont répétées par cycle à la suite au moins trois fois pour effectuer un inertage dans le contenant. Advantageously, steps 3 to 5 are repeated per cycle in succession at least three times to perform inerting in the container.
[0065] Selon un mode de réalisation, l’étape 4 pourra comprendre une étape de chauffage du contenant afin de vaporiser des traces d’eau dans ce dernier et les évacuer à travers la rampe à vide. According to one embodiment, step 4 may include a step of heating the container in order to vaporize traces of water in the latter and evacuate them through the vacuum ramp.
[0066] Les modes de réalisation qui ont été décrits en détails ci-dessus ne sont pas limitatifs de l’invention. En tout état de cause, l'invention ne saurait se limiter aux modes de réalisation spécifiquement décrits dans ce document, et s'étend en particulier à tous moyens équivalents et à toute combinaison techniquement opérante de ces moyens. The embodiments which have been described in detail above are not limiting of the invention. In any event, the invention cannot be limited to the embodiments specifically described in this document, and extends in particular to all equivalent means and to any technically effective combination of these means.
REFERENCES NUMERIQUES DIGITAL REFERENCES
1 - Système de l’art antérieur 1 - Prior art system
2 - Dispositif de l’invention 2 - Device of the invention
3 - Double rampe en verre 3 - Double glass ramp
4 - Première rampe à vide 4 - First empty ramp
6 - Seconde rampe à gaz 6 - Second gas ramp
7 - Contenant 7 - Container
8 - Manomètre 8 - Manometer
9 - Source de gaz 9 - Gas source
10 - Robinet 10 - Faucet
11 - Source de vide 12 - Vanne trois voies 11 - Vacuum source 12 - Three-way valve
13 - Premier piège 13 - First trap
14 - Moyen de connexion 14 - Means of connection
15 - Second piège 16 - Embout cannelé 15 - Second trap 16 - Grooved tip
18 - Raccord adaptateur 18 - Adapter fitting
20 - Collier 20 - Necklace
22 - Joint 22 - Gasket
24 - Té d’union 25 - Clapet de surpression 24 - Union tee 25 - Pressure relief valve
26 - Coude 26 - Elbow
28 - Tube cintré 28 - Curved tube
30 - Connecteur pour flexible 30 - Connector for hose
32 - Anneau de centrage avec filtre 34 - Anneau de centrage 32 - Centering ring with filter 34 - Centering ring
36 - Obturateur 36 - Shutter

Claims

REVENDICATIONS
1. Dispositif (2) de rampe à vide pour la synthèse et/ou la manipulation de composants sensibles à l’air comprenant au moins une première rampe à vide (4) destinée à être connectée à une source de vide et une seconde rampe à gaz (6) destinée à être connectée à une source de gaz, et au moins un robinet (10), ce dernier étant au moins à trois voies (12) disposé de sorte à connecter alternativement la première rampe à vide (4) ou la seconde rampe à gaz (6) en surpression à un contenant, caractérisé en ce que la seconde rampe à gaz (6) est apte à résister à une surpression comprise entre 0,10 et 0,40 bar, la première rampe à vide (4) est en acier inoxydable et/ou en polytétrafluoroéthylène, et la seconde rampe à gaz (6) est en acier inoxydable et/ou en polytétrafluoroéthylène. 1. Vacuum ramp device (2) for the synthesis and/or manipulation of air-sensitive components comprising at least a first vacuum ramp (4) intended to be connected to a vacuum source and a second vacuum ramp (6) intended to be connected to a source of gas, and at least one tap (10), the latter being at least three-way (12) arranged so as to alternately connect the first vacuum ramp (4) or the second gas ramp (6) under overpressure to a container, characterized in that the second gas ramp (6) is capable of withstanding an overpressure of between 0.10 and 0.40 bar, the first vacuum ramp (4 ) is made of stainless steel and/or polytetrafluoroethylene, and the second gas manifold (6) is made of stainless steel and/or polytetrafluoroethylene.
2. Dispositif (2) selon la revendication 1 dans lequel la seconde rampe à gaz est apte à résister à une surpression constante et/ou variable, de préférence constante à 0,15 bar. 2. Device (2) according to claim 1 wherein the second gas train is able to withstand a constant and/or variable overpressure, preferably constant at 0.15 bar.
3. Dispositif (2) selon la revendication 1 ou 2, dans lequel la première rampe à vide (4) et la seconde rampe à gaz (6) sont en acier inoxydable. 3. Device (2) according to claim 1 or 2, wherein the first vacuum ramp (4) and the second gas ramp (6) are made of stainless steel.
4. Dispositif (2) selon la revendication 1 ou 2, dans lequel la première rampe à vide (4) et la seconde rampe à gaz (6) sont en polytétrafluoroéthylène. 4. Device (2) according to claim 1 or 2, wherein the first vacuum ramp (4) and the second gas ramp (6) are made of polytetrafluoroethylene.
5. Dispositif (2) selon la revendication 1 ou 2, dans lequel la première rampe à vide (4) est en acier inoxydable et la seconde rampe à gaz (6) est en polytétrafluoroéthylène. 5. Device (2) according to claim 1 or 2, wherein the first vacuum ramp (4) is made of stainless steel and the second gas ramp (6) is made of polytetrafluoroethylene.
6. Dispositif (2) selon la revendication 1 ou 2, dans lequel la première rampe à vide (4) est en polytétrafluoroéthylène et la seconde rampe à gaz (6) est en acier inoxydable. 6. Device (2) according to claim 1 or 2, wherein the first vacuum ramp (4) is polytetrafluoroethylene and the second gas ramp (6) is stainless steel.
7. Dispositif (2) selon l’une quelconque des revendications précédentes, selon lequel la seconde rampe à gaz (6) est connectée à sa sortie à une soupape de surpression. Dispositif (2) selon l’une quelconque des revendications précédentes, selon lequel le robinet (10) est en acier inoxydable avec au moins un siège en polytétrafluoroéthylène. Système comportant le dispositif (2) selon l’une quelconque des revendications 1 à 8, selon lequel il comprend une source de vide (11), une source de gaz (9) et une soupape de surpression. Procédé de mise en œuvre du dispositif (2) selon l’une quelconque des revendications 1 à 8, comprenant : une première étape de mise sous vide consistant à chasser tout air compris dans la première rampe à vide (4), à l’aide d’un moyen approprié, tel qu’une pompe à vide ; une deuxième étape de mise en pression de la seconde rampe à gaz (6) à l’aide d’une source de gaz, tel que de l’argon, de l’azote, de l’hélium, de l’oxygène, de l’hydrogène, de l’éthylène ou un mélange de ces derniers ; une troisième étape consistant à fermer chaque robinet (10) comportant une vanne, reliant les deux rampes (4,6) à au moins un contenant, de sorte à positionner la vanne en position fermée ; une quatrième étape consistant à ouvrir la vanne du robinet (10) en position dite « vide » apte à effectuer le vide dans le contenant ; une cinquième étape consistant à tourner cette même vanne du robinet (10) dans une position dite « gaz » apte à remplir le contenant du gaz compris dans la seconde rampe à gaz (6). Procédé selon la revendication précédente, selon lequel les étapes 3 à 5 sont répétées par cycle à la suite au moins deux fois, de préférence trois fois pour effectuer un inertage dans le contenant. Procédé selon l’une des revendications 10 ou 11, selon lequel la mise en pression amène à une suppression, de préférence constante à 0,15 bar. Procédé selon l’une des revendications 10 à 12, selon lequel la quatrième étape comprend une étape de chauffage du contenant pour évacuer l’eau résiduelle. 7. Device (2) according to any one of the preceding claims, wherein the second gas train (6) is connected at its outlet to a pressure relief valve. Device (2) according to any one of the preceding claims, in which the valve (10) is made of stainless steel with at least one seat made of polytetrafluoroethylene. System comprising the device (2) according to any one of Claims 1 to 8, according to which it comprises a vacuum source (11), a gas source (9) and a pressure relief valve. Method for implementing the device (2) according to any one of Claims 1 to 8, comprising: a first vacuum step consisting in expelling any air included in the first vacuum ramp (4), using by a suitable means, such as a vacuum pump; a second step of pressurizing the second gas ramp (6) using a source of gas, such as argon, nitrogen, helium, oxygen, hydrogen, ethylene or a mixture of these; a third step consisting in closing each tap (10) comprising a valve, connecting the two ramps (4,6) to at least one container, so as to position the valve in the closed position; a fourth step consisting in opening the tap valve (10) in the so-called "vacuum" position capable of creating a vacuum in the container; a fifth step consisting in turning this same tap valve (10) into a so-called “gas” position capable of filling the gas container included in the second gas manifold (6). Method according to the preceding claim, according to which steps 3 to 5 are repeated per cycle in succession at least twice, preferably three times to carry out inerting in the container. Method according to one of Claims 10 or 11, according to which the pressurization leads to a suppression, preferably constant at 0.15 bar. Method according to one of Claims 10 to 12, according to which the fourth step comprises a step of heating the container to evacuate the residual water.
PCT/FR2022/052180 2021-11-25 2022-11-25 Positive-pressure multiway inerting device WO2023094781A1 (en)

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FR2112513A FR3129302A1 (en) 2021-11-25 2021-11-25 Overpressure multi-way inerting device
FRFR2112513 2021-11-25

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FR3129302A1 (en) 2023-05-26

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