FR2831646A1 - Purging gas distribution line fed with bottled gas involves using connector with inlets for both gas and purge gas, and equipment to circulate purge gas through distribution line - Google Patents

Abstract

Connector (22) for a gas bottle (2) to a gas distribution line (12), for use on the tap (23) of a gas bottle, has means (11, 13) of circulating a purge gas first in contact with the tap outlet, then to direct the purge gas in the direction of the gas distribution line. The connector has a body on the tap and two inlets, one for a purge gas feed line (8) and the other for the gas distribution line (12). Independent claims are included for; (1) A device for supplying gas from a gas bottle which has a tap to a gas distribution line, containing a connector as described above, a gas distribution line and a purge gas feed line. The device for supplying gas also has means of circulating the purge gas through the tap outlet or in at least part of the gas distribution line. The device also includes means of purging the gas distribution line, means (14, 16, 17) of distributing the gas to at least one gas cell (18), a balancing volume (16) which feeds a gas distribution tube (17), a pump (21), gas outlets from the gas cells with tubes and electromagnetic valves, and discharges for the gas distribution line which carry flow regulators and means of opening and closing. The gas supply system uses several gas bottles, each with a gas feed device as described above and with the various purge gas supply lines connected to a common gas purge inlet; and (2) A cleaning process for a gas distribution system comprising a gas bottle carrying a connector as described above, through which the cleaning or purge gas is supplied, or with the cleaning or purge gas supplied direct to the distribution line so the gas bottle can be removed while the distribution line is filled with cleaning gas under pressure.

Description

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Method for cleaning a conditioning system and filling gas volumes Technical field and prior art
The invention relates to the field of packaging and filling volumes of gas, in particular small volumes of gas, of the order of a few milliliters.

 It also relates to the techniques for cleaning devices for filling volumes or small volumes of gas, such devices having to be able to ensure gas conditioning under very good conditions of cleanliness and purity.

 A device is known, represented diagrammatically in FIG. 1, which makes it possible to fill small cells 18 with gas, of a volume of a few milliliters each, from a standard bottle 2, while retaining a certain quality at point d 'use, that is to say with a maximum impurity content of the order of ppm.

 This known filling machine comprises, in addition to the bottle 2, a valve 4 and a regulator 6 which make it possible to bring the gas to a distribution line 12. A valve 14 and a buffer volume 16 then make it possible to precisely distribute gas in each of the cells 18.

 The system also comprises a purge line 8 for purging the system using an inert gas, generally nitrogen, and a pumping line 20.

 Prior to the filling operations of the cells 18, a cleaning phase of the distribution line 12 is carried out.

 To this end, the gas supply to the bottle 2 is cut off and the volume of the distribution line 12 is pumped.

 Then, the valve 10 is open, the purge gas is injected into the distribution line, into the volume 16 and into the cells 18.

 After closing the valve 10, pumping is again carried out, this time to remove the inert gas present in the distribution system.

 This produces a succession of pressurization cycles, with the inert gas, and pumping, of the distribution system.

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 In practice, approximately 10 pressurization and pumping cycles are carried out, which makes it possible to obtain a certain rate of decontamination or purity.

 However, this system does not allow satisfactory decontamination or purity levels to be achieved.

 The problem therefore arises of finding another method and a new filling device, more efficient than the known method.

Statement of the invention
The invention firstly relates to a connecting element of a gas cylinder to a distribution line of this gas, intended to be mounted on a valve of a gas bottle, comprising means for circulating a purge gas, first in contact with the valve outlet, then to direct the purge gas towards a gas distribution line.

 The invention also relates to an element for connecting a tap of a gas cylinder to a distribution line for this gas, intended to be mounted on said tap, comprising two inlets, one for a line of supply of purge gas, and the other for said distribution line of this gas.

 Such a connecting element makes it possible to pass the purge gas, first in contact with the outlet of the tap of the gas supply bottle, then in the line the gas distribution.

 It is thus possible to purge the outlet of the tap as well as at least part of the distribution system, located upstream, near the tap of the bottle.

 A device for supplying gas to a gas distribution line, according to the invention, comprises a connection element as above, a line for supplying purge gas, and a gas distribution line .

 Means can be provided for passing the purge gas directly from the purge gas supply line to the gas distribution line.

 Thus, the gas distribution line can be kept under purge gas pressure even when the bottle or the valve is not

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 connected or not connected to the connection element or the distribution line.

 According to another aspect, purging means can be provided on the distribution line, in particular near the connection element of the gas cylinder, thus making it possible to purge the connection element itself as well as the outlet of the tap, and the part of the distribution line located near the cylinder valve, regardless of any bleeding of the entire distribution line.

 According to yet another aspect, a gas supply device according to the invention may also comprise means for discharging the distribution line, located at a point downstream from this line.

 Thus, it is possible, during a cleaning cycle using pressurization of the distribution line with an inert gas, to let part of the inert gas escape by the discharging means, which reinforces the cleaning efficiency by sweeping inert gas.

 In order to be able to fill at least one gas cell, gas distribution means can also be provided, as well as means for discharging these distribution means.

 It is thus possible, when the inert gas is pressurized from the distribution line and the distribution means, an escape of part of this inert gas. The dynamic effect caused by the scanning of the system by the inert gas to its exhaust point then improves the quality of the cleaning of the system.

 According to one example, the distribution means comprise a buffer volume, and discharge means are provided at the outlet of this buffer volume.

 According to yet another aspect, evacuation means can be provided to let escape an overflow of gas distributed in the cell (s) to be filled.

 Spill means can then be provided at the outlet of these evacuation means.

 It is therefore possible to pressurize, by inert gas, the entire distribution system. The discharge means allow part of the inert gas or the purge gas to escape, thereby creating a sweep of the entire part of the

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 distribution located upstream of the discharge means, including in the cells, which reinforces the efficiency of the cleaning operation with inert gas.

 When the discharge means are located at the outlet of the discharge means, the entire distribution system, as well as the cells, which is traversed by a stream of inert gas or purge (impurities sweeping effect), which allows significantly improve the conditions of cleanliness and purity for any subsequent packaging or filling operation.

 In order to facilitate the pumping operations, implemented during the cleaning phase, one or more valve (s) may or may be provided on the gas evacuation means from the cells. These valves are closed during pumping operations. Thus, pumping does not have to be carried out on the entire gas sampling system, which is particularly advantageous when this system comprises one or more tubes of diameter narrower than the diameter of the tubes of the distribution system. This also avoids back-contamination of the system.

 The subject of the invention is also a device for supplying gas to a gas distribution line, comprising a purge gas supply line, a gas distribution line, and distribution means for distributing the gas from the distribution line to at least one cell, characterized in that it also comprises means for discharging the distribution line or distribution means.

 Thus, it is possible, during a cleaning cycle using a pressurization of the distribution line with an inert gas, to let part of the inert gas escape by the discharging means, which promotes cleaning effective, by a dynamic sweeping effect of the impurities, in particular of all the part of the distribution system located upstream of the discharging means.

 The discharge means may be located at the outlet or downstream of the distribution line, between this line and the distribution means, or at the outlet of the distribution means, for example at the outlet of a buffer volume which feeds at least one gas distribution.

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 According to yet another aspect, the invention also relates to a device for supplying gas to a gas distribution line, comprising a line for supplying purge gas, a gas distribution line, means distribution means for distributing the gas from the distribution line to at least one cell, means for discharging at least part (the overflow) of a gas located in said gas cell or cells, and discharge means of the discharge means located at the outlet or downstream of these discharge means.

 It is then the entire distribution line, distribution means, and sample tubes which is swept by a weak stream of cleaning gas.

 The invention also relates to a method for cleaning a gas distribution system using a device according to the invention, as described above, in one or other of the embodiments.

 It relates in particular to a method of cleaning a gas distribution system, comprising a gas bottle fitted with a tap and a gas distribution line, into which a cleaning or purging gas is introduced in contact with the outlet. from the cylinder valve, then to at least part of the gas distribution line located near the cylinder and its valve.

 It also relates to a process for conditioning gas in cells, previously implementing a cleaning process according to the invention or using a device according to the invention, as described above, in one or the another of the embodiments.

 Brief description of the figures - FIG. 1 represents a known device for distributing gas in cells, - FIGS. 2A to 4 represent various embodiments of the invention for the injection of inert gas into a gas distribution system,

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 - Figures 5 to 7 show various embodiments of a gas distribution system according to the invention, with overflow means, - Figure 8 shows a variant of a gas distribution system according to the invention, - FIG. 9 shows another embodiment of the invention, with several gas distribution lines.

Detailed description of embodiment of the invention
In the different zero-rated figures below, the references 2 - 8, 12-20 designate elements identical or similar to those already described above in connection with FIG. 1.

 FIG. 2A represents a first embodiment, in accordance with the invention, of an inert gas injection system in a gas distribution system.

 Unlike FIG. 1, the line 8 for injecting inert gas is connected to the valve 23 of the bottle 2, and this by means of a double-inlet connector 22 making it possible to connect to the valve at the same time. line 8 for injecting inert gas and line 12 for distributing gas.

 The injection of inert gas is controlled by the opening of a variable flow valve 24.

 Thus, a purge gas, for example nitrogen, performs a path indicated by arrow 7 and therefore first circulates in the vicinity of, or against, the outlet of the tap 23 (or again: against the valve or the valve outlet shutter), then is directed (arrow 9) in the direction of distribution line 12.

 An effective cleaning is thus obtained on the one hand from the part of the valve 23 which is in contact with the purge gas, and on the other hand from the part of the distribution line located between the regulator 6 and the valve 23.

 Cleaning can be carried out using pumping means 21, which make it possible to pump the distribution line after it has been pressurized with inert gas. It is thus possible to carry out a succession of cycles each comprising a pressurization phase under inert gas, then a pumping phase.

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Reference 25 designates means for cryogenic trapping of impurities.

 FIG. 2B shows an exemplary embodiment of a double-inlet connector 22. This connector has a longitudinal main body 5, traversed by two conduits 11 and 13 opening onto openings 15 and 27.

 The connector comes to bear, by means of a tonic seal 31, on a tap of a gas cylinder, and is fixed to this tap by screwing a part 29 provided with an internal thread 19.

 An inert gas enters through the opening 15, circulates in the conduit 11, passes in contact with the outlet of the tap, then circulates in the conduit 13 and exits, towards the distribution line, through the opening 27.

 According to a variant, shown in FIG. 3, means 26 (here a valve) make it possible to pass the purge gas directly from the supply line 8 of purge gas to the gas distribution line 12.

This variant makes it possible to leave the gas distribution system in purge, under inert gas pressure, even when no bottle is connected to the double-inlet connector 2: the valves 4 and 24 are then closed and the valve 26 is opened. .

 FIG. 4 represents yet another variant: purging means 28 make it possible to clean only the outlet of the valve 23 and the part of the distribution line located near the valve, between the latter and the valve 28 purge. To this end, the valve 4 is closed and the valves 24 and 28 are opened.

 It is thus not necessary to purge the entire system in order to be able to purge or clean the outlet of the tap and the part of the distribution line located near the tap. This variant can be combined with the variant of Figure 3 above.

 FIGS. 5A and 5B represent another aspect of the invention, in which discharge means are provided on the distribution line 12, or at the outlet or at a point situated downstream of this line, upstream of the distribution means 14, 16.

 These discharge means comprise pressure regulation means, for example a valve 32 with variable flow and a valve 34.

 When the gas distribution system is pressurized with inert or purge gas, it is possible to slightly open the

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 valve 32 and open valve 34, thus allowing part of the inert or purge gas to escape.

 The distribution line 12 is then traversed and swept by a stream of inert gas, which reinforces the effectiveness of the cleaning, impurities being entrained by this stream even before any pumping phase.

It is possible to carry out a succession of pressurization, by inert gas, then of pumping, of the distribution system; but, during the pressurization phase, the distribution line can thus be dynamically cleaned
This cleaning effect by a stream of inert gas or purging occurs, whether the injection of this gas takes place directly on the valve of the gas bottle 2, as illustrated in FIG. 5A, or on the distribution line 12 , as shown in Figure 5B. The device of FIG. 5B does not use the double inlet connection of FIGS. 2A-5A, nor the cleaning of the tap 23.

 Cleaning of the entire distribution line, from the valve 23, is however only achieved with the embodiment of FIG. 5A, the injection of purge gas on the valve of the bottle 2 can also take place according to one of the embodiments already indicated above in conjunction with FIGS. 3 and 4.

 FIG. 6 represents a variant in which the overflow means are connected, not on the distribution line 12 but more downstream in the distribution system, on the buffer volume 16 or downstream of this volume.

 The discharge means comprise pressure regulation means, for example two valves 42, 44, the valve 42 being of variable flow.

 It is then possible, as in the case explained above in connection with FIGS. 5A and 5B, to carry out a dynamic pressurization of inert gas or purge, by sweeping using this gas. This scanning concerns not only the distribution line 12 but also the distribution means 14, 16 which are also traversed by a stream of nitrogen or inert gas when the entire distribution system is pressurized.

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 Again, the injection of inert gas can take place either on the cylinder valve, as shown in Figure 6, or directly on the distribution line, as in the case of Figure 5B.

 It is however preferable, to obtain the best possible cleanliness, to clean the whole line and the outlet of the tap of the bottle, as shown in Figure 6.

 Again, the injection of inert gas can take place according to one of the embodiments illustrated above in conjunction with FIGS. 2A, 2B, 3 or 4, FIG. 6 representing the case where all the options (valve 26 and 28) are included.

 FIG. 7 represents yet another embodiment, in which evacuation means (here: tubes) 56 make it possible to evacuate the overflow of gas introduced into the cells 18.

 Spill means 50, located downstream or at the outlet of these evacuation means, and comprising pressure regulation means, for example two valves 52, 54, allow the overflow of gas coming from the cells 18 to escape.

 It is thus possible to carry out dynamic cleaning, not only of the distribution line 12 (as in FIG. 5A or 5B) or of the distribution means 14, 16, located upstream of the cells to be filled (as in FIG. 6 ), but also cells 18 themselves.

 The inert gas can therefore be introduced under pressure into the entire distribution system, including into the cells, a stream of gas passing through the entire system when the valves 52, 54 are open.

 One can then proceed, as in the other embodiments, to a succession of pressurization cycles, by an inert gas, throughout the distribution system, then pumping of the entire system.

 According to a particular embodiment, valves or solenoid valves 58 can be provided on the tubes 56. These valves, or solenoid valves, allow, during the pumping phase of a cleaning cycle, to isolate the part located downstream of the cells 18, which avoids imposing too great a pressure drop on the

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 pumping, and to avoid back contamination by pollution which may be downstream.

 This may also be particularly advantageous when the tubes 56 are of smaller diameter than the diameter of the tubes used for the distribution system, upstream of the cells 18 (this avoids imposing an additional pressure drop).

 Again, there is shown in Figure 7 a distribution system with injection of purge gas at the valve 23 of the gas bottle. However, the purge gas can also be injected directly onto the distribution line 12 (as in the case of FIG. 5B), the first embodiment being however more advantageous for a complete cleaning of the entire system of distribution.

 According to a variant, the injection of inert gas at the level of the tap of the bottle can be carried out according to one or other of the embodiments described above in conjunction with FIGS. 2A to 4.

 FIG. 8 represents yet another variant, in which the buffer volume 16 is put directly in contact with! e pumping system 21 by means 60, and in particular of a valve 62. It is thus possible to pump as close as possible to the cells 18, and thus improve the quality of the vacuum, and therefore of the cleaning, of these cells. This embodiment can be used in combination with any of the embodiments already described above.

 Figure 9 shows the use of a purge system according to the invention, but in connection with a plurality of distribution lines.

As can be seen in this figure, a common inlet 71 for inert gas can be used for different bottles 72, 82, 92, 102, the gas injection being carried out at the valve 73, 83, 93, 103 of each of the bottles. As a variant, this injection can in fact take place according to one or other of the embodiments of the invention described above in conjunction with the preceding figures.

 Furthermore, overflow means 70.80, 90.100 can be provided for each distribution line. These overflow means are represented, in FIG. 9, in the variant explained above in conjunction with FIG. 5 A. It is however also possible to use, for one or the other of the distribution lines, one of the modes of Figures 6 or 7. Similarly, direct communication between each

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 buffer volume and the corresponding pumping system can be established for one or more of the distribution systems, in accordance with what has been described above in connection with FIG. 8.

 Whatever the embodiment envisaged, it is possible to carry out a succession of filling cycles of the distribution system with inert gas, then pumping.

A process for packaging or filling cells
18 with inert gas will first implement a cleaning process according to one of the embodiments described above. The inert gas supply will then be closed. pumping of the entire distribution system, then opening the tap 23. A cell filling step is thus carried out.

Claims (28)

1. Connection element (22) of a gas cylinder (2) to a line (12) for distributing this gas, intended to be mounted on a tap (23) of a gas cylinder, comprising means ( 11,13) to circulate a purge gas, first in contact with the outlet of the tap, then to direct the purge gas towards a gas distribution line (12).  2. Connection element (22) according to claim 1, comprising a body (5,29), intended to be mounted on said tap (23) and two inlets (15,27), one for a line (8) purge gas supply, and the other for said line (12) of distribution of this gas.  3. Device for supplying gas from a gas bottle (2) fitted with a tap (23), a gas distribution line, comprising a connection element (22) according to the one of claims 1 or 2, a gas distribution line (12) and a purge gas supply line (8).  4. Device for supplying gas, from a gas cylinder (2.72, 82.92, 102) provided with a tap (23.73, 83.93, 103), of a line (12) gas distribution, comprising a line (8,71) for supplying purge gas, and means (22) for circulating the purge gas first in contact with the outlet of the valve, then in at least part of the gas distribution line 5. Device according to claim 4, the means for circulating the purge gas comprising a connecting element (22) to said line (12) of distribution of this gas, intended to be mounted on said valve (23), this element connection comprising two inlets (15, 27), one for the line (8) for supplying purge gas, and the other for said line (12) for distributing this gas, and making it possible to circulate the purge gas, first in contact with the valve outlet, then in at least part of the gas distribution line. <Desc / Clms Page number 13>  6. Device according to one of claims 3 to 5, further comprising means (26) for passing the purge gas directly from the supply line (8) of purge gas to the gas distribution line ( 12).  7. Device according to one of claims 3 to 6, further comprising means (28) for purging the distribution line (12), connected to the part of the gas distribution line, in which the gas can flow purge.  8. Device according to one of claims 3 to 7, further comprising means (14,16, 17) for distributing gas to at least one gas cell (18).  9. Device according to claim 8, the means (14, 16, 17) of gas distribution comprising a buffer volume (16) which feeds at least one tube (17) of gas distribution.  10. Device according to claim 8 or 9, further comprising pumping means (21) and means (60,62) for putting in direct contact these pumping means and said means (14,16,17) for distributing gas.  11. Device according to one of claims 8 to 10, further comprising means (56,58) for discharging a gas located in said or said ce "u! E (s) (18) of gas.  12. Device according to claim 11, said discharge means comprising at least one discharge tube (56).  13. Device according to claim 11 or 12, said discharge means further comprising at least one valve or an electromagnetic valve (58). <Desc / Clms Page number 14>  14. Device according to one of claims 3 to 13, further comprising overflow means (30,70, 80,90, 100) of the gas distribution line (12).  15. Device according to one of claims 8 to 13, further comprising overflow means (40) means (14,16, 17) of gas distribution.  16. Device according to one of claims 11 to 13, further comprising discharge means (50) means (56,58) for evacuation.  17. Device according to one of claims 14 to 16, said overflow means comprising means (32,42, 52) for adjusting the flow rate of a gas escaping through these overflow means.  18. Device according to one of claims 14 to 17, said overflow means comprising means (34,44, 54) for opening and closing.  19. Gas supply device, from a plurality of gas bottles (72,82, 92,102), each bottle being associated with a gas supply device according to one of claims 3 to 18, the various purge gas supply lines being connected to a common purge gas inlet (71).  20. Method for cleaning a gas distribution system, comprising a gas bottle (2) provided with a tap (23) and a gas distribution line (12), into which a cleaning gas is introduced or purge in contact with the outlet of the valve (23) of the cylinder, then in at least part of the gas distribution line.  21. The method of claim 20, wherein the supply of cleaning gas is closed in the direction of the tap (23) and the cleaning gas is introduced directly into the gas distribution line. <Desc / CRUD Page number 15>  22. Method according to the preceding claim, wherein the gas distribution line is left under cleaning gas pressure, after having dismantled the gas bottle.  23. Method according to one of claims 20 to 22, in which the cleaning gas is purged using purging means (28), connected to a point in the part of the distribution line in which the cleaning gas cleaning is introduced.  24. Method according to one of the preceding claims 20 to 23 wherein, during cleaning, part of the cleaning gas contained in the distribution line escapes from a point located downstream of the distribution line.  25. Method according to one of claims 20 to 23, wherein the cleaning gas is introduced into gas distribution means (14,16) located downstream of the gas distribution line, part of the cleaning gas contained in the distribution line (12) and in the distribution means escaping, during cleaning, from a point located downstream of the distribution means.  26. Method according to one of claims 20 to 23, in which the cleaning gas is introduced into cells (18), an overflow of this cleaning gas contained in these cells is evacuated by evacuation means ( 56,58) then escapes, during cleaning, from a point downstream of these means of evacuation- 27. The method of claim 23, wherein only cleaning, by purging with the cleaning gas, said part of the distribution line near the bottle (2) and its valve (23).  28. Method for filling at least one cell (18) with a gas originating from a bottle (2) connected to a gas distribution line (12), comprising: - a cleaning phase according to claim 20 to 27, - a filling phase of the cell (s).