JP5899883B2 - High pressure gas supply method, apparatus having shock wave attenuation mechanism, and high pressure gas supply device - Google Patents

Description

  The present invention relates to a method for supplying high-pressure gas in the case where high-pressure gas is supplied from a high-pressure filled container to various facilities.

  The high-pressure gas here includes widely used combustible gas, combustion-supporting gas, and the like. Generally, it means a gas supplied from a high-pressure filled container, but also includes a gas in a process of being stored in a high-pressure container.

  The gas supplied from the high-pressure filled container is supplied to each device through a valve for introduction. In recent years, the pressure of high-pressure gas filled in a high-pressure vessel tends to increase in order to reduce production loss due to container replacement. In addition, the pressure of the high-pressure gas to be filled tends to increase because of the management merit that the production cost can be reduced by reducing the number of transportation times or the number of cylinders managed on site can be reduced. . Furthermore, the direction in which high-pressure gas filled with high pressure is used at a higher pressure than in the past has become prominent.

  Thus, when increasing the pressure of the gas used, it is necessary to substantially increase the strength of the container itself, the container valve, and the conduit. As a countermeasure, it is more effective to use a thick material for the container itself, the container valve and the conduit. However, due to workability problems, it is desirable to reduce the diameter of the conduit as much as possible, or at least keep the current dimensions. Further, when the diameter of the conduit is increased, it is necessary to increase the thickness from the viewpoint of safety, but the increase in cost cannot be denied. Furthermore, there is a strong demand from the user side to make the most of existing equipment as much as possible. For example, it is practically difficult to switch a currently used 1/8 to 1 inch pipe to a thicker pipe.

  On the other hand, prevention of leakage is extremely important from the viewpoint of safety. That is, the target gas is a flammable gas, a flammable gas, and the like, and leakage causes various major problems such as a fire and an explosion accident. For this reason, in addition to preventing leakage from the container itself, the container valve, and the conduit cylinder, it is extremely important to prevent leakage from a portion connecting the container valve, the conduit, and the like. Portions connecting container valves, conduits, and the like are particularly important because they can take a complex structure and are prone to leakage. If it is assumed that the container valve is closed, a leak may result in a major accident if the container valve results in a state similar to opening. Among various parts in the container valve, the sealing material is likely to cause a leakage problem. In addition, the sealing portion is improved by using packing or the like in the connecting portion, but there are many leaks from this portion. For this reason, the confidentiality of the sealing material has been particularly reviewed, and since its shape followability is important, generally soft resin materials tend to be used.

  However, a resin material having good shape followability generally has a problem that it is weak in chemical durability and thermal durability. That is, depending on the high-pressure gas and its atmosphere, in addition to deterioration of strength and cracks, thermal deformation and melting phenomenon may occur, and in some cases, it may burn out. However, there are many unclear points as to under what conditions such a phenomenon occurs, and therefore the countermeasures cannot be fully taken.

  In Patent Document 1, a part of the gas cylinders is opened and high pressure is supplied to the air supply source valve so as not to cause troubles such as the heat generation in the piping accompanying the adiabatic compression and the combustion of the combustible gas. A high-pressure gas introduction method is disclosed in which gas is introduced and then the remaining gas cylinders are opened.

Patent Document 2 discloses a high-pressure gas quantitative supply device that opens and closes a gas supply channel and a gas circulation channel in a short cycle by a switching means so that a high-pressure gas such as a foaming agent can be quantitatively supplied in a gas state. It is disclosed. Further, this document also discloses that the differential pressure between the primary side and the secondary side is maintained at about 3 MPa (30 kg / cm ² ) or less by the flow rate adjusting valve.

  In Patent Document 3, in order to supply a high-pressure gas having a high Joule-Thompson effect from a gas container to a user stably over a long period of time, pressure control is performed by using a parallel orifice device and a plurality of decompression lines thereof. A gas supply device and a gas supply method are disclosed.

Patent Document 4 discloses that a high-pressure water vapor at 200 to 400 ° C. is instantaneously injected to generate a shock wave, and further converged to generate a convergent shock wave. A manufacturing method is disclosed.
Patent Document 5 discloses a container valve that supplies a high concentration fluorine gas to a semiconductor manufacturing system at a high pressure.

  Further, Patent Document 6 discloses a valve in which a rubber seal is disposed at a position recessed from a flame flow path in order to cope with burnout of the rubber seal and a decrease in the sealing function of the seal portion of the valve.

Japanese Patent Laying-Open No. 2005-308185 JP 2004-44650 A JP 2007-255666 A Japanese Patent Laid-Open No. 2004-20412 JP 2005-207480 A JP 2000-291500 A

  The feature of the method described in Patent Document 1 is that the valve of the gas cylinder is opened in a plurality of times, but even if this method is adopted, the ignition phenomenon is not eliminated. It is described that the lower the number opened first, the lower the temperature raised by adiabatic compression. However, this is not necessarily the case, and the ignition phenomenon may become conspicuous.

In the method described in Patent Document 2, an effect is recognized in terms of stability, but the phenomenon of high temperature cannot be avoided. In recent years, there has been an increasing demand for a condition in which the differential pressure between the primary side and the secondary side cannot be about 3 MPa (30 kg / cm ² ) or less.

  Even in the method and apparatus of Patent Document 3, an effect is recognized in terms of stability, but the phenomenon of a high temperature on the downstream side cannot always be avoided.

  Although it is understood from Patent Document 4 that a high-temperature field may accompany when a shock wave is generated, high-temperature water vapor or a converging tube is necessary, and the high-pressure gas filled at high pressure is not high-temperature and has a converging tube. It is not possible to infer whether or not a shock wave is generated under the conditions that do not.

Since the container valve described in Patent Document 5 is a valve that opens and closes a gas flow path with a seat disk and seals the airtightness with the outside with a diaphragm, a dead space in which the gas in the valve chamber tends to stay increases.

  The valve described in Patent Document 6 is a countermeasure against backfire, and cannot be applied to a high-pressure gas filled at a high pressure as it is.

As described above, in the prior art, leakage due to melting, burning, or deterioration of the sealing material generated on the downstream side of the high-pressure gas, particularly high-pressure gas filled with a pressure of 4 MPaG (about 40 kg / cm ² ) or more. It was not possible to prevent the occurrence of

  For example, when a highly corrosive and combustion-supporting halogen gas such as fluorine gas or nitrogen trifluoride gas is introduced into an external device through a supply valve from a container filled with high pressure, the introduction valve on the introduction side The surface corrosion in the valve chamber and the burning and melting of the sealing material become remarkable, and even when the above-described conventional valve is used as the introduction valve, the burning and melting of the sealing material cannot be prevented. In addition, there are many cases where leakage from the connecting portion occurs, and it has been known that this is due to deterioration of the sealing material, but it cannot be said that the countermeasure is sufficient.

The present invention has been made in view of the above-described problems, and is used for surface corrosion of an introduction valve for introducing a filled high-pressure gas to an external device at a pressure of 4 MPaG (about 40 kg / cm ² ) or more, and for an introduction valve. The purpose is to suppress material deterioration such as burning and melting of the sealing material used, or generation of cracks.

When supplying high-pressure gas from a high-pressure filled container to an external device, the present invention has found that a high temperature phenomenon that cannot be explained by simple adiabatic compression phenomenon occurs on the downstream side of the high-pressure filled container. It was made. This phenomenon becomes prominent when the filled high-pressure gas is led to an external device particularly at a pressure of 4 MPaG (about 40 kg / cm ² ) or more.

In the present invention, when a high-pressure gas containing a combustible gas or a combustion-supporting gas filled in a container at high pressure is supplied to an external device at a pressure of 4 MPaG or more through a conduit connected to the on- off valve of the container. The gas is a high-pressure gas supply method that is led to an external device through a device having a shock wave attenuation mechanism and a valve using a sealing material made of a resin material .

The present invention also provides a high-pressure gas supply method in which the conduit has a supply valve for supplying gas from the container to an external device, and the device having the shock wave attenuation mechanism is located downstream of the supply valve. It is.

Further, the present invention, a device having the shock wave attenuation mechanism is a method of supplying high-pressure gas is a device having a mechanism for changing the acoustic shock wave.

In addition, the present invention is a method for supplying high-pressure gas, wherein the device having the shock wave attenuation mechanism is a device having a mechanism that prevents straightness of the shock wave.

In addition, the present invention is an apparatus having a shock wave attenuating mechanism used in the above-described high-pressure gas supply method, in which a baffle plate is disposed in the course of shock waves. In addition, the present invention is an apparatus having a shock wave attenuating mechanism used in the above-described high-pressure gas supply method, in which a spherical, elliptical, or polygonal object is arranged in the course of the shock wave.

In addition, the present invention is a device having a container filled with a high-pressure gas containing a combustible gas or a combustion-supporting gas, an opening / closing valve of the container, and the shock wave attenuation mechanism of the present invention interposed downstream of the opening / closing valve. And a conduit for guiding the gas to an external device through an apparatus having the shock wave attenuating mechanism and a valve using a sealing material made of a resin material.

  According to the present invention, when supplying from a container filled with high pressure to an external device, on the downstream side of the container filled with high pressure, it is supplied to the external device through a shock wave attenuating mechanism that prevents the generation of shock waves. Burnout and deterioration of the introduction valve for guiding the high-pressure gas to the external device and the sealing material in the connecting portion can be suppressed.

It is a systematic diagram for demonstrating the outline | summary of this invention. BRIEF DESCRIPTION OF THE DRAWINGS It is the external appearance schematic of the apparatus which has the shock wave attenuation | damping mechanism in Example 1 of this invention. It is an internal schematic of the apparatus which has the shock wave attenuation | damping mechanism in Example 1 of this invention. It is a systematic diagram for demonstrating Example 3 of this invention. It is an internal schematic which shows arrangement | positioning of the baffle plate of the apparatus which has the shock wave attenuation | damping mechanism in Example 3 of this invention. It is an internal schematic which shows arrangement | positioning of the baffle plate of the apparatus which has the shock wave attenuation | damping mechanism in Example 4 of this invention. It is an internal schematic which shows arrangement | positioning of the baffle plate of the apparatus which has the shock wave attenuation | damping mechanism in Example 5 of this invention. FIG. 10 is an internal schematic diagram of a device of a type in which a baffle plate is not installed inside in Comparative Example 4.

In the high-pressure gas supply method according to the embodiment of the present invention, a supply valve is supplied from a container filled with high pressure to an external device, and a supply valve for supplying high-pressure gas from the container and upstream of the supply valve or A shock wave attenuating mechanism provided downstream. Conventionally, in the supply method and apparatus of this aspect, the influence of shock waves is hardly considered. Conventionally, as disclosed in, for example, Patent Document 1, it is known that the temperature may rise due to adiabatic compression, but it is not the influence of the shock wave, or the influence is extremely small. In addition to the fact that the impact of the shock wave is instantaneous, the need for a special device to confirm the occurrence of the shock wave is one of the major factors that have not taken into account the impact of the shock wave. Seem. The present invention confirms the influence of shock waves that have been ignored so far, and is an epoch-making solution that solves conventional problems all at once.

  An external device is a variety of manufacturing equipment made using high-pressure gas. For example, a heat insulation panel manufacturing apparatus and a semiconductor manufacturing apparatus for mixing a foaming agent are typical examples, but there is no particular limitation, and it may be considered as various types of manufacturing equipment generally used.

  Furthermore, related facilities such as storage facilities in production and maintenance of high-pressure gas are also included. In other words, the present invention can be applied to production facilities where high-pressure gas is produced. That is, it is also applicable when the produced gas is stored in a container and introduced into the next step through a conduit. In the normal case, there is little problem when the production is continuously performed, but the present invention is effective when it becomes suddenly discontinuous. It is unlikely that production will continue forever, and production is usually interrupted by regular repairs, modifications, or unexpected accidents. When resuming production, the problems described above may occur, so it is extremely useful to use the present invention as a countermeasure. In this sense, equipment arranged on the downstream side of the production equipment, for example, a container for storing high-pressure gas and related equipment are also included in the external device.

  The high-pressure gas referred to in the present invention includes commonly used combustible gas, combustion-supporting gas, and the like. Combustible gas sources include acrylonitrile, acrolein, acetylene, acetaldehyde, arsine, ammonia, carbon monoxide, ethane, ethylamine, ethylbenzene, ethylene, ethyl chloride, vinyl chloride, chloromethyl, ethylene oxide, propylene oxide, hydrogen cyanide, cyclopropane, Disilane, diborane, dimethylamine, hydrogen, hydrogen selenide, trimethylamine, carbon disulfide, butadiene, butane, butylene, propane, propylene, bromomethyl, benzene, phosphine, methane, monogermane, monosilane, monomethylamine, methyl ether, hydrogen sulfide Is a typical example.

  In addition, oxygen, ozone, nitrous oxide, nitrogen monoxide, nitrogen dioxide, fluorine, chlorine, chlorine dioxide, nitrogen trifluoride, chlorine trifluoride, silicon tetrachloride, oxygen difluoride, Perchloryl fluoride and the like are included.

  The high-pressure gas described above is a list of typical ones, and is not limited to the characteristics. For example, many halogen gases have both flammability and toxicity.

  The concentration of various gases in the high-pressure gas is not particularly limited, and two or more mixed gases may be used as long as at least one kind of the high-pressure gas described above is included. For example, in the case of a combustion-supporting gas, at least one of fluorine gas, chlorine gas, and the like is in the range of 0.1 vol% or more and 100 vol% or less.

  Hereinafter, a high-pressure gas supply method according to an embodiment of the present invention will be described in detail with reference to FIG.

  A container 1 filled with a high-pressure gas at a high pressure is provided with an on-off valve 2 and can seal the high-pressure gas. The container 1 may be used singly or a plurality of containers 1 connected in parallel. The number of containers is not particularly limited. A conduit 3 is connected to the on-off valve 2 of the container 1, and a supply valve 4 for supplying high-pressure gas from the container 1 to the external device 100 is provided in the conduit 3. A device 50 having a shock wave attenuating mechanism is often provided downstream of the supply valve 4, but the supply valve 4 may be disposed downstream of the device 50 having a shock wave attenuating mechanism. Any one of the on-off valve 2 and the supply valve 4 may have a pressure adjusting function when supplying high-pressure gas downstream. Furthermore, only one of the on-off valve 2 and the supply valve 4 can be used. The container 1 to the conduit 6 are configured as a high-pressure gas supply facility.

A conduit 6 for introducing high-pressure gas into the external device 100 is provided downstream of the device 50 having a shock wave attenuation mechanism, and a receiving valve 101 of the external device 100 is provided upstream of the external device 100. A conduit 102 is connected downstream of the receiving valve 101, and a conduit 103 connected to the external device 100 and an evacuation facility 105 are disposed on the downstream side thereof via the on-off valve 104. In addition, the waste gas treatment facility 130 is generally provided on the downstream side of the external device 100 via the conduits 111 and 112 and the on-off valve 110. However, depending on the gas to be handled, it may be released to the atmosphere. If the high-pressure gas supply part and the external device are in a very close relationship, the receiving valve 101 can be deleted. In this case, it is useful to arrange the device 50 having the shock wave attenuation mechanism as close as possible to the upstream portion of the external device 100.

  The present invention is implemented as follows. The on-off valve 2 and the on-off valve 110 are closed, the supply valve 4 and the receiving valve 101 are opened, and then the on-off valve 104 of the vacuum exhaust equipment 105 is opened to perform vacuum deaeration. After confirming that a predetermined vacuum state has been reached, the supply valve 4 and the on-off valve 104 are closed. Thereafter, the on-off valve 2 is opened while adjusting to a predetermined pressure. After a predetermined pressure is obtained, the supply valve 4 is opened, a predetermined gas is introduced into the external device 100, and production is performed. Although the opening / closing of the on-off valve 110 differs depending on the equipment content of the external device 100 and the gas to be handled, the on-off valve 110 is often opened / closed while observing the production status, and the supply valve 4 is also opened / closed accordingly.

  In particular, it seems that a problem has occurred immediately after the supply valve 4 is opened, but it has not been confirmed. However, by interposing the device 50 having the shock wave attenuation mechanism, the problem occurrence on the downstream side can be eliminated. That is, by implementing the present invention, it was possible to prevent the occurrence of leakage based on melting, burning, or deterioration of the sealing material, which has been considered a problem in the past.

  The shock wave attenuating mechanism is intended to greatly attenuate the shock wave, and is preferably a mechanism that completely eliminates the shock wave. However, if the temperature rise due to the influence of the shock wave is not so large, the effect may be recognized even with slight attenuation.

  It is important that the materials of the container, various valves, conduits, equipment, etc. used in the present invention satisfy the pressure resistance. Stainless steel is often used, but other factors depend on the type of high-pressure gas. For example, manganese steel, stainless steel, and an alloy containing nickel (Hastelloy, Inconel, Monel, etc.) are used.

  It is desirable that the high-pressure gas filled in the container is supplied to the external device at a pressure of 4 MPaG or more. If the pressure is less than 4 MPaG, the generation of shock waves is negligible or negligible. Therefore, the temperature rise in the external device is small, and the burnout and deterioration of the sealing material are unlikely to occur, so the contribution of the present invention is small. At this time, 14.7 MPaG is the practical maximum value, and even if it exceeds 14.7 MPaG, the temperature rise inside the introduction valve can be prevented or reduced by using the present invention. It becomes complicated and large, and practically it is difficult to apply. In addition, depending on the type of gas, there is a problem that corrosion of the surface of the gas contact portion is likely to occur. Therefore, it is preferably 4.5 MPaG or more and 14.7 MPaG or less, more preferably 5 MPaG or more and 14.5 MPaG or less.

  When high-pressure gas is supplied from a supply valve, a shock wave may be generated when the moving speed of the supplied gas exceeds a certain level. This shock wave generation phenomenon is an extremely complicated phenomenon, and it is very difficult to confirm whether or not the shock wave has occurred. When analyzing the effects of shock wave generation, it is extremely difficult unless special equipment is used.

  The shock wave attenuating mechanism is a shock wave attenuating mechanism that attenuates the generated shock wave or a shock wave suppressing mechanism that suppresses the generation of the shock wave by using the property of the shock wave. Hereinafter, representative examples will be shown, but the present invention is not limited thereto.

  A device 50 having a shock wave attenuating mechanism has a structure in which a shock wave inlet and outlet are provided in a stainless steel pipe or the like. The device is preferably located downstream of the on-off valve 2 of the container. This is because when the shock wave attenuating mechanism is located upstream of the container valve, almost no shock wave is generated, so that the effect of the present invention becomes extremely small. Naturally, the device 50 having the shock wave attenuation mechanism may be provided upstream of the receiving valve 101 where the problem of damage to the sealing material of the external device 100 is likely to occur, or two or more devices may be used in combination. . The important point is that it is arranged downstream of the on-off valve 2 of the container. As described above, the external apparatus 100 also includes a high-pressure gas production apparatus. In this case, the downstream side of the high-pressure gas production equipment is also the object.

  It is desirable to have a shock wave attenuating mechanism that converts shock waves into sound waves. Shock waves are generally significantly attenuated, but by changing the shock waves into sound waves, the generation of shock waves can be reduced more effectively. That is, by providing a mechanism for irregularly reflecting or absorbing a shock wave, it can be changed to a sound wave. As specific examples, the methods described below are also effective, but are not limited thereto.

  As the shock wave attenuating mechanism, it is desirable to have a structure that prevents straightness of the shock wave. In general, shock waves generated by gas movement have high straightness. Therefore, by suppressing the straightness, growth of shock waves can be suppressed. For example, it is effective to arrange various baffle plates in the course of the shock wave in the shock wave attenuation mechanism. Further, a spherical object may be arranged in the path of the shock wave in the shock wave attenuation mechanism. In this case, it is more effective to arrange a plurality of spherical objects. The incident shock wave collides with a spherical object and is reflected. By repeating such reflection, the shock wave attenuates and approaches the sound wave as much as possible. Of course, an elliptical object or a polygonal shape may be used. It is also effective to incorporate a mechanism for absorbing shock waves. An arrangement in which the shock wave input to the shock wave attenuating mechanism repeats some reflections and the like repeatedly without going straight is useful.

  Further, it is desirable to use a conduit having a curved portion as the conduit having the shock wave attenuation mechanism. For example, a structure in which the conduit is wound in a coil shape may be used. In this structure, since the conduit is coiled, it is difficult for gas to flow linearly through the conduit, and the growth of the shock wave in the conduit tends to be suppressed. As a result, the shock wave is attenuated.

  Hereinafter, the present invention will be described in detail by way of examples.

  An embodiment will be described with reference to FIG. An on-off valve 2 is mounted on the high-pressure vessel 1 containing a mixed gas composed of fluorine gas and nitrogen gas. The supply valve 4 is disposed between the external device 100 and the on-off valve 2 and the supply valve 4 are connected by a linear stainless steel conduit 3 having an inner diameter of 10.7 mm and a length of 50 mm. Downstream of the supply valve 4 are a conduit 5 for introducing fluorine gas and nitrogen gas to the external device 100, a device 50 having a shock wave attenuation mechanism, and a conduit 6. The conduits 5 and 6 are also made of straight stainless steel having an inner diameter of 10.7 mm, but the length of the conduit 5 is 300 mm. A receiving valve 101 provided upstream of the external device 100 is attached to the downstream side of the conduit 6. In addition to the external device 100, an evacuation facility 105 is connected to the downstream of the receiving valve 101 via an on-off valve 104. The sealing material of the receiving valve 101 is PCTFE (ethylene trifluoride chloride). The evacuation equipment 105 is mainly used for gas replacement in the pipe downstream of the supply valve 4 and in the external device 100. In the present embodiment, the external device 100 is a container similar to the high-pressure container 1. Further, an on-off valve 110 for exhausting is connected downstream of the external device 100.

  A device 50 having the above-described shock wave attenuation mechanism is provided between the supply valve 4 and the receiving valve 101. FIG. 2 shows an appearance of the device 50, and FIG. As shown in FIG. 2, there are an inlet 50 a and an outlet 50 b on the inflow side and the outflow side of the device 50 having a shock wave attenuation mechanism, which match the inner diameters of the conduit 5, the conduit 6, and the receiving valve 101, respectively. The device 50 having the shock wave attenuation mechanism and the receiving valve 101 are connected by a conduit 6, and the receiving valve 101 and the external device 100 are connected by conduits 102 and 103. As shown in FIG. 3, a device 50 having a shock wave attenuating mechanism includes six stainless steel balls 52a having a diameter of 100 mm and an inner diameter of 12 mm and six stainless steel balls 52a having a diameter of 4 mm and a stainless steel ball 52b having a diameter of 4 mm. Are inserted at random. It is presumed that the stainless steel balls arranged at random are acting to exhibit shock wave attenuation. As a result, almost no shock wave is generated at the outlet 50b of the shock wave attenuating mechanism 50.

  The stainless steel container 1 was filled with 20% fluorine gas (the rest was nitrogen gas) that had been filled at a high pressure of 5 MPaG. First, all the valves other than the on-off valve 2 and the discharge valve 110 are opened, and the insides of the conduits 3, 5, 6, 102, 103, and 111, the device 50 having the shock wave attenuation mechanism, and the external device 100 are evacuated. Later, all valves were closed. Thereafter, the on-off valve 2 was opened, and the pressure in the conduit 3 was set to 5 MPaG. Next, the supply valve 4 and the receiving valve 101 are opened almost simultaneously. After 30 seconds have passed after introducing 20% fluorine gas (remaining nitrogen gas) into the external device 100, all the valves are closed, and then The on-off valve 110 was opened, and the nitrogen gas filled in the external device 100 was exhausted.

After the above operation was repeated 10 times, the receiving valve 101 was removed, and when the internal leak amount was measured with a leak detector (HELIOT 102+ manufactured by ULVAC), the leak amount was less than the detection lower limit (1.0 × 10 ⁻⁷ Pa). It was less than m ³ / s) and it was confirmed that there was no leak. Further, when the receiving valve 101 was disassembled and the sealing material was visually observed, no melting, burning, or cracking of the sealing material was observed.

  Next, a conduit having 3 mm-thick PCTFE (ethylene trifluoride chloride) fixed therein was inserted into the receiving valve 101 and used instead. Thereafter, 20% fluorine gas (remaining nitrogen gas) was introduced into the external device 100 under the same conditions as before. After this operation was repeated 10 times, the PCTFE was visually observed, but no PCTFE melting, burning, or cracking was observed.

  Nitrogen trifluoride gas filled at a high pressure of 10.5 MPa was used. The apparatus was almost the same as that of Example 1, but first, a conduit with 3 mm thick PCTFE (ethylene trifluoride chlorochloride) fixed therein was inserted into the position of the conventional receiving valve 101 instead. In the same manner as in the first embodiment, all the valves other than the on-off valve 2 and the discharge valve 110 are opened, and the conduits 3, 5, 6, 102, 103, 111, the device 50 having the shock wave attenuation mechanism, and the external device 100 All the valves were closed after vacuuming. Thereafter, the on-off valve 2 was opened and the pressure in the conduit 3 was set to 10.5 MPaG. Next, the supply valve 4 and the receiving valve 101 are opened almost simultaneously. After 30 seconds have passed after introducing nitrogen trifluoride gas into the external device 100, all the valves are closed and the on-off valve 110 is connected to the external device 100. The nitrogen trifluoride gas filled inside was exhausted. After repeating this operation 10 times, visual observation of PCTFE was carried out, but no melting, burning or cracking of PCTFE was observed.

Next, the receiving valve 101 which made the sealing material PCTFE (ethylene trifluoride chloride) was inserted. After the same operation as in Example 1 was repeated 10 times, the internal leak amount of the introduction valve 5 was measured with a leak detector, and the leak amount was less than 1.0 × 10 ⁻⁷ Pa · m ³ / s. Confirmed that there is no leak. In addition, the receiving valve 101 was disassembled and the sealing material was visually observed, but no melting, burning, or cracking of the sealing material was observed.

  Although it was based on Example 1, the test method was partially changed. FIG. 4 is a system diagram for explanation. An on-off valve 2 is mounted on the high-pressure vessel 1 containing a mixed gas composed of fluorine gas and nitrogen gas. Further, a supply valve 4 is mounted downstream of the on-off valve 2 via a linear stainless steel conduit 3 having an inner diameter of 10.7 mm and a length of 50 mm. Downstream of the supply valve 4 is a conduit 5 for introducing fluorine gas and nitrogen gas. The conduit 5 includes a conduit 5A upstream of the partition wall 55 and a conduit 5B downstream of the partition wall 55, and the length including the partition wall 55 is 300 mm. The conduit 5A and the conduit 5B are also made of linear stainless steel having an inner diameter of 10.7 mm. A Mylar (diaphragm) can be inserted into the partition wall 55, and 50 μm thick Mylar (polyethylene terephthalate) was used. Downstream of the conduit 5B, the conduit 6 is mounted via a device 50 having a shock wave attenuation mechanism. The downstream side of the conduit 6 is inserted into the sealed container 140 in a so-called atmospheric open type state. Downstream of this, there is a conduit 112 provided for introducing waste gas to the waste gas treatment facility 130, and this conduit 112 is inserted into the hermetic container 140 in an open state like the conduit 6. Therefore, the gas fluid exiting from the conduit 6 is once released into the atmosphere, and then led to the waste gas treatment facility 130 through the conduit 112, but all is done in the sealed container 140. A part of the container wall of the sealed container 140 is provided with 140A and 140B glass windows facing each other so that light from the outside can be transmitted. Observation of shock wave generation by the Schlieren method described later is performed through this window.

  FIG. 5 shows the arrangement of baffle plates inside the device 50 having a shock wave attenuation mechanism. As shown in FIG. 2, there are an inlet 50a and an outlet 50b on the inflow side and the outflow side of the device 50 having the shock wave attenuation mechanism, which match the inner diameters of the conduit 5B and the conduit 6, respectively. As is clear from FIG. 5, a baffle plate having an angle of about 60 degrees toward the gas traveling direction is formed inside the device 50 having the shock wave attenuation mechanism.

  The stainless steel container 1 was filled with 20% fluorine gas (the rest was nitrogen gas) that had been filled to a pressure of 7 MPaG. The on-off valve 2 was opened with the supply valve 4 closed, and then the supply valve 4 was opened little by little. When the pressure in the conduit 5A reached about 5 MPaG, the Mylar burst. At this time, whether or not a shock wave is generated from the end portion of the conduit 6 was examined by the Schlieren method. As a result, the generation of shock waves was not confirmed at all.

  Further, the same confirmation as in Example 1 was performed except that the device 50 having the baffle plate of this test was used as the device 50 having the shock wave attenuation mechanism. That is, a tube with 3 mm thick PCTFE (ethylene trifluoride chloride) fixed inside was inserted into the position of the receiving valve 101 and repeated 10 times, and then the PCTFE was visually observed. Neither burning nor cracking was observed.

  A test similar to that of Example 3 was performed except that nitrogen trifluoride gas was used as the gas filled in the container 1 and the apparatus 50 having a shock wave attenuation mechanism having a different baffle plate configuration was used.

  FIG. 6 shows the arrangement of baffle plates inside the device 50 having the shock wave attenuation mechanism used in this test. Even in this case, there are an inlet 50a and an outlet 50b on the inflow side and the outflow side of the device 50 having the shock wave attenuation mechanism, which match the inner diameters of the conduit 5B and the conduit 6, respectively. As is clear from FIG. 6, a baffle plate is formed inside the device 50 having the shock wave attenuating mechanism, and has an angle of about 60 degrees in the traveling direction, but the shock wave attenuating mechanism used in the third embodiment is the same. The number of baffle plates of the device 50 is about half.

  As in Example 3, after opening the on-off valve 2 with the supply valve 4 closed, the supply valve 4 was opened little by little. When the pressure in the conduit 5A reached about 5 MPaG, Mylar burst. At this time, whether or not a shock wave is generated from the end portion of the conduit 6 was examined by the Schlieren method. As a result, the generation of shock waves was not confirmed at all.

  Further, as in Example 3, a pipe with 3 mm thick PCTFE (ethylene trifluoride chloride) fixed therein was inserted into the position of the receiving valve 101 and repeated 10 times, and then PCTFE was visually observed. PCTFE was not damaged, burned, or cracked.

  A test was performed in substantially the same manner as in Example 3 except that the device 50 having a shock wave attenuation mechanism with a different baffle plate configuration was used. In this test, the baffle plate of the device 50 having the shock wave attenuating mechanism is perpendicular to the gas flow, and FIG. 7 shows the arrangement of the internal baffle plate. Even in this case, there are an inlet 50a and an outlet 50b on the inflow side and the outflow side of the device 50 having the shock wave attenuation mechanism, which match the inner diameters of the conduit 5B and the conduit 6, respectively. Even in this case, when there is a device 50 having a shock wave attenuation mechanism, the generation of shock waves by the Schlieren method was not confirmed at all.

  Further, as in Example 3, a pipe with 3 mm thick PCTFE (ethylene trifluoride chloride) fixed therein was inserted into the position of the receiving valve 101 and repeated 10 times, and then PCTFE was visually observed. PCTFE was not damaged, burned, or cracked.

[Comparative Example 1]
A straight stainless steel pipe having the same length and inner diameter as the device 50 having the shock wave attenuation mechanism was inserted without using the device 50 having the shock wave attenuation mechanism used in Example 2. Other than that, it carried out similarly to Example 2, However, It carried out similarly to Example 2 from the test of the pipe | tube which fixed 3 mm-thick PCTFE (ethylene trifluoride chloride) inside. As a result, it was confirmed that PCTFE was burned out. For this reason, it was speculated that at least a thermal load causing self-combustion was applied, that is, a shock wave was generated.

Next, a test was performed using the same receiving valve as in Example 1. As a result, the amount of internal leakage of the receiving valve 101 measured by the leak detector was 1.3 × 10 ⁻¹ Pa · m ³ / s, which was poorly sealed. Further, when the receiving valve 101 was disassembled and the sealing material was visually observed, a part of the sheet material was deformed and deterioration due to burning was recognized.

[Comparative Example 2]
A straight stainless steel pipe having the same length and inner diameter as the device 50 having the shock wave attenuation mechanism was inserted without using the device 50 having the shock wave attenuation mechanism used in Example 2. Other than that, it carried out similarly to Example 2, However, It carried out similarly to Example 2 from the test of the pipe | tube which fixed 3 mm-thick PCTFE (ethylene trifluoride chloride) inside.

  As a result, it was confirmed that PCTFE was burned out. For this reason, it was presumed that at least a thermal load causing self-combustion was applied, that is, a shock wave was generated.

Next, a test with an acceptance valve similar to that in Example 2 was performed. As a result, the amount of internal leakage of the receiving valve 101 measured by the leak detector was 1.3 × 10 ⁻¹ Pa · m ³ / s, which was poorly sealed. Further, when the receiving valve 101 was disassembled and the sealing material was visually observed, a part of the sheet material was deformed and deterioration due to burning was recognized.

[Comparative Example 3]
Existence of the occurrence of shock waves by the Schlieren method was examined in the same manner as in Example 3 except that the apparatus 50 having the shock wave attenuation mechanism was not provided and instead a straight stainless steel conduit having the same length was disposed.

  As in Example 3, the on-off valve 2 was opened with the supply valve 4 closed, and then the supply valve 4 was opened little by little. When the pressure in the conduit 5A reached about 5 MPaG, Mylar burst. At this time, whether or not a shock wave is generated from the end portion of the conduit 6 was examined by the Schlieren method. As a result, a clear outline appeared at the tip of the conduit 6 and was confirmed by visualizing the occurrence of a shock wave.

  In the same manner as in Example 3, a test was conducted on a conduit in which 3 mm thick PCTFE (ethylene trifluorochloride) was fixed. As a result, it was confirmed that PCTFE was burned out. For this reason, it was speculated that a thermal load causing at least self-combustion was applied, and the generated shock wave had an influence.

[Comparative Example 4]
The schlieren method is used in the same manner as in the third embodiment, except that the device 50 having the shock wave attenuating mechanism used in the third embodiment and the device 60 (outlined in FIG. 8) except for the entire baffle plate is used. The presence or absence of shock waves was examined.

  As in Example 3, the on-off valve 2 was opened with the supply valve 4 closed, and then the supply valve 4 was opened little by little. When the pressure in the conduit 5A reached about 5 MPaG, Mylar burst. At this time, whether or not a shock wave is generated from the end of the conduit 6 was examined by the Schlieren method. As a result, a clear outline appeared at the tip of the conduit 6 and was confirmed by visualizing the occurrence of a shock wave.

  In the same manner as in Example 3, the test was performed on a conduit having PCTFE (ethylene trifluoride chloride) having a thickness of 3 mm fixed therein. As a result, it was confirmed that PCTFE was burned out. For this reason, it was speculated that a thermal load causing at least self-combustion was applied, and the generated shock wave had an influence.

  The high-pressure gas supply method of the present invention can be used to safely supply a high-pressure filled gas to each downstream device, and can contribute to an improvement in the safety of high-pressure gas production.

1 High-pressure vessel 2 On-off valve (pressure regulating valve)
3 Conduit 4 Supply valve 5 Conduit 5A Conduit 5B Conduit 6 Conduit 50 Equipment having shock wave attenuation mechanism 50a Inflow side of equipment having shock wave attenuation mechanism 50b Outflow side of equipment having shock wave attenuation mechanism 51 Stainless steel pipe of equipment having shock wave attenuation mechanism 52a Stainless steel ball of equipment with shock wave attenuation (diameter 10mm)
52b Stainless steel ball of equipment with shock wave attenuation (4mm diameter)
53 Baffle plate 55 Bulkhead 100 External device 101 Accepting valve 102 of external processing device Conduit 103 Conduit 104 On-off valve 105 Vacuum processing equipment 110 On-off valve 111 Conduit 112 Conduit 130 Waste gas treatment equipment (atmosphere)
140 Sealing device 140A Glass window 140B Glass window

Claims (7)

In a gas supply method for supplying a high-pressure gas containing a combustible gas or a combustion-supporting gas filled in a container to a high pressure to an external device at a pressure of 4 MPaG or more through a conduit connected to the on- off valve of the container. A method for supplying high-pressure gas, characterized in that the gas is guided to an external device through a device having a shock wave attenuation mechanism and a valve using a sealing material made of a resin material . The conduit has a supply valve for supplying gas from the container to an external device;
Device having the shock wave attenuation mechanism, the method of supplying the high-pressure gas as claimed in claim 1, characterized in that located downstream of the supply valve. The shock wave attenuation mechanism, the method of supplying the high-pressure gas as claimed in claim 1 or 2, characterized in that it has a mechanism for changing a shock wave to wave. The high-pressure gas supply method according to any one of claims 1 to 3 , wherein the shock wave attenuating mechanism has a structure that prevents straightness of the shock wave. Apparatus having a shock wave attenuation mechanism used in the method of supplying high pressure gas as claimed in any one of claims 1 to 4, characterized in that it arranged baffles in the path of the shockwave. The shock wave attenuating mechanism used for the high pressure gas supply method according to any one of claims 1 to 4 , wherein an object having a spherical shape, an elliptical shape, or a polygonal shape is arranged in a path of the shock wave. Equipment you have. The shock wave attenuating mechanism according to claim 5 or 6, comprising a container filled with a gas containing a combustible gas or a combustion-supporting gas at a high pressure, an opening / closing valve of the container, and a downstream of the opening / closing valve. A high-pressure gas supply device comprising: a device; and a conduit for guiding the gas to an external device through a device having the shock wave attenuation mechanism and a valve using a sealing material made of a resin material.

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