JP6110967B1 - Gas leak prevention sealing material, gas leak prevention structure, and repair method of gas leak location - Google Patents

Abstract

Provided is a gas leakage prevention sealing material capable of improving workability and effectively preventing gas leakage under various environments. A gas leakage prevention sealing material 12 prevents gas leakage by a cured product obtained by reacting a main agent and a curing agent. The main agent includes a bifunctional epoxy resin having a bisphenol A type skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain, and a bifunctional naphthalene type epoxy resin. The curing agent includes a polythiol-based curing agent and a curing accelerator. [Selection] Figure 1

Description

  The present invention relates to a gas leakage prevention sealing material (hereinafter referred to as a gas leakage prevention sealing material) used for preventing gas leakage in a flange serving as a joint of pipes in gas insulated power equipment such as a gas circuit breaker, a gas insulated switchgear and a gas insulated transformer. In other words, the present invention relates to a gas leak prevention structure and a gas leak repair method for repairing a gas leak spot.

In substations and power plants, gas circuit breakers (GCB (Gas Circuit Breaker)) that shut off the current using an insulating gas such as sulfur hexafluoride gas (SF ₆ gas), and the switchgear are housed in an insulating gas-filled tank The gas insulated switchgear (GIS (Gas Insulated Switch)), the gas insulated transformer (GIT (Gas Insulated Transformer)) which accommodated the transformer, etc. are used. The insulating gas is used in each apparatus in a high pressure environment of about 0.5 MPa. In addition, each device is often provided outdoors, and is exposed to a difference in temperature depending on the season.

  About each apparatus mentioned above, insulating gas is supplied using a tubular body. A connection portion between members constituting the tubular body, for example, a joint between a flange and a flange constituting the pipe is sealed with an O (O) ring in order to prevent gas leakage. Here, due to aging deterioration of the O-ring or the like, for example, gas leakage may occur from a joint between the flanges. When such a gas leak occurs, it is necessary to repair in order to prevent the gas leak promptly. That is, it is necessary to take measures to prevent gas leakage.

  A technique related to a gas leakage repair method for a gas-insulated power device is disclosed in Japanese Patent Application Laid-Open No. 2012-253963 (Patent Document 1). Moreover, the technique regarding the gas leak prevention method of a gas enclosure apparatus is disclosed by Unexamined-Japanese-Patent No. 2015-173552 (patent document 2).

  According to the gas leakage repair method for a gas insulated power device disclosed in Patent Document 1, a container for repairing a gas leak generated from a joint portion between a plurality of container members constituting an insulated gas sealed container of the gas insulated power device The insulating gas pressure in the container is lowered by partially collecting the insulating gas in the container, and then the caulking process is performed on the joint portion between the plurality of container members. Further, the pressure P of the insulating gas in the container during the caulking process is set to 0.1 MPa <P ≦ 0.2 MPa.

  A gas leakage prevention method for repairing gas leakage disclosed in Patent Document 2 includes a tubular member having a through-hole inside and a wing nut-shaped member including a wing member extending in the axial direction from the outer periphery of the tubular member. , Attached to the flange coupling part from the wing member side, arranged the braided string member over the entire circumference along the flange coupling part, and arranged to be adjacent to the wing member side of the through hole of the wing nut-shaped member, Caulking is performed so as to cover the outer periphery of the braided string member and the wing nut-shaped member except for the through-holes, and the through-holes of the wing nut-shaped member are closed with wing nut-shaped member bolts. In addition, caulking is performed with an acrylic adhesive.

JP 2012-253962 A Japanese Patent Laying-Open No. 2015-173552

  According to the technique disclosed in Patent Document 1, it is necessary to temporarily reduce the gas pressure when performing repair work. Such a method is not preferable from the viewpoint of workability. In particular, when used in a gas-insulated switchgear, an arc may fly if the pressure of the insulating gas does not ensure 0.4 MPa or more. Therefore, it is preferable to avoid repairing by such a method as much as possible. Further, in the technique disclosed in Patent Document 2, an acrylic adhesive for oil leakage repair is used as caulking, and when the gas-filled equipment is in operation, particularly in the summer, the equipment itself is at a high temperature. There is a possibility that the elastic modulus of the agent is lowered and the pressure resistance is insufficient. That is, there is a risk that gas leakage prevention may be insufficient.

  An object of the present invention is to provide a gas leakage prevention sealing material capable of improving workability and effectively preventing gas leakage under various environments.

  Another object of the present invention is to provide a gas leakage prevention structure capable of improving workability and effectively preventing gas leakage under various environments.

  Still another object of the present invention is to provide a method for repairing a gas leak location that can improve workability and effectively prevent gas leak in various environments.

  The inventors of the present application considered that a sealing material for preventing gas leakage to prevent gas leakage is required to be able to work without reducing the gas pressure during repair work from the viewpoint of improving workability. That is, it was considered that the strength of the sealing material that can withstand a gas pressure of 0.5 MPa is necessary even during repair work. In addition, in order to reliably prevent gas leakage even in cold and hot environments, especially at high temperatures, it was considered that heat resistance was required in addition to the flexibility and toughness of the sealing material. The inventors of the present invention have made extensive studies and have come to construct the present invention.

  That is, the gas leakage preventing sealing material according to the present invention prevents gas leakage by a cured product obtained by reacting the main agent and the curing agent. The main agent includes a bifunctional epoxy resin having a bisphenol A type skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain, and a bifunctional naphthalene type epoxy resin. The curing agent includes a polythiol-based curing agent and a curing accelerator.

  According to the gas leakage prevention sealing material having such a structure, the main agent is a bifunctional epoxy resin having a bisphenol A skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain, and Since the bifunctional naphthalene type epoxy resin is included and the curing agent includes a polythiol-based curing agent and a curing accelerator, the obtained cured product can have performance required as a sealing material for preventing gas leakage. That is, the curing reaction can be completed to some extent within a relatively short time after the sealing material is applied to prevent gas leakage and repair work can be performed without lowering the gas pressure. Furthermore, the obtained sealing material for preventing gas leakage can exhibit flexibility and toughness, and can improve heat resistance.

  Moreover, you may comprise so that the content rate of the bifunctional naphthalene type epoxy resin with respect to a bifunctional epoxy resin may be 30 weight part or less with respect to 100 weight part of bifunctional epoxy resins. By doing so, it is possible to appropriately maintain the balance of flexibility and toughness required as a gas leakage prevention sealing material, as well as weather resistance and heat resistance.

  In addition, you may comprise a main ingredient so that a reactive diluent may be included. By doing so, the viscosity of the main agent can be easily adjusted, and for example, the handleability of the material can be appropriately improved even when working in a low temperature environment.

  Further, the curing agent may include an amine curing agent. By carrying out like this, while being able to aim at adjustment of hardening time easily, the intensity | strength and heat resistance of hardened | cured material can be improved and durability can be improved more.

  Note that at least one of the main agent and the curing agent may further include a filler. By doing so, it becomes easy to adjust the viscosity of the main agent and the curing agent so as to be easy to handle, improve the so-called thixotropy, and improve the handleability during work. That is, it is possible to more easily avoid phenomena such as dripping, movement, and uneven distribution of the mixed solution before the curing reaction in which the main agent and the curing agent are mixed, and the sealing material can be disposed at a more appropriate location.

  As the filler, fine powder silica gel or calcium carbonate can be selected. These fillers are versatile and can be obtained at low cost. From the viewpoint of improving thixotropy, etc., it is preferable to select finely divided silica gel.

  Note that at least one of the main agent and the curing agent may further include a reinforcing material. The reinforcing material is composed of an inorganic powder or a fibrous material. By including the reinforcing material, it is possible to increase the mechanical strength of the cured product and to withstand a higher internal pressure of the gas.

  The reinforcing material may include at least one of aluminum powder, glass fiber, carbon fiber, aramid fiber, and vinylon fiber. These reinforcing materials are versatile and can be obtained at low cost.

  Here, the reinforcing material is at least one of glass fiber, carbon fiber, aramid fiber, and vinylon fiber, and the content of the reinforcing material is bifunctional epoxy resin, bifunctional naphthalene type epoxy resin, and It is good to comprise so that it may be 3 weight% or less of the total amount of a reactive diluent. By doing so, it is possible to optimize the handleability and the like by appropriately adjusting the content of the reinforcing material of the above-described fiber group.

  Further, the reinforcing material may be aluminum powder, and the content of the reinforcing material may be 20% by weight or less of the total amount of the bifunctional epoxy resin, the bifunctional naphthalene type epoxy resin, and the reactive diluent. . By carrying out like this, content of the above-mentioned inorganic powder type reinforcement | strengthening material can be made appropriate, and optimization, such as handleability, can be aimed at.

  In another aspect of the present invention, the gas leakage prevention structure is composed of a plurality of members, a gas sealing device in which gas is sealed therein, a gas leakage device in which the gas leakage device is disposed, A gas leakage prevention sealing material for preventing gas leakage by a cured product obtained by reacting with a curing agent is provided. The main agent includes a bifunctional epoxy resin having a bisphenol A type skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain, and a bifunctional naphthalene type epoxy resin. The curing agent includes a polythiol-based curing agent and a curing accelerator.

  According to the gas leakage prevention structure having such a configuration, workability can be improved and gas leakage under various environments can be effectively prevented.

  Moreover, you may comprise so that it may be attached so that it may be fixed to the outer peripheral side of a gas leak location with hardened | cured material, and the coating | coated member which covers a gas leak location may be provided. By configuring in this way, for example, gas leakage can be prevented even in a harsh environment where the temperature change is more severe.

  Note that the covering member may have a band shape and may include a spring material bent into a cylindrical shape. Such a spring material can be appropriately disposed along the outer shape of the flange and the tube body, and an elastic force that tightens the tube body and the like is generated. it can. Further, gas leakage can be prevented more reliably.

  According to still another aspect of the present invention, there is provided a gas leak repair method for repairing a gas leak spot of a gas sealing device that is constituted by a plurality of members and in which a gas is sealed. A gas leakage repair method includes a main agent containing a bifunctional epoxy resin having a bisphenol A type skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain, and a bifunctional naphthalene type epoxy resin, And a preparation step of preparing a curing agent containing a polythiol-based curing agent and a curing accelerator, a mixing step of mixing the prepared main agent and a curing agent, and an application for applying the mixture obtained by the mixing step to a gas leaking place And a curing step of curing the mixture after the coating step.

  According to such a method for repairing a gas leak location, workability can be improved and gas leak in various environments can be effectively prevented.

  Further, the preparation step includes a step of preparing a covering member that is fixed so as to be fixed to the outer peripheral side of the gas leaking part and covers the gas leaking part, and after the curing process, the mixture obtained by the mixing process is again obtained. You may make it provide the attachment process attached so that a coating | coated member may be fixed to the outer peripheral side of a gas leak location, before the mixture which apply | coated and apply | coated again is hardened | cured. By doing so, when using the covering member, it is possible to more appropriately prevent gas leakage in a severe environment where the temperature change is severe.

Further, the main agent is different from the first main agent and the first main agent in the type of any of the main agents described above, and includes any of the main agents described above as the second main agent, and the curing agent is any of the above-described main agents. The curing agent is different from the first curing agent and the first curing agent, and includes any one of the curing agents described above as the second curing agent, and the mixing step includes the first main agent and the first curing agent. And mixing the second main agent and the second curing agent to obtain the second mixture, and applying the first mixture to the gas leak point. Then, after the first mixture is cured, a recoating step of applying and curing the second mixture on the cured first mixture may be provided. By doing so, gas leakage can be prevented in a harsh environment where the temperature changes drastically.

  Such a gas leakage prevention sealing material can improve workability and effectively prevent gas leakage under various environments.

  Such a gas leakage prevention structure can improve workability and can effectively prevent gas leakage under various environments.

  Moreover, such a repair method of a gas leak location can improve workability | operativity and can prevent the gas leak in various environments effectively.

It is an external view which shows a part of gas leak prevention structure which concerns on one Embodiment of this invention. It is an external view which shows a part of gas leak prevention structure which concerns on other embodiment of this invention. It is a perspective view which shows the external appearance of a spring material. It is a flowchart which shows the typical process of the repair method of the gas leak location which concerns on one Embodiment of this invention. It is a flowchart which shows the typical process of the repair method of the gas leak location which concerns on other embodiment of this invention. It is a flowchart which shows the typical process of the repair method of the gas leak location which concerns on further another embodiment of this invention. It is sectional drawing which shows schematic structure of a test apparatus. It is a figure which shows a part of test apparatus.

  Embodiments of the present invention will be described below. First, the structure of the sealing material for preventing gas leakage according to one embodiment of the present invention will be described.

  The gas leakage prevention sealing material prevents gas leakage by a cured product obtained by reacting the main agent and the curing agent. The sealing material for preventing gas leakage mixes a main agent mainly composed of a bifunctional epoxy resin and a bifunctional naphthalene type epoxy resin with a curing agent mainly composed of a polythiol-based curing agent and a curing accelerator to cause a curing reaction. Obtained.

  First, the main agent will be described. The main agent contains a bifunctional epoxy resin having a bisphenol A skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain. Specifically, a bifunctional epoxy resin having a structure as shown in Chemical Formula 1 below is preferable.

Here, R ₁ in the formula means a long-chain hydrocarbon chain, and R ₂ and R ₃ in the formula mean a bisphenol A type skeleton structure. As the aliphatic skeleton composed of a long hydrocarbon chain, for example, an alkyl group having 4 to 12 carbon atoms, preferably about 6 carbon atoms is used. The number of n in the above formula is preferably about 1 to 6, more preferably about 1 to 2. The molecular weight of the bifunctional epoxy resin is preferably about 600 to 1000. Moreover, as a viscosity of such a bifunctional epoxy resin, it is about 1 million-2 million mPa * s in 25 degreeC. In this case, in the resin structure, the portion constituting the long-chain hydrocarbon chain ensures the flexibility required mainly as a sealing material, and the portion constituting the bisphenol A-type skeleton mainly serves as the toughness required as a sealing material. It is considered that the property and durability are secured. In addition, as a specific product of this bifunctional epoxy resin, EPICLON EXA-4816 (made by DIC Corporation) is mentioned, for example.

  The main agent contains a bifunctional naphthalene type epoxy resin. Specifically, a bifunctional naphthalene type epoxy resin having a structure as shown in Chemical Formula 2 below is preferable.

  The bifunctional naphthalene type epoxy resin shown in Chemical Formula 2 is a kind of naphthalene type epoxy resin, has a naphthalene skeleton, and has epoxy groups at both ends. Specifically, it is called 1,6-bis (2,3-epoxypropoxy) naphthalene. Such a bifunctional naphthalene type epoxy resin has a low viscosity, a high heat resistance, a low linear expansion coefficient, and a high adhesiveness, and also has good compatibility with the above-described bifunctional epoxy resin. The viscosity of such a bifunctional naphthalene type epoxy resin is about 500 to 600 mPa · s at 50 ° C. In addition, as a specific product of this bifunctional naphthalene type epoxy resin, EPICLON HP-4032D (made by DIC Corporation) is mentioned, for example.

  The main agent may comprise a predetermined amount of reactive diluent. By carrying out like this, the viscosity of the main ingredient containing the above-mentioned bifunctional epoxy resin (Chemical formula 1) and a bifunctional naphthalene type epoxy resin (Chemical formula 2) can be adjusted easily. Specifically, for example, when the bifunctional epoxy resin (Chemical Formula 1) is semi-solid, the bifunctional epoxy resin (Chemical Formula 1) has a high viscosity, or in winter, the outside temperature is relatively low. In this case, by adding a predetermined amount of the reactive diluent, the viscosity of the main agent can be lowered, and the stirrability during mixing can be improved.

  Here, you may comprise so that the content rate of the bifunctional naphthalene type epoxy resin with respect to a bifunctional epoxy resin may be 30 weight part or less with respect to 100 weight part of bifunctional epoxy resins. By doing so, it is possible to appropriately maintain the balance of flexibility and toughness required as a sealing material for preventing gas leakage and heat resistance. In addition, what is necessary is just to increase the content rate of bifunctional naphthalene type epoxy resin (Chemical Formula 2), when improving heat resistance.

  The reactive diluent preferably has good affinity with the bifunctional epoxy resin (Chemical Formula 1) and the bifunctional naphthalene type epoxy resin (Chemical Formula 2). Furthermore, from the viewpoint of improving the heat resistance of the cured product, a bifunctional epoxy resin is more desirable than a monofunctional epoxy resin. Examples of the reactive diluent include bifunctional epoxy resins having an epoxy group at both ends of the alkyl group, such as 1,6-hexanediol diglycidyl ether, and specific products include SR-16H ( Sakamoto Pharmaceutical Co., Ltd.), YED216D (Mitsubishi Chemical Corporation), EX-212 (Nagase ChemteX Corporation), and the like.

  About the compounding quantity of a reactive diluent, it sets sequentially according to the viscosity etc. of the main ingredient calculated | required, For example, the content rate of the reactive diluent with respect to bifunctional epoxy resin (Chemical Formula 1) is bifunctional epoxy. You may comprise so that it may be 20 weight part or less with respect to 100 weight part of resin (Formula 1). Specifically, for example, it is 5 parts by weight with respect to 100 parts by weight of the bifunctional epoxy resin (Chemical Formula 1). By doing so, the viscosity of the main agent can be made more appropriate, and the flexibility, toughness, heat resistance, etc. as a sealing material for preventing gas leakage can be made more appropriate.

  The curing agent includes a polythiol-based curing agent and a curing accelerator. By using a polythiol-based curing agent, it is possible to prevent gas leakage before the curing reaction is completely completed even during repair of gas leakage under a high pressure environment of 0.5 MPa by expressing an appropriate fast curability. it can. Moreover, what is called quick-hardening property is securable by using a hardening accelerator. Specific products of polythiol-based curing agents include MR-94, MR-122 (all manufactured by Daito Sangyo Co., Ltd.), EH317 (manufactured by ADEKA Corporation), jer Cure QX11, jer Cure QX-40 (any As well as Mitsubishi Chemical Corporation). As the curing accelerator, for example, a trisdimethylaminophenol type or an ethyleneamine type tertiary amine type is used. Specific examples of the curing accelerator include HD-Acc43 and HD-Acc65 (both Daito Sangyo Co., Ltd.). )), EHC-30 (manufactured by ADEKA Corporation), jer cure 3010 (manufactured by Mitsubishi Chemical Corporation), and the like.

  In addition, a hardening | curing agent is good also as an amine type hardening | curing agent being included as needed. By using an amine-based curing agent, the curing time can be easily adjusted, and the strength and heat resistance of the cured product can be increased to further improve the durability. As the amine curing agent, for example, an isophorodiamine type is used, and specific products of the amine curing agent include, for example, Daitokural I-2237, Daitokural I-5136 (both Daito Sangyo Co., Ltd.) and the like. Is mentioned. The content of the amine curing agent is preferably 20 parts by weight or less with respect to 100 parts by weight of the bifunctional epoxy resin from the viewpoint of optimizing the curing time.

  You may comprise so that the compounding ratio of a main ingredient and a hardening | curing agent exists in the range of 1: 0.2-1: 1.2. By carrying out like this, the flexibility, toughness, heat resistance, etc. as a sealing material for gas leakage prevention can be made more appropriate within the proper range of the curing time and the strength of the obtained cured product.

  In addition, you may comprise so that the filler of an inorganic powder may be included in at least any one of a main ingredient and a hardening | curing agent. By doing so, it becomes easy to adjust the viscosity of the main agent and the curing agent so as to be easy to handle, improve the so-called thixotropy, and improve the handleability during work. Specifically, it is possible to more easily avoid phenomena such as dripping, movement, and uneven distribution of the mixed solution before the curing reaction in which the main agent and the curing agent are mixed, and the sealing material can be disposed at a more appropriate location.

  Fine silica gel is selected as the type of filler. Note that calcium carbonate may be selected as the filler. As a specific product of finely divided silica gel, AEROSIL 300 (manufactured by Nippon Aerosil Co., Ltd.) is selected.

  You may comprise in a main ingredient so that an inorganic powder and a fibrous member may be included as a hardening | curing agent. By carrying out like this, the mechanical strength of hardened | cured material can be raised. As the kind of the reinforcing material, aluminum powder, glass fiber, carbon fiber, aramid fiber, vinylon fiber, or the like is selected.

  For concrete products of reinforcing materials, aluminum powder YP-580 (manufactured by Yamaishi Metal Co., Ltd.) and GS-77 (manufactured by Yamato Metal Powder Industry Co., Ltd.) as the aluminum powder, and cut fiber SS 05C-404 (glass fiber) Nittobo Co., Ltd.), Torayca Cut Fiber 3mm (Toray DuPont) as carbon fiber, Kevlar Cut Fiber 3mm (Toray DuPont) as aramid fiber, Technora Chopped Fiber 3mm (Teijin) And KURALON K-II RMS702 × 6 (manufactured by Kuraray Co., Ltd.).

  Here, if the reinforcing material is at least one of glass fiber, carbon fiber, aramid fiber, and vinylon fiber, the content of the reinforcing material is bifunctional epoxy resin and bifunctional naphthalene type epoxy resin. It is preferable that the total amount be 3% by weight or less. That is, if it is a fiber type reinforcing material, it is preferable to set it as 3 weight% or less. By carrying out like this, viscosity can be adjusted and the mechanical strength of hardened | cured material can be improved, ensuring appropriate thixotropy property and handleability.

  If the reinforcing material is an aluminum powder, the content of the aluminum powder may be configured to be 20% by weight or less of the total amount of the bifunctional epoxy resin, the bifunctional naphthalene type epoxy resin, and the reactive diluent. preferable. That is, in the case of an inorganic powder-based reinforcing material, it is preferably 20% by weight or less. This also makes it possible to adjust the viscosity and improve the mechanical strength of the cured product while ensuring appropriate thixotropy and handling properties.

  Next, the configuration of the gas leakage preventing structure according to the present invention will be described. FIG. 1 is an external view showing a part of a gas leakage preventing structure according to an embodiment of the present invention. Referring to FIG. 1, a gas leakage prevention structure 10 according to an embodiment of the present invention includes a gas sealing device 11 including a plurality of members, in which a gas is sealed, and a gas sealing device 11. The gas leakage prevention sealing material 12 is disposed at the gas leakage location and prevents gas leakage by a cured product obtained by reacting the main agent and the curing agent.

  The gas sealing device 11 seals the gas supplied via the connected valve 13a. The internal pressure of the gas sealing device 11 is measured by a pressure gauge 14 via a valve 13b. As the gas sealing device 11, for example, a gas circuit breaker, a gas insulated switchgear, or a gas insulated transformer is assumed. For example, the gas sealing device 11 may be a radiator or the like.

  The gas sealing device 11 includes a gas sealing member 15, a first member 16, and a second member 17. Illustration of a specific configuration of the gas sealing member 15 is omitted. A flange 15 a is provided on the upper part of the gas sealing member 15. A flange 16 a is provided below the first member 16 disposed on the upper side of the paper in FIG. 1 with respect to the gas sealing member 15. The gas sealing device 11 includes an O-ring (not shown) as a rubber packing disposed so as to be interposed between the flange 15a and the flange 16a. The flange 15a and the flange 16a are provided with four through-holes (not shown) penetrating in the vertical direction on the paper surface, avoiding the position where the O-ring is disposed. In addition, in FIG. 1, it has illustrated about the position where two through-holes are arrange | positioned, and it abbreviate | omits about the position where other through-holes are arrange | positioned, and those corresponding. Bolts 18a and 18b are inserted into the two through holes, respectively, and the flange 15a and the flange 16a are fastened by nuts 20a and 20b that are screwed on one end portions 19a and 19b of the bolts 18a and 18b, respectively.

  Here, the sealing material 12 for preventing gas leakage is arranged on the surface exposed to the outer diameter side of the flanges 15a and 16a. Specifically, the gas leakage preventing sealing material 12 is provided so as to cover a part or all of the outer diameter surfaces of the flange 15a and the flange 16a. On the outer diameter surfaces of the flange 15a and the flange 16a, the gas leakage preventing sealing material 12 is provided so as to form a thin film. In addition, as thickness of this sealing material 12 for gas leak prevention, 1-2 mm (millimeter) is selected, for example. Further, the sealing material 12 is disposed so as to penetrate the joint of the flange 15a and the flange 16a.

  Here, for the sealing material 12, as described above, a main reaction mainly comprising a bifunctional epoxy resin and a bifunctional naphthalene type epoxy resin and a curing agent mainly comprising a polythiol-based curing agent are mixed together to effect a curing reaction. Can be obtained.

  According to such a gas leakage prevention structure, workability can be improved and gas leakage under various environments can be effectively prevented.

  Further, when used in a harsh environment from a low temperature to a high temperature, the gas leakage prevention structure may be configured to use a covering member. FIG. 2 is an external view showing a part of a gas leakage preventing structure according to another embodiment of the present invention. Referring to FIG. 2, the gas leakage prevention structure 21 includes a gas sealing device 22, a sealing material 12, and a spring material 23 that covers the gas leakage portion. The gas sealing device 22 includes a gas sealing member 24, a first member 25, bolts 26a and 26b, nuts 27a and 27b, and an O-ring (not shown). Illustration of a specific configuration of the gas sealing member 24 is omitted. A flange 24 a is provided on the upper portion of the gas sealing member 24. A flange 25 a is provided at the lower portion of the first member 25. In addition, in FIG. 2, it has illustrated about the position where two through-holes are arrange | positioned, and it abbreviate | omits about the position where other through-holes are arrange | positioned, and those corresponding. The gas leakage prevention structure 21 includes the above-described sealing material 12 shown in FIG. 1 disposed inside the spring material 23 as a primary seal. The spring material 23 is used as a secondary seal. The spring material 23 is obtained by mixing a main agent mainly composed of a bifunctional epoxy resin and a bifunctional naphthalene type epoxy resin with a curing agent mainly composed of a polythiol-based curing agent and an amine-based curing agent, and causing a curing reaction. It is attached so as to adhere and be fixed to the outer peripheral side of the gas leaking portion by a sealing material.

  The outer shape of the spring member 23 is shown in FIG. The spring material 23 has a band shape and is configured to be bent into a cylindrical shape. Specifically, such a spring material 23 can be obtained, for example, by heating to 450 ° C. in an electric furnace in a state of being rolled into a predetermined shape, and then rapidly cooling.

  The gas leakage prevention structure 21 shown in FIG. 2 covers a part or all of the outer diameter surfaces of the flange 24a of the gas sealing member 24 and the flange 25a of the first member 25 constituting the gas sealing device 22, The sealing material 12 shown in FIG. 1 is disposed and cured as a primary sealing material, and after confirming that gas leakage has stopped, the mixture is applied again, and before the curing reaction is completed, the spring is placed on the outer diameter side. The material 23 is arranged. Then, the curing reaction is terminated, and the spring material 23 as a secondary seal is fixed to the outer diameter side of the primary sealing material 12. In this way, the gas leakage prevention structure 21 is configured.

  By configuring in this way, gas leakage can be prevented by the secondary sealing with the primary sealing material 12 and the spring material 23 even in a severe environment where the temperature change is severe. In this case, since it is a belt-like structure including the spring material 23 bent into a cylindrical shape, it can be appropriately arranged along the outer shape of the gas sealing member 24 and the first member 25, and the tubular body Since an elastic force that tightens the bolts or the like is generated, it can be more reliably disposed at the gas leak location. Further, gas leakage can be prevented more reliably.

  In addition, the gas leakage prevention structure may be configured such that a sealing material is configured by stacking a mixture of different combinations of the main agent and the curing agent described above in layers. Specifically, for example, after applying a primary sealant by applying a mixture that does not contain a reinforcing material, the mixture containing the reinforcing material is further applied from above to perform a secondary seal to obtain a sealing material. May be. By doing so, it is possible to prevent gas leakage in a harsh environment where the temperature changes drastically.

  Next, a gas leak repair method according to the present invention will be described. FIG. 4 is a flowchart showing a typical process of the gas leakage spot repair method according to the embodiment of the present invention.

  With reference to FIG. 4, the repair method of the gas leak location which concerns on one Embodiment of this invention wash | cleans the location where the gas leak has generate | occur | produced before work. Specifically, paint, oil, moisture, dirt, etc. are removed from the gas leak location.

  As a repair method, first, a main agent and a curing agent are prepared (in FIG. 4, step S11, hereinafter, “step” is omitted). In this case, it is advisable to adjust the viscosity by mixing a reactive diluent and a filler as the main agent in advance if necessary. Moreover, also about a hardening | curing agent, it is good to mix a hardening accelerator and a filler beforehand as needed.

  Thereafter, the prepared main agent and the prepared curing agent are mixed (S12). About mixing of a main ingredient and a hardening | curing agent, it measures according to a compounding ratio, respectively, mixes the agent of the other side in the agent of one side, and performs it by fully stirring and mixing. In this case, a predetermined stirrer such as a rotation / revolution mixer may be used, or stirring and mixing may be performed by an operator's hand.

  Next, the mixed mixture is applied to the gas leaking part (S13). The case where the mixture is applied using the gas leakage prevention structure 10 shown in FIG. 1 will be described. Specifically, the mixture is applied so as to cover the outer diameter side surfaces of the flanges 15a and 16a. That is, it is applied with a certain width around the joint portion of the flanges 15a and 16a. In this case, for example, the work may be performed by a worker's hand, or a dedicated jig, brush, brush, or the like may be used.

  Thereafter, after a predetermined time has elapsed, the curing reaction of the applied mixture is terminated (S14). In this way, repair of the gas leak point is performed.

  According to such a method for repairing a gas leak location, workability can be improved and gas leak in various environments can be effectively prevented.

  In addition, when repairing a gas leak location using the gas leak prevention structure 21 containing the spring material 23 as a covering member shown in FIG. 2, it becomes the following processes. FIG. 5 is a flowchart showing a typical process of a gas leakage spot repair method according to another embodiment of the present invention, and shows a typical configuration of a gas leak spot repair method using the gas leak prevention structure 21. It is a flowchart to show.

  Referring to FIG. 5, a main agent, a curing agent, and a spring material 23 as a covering member are prepared (S21). An example of the spring member 23 is shown in FIG. That is, a preparation process includes the process of preparing the coating | coated member which is attached so that it may be fixed to the outer peripheral side of a gas leak location, and covers a gas leak location.

  The subsequent steps S22 and S23 are the same as the steps S12 and S13 shown in FIG. 4 described above, and a description thereof will be omitted.

  After completion of the curing reaction, check for gas leaks. The gas leak check confirms that there is no pressure drop with a pressure gauge and that no bubbles are produced by the soapy water foaming method (S24). The sealing material at this point is called a primary seal.

  The subsequent step S25 is the same as the step S12 shown in FIG. 4 described above, and a description thereof will be omitted. And the obtained mixture is again apply | coated on the primary sealing material 12 in which hardening reaction was complete | finished (S26). After the coating process and before the curing process, the spring material 23 is attached so as to be fixed to the outer peripheral side of the gas leakage portion (S27). That is, the gas leakage spot repairing method includes an attachment process after the application process and before the curing process, so as to fix the spring member 23 as a covering member on the outer peripheral side of the gas leakage spot. In this case, when the spring member 23 is attached in a so-called stretched state and then released, the spring member 23 is rounded to the inner diameter side by elastic force. The primary seal itself is tightened by the elastic force of the spring material 23. That is, the spring material 23 is used as a secondary seal by using a mixture having the same composition as the primary seal as an adhesive. The primary seal and the secondary seal constitute a sealing material according to another embodiment of the present invention.

  Then, after a predetermined time has elapsed, the curing reaction of the applied mixture is terminated (S28). In this way, repair of the gas leak point is performed.

  According to such a method for repairing a gas leak location, when a covering member is used, it is possible to more appropriately prevent gas leak in a severe environment where the temperature change is severe.

  In addition, when a mixture of different combinations of the main agent and the curing agent described above is stacked to form a sealing material, a method for repairing a gas leakage portion is as follows. FIG. 6 is a flowchart showing a typical process of a gas leakage point repair method according to still another embodiment of the present invention.

  Referring to FIG. 6, a primary seal main agent and curing agent, and a secondary seal main agent and curing agent are prepared (S31). Specifically, for example, the primary seal main agent and the curing agent are a system that does not include a reinforcing material, and the secondary seal main agent and the curing agent are a system that includes a reinforcing material.

  Then, the main agent for primary sealing and the curing agent are mixed (S32). After mixing, the mixture is applied to the gas leak location (S33).

  After the curing reaction is completed, the presence or absence of gas leakage is checked (S34). The check for gas leakage is performed in the same manner as in step S24 shown in FIG.

  After confirming that no gas is leaking, the main agent for secondary sealing and the curing agent are mixed (S35). And the mixture as a secondary seal is apply | coated on the primary seal which complete | finished hardening reaction (S36).

  Thereafter, the curing reaction of the mixture applied as a secondary seal is completed to obtain a sealing material according to still another embodiment of the present invention.

That is, in the gas leak repair method according to still another embodiment of the present invention, the main agent is different from the first main agent and the first main agent in the type of any of the above main agents. The main agent is included as the second main agent, and the curing agent is different from the first curing agent and the first curing agent in any of the above-described curing agents, and any of the above-described curing agents is used as the second curing agent. Contains as an agent. The mixing step includes a step of mixing the first main agent and the first curing agent to obtain a first mixture, and a step of mixing the second main agent and the second curing agent to obtain a second mixture. including. And the repair method of a gas leak location applies the 2nd mixture on the hardened 1st mixture, after hardening the 1st mixture by applying the 1st mixture to the gas leak location, and hardening. A re-coating step.

  Also with this configuration, it is possible to prevent gas leakage in a harsh environment where the temperature changes drastically. In particular, since the mechanical strength can be increased by the secondary seal, durability can be ensured.

  In the above embodiment, if necessary, the coating material may be applied to the upper layer side so as to cover the sealing material 12 or the spring material 23, that is, the sealing material or the spring material 23. . By doing so, the appearance can be improved and the weather resistance and the like can be improved.

  In the above embodiment, the main agent, the curing agent, and the mixture may be slightly heated as necessary. In this way, the viscosity of each agent can be adjusted to improve the handleability, and the curing time can be adjusted.

  In the above-described embodiment, the filler is included in the main agent and the curing agent. However, the present invention is not limited to this, and the filler may be included only in at least one of the main agent and the curing agent. However, depending on the working environment, it is not necessary to include a filler in either the main agent or the curing agent.

  Further, the covering member is a belt-like spring material that is bent into a cylindrical shape, but is not limited to the spring material, and other members such as a metal belt-like member or a plate-like member such as a metal A cable tie may be used. As an example of a cable tie product, there is a metal tie manufactured by Heraman Tighton Co., Ltd., a stainless steel band manufactured by Band Whit Corporation, or the like.

In the above embodiment, the gas circuit breaker as the gas sealing device 11, the gas insulated switchgear, and the gas insulated transformer are used for preventing gas leakage. This is applied when a gas leak occurs in a member enclosing gas. Of course, the present invention is also applied to the case where a gas other than an insulating gas such as sulfur hexafluoride gas (SF ₆ gas) is used.

Example 1
The sealing material for preventing gas leakage according to Example 1 was obtained by the method described below. First, EPICLON EXA-4816 (manufactured by DIC Corporation) was prepared as a bifunctional epoxy resin contained in the main agent. This EPICLON EXA-4816 was semi-solid at room temperature (25 ° C.). Moreover, EPICLON HP-4032D (made by DIC Corporation) was prepared as a bifunctional naphthalene type epoxy resin contained in the main agent. 20 parts by weight of EPICLON HP-4032D was added to 100 parts by weight of EPICLON EXA-4816. Furthermore, 5 parts by weight of SR-16H (manufactured by Sakamoto Pharmaceutical Co., Ltd.) as a reactive diluent and 1 part by weight of AEROSIL 300 (manufactured by Nippon Aerosil Co., Ltd.) as a filler were added and mixed thoroughly. In this way, the main agent according to Example 1 was obtained. The base agent according to Example 1 was putty at 20 ° C.

  Next, MR-122 (manufactured by Daito Sangyo Co., Ltd.) was prepared as a polythiol-based curing agent contained in the curing agent. Moreover, HD-Acc65 (manufactured by Daito Sangyo Co., Ltd.) was prepared as a curing accelerator contained in the curing agent. In addition, I-5136 (manufactured by Daito Sangyo Co., Ltd.) was prepared as an amine-based curing agent contained in the curing agent. 20 parts by weight of I-5136 was added to 80 parts by weight of MR-122. Furthermore, 6 parts by weight of HD-Acc65 (manufactured by Daito Sangyo Co., Ltd.) and 2 parts by weight of AEROSIL 300 as a filler were added and stirred sufficiently. Thus, the hardening | curing agent which concerns on Example 1 was obtained. The curing agent according to Example 1 was also putty at 20 ° C.

  With respect to the main agent and the curing agent thus obtained, 33 parts by weight of the curing agent was added to 100 parts by weight of the main agent, followed by stirring and mixing to obtain a mixture according to Example 1.

  Next, the obtained mixture according to Example 1 was applied to a predetermined portion serving as a gas leakage portion of a test apparatus described later as a gas sealing apparatus in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, a gas leakage preventing sealing material and a gas leakage preventing structure according to Example 1 were obtained.

  In addition, it shows in Table 1 about the kind of resin etc. which comprise the main ingredient based on above-mentioned Example 1, and a hardening | curing agent, and compounding quantity. In Table 1, the numerical values of the blending amount and blending ratio are shown in parts by weight. Hereinafter, the types of the main agent and curing agent according to Examples 2 to 7 are also shown in Table 1.

(Example 2)
A curing agent according to Example 2 was obtained in the same manner as in Example 1 except that the amine-based curing agent contained in the curing agent was excluded.

  The same main agent as in Example 1 was prepared. And the mixture which concerns on Example 2 was obtained for the blending quantity of the hardening | curing agent with respect to 100 weight part of main ingredients as 49 parts. Further, from the mixture according to Example 2, the sealing material for preventing gas leakage and the gas leakage preventing structure according to Example 2 were obtained in the same manner as in Example 1.

(Example 3)
AEROSIL 300 was added to 1 part by weight as a filler contained in the main agent, and 3.8 parts by weight of KURALON K-II RMS702 × 6 (manufactured by Kuraray Co., Ltd.), which is a vinylon fiber, was added as a reinforcing material. Other than that, the base agent according to Example 3 was obtained in the same manner as Example 1.

  The same curing agent as in Example 1 was prepared. And the content rate of the hardening | curing agent with respect to a main ingredient was similarly obtained, and the mixture which concerns on Example 3 was obtained. Further, the gas leakage prevention sealing material and gas leakage prevention structure according to Example 3 were obtained from the mixture according to Example 3 in the same manner as in Example 1.

Example 4
AEROSIL 300 was added to 1 part by weight as a filler contained in the main agent, and 25 parts by weight of aluminum powder YP-580 (Yamaishi Metal Co., Ltd.), which is an aluminum powder, was added as a reinforcing material. Other than that, the base agent according to Example 4 was obtained in the same manner as Example 1.

  The same curing agent as in Example 1 was prepared. With respect to the main agent and the curing agent thus obtained, 28 parts by weight of the curing agent was added to 100 parts by weight of the main agent, followed by stirring and mixing to obtain a mixture according to Example 4. Furthermore, the gas leakage prevention sealing material and gas leakage prevention structure according to Example 4 were obtained from the mixture according to Example 4 in the same manner as in Example 1.

(Example 5)
About bifunctional naphthalene type epoxy resin contained in the main agent, 30 parts by weight of EPICLON HP-4032D was added to 100 parts by weight of EPICLON EXA-4816. Other than that, the base agent according to Example 5 was obtained in the same manner as Example 1.

  The same curing agent as in Example 1 was prepared. With respect to the main agent and the curing agent thus obtained, 36 parts by weight of the curing agent was added to 100 parts by weight of the main agent, followed by stirring and mixing to obtain a mixture according to Example 5. Further, from the mixture according to Example 5, the sealing material for preventing gas leakage and the gas leakage preventing structure according to Example 5 were obtained in the same manner as in Example 1.

(Example 6)
AEROSIL 300 was added to 1 part by weight as a filler contained in the main agent, and 4.1 parts by weight of Claron K-II RMS702 × 6, which is a vinylon fiber, was added as a reinforcing material. Others were the same as in Example 5, and the main agent according to Example 6 was obtained.

  The same curing agent as in Example 1 was prepared. With respect to the main agent and the curing agent thus obtained, 35 parts by weight of the curing agent was added to 100 parts by weight of the main agent, followed by stirring and mixing to obtain a mixture according to Example 6. Furthermore, the gas leakage prevention sealing material and gas leakage prevention structure according to Example 6 were obtained from the mixture according to Example 6 in the same manner as in Example 1.

(Example 7)
AEROSIL 300 was added to 1 part by weight as a filler contained in the main agent, and 27 parts by weight of aluminum powder YP-580, which is an aluminum powder, was added as a reinforcing material. Others were the same as in Example 5, and the base agent according to Example 7 was obtained.

  The same curing agent as in Example 1 was prepared. With respect to the main agent and the curing agent thus obtained, 30 parts by weight of the curing agent was added to 100 parts by weight of the main agent, followed by stirring and mixing to obtain a mixture according to Example 7. Further, from the mixture according to Example 7, in the same manner as in Example 1, the gas leakage preventing sealing material and the gas leakage preventing structure according to Example 7 were obtained.

(Example 8)
The same main agent and curing agent as in Example 1 were prepared. And the repair method shown in FIG. 5 was adopted. That is, the content ratio of the curing agent with respect to the main agent was similarly obtained to obtain a mixture similar to Example 1. The obtained mixture was applied as a primary seal in a predetermined location, which is a gas leak location of a test apparatus, which will be described later, as a gas sealing device in an atmosphere of 20 ° C. Then, after the gas leakage stops, a spring mixed with the same main agent and curing agent as the above primary sealing material is applied onto the primary seal, and then folded into a ring shape as a covering member before the curing reaction is completed. The material was placed thereon as a secondary seal and further adhered using the mixture. As the spring material, a quenched ribbon steel strip (material: SK-5, plate thickness 0.2 mm, plate width 20 mm) was used. Thereafter, the curing reaction was completed. Thus, the gas leakage preventing sealing material and gas leakage preventing structure according to Example 8 were obtained.

  In addition, regarding the sealing material and the gas leakage prevention structure according to Example 8, the contents of the configuration are shown in Table 2. Hereinafter, the sealing materials and gas leakage prevention structures according to Examples 9 to 11 are similarly shown in Table 2.

Example 9
The same main agent and curing agent as those in Example 1 and Example 3 were prepared, respectively. And the repair method shown in FIG. 6 was adopted. That is, the mixture similar to Example 1 was obtained by making the content rate of the hardening | curing agent with respect to a main ingredient into the same. The obtained mixture according to Example 1 was applied to a predetermined portion serving as a gas leakage portion of a test apparatus to be described later as a gas sealing apparatus in an atmosphere of 20 ° C. After the air leakage stopped, the same mixture as in Example 3 was obtained in the same manner as the content ratio of the curing agent to the main agent. On top of that, the mixture according to Example 3 was applied as a secondary seal to complete the curing reaction. Thus, the gas leakage preventing sealing material and the gas leakage preventing structure according to Example 9 were obtained.

(Example 10)
The same main agent and curing agent as in Example 5 were prepared. And the content rate of the hardening | curing agent with respect to a main ingredient was similarly done, and the mixture similar to Example 5 was obtained. The obtained mixture was applied as a primary seal in a predetermined location, which is a gas leak location of a test apparatus, which will be described later, as a gas sealing device in an atmosphere of 20 ° C. Then, after the gas leakage stops, a spring mixed with the same main agent and curing agent as the above primary sealing material is applied onto the primary seal, and then folded into a ring shape as a covering member before the curing reaction is completed. The material was placed thereon as a secondary seal and further adhered using the mixture. As the spring material, the same quenched ribbon steel strip as in Example 8 was used. Thereafter, the curing reaction was completed. In this way, a gas leakage preventing sealing material and a gas leakage preventing structure according to Example 10 were obtained.

(Example 11)
The same main agent and curing agent as those in Example 5 and Example 6 were prepared. And the content rate of the hardening | curing agent with respect to a main ingredient was similarly performed, and the mixture similar to Example 5 and Example 6 was obtained. The obtained mixture according to Example 5 was applied under a 20 ° C. atmosphere to a predetermined portion serving as a gas leakage portion of a test apparatus described later as a gas sealing apparatus. After air leakage stopped, the mixture according to Example 6 was applied as a secondary seal thereon to complete the curing reaction. In this way, a gas leakage preventing sealing material and a gas leakage preventing structure according to Example 11 were obtained.

(Comparative Example 1)
A general-purpose bisphenol A type epoxy resin EP-4100 (manufactured by ADEKA) was prepared as a bifunctional epoxy resin contained in the main agent. 66 parts by weight of YP-580 as a reinforcing material was added to 100 parts by weight of EP-4100, and the mixture was sufficiently stirred and mixed. Thus, the main ingredient which concerns on the comparative example 1 was obtained.

  Next, EH-317 (manufactured by ADEKA Corporation) was prepared as a polythiol-based curing agent contained in the curing agent. In addition, the amine type hardening | curing agent is not contained. 100 parts by weight of EH-317, 25 parts by weight of EHC-30 (manufactured by ADEKA Co., Ltd.) as a curing accelerator, 5 parts by weight of AEROSIL 300 which is a fine silica gel as a filler, and further as a filler 88 parts by weight of Silver-W (produced by Shiroishi Kogyo Co., Ltd.), which is calcium carbonate, and 32 parts by weight of Hakucho Hana CC (produced by Shiraishi Kogyo Co., Ltd.), which are also calcium carbonate, were added and sufficiently stirred. Thus, the hardening | curing agent which concerns on the comparative example 1 was obtained.

  With respect to the main agent and the curing agent thus obtained, 100 parts by weight of the curing agent was added to 100 parts by weight of the main agent, followed by stirring and mixing to obtain a mixture according to Comparative Example 1.

  Next, the obtained mixture according to Comparative Example 1 was applied to a predetermined portion serving as a gas leakage portion of a test apparatus to be described later as a gas sealing device in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, a gas leakage preventing sealing material and a gas leakage preventing structure according to Comparative Example 1 were obtained.

  In addition, it shows in Table 3 about the kind of resin etc. which comprise the main ingredient concerning the above-mentioned comparative example 1, and a hardening | curing agent, and compounding quantity. In Table 3, the numerical values of the blending amount and blending ratio are shown in parts by weight. Hereinafter, the types of the main agent and the curing agent according to Comparative Examples 2 to 4 are also shown in Table 3.

(Comparative Example 2)
A main agent according to Comparative Example 1 was obtained in the same manner as in Example 1 except that the bifunctional naphthalene type epoxy resin contained in the main agent was excluded. The same curing agent as in Example 2 was prepared. And the mixture which concerns on the comparative example 2 was obtained for the compounding quantity of the hardening | curing agent with respect to 100 weight part of main agents as 39 parts. Further, from the mixture according to Comparative Example 2, a gas leakage preventing sealing material and a gas leakage preventing structure according to Comparative Example 2 were obtained in the same manner as in Example 1.

(Comparative Example 3)
The same main agent as in Comparative Example 2 was prepared. The same curing agent as in Example 1 was prepared. And the mixture which concerns on the comparative example 3 was obtained for the compounding quantity of the hardening | curing agent with respect to 100 weight part of main ingredients as 26 parts. Further, from the mixture according to Comparative Example 3, the sealing material for preventing gas leakage and the gas leakage preventing structure according to Comparative Example 3 were obtained in the same manner as in Example 1.

(Comparative Example 4)
As an epoxy resin contained in the main agent, 1 part by weight of AEROSIL 300 as a filler is added to 100 parts by weight of the bifunctional naphthalene-type epoxy resin EPICRONHP-4032D, and the mixture is sufficiently stirred to obtain the main agent according to Comparative Example 4. It was. The same curing agent as in Example 1 was prepared. And the mixture which concerns on the comparative example 4 was obtained for the compounding quantity of the hardening | curing agent with respect to 100 weight part of main ingredients as 71 parts. Further, from the mixture according to Comparative Example 4, the sealing material for preventing gas leakage and the gas leakage preventing structure according to Comparative Example 4 were obtained in the same manner as in Example 1.

  Next, for the obtained gas leakage prevention sealing materials according to Examples 1 to 11 and Comparative Examples 1 to 4, a gas leakage test for confirming the presence or absence of gas leakage, a so-called air leakage test, and various environments A heat cycle test was performed to evaluate the durability at the bottom. The test results are shown in Table 4.

  First, the gas leak test will be described. The gas leak test was performed by confirming whether or not gas leak occurred at the gas leak location where the sealing material was applied. That is, the gas leak check was performed by confirming that there was no pressure drop with a pressure gauge and that no bubbles were generated by the soapy water foaming method. As a test method, a test apparatus having the following configuration was used.

  Here, the configuration of the test apparatus will be described. FIG. 7 is a cross-sectional view showing a schematic configuration of the test apparatus. FIG. 8 is a diagram showing a part of the test apparatus. Test results using the test apparatus are shown in Table 4 below.

  7 and 8, the test apparatus 31 includes a pressure gauge 33 that measures the pressure of the gas sealed in the gas sealing device 32, and a valve 34 that adjusts the gas sealed in the gas sealing device 32. With. The gas sealing device 32 includes a first member 35, a second member 36, and a third member 37. The first member 35 has a cylindrical shape, and flanges 35a and 35b are provided on both ends in the vertical direction. Flange 36a, 37a is provided also in the upper end side of the 2nd member 36, and the lower end side of the 3rd member 37, respectively. The flange 36a is a so-called blind flange. The flange 36a of the second member 36 and the flange 35b of the first member 35 are provided with grooves 42a and 42b into which O-rings 41a and 41b are fitted, respectively. The O-ring 41a is fitted into the groove 42a so that the O-ring 41a is interposed between the flange 36a and the flange 35a. Then, the second member 36 is attached to the first member 35 with bolts and nuts (not shown). Similarly, the O-ring 41b is fitted into the groove 42b so that the O-ring 41b is interposed between the flange 36a and the flange 37a. Then, the first member 35 is attached to the third member 37 with bolts and nuts (not shown). The basic configuration of the gas sealing device 32 is as described above. Gas is sealed from the third member 37 side.

And in order to let gas leak artificially in the test apparatus 31, as shown in FIG. 8, it straddles a part of annular | circular shaped O-ring 41a between the 1st member 35 and the 2nd member 36. In this way, strip-shaped plain paper 43 is arranged. For the plain paper 43, so-called copy paper is used. That is, the plain paper 43 is sandwiched between the O-ring 41a and the flange 35a to form a slight gap, and gas is leaked from this portion. FIG. 8 is a view from the direction toward the lower O-ring 41a from the upper side indicated by the arrow D ₁ of the in Fig.

  As the amount of gas leakage, the test is performed assuming an initial gas pressure of 0.5 MPa and assuming 50 ml (milliliter) / min. In the case where the above-described configuration is shown as an example, when the width of the plain paper 43 is 2 mm, the gas leakage rate is 54 ml / min and the gas pressure decrease rate is 0.029 MPa / min. When the width of the plain paper 43 is 10 mm, the gas leak rate is 98 ml / min, and the gas pressure decrease rate is 0.053 MPa / min. Note that nitrogen gas is used as the gas.

  Thus, when gas is artificially leaked from the joint of the flange 36a of the second member 36 and the flange 35a of the first member 35, a bolt (not shown) is passed through a through-hole of a bolt (not shown). There is a risk of gas leaking from the nut portion. In order to prevent this, a ring-shaped silicone rubber punched gasket is disposed between the flange 36a and the flange 35a, avoiding the position where the O-ring is disposed, and is disposed around a through hole of a bolt (not shown). Let As a result, gas leaks only from the joint between the flange 36a of the second member 36 and the flange 35a of the first member 35.

  Using such a test apparatus 31, the gas leakage rate is adjusted to 50 ml / min. And the sealing using a sealing material was performed and the air leak test was done. That is, in order to stop the gas leaking from between the flange 36a of the second member 36 and the flange 35a of the first member 35, whether or not the leakage can be prevented by applying a sealing material or the like in the above process. Was tested. The test results of Examples 1 to 11 and Comparative Examples 1 to 4 are shown in Table 4. In Table 4, “no” is indicated for air leakage, ie, gas leaked, and “good” is indicated for no gas leak, ie, no gas leak.

  Next, a heat cycle test using the test apparatus 31 will be described. The heat cycle test was performed as follows after overnight curing for those that cleared the above air leakage test.

  In the heat cycle test, as condition 1, after holding at −20 ° C. for 3 hours, holding at 20 ° C. for 30 minutes, holding at 50 ° C. for 3 hours, and then holding again at 20 ° C. for 30 minutes is one cycle. It was. In each cycle, the presence or absence of gas leakage was confirmed in the same manner as in the air leakage test, and only when there was no gas leakage, the condition 1 was further repeated for 1 cycle and repeated up to 10 cycles. About the heat cycle test result, the number of cleared cycles is shown. That is, 0 was displayed when it was not cleared once, 1 was cleared, but 1 was displayed when air leaked for the second time, and 10 was displayed when cleared 10 times.

  In addition, when durability under a higher temperature environment is required, tests of Condition 2, Condition 3, Condition 4, and Condition 5 are performed instead of Condition 1. As condition 2, a cycle of holding at −20 ° C. for 3 hours, holding at 20 ° C. for 30 minutes, holding at 60 ° C. for 3 hours, and then holding again at 20 ° C. for 30 minutes was defined as one cycle. This cycle was repeated a maximum of 10 times to obtain test results as Condition 2. Condition 3 is a condition in which the step of holding at 60 ° C. in condition 2 is set to 70 ° C. Condition 4 is a condition in which the step of holding at 60 ° C. in condition 2 is set to 80 ° C. Condition 5 is a condition in which the step of holding at 60 ° C. in condition 2 is 100 ° C. That is, the higher the numerical value indicating the condition, the more severe the situation in a high temperature environment. The higher the temperature, the higher the internal pressure. According to Boyle-Charles' law, the initial pressure of 0.5 MPa at 20 ° C. is 0.55 MPa at 50 ° C., 0.57 MPa at 60 ° C., 0.59 MPa at 70 ° C., 0.60 MPa at 80 ° C., and at 100 ° C. It rises to 0.64 MPa. Therefore, as the condition 1 changes to the condition 5, it becomes a severe condition of high temperature and high pressure. In conditions 2 to 5, the number of times the air leakage test was cleared was displayed. In addition, when the test is not performed, it is indicated by “−” in Table 4.

表１〜表４を参照して、漏気試験については、比較例１の結果から、２０℃での漏気が確認された。比較例２〜４については、２０℃での漏気試験をクリアしたが、ヒートサイクル試験の条件１を１回もクリアしなかった。すなわち、５０℃で３時間保持するという工程を含むヒートサイクル試験において、比較例２〜４は、１回目で漏気が確認された。この結果から、比較例２〜比較例４におけるシーリング材は、ガス漏れ防止用シーリング材として具備すべき要件が整っていないことが把握できる。なお、比較例１については、漏気試験をクリアしていないため、ヒートサイクル試験を実施していない。

With reference to Table 1-Table 4, about the air leak test, the air leak at 20 degreeC was confirmed from the result of the comparative example 1. FIG. About Comparative Examples 2-4, although the leak test at 20 degreeC was cleared, the conditions 1 of the heat cycle test were not cleared even once. That is, in the heat cycle test including the step of holding at 50 ° C. for 3 hours, in Comparative Examples 2 to 4, leakage was confirmed at the first time. From this result, it can be understood that the sealing materials in Comparative Examples 2 to 4 do not have the requirements to be provided as a sealing material for preventing gas leakage. In addition, about the comparative example 1, since the air leak test is not cleared, the heat cycle test is not implemented.

  On the other hand, for the sealing materials shown in Examples 1 to 11, all the air leakage tests at 20 ° C. were cleared. And also in the condition 1, about the sealing material shown in Example 2, Example 3, and Example 6, the heat cycle test was cleared twice, respectively, and it leaked in the 3rd time. The sealing materials shown in the other examples were cleared 10 times. In Condition 2, the sealing materials shown in Example 4 and Example 5 each cleared the heat cycle test once and leaked air at the second time. All the sealing materials shown in Examples 7 to 11 were cleared 10 times. In condition 3, the sealing material shown in Example 7 cleared the heat cycle test once and leaked air at the second time. About the sealing material shown in Example 8, Example 10, and Example 11, it cleared 10 times. In addition, about the sealing material shown in Example 9, it leaked in the 1st heat cycle test. In Condition 4, the sealing material shown in Example 11 was cleared twice, but leaked at the third time. The sealing materials shown in Example 8 and Example 10 were cleared 10 times. In condition 5, the sealing materials shown in Example 8 and Example 10 were cleared 10 times.

  Therefore, the leak test was cleared about the sealing materials shown in Examples 1 to 11. Some of the conditions 1 were also cleared. Any of the sealing materials shown in Examples 1 to 11 is selected in consideration of required heat resistance, handling property, cost, and the like.

  As described above, according to the sealing material for preventing gas leakage, the structure for preventing gas leakage, and the method for repairing the gas leakage portion, it is possible to improve workability and effectively prevent gas leakage under various environments. it can.

  It should be understood that the embodiments and examples disclosed herein are illustrative in all respects and are not restrictive in any respect. The scope of the present invention is defined by the scope of the claims, rather than the description above, and is intended to include any modifications within the scope and meaning equivalent to the scope of the claims.

  The gas leak prevention sealing material, the gas leak prevention structure, and the gas leak repair method according to the present invention improve workability and are required to effectively prevent gas leaks in various environments. , Especially useful.

  10, 21 Gas leakage prevention structure, 11, 22, 32 Gas sealing device, 12 Sealing material, 13a, 13b, 34 Valve, 14, 33 Pressure gauge, 15, 24 Gas sealing member, 15a, 16a, 24a, 25a, 35a , 35b, 36a, 37a Flange, 16, 25, 35 First member, 17, 36 Second member, 18a, 18b, 26a, 26b Bolt, 19a, 19b One end, 20a, 20b, 27a, 27b Nut , 23 Spring material, 31 Test device, 37 Third member, 41a, 41b O-ring, 42a, 42b Groove, 43 Plain paper.

Claims (15)

A gas leakage prevention sealing material for preventing gas leakage by a cured product obtained by reacting a main agent and a curing agent,
The main agent includes a bifunctional epoxy resin having a bisphenol A type skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain, and a bifunctional naphthalene type epoxy resin, respectively.
The said hardening | curing agent is a sealing material for gas leak prevention containing a polythiol type hardening | curing agent and a hardening accelerator. The sealing material for gas leakage prevention according to claim 1, wherein a content ratio of the bifunctional naphthalene type epoxy resin to the bifunctional epoxy resin is 30 parts by weight or less with respect to 100 parts by weight of the bifunctional epoxy resin. . The sealing material for preventing gas leakage according to claim 1 or 2, wherein the main agent contains a reactive diluent. The sealing material for gas leakage prevention according to any one of claims 1 to 3, wherein the curing agent includes an amine curing agent. The sealing material for gas leakage prevention according to any one of claims 1 to 4, wherein at least one of the main agent and the curing agent includes a filler. The sealing material for gas leakage prevention according to any one of claims 1 to 5, wherein at least one of the main agent and the curing agent further contains a reinforcing material. The sealing material for gas leakage prevention according to claim 6, wherein the reinforcing material includes at least one of aluminum powder, glass fiber, carbon fiber, aramid fiber, and vinylon fiber. The reinforcing material is at least one of glass fiber, carbon fiber, aramid fiber, and vinylon fiber,
The gas leakage prevention sealing material according to claim 7, wherein the content of the reinforcing material is 3% by weight or less of the total amount of the bifunctional epoxy resin and the bifunctional naphthalene type epoxy resin. The reinforcing material is aluminum powder,
The sealing for gas leakage prevention according to claim 7, wherein the content of the reinforcing material is 20% by weight or less of the total amount of the bifunctional epoxy resin, the bifunctional naphthalene type epoxy resin, and the reactive diluent. Wood. The gas sealing device is composed of a plurality of members, and gas is sealed by a cured product obtained by reacting the main agent and the curing agent, which is disposed at a gas leaking portion of the gas sealing device and in which gas is sealed. With a gas leakage prevention sealing material to prevent leakage,
The main agent includes a bifunctional epoxy resin having a bisphenol A type skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain, and a bifunctional naphthalene type epoxy resin, respectively.
The said hardening | curing agent is a gas leak prevention structure containing a polythiol type hardening | curing agent and a hardening accelerator. The gas leakage prevention structure according to claim 10, further comprising a covering member that is attached so as to be fixed to the outer peripheral side of the gas leakage location by the cured product and covers the gas leakage location. The gas leakage prevention structure according to claim 11, wherein the covering member has a band shape and includes a spring material bent into a cylindrical shape. It is composed of a plurality of members, and is a gas leakage repair method for repairing a gas leakage spot of a gas sealing device in which gas is sealed.
A main agent containing a bifunctional epoxy resin having a bisphenol A type skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain, and a bifunctional naphthalene type epoxy resin, and a polythiol curing agent and curing acceleration A preparation step of preparing a curing agent containing an agent;
A mixing step of mixing the prepared main agent and the curing agent;
An application step of applying the mixture obtained by the mixing step to a gas leak point;
A method for repairing a gas leak portion, comprising: a curing step of curing the mixture after the coating step. The preparation step includes a step of preparing a covering member that is attached so as to be fixed to the outer peripheral side of the gas leaking part and covers the gas leaking part,
After the curing step, the mixture obtained by the mixing step is applied again, and the attachment member is attached so as to fix the covering member to the outer peripheral side of the gas leakage point before the applied mixture is cured again. The method for repairing a gas leak point according to claim 13, comprising a step. The main agent is different from the main agent according to any one of claims 1 to 3 and claims 5 to 9 in the type of the first main agent and the first main agent. The main ingredient according to any one of Items 5 to 9 is included as a second main ingredient,
The said hardening | curing agent differs in the kind of one hardening | curing agent of Claim 1 and any one of Claims 4-9 from the 1st hardening | curing agent and said 1st hardening | curing agent, Claim 1 and Claim. The one curing agent according to any one of Items 4 to 9 is included as a second curing agent,
The mixing step includes mixing the first main agent and the first curing agent to obtain a first mixture, and mixing the second main agent and the second curing agent to obtain a second mixture. Obtaining a mixture of
A recoating step of applying the first mixture to a gas leaking portion to cure the first mixture and then applying and curing the second mixture on the cured first mixture. The method for repairing a gas leak point according to claim 13.

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