JP5744158B2 - Oil leakage prevention sealing material, oil leakage prevention structure, and method for repairing oil leakage points - Google Patents

Description

The present invention relates to an oil leakage prevention sealing material (hereinafter also simply referred to as a “sealing material”), an oil leakage prevention structure, and an oil leakage point repair for repairing an oil leakage point . It is about the method.

  Inside the transformer installed in the substation or power plant, a magnetic core coil is housed and insulating oil is sealed. Transformers are often placed outdoors and are often exposed to wind and rain, and may be attached to locations where vibrations occur. Moreover, it may be used in a high temperature environment.

  Such a transformer is comprised from many members. In order to prevent leakage of insulating oil sealed in the transformer, that is, oil leakage, rubber packing, for example, is inserted into the joint of the members constituting the transformer. Even if a transformer is attached to a place where vibration is generated, the absorption of vibration by this packing effectively prevents leakage of the lubricating oil enclosed in the transformer.

  If the rubber packing deteriorates due to use over a long period of time, the sealed insulating oil may leak out from or near the place where the packing is disposed. In this case, the problem of oil leakage can be solved by exchanging the packing. However, in order to replace the packing, it is necessary to stop the operation of the transformer and disassemble the transformer. Transformer outages may take several days. It is preferable to avoid stopping the operation of the transformer for a long period of time as much as possible because it causes a situation of stopping the power transmission for a long period of time. That is, it is required to shorten the period during which the operation of the transformer is stopped as much as possible.

  As a method of preventing oil leakage without disassembling the transformer, a method of repairing by applying a sealing material to the oil leakage location of the transformer has been adopted. According to the repair method using such a sealing material, the period during which the operation of the transformer is stopped can be shortened as compared with the case of disassembling the transformer. Japanese Unexamined Patent Application Publication No. 2009-292972 (Patent Document 1) and Japanese Unexamined Patent Application Publication No. 2012-211652 (Patent Document 2) disclose a repair method for preventing oil leakage of a transformer using a sealing material.

JP 2009-292972 A JP 2012-211162 A

  According to Patent Document 1, as a method of repairing oil leakage, a first application step of instantaneously curing by spraying a curing accelerator after applying an α-cyanoacrylate resin-based sealing material to a junction of a transformer An oil leakage repair method comprising a second coating step in which an α-cyanoacrylate resin-based sealing material is applied thereon and reinforced with a nonwoven fabric, and a third coating step in which a vinyl ester resin is coated on the nonwoven fabric is proposed. Yes. According to such an oil leakage repair method, a primary seal is performed in the first application process to stop the oil leakage first, and then a secondary seal such as a subsequent second application process and a third application process is performed to provide an oil leak location. The strength of the steel is reinforced, and durability that is insufficient with only the primary seal is secured.

  According to Patent Document 2, after applying the anticorrosion primer, a vinyl ester resin-based filler is attached so as to surround the oil leakage location, and the oil leakage is stopped by a fast-curing epoxy resin sealant at the oil leakage location. On top of that, a method has been proposed in which a vinyl ester resin-based filler is attached to form a shape, and a plurality of coating layers are formed with an epoxy resin-based sealing material and glass wool. According to such a construction method, first of all, oil leakage is stopped by a vinyl ester resin filler and a fast-curing epoxy resin sealant as a primary seal, and then a secondary seal is formed by forming a plurality of coating layers. It is supposed to improve durability by strengthening.

  As described above, conventionally, by laminating a plurality of seals having different characteristics such as a primary seal and a secondary seal, oil leakage is prevented at an early stage and strength is reinforced. Each of Patent Documents 1 and 2 requires a plurality of steps. In the repair of oil leakage that performs such a plurality of steps, not only the workability decreases due to the increase in the number of steps, but also the curing time of the thermosetting resin in each step must be ensured. As a result, there is a disadvantage that the period of repair work for oil leakage becomes longer as a whole, and the period during which the transformer is stopped becomes longer. Note that only the primary seal using the α-cyanoacrylate resin system or the vinyl ester resin system has a problem from the viewpoint of durability to prevent oil leakage as described above. That is, in Patent Literature 1 and Patent Literature 2, there is a problem in preventing oil leakage over a long period of time from the viewpoint of insufficient strength with only the primary seal. The so-called secondary seals in Patent Document 1 and Patent Document 2 are indispensable and cannot be omitted.

  An object of the present invention is to provide an oil leakage preventing sealing material capable of improving workability and effectively preventing oil leakage over a long period of time.

  Another object of the present invention is to provide an oil leakage prevention structure capable of improving workability and effectively preventing oil leakage over a long period of time.

Still another object of the present invention is to provide a method for repairing an oil leakage location that can improve workability and can effectively prevent oil leakage over a long period of time.

  The inventors of the present application, for example, need to improve workability on the premise that the oil leakage prevention sealing material for preventing oil leakage of the transformer is provided with a function that has been conventionally required. I thought about that. That is, the function required as a sealing material for preventing oil leakage to prevent oil leakage of the transformer, specifically, for example, can withstand vibration over a long period of time, and has good weather resistance and heat resistance. In addition to having durability such as, it is fast-curing from the viewpoint of preventing oil leakage at an early stage, and as a work to prevent oil leakage, without performing multiple application processes and repair processes once It was considered necessary to obtain a sealing material for preventing oil leakage having the various functions described above in the repair process. The inventors of the present invention have made extensive studies and have come to construct the present invention.

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

  Such an oil leakage prevention sealing material includes, as a main agent, 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, respectively, and a curing agent. Since the polythiol-based curing agent and the curing accelerator are included, the obtained cured product can exhibit flexibility and toughness, and can be improved in weather resistance and heat resistance. The durability required as a sealing material for prevention can be improved. Moreover, since it is not necessary to perform the operation | work which forms the further seal | sticker for reinforcing intensity | strength later, an operation | work process can be decreased and workability | operativity can be improved. That is, it is not necessary to perform secondary sealing that gives strength later, and it is possible to form an oil leakage preventing sealing material having a function required as an oil leakage preventing sealing material in a single operation. In addition, according to such an oil leakage prevention sealing material, it is possible to shorten the time required for the curing reaction of the thermosetting resin as a whole, compared to the repair method in which a plurality of coating processes are performed. The period during which the operation is stopped can be greatly shortened. Therefore, such an oil leakage preventing sealing material can improve workability and effectively prevent oil leakage over a long period of time.

  Moreover, you may comprise a hardening | curing agent so that an amine-type hardening | curing agent may be included. 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.

  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 handling property of the material can be appropriately improved even when working in a low temperature environment.

  Moreover, you may comprise so that the content rate of the reactive diluent with respect to bifunctional epoxy resin may be 20 weight part or less with respect to 100 weight part of bifunctional epoxy resin. By carrying out like this, the viscosity of a main ingredient can be made more appropriate, and the softness | flexibility and toughness as a sealing material for oil leak prevention can be made more appropriate.

  In addition, you may comprise so that the compounding ratio of a main ingredient and a hardening | curing agent may exist in the range of 1: 0.1-1: 1.2. By carrying out like this, hardening reaction can be advanced more efficiently and the softness | flexibility and toughness as a sealing material for oil leak prevention can be made more appropriate.

  In another aspect of the present invention, the oil leakage prevention structure is composed of a plurality of members, and is disposed in an oil sealing member in which oil is sealed and an oil leakage point of the oil sealing member. And a hardened material obtained by reacting a hardener with a sealant for preventing oil leakage, and the main agent is a bisphenol A type at both ends of an aliphatic skeleton composed of long-chain hydrocarbon chains. A bifunctional epoxy resin having a skeleton and an epoxy group is included, and the curing agent includes a polythiol-based curing agent and a curing accelerator.

In still another aspect of the present invention, the method for repairing an oil leakage point is composed of a plurality of members, and an oil leakage point for repairing the oil leakage point of an oil sealing member in which oil is sealed is contained. A repair method comprising: a main agent comprising 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; a polythiol-based curing agent and a curing accelerator; A preparation step for preparing a curing agent to be included, a mixing step for mixing the prepared main agent and a curing agent, an application step for applying the mixture obtained in the mixing step to the oil leakage location, and curing the mixture after the application step A curing step.

  Such an oil leakage prevention sealing material includes, as a main agent, 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, respectively, and a curing agent. Since the polythiol-based curing agent and the curing accelerator are included, the obtained cured product can exhibit flexibility and toughness, and can be improved in weather resistance and heat resistance. The durability required as a sealing material for prevention can be improved. Moreover, since it is not necessary to perform the operation | work which forms the further seal | sticker for reinforcing intensity | strength later, an operation | work process can be decreased and workability | operativity can be improved. That is, it is not necessary to perform secondary sealing that gives strength later, and it is possible to form an oil leakage preventing sealing material having a function required as an oil leakage preventing sealing material in a single operation. In addition, according to such an oil leakage prevention sealing material, it is possible to shorten the time required for the curing reaction of the thermosetting resin as a whole, compared to the repair method in which a plurality of coating processes are performed. The period during which the operation is stopped can be greatly shortened. Therefore, such an oil leakage preventing sealing material can improve workability and effectively prevent oil leakage over a long period of time.

It is a schematic sectional drawing which shows a part of oil leakage prevention structure which concerns on one Embodiment of this invention. It is a flowchart which shows the typical process of the repair method of the oil leak location which concerns on one Embodiment of this invention.

  Embodiments of the present invention will be described below. First, the configuration of a sealing material for preventing oil leakage according to an embodiment of the present invention will be described.

  The oil leakage preventing sealant prevents oil leakage by a cured product obtained by reacting the main agent and the curing agent. The oil leakage prevention sealing material is obtained by mixing a main agent mainly containing a bifunctional epoxy resin and a curing agent mainly containing a polythiol-based curing agent and causing a curing reaction.

  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. Moreover, since the part which comprises a long-chain hydrocarbon chain is lipophilic, it is thought that moderate oil absorbency is exhibited. This point is preferable from the viewpoint of adhesiveness to an adherend as a sealing material for preventing oil leakage. 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 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) 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.

  The reactive diluent preferably has good affinity with the bifunctional epoxy resin (Chemical Formula 1) and is lipophilic. This is because oil leakage proceeds even in the initial state of application in which the curing reaction has not progressed at all, and it is necessary to absorb the oil that leaks to some extent from the viewpoint of adhesiveness. 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, the content rate of the reactive diluent with respect to bifunctional epoxy resin (Chemical Formula 1) is 20 weight part or less with respect to 100 weight part of bifunctional epoxy resin (Chemical formula 1), for example. You may comprise. By carrying out like this, the viscosity of a main ingredient can be made more appropriate, and the softness | flexibility and toughness as a sealing material for oil leak prevention can be made more appropriate.

  Moreover, you may comprise so that a powdery filler, such as inorganic powder, may be included in a main ingredient. By doing so, it becomes easy to adjust the viscosity of the main agent containing the bifunctional epoxy resin (Chemical Formula 1) so that it can be easily handled, and so-called thixotropic property is improved, and handling property during work is improved. Can do. 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 type of filler, silica gel, calcium carbonate, carbon black, aluminum powder, alumina, talc, glass fiber, titanium oxide and the like are selected. Specific products include AEROSIL 300 (Nippon Aerosil Co., Ltd.), Shiraka Hana CC, Silver W (all manufactured by Shiroishi Kogyo Co., Ltd.), Carbon Black # 70G (Asahi Carbon Co., Ltd.), Aluminum Powder YP580 (Yamaishi Metal Co., Ltd.), Alumina A-42-2 (Showa Denko Co., Ltd.), Talc MS-P (Nihon Talc Co., Ltd.), Cut Fiber SS 05C-404 (Nittobo Co., Ltd.) ), Titanium A-150 (manufactured by Sakai Chemical Industry Co., Ltd.), and the like.

  The curing agent includes a polythiol-based curing agent and a curing accelerator. By comprising in this way, what is called quick-curing property can be ensured, and the softness | flexibility of hardened | cured material can also be ensured. 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). Further, as the curing accelerator, for example, a trisdimethylaminophenol type or an ethyleneamine type tertiary amine type is used, and 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.

  The curing agent may be configured to 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. 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.

  Further, the curing agent may be configured to include a predetermined amount of powdery filler. This makes it easy to adjust the viscosity of the curing agent so that it can be easily handled, improves so-called thixotropy, and makes it easy to handle during work. In addition, as a specific product of a filler, the thing similar to the filler contained in the above-mentioned main ingredient is mentioned.

  That is, according to the oil leakage preventing sealing material according to the present invention, at least one of the main agent and the curing agent may be configured to include a powdery filler.

  In addition, you may comprise so that the compounding ratio of a main ingredient and a hardening | curing agent may exist in the range of 1: 0.1 to 1: 1.2. By carrying out like this, the softness | flexibility and toughness as a sealing material for oil-leakage prevention can be made more appropriate by making hardening time, the intensity | strength of the hardened | cured material, etc. into an appropriate range. In addition, about the equivalent compounding ratio of the bifunctional epoxy resin (Chemical Formula 1) contained in the main agent and the polythiol-based curing agent contained in the curing agent, those within the range of 1: 0.8 to 1: 1.2 It is preferably applied.

  Next, the structure of the oil leakage prevention structure according to the present invention will be described. FIG. 1 is a schematic sectional view showing a part of an oil leakage prevention structure according to an embodiment of the present invention. With reference to FIG. 1, an oil leakage prevention structure 11 according to an embodiment of the present invention is composed of a plurality of members, and an oil sealing member 12 in which oil is sealed, and an oil sealing member 12. The oil leakage prevention sealing material 13 is provided to prevent oil leakage by a cured product obtained by reacting the main agent and the curing agent.

  The oil sealing member 12 seals oil such as lubricating oil in a space located on the left side of the drawing (not shown). An example of the oil sealing member 12 is a transformer.

  The oil sealing member 12 is arranged on the upper side in FIG. 1 and provided with a flange, and the second member 15 is provided on the lower side in FIG. 1 and also provided with a flange. And a thin rubber packing 16 disposed between the first member 14 and the second member 15. The first and second members 14 and 15 are provided with through holes 17 and 18 penetrating in the vertical direction of the drawing. Further, the packing 16 is also provided with a through-hole penetrating in the vertical direction on the paper surface. Bolts 19 are inserted into the through holes 17 and 18, and the first and second members 14 and 15 are fastened by a nut 21 that is screwed on one end 20 side of the bolt 19.

Here, among the first and second members 14 and 15, the packing 16, the bolt 19, and the nut 21, the oil leakage preventing sealing material 13 is disposed on the surface 22 exposed to the outside. Specifically, the oil leakage preventing sealing material 13 is provided so as to form a thin film so as to cover the entire surface of the member constituting the oil sealing member 12. The surface of up to 24 length of leakage oil for preventing sealant 13 from the surface 23 of the nut 21 which is represented by the length t ₁ in FIG. 1, i.e., as the thickness of the leakage oil for preventing sealant 13, For example, 1 to 2 mm (millimeter) is selected.

  Here, for the sealing material, as described above, 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, and is cured. The agent includes a polythiol-based curing agent and a curing accelerator.

  According to such an oil leakage prevention structure, workability can be improved and oil leakage can be effectively prevented over a long period of time.

Next, a method for repairing an oil leakage location according to the present invention will be described. FIG. 2 is a flowchart showing a typical process of a method for repairing an oil leakage location according to an embodiment of the present invention.

With reference to FIG. 2, the method for repairing an oil leak location according to one embodiment of the present invention cleans the location where the oil leak occurs prior to the work. Specifically, the oil leakage portion, oil content, moisture, dirt, etc. are removed.

  As a repair method, first, a main agent and a curing agent are prepared (S1). In this case, it is advisable to add a reactive diluent as the main agent in advance to adjust the viscosity and to mix the filler. Moreover, about a hardening | curing agent, it is good to mix a hardening accelerator and a filler beforehand.

  Thereafter, the prepared main agent and the prepared curing agent are mixed (S2). 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 oil leakage location (S3). The case where the mixture is applied using the oil leakage prevention structure shown in FIG. 1 will be described. Specifically, first, the joint portion of the bolt 19 and the nut 21 is applied, and then the first and second portions are applied. The members 14 and 15 and the surface 22 of the packing 16 are applied so as to cover them. In this case, it may be performed manually by an operator, 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 (S4). In this way, the oil leakage point is repaired.

According to such a method for repairing an oil leakage location , workability can be improved and oil leakage can be effectively prevented over a long period of time.

  If necessary, the coating material may be applied on the upper side of the sealing material, that is, on the upper layer side so as to cover the sealing material. By doing so, the appearance can be improved and the weather resistance and the like can be improved.

  In the above embodiment, the sealing material is provided so as to cover the entire surface of the member constituting the oil sealing member. However, the present invention is not limited to this. It is good also as providing so that a part may be exposed and another part may be covered.

  In the above-described 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 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.

  In the above embodiment, it is used to prevent oil leakage of the transformer. However, the present invention is not limited to this, and when oil leakage occurs in a member in which oil is sealed, The present invention is applied to a confirmation window provided in a device using electrical insulating oil such as a machine or an oil filled device.

Example 1
The oil leakage prevention sealing material 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.). 100 parts by weight of EPICLON EXA-4816, 5 parts by weight of SR-16H (Sakamoto Yakuhin Kogyo Co., Ltd.) as a reactive diluent, and Aerosil (AEROSIL 300 (Nippon Aerosil Co., Ltd.)) as a filler 1 part by weight) was added and mixed thoroughly with stirring. 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. 100 parts by weight of MR-122, 7 parts by weight of HD-Acc65 (manufactured by Daito Sangyo Co., Ltd.) as a hardening accelerator, and 60 parts of calcium carbonate (Shiraka Hana CC (manufactured by Shiraishi Kogyo Co., Ltd.)) as a filler 2 parts by weight of Aerosil (AEROSIL 300) was added as a filler, and the mixture was sufficiently stirred. 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, 61 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. In addition, this Example 1, Example 2-Example 3, Example 6-Example 10, and Comparative Example 1-Comparative Example 3 shown below are making the main ingredient and the hardening | curing agent into an equivalent mixture.

  Next, the obtained mixture according to Example 1 was applied to a predetermined portion serving as an oil leakage portion of a test apparatus described later as an oil sealing member in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Example 1 was 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 10 are also shown in Table 1.

(Example 2)
EPICLON EXA-4816 was prepared as a bifunctional epoxy resin contained in the main agent. Then, 1 part by weight of Aerosil (AEROSIL 300) as a filler was added to 100 parts by weight of EPICLON EXA-4816, and the mixture was sufficiently stirred and mixed while being heated to about 40 ° C. In this way, a base agent according to Example 2 was obtained. The main agent according to Example 1 was putty at 20 ° C.

  The same curing agent as in Example 1 was prepared. Then, 54 parts by weight of the curing agent was added to 100 parts by weight of the main agent, and stirring and mixing were performed to obtain a mixture according to Example 2.

  Next, the obtained mixture according to Example 2 was applied to a predetermined portion of the test apparatus in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. Thus, an oil leakage preventing sealing material according to Example 2 was obtained.

(Example 3)
EPICLON EXA-4816 was prepared as a bifunctional epoxy resin contained in the main agent. To 100 parts by weight of this EPICLON EXA-4816, 20 parts by weight of SR-16H as a reactive diluent and 1 part by weight of Aerosil (AEROSIL 300) as a filler were added and mixed thoroughly. Thus, the main ingredient which concerns on Example 3 was obtained. The main agent according to Example 1 was putty at 20 ° C.

  As the curing agent according to Example 3, the same curing agent as in Example 1 was prepared. Then, 67 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 3.

  Next, the obtained mixture according to Example 3 was applied to a predetermined portion of the test apparatus in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Example 3 was obtained.

Example 4
The same main agent and curing agent as in Example 1 were prepared. Then, 55 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. In Example 4, the curing agent was reduced by about 10% with respect to the equivalent compounding ratio.

  Next, the obtained mixture according to Example 4 was applied to a predetermined portion of the test apparatus. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Example 4 was obtained.

(Example 5)
The same main agent and curing agent as in Example 1 were prepared. Then, 67 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. In Example 4, the curing agent was increased by about 10% with respect to the equivalent compounding ratio.

  Next, the obtained mixture according to Example 5 was applied to a predetermined portion of the test apparatus in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Example 5 was obtained.

(Example 6)
As the main agent according to Example 6, the same main agent as in Example 1 was prepared. MR-122 is prepared as a polythiol-based curing agent included in the curing agent according to Example 6, and I-5136 (Itotsu Sangyo Co., Ltd.) is an isophoronediamine-based curing agent as an amine-based curing agent included in the curing agent according to Example 6. (Made by Co., Ltd.) was prepared. Then, 80 parts by weight of MR-122, 20 parts by weight of I-5136, 6 parts by weight of HD-Acc65 as a curing accelerator, 50 parts by weight of calcium carbonate (white gloss flower CC) as a filler, and the same filler 2 parts by weight of Aerosil (AEROSIL 300) was added and sufficiently stirred. Thus, the hardening | curing agent which concerns on Example 5 was obtained. The curing agent according to Example 6 was also putty-like at 20 ° C.

  And about the main ingredient and hardening agent which were obtained in this way, 42 weight part of hardening | curing agents were added with respect to 100 weight part of main ingredients, and stirring mixing was performed, and the mixture which concerns on Example 6 was obtained.

  And the obtained mixture which concerns on Example 6 was apply | coated to the predetermined location of the test apparatus in 20 degreeC atmosphere. Then, 2 hours passed and the curing reaction was completed. Thus, an oil leakage preventing sealing material according to Example 6 was obtained.

(Example 7)
As the main agent according to Example 7, the same main agent as in Example 1 was prepared. MR-122 was prepared as a polythiol-based curing agent contained in the curing agent according to Example 7. 100 parts by weight of MR-122, 5 parts by weight of HD-Acc65 as a curing accelerator, 5 parts by weight of calcium carbonate (white glossy CC) as a filler, and 2 parts by weight of Aerosil (AEROSIL 300) as a filler In addition, well stirred. In this way, a curing agent according to Example 6 was obtained. The curing agent according to Example 7 was also putty-like at 20 ° C.

  And about the obtained main ingredient and hardening | curing agent, 60 weight part of hardening | curing agents were added with respect to 100 weight part of main ingredients, and stirring mixing was performed, and the mixture which concerns on Example 7 was obtained.

  Next, the obtained mixture according to Example 7 was applied to a predetermined portion of the test apparatus in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Example 7 was obtained.

(Example 8)
As the main agent according to Example 8, the same main agent as in Example 1 was prepared. MR-122 was prepared as a polythiol-based curing agent contained in the curing agent according to Example 8. Based on 100 parts by weight of MR-122, 10 parts by weight of HD-Acc65 as a curing accelerator, 50 parts by weight of calcium carbonate (white glaze CC) as a filler, and 2 parts by weight of Aerosil (AEROSIL 300) as a filler In addition, well stirred. Thus, the hardening | curing agent which concerns on Example 7 was obtained. The curing agent according to Example 8 was also putty at 20 ° C.

  And about the obtained main ingredient and hardening | curing agent, 62 weight part of hardening | curing agents were added with respect to 100 weight part of main ingredients, and stirring mixing was performed, and the mixture which concerns on Example 8 was obtained.

  Next, the obtained mixture according to Example 8 was applied to a predetermined portion of the test apparatus in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Example 8 was obtained.

Example 9
As the main agent according to Example 9, the same main agent as in Example 1 was prepared. EH317 (manufactured by ADEKA Corporation) was prepared as a polythiol-based curing agent contained in the curing agent according to Example 9. To 100 parts by weight of this EH317, 7 parts by weight of HD-Acc65 as a curing accelerator, 50 parts by weight of calcium carbonate (white glaze CC) as a filler, and 2 parts by weight of Aerosil (AEROSIL 300) as a filler are added, Stir well. Thus, the hardening | curing agent which concerns on Example 9 was obtained. The curing agent according to Example 9 was also putty at 20 ° C.

  And about the obtained main ingredient and hardening | curing agent, 52 weight part of hardening | curing agents were added with respect to 100 weight part of main ingredients, and stirring mixing was performed, and the mixture which concerns on Example 9 was obtained.

  Next, the obtained mixture according to Example 9 was applied to a predetermined portion of the test apparatus in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Example 9 was obtained.

(Example 10)
As the main agent according to Example 10, the same main agent as in Example 1 was prepared. MR-122 was prepared as a polythiol-based curing agent contained in the curing agent according to Example 10. Based on 100 parts by weight of this MR-122, 7 parts by weight of HD-Acc43 (manufactured by Daito Sangyo Co., Ltd.) as a curing accelerator, 50 parts by weight of calcium carbonate (white glaze CC) as a filler, and Aerosil as a filler 2 parts by weight of (AEROSIL 300) was added and stirred thoroughly. Thus, the hardening | curing agent which concerns on Example 10 was obtained. The curing agent according to Example 10 was also putty at 20 ° C.

  And about the main ingredient and hardening | curing agent which were obtained in this way, 61 weight part of hardening | curing agents were added with respect to 100 weight part of main ingredients, and stirring mixing was performed, and the mixture which concerns on Example 10 was obtained.

  And the obtained mixture which concerns on Example 10 was apply | coated to the predetermined location of the test apparatus in 20 degreeC atmosphere. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Example 10 was obtained.

(Comparative Example 1)
As a main agent according to Comparative Example 1, instead of the bifunctional epoxy resin in Example 1, EP-4100 (manufactured by ADEKA), which is a bisphenol A type epoxy resin, was used. This EP-4100 was a liquid having a low viscosity at room temperature. To 100 parts by weight of this EP-4100, 66 parts by weight of calcium carbonate (white gloss flower CC) as a filler and 1 part by weight of Aerosil (AEROSIL 300) were added and stirred sufficiently. Thus, the main ingredient which concerns on the comparative example 1 was obtained. The main agent according to Comparative Example 1 was putty at 20 ° C. The curing agent according to Comparative Example 1 was the same as the curing agent according to Example 1.

  And about the main ingredient and the hardening | curing agent, 68 weight part of hardening | curing agents were added with respect to 100 weight part of main ingredients, and stirring mixing was performed, and the mixture which concerns on the comparative example 1 was obtained.

  And the mixture which concerns on the comparative example 1 was apply | coated to the predetermined location of the test apparatus in 20 degreeC atmosphere. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Comparative Example 1 was obtained.

  In addition, it shows in Table 2 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 2, 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 Comparative Examples 2 to 3 are also shown in Table 2.

(Comparative Example 2)
The main ingredient according to Comparative Example 2 was the same as the main ingredient according to Example 1. As an amine-based curing agent contained in the curing agent according to Comparative Example 2, I-5136 (manufactured by Daito Sangyo Co., Ltd.), which is an isophoronediamine-based curing agent, was prepared. Then, 50 parts by weight of calcium carbonate (white gloss flower CC) as a filler and 2 parts by weight of Aerosil (AEROSIL 300) as a filler were added to 100 parts by weight of I-5136, and the mixture was sufficiently stirred. Thus, the hardening | curing agent which concerns on the comparative example 2 was obtained. The curing agent according to Comparative Example 2 was also putty at 20 ° C.

  And about the main ingredient and the hardening | curing agent, 18 weight part of hardening | curing agents were added with respect to 100 weight part of main ingredients, and stirring mixing was performed, and the mixture which concerns on the comparative example 2 was obtained.

  And the mixture which concerns on the comparative example 2 was apply | coated to the predetermined location of the test apparatus in 20 degreeC atmosphere. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Comparative Example 2 was obtained.

(Comparative Example 3)
The main ingredient according to Comparative Example 3 was the same as the main ingredient according to Example 1. MR-122 was prepared as a polythiol-based curing agent contained in the curing agent according to Comparative Example 3. To 100 parts by weight of MR-122, 50 parts by weight of calcium carbonate (white gloss flower CC) as a filler and 2 parts by weight of Aerosil (AEROSIL 300) as a filler were added and sufficiently stirred. Thus, the hardening | curing agent which concerns on the comparative example 3 was obtained. The curing agent according to Comparative Example 3 was also putty at 20 ° C.

  And about the main ingredient and hardening | curing agent which were obtained in this way, 58 weight part of hardening | curing agents were added with respect to 100 weight part of main ingredients, and stirring mixing was performed, and the mixture which concerns on the comparative example 3 was obtained.

  Next, the obtained mixture according to Comparative Example 3 was applied to a predetermined portion of the test apparatus in an atmosphere of 20 ° C. Then, 2 hours passed and the curing reaction was completed. In this way, an oil leakage preventing sealing material according to Comparative Example 3 was obtained.

  Next, for the obtained oil leakage prevention sealing materials according to Examples 1 to 10 and Comparative Examples 1 to 3, a sealing test for confirming the presence or absence of oil leakage, a heat cycle test for evaluating durability, and A tensile shear bond strength test was performed. The test results are shown in Table 3.

  First, the sealing test will be described. The sealing test was performed by confirming whether or not oil leakage occurred at the oil leakage location where the sealing material was applied. In the sealing test, a microcheck developer (manufactured by Taiho Kosai Co., Ltd.) was used as a penetrant flaw detector. As a test method, this penetrant was sprayed on the surface of the portion where the sealing material was applied. Then, if the powder was dried in white at the location where the penetrant was sprayed, it was judged that there was no oil leakage and evaluated as “good”. On the other hand, if the powder was not dried in white at the location where the penetrant was sprayed, it was judged that oil had leaked and was evaluated as “bad”. The test results are shown in Table 3 below.

  Next, the heat cycle test will be described. The heat cycle test was performed as follows. First, as an apparatus to be used, a copper wire having a diameter of 0.8 mm is sandwiched between the end face of the flange of the insulating oil-sealed chamber and the cork packing, and pressure is applied by 0.05 MPa of nitrogen to artificially leak oil. A test device was used. Using this test apparatus, oil leakage was stopped, that is, the mixture according to Example 1 was applied to complete the curing reaction, and then the chamber was placed in a thermostat and a heat cycle test was performed. The durability of the sealing material was evaluated based on the results of this heat cycle 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 80 ° C. for 3 hours, and then holding again at 20 ° C. for 30 minutes is one cycle. It was. Then, this cycle was repeated 10 times, and then the presence or absence of oil leakage was confirmed in the same manner as in the sealing test, and the test result as Condition 1 was obtained. About this heat cycle test, it evaluated by the sample number of the sample which was evaluated as "good" in the sealing test among the samples which are not oil-leaked out of 10 samples. The greater the number of samples, the better the durability and the better the sealing material. In addition, when durability under a high temperature atmosphere of 100 ° C. is required, tests of condition 2 and condition 3 are performed instead of condition 1. That is, as conditions 2 and 3, a cycle of holding at −10 ° C. for 3 hours, holding at 20 ° C. for 30 minutes, holding at 100 ° C. for 3 hours, and then holding again at 20 ° C. for 30 minutes is one cycle. It was. And this cycle was repeated 5 times, and it was set as the test result as the condition 2. Further, this cycle was repeated 10 times, and the test result as Condition 3 was obtained. The test results are shown in Table 3.

  Next, the tensile shear bond strength test will be described. In the tensile shear bond strength test, the atmosphere temperature was set to 23 ° C., and the sealing materials according to Examples 1 to 10 and Comparative Examples 1 to 3 were interposed between the steel and steel. The steel was bonded. In this case, it was cured in a 23 ° C. atmosphere. After hardening for 24 hours, one steel was fixed, the other steel was pulled, and the bond strength when the steel was removed was measured. Specifically, it was performed according to JIS K6850. The test results are shown in Table 3. The unit of the numerical value representing the tensile shear bond strength is MPa (megapascal).

  Referring to Tables 1 to 3, the sealing test was “bad” in the results of Comparative Examples 2 and 3. In the case of Comparative Example 2 and Comparative Example 3, since the curing reaction is slow, the oil that gradually oozes out from the oil leakage location cannot be stopped, and oil leakage prevention is considered to be incomplete. On the other hand, the results of Examples 1 to 10 and Comparative Example 1 were good. In addition, about the comparative example 2 and the comparative example 3, the sealing test is not cleared and the heat cycle test is not performed.

  As for the results of the heat cycle test, in the case of Condition 1, none of them was cleared in Comparative Example 1. Although the sealing material according to Comparative Example 1 was good as a result of the sealing test, it was inferior in flexibility and toughness as a sealing material, and as a result, the durability was insufficient. This is considered to be due to the fact that the sealing material could not withstand the specified conditions and a gap was formed between the sealing material and the adherend, or that the sealing material itself was cracked or damaged. In Examples 1 to 10, all the samples were cleared under Condition 1. Therefore, it is judged that the sealing material is good. This tendency appears even when the numerical values of the tensile shear bond strength are compared. That is, for Examples 1 to 10, the value of tensile shear bond strength is high, and the minimum value is 10 MPa or more, while for Comparative Examples 1 to 3, the value of tensile shear bond strength is Is low and less than 10 MPa.

  Moreover, in the conditions prescribed | regulated to the conditions 2, the thing of Example 1, Example 2, Example 4, Example 5, Example 6, Example 8 cleared by all the samples. When use under harsher conditions is required, the sealing material according to Example 1, Example 2, Example 4, Example 5, Example 6, and Example 8 may be used. Furthermore, in the conditions specified in Condition 3, the sample of Example 6 was cleared in all samples. Therefore, when use under further severe conditions is required, the sealing material according to Example 6 may be used.

As described above, according to such an oil leakage prevention sealing material, an oil leakage prevention structure, and a method for repairing an oil leakage location , it is possible to improve workability and effectively prevent oil leakage over a long period of time. it can.

  It should be understood that the embodiments and examples disclosed this time are illustrative in all points and are not restrictive. The scope of the present invention is not intended to be described above, but is intended to include the scope indicated by the claims, and all modifications and improvements within the meaning and scope equivalent to the claims.

The oil leakage prevention sealing material, the oil leakage prevention structure, and the oil leakage location repair method according to the present invention are particularly effectively used when preventing oil leakage of a transformer disposed outdoors.

DESCRIPTION OF SYMBOLS 11 Oil leak prevention structure, 12 Oil enclosure member, 13 Sealing material for oil leak prevention, 14 1st member, 15 2nd member, 16 Packing, 17, 18 Through-hole, 19 bolt, 20 edge part, 21 Nut, 22, 23, 24 Surface.

Claims (7)

An oil leakage prevention sealing material for preventing oil 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 skeleton and an epoxy group on both ends of an aliphatic skeleton composed of a long hydrocarbon chain,
The said hardening | curing agent is a sealing material for oil-leakage prevention containing a polythiol type hardening | curing agent and a hardening accelerator. The oil leakage prevention sealing material according to claim 1, wherein the curing agent includes an amine-based curing agent. The oil leakage prevention sealing material according to claim 1 or 2, wherein the main agent contains a reactive diluent. The sealing material for oil leakage prevention according to claim 3, wherein a content ratio of the reactive diluent with respect to the bifunctional epoxy resin is 20 parts by weight or less with respect to 100 parts by weight of the bifunctional epoxy resin. The oil leakage prevention sealing material according to any one of claims 1 to 4, wherein a mixing ratio of the main agent and the curing agent is in a range of 1: 0.1 to 1: 1.2. It is composed of a plurality of members, and the oil-sealed member in which oil is sealed and the oil-sealed portion of the oil-sealed member are disposed at the oil leakage location and leaks by a cured product obtained by reacting the main agent and the curing agent. With oil leakage prevention sealing material to prevent oil,
The main agent includes 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,
The said hardening | curing agent is an oil leakage prevention structure containing a polythiol type hardening | curing agent and a hardening accelerator. It is composed of a plurality of members, and is a method of repairing a leaked oil location that repairs a leaked location of an oil-sealed member in which oil is sealed.
Preparation of a main agent containing 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 a curing agent containing a polythiol-based curing agent and a curing accelerator A preparation process to
A mixing step of mixing the prepared main agent and the curing agent;
An application step of applying the mixture obtained in the mixing step to an oil leakage location;
An oil leakage repair method comprising: a curing step of curing the mixture after the coating step.

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