JP7068043B2 - Electrical insulating oil composition - Google Patents

Electrical insulating oil composition Download PDF

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JP7068043B2
JP7068043B2 JP2018103631A JP2018103631A JP7068043B2 JP 7068043 B2 JP7068043 B2 JP 7068043B2 JP 2018103631 A JP2018103631 A JP 2018103631A JP 2018103631 A JP2018103631 A JP 2018103631A JP 7068043 B2 JP7068043 B2 JP 7068043B2
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insulating oil
oil composition
electrically insulating
ethylphenyl
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JP2019207826A (en
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敦史 亀山
晴菜 福永
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Eneos Corp
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/46—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes silicones
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/32—Wound capacitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G2/00—Details of capacitors not covered by a single one of groups H01G4/00-H01G11/00
    • H01G2/10—Housing; Encapsulation

Description

本発明は、電気絶縁油組成物に関する。 The present invention relates to an electrically insulating oil composition.

電気絶縁油に対して主に求められる性能は、絶縁破壊電圧が高いことをはじめ、水素ガス吸収性が高いこと、粘度が低いこと、更に融点が低いこと等が挙げられる。近年、コンデンサをはじめとする各種油入電気機器（油含浸電気機器）が世界中で使用されるに当たり、より絶縁破壊電圧の高い電気絶縁油が使用されつつある。 The performances mainly required for electrical insulating oil include high dielectric breakdown voltage, high hydrogen gas absorption, low viscosity, and low melting point. In recent years, as various oil-filled electric devices (oil-impregnated electric devices) such as capacitors are used all over the world, electric insulating oil having a higher dielectric breakdown voltage is being used.

１－フェニル－１－キシリルエタン及び１－エチルフェニル－１－フェニルエタンは、その製造が容易であり、絶縁破壊電圧が比較的高く、誘電損失が小さい、融点が低い等の優れた特性を有していることから、電気絶縁油として広く用いられている。例えば、特許文献１には、電気絶縁油組成物として、１－フェニル－１－（２，４－ジメチルフェニル）エタン又は１－フェニル－１－（２，５－ジメチルフェニル）エタンを含有する組成物が記載されている。 1-Phenyl-1-kisilylethane and 1-ethylphenyl-1-phenylethane have excellent properties such as easy production, relatively high breakdown voltage, low dielectric loss, and low melting point. Therefore, it is widely used as an electrically insulating oil. For example, Patent Document 1 describes a composition containing 1-phenyl-1- (2,4-dimethylphenyl) ethane or 1-phenyl-1- (2,5-dimethylphenyl) ethane as an electrically insulating oil composition. The thing is listed.

特開昭５７－５０７０８号公報Japanese Unexamined Patent Publication No. 57-50708

近年、世界経済の発展に伴って、油含浸電気機器には、これまで使用されていなかった地域（例えば、極低温の地域等）での使用が求められ、それに対応できるような低温特性に優れた電気絶縁油の検討が進められている。また、屋外に設置させることの多い産業用電気機器の場合、その使用形態ゆえに高温における特性も重要である。しかしながら、上述したような従来の電気絶縁油組成物は、温度領域によってはその絶縁破壊電圧が必ずしも満足できるものではなかった。 In recent years, with the development of the world economy, oil-impregnated electrical equipment has been required to be used in areas that have not been used before (for example, extremely low temperature areas), and it has excellent low temperature characteristics that can cope with it. The study of electrical insulating oil is underway. In addition, in the case of industrial electrical equipment that is often installed outdoors, the characteristics at high temperatures are also important because of its usage pattern. However, the conventional electric insulating oil composition as described above is not always satisfactory in its dielectric breakdown voltage depending on the temperature range.

本発明は、このような実情に鑑みてなされたものであり、広範な温度領域において良好な絶縁破壊電圧を達成し得る電気絶縁油組成物を提供することを目的とする。 The present invention has been made in view of such circumstances, and an object of the present invention is to provide an electrically insulating oil composition capable of achieving a good dielectric breakdown voltage in a wide temperature range.

本発明は、（エチルフェニル）フェニルメタンと、１－エチルフェニル－１－フェニルエタンと、１－エチルフェニル－２－フェニルエタンと、を含む電気絶縁油組成物を提供する。 The present invention provides an electrically insulating oil composition comprising (ethylphenyl) phenylmethane, 1-ethylphenyl-1-phenylethane and 1-ethylphenyl-2-phenylethane.

電気絶縁油組成物は、ビス（エチルフェニル）メタン及び（ジエチルフェニル）フェニルメタンを更に含んでいてもよい。 The electrically insulating oil composition may further contain bis (ethylphenyl) methane and (diethylphenyl) phenylmethane.

電気絶縁油組成物は、１，１－ビス（エチルフェニル）エタン及び１－ジエチルフェニル－１－フェニルエタンを更に含んでいてもよい。 The electrically insulating oil composition may further contain 1,1-bis (ethylphenyl) ethane and 1-diethylphenyl-1-phenylethane.

（エチルフェニル）フェニルメタンの含有量は、電気絶縁油組成物全量を基準として１０～３５質量％であり、１－エチルフェニル－１－フェニルエタンの含有量は、電気絶縁油組成物全量を基準として、２０～６０質量％であり、１－エチルフェニル－２－フェニルエタンの含有量は、電気絶縁油組成物全量を基準として、５～３０質量％であってもよい。 The content of (ethylphenyl) phenylmethane is 10 to 35% by mass based on the total amount of the electrically insulating oil composition, and the content of 1-ethylphenyl-1-phenylethane is based on the total amount of the electrically insulating oil composition. The content of 1-ethylphenyl-2-phenylethane may be 20 to 60% by mass, and the content of 1-ethylphenyl-2-phenylethane may be 5 to 30% by mass based on the total amount of the electrically insulating oil composition.

電気絶縁油組成物は、エポキシ化合物を、電気絶縁油組成物全量を基準として０．０１～１．０質量％含んでいてもよい。 The electric insulating oil composition may contain an epoxy compound in an amount of 0.01 to 1.0% by mass based on the total amount of the electric insulating oil composition.

電気絶縁油組成物は、４０℃における動粘度が５ｍｍ２／ｓ以下であってもよい。 The electrically insulating oil composition may have a kinematic viscosity of 5 mm 2 / s or less at 40 ° C.

本発明によれば、広範な温度領域において良好な絶縁破壊電圧を達成し得る電気絶縁油組成物を提供することができる。 According to the present invention, it is possible to provide an electrically insulating oil composition capable of achieving a good dielectric breakdown voltage in a wide temperature range.

以下、本発明の実施形態について詳細に説明する。 Hereinafter, embodiments of the present invention will be described in detail.

本実施形態に係る電気絶縁油組成物は、（エチルフェニル）フェニルメタンと、１－エチルフェニル－１－フェニルエタンと、１－エチルフェニル－２－フェニルエタンと、を含む。上記電気絶縁油組成物は、広範な温度領域（例えば、－５０℃～８０℃）において良好な絶縁破壊電圧を達成し得る。 The electrically insulating oil composition according to the present embodiment contains (ethylphenyl) phenylmethane, 1-ethylphenyl-1-phenylethane, and 1-ethylphenyl-2-phenylethane. The electrical insulating oil composition can achieve good dielectric breakdown voltage over a wide temperature range (eg, −50 ° C. to 80 ° C.).

本実施形態に係る電気絶縁油組成物が上記のような効果を奏する理由を、本発明者等は以下のように推察する。まず、従来の電気絶縁油組成物が、低温環境下において絶縁破壊電圧を低下させる原因として、使用の際に電気絶縁油組成物に含まれる成分が凝固することで油中に固形物が析出し、その部分から放電が発生しやすくなることが考えられる。一方で、高温環境下においては、コンデンサを構成する部材の一つである電極間の誘電体として使用されるポリプロピレンフィルム等のフィルムが、電気絶縁油組成物により膨潤することに起因して、フィルムの機械的ストレスの上昇やフィルム密度の低下が発生し、コンデンサの性能低下が起こりやすくなると考えられる。 The present inventors presume the reason why the electrically insulating oil composition according to the present embodiment exerts the above-mentioned effects as follows. First, as a cause of lowering the dielectric breakdown voltage of the conventional electrically insulating oil composition in a low temperature environment, solid matter is deposited in the oil due to solidification of the components contained in the electrically insulating oil composition during use. , It is conceivable that discharge is likely to occur from that part. On the other hand, in a high temperature environment, a film such as a polypropylene film used as a dielectric between electrodes, which is one of the members constituting a capacitor, swells due to the electrically insulating oil composition. It is considered that the mechanical stress of the capacitor increases and the film density decreases, and the performance of the capacitor tends to decrease.

これに対し、本実施形態に係る電気絶縁油組成物は、（エチルフェニル）フェニルメタンと、１－エチルフェニル－１－フェニルエタンと、１－エチルフェニル－２－フェニルエタンと、を含むことで、低温環境下及び高温環境下において、上述したような絶縁破壊電圧を低下させる要因の発生をバランスよく抑制することができたためと、本発明者等は推察する。具体的な理由は必ずしも明らかではないが、まず、上述した３成分ともに、分子中の芳香族炭素の比率が比較的高いため、水素ガス吸収性が高く、耐電圧特性に優れると考えられる。そして、上記３成分を含むことで、凝固点降下が起こり、低温環境下において電気絶縁油組成物に含まれる成分の凝固を効果的に抑制できたと推察する。また、（エチルフェニル）フェニルメタンは、特にポリプロピレンフィルム等のフィルムに対する膨潤性が小さく、高温環境下において絶縁破壊電圧の低下を効果的に抑制することができたと考えられる。 On the other hand, the electrically insulating oil composition according to the present embodiment contains (ethylphenyl) phenylmethane, 1-ethylphenyl-1-phenylethane, and 1-ethylphenyl-2-phenylethane. It is presumed by the present inventors that it was possible to suppress the occurrence of the factors that lower the dielectric breakdown voltage as described above in a well-balanced manner in a low temperature environment and a high temperature environment. Although the specific reason is not always clear, first, it is considered that all of the above-mentioned three components have a relatively high proportion of aromatic carbon in the molecule, so that they have high hydrogen gas absorption and excellent withstand voltage characteristics. It is presumed that the inclusion of the above three components caused a freezing point depression and effectively suppressed the solidification of the components contained in the electrically insulating oil composition in a low temperature environment. Further, it is considered that (ethylphenyl) phenylmethane has a small swelling property particularly for a film such as a polypropylene film, and can effectively suppress a decrease in the dielectric breakdown voltage in a high temperature environment.

電気絶縁油組成物における（エチルフェニル）フェニルメタンの含有量は、更に良好な絶縁破壊電圧を達成する観点から、電気絶縁油組成物全量を基準として、好ましくは１０質量％以上、より好ましくは１２質量％以上、更に好ましくは１５質量％以上である。電気絶縁油組成物における（エチルフェニル）フェニルメタンの含有量は、更に良好な絶縁破壊電圧を達成する観点から、電気絶縁油組成物全量を基準として、好ましくは３５質量％以下、より好ましくは３３質量％以下、更に好ましくは３０質量％以下である。 The content of (ethylphenyl) phenylmethane in the electrically insulating oil composition is preferably 10% by mass or more, more preferably 12 based on the total amount of the electrically insulating oil composition, from the viewpoint of achieving a better dielectric breakdown voltage. It is by mass% or more, more preferably 15% by mass or more. The content of (ethylphenyl) phenylmethane in the electrically insulating oil composition is preferably 35% by mass or less, more preferably 33, based on the total amount of the electrically insulating oil composition from the viewpoint of achieving a better dielectric breakdown voltage. It is mass% or less, more preferably 30 mass% or less.

電気絶縁油組成物における１－エチルフェニル－１－フェニルエタンの含有量は、更に良好な絶縁破壊電圧を達成する観点から、電気絶縁油組成物全量を基準として、好ましくは２０質量％以上、より好ましくは２５質量％以上、更に好ましくは３０質量％以上である。電気絶縁油組成物における１－エチルフェニル－１－フェニルエタンの含有量は、更に良好な絶縁破壊電圧を達成する観点から、電気絶縁油組成物全量を基準として、好ましくは６０質量％以下、より好ましくは５５質量％以下、更に好ましくは５０質量％以下である。 The content of 1-ethylphenyl-1-phenylethane in the electrically insulating oil composition is preferably 20% by mass or more based on the total amount of the electrically insulating oil composition from the viewpoint of achieving a better dielectric breakdown voltage. It is preferably 25% by mass or more, more preferably 30% by mass or more. The content of 1-ethylphenyl-1-phenylethane in the electrically insulating oil composition is preferably 60% by mass or less based on the total amount of the electrically insulating oil composition from the viewpoint of achieving a better dielectric breakdown voltage. It is preferably 55% by mass or less, more preferably 50% by mass or less.

電気絶縁油組成物における１－エチルフェニル－２－フェニルエタンの含有量は、更に良好な絶縁破壊電圧を達成する観点から、電気絶縁油組成物全量を基準として、好ましくは５質量％以上、より好ましくは７質量％以上、更に好ましくは１０質量％以上である。電気絶縁油組成物における１－エチルフェニル－２－フェニルエタンの含有量は、更に良好な絶縁破壊電圧を達成する観点から、電気絶縁油組成物全量を基準として、好ましくは３０質量％以下、より好ましくは２７質量％以下、更に好ましくは２５質量％以下である。 The content of 1-ethylphenyl-2-phenylethane in the electrically insulating oil composition is preferably 5% by mass or more based on the total amount of the electrically insulating oil composition from the viewpoint of achieving a better dielectric breakdown voltage. It is preferably 7% by mass or more, more preferably 10% by mass or more. The content of 1-ethylphenyl-2-phenylethane in the electrically insulating oil composition is preferably 30% by mass or less based on the total amount of the electrically insulating oil composition from the viewpoint of achieving a better dielectric breakdown voltage. It is preferably 27% by mass or less, more preferably 25% by mass or less.

本実施形態に係る電気絶縁油組成物は、本発明の効果を著しく阻害しない範囲において、上述した各成分以外に、他の炭化水素を更に含んでいてもよい。このような他の炭化水素を更に含む場合、当該炭化水素の沸点が２２０℃以上であってよく、２５０℃以上であってよい。また、当該炭化水素の沸点が４２０℃以下であってよく、３５０℃以下であってよい。 The electrically insulating oil composition according to the present embodiment may further contain other hydrocarbons in addition to the above-mentioned components as long as the effects of the present invention are not significantly impaired. When such other hydrocarbons are further contained, the boiling point of the hydrocarbon may be 220 ° C. or higher, and may be 250 ° C. or higher. Further, the boiling point of the hydrocarbon may be 420 ° C. or lower, and may be 350 ° C. or lower.

他の炭化水素としては、例えば、ビス（エチルフェニル）メタン、（ジエチルフェニル）フェニルメタン、１，１－ビス（エチルフェニル）エタン、１－ジエチルフェニル－１－フェニルエタン、１，１－ジフェニルエタン、１，２－ジフェニルエタン、ベンジルトルエン等の２環の芳香族化合物、アルキルナフタレン、ジベンジルトルエン等の多環芳香族化合物などが挙げられる。 Other hydrocarbons include, for example, bis (ethylphenyl) methane, (diethylphenyl) phenylmethane, 1,1-bis (ethylphenyl) ethane, 1-diethylphenyl-1-phenylethane, 1,1-diphenylethane. , 1,2-Diphenylethane, benzyltoluene and the like, bicyclic aromatic compounds, alkylnaphthalene, dibenzyltoluene and the like, polycyclic aromatic compounds and the like.

他の炭化水素の含有量は特に制限されないが、電気絶縁油組成物全量を基準として、例えば６５質量％以下、５０質量％以下、又は３５質量％以下であってよい。他の炭化水素の含有量は、電気絶縁油組成物全量を基準として、例えば０．１質量％以上、１質量％以上、又は５質量％以上であってよい。 The content of other hydrocarbons is not particularly limited, but may be, for example, 65% by mass or less, 50% by mass or less, or 35% by mass or less based on the total amount of the electrically insulating oil composition. The content of other hydrocarbons may be, for example, 0.1% by mass or more, 1% by mass or more, or 5% by mass or more, based on the total amount of the electrically insulating oil composition.

上述した本実施形態に係る電気絶縁油組成物に含まれる各成分の入手方法には特に制限はなく、市販品を用いてもよいし、自ら製造してもよい。 The method for obtaining each component contained in the electrically insulating oil composition according to the above-described embodiment is not particularly limited, and a commercially available product may be used or the product may be produced by itself.

電気絶縁油組成物は、水等の極性物質の含有により誘電正接が高くなり、絶縁性能が低下する。そのため、電気絶縁油組成物は、活性白土と接触させて水等の極性物質を除去したうえで使用することが好ましい。このときに使用する活性白土は、特に限定されない。活性白土の形状としては、特に限定されないが、実用上の観点から成型体の方が好ましい。 The electric insulating oil composition has a high dielectric loss tangent due to the inclusion of a polar substance such as water, and the insulating performance is lowered. Therefore, it is preferable to use the electrically insulating oil composition after contacting it with activated clay to remove polar substances such as water. The activated clay used at this time is not particularly limited. The shape of the activated clay is not particularly limited, but a molded body is preferable from a practical point of view.

電気絶縁油組成物は、各成分の製造方法によっては塩素分が含まれる場合がある。塩素分は電気絶縁油組成物の性能を悪化させる傾向があるため、塩素分の含有量を抑えることで電気絶縁油組成物の性能の悪化を抑制することができる。塩素分については必ずしも上記活性白土で除去できないため、電気絶縁油組成物は、塩素トラップ剤（塩素捕獲剤）としてエポキシ化合物を更に含むことが好ましい。なお、エポキシ化合物は、活性白土と接触させることによってある程度除去されてしまうことから、電気絶縁油組成物が白土処理された後にエポキシ化合物を添加することが望ましい。 The electrically insulating oil composition may contain chlorine depending on the production method of each component. Since the chlorine content tends to deteriorate the performance of the electric insulating oil composition, it is possible to suppress the deterioration of the performance of the electric insulating oil composition by suppressing the chlorine content. Since chlorine content cannot always be removed with the above-mentioned activated clay, it is preferable that the electrically insulating oil composition further contains an epoxy compound as a chlorine trapping agent (chlorine trapping agent). Since the epoxy compound is removed to some extent by contacting with active clay, it is desirable to add the epoxy compound after the electrically insulating oil composition has been treated with clay.

エポキシ化合物としては、例えば、３，４－エポキシシクロヘキシルメチル（３，４－エポキシシクロヘキサン）カルボキシレート、ビニルシクロヘキセンジエポキサイド、３，４－エポキシ－６－メチルシクロヘキシルメチル（３，４－エポキシ－６－メチルヘキサン）カルボキシレート等の脂環式エポキシ化合物、フェノールノボラック型エポキシ化合物、オルソクレゾールノボラック型エポキシ化合物等のビスフェノールＡのジグリシジルエーテル型エポキシ化合物などが例示される。エポキシ化合物の含有量は、電気絶縁油組成物全量を基準として０．０１～１．０質量％であることが好ましく、０．３～０．８質量％であることがより好ましい。含有量が０．０１質量％以上であれば塩素分をトラップする効果が充分に発揮される傾向があり、１．０質量％以下であれば電気絶縁油組成物の電気特性に悪影響を及ぼしにくい。 Examples of the epoxy compound include 3,4-epoxycyclohexylmethyl (3,4-epoxycyclohexane) carboxylate, vinylcyclohexendiepoxide, and 3,4-epoxy-6-methylcyclohexylmethyl (3,4-epoxy-6-). Examples thereof include alicyclic epoxy compounds such as methylhexane) carboxylate, phenol novolac type epoxy compounds, and bisphenol A diglycidyl ether type epoxy compounds such as orthocresol novolac type epoxy compounds. The content of the epoxy compound is preferably 0.01 to 1.0% by mass, more preferably 0.3 to 0.8% by mass, based on the total amount of the electrically insulating oil composition. If the content is 0.01% by mass or more, the effect of trapping chlorine tends to be sufficiently exhibited, and if it is 1.0% by mass or less, the electric characteristics of the electrically insulating oil composition are less likely to be adversely affected. ..

本実施形態に係る電気絶縁油組成物の４０℃における動粘度は、流動性の低下による絶縁破壊電圧の低下をより効果的に抑制する観点から、好ましくは５ｍｍ２／ｓ以下であり、より好ましくは４．５ｍｍ２／ｓ以下であり、更に好ましくは４ｍｍ２／ｓ以下である。電気絶縁油組成物の４０℃における動粘度は、臭気又は引火点の低下を効果的に抑制する観点から、２．５ｍｍ２／ｓ以上であることが好ましい。本明細書における動粘度は、ＪＩＳ Ｋ ２２８３に準拠して測定される動粘度を意味する。 The kinematic viscosity of the electrically insulating oil composition according to the present embodiment at 40 ° C. is preferably 5 mm 2 / s or less, more preferably, from the viewpoint of more effectively suppressing the decrease in the dielectric breakdown voltage due to the decrease in fluidity. Is 4.5 mm 2 / s or less, more preferably 4 mm 2 / s or less. The kinematic viscosity of the electrically insulating oil composition at 40 ° C. is preferably 2.5 mm 2 / s or more from the viewpoint of effectively suppressing the decrease in odor or flash point. The kinematic viscosity in the present specification means the kinematic viscosity measured according to JIS K 2283.

本実施形態に係る電気絶縁油組成物は、油含浸電気機器に好適に用いられ、特にプラスチックフィルムを絶縁材料又は誘電体材料の少なくとも一部に使用した油含浸コンデンサに含浸させるために好適に用いられる。 The electrically insulating oil composition according to the present embodiment is suitably used for oil-impregnated electrical equipment, and particularly preferably used for impregnating an oil-impregnated capacitor used for at least a part of an insulating material or a dielectric material with a plastic film. Be done.

プラスチックフィルムとしては、ポリエステルフィルム、ポリフッ化ビニリデンフィルム等の他、ポリプロピレンフィルム、ポリエチレンフィルム等のポリオレフィンフィルムなどを用いることができるが、それらの中でもポリオレフィンフィルムが好適である。特に好適なポリオレフィンフィルムは、ポリプロピレンフィルムである。 As the plastic film, polyester film, polyvinylidene fluoride film and the like, as well as polyolefin films such as polypropylene film and polyethylene film can be used, and among them, the polyolefin film is preferable. A particularly suitable polyolefin film is a polypropylene film.

本実施形態において好適な油含浸コンデンサは、導体としてアルミニウム等の金属箔と、上記絶縁材料又は誘電体材料としてのプラスチックフィルムとを、必要に応じて絶縁紙等の他の材料とともに巻回し、常法により電気絶縁油組成物を含浸させることにより製造される。あるいは、油含浸コンデンサは、上記絶縁材料又は誘電体材料としてのプラスチックフィルム上に、アルミニウム、亜鉛等の導体としての金属箔を蒸着などの方法により形成した金属蒸着プラスチックフィルム（メタライズド・フィルム）を、必要に応じてプラスチックフィルム又は絶縁紙とともに巻回し、常法により電気絶縁油組成物を含浸させることによっても製造される。 In the oil-impregnated capacitor suitable for this embodiment, a metal foil such as aluminum as a conductor and a plastic film as an insulating material or a dielectric material are wound together with other materials such as insulating paper as necessary. Manufactured by impregnating an electrically insulating oil composition by the method. Alternatively, the oil-impregnated capacitor is a metal-deposited plastic film (metallized film) in which a metal foil as a conductor such as aluminum or zinc is formed on a plastic film as an insulating material or a dielectric material by a method such as vapor deposition. It is also produced by winding it with a plastic film or insulating paper, if necessary, and impregnating it with an electrically insulating oil composition by a conventional method.

以上、本実施形態に係る電気絶縁油組成物について説明したが、本発明は、上記実施形態に何ら限定されることはない。例えば、本実施形態に係る各成分を含む組成物は、電気絶縁油としてだけでなく、溶剤、洗浄剤等としても用いることができる。 Although the electrically insulating oil composition according to the present embodiment has been described above, the present invention is not limited to the above embodiment. For example, the composition containing each component according to the present embodiment can be used not only as an electrically insulating oil but also as a solvent, a cleaning agent and the like.

以下、実施例により本発明を更に具体的に説明するが、本発明はこれらの実施例に限定されるものではない。 Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to these Examples.

［調製例１：触媒の調製］
硫酸アルミニウム、硫酸、ｎ－プロピルアミン、ｎ－プロピルブロマイドを水に溶解させ、この溶液に水ガラスを撹拌しながら徐々に加え、できるだけ均一なゲル状スラリーを調製した。これをオートクレーブに入れ、撹拌しながら１６０℃で７２時間かけて結晶化させた。結晶を濾別し、水洗液が中性になるまで水洗及び濾過を繰り返すことにより、ＳｉＯ２／Ａｌ２Ｏ３モル比が７０のゼオライトＺＳＭ－５を得た。得られたゼオライトを空気中で焼成することにより触媒を調製した。 [Preparation Example 1: Preparation of catalyst]
Aluminum sulfate, sulfuric acid, n-propylamine, and n-propyl bromide were dissolved in water, and water glass was gradually added to this solution with stirring to prepare a gel-like slurry as uniform as possible. This was placed in an autoclave and crystallized at 160 ° C. for 72 hours with stirring. The crystals were separated by filtration, and washing and filtration were repeated until the washing liquid became neutral to obtain a zeolite ZSM-5 having a SiO 2 / Al 2 O 3 molar ratio of 70. A catalyst was prepared by calcining the obtained zeolite in air.

［調製例２：（エチルフェニル）フェニルメタン（ＥＤＰＭ）の調製］
上記調製例１で得られたゼオライトＺＳＭ－５を塩酸でイオン交換させることにより水素型に変換した水素型ＺＳＭ－５（１２～１４メッシュ）２００ｍｌを、内容積２５０ｍｌの反応容器に充填し、乾燥窒素を送りながら４８０℃で３時間乾燥した。 [Preparation Example 2: Preparation of (Ethylphenyl) Phenylmethane (EDPM)]
200 ml of hydrogen type ZSM-5 (12 to 14 mesh) converted into hydrogen type by ion exchange of zeolite ZSM-5 obtained in Preparation Example 1 with hydrochloric acid is filled in a reaction vessel having an internal volume of 250 ml and dried. It was dried at 480 ° C. for 3 hours while feeding nitrogen.

反応温度２７０℃、圧力２０気圧（窒素雰囲気下）、ＬＨＳＶ＝１．０にて、エチルベンゼン及びジフェニルメタンの混合液（モル比；エチルベンゼン：ジフェニルメタン＝２：１）を通油し、通油された反応液を蒸留することにより、ＥＤＰＭの含有量が８５質量％である混合物を得た。なお、当該混合物には他の成分として、ビス（エチルフェニル）メタン及び（ジエチルフェニル）フェニルメタン（ＤＥＤＰＭ）が含まれていた（合計含有量：１５質量％）。 Reaction by passing oil through a mixture of ethylbenzene and diphenylmethane (molar ratio; ethylbenzene: diphenylmethane = 2: 1) at a reaction temperature of 270 ° C., a pressure of 20 atm (under a nitrogen atmosphere), and LHSV = 1.0. By distilling the liquid, a mixture having an EDPM content of 85% by mass was obtained. The mixture contained bis (ethylphenyl) methane and (diethylphenyl) phenylmethane (DEDPM) as other components (total content: 15% by mass).

［調製例３：１－エチルフェニル－１－フェニルエタン（１，１－ＥＤＰＥ）の調製］
ジフェニルメタンの代わりに、１，１－ジフェニルエタンを用いた以外は、調製例２と同様の操作を行い、１，１－ＥＤＰＥの含有量が８６質量％である混合物を得た。なお、当該混合物には他の成分として、１，１－ビス（エチルフェニル）エタン及び１－ジエチルフェニル－１－フェニルエタン（１，１－ＤＥＤＰＥ）が含まれていた（合計含有量：１４質量％）。 [Preparation Example 3: Preparation of 1-Ethylphenyl-1-phenylethane (1,1-EDPE)]
The same operation as in Preparation Example 2 was carried out except that 1,1-diphenylethane was used instead of diphenylmethane to obtain a mixture having a content of 1,1-EDPE of 86% by mass. The mixture contained 1,1-bis (ethylphenyl) ethane and 1-diethylphenyl-1-phenylethane (1,1-DEDPE) as other components (total content: 14 mass). %).

［調製例４：１－エチルフェニル－２－フェニルエタン（１，２－ＥＤＰＥ）の調製］
ジフェニルメタンの代わりに、１，２－ジフェニルエタンを用いた以外は、調製例２と同様の操作を行い、１，２－ＥＤＰＥを得た。 [Preparation Example 4: Preparation of 1-Ethylphenyl-2-phenylethane (1,2-EDPE)]
The same operation as in Preparation Example 2 was carried out except that 1,2-diphenylethane was used instead of diphenylmethane to obtain 1,2-EDPE.

（実施例１）
上記調製例２～４で得られた各成分を混合し、表１に示す組成を有する電気絶縁油組成物を調製した。実施例１の電気絶縁油組成物の組成及び４０℃における動粘度を表１に示す。 (Example 1)
Each component obtained in Preparation Examples 2 to 4 was mixed to prepare an electrically insulating oil composition having the composition shown in Table 1. Table 1 shows the composition of the electrically insulating oil composition of Example 1 and the kinematic viscosity at 40 ° C.

（比較例１）
特開昭５３－１３５９５９号公報に記載の方法に従ってスチレンと混合キシレンとのアラルキル化を行い、１，１－ＥＤＰＥの含有量が３０質量％であり、１－フェニル－１－キシリルエタン（ＰＸＥ）の含有量が７０質量％である電気絶縁油組成物を得た。比較例１の電気絶縁油組成物の組成及び４０℃における動粘度を表１に示す。 (Comparative Example 1)
Aralkylation of styrene and mixed xylene was carried out according to the method described in JP-A-53-135959, and the content of 1,1-EDPE was 30% by mass, and that of 1-phenyl-1-xylene ethane (PXE). An electrically insulating oil composition having a content of 70% by mass was obtained. Table 1 shows the composition of the electrically insulating oil composition of Comparative Example 1 and the kinematic viscosity at 40 ° C.

＜モデルコンデンサによる試験油（電気絶縁油組成物）の評価＞
試験に用いたコンデンサは次のとおりである。固体絶縁体として、チューブラー法で得られた厚み１２．７μｍ（重量法）の信越フィルム（株）製の易含浸タイプ同時二軸延伸ポリプロピレンフィルムを使用し、電極としてアルミニウム箔を使用した。また、誘電体としては、厚み１２．７μｍ（重量法）の信越フィルム（株）製のインフレーション法ポリプロピレンフィルムを２枚重ねたものを使用した。これらを常法に従って、巻回、積層することにより、油含浸用のモデルコンデンサ素子を作製した。 <Evaluation of test oil (electrically insulating oil composition) using a model capacitor>
The capacitors used in the test are as follows. As a solid insulator, an easily impregnated type simultaneous biaxially stretched polypropylene film manufactured by Shin-Etsu Film Co., Ltd. with a thickness of 12.7 μm (weight method) obtained by the tubular method was used, and an aluminum foil was used as an electrode. As the dielectric, two inflation polypropylene films manufactured by Shin-Etsu Film Co., Ltd. with a thickness of 12.7 μm (weight method) were stacked. A model capacitor element for oil impregnation was manufactured by winding and laminating these according to a conventional method.

この素子は０．２～０．３μＦの静電容量を有している。この素子をブリキ製の缶に入れた。缶は絶縁体が低温で収縮したときに充分に対応できるように柔軟な構造にした。また、電極の端部はスリットしたままで折り曲げていない状態とした。電極から端子までを結線する方法として、高周波用コンデンサに用いられる方法と同じく、電極の一端をそれぞれポリプロピレンフィルムからはみ出した構造で巻き、はみ出した部分をまとめてリード線とスポット溶接する構造にした。 This device has a capacitance of 0.2 to 0.3 μF. This element was placed in a tin can. The can has a flexible structure so that it can sufficiently cope with the shrinkage of the insulator at low temperature. In addition, the end of the electrode was left in a slit state and not bent. As a method of connecting from the electrode to the terminal, as in the method used for the high frequency capacitor, one end of the electrode is wound with a structure protruding from the polypropylene film, and the protruding part is collectively spot welded to the lead wire.

このようにして準備した缶型コンデンサを、常法に従って真空乾燥した後、同じ真空下で試験油（実施例１及び比較例１で得られた各電気絶縁油組成物）を含浸し、封口した。なお、含浸にあたっては各試験油を予め活性白土で処理してから用いた。すなわち、水澤化学工業（株）製の活性白土ガレオナイト＃０３６を試験油に１０質量％添加し、液温２５℃で３０分間撹拌した後、濾過した。濾過後、塩素捕獲剤としてエポキシ化合物（脂環式エポキシ化合物、商品名：セロキサイド２０２１Ｐ、ダイセル化学工業（株）製）を、電気絶縁油組成物全量を基準として０．６５質量％となるように添加し、得られた電気絶縁油組成物を試験油として、含浸に用いた。 The can-type capacitor thus prepared was vacuum-dried according to a conventional method, impregnated with test oil (each electric insulating oil composition obtained in Example 1 and Comparative Example 1) under the same vacuum, and sealed. .. For impregnation, each test oil was treated with activated clay in advance before use. That is, 10% by mass of activated clay galeonite # 036 manufactured by Mizusawa Industrial Chemicals Co., Ltd. was added to the test oil, and the mixture was stirred at a liquid temperature of 25 ° C. for 30 minutes and then filtered. After filtration, an epoxy compound (alicyclic epoxy compound, trade name: seroxide 2021P, manufactured by Daicel Chemical Industry Co., Ltd.) as a chlorine trapping agent is added to 0.65% by mass based on the total amount of the electrically insulating oil composition. The electric insulating oil composition obtained after addition was used as a test oil for impregnation.

次に、コンデンサ内部での含浸状況を均一にして安定化するために、恒温槽中、８０℃で２昼夜熱処理を施した。その後、コンデンサを室温で５日間静置した後、ＡＣ１２７０Ｖ（５０Ｖ／μｍに相当）にて３０℃の恒温槽で１６時間課電処理をした後に試験に供した。これを予備課電と称する。 Next, in order to make the impregnation state inside the capacitor uniform and stable, heat treatment was performed at 80 ° C. for two days and nights in a constant temperature bath. Then, the capacitor was allowed to stand at room temperature for 5 days, and then subjected to a power charge treatment at a constant temperature bath of 30 ° C. at AC1270V (corresponding to 50V / μm) for 16 hours before being subjected to the test. This is called a preliminary power charge.

次に、これら油含浸コンデンサを所定の温度下で所定の課電方法で交流電圧を課電して、コンデンサが絶縁破壊を起こした電圧と時間から下記式（１）により絶縁破壊電圧を求めた。なお、所定の温度は、－５０℃、－３０℃、３０℃及び８０℃とした。所定の課電方法とは、電位傾度５０ｖ／μｍから、２４時間ごとに１０ｖ／μｍの割合で段階的に課電電圧を上昇させる方法である。結果を表１に示す。 Next, the AC voltage was applied to these oil-impregnated capacitors under a predetermined temperature by a predetermined charging method, and the dielectric breakdown voltage was obtained from the voltage and time at which the capacitor caused dielectric breakdown by the following equation (1). .. The predetermined temperatures were −50 ° C., −30 ° C., 30 ° C. and 80 ° C. The predetermined charging method is a method in which the charging voltage is gradually increased from a potential gradient of 50 v / μm at a rate of 10 v / μm every 24 hours. The results are shown in Table 1.

絶縁破壊電圧（ｖ／μｍ）＝Ｖ＋ｓ×（Ｔ／１４４０） ・・・（１） Dielectric breakdown voltage (v / μm) = V + s × (T / 1440) ・ ・ ・ (1)

式（１）中、Ｖは絶縁破壊時の課電電圧（ｖ／μｍ）を、Ｓは２４時間ごとの上昇電圧（ｖ／μｍ）を、Ｔは課電電圧上昇後、絶縁破壊までの経過時間（分）をそれぞれ示す。 In the formula (1), V is the charging voltage (v / μm) at the time of dielectric breakdown, S is the rising voltage (v / μm) every 24 hours, and T is the progress from the rising voltage to the dielectric breakdown. Shows the hours (minutes) respectively.

Figure 0007068043000001
Figure 0007068043000001

Claims (6)

（エチルフェニル）フェニルメタンと、１－エチルフェニル－１－フェニルエタンと、１－エチルフェニル－２－フェニルエタンと、を含む電気絶縁油組成物。 (Ethylphenyl) An electrically insulating oil composition containing phenylmethane, 1-ethylphenyl-1-phenylethane, and 1-ethylphenyl-2-phenylethane. ビス（エチルフェニル）メタン及び（ジエチルフェニル）フェニルメタンを更に含む、請求項１に記載の電気絶縁油組成物。 The electrically insulating oil composition according to claim 1, further comprising bis (ethylphenyl) methane and (diethylphenyl) phenylmethane. １，１－ビス（エチルフェニル）エタン及び１－ジエチルフェニル－１－フェニルエタンを更に含む、請求項１又は２に記載の電気絶縁油組成物。 The electrically insulating oil composition according to claim 1 or 2, further comprising 1,1-bis (ethylphenyl) ethane and 1-diethylphenyl-1-phenylethane. 前記（エチルフェニル）フェニルメタンの含有量が、電気絶縁油組成物全量を基準として１０～３５質量％であり、前記１－エチルフェニル－１－フェニルエタンの含有量が、電気絶縁油組成物全量を基準として、２０～６０質量％であり、前記１－エチルフェニル－２－フェニルエタンの含有量が、電気絶縁油組成物全量を基準として、５～３０質量％である、請求項１～３のいずれか一項に記載の電気絶縁油組成物。 The content of the (ethylphenyl) phenylmethane is 10 to 35% by mass based on the total amount of the electric insulating oil composition, and the content of the 1-ethylphenyl-1-phenylethane is the total amount of the electric insulating oil composition. 1 to 60% by mass, and the content of 1-ethylphenyl-2-phenylethane is 5 to 30% by mass based on the total amount of the electrically insulating oil composition. The electrically insulating oil composition according to any one of the above. エポキシ化合物を、電気絶縁油組成物全量を基準として０．０１～１．０質量％含む、請求項１～４のいずれか一項に記載の電気絶縁油組成物。 The electric insulating oil composition according to any one of claims 1 to 4, which contains an epoxy compound in an amount of 0.01 to 1.0% by mass based on the total amount of the electric insulating oil composition. ４０℃における動粘度が５ｍｍ２／ｓ以下である、請求項１～５のいずれか一項に記載の電気絶縁油組成物。 The electrically insulating oil composition according to any one of claims 1 to 5, wherein the kinematic viscosity at 40 ° C. is 5 mm 2 / s or less.
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JP2002265967A (en) 2000-12-20 2002-09-18 Toshiba Corp Insulating oil in which x-ray tube is immersed, and x-ray tube device
JP2002363585A (en) 2001-06-06 2002-12-18 Idemitsu Kosan Co Ltd Lubricating oil base oil composition

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JP2002265967A (en) 2000-12-20 2002-09-18 Toshiba Corp Insulating oil in which x-ray tube is immersed, and x-ray tube device
JP2002363585A (en) 2001-06-06 2002-12-18 Idemitsu Kosan Co Ltd Lubricating oil base oil composition

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