JP2002121359A - Epoxy resin composition and electronic parts of high- pressure electricity using the same - Google Patents
Epoxy resin composition and electronic parts of high- pressure electricity using the sameInfo
- Publication number
- JP2002121359A JP2002121359A JP2000315939A JP2000315939A JP2002121359A JP 2002121359 A JP2002121359 A JP 2002121359A JP 2000315939 A JP2000315939 A JP 2000315939A JP 2000315939 A JP2000315939 A JP 2000315939A JP 2002121359 A JP2002121359 A JP 2002121359A
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- resin composition
- agent
- curing
- electronic parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
- Organic Insulating Materials (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、電気機器の充填用
樹脂として有用なエポキシ樹脂組成物及びこれを用いた
高圧電気電子部品に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an epoxy resin composition useful as a resin for filling electric equipment and a high-voltage electric / electronic component using the same.
【０００２】[0002]
【従来の技術】従来、高圧電気電子部品の製造法として
は、ケース又は金型内に部品をセットし、エポキシ樹脂
と無機充填剤との均一混合物に酸無水物及びその硬化促
進剤を混合したエポキシ樹脂組成物を常圧又は真空下で
注入して硬化させるポッティング法が知られている。2. Description of the Related Art Conventionally, as a method of manufacturing a high-voltage electric / electronic component, a component is set in a case or a mold, and an acid anhydride and a curing accelerator thereof are mixed in a homogeneous mixture of an epoxy resin and an inorganic filler. A potting method of injecting and curing an epoxy resin composition under normal pressure or under vacuum is known.
【０００３】しかし、この方法ではエポキシ樹脂そのも
のが高粘稠であるため混合する無機充填剤の量に限界が
あり、硬化する際にエポキシ樹脂組成物に体積収縮が生
じるため、硬化物にクラックが生じ、内蔵されているコ
イル及び部品やケースに剥離やクラックが発生し易く、
また、熱伝導率が悪いために電気機器の温度が高くな
り、使用する温度が制限されるなどの問題がある。さら
に、エポキシ樹脂組成物と無機充填剤を混合して減圧下
で脱泡した後に注入し作業を行うため、エポキシ樹脂組
成物の硬化時間の長いものを使用する必要があり、注入
後の硬化時間も長くなり、作業工程の合理化、省エネル
ギー化に限界がある。However, in this method, the amount of the inorganic filler to be mixed is limited because the epoxy resin itself is highly viscous, and the epoxy resin composition undergoes volume shrinkage upon curing, so that the cured product has cracks. Peeling and cracking easily occur in the built-in coil and parts and case,
In addition, there is a problem that the temperature of the electric device becomes high due to poor heat conductivity, and the temperature used is limited. Furthermore, since the epoxy resin composition and the inorganic filler are mixed and defoamed under reduced pressure and then injected, the epoxy resin composition needs to have a long curing time, and the curing time after the injection is required. And there are limits to the rationalization of work processes and energy saving.
【０００４】また、これら高圧電気・電子部品の設置場
所には、その他の構成部品が多数配置されており、これ
ら構成部品のほとんどが黒色、濃紺色、又は濃黒茶色系
であることから、高圧電気・電子部品に用いるエポキシ
樹脂組成物も黒色、濃紺色、又は濃黒茶色系への着色要
求がある。[0004] In addition, many other components are arranged in the place where these high-voltage electric / electronic components are installed. Most of these components are black, dark blue or dark black-brown, so that high voltage Epoxy resin compositions used for electric / electronic parts are also required to be colored black, dark blue, or dark black brown.
【０００５】さらに、従来、エポキシ樹脂組成物の黒色
系着色に実績のあるカーボンブラック顔料は、カーボン
が導電性材料であることから、高圧電気・電子部品ユー
ザーは信頼性を向上させるため、使用を控える傾向があ
る。一方で、黒色、濃紺色、又は濃黒茶色のカーボンの
代替着色剤として考えられる。アジン結合を有する化合
物又はジアゾ結合を有する化合物は、エポキシ樹脂組成
物にしたとき、初期の発色は良いものの、１３０℃以上
の高温下で長時間熱履歴を受けると色抜けが目立ち、黒
色、濃紺色、又は濃黒茶色を保持することができない。[0005] Furthermore, carbon black pigments which have been used in black coloring of epoxy resin compositions have been used for high voltage electric and electronic parts since carbon is a conductive material. There is a tendency to refrain. On the other hand, it is considered as an alternative colorant for black, dark blue or dark brown carbon. A compound having an azine bond or a compound having a diazo bond has good initial coloration when formed into an epoxy resin composition, but when subjected to a long-term heat history under a high temperature of 130 ° C. or more, color loss is conspicuous, and black and dark blue Color or dark brown cannot be retained.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、上記の従来
技術の問題点を解消し、粘度が低く、注入作業性に優れ
るとともに、高温下で長時間熱履歴を受けても黒色系硬
化物の色抜けがなく、黒色、濃紺色又は濃黒茶色を保持
しうるエポキシ樹脂組成物及びこれを用いた絶縁性に優
れる高圧電気電子部品を提供するものである。DISCLOSURE OF THE INVENTION The present invention solves the above-mentioned problems of the prior art, has a low viscosity, is excellent in injection workability, and has a black-based cured product even when subjected to a long-term heat history at a high temperature. The present invention provides an epoxy resin composition capable of retaining black, dark blue or dark black brown without color loss, and a high-voltage electric / electronic component using the epoxy resin composition and having excellent insulation properties.
【０００７】[0007]
【課題を解決するための手段】本発明は、酸無水物に無
機充填剤及び硬化促進剤を配合した組成物をＡ剤、エポ
キシ樹脂をＢ剤とする酸無水物硬化型エポキシ樹脂組成
物であって、Ｂ剤に縮合アゾ構造の有機顔料及びジアゾ
系染料を配合したことを特徴とするエポキシ樹脂組成物
に関する。また本発明は、前記エポキシ樹脂組成物を注
入し、硬化させてなる高圧電気電子部品に関する。The present invention relates to an acid anhydride-curable epoxy resin composition comprising a composition obtained by mixing an inorganic anhydride and a curing accelerator with an acid anhydride, and a composition comprising an A agent and an epoxy resin as a B agent. In addition, the present invention relates to an epoxy resin composition characterized in that an organic pigment having a condensed azo structure and a diazo-based dye are blended with the agent B. The present invention also relates to a high-voltage electric / electronic component obtained by injecting and curing the epoxy resin composition.
【０００８】[0008]
【発明の実施の形態】本発明のエポキシ樹脂組成物にお
いて、前記のように、Ａ剤は、酸無水物に無機充填剤及
び硬化促進剤を配合した組成物である。使用しうる酸無
水物としては、特に制限はないが、常温で液体のものが
好ましく、例えば、メチルテトラヒドロ無水フタル酸、
メチルヘキサヒドロ無水フタル酸、メチルエンドメチレ
ン無水フタル酸、ドデセニル無水フタル酸などが用いら
れる。市販品としては、ＨＮ−２２００（日立化成工業
(株)製商品名）、ＱＨ−２００（日本ゼオン(株)製商品
名）などが挙げられる。これらは単独で又は２種以上組
み合わせて用いることもできる。BEST MODE FOR CARRYING OUT THE INVENTION In the epoxy resin composition of the present invention, as described above, the agent A is a composition in which an inorganic filler and a curing accelerator are mixed with an acid anhydride. The acid anhydride that can be used is not particularly limited, but is preferably a liquid at room temperature, for example, methyltetrahydrophthalic anhydride,
Methylhexahydrophthalic anhydride, methylendomethylene phthalic anhydride, dodecenyl phthalic anhydride and the like are used. As a commercially available product, HN-2200 (Hitachi Chemical Industries, Ltd.)
(Trade name, manufactured by Nippon Zeon Co., Ltd.) and the like. These can be used alone or in combination of two or more.
【０００９】酸無水物の硬化促進剤としては、例えば２
−エチル−４−メチルイミダゾール、１−シアノエチル
−４−メチルイミダゾール、１−ベンジル−２−エチル
イミダゾール等のイミダゾール及びその誘導体、トリス
ジメチルアミノフェノール、ベンジルジメチルアミン等
の第３級アミン類などが用いられる。市販品としては２
Ｅ４ＭＺ（四国化成工業(株)製商品名）、ＢＤＭＡ（花
王(株)製商品名）などが挙げられる。硬化促進剤は、単
独で又は２種類以上を組み合わせて用いられる。これら
の硬化促進剤の配合量は、酸無水物１００重量部当たり
０．１〜１０重量部が反応性の点で好ましく、０．１〜
５重量部がより好ましく、０．１〜３重量部が特に好ま
しい。As a curing accelerator for acid anhydrides, for example, 2
Imidazole and derivatives thereof such as -ethyl-4-methylimidazole, 1-cyanoethyl-4-methylimidazole and 1-benzyl-2-ethylimidazole, and tertiary amines such as trisdimethylaminophenol and benzyldimethylamine are used. Can be 2 for commercial products
E4MZ (trade name, manufactured by Shikoku Kasei Kogyo Co., Ltd.), BDMA (trade name, manufactured by Kao Corporation) and the like can be mentioned. The curing accelerator is used alone or in combination of two or more. The compounding amount of these curing accelerators is preferably from 0.1 to 10 parts by weight per 100 parts by weight of acid anhydride in view of reactivity, and from 0.1 to 10 parts by weight.
5 parts by weight is more preferable, and 0.1 to 3 parts by weight is particularly preferable.
【００１０】無機充填剤としては、例えば、結晶シリ
カ、溶融シリカ、水和アルミナ、酸化アルミナ、タル
ク、炭酸カルシウム、ガラスビーズ、クレー、酸化マグ
ネシウムなどが用いられる。この市販品としては、ＣＲ
Ｔ−ＡＡ、ＣＲＴ−Ｄ、ＲＤ−８（(株)龍森製商品
名）、ＣＯＸ−３１（(株)マイクロ製商品名）、Ｃ−３
０３Ｈ、Ｃ−３１５Ｈ、Ｃ−３０８（住友化学工業(株)
製商品名）、ＳＬ−７００（竹原化学工業(株)製商品
名）などが挙げられる。これらの無機充填剤は、単独で
又は２種類以上を組み合わせて用いられる。As the inorganic filler, for example, crystalline silica, fused silica, hydrated alumina, alumina oxide, talc, calcium carbonate, glass beads, clay, magnesium oxide and the like are used. As this commercial product, CR
T-AA, CRT-D, RD-8 (trade name, manufactured by Tatsumori Co., Ltd.), COX-31 (trade name, manufactured by Micro Co., Ltd.), C-3
03H, C-315H, C-308 (Sumitomo Chemical Industries, Ltd.)
Trade name), SL-700 (trade name, manufactured by Takehara Chemical Industry Co., Ltd.) and the like. These inorganic fillers are used alone or in combination of two or more.
【００１１】無機充填剤の配合量は、酸無水物１００重
量部に対して５０〜５００重量部が好ましく、８０〜４
００重量部がさらに好ましく、１００〜３００重量部が
より好ましい。無機充填剤が少なすぎると、硬化物にし
た時の熱伝導率又は線膨張係数に悪影響を及ぼし、無機
充填剤が多すぎると注入作業性に劣る傾向がある。The amount of the inorganic filler is preferably from 50 to 500 parts by weight, more preferably from 80 to 4 parts by weight, per 100 parts by weight of the acid anhydride.
00 parts by weight is more preferable, and 100 to 300 parts by weight is more preferable. If the amount of the inorganic filler is too small, the thermal conductivity or the coefficient of linear expansion of the cured product is adversely affected, and if the amount of the inorganic filler is too large, the injection workability tends to be poor.
【００１２】また、本発明のエポキシ樹脂組成物におけ
るＢ剤は、エポキシ樹脂を必須成分として含有するもの
である。本発明に使用しうるエポキシ樹脂としては、１
分子中に少なくとも２個のエポキシ基を有する化合物が
用いられるが、エポキシ当量が１００〜４０００のもの
が好ましく、エポキシ当量が１５０〜１０００のものが
より好ましく、特に、エポキシ当量が１７０〜５００の
ものが好ましい。The B agent in the epoxy resin composition of the present invention contains an epoxy resin as an essential component. Epoxy resins that can be used in the present invention include:
Although a compound having at least two epoxy groups in the molecule is used, those having an epoxy equivalent of 100 to 4000 are preferable, those having an epoxy equivalent of 150 to 1000 are more preferable, and those having an epoxy equivalent of 170 to 500 are particularly preferable. Is preferred.
【００１３】使用しうるエポキシ樹脂としては、具体的
には例えば、ビスフェノールＡ型エポキシ樹脂、ビスフ
ェノールＦ型エポキシ樹脂、ビスフェノールＡＤ型エポ
キシ樹脂、多価アルコールのポリグリシジルエーテルな
どが用いられる。これらの樹脂としては、特に制限はな
いが、常温で液状のものが好ましく、市販品としてはエ
ピコート８２８（油化シェルエポキシ(株)製商品名）、
ＧＹ−２６０（チバガイギ社製商品名）、ＤＥＲ−３３
１（ダウケミカル日本(株)製商品名）などが挙げられ
る。これらは単独で又は併用して用いることができる。Examples of usable epoxy resins include, for example, bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol AD type epoxy resin, polyglycidyl ether of polyhydric alcohol and the like. These resins are not particularly limited, but are preferably liquid at room temperature, and commercially available products are Epikote 828 (trade name, manufactured by Yuka Shell Epoxy Co., Ltd.),
GY-260 (trade name, manufactured by Ciba-Geigy), DER-33
1 (trade name of Dow Chemical Japan Co., Ltd.). These can be used alone or in combination.
【００１４】また、エポキシ樹脂として、ポリプロピレ
ングリコールジグリシジルエーテル、ポリエチレングリ
コールジグリシジルエーテル、ブタンジオールジグリシ
ジルエーテル等の反応性希釈剤となる低分子量エポキシ
樹脂を使用する場合には、それより高分子量のものと併
用することが好ましい。When a low molecular weight epoxy resin serving as a reactive diluent such as polypropylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether or butanediol diglycidyl ether is used as the epoxy resin, a higher molecular weight epoxy resin is used. It is preferable to use them together.
【００１５】さらに、エポキシ樹脂として、１分子中に
エポキシ基を１個だけ有するエポキシ化合物を含んでい
てもよい。このようなエポキシ化合物は、エポキシ樹脂
全量に対して０〜４０重量％の範囲で使用することが好
ましく、０〜２０重量％の範囲で使用することがより好
ましい。このようなエポキシ化合物としては、ｎ−ブチ
ルグリシジルエーテル、フェニルグリシジルエーテル、
ジブロモフェニルグリシジルエーテル、ジブロモクレジ
ルグリシジルエーテルなどがある。Further, the epoxy resin may contain an epoxy compound having only one epoxy group in one molecule. Such an epoxy compound is preferably used in the range of 0 to 40% by weight, more preferably in the range of 0 to 20% by weight, based on the total amount of the epoxy resin. Such epoxy compounds include n-butyl glycidyl ether, phenyl glycidyl ether,
Examples include dibromophenyl glycidyl ether and dibromocresyl glycidyl ether.
【００１６】これらエポキシ樹脂の配合量は、酸無水物
１００重量部に対して７０〜１００重量部であるのが好
ましく、９０〜１５０重量部がより好ましく、１００〜
１４０重量部がさらに好ましい。エポキシ樹脂が少なす
ぎても多すぎても、酸無水物とエポキシ樹脂のバランス
が崩れて、充分に硬化が進まない。The amount of the epoxy resin is preferably 70 to 100 parts by weight, more preferably 90 to 150 parts by weight, more preferably 100 to 100 parts by weight, based on 100 parts by weight of the acid anhydride.
140 parts by weight is more preferred. If the amount of the epoxy resin is too small or too large, the balance between the acid anhydride and the epoxy resin is lost, and the curing does not proceed sufficiently.
【００１７】本発明のエポキシ樹脂組成物のＢ剤は、さ
らに縮合アゾ構造を有する有機顔料及びジアゾ系染料を
含有する。The agent B of the epoxy resin composition of the present invention further contains an organic pigment having a condensed azo structure and a diazo dye.
【００１８】縮合アゾ構造を有する有機顔料とは、ビス
アゾ型の不溶性アゾ顔料であって、一般に、アゾ染料か
ら縮合反応により製造されたものをさす。本発明におい
て、縮合アゾ構造を有する有機顔料としては、茶色系の
微粉末が好ましく、中でも下記一般式（Ｉ）The organic pigment having a condensed azo structure is an insoluble azo pigment of the bisazo type, which is generally produced by a condensation reaction from an azo dye. In the present invention, as the organic pigment having the condensed azo structure, a brownish fine powder is preferable, and among them, the following general formula (I)
【化１】 の構造を有するものが好ましいものとして挙げられる。
この製品は、例えば、クロモフタールブラウン５Ｒ（チ
バ・スペシャルティ・ケミカルズ(株)製商品名）として
市販されている。Embedded image Preferred are those having the following structure:
This product is commercially available, for example, as Chromophtal Brown 5R (trade name of Ciba Specialty Chemicals Co., Ltd.).
【００１９】一方、ジアゾ系染料としては、種々の公知
のものが挙げられ、特に制限はない。この市販品として
は、例えば、オイルブラックＨＢＢ（オリエント化学工
業(株)製商品名）として市販されている。On the other hand, examples of the diazo dye include various known dyes, and there is no particular limitation. This commercially available product is, for example, commercially available as Oil Black HBB (trade name, manufactured by Orient Chemical Industries, Ltd.).
【００２０】縮合アゾ構造を有する有機顔料とジアゾ系
染料の配合比率としては、縮合アゾ構造を有する有機顔
料／ジアゾ系染料（重量比）で３０／７０〜７０／３０
の範囲で使用するのが着色の点から好ましい。縮合アゾ
構造を有する有機顔料が３０／７０より少ない場合は、
高温下で長時間熱履歴を受けるとエポキシ樹脂組成物の
色抜けが目立つ傾向があり、７０／３０より多いと、縮
合アゾ構造特有の赤色の発色が目立つことになり、いず
れの場合にも黒色又は濃黒茶色の色相を保持することが
できない。配合比率は４０／６０〜６０／４０の範囲が
より好ましく、４５／５５〜５５／４５の範囲が特に好
ましい。The mixing ratio of the organic pigment having a condensed azo structure and the diazo dye is 30/70 to 70/30 in terms of the weight ratio of the organic pigment having the condensed azo structure / diazo dye (weight ratio).
It is preferable to use in the range of from the point of coloring. When the organic pigment having a condensed azo structure is less than 30/70,
When subjected to a long-term heat history at a high temperature, the color loss of the epoxy resin composition tends to be conspicuous. Or, it cannot maintain a dark black brown hue. The mixing ratio is more preferably in the range of 40/60 to 60/40, and particularly preferably in the range of 45/55 to 55/45.
【００２１】縮合アゾ構造を有する有機顔料とジアゾ系
染料の着色剤は、エポキシ樹脂組成物全量に対して０．
１〜１０重量％の範囲で使用するのが着色の点から好ま
しく、０．１〜５重量％の範囲がより好ましく、０．２
〜３重量％の範囲が特に好ましい。The organic pigment having a condensed azo structure and the colorant of the diazo dye are used in an amount of 0.1% based on the total amount of the epoxy resin composition.
It is preferably used in the range of 1 to 10% by weight from the viewpoint of coloring, more preferably in the range of 0.1 to 5% by weight, and 0.2 to 5% by weight.
Particularly preferred is a range of ３3% by weight.
【００２２】本発明のエポキシ樹脂組成物には、さらに
必要に応じて、赤リン、ヘキサブロモベンゼン、三酸化
アンチモン等の難燃剤、シラン系カップリング剤、シリ
コーン剤等の消泡剤などを配合することができる。The epoxy resin composition of the present invention may further contain, if necessary, a flame retardant such as red phosphorus, hexabromobenzene and antimony trioxide, a silane coupling agent, and a defoaming agent such as a silicone agent. can do.
【００２３】本発明の高圧電気電子部品は、上記Ａ剤と
上記Ｂ剤を混合したエポキシ樹脂組成物を注入し、硬化
させることによって得られる。具体的には、Ａ剤及びＢ
剤を混合してエポキシ樹脂組成物とし、これを好ましく
は３０〜７０℃に予熱し、減圧下（好ましくは１３３．
３Pa（１Torr）以下）で脱泡した後、高圧電気電子部品
が搭載されたケース又は金型に注入し、好ましくは６０
〜１７０℃（特に好ましくは８０〜１６０℃）で１〜８
時間加熱硬化させることにより、また、金型を用いた場
合には硬化後金型から取り外すことにより高圧電気電子
部品が得られる。The high-voltage electric / electronic component of the present invention is obtained by injecting and curing an epoxy resin composition obtained by mixing the above-mentioned agent A and agent B. Specifically, agent A and B
The epoxy resin composition is mixed with the agent, and the epoxy resin composition is preferably preheated to 30 to 70 ° C. and reduced under reduced pressure (preferably 133.
After degassing at 3 Pa (1 Torr or less), the mixture is poured into a case or a mold on which high-voltage electrical and electronic components are mounted, and preferably 60
1 to 8 at 170 to 170 ° C (particularly preferably 80 to 160 ° C)
A high-voltage electric / electronic component can be obtained by heating and curing for a time, and, if a mold is used, by removing from the mold after curing.
【００２４】また、Ａ剤及びＢ剤をそれぞれ好ましくは
３０〜７０℃に予熱し、減圧下（好ましくは１３３．３
Pa（１Torr）以下）で脱泡した後、空気が入らないよう
に混合してエポキシ樹脂組成物とし、その後は上記のよ
うにして成形し、高圧電気電子部品を製造することがで
きる。Further, each of the agent A and the agent B is preferably preheated to 30 to 70 ° C., and is reduced under reduced pressure (preferably 133.3).
After defoaming at Pa (1 Torr or less), the mixture is mixed so that air does not enter to form an epoxy resin composition, and then molded as described above to produce a high-voltage electric / electronic component.
【００２５】本発明のエポキシ樹脂組成物を用いて絶縁
処理される高圧電気電子部品としては、例えば、プラス
チック又は金属製のケース又は金型内に部品を収納した
トランス、フライバックトランス、ネオントランス、イ
グニッションコイル又はこれらのケースレスタイプのト
ランス等が挙げられる。Examples of the high-voltage electrical and electronic parts to be insulated by using the epoxy resin composition of the present invention include, for example, transformers, flyback transformers, neon transformers, and the like which are housed in a plastic or metal case or mold. Examples include an ignition coil and a caseless type transformer thereof.
【００２６】[0026]
【実施例】次に、本発明を実施例によりさらに具体的に
説明する。Next, the present invention will be described more specifically with reference to examples.
【００２７】実施例１及び比較例１〜３ 表１に示す配合のエポキシ樹脂組成物を６０℃に加温
し、６６．６５Pa（０．５Torr）で５分間脱泡した後、
１３３３．２Pa（１０Torr）の減圧下で注入し、８０℃
で２時間、１３５℃で２時間硬化させた後、各種評価の
試験片とした。Example 1 and Comparative Examples 1 to 3 An epoxy resin composition having the composition shown in Table 1 was heated to 60 ° C. and defoamed at 66.65 Pa (0.5 Torr) for 5 minutes.
Inject under reduced pressure of 1333.2 Pa (10 Torr), 80 ° C
After curing for 2 hours at 135 ° C. for 2 hours, test pieces for various evaluations were obtained.
【００２８】なお、実施例及び比較例に用いた物質は、
下記のものである。 〔Ａ剤〕 酸無水物：メチルテトラヒドロ無水フタル酸（日立化成
工業株式会社製、商品名ＨＮ−２２００） 硬化促進剤：２−エチル−４−メチルイミダゾール（四
国化成工業株式会社製、商品名２Ｅ４ＭＺ） 充填剤：平均粒径７μｍの結晶シリカ（株式会社龍森
製、商品名ＣＲＴ−ＡＡ）The substances used in Examples and Comparative Examples were as follows:
These are: [Agent A] Acid anhydride: methyltetrahydrophthalic anhydride (HN-2200, manufactured by Hitachi Chemical Co., Ltd.) Curing accelerator: 2-ethyl-4-methylimidazole (2E4MZ, manufactured by Shikoku Chemical Industry Co., Ltd.) Filler: crystalline silica having an average particle size of 7 μm (CRT-AA, manufactured by Tatsumori Co., Ltd.)
【００２９】〔Ｂ剤〕 エポキシ樹脂：ビスフェノールＡ型ＥＰ（油化シェル株
式会社製、商品名エピコート８２８） 縮合アゾ構造を有する有機顔料：クロモフタールブラウ
ン５Ｒ（チバ・スペシャルティ・ケミカルズ株式会社
製、商品名） ジアゾ系染料：オイルブラックＨＢＢ（オリエント化学
工業株式会社製、商品名）[Agent B] Epoxy resin: bisphenol A type EP (Epicoat 828, manufactured by Yuka Shell Co., Ltd.) Organic pigment having a condensed azo structure: Chromophtal Brown 5R (manufactured by Ciba Specialty Chemicals Co., Ltd.) Product name) Diazo dye: Oil black HBB (trade name, manufactured by Orient Chemical Co., Ltd.)
【００３０】試験片の評価は、下記の方法で行った。 （１）硬化物の色相変化 表１に示す配合のエポキシ樹脂組成物硬化後の試験片
を、１５０℃の恒温槽に投入、規定時間放置後の試験片
の色相変化を目視で判断した。The test pieces were evaluated by the following methods. (1) Change in Hue of Cured Product A test piece after curing the epoxy resin composition having the composition shown in Table 1 was put into a thermostat at 150 ° C., and the hue change of the test piece after standing for a prescribed time was visually determined.
【００３１】（２）絶縁破壊の強さ ５０mm×１００mm×２mmの金型内で、ＢＤＶ測定機（明
和電機(株)製）を用いて、油槽中で試験片を直径２０mm
の球電極と直径２０mmの円板電極の間に挟んでセット
し、絶縁破壊電圧を測定し、絶縁破壊の強さを求めた。(2) Insulation Breakdown Strength In a mold of 50 mm × 100 mm × 2 mm, a test piece was cut into a diameter of 20 mm in an oil bath using a BDV measuring machine (manufactured by Meiwa Electric Co., Ltd.).
Was set between a spherical electrode and a disc electrode having a diameter of 20 mm, and the breakdown voltage was measured to determine the strength of the breakdown.
【００３２】（３）モデル含浸率 直径１５mmのポリプロピレン製試験管に１００℃で１時
間乾燥したガラスビーズ（平均粒径が８０μｍ）を振動
させながら試験管内に高さで約６０mmになるように充填
した後秤量してガラスビーズの重量（Ｗ0ｇ）を測定し
た。次いで、樹脂組成物をガラスビーズ充填済みのポリ
プロピレン製試験管に高さで約６０mmになるように注入
し、１３３３．２Pa（１０mmHg）に減圧して１０分間放
置した後、規定の条件で熱硬化させた。この後、含浸さ
れずに硬化物から分離されるガラスビーズを集めてその
重量（Ｗ1ｇ）を測定した。次の式からモデル含浸率を
算出した。(3) Model impregnation rate Glass beads (average particle size: 80 μm) dried at 100 ° C. for 1 hour were filled into a polypropylene test tube having a diameter of 15 mm while vibrating so as to have a height of about 60 mm in the test tube. After weighing, the weight (W 0 g) of the glass beads was measured. Next, the resin composition was poured into a polypropylene test tube filled with glass beads so as to have a height of about 60 mm, left under reduced pressure of 1333.2 Pa (10 mmHg) for 10 minutes, and then heat-cured under specified conditions. I let it. Thereafter, the glass beads separated from the cured product without being impregnated were collected and their weight (W 1 g) was measured. The model impregnation rate was calculated from the following equation.
【００３３】[0033]
【数１】 (Equation 1)
【００３４】[0034]
【表１】 [Table 1]
【００３５】表１に示した結果から、本発明のエポキシ
樹脂組成物を用いた場合、ジアゾ系の染料だけを用いた
場合（比較例１）とは異なり、高温下で熱履歴を受けて
も試験片の色抜けがなく、また、縮合アゾ構造を有する
有機顔料だけを用いた場合（比較例２）とも異なり、試
験片の色相を濃黒茶色に着色できることがわかった。From the results shown in Table 1, when the epoxy resin composition of the present invention was used, unlike the case where only the diazo dye was used (Comparative Example 1), even when the epoxy resin composition was subjected to heat history at a high temperature. It was found that there was no color loss of the test piece and that the hue of the test piece could be colored dark black brown unlike the case where only an organic pigment having a condensed azo structure was used (Comparative Example 2).
【００３６】また、本発明のエポキシ樹脂組成物を用い
た場合には、絶縁破壊の強さにおいても高い値を示すこ
とから、比較例３に示す従来技術の無着色品エポキシ樹
脂組成物と同等の特性が得られることがわかった。さら
に、縮合アゾ構造を有する有機顔料及びジアゾ系染料を
配合した本発明のエポキシ樹脂組成物を用いた場合、着
色も濃黒茶色の色相となり、その他の構成部品と同様の
色相になり、高圧電気電子部品ユーザーの要求を満たす
ことができる。Further, when the epoxy resin composition of the present invention was used, a high value was also obtained in the dielectric breakdown strength, so that it was equivalent to the non-colored epoxy resin composition of the prior art shown in Comparative Example 3. It turned out that the characteristic of was obtained. Further, when the epoxy resin composition of the present invention containing an organic pigment having a condensed azo structure and a diazo-based dye is used, the coloring also becomes a dark black-brown hue, and the same hue as the other constituent parts. It can meet the demands of electronic components users.
【００３７】[0037]
【発明の効果】本発明のエポキシ樹脂組成物は、粘度が
低く注入作業性に優れるとともに、高い絶縁性を有し、
高温下で長時間熱履歴を受けても黒色系硬化物の色抜け
がなく、黒色又は濃黒茶色を保持しうる黒色又は濃黒茶
系の高圧電気電子部品を提供することができる。EFFECT OF THE INVENTION The epoxy resin composition of the present invention has a low viscosity and excellent workability for injection, and has high insulation properties.
It is possible to provide a black or dark black brown high-voltage electrical / electronic component that does not lose color of a black cured product even when subjected to a heat history for a long time at a high temperature and can maintain black or dark black brown.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｈ０１Ｌ 23/29 Ｈ０１Ｌ 23/30 Ｒ 23/31 Ｆターム(参考） 4J002 CD031 CD051 EQ016 FD010 GQ00 GQ01 4J036 AA01 AD01 AD08 DA04 DA05 DB15 DC02 DC05 DC40 DC41 JA07 KA01 4M109 AA01 BA01 CA02 DB09 EA02 EB02 EB04 EB08 EB12 EC07 EC20 5G305 AA13 AB36 AB40 BA09 CA15 CB13 CB15 CD08 CD20 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI theme coat ゛ (Reference) H01L 23/29 H01L 23/30 R 23/31 F-term (Reference) 4J002 CD031 CD051 EQ016 FD010 GQ00 GQ01 4J036 AA01 AD01 AD08 DA04 DA05 DB15 DC02 DC05 DC40 DC41 JA07 KA01 4M109 AA01 BA01 CA02 DB09 EA02 EB02 EB04 EB08 EB12 EC07 EC20 5G305 AA13 AB36 AB40 BA09 CA15 CB13 CB15 CD08 CD20
Claims (2)
配合した組成物をＡ剤、エポキシ樹脂をＢ剤とする酸無
水物硬化型エポキシ樹脂組成物であって、Ｂ剤に縮合ア
ゾ構造を有する有機顔料及びジアゾ系染料を配合したこ
とを特徴とするエポキシ樹脂組成物。1. An acid anhydride-curable epoxy resin composition comprising a composition prepared by mixing an inorganic anhydride and a curing accelerator with an acid anhydride, and an epoxy resin composition comprising an epoxy resin as a B agent. An epoxy resin composition comprising an organic pigment having a structure and a diazo dye.
入し、硬化させてなる高圧電気電子部品。2. A high-voltage electric / electronic component obtained by injecting and curing the epoxy resin composition according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000315939A JP2002121359A (en) | 2000-10-16 | 2000-10-16 | Epoxy resin composition and electronic parts of high- pressure electricity using the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000315939A JP2002121359A (en) | 2000-10-16 | 2000-10-16 | Epoxy resin composition and electronic parts of high- pressure electricity using the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2002121359A true JP2002121359A (en) | 2002-04-23 |
Family
ID=18794962
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000315939A Pending JP2002121359A (en) | 2000-10-16 | 2000-10-16 | Epoxy resin composition and electronic parts of high- pressure electricity using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2002121359A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012223063A (en) * | 2011-04-14 | 2012-11-12 | Nikkiso Co Ltd | Canned motor pump and method for filling stator chamber of the canned motor pump with filler |
| CN110272522A (en) * | 2019-06-04 | 2019-09-24 | 东莞爱的合成材料科技有限公司 | A kind of photosensitive resin material |
-
2000
- 2000-10-16 JP JP2000315939A patent/JP2002121359A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012223063A (en) * | 2011-04-14 | 2012-11-12 | Nikkiso Co Ltd | Canned motor pump and method for filling stator chamber of the canned motor pump with filler |
| US8729756B2 (en) | 2011-04-14 | 2014-05-20 | Nikkiso Co., Ltd. | Canned motor pump and method for filling filling member into stator chamber thereof |
| CN110272522A (en) * | 2019-06-04 | 2019-09-24 | 东莞爱的合成材料科技有限公司 | A kind of photosensitive resin material |
| CN110272522B (en) * | 2019-06-04 | 2022-08-16 | 东莞爱的合成材料科技有限公司 | Photosensitive resin material |
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