JP2016060898A - Two-pack casting epoxy resin composition, and coil component - Google Patents
Two-pack casting epoxy resin composition, and coil component Download PDFInfo
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Abstract
Description
本発明は、２液性注型用エポキシ樹脂組成物、及びコイル部品に関する。 The present invention relates to a two-component casting epoxy resin composition and a coil component.
電気・電子部品等のコイルには周囲に対して電気的絶縁性を確保しなければならないという観点から、樹脂組成物で注型封止して用いるのが常識となっている。このような樹脂組成物に対しては、高含浸性、高絶縁性が要求され、上記観点から従来エポキシ樹脂組成物が汎用されている。
しかしながら、自動車等の各種機器に使用されるコイル、特にイグニッションコイルは高電圧が印加されるため、単に通常のエポキシ樹脂組成物を用いたのみでは、絶縁性が不十分であって絶縁破壊等が生じたり、封止樹脂硬化物の熱サイクルに起因した応力によって、封止樹脂にクラックが生じたりしてしまう場合があった。封止樹脂にクラックが生じると、コイルに電流を流した際に、前記クラック部分で異常放電等が発生することになり、上記コイル部品を正常に動作させることができない。加えて、近年のイグニッションコイルにおいては、使用環境温度が上昇し、１５０℃条件下での絶縁破壊強度が必須となっている。
It is common knowledge that coils such as electric and electronic parts are cast and sealed with a resin composition from the viewpoint of ensuring electrical insulation with respect to the surroundings. For such a resin composition, high impregnation properties and high insulation properties are required, and conventionally epoxy resin compositions have been widely used from the above viewpoint.
However, since a high voltage is applied to coils used in various devices such as automobiles, in particular, ignition coils, simply using a normal epoxy resin composition results in insufficient insulation and dielectric breakdown. In some cases, the sealing resin may be cracked due to the stress generated due to the thermal cycle of the cured sealing resin. If a crack occurs in the sealing resin, when a current is passed through the coil, abnormal discharge or the like occurs in the crack portion, and the coil component cannot be operated normally. In addition, in recent ignition coils, the operating environment temperature rises, and the dielectric breakdown strength under the condition of 150 ° C. is essential.
このような問題に鑑み、無機充填材を含有することにより、検討がなされている。特許文献１においては、エポキシ樹脂組成物に対して特定範囲の粒径からなるシリカ粒子を所定量含有させることによってトリー経路を形成しにくくし、エポキシ樹脂組成物の絶縁破壊強度を向上させ、コイル部品に高電圧が印加された場合においても絶縁破壊が生じないような試みがなされている。
また、特許文献２においては、特定粒径の球状シリカと酸無水物と硬化促進剤とからなるＡ剤を、エポキシ樹脂のＢ剤と混合してエポキシ樹脂組成物を得、エポキシ樹脂組成物の硬化物の線膨張率を低減させることによって熱応力によるクラックの発生を防止する試みがなされている。
しかしながら、上述したような無機充填材を含有する方法では、注型封止した樹脂組成物の絶縁破壊や冷熱サイクルに起因した応力によるクラックの発生を十分に防止することができず、さらなる改善が求められていた。
In view of such a problem, studies have been made by including an inorganic filler. In Patent Document 1, it is difficult to form a tree path by containing a predetermined amount of silica particles having a particle size in a specific range with respect to the epoxy resin composition, the dielectric breakdown strength of the epoxy resin composition is improved, and the coil Attempts have been made to prevent dielectric breakdown even when a high voltage is applied to the component.
Moreover, in patent document 2, A agent which consists of spherical silica of a specific particle size, an acid anhydride, and a hardening accelerator is mixed with B agent of an epoxy resin, an epoxy resin composition is obtained, and an epoxy resin composition of Attempts have been made to prevent the occurrence of cracks due to thermal stress by reducing the linear expansion coefficient of the cured product.
However, in the method containing the inorganic filler as described above, it is not possible to sufficiently prevent the occurrence of cracks due to the stress caused by the dielectric breakdown and the thermal cycle of the cast-sealed resin composition. It was sought after.
一方、可とう性構造を導入する方法でも検討がなされている。
特許文献３においては、可とう性のエポキシ樹脂等を含む主剤成分と、この主剤に対する硬化剤成分との２液性のエポキシ樹脂組成物とし、柔軟な骨格を導入することにより、応力の発生を低減しクラックの発生を防止する試みがなされている。
また、特許文献４では、酸無水物とポリエーテルジオール等とを硬化剤成分とし、エポキシ樹脂等を主成分としたエポキシ樹脂組成物を使用して、エポキシ樹脂の硬化物の絶縁破壊強度を向上させる試みがなされた。しかしながら、可とう性構造を硬化物に導入した場合、通常、絶縁性の低い構造及び官能基を多く有する為、常温での絶縁破壊強度はあるものの、高温環境下での絶縁破壊強度は満足いくものではなかった。
On the other hand, a method of introducing a flexible structure has also been studied.
In Patent Document 3, a two-component epoxy resin composition composed of a main component containing a flexible epoxy resin and the like and a curing agent component for the main component is used, and stress is generated by introducing a flexible skeleton. Attempts have been made to reduce and prevent the occurrence of cracks.
Moreover, in patent document 4, the dielectric breakdown strength of the hardened | cured material of an epoxy resin is improved by using the epoxy resin composition which has an acid anhydride, polyetherdiol, etc. as a hardening | curing agent component and has an epoxy resin etc. as a main component. An attempt was made to However, when a flexible structure is introduced into a cured product, it usually has a low insulating property and a large number of functional groups, so it has a dielectric breakdown strength at room temperature, but is satisfactory in a high temperature environment. It was not a thing.
本発明は、熱サイクルによるクラックの発生を防止し、絶縁破壊特性及び耐熱性、つまり１５０℃下での絶縁破壊強度に優れた２液注型用樹脂組成物、及びこの注形用樹脂組成物を用いたコイル部品を提供することを目的とする。 The present invention relates to a two-liquid casting resin composition that prevents cracking due to thermal cycling and has excellent dielectric breakdown characteristics and heat resistance, that is, excellent dielectric breakdown strength at 150 ° C., and this casting resin composition It aims at providing the coil components using.
本発明者らは、上記課題を解決すべき鋭意検討を実施した。その結果、コイルの絶縁分野で現在、封止樹脂としてエポキシ樹脂が汎用されていることに着目し、このエポキシ樹脂に種々の工夫を加えることで上記課題の解決を試みた。その結果、可とう性骨格を有し、長鎖アルキル鎖を有する芳香族アミンを含む硬化剤を添加することにより得られるエポキシ樹脂組成物を用いることにより上記課題を解決できることを見出した。
すなわち、最終的に得られるエポキシ樹脂組成物において、特定の硬化剤を用いて、エポキシ樹脂組成物の硬化物の骨格を柔らかくすることでクラックの発生を防止し、加えて、特定の高絶縁性構造を有する官能基をエポキシ樹脂組成物に導入することで、 １５０℃条件下での絶縁破壊強度に優れた硬化物を得ることができる。
また、本発明のエポキシ樹脂組成物は、このような高絶縁性及び耐クラック性に優れた樹脂組成を含有することで、従来行われてきたフィラー導入によるクラック対策の必要がないため、粘度低下により大幅な作業性改善がなされ、コイル等への含浸性が向上する。
その結果、本発明のエポキシ樹脂組成物によれば、エポキシ樹脂組成物の硬化物に高い絶縁特性を付与するとともに、エポキシ樹脂組成物の硬化物に可とう性を付与する硬化剤を含有するので、冷熱サイクル時のクラックの発生を抑制することができる。この結果、エポキシ樹脂組成物の硬化物の絶縁破壊特性を十分に確保することができる。
The present inventors have conducted intensive studies to solve the above problems. As a result, attention has been paid to the fact that epoxy resins are widely used as sealing resins in the field of coil insulation, and attempts have been made to solve the above problems by adding various ideas to the epoxy resins. As a result, it has been found that the above problem can be solved by using an epoxy resin composition obtained by adding a curing agent containing an aromatic amine having a flexible skeleton and a long alkyl chain.
That is, in the finally obtained epoxy resin composition, the use of a specific curing agent prevents the occurrence of cracks by softening the skeleton of the cured product of the epoxy resin composition, and in addition, a specific high insulation property By introducing a functional group having a structure into the epoxy resin composition, a cured product having excellent dielectric breakdown strength under 150 ° C. conditions can be obtained.
In addition, the epoxy resin composition of the present invention contains such a resin composition excellent in high insulation and crack resistance, so there is no need for countermeasures against cracks by introducing fillers, which has been conventionally performed, so that the viscosity decreases. As a result, the workability is greatly improved, and the impregnation of the coil and the like is improved.
As a result, according to the epoxy resin composition of the present invention, the epoxy resin composition contains a curing agent that imparts high insulating properties to the cured product of the epoxy resin composition and also gives flexibility to the cured product of the epoxy resin composition. In addition, it is possible to suppress the occurrence of cracks during the cooling and heating cycle. As a result, the dielectric breakdown characteristics of the cured product of the epoxy resin composition can be sufficiently ensured.
上記目的を達成すべく、本発明は、以下のものに関する。
［１］（Ａ）エポキシ樹脂と、（Ｂ）長鎖アルキル鎖を有する芳香族アミンを含む硬化剤とを含有する、２液性注形用エポキシ樹脂組成物。
［２］前記（Ａ）エポキシ樹脂が、液状エポキシ樹脂である、上記［１］に記載の２液性注形用エポキシ樹脂組成物。
［３］前記（Ｂ）長鎖アルキル鎖を有する芳香族アミンは、下記一般式（ＩＩ）に示される構造を有する、上記［１］又は［２］に記載の２液性注形用エポキシ樹脂組成物。
［４］前記硬化剤は、前記（Ｂ）長鎖アルキル鎖を有する芳香族アミンを５０質量％以上含む、上記［１］〜［３］のいずれか１つに記載の２液性注形用エポキシ樹脂組成物。
［５］前記エポキシ樹脂組成物の硬化物の弾性率が１０００ＭＰａ以下であり、加えて当該硬化物を１５０℃で５００時間放置下後の硬化物の硬度変化率が１３０%以下である、上記［１］〜［４］のいずれか１つに記載の２液性注形用エポキシ樹脂組成物。
［６］前記エポキシ樹脂組成物の硬化物の１５０℃の絶縁破壊強度が１５ｋＶ／ｍｍ以上である、上記［１］〜［５］のいずれか１つに記載の２液性注形用エポキシ樹脂組成物。
［７］上記［１］〜［６］のいずれか１つに記載の２液性注形用エポキシ樹脂組成物で注形された、コイル部品。
［８］前記コイル部品は、イグニッションコイルである、上記［７］に記載のコイル部品。
In order to achieve the above object, the present invention relates to the following.
[1] A two-component casting epoxy resin composition containing (A) an epoxy resin and (B) a curing agent containing an aromatic amine having a long-chain alkyl chain.
[2] The epoxy resin composition for two-component casting according to the above [1], wherein the (A) epoxy resin is a liquid epoxy resin.
[3] The aromatic resin having a long-chain alkyl chain (B) has a structure represented by the following general formula (II) and is a two-component casting epoxy resin according to the above [1] or [2] Composition.
[4] The two-part casting according to any one of [1] to [3], wherein the curing agent includes 50% by mass or more of the aromatic amine having (B) a long alkyl chain. Epoxy resin composition.
[5] The elastic modulus of the cured product of the epoxy resin composition is 1000 MPa or less, and in addition, the hardness change rate of the cured product after being left standing at 150 ° C. for 500 hours is 130% or less. The epoxy resin composition for two-component casting according to any one of [1] to [4].
[6] The epoxy resin for two-component casting according to any one of the above [1] to [5], wherein the cured product of the epoxy resin composition has a dielectric breakdown strength at 150 ° C. of 15 kV / mm or more. Composition.
[7] A coil component cast with the two-component casting epoxy resin composition according to any one of [1] to [6] above.
[8] The coil component according to [7], wherein the coil component is an ignition coil.
以上より、本発明によれば、冷熱サイクルによって発生する応力によるクラックの発生を防止し、１５０℃条件下での絶縁破壊強度に優れた２液性注型用エポキシ樹脂組成物、及びこの２液性注形用エポキシ樹脂組成物を用いたコイル部品を提供することができる。 As described above, according to the present invention, the two-component casting epoxy resin composition that prevents the occurrence of cracks due to the stress generated by the cooling cycle and has excellent dielectric breakdown strength under the condition of 150 ° C., and the two-component A coil component using the epoxy resin composition for castability can be provided.
以下、本発明のその他の特徴及び利点について、発明を実施するための形態に基づいて詳細に説明する。 Hereinafter, other features and advantages of the present invention will be described in detail based on embodiments for carrying out the invention.
（２液注形用エポキシ樹脂組成物）
本発明の２液性注形用エポキシ樹脂組成物は、（Ａ）エポキシ樹脂と、（Ｂ）長鎖アルキル鎖を有する芳香族アミンを含む硬化剤とを含有する。
(Epoxy resin composition for two-liquid casting)
The two-component casting epoxy resin composition of the present invention contains (A) an epoxy resin and (B) a curing agent containing an aromatic amine having a long-chain alkyl chain.
本発明の２液性注形用エポキシ樹脂組成物に用いる（Ａ）エポキシ樹脂は、本発明の２液性注形用エポキシ樹脂組成物の母材をなすものであって、１分子中に２個以上のエポキシ基を有するものであれば、分子量、分子構造等に制限されることなく、一般的に用いられているものを用いることができる。（Ａ）エポキシ樹脂には、例えば、ビスフェノール型、ノボラック型、ビフェニル型等の芳香族系エポキシ樹脂、ポリカルボン酸のグリシジルエーテル、シクロヘキサン誘導体等のエポキシ化によって得られる脂環族系エポキシ樹脂等が挙げられ、これらは単独又は２種以上混合して使用することができる。本発明の２液性注形用エポキシ樹脂組成物に用いる（Ａ）エポキシ樹脂は、好ましくは液状エポキシ樹脂である。 The (A) epoxy resin used in the two-part casting epoxy resin composition of the present invention forms the base material of the two-part casting epoxy resin composition of the present invention, and 2 per molecule. As long as it has one or more epoxy groups, those generally used can be used without being limited by molecular weight, molecular structure and the like. (A) Epoxy resins include, for example, aromatic epoxy resins such as bisphenol type, novolak type, and biphenyl type, alicyclic epoxy resins obtained by epoxidation of glycidyl ethers of polycarboxylic acids, cyclohexane derivatives, and the like. These may be used alone or in combination of two or more. The (A) epoxy resin used in the two-part casting epoxy resin composition of the present invention is preferably a liquid epoxy resin.
本発明の２液性注形用エポキシ樹脂組成物に用いる硬化剤は（Ｂ）長鎖アルキル鎖を有する芳香族アミンを含む。上記硬化剤における（Ｂ）長鎖アルキル鎖を有する芳香族アミンの含有割合は、好ましくは５０質量％以上であり、より好ましくは８０〜１００質量％であり、さらに好ましくは９０〜１００質量％であり、とくに好ましくは１００質量％である。上記硬化剤における（Ｂ）長鎖アルキル鎖を有する芳香族アミンの含有割合が５０質量％以上であると、本発明の２液性注形用エポキシ樹脂組成物の硬化物に可とう性を充分に付与することができる。 The curing agent used in the two-part casting epoxy resin composition of the present invention contains (B) an aromatic amine having a long-chain alkyl chain. The content of the aromatic amine having a long chain alkyl chain (B) in the curing agent is preferably 50% by mass or more, more preferably 80 to 100% by mass, and still more preferably 90 to 100% by mass. Yes, particularly preferably 100% by mass. When the content of the aromatic amine having a long-chain alkyl chain (B) in the curing agent is 50% by mass or more, the cured product of the two-part casting epoxy resin composition of the present invention has sufficient flexibility. Can be granted.
本発明の２液性注形用エポキシ樹脂組成物に用いる硬化剤が含む長鎖アルキル鎖を有する芳香族アミンは、（Ａ）エポキシ樹脂と反応して（Ａ）エポキシ樹脂を硬化させることができるものであればとくに限定されない。エポキシ樹脂組成物の硬化物に可とう性を付与するという観点から、上記長鎖アルキル鎖を有する芳香族アミンは、好ましくは２つ以上のアミノ基を含むものであり、より好ましくは下記一般式（Ｉ）に示される構造を有するものであり、さらに好ましくは下記一般式（ＩＩ）に示される構造を有するものである。 The aromatic amine having a long alkyl chain contained in the curing agent used in the two-part casting epoxy resin composition of the present invention can react with (A) the epoxy resin to cure the (A) epoxy resin. If it is a thing, it will not specifically limit. From the viewpoint of imparting flexibility to the cured product of the epoxy resin composition, the aromatic amine having a long alkyl chain preferably contains two or more amino groups, and more preferably the following general formula: It has a structure shown by (I), More preferably, it has a structure shown by the following general formula (II).
上記一般式（ＩＩ）に示される構造を有する長鎖アルキル鎖を有する芳香族アミンを含む硬化剤には、例えば、エラスマー１０００、エラスマー６５０Ｐ（以上、イハラケミカル工業株式会社製、商品名）等がある。
上記硬化剤は、長鎖アルキル鎖を有する１種の芳香族アミンを含んでもよく、長鎖アルキル鎖を有する２種以上の芳香族アミンを含んでもよい。
Examples of the curing agent containing an aromatic amine having a long alkyl chain having the structure represented by the general formula (II) include Elastomer 1000, Elastomer 650P (above, trade name, manufactured by Ihara Chemical Industry Co., Ltd.) and the like. is there.
The curing agent may include one type of aromatic amine having a long chain alkyl chain, or may include two or more types of aromatic amines having a long chain alkyl chain.
なお、これらの硬化剤の含有割合は、（Ａ）エポキシ樹脂の量に応じて適宜に設定する。
上記硬化剤の含有割合は、例えば、（Ａ）エポキシ樹脂１００質量部に対して、好ましくは８６〜２００質量部、より好ましくは１３０〜２００質量部である。このような含有割合の硬化剤を用いることで、本発明の特性を発現することができる。
この場合、最終的に得る２液性注形用エポキシ樹脂組成物の硬化物は、可とう性を有する構造を有する為、冷熱サイクル時のクラックの発生を防止することができる。また、最終的に得る２液性注形用エポキシ樹脂組成物の硬化物は高絶縁性構造を有する為、エポキシ樹脂組成物の硬化物の絶縁破壊特性を十分に確保することができる。
In addition, the content rate of these hardening | curing agents is suitably set according to the quantity of (A) epoxy resin.
The content rate of the said hardening | curing agent becomes like this. Preferably it is 86-200 mass parts with respect to 100 mass parts of (A) epoxy resins, More preferably, it is 130-200 mass parts. By using the curing agent having such a content, the characteristics of the present invention can be expressed.
In this case, since the cured product of the epoxy resin composition for two-part casting finally obtained has a flexible structure, it is possible to prevent the occurrence of cracks during the cooling and heating cycle. Moreover, since the cured | curing material of the epoxy resin composition for two-component casting finally obtained has a highly insulating structure, the dielectric breakdown characteristic of the cured | curing material of an epoxy resin composition can fully be ensured.
本発明の２液性注形用エポキシ樹脂組成物は、無機フィラー及び有機フィラー等のフィラーを含むことができる。フィラーの含有割合は、エポキシ樹脂１００質量部に対して、好ましくは０〜５０質量部、より好ましくは０〜２０質量部である。
本発明の２液性注形用エポキシ樹脂組成物に用いる無機フィラーは、樹脂組成物用のフィラーとして通常使用されているものであり、かつ、繊維状でないものであれば、特に限定されない。本発明の２液性注形用エポキシ樹脂組成物に用いる無機フィラーには、例えば、シリカ、水酸化アルミニウム、水酸化マグネシウム及びタルク等が挙げられる。
本発明の２液性注形用エポキシ樹脂組成物に用いる有機フィラーも、樹脂組成物用のフィラーとして通常使用されているものであり、かつ、繊維状でないものであれば、特に限定されない。本発明の２液性注形用エポキシ樹脂組成物に用いる有機フィラーには、例えば、シリコーン樹脂粉及びスチレン樹脂粉等が挙げられる。
樹脂組成物の粘度及び樹脂組成物の保存安定性の観点から、上記フィラーの平均粒径は、好ましくは約０．５〜約３０μｍであり、より好ましくは３〜２０μｍである。
The epoxy resin composition for two-component casting of the present invention can contain fillers such as inorganic fillers and organic fillers. The content of the filler is preferably 0 to 50 parts by mass, more preferably 0 to 20 parts by mass with respect to 100 parts by mass of the epoxy resin.
The inorganic filler used in the two-part casting epoxy resin composition of the present invention is not particularly limited as long as it is normally used as a filler for a resin composition and is not fibrous. Examples of the inorganic filler used in the two-part casting epoxy resin composition of the present invention include silica, aluminum hydroxide, magnesium hydroxide and talc.
The organic filler used in the two-part casting epoxy resin composition of the present invention is not particularly limited as long as it is usually used as a filler for a resin composition and is not fibrous. Examples of the organic filler used in the two-part casting epoxy resin composition of the present invention include silicone resin powder and styrene resin powder.
From the viewpoint of the viscosity of the resin composition and the storage stability of the resin composition, the average particle size of the filler is preferably about 0.5 to about 30 μm, more preferably 3 to 20 μm.
本発明の２液性注形用エポキシ樹脂組成物には、以上の各成分の他に、本発明の効果を阻害しない範囲で、この種の組成物に一般に配合される、カップリング剤、消泡剤、顔料などのその他の添加剤を必要に応じて配合することができる。但し、コイルへの含浸性から、繊維質充填剤を含まないことが好ましい。その他の添加剤の含有割合は、例えば、エポキシ樹脂１００質量部に対して、好ましくは０．１〜５．０質量部、より好ましくは０．１〜１．０質量部である。 In addition to the above-described components, the two-part casting epoxy resin composition of the present invention includes a coupling agent and an antibacterial compound that are generally blended in this type of composition within a range that does not impair the effects of the present invention. Other additives such as foaming agents and pigments can be blended as necessary. However, it is preferable not to include a fibrous filler from the viewpoint of impregnation into the coil. The content of other additives is, for example, preferably 0.1 to 5.0 parts by mass, more preferably 0.1 to 1.0 parts by mass with respect to 100 parts by mass of the epoxy resin.
本発明の効果を発現するという観点から、２液性注形用エポキシ樹脂組成物における（Ａ）エポキシ樹脂と（Ｂ）長鎖アルキル鎖を有する芳香族アミンを含む硬化剤との合計の含有割合は、例えば、好ましくは５０〜１００質量％であり、より好ましくは８０〜１００質量％である。 From the standpoint of expressing the effects of the present invention, the total content of (A) epoxy resin and (B) a curing agent containing an aromatic amine having a long-chain alkyl chain in the two-part casting epoxy resin composition Is, for example, preferably 50 to 100% by mass, more preferably 80 to 100% by mass.
本発明の２液性注形用エポキシ樹脂組成物を、注形材料として調製するにあたっては、（Ａ）エポキシ樹脂、及び（Ｂ）可とう性硬化剤、並びに上述したような必要に応じて配合される成分を充分混合し均一に混合することにより製造することができる。本発明のエポキシ樹脂組成物の硬化物における１５０℃条件下での絶縁破壊強度は、好ましくは１５ｋＶ／ｍｍ以上であり、より好ましくは２０ｋＶ／ｍｍ以上である。また、本発明のエポキシ樹脂組成物をコイル部品に用いた際に、本発明のエポキシ樹脂組成物はコイルに対して高含浸性であることが好ましい。 In preparing the two-part casting epoxy resin composition of the present invention as a casting material, (A) an epoxy resin, and (B) a flexible curing agent, and blending as necessary as described above. The components to be produced can be sufficiently mixed and mixed uniformly. The dielectric breakdown strength of the cured product of the epoxy resin composition of the present invention at 150 ° C. is preferably 15 kV / mm or more, and more preferably 20 kV / mm or more. Moreover, when the epoxy resin composition of the present invention is used for a coil part, the epoxy resin composition of the present invention is preferably highly impregnated with respect to the coil.
このようにして得られた２液性注形用エポキシ樹脂組成物は、電気機器部品、特にコイル部品、特にイグニッションコイル、特に自動車用のイグニッションコイルの封止、被覆、絶縁等に適用すれば、優れた特性と信頼性とをコイル部品に付与することができる。これらの用途に適用するためには、本発明の２液性注形用エポキシ樹脂組成物から得られる硬化物は柔軟性を有することから、本発明の２液性注形用エポキシ樹脂組成物の硬化物は以下の特性を有する。ガラス転移温度は、好ましくは２５℃以下であり、より好ましくは０℃以下である、また、２５℃における弾性率は、好ましくは１０００ＭＰａ以下、より好ましくは９００ＭＰａ以下である。さらに、１５０℃で５００時間保持後の硬度及び硬度変化率は、それぞれ、好ましくは８０以下及び１３０％以下であり、より好ましくは７５以下及び１１５％以下である。なお、弾性率は、ＪＩＳ Ｋ ７１６１の試験方法で、測定を行ったときの値である。 If the epoxy resin composition for two-component casting thus obtained is applied to sealing, coating, insulation, etc. of electrical equipment parts, especially coil parts, especially ignition coils, especially automobile ignition coils, Excellent characteristics and reliability can be imparted to the coil component. In order to apply to these uses, since the cured product obtained from the two-part casting epoxy resin composition of the present invention has flexibility, the two-part casting epoxy resin composition of the present invention The cured product has the following characteristics. The glass transition temperature is preferably 25 ° C. or lower, more preferably 0 ° C. or lower. The elastic modulus at 25 ° C. is preferably 1000 MPa or lower, more preferably 900 MPa or lower. Furthermore, the hardness and hardness change rate after holding at 150 ° C. for 500 hours are preferably 80 or less and 130% or less, and more preferably 75 or less and 115% or less, respectively. The elastic modulus is a value when measurement is performed by a test method of JIS K 7161.
（イグニッションコイル）
次に、上述した２液性注形用エポキシ樹脂組成物を注形するコイル部品の一例としてイグニッションコイルについて説明する。
図１は、本発明の一実施形態におけるコイル部品としてのイグニッションコイルの構成を示す断面図である。なお、図１（ｂ）は、図１（ａ）の領域９における２次線の抜けの一例を示す図である。本発明の２液性注形用エポキシ樹脂組成物を用いることにより、このような２次線の抜けが発生しないようにすることができる。
(ignition coil)
Next, an ignition coil will be described as an example of a coil component for casting the above-described two-component casting epoxy resin composition.
FIG. 1 is a cross-sectional view showing a configuration of an ignition coil as a coil component in one embodiment of the present invention. Note that FIG. 1B is a diagram illustrating an example of missing secondary lines in the region 9 of FIG. By using the two-component casting epoxy resin composition of the present invention, it is possible to prevent such secondary line from coming off.
イグニッションコイルは、磁性体の中心コア１、不図示の外部コア、一次ボビン２、一次コイル３、二次ボビン４、二次コイル５、端子６などで構成される。一次コイル３は、例えば直径０．５ｍｍ程度のエナメル線を約２００回、二次コイル５は、例えば直径０．０５ｍｍ程度のエナメル細線を２００００回程度ボビンに巻線されている。一次コイル３はバッテリーに接続され直流電流が流れるが、点火タイミング調整電子回路部品８及び図示しないパワースイッチにより電流を断続させて磁束を変化させ、自己誘導作用により一次電圧を得る。この一次電圧を一次コイル３と二次コイル５の相互誘導作用により２０〜４０ｋＶの高電圧とし、端子６に接続した点火プラグに火花放電を起こさせる。
なお、点火タイミング調整電子回路部品は、電子部品が本発明の２液性注形用エポキシ樹脂組成物８によって、封止されたような形態を採る。
上述した中心コア１等は、例えばポリフェニレンサルファイド（ＰＰＳ）からなるケース７中に収納され、ケース７と中心コア１等との空隙は、上述した本発明の２液性注形用樹脂組成物の硬化物８によって充填される。
The ignition coil includes a magnetic core 1, an external core (not shown), a primary bobbin 2, a primary coil 3, a secondary bobbin 4, a secondary coil 5, and a terminal 6. The primary coil 3 is wound about 200 mm of enameled wire with a diameter of about 0.5 mm, for example, and the secondary coil 5 is wound about 20000 times of enameled thin wire with a diameter of about 0.05 mm, for example. The primary coil 3 is connected to the battery and a direct current flows. However, the current is intermittently changed by the ignition timing adjusting electronic circuit component 8 and a power switch (not shown) to change the magnetic flux, and a primary voltage is obtained by a self-induction action. This primary voltage is set to a high voltage of 20 to 40 kV by the mutual induction action of the primary coil 3 and the secondary coil 5, and spark discharge is caused in the spark plug connected to the terminal 6.
The ignition timing adjusting electronic circuit component takes a form in which the electronic component is sealed with the two-part casting epoxy resin composition 8 of the present invention.
The above-described central core 1 and the like are accommodated in a case 7 made of, for example, polyphenylene sulfide (PPS), and the gap between the case 7 and the central core 1 and the like is the above-described two-component casting resin composition of the present invention. It is filled with the cured product 8.
図１に示すイグニッションコイルは、上述したように、点火タイミング調整電子回路部品８及び図示しないパワースイッチにより生じた一次電圧が、一次コイル３及び二次コイル５に印加されるようになるので、瞬時に高電圧の一次電圧が印加され、電流の流入及び停止を頻繁に繰り返す場合がある。
このように高電圧が瞬時に印加されると、イグニッションコイルを封止している２液性注形用エポキシ樹脂組成物８にも瞬時に高電圧が印加されるが、２液性注形用エポキシ樹脂組成物の硬化物８は、上述のように絶縁破壊特性に優れた本発明の２液性注形用エポキシ樹脂組成物からなるので、２液性注形用エポキシ樹脂組成物の硬化物８は絶縁破壊を引き起こすことなく、イグニッションコイルに対する絶縁性を確保することができる。
In the ignition coil shown in FIG. 1, the primary voltage generated by the ignition timing adjusting electronic circuit component 8 and the power switch (not shown) is applied to the primary coil 3 and the secondary coil 5 as described above. In some cases, a high primary voltage is applied to the capacitor, and the inflow and stop of the current are frequently repeated.
When a high voltage is instantaneously applied in this way, a high voltage is also instantaneously applied to the two-component casting epoxy resin composition 8 sealing the ignition coil. Since the cured product 8 of the epoxy resin composition is composed of the two-component casting epoxy resin composition of the present invention having excellent dielectric breakdown characteristics as described above, the cured product of the two-component casting epoxy resin composition. No. 8 can secure insulation against the ignition coil without causing dielectric breakdown.
以下、本発明を実施例に基づいて具体的に説明するが、本発明はこれら実施例に限定されるものではない。 EXAMPLES Hereinafter, although this invention is demonstrated concretely based on an Example, this invention is not limited to these Examples.
２液性注形用エポキシ樹脂組成物の製造
（実施例１）
最初に、ビスフェノールＡジグリシジルエーテル型エポキシ樹脂としてＲ−１４０Ｐ（三井化学株式会社製、商品名） １００質量部、消泡剤としてＴＳＡ７２０ （モメンティブ・パフォーマンス・マテリアルズ社製、商品名） ０．１質量部を、１時間混合を行って主剤成分を製造した。
上記エポキシ樹脂１００質量部に対して、可とう性芳香族アミン硬化剤としてエラスマー１０００ （イハラケミカル工業株式会社製、商品名）を１６６質量部混合したものを注形用エポキシ樹脂組成物として得た。
Production of two-part casting epoxy resin composition (Example 1)
First, 100 parts by mass of R-140P (trade name, manufactured by Mitsui Chemicals, Inc.) as a bisphenol A diglycidyl ether type epoxy resin, and TSA720 (trade name, manufactured by Momentive Performance Materials) as an antifoaming agent 0.1 The main component was manufactured by mixing 1 part by mass for 1 hour.
An epoxy resin composition for casting was obtained by mixing 166 parts by mass of Elastomer 1000 (trade name, manufactured by Ihara Chemical Industry Co., Ltd.) as a flexible aromatic amine curing agent with respect to 100 parts by mass of the epoxy resin. .
（実施例２〜７、比較例１〜５）
表１に示す量の配合成分を用いる以外は実施例１と同様にしてコイル注形用樹脂組成物及び比較用の樹脂組成物を調製し、実施例１と同様の評価を行った。結果を表１に示す。
尚、その他の使用材料は以下に示す。
(Examples 2-7, Comparative Examples 1-5)
A resin composition for coil casting and a resin composition for comparison were prepared in the same manner as in Example 1 except that the blending components in the amounts shown in Table 1 were used, and the same evaluation as in Example 1 was performed. The results are shown in Table 1.
Other materials used are shown below.
（１）エポキシ樹脂:ビスフェノールＡ型エポキシ樹脂ＥＰ４０００ （ＡＤＥＫＡ株式会社製、商品名）
（２）芳香族アミン:エラスマー６５０Ｐ（イハラケミカル工業株式会社製、商品名）
（３）脂肪族アミン：ジェファーミンＤ２０００ （ハンツマン・コーポレーション社製、商品名）
（４）脂肪族アミン:ジェファーミンＤ４００ （ハンツマン・コーポレーション社製、商品名）
（５）脂肪族アミン:ジェファーミンＤ２３０ （ハンツマン・コーポレーション社製、商品名）
（６）酸無水物：ＨＮ−２０００（日立化成株式会社製、商品名）
（７）硬化促進剤：ＢＤＭＡ（Ｎ，Ｎ−ジメチルベンジルアミン）
（比較列６）
最初に、ビスフェノールＡジグリシジルエーテル型エポキシ樹脂としてＲ-１４０Ｐ（三井化学株式会社製、商品名） １００質量部、消泡剤としてＴＳＡ７２０ (モメンティブ・パフォーマンス・マテリアルズ社製、商品名）０．１質量部、充填剤としてクリスタライトＡＡ（株式会社龍森製、商品名）を１６０質量部、１時間混合を行って主剤成分を製造した。
上記エポキシ樹脂１００質量部に対して、硬化剤としてＨＮ−２０００（日立化成株式会社製、商品名）を８７質量部、硬化促進剤としてＢＤＭＡ（Ｎ，Ｎ−ジメチルベンジルアミン）を混合したものを注形用エポキシ樹脂組成物として得た。
(1) Epoxy resin: bisphenol A type epoxy resin EP4000 (made by ADEKA Corporation, trade name)
(2) Aromatic amine: Elastomer 650P (Ihara Chemical Industry Co., Ltd., trade name)
(3) Aliphatic amine: Jeffamine D2000 (trade name, manufactured by Huntsman Corporation)
(4) Aliphatic amine: Jeffamine D400 (trade name, manufactured by Huntsman Corporation)
(5) Aliphatic amine: Jeffamine D230 (trade name, manufactured by Huntsman Corporation)
(6) Acid anhydride: HN-2000 (manufactured by Hitachi Chemical Co., Ltd., trade name)
(7) Curing accelerator: BDMA (N, N-dimethylbenzylamine)
(Comparison column 6)
First, 100 parts by mass of R-140P (trade name, manufactured by Mitsui Chemicals, Inc.) as a bisphenol A diglycidyl ether type epoxy resin, TSA720 (trade name, manufactured by Momentive Performance Materials, Inc.) 0.1 as an antifoaming agent The main component was manufactured by mixing 160 parts by mass of crystallite AA (manufactured by Tatsumori Co., Ltd., trade name) as a mass part and a filler for 1 hour.
What mixed 87 parts by mass of HN-2000 (manufactured by Hitachi Chemical Co., Ltd., trade name) as a curing agent and BDMA (N, N-dimethylbenzylamine) as a curing accelerator with respect to 100 parts by mass of the epoxy resin. It was obtained as an epoxy resin composition for casting.
評価
次いで、上述のようにして得た注型用エポキシ樹脂組成物に対して、ガラス転移温度、絶縁破壊強度、含浸性、硬度を測定することにより、上記注型用エポキシ樹脂組成物の実用特性を評価した。
Evaluation Next, by measuring the glass transition temperature, the dielectric breakdown strength, the impregnation property, and the hardness of the casting epoxy resin composition obtained as described above, the practical properties of the casting epoxy resin composition are measured. Evaluated.
・ガラス転移温度：樹脂組成物を１５０℃／１０時間（１５０℃の温度で１０時間保持することを示す。以下、同じ）で硬化させて、ＤＳＣ法により、昇温速度１５℃／ｍｉｎとして、室温から２００℃まで昇温させて測定した。 Glass transition temperature: The resin composition is cured at 150 ° C./10 hours (indicating that the resin composition is held at a temperature of 150 ° C. for 10 hours. The same applies hereinafter), and the heating rate is 15 ° C./min by DSC method. The temperature was raised from room temperature to 200 ° C. and measured.
・絶縁破壊強度：樹脂組成物を１５０℃／１０時間で硬化させて、ＪＩＳ Ｃ２１１０の試験法で、サンプルが破壊するまでの変位を求めた。 -Dielectric breakdown strength: The resin composition was cured at 150 ° C./10 hours, and the displacement until the sample was broken was determined by the test method of JIS C2110.
・含浸性：ボビン径直径１８ｍｍ、巻き線径直径４５μｍ、巻き数１５０００ターン、ケース径直径２３ｍｍのコイルにエポキシ樹脂組成物を注形し、９０℃／３時間→１５０℃／３時間の２ステップで硬化後のコイルの断面を確認した。
（表１；○：含浸率１００％、△：含浸率５０%以上１００％未満、×：含浸率５０%未満）
・ Impregnation: Bobbin diameter 18 mm, winding diameter 45 μm, number of turns 15000 turns, epoxy resin composition cast into coil with case diameter 23 mm, 90 ° C / 3 hours → 150 ° C / 3 hours 2 steps The cross section of the coil after curing was confirmed.
(Table 1: O: impregnation rate 100%, Δ: impregnation rate 50% or more and less than 100%, x: impregnation rate less than 50%)
・弾性率：樹脂組成物を１５０℃／１０時間で硬化させて、ＪＩＳ Ｋ ７１６１の試験方法で、測定を行った。 Elastic modulus: The resin composition was cured at 150 ° C./10 hours, and measured by the test method of JIS K 7161.
・硬度：樹脂組成物を１５０℃／１０時間で硬化させて、ＪＩＳ Ｋ６２５３の試験方法で、サンプルが破壊するまでの変位を求めた。硬度はデュロメータのタイプＡにて測定を行った。測定は、樹脂硬化後の硬度と、硬化後の樹脂を１５０℃で５００時間放置した後の硬度を測定した。 Hardness: The resin composition was cured at 150 ° C./10 hours, and the displacement until the sample was broken was determined by the test method of JIS K6253. The hardness was measured with a durometer type A. The measurement was carried out by measuring the hardness after curing the resin and the hardness after leaving the cured resin at 150 ° C. for 500 hours.
・硬度変化率：以下の計算式を用いて算出した。
硬度変化率＝（１５０℃で５００時間放置した後の硬度÷樹脂硬化後の硬度）×１００
Hardness change rate: calculated using the following formula.
Hardness change rate = (hardness after standing at 150 ° C. for 500 hours ÷ hardness after resin curing) × 100
・クラック性試験
エポキシ樹脂組成物をワッシャーの入った金属シャーレに注型し、９０℃／３時間→１５０℃／３時間の２ステップで硬化後の構造物に対して、 １５０℃〜−４０℃の冷熱サイクル試験で評価した。
金属シャーレは直径６ｃｍ、高さ１．５ｃｍのものを用いた。
また、ワッシャーは、図２に示す直径３０ｍｍのものを用い、直径３ｍｍの金属ボールを上面３か所、下面３か所に設置したものを作製し、評価に用いた。なお、図２（ａ）はワッシャーの上面図であり、図２（ｂ）は、ワッシャーをおよそ側面側から見た図である。
（表１；○：２０サイクル以上、×：２０サイクル以下）
・ Crack property test The epoxy resin composition was cast into a metal petri dish containing a washer, and the structure after curing in two steps of 90 ° C./3 hours → 150 ° C./3 hours, 150 ° C. to −40 ° C. This was evaluated by a cold cycle test.
A metal petri dish having a diameter of 6 cm and a height of 1.5 cm was used.
Further, the washer having a diameter of 30 mm shown in FIG. 2 was used, and metal balls having a diameter of 3 mm were installed at three places on the upper surface and three places on the lower surface, and used for evaluation. 2A is a top view of the washer, and FIG. 2B is a view of the washer viewed from the side surface.
(Table 1; ○: 20 cycles or more, x: 20 cycles or less)
表１から明らかなように、本発明に従った実施例における注形用エポキシ樹脂組成物においては、ガラス転移温度が２５℃以下であることや、弾性率が１０００ＭＰ以下であることから、柔軟性に優れていることが分かる。
加えて、硬度変化率が比較例１より少ないことから、高温放置後でも、優れた柔軟性を示す。
また、１５０℃下の絶縁破壊強度も２０ｋＶ／ｍｍ以上であり、絶縁破壊特性も優れていることが分かる。
As is apparent from Table 1, in the epoxy resin composition for casting in the examples according to the present invention, the glass transition temperature is 25 ° C. or less and the elastic modulus is 1000 MP or less, so that flexibility It turns out that it is excellent in.
In addition, since the rate of change in hardness is smaller than that of Comparative Example 1, excellent flexibility is exhibited even after being left at a high temperature.
In addition, the dielectric breakdown strength at 150 ° C. is 20 kV / mm or more, which indicates that the dielectric breakdown characteristics are excellent.
以上、本発明を上記具体例に基づいて詳細に説明したが、本発明は上記具体例に限定されるものではなく、本発明の範疇を逸脱しない限りにおいて、あらゆる変形や変更が可能である。 The present invention has been described in detail based on the above specific examples. However, the present invention is not limited to the above specific examples, and various modifications and changes can be made without departing from the scope of the present invention.
１：中心コア
２：一次ボビン
３：一次コイル
４：二次ボビン
５：二次コイル
６：端子
７：ケース
８：２液性注形用エポキシ樹脂組成物の硬化物（点火タイミング調整電子回路部品）
1: Central core 2: Primary bobbin 3: Primary coil 4: Secondary bobbin 5: Secondary coil 6: Terminal 7: Case 8: Cured product of epoxy resin composition for two-liquid casting (ignition timing adjustment electronic circuit component )
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2014192542A JP2016060898A (en) | 2014-09-22 | 2014-09-22 | Two-pack casting epoxy resin composition, and coil component |
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| Application Number | Priority Date | Filing Date | Title |
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| JP2014192542A JP2016060898A (en) | 2014-09-22 | 2014-09-22 | Two-pack casting epoxy resin composition, and coil component |
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| JP2016060898A true JP2016060898A (en) | 2016-04-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| JP2014192542A Pending JP2016060898A (en) | 2014-09-22 | 2014-09-22 | Two-pack casting epoxy resin composition, and coil component |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170141102A (en) * | 2016-06-14 | 2017-12-22 | 삼성전기주식회사 | Coil device and manufacturing method of the same |
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| JP2010100726A (en) * | 2008-10-23 | 2010-05-06 | Kyocera Chemical Corp | Epoxy resin composition for impregnation casting of molded coil, molded coil device and method for producing molded coil device |
| JP2010265353A (en) * | 2009-05-13 | 2010-11-25 | Kyocera Chemical Corp | Halogen-free flame retardant adhesive composition, flexible copper-clad laminate, coverlay, and adhesive film |
| JP2011233883A (en) * | 2010-04-09 | 2011-11-17 | Kyocera Chemical Corp | Dry film for coverlay, coverlay, flexible printed wiring board and method for manufacturing flexible printed wiring board |
| JP2012201711A (en) * | 2011-03-23 | 2012-10-22 | Kyocera Chemical Corp | Casting epoxy resin composition, and coil part |
| JP2013072073A (en) * | 2011-09-29 | 2013-04-22 | Dic Corp | Amine-based curing agent, epoxy resin composition containing amine-based curing agent, and cured product of the same |
| JP2013155346A (en) * | 2012-01-31 | 2013-08-15 | Kyocera Chemical Corp | Resin composition for impregnating large-scaled mold coil and large-scaled mold coil using the same |
| JP2013203950A (en) * | 2012-03-29 | 2013-10-07 | Tamura Seisakusho Co Ltd | Thermosetting resin composition, resin film, copper-clad sheet and flexible printed wiring board |
| JP2015507677A (en) * | 2011-12-28 | 2015-03-12 | ポスコ | Insulating adhesive composition for MCCL, painted metal plate using the same, and method for producing the same |
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| JPS63170411A (en) * | 1986-08-28 | 1988-07-14 | ハ−キュルス・インコ−ポレ−テッド | Multiphase epoxy heat-set article having rubber in disperse phase |
| JPS6466229A (en) * | 1987-09-07 | 1989-03-13 | Katsumi Yano | High polymer piezoelectric material and production thereof |
| JPS6467986A (en) * | 1987-09-08 | 1989-03-14 | Katsumi Yano | Piezoelectric type pressure sensitive element and manufacture thereof |
| JPH0347848A (en) * | 1989-04-26 | 1991-02-28 | Takeda Chem Ind Ltd | Production of prepreg |
| JP2003332742A (en) * | 2002-05-16 | 2003-11-21 | Kyocera Chemical Corp | Multilayer flex-rigid wiring board and its manufacturing method |
| JP2008106182A (en) * | 2006-10-26 | 2008-05-08 | Matsushita Electric Works Ltd | Epoxy resin composition and adhesive |
| JP2009062447A (en) * | 2007-09-06 | 2009-03-26 | Hokko Chem Ind Co Ltd | Liquid epoxy resin composition |
| JP2010053164A (en) * | 2008-08-26 | 2010-03-11 | Kyocera Chemical Corp | Resin composition for encapsulation and resin-encapsulated semiconductor device |
| JP2010100726A (en) * | 2008-10-23 | 2010-05-06 | Kyocera Chemical Corp | Epoxy resin composition for impregnation casting of molded coil, molded coil device and method for producing molded coil device |
| JP2010265353A (en) * | 2009-05-13 | 2010-11-25 | Kyocera Chemical Corp | Halogen-free flame retardant adhesive composition, flexible copper-clad laminate, coverlay, and adhesive film |
| JP2011233883A (en) * | 2010-04-09 | 2011-11-17 | Kyocera Chemical Corp | Dry film for coverlay, coverlay, flexible printed wiring board and method for manufacturing flexible printed wiring board |
| JP2012201711A (en) * | 2011-03-23 | 2012-10-22 | Kyocera Chemical Corp | Casting epoxy resin composition, and coil part |
| JP2013072073A (en) * | 2011-09-29 | 2013-04-22 | Dic Corp | Amine-based curing agent, epoxy resin composition containing amine-based curing agent, and cured product of the same |
| JP2015507677A (en) * | 2011-12-28 | 2015-03-12 | ポスコ | Insulating adhesive composition for MCCL, painted metal plate using the same, and method for producing the same |
| JP2013155346A (en) * | 2012-01-31 | 2013-08-15 | Kyocera Chemical Corp | Resin composition for impregnating large-scaled mold coil and large-scaled mold coil using the same |
| JP2013203950A (en) * | 2012-03-29 | 2013-10-07 | Tamura Seisakusho Co Ltd | Thermosetting resin composition, resin film, copper-clad sheet and flexible printed wiring board |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170141102A (en) * | 2016-06-14 | 2017-12-22 | 삼성전기주식회사 | Coil device and manufacturing method of the same |
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