JPH11181243A - Flame-retardant epoxy resin composition and electric parts using the same - Google Patents
Flame-retardant epoxy resin composition and electric parts using the sameInfo
- Publication number
- JPH11181243A JPH11181243A JP9348399A JP34839997A JPH11181243A JP H11181243 A JPH11181243 A JP H11181243A JP 9348399 A JP9348399 A JP 9348399A JP 34839997 A JP34839997 A JP 34839997A JP H11181243 A JPH11181243 A JP H11181243A
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- JP
- Japan
- Prior art keywords
- epoxy resin
- flame
- resin composition
- retardant epoxy
- retardant
- 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.)
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- Compositions Of Macromolecular Compounds (AREA)
- Organic Insulating Materials (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、難燃性エポキシ樹
脂組成物及びこの組成物を用いて絶縁処理した電気部品
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a flame-retardant epoxy resin composition and an electric part insulated using the composition.
【０００２】[0002]
【従来の技術】従来、エポキシ樹脂は優れた電気特性、
機械特性、耐クラック性を有するとともに、各種材料と
の接着性に優れているため、電気絶縁用、特に注型用と
して多用され、特に絶縁保護、高電圧特性（耐アーク
性、耐トラッキング性）、耐クラック性などの向上を目
的として、例えば、酸無水物硬化型エポキシ樹脂に多量
の充填剤および難燃剤を含んだ難燃性エポキシ樹脂組成
物が用いられている。難燃性エポキシ樹脂組成物には、
一般にハロゲン系難燃剤、リン系難燃剤、無機系充填剤
等が添加されて難燃性が付与されている。しかしなが
ら、これらの材料が燃焼すると、一酸化炭素、シアン化
水素、亜硫酸ガス、ハロゲン化水素などの有害ガスが生
成し、特にハロゲン系難燃剤を用いた場合には、ハロゲ
ン化ベンゾダイオキシン、ジベンゾフランなどの有害物
質の生成が心配されている。ハロゲン系難燃剤を含まな
い難燃性エポキシ樹脂組成物としては、従来よりリン系
難燃剤が用いられているが、この組成物は、耐湿性、耐
熱性に劣るという問題があった。また無機系難燃剤を用
いる場合には充分な難燃性が得られず、これを増量配分
すると粘度が著しく上昇し、作業性が低下する問題点が
あった。2. Description of the Related Art Conventionally, epoxy resins have excellent electrical properties,
Due to its excellent mechanical properties and crack resistance, and excellent adhesion to various materials, it is widely used for electrical insulation, especially for casting, especially for insulation protection and high voltage characteristics (arc resistance, tracking resistance). For the purpose of improving crack resistance and the like, for example, a flame-retardant epoxy resin composition containing a large amount of a filler and a flame retardant in an acid anhydride-curable epoxy resin is used. The flame-retardant epoxy resin composition includes
Generally, halogen-based flame retardants, phosphorus-based flame retardants, inorganic fillers and the like are added to impart flame retardancy. However, when these materials burn, harmful gases such as carbon monoxide, hydrogen cyanide, sulfurous acid gas, and hydrogen halide are generated. Particularly when halogen-based flame retardants are used, harmful gases such as halogenated benzodioxin and dibenzofuran are generated. There is concern over the generation of substances. As a flame-retardant epoxy resin composition containing no halogen-based flame retardant, a phosphorus-based flame retardant has been conventionally used, but this composition has a problem that it is inferior in moisture resistance and heat resistance. In addition, when an inorganic flame retardant is used, sufficient flame retardancy cannot be obtained. When the amount of the flame retardant is increased, the viscosity is remarkably increased and the workability is reduced.
【０００３】[0003]
【発明が解決しようとする課題】本発明は、前記の従来
技術の問題点を解決し、ハロゲン系難燃剤を用いず、有
害ガスの発生が少なく、難燃性に優れ、しかも低粘度で
作業性に優れた難燃性エポキシ樹脂組成物及びこれを用
いて絶縁処理された電気部品を提供するものである。SUMMARY OF THE INVENTION The present invention solves the above-mentioned problems of the prior art, does not use a halogen-based flame retardant, generates little harmful gas, has excellent flame retardancy, and operates with low viscosity. An object of the present invention is to provide a flame-retardant epoxy resin composition having excellent heat resistance and an electric component insulated using the same.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、充填剤を
多量に含有するエポキシ樹脂組成物に特定の湿潤分散剤
を配合することにより、前記の問題点が解決されること
を見出し、本発明に到達した。すなわち、本発明は、エ
ポキシ樹脂、酸無水物及び水和アルミナを含有するエポ
キシ樹脂組成物において、湿潤分散剤としてアルミニウ
ムキレート化合物をエポキシ樹脂に対して１重量％以上
添加した難燃性エポキシ樹脂組成物及びこの組成物を用
いて絶縁処理された電気部品に関する。Means for Solving the Problems The present inventors have found that the above problems can be solved by blending a specific wetting and dispersing agent into an epoxy resin composition containing a large amount of a filler, The present invention has been reached. That is, the present invention relates to an epoxy resin composition containing an epoxy resin, an acid anhydride and a hydrated alumina, wherein an aluminum chelate compound as a wetting and dispersing agent is added in an amount of 1% by weight or more based on the epoxy resin. The present invention relates to a product and an electric component which has been subjected to insulation treatment using the composition.
【０００５】[0005]
【発明の実施の形態】本発明の難燃性エポキシ樹脂組成
物に用いられ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。エポキシ樹脂としては、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、１，４−ブタ
ンジオール、１，６−ヘキサンジオール、ポリエチレン
グリコール、ポリプロピレングリコール、トリメチロー
ルプロパン等の多価アルコールのポリグリシジルエーテ
ル、フタル酸、テトラヒドロフタル酸、ヘキサヒドロフ
タル酸、セバチン酸、ドデカン二酸等のポリカルボン酸
のポリグリシジルエステル、ポリブタジエンのポリエポ
キシ化物などが用いられる。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（チバガイギー社製、商品
名）、ＤＥＲ−３３１（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。DESCRIPTION OF THE PREFERRED EMBODIMENTS As the epoxy resin used in the flame-retardant epoxy resin composition of the present invention, a compound having at least two epoxy groups in one molecule is used. 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. Examples of the epoxy resin include bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol AD epoxy resin, 1,4-butanediol, 1,6-hexanediol, polyethylene glycol, polypropylene glycol, and trimethylolpropane. Polyglycidyl ethers of polyhydric alcohols, phthalic acid, tetrahydrophthalic acid, hexahydrophthalic acid, polyglycidyl esters of polycarboxylic acids such as sebacic acid and dodecane diacid, and polyepoxidized products of polybutadiene are used. These resins are not particularly limited, but are preferably liquid at room temperature, and are commercially available as Epicoat 828 (Yuika Shell Epoxy Co., Ltd.).
GY-260 (trade name, manufactured by Ciba Geigy), DER-331 (trade name, manufactured by Dow Chemical Japan Co., Ltd.), and the like. These can be used alone or in combination.
【０００６】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。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。また、メチル
（３，４−エポキシシクロヘキサン）カルボキシレート
等の脂環式エポキシ化合物を使用することもできる。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. Furthermore, as epoxy resin,
An epoxy compound having only one epoxy group in one molecule may be included. Such an epoxy compound is preferably used in the range of 0 to 40% by weight, and 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, dibromophenyl glycidyl ether, dibromocresyl glycidyl ether and the like. Also, an alicyclic epoxy compound such as methyl (3,4-epoxycyclohexane) carboxylate can be used.
【０００７】本発明に用いられる酸無水物としては、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、無水フタル酸、ヘキサヒドロ無水フ
タル酸、エンドメチレンテトラヒドロ無水フタル酸、ド
デセニル無水コハク酸、オクテニル無水コハク酸、ポリ
アゼライン酸ポリ無水物などが挙げられる。酸無水物の
使用量は、エポキシ樹脂に含まれるエポキシ基１当量当
たり０．６〜１．３当量の範囲が好ましい。The acid anhydride used in the present invention includes, for example, methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, phthalic anhydride, hexahydrophthalic anhydride, endomethylenetetrahydrophthalic anhydride, dodecenylsuccinic anhydride, octenyl Succinic anhydride, polyazelaic acid polyanhydride and the like. The amount of the acid anhydride used is preferably in the range of 0.6 to 1.3 equivalents per equivalent of epoxy group contained in the epoxy resin.
【０００８】また、本発明の難燃性エポキシ樹脂組成物
には、水和アルミナが充填剤として用いられるが、その
他の充填剤を併用することができる。他の充填剤として
は、通常の溶融シリカ、結晶シリカ、タルク、炭酸カル
シウム、クレーなどが挙げられる。水和アルミナの使用
量は、エポキシ樹脂に対して１５０〜１７０重量％が好
ましく、他の充填剤と併用して用いる場合には、全充填
剤の８０重量％を水和アルミナとするのが好ましい。水
和アルミナの量がエポキシ樹脂に対して１５０重量％未
満であると、樹脂組成物の難燃性が低下しやすくなり、
１７０重量％を超えると、粘度が高くなりすぎる。In the flame-retardant epoxy resin composition of the present invention, hydrated alumina is used as a filler, but other fillers can be used in combination. Other fillers include ordinary fused silica, crystalline silica, talc, calcium carbonate, clay and the like. The amount of the hydrated alumina is preferably 150 to 170% by weight based on the epoxy resin, and when used in combination with other fillers, it is preferable that 80% by weight of the total filler be hydrated alumina. . When the amount of the hydrated alumina is less than 150% by weight based on the epoxy resin, the flame retardancy of the resin composition tends to decrease,
If it exceeds 170% by weight, the viscosity becomes too high.
【０００９】本発明に難燃性エポキシ樹脂組成物には、
さらに湿潤分散剤としてアルミニウムキレート化合物が
添加される。この湿潤分散剤は、難燃性エポキシ樹脂組
成物を低粘度化させる役割を有する。本発明に使用しう
るアルミニウムキレート化合物としては、例えば、下記
の式で示されるアルキルアセトアセテート・アルミニウ
ム・ジイソプロピレートなどが挙げられる。これらの市
販品としては、川研ファインケミカル(株)製アルミキレ
ートＭが挙げられる。The flame-retardant epoxy resin composition of the present invention comprises:
Further, an aluminum chelate compound is added as a wetting and dispersing agent. This wetting and dispersing agent has a role of reducing the viscosity of the flame-retardant epoxy resin composition. Examples of the aluminum chelate compound that can be used in the present invention include alkyl acetoacetate aluminum diisopropylate represented by the following formula. Examples of these commercially available products include aluminum chelate M manufactured by Kawaken Fine Chemical Co., Ltd.
【００１０】[0010]
【化１】 〔式中、Ｒはイソプロピル基を表し、Ｒ′はアルキル基
を表す〕Embedded image [Wherein, R represents an isopropyl group, and R ′ represents an alkyl group]
【００１１】湿潤分散剤の配合量は、組成物の低粘度化
の点からはエポキシ樹脂に対して１重量％以上であり、
より好ましくは１〜３重量％の範囲である。The compounding amount of the wetting and dispersing agent is 1% by weight or more based on the epoxy resin from the viewpoint of reducing the viscosity of the composition.
More preferably, it is in the range of 1 to 3% by weight.
【００１２】本発明の難燃性エポキシ樹脂組成物は、さ
らに硬化促進剤を含有することが好ましい。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メチルフェノール
等の第３級アミン類などが挙げられる。硬化促進剤の使
用量は、酸無水物１００重量部当たり０．１〜５．０重
量部の範囲が好ましい。The flame-retardant epoxy resin composition of the present invention preferably further contains a curing accelerator. Examples of the curing accelerator include 2-ethyl-4-methylimidazole, 1-cyanoethyl-4-methylimidazole,
Imidazole and its derivatives such as benzyl-2-ethylimidazole; and tertiary amines such as trisdimethylaminomethylphenol. The amount of the curing accelerator used is preferably in the range of 0.1 to 5.0 parts by weight per 100 parts by weight of the acid anhydride.
【００１３】本発明の難燃性エポキシ樹脂組成物には、
必要に応じてさらに、三酸化アンチモン、ベンガラ、酸
化第２鉄、カーボン、チタンホワイト等の着色剤、シラ
ン系あるいはチタン系カップリング剤、シリコーン系消
泡剤、モノグリシジルエーテル、ジグリシジルエーテル
等のエポキシ反応性希釈剤などを配合することができ
る。The flame-retardant epoxy resin composition of the present invention comprises:
If necessary, antimony trioxide, red iron oxide, ferric oxide, carbon, a coloring agent such as titanium white, a silane or titanium coupling agent, a silicone antifoaming agent, monoglycidyl ether, diglycidyl ether, etc. An epoxy reactive diluent or the like can be blended.
【００１４】本発明の難燃性エポキシ樹脂組成物は、高
い難燃性を有すると共に、絶縁処理時における操作性に
優れ、フライバックトランス、高圧トランス、電源トラ
ンス、スイッチングトランス、ソレノイドコイル等の電
気部品に、公知の方法によって含浸、注型して硬化する
ことにより、絶縁処理された電気部品を効率よく提供す
ることができる。The flame-retardant epoxy resin composition of the present invention has high flame retardancy and excellent operability at the time of insulation treatment, and is suitable for use in a flyback transformer, a high-voltage transformer, a power supply transformer, a switching transformer, a solenoid coil and the like. By impregnating, casting and hardening the component by a known method, an electrical component that has been subjected to insulation treatment can be efficiently provided.
【００１５】[0015]
【実施例】以下、本発明を実施例により詳しく説明する
が、本発明はこれらに限定されるものではない。The present invention will be described in more detail with reference to the following Examples, which should not be construed as limiting the invention thereto.
【００１６】実施例１〜２及び比較例１〜３ 表１に示す成分及び配合量で難燃性エポキシ樹脂組成物
を製造し、その粘度及び硬化物の難燃性を調べ、結果を
表１に示した。なお、難燃性エポキシ樹脂組成物は７０
℃で２．５時間、次いで１１０℃で２．５時間硬化させ
た。また、各特性は以下に示す方法により測定した。 （１）粘度：Ｂ型回転粘度計を用い、温度２５℃で測定
した。 （２）難燃性：ＵＬ９４に従って試験片厚み１．５８mm
（１／４インチ）の試料を作製して評価した。 なお、使用した成分は、下記のものである。 エポキシ樹脂：シェル化学(株)製、商品名ＥＰ−８２８ 水和アルミナ：住友化学工業(株)製、商品名Ｃ−３０８ 炭酸カルシウム：竹原化学工業(株)製、商品名ＳＬ−７
００ シリコーン系消泡剤：信越化学工業(株)製、商品名ＫＳ
−６０３ シランカップリング剤：東芝シリコーン(株)製、商品名
ＴＳＬ−８３５０ 湿潤分散剤：川研ファインケミカル(株)製、商品名アル
ミキレートＭ 酸無水物：日立化成工業(株)製、商品名ＨＮ−２０００ 硬化促進剤：四国化成工業(株)製、商品名２Ｅ４ＭＺExamples 1 and 2 and Comparative Examples 1 to 3 Flame-retardant epoxy resin compositions were prepared with the components and amounts shown in Table 1, and the viscosity and the flame retardancy of the cured product were examined. It was shown to. Incidentally, the flame-retardant epoxy resin composition is 70
Cured for 2.5 hours at 110 ° C, then 2.5 hours at 110 ° C. Each characteristic was measured by the following method. (1) Viscosity: Measured at a temperature of 25 ° C. using a B-type rotational viscometer. (2) Flame retardancy: test piece thickness 1.58 mm according to UL94
(1/4 inch) sample was prepared and evaluated. The components used are as follows. Epoxy resin: Shell Chemical Co., Ltd., trade name EP-828 Hydrated alumina: Sumitomo Chemical Co., Ltd., trade name C-308 Calcium carbonate: Takehara Chemical Co., Ltd., trade name SL-7
00 Silicone-based defoamer: KS, manufactured by Shin-Etsu Chemical Co., Ltd.
-603 Silane coupling agent: manufactured by Toshiba Silicone Co., Ltd., trade name: TSL-8350 Wetting dispersant: manufactured by Kawaken Fine Chemical Co., Ltd., trade name: Aluminum chelate M Acid anhydride: manufactured by Hitachi Chemical Co., Ltd., trade name HN-2000 curing accelerator: Shikoku Chemical Industry Co., Ltd. product name 2E4MZ
【００１７】[0017]
【表１】 [Table 1]
【００１８】表１から明らかなとおり、湿潤分散剤を１
〜２重量部加えた組成物（実施例１〜２）は、湿潤分散
剤を加えない組成物（比較例１）と異なり、低粘度で作
業性に優れている。また、湿潤分散剤の添加量が少なす
ぎると（比較例２）、粘度低下に著しい効果が見られ
ず、さらに、湿潤分散剤を添加せずに水和アルミナの添
加量を減らした組成物（比較例３）では、低粘度で作業
性は向上するが、難燃性はＶ−１に低下することが分か
る。As is clear from Table 1, 1
The composition (Examples 1 and 2) in which no more than 2 parts by weight was added, unlike the composition in which no wetting and dispersing agent was added (Comparative Example 1), had a low viscosity and excellent workability. On the other hand, when the addition amount of the wetting and dispersing agent is too small (Comparative Example 2), no remarkable effect on the viscosity reduction is observed, and further, a composition in which the addition amount of the hydrated alumina is reduced without adding the wetting and dispersing agent ( In Comparative Example 3), although the workability is improved at a low viscosity, the flame retardancy is reduced to V-1.
【００１９】[0019]
【発明の効果】本発明の難燃性エポキシ樹脂組成物は、
ハロゲン系難燃剤を含まないため、有害ガスの発生量が
少なく、また、難燃性はＵＬ９４試験においてＶ−０と
いう高いレベルを有し、さらに低粘度であるため作業性
に優れるものである。本発明の難燃性エポキシ樹脂組成
物は、フライバックトランス、高圧トランス、電源トラ
ンス、スイッチングトランス、ソレノイドコイルなどの
電気部品の含浸、注型用として広く用いることができ
る。The flame-retardant epoxy resin composition of the present invention comprises:
Since it does not contain a halogen-based flame retardant, the amount of harmful gas generated is small, and the flame retardancy has a high level of V-0 in the UL94 test, and the workability is excellent due to its low viscosity. INDUSTRIAL APPLICABILITY The flame-retardant epoxy resin composition of the present invention can be widely used for impregnating and casting electric components such as a flyback transformer, a high-voltage transformer, a power supply transformer, a switching transformer, and a solenoid coil.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｃ０８Ｋ 5:09 3:22 5:057） ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 6 Identification code FI C08K 5:09 3:22 5: 057)
Claims (3)
ナを含有するエポキシ樹脂組成物において、湿潤分散剤
としてアルミニウムキレート化合物をエポキシ樹脂に対
して１重量％以上添加した難燃性エポキシ樹脂組成物。1. A flame-retardant epoxy resin composition comprising an epoxy resin, an acid anhydride, and hydrated alumina, wherein an aluminum chelate compound as a wetting and dispersing agent is added in an amount of 1% by weight or more based on the epoxy resin. .
・アルミニウム・ジイソプロピレートである請求項１記
載の難燃性エポキシ樹脂組成物。2. The flame-retardant epoxy resin composition according to claim 1, wherein the wetting and dispersing agent is an alkyl acetoacetate aluminum diisopropylate.
脂組成物を用いて絶縁処理してなる電気部品。3. An electric component obtained by performing insulation treatment using the flame-retardant epoxy resin composition according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9348399A JPH11181243A (en) | 1997-12-18 | 1997-12-18 | Flame-retardant epoxy resin composition and electric parts using the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9348399A JPH11181243A (en) | 1997-12-18 | 1997-12-18 | Flame-retardant epoxy resin composition and electric parts using the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11181243A true JPH11181243A (en) | 1999-07-06 |
Family
ID=18396767
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9348399A Pending JPH11181243A (en) | 1997-12-18 | 1997-12-18 | Flame-retardant epoxy resin composition and electric parts using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11181243A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6706409B2 (en) | 2000-10-13 | 2004-03-16 | Hitachi Chemical Co., Ltd. | Incombustible resin composition, prepreg, laminated plate, metal-clad laminated plate, printed wiring board and multi-layer printed wiring board |
-
1997
- 1997-12-18 JP JP9348399A patent/JPH11181243A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6706409B2 (en) | 2000-10-13 | 2004-03-16 | Hitachi Chemical Co., Ltd. | Incombustible resin composition, prepreg, laminated plate, metal-clad laminated plate, printed wiring board and multi-layer printed wiring board |
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