JPS61218622A - Epoxy resin composition - Google Patents

Epoxy resin composition

Info

Publication number
JPS61218622A
JPS61218622A JP5945385A JP5945385A JPS61218622A JP S61218622 A JPS61218622 A JP S61218622A JP 5945385 A JP5945385 A JP 5945385A JP 5945385 A JP5945385 A JP 5945385A JP S61218622 A JPS61218622 A JP S61218622A
Authority
JP
Japan
Prior art keywords
epoxy resin
alumina
alumina particles
weight
resin composition
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.)
Granted
Application number
JP5945385A
Other languages
Japanese (ja)
Other versions
JPH0611844B2 (en
Inventor
Naoyuki Kokuni
小国 尚之
Min Tai Kao
ミン タイ カオ
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toshiba Corp
Original Assignee
Toshiba Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Toshiba Corp filed Critical Toshiba Corp
Priority to JP60059453A priority Critical patent/JPH0611844B2/en
Publication of JPS61218622A publication Critical patent/JPS61218622A/en
Publication of JPH0611844B2 publication Critical patent/JPH0611844B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Compositions Of Macromolecular Compounds (AREA)
  • Epoxy Resins (AREA)

Abstract

PURPOSE:The titled composition which provides a cured material having improved mechanical characteristics and crack resistance, and has improved fluidity, comprising epoxy sin, a curing agent and a mixture of alumina particles and alumina fibers in a specific ratio. CONSTITUTION:The aimed composition comprising (A) 100pts.wt. epoxy resin, (B) 8-120pts.wt. curing agent (e.g., phthalic anhydride, etc.), and (C) 100-500pts. wt., preferably 200-400pts.wt. mixture of alumina particles [preferably compris ing <20wt% alumina particles having >=30mu particle diameter and >=50wt% alumina particles having >=15mu particle diameter] and alumina fibers (preferably having 2-15mu diameter and 2-500mu length).

Description

【発明の詳細な説明】 〔発明の技術分野〕 本発明はエポキシ樹脂組成物に関し、さらに詳しくは、
エポキシ樹脂、硬化剤、並びにアルミナ粒子及びアルミ
ナ繊維よりなる流動性が良好なエポキシ樹脂組成物に関
するものである。
DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to an epoxy resin composition, and more particularly,
The present invention relates to an epoxy resin composition having good fluidity and comprising an epoxy resin, a curing agent, and alumina particles and alumina fibers.

〔発明の技術的背景とその問題点〕[Technical background of the invention and its problems]

エポキシ樹脂に、徨々の硬化剤及び充てん剤を配合し、
加熱硬化させることによって得られる硬化物は、電気機
器用絶縁物として広く使用されている。このエポキシ樹
脂硬化物は六フフ化イオウよシ発生する分解ガスへの耐
性9機械的特性、及び耐クラツク性などの、物理的、化
学的性質が優れていることが要求される。
Mixing various curing agents and fillers with epoxy resin,
Cured products obtained by heating and curing are widely used as insulators for electrical equipment. This cured epoxy resin is required to have excellent physical and chemical properties such as resistance to sulfur hexafluoride and decomposition gases generated, mechanical properties, and crack resistance.

従来エポキシ樹脂硬化物の物理的、化学的性質を向上さ
せる目的で、充てん剤として、ガラス繊維等の無機繊維
質のものが使用されている。しかし一般に、エポキシ樹
脂には種々の目的でアルミナ等の無機質の粉末が充てん
剤として使用されているが、これに更に補強のために繊
維質の充てん剤を使用すると、組成物の粘度が著しく増
大し流動性が劣るのでエポキシ樹脂組成物の効果的な注
型が困難であった。
Conventionally, inorganic fibers such as glass fibers have been used as fillers for the purpose of improving the physical and chemical properties of cured epoxy resin products. However, in general, inorganic powders such as alumina are used as fillers in epoxy resins for various purposes, but when fibrous fillers are used for reinforcement, the viscosity of the composition increases significantly. However, since the fluidity is poor, effective casting of the epoxy resin composition has been difficult.

〔発明の目的〕[Purpose of the invention]

本発明は流動性が良好であシ注型作業性が良好なエポキ
シ樹脂組成物の提供を目的とする。
The object of the present invention is to provide an epoxy resin composition that has good fluidity and good casting workability.

〔発明の概要〕[Summary of the invention]

本発明は、エポキシ樹脂、硬化剤並びに特定の粒度を有
するアルミナ粒子及び特定の直径と長さを有するアルミ
ナ繊維よシなるエポキシ樹脂組成物に関するものである
The present invention relates to an epoxy resin composition comprising an epoxy resin, a curing agent, and alumina particles having a specific particle size and alumina fibers having a specific diameter and length.

本発明に使用されるエポキシ樹脂は、通常、エポキシ樹
脂として公知のものであればいかなるものであってもよ
い。この樹脂の具体例としては、ビスフェノールAジグ
リシジルエーテル及びその二量体、二量体、ノボラック
型フェノール樹脂とエピクロルヒドリンとから得られる
エポキシ樹脂、多価アルコールやポリアルキレンオキシ
ドとエピクロルヒドリンとから得られるエポキシ樹脂、
シクロヘキセンオキシド基を含むエポキシ樹脂が挙げら
れる。
The epoxy resin used in the present invention may be of any type as long as it is generally known as an epoxy resin. Specific examples of this resin include bisphenol A diglycidyl ether and its dimer, dimer, epoxy resin obtained from novolac type phenol resin and epichlorohydrin, and epoxy resin obtained from polyhydric alcohol or polyalkylene oxide and epichlorohydrin. resin,
Examples include epoxy resins containing cyclohexene oxide groups.

本発明に使用される硬化剤は、通常、エポキシ樹脂の硬
化剤として公知のものであればいかなるものであっても
よい。この硬化剤の具体例としては、無水7タル酸、ヘ
キサヒドロ無水7タル酸、テトラヒドロ無水フタル酸、
メチル−ヘキサヒドロ無水7タル酸、メチル−テトラヒ
ドロ無水7タル酸、メチル−無水ナジック散、ドデセニ
ル無水コハク駿、無水ピロメリット酸等の酸無水物;ト
リエチレンテトラミン、メタフェニレンジアミン、トリ
ス(ジメチルアミノメチル)フェノール等のアミン類;
ジシアンジアミド;三7ツ化ホウ素−アミン錯体;イミ
ダゾール等が挙げられ、これらから成る群よシ選ばれる
1種もしくは2種以上の混合系で使用される。
The curing agent used in the present invention may be any known curing agent for epoxy resins. Specific examples of this curing agent include 7-talic anhydride, hexahydroheptalic anhydride, tetrahydrophthalic anhydride,
Acid anhydrides such as methyl-hexahydro-7-talic anhydride, methyl-tetrahydro-7-talic anhydride, methyl-Nadic anhydride, dodecenyl succinic anhydride, pyromellitic anhydride; triethylenetetramine, meta-phenylenediamine, tris(dimethylaminomethyl) ) Amines such as phenol;
Examples include dicyandiamide; boron trisulfide-amine complex; imidazole, etc., and one type or a mixture of two or more types selected from the group consisting of these can be used.

本発明に使用されるアルミナ粒子は、粒径が30βm以
上のものがアルミナ粒子全体の20重量%未満でかつ1
5μm以下のものが50重量%以上の粒度分布を有する
粒子である。粒度分布が上記の範囲を外れる場合には本
発明によるアルミナ繊維と併用した場合、極めて大きな
粘度上昇を招くかあるいは機械的特性の向上がほとんど
なくなる。
The alumina particles used in the present invention have a particle size of 30βm or more, which accounts for less than 20% by weight of the total alumina particles, and 1
Particles having a particle size distribution of 50% by weight or more are particles having a diameter of 5 μm or less. If the particle size distribution is outside the above range, when used in combination with the alumina fibers according to the present invention, either a very large increase in viscosity will result or there will be little improvement in mechanical properties.

本発明に使用されるアルミナ繊維は、直径が2〜15μ
mで長さが2〜500μmの繊維である。
The alumina fiber used in the present invention has a diameter of 2 to 15 μm.
The fibers have a length of 2 to 500 μm.

繊維の直径および長さが上記範囲を外れる場合には、粘
度が高くなシ注型作業に不適となる。かかるアルミナ繊
維としてはサフイル(アイ・シー会アイ社製)、ネクス
テル(スリー・エム社製) 、 MAF(三菱化成社製
ンの他ファイバーマックス(東芝モノ7ラツクス社展)
、アルセン(電気化学工業社製)などのセラミックファ
イバーを例えばボールミルで粉砕後、分級して所望の長
さのものを使用してもよい。(a)エポキシ樹脂とφ)
硬化剤の配合割合はエポキシ樹脂100重量部に対して
硬化剤8〜200重量部である。(C−1)アルミナ粒
子及び(C−2)アルミナ繊維の配合量は組成物の用途
又は要求特性に応じて異なるが通常間成分の混合物とし
てエポキシ樹脂100重量部に対して、100〜500
重量部、好ましくは200〜400重量部が用いられる
。100重量部未満ではアルミナ粒子及びアルミナ繊維
が沈降し均一に分散せず、500重量部以上では粘度が
極めて高くなシ充てんが困難である。
If the diameter and length of the fibers are outside the above ranges, the fibers will have a high viscosity and will be unsuitable for casting operations. Such alumina fibers include Safil (manufactured by IC Corporation), Nextel (manufactured by 3M Corporation), MAF (manufactured by Mitsubishi Kasei Corporation), and Fibermax (manufactured by Toshiba Mono7 Lux Co., Ltd.).
For example, ceramic fibers such as Alsene (manufactured by Denki Kagaku Kogyo Co., Ltd.) may be pulverized with a ball mill, and then classified to use those having a desired length. (a) Epoxy resin and φ)
The mixing ratio of the curing agent is 8 to 200 parts by weight per 100 parts by weight of the epoxy resin. The blending amounts of (C-1) alumina particles and (C-2) alumina fibers vary depending on the use or required properties of the composition, but are usually 100 to 500 parts by weight per 100 parts by weight of the epoxy resin as a mixture of the components.
Parts by weight are used, preferably from 200 to 400 parts by weight. If it is less than 100 parts by weight, the alumina particles and alumina fibers will settle and will not be uniformly dispersed, and if it is more than 500 parts by weight, the viscosity will be extremely high and filling will be difficult.

アルミナ粒子及びアルミナ繊維の配合比は使用するアル
ミナ粒子の粒度分布、及びアルミナ繊維の直径と長さに
基づき流動性及び硬化物に対する要求特性に応じて適宜
選択されるが’0−”/(C−1)+(C−21が重量
比で帆1〜0.8、好ましくは0.2〜0.7の範囲内
である。0.1未満では硬化物の耐クラツク性の改善効
果が微弱であ!り 0.8を越えると組成物の粘度が高
くなシ過ぎ注型作業が困難となる。
The blending ratio of alumina particles and alumina fibers is appropriately selected depending on the particle size distribution of the alumina particles used, the diameter and length of the alumina fibers, and the fluidity and required properties of the cured product. -1) + (C-21 weight ratio is within the range of 1 to 0.8, preferably 0.2 to 0.7. If it is less than 0.1, the effect of improving the crack resistance of the cured product is weak. If the value exceeds 0.8, the viscosity of the composition becomes too high and the casting operation becomes difficult.

本発明のエポキシ樹脂組成物には、本発明の効果を損な
わない範囲内で、必要に応じ一般に用られている粒径の
アルミナ粒子、耐大7ツ化イオウ分解ガス性のマグネシ
ウム、カルシウム、バリウム、アルミニウムの7ツ化物
、硫酸塩、炭酸塩、ドロマイト粉末、酸化チタン粉末の
他、有機、無機の着色剤。
The epoxy resin composition of the present invention may contain alumina particles of commonly used particle sizes, large sulfur heptadide decomposition gas-resistant magnesium, calcium, barium, etc., as necessary, within a range that does not impair the effects of the present invention. , aluminum heptadide, sulfate, carbonate, dolomite powder, titanium oxide powder, as well as organic and inorganic colorants.

シランカッグリン剤等の表面改質剤、イミダール系、三
級アミン系、金属錯体系等の硬化促進剤等の添加剤を適
宜配合しても曳い。
Additives such as surface modifiers such as silane cagulin agents, curing accelerators such as imidal-based, tertiary amine-based, and metal complex-based agents may be appropriately blended.

本発明のエポキシ樹脂組成物の製造方法は特に限定され
ず各成分を適当な方法、例えば万能混合機等の混合機に
投入し均一となるように、混合、撹拌すればよい。
The method for producing the epoxy resin composition of the present invention is not particularly limited, and each component may be put into a mixer such as an all-purpose mixer and mixed and stirred uniformly.

本発明のエポキシ樹脂組成物は種々の電気機器用絶縁物
、特に六7ツ化イオウ絶縁電気機器用固体絶縁物の製造
原料として使用される。
The epoxy resin composition of the present invention is used as a raw material for producing various insulators for electrical equipment, particularly solid insulators for electrical equipment insulated with sulfur hexa7tide.

〔発明の効果〕〔Effect of the invention〕

本発明のエポキシ樹脂組成物は、流動性がよいためその
注型作業が容易となり、又従来品に比して充てん材を多
量に配合することができるため製造コストを低減するこ
とができる。
The epoxy resin composition of the present invention has good fluidity, which facilitates the casting operation, and allows for the inclusion of a larger amount of filler than in conventional products, thereby reducing manufacturing costs.

〔発明の実施例及び試験例〕[Examples and test examples of the invention]

実施例1 表2に示す各成分を万能混合機((株〕三英製作所社表
ンに投入し、混合撹拌し、本発明の組成物380F(本
発明品1)を得た。
Example 1 Each component shown in Table 2 was put into a universal mixer (Sanei Seisakusho Co., Ltd.) and mixed and stirred to obtain Composition 380F of the present invention (Product 1 of the present invention).

実施例2及び3 表2に示する各成分を、実施例1と同様に処理し、各々
本発明の組成物3802 (本発明品2及び3)を得た
Examples 2 and 3 Each component shown in Table 2 was treated in the same manner as in Example 1 to obtain composition 3802 of the present invention (present invention products 2 and 3).

試験例 表2に示す各成分を実施例1と同様に処理し比較品1.
2及び3各々3802を得た。
Test Example Each component shown in Table 2 was treated in the same manner as in Example 1, and a comparative product 1.
3802 each of 2 and 3 were obtained.

本発明品1.2及び3、ならびに比較品1.2及び3を
原料としこれを十分混合脱気後、所定の金型へ真空注型
し、115℃で10時間、さらに130°℃で15時間
加熱し、本発明品の硬化物4゜5及び6ならびに比較品
の硬化物4,5及び6を得た。
Inventive products 1.2 and 3 and comparative products 1.2 and 3 were used as raw materials, and after thorough mixing and degassing, the mixture was vacuum cast into a predetermined mold, heated to 115°C for 10 hours, and further heated to 130°C for 15 hours. After heating for a period of time, cured products 4.5 and 6 of the present invention and cured products 4, 5 and 6 of comparative products were obtained.

さらに、本発明品1.2及び3ならびに比較品1.2、
及び3を用いて流動性を試験した。
Furthermore, the present invention products 1.2 and 3 and the comparative product 1.2,
and 3 were used to test the flowability.

流動性は本発明品1,2及び3ならびに比較品1.2及
び3を脱気後、所定の金型へ自重を利用して注ぐ時の粘
性および注型後真空脱泡する時の作業性を目測によル判
定した。◎印は粘性が低く注型後の脱泡が容易、Δ印は
注型はできるが真空脱泡が不可、X印は注型が不可能で
あることをそれぞれ示す。
Fluidity is determined by the viscosity when inventive products 1, 2, and 3 and comparative products 1.2 and 3 are poured into a predetermined mold using their own weight after degassing, and the workability when vacuum degassing is performed after casting. was determined by visual inspection. The mark ◎ indicates that the viscosity is low and defoaming after casting is easy, the mark Δ indicates that casting is possible but vacuum defoaming is not possible, and the mark X indicates that casting is impossible.

本発明品の硬化物4,5及び6ならびに比較品の硬化物
4,5及び6t−用いて機械的特性及び耐クラツク性を
試験した。機械的特性は曲げ強さとして、JIS  K
−6911に規定されている方法によシ測定した。
The cured products 4, 5 and 6 of the invention and the comparative cured products 4, 5 and 6t were used to test mechanical properties and crack resistance. Mechanical properties are determined by JIS K as bending strength.
-6911.

耐クラツク性は厚さ0.64αのオリファントワッシャ
ーを埋め込んだ円板状の硬化物試験片を急熱急冷し、硬
化物層にクラックが発生するか否かを調べて、硬化物の
耐熱衝撃性を評価する方法、すなわち、オリファントワ
ッシャー試験法によった。すなわち、表1に示す冷熱サ
イクルを硬化物に与え、試験片にクラックが発生したと
きのサイクル番号の算術平均値を耐クラツク指数として
示したものである。従って耐クラツク指数の大きな硬化
物はど耐クラツク性(耐熱衝撃性)が優れていることを
示している。
Crack resistance was determined by rapidly heating and rapidly cooling a disc-shaped cured product test piece with an oliphant washer embedded in it with a thickness of 0.64α, and examining whether or not cracks occurred in the cured product layer. was evaluated using the Oliphant washer test method. That is, the cured product was subjected to the cooling and heating cycles shown in Table 1, and the arithmetic mean value of the cycle numbers at which cracks occurred in the test piece was shown as the crack resistance index. This indicates that a cured product with a large crack resistance index has excellent crack resistance (thermal shock resistance).

〔発明の結果〕[Results of the invention]

表2に示す結果よシ明らかなとおシ本発明品は流動性に
おいて比較品よシ優れていた。
As is clear from the results shown in Table 2, the product of the present invention was superior to the comparative product in fluidity.

又、表3に示す結果よシ明らかなとおシ、本発明品の硬
化物は機械的特性及び耐クラツク性において比較品の硬
化物よシ優れていた。
Further, as is clear from the results shown in Table 3, the cured products of the present invention were superior to the cured products of the comparative product in terms of mechanical properties and crack resistance.

表  1 (注)高温側(25℃):25〜30℃に保たれた熱風
循環式恒温槽中に試験片を30分保持
Table 1 (Note) High temperature side (25℃): Hold the test piece for 30 minutes in a hot air circulation constant temperature bath maintained at 25 to 30℃.

Claims (1)

【特許請求の範囲】 1、(a)エポキシ樹脂100重量部、(b)硬化剤8
〜120重量部及びアルミナ粒子とアルミナ繊維の混合
物100〜500重量部よりなることを特徴とするエポ
キシ樹脂組成物。 2、アルミナ粒子が粒径30μm以上のものを該アルミ
ナ粒子全体の20重量%未満、かつ15μm以上のもの
を50重量%以上含有するものであり、アルミナ繊維が
直径2〜15μmでかつ長さが2〜500μmのもので
ある特許請求の範囲第1項記載のエポキシ樹脂組成物。 3、アルミナ粒子及びアルミナ繊維混合物全体に対する
アルミナ粒子の配合比が、重量で、0.1〜0.8であ
る特許請求の範囲第1項記載のエポキシ樹脂組成物。
[Claims] 1. (a) 100 parts by weight of epoxy resin, (b) curing agent 8
-120 parts by weight and 100-500 parts by weight of a mixture of alumina particles and alumina fibers. 2. The alumina particles contain less than 20% by weight of the total alumina particles having a particle size of 30 μm or more, and 50% by weight or more of the alumina particles having a particle size of 15 μm or more, and the alumina fibers have a diameter of 2 to 15 μm and a length of The epoxy resin composition according to claim 1, which has a diameter of 2 to 500 μm. 3. The epoxy resin composition according to claim 1, wherein the blending ratio of alumina particles to the entire alumina particle and alumina fiber mixture is 0.1 to 0.8 by weight.
JP60059453A 1985-03-26 1985-03-26 Composition for electrical equipment insulation Expired - Lifetime JPH0611844B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP60059453A JPH0611844B2 (en) 1985-03-26 1985-03-26 Composition for electrical equipment insulation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP60059453A JPH0611844B2 (en) 1985-03-26 1985-03-26 Composition for electrical equipment insulation

Publications (2)

Publication Number Publication Date
JPS61218622A true JPS61218622A (en) 1986-09-29
JPH0611844B2 JPH0611844B2 (en) 1994-02-16

Family

ID=13113732

Family Applications (1)

Application Number Title Priority Date Filing Date
JP60059453A Expired - Lifetime JPH0611844B2 (en) 1985-03-26 1985-03-26 Composition for electrical equipment insulation

Country Status (1)

Country Link
JP (1) JPH0611844B2 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5747557A (en) * 1993-08-20 1998-05-05 Kabushiki Kaisha Toshiba Method of manufacturing a castable epoxy resin composition comprising acrylic rubber particles predispersed in an anhydride hardener
WO2007142262A1 (en) * 2006-06-07 2007-12-13 Sumitomo Chemical Company, Limited Epoxy resin composition and cured epoxy resin
JP2008013759A (en) * 2006-06-07 2008-01-24 Sumitomo Chemical Co Ltd Epoxy resin composition and epoxy resin cured product

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5961211A (en) * 1982-09-29 1984-04-07 Toshiba Corp Surface acoustic wave device
JPS59201510A (en) * 1983-04-28 1984-11-15 Mitsubishi Electric Corp Attenuation circuit with phase inverting control
JPS59201964A (en) * 1983-04-30 1984-11-15 Kiyousan Denki Kk Diaphragm type fuel pump
JPS60110755A (en) * 1983-11-21 1985-06-17 Matsushita Electric Works Ltd Resin composition for casting

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5961211A (en) * 1982-09-29 1984-04-07 Toshiba Corp Surface acoustic wave device
JPS59201510A (en) * 1983-04-28 1984-11-15 Mitsubishi Electric Corp Attenuation circuit with phase inverting control
JPS59201964A (en) * 1983-04-30 1984-11-15 Kiyousan Denki Kk Diaphragm type fuel pump
JPS60110755A (en) * 1983-11-21 1985-06-17 Matsushita Electric Works Ltd Resin composition for casting

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5747557A (en) * 1993-08-20 1998-05-05 Kabushiki Kaisha Toshiba Method of manufacturing a castable epoxy resin composition comprising acrylic rubber particles predispersed in an anhydride hardener
WO2007142262A1 (en) * 2006-06-07 2007-12-13 Sumitomo Chemical Company, Limited Epoxy resin composition and cured epoxy resin
JP2008013759A (en) * 2006-06-07 2008-01-24 Sumitomo Chemical Co Ltd Epoxy resin composition and epoxy resin cured product

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