JPH0812741A - Liquid epoxy resin composition - Google Patents
Liquid epoxy resin compositionInfo
- Publication number
- JPH0812741A JPH0812741A JP6152019A JP15201994A JPH0812741A JP H0812741 A JPH0812741 A JP H0812741A JP 6152019 A JP6152019 A JP 6152019A JP 15201994 A JP15201994 A JP 15201994A JP H0812741 A JPH0812741 A JP H0812741A
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- JP
- Japan
- Prior art keywords
- epoxy resin
- resin composition
- weight
- parts
- liquid epoxy
- 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)
- Epoxy Resins (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- Organic Insulating Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、液状エポキシ樹脂組成
物に関する。この液状エポキシ樹脂組成物は、低粘度で
含浸性が良好であり、当該樹脂組成物から得られる硬化
物は、耐熱性、耐湿性、電気絶縁性に優れ、コイル、フ
ィルムコンデンサ等の電気、電子部品の含浸剤として好
適である。FIELD OF THE INVENTION The present invention relates to a liquid epoxy resin composition. This liquid epoxy resin composition has a low viscosity and good impregnability, and a cured product obtained from the resin composition has excellent heat resistance, moisture resistance, and electrical insulation properties, and can be used for electrical and electronic applications such as coils and film capacitors. It is suitable as an impregnating agent for parts.
【０００２】[0002]
【従来の技術】エポキシ樹脂は、優れた電気絶縁性、機
械強度、耐熱性、耐湿性、接着性等の材料特性を有して
いることから電気、電子部品の電気絶縁用材料として用
いられている。2. Description of the Related Art Epoxy resin is used as a material for electrical insulation of electric and electronic parts because it has excellent material properties such as electrical insulation, mechanical strength, heat resistance, moisture resistance and adhesiveness. There is.
【０００３】かかる用途に使用されるエポキシ樹脂組成
物は、優れた耐電圧性、電気絶縁性を必要とされる結
果、通常、無溶剤型の組成物が使用されており、更に含
浸性を向上させるためには低粘度で、且つ高耐熱性であ
ることが望まれる。Epoxy resin compositions used for such applications are required to have excellent withstand voltage and electrical insulation properties, and as a result, solventless compositions are usually used, and the impregnation property is further improved. In order to achieve this, it is desired that the viscosity be low and the heat resistance be high.
【０００４】従来、エポキシ樹脂組成物の粘度を低下さ
せる目的で、ブチルグリシジルエーテル、フェニルグリ
シジルエーテル等のモノグリシジルエーテル、１，６−
ヘキサンジオールジグリシジルエーテル、ネオデカン酸
グリシジルエステル等、各種のエポキシ樹脂希釈剤が提
案されており、かかるエポキシ樹脂希釈剤を配合してな
るエポキシ樹脂組成物の粘度（２５℃）は３５０〜４０
０ｃｐｓ程度であり、又、ガラス転移温度（Ｔｇ）は１
００〜１０５℃程度である。Conventionally, for the purpose of lowering the viscosity of epoxy resin compositions, monoglycidyl ethers such as butyl glycidyl ether and phenyl glycidyl ether, 1,6-
Various epoxy resin diluents such as hexanediol diglycidyl ether and neodecanoic acid glycidyl ester have been proposed, and the viscosity (25 ° C.) of the epoxy resin composition containing the epoxy resin diluent is 350 to 40.
0 cps and glass transition temperature (Tg) is 1
It is about 00 to 105 ° C.
【０００５】しかしながら、上記エポキシ樹脂希釈剤
は、エポキシ樹脂組成物の粘度を低減することに対して
は一定の効果を示すものの、当該エポキシ樹脂組成物の
硬化物は、耐熱性が著しく低下したり、耐湿性、機械強
度、電気特性等が十分でない等の問題があった。However, although the above-mentioned epoxy resin diluent has a certain effect in reducing the viscosity of the epoxy resin composition, the cured product of the epoxy resin composition has a significantly reduced heat resistance. However, there are problems such as insufficient moisture resistance, mechanical strength, and electrical characteristics.
【０００６】従って、コンデンサの長期使用の信頼性を
改良するためには、優れた耐熱性（高Ｔｇ）を維持しつ
つ、従来以上にエポキシ樹脂組成物の低粘度化を図るこ
とが強く要求されている。Therefore, in order to improve the reliability of long-term use of the capacitor, it is strongly required to lower the viscosity of the epoxy resin composition more than ever while maintaining excellent heat resistance (high Tg). ing.
【０００７】[0007]
【発明が解決しようとする課題】本発明は、低粘度で、
使用時に各種部品に良好な含浸性を有し、しかも硬化性
を低下することなく、優れた耐熱性、耐電圧性、電気絶
縁性、耐湿性、機械強度、接着性を具備する液状エポキ
シ樹脂組成物を提供することを目的とする。The present invention has a low viscosity,
A liquid epoxy resin composition that has good impregnation properties for various parts during use, and has excellent heat resistance, voltage resistance, electrical insulation, moisture resistance, mechanical strength, and adhesiveness without decreasing curability. The purpose is to provide things.
【０００８】[0008]
【課題を解決するための手段】本発明者らは、上記課題
を解決すべく鋭意検討した結果、特定のエポキシ系化合
物をエポキシ樹脂希釈剤として所定量適用することによ
り、所期の目的が達成されることを見いだし、かかる知
見に基づいて本発明を完成するに至った。Means for Solving the Problems As a result of intensive studies to solve the above problems, the present inventors achieved a desired object by applying a predetermined amount of a specific epoxy compound as an epoxy resin diluent. The present invention has been completed, and the present invention has been completed based on such findings.
【０００９】即ち、本発明に係る液状エポキシ樹脂組成
物は、エポキシ樹脂１００重量部に対し、１，４−シク
ロヘキサンジメタノールジグリシジルエーテル５０〜１
５０重量部、酸無水物系硬化剤をエポキシ基の合計当量
に対し０．８〜１．１当量及び硬化促進剤０．１〜５重
量部含有することを特徴とする。That is, the liquid epoxy resin composition according to the present invention contains 50-1 parts of 1,4-cyclohexanedimethanol diglycidyl ether per 100 parts by weight of the epoxy resin.
It is characterized by containing 50 parts by weight, 0.8 to 1.1 equivalents of an acid anhydride type curing agent with respect to the total equivalents of epoxy groups, and 0.1 to 5 parts by weight of a curing accelerator.
【００１０】本発明に係るエポキシ樹脂としては、液状
ビスフェノールＡ型エポキシ樹脂、ビスフェノールＦ型
エポキシ樹脂等が例示され、必要に応じてフェノールノ
ボラックエポキシ樹脂、クレゾールノボラックエポキシ
樹脂等のグリシジルエーテル型、グリシジルエステル型
エポキシ樹脂、グリシジルアミン型エポキシ樹脂、ハロ
ゲン化エポキシ樹脂等を混合して使用することができ
る。特に液状ビスフェノールＡ型グリシジルエーテル、
ビスフェノールＦ型グリシジルエーテル等が推奨され
る。Examples of the epoxy resin according to the present invention include liquid bisphenol A type epoxy resin and bisphenol F type epoxy resin. If necessary, glycidyl ether type glycidyl ester such as phenol novolac epoxy resin and cresol novolac epoxy resin may be used. Type epoxy resin, glycidyl amine type epoxy resin, halogenated epoxy resin and the like can be mixed and used. Liquid bisphenol A type glycidyl ether,
Bisphenol F-type glycidyl ether is recommended.
【００１１】本発明において、エポキシ樹脂希釈剤とし
て適用される１，４−シクロヘキサンジメタノールジグ
リシジルエーテルは、１，４−シクロヘキサンジメタノ
ールとエピクロルヒドリンとを５０〜１５０℃程度の加
熱下に脱塩酸して調製されるエポキシ系化合物である。In the present invention, 1,4-cyclohexanedimethanol diglycidyl ether applied as an epoxy resin diluent dehydrochlorinates 1,4-cyclohexanedimethanol and epichlorohydrin under heating at about 50 to 150 ° C. It is an epoxy compound prepared by.
【００１２】１，４−シクロヘキサンジメタノールジグ
リシジルエーテルの配合量としては、エポキシ樹脂１０
０重量部に対して５０〜１５０重量部、より好ましくは
８０〜１１０重量部が推奨される。５０重量部未満では
含浸性を改良できる程の粘度低下が得られにくく、１５
０重量部を越えて配合した場合にはエポキシ樹脂硬化剤
の耐熱性が低下して目的とする硬化物の特性が得られに
くい。The compounding amount of 1,4-cyclohexanedimethanol diglycidyl ether is epoxy resin 10
50 to 150 parts by weight, more preferably 80 to 110 parts by weight, is recommended for 0 parts by weight. If the amount is less than 50 parts by weight, it is difficult to obtain a viscosity decrease enough to improve the impregnability,
When the amount is more than 0 parts by weight, the heat resistance of the epoxy resin curing agent is lowered and it is difficult to obtain the desired properties of the cured product.
【００１３】本発明に使用される酸無水物系硬化剤とし
ては、ヘキサヒドロ無水フタル酸、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、ヘキ
サヒドロ無水フタル酸、メチルナジック酸無水物等の酸
無水物硬化剤が推奨され、それぞれ単独で又は２種以上
を適宜組み合わせて適用される。Examples of the acid anhydride curing agent used in the present invention include acid anhydrides such as hexahydrophthalic anhydride, methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride and methylnadic acid anhydride. A material curing agent is recommended, and each is applied alone or in an appropriate combination of two or more kinds.
【００１４】当核酸無水物系硬化剤の配合量としては、
エポキシ樹脂及び１，４−シクロヘキサンジメタノール
ジグリシジルエーテルに起因するエポキシ基の合計当量
に対して０．８〜１．１倍当量が推奨される。０．８当
量未満又は１．１当量を越えて配合した場合には耐湿
性、耐熱性、機械強度等の特性が低下し、いずれの場合
も好ましくない。The content of the nucleic acid anhydride-based curing agent is as follows:
0.8 to 1.1 times equivalents are recommended with respect to the total equivalents of epoxy groups resulting from the epoxy resin and 1,4-cyclohexanedimethanol diglycidyl ether. If the amount is less than 0.8 equivalent or more than 1.1 equivalent, the properties such as moisture resistance, heat resistance and mechanical strength are deteriorated, which is not preferable.
【００１５】又、硬化促進剤としては、従来から使用さ
れている各種の硬化促進剤を使用することができ、より
具体的には、ベンジルジメチルアミン、トリス（ジメチ
ルアミノメチル）フェノール、ジメチルシクロヘキシル
アミン等の第３級アミン類、２−エチル−４−メチルイ
ミダゾール、２−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類、１，８−
ジアザビシクロ（５，４，０）ウンデセン−７等のジア
ザビシクロアルケン類及びそれらの２−エチルヘキサン
酸塩等の塩類、オクチル酸亜鉛、オクチル酸錫、アルミ
ニウムエチルアセトン錯体等の有機金属化合物、第４級
アンモニウム化合物、トリフェニルフォスフィン等の有
機フォスフィン化合物が例示される。As the curing accelerator, various conventionally used curing accelerators can be used, and more specifically, benzyldimethylamine, tris (dimethylaminomethyl) phenol, dimethylcyclohexylamine. And the like tertiary amines, 2-ethyl-4-methylimidazole, 2-methylimidazole, 1-benzyl-
Imidazoles such as 2-ethylimidazole, 1,8-
Diazabicycloalkenes such as diazabicyclo (5,4,0) undecene-7 and salts thereof such as 2-ethylhexanoate, zinc octylate, tin octylate, organometallic compounds such as aluminum ethylacetone complex, Examples thereof include quaternary ammonium compounds and organic phosphine compounds such as triphenylphosphine.
【００１６】硬化促進剤の添加量としては、エポキシ樹
脂１００重量部に対して０．１〜５重量部、好ましくは
０．５〜２重量部が推奨される。０．１重量部未満では
硬化に長時間を要し、作業性が低下し実用的でない。一
方、５重量部を越えて配合した場合には硬化時の発熱が
大きく硬化物の特性低下につながる。The amount of the curing accelerator added is recommended to be 0.1 to 5 parts by weight, preferably 0.5 to 2 parts by weight, based on 100 parts by weight of the epoxy resin. If the amount is less than 0.1 parts by weight, it takes a long time to cure and the workability is deteriorated, which is not practical. On the other hand, when the amount is more than 5 parts by weight, the heat generated during curing is large and the properties of the cured product deteriorate.
【００１７】本発明に係る液状エポキシ樹脂組成物を調
製する方法としては、公知の方法で行うことができる。
例えば、所定量のエポキシ樹脂、エポキシ樹脂希釈剤、
酸無水物系硬化剤、硬化促進剤及び必要に応じて難燃
剤、顔料、染料、カップリング剤、表面改質剤等を適宜
配合し、一般的な攪拌機を用いて均一混合する方法が挙
げられる。The liquid epoxy resin composition according to the present invention can be prepared by a known method.
For example, a predetermined amount of epoxy resin, epoxy resin diluent,
An acid anhydride-based curing agent, a curing accelerator, and optionally a flame retardant, a pigment, a dye, a coupling agent, a surface modifier, etc. may be appropriately mixed, and a method of uniformly mixing using a general stirrer may be mentioned. .
【００１８】かくして得られる液状エポキシ樹脂組成物
が含浸剤として適用される電子部品としては、ソレノイ
ドコイル、モーターのステーター、計測器用コイル
（Ｐ．Ｔ、Ｃ．Ｔ）等のコイル、ガラスクロス、プラス
チック不織布等の絶縁基材及びＤＣ用又はＡＣ用のフィ
ルムコンデンサ等が例示され、中でもフィルムコンデン
サが推奨される。The electronic parts to which the liquid epoxy resin composition thus obtained is applied as an impregnating agent include solenoid coils, motor stators, coils for measuring instruments (PT, CT), etc., glass cloth, plastics. Examples include insulating substrates such as non-woven fabrics and film capacitors for DC or AC, among which film capacitors are recommended.
【００１９】本発明に係る液状エポキシ樹脂組成物のフ
ィルムコンデンサに対する含浸方法としては、常温で減
圧下（例えば、１０〜３０mmHg程度）に含浸する方法や
予めコンデンサを１００〜１３０℃に加熱し、次いで２
０〜５０℃程度の液状エポキシ樹脂組成物中に浸漬して
含浸する方法等が挙げられる。The liquid epoxy resin composition according to the present invention may be impregnated into a film capacitor by impregnating the film capacitor under reduced pressure (for example, about 10 to 30 mmHg) at room temperature or by heating the capacitor to 100 to 130 ° C. in advance and then Two
Examples thereof include a method of immersing and impregnating in a liquid epoxy resin composition at about 0 to 50 ° C.
【００２０】[0020]
【実施例】以下に実施例を揚げ、本発明を詳しく説明す
る。尚、各例におけるエポキシ樹脂組成物の物理的特性
（粘度とガラス転移温度との相関）及びコンデンサ特性
特性（静電容量変化率、誘電正接、絶縁抵抗）は以下の
方法により測定し、評価した。EXAMPLES The present invention will be described in detail with reference to the following examples. The physical characteristics (correlation between viscosity and glass transition temperature) and capacitor characteristic characteristics (rate of change in capacitance, dielectric loss tangent, insulation resistance) of the epoxy resin composition in each example were measured and evaluated by the following methods. .
【００２１】エポキシ樹脂組成物の物理的特性 エポキシ樹脂組成物の粘度とガラス転移温度とは、一般
に正の相関を有する（即ち、希釈剤の作用により樹脂組
成物の粘度が低下するに従って、ガラス転移温度が低下
する。）。今般の物理的特性の評価においては、実用的
なガラス転移温度（１００℃又は１１０℃）に相当する
粘度をそれらの相関図より求め、そのときの粘度の大小
でもって当該樹脂組成物の含浸性を評価した（即ち、低
粘度であるほど含浸性に優れる）。尚、粘度（ｃｐｓ）
は、Ｂ型粘度計を用いて、２５℃で測定する。又、ガラ
ス転移温度（Ｔｇ、℃）は、１２０℃×５時間の硬化条
件下で得た硬化物のＴｇをＤＳＣ法に基づいて測定す
る。Physical Properties of Epoxy Resin Composition The viscosity of the epoxy resin composition and the glass transition temperature generally have a positive correlation (that is, as the viscosity of the resin composition decreases due to the action of the diluent, the glass transition temperature becomes lower). The temperature drops.). In this evaluation of physical properties, a viscosity corresponding to a practical glass transition temperature (100 ° C. or 110 ° C.) was obtained from the correlation diagram, and the impregnating property of the resin composition was determined according to the magnitude of the viscosity at that time. Was evaluated (that is, the lower the viscosity, the better the impregnation property). The viscosity (cps)
Is measured at 25 ° C. using a B type viscometer. Further, the glass transition temperature (Tg, ° C) is measured by the Tg of the cured product obtained under the curing condition of 120 ° C x 5 hours based on the DSC method.
【００２２】静電容量変化率（ΔＣａｐ、％） メタライズドポリエステルフィルムコンデンサ（０．０
０４７μＦ×２５０Ｖ，０．０４７μＦ×２５０Ｖ）を
予め１２０℃に加熱し、次いで常温の液状エポキシ樹脂
組成物中に１０秒間浸漬して含浸し、次いで流動浸漬法
によりエポキシ粉体塗料を当該含浸物に外装して試料を
調製し、当該試料を８５℃、８５％ＲＨの条件下で５０
０時間放置する（耐湿テスト）。上記試験前後の静電容
量をキャパシタンスブリッジを用いて２５℃、１kHzで
測定し、その変化率を算定する。Capacitance change rate (ΔCap,%) Metallized polyester film capacitor (0.0
(047 μF × 250 V, 0.047 μF × 250 V) is heated to 120 ° C. in advance and then immersed in a liquid epoxy resin composition at room temperature for 10 seconds to impregnate it, and then the epoxy powder coating is applied to the impregnated product by a fluidized dipping method. The sample is prepared by packaging, and the sample is heated at 85 ° C and 85% RH for 50 minutes.
Leave for 0 hours (moisture resistance test). The capacitance before and after the test is measured at 25 ° C. and 1 kHz using a capacitance bridge, and the rate of change is calculated.
【００２３】誘電正接（ｔａｎδ） 静電容量変化率と同様にして評価する。Dielectric loss tangent (tan δ) Evaluation is performed in the same manner as the rate of change in capacitance.
【００２４】絶縁抵抗 市販の抵抗測定装置による。Insulation resistance By a commercially available resistance measuring device.
【００２５】実施例１ ビスフェノールＡ型エポキシ樹脂（商品名「エピコート
８２８」、油化シェルエポキシ社製、エポキシ当量１９
０）５０重量部、１，４−シクロヘキサンジメタノール
ジグリシジルエーテル（商品名「リカレジンＤＭＥ−１
００」、新日本理化社製、エポキシ当量１５５）５０重
量部、メチルテトラヒドロ無水フタル酸（商品名「リカ
シッドＭＴ−５００」、新日本理化社製）９３重量部
（当該樹脂組成物中のエポキシ基の合計当量に対して
０．９５倍当量に相当）及び２−エチル−４−メチルイ
ミダゾール（商品名「キュアゾール２Ｅ４ＭＺ」、四国
化成社製）１重量部からなる液状エポキシ樹脂組成物を
調製し、その物理的特性を測定した。その結果、１００
℃のガラス転移温度を有する樹脂組成物の粘度は１６０
ｃｐｓであった。Example 1 Bisphenol A type epoxy resin (trade name "Epicoat 828", manufactured by Yuka Shell Epoxy Co., epoxy equivalent 19
0) 50 parts by weight of 1,4-cyclohexanedimethanol diglycidyl ether (trade name “Licalesin DME-1
00 ", manufactured by Shin Nippon Rika Co., Ltd., epoxy equivalent 155) 50 parts by weight, methyltetrahydrophthalic anhydride (trade name" Rikacid MT-500 ", manufactured by Shin Nippon Rika Co., Ltd.) 93 parts by weight (epoxy group in the resin composition) To a total equivalent weight of 0.95 times) and 2-ethyl-4-methylimidazole (trade name "Curezole 2E4MZ", manufactured by Shikoku Chemicals Co., Ltd.) 1 part by weight of a liquid epoxy resin composition, Its physical properties were measured. As a result, 100
The viscosity of the resin composition having a glass transition temperature of ℃ is 160
It was cps.
【００２６】比較例１ 「エピコート８２８」１００重量部、１，６−ヘキサン
ジオールジグリシジルエーテル（エポキシ当量１５０）
３０重量部、「リカシッドＭＴ−５００」８７重量部
（当該樹脂組成物中のエポキシ基の合計当量に対して
０．９５倍当量に相当）及び「キュアゾール２Ｅ４Ｍ
Ｚ」１重量部からなる液状エポキシ樹脂組成物を調製
し、その物理的特性を測定した。その結果、１００℃の
ガラス転移温度を有する樹脂組成物の粘度は粘度は２７
０ｃｐｓであった。Comparative Example 1 100 parts by weight of "Epicoat 828", 1,6-hexanediol diglycidyl ether (epoxy equivalent 150)
30 parts by weight, 87 parts by weight of "Ricacid MT-500" (corresponding to 0.95 times the equivalent of the total equivalents of epoxy groups in the resin composition) and "Curezol 2E4M".
A liquid epoxy resin composition consisting of 1 part by weight of "Z" was prepared and its physical properties were measured. As a result, the viscosity of the resin composition having a glass transition temperature of 100 ° C. was 27.
It was 0 cps.
【００２７】比較例２ 「エピコート８２８」１００重量部、ネオデカン酸グリ
シジルエステル（商品名「カージュラＥ」、油化シェル
エポキシ社製、エポキシ当量２５０）２３重量部、「リ
カシッドＭＴ−５００」７９重量部（当該樹脂組成物中
のエポキシ基の合計当量に対して０．９５倍当量に相
当）及び「キュアゾール２Ｅ４ＭＺ」１重量部からなる
液状エポキシ樹脂組成物を調製し、その物理的特性を測
定した。その結果、１００℃のガラス転移温度を有する
樹脂組成物の粘度は粘度は３４０ｃｐｓであった。Comparative Example 2 100 parts by weight of "Epicoat 828", 23 parts by weight of neodecanoic acid glycidyl ester (trade name "CARDURA E", manufactured by Yuka Shell Epoxy Co., Ltd., epoxy equivalent 250), and "RIKACID MT-500" 79 parts by weight. (Equivalent to 0.95 times equivalent to the total equivalents of epoxy groups in the resin composition) and 1 part by weight of "Curazole 2E4MZ" were prepared, and a liquid epoxy resin composition was prepared, and its physical properties were measured. As a result, the viscosity of the resin composition having a glass transition temperature of 100 ° C. was 340 cps.
【００２８】比較例３ 「エピコート８２８」１００重量部、ラウリルグリシジ
ルエーテル（エポキシ当量２８０）１７重量部、「リカ
シッドＭＴ−５００」８１重量部（当該樹脂組成物中の
エポキシ基の合計当量に対して０．９５倍当量に相当）
及び「キュアゾール２Ｅ４ＭＺ」１重量部からなる液状
エポキシ樹脂組成物を調製し、その物理的特性を測定し
た。その結果、１００℃のガラス転移温度を有する樹脂
組成物の粘度は３４０ｃｐｓであった。Comparative Example 3 100 parts by weight of "Epicoat 828", 17 parts by weight of lauryl glycidyl ether (epoxy equivalent: 280), 81 parts by weight of "Ricacid MT-500" (based on the total equivalent of epoxy groups in the resin composition). (Equivalent to 0.95 times equivalent)
And a liquid epoxy resin composition consisting of 1 part by weight of "Curesol 2E4MZ" were measured and the physical properties thereof were measured. As a result, the viscosity of the resin composition having a glass transition temperature of 100 ° C. was 340 cps.
【００２９】実施例２ 「エピコート８２８」５０重量部、「リカレジンＤＭＥ
−１００」５０重量部、メチルヘキサヒドロ無水フタル
酸（商品名「リカシッドＭＨ−７００」、新日本理化社
製）９１重量部（当該樹脂組成物中のエポキシ基の合計
当量に対して０．９５倍当量に相当）及び「キュアゾー
ル２Ｅ４ＭＺ」１重量部からなる液状エポキシ樹脂組成
物を調製し、その物理的特性を測定した。その結果、１
１０℃のガラス転移温度を有する樹脂組成物の粘度は２
８０ｃｐｓであった。Example 2 50 parts by weight of "Epicoat 828", "Likaresin DME"
-100 "50 parts by weight, methylhexahydrophthalic anhydride (trade name" Ricacid MH-700 ", manufactured by Shin Nippon Rika Co., Ltd.) 91 parts by weight (0.95 based on the total equivalent of epoxy groups in the resin composition). (Corresponding to a double equivalent) and 1 part by weight of "Curazole 2E4MZ" was prepared, and its physical properties were measured. As a result, 1
The viscosity of a resin composition having a glass transition temperature of 10 ° C. is 2
It was 80 cps.
【００３０】又、当該液状エポキシ樹脂組成物の各種コ
ンデンサ特性を評価したところ、定格０．０４７μＦ
（２５０Ｖ）のフィルムコンデンサにおいて、ΔＣａｐ
は＋２．５％であり、試験前０．３９％のｔａｎδは試
験後０．４０％とほとんど変わらず、更に試験前５０×
１０4ＭΩの抵抗値は試験後４８×１０4ＭΩと極めて少
ない低下に留まった。一方、定格０．４７μＦ（２５０
Ｖ）のフィルムコンデンサにおいても、ΔＣａｐは＋
２．２％であり、試験前０．３９％のｔａｎδは試験後
０．４０％とほとんど変わらず、更に試験前８３×１０
3ＭΩの抵抗値は試験後７９×１０3ＭΩと極めて少ない
低下に留まった。Further, when various capacitor characteristics of the liquid epoxy resin composition were evaluated, the rating was 0.047 μF.
In a (250V) film capacitor, ΔCap
Is + 2.5%, tan δ of 0.39% before the test is almost the same as 0.40% after the test, and 50 × before the test.
The resistance value of 10 4 MΩ was 48 × 10 4 MΩ, which was a very small decrease after the test. On the other hand, the rating is 0.47μF (250
VCap is also + in the film capacitor of V)
2.2%, the tan δ of 0.39% before the test was almost the same as 0.40% after the test, and further 83 × 10 before the test.
The resistance value of 3 MΩ was 79 × 10 3 MΩ, which was a very small decrease after the test.
【００３１】比較例４ 「エピコート８２８」１００重量部、「カージュラＥ」
３０重量部、「リカシッドＭＨ−７００」８６重量部
（当該樹脂組成物中のエポキシ基の合計当量に対して
０．９５倍当量に相当）及び「キュアゾール２Ｅ４Ｍ
Ｚ」１重量部からなる液状エポキシ樹脂組成物を調製
し、その物理的特性を測定した。その結果、１１０℃の
ガラス転移温度を有する樹脂組成物の粘度は６００ｃｐ
ｓであった。Comparative Example 4 100 parts by weight of "Epicote 828", "Curdra E"
30 parts by weight, 86 parts by weight of "Ricacid MH-700" (corresponding to 0.95 times equivalent to the total equivalents of epoxy groups in the resin composition) and "Curazole 2E4M".
A liquid epoxy resin composition consisting of 1 part by weight of "Z" was prepared and its physical properties were measured. As a result, the viscosity of the resin composition having a glass transition temperature of 110 ° C. is 600 cp.
It was s.
【００３２】又、当該液状エポキシ樹脂組成物の各種コ
ンデンサ特性を評価したところ、定格０．０４７μＦ
（２５０Ｖ）のフィルムコンデンサにおいて、ΔＣａｐ
は＋４．５％であり、試験前０．３９％のｔａｎδは試
験後０．４５％と増加し、更に試験前５０×１０4ＭΩ
の抵抗値は試験後４２×１０4ＭΩと大きく低下した。
一方、定格０．４７μＦ（２５０Ｖ）のフィルムコンデ
ンサにおいても、ΔＣａｐは＋３．１％と大きく、試験
前０．４０％のｔａｎδは試験後０．４４％と増加し、
更に試験前７４×１０3ＭΩの抵抗値は試験後６２×１
０3ＭΩと大きく低下した。Further, when various capacitor characteristics of the liquid epoxy resin composition were evaluated, the rating was 0.047 μF.
In a (250V) film capacitor, ΔCap
Is + 4.5%, tan δ of 0.39% before the test increases to 0.45% after the test, and further 50 × 10 4 MΩ before the test.
After the test, the resistance value of No. 42 was greatly reduced to 42 × 10 4 MΩ.
On the other hand, also in a film capacitor with a rating of 0.47 μF (250 V), ΔCap is as large as + 3.1%, tan δ of 0.40% before the test increases to 0.44% after the test,
Furthermore, the resistance value of 74 × 10 3 MΩ before the test is 62 × 1 after the test.
It was greatly reduced to 0 3 MΩ.
【００３３】[0033]
【発明の効果】本発明に係る所定の組成からなる液状エ
ポキシ樹脂組成物は、低粘度で、使用時に各種部品に良
好な含浸性を有し、硬化性を低下することなく、優れた
耐熱性、耐電圧性、電気絶縁性、耐湿性、機械強度、接
着性を具備する。The liquid epoxy resin composition having a predetermined composition according to the present invention has a low viscosity, has a good impregnation property in various parts at the time of use, and has excellent heat resistance without lowering the curability. , Withstand voltage, electrical insulation, moisture resistance, mechanical strength, and adhesiveness.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成７年４月２０日[Submission date] April 20, 1995
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】０００９[Correction target item name] 0009
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【０００９】 即ち、本発明に係る液状エポキシ樹脂組
成物は、エポキシ樹脂１００重量部に対し、１，４−シ
クロヘキサンジメタノールジグリシジルエーテル５０〜
１５０重量部、酸無水物系硬化剤をエポキシ基の合計当
量に対し０．８〜１．１倍当量及び硬化促進剤０．１〜
５重量部含有することを特徴とする。That is, the liquid epoxy resin composition according to the present invention contains 50 parts by weight of 1,4-cyclohexanedimethanol diglycidyl ether per 100 parts by weight of the epoxy resin.
150 parts by weight, 0.8 to 1.1 times equivalent amount of acid anhydride type curing agent with respect to total equivalent amount of epoxy groups, and 0.1 to 0.1 % of curing accelerator.
It is characterized by containing 5 parts by weight.
【手続補正２】[Procedure Amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１０[Correction target item name] 0010
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００１０】 本発明に係るエポキシ樹脂としては、液
状ビスフェノールＡ型エポキシ樹脂、ビスフェノールＦ
型エポキシ樹脂等が例示され、必要に応じてフェノール
ノボラックエポキシ樹脂、クレゾールノボラックエポキ
シ樹脂等のグリシジルエーテル型エポキシ樹脂、グリシ
ジルエステル型エポキシ樹脂、グリシジルアミン型エポ
キシ樹脂、ハロゲン化エポキシ樹脂等を混合して使用す
ることができる。特に液状ビスフェノールＡ型グリシジ
ルエーテル、ビスフェノールＦ型グリシジルエーテル等
が推奨される。Examples of the epoxy resin according to the present invention include liquid bisphenol A type epoxy resin and bisphenol F.
Type epoxy resin and the like, if necessary, by mixing glycidyl ether type epoxy resin such as phenol novolac epoxy resin, cresol novolac epoxy resin , glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, halogenated epoxy resin, etc. Can be used. In particular, liquid bisphenol A type glycidyl ether, bisphenol F type glycidyl ether and the like are recommended.
【手続補正３】[Procedure 3]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１２[Correction target item name] 0012
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００１２】 １，４−シクロヘキサンジメタノールジ
グリシジルエーテルの配合量としては、エポキシ樹脂１
００重量部に対して５０〜１５０重量部、より好ましく
は８０〜１１０重量部が推奨される。５０重量部未満で
は含浸性を改良できる程の粘度低下が得られにくく、１
５０重量部を越えて配合した場合にはエポキシ樹脂硬化
物の耐熱性が低下して目的とする硬化物の特性が得られ
にくい。The compounding amount of 1,4-cyclohexanedimethanol diglycidyl ether is epoxy resin 1
50 to 150 parts by weight, and more preferably 80 to 110 parts by weight, are recommended with respect to 00 parts by weight. If the amount is less than 50 parts by weight, it is difficult to obtain a viscosity decrease enough to improve the impregnation property.
Epoxy resin curing when compounded in excess of 50 parts by weight
The heat resistance of the product is reduced, and it is difficult to obtain the desired properties of the cured product.
【手続補正４】[Procedure amendment 4]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２０[Correction target item name] 0020
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００２０】[0020]
【実施例】以下に実施例を揚げ、本発明を詳しく説明す
る。尚、各例におけるエポキシ樹脂組成物の物理的特性
（粘度とガラス転移温度との相関）及びコンデンサ特性
（静電容量変化率、誘電正接、絶縁抵抗）は以下の方法
により測定し、評価した。EXAMPLES The present invention will be described in detail with reference to the following examples. The physical characteristics (correlation between viscosity and glass transition temperature) and capacitor characteristics (rate of change in capacitance, dielectric loss tangent, insulation resistance) of the epoxy resin composition in each example were measured and evaluated by the following methods.
【手続補正５】[Procedure Amendment 5]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２５[Name of item to be corrected] 0025
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００２５】 実施例１ ビスフェノールＡ型エポキシ樹脂（商品名「エピコート
８２８」、油化シェルエポキシ社製、エポキシ当量１９
０）５０重量部、１，４−シクロヘキサンジメタノール
ジグリシジルエーテル（商品名「リカレジンＤＭＥ−１
００」、新日本理化社製、エポキシ当量１５５）５０重
量部、メチルテトラヒドロ無水フタル酸（商品名「リカ
シッドＭＴ−５００」、新日本理化社製）９３重量部
（当該樹脂組成物中のエポキシ基の合計当量に対して
０．９５倍当量に相当）及び２−エチル−４−メチルイ
ミダゾール（商品名「キュアゾール２Ｅ４ＭＺ」、四国
化成工業社製）１重量部からなる液状エポキシ樹脂組成
物を調製し、その物理的特性を測定した。その結果、１
００℃のガラス転移温度を有する樹脂組成物の粘度は１
６０ｃｐｓであった。Example 1 Bisphenol A type epoxy resin (trade name “Epicoat 828”, manufactured by Yuka Shell Epoxy Co., Ltd., epoxy equivalent 19
0) 50 parts by weight of 1,4-cyclohexanedimethanol diglycidyl ether (trade name “Licalesin DME-1
00 ", manufactured by Shin Nippon Rika Co., Ltd., epoxy equivalent: 155) 50 parts by weight, methyltetrahydrophthalic anhydride (trade name" Rikacid MT-500 "manufactured by Shin Nippon Rika Co., Ltd.) 93 parts by weight (epoxy group in the resin composition) total equivalent corresponding to 0.95 equivalents relative to the amount) and 2-ethyl-4-methylimidazole (trade name "Curezol 2E4MZ", Shikoku Kasei Kogyo Co., Ltd.) liquid epoxy resin composition comprising 1 part by weight of the prepared , Its physical properties were measured. As a result, 1
The viscosity of a resin composition having a glass transition temperature of 00 ° C. is 1
It was 60 cps.
【手続補正６】[Procedure correction 6]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２６[Correction target item name] 0026
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００２６】 比較例１ 「エピコート８２８」１００重量部、１，６−ヘキサン
ジオールジグリシジルエーテル（エポキシ当量１５０）
３０重量部、「リカシッドＭＴ−５００」８７重量部
（当該樹脂組成物中のエポキシ基の合計当量に対して
０．９５倍当量に相当）及び「キュアゾール２Ｅ４Ｍ
Ｚ」１重量部からなる液状エポキシ樹脂組成物を調製
し、その物理的特性を測定した。その結果、１００℃の
ガラス転移温度を有する樹脂組成物の粘度は２７０ｃｐ
ｓであった。Comparative Example 1 100 parts by weight of "Epicoat 828", 1,6-hexanediol diglycidyl ether (epoxy equivalent 150)
30 parts by weight, 87 parts by weight of "Ricacid MT-500" (corresponding to 0.95 times the equivalent of the total equivalents of epoxy groups in the resin composition) and "Curezol 2E4M".
A liquid epoxy resin composition consisting of 1 part by weight of "Z" was prepared and its physical properties were measured. As a result, the viscosity of the resin composition having a glass transition temperature of 100 ° C. was 270 cp.
It was s.
【手続補正７】[Procedure Amendment 7]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２７[Name of item to be corrected] 0027
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００２７】 比較例２ 「エピコート８２８」１００重量部、ネオデカン酸グリ
シジルエステル（商品名「カージュラＥ」、油化シェル
エポキシ社製、エポキシ当量２５０）２３重量部、「リ
カシッドＭＴ−５００」７９重量部（当該樹脂組成物中
のエポキシ基の合計当量に対して０．９５倍当量に相
当）及び「キュアゾール２Ｅ４ＭＺ」１重量部からなる
液状エポキシ樹脂組成物を調製し、その物理的特性を測
定した。その結果、１００℃のガラス転移温度を有する
樹脂組成物の粘度は３４０ｃｐｓであった。Comparative Example 2 100 parts by weight of "Epicoat 828", 23 parts by weight of neodecanoic acid glycidyl ester (trade name "CARDURA E", manufactured by Yuka Shell Epoxy Co., epoxy equivalent 250), and 79 parts by weight of "RICACID MT-500" (Equivalent to 0.95 times equivalent to the total equivalents of epoxy groups in the resin composition) and 1 part by weight of "Curazole 2E4MZ" were prepared, and a liquid epoxy resin composition was prepared, and its physical properties were measured. As a result, the viscosity of the resin composition having a glass transition temperature of 100 ° C. was 340 cps .
Claims (3)
４−シクロヘキサンジメタノールジグリシジルエーテル
５０〜１５０重量部、酸無水物系硬化剤をエポキシ基の
合計当量に対し０．８〜１．１倍当量及び硬化促進剤
０．１〜５重量部含有することを特徴とする液状エポキ
シ樹脂組成物。1. To 100 parts by weight of epoxy resin, 1,
50-150 parts by weight of 4-cyclohexanedimethanol diglycidyl ether, 0.8-1.1 times equivalent amount of acid anhydride type curing agent based on the total equivalents of epoxy groups, and 0.1-5 parts by weight of curing accelerator. A liquid epoxy resin composition comprising:
物を含浸してなる電子部品。2. An electronic component obtained by impregnating the liquid epoxy resin composition according to claim 1.
物を含浸してなるフィルムコンデンサ。3. A film capacitor impregnated with the liquid epoxy resin composition according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15201994A JP3399095B2 (en) | 1994-07-04 | 1994-07-04 | Liquid epoxy resin composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15201994A JP3399095B2 (en) | 1994-07-04 | 1994-07-04 | Liquid epoxy resin composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0812741A true JPH0812741A (en) | 1996-01-16 |
| JP3399095B2 JP3399095B2 (en) | 2003-04-21 |
Family
ID=15531287
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15201994A Expired - Fee Related JP3399095B2 (en) | 1994-07-04 | 1994-07-04 | Liquid epoxy resin composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3399095B2 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000079582A1 (en) * | 1999-06-17 | 2000-12-28 | Loctite Corporation | Controllably degradable composition of heteroatom carbocyclic or epoxy resin and curing agent |
| US7012120B2 (en) | 2000-03-31 | 2006-03-14 | Henkel Corporation | Reworkable compositions of oxirane(s) or thirane(s)-containing resin and curing agent |
| JP2010202880A (en) * | 2002-10-07 | 2010-09-16 | Momentive Performance Materials Inc | Epoxy resin composition, solid state device encapsulated therewith and method |
| US8053587B2 (en) | 2000-03-31 | 2011-11-08 | Henkel Corporation | Reworkable thermosetting resin composition |
| JP2013139564A (en) * | 2011-12-30 | 2013-07-18 | Eternal Chemical Co Ltd | Electrolyte material formulation, electrolyte material composition formed therefrom and use thereof |
| JP2015209516A (en) * | 2014-04-28 | 2015-11-24 | 株式会社クラレ | Curable composition, and cured product |
| JP2016079300A (en) * | 2014-10-17 | 2016-05-16 | 京セラケミカル株式会社 | Epoxy resin composition for impregnation casting, coil component and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58219173A (en) * | 1982-06-01 | 1983-12-20 | ウイルミントン・ケミカル・コ−ポレ−シヨン | Bifunctional epoxide and epoxy resin |
| JPH0348416A (en) * | 1989-07-17 | 1991-03-01 | Nitsuko Corp | Primary coating impregnant for film capacitor |
| JPH061907A (en) * | 1992-06-18 | 1994-01-11 | Mitsui Toatsu Chem Inc | Unsaturated epoxy ester resin composition |
| JPH065464A (en) * | 1992-06-19 | 1994-01-14 | Hitachi Chem Co Ltd | Epoxy resin composition for capacitor |
| EP0590975A1 (en) * | 1992-10-02 | 1994-04-06 | W.R. Grace & Co.-Conn. | Low viscosity and solvent-free one-component type epoxy resin adhesive composition |
| JPH06120016A (en) * | 1992-10-01 | 1994-04-28 | Sumitomo Metal Mining Co Ltd | Bonded magnet composition and bonded magnet |
| JPH06136092A (en) * | 1992-10-27 | 1994-05-17 | New Japan Chem Co Ltd | Epoxy resin composition |
| JPH06248053A (en) * | 1993-02-23 | 1994-09-06 | Dainippon Toryo Co Ltd | Epoxy resin coating composition |
| JPH0790050A (en) * | 1993-09-14 | 1995-04-04 | New Japan Chem Co Ltd | Epoxy resin and its production |
| JPH07196905A (en) * | 1993-12-28 | 1995-08-01 | Kobe Steel Ltd | Curable resin composition |
-
1994
- 1994-07-04 JP JP15201994A patent/JP3399095B2/en not_active Expired - Fee Related
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58219173A (en) * | 1982-06-01 | 1983-12-20 | ウイルミントン・ケミカル・コ−ポレ−シヨン | Bifunctional epoxide and epoxy resin |
| JPH0348416A (en) * | 1989-07-17 | 1991-03-01 | Nitsuko Corp | Primary coating impregnant for film capacitor |
| JPH061907A (en) * | 1992-06-18 | 1994-01-11 | Mitsui Toatsu Chem Inc | Unsaturated epoxy ester resin composition |
| JPH065464A (en) * | 1992-06-19 | 1994-01-14 | Hitachi Chem Co Ltd | Epoxy resin composition for capacitor |
| JPH06120016A (en) * | 1992-10-01 | 1994-04-28 | Sumitomo Metal Mining Co Ltd | Bonded magnet composition and bonded magnet |
| EP0590975A1 (en) * | 1992-10-02 | 1994-04-06 | W.R. Grace & Co.-Conn. | Low viscosity and solvent-free one-component type epoxy resin adhesive composition |
| JPH06207152A (en) * | 1992-10-02 | 1994-07-26 | W R Grace & Co | Low-viscosity solventless one-pack epoxy resin adhesive composition |
| JPH06136092A (en) * | 1992-10-27 | 1994-05-17 | New Japan Chem Co Ltd | Epoxy resin composition |
| JPH06248053A (en) * | 1993-02-23 | 1994-09-06 | Dainippon Toryo Co Ltd | Epoxy resin coating composition |
| JPH0790050A (en) * | 1993-09-14 | 1995-04-04 | New Japan Chem Co Ltd | Epoxy resin and its production |
| JPH07196905A (en) * | 1993-12-28 | 1995-08-01 | Kobe Steel Ltd | Curable resin composition |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000079582A1 (en) * | 1999-06-17 | 2000-12-28 | Loctite Corporation | Controllably degradable composition of heteroatom carbocyclic or epoxy resin and curing agent |
| EP1194953A4 (en) * | 1999-06-17 | 2002-09-04 | Loctite Corp | Controllably degradable composition of heteroatom carbocyclic or epoxy resin and curing agent |
| JP2003502484A (en) * | 1999-06-17 | 2003-01-21 | ヘンケル ロックタイト コーポレイション | Controllable degradable compositions of heteroatom carbocyclic or epoxy resins and curing agents |
| JP4718070B2 (en) * | 1999-06-17 | 2011-07-06 | ヘンケル コーポレイション | Underfill sealing and repair method |
| US7012120B2 (en) | 2000-03-31 | 2006-03-14 | Henkel Corporation | Reworkable compositions of oxirane(s) or thirane(s)-containing resin and curing agent |
| US8053587B2 (en) | 2000-03-31 | 2011-11-08 | Henkel Corporation | Reworkable thermosetting resin composition |
| JP2010202880A (en) * | 2002-10-07 | 2010-09-16 | Momentive Performance Materials Inc | Epoxy resin composition, solid state device encapsulated therewith and method |
| JP2013139564A (en) * | 2011-12-30 | 2013-07-18 | Eternal Chemical Co Ltd | Electrolyte material formulation, electrolyte material composition formed therefrom and use thereof |
| JP2015129309A (en) * | 2011-12-30 | 2015-07-16 | 長興材料工業股▲ふん▼有限公司 | Electrolyte material formulation, electrolyte material composition formed therefrom and use thereof |
| US9691551B2 (en) | 2011-12-30 | 2017-06-27 | Eternal Materials Co., Ltd. | Electrolyte material formulation, electrolyte material composition formed therefrom and use thereof |
| JP2015209516A (en) * | 2014-04-28 | 2015-11-24 | 株式会社クラレ | Curable composition, and cured product |
| JP2016079300A (en) * | 2014-10-17 | 2016-05-16 | 京セラケミカル株式会社 | Epoxy resin composition for impregnation casting, coil component and manufacturing method thereof |
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| JP3399095B2 (en) | 2003-04-21 |
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