JPH0717815B2 - Epoxy resin composition - Google Patents
Epoxy resin compositionInfo
- Publication number
- JPH0717815B2 JPH0717815B2 JP61223714A JP22371486A JPH0717815B2 JP H0717815 B2 JPH0717815 B2 JP H0717815B2 JP 61223714 A JP61223714 A JP 61223714A JP 22371486 A JP22371486 A JP 22371486A JP H0717815 B2 JPH0717815 B2 JP H0717815B2
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- resin composition
- inorganic filler
- present
- disperse
- 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.)
- Expired - Fee Related
Links
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Description
【発明の詳細な説明】 ［発明の目的］ （産業上の利用分野） 本発明は、無機質充填剤の分散性、沈降防止性に優れた
エポキシ樹脂組成物に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Field of Industrial Application) The present invention relates to an epoxy resin composition having excellent dispersibility of an inorganic filler and anti-settling property.
（従来の技術） 液状エポキシ樹脂は、フライバックトランス、イグニッ
ションコイル、リレー、ハイブリッドIC、IC・LSI等の
電気・電子部品の封入、封止、ディッピング等として広
く使用されている。そして、これらいずれの場合にも、
熱膨脹率の低下、熱伝導性の向上、耐熱性の付与等の目
的で無機質充填剤が混合使用されている。(Prior Art) Liquid epoxy resins are widely used for encapsulating, encapsulating, dipping, etc., electric and electronic parts such as flyback transformers, ignition coils, relays, hybrid ICs, and IC / LSIs. And in any of these cases,
An inorganic filler is mixed and used for the purpose of lowering the coefficient of thermal expansion, improving thermal conductivity, imparting heat resistance and the like.
しかしながら、これらの無機質充填剤を混合させると樹
脂の粘度が著しく上昇し、作業性が悪くなるという欠点
がある。この粘度上昇を小さくするため一般的には粒度
の荒い充填剤を用いるが、この場合、樹脂組成物の保管
中に充填剤がよく分散されずに沈降し、組成物が不均一
になるという問題点があった。充填剤の沈降を防止する
ため、粒子の細かいチクソ性の出る充填剤を併用した
り、ゲル化剤等の添加剤を用いる方法が行われている。
しかしこれらは作業性のすぐれた低粘度の樹脂組成物に
は効果が少なく、また用いられる充填剤が限られたり、
添加剤の混入によって不純物が混入されるという問題点
があった。However, when these inorganic fillers are mixed, there is a drawback that the viscosity of the resin is significantly increased and the workability is deteriorated. In order to reduce this increase in viscosity, a filler having a coarse particle size is generally used. In this case, however, the filler is not well dispersed during the storage of the resin composition and settles, resulting in a non-uniform composition. There was a point. In order to prevent the settling of the filler, a method is used in which a filler having fine thixotropic properties of particles is used in combination, or an additive such as a gelling agent is used.
However, these are less effective for low viscosity resin compositions with excellent workability, and the fillers used are limited,
There is a problem that impurities are mixed due to the mixing of the additive.
（発明が解決しようとする問題点） 本発明は、上記の問題点を解決するためになされたもの
で、無機質充填剤の分散性、沈降防止性に優れ、不純物
等の混入がなく、作業性のよいエポキシ樹脂組成物を提
供しようとするものである。(Problems to be Solved by the Invention) The present invention has been made in order to solve the above problems, and is excellent in dispersibility of an inorganic filler and anti-sedimentation property, without inclusion of impurities and the like, and workability. It is intended to provide a good epoxy resin composition.
［発明の構成］ （問題点を解決するための手段） 本発明者らは、上記の目的を達成しようと鋭意研究を重
ねた結果、液状エポキシ樹脂および無機質充填剤共存下
でデイスパースにより高速度撹拌させることにより、か
なり荒い無機質充填剤でも著しく沈降しにくくなること
を見いだし、本発明を完成させたものである。[Structure of the Invention] (Means for Solving the Problems) As a result of intensive studies aimed at achieving the above-mentioned objects, the present inventors have found that high-speed stirring by a disperse coexistence in the presence of a liquid epoxy resin and an inorganic filler. By doing so, it was found that even a fairly rough inorganic filler is unlikely to settle, and the present invention has been completed.
即ち、本発明は、液状エポキシ樹脂および無機質充填剤
を、ディスパースにおけるランナーとステーターの相対
周速度として5m/秒以上、撹拌時間が10分間以上の高速
撹拌をさせてなることを特徴とするエポキシ樹脂組成物
である。That is, the present invention, the liquid epoxy resin and the inorganic filler, 5m / sec or more as a relative peripheral speed of the runner and the stator in the disperse, stirring time is 10 minutes or more characterized by high-speed stirring epoxy It is a resin composition.
本発明でいうデイスパースは、円錘形のランナーとステ
ーターの間の間隙のせん断力で粉砕、懸濁、乳化を行う
型式の撹拌混合機をいう。ディスパースはディスパーミ
ルともいわれる。ディスパーミルと同じ円錘形のランナ
ーとステーターのほかにインペラーとノックをもつもの
にミクロンコロイドミルがあるが、本発明のディスパー
スの中にはミクロンコロイドミルも含まれる。The term "disperse" as used in the present invention refers to a stirring mixer of a type in which crushing, suspension, and emulsification are performed by the shearing force in the gap between the conical runner and the stator. Disperse is also called Dispermill. The micron colloid mill has the same conical runner and stator as the disper mill but also has an impeller and a knock, and the disperse of the present invention also includes the micron colloid mill.
本発明に用いる液状エポキシ樹脂としては、例えばビス
フェノールＡ若しくはビスフェノールＦ又はそれらのハ
ロゲン化合物とエピクロルドリンとの重縮合によって得
られるエポキシ樹脂、エポキシ化ノボラック樹脂、エポ
キシ化クレゾール樹脂、エポキシ変性ポリブタジエンゴ
ム、脂環式エポキシ樹脂等が挙げられ、これらは１種又
は２種以上の混合系として使用できる。更に必要に応じ
てブチルグリシジルエーテル、フェニルグリシジルエー
テル等の低粘度の反応性希釈剤等を併用することができ
る。Examples of the liquid epoxy resin used in the present invention include an epoxy resin obtained by polycondensation of bisphenol A or bisphenol F or a halogen compound thereof and epichlordrin, an epoxidized novolac resin, an epoxidized cresol resin, an epoxy-modified polybutadiene rubber, Examples thereof include alicyclic epoxy resins, and these can be used as one type or as a mixed system of two or more types. Furthermore, if necessary, a low-viscosity reactive diluent such as butyl glycidyl ether or phenyl glycidyl ether can be used in combination.
本発明に用いる無機質充填剤としては、結晶性シリカ、
溶融シリカ、水酸化アルミニウム、タルク、炭酸カルシ
ウム等が挙げられ、これらはいずれも単独もしくは２種
以上混合して使用される。無機質充填剤の配合割合は、
エポキシ樹脂組成物に対して10〜80重量％配合すること
が望ましい。配合割合が10重量％未満では、無機質充填
剤の添加効果が小さく、また80重量％を超えると粘度が
高くなり好ましくない。As the inorganic filler used in the present invention, crystalline silica,
Examples thereof include fused silica, aluminum hydroxide, talc, calcium carbonate, and the like, all of which are used alone or in combination of two or more. The blending ratio of the inorganic filler is
It is desirable to add 10 to 80% by weight to the epoxy resin composition. If the blending ratio is less than 10% by weight, the effect of adding the inorganic filler is small, and if it exceeds 80% by weight, the viscosity becomes high, which is not preferable.
本発明のエポキシ樹脂組成物は、液状エポキシ樹脂、無
機質充填剤を含むが必要に応じて硬化剤、硬化促進剤、
カップリング剤、染料，顔料等の着色剤、三酸化アンチ
モン等の難燃剤などを適宜添加配合することができる。The epoxy resin composition of the present invention contains a liquid epoxy resin and an inorganic filler, but if necessary, a curing agent, a curing accelerator,
Coupling agents, colorants such as dyes and pigments, flame retardants such as antimony trioxide, and the like can be appropriately added and blended.
本発明のエポキシ樹脂組成物は、前述した液状エポキシ
樹脂と無機質充填剤を高速度撹拌することが最も重要な
ことである。高速度撹拌はディスパースで行うが、ディ
スパースの周速として5m/秒以上であることが望まし
い。周速が5m/秒未満では分散性が悪く好ましくない。
また高速度撹拌を行う時間は、ディスパースの能力と樹
脂量によって異なるが10分間以上であることが望まし
い。10分間未満では分散性が悪く好ましくないからであ
る。In the epoxy resin composition of the present invention, it is most important to stir the above-mentioned liquid epoxy resin and the inorganic filler at a high speed. The high speed stirring is performed by a disperse, and the peripheral speed of the disperse is preferably 5 m / sec or more. If the peripheral speed is less than 5 m / sec, the dispersibility is poor and it is not preferable.
Further, the time for performing the high speed stirring is preferably 10 minutes or more, though it depends on the ability of the disperse and the amount of the resin. This is because if it is less than 10 minutes, the dispersibility is poor and it is not preferable.
本発明で行う高速度撹拌は無機質充填剤だけでなく、ニ
ッケル、銅、銀等の金属充填剤にも有効である。また用
いる樹脂としてはエポキシ樹脂以外のポリイミド、ポリ
エステル、ウレタン、アクリル等の樹脂系にも応用する
ことが可能である。The high-speed stirring performed in the present invention is effective not only for inorganic fillers but also for metal fillers such as nickel, copper and silver. Further, as the resin to be used, it is possible to apply to resin systems such as polyimide, polyester, urethane and acrylic other than the epoxy resin.
（作用） ディスパースによる高速度撹拌によって、なぜ無機質充
填剤の分散性がよく沈降性が小さくなるかは明らかでな
いが、エポキシオリゴマー共存下で無機質充填剤にディ
スパースによる高速度撹拌の機械的作用を加えると無機
質表面とエポキシオリゴマーとの間に化学反応が起こ
り、無機質表面が改善され濡れ性等が大幅に変化するも
のと推定される。(Action) It is not clear why the disperse property of the inorganic filler is good and the sedimentation property is reduced by the high-speed stirring by the disperse, but the mechanical action of the high-speed stirring by the disperse in the inorganic filler in the presence of the epoxy oligomer It is presumed that the addition of the compound causes a chemical reaction between the inorganic surface and the epoxy oligomer, improves the inorganic surface, and significantly changes the wettability and the like.
（実施例） 次に本発明を実施例によって説明するが本発明はこれら
の実施例によって限定されるものではない。(Examples) Next, the present invention will be described with reference to examples, but the present invention is not limited to these examples.
実施例 １ エポン828（油化シェルエポキシ社製ビスフェノールＡ
型エポキシ樹脂、商品名）600gに、クリスタライトVX−
Ｓ（龍森社製結晶性シリカ、商品名）400gを配合し、こ
れをディスパース（羽根径50mm）5000r.p.mで40分間撹
拌し均一なエポキシ樹脂組成物を得た。この組成物を１
の広口ポリエチレンビンで25℃、30日間保管後、沈降
性を試験したが全く充填剤が沈降せず、従って均一な組
成物であり、本発明の優れた効果が確認された。Example 1 Epon 828 (bisphenol A manufactured by Yuka Shell Epoxy Co., Ltd.
Type epoxy resin, trade name) 600g, Crystallite VX-
400 g of S (Crystalline Silica manufactured by Tatsumori Co., Ltd.) was blended, and this was stirred for 40 minutes at a dispersion (blade diameter 50 mm) of 5000 rpm to obtain a uniform epoxy resin composition. 1 of this composition
After storing in a wide-mouth polyethylene bottle for 30 days at 25 ° C., the sedimentation property was tested, but the filler did not sediment at all, and thus the composition was uniform, and the excellent effect of the present invention was confirmed.
実施例 ２〜４ 第１表に示した組成で実施例１と同様にしてエポキシ樹
脂組成物を得た。この組成物について実施例１と同様に
沈降性の試験を行ったところ、全く沈降は見られず、本
発明の優れた効果が確認された。Examples 2 to 4 Epoxy resin compositions having the compositions shown in Table 1 were obtained in the same manner as in Example 1. When the composition was subjected to a sedimentation test in the same manner as in Example 1, no sedimentation was observed and the excellent effect of the present invention was confirmed.
比較例１〜４ 第１表に示した組成で実施例１と同様にしてエポキシ樹
脂組成物を得た。この組成物について実施例１と同様に
沈降性の試験を行ったところ、第１表に示したようにそ
れぞれ沈降しており、従って均一な組成物ではなかっ
た。Comparative Examples 1 to 4 Epoxy resin compositions having the compositions shown in Table 1 were obtained in the same manner as in Example 1. When the composition was subjected to a sedimentation test in the same manner as in Example 1, it was found to be sedimented as shown in Table 1, and thus the composition was not uniform.
［発明の効果］ 以上の説明および第１表から明らかなように、本発明の
エポキシ樹脂組成物は、ディスパースによる高速度撹拌
を行うことによって無機質充填剤が均一に分散し、かつ
沈降は全くみられず、作業性のよいものである。従っ
て、このエポキシ樹脂組成物を用いることによって優れ
た電気・電子部品を得ることができる。 [Effects of the Invention] As is clear from the above description and Table 1, in the epoxy resin composition of the present invention, the inorganic filler is uniformly dispersed by performing high speed stirring by disperse, and no sedimentation occurs. It is not seen and has good workability. Therefore, an excellent electric / electronic component can be obtained by using this epoxy resin composition.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭57−51427（ＪＰ，Ａ) 特開 昭57−65744（ＪＰ，Ａ) 特開 昭58−213018（ＪＰ，Ａ) 特開 昭61−26622（ＪＰ，Ａ) 特開 昭49−117541（ＪＰ，Ａ) 特開 昭58−61121（ＪＰ，Ａ) 特開 昭59−138242（ＪＰ，Ａ) 特公 昭53−20277（ＪＰ，Ｂ２) ─────────────────────────────────────────────────── ─── Continuation of front page (56) Reference JP 57-51427 (JP, A) JP 57-65744 (JP, A) JP 58-213018 (JP, A) JP 61- 26622 (JP, A) JP 49-117541 (JP, A) JP 58-61121 (JP, A) JP 59-138242 (JP, A) JP 53-20277 (JP, B2)
Claims (1)
ディスパースにおけるランナーとステーターの相対周速
度として5m/秒以上、撹拌時間が10分間以上の高速撹拌
をさせてなることを特徴とするエポキシ樹脂組成物。1. A liquid epoxy resin and an inorganic filler,
An epoxy resin composition characterized by being subjected to high-speed stirring at a relative peripheral velocity of a runner and a stator in a dispersion of 5 m / sec or more and a stirring time of 10 minutes or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61223714A JPH0717815B2 (en) | 1986-09-24 | 1986-09-24 | Epoxy resin composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61223714A JPH0717815B2 (en) | 1986-09-24 | 1986-09-24 | Epoxy resin composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6381155A JPS6381155A (en) | 1988-04-12 |
| JPH0717815B2 true JPH0717815B2 (en) | 1995-03-01 |
Family
ID=16802517
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61223714A Expired - Fee Related JPH0717815B2 (en) | 1986-09-24 | 1986-09-24 | Epoxy resin composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0717815B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5228327B2 (en) * | 2007-01-30 | 2013-07-03 | 東ソー株式会社 | Method for producing polymer solution |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4072592A (en) * | 1974-05-20 | 1978-02-07 | Mobil Oil Corporation | Radiation curable coating |
| JPS5751427A (en) * | 1980-09-12 | 1982-03-26 | Toyobo Co Ltd | Preparation of polyamide laminated film |
| US4383061A (en) * | 1981-06-25 | 1983-05-10 | The United States Of America As Represented By The Secretary Of The Navy | Epoxy smoothing compound |
| JPS5765744A (en) * | 1981-08-03 | 1982-04-21 | Mitsui Toatsu Chem Inc | Prevention of spotting of vinyl chloride resin product |
| JPS58213018A (en) * | 1982-06-03 | 1983-12-10 | Mitsubishi Electric Corp | Epoxy resin composition |
| JPS6126622A (en) * | 1984-07-13 | 1986-02-05 | Matsushita Electric Works Ltd | Preparation of molding material for commutator |
-
1986
- 1986-09-24 JP JP61223714A patent/JPH0717815B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6381155A (en) | 1988-04-12 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |