JP4451093B2 - One-part casting epoxy resin composition and coil using the same - Google Patents
One-part casting epoxy resin composition and coil using the same Download PDFInfo
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- JP4451093B2 JP4451093B2 JP2003277592A JP2003277592A JP4451093B2 JP 4451093 B2 JP4451093 B2 JP 4451093B2 JP 2003277592 A JP2003277592 A JP 2003277592A JP 2003277592 A JP2003277592 A JP 2003277592A JP 4451093 B2 JP4451093 B2 JP 4451093B2
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- 239000003822 epoxy resin Substances 0.000 title claims description 49
- 229920000647 polyepoxide Polymers 0.000 title claims description 49
- 239000000203 mixture Substances 0.000 title claims description 47
- 238000005266 casting Methods 0.000 title claims description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- -1 boron trichloride amine Chemical class 0.000 claims description 14
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims description 13
- 239000011256 inorganic filler Substances 0.000 claims description 11
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 238000003860 storage Methods 0.000 description 16
- 150000008065 acid anhydrides Chemical class 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 150000001412 amines Chemical class 0.000 description 6
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 description 5
- 239000002518 antifoaming agent Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- 230000009477 glass transition Effects 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- GJTUEPSATYEPPR-UHFFFAOYSA-N octan-1-amine;trichloroborane Chemical compound ClB(Cl)Cl.CCCCCCCCN GJTUEPSATYEPPR-UHFFFAOYSA-N 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 2
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 125000000113 cyclohexyl group Chemical class [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
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- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
本発明は一液型注形用エポキシ樹脂組成物およびそれを用いたコイルに係り、特に保存安定性、作業性、信頼性に優れた一液型注形用エポキシ樹脂組成物に関する。 The present invention relates to a one-pack type epoxy resin composition for casting and a coil using the same, and particularly to a one-pack type epoxy resin composition for casting which is excellent in storage stability, workability and reliability.
従来より、エポキシ樹脂組成物は自動車に内蔵される点火コイルや、テレビジョン受像機、コンピュータのディスプレイ装置に内蔵されるフライバックトランス等の絶縁処理に広く用いられている。 Conventionally, epoxy resin compositions have been widely used for insulation treatment of ignition coils incorporated in automobiles, television receivers, flyback transformers incorporated in computer display devices, and the like.
このような注形用エポキシ樹脂組成物は保存安定性を重視して、エポキシ樹脂を主成分とする主剤と、酸無水物やアミンを主成分とする硬化剤との二液に分けて、使用直前に混合する二液型のものが主流となっている。 Such an epoxy resin composition for casting is used by separating into two parts, a main agent mainly composed of epoxy resin and a curing agent mainly composed of acid anhydride and amine, with an emphasis on storage stability. The two-pack type that is mixed immediately before is the mainstream.
しかしながら、二液型の注形用エポキシ樹脂組成物については、いくつかの課題がある。第一に、二液計量機および混合機が不可欠であり、それらの購入、維持に費用がかかる。第二に、主剤と硬化剤との混合比ずれ、混合不十分等、二液型特有の混合作業に伴う不良要因がある。第三に、混合後の使用可能時間（可使時間）が短いため混合後、速やかに注形、硬化する必要があり、ライントラブル等の異常に対応しにくい。 However, there are several problems with the two-pack type epoxy resin composition for casting. First, a two-component weigher and a mixer are essential, and they are expensive to purchase and maintain. Secondly, there are failure factors associated with the mixing operation peculiar to the two-component type, such as a mixing ratio shift between the main agent and the curing agent, and insufficient mixing. Third, since the usable time (pot life) after mixing is short, it is necessary to cast and cure immediately after mixing, and it is difficult to cope with abnormalities such as line troubles.
これらの問題を解決するのに最も有効なのは一液型に変更することであるが、従来の二液型エポキシ樹脂組成物を単に混合しただけでは保存安定性を向上させることは困難である。保存安定性を向上させるため、例えば酸無水物を硬化剤として用いると共に、潜在型の硬化促進剤を用いることが検討されている（例えば、特許文献１参照。）。 The most effective way to solve these problems is to change to a one-pack type, but it is difficult to improve the storage stability simply by mixing conventional two-pack type epoxy resin compositions. In order to improve storage stability, for example, an acid anhydride is used as a curing agent, and the use of a latent curing accelerator has been studied (for example, see Patent Document 1).
しかしながら、硬化剤として酸無水物を使用する場合、酸無水物が吸湿に極めて弱い為（水と反応して酸になる）、保存安定性を向上させるためには製造時の吸湿防止、充填材に付着した水分の除去等の課題がある。 However, when an acid anhydride is used as a curing agent, the acid anhydride is extremely vulnerable to moisture absorption (reacts with water to form an acid). There are problems such as removal of water adhering to the surface.
本発明は上記したような課題を解決するためになされたものであって、自動車に内蔵される点火コイルや、テレビジョン受像機、コンピュータのディスプレイ装置に内蔵されるフライバックトランス等の絶縁処理に好適に用いられるものであって、保存安定性に優れるとともに、その製造が容易である一液型注形用エポキシ樹脂組成物およびそれを用いたコイルを提供することを目的としている。 The present invention has been made to solve the above-described problems, and is used for insulation processing of an ignition coil incorporated in an automobile, a television receiver, a flyback transformer incorporated in a computer display device, and the like. It is an object of the present invention to provide a one-pack type epoxy resin composition for casting and a coil using the same, which are suitably used and have excellent storage stability and are easy to produce.
本発明者は上記目的を違成しようと鋭意研究を進めた結果、後述のエポキシ樹脂組成物を用いることによって、上記目的を達成できることを見いだし、本発明を完成したものである。 As a result of diligent research to make the above object unusable, the present inventor has found that the above object can be achieved by using an epoxy resin composition described later, and has completed the present invention.
即ち、本発明の一液型注形用エポキシ樹脂組成物は、（Ａ）液状エポキシ樹脂、（Ｂ）硬化剤として三塩化ホウ素アミン錯体のみ、および（Ｃ）無機質充填材としてシリカを必須成分としてなるものであって、前記（Ｃ）無機質充填材としてのシリカの含有量が前記（Ａ）液状エポキシ樹脂１００重量部に対して５０〜２５０重量部であることを特徴とするものである。 That is, the one-part casting epoxy resin composition of the present invention comprises (A) a liquid epoxy resin, (B) only a boron trichloride amine complex as a curing agent , and (C) silica as an essential component as an inorganic filler. The content of silica as the inorganic filler (C) is 50 to 250 parts by weight with respect to 100 parts by weight of the liquid epoxy resin (A) .
本発明のコイルは、上述したような一液型注形用エポキシ樹脂組成物で注形、硬化させたことを特徴とするものである。 The coil of the present invention is characterized by being cast and cured with the above-described one-pack type epoxy resin composition for casting.
本発明では、一液型注形用エポキシ樹脂組成物に用いられる硬化剤として三塩化ホウ素アミン錯体のみを用い、無機質充填材として所定量のシリカを用いることで、製造が容易で、かつ優れた保存安定性、作業性、信頼性を有する一液型注形用エポキシ樹脂組成物を提供することができる。 In the present invention, only the boron trichloride amine complex is used as the curing agent used in the one-part casting epoxy resin composition, and a predetermined amount of silica is used as the inorganic filler , so that the production is easy and excellent. An epoxy resin composition for one-part casting having storage stability, workability, and reliability can be provided.
また、このような一液型注形用エポキシ樹脂組成物を用いてコイルを製造することにより、コイルの製造が容易になるとともに、優れた信頼性を有するコイルを提供することができる。 Moreover, by manufacturing a coil using such a one-pack type epoxy resin composition for casting, the coil can be easily manufactured and a coil having excellent reliability can be provided.
本発明に用いられる（Ａ）液状エポキシ樹脂としては、１分子中に２個以上のエポキシ基を有する化合物であればよく、分子構造、分子量等は特に制限されることなく一般に使用されているものを広く用いることができる。（Ａ）液状エポキシ樹脂は、特に粘度が１〜１５Ｐａ・ｓ（２５℃）であれば好ましい。 The (A) liquid epoxy resin used in the present invention may be a compound having two or more epoxy groups in one molecule, and the molecular structure, molecular weight, etc. are generally used without any particular limitation. Can be widely used. The (A) liquid epoxy resin is particularly preferable if the viscosity is 1 to 15 Pa · s (25 ° C.).
（Ａ）液状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、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のエポキシ化により得られるエポキシ樹脂等が挙げられ、これらは単独または２種以上混合して用いることができる。これらの他に必要に応じて液状のモノエポキシ樹脂を用いることができる。 Examples of the (A) liquid epoxy resin include bisphenol A type epoxy resin, bisphenol F type epoxy resin, glycidyl ether of polycarboxylic acid, and epoxy resins obtained by epoxidation of cyclohexane derivatives. A mixture of the above can be used. In addition to these, a liquid monoepoxy resin can be used as necessary.
本発明に用いられる（Ｂ）三塩化ホウ素アミン錯体は、三塩化ホウ素にアミン類が配位したものであり、このアミン類は特に制限されるものではなく、例えばモノエチルアミン（Ｃ２Ｈ５−ＮＨ２）等のアルキルアミン、ベンジルアミン（Ｃ６Ｈ５−ＣＨ２−ＮＨ２）等が挙げられる。 The (B) boron trichloride amine complex used in the present invention is one in which amines are coordinated to boron trichloride, and these amines are not particularly limited. For example, monoethylamine (C 2 H 5 − NH 2) alkylamines such as benzylamine (C 6 H 5 -CH 2 -NH 2) , and the like.
（Ｂ）三塩化ホウ素アミン錯体としては市販されているものを使用することができ、このようなものとしては例えば三塩化ホウ素オクチルアミン錯体であるＤＹ９５７７（バンティコ（株）製、商品名）等を用いることができる。上述したような（Ｂ）三塩化ホウ素アミン錯体は１種のみを用いてもよいし、２種以上を混合して用いてもよい。 (B) A commercially available boron trichloride amine complex can be used. Examples of such a boron trichloride amine complex include DY9577 (trade name, manufactured by Bantico Co., Ltd.) which is a boron trichloride octylamine complex. Can be used. As for the (B) boron trichloride amine complex as described above, only one kind may be used, or two or more kinds may be mixed and used.
本発明では一液型注形用エポキシ樹脂組成物において硬化剤として（Ｂ）三塩化ホウ素アミン錯体を用いることで、硬化物のガラス転移点、機械的強度および体積抵抗率を従来と同程度としたまま、保存安定性や作業性を向上させることができる。例えば、ガラス転移点については１００℃以上とすることができる。 In the present invention, the (B) boron trichloride amine complex is used as the curing agent in the one-part type epoxy resin composition for casting, so that the glass transition point, mechanical strength, and volume resistivity of the cured product are approximately the same as those in the past. Thus, the storage stability and workability can be improved. For example, the glass transition point can be 100 ° C. or higher.
本発明の一液型注形用エポキシ樹脂組成物では保存安定性や作業性を向上させるため、硬化剤として（Ｂ）三塩化ホウ素アミン錯体のみを添加し、それ以外に硬化剤として酸無水物やアミン類を添加しないことが好ましい。 In the one-part type epoxy resin composition for casting according to the present invention, in order to improve storage stability and workability, only (B) boron trichloride amine complex is added as a curing agent, and in addition to that, an acid anhydride as a curing agent It is preferable that no amines are added.
例えば、酸無水物は水分と容易に反応して酸になり、エポキシ樹脂組成物の保存安定性を低下させてしまう。このため硬化剤として酸無水物を用いる場合には保存安定性の低下を抑制するために、製造行程での雰囲気からの吸湿を抑制するような処置を採る必要があり、また、エポキシ樹脂組成物に添加する充填材等に付着した水分も除去しなければならない。 For example, an acid anhydride easily reacts with moisture to become an acid, thereby reducing the storage stability of the epoxy resin composition. For this reason, when an acid anhydride is used as a curing agent, it is necessary to take measures to suppress moisture absorption from the atmosphere in the manufacturing process in order to suppress a decrease in storage stability, and an epoxy resin composition The water adhering to the filler added to the water must also be removed.
本発明では硬化剤として（Ｂ）三塩化ホウ素アミン錯体のみを添加し、酸無水物やアミン類を添加しないようにすることで、上述したような水分の混入を抑制するための特別な吸湿防止処置等を採ることなく、保存安定性、作業性に優れた一液型注形用エポキシ樹脂組成物を容易に得ることができる。 In the present invention, by adding only the boron trichloride amine complex (B) as a curing agent and not adding an acid anhydride or amines, a special moisture absorption prevention for suppressing the mixing of moisture as described above. Without taking any treatment or the like, it is possible to easily obtain an epoxy resin composition for one-part casting excellent in storage stability and workability.
一液型注形用エポキシ樹脂組成物における（Ｂ）三塩化ホウ素アミン錯体の含有量は、（Ａ）液状エポキシ樹脂１００重量部に対して１〜１０重量部の範囲とすることが好ましい。（Ｂ）三塩化ホウ素アミン錯体の含有量が１重量部未満であると硬化剤としての効果が低く、１０重量部を超える場合、一液型注形用エポキシ樹脂組成物の保存安定性が低下するおそれがある。（Ｂ）三塩化ホウ素アミン錯体の含有量は、（Ａ）液状エポキシ樹脂１００重量部に対して１〜５重量部の範囲であればより好ましい。 The content of (B) boron trichloride amine complex in the one-pack type casting epoxy resin composition is preferably in the range of 1 to 10 parts by weight with respect to 100 parts by weight of (A) liquid epoxy resin. (B) If the content of the boron trichloride amine complex is less than 1 part by weight, the effect as a curing agent is low, and if it exceeds 10 parts by weight, the storage stability of the one-part casting epoxy resin composition decreases. There is a risk. The content of (B) boron trichloride amine complex is more preferably in the range of 1 to 5 parts by weight with respect to 100 parts by weight of (A) liquid epoxy resin.
本発明に用いられる（Ｃ）無機質充填材としては特に制限されるものではなく、一般に知られているものを広く使用することができる。（Ｃ）無機質充填材としては、例えばシリカ、タルク、水酸化アルミニウム、炭酸カルシウム等が挙げられ、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。本発明では、（Ｃ）無機質充填材として平均粒径が１〜３０μｍのシリカを用いれば特に好ましい。 The (C) inorganic filler used in the present invention is not particularly limited, and generally known materials can be widely used. (C) As an inorganic filler, silica, talc, aluminum hydroxide, calcium carbonate etc. are mentioned, for example, These can be used individually or in mixture of 2 or more types. In the present invention, it is particularly preferable to use silica having an average particle diameter of 1 to 30 μm as the inorganic filler (C).
（Ｃ）無機質充填材の含有量は、（Ａ）液状エポキシ樹脂１００重量部に対して５０〜２５０重量部の範囲とすることが好ましい。（Ｃ）無機質充填材の含有量が５０重量部未満であると、耐熱衝撃性や機械的強度が十分でなくなるおそれがあり、一方、２５０重量部を超えると一液型注形用エポキシ樹脂組成物の粘度が上昇し、作業性の低下等が発生するため好ましくない。 (C) It is preferable that content of an inorganic filler shall be 50-250 weight part with respect to 100 weight part of (A) liquid epoxy resins. (C) If the content of the inorganic filler is less than 50 parts by weight, the thermal shock resistance and mechanical strength may not be sufficient. On the other hand, if it exceeds 250 parts by weight, the epoxy resin composition for one-part casting This is not preferable because the viscosity of the product increases and workability decreases.
本発明の一液型注形用エポキシ樹脂組成物は、少なくとも上述した（Ａ）液状エポキシ樹脂、（Ｂ）三塩化ホウ素アミン錯体および（Ｃ）無機質充填材を必須成分として配合し、十分に混合することによって得ることができる。 The epoxy resin composition for one-part casting of the present invention contains at least the above-described (A) liquid epoxy resin, (B) boron trichloride amine complex, and (C) inorganic filler as essential components, and sufficiently mixed Can be obtained.
本発明の一液型注形用エポキシ樹脂組成物においては、本発明の目的に反しない範囲において、カップリング剤、消泡剤、顔料、その他成分を添加配合してもよい。 In the one-pack type epoxy resin composition for casting according to the present invention, a coupling agent, an antifoaming agent, a pigment, and other components may be added and blended within the range not contrary to the object of the present invention.
本発明のコイルは、上述したような一液型注形用エポキシ樹脂組成物を常法によりコイルに含浸、注形することにより製造されるものである。本発明の一液型注形用エポキシ樹脂組成物を用いて製造されるコイルは特に限定されるものではなく、例えば自動車に内蔵される点火コイル、テレビジョン受像機やコンピュータのディスプレイ装置に内蔵されるフライバックトランス等に好適に用いることができる。 The coil of the present invention is produced by impregnating and casting the above-described one-pack type epoxy resin composition for casting into a coil by a conventional method. The coil manufactured using the one-part casting epoxy resin composition of the present invention is not particularly limited. For example, an ignition coil incorporated in an automobile, a television receiver, or a display device of a computer. The flyback transformer can be suitably used.
本発明の一液型注形用エポキシ樹脂組成物は保存安定性、作業性に優れるため上述したようなコイルの作製が容易となり、また本発明の一液型注形用エポキシ樹脂組成物の硬化物は従来と同程度のガラス転移点、機械的強度および体積抵抗率等を有するためコイルの信頼性も確保することができる。 The one-part casting epoxy resin composition of the present invention is excellent in storage stability and workability, so that the coil as described above can be easily produced, and the one-part casting epoxy resin composition of the present invention is cured. Since the object has the same glass transition point, mechanical strength, volume resistivity, etc. as the conventional one, the reliability of the coil can be ensured.
以下、本発明について実施例を参照して具体的に説明する。なお、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。 Hereinafter, the present invention will be specifically described with reference to examples. In addition, this invention is not limited by these Examples.
（実施例１）
液状エポキシ樹脂ビスフェノールＡジグリシジルエーテル１００重量部、三塩化ホウ素オクチルアミン錯体ＤＹ９５７７（バンティコ（株）製、商品名）３重量部、シリカ充填材クリスタライトＡ−１（龍森（株）製、商品名）１００重量部、消泡剤ＴＳＡ７２０（東芝シリコーン社製、商品名）０．１重量部、シランカップリング剤０．５重量部を真空下（１３３３Ｐａ）で混合し、一液型注形用エポキシ樹脂組成物を製造した。
Example 1
Liquid epoxy resin bisphenol A diglycidyl ether 100 parts by weight, boron trichloride octylamine complex DY9577 (Bantico Co., Ltd., trade name) 3 parts by weight, silica filler crystallite A-1 (Tatsumori Co., Ltd., product) Name) 100 parts by weight, defoaming agent TSA720 (manufactured by Toshiba Silicone Co., Ltd., trade name) 0.1 part by weight, silane coupling agent 0.5 part by weight are mixed under vacuum (1333 Pa) for one-part casting An epoxy resin composition was produced.
（実施例２）
液状エポキシ樹脂ビスフェノールＡジグリシジルエーテル１００重量部、三塩化ホウ素オクチルアミン錯体ＤＹ９５７７（バンティコ（株）製、商品名）１０重量部、シリカ充填材クリスタライトＡ−１（龍森（株）製、商品名）１００重量部、消泡剤ＴＳＡ７２０（東芝シリコーン社製、商品名）０．１重量部、シランカップリング剤０．５重量部を真空下（１３３３Ｐａ）で混合し、一液型注形用エポキシ樹脂組成物を製造した。
(Example 2)
Liquid epoxy resin bisphenol A diglycidyl ether 100 parts by weight, boron trichloride octylamine complex DY9577 (manufactured by Bantico Co., Ltd., trade name), silica filler Crystallite A-1 (manufactured by Tatsumori Co., Ltd., commodity) Name) 100 parts by weight, defoaming agent TSA720 (manufactured by Toshiba Silicone Co., Ltd., trade name) 0.1 part by weight, silane coupling agent 0.5 part by weight are mixed under vacuum (1333 Pa) for one-part casting An epoxy resin composition was produced.
（比較例１）
ビスフェノールＡジグリシジルエーテル８０重量部、ビスフェノールＡジグリシジルエーテルの変性品ＥＰ４０００（旭電化工業（株）製、商品名）２０重量部、シリカ充填材クリスタライトＡ−１（龍森（株）製、商品名）１３０重量部、消泡剤ＴＳＡ７２０（東芝シリコーン社製、商品名）０．１重量部、およびシランカップリング剤０．５重量部を真空下（１３３３Ｐａ）で混合し、主剤（以下、第１液と呼称する）とした。
(Comparative Example 1)
Bisphenol A diglycidyl ether 80 parts by weight, modified bisphenol A diglycidyl ether EP4000 (Asahi Denka Kogyo Co., Ltd., trade name) 20 parts by weight, silica filler Crystallite A-1 (manufactured by Tatsumori Co., Ltd.) (Trade name) 130 parts by weight, antifoaming agent TSA720 (manufactured by Toshiba Silicone Co., Ltd., trade name) 0.1 part by weight, and silane coupling agent 0.5 part by weight are mixed under vacuum (1333 Pa), (Referred to as the first liquid).
次に、硬化剤としてのメチルテトラヒドロ無水フタル酸１００重量部、硬化促進剤としてのベンジルジメチルアミン０．５重量部を混合し、硬化剤（以下、第２液と呼称する）とした。第１液と第２液とを１００：３０（質量比）で混合して注形用エポキシ樹脂組成物を製造した。 Next, 100 parts by weight of methyltetrahydrophthalic anhydride as a curing agent and 0.5 parts by weight of benzyldimethylamine as a curing accelerator were mixed to obtain a curing agent (hereinafter referred to as the second liquid). The first liquid and the second liquid were mixed at 100: 30 (mass ratio) to produce a casting epoxy resin composition.
（比較例２）
ビスフェノールＡジグリシジルエーテル１００重量部、シリカ充填材クリスタライトＡ−１（隷森（株）製、商品名）１３０重量部、消泡剤ＴＳＡ７２０（東芝シリコーン社製、商品名）０．１重量部、およびシランカップリング剤０．５重量部を真空下（１３３３Ｐａ）で混合し、第１液とした。
(Comparative Example 2)
Bisphenol A diglycidyl ether 100 parts by weight, silica filler crystallite A-1 (manufactured by Slave Mori Co., Ltd., trade name) 130 parts by weight, antifoaming agent TSA720 (manufactured by Toshiba Silicone, trade name) 0.1 parts by weight And 0.5 part by weight of a silane coupling agent were mixed under vacuum (1333 Pa) to obtain a first liquid.
次に、硬化剤としてのメチルヘキサヒドロ無水フタル酸１００重量部、硬化促進剤としてベンジルジメチルアミン０．５重量部を混合し、第２液とした。第１液と第２液とを１００：３０（質量比）で混合して注形用エポキシ樹脂組成物を製造した。 Next, 100 parts by weight of methylhexahydrophthalic anhydride as a curing agent and 0.5 parts by weight of benzyldimethylamine as a curing accelerator were mixed to obtain a second liquid. The first liquid and the second liquid were mixed at 100: 30 (mass ratio) to produce a casting epoxy resin composition.
実施例１〜２の一液型注形用エポキシ樹脂組成物および比較例１〜２の注形用エポキシ樹脂組成物について保存安定性、ゲルタイムおよび含浸性を評価した。また、実施例１〜２の一液型注形用エポキシ樹脂組成物および比較例１〜２の注形用エポキシ樹脂組成物を加熱硬化し、得られた硬化物についてガラス転移点、曲げ強さおよび体積抵抗率を評価した。結果を表１に示す。 Storage stability, gel time, and impregnation property were evaluated for the one-part casting epoxy resin compositions of Examples 1-2 and the casting epoxy resin compositions of Comparative Examples 1-2. Also, the one-part casting epoxy resin compositions of Examples 1 and 2 and the casting epoxy resin compositions of Comparative Examples 1 and 2 were heat-cured, and the obtained cured products had a glass transition point and bending strength. And volume resistivity was evaluated. The results are shown in Table 1.
なお、保存安定性の評価は、各注形用エポキシ樹脂組成物を４０℃で放置し、初期粘度の２倍の粘度になるまでの日数で評価した。ゲルタイムの評価は、注形用エポキシ樹脂組成物を１００℃の熱板上で練り合わせ、試料が増粘し、最終的に粘りがなくなったときの時間（分）で評価した。 The storage stability was evaluated by allowing each casting epoxy resin composition to stand at 40 ° C. and evaluating the number of days until the viscosity reached twice the initial viscosity. The gel time was evaluated by measuring the time (minutes) when the casting epoxy resin composition was kneaded on a hot plate at 100 ° C. and the sample was thickened and finally no longer sticky.
含浸性は濾紙法により評価するものとし、濾紙５Ｃ（東洋濾紙社製、商品名）を８分割に折り、その中に各注形用エポキシ樹脂組成物を入れ、この状態で台座に設置しオーブン中で１００℃、３時間の熱処理を行い、その間に濾紙から滴下した樹脂成分の量を測定することにより評価した。 The impregnation property is evaluated by the filter paper method. Fold the filter paper 5C (product name, manufactured by Toyo Roshi Kaisha Co., Ltd.) into 8 parts, put the epoxy resin composition for casting into it, and place it on the pedestal in this state. In this, heat treatment was performed at 100 ° C. for 3 hours, and the amount of the resin component dripped from the filter paper was measured during the heat treatment.
表１から明らかなように、硬化剤として三塩化ホウ素アミンを用いた実施例１、２の一液型注形用エポキシ樹脂組成物においては、硬化剤としてアミン類や酸無水物を用いた比較例１、２の注形用エポキシ樹脂組成物と比べて保存安定性、作業性に優れると共に、その硬化物の特性を比較例１、２の注形用エポキシ樹脂組成物と同程度に確保できることが認められた。 As is apparent from Table 1, in the one-part type epoxy resin composition for casting of Examples 1 and 2 using boron trichloride as a curing agent, a comparison using amines or acid anhydrides as the curing agent was performed. Compared to the casting epoxy resin compositions of Examples 1 and 2, the storage stability and workability are excellent, and the properties of the cured products can be secured to the same extent as the casting epoxy resin compositions of Comparative Examples 1 and 2. Was recognized.
Claims (2)
前記（Ｃ）無機質充填材としてのシリカの含有量が前記（Ａ）液状エポキシ樹脂１００重量部に対して５０〜２５０重量部であることを特徴とする一液型注形用エポキシ樹脂組成物。 (A) a liquid epoxy resin, (B) a boron trichloride amine complex only as a curing agent , and (C) a one-pack type epoxy resin composition for casting containing silica as an essential component as an inorganic filler ,
Content of silica as said (C) inorganic filler is 50-250 weight part with respect to 100 weight part of said (A) liquid epoxy resin , The epoxy resin composition for one-pack type castings characterized by the above-mentioned.
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