JPH03227317A - Liquid epoxy resin composition - Google Patents
Liquid epoxy resin compositionInfo
- Publication number
- JPH03227317A JPH03227317A JP2355490A JP2355490A JPH03227317A JP H03227317 A JPH03227317 A JP H03227317A JP 2355490 A JP2355490 A JP 2355490A JP 2355490 A JP2355490 A JP 2355490A JP H03227317 A JPH03227317 A JP H03227317A
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- component
- succinic anhydride
- parts
- bisphenol
- 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.)
- Pending
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 20
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 title claims description 5
- 239000003822 epoxy resin Substances 0.000 claims abstract description 51
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 51
- 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 claims abstract description 18
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 14
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229940014800 succinic anhydride Drugs 0.000 claims abstract description 10
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 7
- 229920005862 polyol Polymers 0.000 claims abstract description 7
- -1 polyol compound Chemical class 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 238000005266 casting Methods 0.000 abstract description 5
- 238000007789 sealing Methods 0.000 abstract description 3
- FLISWPFVWWWNNP-BQYQJAHWSA-N dihydro-3-(1-octenyl)-2,5-furandione Chemical compound CCCCCC\C=C\C1CC(=O)OC1=O FLISWPFVWWWNNP-BQYQJAHWSA-N 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical class C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 7
- 239000004593 Epoxy Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 3
- WVRNUXJQQFPNMN-VAWYXSNFSA-N 3-[(e)-dodec-1-enyl]oxolane-2,5-dione Chemical compound CCCCCCCCCC\C=C\C1CC(=O)OC1=O WVRNUXJQQFPNMN-VAWYXSNFSA-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 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 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
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229920002857 polybutadiene Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- KAYAKFYASWYOEB-UHFFFAOYSA-N 3-octadec-1-enyloxolane-2,5-dione Chemical compound CCCCCCCCCCCCCCCCC=CC1CC(=O)OC1=O KAYAKFYASWYOEB-UHFFFAOYSA-N 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- OWYWGLHRNBIFJP-UHFFFAOYSA-N Ipazine Chemical compound CCN(CC)C1=NC(Cl)=NC(NC(C)C)=N1 OWYWGLHRNBIFJP-UHFFFAOYSA-N 0.000 description 1
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 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
- 238000002156 mixing Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、電気部品や電子部品の分野において用いて好
適な液状エポキシ樹脂組成物に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a liquid epoxy resin composition suitable for use in the fields of electrical parts and electronic parts.
エポキシ樹脂は、耐熱性、耐薬品性に優れ、近年、電気
・電子部品の絶縁、保護を目的とした注型又は封止材料
として広く用いられている。Epoxy resin has excellent heat resistance and chemical resistance, and has recently been widely used as a casting or sealing material for the purpose of insulating and protecting electrical and electronic components.
しかしながら、エポキシ樹脂を前記用途で温度変化の激
しい電気・電子部品、例えば、セラミックコンデンサー
、フォーカス抵抗、ハイブリッドＩＣ、フライバックト
ランス等の注型材料として使用する場合、電気・電子部
品と硬化エポキシ樹脂とでは、その線膨張係数に差があ
る為に、冷熱サイクル時に部品と硬化エポキシ樹脂との
間の界面に剥離が生じたり、硬化エポキシ樹脂にクラッ
クが発生し、絶縁不良の原因になっていた。However, when epoxy resin is used as a casting material for electrical/electronic parts subject to large temperature changes, such as ceramic capacitors, focus resistors, hybrid ICs, flyback transformers, etc., the electrical/electronic parts and the cured epoxy resin are However, due to the difference in linear expansion coefficient, peeling occurs at the interface between the component and the cured epoxy resin during cooling and heating cycles, and cracks occur in the cured epoxy resin, causing insulation failure.
そこで、これまでに、エポキシ樹脂注型部品の冷熱サイ
クル性を向上させる為に、樹脂中に充填剤を高充填させ
て硬化物の線膨張係数を低下させることや、可撓性エポ
キシ樹脂、例えばダイマー酸変性エポキシ樹脂、グリコ
ール変性エポキシ樹脂、ウレタン変性エポキシ樹脂等を
用いて硬化物の弾性率を低下させることが行われている
。またエポキシ樹脂にゴム状物質を添加して硬化に際し
ての応力を吸収することも知られている。Therefore, in order to improve the thermal cycle performance of epoxy resin cast parts, methods have been developed to lower the linear expansion coefficient of the cured product by filling the resin with a high filler, and to improve the thermal cycle properties of epoxy resin cast parts. Dimer acid-modified epoxy resins, glycol-modified epoxy resins, urethane-modified epoxy resins, and the like have been used to lower the elastic modulus of cured products. It is also known to add rubber-like substances to epoxy resins to absorb stress during curing.
しかしながら、冷熱サイクル性を向上させるために提案
された従来のエポキシ樹脂組成物では、粘度上昇に伴う
作業性の低下や、その硬化物の絶縁性、耐湿性の低下等
の問題が残り、未だ満足し得るまでには至っていない。However, conventional epoxy resin compositions proposed to improve thermal cycle performance remain unsatisfactory due to problems such as decreased workability due to increased viscosity and decreased insulation and moisture resistance of the cured product. I haven't reached the point where I can do it.
本発明は、従来技術に見られる前記問題点を解決し、冷
熱サイクル性、電気特性、耐湿性に優れた液状エポキシ
樹脂組成物を提供することをその課題とする。An object of the present invention is to solve the above-mentioned problems found in the prior art and to provide a liquid epoxy resin composition that has excellent thermal cycleability, electrical properties, and moisture resistance.
本発明者らは、前記課題を解決すべく鋭意研究を重ねた
結果、汎用エポキシ樹脂と、特定のビスフェノールＡ型
エポキシ樹脂を併用し、特定の硬化剤を用いて得た硬化
物は、冷熱サイクル性、電気特性、耐湿性に優れている
ことを見出し、本発明を完成するに至った。As a result of extensive research to solve the above problems, the present inventors have found that a cured product obtained by using a general-purpose epoxy resin and a specific bisphenol A type epoxy resin together and using a specific curing agent can be cured by heating and cooling cycles. The present inventors have discovered that this material has excellent properties such as electrical properties, electrical properties, and moisture resistance, and have completed the present invention.
すなわち本発明によれば、エポキシ樹脂と、般式
（式中、Ｒ１は水素原子又はアルキル基、Ｒ２はアルキ
ル基である）
で示されるビスフェノールＡ型エポキシ樹脂（以下特殊
エポキシ樹脂という）と、アルケニル基含有無水コハク
酸からなる液状エポキシ樹脂組成物が提供される。That is, according to the present invention, an epoxy resin, a bisphenol A type epoxy resin (hereinafter referred to as special epoxy resin) represented by the general formula (wherein R1 is a hydrogen atom or an alkyl group, and R2 is an alkyl group), and an alkenyl Liquid epoxy resin compositions comprising group-containing succinic anhydride are provided.
本発明に用いられるエポキシ樹脂としては、そのエポキ
シ当量、化学構造、分子量は特に制限が無く、例えばビ
スフェノールＡ型エポキシ樹脂、水添ビスフェノールＡ
型エポキシ樹脂、ビスフェノールＦ型エポキシ樹脂、ビ
スフェノールＡＤ型エポキシ樹脂、環式脂肪族エポキシ
樹脂等が用いられ、これらの樹脂は単独又は混合物の形
で液状で用いられる。The epoxy resin used in the present invention is not particularly limited in its epoxy equivalent, chemical structure, or molecular weight, and examples include bisphenol A type epoxy resin, hydrogenated bisphenol A
Type epoxy resins, bisphenol F type epoxy resins, bisphenol AD type epoxy resins, cycloaliphatic epoxy resins, etc. are used, and these resins are used alone or in the form of a mixture in liquid form.
本発明における特殊エポキシ樹脂は、前記一般式（Ｉ）
で示されるもので、その粘度は約１０００ＵＰＳ７２５
℃である。この特殊エポキシ樹脂成分は、汎用エポキシ
樹脂との合計量に対して１０〜５００〜５０重量部くは
１５〜４０Ｍ量２の割合で配合することができる。The special epoxy resin in the present invention has the general formula (I)
The viscosity is approximately 1000UPS725
It is ℃. This special epoxy resin component can be blended in an amount of 10 to 500 to 50 parts by weight or 15 to 40 M2 based on the total amount of the general-purpose epoxy resin.
本発明に用いられるアルケニル基含有無水コハク酸とし
ては、例えば次の一般式で表わされるものが用いら九る
。Examples of the alkenyl group-containing succinic anhydride used in the present invention include those represented by the following general formula.
前記式中、Ｒ３はアルケニル基を示す。アルケニル基と
しては、ビニル基をはじめとした各種のものが挙げられ
るが、炭素数８〜３０の直鎖又は分岐鎖状のアルケニル
基が好ましい。アルケニル基含有無水コハク酸の具体例
としては、例えば、オクテニル無水コハク酸、ドデセニ
ル無水コハク酸、オクタデセニル無水コハク酸等が挙げ
られる。これらのものは硬化剤として用いられる。また
、前記アルケニル基含有無水コハク酸には、必要に応じ
。In the above formula, R3 represents an alkenyl group. Examples of the alkenyl group include various types including vinyl groups, but straight chain or branched alkenyl groups having 8 to 30 carbon atoms are preferred. Specific examples of the alkenyl group-containing succinic anhydride include octenyl succinic anhydride, dodecenyl succinic anhydride, octadecenyl succinic anhydride, and the like. These materials are used as curing agents. In addition, for the alkenyl group-containing succinic anhydride, as necessary.
本発明の目的を阻害しない範囲で、メチルテトラヒドロ
無水フタル酸、メチルへキサヒドロ無水フタル酸等の常
温で液状のポリカルボン酸を補助硬化剤として用いるこ
とができる。これらの硬化剤は、全エポキシ樹脂１当量
に対して、０．６〜１．２当量、好ましくは０．７〜１
．１当量で用いられる。重量基準で表現すると、硬化剤
成分は、全エポキシ樹脂１００重量部に対し、５０〜２
５０重量部、好ましくは７０〜２００重量部の割合であ
る。Polycarboxylic acids that are liquid at room temperature, such as methyltetrahydrophthalic anhydride and methylhexahydrophthalic anhydride, can be used as an auxiliary curing agent within a range that does not impede the object of the present invention. These curing agents are used in an amount of 0.6 to 1.2 equivalents, preferably 0.7 to 1 equivalent, per equivalent of the total epoxy resin.
．． 1 equivalent is used. Expressed on a weight basis, the curing agent component is 50 to 2 parts by weight per 100 parts by weight of the total epoxy resin.
The proportion is 50 parts by weight, preferably 70 to 200 parts by weight.
本発明の組成物には、冷熱サイクル性の向上を目的とし
て、前記硬化剤に分子量が５００〜５０００のゴム状ポ
リオール化合物を配合することができる。In the composition of the present invention, a rubbery polyol compound having a molecular weight of 500 to 5,000 can be blended with the curing agent for the purpose of improving thermal cycle properties.
このポリオール成分としては、分子量８００〜４０００
の比較的低粘度の水酸基を末端に有するゴム状物質、例
えばポリブタジェンが好適である。また、このポリオー
ル成分は、全エポキシ樹脂１００重量部に対して、５〜
６０重量部、好ましくは１０〜４０重量部である。この
ポリオール化合物は、アルケニル基含有無水コハク酸に
添加し、８０〜１５０℃で２〜５時間加熱して部分エス
テルとして使用できる。ポリオール化合物添加量が５重
量部未満であると、冷熱サイクル性は向上するまでに至
らず、一方６０重量部を越えると、高温時の電気的特性
及び耐湿性が低下する。This polyol component has a molecular weight of 800 to 4000.
Hydroxyl-terminated rubbery materials of relatively low viscosity, such as polybutadiene, are preferred. Moreover, this polyol component is 5 to 5 parts by weight based on 100 parts by weight of the total epoxy resin.
The amount is 60 parts by weight, preferably 10 to 40 parts by weight. This polyol compound can be used as a partial ester by adding it to alkenyl group-containing succinic anhydride and heating it at 80 to 150°C for 2 to 5 hours. If the amount of the polyol compound added is less than 5 parts by weight, the thermal cycleability will not improve, while if it exceeds 60 parts by weight, the electrical properties and moisture resistance at high temperatures will deteriorate.
本発明においては、前記成分以外に補助成分として、シ
ランカップリング剤、硬化促進剤、無機充填剤、希釈剤
、難燃剤、消泡剤、着色剤等を必要に応じて添加するこ
とができる。シランカップリング剤の添加量は、全エポ
キシ樹脂１００重量部に対し０．５〜５重量部の割合で
あり、無機充填剤の添加量は、５０−３００重量部の割
合である。In the present invention, in addition to the above-mentioned components, auxiliary components such as a silane coupling agent, a curing accelerator, an inorganic filler, a diluent, a flame retardant, an antifoaming agent, a coloring agent, etc. can be added as necessary. The amount of the silane coupling agent added is 0.5 to 5 parts by weight based on 100 parts by weight of the total epoxy resin, and the amount of the inorganic filler added is 50 to 300 parts by weight.
本発明のエポキシ樹脂組成物は、エポキシ樹脂に特殊エ
ポキシ樹脂を配合するとともに、硬化剤にアルケニル基
含有無水コハク酸を用いたことにより、冷熱サイクル性
、電気特性、耐湿性にすくれたもので、電気・電子部品
の封止ないし注型材料として好適のものである。即ち、
本発明のエポキシ樹脂組成物を用いて封止又は注型処理
して得た電気・電子部品は過酷な冷熱サイクルを受けて
も、電気・電子部品と硬化樹脂膜との間に剥離を生じた
り、硬化樹脂膜にクラックを生じるようなことがない上
、高温時の電気特性、特に抵抗値低下が少なく、かつ耐
湿性に極めてすぐれている。The epoxy resin composition of the present invention has excellent cold/heat cycle properties, electrical properties, and moisture resistance by blending a special epoxy resin with the epoxy resin and using alkenyl group-containing succinic anhydride as a curing agent. It is suitable as a sealing or casting material for electric/electronic parts. That is,
Electrical/electronic parts obtained by sealing or casting using the epoxy resin composition of the present invention do not cause peeling between the electrical/electronic parts and the cured resin film even when subjected to severe cooling and heating cycles. In addition to not causing cracks in the cured resin film, the electrical properties at high temperatures, especially the decrease in resistance value, are small, and the moisture resistance is extremely excellent.
本発明の組成物は、絶縁用接着剤としても好適なもので
ある。この場合、組成物にはチクソ性付与剤、例えば、
シリコーンオイル処理した微細シリカを全エポキシ樹脂
１００重量部に対し、０．５〜１０重量部の割合で無機
充填剤とともに配合し、適度のチクソ性を付与させる。The composition of the present invention is also suitable as an insulating adhesive. In this case, the composition includes a thixotropic agent, e.g.
Fine silica treated with silicone oil is blended with an inorganic filler in an amount of 0.5 to 10 parts by weight based on 100 parts by weight of the total epoxy resin to impart appropriate thixotropy.
本発明の組成物は、一般には、エポキシ樹脂５０〜９０
重量Ｘと、前記一般式（１）で表わされる特殊エポキシ
樹脂１０〜５０重量％とからなる混合エポキシ樹脂成分
１００重量部と、硬化剤５０〜２５０重量部からなる２
液型のエポキシ樹脂組成物として有利に取扱われる。The composition of the present invention generally has an epoxy resin of 50 to 90%
100 parts by weight of a mixed epoxy resin component consisting of weight
It is advantageously handled as a liquid type epoxy resin composition.
次に本発明を実施例によりさらに詳細に説明する。 Next, the present invention will be explained in more detail with reference to Examples.
実施例１
表−１に示す成分組成のエポキシ樹脂成分（Ａ）と硬化
剤成分（Ｂ）とを調製した。Example 1 An epoxy resin component (A) and a curing agent component (B) having the component compositions shown in Table 1 were prepared.
実施例２
冷熱サイクル性のより向上したエポキシ樹脂組成物とし
て、表−２に示す成分組成のエポキシ樹脂成分（Ａ）と
硬化剤成分（Ｂｌとをｇａした。Example 2 As an epoxy resin composition with improved thermal cycleability, the epoxy resin component (A) and the curing agent component (Bl) having the component composition shown in Table 2 were used in ga.
なお、表−１、表−２中の各成分に関する具体的内容を
以下に示す。In addition, the specific content regarding each component in Table-1 and Table-2 is shown below.
エポキシ樹脂（８２８） ：油化シェルエポキシ社製、
製品名：エピコート８８２８．エポ
キシ当量：１８８
特殊エポキシ樹脂：日本チバガイギー社製、製品名：エ
ポキシ樹脂ＸＢ４１２２（一般
式（１）におけるＲ＝Ｃ，Ｈ，）、エポキシ当量：３２
０
側鎖型ビスフェノールＡ型エポキシ樹脂：加電化工業社
製、製品名；アデカＥＰ−４００
０（下記式で表わされる）、エポ
キシ当量＝３２５
ポリプロピレングリコールエポキシ樹脂：旭電化工業社
製、製品名ニアデカＥＤ−
５０６、エポキシ当量：３００
エポキシ樹脂（８７１）：油化シェルエポキシ社製、製
品名：エピコート＃８７１、エポキシ当量：４３０メチ
ルテトラヒドロ無水フタル酸二大日本インキ化学社製、
製品名：エピクロン
−５７０
ドデセニル無水コハク酸：三洋化成社製、製品名：ＤＤ
ＳＡ （下記式で表わされる）
アルケニル無水フタル酸：東邦化学社製、製品名：Ｂ−
３０Ｏ３（下記式で表わされる）
Ｉ？５
（Ｒ４，Ｒ５：炭素原子数１３〜１７のアルキル基）２
．４．６−トリス（ジメチルアミノメチル）フェノール
のトリー２−エチルヘキシル酸塩：日本化薬社製、製品
名：に−６１Ｂ
トリフェニルホスフィン：ケイ・アイ化成社製、製品名
：ＰＰ−３６０
結晶性シリカ：龍森社製、製品名：クリスタライトＡ−
１
シリコーンオイル処理微細シリカニ日本アエロジル社製
、製品名：アエロジルＲ
０２
３−グリシドキシプロピルトリメトキシシラン：チッソ
社製、製品名：Ｓ−５１０
末端水酸基ポリブタジェン：出光石油化学社製、製品名
：Ｒ−１５ＨＴ、分子量：１２００次に実施例１、実施
例２で調製したエポキシ樹脂成分〔Ａ］と硬化剤成分Ｃ
Ｂ）とを理論当量で配合し、１００℃、５時間で硬化さ
せて、その硬化物について、■冷熱サイクル性、■高温
時の電気特性、■耐湿性を以下のようにして評価した。Epoxy resin (828): Manufactured by Yuka Shell Epoxy Co., Ltd.
Product name: Epicote 8828. Epoxy equivalent: 188 Special epoxy resin: Manufactured by Ciba Geigy Japan, product name: Epoxy resin XB4122 (R=C, H, in general formula (1)), epoxy equivalent: 32
0 Side chain type bisphenol A type epoxy resin: Manufactured by Kadenka Kogyo Co., Ltd., product name: ADEKA EP-400 0 (represented by the formula below), epoxy equivalent = 325 Polypropylene glycol epoxy resin: Manufactured by Asahi Denka Kogyo Co., Ltd., product name: NIADEKA ED-506, epoxy equivalent: 300 Epoxy resin (871): manufactured by Yuka Shell Epoxy Co., Ltd., product name: Epicote #871, epoxy equivalent: 430 Methyltetrahydrophthalic anhydride, manufactured by Nippon Ink Chemical Co., Ltd.
Product name: Epiclon-570 Dodecenyl succinic anhydride: Manufactured by Sanyo Chemical Co., Ltd., Product name: DD
SA (represented by the following formula) Alkenyl phthalic anhydride: Manufactured by Toho Chemical Co., Ltd., product name: B-
30O3 (represented by the following formula) I? 5 (R4, R5: alkyl group having 13 to 17 carbon atoms) 2
．． 4. Tri-2-ethylhexylate of 6-tris(dimethylaminomethyl)phenol: Nippon Kayaku Co., Ltd., product name: Ni-61B Triphenylphosphine: K.I. Kasei Co., Ltd., product name: PP-360 Crystallinity Silica: Manufactured by Ryumorisha, product name: Crystallite A-
1 Silicone oil treated fine silica Nippon Aerosil Co., Ltd., product name: Aerosil R 02 3-Glycidoxypropyltrimethoxysilane: Chisso Co., Ltd., product name: S-510 Terminal hydroxyl group polybutadiene: Idemitsu Petrochemical Co., Ltd., product name: R-15HT, molecular weight: 1200 Next, the epoxy resin component [A] prepared in Example 1 and Example 2 and the curing agent component C
B) was blended in a theoretical equivalent amount and cured at 100° C. for 5 hours, and the cured product was evaluated for (1) thermal cycleability, (2) electrical properties at high temperatures, and (2) moisture resistance as follows.
その結果を表−３゜表−４に示す。The results are shown in Tables 3 and 4.
■冷熱サイクル性
ＪＩＳ Ｃ−２１０５に準じ、５個の試験片を作成して
、試験片にクラックの入るサイクルを測定し、２段階評
価法にて評価した。(cold/heat cycle property) Five test pieces were prepared according to JIS C-2105, and the cycles at which cracks appeared in the test pieces were measured and evaluated using a two-step evaluation method.
実施例１の評価
Ｏ：硬化物にクラックが入るサイクル数が１０以上のも
の。Evaluation of Example 1: O: The number of cycles at which cracks appeared in the cured product was 10 or more.
Ｘ：硬化物にクラックが入るサイクル数が１０未満のも
の。X: The number of cycles at which cracks appear in the cured product is less than 10.
実施例２の評価
Ｏ：硬化物にクラックが入るサイクル数が５０以上のも
の。Evaluation of Example 2: O: The number of cycles at which cracks appeared in the cured product was 50 or more.
×：硬化物にクラックが入るサイクル数が５０未満のも
の。×: The number of cycles in which cracks appeared in the cured product was less than 50.
■高温時の電気特性
実施例１の評価
ＪＩＳ Ｋ６９１１に準じ、１２０℃における硬化物の
体積固有抵抗を測定し、２段階評価法にて評価した。■Evaluation of Electrical Properties at High Temperature Example 1 According to JIS K6911, the volume resistivity of the cured product at 120°C was measured and evaluated using a two-step evaluation method.
Ｏ：体積固有抵抗が１０１３Ω・０ｍ以上のもの。O: Volume resistivity is 1013Ω・0m or more.
×：体積固有抵抗が１０１３Ω・ｃｍ未滴のもの、実施
例２の評価
ＪＩＳ Ｋ６９１１に準じ、１００℃における硬化物の
体積固有抵抗を測定し、２段階評価法にて評価した。×: Volume resistivity was 1013 Ω·cm. Evaluation of Example 2. The volume resistivity of the cured product at 100° C. was measured according to JIS K6911, and evaluated using a two-step evaluation method.
０：体積固有抵抗が１０１２Ω・Ｃｌ１１以上のもの。0: Volume resistivity is 1012Ω・Cl11 or more.
×：体積固有抵抗が１０１２Ω・ｃｍ未溝のもの。×: Ungrooved product with volume resistivity of 1012 Ω·cm.
■耐湿性
ＪＩＳ Ｋ６９１１に準じ、硬化物を作成し、１２０℃
、２気圧、湿度９５％で１００時間加湿した後、２５°
Ｃ硬化物の体積固有抵抗を測定し、２段階評価法にて評
価した。なお実施例１，２とも同様の評価基準で評価し
た。■Moisture resistance Create a cured product according to JIS K6911 and heat it at 120°C.
, after 100 hours of humidification at 2 atm and 95% humidity, 25°
The volume resistivity of the C cured product was measured and evaluated using a two-step evaluation method. Note that both Examples 1 and 2 were evaluated using the same evaluation criteria.
Ｏ：体積固有抵抗が１０１５Ω・ａｍ以上のもの。O: Volume resistivity is 1015 Ω・am or more.
Ｘ：体積固有抵抗が１０１５Ω・ｃｍ未滴のもの。X: Volume resistivity is 1015 Ω·cm without any drops.
表−３ ９比較例を示す。Table-3 9 Comparative Examples are shown below.
表−４ ９比較例を示す。Table-4 9 Comparative Examples are shown below.
Claims (2)
ルキル基である） で示されるビスフェノールＡ型エポキシ樹脂と、アルケ
ニル基含有無水コハク酸からなる液状エポキシ樹脂組成
物。(1) Epoxy resin and bisphenol A type epoxy resin represented by the general formula ▲Mathematical formula, chemical formula, table, etc.▼ (In the formula, R^1 is a hydrogen atom or an alkyl group, and R^2 is an alkyl group.) and a liquid epoxy resin composition comprising alkenyl group-containing succinic anhydride.
ール化合物を含有する請求項１の組成物。(2) The composition according to claim 1, wherein the alkenyl group-containing succinic anhydride contains a rubbery polyol compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2355490A JPH03227317A (en) | 1990-01-31 | 1990-01-31 | Liquid epoxy resin composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2355490A JPH03227317A (en) | 1990-01-31 | 1990-01-31 | Liquid epoxy resin composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03227317A true JPH03227317A (en) | 1991-10-08 |
Family
ID=12113719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2355490A Pending JPH03227317A (en) | 1990-01-31 | 1990-01-31 | Liquid epoxy resin composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03227317A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015131915A (en) * | 2014-01-14 | 2015-07-23 | ソマール株式会社 | Two-liquid type epoxy resin composition and method of producing case mold type capacitor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS565472A (en) * | 1979-06-15 | 1981-01-20 | Ciba Geigy Ag | Diglycidylether* its manufacture and hardening composition containing same |
| JPS5670023A (en) * | 1979-11-12 | 1981-06-11 | Daicel Chem Ind Ltd | Curing agent for heat stable epoxy resin |
| JPS6248721A (en) * | 1985-08-28 | 1987-03-03 | Somar Corp | Epoxy resin composition |
-
1990
- 1990-01-31 JP JP2355490A patent/JPH03227317A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS565472A (en) * | 1979-06-15 | 1981-01-20 | Ciba Geigy Ag | Diglycidylether* its manufacture and hardening composition containing same |
| JPS5670023A (en) * | 1979-11-12 | 1981-06-11 | Daicel Chem Ind Ltd | Curing agent for heat stable epoxy resin |
| JPS6248721A (en) * | 1985-08-28 | 1987-03-03 | Somar Corp | Epoxy resin composition |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015131915A (en) * | 2014-01-14 | 2015-07-23 | ソマール株式会社 | Two-liquid type epoxy resin composition and method of producing case mold type capacitor |
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