JPS58103525A - Epoxy resin composition - Google Patents

Epoxy resin composition

Info

Publication number
JPS58103525A
JPS58103525A JP20264481A JP20264481A JPS58103525A JP S58103525 A JPS58103525 A JP S58103525A JP 20264481 A JP20264481 A JP 20264481A JP 20264481 A JP20264481 A JP 20264481A JP S58103525 A JPS58103525 A JP S58103525A
Authority
JP
Japan
Prior art keywords
curing agent
curing
catalyst
epoxy resin
compound
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
Application number
JP20264481A
Other languages
Japanese (ja)
Inventor
Masahiro Matsumura
松村 昌弘
Tetsuo Kunitomi
国富 哲夫
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Panasonic Electric Works Co Ltd
Original Assignee
Matsushita Electric Works Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Matsushita Electric Works Ltd filed Critical Matsushita Electric Works Ltd
Priority to JP20264481A priority Critical patent/JPS58103525A/en
Publication of JPS58103525A publication Critical patent/JPS58103525A/en
Pending legal-status Critical Current

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

Abstract

PURPOSE:A composition having long-term storage stability, a high curing rate and a short molding cycle, prepared by mixing an epoxy resin with a curing agent comprising a combination of a phenol novolak resin and a specified curing agent compound and a specified curing catalyst. CONSTITUTION:An epoxy resin composition prepared by mixing (A) an epoxy resin with (B) a curing agent comprising a combination of a phenol novolak resin and a curing agent compound of the formula (wherein n is 0 or a positive integer), e.g., a compound of the formula (wherein n=2-20) and (C) a curing catalyst comprising a 2-methylimidazole/pyromellitic anhydride complex. The use of catalyst C provides long-term storage stability. Besides, the co-use of the above compound as a curing agent provides an accelerated curing rate, so that shortening of a molding cycle can be made and molding with good production efficiencies becomes possible in spite of the use of catalyst C.

Description

【発明の詳細な説明】 本発明はXボ中シ樹脂組成物に関し、x4中シ樹脂に硬
化剤としてフェノールノll5v:)り樹脂及び一般式
が で示される化合物を併用して配合すると共に硬化触媒と
して2−メチルイ三タリールー無水ピ0メリット酸錯体
を配合することを特徴とするエボ中シ樹脂組成物に係る
ものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an X4 medium resin composition, which is prepared by blending a phenol resin as a curing agent and a compound represented by the general formula into an X4 medium resin, and curing the composition. This invention relates to an Evo medium resin composition which is characterized in that it contains a 2-methylitalylphimellitic anhydride complex as a catalyst.

フェノールボラ・シフ樹脂を硬化剤として用いたエボ中
シ樹脂組成物の一般的な配合は、例えばIボ中シ樹脂2
0重量−程度、フェノールノボ5ウク樹脂lO重量%程
度、硬化触mとしてベシジルジメチルア三シ等の三級ア
!シや2−メチルイ!タリール、2−エチルイ!:タリ
ール、2−フェニルイ:タリール等のイ!タリール類を
0.2〜1.0重量−程度、無機充填材としてシリカ6
5重量−程度、−燃剤としてgb、0.4重量饅程度、
離型剤としてカルナバワックス1重量慢程度である。こ
の配合によれば硬化速度が速く成形サイクルの短いXボ
十シ樹脂組成物を得ることができるが、この反面保存性
が悪く5℃以下の冷蔵状態で保存する必要があシ、5℃
以下で保存しても2力月程度のライフしかないという欠
点があった。そこで上記配合のうち、硬化触媒である三
級アエシやイミダリール類の替シに2−メチルイミタリ
ールー無水ピ0メリラト鍍錯塩を1〜5重量%用いるこ
とKよfi、20Cで6力月以上という長期の保存性を
有するエボ中シ樹脂組成物を得ることができることが見
出されたが、このものでは逆に多tの硬化触媒を用いて
も硬化速度か遅く、成形加工サイクルが長くなるという
欠点があった。
A general formulation of an Evo medium resin composition using Phenol Bora Schiff resin as a curing agent is, for example, I Bo medium resin 2.
0% by weight, about 10% by weight of phenolic resin, and tertiary acetic acid such as besidyl dimethyl acetate as a curing catalyst. Shiya 2-Methyrui! TARIL, 2-ETHILI! : Tarir, 2-phenyl: Tarir etc.! About 0.2 to 1.0 weight of taryl and silica 6 as an inorganic filler.
5 weight - degree, - GB as fuel, 0.4 weight cake degree,
As a mold release agent, about 1 weight of carnauba wax is used. According to this formulation, it is possible to obtain an X-Boss resin composition with a fast curing speed and a short molding cycle, but on the other hand, it has poor storage stability and must be stored in a refrigerated state below 5°C.
There was a drawback that even if you saved it below, you would only have about 2 months of life. Therefore, in the above formulation, it is recommended to use 1 to 5% by weight of 2-methylimitary-anhydride-melilato complex salt as a replacement for the curing catalysts such as tertiary acetic acid and imidalyl. It has been found that it is possible to obtain an evo-medium resin composition with long-term storage stability.However, in this composition, even if a high-t curing catalyst is used, the curing speed is slow and the molding cycle becomes long. There was a drawback.

本発明は上記の点に鑑みてなされ次ものであって、長期
保存性含有すると共に硬化速度が速く成形サイクルが短
いX$十シ樹脂組成物を提供するコトを目的とするもの
である。
The present invention was made in view of the above-mentioned points, and an object of the present invention is to provide a resin composition having a long shelf life, a fast curing speed, and a short molding cycle.

以下本発明の詳細な説明する。The present invention will be explained in detail below.

本発明に係る工率中シ樹脂組成物は、エボ士シ樹脂に、
硬化剤としてフェノールノボラック樹脂と一般式が で示される化合物(以下硬化剤化合物と称す)とを併用
して配合すると共に、硬化触媒として2−メチルイニタ
リールー無水ピ0メリもシト酸錯体を配合し、さらに必
要に応じて常用される無機充填材、離燃剤、離型剤等を
配合して調製したものである。
The medium-efficiency resin composition according to the present invention includes:
A phenol novolak resin and a compound represented by the general formula (hereinafter referred to as a curing agent compound) are combined as a curing agent, and a 2-methylinital-anhydride-meritic acid complex is blended as a curing catalyst. In addition, it is prepared by adding commonly used inorganic fillers, flame retardants, mold release agents, etc. as necessary.

ここで、工車十シ衝脂七しては任意のものを使用するこ
とか可能であるが、特に0−クレリールノIA5ラクエ
ボ+シ樹脂やフェノールノボ5ツク工卓中シ稠MWI等
の多官能工車十シw脂が好ましい。この多官能工卓中シ
樹脂としては、エボ+シ基が特に好ましい・ 硬化剤としては上記のようにフェノールノボ5で示され
る硬化剤化合物を用いることにより、フェノールノボラ
ック樹脂と該硬化剤化合物とを併用するものであり、該
硬化剤化合物の使用量はフェノールノボ5ツク樹脂の使
用可能量の範囲内においては特に限定されるものでない
。該硬化剤化合物の増量は硬化速度の向上に関係するの
で、好ましい硬化速度を達成するのに必要な量だけ使用
すればよいのである。ま次上記硬化剤化合物におけるn
の数は限定されるもので蝶ないが、通常n〜0.8の条
件下反応させることにより得られるものである。従って
該硬化剤化合物としてはレリルシシ一本ル乙アルデヒド
樹脂、カテコール−ホルムアルデヒド樹脂、ハイド0中
ノシーホルムアルヂしド樹脂が主として用いられること
になるが、このうちレリルシシーホルムアルデヒド樹脂
が用いて好適である。尚、しリルシシ、カテコール、て
いる化合物であれば使用可能である。
Here, it is possible to use any desired resin, but in particular, multifunctional resins such as 0-Clearyl resin and phenol resin MWI can be used. Koguruma Jushi w fat is preferred. As this polyfunctional resin, Evo+C group is particularly preferable. By using the curing agent compound represented by Phenol Novo 5 as the curing agent, the phenol novolac resin and the curing agent compound can be combined. The amount of the curing agent compound to be used is not particularly limited within the usable amount of the phenolic resin. Increasing the amount of the curing agent compound is related to increasing the cure rate, so only the amount necessary to achieve the desired cure rate may be used. n in the above curing agent compound
Although the number of n is limited, it is usually obtained by reacting under conditions of n to 0.8. Therefore, as the curing agent compound, Relyl-formaldehyde resin, catechol-formaldehyde resin, and Hyde-0 medium formaldehyde resin are mainly used, but among these, Relyl-formaldehyde resin is preferably used. be. Incidentally, any compound such as trichloride, catechol, etc. can be used.

硬化触媒である2−メチルイ!:タリールー無水ピ0メ
リット酸錯体は、例えば2−メチルイミタリールと無水
ピロメリット駿とをそれぞれナト5ヒト0フ5シ溶液と
し、2−メチルイ!タリール/無水ピ0メリウト酸=2
.00℃ル比率となるように両溶液を撹拌−混合するこ
とにょシ、生じる沈殿をP別・乾燥して粉体として得ら
れる。これと同等なものとして商品名スリ中ニア−MP
M(丸善石油株式会社製)として市販されているものを
用いることができる。この2−メチルイエタリールー無
水ピOメリウト酸錯体の使用量は特に限定されるもので
ないが、通常Iボ中シ樹脂組成物全量に対して0.5〜
5.0重量が好適である。
2-Methyl, a curing catalyst! :Tary-pyromellitic anhydride complex can be prepared, for example, by preparing a solution of 2-methylimitaryl and pyromellitic anhydride, respectively. Taryl/pimeliutic anhydride = 2
.. Both solutions are stirred and mixed at a ratio of 00°C, and the resulting precipitate is separated from P and dried to obtain a powder. The equivalent product name is Surichunia-MP.
M (manufactured by Maruzen Sekiyu Co., Ltd.) commercially available can be used. The amount of the 2-methylyetary-piomelutic anhydride complex to be used is not particularly limited, but is usually 0.5 to 0.5 to
5.0 weight is preferred.

上述のように得られたIボ中シ樹脂組成物は、2−メチ
ルイエタリールー・ピロメリット酸錯体によって長期に
亘る保存性を有するものであり、しかも硬化剤としてフ
ェノールノボ55り樹脂と併用する硬化剤化合物によっ
て硬化速度が促進され2−メチルイ!!タリールーピO
メリウト酸錯体を用いたくもかかわらず成形サイクルを
短縮して生産効率よく成形加工が行なえるものである。
The I-bodied resin composition obtained as described above has long-term storage stability due to the 2-methylyetary-pyromellitic acid complex, and it can also be used in combination with phenol novo-55 resin as a curing agent. The curing rate is accelerated by the curing agent compound that 2-methyl! ! Tully Lupi O
Even though a meliut acid complex is used, the molding cycle can be shortened and molding processing can be carried out with high production efficiency.

次に本關を実施例により具体的に説明する。Next, the main subject will be specifically explained using examples.

第1表に示す配合によって原料を計量して容器中で十分
撹拌混合し、これを温度85 C1回転数15 wpm
の前0−ルと温度120℃、回転数12vpmの後ロー
ルとで構成される試験用0−ル機にて6分間溶融混練し
、こののちシート状材料を得た。このものを三方式万能
粉砕機にて粉砕することにより、実施例1−5、比較例
1〜2、従来例第1表(重量部) 上記のようにして得られ次実施例1〜5、比較例1〜2
、従来例のエポ士シ樹脂組成物について、30℃の条件
下における保存性及び硬化速度の測定試験を行なっ几。
The raw materials were weighed according to the formulation shown in Table 1, stirred and mixed thoroughly in a container, and mixed at a temperature of 85 C1 and a rotation speed of 15 wpm.
The mixture was melt-kneaded for 6 minutes in a testing machine consisting of a front roll and a rear roll at a temperature of 120° C. and a rotational speed of 12 vpm, after which a sheet material was obtained. By pulverizing this material with a three-way universal pulverizer, Examples 1-5, Comparative Examples 1-2, Conventional Examples Table 1 (parts by weight) were obtained as described above, and the following Examples 1-5, Comparative examples 1-2
A conventional epoxy resin composition was tested for storage stability and curing speed at 30°C.

その結果を第2表に示す。The results are shown in Table 2.

第  2  表 30℃保存性は、材料5yを直圧プレスで175℃に於
て成形した月板延びの初期値に対する90−保持率に達
するまでの1数で示し、また硬化速度は、°トランスフ
ァー成形にて17S℃の条件で成形する際の注入開始か
ら成形品を取り出し得るまでの最少時間で示した。第2
表の結果より、実施例のものは、良好な保存性を有する
と共に2従米通りの速い硬化速度を有して速い成形サイ
クルで成形を行ないえることが確隠され九〇
Table 2 The storage stability at 30°C is expressed as the number of times it takes to reach a 90-retention rate with respect to the initial value of the elongation of the moon plate formed by molding material 5y at 175°C with a direct pressure press, and the curing speed is expressed by the degree of retention at 175°C. It is shown as the minimum time from the start of injection until the molded product can be taken out when molding is performed at 17S°C. Second
From the results in the table, it is confirmed that the products of Examples have good storage stability, a fast curing speed comparable to that of the conventional US, and can be molded in a fast molding cycle.90

Claims (1)

【特許請求の範囲】[Claims] +11  エボ中シ樹脂に硬化剤としてフェノールノで
示される化合物を併用して配合すると共に硬化触媒とし
て2−メチルイエタリールー無水ピ0メリット酸錯体を
配合することを特徴とするll1lc中シam組成物。
+11 A ll1lc medium composition characterized by blending a compound represented by phenol as a curing agent with an evo medium resin and a 2-methylyetary-piomellitic anhydride complex as a curing catalyst. thing.
JP20264481A 1981-12-15 1981-12-15 Epoxy resin composition Pending JPS58103525A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP20264481A JPS58103525A (en) 1981-12-15 1981-12-15 Epoxy resin composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP20264481A JPS58103525A (en) 1981-12-15 1981-12-15 Epoxy resin composition

Publications (1)

Publication Number Publication Date
JPS58103525A true JPS58103525A (en) 1983-06-20

Family

ID=16460751

Family Applications (1)

Application Number Title Priority Date Filing Date
JP20264481A Pending JPS58103525A (en) 1981-12-15 1981-12-15 Epoxy resin composition

Country Status (1)

Country Link
JP (1) JPS58103525A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6084037A (en) * 1996-12-19 2000-07-04 Shin -Etsu Chemical Co., Ltd. Epoxy resin composition and semiconductor device
US6376923B1 (en) * 1999-06-08 2002-04-23 Shin-Etsu Chemical Co., Ltd. Flip-chip type semiconductor device sealing material and flip-chip type semiconductor device
WO2003075339A1 (en) * 2002-03-01 2003-09-12 National Starch And Chemical Investment Holding Corporation B-stageable underfill encapsulant and method for its application
US7037399B2 (en) 2002-03-01 2006-05-02 National Starch And Chemical Investment Holding Corporation Underfill encapsulant for wafer packaging and method for its application

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6084037A (en) * 1996-12-19 2000-07-04 Shin -Etsu Chemical Co., Ltd. Epoxy resin composition and semiconductor device
US6376923B1 (en) * 1999-06-08 2002-04-23 Shin-Etsu Chemical Co., Ltd. Flip-chip type semiconductor device sealing material and flip-chip type semiconductor device
WO2003075339A1 (en) * 2002-03-01 2003-09-12 National Starch And Chemical Investment Holding Corporation B-stageable underfill encapsulant and method for its application
US7037399B2 (en) 2002-03-01 2006-05-02 National Starch And Chemical Investment Holding Corporation Underfill encapsulant for wafer packaging and method for its application
US7608487B2 (en) 2002-03-01 2009-10-27 Henkel Ag & Co. Kgaa B-stageable underfill encapsulant and method for its application

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