JP2007314753A - 繊維強化複合材料用エポキシ樹脂組成物 - Google Patents
繊維強化複合材料用エポキシ樹脂組成物 Download PDFInfo
- Publication number
- JP2007314753A JP2007314753A JP2006264577A JP2006264577A JP2007314753A JP 2007314753 A JP2007314753 A JP 2007314753A JP 2006264577 A JP2006264577 A JP 2006264577A JP 2006264577 A JP2006264577 A JP 2006264577A JP 2007314753 A JP2007314753 A JP 2007314753A
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- JP
- Japan
- Prior art keywords
- epoxy resin
- resin
- fiber
- resin composition
- reinforced composite
- 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.)
- Granted
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Abstract
【解決手段】エポキシ樹脂(A)、熱可塑性樹脂(B)、固形樹脂微粒子(C)及び硬化剤(D)を含むエポキシ樹脂組成物であって、該エポキシ樹脂組成物の硬化後の形態が、前記エポキシ樹脂(A)及び熱可塑性樹脂(B)が共連続相を形成し、該共連続相における少なくとも前記エポキシ樹脂(A)の連続相中に前記固形樹脂微粒子(C)が分散することを特徴とする。
【選択図】 なし
Description
エポキシ樹脂(A)、熱可塑性樹脂(B)、固形樹脂微粒子(C)及び硬化剤(D)を下記に列記されたものの中から、それぞれ表1の実施例1〜5、比較例1〜2に記載する配合割合において、エポキシ樹脂組成物を調製し、その特性を評価した。先ずエポキシ樹脂(A)及び熱可塑性樹脂(B)の全量を、温度125℃に設定したプラネタリミキサを用いて、均一な溶液になるまで75分間、撹拌・混合した。その後、このプラネタリミキサの温度を70℃に設定し、樹脂温度が均一になったところで、固形樹脂微粒子(C)及び硬化剤(D)の全量をこの溶液中に加え、撹拌・混合してエポキシ樹脂組成物を調製した。
樹脂A−1:N,N,O−トリグリシジル−p−アミノフェノール樹脂(ハンツマン・アドバンスト・マテリアルズ社製MY−0510)、常温で液状、温度25℃の粘度が7ポイズ。
樹脂A−2:トリグリシジル化アルキルアミノフェノール樹脂(住友化学社製ELM−100)、常温で液状、温度25℃の粘度が10ポイズ。
樹脂A−3:ビスフェノールF型エポキシ樹脂(東都化成社製YDF−170)、常温で液状、温度25℃の粘度が35ポイズ。
樹脂B−1:ポリエーテルスルホン樹脂(住友化学社製スミカエクセルPES5003P)衝撃粉砕により、粒子径100μm以下の微細粒子
粒子C−1:ビスフェノールA型エポキシ樹脂(東都化成社製YD−019)、衝撃粉砕により粒子径100μm以下の微細粒子。
粒子C−2:ビスフェノールA型エポキシ樹脂(東都化成社製YD−020N)、衝撃粉砕により粒子径100μm以下の微細粒子。
粒子C−3:フェノキシ型ビスフェノールエポキシ樹脂(東都化成社製YP−70)、衝撃粉砕により粒子径100μm以下の微細粒子。
硬化剤D−1:3,3′−ジアミノジフェニルスルホン(ハンツマン・アドバンスト・マテリアルズ社製ARADUR9719−1)
硬化剤D−2:ジシアンジアミド(ジャパンエポキシレジン社製エピキュアDICY 15)、潜在性硬化剤
得られたエポキシ樹脂組成物を試料にして、温度25℃から200℃までの間で、昇温速度2℃/分、周波数10rad/秒、ひずみ1%の条件の動的粘弾性測定における複素粘性率の最低値を測定した。
得られたエポキシ樹脂組成物を用いて離型紙上に樹脂フィルムを形成し、このフィルムを炭素繊維平織織物(東レ社製T−300−3K)に、樹脂含有量が41重量%となるように加熱加圧して転写しプリプレグを得た。
プリプレグのタック性評価
○: 十分な粘着性が感じられたもの
△: やや粘着性が感じられたもの
×: ほぼ粘着性が感じられなかったもの
プリプレグのドレープ性評価
○: 十分な柔軟性が感じられたもの
△: やや柔軟性が感じられたもの
×: ほぼ柔軟性が感じられなかったもの
得られたエポキシ樹脂組成物を使用して、プログラムオーブンにて温度180℃で、2時間硬化し、樹脂硬化物を作製した。
上記で得られた樹脂硬化物を、ASTM D5045−91に準拠して、試験サンプルを作製し、23℃(乾燥状態)における破壊靭性値(MPa・√m)を測定した。
得られたエポキシ樹脂組成物からなるプリプレグを2枚積層し、これをハニカムコア(昭和飛行機工業社製ノーメックスハニカムSAH−1/8−8.0)の両面に配置した後、バッグに入れ、これをオ−トクレ−ブ内で温度180℃、2時間(昇温速度2.8℃/分)加熱し、硬化させてハニカムパネルを作製した。この間、オ−トクレ−ブ内を圧空で0.32MPaに加圧した。
Claims (22)
- エポキシ樹脂(A)、熱可塑性樹脂(B)、固形樹脂微粒子(C)及び硬化剤(D)を含むエポキシ樹脂組成物であって、該エポキシ樹脂組成物の硬化後の形態が、前記エポキシ樹脂(A)及び熱可塑性樹脂(B)が共連続相を形成し、該共連続相における少なくとも前記エポキシ樹脂(A)の連続相中に前記固形樹脂微粒子(C)が分散する繊維強化複合材料用エポキシ樹脂組成物。
- 前記熱可塑性樹脂(B)が、分子末端に反応性官能基を有する請求項1に記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記熱可塑性樹脂(B)が、ポリエーテルスルホン樹脂の粒子及び/又はポリエーテルイミド樹脂の粒子であり、その粒子径が200μm以下である請求項1又は2に記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記固形樹脂微粒子(C)が、常温で固形のエポキシ樹脂、マレイミド樹脂、又はシアネート樹脂からなる請求項1、2又は3に記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記固形樹脂微粒子(C)が、熱可塑性樹脂からなる請求項1、2又は3に記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記固形樹脂微粒子(C)を構成する樹脂の分子量が10,000〜100,000である請求項1〜5のいずれかに記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記固形樹脂微粒子(C)が、分子量10,000〜35,000のエポキシ樹脂からなる請求項1〜4のいずれかに記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記固形樹脂微粒子(C)が、エポキシ当量1000〜8000g/eqのビスフェノールA型エポキシ樹脂からなる請求項1、2、3、4、6又は7に記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記固形樹脂微粒子(C)が、分子末端にエポキシ基を有するフェノキシ骨格型樹脂からなる請求項1、2、3、4、6、7又は8に記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記フェノキシ骨格型樹脂の分子量が、50,000〜60,000である請求項9に記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記フェノキシ骨格型樹脂のエポキシ当量が、8,000〜20,000g/eqである請求項9又は10に記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記固形樹脂微粒子(C)の粒子径が、前記エポキシ樹脂組成物の硬化後の形態において、0.1〜2μmである請求項1〜11のいずれかに記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記硬化剤(D)が、ジアミノジフェニルスルホン及び/又は潜在性硬化剤からなる請求項1〜12のいずれかに記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記エポキシ樹脂組成物の硬化後に、ASTM D5045−91に準拠して測定される破壊靭性値が、1.8MPa・√m以上である請求項1〜13のいずれかに記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記エポキシ樹脂組成物が、前記エポキシ樹脂(A)100重量部に対し、前記熱可塑性樹脂(B)を20〜60重量部、前記熱硬化性樹脂の粒子(C)を2〜20重量部配合する請求項1〜14のいずれかに記載の繊維強化複合材料用エポキシ樹脂組成物。
- 前記エポキシ樹脂組成物の昇温速度2℃/分における動的粘弾性測定による最低粘度が10〜150Pa・sである請求項1〜15のいずれかに記載の繊維強化複合材料用エポキシ樹脂組成物。
- 請求項1〜16のいずれかに記載のエポキシ樹脂組成物をマトリックス樹脂として、強化繊維と複合させた繊維強化プリプレグ。
- 前記固形樹脂微粒子(C)の粒子径が、100μm以下である請求項17に記載の繊維強化プリプレグ。
- 前記マトリックス樹脂の含有量が30〜50重量%である請求項17又は18に記載の繊維強化プリプレグ。
- 前記強化繊維が炭素繊維である請求項17、18又は19に記載の繊維強化プリプレグ。
- 請求項17〜20のいずれかに記載の繊維強化プリプレグとハニカムコアとを積層したハニカムサンドイッチパネル。
- 前記ハニカムコアが、アラミドハニカム、アルミハニカム、ペーパーハニカム、ガラスハニカムから選ばれるいずれかである請求項21に記載のハニカムサンドイッチパネル。
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AU2007244332A AU2007244332B2 (en) | 2006-04-25 | 2007-04-24 | Epoxy resin composition for fiber-reinforced composite material |
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JP4475880B2 (ja) * | 2003-03-13 | 2010-06-09 | 東邦テナックス株式会社 | エポキシ樹脂組成物 |
JP2004346092A (ja) | 2003-04-28 | 2004-12-09 | Yokohama Rubber Co Ltd:The | プリプレグ用樹脂組成物 |
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-
2006
- 2006-09-28 JP JP2006264577A patent/JP4141487B2/ja active Active
-
2007
- 2007-04-24 CA CA2650559A patent/CA2650559C/en not_active Expired - Fee Related
- 2007-04-24 KR KR1020087028770A patent/KR101393763B1/ko active IP Right Grant
- 2007-04-24 AU AU2007244332A patent/AU2007244332B2/en active Active
- 2007-04-24 CN CN2007800149029A patent/CN101432359B/zh active Active
- 2007-04-24 US US12/298,040 patent/US8137786B2/en active Active
- 2007-04-24 TW TW96114353A patent/TWI457394B/zh active
- 2007-04-24 ES ES07742311.9T patent/ES2517565T3/es active Active
- 2007-04-24 BR BRPI0709483-3A patent/BRPI0709483A2/pt not_active IP Right Cessation
- 2007-04-24 WO PCT/JP2007/058876 patent/WO2007125926A1/ja active Application Filing
- 2007-04-24 EP EP20070742311 patent/EP2014721B1/en not_active Not-in-force
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JP2008144110A (ja) * | 2006-12-13 | 2008-06-26 | Yokohama Rubber Co Ltd:The | 繊維強化複合材料用エポキシ樹脂組成物 |
WO2008133054A1 (ja) * | 2007-04-13 | 2008-11-06 | Toho Tenax Co., Ltd. | 樹脂組成物、及びプリプレグ |
US8211537B2 (en) | 2007-04-13 | 2012-07-03 | Toho Tenax Co., Ltd. | Resin composition, and prepreg |
WO2009107697A1 (ja) | 2008-02-26 | 2009-09-03 | 東レ株式会社 | エポキシ樹脂組成物、プリプレグおよび繊維強化複合材料 |
US8309631B2 (en) | 2008-02-26 | 2012-11-13 | Toray Industries, Inc. | Epoxy resin composition, prepreg, and fiber reinforced composite material |
WO2010035859A1 (ja) | 2008-09-29 | 2010-04-01 | 東レ株式会社 | エポキシ樹脂組成物、プリプレグおよび繊維強化複合材料 |
US9243139B2 (en) | 2008-09-29 | 2016-01-26 | Toray Industries, Inc. | Epoxy resin composition, prepreg and fiber-reinforced composite material |
EP2886586A1 (en) | 2008-09-29 | 2015-06-24 | Toray Industries, Inc. | Epoxy resin composition, prepreg, and fiber-reinforced composite material |
US8658736B2 (en) | 2008-09-29 | 2014-02-25 | Toray Industries, Inc. | Epoxy resin composition, prepreg and fiber-reinforced composite material |
JP5469086B2 (ja) * | 2008-11-13 | 2014-04-09 | 東邦テナックス株式会社 | 熱硬化性樹脂組成物とそれを用いたプリプレグ |
WO2010055811A1 (ja) * | 2008-11-13 | 2010-05-20 | 東邦テナックス株式会社 | 熱硬化性樹脂組成物とそれを用いたプリプレグ |
US8685537B2 (en) | 2009-03-16 | 2014-04-01 | Toray Industries, Inc. | Fiber reinforced resin composition, molding material, and method for producing fiber reinforced resin composition |
JP5505304B2 (ja) * | 2009-03-16 | 2014-05-28 | 東レ株式会社 | 繊維強化樹脂組成物、成形材料および繊維強化樹脂組成物の製造方法 |
WO2010107022A1 (ja) * | 2009-03-16 | 2010-09-23 | 東レ株式会社 | 繊維強化樹脂組成物、成形材料および繊維強化樹脂組成物の製造方法 |
JP2013503249A (ja) * | 2009-08-31 | 2013-01-31 | サイテク・テクノロジー・コーポレーシヨン | 高性能接着剤組成物 |
JP2016148050A (ja) * | 2010-06-14 | 2016-08-18 | ヘクセル コンポジッツ、リミテッド | 複合材料の改善 |
WO2016067736A1 (ja) * | 2014-10-29 | 2016-05-06 | 東レ株式会社 | エポキシ樹脂組成物、樹脂硬化物、プリプレグおよび繊維強化複合材料 |
JP6052426B2 (ja) * | 2014-10-29 | 2016-12-27 | 東レ株式会社 | エポキシ樹脂組成物、樹脂硬化物、プリプレグおよび繊維強化複合材料 |
JP2022501213A (ja) * | 2018-09-06 | 2022-01-06 | エコール・ポリテクニーク・フェデラル・ドゥ・ローザンヌ (ウ・ペ・エフ・エル)Ecole Polytechnique Federale De Lausanne (Epfl) | 複合材料 |
JP7448971B2 (ja) | 2018-09-06 | 2024-03-13 | エコール・ポリテクニーク・フェデラル・ドゥ・ローザンヌ (ウ・ペ・エフ・エル) | 複合材料 |
Also Published As
Publication number | Publication date |
---|---|
ES2517565T3 (es) | 2014-11-03 |
TW200804502A (en) | 2008-01-16 |
AU2007244332A1 (en) | 2007-11-08 |
BRPI0709483A2 (pt) | 2011-07-19 |
CA2650559A1 (en) | 2007-11-08 |
US20090098335A1 (en) | 2009-04-16 |
KR101393763B1 (ko) | 2014-05-12 |
US8137786B2 (en) | 2012-03-20 |
AU2007244332B2 (en) | 2010-08-05 |
JP4141487B2 (ja) | 2008-08-27 |
TWI457394B (zh) | 2014-10-21 |
CN101432359B (zh) | 2011-09-07 |
EP2014721A4 (en) | 2012-07-11 |
EP2014721B1 (en) | 2014-10-08 |
EP2014721A1 (en) | 2009-01-14 |
WO2007125926A1 (ja) | 2007-11-08 |
CN101432359A (zh) | 2009-05-13 |
CA2650559C (en) | 2015-04-14 |
KR20090015082A (ko) | 2009-02-11 |
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