JP6512379B1 - 繊維集束剤、繊維材料、成形材料及び成形品 - Google Patents
繊維集束剤、繊維材料、成形材料及び成形品 Download PDFInfo
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- JP6512379B1 JP6512379B1 JP2018552895A JP2018552895A JP6512379B1 JP 6512379 B1 JP6512379 B1 JP 6512379B1 JP 2018552895 A JP2018552895 A JP 2018552895A JP 2018552895 A JP2018552895 A JP 2018552895A JP 6512379 B1 JP6512379 B1 JP 6512379B1
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- Prior art keywords
- fiber
- sizing agent
- resin
- mass
- vinyl ester
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- 239000012736 aqueous medium Substances 0.000 claims abstract description 12
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 7
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Reinforced Plastic Materials (AREA)
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Abstract
Description
測定装置:高速GPC装置(東ソー株式会社製「HLC−8220GPC」)
カラム:東ソー株式会社製の下記のカラムを直列に接続して使用した。
「TSKgel G5000」(7.8mmI.D.×30cm)×1本
「TSKgel G4000」(7.8mmI.D.×30cm)×1本
「TSKgel G3000」(7.8mmI.D.×30cm)×1本
「TSKgel G2000」(7.8mmI.D.×30cm)×1本
検出器:RI(示差屈折計)
カラム温度:40℃
溶離液:テトラヒドロフラン(THF)
流速:1.0mL/分
注入量:100μL(試料濃度4mg/mLのテトラヒドロフラン溶液)
標準試料:下記の単分散ポリスチレンを用いて検量線を作成した。
東ソー株式会社製「TSKgel 標準ポリスチレン A−500」
東ソー株式会社製「TSKgel 標準ポリスチレン A−1000」
東ソー株式会社製「TSKgel 標準ポリスチレン A−2500」
東ソー株式会社製「TSKgel 標準ポリスチレン A−5000」
東ソー株式会社製「TSKgel 標準ポリスチレン F−1」
東ソー株式会社製「TSKgel 標準ポリスチレン F−2」
東ソー株式会社製「TSKgel 標準ポリスチレン F−4」
東ソー株式会社製「TSKgel 標準ポリスチレン F−10」
東ソー株式会社製「TSKgel 標準ポリスチレン F−20」
東ソー株式会社製「TSKgel 標準ポリスチレン F−40」
東ソー株式会社製「TSKgel 標準ポリスチレン F−80」
東ソー株式会社製「TSKgel 標準ポリスチレン F−128」
東ソー株式会社製「TSKgel 標準ポリスチレン F−288」
東ソー株式会社製「TSKgel 標準ポリスチレン F−550」
温度計、撹拌装置、還流冷却管、滴下装置を備えた4ツ口フラスコに、フェノ−ルノボラック型エポキシ樹脂(DIC株式会社製「エピクロンN−740-80M」、固形分エポキシ当量:180g/当量、有効成分80%)620質量部、アクリル酸205質量部、t−ブチルハイドロキノン1質量部、2−メチルイミダゾール10質量部を仕込み、40℃で十分に撹拌溶解した。その後、窒素と空気とを1対1で混合したガス流通下で、75〜80℃まで昇温した。更に、75〜80℃で10時間反応させると、酸価が1(mgKOH/g)以下になったので、反応を終了し、ビニルエステル樹脂(B−2)を得た。
温度計、撹拌装置、還流冷却管、滴下装置を備えた4ツ口フラスコに、ポリオキシエチレンモノエチルエーテル(日油株式会社製「ユニオックスM−550」、水酸基価:100)124質量部、及びビスフェノールA型エポキシ樹脂(DIC株式会社製「エピクロン1050」、エポキシ当量:477g/当量)99質量部、及びメチルエチルケトン65質量部を加え、40℃で十分に撹拌溶解した。次いで、40℃でトリレンジイソシアネート38質量部を添加し、60〜65℃で6時間反応させ赤外線吸収スペクトルによりNCOの2260cm-1の特性ピ−クの消失を確認した。その後、40℃まで冷却しアクリル酸15質量部、t−ブチルハイドロキノン1質量部、2−メチルイミダゾール3質量部を仕込み、窒素と空気とを1対1で混合したガス流通下で、75〜80℃まで昇温した。更に、75〜80℃で10時間反応させると、酸価が1(mgKOH/g)以下になったので、反応を終了し、ビニルエステル樹脂(A−1)を得た。ビニルエステル樹脂(A−1)の重量平均分子量は、13,000であった。
次いで、40℃まで冷却し、ポリオキシエチレンジスチレン化フェニルエーテル(花王株式会社製「エマルゲンA−500」)27質量部を加え十分に攪拌した。次いで、イオン交換水850質量部を30分かけて滴下し、更に15分間攪拌混合した。この水分散物を減圧蒸留により濃縮して、不揮発分30質量%のビニルエステル樹脂の水分散体である繊維集束剤(1)を得た。
ポリアクリロニトリル系炭素繊維(単糸径7μm、ストランド強度4,400MPa、弾性率235GPa、6000本)のノーサイズ糸を束ね、繊維集束剤(1)をイオン交換水で不揮発分5質量%に希釈したものを浸漬法で含浸し、ローラーで絞ることで有効成分の付着量を1質量%に調整し、次いで、150℃で30分間熱処理することによって、繊維集束剤(1)によって表面処理の施された炭素繊維束(1)を得た。
TM式摩擦抱合力試験機TM−200(大栄科学精機製作所製)を用い、ジグザグに配置した鏡面クロムメッキステンレス針3本を介して50gの張力で、炭素繊維束(1)を1000回擦過させ(往復運動速度300回/分)、炭素繊維束(1)の毛羽立ちの状態を下記の基準で目視判定した。
○:数本の毛羽は見られたものの、実用上問題ないレベルであった。
△:毛羽立ちが確認でき、糸切れも若干見られた。
×:毛羽立ち及び単糸の糸切れが非常に多く確認できた。
室温下、炭素繊維クロス(織物の重さ200g/m2、単糸径7μm、ストランド強度4,400MPa、弾性率235GPa、サイジング処理(表面処理)の施されたポリアクリロニトリル系炭素繊維クロス)を裁断して得た約300mm×300mmの大きさのクロスを、該クロスの質量部に対して約30倍の質量のアセトン中に浸漬し、12時間放置した。浸漬後、クロスを80℃の乾燥機を用いて2時間乾燥することで、炭素繊維の表面に付着した樹脂分等を除去し、サイジング処理(表面処理)のされていない状態の炭素繊維クロスを得た。
上記炭素繊維クロスに、繊維集束剤(1)をイオン交換水で不揮発分5質量%に希釈したものを、固形分の付着量が1質量%となるように含浸させ、乾燥機を用いて、150℃で30分間乾燥処理をして炭素繊維クロス(1)を得た。
ビニルエステル樹脂溶液(DICマテリアル株式会社製「エクスド−マ9102−01NP」)100質量部に、6質量%ナフテン酸コバルト0.5質量部及びメチルエチルケトンパーオキサイド(日本油脂株式会社製「パーメックN」)1.0質量部を混合した混合物を、離型処理の施された350mm×350mmのガラス板上に流し、上記で得た炭素繊維クロス(1)を載せ、ハンドレイアップ成形法(8プライ)によって積層し、常温(25℃)で12時間硬化させた後、更に60℃で3時間硬化させることによって、炭素繊維強化プラスチック(炭素繊維の含有率;50体積%)である成形品(1)を得た。
上記で得た成形品(1)について、幅15mm×長さ100mm×厚さ2mmの試験片を使用し、JIS K 7181に準拠して測定した。
上記で得た成形品(1)について、幅13mm×長さ77mm×厚さ2mmのダンベル試験片を使用しJIS K 7074に準拠して測定した。
上記で得た成形品(1)について、幅10mm×長さ15mm×厚さ2mmの試験片を使用しJIS K 7078に準拠して測定した。
温度計、撹拌装置、還流冷却管、滴下装置を備えた4ツ口フラスコに、ポリエチレングリコール(エチレンオキサイド付加モル数12)81質量部、ポリオキシエチレンモノエチルエーテル(日油株式会社製「ユニオックスM−550」、水酸基価:100)30質量部、メチルエチルケトン64質量部を加えて40℃で十分に撹拌溶解した。次いで、40℃でトリレンジイソシアネート47質量部を添加し、75℃で2時間反応させた。次いで、ビスフェノールA型エポキシ樹脂(DIC株式会社製「エピクロン1050」、エポキシ当量:477g/当量)97質量部、60〜65℃で6時間反応させ赤外線吸収スペクトルによりNCOの2260cm-1の特性ピ−クの消失を確認した。その後、40℃まで冷却しアクリル酸15質量部、t−ブチルハイドロキノン1質量部、2−メチルイミダゾール3質量部を仕込み、窒素と空気とを1対1で混合したガス流通下で、75〜80℃まで昇温した。更に、75〜80℃で10時間反応させると、酸価が1(mgKOH/g)以下になったので、反応を終了し、ビニルエステル樹脂(A−2)を得た。ビニルエステル樹脂(A−2)の重量平均分子量は、13,500であった。
次いで、40℃まで冷却し、ポリオキシエチレンジスチレン化フェニルエーテル(花王株式会社製「エマルゲンA−500」)27質量部を加え十分に攪拌した。次いで、イオン交換水850質量部を30分かけて滴下し、更に15分間攪拌混合した。この水分散物を減圧蒸留により濃縮して、不揮発分30質量%のビニルエステル樹脂の水分散体である繊維集束剤(2)を得た。
温度計、撹拌装置、還流冷却管、滴下装置を備えた4ツ口フラスコに、実施例1で得たビニルエステル樹脂(A−1)274質量部を加え40℃に調整した後、ビスフェノールA型エポキシアクリレ−ト樹脂(DIC株式会社製「ユニディックV−5500」、有効成分99%以上、以下、ビニルエステル樹脂(B−1)と略記する。)115質量部、及びポリオキシエチレンジスチレン化フェニルエーテル(花王株式会社製「エマルゲンA−500」)20質量部を加え十分に攪拌した。次いで、イオン交換水950質量部を30分かけて滴下し、更に15分間攪拌混合した。この水分散物を減圧蒸留により濃縮して、不揮発分30質量%のビニルエステル樹脂の水分散体である繊維集束剤(3)を得た。
温度計、撹拌装置、還流冷却管、滴下装置を備えた4ツ口フラスコに、実施例1で得たビニルエステル樹脂(A−1)300質量部を加え40℃に調整した後、合成例1で得たビニルエステル樹脂(B−2)150質量部、及びポリオキシエチレンジスチレン化フェニルエーテル(花王株式会社製「エマルゲンA−500」)21質量部を加え十分に攪拌した。次いで、イオン交換水1000質量部を30分かけて滴下し、更に15分間攪拌混合した。この水分散物を減圧蒸留により濃縮して、不揮発分30質量%のビニルエステル樹脂の水分散体である繊維集束剤(4)を得た。
温度計、撹拌装置、還流冷却管、滴下装置を備えた4ツ口フラスコに、グリセリンジメタクリレートヘキサメチレンジイソシアネート(共栄社化学製「UA101H」、末端不飽和基数:4個)149重量部、ノニオン系乳化剤(ポリオキシエチレン(70モル)スチレン化(5モル)クミルフェノール(質量比90:10))16.5質量部、及びメチルエチルケトン142質量部を加え50℃で均一に溶解した。その後、乳化槽に内容物を移し、ポリグリセリンポリグリシジルエーテル(ナガセケムテックス株式会社製「デナコール EX−521」、エポキシ当量:183g/当量、エポキシ基数:3以上)166重量部を加え均一に分散攪拌後に、ホモミキサ−により強制攪拌しながら、イオン交換水3000質量部を10分間で加え強制乳化した。その後、この水分散物を減圧蒸留により濃縮して、不揮発分15質量%の樹脂混合物の水分散体である繊維集束剤(R1)を得た。
Claims (6)
- アルコキシポリオキシアルキレン構造及びウレタン結合を有するビニルエステル樹脂(A)と、水性媒体とを含有する繊維集束剤であって、前記ビニルエステル樹脂(A)の(メタ)アクリロイル当量が500〜3,000g/当量の範囲であることを特徴とする繊維集束剤。
- 前記ビニルエステル樹脂(A)が、ビスフェノールA型エポキシ樹脂由来の構造を有するものである請求項1記載の繊維集束剤。
- 前記ビニルエステル樹脂(A)以外のビニルエステル樹脂(B)をさらに含有する請求項1又は2記載の繊維集束剤。
- 請求項1〜3のいずれか1項記載の繊維集束剤を有することを特徴とする繊維材料。
- 請求項4記載の繊維材料及び熱硬化性樹脂を含有することを特徴とする成形材料。
- 請求項5記載の成形材料の硬化物であることを特徴とする成形品。
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