JP6881936B2 - テープワインディング成形法、テープワインディング成形用繊維強化樹脂組成物 - Google Patents
テープワインディング成形法、テープワインディング成形用繊維強化樹脂組成物 Download PDFInfo
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- JP6881936B2 JP6881936B2 JP2016199455A JP2016199455A JP6881936B2 JP 6881936 B2 JP6881936 B2 JP 6881936B2 JP 2016199455 A JP2016199455 A JP 2016199455A JP 2016199455 A JP2016199455 A JP 2016199455A JP 6881936 B2 JP6881936 B2 JP 6881936B2
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Landscapes
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
(C)強化繊維20〜80質量%
を含む繊維強化樹脂組成物であって、カルボン酸基を有する構造単位の含有率が0.025〜0.1質量%である前記繊維強化樹脂組成物(但し、前記(I)成分と前記(C)成分の合計を100質量%とする)を含むテープを用いたレーザーによるテープワインディング成形法において、
前記繊維強化樹脂組成物は、マトリックス樹脂として、未変性のプロピレン系樹脂(未変性体)とカルボン酸構造又はカルボン酸塩構造を含む変性プロピレン系樹脂(変性体)の未変性体/変性体の質量比が80/21〜93/7であるプロピレン系樹脂(D)を含み、
前記繊維強化樹脂組成物は、(II)波長が300〜3000μmの光を吸収する色素0.01〜5質量%(但し、前記(I)成分と前記(C)成分の合計を100質量%とする)をさらに含むレーザーによるテープワインディング成形法。
(C)強化繊維20〜80質量%
を含む繊維強化樹脂組成物であって、カルボン酸基を有する構造単位の含有率が0.025〜0.1質量%であるテープワインディング成形用繊維強化樹脂組成物(但し、前記(I)成分と前記(C)成分の合計を100質量%とする)において、
マトリックス樹脂として、未変性のプロピレン系樹脂(未変性体)とカルボン酸構造又はカルボン酸塩構造を含む変性プロピレン系樹脂(変性体)の未変性体/変性体の質量比が80/21〜93/7であるプロピレン系樹脂(D)を含み、
(II)波長が300〜3000μmの光を吸収する色素0.01〜5質量%(但し、前記(I)成分と前記(C)成分の合計を100質量%とする)をさらに含むレーザーによるテープワインディング成形用繊維強化樹脂組成物。
酸価=(5.611×A×F)/B (mgKOH/g)
A:0.1規定水酸化カリウム−エタノール標準液使用量(ml)
F:0.1規定水酸化カリウム−エタノール標準液のファクター
B:試料採取量(g)。
中和されていないカルボン酸基のモル数=酸価×1000/56(モル/g)。
転化率%=(1−r)×100(%)
r:中和されていないカルボン酸基のモル数/カルボン酸基の総モル数。
また好ましいメルトフローレート範囲としては、ASTM1238規格、190℃、2.16kg荷重での測定値が上記と同様の数値範囲である場合もある。
本発明において、強化繊維(C)と効率的に接触させる観点からは、プロピレン系樹脂(A)やプロピレン系樹脂(B) は、エマルション状態で用いることが好ましい。
プロピレン系樹脂(A)>プロピレン系樹脂(D)>プロピレン系樹脂(B)
プロピレン系樹脂(D)は、主として強化繊維、プロピレン系樹脂(A)、プロピレン系樹脂(B)を含む強化繊維束の周りに接着するような態様になっていることが好ましい。
前記樹脂の重量平均分子量としては、具体的には5万〜40万の範囲にあることが好ましく、より好ましくは10万〜37万であり、更に好ましくは15万〜35万である。
○:短繊維が裁断前とほぼ同じ状態を保っている。
×:短繊維が大きくばらけたり、割れが生じている 。
プロピレン系樹脂の付着した強化繊維束を約5g取り、120℃で3時間乾燥し、その質量W1(g)を測定した。次いで強化繊維束を窒素雰囲気中で、450℃で15分間加熱後、室温まで冷却しその質量W2(g)を測定した。W1(g)およびW2(g)を用いて付着量は次式にて算出した。
付着量=[(W1−W2)/W2]×100(質量%)。
分子量は、以下の条件でのGPC法で求めた。
液体クロマトグラフ:Polymer Laboratories社製 PL−GPC220型高温ゲル浸透クロマトグラフ(示差屈折率計装置内蔵)
カラム:東ソー株式会社製 TSKgel GMHHR−H(S)−HT×2本および同GMHHR−H(S)×1本を直列接続した。
移動相媒体:1,2,4−トリクロロベンゼン(安定剤0.025%含有)
流速:1.0ml/分
測定温度:150℃
検量線の作成方法:標準ポリスチレンサンプルを使用した。
サンプル濃度:0.15%(w/v)
サンプル溶液量:500μl
検量線作成用標準サンプル:東ソー社製単分散ポリスチレン
分子量較正方法:標準較正法(ポリスチレン換算)
第1および第2の各プロピレン系樹脂について、有機化合物元素分析、誘導結合プラズマ(ICP)発光分析、IR(赤外吸収)スペクトル分析、1H−NMR測定および13C−NMR測定を実施し、プロピレン系樹脂の含有元素量、官能基構造の同定、各帰属プロトン、カーボンのピーク強度より単量体構造の含有割合について評価を実施した。
第1および第2の各プロピレン系樹脂に対して、以下の操作をおこなうことでカルボン酸塩含有量および中和されていないカルボン酸含有量を測定した。
酸価=(5.611×A×F)/B (mgKOH/g)
A:0.1規定水酸化カリウム−エタノール標準液使用量(ml)
F:0.1規定水酸化カリウム−エタノール標準液のファクター(1.02)
B:試料採取量(0.50g)。
中和されていないカルボン酸基のモル数=酸価×1000/56(モル/g)
転化率%=(1−r)×100(%)
r:中和されていないカルボン酸基のモル数/カルボン酸基の総モル数。
(5)擦過毛羽数測定
特許5584977号の実施例に記載の方法と同様にして決定した。
擦過毛羽数が0〜5個/mを合格とし、それを超えると不合格とした。
ワインディング成形体の外観は、目視で評価した。評価項目は、樹脂の絞り出し、繊維の飛び出し、表面低滑性、表面光沢である。
(7)融点の測定方法
本発明における重合体の融点(Tm)は、セイコーインスツルメンツ社製DSC220C装置で示差走査熱量計(DSC)により測定した。試料7〜12mgをアルミニウムパン中に密封し、室温から10℃/分で200℃まで加熱した。その試料を、全ての結晶を完全融解させるために200℃で5分間保持し、次いで10℃/分で−50℃まで冷却した。−50℃で5分間置いた後,その試料を10℃/分で200℃まで2度目に加熱した。この2度目の加熱試験で、ピーク温度を融点(Tm−II)として採用した。
炭素繊維束(三菱レイヨン社製、製品名:パイロフィルTR50S12L、フィラメント数12000本、ストランド強度5000MPa、ストランド弾性率242GPa)をアセトン中に浸漬し、10分間超音波を作用させた後、炭素繊維束を引き上げさらに3回アセトンで洗浄し、室温で8時間乾燥することにより付着しているサイジング剤を除去して用いた。
プロピレン系樹脂(A)として、GPCで測定した重量平均分子量が12万、融点を持たないプロピレン・ブテン・エチレン共重合体を100質量部、プロピレン系樹脂(B)の原料として、無水マレイン酸変性プロピレン系重合体(重量平均分子量Mw=20,000、酸価:45mg−KOH/g、無水マレイン酸含有率:4質量%、融点:140℃)10質量部、界面活性剤として、オレイン酸カリウム3質量部を混合した。この混合物を2軸スクリュー押出機(池貝鉄工株式会社製、PCM−30,L/D=40)のホッパーより3000g/時間の速度で供給し、同押出機のベント部に設けた供給口より、20%の水酸化カリウム水溶液を90g/時間の割合で連続的に供給し、加熱温度210℃で連続的に押出した。押出した樹脂混合物を、同押出機口に設置したジャケット付きスタティックミキサーで110℃まで冷却し、さらに80℃の温水中に投入してエマルジョンを得た。得られたエマルジョンは固形分濃度:45%であった。
製造例1で製造したエマルションを、ローラー含浸法を用いて、前記三菱レーヨン製強化繊維に付着させた。次いで、オンラインで130℃、2分乾燥して低沸点成分を除去し、本発明の強化繊維束を得た。エマルションの付着量は0.87%であった。炭素繊維束の毛羽立ち性は合格であった。
変性ポリプロピレンを、無水マレイン酸を0.8質量%グラフトした変性ポリプロピレン(ASTM D1238に準じ、190℃、荷重2.16kgで測定したメルトフローレートが220g/10分、融点が160℃)に変更し、前記J106MGと変性ポリプロピレンとの質量比は90/10(重量平均分子量は29万に相当)に変更した以外は、実施例1と同様にしてワインディングパイプを得た。カルボン酸基含有構造単位の含有率は、0.0035質量%であった。
前記J106MGと変性ポリプロピレンとの質量比を90/10(重量平均分子量は31万に相当)とした以外は実施例1と同様にしてワインデングパイプを得た。カルボン酸基含有構造単位の含有率は、0.023質量%であった。
Claims (2)
- (I)炭素数2〜20のオレフィン由来単位を含み、融点および/またはガラス転移温度が50〜300℃のカルボン酸基を有する重合体20〜80質量%、および
(C)強化繊維20〜80質量%
を含む繊維強化樹脂組成物であって、カルボン酸基を有する構造単位の含有率が0.025〜0.1質量%である前記繊維強化樹脂組成物(但し、前記(I)成分と前記(C)成分の合計を100質量%とする)を含むテープを用いたレーザーによるテープワインディング成形法において、
前記繊維強化樹脂組成物は、マトリックス樹脂として、未変性のプロピレン系樹脂(未変性体)とカルボン酸構造又はカルボン酸塩構造を含む変性プロピレン系樹脂(変性体)の未変性体/変性体の質量比が80/21〜93/7であるプロピレン系樹脂(D)を含み、
前記繊維強化樹脂組成物は、(II)波長が300〜3000μmの光を吸収する色素0.01〜5質量%(但し、前記(I)成分と前記(C)成分の合計を100質量%とする)をさらに含むレーザーによるテープワインディング成形法。 - (I)炭素数2〜20のオレフィン由来単位を含み、融点および/またはガラス転移温度が50〜300℃のカルボン酸基を有する重合体20〜80質量%、および
(C)強化繊維20〜80質量%
を含む繊維強化樹脂組成物であって、カルボン酸基を有する構造単位の含有率が0.025〜0.1質量%であるテープワインディング成形用繊維強化樹脂組成物(但し、前記(I)成分と前記(C)成分の合計を100質量%とする)において、
マトリックス樹脂として、未変性のプロピレン系樹脂(未変性体)とカルボン酸構造又はカルボン酸塩構造を含む変性プロピレン系樹脂(変性体)の未変性体/変性体の質量比が80/21〜93/7であるプロピレン系樹脂(D)を含み、
(II)波長が300〜3000μmの光を吸収する色素0.01〜5質量%(但し、前記(I)成分と前記(C)成分の合計を100質量%とする)をさらに含むレーザーによるテープワインディング成形用繊維強化樹脂組成物。
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