JP2023040186A - 炭素繊維及び炭素繊維強化樹脂組成物の製造方法 - Google Patents
炭素繊維及び炭素繊維強化樹脂組成物の製造方法 Download PDFInfo
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Abstract
Description
[1]
炭素繊維複合材料(CFC)を、酸性水溶液に浸漬して、CFCの樹脂分の少なくとも一部を溶出して略繊維状物を得る工程(1)、及び
工程(1)で得られた略繊維状物をアルカリ性水溶液に浸漬して、略繊維状物の樹脂分の少なくとも一部を溶出して繊維状物を得る工程(2)、
を含む、炭素繊維の製造方法。
[2]
工程(1)における樹脂分の溶出量は、浸漬前のCFCの質量を100としたときに、0.1~99.9の範囲である、[1]に記載の製造方法。
[3]
工程(2)における樹脂分の溶出量は、浸漬前のCFCの質量を100としたときに、0.1~99.9の範囲である、[1]又は[2]に記載の製造方法。
[4]
略繊維状物は、一部または全部が繊維状である、[1]~[3]のいずれかに記載の製造方法。
[5]
CFCが、未硬化プリプレグ又は硬化済プリプレグである、[1]~[4]のいずれかに記載の製造方法。
[6]
CFCが、未硬化プリプレグであり、工程(1)において、未硬化プリプレグの一部が繊維状に分解するまで、酸性水溶液に浸漬して略繊維状物を得る、[1]~[4]のいずれかに記載の製造方法。
[7]
CFCが、硬化済みプリプレグであり、工程(1)において、硬化済みプリプレグの全部が繊維状に分解するまで、酸性水溶液に浸漬して略繊維状物を得る、[1]~[4]のいずれかに記載の製造方法。
[8]
工程(2)で得られた繊維状物を酸性水溶液に浸漬して、繊維状物に付着する樹脂分および/またはサイジング剤をさらに溶出して、水分散性が向上した繊維状物を得る工程(3)をさらに含む[1]~[7]のいずれかに記載の製造方法。
[9]
[1]~[8]のいずれかに記載の方法により、炭素繊維を製造する工程、得られた炭素繊維を用いて、炭素繊維強化樹脂組成物を製造する工程を含む、炭素繊維強化樹脂組成物の製造方法。
[10]
前記炭素繊維強化樹脂組成物は、炭素繊維と熱可塑性樹脂及び/又は熱硬化性樹脂を含む樹脂組成物であって、(A)炭素繊維と(B)熱可塑性樹脂及び/又は熱硬化性樹脂の合計量を100質量%として、(A)炭素繊維5~95質量%、(B)熱可塑性樹脂及び/又は熱硬化性樹脂5~95質量%からなる炭素繊維強化樹脂組成物である、[9]に記載の製造方法。
[11]
熱可塑性樹脂がポリオレフィン系樹脂、ポリアミド系樹脂、スチレン系樹脂、ポリカーボネート系樹脂、ポリエステル系樹脂、ポリフェニレンエーテル樹脂、ポリフェニレンスルファイド樹脂、ポリアセタール樹脂、アクリル系樹脂及び塩化ビニル樹脂からなる群より選ばれた少なくとも一種である[10]に記載の製造方法。
[12]
熱硬化性樹脂が、エポキシ樹脂、フェノール樹脂、メラミン樹脂、ユリア樹脂、ジアリルフタレート樹脂、不飽和ポリエステル樹脂からなる群より選ばれた少なくとも一種である [10]に記載の製造方法。
本発明の炭素繊維の製造方法は、CFCを酸性水溶液に浸漬して、CFCの樹脂分の少なくとも一部を溶出して略繊維状物を得る工程(1)、及び
工程(1)で得られた略繊維状物をアルカリ性水溶液に浸漬して、略繊維状物の樹脂分の少なくとも一部を溶出して
繊維状物を得る工程(2)、
を含む。
CFCを、酸性水溶液に浸漬し、CFCの樹脂分の少なくとも一部を溶出して略繊維状物を得る。CFCは、特に制限はないが、炭素繊維と熱硬化型樹脂を複合した複合材料であり、熱硬化型樹脂を硬化する前の未硬化プリプレグであっても、硬化済プリプレグであってもよい。未硬化プリプレグは、CFC製品を製造する過程で生じる端材や不良品等として回収される物であることができる。硬化済プリプレグは、使用済みのCFC、例えば、炭素繊維強化プラスチック(CFRP)であっても、製造する過程で生じる端材や不良品等であってもよい。いずれもこれまでは廃材として主に焼却あるいは埋設処理されていた物である。
工程(1)で得られた略繊維状物をアルカリ性水溶液に浸漬して、全部が繊維状となった繊維状物を得る。酸性水溶液中にさらに長時間浸漬しても、樹脂の残渣等の除去の進行は難しい工程(1)で得られた略繊維状物をアルカリ性水溶液に浸漬することで、比較的容易に樹脂の残渣等の除去が可能である。
本発明の炭素繊維強化樹脂組成物の製造方法は、上記本発明の方法により、炭素繊維を製造する工程、及び得られた炭素繊維を用いて、炭素繊維強化樹脂組成物を製造する工程を含む。
工程(1)
6Mに希釈した濃硝酸を反応容器に入れ、湯浴中で60~70℃に加熱し、攪拌しながら硝酸100質量部に対して、炭酸水素ナトリウム水溶液にて前処理し、切断済みの未硬化プリプレグを10~20質量部加え、10~20分加熱攪拌を行った。発熱を伴う場合もあるが、内温を80℃以下に保った。反応物を硝酸から取り出し、直ちに水に放つと、エポキシ樹脂の一部が溶解した、茶色の炭素繊維が得られた。なお、濃硝酸は酸化力を高めるため、硫酸と任意の割合で混合した混酸でもよい。(表1-1サンプルNo.1,2および図1)また、混酸100質量部に対し、硬化プリプレグを30部加え、120時間加熱浸漬するとエポキシ樹脂の大部分が溶解した、繊維状の炭素繊維が得られた。(表1-1、サンプルNo.3)
次に、表1-2に示す組成のアルカリ性水溶液100部に対し、サンプルNo.1~3の炭素繊維をそれぞれ10部加え攪拌すると、エポキシ樹脂の大部分が溶解し、開繊した羊毛状の炭素繊維が得られた。(表1-2および図2)
炭素繊維の水に対する分散性は、水1000mLに対し、炭素繊維1gをホモジナイザーを用いて8000rpmで1分間攪拌したもので比較した。
炭素繊維を走査型電子顕微鏡により観察し、炭素繊維表面の樹脂残渣の有無を確認した。
表1-3~表1-6の各炭素繊維サンプルを用い、抄紙法にてPPとの組成物(炭素繊維複合材シート)を作成した。
表1-3~表1-6の各炭素繊維サンプルから、適当なサンプルを選び、表2に記載する各熱可塑性樹脂との組成物を作成した。
実施例2、3により作成した、各熱可塑性樹脂組成物の力学物性の結果を下記の表2に示す(実施例2:サンプルNo101~106、実施例3:サンプルNo.107~130)。
Claims (12)
- 炭素繊維複合材料(以下、CFCと呼ぶ)を、酸性水溶液に浸漬して、CFCの樹脂分の少なくとも一部を溶出して略繊維状物を得る工程(1)、及び
工程(1)で得られた略繊維状物をアルカリ性水溶液に浸漬して、略繊維状物の樹脂分の少なくとも一部を溶出して繊維状物を得る工程(2)、
を含む、炭素繊維の製造方法。 - 工程(1)における樹脂分の溶出量は、浸漬前のCFCの質量を100としたときに、0.1~99.9の範囲である、請求項1に記載の製造方法。
- 工程(2)における樹脂分の溶出量は、浸漬前のCFCの質量を100としたときに、0.1~99.9の範囲である、請求項1又は2に記載の製造方法。
- 略繊維状物は、一部または全部が繊維状である、請求項1~3のいずれかに記載の製造方法。
- CFCが、未硬化プリプレグ又は硬化済プリプレグである、請求項1~4のいずれかに記載の製造方法。
- CFCが、未硬化プリプレグであり、工程(1)において、未硬化プリプレグの一部が繊維状に分解するまで、酸性水溶液に浸漬して略繊維状物を得る、請求項1~4のいずれかに記載の製造方法。
- CFCが、硬化済みプリプレグであり、工程(1)において、硬化済みプリプレグの全部が繊維状に分解するまで、酸性水溶液に浸漬して略繊維状物を得る、請求項1~4のいずれかに記載の製造方法。
- 工程(2)で得られた繊維状物を酸性水溶液に浸漬して、繊維状物に付着する樹脂分および/またはサイジング剤をさらに溶出して、水分散性が向上した繊維状物を得る工程(3)をさらに含む請求項1~7のいずれかに記載の製造方法。
- 請求項1~8のいずれかに記載の方法により、炭素繊維を製造する工程、得られた炭素繊維を用いて、炭素繊維強化樹脂組成物を製造する工程を含む、炭素繊維強化樹脂組成物の製造方法。
- 前記炭素繊維強化樹脂組成物は、炭素繊維と熱可塑性樹脂及び/又は熱硬化性樹脂を含む樹脂組成物であって、(A)炭素繊維と(B)熱可塑性樹脂及び/又は熱硬化性樹脂の合計量を100質量%として、(A)炭素繊維5~95質量%、(B)熱可塑性樹脂及び/又は熱硬化性樹脂5~95質量%からなる炭素繊維強化樹脂組成物である、請求項9に記載の製造方法。
- 熱可塑性樹脂がポリオレフィン系樹脂、ポリアミド系樹脂、スチレン系樹脂、ポリカーボネート系樹脂、ポリエステル系樹脂、ポリフェニレンエーテル樹脂、ポリフェニレンスルファイド樹脂、ポリアセタール樹脂、アクリル系樹脂及び塩化ビニル樹脂からなる群より選ばれた少なくとも一種である請求項10に記載の製造方法。
- 熱硬化性樹脂が、エポキシ樹脂、フェノール樹脂、メラミン樹脂、ユリア樹脂、ジアリルフタレート樹脂、不飽和ポリエステル樹脂からなる群より選ばれた少なくとも一種である 請求項10に記載の製造方法。
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