JP6179591B2 - サイジング剤塗布強化繊維、サイジング剤塗布強化繊維の製造方法、プリプレグおよび繊維強化複合材料 - Google Patents
サイジング剤塗布強化繊維、サイジング剤塗布強化繊維の製造方法、プリプレグおよび繊維強化複合材料 Download PDFInfo
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- LTUKBRXELKXITI-UHFFFAOYSA-N n-(oxiran-2-ylmethyl)benzamide Chemical compound C=1C=CC=CC=1C(=O)NCC1CO1 LTUKBRXELKXITI-UHFFFAOYSA-N 0.000 description 1
- FZZQNEVOYIYFPF-UHFFFAOYSA-N naphthalene-1,6-diol Chemical compound OC1=CC=CC2=CC(O)=CC=C21 FZZQNEVOYIYFPF-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- JOHZOQCMGQMKML-UCQHMBSKSA-N octakis(2,3,6-tri-o-methyl)-γ-cyclodextrin Chemical compound COC[C@H]([C@H]([C@@H]([C@H]1OC)OC)O[C@@H]2O[C@@H]([C@@H](O[C@@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O[C@@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O[C@@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O[C@@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O[C@@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O3)[C@H](OC)[C@H]2OC)COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H]3O[C@@H]1COC JOHZOQCMGQMKML-UCQHMBSKSA-N 0.000 description 1
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- JOXIMZWYDAKGHI-UHFFFAOYSA-N p-toluenesulfonic acid Substances CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
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- 125000005499 phosphonyl group Chemical group 0.000 description 1
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- 239000011574 phosphorus Substances 0.000 description 1
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- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- SCUZVMOVTVSBLE-UHFFFAOYSA-N prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1 SCUZVMOVTVSBLE-UHFFFAOYSA-N 0.000 description 1
- 229960000380 propiolactone Drugs 0.000 description 1
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- 125000005372 silanol group Chemical group 0.000 description 1
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- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910021647 smectite Inorganic materials 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
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- 235000019698 starch Nutrition 0.000 description 1
- 150000003431 steroids Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- DIRLEDPEXJLCIL-JCWBWLHSSA-N succinyl-β-cyclodextrin Chemical compound OC(=O)CCC(=O)OC[C@H]([C@H]([C@H]([C@@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](COC(=O)CCC(O)=O)[C@H]([C@H]([C@@H]3O)O)O[C@H]3O[C@H](COC(=O)CCC(O)=O)[C@H]([C@H]([C@@H]3O)O)O[C@H]3O[C@H](COC(=O)CCC(O)=O)[C@H]([C@H]([C@@H]3O)O)O[C@H]3O[C@H](COC(=O)CCC(O)=O)[C@H]([C@H]([C@@H]3O)O)O3)[C@@H](O)[C@@H]2O)COC(=O)CCC(=O)C)O[C@@H]1O[C@H]1[C@@H](O)[C@H](O)[C@@H]3O[C@@H]1COC(=O)CCC(O)=O DIRLEDPEXJLCIL-JCWBWLHSSA-N 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 125000000475 sulfinyl group Chemical group [*:2]S([*:1])=O 0.000 description 1
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- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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- 238000004448 titration Methods 0.000 description 1
- 125000002088 tosyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1C([H])([H])[H])S(*)(=O)=O 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
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- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 1
- RKBCYCFRFCNLTO-UHFFFAOYSA-N triisopropylamine Chemical compound CC(C)N(C(C)C)C(C)C RKBCYCFRFCNLTO-UHFFFAOYSA-N 0.000 description 1
- DSDAICPXUXPBCC-MWDJDSKUSA-N trimethyl-β-cyclodextrin Chemical compound COC[C@H]([C@H]([C@@H]([C@H]1OC)OC)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O[C@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O[C@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O[C@H]3O[C@H](COC)[C@H]([C@@H]([C@H]3OC)OC)O3)[C@H](OC)[C@H]2OC)COC)O[C@@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@@H]3O[C@@H]1COC DSDAICPXUXPBCC-MWDJDSKUSA-N 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/248—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using pre-treated fibres
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/11—Compounds containing epoxy groups or precursors thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/165—Ethers
- D06M13/17—Polyoxyalkyleneglycol ethers
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/11—Starch or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/507—Polyesters
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- D—TEXTILES; PAPER
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2363/02—Polyglycidyl ethers of bis-phenols
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- C08J2481/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2481/06—Polysulfones; Polyethersulfones
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
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- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Reinforced Plastic Materials (AREA)
Description
ポリロタキサンに用いられる環状分子は、その開口部に直鎖状分子が串刺し状に包接され得る分子であれば、特に限定されない。
ポリロタキサンの直鎖状分子は、環状分子の開口部に串刺し状に包接され得るものであれば、特に限定されない。
複数の環状分子が直鎖状分子を串刺し状に包接する際に、1本の直鎖状分子を環状分子が最大限に包接する量を1とした場合、前記環状分子が0.001〜0.6、好ましくは0.01〜0.5、より好ましくは0.05〜0.4の範囲の量で直鎖状分子を包接するのがよい。
ポリロタキサンの封鎖基は、直鎖状分子の両端に配置され、環状分子が脱離しないように作用する基であれば、特に限定されない。
(A−1)“デナコール(登録商標)”EX−521(ナガセケムテックス(株)製:ポリグリセリンポリグリシジルエーテル)
(A−2)“デナコール(登録商標)”EX−411(ナガセケムテックス(株)製:ペンタエリスリトールポリグリシジルエーテル)
(A−3)“デナコール(登録商標)”EX−611(ナガセケムテックス(株)製:ソルビトールポリグリシジルエーテル)。
(B−1)“セルム(登録商標)”スーパーポリマーSH2400P(アドバンストソフトマテリアルズ(株)製:環状分子はα−シクロデキストリン;直鎖状分子は重量平均分子量20,000のポリエチレングリコール;封鎖基はアダマンタン基;環状分子はポリ(ε−カプロラクトン)からなるグラフト鎖により修飾されている)
(B−2)“セルム(登録商標)”スーパーポリマーSH1310P(アドバンストソフトマテリアルズ(株)製:環状分子はα−シクロデキストリン;直鎖状分子は重量平均分子量11,000のポリエチレングリコール;封鎖基はアダマンタン基;環状分子はポリ(ε−カプロラクトン)からなるグラフト鎖により修飾されている)
(B−3)“セルム(登録商標)”スーパーポリマーSH3400P(アドバンストソフトマテリアルズ(株)製:環状分子はα−シクロデキストリン;直鎖状分子は重量平均分子量35,000のポリエチレングリコール;封鎖基はアダマンタン基;環状分子はポリ(ε−カプロラクトン)からなるグラフト鎖により修飾されている)。
本実施例では、強化繊維として炭素繊維を用いた。本実施例は、次の第Iの工程、第IIの工程および第IIIの工程からなる。
アクリロニトリル99モル%とイタコン酸1モル%からなる共重合体を紡糸した後、焼成し、総フィラメント数12,000本、比重1.8、ストランド引張強度700kgf/mm2、ストランド引張弾性率33,000kgf/mm2の炭素繊維を得た。次いで、その炭素繊維を、濃度0.1モル/リットルの炭酸水素アンモニウム水溶液を電解液として、液相電解酸化処理した。この液相電解酸化処理を施された炭素繊維を続いて水洗し、150℃の温度の加熱空気中で乾燥し、表面酸化処理された炭素繊維を得た。
エポキシ基を有する化合物として(A−1)を70質量部、ポリロタキサンとして(B−1)が30質量部を、溶媒としてジメチルホルムアミドに溶解してサイジング剤溶液を調合した。このサイジング剤溶液を浸漬法を用いて、上記により得られた表面酸化処理された炭素繊維に塗布した後、210℃の温度で180秒間熱処理をして、サイジング剤塗布炭素繊維束を得た。サイジング剤の付着量を、以下に記す方法により測定し、サイジング剤塗布炭素繊維100質量部に対して、サイジング剤の付着量が0.5質量部となるように調整した。
約2gのサイジング剤塗布炭素繊維束を秤量(W1)(小数第4位まで読み取り)した後、50ミリリットル/分の窒素気流中、450℃の温度に設定した電気炉(容量120cm3)に15分間放置し、サイジング剤を完全に熱分解させた。そして、20リットル/分の乾燥窒素気流中の容器に移し、15分間冷却した後の炭素繊維束を秤量(W2)(少数第4位まで読み取り)した。次式よりサイジング剤塗布炭素繊維束100質量部に対するサイジング剤付着量を求めた。
サイジング剤付着量(質量部)=[W1(g)−W2(g)]/[W1(g)]×100
本実施例では、測定は2回おこない、その平均値をサイジング剤付着量とした。
界面剪断強度(IFSS)の測定は、次の(a)〜(d)の手順でおこなった。
ビスフェノールA型エポキシ樹脂化合物“jER”(登録商標)828(三菱化学(株)製)100質量部とメタフェニレンジアミン(シグマアルドリッチジャパン(株)製)14.5質量部を、それぞれ容器に入れた。その後、上記のjER828の粘度低下とメタフェニレンジアミンの溶解のため、75℃の温度で15分間加熱をおこなった後、両者をよく混合し、80℃の温度で約15分間真空脱泡をおこなった。
炭素繊維束から単繊維を抜き取り、単繊維に一定張力を与えた状態で、単繊維の両端をダンベル型モールドの長手方向に接着剤で固定した。その後、炭素繊維およびモールドに付着した水分を除去するため、80℃の温度で30分間以上真空乾燥をおこなった。ダンベル型モールドは、シリコーンゴム製で、注型部分の形状は、中央部分巾5mm、長さ25mm、両端部分巾10mm、全体長さ150mmである。
上記(b)の手順の真空乾燥後のダンベル型モールド内に、上記(a)の手順で調製した樹脂を流し込み、オーブンを用いて、昇温速度1.5℃/分で75℃の温度まで上昇し、75℃で2時間保持後、昇温速度1.5分で125℃の温度まで上昇し、125℃で2時間保持後、降温速度2.5℃/分で30℃の温度まで降温させた。その後、脱型して試験片を得た。
上記(c)の手順で得られた試験片に、繊維軸方向(長手方向)に引張力を与え、歪みを12%生じさせた後、偏光顕微鏡を用いて試験片中心部22mmの範囲における繊維破断数N(個)を測定した。次に、平均破断繊維長laを、la(μm)=22×1000(μm)/N(個)の式により計算し、さらに平均破断繊維長laから臨界繊維長lcを、lc(μm)=(4/3)×la(μm)の式により計算した。ストランド引張強度σと炭素繊維単糸の直径dを測定し、界面剪断強度IFSSを、次式で算出した。実施例では、測定数n=5の平均を試験結果とした。
界面剪断強度IFSS(MPa)=σ(MPa)×d(μm)/(2×lc)(μm)
なお、ストランド引張強度は、JIS−R−7608(2004)の樹脂含浸ストランド試験法に準拠し、次の手順に従い求めた。含浸させる樹脂としては、“セロキサイド”(登録商標)2021P(ダイセル化学工業社製)/三フッ化ホウ素モノエチルアミン(東京化成工業(株)製)/アセトン=100/3/4(質量部)を用いた。樹脂の硬化条件としては、常圧、温度125℃、硬化時間30分とした。炭素繊維束のストランド10本を測定し、その平均値をストランド引張強度とした。
<プリプレグの作製>
まず、ビスフェノールA型エポキシ樹脂、“jER(登録商標)”828(三菱化学(株)製)60質量部、テトラグリシジルジアミノジフェニルメタン、ELM434(住友化学(株)製)40質量部、4,4’−ジアミノジフェニルスルホン、“セイカキュア(登録商標)”S(和歌山精化(株)製)40質量部および、ポリエーテルスルホン“スミカエクセル(登録商標)”PES5003P(住友化学(株)製)10質量部を混練したエポキシ樹脂組成物を調製し、これをナイフコーターを用いて樹脂目付30g/m2で離型紙上にコーティングし、1次樹脂フィルムを作製した。この1次樹脂フィルムを1方向に引き揃えたサイジング剤塗布炭素繊維(目付190g/m2)の両側に重ね合わせて、ヒートロールを用い加熱加圧しながらエポキシ樹脂組成物をサイジング剤塗布炭素繊維に含浸させることにより、1次プリプレグを作製した。次に、上記のエポキシ樹脂組成物にさらに“トレパール(登録商標)”TN(東レ(株)製、平均粒子径:13.0μm)80質量部を混練した樹脂組成物を調製し、これをナイフコーターを用いて樹脂目付20g/m2で離型紙上にコーティングし、2次樹脂フィルムを作製した。この2次樹脂フィルムを1次プリプレグの両側に重ね合せて、樹脂組成物を1次プリプレグに含浸させ、目的のプリプレグを作製した。
前記のようにして作製したプリプレグを裁断し、一方向積層した後、オートクレーブを用いて加熱硬化させ、一方向強化材(炭素繊維強化複合材料)を作製した。JIS K7086(1993)に記載の双方持ちはり試験に従って、亀裂進展初期のモードI層間破壊靱性(GIc)を求めたところ、十分に高い値を示した。結果を表1に示す。
第Iの工程:原料となる炭素繊維を製造する工程
実施例1と同様にした。
各成分の比が表1に記載のようになるようにした以外は、実施例1と同様の方法でサイジング剤塗布炭素繊維を得た。続いて、得られたサイジング剤塗布炭素繊維を用いて、実施例1と同様に界面剪断強度(IFSS)を測定したところ、接着性が十分に高いことがわかった。結果を表1に示す。
実施例1と同様に、一方向強化材(炭素繊維強化複合材料)を作製し、力学特性を評価したところ、モードI層間破壊靱性(GIc)は十分に高い値を示した。結果を表1に示す。
第Iの工程:炭素繊維を製造する工程
実施例1と同様にした。
サイジング剤の付着量をサイジング剤塗布炭素繊維100質量部に対して1質量部となるようにサイジング剤溶液濃度を調整した以外は、実施例1と同様の方法でサイジング剤塗布炭素繊維を得た。続いて、得られたサイジング剤塗布炭素繊維を用いて、実施例1と同様に界面剪断強度(IFSS)を測定したところ、接着性が十分に高いことがわかった。結果を表1に示す。
実施例1と同様に、一方向強化材(炭素繊維強化複合材料)を作製し、力学特性を評価したところ、モードI層間破壊靱性(GIc)は十分に高い値を示した。結果を表1に示す。
第Iの工程:炭素繊維を製造する工程
実施例1と同様にした。
サイジング剤溶液を、(A−2)成分のみで調合した以外は、実施例1と同様の方法でサイジング剤塗布炭素繊維を得た。続いて、得られたサイジング剤塗布炭素繊維を用いて、実施例1と同様に界面剪断強度(IFSS)を測定したところ、接着性が十分に高いことがわかった。結果を表1に示す。
実施例1と同様に、一方向強化材(炭素繊維強化複合材料)を作製し、力学特性を評価したところ、モードI層間破壊靱性(GIc)は低い値を示した。結果を表1に示す。
Claims (15)
- 強化繊維にポリロタキサンを含むサイジング剤が塗布されてなるサイジング剤塗布強化繊維。
- 前記サイジング剤が、エポキシ基を有する化合物をさらに含む、請求項1に記載のサイジング剤塗布強化繊維。
- 前記エポキシ基を有する化合物が、分子内にエポキシ基を2以上有する化合物であって、ポリエーテル型ポリエポキシ化合物およびポリオール型ポリエポキシ化合物から選ばれた化合物である、請求項2に記載のサイジング剤塗布強化繊維。
- 前記エポキシ基を有する化合物が、グリセリン、ジグリセリン、ポリグリセリン、トリメチロールプロパン、ペンタエリスリトール、ソルビトール、およびアラビトールから選択される1種以上の化合物と、エピクロロヒドリンとの反応により得られるグリシジルエーテル型エポキシ化合物である、請求項3に記載のサイジング剤塗布強化繊維。
- 前記サイジング剤が、サイジング剤全量に対してポリロタキサンを5〜80質量%含む、請求項1〜4のいずれかに記載のサイジング剤塗布強化繊維。
- 前記ポリロタキサンの構成成分である直鎖状分子の重量平均分子量が15,000以上30,000以下である、請求項1〜5のいずれかに記載のサイジング剤塗布強化繊維。
- 前記ポリロタキサンが、シクロデキストリンおよびポリエチレングリコールを構成成分とする、請求項1〜6のいずれかに記載のサイジング剤塗布強化繊維。
- 前記シクロデキストリンが、高分子鎖により修飾されており、該高分子鎖は、−O−結合および−NH−結合から選ばれた結合、ならびに、アルキレン基およびアルケニレン基から選ばれた基を含む請求項7に記載のサイジング剤塗布強化繊維。
- 強化繊維が炭素繊維である請求項1〜8のいずれかに記載のサイジング剤塗布強化繊維。
- 強化繊維にポリロタキサンを含むサイジング剤を塗布した後、熱処理することによってサイジング剤塗布強化繊維を製造する方法であって、前記サイジング剤を塗布する工程において、サイジング剤の付着量がサイジング剤塗布強化繊維100質量部に対して0.1〜10質量部となるようにし、かつ、前記熱処理する工程の条件が160〜260℃の温度範囲で30〜600秒間であるサイジング剤塗布強化繊維の製造方法。
- 請求項1〜9のいずれかに記載のサイジング剤塗布強化繊維と、熱硬化性樹脂とを含むプリプレグ。
- 前記熱硬化性樹脂がエポキシ樹脂である請求項11に記載のプリプレグ。
- 請求項11または12に記載のプリプレグを硬化させてなる繊維強化複合材料。
- 請求項1〜9のいずれかに記載のサイジング剤塗布強化繊維と熱硬化性樹脂の硬化物からなる繊維強化複合材料。
- 前記熱硬化性樹脂がエポキシ樹脂である請求項14に記載の繊維強化複合材料。
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WO2015129513A1 (ja) | 2014-02-25 | 2015-09-03 | 東レ株式会社 | エポキシ樹脂組成物、樹脂硬化物、繊維強化複合材料およびプリプレグ |
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EP3118370B1 (en) | 2019-08-07 |
US10208173B2 (en) | 2019-02-19 |
EP3118370A4 (en) | 2017-09-27 |
JPWO2015137206A1 (ja) | 2017-04-06 |
WO2015137206A1 (ja) | 2015-09-17 |
US20170002154A1 (en) | 2017-01-05 |
CN106068346B (zh) | 2018-12-11 |
KR20160132040A (ko) | 2016-11-16 |
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