JP2019089931A - プリプレグ、繊維強化複合材料及び成形体 - Google Patents
プリプレグ、繊維強化複合材料及び成形体 Download PDFInfo
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- JP2019089931A JP2019089931A JP2017219064A JP2017219064A JP2019089931A JP 2019089931 A JP2019089931 A JP 2019089931A JP 2017219064 A JP2017219064 A JP 2017219064A JP 2017219064 A JP2017219064 A JP 2017219064A JP 2019089931 A JP2019089931 A JP 2019089931A
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- JP
- Japan
- Prior art keywords
- mass
- reinforced composite
- prepreg
- composite material
- fiber
- 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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- 239000003733 fiber-reinforced composite Substances 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 68
- 239000011342 resin composition Substances 0.000 claims abstract description 71
- 239000003822 epoxy resin Substances 0.000 claims abstract description 54
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 54
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 39
- 239000004917 carbon fiber Substances 0.000 claims abstract description 39
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical group C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims abstract description 30
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 235000010290 biphenyl Nutrition 0.000 claims abstract description 15
- 239000004305 biphenyl Substances 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 11
- 238000002485 combustion reaction Methods 0.000 claims description 21
- 238000011156 evaluation Methods 0.000 claims description 17
- 238000010030 laminating Methods 0.000 claims description 6
- 125000004437 phosphorous atom Chemical group 0.000 claims description 4
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 23
- 239000003063 flame retardant Substances 0.000 abstract description 23
- 239000011574 phosphorus Substances 0.000 abstract description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052736 halogen Inorganic materials 0.000 abstract description 8
- 150000002367 halogens Chemical class 0.000 abstract description 8
- 238000001723 curing Methods 0.000 description 27
- 229920005989 resin Polymers 0.000 description 16
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 8
- 230000009477 glass transition Effects 0.000 description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 7
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- 230000000052 comparative effect Effects 0.000 description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 6
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- 239000004843 novolac epoxy resin Substances 0.000 description 3
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- 229920006287 phenoxy resin Polymers 0.000 description 3
- -1 phosphorus compound Chemical class 0.000 description 3
- 125000004189 3,4-dichlorophenyl group Chemical group [H]C1=C([H])C(Cl)=C(Cl)C([H])=C1* 0.000 description 2
- XMTQQYYKAHVGBJ-UHFFFAOYSA-N 3-(3,4-DICHLOROPHENYL)-1,1-DIMETHYLUREA Chemical compound CN(C)C(=O)NC1=CC=C(Cl)C(Cl)=C1 XMTQQYYKAHVGBJ-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000011304 carbon pitch Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- 239000010419 fine particle Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000011295 pitch Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 description 1
- MGJKQDOBUOMPEZ-UHFFFAOYSA-N N,N'-dimethylurea Chemical compound CNC(=O)NC MGJKQDOBUOMPEZ-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000004842 bisphenol F epoxy resin Substances 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- XXOYNJXVWVNOOJ-UHFFFAOYSA-N fenuron Chemical compound CN(C)C(=O)NC1=CC=CC=C1 XXOYNJXVWVNOOJ-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- BMLIZLVNXIYGCK-UHFFFAOYSA-N monuron Chemical compound CN(C)C(=O)NC1=CC=C(Cl)C=C1 BMLIZLVNXIYGCK-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
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Abstract
Description
本実施形態に係るプリプレグは、炭素繊維と、ビフェニル構造を有するエポキシ樹脂、硬化剤及びメラミンシアヌレートを含有する樹脂組成物と、を含む。このようなプリプレグによれば、ハロゲン系難燃剤及びリン系難燃剤を使用することなく、薄さと難燃性とを両立した繊維強化複合材料を形成することができる。
本実施形態に係る繊維強化複合材料は、複数のプリプレグの積層及び硬化してなるものであり、複数のプリプレグのうち少なくとも一つは、上記実施形態に係るプリプレグである。本実施形態では、複数のプリプレグのうち、半数以上が上記実施形態に係るプリプレグであってよく、全てが上記実施形態に係るプリプレグであってよい。積層及び硬化される複数のプリプレグはそれぞれ、その構成が同じものであってよく、異なるものであってもよい。
ビフェニル構造を有するエポキシ樹脂(NC−3000、日本化薬社製)40質量部、ビスフェノールA型エポキシ樹脂(YD−128、新日鉄住金化学社製)14質量部、フェノールノボラック型エポキシ樹脂(YDPN−638、新日鉄住金化学社製)20質量部、メラミンシアヌレート(MC−6000、日産化学社製)40質量部、ジシアンジアミド(DICY)4質量部及び3−(3,4−ジクロロフェニル)−1,1−ジメチル尿素(DCMU)3質量部を混合して、樹脂組成物A−1を得た。得られた樹脂組成物A−1の30℃における粘度は60100Pa・sであった。また、140℃で2時間硬化した後の樹脂硬化物のガラス転移温度は155℃であり、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
ビフェニル構造を有するエポキシ樹脂、ビスフェノールA型エポキシ樹脂及びフェノールノボラック型エポキシ樹脂の配合量を、それぞれ35質量部、19質量部及び13質量部に変更したこと以外は実施例A−1と同様にして、樹脂組成物A−2を得た。得られた樹脂組成物A−2の30℃における粘度は、22100Pa・sであった。また、140℃で2時間硬化した後の樹脂組成物のガラス転移温度は151℃であり、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
ビフェニル構造を有するエポキシ樹脂、ビスフェノールA型エポキシ樹脂及びフェノールノボラック型エポキシ樹脂の配合量を、それぞれ30質量部、14質量部及び23質量部に変更し、フェノキシ樹脂(YP−70、新日鉄住金化学社製)5質量部を更に混合したこと以外は実施例A−1と同様にして、樹脂組成物A−3を得た。得られた樹脂組成物A−3の30℃における粘度は、113000Pa・sであった。また、140℃で2時間硬化した後のガラス転移温度は153℃であり、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
ビフェニル構造を有するエポキシ樹脂、ビスフェノールA型エポキシ樹脂及びフェノールノボラック型エポキシ樹脂の配合量を、それぞれ30質量部、32質量部及び0質量部に変更し、フェノキシ樹脂(YP−70、新日鉄住金化学社製)10質量部を更に混合したこと以外は実施例A−1と同様にして、樹脂組成物A−4を得た。得られた樹脂組成物A−4の30℃における粘度は、35000Pa・sであった。また、140℃で2時間硬化した後の樹脂組成物のガラス転移温度は128℃であり、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
炭素繊維としてT700S(東レ社製、引張弾性率230GPa)を用いたこと以外は、実施例A−2と同様にしてプリプレグの作製を行い、単位面積当たりの炭素繊維の量が200g/m2、樹脂含有率が32%のプリプレグ(プリプレグA−5)を得た。
ビスフェノールA型エポキシ樹脂(YD−128、新日鉄住金化学社製)37質量部、ビスフェノールA型エポキシ樹脂(YD−11、新日鉄住金化学社製)33質量部、フェノールノボラック型エポキシ樹脂(YDPN−638、新日鉄住金化学社製)30質量部、フェノキシ樹脂(YP−70、新日鉄住金化学社製)15質量部、ジシアンジアミド(DICY)4質量部及び3−(3,4−ジクロロフェニル)−1,1−ジメチル尿素(DCMU)3質量部を混合して、樹脂組成物X−1を得た。得られた樹脂組成物X−1の30℃における粘度は24100Pa・sであった。また、140℃で2時間硬化した後の樹脂硬化物のガラス転移温度は131℃であり、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−not相当であった。
YD−11の配合量を13質量部に変更し、メラミンシアヌレート(MC−6000、日産化学社製)20質量部を更に混合したこと以外は、比較例X−1と同様にして樹脂組成物X−2を得た。得られた樹脂組成物X−2の30℃における粘度は10600Pa・sであった。また、140℃で2時間硬化した後の樹脂硬化物のガラス転移温度は128℃であり、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−2相当であった。
YP−70及びMC−6000の配合量をそれぞれ5質量部及び0質量部に変更し、ビフェニル構造を有するエポキシ樹脂(NC−3000、日本化薬社製)30質量部を更に混合したこと以外は、比較例X−2と同様にして樹脂組成物X−3を得た。得られた樹脂組成物X−3の30℃における粘度は16600Pa・sであった。また、140℃で2時間硬化した後の樹脂硬化物のガラス転移温度は134℃であり、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−not相当であった。
プリプレグA−1を4枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み0.57mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
プリプレグA−2を4枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み0.43mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
プリプレグA−3を4枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み0.57mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
プリプレグA−4を4枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み0.57mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−1相当であった。
プリプレグA−5を4枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み0.85mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
プリプレグA−2を10枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み1.1mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
プリプレグA−5を3枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み0.67mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−1相当であった。
プリプレグA−2及びプリプレグA−5を、A−2/A−2/A−5/A−2/A−2の順で5枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み0.65mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−0相当であった。
プリプレグX−1を16枚積層し、オートクレーブ中で圧力0.6MPa、140℃×2時間の条件で硬化して、厚み2.4mmの繊維強化複合材料板を得た。得られた繊維強化複合材料板について、UL94燃焼試験と同等の難燃性評価を行ったところ、結果はV−not相当であった。
Claims (8)
- 炭素繊維と、
ビフェニル構造を有するエポキシ樹脂、硬化剤及びメラミンシアヌレートを含有する樹脂組成物と、
を含む、プリプレグ。 - 前記メラミンシアヌレートの含有量が、樹脂組成物の全量基準で20〜40質量%である、請求項1に記載のプリプレグ。
- 前記樹脂組成物中の塩素原子の含有量が1質量%以下である、請求項1又は2に記載のプリプレグ。
- 前記樹脂組成物中のリン原子の含有量が0.1質量%以下である、請求項1〜3のいずれか一項に記載のプリプレグ。
- 複数のプリプレグを積層及び硬化してなる繊維強化複合材料であって、
前記プリプレグの少なくとも一つが、請求項1〜4のいずれか一項に記載のプリプレグである、繊維強化複合材料。 - 積層方向の厚さが1.5mm以下である、請求項5に記載の繊維強化複合材料。
- UL94燃焼試験による難燃性評価がV−0又はV−1である、請求項5に記載の繊維強化複合材料。
- 請求項5〜7のいずれか一項に記載の繊維強化複合材料を含む、成形体。
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CN111344338A (zh) | 2020-06-26 |
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CN111344338B (zh) | 2022-08-23 |
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