JP5640747B2 - ガラス繊維強化難燃性ポリアミド樹脂組成物 - Google Patents
ガラス繊維強化難燃性ポリアミド樹脂組成物 Download PDFInfo
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- JP5640747B2 JP5640747B2 JP2010548437A JP2010548437A JP5640747B2 JP 5640747 B2 JP5640747 B2 JP 5640747B2 JP 2010548437 A JP2010548437 A JP 2010548437A JP 2010548437 A JP2010548437 A JP 2010548437A JP 5640747 B2 JP5640747 B2 JP 5640747B2
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- glass fiber
- polyamide resin
- flame retardant
- resin composition
- fiber reinforced
- Prior art date
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- 239000003365 glass fiber Substances 0.000 title claims description 121
- 229920006122 polyamide resin Polymers 0.000 title claims description 89
- 239000003063 flame retardant Substances 0.000 title claims description 64
- 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 title claims description 60
- 239000011342 resin composition Substances 0.000 title claims description 46
- 238000012360 testing method Methods 0.000 claims description 70
- 229920005989 resin Polymers 0.000 claims description 52
- 239000011347 resin Substances 0.000 claims description 52
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 23
- -1 phosphazene compound Chemical class 0.000 claims description 23
- 239000004952 Polyamide Substances 0.000 claims description 20
- 229920002647 polyamide Polymers 0.000 claims description 20
- 238000004898 kneading Methods 0.000 claims description 18
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 17
- 229910052698 phosphorus Inorganic materials 0.000 claims description 17
- 239000011574 phosphorus Substances 0.000 claims description 17
- 229920000877 Melamine resin Polymers 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical class O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 14
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 229920006020 amorphous polyamide Polymers 0.000 claims description 8
- 239000007795 chemical reaction product Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 125000003118 aryl group Chemical group 0.000 claims description 7
- 229920006039 crystalline polyamide Polymers 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- 230000008878 coupling Effects 0.000 claims description 6
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- 238000005859 coupling reaction Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
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- 206010017076 Fracture Diseases 0.000 description 59
- 239000006087 Silane Coupling Agent Substances 0.000 description 19
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 16
- 239000000835 fiber Substances 0.000 description 15
- 125000003277 amino group Chemical group 0.000 description 12
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 12
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 10
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- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 8
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- 125000004432 carbon atom Chemical group C* 0.000 description 6
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- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 description 5
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000806 elastomer Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
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- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 description 3
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- 150000000182 1,3,5-triazines Chemical class 0.000 description 2
- YZEZMSPGIPTEBA-UHFFFAOYSA-N 2-n-(4,6-diamino-1,3,5-triazin-2-yl)-1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(NC=2N=C(N)N=C(N)N=2)=N1 YZEZMSPGIPTEBA-UHFFFAOYSA-N 0.000 description 2
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical class C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical group [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
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- 150000004985 diamines Chemical class 0.000 description 2
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 2
- BEQVQKJCLJBTKZ-UHFFFAOYSA-N diphenylphosphinic acid Chemical compound C=1C=CC=CC=1P(=O)(O)C1=CC=CC=C1 BEQVQKJCLJBTKZ-UHFFFAOYSA-N 0.000 description 2
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- YSRVJVDFHZYRPA-UHFFFAOYSA-N melem Chemical compound NC1=NC(N23)=NC(N)=NC2=NC(N)=NC3=N1 YSRVJVDFHZYRPA-UHFFFAOYSA-N 0.000 description 2
- 239000006082 mold release agent Substances 0.000 description 2
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- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 2
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- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical group CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- MLCHBQKMVKNBOV-UHFFFAOYSA-N phenylphosphinic acid Chemical compound OP(=O)C1=CC=CC=C1 MLCHBQKMVKNBOV-UHFFFAOYSA-N 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- CZQYVJUCYIRDFR-UHFFFAOYSA-N phosphono dihydrogen phosphate;1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(N)=N1.NC1=NC(N)=NC(N)=N1.OP(O)(=O)OP(O)(O)=O CZQYVJUCYIRDFR-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920001955 polyphenylene ether Polymers 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000010998 test method Methods 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
- 150000003852 triazoles Chemical class 0.000 description 1
- KLNPWTHGTVSSEU-UHFFFAOYSA-N undecane-1,11-diamine Chemical compound NCCCCCCCCCCCN KLNPWTHGTVSSEU-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
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- 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
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- 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
- C08J5/10—Reinforcing macromolecular compounds with loose or coherent fibrous material characterised by the additives used in the polymer mixture
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Description
(1)ポリアミド樹脂(A)25〜50重量部及び赤燐以外のリン系難燃剤(B)2〜20重量部に対して偏平度1.5〜8の偏平断面ガラス繊維からなる625℃、0.5hrにおける強熱減量が0.8重量%以下のガラス繊維束(C)30〜70重量部を添加した混合物を溶融混練して得られるガラス繊維強化ポリアミド樹脂組成物であって、前記ポリアミド樹脂が、ポリカプロアミド樹脂(a1)及び/又は前記ポリカプロアミド樹脂(a1)より20℃以上高い融点を有する結晶性ポリアミド樹脂(a2)と、芳香族成分を有する非晶性ポリアミド樹脂(a3)とを((a1)及び/又は(a2))/(a3)=90/10〜35/65の重量比で含むこと、及び前記溶融混練時に前記混合物に対してポリアミド反応性シランカップリング剤(D)が前記ガラス繊維束(C)の0.1〜1.0重量%の割合で添加されることを特徴とするガラス繊維強化難燃性ポリアミド樹脂組成物。
(2)ポリアミド樹脂(A)を100重量%としたときに、ポリカプロアミド樹脂(a1)95〜20重量%、前記ポリカプロアミド樹脂(a1)より20℃以上高い融点を有する結晶性ポリアミド樹脂(a2)0〜80重量%及び芳香族成分を有する非晶性ポリアミド樹脂(a3)5〜50重量%であることを特徴とする(1)に記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
(3)前記ポリカプロアミド樹脂(a1)の96%硫酸溶液における相対粘度が1.2〜2.0でありかつ末端カルボキシル基濃度が70meq/kg以上であることを特徴とする(1)又は(2)に記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
(4)赤燐以外のリン系難燃剤(B)が、ジホスフィン酸金属塩(b1)、メラミンとリン酸からなる反応生成物(b2)、ホスファゼン化合物(b3)及びホスフィン酸誘導体(b4)の中から選ばれる少なくとも1種類であることを特徴とする(1)〜(3)のいずれかに記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
(5)前記ガラス繊維強化難燃性ポリアミド樹脂組成物が、UL94規格V−0(1/32インチ厚)の難燃性を示すこと、及び前記ガラス繊維強化難燃性ポリアミド樹脂組成物のシャルピー衝撃強度試験(ISO 179−1に準拠、切削ノッチ)における試験後の試験片の破断面において、みかけの破断面表面積(SA)/ノッチ部断面積(SB)の面積比が2.2〜4.0であることを特徴とする(1)〜(4)のいずれかに記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
(6)前記シャルピー衝撃強度試験において、シャルピー衝撃強度が18kJ/m2以上であることを特徴とする(5)に記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
ポリアミド樹脂0.25gを96.3%の硫酸25mlに溶解し、この溶液10mlをオズワルド粘度管に入れ、20℃で測定し、以下の式より算出した。
RV=T/T0
RV:相対粘度、T:サンプル溶液の落下時間、T0:溶媒の落下時間
ポリアミド樹脂0.2gにベンジルアルコール10mlを加え、180℃±5℃にて5分間溶解した。この溶液を水中にて15秒間冷却し、フェノールフタレインを指示薬としてエタノール性水酸化カリウム溶液(0.5N−KOH 80mlにエタノールを加え1000mlに調整した)で滴定し、以下の式で算出した。
CEG(meq/kg)={〔(A−B)×N×f〕/(W×1000)}×106
A: 滴定量(ml)
B: 溶媒のブランク滴定量(ml)
N: エタノール性水酸化カリウムの濃度(mol/l)
f: エタノール性水酸化カリウムのファクター
W: 結晶化ポリアミド樹脂の重量(g)
シャルピー衝撃試験で破断した測定試験片をデジタルマイクロスコープ(株式会社 ハイロックス製 KH−7700)を用いて試験片の幅上方から20倍の倍率で撮影し、破断(亀裂)部分の画像をデジタルマイクロスコープver.1.5の解析ソフトを用いて二値化し、得られた投影画像(図3参照)について、約200μ以下の凹凸を無視してノッチ先端からノッチの反対側までの長さを測定する。20倍の拡大率で画面に入りきらない場合は画像を分割して破断面長さを求める。
次いで、破断(亀裂)長さ×シャルピー衝撃試験片の厚みで、みかけの破断面表面積(SA)を算出する。なお、みかけの破断面表面積(SA)は10本の試験片の平均値である。また、ノッチ部断面積(SB)を、ノッチ部幅×試験片厚みで算出する。
そして、みかけの破断面表面積(SA)/ノッチ部断面積(SB)の比を求める。
(a1A)相対粘度(96%硫酸溶液におけるもの、以下同様)RV=1.9のポリアミド6、東洋紡社製「ナイロンT−860」、末端カルボキシル基濃度(CEG)=80、融点225℃
(a1B)相対粘度RV=2.4のポリアミド6、東洋紡社製「ナイロンT−840」、CEG=65、融点225℃
(a2)相対粘度RV=2.4のポリアミド66、東レ社製「アミランE3000F」、CEG=95、融点265℃
(a3A)相対粘度RV=2.0のポリアミド6T6I、エムス社製「グリボリーG21」、CEG=87
(b1)ホスフィン酸アルミニウム塩、クラリアント社製「エクソリットOP1230」
(b2)ポリリン酸メラミン、チバスペシャリティケミカルズ社製「melapur200/70」
(b3)環状フェノキシホスファゼン、大塚化学社製「SPE−100」
(b4)10−ベンジル−10−ヒドロ−9−オキサ−10−ホスファフェナントレン−10−オキシド、三光社製「BCA」
(c1)偏平断面ガラス繊維チョップドストランドとして日東紡社製「CSG3PA820S」、偏平度4、短径7μm、繊維長3mm、625℃×0.5hrの強熱減量0.54重量%
(c2)円形断面ガラス繊維チョップドストランドとしてオーエンスコーニング社製「MAFT2A」、直径13μm、繊維長3mm、625℃×0.5hrの強熱減量0.51重量%
(d1)アミノシランカップリング剤として信越化学社製「KBE903」
(d2)エポキシシランカップリング剤として信越化学社製「KBM403」
離型剤:クラリアント社製、モンタン酸エステルワックス「WE40」
安定剤:チバスペシャリティケミカルズ製「イルガノックスB1171」
表1〜3に示す配合割合で、ポリアミド樹脂(A)及び難燃剤(B)と、他の成分(E)をドライブレンドし、日本製鋼所社製ベント式2軸押出機「TEX44α」(バレル14ブロック構成)を用いてシリンダー温度280℃、スクリュウ回転数300rpmの押出条件で溶融混合し、次いでガラス繊維(C)をサイドフィード方式で供給し溶融混練を行った。カップリング剤を添加する場合は、ガラス繊維(C)の投入直後のブロックから液注添加する方法(I)またはポリアミド樹脂(A)及び難燃性剤(B)と他の成分(E)と一緒にドライブレンドしてメインホッパーから投入する方法(II)のいずれかを採用した。押出機から押出されたストランドは急冷してストランドカッターでペレット化した。得られたペレットを100℃で12時間乾燥した後、射出成形機(東芝機械株式会社製、IS80)でシリンダー温度285℃、金型温度100℃にて各種試験用試験片を成形して評価に供した。評価結果も表1〜3に記した。
Claims (6)
- ポリアミド樹脂(A)25〜50重量部及び赤燐以外のリン系難燃剤(B)2〜20重量部に対して偏平度1.5〜8の偏平断面ガラス繊維からなる625℃、0.5hrにおける強熱減量が0.8重量%以下のガラス繊維束(C)30〜70重量部を添加した混合物を溶融混練して得られるガラス繊維強化ポリアミド樹脂組成物であって、前記ポリアミド樹脂が、ポリカプロアミド樹脂(a1)及び/又は前記ポリカプロアミド樹脂(a1)より20℃以上高い融点を有する結晶性ポリアミド樹脂(a2)と、芳香族成分を有する非晶性ポリアミド樹脂(a3)とを((a1)及び/又は(a2))/(a3)=90/10〜35/65の重量比で含むこと、及び前記溶融混練時に前記混合物に対してポリアミド反応性シランカップリング剤(D)が前記ガラス繊維束(C)の0.1〜1.0重量%の割合で添加されることを特徴とするガラス繊維強化難燃性ポリアミド樹脂組成物。
- ポリアミド樹脂(A)を100重量%としたときに、ポリカプロアミド樹脂(a1)95〜20重量%、前記ポリカプロアミド樹脂(a1)より20℃以上高い融点を有する結晶性ポリアミド樹脂(a2)0〜80重量%及び芳香族成分を有する非晶性ポリアミド樹脂(a3)5〜50重量%であることを特徴とする請求項1に記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
- 前記ポリカプロアミド樹脂(a1)の96%硫酸溶液における相対粘度が1.2〜2.0でありかつ末端カルボキシル基濃度が70meq/kg以上であることを特徴とする請求項1又は2に記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
- 赤燐以外のリン系難燃剤(B)が、ジホスフィン酸金属塩(b1)、メラミンとリン酸からなる反応生成物(b2)、ホスファゼン化合物(b3)及びホスフィン酸誘導体(b4)の中から選ばれる少なくとも1種類であることを特徴とする請求項1〜3のいずれかに記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
- 前記ガラス繊維強化難燃性ポリアミド樹脂組成物が、UL94規格V−0(1/32インチ厚)の難燃性を示すこと、及び前記ガラス繊維強化難燃性ポリアミド樹脂組成物のシャルピー衝撃強度試験(ISO 179−1に準拠、切削ノッチ)における試験後の試験片の破断面において、みかけの破断面表面積(SA)/ノッチ部断面積(SB)の面積比が2.2〜4.0であることを特徴とする請求項1〜4のいずれかに記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
- 前記シャルピー衝撃強度試験において、シャルピー衝撃強度が18kJ/m2以上であることを特徴とする請求項5に記載のガラス繊維強化難燃性ポリアミド樹脂組成物。
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