JP5706583B2 - 耐熱ポリアミド組成物及びその利用 - Google Patents
耐熱ポリアミド組成物及びその利用 Download PDFInfo
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- JP5706583B2 JP5706583B2 JP2014515019A JP2014515019A JP5706583B2 JP 5706583 B2 JP5706583 B2 JP 5706583B2 JP 2014515019 A JP2014515019 A JP 2014515019A JP 2014515019 A JP2014515019 A JP 2014515019A JP 5706583 B2 JP5706583 B2 JP 5706583B2
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- resistant polyamide
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- polyamide composition
- fiber
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- 239000000203 mixture Substances 0.000 title claims description 32
- 239000004952 Polyamide Substances 0.000 title claims description 26
- 229920002647 polyamide Polymers 0.000 title claims description 26
- 229920006122 polyamide resin Polymers 0.000 claims description 28
- -1 aliphatic diamine Chemical class 0.000 claims description 22
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 16
- 239000003963 antioxidant agent Substances 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- 150000004985 diamines Chemical class 0.000 claims description 11
- 125000003277 amino group Chemical group 0.000 claims description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 10
- 239000003365 glass fiber Substances 0.000 claims description 9
- 239000002557 mineral fiber Substances 0.000 claims description 9
- 239000000835 fiber Substances 0.000 claims description 8
- 239000004611 light stabiliser Substances 0.000 claims description 8
- 239000012764 mineral filler Substances 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 239000010456 wollastonite Substances 0.000 claims description 3
- 229910052882 wollastonite Inorganic materials 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 159000000007 calcium salts Chemical class 0.000 claims description 2
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 229920000587 hyperbranched polymer Polymers 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- YKIBJOMJPMLJTB-UHFFFAOYSA-M sodium;octacosanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCCCCCCCCCCC([O-])=O YKIBJOMJPMLJTB-UHFFFAOYSA-M 0.000 claims description 2
- 150000007970 thio esters Chemical class 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims 1
- 239000012965 benzophenone Substances 0.000 claims 1
- 239000012964 benzotriazole Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 13
- 239000011342 resin composition Substances 0.000 description 10
- 239000000523 sample Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 238000005476 soldering Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical compound NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000012463 white pigment Substances 0.000 description 2
- PWGJDPKCLMLPJW-UHFFFAOYSA-N 1,8-diaminooctane Chemical compound NCCCCCCCCN PWGJDPKCLMLPJW-UHFFFAOYSA-N 0.000 description 1
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- JCUZDQXWVYNXHD-UHFFFAOYSA-N 2,2,4-trimethylhexane-1,6-diamine Chemical compound NCCC(C)CC(C)(C)CN JCUZDQXWVYNXHD-UHFFFAOYSA-N 0.000 description 1
- BTUDGPVTCYNYLK-UHFFFAOYSA-N 2,2-dimethylglutaric acid Chemical compound OC(=O)C(C)(C)CCC(O)=O BTUDGPVTCYNYLK-UHFFFAOYSA-N 0.000 description 1
- KSQSUDDRZLCKSW-UHFFFAOYSA-N 2,4-dimethylhexane-1,6-diamine Chemical compound NCC(C)CC(C)CCN KSQSUDDRZLCKSW-UHFFFAOYSA-N 0.000 description 1
- DNXOCFKTVLHUMU-UHFFFAOYSA-N 2-[4-(carboxymethoxy)phenoxy]acetic acid Chemical compound OC(=O)COC1=CC=C(OCC(O)=O)C=C1 DNXOCFKTVLHUMU-UHFFFAOYSA-N 0.000 description 1
- NWYDEWXSKCTWMJ-UHFFFAOYSA-N 2-methylcyclohexane-1,1-diamine Chemical compound CC1CCCCC1(N)N NWYDEWXSKCTWMJ-UHFFFAOYSA-N 0.000 description 1
- GAGWMWLBYJPFDD-UHFFFAOYSA-N 2-methyloctane-1,8-diamine Chemical compound NCC(C)CCCCCCN GAGWMWLBYJPFDD-UHFFFAOYSA-N 0.000 description 1
- JZUHIOJYCPIVLQ-UHFFFAOYSA-N 2-methylpentane-1,5-diamine Chemical compound NCC(C)CCCN JZUHIOJYCPIVLQ-UHFFFAOYSA-N 0.000 description 1
- 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
- FJSUFIIJYXMJQO-UHFFFAOYSA-N 3-methylpentane-1,5-diamine Chemical compound NCCC(C)CCN FJSUFIIJYXMJQO-UHFFFAOYSA-N 0.000 description 1
- DZIHTWJGPDVSGE-UHFFFAOYSA-N 4-[(4-aminocyclohexyl)methyl]cyclohexan-1-amine Chemical compound C1CC(N)CCC1CC1CCC(N)CC1 DZIHTWJGPDVSGE-UHFFFAOYSA-N 0.000 description 1
- VTDMBRAUHKUOON-UHFFFAOYSA-N 4-[(4-carboxyphenyl)methyl]benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1CC1=CC=C(C(O)=O)C=C1 VTDMBRAUHKUOON-UHFFFAOYSA-N 0.000 description 1
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- MBRGOFWKNLPACT-UHFFFAOYSA-N 5-methylnonane-1,9-diamine Chemical compound NCCCCC(C)CCCCN MBRGOFWKNLPACT-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 150000008366 benzophenones Chemical class 0.000 description 1
- 125000003354 benzotriazolyl group Chemical class N1N=NC2=C1C=CC=C2* 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- YMHQVDAATAEZLO-UHFFFAOYSA-N cyclohexane-1,1-diamine Chemical compound NC1(N)CCCCC1 YMHQVDAATAEZLO-UHFFFAOYSA-N 0.000 description 1
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical compound NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- OREAFAJWWJHCOT-UHFFFAOYSA-N dimethylmalonic acid Chemical compound OC(=O)C(C)(C)C(O)=O OREAFAJWWJHCOT-UHFFFAOYSA-N 0.000 description 1
- QFTYSVGGYOXFRQ-UHFFFAOYSA-N dodecane-1,12-diamine Chemical group NCCCCCCCCCCCCN QFTYSVGGYOXFRQ-UHFFFAOYSA-N 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010101 extrusion blow moulding Methods 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- DIOQZVSQGTUSAI-UHFFFAOYSA-N n-butylhexane Natural products CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- CASUWPDYGGAUQV-UHFFFAOYSA-M potassium;methanol;hydroxide Chemical compound [OH-].[K+].OC CASUWPDYGGAUQV-UHFFFAOYSA-M 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920006012 semi-aromatic polyamide Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K7/08—Oxygen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K7/10—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/58—Optical field-shaping elements
- H01L33/60—Reflective elements
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
)、鉱物繊維A(5〜35%)、鉱物充填材B(14.2〜35%)、光安定剤(0.1〜1%)、流動性改良剤(0.1〜1%)、酸化防止剤(0.1〜1%)を含む耐熱ポリアミド組成物であって、耐熱ポリアミド樹脂は、ジカルボン酸成分ユニットaとジアミン成分ユニットbを含み、ジカルボン酸成分ユニットaが芳香族ジカルボン酸であり、耐熱ポリアミド樹脂中のジカルボン酸成分ユニットaの含有量が25mol%以上であり、ジアミン成分ユニットbは、炭素原子数が4〜20である直鎖脂肪族ジアミン成分ユニット及び/又は分枝鎖脂肪族ジアミン成分ユニット及び/又は脂環式ジアミン成分ユニットを含み、耐熱ポリアミド樹脂は末端アミノ基と末端カルボキシル基との濃度の比値が0.1〜0.71に制御される。
ポリマー0.5gを取り、フェノール45ml及び無水メタノール3mlを、電気熱板上に置かれた100mlのコニカルフラスコに入れて、サンプルが完全に溶解するまで還流し、この混合物を加熱する。チモールブルーを指示薬として使用し、取得した溶液のサンプルを0.01Nの塩酸水溶液で滴定して、末端アミノ基の数量を測定する。
ポリマー0.5gを取り、クレゾール50mlを、電気熱板上に置かれた100mlのコニカルフラスコに入れて、サンプルが完全に溶解するまで還流し、この混合物を加熱し、冷却してから迅速にホルムアルデヒド溶液400μlを入れ、取得した溶液のサンプルを0.1Nの水酸化カリウムのメタノール溶液で滴定して、末端カルボキシル基の数量を測定する。
ポリアミド樹脂0.5gを96.5%濃硫酸溶液50mlに溶解させ、25℃±0.05℃の条件で、ウベローデ粘度計を使用してサンプル溶液の流下時間t1を測定する。更に、ウベローデ粘度計を使用して濃硫酸溶液96.5%の流下時間t2を測定し、下式で相対粘度η相対を算出する。
η相対=t1/t2
PE社製のDSC7を使用して、まず、急速に330℃にサンプルを加熱し、5分間、温度を保ち、10℃/minの速度で温度を50℃まで降下させる。その後、10℃/minの速度で温度を330℃まで上昇させ、吸熱曲線のピーク温度を融点にする。
評価する耐熱ポリアミド組成物の顆粒素材を120℃で4hに乾燥させてから、成形螺旋状サンプルを入れた金型の注射成形機で320℃のバレル温度と120℃の金型温度で素材の顆粒を成形させ、幅5mm、厚さ2.5mmの螺旋状のサンプルを取得し、サンプルの長さを読み取って耐熱ポリアミド組成物の流動性を観察する。サンプルは図1に示す。
機械的特性は、ISO規格に従って測定され、引張りおよび曲げ性能をInstron電子万能試験機により測定し、衝撃強度をZwickアイゾット衝撃試験機により測定する。
評価する耐熱ポリアミド組成物顆粒素材を120℃で4時間、乾燥させてから、成形長さ64mm、幅64mm、厚さ1mmのテストピースを得るために、金型の注射成形機で320℃のバレル温度と120℃の金型温度で素材の顆粒を成形させ、64×64×1mmのテストピースを取得する。テストピースを完全に乾燥させてからテストピースの長さ(L0)を測定する。該テストピースを23℃の水に24時間浸してテストピースの長さ(L1)を測定する。
寸法の安定性(%)=[(L1-L0)/L0]×100
Color-Eye 7000A分光光度計で光学性能のテストを行う。このテストで反射率及びL、a、b値、計算でハンター白色度値Wを取得できる。
W=100−[(100−L)2+a2+b2]1/2
寸法の安定性を測定する際に成形した64mm×64mm×1mmテストピースを、3回、赤外線ウェーブはんだ付装置(SMT)に通過させる。SMTはピーク温度が265℃である。SMTを通過したテストピースをColor-Eye 7000A分光光度計でテストすることにより、SMTを通過した反射率及びハンター白色度値Wを取得できる。
窒素ガス雰囲気下、磁気カップリング・ミキサー、凝縮配管、ガス口、投入口及び圧力防爆口のある20Lの圧力容器に、テレフタル酸3323g(20mol)、デカンジアミン3446g(20mol)、安息香酸73.27g(0.6mol)、次亜リン酸ナトリウム6.77g(原材料の総重量に基づいて0.1wt%として測定)及び脱イオン水2.2Lを入れ、窒素ガスで吹いてから温度を上昇させる。撹拌しながら温度を170℃に上昇させてから脱水を始める。脱水が完了してから再び温度を220℃に上昇させ、反応混合物を220℃で1時間撹拌し、撹拌しながら温度を230℃に上昇させる。温度を230℃に保ち、2.5MPaで続いて2時間、反応させる。反応が完了してから混合物を排出して、相対粘度が1.08であるプレポリマーを取得する。プレポリマーを80℃で真空中において24時間、乾燥させて、260℃窒素ガスの雰囲気で10時間、固相粘着付与を行って、融点が320℃、相対粘度が2.6、末端アミノ基の含有量が75mmol/kg、末端カルボキシル基の含有量が94mmol/kgである耐熱ポリアミド樹脂を取得する。この場合、[アミノ基]/[カルボキシル基]が0.8である。
Claims (7)
- 重量百分率で、耐熱ポリアミド樹脂(40〜90%)、鉱物繊維A(5〜35%)、鉱物充填材B(14.2〜35%)、光安定剤(0.1〜1%)、流動性改良剤(0.1〜1%)、酸化防止剤(0.1〜1%)を含む耐熱ポリアミド組成物であって、
耐熱ポリアミド樹脂は、ジカルボン酸成分ユニットaとジアミン成分ユニットbを含み、前記ジカルボン酸成分ユニットaが芳香族ジカルボン酸であり、耐熱ポリアミド樹脂中の前記ジカルボン酸成分ユニットaの含有量が25mol%以上であり、前記ジアミン成分ユニットbは、炭素原子数が4〜20である直鎖脂肪族ジアミン成分ユニット及び/又は分枝鎖脂肪族ジアミン成分ユニット及び/又は脂環式ジアミン成分ユニットを含み、前記耐熱ポリアミド樹脂の末端アミノ基と末端カルボキシル基との濃度の比値が0.1〜0.71に制御され、
前記耐熱ポリアミド樹脂の相対粘度が2.0〜3.5にあり、融点が少なくとも280℃であり、
前記鉱物繊維Aが円形断面のガラス繊維、非円形断面のガラス繊維、珪灰石繊維、ホウ酸繊維、チタン酸カリウム繊維、炭酸カルシウムのウィスカ又は硫酸バリウムのウィスカからなる群より選ばれる少なくとも1種であり、
前記鉱物充填材Bが、酸化チタン又はナノ酸化亜鉛であり、酸化チタンの粒径が0.2〜0.3μm、ナノ酸化亜鉛の粒径が20〜80nm、ナノ酸化亜鉛の純度が98%以上であることを特徴とする耐熱ポリアミド組成物。 - 前記耐熱ポリアミド樹脂を60〜80%、前記鉱物繊維Aを10〜30%、前記鉱物充填材Bを14.2〜20%、前記光安定剤を0.1〜0.5%、前記流動性改良剤を0.1〜0.5%、及び前記酸化防止剤を0.1〜0.5%含むことを特徴とする請求項1に記載の耐熱ポリアミド組成物。
- 前記鉱物繊維Aが非円形断面のガラス繊維であり、扁平率が2〜6であることを特徴とする請求項1または請求項2に記載の耐熱ポリアミド組成物。
- 前記光安定剤が、ベンゾフェノン化合物、サリチル酸エステル化合物、及びベンゾトリアゾール化合物からなる群より選ばれる少なくとも1種であることを特徴とする請求項1または請求項2に記載の耐熱ポリアミド組成物。
- 前記流動性改良剤が、フッ素を含むポリマー、PEワックス、EBS、モンタン酸ナトリウム塩またはカルシウム塩、及びハイパーブランチポリマーからなる群より選ばれる少なくとも1種であることを特徴とする請求項1または請求項2に記載の耐熱ポリアミド組成物。
- 前記酸化防止剤が、ヒンダードフェノール類酸化防止剤、リン酸エステル類酸化防止剤、及びチオエステル類酸化防止剤からなる群より選ばれる少なくとも1種であることを特徴とする請求項1または請求項2に記載の耐熱ポリアミド組成物。
- LED用反射スタンドの調製に用いられることを特徴とする請求項1または請求項2に記載の耐熱ポリアミド組成物。
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