CN104919001B - 半芳香族聚酰胺树脂组合物 - Google Patents
半芳香族聚酰胺树脂组合物 Download PDFInfo
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- CN104919001B CN104919001B CN201480004931.7A CN201480004931A CN104919001B CN 104919001 B CN104919001 B CN 104919001B CN 201480004931 A CN201480004931 A CN 201480004931A CN 104919001 B CN104919001 B CN 104919001B
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- semi
- aromatic polyamide
- polyamide resin
- composition
- acid
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- 229920006012 semi-aromatic polyamide Polymers 0.000 title claims abstract description 110
- 239000011342 resin composition Substances 0.000 title claims abstract description 8
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 claims abstract description 41
- -1 aliphatic diamine Chemical class 0.000 claims abstract description 35
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 125000003118 aryl group Chemical group 0.000 claims abstract description 19
- 239000012463 white pigment Substances 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 88
- 229920005989 resin Polymers 0.000 claims description 82
- 239000011347 resin Substances 0.000 claims description 82
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 31
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 24
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 21
- 238000000465 moulding Methods 0.000 claims description 19
- 239000011787 zinc oxide Substances 0.000 claims description 19
- 235000014692 zinc oxide Nutrition 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 8
- 239000000347 magnesium hydroxide Substances 0.000 claims description 7
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 7
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000920 calcium hydroxide Substances 0.000 claims description 6
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 6
- 150000004985 diamines Chemical class 0.000 claims description 5
- 125000001931 aliphatic group Chemical group 0.000 claims description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 2
- 229940116364 hard fat Drugs 0.000 claims description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 claims 1
- 150000004692 metal hydroxides Chemical class 0.000 claims 1
- 239000003963 antioxidant agent Substances 0.000 description 26
- 230000003078 antioxidant effect Effects 0.000 description 26
- 238000000034 method Methods 0.000 description 21
- 238000002347 injection Methods 0.000 description 17
- 239000007924 injection Substances 0.000 description 17
- 229910052757 nitrogen Inorganic materials 0.000 description 15
- 239000000835 fiber Substances 0.000 description 13
- 239000004611 light stabiliser Substances 0.000 description 13
- 239000003365 glass fiber Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- 238000005452 bending Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 150000002148 esters Chemical group 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 238000006116 polymerization reaction Methods 0.000 description 9
- 238000007789 sealing Methods 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 235000021355 Stearic acid Nutrition 0.000 description 7
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical group OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 7
- 239000008117 stearic acid Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 6
- 238000001746 injection moulding Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 5
- 238000007334 copolymerization reaction Methods 0.000 description 5
- 150000001991 dicarboxylic acids Chemical class 0.000 description 5
- 239000006081 fluorescent whitening agent Substances 0.000 description 5
- 229940059574 pentaerithrityl Drugs 0.000 description 5
- 150000002989 phenols Chemical class 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910000077 silane Inorganic materials 0.000 description 5
- 238000005476 soldering Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 5
- 239000005711 Benzoic acid Substances 0.000 description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- 208000037656 Respiratory Sounds Diseases 0.000 description 4
- 235000010233 benzoic acid Nutrition 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical compound NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 4
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 4
- 239000002685 polymerization catalyst Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000012321 sodium triacetoxyborohydride Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910021532 Calcite Inorganic materials 0.000 description 3
- 244000247747 Coptis groenlandica Species 0.000 description 3
- 235000002991 Coptis groenlandica Nutrition 0.000 description 3
- RSJKGSCJYJTIGS-UHFFFAOYSA-N N-undecane Natural products CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical class CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 241000894007 species Species 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 3
- 239000010456 wollastonite Substances 0.000 description 3
- 229910052882 wollastonite Inorganic materials 0.000 description 3
- GXURZKWLMYOCDX-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;dihydroxyphosphanyl dihydrogen phosphite Chemical class OP(O)OP(O)O.OCC(CO)(CO)CO GXURZKWLMYOCDX-UHFFFAOYSA-N 0.000 description 2
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical class CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 description 2
- 235000021357 Behenic acid Nutrition 0.000 description 2
- PWLXTFFHCFWCGG-UHFFFAOYSA-N Heneicosanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCCCCCC(O)=O PWLXTFFHCFWCGG-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000005639 Lauric acid Substances 0.000 description 2
- 235000017858 Laurus nobilis Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical class C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 244000125380 Terminalia tomentosa Species 0.000 description 2
- 235000005212 Terminalia tomentosa Nutrition 0.000 description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 229920013822 aminosilicone Polymers 0.000 description 2
- 150000004984 aromatic diamines Chemical class 0.000 description 2
- 229960000892 attapulgite Drugs 0.000 description 2
- 239000010428 baryte Substances 0.000 description 2
- 229910052601 baryte Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003750 conditioning effect Effects 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- OQRWAMBQGTYSRD-UHFFFAOYSA-N dipotassium;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[K+].[K+].[Ti+4].[Ti+4].[Ti+4].[Ti+4] OQRWAMBQGTYSRD-UHFFFAOYSA-N 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- JFCQEDHGNNZCLN-UHFFFAOYSA-N glutaric acid Chemical compound OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000006872 improvement Effects 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
- 238000004898 kneading Methods 0.000 description 2
- 150000003951 lactams Chemical class 0.000 description 2
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical compound NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 229910052625 palygorskite Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- LGOPTUPXVVNJFH-UHFFFAOYSA-N pentadecanethioic s-acid Chemical class CCCCCCCCCCCCCCC(O)=S LGOPTUPXVVNJFH-UHFFFAOYSA-N 0.000 description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
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- 239000007790 solid phase Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- MHSKRLJMQQNJNC-UHFFFAOYSA-N terephthalamide Chemical compound NC(=O)C1=CC=C(C(N)=O)C=C1 MHSKRLJMQQNJNC-UHFFFAOYSA-N 0.000 description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 2
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- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 description 1
- WIXDSJRJFDWTNY-UHFFFAOYSA-N 1,3-ditert-butyl-5-methylbenzene Chemical compound CC1=CC(C(C)(C)C)=CC(C(C)(C)C)=C1 WIXDSJRJFDWTNY-UHFFFAOYSA-N 0.000 description 1
- OYNOCRWQLLIRON-UHFFFAOYSA-N 1-n,3-n-bis(2,2,6,6-tetramethylpiperidin-4-yl)benzene-1,3-dicarboxamide Chemical compound C1C(C)(C)NC(C)(C)CC1NC(=O)C1=CC=CC(C(=O)NC2CC(C)(C)NC(C)(C)C2)=C1 OYNOCRWQLLIRON-UHFFFAOYSA-N 0.000 description 1
- LNETULKMXZVUST-UHFFFAOYSA-N 1-naphthoic acid Chemical compound C1=CC=C2C(C(=O)O)=CC=CC2=C1 LNETULKMXZVUST-UHFFFAOYSA-N 0.000 description 1
- 150000005210 1-naphthoic acids Chemical class 0.000 description 1
- CBJPRTGKMYOVJO-UHFFFAOYSA-N 1-phenyl-2-(2-phenylethenyl)benzene Chemical group C=1C=CC=CC=1C=CC1=CC=CC=C1C1=CC=CC=C1 CBJPRTGKMYOVJO-UHFFFAOYSA-N 0.000 description 1
- GUOSQNAUYHMCRU-UHFFFAOYSA-N 11-Aminoundecanoic acid Chemical class NCCCCCCCCCCC(O)=O GUOSQNAUYHMCRU-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- 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 description 1
- JFGVTUJBHHZRAB-UHFFFAOYSA-N 2,6-Di-tert-butyl-1,4-benzenediol Chemical class CC(C)(C)C1=CC(O)=CC(C(C)(C)C)=C1O JFGVTUJBHHZRAB-UHFFFAOYSA-N 0.000 description 1
- JLZIIHMTTRXXIN-UHFFFAOYSA-N 2-(2-hydroxy-4-methoxybenzoyl)benzoic acid Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1C(O)=O JLZIIHMTTRXXIN-UHFFFAOYSA-N 0.000 description 1
- ORACIQIJMCYPHQ-MDZDMXLPSA-N 2-[4-[(e)-2-[4-(1,3-benzoxazol-2-yl)phenyl]ethenyl]phenyl]-1,3-benzoxazole Chemical compound C1=CC=C2OC(C3=CC=C(C=C3)/C=C/C=3C=CC(=CC=3)C=3OC4=CC=CC=C4N=3)=NC2=C1 ORACIQIJMCYPHQ-MDZDMXLPSA-N 0.000 description 1
- ZQBLNTCPPVGEST-UHFFFAOYSA-N 2-[[2-[(2-hydroxyphenyl)methylidene]hydrazinyl]methyl]phenol Chemical compound Oc1ccccc1CNN=Cc1ccccc1O ZQBLNTCPPVGEST-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Abstract
一种半芳香族聚酰胺树脂组合物,其特征在于,含有半芳香族聚酰胺(A)100质量份、白色颜料(B)10~150质量份,半芳香族聚酰胺(A)由芳香族二羧酸成分、脂肪族二胺成分和单羧酸成分构成,作为单羧酸成分,含有分子量为140以上的单羧酸,其含量为半芳香族聚酰胺(A)的1~8质量%。
Description
技术领域
本发明涉及耐热性、白度、机械特性以及流动性、耐回焊性、反射性优异的半芳香族聚酰胺树脂组合物。
背景技术
由于发光二极管(LED)是低功耗、长寿命的光源,因此,其作为照明、显示元件的需要迅速放大,且逐渐大型化、高功率化。由于LED能够有效地利用光,因此兼具壳体的反射器是重要的构成部件。对于构成反射器的树脂材料而言,不仅要求优异的白度和反射率,还要求贴装到电子基板时能耐受通常进行的回流焊工序的耐热性(耐回焊性)。
作为适于反射器的树脂材料,已知有含有氧化钛、碳酸钙的半芳香族聚酰胺。例如,专利文献1中公开了一种在聚对苯二甲酰壬二胺(PA9T)中配合氧化钛而成的树脂组合物,专利文献2中公开了一种在聚对苯二甲酰己二胺(PA6T)系或聚对苯二甲酰癸二胺(PA10T)系的共聚树脂中配合氧化钛、碳酸钙以及玻璃纤维而成的树脂组合物。
专利文献1:日本特开2004-75994号公报
专利文献2:日本特开2011-241398号公报
发明内容
然而,由于专利文献1、2的半芳香族聚酰胺树脂组合物的注塑成型时的流动性低,因此,存在如下问题:在注塑成型时薄壁部的填充不足,或模具转印性不良、已成型的反射器的表面的平滑性降低而使反射率降低的问题;耐回焊性降低且产生裂缝(裂纹),或在与透明密封树脂之间发生剥离的问题。
本发明是为了解决上述课题而完成的,其目的在于提供一种不仅耐热性、白度、机械特性优异,而且注塑成型时的流动性、耐回焊性、反射性也优异的半芳香族聚酰胺树脂组合物。
本发明人等为了解决上述课题而进行反复深入研究,结果发现,通过使用具有特定的单羧酸成分的半芳香族聚酰胺,能够实现上述目的,从而完成了本发明。即,本发明的主旨如下。
[1]一种半芳香族聚酰胺树脂组合物,其特征在于,含有半芳香族聚酰胺(A)100质量份和白色颜料(B)10~150质量份,
半芳香族聚酰胺(A)由芳香族二羧酸成分、脂肪族二胺成分和单羧酸成分构成,
作为单羧酸成分,含有分子量为140以上的单羧酸,其含量为半芳香族聚酰胺(A)的1~8质量%。
[2]根据[1]记载的半芳香族聚酰胺树脂组合物,其特征在于,进一步含有10~80质量份的纤维状强化材料(C)。
[3]根据[1]或[2]记载的半芳香族聚酰胺树脂组合物,其特征在于,单羧酸为脂肪族单羧酸。
[4]根据[3]记载的半芳香族聚酰胺树脂组合物,其特征在于,脂肪族单羧酸为硬脂酸。
[5]根据[1]~[4]中任一项记载的半芳香族聚酰胺树脂组合物,其特征在于,脂肪族二胺成分含有1,10-癸二胺。
[6]根据[1]~[5]中任一项记载的半芳香族聚酰胺树脂组合物,其特征在于,白色颜料(B)是选自氧化钛、碳酸钙及硫酸钡中的1种以上。
[7]根据[1]~[6]中任一项记载的半芳香族聚酰胺树脂组合物,其特征在于,进一步含有0.1~30质量份选自氢氧化铝、氢氧化镁及氢氧化钙中的1种以上的金属氢氧化物。
[8]一种反射板,将上述[1]~[7]中任一项记载的半芳香族聚酰胺树脂组合物成型而成。
[9]一种LED封装体,其具备上述[8]记载的反射板。
[10]一种照明装置,其具备上述[9]记载的LED封装体。
根据本发明,可提供一种不仅耐热性、白度、机械特性优异,而且注塑成型时的流动性、耐回焊性、反射性也优异的半芳香族聚酰胺树脂组合物。
附图说明
图1是表示将本发明的树脂组合物用于反射板的表面贴装型LED封装体的截面的示意图。
具体实施方式
以下,详细说明本发明。
本发明的半芳香族聚酰胺树脂组合物含有半芳香族聚酰胺(A)和白色颜料(B),半芳香族聚酰胺(A)由芳香族二羧酸成分和脂肪族二胺成分以及单羧酸成分构成。
本发明中,为了提高耐热性,构成半芳香族聚酰胺(A)的芳香族二羧酸成分优选含有对苯二甲酸。
作为对苯二甲酸以外的芳香族二羧酸,例如,可举出邻苯二甲酸、间苯二甲酸、萘二羧酸。另外,除了芳香族二羧酸成分以外,作为共聚的成分,可举出草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一烷二酸、十二烷二酸等脂肪族二羧酸,环己烷二羧酸等脂环式二羧酸等二羧酸。然而,为了不使半芳香族聚酰胺(A)的耐热性降低,对苯二甲酸以外的芳香族二羧酸、脂肪族二羧酸、脂环式二羧酸的共聚量相对于原料单体的总摩尔数,优选为5摩尔%以下,更优选实质上不含有。
本发明中,作为构成半芳香族聚酰胺(A)的脂肪族二胺成分,例如,可举出1,2-乙二胺、1,3-丙二胺、1,4-丁二胺、1,5-戊二胺、1,6-己二胺、1,7-庚二胺、1,8-辛二胺、1,9-壬二胺、1,10-癸二胺、1,11-十一烷二胺、1,12-十二烷二胺、2-甲基-1,5-戊二胺、2-甲基-1,8-辛二胺。其中,从结晶性增高、白度和反射率提高的角度考虑,优选1,8-癸二胺、1,10-癸二胺、1,12-十二烷二胺,从成型流动性、机械强度的平衡良好的角度考虑,更优选1,10-癸二胺。上述脂肪族二胺成分可以并用多种。
除了脂肪族二胺成分以外,作为共聚的成分,可举出环己烷二胺等脂环式二胺、亚二甲苯二胺、苯二胺等芳香族二胺等二胺成分。然而,由于其会损害由脂肪族二胺成分带来的上述特性,因此脂环式二胺、芳香族二胺的共聚量相对于原料单体的总摩尔数,优选为5摩尔%以下,更优选实质上不含有。
本发明中,半芳香族聚酰胺(A)根据需要可以共聚己内酰胺、月桂内酰胺等内酰胺类、氨基己酸、11-氨基十一烷酸等ω-氨基羧酸。
本发明中,构成半芳香族聚酰胺(A)的单羧酸成分需含有分子量为140以上的单羧酸,优选单羧酸的分子量为170以上。单羧酸的分子量若小于140,则半芳香族聚酰胺树脂(A)的成型流动性的提高效果差,成型时的模具填充性不充分,在得到的LED封装体的反射板中,因回流焊试验时的热量而产生裂缝(裂纹),或在与透明密封树脂之间发生剥离。
作为单羧酸,可举出脂肪族单羧酸、脂环族单羧酸、芳香族单羧酸,其中,从流动性的提高效果高的角度考虑,优选脂肪族单羧酸。
作为分子量为140以上的脂肪族单羧酸,可举出辛酸、壬酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、山萮酸。其中,从通用性高的角度考虑,优选硬脂酸。
作为分子量为140以上的脂环族单羧酸,可举出4-乙基环己烷羧酸、4-己基环己烷羧酸、4-月桂基环己烷羧酸。
作为分子量为140以上的芳香族单羧酸,可举出4-乙基苯甲酸、4-己基苯甲酸、4-月桂基苯甲酸等烷基苯甲酸类、1-萘甲酸、2-萘甲酸等萘甲酸类以及它们的衍生物。
单羧酸成分可以并用多种,例如,可以并用分子量为140以上的单羧酸和分子量小于140的单羧酸。
半芳香族聚酰胺(A)中的分子量为140以上的单羧酸的含量需要为1~8质量%,优选为2~5质量%。如果分子量为140以上的单羧酸的含量小于1质量%,则有时成型流动性降低,成型周期变长,得到的成型体的外观差。另一方面,如果含量超过8质量%,则有时机械强度降低。应予说明,本发明中,单羧酸的含量是指,半芳香族聚酰胺(A)中的单羧酸的残基、即末端基团的羟基从单羧酸脱离之后的单羧酸残基的含量。
一般已知聚合物中存在晶相和非晶相,熔点等结晶特性主要由晶相的状态决定。由于聚合物中的末端基团存在于非晶相,所以熔点不会因末端基团的有无、种类而变化。而且,由于作为封端剂发挥作用的单羧酸成分也存在于非晶相,所以与熔融混炼其他成分时不同,不会因含有单羧酸成分而降低半芳香族聚酰胺的熔点。
本发明中,半芳香族聚酰胺(A)的熔点优选为300℃以上。
另外,本发明中,半芳香族聚酰胺(A)在96%硫酸中、25℃、浓度1g/dL下测定时的相对粘度优选为1.8以上,更优选为1.8~2.6,进一步优选为1.9~2.4。相对粘度小于1.8时,树脂组合物的成型流动性本来就优异,因此不一定需要在本发明中进行的这种流动性改进的手法。应予说明,相对粘度可以作为分子量的指标。
半芳香族聚酰胺(A)可以使用以往已知的加热聚合法、溶液聚合法的方法来制造。其中,从对工业有利这点考虑,优选使用加热聚合法。作为加热聚合法,可举出由下述工序(i)和下述工序(ii)构成的方法,工序(i)是由芳香族二羧酸成分、脂肪族二胺成分和单羧酸成分得到反应物,工序(ii)是将得到的反应物聚合。
作为工序(i),例如,可举出将芳香族二羧酸粉末和单羧酸混合,预先加热至为脂肪族二胺的熔点以上且为芳香族二羧酸的熔点以下的温度,以保持芳香族二羧酸的粉末的状态的方式,在实质上不含水的条件下,向该温度的芳香族二羧酸粉末和单羧酸中添加脂肪族二胺的方法。或者,作为其他的方法,可举出将由熔融状态的脂肪族二胺和固体的芳香族二羧酸构成的悬浮液搅拌混合,得到混合液后,在低于最终生成的半芳香族聚酰胺的熔点的温度下,进行基于芳香族二羧酸、脂肪族二胺和单羧酸的反应的盐的生成反应以及基于生成的盐的聚合的低聚物的生成反应,得到盐和低聚物的混合物的方法。此时,可以边反应边进行粉碎,也可以在反应后暂时取出然后进行粉碎。工序(i)优选容易控制反应物的形状的前者。
作为工序(ii),例如,可举出将工序(i)中得到的反应物在低于最终生成的半芳香族聚酰胺的熔点的温度下固相聚合,使其高分子量化直至达到规定的分子量,得到半芳香族聚酰胺的方法。固相聚合优选在聚合温度180~270℃、反应时间0.5~10小时、氮等非活性气体气流中进行。
作为工序(i)和工序(ii)的反应装置,没有特别限定,使用公知的装置即可。可以用相同的装置实施工序(i)和工序(ii),也可以用不同的装置实施。
另外,作为加热聚合法中的加热的方法,没有特别限定,可举出用水、蒸气、载热油等介质加热反应容器的方法,用电加热器加热反应容器的方法,利用由搅拌产生的搅拌热等伴随内容物的运动所产生的摩擦热的方法。另外,可以组合这些方法。
在半芳香族聚酰胺(A)的制造中,可以使用用于提高聚合效率的聚合催化剂。作为聚合催化剂,可举出磷酸、亚磷酸、次磷酸或者它们的盐,聚合催化剂的添加量通常相对于芳香族二羧酸和脂肪族二胺的总摩尔,优选在2摩尔%以下使用。
作为构成本发明的半芳香族聚酰胺树脂组合物的白色颜料(B),例如,可举出氧化钛、氧化锌、硫化锌、硫酸锌、硫酸钡、碳酸钙、氧化铝,其中,优选氧化钛、硫酸钡、碳酸钙。作为白色颜料,在氧化钛、硫酸钡、碳酸钙中通过并用2种以上,能够提高反射率的保持率。
氧化钛优选折射率高且光稳定性良好的金红石型。氧化钛的粒径优选为0.05~2.0μm,更优选为0.05~0.5μm。作为硫酸钡,可以是天然产出的,也可以是合成品,作为前者,可举出重晶石(Barite),作为后者,可举出沉淀性硫酸钡。硫酸钡的粒径优选为0.005~10μm,更优选为0.01~1μm。作为碳酸钙,例如,可举出方解石(Calcite)、文石(Aragonite)、天然碳酸钙(重质碳酸钙)、合成碳酸钙(沉淀碳酸钙),其中,优选方解石、文石。碳酸钙的粒径优选为0.05~10μm,更优选为0.1~5μm。
为了使其中性化、改善与树脂的润湿性,可以对白色颜料(B)进行表面处理。作为表面处理剂,例如,可举出氧化铝、二氧化硅、氧化锌、氧化锆等金属氧化物、硬脂酸等有机酸或它们的金属盐、多元醇、硅烷偶联剂、钛偶联剂。
白色颜料(B)的含量相对于半芳香族聚酰胺(A)100质量份,需为10~150质量份,优选为20~130质量份,更优选为20~100质量份,进一步优选为30~100质量份。白色颜料(B)的含量小于10质量份时,有白度和反射率降低的情况,并且得到的成型体有时会由于热而变色从而耐回焊性变差。另一方面,含量超过150质量份时,不仅机械强度的加强效率降低,而且熔融混炼时的作业性也降低,很难得到半芳香族聚酰胺树脂组合物的颗粒。
从提高机械强度的观点考虑,本发明的半芳香族聚酰胺树脂组合物可以含有纤维状强化材料(C)。作为纤维状强化材料(C),例如,可举出玻璃纤维、钛酸钾纤维、氧化铝纤维、二氧化硅纤维、氧化锆纤维、碳化硅纤维、陶瓷纤维、硅灰石、海泡石、绿坡缕石。其中,从在半芳香族聚酰胺(A)的熔融温度不熔融且保持白度的方面考虑,优选玻璃纤维、钛酸钾纤维、硅灰石、海泡石、绿坡缕石,优选并用玻璃纤维和钛酸钾纤维、并用玻璃纤维和硅灰石。
玻璃纤维优选用硅烷偶联剂进行表面处理。可以将硅烷偶联剂分散在用于捆扎玻璃纤维的集束剂中进行玻璃纤维的表面处理。作为硅烷偶联剂,例如,可举出乙烯基硅烷系、丙烯酸硅烷系、环氧硅烷系、氨基硅烷系,从易于得到半芳香族聚酰胺(A)与玻璃纤维的密合效果考虑,优选氨基硅烷系。
纤维状强化材料(C)的纤维长优选为0.1~7mm,更优选为0.5~6mm。另外,纤维直径优选为3~20μm,更优选为5~13μm。通过使纤维长为0.1~7mm、纤维直径为3~20μm,能够不对成型性造成负面影响,有效加强。
含有纤维状强化材料(C)时,其含量相对于半芳香族聚酰胺(A)100质量份,优选为10~80质量份,更优选为15~60质量份,进一步优选为20~40质量份。纤维状强化材料(C)的含量为5质量份时,有时得不到机械强度提高的效果。另一方面,超过80质量份时,有时机械强度的加强效率降低,或熔融混炼时的作业性降低,很难得到半芳香族聚酰胺树脂组合物的颗粒。另外,纤维状强化材料在成型体表面浮出,从而反射率降低。
含有纤维状强化材料(C)的方法,只要不损害其加强效果就没有特别限定,优选使用了双轴混炼机的熔融混炼。混炼温度必须为半芳香族聚酰胺(A)的熔点以上,优选小于(熔点+80℃)。若混炼温度小于熔点,则混炼机超负荷,产生弯曲等不良情况。另外,若混炼温度过高,则引起半芳香族聚酰胺(A)的分解、黄变。
本发明的半芳香族聚酰胺树脂组合物进一步含有氢氧化铝、氢氧化镁、氢氧化钙等金属氢氧化物。通过含有金属氢氧化物,能够提高反射率的保持率。应予说明,为了进行中性化、改善与树脂的润湿性,可以对金属氢氧化物进行表面处理。金属氢氧化物的含量相对于半芳香族聚酰胺(A)100质量份,优选为0.1~30质量份,更优选为1~20质量份。
本发明的半芳香族聚酰胺树脂组合物可以进一步含有抗氧化剂。
抗氧化剂通常是以防止半芳香族聚酰胺(A)的分子量降低和褪色为目的而含有。本发明中,除了这些效果以外,还能够提高树脂组合物的滞留稳定性。即,含有纤维状强化材料(C)的半芳香族聚酰胺树脂组合物在高温的料筒内长时间滞留时,纤维状强化材料(C)的表面处理剂会热分解,有时引起机械强度降低。然而,通过含有抗氧化剂,树脂组合物在料筒内长时间滞留时,即,即使是注塑成型时成型周期长的情况、或注射量少而树脂在料筒内长时间滞留的情况,也能够抑制树脂组合物的拉伸强度的降低。
含有抗氧化剂时,其含量相对于半芳香族聚酰胺(A)100质量份优选为0.05~5质量份,进一步优选为0.2~5质量份。含量小于0.05质量份时,上述效果小,若超过5质量份,则成型时模具容易受到污染,有时发生成型不良的情况。
作为抗氧化剂,例如,可举出磷系抗氧化剂、受阻酚系抗氧化剂、受阻胺系抗氧化剂、三嗪系化合物、硫系化合物,其中,优选磷系抗氧化剂、受阻酚系抗氧化剂、硫系化合物。
磷系抗氧化剂可以是无机化合物,也可以是有机化合物。作为磷系抗氧化剂,例如,可举出磷酸二氢钠、磷酸氢二钠、磷酸三钠、亚磷酸钠、亚磷酸钙、亚磷酸镁、亚磷酸锰等无机盐、亚磷酸三苯酯、亚磷酸三(十八烷基)酯、亚磷酸三癸酯、亚磷酸三壬基苯酯、亚磷酸二苯基异癸基酯、双(2,6-二-叔丁基-4-甲基苯基)季戊四醇二亚磷酸酯、三(2,4-二-叔丁基苯基)亚磷酸酯、二硬脂基季戊四醇二亚磷酸酯、双(壬基苯基)季戊四醇二亚磷酸酯、四(2,4-二-叔丁基苯基)-4,4-亚联苯基二亚磷酸酯。其中,优选双(2,6-二-叔丁基-4-甲基苯基)季戊四醇二亚磷酸酯、四(2,4-二-叔丁基苯基)-4,4-亚联苯基二亚磷酸酯。这些可以单独使用,也可以并用。
作为市售的磷系抗氧化剂,例如,可举出Adeka公司制“ADEKA STAB”PEP-8、PEP-36、PEP-4C、Clariant公司制“Hostanox”P-EPQ。
作为受阻酚系抗氧化剂,例如,可举出正十八烷基-3-(3′,5′-二-叔丁基-4′-羟基苯基)-丙酸酯、正十八烷基-3-(3′-甲基-5′-叔丁基-4′-羟基苯基)-丙酸酯、正十四烷基-3-(3′,5′-二-叔丁基-4′-羟基苯基)-丙酸酯、1,6-己二醇-双-[3-(3,5-二-叔丁基-4-羟基苯基)-丙酸酯]、1,4-丁二醇-双-[3-(3,5-二-叔丁基-4-羟基苯基)-丙酸酯]、2,2′-亚甲基双-(4-甲基-叔丁基苯酚)、三乙二醇-双-[3-(3-叔丁基-5-甲基-4-羟基苯基)-丙酸酯]、四[亚甲基-3-(3′,5′-二-叔丁基-4′-羟基苯基)丙酸酯]甲烷、3,9-双[2-{3-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基}-1,1-二甲基乙基]2,4,8,10-四氧杂螺(5,5)十一烷、N,N′-双-3-(3′,5′-二-叔丁基-4′-羟基苯基)丙酰基六亚甲基二胺、N,N′-四亚甲基-双-3-(3′-甲基-5′-叔丁基-4′-羟基苯酚)丙酰基二胺、N,N′-双-[3-(3,5-二-叔丁基-4-羟基苯酚)丙酰基]肼、N-水杨酰基-N′-亚水杨基肼、3-(N-水杨酰基)氨基-1,2,4-三唑、N,N′-双[2-{3-(3,5-二-叔丁基-4-羟基苯基)丙酰氧基}乙基]氧基酰胺、季戊四醇基-四[3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯]、N,N′-六亚甲基双-(3,5-二-叔丁基-4-羟基-氢化肉桂酰胺)。其中,优选三乙二醇-双-[3-(3-叔丁基-5-甲基-4-羟基苯基)-丙酸酯]、四[亚甲基-3-(3′,5′-二-叔丁基-4′-羟基苯基)丙酸酯]甲烷、1,6-己二醇-双-[3-(3,5-二-叔丁基-4-羟基苯基)-丙酸酯]、季戊四醇基-四[3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯]、N,N′-六亚甲基双-(3,5-二-叔丁基-4-羟基-氢化肉桂酰胺)。这些可以单独使用,也可以并用。
作为市售的受阻酚系抗氧化剂,例如,可举出Adeka公司制“ADEKA STAB”AO-20、AO-30、AO-40、AO-50、AO-60、AO-70、AO-80、AO-330,Ciba Specialty Chemicals制“Irganox”245、259、565、1010、1035、1076、1098、1222、1330、1425、1520、3114、5057,住友化学工业公司制“Sumilizer”BHT-R、MDP-S、BBM-S、WX-R、NW、BP-76、BP-101、GA-80、GM、GS,Cyanamid公司制“Cyanox”CY-1790。
作为硫系抗氧化剂,例如,可举出3,3′-硫代二丙酸二硬脂酯、四(3-月桂基硫代丙酸)季戊四醇酯、2-巯基苯并咪唑、3,3′-硫代二丙酸二(十二烷基)酯、3,3′-硫代二丙酸二(十八烷基)酯、3,4′-硫代二丙酸二(十三烷基)酯、2,2-双[[3-(十二烷基硫)-1-氧代丙氧基]甲基]-1,3-丙烷二基酯。其中,优选3,3′-硫代二丙酸二硬脂酯、四(3-月桂基硫代丙酸)季戊四醇酯。它们可以单独使用,也可以并用。
作为市售的硫系抗氧化剂,例如,可举出住友化学工业公司制“Sumilizer”TP-D。
本发明的半芳香族聚酰胺树脂组合物可以进一步含有光稳定剂。特别是使用氧化钛作为白色颜料时,氧化钛会促进光分解,所以优选含有光稳定剂。作为光稳定剂,例如,可举出二苯甲酮系化合物、苯并三唑系化合物、水杨酸酯系化合物、受阻胺系化合物(HALS)、受阻酚系化合物,其中,从与半芳香族聚酰胺的亲和性、耐热性高的角度考虑,优选受阻胺系化合物。
作为市售的光稳定剂,例如,可举出Clariant Japan公司制“Nylostab”S-EED、共同药品公司制“Biosorb”04、Ciba Specialty Chemicals公司制“Tinuvin”622、765、Cytec公司制“Cyasorb”UV-3346、旭电化工业公司制“ADEKA STAB”LA-57、BASF公司制“Chimassorb”119、944。
含有光稳定剂时,其含量相对于半芳香族聚酰胺(A)100质量份优选为0.1~5质量份,进一步优选为0.2~5质量份。通过使光稳定剂的含量为0.1~5质量份,能够提高反射率的保持率。
本发明中,优选并用抗氧化剂和光稳定剂。通过并用抗氧化剂和光稳定剂,能够提高成型时的滞留稳定性,同时有效地防止在使用时因紫外线等引起的光劣化,使反射率和白度提高。
本发明的半芳香族聚酰胺树脂组合物可以进一步含有荧光增白剂。作为荧光增白剂,例如,可举出双苯并唑、双(苯乙烯基)联苯、苯基香豆素(具体而言,三嗪-苯基香豆素、苯并三唑-苯基香豆素以及萘三唑-苯基香豆素)、三嗪-均二苯乙烯。
作为市售的荧光增白剂,例如,可举出Ciba Specialty Chemicals制“TINOPAL”OB、Clariant公司制“Hostanox”KS、Eastman公司制“Eastobrite”OB-1。
本发明的半芳香族聚酰胺树脂组合物可以根据需要添加其它添加剂。作为其它添加剂,例如,可举出板状强化材料、滑石、膨润性粘土矿物、二氧化硅、玻璃珠等填充材料、防静电剂、阻燃剂、阻燃助剂。
在本发明的半芳香族聚酰胺树脂组合物中添加上述纤维状强化材料、白色颜料、抗氧化剂、光稳定剂、荧光增白剂以及其它添加剂的方法,只要不损害其效果就没有特别限定,例如,可举出在半芳香族聚酰胺(A)的聚合时或熔融混炼时添加的方法。
作为将本发明的半芳香族聚酰胺树脂组合物成型的方法,例如,可举出注塑成型法、挤出成型法、吹塑成型法,其中,优选注塑成型法。
作为注塑成型机,没有特别限定,例如,可举出同轴往复螺杆式注射成型机、柱塞式注塑成型机。
在注射成型机的料筒内被加热熔融的半芳香族聚酰胺树脂组合物按每次注射计量,以熔融状态注射到模具内,以规定的形状冷却、固化后,作为成型体从模具取出。注塑成型时的树脂温度需要为半芳香族聚酰胺树脂组合物的熔点以上,优选小于(熔点+100℃)。
应予说明,在半芳香族聚酰胺树脂组合物的加热熔融时,使用的半芳香族聚酰胺树脂组合物优选使用经充分干燥的树脂组合物。如果含有的水分量多,则树脂在注塑成型机的料筒内发泡,难以得到最佳的成型体。注塑成型中使用的半芳香族聚酰胺树脂组合物的水分率优选小于0.3质量%,更优选小于0.1质量%。
另外,构成本发明的树脂组合物的半芳香族聚酰胺(A)与聚酰胺6、聚酰胺66相比,熔点高,用于得到成型体的熔融温度高,因此树脂长时间在成型机料筒内滞留时,上述树脂容易劣化,并容易产生分解气体。因此,为了使本发明的半芳香族聚酰胺树脂组合物成型而得到耐热性优异的成型体,优选缩短成型周期,极力抑制熔融树脂在成型机料筒内的滞留。
本发明的半芳香族聚酰胺树脂组合物不仅机械强度、耐热性、成型性优异,而且白度、反射率、耐回焊性也优异,因此能够在汽车部件、电气电子部件等广范围用途中使用。作为汽车部件,例如,可举出灯反射器、灯壳体、灯延伸区域、灯座的电装系部件。作为电气电子部件,例如,可举出LED封装体的反射板。LED封装体可用于LED照明装置。
实施例
以下,利用实施例对本发明进行具体说明,但本发明不限于这些实施例。
1.测定方法
(1)半芳香族聚酰胺的相对粘度
以96质量%硫酸为溶剂,在浓度1g/dL、25℃下测定。
(2)半芳香族聚酰胺的熔点
使用Perkin Elmer制差示扫描式量热计DSC-7,将以升温速度20℃/分钟升温至350℃后在350℃保持5分钟、以降温速度20℃/分钟降温至25℃、进而在25℃保持5分钟后、再次以升温速度20℃/分钟升温测定时的吸热峰的峰顶设为熔点。
(3)半芳香族聚酰胺的组成
关于半芳香族聚酰胺,进行1H-NMR测定来求得各成分的组成(溶剂:氘代三氟乙酸,温度:25℃)。
(4)半芳香族聚酰胺树脂组合物的熔体流动速率(MFR)
使用半芳香族聚酰胺树脂组合物,按照JIS K7210,在340℃、1.2kgf的负载下测定。实用上,优选1~80g/10分钟,更优选20~70g/10分钟。
(5)半芳香族聚酰胺树脂组合物的弯曲强度、弯曲弹性模量
将半芳香族聚酰胺树脂组合物充分干燥后,使用FANUC制注塑成型机(α-100iA),在树脂温度330℃、模具温度135℃、成型周期25秒的条件下,制作符合ISO标准的试验片,按照ISO178测定弯曲强度、弯曲弹性模量。
实用上,弯曲强度优选为120MPa以上,弯曲弹性模量优选为4.0GPa以上。
(6)半芳香族聚酰胺树脂组合物的白度
将半芳香族聚酰胺树脂组合物充分干燥后,使用NIIGATA MACHINE TECHNO公司制注塑成型机(CND-15AII),在树脂温度330℃、模具温度135℃、成型周期15秒的条件下,制作20mm×20mm×0.5mm的成型片。使用得到的成型片,按照JIS Z8730,利用日本电色公司制分光光度计SE6000(光源:C-2),求得基于亨特色差公式的明度(L值)、红色度(a值)及黄色度(b值),按下述式计算白度W。应予说明,根据标准,使用陶瓷玻璃制的ピトロ白板。
W=100-〔(100-L)2+a2+b2〕1/2
实用上,白度优选90以上。
(7)半芳香族聚酰胺树脂组合物的反射率、加热处理后的反射率的保持率
将上述(6)中得到的成型片在140℃用烘箱加热处理300小时,对处理前后的成型片,利用日本电色公司制分光光度计SE6000(光源:C-2)测定460nm的波长的反射率。
实用上,处理前的反射率优选为85%以上,更优选为90%以上,处理后的反射率优选为60%以上,更优选为70%以上,进一步优选为80%以上。
反射率的保持率使用下式求得。
保持率=([处理后的反射率]/[处理前的反射率])×100
(8)流动长度
使用FANUC公司制注塑成型机S2000i-100B,将料筒温度设定为(熔点+25℃),将模具温度设定为(熔点-185℃)后,在合模力100吨、注射压力120MPa、注射速度80mm/秒、注射时间5秒的条件下,安装单侧1点浇口的专用模具进行成型。专用模具是厚度0.4mm、宽度20mm的L字状的成型品能够采取的形状,流动长最大为150mm。流动长越长,流动性越优异。
(9)耐回焊性
在设置于模具内的导线框架中将半芳香族聚酰胺树脂组合物注塑成型来制作反射板,接着,使用银糊固定作为半导体发光元件的由InGaN系蓝色构成的蓝色LED元件。安装金线,其后,注入透明密封树脂,在150℃加热1小时使其固化,得到图1所示的表面贴装型LED封装体。图1中,1表示反射板、2表示导线框架、3表示金线、4表示透明密封树脂、5表示半导体发光元件。
对得到的20个表面贴装型LED封装体进行JEDEC(电子器件工程联合委员会,JointElectron Device Engineering Council)等级3的吸湿处理(环境条件:在温度60℃、湿度60%下处理50小时),之后,基于JEDECJ-STD-020D,重复2次峰值温度260℃10秒的温度条件下的回流焊试验。回流焊试验后,使用实体显微镜观察LED封装体内的反射板1和透明密封树脂4,按以下的基准进行评价。
次品:反射板1有变色、裂缝(裂纹),或反射板1与透明密封树脂4之间发生剥离。
佳品:反射板1没有变色、裂缝(裂纹),反射板1与透明密封树脂4之间也没有剥离。
计算回流焊试验后的次品率(=(次品的数目/试验中使用的封装体数目)×100(%)),将次品率95%以上设为“◎”、90%以上设为“○”、小于90%设为“×”,来评价耐回焊性。
2.原材料
将使用的原材料在以下示出。
(1)芳香族二羧酸成分
·TPA:对苯二甲酸
·IPA:间苯二甲酸
(2)脂肪族二胺成分
·DDA:1,10-癸二胺
·HMDA:1,6-己二胺
·NDA:1,9-壬二胺
(3)单羧酸
·STA:硬脂酸(分子量:284)
·CP:辛酸(分子量:144)
·LA:月桂酸(分子量:200)
·LBA:4-月桂基苯甲酸(分子量:290)
·BHA:山萮酸(分子量:341)
·CA:己酸(分子量:116)
·BA:苯甲酸(分子量:122)
(4)白色颜料
·TI:氧化钛(石原工业公司制,TIPAQUE PC-3,平均粒径0.21μm)
·BS:硫酸钡(堺化学公司制,BARIFINE BF-20,平均粒径0.03μm)
·CC:碳酸钙(白石工业公司制,Brilliant-1500,平均粒径0.20μm)
(5)纤维状强化材料
·GF-1:玻璃纤维(Nippon Electric Glass公司制,ECS03T-786H,平均纤维直径10.5μm,平均纤维长3mm)
·GF-2:玻璃纤维(日东纺织公司制,CS3J256,平均纤维直径11μm,平均纤维长3mm)
(6)抗氧化剂
·AO-1:双(2,6-二-叔丁基-4-甲基苯基)季戊四醇二亚磷酸酯(磷系抗氧化剂,Adeka公司制,ADEKA STAB PEP-36)
·AO-2:3,9-双[2-{3-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基}-1,1-二甲基乙基]2,4,8,10-四氧杂螺(5,5)十一烷(受阻酚系抗氧化剂,Adeka公司制,AO-80)
·AO-3:四(3-月桂基硫代丙酸)季戊四醇酯(硫系抗氧化剂,住友化学工业公司制,Sumilizer TP-D)
(7)光稳定剂
·LS:2-乙基-2-乙氧基-草酰苯胺(Clariant Japan公司制,Nylostab S-EED)
(8)荧光增白剂
·FB:2,2′-(1,2-亚乙基二基二-4,1-亚苯基)双苯并唑(Eastman公司制,Eastobrite OB-1)
(9)金属氢氧化物
·MH:氢氧化镁(协和化学工业公司制,KISUMA 5E)
制造例1
将作为芳香族二羧酸成分的粉末状的对苯二甲酸(TPA)4.70kg、作为单羧酸的分子量284的硬脂酸(STA)0.32kg和作为聚合催化剂的次磷酸钠一水合物9.3g投入螺带混合式的反应装置中,在氮密闭下,以转速30rpm边搅拌边加热到170℃。其后,将温度保持在170℃,且将转速保持在30rpm,使用注液装置,将作为脂肪族二胺成分的加热到100℃的1,10-癸二胺(DDA)4.98kg用2.5小时连续(连续注液方式)添加,得到反应物。
其后,用相同的反应装置,在氮气流下、250℃、以转速30rpm对得到的反应物加热8小时进行聚合,呈线状牵引出后,通过水槽来冷却固化,将其用造粒机切割而得到颗粒状的半芳香族聚酰胺(P-1)颗粒。
制造例2~17
将各成分的种类、配合量按表1所示的树脂组成进行变更,除此以外,与制造例1同样地得到半芳香族聚酰胺颗粒(P-2~P-17)。
将制造例1~17中得到的半芳香族聚酰胺的组成、熔点、相对粘度在表1中示出。
实施例1
使用Kubota公司制Loss-in-weight式连续定量供给装置CE-W-1向同方向双轴挤出机(东芝机械公司制TEM26SS、螺杆直径26mm、L/D49)的主供给口供给已计量的半芳香族聚酰胺(P-1)100质量份、白色颜料(TI)40质量份、抗氧化剂(AO-1)0.5质量份、光稳定剂(LS)0.5质量份、荧光增白剂(FB)0.1质量份,利用侧进料口供给25质量份纤维状强化材料(GF-1),进行熔融混炼。熔融温度为320℃~340℃,螺杆转速为250rpm,喷出量为35kg/小时。其后,呈线状牵引出后,通过水槽来冷却固化,将其用造粒机切割而得到半芳香族聚酰胺树脂组合物。
实施例2~31、比较例1,3~7
按表2和表3所示的种类、含量变更树脂组成,除此以外,与制造例1同样地得到半芳香族聚酰胺树脂组合物。应予说明,玻璃纤维从侧进料口供给,其他从主供给口供给。
比较例2
变更白色颜料的含量,除此以外,进行与实施例1相同的操作,由于白色颜料的含量高,因此,无法将线束切断而得到半芳香族聚酰胺树脂组合物。
将实施例和比较例中得到的半芳香族聚酰胺树脂组合物的组成及其特性在表2、3中示出。
实施例1~31中,不仅耐热性、白度、弯曲强度、弯曲弹性模量优异,流动性、耐回焊性、反射率也优异。
在并用氧化钛、碳酸钙、硫酸钡中的2种作为白色颜料的实施例26、27中,与仅使用氧化钛的实施例25相比,认为其反射率的保持率提高。另外,在含有金属氢氧化物(氢氧化镁)的实施例31中,与不含有金属氢氧化物的实施例1相比,认为反射率的保持率提高。
由于比较例1的白色颜料的含量少,因此白度、反射率低,且耐回焊性差。
由于比较例3的半芳香族聚酰胺中的单羧酸的含量比本发明中规定的范围少,因此成型流动性降低、流动长短。比较例4的半芳香族聚酰胺中的单羧酸的含量比本发明中规定的范围多,因此弯曲强度低。
比较例5中,作为半芳香族聚酰胺中的单羧酸,使用分子量小于140的己酸,因此成型流动性提高效果差,流动长短。
比较例6中,作为半芳香族聚酰胺中的单羧酸,使用分子量小于140未满的苯甲酸,因此与比较例5同样,流动长短。另外,耐回焊性也差。
比较例7中,增加苯甲酸的含量使用相对粘度下降的半芳香族聚酰胺,结果流动长增长,但耐回焊性仍差。另外,与实施例1相比,单羧酸的含量几乎相同,处理前的反射率低,反射率的保持率也低。
符号说明
1 反射板
2 导线框架
3 金线
4 透明密封树脂
5 半导体发光元件
Claims (14)
1.一种半芳香族聚酰胺树脂组合物,其特征在于,含有100质量份的半芳香族聚酰胺A和10~150质量份的白色颜料B,
半芳香族聚酰胺A由芳香族二羧酸成分、脂肪族二胺成分和单羧酸成分构成,
作为单羧酸成分,含有分子量为140以上的单羧酸,其含量为半芳香族聚酰胺A的1~8质量%。
2.根据权利要求1所述的半芳香族聚酰胺树脂组合物,其特征在于,进一步含有10~80质量份的纤维状强化材料C。
3.根据权利要求1所述的半芳香族聚酰胺树脂组合物,其特征在于,单羧酸为脂肪族单羧酸。
4.根据权利要求3所述的半芳香族聚酰胺树脂组合物,其特征在于,脂肪族单羧酸为硬脂酸。
5.根据权利要求1~4中任一项所述的半芳香族聚酰胺树脂组合物,其特征在于,脂肪族二胺成分含有1,10-癸二胺。
6.根据权利要求1~4中任一项所述的半芳香族聚酰胺树脂组合物,其特征在于,白色颜料B是选自氧化钛、碳酸钙及硫酸钡中的1种以上。
7.根据权利要求5所述的半芳香族聚酰胺树脂组合物,其特征在于,白色颜料B是选自氧化钛、碳酸钙及硫酸钡中的1种以上。
8.根据权利要求1~4中任一项所述的半芳香族聚酰胺树脂组合物,其特征在于,进一步含有0.1~30质量份的选自氢氧化铝、氢氧化镁及氢氧化钙中的1种以上的金属氢氧化物。
9.根据权利要求5所述的半芳香族聚酰胺树脂组合物,其特征在于,进一步含有0.1~30质量份的选自氢氧化铝、氢氧化镁及氢氧化钙中的1种以上的金属氢氧化物。
10.根据权利要求6所述的半芳香族聚酰胺树脂组合物,其特征在于,进一步含有0.1~30质量份的选自氢氧化铝、氢氧化镁及氢氧化钙中的1种以上的金属氢氧化物。
11.根据权利要求7所述的半芳香族聚酰胺树脂组合物,其特征在于,进一步含有0.1~30质量份的选自氢氧化铝、氢氧化镁及氢氧化钙中的1种以上的金属氢氧化物。
12.一种反射板,将权利要求1~11中任一项所述的半芳香族聚酰胺树脂组合物成型而成。
13.一种LED封装体,其具备权利要求12所述的反射板。
14.一种照明装置,其具备权利要求13所述的LED封装体。
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TW201439210A (zh) | 2014-10-16 |
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