CN101076562B - 玻璃纤维增强的聚合物组合物 - Google Patents
玻璃纤维增强的聚合物组合物 Download PDFInfo
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- CN101076562B CN101076562B CN2005800424760A CN200580042476A CN101076562B CN 101076562 B CN101076562 B CN 101076562B CN 2005800424760 A CN2005800424760 A CN 2005800424760A CN 200580042476 A CN200580042476 A CN 200580042476A CN 101076562 B CN101076562 B CN 101076562B
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- LNCPIMCVTKXXOY-UHFFFAOYSA-N hexyl 2-methylprop-2-enoate Chemical compound CCCCCCOC(=O)C(C)=C LNCPIMCVTKXXOY-UHFFFAOYSA-N 0.000 description 1
- 229920006017 homo-polyamide Polymers 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
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- 230000007062 hydrolysis Effects 0.000 description 1
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- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
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- 239000011147 inorganic material Substances 0.000 description 1
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- 239000011976 maleic acid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical class CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- OLAPPGSPBNVTRF-UHFFFAOYSA-N naphthalene-1,4,5,8-tetracarboxylic acid Chemical compound C1=CC(C(O)=O)=C2C(C(=O)O)=CC=C(C(O)=O)C2=C1C(O)=O OLAPPGSPBNVTRF-UHFFFAOYSA-N 0.000 description 1
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 description 1
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- 150000002896 organic halogen compounds Chemical class 0.000 description 1
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- 235000006408 oxalic acid Nutrition 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical class [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
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- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
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- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
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- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
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- 239000004814 polyurethane Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 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
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- TUQLLQQWSNWKCF-UHFFFAOYSA-N trimethoxymethylsilane Chemical compound COC([SiH3])(OC)OC TUQLLQQWSNWKCF-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 description 1
- HQUQLFOMPYWACS-UHFFFAOYSA-N tris(2-chloroethyl) phosphate Chemical compound ClCCOP(=O)(OCCCl)OCCCl HQUQLFOMPYWACS-UHFFFAOYSA-N 0.000 description 1
- LIPMRGQQBZJCTM-UHFFFAOYSA-N tris(2-propan-2-ylphenyl) phosphate Chemical compound CC(C)C1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C(C)C)OC1=CC=CC=C1C(C)C LIPMRGQQBZJCTM-UHFFFAOYSA-N 0.000 description 1
- XHGIFBQQEGRTPB-UHFFFAOYSA-N tris(prop-2-enyl) phosphate Chemical compound C=CCOP(=O)(OCC=C)OCC=C XHGIFBQQEGRTPB-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 125000002256 xylenyl group Chemical group C1(C(C=CC=C1)C)(C)* 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
本发明涉及以长玻璃纤维增强的且具有更好机械性能的聚合物组合物,以及由组合物制得的模制体。
Description
本发明涉及以长纤维增强的、具有改善的机械性能的聚合物组合物,以及由该组合物制得的模制体。
DE10232485A1描述了一种制备玻璃纤维和/或碳纤维增强的模制体的方法。提到了将聚酰胺、聚亚烷基对苯二甲酸酯和聚苯硫醚作为热塑性塑料。根据DE10232485A1制备的增强聚酰胺组合物的特点在于有着良好的弯曲应力、弯曲强度和弯曲模量。
玻璃纤维增强的聚碳酸酯模塑组合物同样是已知的。其特点是具有特别的刚度并结合有小的热膨胀性。在实际应用中,在低温下其具有脆的断裂性,这可意味着其应用很有局限或者需要对***件作为昂贵的改造。
本发明的任务在于制备具有卓越机械性能组合,特别是拉伸强度、E-模量和冲击韧性的组合物。
该任务通过向热塑性塑料、特别是共混物中设置长玻璃纤维而得以完成。这种结构部件的特点特别在于其低温下的断裂性能。
因此,本发明的主题在于含有以下组分的组合物:
a)至少一种选自聚酰胺、聚碳酸酯、聚酯碳酸酯、接枝聚合物和共聚物的聚合物,
b)苯乙烯、丙烯腈和马来酸酐的三元聚合物和
c)长玻璃纤维,其中纤维丝的直径为7至25μm。
优选的组合物包括:
A)至少一种选自聚酰胺、聚碳酸酯和聚酯碳酸酯的聚合物,
B)至少一种选自接枝聚合物和共聚物(B.3)的聚合物,
B.4)苯乙烯、丙烯腈和马来酸酐的三元聚合物和
C)长玻璃纤维,其中纤维丝的直径为7至25μm。
在本发明上下文中,术语“长玻璃纤维”和“丝”用作同义词,并且都是表示一种环形头尾相接的(endlose)或者连续的玻璃纤维,而且其在纵向上只是受到丝缠绕于其上的纱筒(Spule)的接受能力的限制。丝的纤维长度通过颗粒的切割长度来确定。
该组合物优选含有30至99、更优选45至95、特别优选50至95、极其优选50至90重量份的成分A),
1至50、优选1至40、更优选3至35、特别优选5至30重量份的成分B),
0.1至10、优选0.3至7、更优选0.5至6、特别优选0.8至4重量%(以A)和B)的重量份的总和计)的三元聚合物B.4,
和3至60、优选3至50、更优选5至40、特别优选7至35和极其优选7至30重量%(以A)和B)的重量份为100计)的成分C。
成分A
适于本发明的成分A的芳族聚碳酸酯和/或芳族聚酯碳酸酯是文献中公开的或者可根据文献中公开的方法制得的那些(为制备芳族聚碳酸酯,可参见,例如,Schnell,“Chemistry and Physics of Polycarbonates”,Interscience Publishers,1964以及DE-AS 1495626,DE-A 2232877,DE-A2703376,DE-A 2714544,DE-A 3000610,DE-A3832396;为制备芳族聚酯碳酸酯例如可参见DE-A 3077934)。
芳族聚碳酸酯可例如通过二酚与碳酰卤、优选碳酰氯和/或与芳族二羧酸二酰卤、优选苯二羧酸二酰卤,根据相界面法且适当时还在使用例如单酚的链终止剂和适当时还在使用三官能或超过三官能的支化剂,例如三酚或四酚的条件下进行反应而制得。
用于制备芳族聚碳酸酯和/或芳族聚酯碳酸酯的双酚优选是具有式(I)的那些,
其中
A可以是单键、C1至C5-亚烷基、C2至C5-烷叉基(Alkyliden)、C5至C6-环烷叉基、-O-、-SO-、-CO-、-S-、-SO2-、C6至C12-亚芳基并且其上可缩合其他芳族的且可任选含有杂原子的环,或者式(II)或(III)的基团
B分别为C1至C12-烷基,优选甲基,卤素,优选氯和/或溴,
x分别相互独立地为0,1或2。
p1或0,且
R5和R6对于每个X1各自为可选的、相互独立地为氢或C1至C6-烷基,优选为氢、甲基或乙基,
X1碳和
m表示4至7的整数,优选为4或5,前提是,在至少一个原子X1上,R5和R6同时为烷基。
优选的二酚是氢醌、间苯二酚、二羟基联苯酚、二-(羟苯基)-C1-C5烷、二-(羟苯基)-C5-C6环烷、二-(羟苯基)醚、二-(羟苯基)-亚砜、二-(羟苯基)酮、二-(羟苯基)砜和α,α-二-(羟苯基)-二异丙基苯以及它们的核上溴代和/或核上氯代的衍生物。
特别优选的二酚是4,4’-二羟基联苯、双酚-A、2,4-二(4-羟苯基)-2-甲基丁烷、1,1-二-(4-羟苯基)-环己烷、1,1-二-(4-羟苯基)-3,3,5-三甲基环己烷、4,4’-二羟基二苯基硫醚、4,4’-二羟基二苯基砜以及它们的二溴代和四溴代的或者氯代的衍生物如2,2-二(3-氯-4-羟苯基)-丙烷、2,2-二-(3,5-二氯-4-羟苯基)-丙烷或2,2-二-(3,5-二溴-4-羟苯基)丙烷。特别优选的是2,2-二-(4-羟苯基)丙烷(双酚-A)。
可以单独或任意混合物的形式使用二酚。二酚是文献中已知的或者可以根据文献中公开的方法制得。
适于热塑性芳族聚碳酸酯制备中的链终止剂是,例如苯酚,对氯代苯酚,对-叔丁基苯酚或2,4,6-三溴苯酚,但也可以是长链的烷基苯酚,如DE-A 2842005中所述的4-[2-(2,4,4-三甲基戊基)]-苯酚或者在烷基取代基中总共具有8至20个C原子的单烷基苯酚或二烷基苯酚,如3,5-二叔丁基苯酚、对-异辛基苯酚、对-叔辛基苯酚、对-十二烷基苯酚和2-(3,5-二甲基庚基)-苯酚和4-(3,5-二甲基庚基)-苯酚。所用链转移剂的量通常为0.5Mol%至10Mol%,以各个所用二酚的摩尔总量计。
热塑性的芳族聚碳酸酯和聚酯碳酸酯具有10000至200000、优选15000至80000的平均重均分子量(Mw,例如通过超离心法或散射光测量法测量)。
热塑性的芳族聚碳酸酯和聚酯碳酸酯可以以已知的方法进行接枝,更确切说是优选通过嵌入相对于所用二酚总量的0.05至2.0Mol%的三官能或超过三官能的化合物,例如具有三个或更多酚基的那些进行。
合适的既有均聚碳酸酯也有共聚碳酸酯。为制备本发明的成分A的共聚碳酸酯,也可以使用1至25重量%、优选2.5至25重量%(以所用二酚的总量计)具有羟基芳氧基端基的聚二有机硅氧烷。它们都是已知的(例如US3419634)或者可根据文献中公开的方法制得。在例如DE-A3334782中记载了含聚二有机硅氧烷的共聚碳酸酯的制备。
优选的聚碳酸酯除了双酚-A均聚碳酸酯外,还有双酚A与相对于二酚摩尔总量计至多15Mol%的其他优选或特别优选所列的二酚,特别是2,2-二(3,5-二溴-4-羟苯基)-丙烷形成的共聚碳酸酯。
用于制备芳族聚酯碳酸酯的芳族二酰二卤,优选是间苯二甲酸、对苯二甲酸、二苯醚-4,4’-二羧酸和萘-2,6-二羧酸的二酰二氯物。
特别优选间苯二酸和对苯二酸的二酰二氯按照1∶20至20∶1的比例组成的混合物。
在制备聚酯碳酸酯时,还可另外结合使用碳酰卤、优选碳酰氯作为二官能的酸衍生物。
除了业已公知的单酚之外,作为制备芳族聚酯碳酸酯中的链终止剂,还可考虑它们的氯代羧酸酯以及可任选被C1至C22烷基或被卤素原子取代的芳族单羧酸的酰氯,以及脂族的C2至C22-单羧酰氯。
链终止剂的量各自为0.1至10Mol%,如果是酚类链终止剂则以二酚的摩尔计并且如果是单羧酰氯链终止剂则以二羧酰二氯的摩尔计。
芳族聚酯碳酸酯也可以含有***的芳族羟基羧酸。
芳族聚酯碳酸酯可以是直链的以及以已知方法接枝的(同样可参见DE-A 2940024和DE-A 3007934)。
作为接枝剂可以使用例如三官能或多官能的羧酰氯,如均苯三酰三氯、三聚氰酰氯、3,3’,4,4’-二苯甲酮-四羧酰四氯、1,4,5,8-萘四羧酰四氯或均苯四酰四氯,且其用量为0.01至1.0Mol%(以所用的二羧酰二氯计),或者三官能或更多官能的酚,如间苯三酚、4,6-二甲基-2,4,6-三-(4-羟苯基)-庚-2-烯、4,6-二甲基-2,4,6-三-(4-羟苯基)-庚烷、1,3,5-三-(4-羟苯基)-苯、1,1,1-三-(4-羟苯基)-乙烷、三-(4-羟苯基)-苯甲烷、2,2-二[4,4-二(4-羟基-苯基)-环己基]-丙烷、2,4-二(4-羟苯基-异丙基)-苯酚、四-(4-羟苯基)-甲烷、2,6-二(2-羟基-5-甲基-苄基)-4-甲基-苯酚、2-(4-羟苯基)-2-(2,4-二羟苯基)-丙烷、四-(4-[4-羟苯基-异丙基]-苯氧基)-甲烷、1,4-二[(4,4’-二羟基三苯基)-甲基]-苯,且其用量为以所用双酚的量计0.01至1.0Mol%。酚类接枝剂可以与二酚一起预先置入反应器中,酰氯-接枝剂可以与酰二氯一起引入。
在热塑性芳族聚酯碳酸酯中,碳酸酯结构单元得含量可以任意变化。优选碳酸酯基团的含量为多至80Mol%、更优选多至50Mol%,以酯基和碳酸酯基团的总和计。芳族聚酯碳酸酯的酯和碳酸酯成分可以嵌段或无规形式分布于缩聚物中。
适于本发明的聚酰胺是已知的或者可根据文献中公开的方法制备得到。
适于本发明的聚酰胺是已知的均聚酰胺、共聚酰胺和这些聚酰胺的混合物。其可以是部分结晶和/或无定形的聚酰胺。适合作为部分结晶聚酰胺的是聚酰胺-6、聚酰胺-6,6、这些成分的混合物和相应共聚物。此外,还可考虑以下的部分结晶的聚酰胺,即其酸成分完全或部分地由对苯二甲酸和/或间苯二甲酸和/或辛二酸和/或癸二酸和/或壬二酸和/或己二酸和/或环己二酸组成,且其二胺成分完全或部分地由间-和/或对-亚二甲苯基二胺和/或六亚甲基二胺和/或2,2,4-三甲基六亚甲基二胺和/或2,4,4-三甲基六亚甲基二胺和/或异佛乐酮二胺组成,并且它们的组成都是原则上已知的。
另外值得一提的聚酰胺还是完全或部分地由环中具有7至12个碳原子的内酰胺,且适当时还在并用一种或多种上述原料成分的条件下制备得到的那些。
特别优选的部分结晶聚酰胺时聚酰胺-6和聚酰胺-6,6及其混合物。用作无定形聚酰胺的可以是已知产品。它们通过诸如乙二胺、六亚甲基二胺、十亚甲基二胺、2,2,4-和/或2,4,4-三甲基六亚甲基二胺、间-和/或对-亚二甲苯基二胺、二-(4-氨基环己基)-甲烷、二-(4-氨基环己基)-丙烷、3,3’-二甲基-4,4’-二氨基-二环己基-甲烷、3-氨甲基-3,5,5-三甲基环己胺、2,5-和/或2,6-二-(氨甲基)-降莰烷和/或1,4-二氨甲基环己烷的二胺,与诸如草酸、己二酸、壬二酸、癸二酸、十七烷基二酸、2,2,4-和/或2,4,4-三甲基己二酸、间苯二甲酸和对苯二甲酸的二羧酸进行的缩合反应而制得。
适合的还有通过多种单体的缩聚而得到的共聚物,还有含有ε-氨基己酸、ω-氨基十一烷酸、ω-氨基月桂酸或它们的内酰胺。
特别合适的无定形聚酰胺是由间苯二甲酸、六亚甲基二胺和其他二胺如4,4-二氨基二环己基甲烷、异佛乐酮二胺、2,2,4-和/或2,4,4-三甲基六亚甲基二胺、2,5-和/或2,6-二-(氨甲基)-降冰片烯制得;或者由间苯二甲酸、44,’-二氨基-二环己基甲烷和ε-己内酰胺制得;或者由间苯二甲酸、3,3’-二甲基-4,4’-二氨基二环己基甲烷和月桂内酰胺制得;或者由对苯二甲酸与由2,2,4-和/或2,4,4-三甲基六亚甲基二胺组成的异构体混合物制得。
也可使用位置异构的二胺二环己醛甲烷(Diamindicyclohexalmethane)的混合物代替纯的4,4’-二氨基二环己基甲烷,且它们由以下成分组成
70至99mol%的4,4’-二氨基-异构体,
1至30mol%的2,4’-二氨基-异构体和
0至2mol%的2,2’-二氨基-异构体,
任选的相应更高程度缩合的二胺,且它们是通过氢化工业品质的二氨基二苯基甲烷而获得的。间苯二甲酸可以有不超过30%被对苯二甲酸取代。
聚酰胺优选具有2.0至5.0、特别优选2.5至4.0的相对粘度(25℃下于1重量%的间甲酚溶液中测得)。
成分A中可以含有单独或相互之间任意混合物形式的聚酰胺。
成分B
成分B包括一种或多种以下形成的接枝聚合物,
B.1 5至95、优选30至90重量%的至少一种乙烯基单体接枝于
B.2 95至5、优选70至10重量%的一种或多种玻璃化转变温度<10℃、优选<0℃、特别优选<-20℃的接枝基体之上。
接枝基体B.2通常具有0.05至10μm、优选0.1至5μm、特别优选0.2至1μm的平均粒径。
单体B.1优选是以下组分的混合物
B.1.1 50至99重量份的乙烯基芳族化物和/或核取代的乙烯基芳族化物(如苯乙烯、α-甲基苯乙烯、对甲基苯乙烯、对氯代苯乙烯)和/或甲基丙烯酸-(C1-C8)-烷基酯(如甲基丙烯酸甲酯、甲基丙烯酸乙酯)和
B.1.2 1至50重量份的乙烯基氰化物(不饱和腈,如丙烯腈和甲基丙烯腈)和/或(甲基)丙烯酸-(C1-C8)-烷基酯(如甲基丙烯酸甲酯、丙烯酸正丁酯、丙烯酸叔丁酯)和/或不饱和羧酸的衍生物(如酸酐和酰亚胺)(例如马来酸酐和N-苯基-马来酰亚胺)。
优选单体B.1.1选自单体苯乙烯、α-甲基苯乙烯和甲基丙烯酸甲酯中的至少一种,优选单体B.1.2选自单体丙烯腈、马来酸酐和甲基丙烯酸甲酯中的至少一种。
特别优选单体B.1.1是苯乙烯而B.1.2是丙烯腈。
适用于接枝聚合物B的接枝基体B.2是例如二烯橡胶,EP(D)M-橡胶,也即基于乙烯/丙烯和任选的二烯烃的那些,丙烯酸酯-,聚氨酯-,硅酮-,氯丁二烯和乙烯/醋酸乙烯酯-橡胶。
优选的接枝基体B.2是二烯橡胶(例如基于丁二烯、异戊二烯等)或二烯橡胶的混合物或者二烯橡胶或它们的混合物与其他可共聚单体(例如B.1.1和B.1.2中所述的那些)的共聚物,前提是,成分B.2的玻璃化转变温度低于<10℃、优选<0℃、特别优选<-10℃。
特别优选的是纯聚丁二烯橡胶。
特别优选的聚合物B是比如ABS-聚合物(乳液-、本体-和悬浮-ABS),例如在DE-A2035390(=US-PS3644574)或在DE-A2248242(=GB-PS1409275)中或在Ulmanns,Enzyklopdie derTechnischen Chemie,第19卷(1980),280页及其后中所记载的那些。接枝基体B.2的凝胶含量为至少30重量%,优选至少40重量%(在甲苯中测得)。
接枝共聚物B通过自由基聚合,例如通过乳液-、悬浮-、溶液-或本体聚合,优选通过乳液或本体聚合而制得。
特别合适的接枝橡胶还有通过如US-P4937285中所述的用由有机氢过氧化物和抗坏血酸组成的引发体系来引发氧化还原而制得的ABS-聚合物。
合适的聚合物B的B.2的丙烯酸酯橡胶优选是由丙烯酸烷基酯任选地与以B.2计不超过40重量%的其他可聚合烯属不饱和单体形成的聚合物。属于优选的可聚合丙烯酸酯的是C1-C8-烷基酯,例如甲基-、乙基-、丁基-、正辛基-和2-乙基己基酯;卤代烷基酯,优选是卤代C1-C8烷基酯,如氯乙基丙烯酸酯以及这些单体的混合物。
为交联可以使具有一个以上可聚合双键的单体共聚合。优选交联单体的例子是具有3至8个C原子的不饱和单羧酸与具有3至12个C原子的不饱和一元醇或者与例如二甲基丙烯酸乙二醇酯、甲基丙烯酸烯丙基酯的具有2至4个OH基团和2至20个C原子的不饱和多元醇形成的酯;例如三乙烯基和三烯丙基氰脲酸酯的多不饱和的杂环化合物;多官能的乙烯基化合物,如二乙烯基苯和三乙烯基苯;但也可以是三烯丙基磷酸酯和二烯丙基邻苯二甲酸酯。
优选交联的单体是甲基丙烯酸烯丙基酯、二甲基丙烯酸乙二醇酯、邻苯二甲酸二烯丙基酯和具有至少三个烯属不饱和基团的杂环化合物。
特别优选交联的单体是环状单体三烯丙基氰脲酸酯、三烯丙基异氰脲酸酯、三丙烯酰六氢-s-三嗪、三烯丙基苯。交联单体的量为优选0.02至5、特别是0.05至2重量%,以接枝基体B.2计。
对于具有至少三个烯属不饱和基团的环状交联单体,优选将用量限制于接枝基体B.2的1重量%以下。
优选的“其他”除了丙烯酸酯外还可任选用于制备接枝基体B.2的可聚合烯属不饱和单体是诸如丙烯腈、苯乙烯、α-甲基苯乙烯、丙烯酰胺、乙烯基-C1-C6烷基醚、甲基丙烯酸甲酯、丁二烯。优选的作为接枝基体B.2的丙烯酸酯橡胶是具有至少60重量%含量的乳液聚合物。
其他合适的B.2的接枝基体是具有接枝活性点位的硅酮橡胶,例如记载在DE-A3704657、DE-A3704655、DE-A3631540和DE-A3631539中的那些。
作为合适的硅酮丙烯酸酯橡胶可以使用其的制备记载于JP08259791-A、JP07316409-A和EP-A0315035中的那些。这些申请的与此相关的内容也引入本申请中。
硅酮丙烯酸酯-复合橡胶中的聚有机硅氧烷成分可以通过有机硅氧烷和多官能交联剂在乳液聚合过程中的反应而制得。另外还可以通过添加合适的不饱和有机硅氧烷而在橡胶中接入接枝活性的位点。
通常,有机硅氧烷是环状的,且其中的环结构优选含有3至6个Si原子。值得一提的例子是六甲基环三硅氧烷、八甲基环四硅氧烷、十甲基环五硅氧烷、十二甲基环六硅氧烷,三甲基三苯基环三硅氧烷,四甲基四苯基环四硅氧烷,八苯基环四硅氧烷,并且它们也可以单独或以2种或更多种化合物混合的形式使用。有机硅氧烷成分应该在硅酮丙烯酸酯橡胶中的硅酮成分结构上占有至少50重量%、优选至少70重量%,以硅酮丙烯酸酯橡胶中的硅酮成分计。
作为交联剂,通常使用3-或4-官能的硅烷化合物。值得一提的此类特别优选的例子是:三甲氧基甲基硅烷、三乙氧基苯基硅烷、四甲氧基硅烷、四乙氧基硅烷、四-正丙氧基硅烷、四丁氧基硅烷。4官能的接枝剂,特别优选是四乙氧基硅烷。接枝剂的量通常为0至30重量%(以硅酮丙烯酸酯橡胶中的聚有机硅氧烷成分计)。
为在硅酮丙烯酸酯橡胶的聚有机硅氧烷成分中引入接枝活性的位点,可以优选使用构成如下一种结构的化合物:
其中,
R5甲基、乙基、丙基或苯基,
R6氢或甲基,
n为0,1或2且
p1至6的数。
(甲基)丙烯酰氧基硅烷是优选的构成结构(GI-1)的化合物。优选的(甲基)丙烯酰氧基硅烷是诸如β-甲基丙烯酰氧基乙基-二甲氧基-甲基硅烷、γ-甲基丙烯酰氧基-丙基甲氧基-三甲基-硅烷、γ-甲基丙烯酰氧基丙基-二甲氧基-甲基-硅烷、γ-甲基丙烯酰氧基丙基-三甲氧基-硅烷、γ-甲基丙烯酰氧基-丙基-乙氧基-二乙基硅烷、γ-甲基丙烯酰氧基丙基-二乙氧基-甲基-硅烷、γ-甲基丙烯酰氧基-丁基-二乙氧基-甲基-硅烷。
乙烯基硅氧烷、特别是四甲基-四乙烯基-环四硅氧烷能够构成结构GI-2。
例如对乙烯基苯基-二甲氧基-甲基硅烷可以构成结构GI-3。γ-巯基丙基二甲氧基-甲基硅烷、γ-巯基丙基甲氧基-二甲基硅烷、γ-巯基丙基二乙氧基甲基硅烷等可以构成结构(GI-4)。
这些化合物的量为0至10重量%、优选0.5至5重量%(以聚有机硅氧烷成分计)。
硅酮丙烯酸酯-复合橡胶中的丙烯酸酯成分可以由(甲基)丙烯酸烷基酯、交联剂和接枝活性的单体单元制得。
作为(甲基)丙烯酸烷基酯例如且优选值得一提的是丙烯酸烷基酯,如丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯、丙烯酸正丁酯、丙烯酸2-乙基己基酯,和甲基丙烯酸烷基酯,如甲基丙烯酸己酯、甲基丙烯酸2-乙基己基酯、甲基丙烯酸正月桂基酯,且特别优选为丙烯酸正丁酯。
作为交联剂可以使用多官能的化合物。值得一提的例子是:二甲基丙烯酸乙二醇酯、二甲基丙烯酸丙二醇酯、二甲基丙烯酸1,3-丁二醇酯和二甲基丙烯酸1,4-丁二醇酯。
为接入接枝活性的位点可以单独或混合物形式使用诸如以下化合物:甲基丙烯酸烯丙基酯、氰脲酸三烯丙基酯、异氰脲酸三烯丙基酯、甲基丙烯酸烯丙基酯。甲基丙烯酸烯丙基酯还可以起到交联剂的作用。这些化合物用量为0.1至20重量%,以硅酮丙烯酸酯-复合橡胶中的丙烯酸酯橡胶成分计。
制备优选用于本发明组合物中的硅酮丙烯酸酯复合橡胶的方法以及它们的单体接枝过程记载在例如,US-A4888388、JP08259791A2、JP07316409A和EP-A0315035中。作为接枝聚合物B的接枝基体B.2,可以考虑那些它们的硅酮和丙烯酸酯成分构成核壳结构的硅酮丙烯酸酯-复合橡胶,以及还有构成网络且在其中丙烯酸酯和硅酮成分完全相互贯穿(“互穿网络”)的那些。
在前述接枝基体上的接枝聚合过程可以以悬浮液、分散液或乳液的形式进行。优选的是连续或非连续的乳液聚合过程。这些接枝聚合过程都以自由基引发剂进行(例如过氧化物、偶氮化合物、过氧化氢、过硫酸盐(Persulfaten)、过磷酸盐(Perphosphaten))且适当时还使用阴离子乳化剂,如碳氧盐(Carboxoniumsalzen)、磺酸盐或有机硫酸盐。其中,会以较高的接枝率形成接枝聚合物,即在橡胶上会化学连接上大量的接枝单体的聚合物。
对于接枝壳体B.1的结构可以优选使用下述成分的混合物
B.1.1 0至80重量%、优选0至50重量%、特别优选0至25重量%(以接枝壳体计)的乙烯基芳族化物或核取代的乙烯基芳族化物(例如苯乙烯、α-甲基苯乙烯、对甲基苯乙烯)、乙烯基氰化物(不饱和的腈,如丙烯腈和甲基丙烯腈)和
B.1.2 100至20重量%、优选100至50重量%、特别优选100至75重量%(以接枝壳体计)的选自(甲基)丙烯酸(C1-C8)烷基酯(如甲基丙烯酸甲酯、丙烯酸正丁酯、丙烯酸叔丁酯)和不饱和羧酸衍生物(如酸酐和酰亚胺)(如马来酸酐和N-苯基-马来酰亚胺)的单体。
特别优选接枝壳由一种纯的(甲基)丙烯酸-(C1-C8)烷基酯组成或由多种纯的(甲基)丙烯酸-(C1-C8)烷基酯的混合物组成,特别优选由纯的甲基丙烯酸甲酯组成。
接枝基体B.2的凝胶含量在25℃下于一种合适的溶剂中确定(M.Hoffmann,H.Krmer,R.Kuhn,Polymeranalytik I und II,GeorgThieme-出版社,斯图加特1977)。
平均粒径d50是分别有50重量%的颗粒高于和低于该值的直径。利用超离心测量法(W.Scholtan,H.Lange,Kolloid,Z.und Z.Polymer250(1972),782-1796)可以来测定该值。
另外,成分B可以包括一种或多种热塑性的乙烯基(共)聚合物B.3。
适合作为乙烯基(共)聚合物B.3的是由至少一种选自乙烯基芳族化物、乙烯基氰化物(不饱和腈)、(甲基)丙烯酸-(C1-C8)烷基酯、不饱和的羧酸以及不饱和羧酸衍生物(如酸酐和酰亚胺)的单体形成的聚合物。特别合适的是由以下成分构成的(共)聚合物:
B.3.1 50至99、优选60至80重量份的乙烯基芳族化物和/或核取代的乙烯基芳族化物(例如苯乙烯、α-甲基苯乙烯、对甲基苯乙烯、对氯代苯乙烯)和/或甲基丙烯酸-(C1-C8)烷基酯(如甲基丙烯酸甲酯、甲基丙烯酸乙酯),和
B.3.2 1至50、优选20至40重量份的乙烯基氰化物(不饱和腈)如丙烯腈和甲基丙烯腈和/或(甲基)丙烯酸-(C1-C8)烷基酯(如甲基丙烯酸甲酯、丙烯酸正丁酯、丙烯酸叔丁酯)和/或不饱和的羧酸(如马来酸)和/或不饱和羧酸的衍生物(如酸酐和酰亚胺)(例如马来酸酐和N-苯基-马来酰亚胺)。
(共)聚合物B.3是树脂状、热塑性和不含橡胶的。
特别优选共聚物由B.3.1的苯乙烯和B.3.2的丙烯腈构成。
还特别优选的是苯乙烯、丙烯腈和马来酸酐的三元共聚物B.4。三元聚合物中的马来酸酐含量通常为0.2至5、优选0.1至1.5Mol%(也可参见EP-A785234)。优选讲三元聚合物用作相容介质。组合物通常含有0.1至10、优选0.3至7、更优选0.5至6、特别优选0.8至4重量%(以A和B计)的三元聚合物B.4。
B.3的(共)聚合物是已知的并且可通过自由基聚合反应得到,特别是通过乳液、悬浮、溶液或本体聚合制得。(共)聚合物优选具有15000至200000之间的平均分子量Mw(重均,通过光散射法或沉降法计算得到)。
成分C
用作成分C的是长玻璃纤维,其是环形头尾相接的(endlose)或者连续的玻璃纤维,而且其在纵向上只是受到丝线缠绕于其上的纱筒的接受能力的限制。热塑性颗粒中的最终纤维长度通过颗粒的剪切长度来确定,即颗粒的剪切长度为5至50mm、优选5至30mm、特别优选7至25mm(术语“颗粒”在上下文中表示塑料球粒。可商购得的颗粒是含有或者不含添加剂的热塑性组合物的常规形式)。一般而言,纤维丝具有7至25、优选7至21微米的直径。
长玻璃纤维可以用一种所谓的浆液来进行表面改性并且它们被浸泡或浸渍于所用的热塑性塑料或热塑性塑料共混物中。为保证在所得含有玻璃纤维的颗粒中且尤其是在由此制得的部件中有着良好的机械性能,应实现尽可能良好的润湿或浸渍过程。浸渍技术记载在例如WO95/28266和US6530246B1中。
组合物可以含有其他添加剂(成分D)。因此其可以通过添加合适的添加剂而赋予阻燃性(特别是基于聚碳酸酯的组合物)。值得一提的阻燃剂例子是卤代化合物,特别是基于含有氯和溴以及磷的化合物的那些。
优选组合物中含有选自单和低聚磷酸酯和膦酸酯、膦酸酯胺和膦腈的含磷阻燃剂,并且其中也可以使用选自这些化合物中一种或不同的多个成分组成的混合物作为阻燃剂。这里没有详细提及的其他一些磷化合物也可以单独或与其他阻燃剂任意组合地进行使用。
优选的单和低聚磷酸酯或膦酸酯是具有通式(IV)的磷化合物,
其中,
R1,R2,R3和R4相互独立地分别为任选卤代的C1至C8-烷基,各自任选被优选是C1至C4-烷基的烷基和/或优选为氯、溴的卤素取代的C5至C6-环烷基、C6至C20芳基或C7至C12芳烷基,
n相互独立地为0或1
q为0至30且
X表示具有6至30个C原子的单核或多核芳基,或者具有2至30个C原子的直链或支链脂族基,且其可被OH取代并且含有至多过8个醚键。
优选R1,R2,R3和R4相互独立地表示C1至C4-烷基、苯基、萘基或苯基-C1-C4-烷基。芳基R1,R2,R3和R4可以本身为卤素和/或烷基,优选氯、溴和/或C1至C4-烷基取代。特别优选芳基是甲苯基、苯基、二甲苯基、丙苯基或丁苯基以及相应的它们的溴代和氯代衍生物。
X在式(IV)中优选表示具有6至30个C原子的单核或多核芳基。其优选衍生自式(I)的二酚。
n在式(IV)中可以相互独立地为0或1,优选n等于1。
q表示0至30的值。式(IV)成分可以以混合物形式存在,q值数均值为0.3至20,优选0.5至10,特别优选0.5至6。
X特别优选表示
或者它们的氯代或溴代衍生物,优选X衍生自间苯二酚、氢醌、双酚A或二苯基苯酚。特别优选X衍生自双酚A。
组合物含有通常以(100份A)和B))计的0.5至25、优选1至20重量%的阻燃剂。
特别优选使用式(IV)的衍生自双酚A的低聚磷酸酯,因为配有这种磷化合物的组合物有着极高的耐应力断裂性和耐水解性以及特别小的在浇铸加工时形成附着层的倾向。此外,以这类阻燃剂也能获得极高的耐热变形性。
式(IV)的单磷化合物特别是三丁基磷酸酯、三-(2-氯乙基)-磷酸酯、三-(2,3-二溴丙基)-磷酸酯、三苯基磷酸酯、三甲苯基磷酸酯、二苯基甲苯基磷酸酯、二苯基辛基磷酸酯、二苯基-2-乙基甲苯基磷酸酯、三-(异丙基苯基)-磷酸酯、卤代芳基磷酸酯、甲基磷酸二甲酯、甲基膦酸二苯酯(Methylphosphensurediphenylester)、苯基磷酸二乙酯、三苯基氧化膦或三甲苯基氧化膦。
具有式(IV)的成分D的磷化合物是已知的(参见例如EP-A0363608,EP-A0640655)或者可根据已知方法类似地制得(例如UllmannEnzyklopdie der technischen Chemie,第18卷,301页及其后,1979;Houben-Weyl,Methoden der organischen Chemie,12/1卷,第43页;Beilstein第6卷,第177页)。
通过以合适的方法(气相色谱法(GC),高压液体色谱法(HPLC),凝胶渗透色谱法(GPC))来确定磷酸酯混合物的组成并由此为q计算出平均值,从而可以确定q的平均值。
作为其他的阻燃剂可以值得一提的是有机卤代化合物,如十溴二苯基醚、四溴双酚,无机卤代化合物,如溴化铵,氮化合物,如蜜胺、蜜胺甲醛树脂,无机氢氧化物,如Mg-、Al-氢氧化物,无机化合物,如氧化锑、偏硼酸钡、羟基锑酸盐(Hydroxoantimonat)、氧化锆、氢氧化锆、氧化钼、钼酸铵、硼酸锌、硼酸铵、偏硼酸钡、滑石、硅酸盐、氧化硅和氧化锡以及硅氧烷化合物。
阻燃剂经常结合所谓的抗滴剂使用,该抗滴剂可在燃烧时减小材料燃烧低落的趋势。这里值得一提的例子是选自氟代聚烯烃、硅酮以及芳族聚酰胺纤维的物质类化合物。它们也可用于本发明的组合物。优选使用氟代聚烯烃作为抗滴剂。
氟代聚烯烃可以纯净物形式,也可以氟代聚烯烃乳液与接枝聚合物(成分B)乳液或与优选基于苯乙烯/丙烯腈上的共聚物的乳液的凝结混合物形式使用,并且其中所述氟代聚烯烃以乳液形式与接枝聚合物或共聚物的乳液混合并接着凝结。
此外,还可以使用作为与接枝聚合物(成分B)或优选基于苯乙烯/丙烯腈的共聚物的预配混物形式的氟代聚烯烃。氟代聚烯烃以粉末形式与接枝聚合物或共聚物的粉末或颗粒混合并通常在例如密炼机、挤出机或双轴挤出机的常规设备中且在200至330℃的温度下熔融配混。
氟代聚烯烃也可以母料形式使用,该母料在氟代聚烯烃水分散液存在条件下通过至少一种单烯不饱和单体的乳液聚合而制得。优选的单体成分是苯乙烯、丙烯腈和它们的混合物。聚合物可在酸性沉淀和其后的干燥之后以具有流淌能力的粉末的形式使用。
凝结物、预配混物或母料通常都具有5至95重量%、优选7至60重量%的固体含量。
在本发明的组合物中可以含有用量优选为0.05至5重量%、更优选0.1至1重量%且特别优选0.1至0.5重量%(以A)和B)计)的抗滴剂。
本发明的模塑组合物还可以含有至少一种常规添加剂,例如润滑剂和脱模剂,如硬脂酸季戊四醇酯,成核剂,抗静电剂,稳定剂,和除了具有所选择纵横比的无机材料外还有具有其他几何结构的无机材料,如其他填料和增强材料以及染料和颜料。
通过将各组分按照已知方法混合并在200至300℃的温度下于例如密炼机、挤出机和双轴挤出机的常规设备中熔融配混和熔融挤出,而制得成分A)和B)和任选的其他添加剂和助剂。
各组分的混合可以已知方法连续以及同时地进行,更确切地说在约20℃(室温)以及在更高温度下进行。长玻璃纤维以连续的所谓粗纱束或玻璃纤维束的形式引入到结构中,并且在结构中也引入了熔融的热塑性塑料或热塑性塑料共混物(参见WO95/28266和US6530246B1)。这也就意味着,要使长玻璃纤维或其他例如碳纤维或芳族聚酰胺纤维连续地经历润湿或浸渍过程(如图1所示)。粗纱中单丝的数目为200至20000,优选300至10000,特别优选500至2000。
本发明的模塑组合物可用于制备各种模制体。它们可以通过浇铸、挤出和吹塑法制备。另一种加工形式是通过深冲压而由预先制得的片材或膜制得模制体。
玻璃纤维在所得的模制件中,其平均纤维长度为0.5至50mm、优选1.0至40mm、特别优选1.5至15mm,且其中至少一部分超过40%、优选超过70%、特别优选超过80%的玻璃纤维具有超过1mm的长度。
长纤维-颗粒中的丝是单向排布的。
本发明的玻璃纤维增强热塑性材料具有良好的超乎所谓的短纤维增强热塑性材料的机械性能。短纤维增强热塑性材料是基于那些其中纤维以切割玻璃的形式在挤出机中与其他成分混合得到的材料。一般而言,短纤维增强的热塑性材料在颗粒中具有0.2至0.5mm的玻璃纤维长度。这些纤维在短纤维颗粒中是随机存在的,即无规分布。
由本发明的玻璃纤维增强的热塑性材料制得的模制体的例子是膜,型材,各种壳件,例如用于汽车内部的,如仪表板,家用设备,如榨汁机、咖啡机、混合机;用于办公机械,如监控器、印刷机、复印机;用于片材、管材、电子设备导管、窗、门和用于建筑部门、内部构件和外部应用的型材;用于诸如开关和插座的电子技术领域。
因此本发明的内容还在于一种制备以长玻璃纤维增强的模塑组合物的方法,该组合物含有至少一种选自聚酰胺、聚碳酸酯、聚酯碳酸酯、接枝聚合物和共聚物的聚合物,以及苯乙烯、丙烯腈和马来酸酐的三元聚合物。
优选的制备颗粒形式的本发明热塑性组合物的方法,其特征在于,
i)用任选至少一种选自聚酰胺、聚碳酸酯和聚酯碳酸酯的聚合物的熔体,用至少一种选自接枝聚合物和共聚物的聚合物的熔体和用苯乙烯、丙烯腈和马来酸酐的三元聚合物的熔体来润湿其中纤维丝直径为7至25μm的长玻璃纤维束,
ii)冷却,并
iii)将润湿的玻璃束切割为颗粒并具有5至50mm的切割长度。
特别优选的制备颗粒形式的本发明热塑性组合物的方法,其特征在于,
i)用至少一种选自聚酰胺、聚碳酸酯和聚酯碳酸酯的聚合物的熔体,用至少一种选自接枝聚合物和共聚物的聚合物的熔体和用苯乙烯、丙烯腈和马来酸酐的三元聚合物的熔体来润湿其中纤维丝直径为7至25μm的长玻璃纤维束,
ii)冷却,并
iii)将润湿的玻璃束切割为颗粒并具有5至50mm的切割长度。
以下实施例用以进一步阐述本发明。
实施例
将表1和2中所述的且以下简略描述的成分于约240℃下并在一个3-l密炼机或ZSK-25上进行配混。在Arburg 270E型注塑机上并于240-260℃下制得模制体。
根据WO95/28266混入长玻璃纤维,也可参见图1。
成分A1
基于相对溶液粘度为1.24的双酚A的直链聚碳酸酯,在作为溶剂的CH2Cl2中且在25℃和0.5g/100ml浓度条件下测得。
成分A2
基于相对溶液粘度为1.28的双酚A的直链聚碳酸酯,在作为溶剂的CH2Cl2中且在25℃和0.5g/100ml浓度条件下测得。
成分B1
40重量份由苯乙烯和丙烯腈按照73∶27的比例生成的共聚物在60重量份颗粒状的交联聚丁二烯橡胶(平均颗粒直径d50=0.3μm)上形成的接枝聚合物,通过乳液聚合制得。
成分B2
苯乙烯/丙烯腈重量比为72∶28且临界粘度为0.55dl/g(20℃下于二甲基甲酰胺中测得)的苯乙烯/丙烯腈-共聚物。
成分B3
Mitsubishi Rayon Co.Ltd,Tokyo,日本公司的Metablen SRK200,苯乙烯/丙烯腈接枝的硅酮-丙烯酸丁酯-复合橡胶。
成分B4
具有66.4重量%苯乙烯、32.5重量%丙烯腈和1.1重量%马来酸酐的苯乙烯/丙烯腈三元聚合物;熔融指数:8.5g/10min(200℃,5kg负载量)。
成分C1
R43SX6 Type 30(长玻璃纤维,平均直径17μm),Owens Corning(Battice,比利时)
成分C2
玻璃纤维(CS 7942,Bayer AG,勒沃库森,德国),短切的,平均长度为4.5mm。
用作添加剂的是硬脂酸季戊四醇酯(PETS)和亚磷酸酯稳定剂(Phosphitstabilisator)。
在实施例1至10中使用以下组合物A和B:
A:17.9重量份A1
43.0重量份A2
5.4重量份B3
23.3重量份B2
0.4重量份PETS
0.1重量份亚磷酸酯稳定剂
B:60.9重量份A1
14.3重量份B1
14.3重量份B2
0.5重量份PETS
0.1重量份亚磷酸酯稳定剂
组合物C是含有组合物A或B且任选还有其他各自具有20重量%长玻璃纤维(成分C1)或各自具有10或20重量%玻璃纤维(成分C2)的混合物。因为长玻璃纤维的加料可能会有些微的偏差,所以表1和2中记录了研磨后特定的玻璃含量。
拉伸强度根据ISO EN 527测定,E-模量根据ISO 527,却贝(Charpy)-冲击韧性(无缺口)根据ISO179 1eU测定。
Claims (13)
1.热塑性塑模组合物,其包括
(a)
A)选自聚酰胺、聚碳酸酯和聚酯碳酸酯的至少一种组分,其中A)部分为50重量份至95重量份,基于A)和B)的总重量份计,和
B)1至50重量份的以下形成的接枝聚合物,
B.1 5至95重量%的至少一种乙烯基单体接枝于
B.2 95至5重量%的一种或多种玻璃化转变温度<10℃的接枝基体,和
B.3任选地树脂状的、热塑性的、不含橡胶的乙烯基聚合物,
(b)相对于所述(a)的0.3至7重量%的苯乙烯、丙烯腈和马来酸酐的三元聚合物,
(c)以A)和B)的重量份为100计3至60重量%的长玻璃纤维,其中纤维丝的直径为7至25μm和长度是5至50mm。
2.如权利要求1所述的组合物,其中,三元聚合物(b)中的马来酸酐含量为0.2至5Mol%。
3.如权利要求1所述的组合物,其中,共聚物B.3由以下成分组成:
B.3.1 50至99重量份的乙烯基芳族化物和/或核取代的乙烯基芳族化物和/或甲基丙烯酸-C1-C8烷基酯和
B.3.2 1至50重量份的乙烯基氰化物和/或丙烯酸-C1-C8烷基酯和/或甲基丙烯酸-C1-C8烷基酯和/或不饱和的羧酸和/或不饱和羧酸的衍生物。
4.制备颗粒形式的热塑性组合物的方法,其特征在于,
i)以A)和B)的重量份为100计,3至60重量%的其中纤维丝直径为7至25μm的长玻璃纤维束用下列热塑性塑模组合物来润湿:
热塑性塑模组合物,其包括
(a)
A)选自聚酰胺、聚碳酸酯和聚酯碳酸酯的至少一种组分,其中A)部分为50重量份至95重量份,基于A)和B)的总重量份 计,和
B)1至50重量份的以下形成的接枝聚合物,
B.15至95重量%的至少一种乙烯基单体接枝于
B.295至5重量%的一种或多种玻璃化转变温度<10℃的接枝基体,和
B.3任选地树脂状的、热塑性的、不含橡胶的乙烯基聚合物,
(b)相对于所述(a)的0.3至7重量%的苯乙烯、丙烯腈和马来酸酐的三元聚合物,
ii)冷却,并
iii)将润湿的玻璃束切割为颗粒并具有5至50mm的切割长度。
5.如权利要求4所述的方法,其中,iii)中的颗粒的剪切长度为5至50mm。
6.如权利要求4所述的方法,其中,iii)中的颗粒的剪切长度为5至30mm。
7.如权利要求4所述的方法,其中,iii)中的颗粒的剪切长度为7至25mm。
8.如权利要求4所述的方法,其中,iii)中的颗粒的剪切长度为7至21mm。
9.含有如权利要求1至3之一所述的组合物的模制体,其中,模制体中的长玻璃纤维C)具有0.5至50mm的平均纤维长度。
10.如权利要求9所述的模制体,其中,长玻璃纤维C)具有1.5至15mm的平均纤维长度。
11.如权利要求9所述的模制体,其中,至少一部分超过40%的玻璃纤维具有超过1mm的长度。
12.如权利要求9所述的模制体,其中,至少一部分超过70%的玻璃纤维具有超过1mm的长度。
13.含有如权利要求1至3之一所述的组合物的型材、壳件、片材、管材、电子设备导管、窗、门、开关和插座。
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CN101076562A (zh) | 2007-11-21 |
EP1802696B1 (de) | 2014-03-12 |
KR20070067195A (ko) | 2007-06-27 |
ES2462017T3 (es) | 2014-05-22 |
WO2006040087A1 (de) | 2006-04-20 |
EP1802696A1 (de) | 2007-07-04 |
JP2008516062A (ja) | 2008-05-15 |
BRPI0516875A (pt) | 2008-09-23 |
TW200628533A (en) | 2006-08-16 |
KR101228232B1 (ko) | 2013-01-31 |
DE102005040620A1 (de) | 2006-04-13 |
CA2583314A1 (en) | 2006-04-20 |
US20060094813A1 (en) | 2006-05-04 |
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