CN102725340B - 具有良好机械性质i的抗划伤、耐冲击的聚碳酸酯模制组合物 - Google Patents
具有良好机械性质i的抗划伤、耐冲击的聚碳酸酯模制组合物 Download PDFInfo
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- CN102725340B CN102725340B CN201080057792.6A CN201080057792A CN102725340B CN 102725340 B CN102725340 B CN 102725340B CN 201080057792 A CN201080057792 A CN 201080057792A CN 102725340 B CN102725340 B CN 102725340B
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Classifications
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
- C08L69/005—Polyester-carbonates
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- 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
- C08K2201/00—Specific properties of additives
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- C08K2201/003—Additives being defined by their diameter
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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
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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
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- 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
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- C08K3/041—Carbon nanotubes
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- 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
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- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- 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
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- C08K5/52—Phosphorus bound to oxygen only
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- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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Abstract
本发明涉及具有良好机械性质和高耐化学性以及良好耐火性质并在加工过程中表现出改进的流动性质的抗划伤、耐冲击的聚碳酸酯(PC)组合物和模制组合物,其包含A)10-90重量份的芳族聚碳酸酯和/或芳族聚酯碳酸酯,B)0.5-30重量份的橡胶改性的接枝聚合物,C)0-40重量份的乙烯基(共)聚合物(C.1)和/或聚对苯二甲酸亚烷基二醇酯(C.2),D)0.1-50重量份的中空陶瓷球,E)0.2-5.0重量份的至少一种聚有机硅氧烷,F)0-20重量份的至少一种含磷耐火剂,G)0-10重量份的至少一种其它添加剂,其中将所述的所有重量份标准化以使所述组合物中所有组分A+B+C+D+E+F+G的重量份之和为100。本发明还涉及该组合物的制备方法和它们用于制造成型制品,特别是平面屏幕装置的外壳的用途。
Description
本发明涉及具有良好机械性质和高耐化学性以及良好防火性质并在加工过程中表现出改进的流动性质的抗划伤、耐冲击的聚碳酸酯(PC)组合物和模制组合物、它们的制备方法和它们用于制造成型制品,特别是平面屏幕装置的外壳(housings)的用途。
JP-A 05-070653描述了作为马来酰亚胺-改性的ABS模制组合物中的添加剂的具有高压缩强度的玻璃中空球体。该模制组合物具有降低的密度、高弯曲模量和良好的热变形温度。没有报道这种添加剂对焊接强度、耐化学性或提高的抗划伤性的有利作用。
EP-A 391 413描述了使用滑石作为抗冲改性的聚碳酸酯中的填料。没有描述对抗划伤性或加工性质的影响。
JP-A 01-104637描述了结晶聚丙烯和改性聚丙烯的混合物,已向其中加入Al2O3-SiO2的中空颗粒。与含滑石的相应混合物相比,通过这些颗粒获得改进的抗划伤性以及降低的弯曲模量。没有描述对焊接强度或耐化学性的作用。
JP 2003-326623描述了聚碳酸酯的多层板,其中中间层带有中空陶瓷球以隔热和隔音。但是,这些球体不与聚碳酸酯共混存在。
EP 2087478 A1描述了通过添加中空陶瓷球获得的具有填料含量并具有提高的对机械性质的要求和改进的流动性质的抗冲改性的聚碳酸酯组合物。但是,没有实现对冲击强度和焊接强度的积极作用。
本发明的目的是提供以高流动性(以熔体粘度测得)、良好的在快速冲击应力下的机械性质,如高冲击强度和高焊接强度和以良好的耐化学性(ESC性质)以及不变的高或更好的抗划伤性为特征的组合物。所述组合物应优选防火并符合UL94 V-0的要求,包括在薄壁厚度(即1.5毫米的壁厚度)下。
本发明还提供所述组合物的制备方法和所述组合物用于制造成型制品的用途。
本发明的组合物可用于制造所有类型的成型制品。这些可通过注射成型、挤出或吹塑法制造。另一加工形式是通过由之前制成的片材或膜热成形来制造成型制品。
这样的成型制品的实例是所有类型的膜、型材、外壳部件,例如用于家用电器,如榨汁机、咖啡机、搅拌机;用于办公器材,如监视器、平面屏幕、笔记本、打印机、复印机;片材、管、电气安装导管、窗、门和建筑部门(室内装饰和室外用途)用的其它型材以及电和电子部件,如开关、插头和插座以及多用途交通工具用的,特别是汽车领域用的车身或内部部件。
本发明的组合物特别也可例如用于制造下列成型制品或模制品:轨道交通工具、船、飞机、公交车和其它机动车的内部装饰部件、含小型变压器的电气设备的外壳、信息处理和传送设备的外壳、医疗设备的外壳和衬里、按摩设备及其外壳、儿童玩具车、平面墙元件(planar wall
element)、安全设备外壳、绝热运输容器、卫浴配件的模制品、通风口的遮盖栅和园艺设备外壳。
已经发现,令人惊讶地,包含以下的的组合物具有所需性质状况:
A) 10 - 90重量份,优选50 - 85重量份,特别优选60 - 75重量份的芳族聚碳酸酯和/或芳族聚酯碳酸酯,
B) 0.5 - 30.0重量份,优选1.0 - 25.0重量份,更优选2.0 - 20.0重量份,特别优选4.0 - 9.0重量份的橡胶改性的接枝聚合物,
C) 0 - 40.0重量份,优选1.0 - 30.0重量份,特别优选1.5 - 10.0重量份的乙烯基(共)聚合物(C.1)和/或聚对苯二甲酸亚烷基二醇酯(C.2),
D) 0.1 - 50.0重量份,优选0.3 - 30.0重量份,更优选1.0 - 20.0重量份,特别优选2.0 - 12.0重量份的中空陶瓷球,
E) 0.2 - 10.0重量份,优选0.5 - 5.0重量份,更优选0.8 - 3.0重量份,特别优选1.0 - 2.0重量份的至少一种优选线型聚有机硅氧烷,
F) 0 - 20重量份,优选1.0 – 18.0重量份,更优选2.0 – 16.0重量份,特别优选3.0 - 15.0重量份的至少一种含磷耐火剂,
G) 0 - 10.0重量份,优选0.5 - 8.0重量份,特别优选1.0 - 6.0重量份的添加剂,
其中将本申请中所述的所有重量份标准化以使所述组合物中所有组分A+B+C+D+E+F+G的重量份之和为100。
在一个优选实施方案中,组分D与组分E的比率为2:1至10:1,优选4:1至6:1,特别优选5:1。
组分
A
根据适用于本发明的组分A的芳族聚碳酸酯和/或芳族聚酯碳酸酯是文献中已知的或可通过文献中已知的方法制备(关于芳族聚碳酸酯的制备,参见例如Schnell,
"Chemistry and Physics of Polycarbonates", Interscience Publishers,
1964和DE-AS 1 495 626、DE-A 2 232 877、DE-A 2 703 376、DE-A 2 714 544、DE-A 3 000 610、DE-A 3 832 396;关于芳族聚酯碳酸酯的制备,例如DE-A 3 077 934)。
例如通过使二酚与碳酰卤,优选光气,和/或与芳族二羧酰二卤(dicarboxylic
acid dihalides),优选苯二羧酰二卤经任选使用链终止剂,例如单酚和任选使用三官能或大于三官能的支化剂,例如三酚或四酚的界面法(interfacial
process)反应来制备芳族聚碳酸酯。也可以通过二酚与例如碳酸二苯酯的反应经由熔体聚合法制备。
用于制备芳族聚碳酸酯和/或芳族聚酯碳酸酯的二酚优选是式(I)的那些
(I)
其中
A是单键、C1至C5-亚烷基、C2至C5-烷叉(alkylidene)、C5至C6-环烷叉、-O-、-SO-、-CO-、-S-、-SO2-、C6至C12-亚芳基,任选含有杂原子的其它芳环可稠合到其上,
或式(II)或(III)的基团
(II)
(III)
B在每种情况下是C1至C12-烷基,优选甲基,卤素,优选氯和/或溴
x在每种情况下彼此独立地为0、1或2,
p是1或0,且
R5和R6对各X1而言独立地且彼此独立地表示氢或C1至C6-烷基,优选氢、甲基或乙基,
X1是指碳,且
m是指4至7,优选4或5的整数,条件是在至少一个原子X1上,R5和R6同时是烷基。
优选二酚是氢醌、间苯二酚、二羟基二酚、双-(羟苯基)-C1-C5-链烷、双-(羟苯基)-C5-C6-环烷、双-(羟苯基)醚、双-(羟苯基)亚砜、双-(羟苯基)酮、双-(羟苯基)砜和α,α-双-(羟苯基)-二异丙基-苯及其在核上溴化和/或在核上氯化的衍生物。
特别优选的二酚是4,4'-二羟基二苯基、双酚A、2,4-双-(4-羟苯基)-2-甲基丁烷、1,1-双-(4-羟苯基)-环己烷、1,1-双-(4-羟苯基)-3,3,5-三甲基环己烷、4,4'-二羟基二苯硫、4,4'-二羟基二苯砜及其二-和四溴化或氯化的衍生物,例如2,2-双-(3-氯-4-羟苯基)-丙烷、2,2-双-(3,5-二氯-4-羟苯基)-丙烷或2,2-双-(3,5-二溴-4-羟苯基)-丙烷。2,2-双-(4-羟苯基)-丙烷(双酚A)特别优选。
二酚可以独自使用或以任何所需混合物的形式使用。二酚是文献中已知的或可通过文献中已知的方法获得。
适用于制备热塑性芳族聚碳酸酯的链终止剂是例如,酚、对氯酚、对叔丁基酚或2,4,6-三溴酚,以及长链烷基酚,如4-[2-(2,4,4-三甲基戊基)]-酚、根据DE-A 2 842 005的4-(1,3-四甲基丁基)]-酚或在烷基取代基中具有总共8至20个碳原子的单烷基酚或二烷基酚,如3,5-二-叔丁基酚、对异辛基酚、对叔辛基酚、对十二烷基酚和2-(3,5-二甲基庚基)-酚和4-(3,5-二甲基庚基)-酚。要用的链终止剂的量通常为所用的特定二酚的摩尔总数的0.5摩尔%至10摩尔%。
该热塑性芳族聚碳酸酯具有10,000至200,000克/摩尔,优选15,000至80,000克/摩尔,特别优选24,000至32,000克/摩尔的平均分子量(重均Mw,通过使用聚碳酸酯标样的GPC(凝胶渗透色谱法)测得)。
该热塑性芳族聚碳酸酯可以以已知方式支化,特别优选通过并入占所用二酚总量的0.05至2.0摩尔%的三官能或大于三官能的化合物,例如具有3个和更多个酚类基团的那些。优选使用线型聚碳酸酯,更优选基于双酚A。
均聚碳酸酯和共聚碳酸酯都合适。占所用二酚总量的1至25重量%,优选2.5至25重量%的具有羟基芳氧基端基的聚二有机硅氧烷也可用于制备根据组分A的本发明的共聚碳酸酯。这些是已知的(US 3 419 634)并可通过文献中已知的方法制备。含聚二有机硅氧烷的共聚碳酸酯也合适;在DE-A 3 334 782中描述了含聚二有机硅氧烷的共聚碳酸酯的制备。
除双酚A均聚碳酸酯外,优选聚碳酸酯还是双酚A与占二酚摩尔总数的最多15摩尔%的作为优选或特别优选提到的其它二酚,特别是2,2-双-(3,5-二溴-4-羟苯基)-丙烷的共聚碳酸酯。
用于制备芳族聚酯碳酸酯的芳族二羧酰二卤优选是间苯二甲酸、对苯二甲酸、二苯基醚4,4'-二羧酸和萘-2,6-二羧酸的二酰二氯(diacid
dichloride)。
比率为1:20至20:1的间苯二甲酸和对苯二甲酸的二酰二氯的混合物特别优选。
碳酰卤,优选光气另外共同用作聚酯碳酸酯制备中的双官能酸衍生物。
除已提到的单酚外,用于制备芳族聚酯碳酸酯的可能的链终止剂还包括其氯碳酸酯和可任选被C1至C22-烷基或被卤素原子取代的芳族单羧酸的酰基氯,以及脂族C2至C22-单羧酰氯。
链终止剂的量在每种情况下为0.1至10摩尔%,在酚类链终止剂的情况下基于二酚的摩尔数,在单羧酰氯链终止剂的情况下基于二羧酰二氯的摩尔数。
一种或多种芳族羟基羧酸可另外用于制备芳族聚酯碳酸酯。
该芳族聚酯碳酸酯可以以已知方式是线型或支化的(在这方面,参见DE-A 2 940 024和DE-A 3 007 934),线型聚酯碳酸酯是优选的。
可用的支化剂是例如,0.01至1.0摩尔%(基于所用二羧酰二氯)的量的三官能或大于三官能的羧酰氯,如苯均三酰三氯、氰尿酰三氯、3,3',4,4'-二苯甲酮-四羧酰四氯、1,4,5,8-萘四羧酰四氯或苯均四酰四氯,或占所用二酚的0.01至1.0摩尔%的量的三官能或大于三官能的酚,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)-苯基甲烷、2,2-双[4,4-双(4-羟苯基)-环己基]-丙烷、2,4-双(4-羟苯基-异丙基)-苯酚、四-(4-羟苯基)-甲烷、2,6-双(2-羟基-5-甲基-苄基)-4-甲基-苯酚、2-(4-羟苯基)-2-(2,4-二羟基苯基)-丙烷、四-(4-[4-羟苯基-异丙基]-苯氧基)-甲烷、1,4-双[4,4'-二羟基三苯基)-甲基]-苯。可首先将酚类支化剂与二酚一起引入;酰基氯支化剂可以与酰二氯一起引入。
可以按需要改变热塑性芳族聚酯碳酸酯中碳酸酯结构单元的含量。碳酸酯基团含量优选为基于酯基团与碳酸酯基团总量最多100摩尔%,特别是最多80摩尔%,特别优选最多50摩尔%。该芳族聚酯碳酸酯的酯和碳酸酯含量都可以以嵌段形式或以无规分布形式存在于该缩聚物中。
该热塑性芳族聚碳酸酯和聚酯碳酸酯可独自使用或以任何所需混合物的形式使用。
组分
B
组分B包括
B.1 5至95,优选20至90重量%,特别优选30至60重量%的至少一种乙烯基单体,在
B.2 95至5,优选80至10重量%,特别优选70至40重量%的一种或多种玻璃化转变温度<10℃,优选<0℃,特别优选<-20℃的接枝基料(graft bases)上
的一种或多种接枝聚合物。
接枝基料B.2通常具有0.05至10.00微米,优选0.10至5.00微米,更优选0.20至1.00微米,特别优选0.25至0.50微米的平均粒度(d50值)。
单体B.1是下列的混合物
B.1.1 50至99重量份的乙烯基芳烃和在核上被取代的乙烯基芳烃(如苯乙烯、α-甲基苯乙烯、对甲基苯乙烯或对氯苯乙烯)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(不饱和腈,如丙烯腈和甲基丙烯腈)、(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(如酐和酰亚胺),例如马来酸酐。
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。特别优选的单体是B.1.1苯乙烯和B.1.2丙烯腈。
适用于接枝聚合物B的接枝基料B.2是例如二烯橡胶、EP(D)M橡胶,即基于乙烯/丙烯和任选二烯的那些,和丙烯酸酯、聚氨酯、有机硅、氯丁二烯和乙烯/乙酸乙烯酯橡胶。
优选接枝基料B.2是二烯橡胶(例如基于丁二烯和异戊二烯)或二烯橡胶的混合物或二烯橡胶的共聚物或它们与其它可共聚单体(例如根据B.1.1和B.1.2)的混合物,条件是组分B.2的玻璃化转变温度低于<10℃,优选<0℃,特别优选< -10℃。纯聚丁二烯橡胶特别优选。
借助动态差示扫描量热法(DSC)根据DIN EN 61006在10 K/min的加热速率下测定玻璃化转变温度,作为中点测定值测定Tg(切线法)。
特别优选的聚合物B是例如DE-OS 2 035
390 (= US 3 644 574)或DE-OS 2 248 242 (= GB 1 409 275)和Ullmanns,
Enzyklopädie der Technischen Chemie, 第19卷 (1980), 第280页及以下各页中所述的ABS聚合物(乳液、本体和悬浮ABS)。接枝基料B.2的凝胶含量为至少30重量%,优选至少40重量%(在甲苯中测量)。
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制备接枝共聚物B。
特别合适的接枝橡胶也是根据US 4 937 285在乳液聚合法中通过用有机氢过氧化物和抗坏血酸的引发剂体系氧化还原引发而制成的ABS聚合物。
由于如已知的那样在接枝反应过程中接枝单体不一定完全接枝到接枝基料上,根据本发明,接枝聚合物B也被理解为是指通过接枝单体在接枝基料存在下的(共)聚合制成并且也在后处理过程中获得的那些产品。
根据聚合物B的B.2的合适的丙烯酸酯橡胶优选是丙烯酸烷基酯的聚合物,任选含有基于B.2最多40重量%的其它可聚合烯键式不饱和单体。优选的可聚合丙烯酸酯包括C1至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,优选卤代-C1-C8-烷基酯,如丙烯酸氯乙酯,和这些单体的混合物。
为了交联,可以使具有多于一个可聚合双键的单体共聚。交联单体的优选实例是具有3至8个C原子的不饱和单羧酸和具有3至12个C原子的不饱和一元醇或具有2至4个OH基团和2至20个C原子的饱和多元醇的酯,如二甲基丙烯酸乙二醇酯、甲基丙烯酸烯丙酯;多不饱和杂环化合物,如三乙烯基和三烯丙基氰尿酸酯;多官能乙烯基化合物,如二-和三乙烯基苯;以及磷酸三烯丙酯和邻苯二甲酸二烯丙酯。优选的交联单体是甲基丙烯酸烯丙酯、二甲基丙烯酸乙二醇酯、邻苯二甲酸二烯丙酯和含有至少三个烯键式不饱和基团的杂环化合物。特别优选的交联单体是环状单体氰尿酸三烯丙酯、异氰尿酸三烯丙酯、三丙烯酰基六氢-s-三嗪、三烯丙基苯。交联单体的量优选为接枝基料B.2的0.02至5.00,特别是0.05至2.00重量%。在具有至少三个烯键式不饱和基团的环状交联单体的情况下,将该量限制为小于接枝基料B.2的1重量%是有利的。
除丙烯酸酯外,可任选用于制备接枝基料B.2的优选的“其它”可聚合烯键式不饱和单体是例如丙烯腈、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。作为接枝基料B.2的优选丙烯酸酯橡胶是具有至少60重量%的凝胶含量的乳液聚合物。
根据B.2的其它合适的接枝基料是如DE-OS 3 704
657、DE-OS 3 704 655、DE-OS 3 631 540和DE-OS 3 631
539中所述的具有接枝活性位点的硅橡胶。
在合适的溶剂中在25ºC下测定接枝基料B.2的凝胶含量(M. Hoffmann,
H. Krömer, R. Kuhn, Polymeranalytik I und II, Georg Thieme-Verlag, Stuttgart
1977)。
平均粒度d50是各有50重量%的颗粒大于和小于该直径。其可借助超速离心机测量法测定(W. Scholtan,
H. Lange, Kolloid, Z. und Z. Polymere 250 (1972), 782-l796)。
组分
C
组分C包括一种或多种热塑性乙烯基(共)聚合物C.1和/或聚对苯二甲酸亚烷基二醇酯C.2。
合适的乙烯基(共)聚合物C.1是至少一种选自乙烯基芳烃、乙烯基氰(不饱和腈)、(甲基)丙烯酸(C1至C8)-烷基酯、不饱和羧酸和不饱和羧酸衍生物(如酐和酰亚胺)的单体的聚合物。合适的(共)聚合物特别是下列的那些(共)聚合物:
C.1.1 50至99,优选60至80重量份的乙烯基芳烃和/或在核上被取代的乙烯基芳烃(如苯乙烯、α-甲基苯乙烯、对甲基苯乙烯、对氯苯乙烯)和(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
C.1.2 1至50,优选20至40重量份的乙烯基氰(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,如马来酸,和/或不饱和羧酸的衍生物,如酐和酰亚胺,例如马来酸酐和N-苯基马来酰亚胺。
该乙烯基(共)聚合物C.1是树脂质的、热塑性的和无橡胶的。C.1.1苯乙烯和C.1.2丙烯腈的共聚物特别优选
根据C.1的(共)聚合物是已知的并可以通过自由基聚合,特别是通过乳液、悬浮、溶液或本体聚合制备。该(共)聚合物优选具有15,000至200,000克/摩尔,特别优选100,000至150,000克/摩尔的平均分子量Mw(重均,通过光散射或沉降测定)。
在一个特别优选的实施方案中,C.1是具有130,000克/摩尔的重均分子量Mw的77重量%苯乙烯和23重量%丙烯腈的共聚物。
组分C.2的聚对苯二甲酸亚烷基二醇酯是芳族二羧酸或它们的反应衍生物,如二甲酯或酐,和脂族、脂环族或芳脂族二醇的反应产物,和这些反应产物的混合物。
优选的聚对苯二甲酸亚烷基二醇酯含有占二羧酸组分的至少80重量%,优选至少90重量%的对苯二甲酸基团和占二醇组分的至少80重量%,优选至少90重量%的乙二醇和/或丁-1,4-二醇的基团。
优选的聚对苯二甲酸亚烷基二醇酯除对苯二甲酸基团外还可含有最多20摩尔%,优选最多10摩尔%的具有8至14个C原子的其它芳族或脂环族二羧酸或具有4至12个C原子的脂族二羧酸的基团,例如邻苯二甲酸、间苯二甲酸、萘-2,6-二羧酸、4,4'-二苯基二羧酸、丁二酸、己二酸、癸二酸、壬二酸、环己二乙酸的基团。
优选的聚对苯二甲酸亚烷基二醇酯除乙二醇或丁-1,4-二醇的基团外还可含有最多20摩尔%,优选最多10摩尔%的其它具有3至12个C原子的脂族二醇或具有6至21个C原子的脂环族二醇,例如丙-1,3-二醇、2-乙基丙-1,3-二醇、新戊二醇、戊-1,5-二醇、己-1,6-二醇、环己-1,4-二甲醇、3-乙基戊-2,4-二醇、2-甲基戊-2,4-二醇、2,2,4-三甲基戊-1,3-二醇、2-乙基己-1,3-二醇、2,2-二乙基丙-1,3-二醇、己-2,5-二醇、1,4-二-(β-羟基乙氧基)-苯、2,2-双-(4-羟基环己基)-丙烷、2,4-二羟基-1,1,3,3-四甲基-环丁烷、2,2-双-(4-β-羟基乙氧基-苯基)-丙烷和2,2-双-(4-羟基丙氧基苯基)-丙烷的基团(DE-A
2 407 674、2 407 776、2 715 932)。
聚对苯二甲酸亚烷基二醇酯可以例如通过根据DE-A
1 900 270和US 3 692 744并入相对少量的3-或4-元醇或3-或4-元羧酸来支化。优选支化剂的实例是苯均三酸、偏苯三酸、三羟甲基乙烷和三羟甲基丙烷和季戊四醇。
仅由对苯二甲酸及其反应性衍生物(例如其二烷基酯)和乙二醇和/或丁-1,4-二醇制成的聚对苯二甲酸亚烷基二醇酯和这些聚对苯二甲酸亚烷基二醇酯的混合物特别优选。
聚对苯二甲酸亚烷基二醇酯的混合物含有1至50重量%,优选1至30重量%的聚对苯二甲酸乙二醇酯和50至99重量%,优选70至99重量%的聚对苯二甲酸丁二醇酯。
优选使用的聚对苯二甲酸亚烷基二醇酯通常具有0.4至1.5 dl/g,优选0.5至1.2 dl/g的在Ubbelohde粘度计中在25 ºC下在酚/邻-二氯苯(1:1重量份)中测得的极限粘度。
该聚对苯二甲酸亚烷基二醇酯可通过已知方法制备(参见例如Kunststoff-Handbuch,
第VIII卷, 第695页及以下各页,
Carl-Hanser-Verlag, Munich 1973)。
组分
D
本发明的模制组合物包含中空陶瓷球,优选中空硅-铝陶瓷球作为组分D。优选的中空陶瓷球具有5.0至25.0重量%,优选7.5至20.0重量%,特别优选10.0至15.0重量%的Al2O3含量。
在一个优选实施方案中,该中空陶瓷球具有2.0 - 3.0克/立方厘米,优选2.2 - 2.6克/立方厘米的比密度。特别优选的中空陶瓷球具有50 - 700 MPa,优选200 - 500 MPa的压缩强度。所述压缩强度是等静压力阻力——在此,球体在液体柱中承受所述压力时80%的球体保持不破坏。
该中空陶瓷球优选具有0.1-100.0微米,优选0.5-50.0微米,更优选1.0-30.0微米,特别优选2.0-10.0微米的平均粒径(d50)。使用Sedigraph
5100, Micrometrics Instruments Corporation, Norcross, Georgia, USA通过在水介质中沉降来测定平均粒径(d50值)。
组分
E
作为根据本发明的组分E的聚有机硅氧烷包含通式IV的单元:
RrSiO(4-r)/2
(IV)
其中R彼此独立地表示取代或未取代的烃基,r是指0、1、2或3,条件是r的平均数值为1.9至2.1。
优选基团R是例如烷基、芳基、烷基芳基、烯基或环烷基,它们各自可以是取代或未取代的并任选被杂原子***。
烃基R的实例是烷基,例如甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、正戊基、异戊基、新戊基、叔戊基,己基,例如正己基,庚基,例如正庚基,辛基,如正辛基和异辛基,例如2,2,4-三甲基戊基或乙基己基,壬基,例如正壬基,癸基,例如正癸基,十二烷基,例如正十二烷基,十八烷基,例如正十八烷基;环烷基,例如环戊基、环己基、环庚基和甲基环己基;芳基,例如苯基、联苯基、萘基和蒽基和菲基;烷芳基,例如邻-、间-、对-甲苯基、二甲苯基和乙基苯基;芳烷基,例如苄基、α-和β-苯乙基。
取代烃基R的实例是卤代烷基,例如3-氯丙基、3,3,3-三氟丙基和全氟己基乙基,卤代芳基,例如对-氯苯基和对-氯苄基。
基团R优选是氢和/或具有1至8个碳原子的烃基,特别优选甲基。
基团R的另一些优选实例是乙烯基、烯丙基、甲基烯丙基、1-丙烯基、1-丁烯基、1-戊烯基、5-己烯基、丁二烯基、己二烯基、环戊烯基、环戊二烯基、环己烯基、乙炔基、炔丙基和1-丙炔基。
在本发明的进一步优选实施方案中,基团R是具有2至8个碳原子的烯基,特别优选乙烯基。
在具有1至8个碳原子的任选取代的烃基的情况下,甲基、乙烯基、苯基和3,3,3-三氟丙基特别优选作为取代基。
优选地,烷基,特别是甲基,键合到式(IV)的单元的聚有机硅氧烷E中所含的至少70摩尔%的Si原子上。
当该聚有机硅氧烷除键合到硅上的甲基或3,3,3-三氟丙基和两者的组合外还含有结合到硅上的乙烯基或苯基和两者的组合时,后者优选以0.001至30摩尔%的量存在。
优选地,聚有机硅氧烷E主要包含二有机硅氧烷单元。该聚有机硅氧烷的端基可以是三烷基甲硅烷氧基,特别是三甲基甲硅烷氧基或二甲基乙烯基甲硅烷氧基;但是,这些烷基中的一个或多个也可以被羟基或烷氧基,如甲氧基或乙氧基替代。
聚有机硅氧烷E可以是液体或高粘物质。聚有机硅氧烷E具有50,000至1,000,000 mm2/s,优选100,000至800,000 mm2/s,特别是200,000至600,000 mm2/s,非常特别优选500,000 mm2/s的在25 ºC下测得的粘度,条件是组分E的平均分子量小于200,000克/摩尔。
可以使用一种聚有机硅氧烷或各种聚有机硅氧烷的混合物作为组分E。
优选在本发明的有机聚硅氧烷颗粒中不使用交联剂。
但是,对某些用途而言,使用交联剂是有利的,例如当希望有机聚硅氧烷键合到热塑性塑料上时。在这种情况下,过氧化物,如过氧化二苯甲酰、过氧化双(2,4-二氯苯甲酰)、过氧化二枯基、过氧化双-4-甲基苯甲酰、2,5-二甲基-己烷-2,5-二-叔丁基过氧化物或2,5-双-(叔丁基过氧基)-2,5-二甲基己烷和它们的混合物优选作为交联剂添加到本发明的聚有机硅氧烷颗粒中。
在本发明中优选使用具有在25ºC下测得的500,000 mm2/s的粘度的线型聚二甲基硅氧烷。
组分
F
含磷耐火剂F在本发明中优选选自单-和低聚磷酸酯和膦酸酯、膦酸酯胺(phosphonatamines)和磷腈(phosphazenes),也可以使用选自一个或各种这些类别的几种组分的混合物作为耐火剂。在本文中没有具体提到的其它无卤素的磷化合物也可独自使用或与其它无卤素的磷化合物以任何所需组合使用。
优选的单-和低聚磷酸酯或膦酸酯是通式(V)的磷化合物
其中
R1、R2、R3和R4彼此独立地表示在每种情况下任选卤化的C1至C8-烷基、或C5至C6-环烷基、C6至C20-芳基或C7至C12-芳烷基,在每种情况下任选被烷基,优选C1至C4-烷基,和/或卤素,优选氯、溴取代,
n彼此独立地表示0或1,
q是指0至30且
X是指具有6至30个C原子的单核或多核芳族基团或具有2至30个C原子的直链或支化脂族基团,它们可以被OH取代并可含有最多8个醚键。
优选地,R1、R2、R3和R4彼此独立地代表C1至C4-烷基、苯基、萘基或苯基-C1-C4-烷基。芳族基团R1、R2、R3和R4又可以被卤素基团和/或烷基,优选氯、溴和/或C1至C4-烷基取代。特别优选的芳基是甲苯基、苯基、二甲苯基、丙基苯基或丁基苯基和它们的相应溴化和氯化衍生物。
式(V)中的X优选是指具有6至30个C原子的单核或多核芳族基团。这优选衍生自式(I)的二酚。
式(V)中的n可以彼此独立地为0或1,n优选为1。
q代表0至30,优选0至20,特别优选0至10的整数值,在混合物的情况下,0.8至5.0,优选1.0至3.0,更优选1.05至2.00,特别优选1.08至1.60的平均值。
X特别优选代表
或它们的氯化或溴化衍生物,X特别衍生自间苯二酚、氢醌、双酚A或二苯基酚。X特别优选衍生自双酚A。
式(V)的磷化合物特别是磷酸三丁酯、磷酸三苯酯、磷酸三甲苯酯、磷酸二苯基甲苯基酯、磷酸二苯基辛酯、磷酸二苯基2-乙基甲苯基酯、磷酸三-(异丙基苯基)酯、间苯二酚-桥连的低聚磷酸酯和双酚A-桥连的低聚磷酸酯。特别优选使用衍生自双酚A的式(V)的低聚磷酸酯。
根据式(Va)的双酚A-基低聚磷酸酯
(Va)
最优选作为组分F。
根据组分F的磷化合物是已知的(参考例如EP-A
0 363 608、EP-A 0 640 655)或可通过已知方法以类似方式制备(例如Ullmanns
Enzyklopädie der technischen Chemie, 第18卷, 第301页及以下各页,1979;
Houben-Weyl, Methoden der organischen Chemie, 第12/1卷, 第43页; Beilstein第6卷, 第177页)。
也可以使用不同化学结构和/或相同化学结构和不同分子量的磷酸酯的混合物作为本发明的组分F。
优选使用相同结构和不同链长的混合物,所述q值是平均q值。可以通过利用合适的方法(气相色谱法(GC)、高压液相色谱法(HPLC)、凝胶渗透色谱法(GPC))测定磷化合物的组成和由其计算q的平均值来确定平均q值。
如WO 00/00541和WO 01/18105中描述的膦酸酯胺和磷腈也可用作耐火剂。
耐火剂可以独自使用或以相互的任何所需混合物或与其它耐火剂的混合物使用。
其它添加剂
G
该组合物还可包含其它常规聚合物添加剂,如防火协作剂(flameproofing
synergist)、防滴落剂(例如氟化聚烯烃、有机硅和芳族聚酰胺纤维的物质类别的化合物)、润滑剂和脱模剂(例如季戊四醇四硬脂酸酯)、成核剂、稳定剂、抗静电剂(例如导电炭黑、碳纤维、碳纳米管和有机抗静电剂,如聚亚烷基醚、烷基磺酸酯或含聚酰胺的聚合物)和染料、颜料、填料和增强物质,特别是玻璃纤维、矿物增强物质和碳纤维。
特别地,使用聚四氟乙烯(PTFE)或含PTFE的组合物,例如PTFE与含苯乙烯或甲基丙烯酸甲酯的聚合物或共聚物的母料,作为防滴落剂。位阻酚和亚磷酸酯或其混合物,例如Irganox© B900
(Ciba Speciality Chemicals)优选用作稳定剂。季戊四醇四硬脂酸酯优选用作脱模剂。
模制组合物的制备和测试
表1中所列的原料物质在双螺杆挤出机(ZSK-25)
(Werner und Pfleiderer)上在260ºC的机器温度下以225 rpm的旋转速度和20千克/小时的生产量配混和造粒。制成的颗粒在注射成型机上加工以产生相应试样(熔体温度240ºC,模具温度80ºC,熔体前沿速度(melt front
speed)240 mm/s)。
下列方法用于表征试样性质:
根据ISO 11443测定流动性(熔体粘度)。
在注射成型的尺寸80x10x4 mm的试验条上在双面上根据ISO 179/1eU测量焊接强度(weld strength)。
在注射成型的尺寸80x10x4 mm的试验条上在一面上根据ISO 179/1eU测量冲击强度。
在注射成型的尺寸80x10x4 mm的试验条上在一面上根据DIN ISO 306(Vicat软化温度,方法B,50N载荷和120 K/h的加热速率)测量热变形温度。
根据ASTM D-3363 (750 g重量)作为铅笔硬度测定抗划伤性。在这种试验中,在表面上在固定压力下划动硬度为3H、2H、H、F、HB、B、2B和3B(在此硬度递减)的铅笔。铅笔硬度指出在表面上不可检出划伤的情况下的最硬铅笔。
在尺寸80 x 10 x 4 mm的条上研究应力开裂性质(ESC性质)。所用的特定试验介质显示在表1中。试样借助圆弧模板预延伸(预延伸ex = 2.4 %)并在室温下存放在试验介质中。通过观察裂纹形成(“CF”)或非裂纹形成(“NCF”)或破裂(“FR”)评测应力开裂性质。
在尺寸127 x 12.7 x
1.5 mm的条上根据UL 94V测量燃烧性质。
下列实施例用于进一步解释本发明。
实施例
组分
A
重均分子量 w为27,500 g/mol(通过在二氯甲烷中的以聚碳酸酯为标样的GPC测得)的基于双酚A的线型聚碳酸酯。
组分
B
通过43重量%(基于ABS聚合物)的27重量%丙烯腈和73重量%苯乙烯的混合物在57重量%(基于ABS聚合物)的以颗粒形式(平均粒径d50
= 0.35微米)交联的聚丁二烯橡胶存在下的乳液聚合制成的ABS聚合物。
组分
C
通过本体法制成的77重量%的苯乙烯和23重量%的丙烯腈的共聚物,具有130,000 g/mol的重均分子量Mw(通过在四氢呋喃中的使用聚苯乙烯标样的GPC测得)。
组分
D
由Al2O3含量为12 %的硅-铝陶瓷制成的中空陶瓷球。该陶瓷中空球体具有2.5克/立方厘米的比密度和420 MPa的等静压强度。该球体具有4微米的平均直径。
组分
E
聚二甲基硅氧烷,线型,粘度500,000 mm2/s,在25 ºC下测得(分子量160,000 g/mol)。
组分
F
基于双酚A的低聚磷酸酯
组分G
G1:聚四氟乙烯粉末, CFP 6000 N,
Du Pont.
G2:作为润滑剂/脱模剂的季戊四醇四硬脂酸酯
G3:亚磷酸酯稳定剂, Irganox®
B 900, Ciba Speciality Chemicals
表1:防火模制组合物的组成和性质
在表1的组合物中,只有根据实施例1和4的本发明的组合物(包含特定陶瓷球和线型聚二甲基硅氧烷的组合)实现本发明的目的,即具有良好的抗划伤性、实现改进的抗应力开裂性和更好的机械性质(即高冲击强度和焊接强度)和改进的流动性。如果只使用陶瓷球(对比例2和5),抗划伤性确实在高水平,但观察到焊接强度、冲击强度和流动性质的显著减弱。如果只使用硅氧烷(对比例3和6),焊接强度和冲击强度确实在高水平,但抗划伤性、热变形温度和抗应力开裂性明显变差。
除提供该组合物外,本发明还提供其用于制造注射成型或热成型制品的用途和包含本发明的组合物的成型制品。
Claims (15)
1.组合物,其包含:
A) 10 - 90重量份的芳族聚碳酸酯和/或芳族聚酯碳酸酯,
B) 0.5 - 30重量份的橡胶改性的接枝聚合物,
C) 0 - 40重量份的乙烯基聚合物(C.1)和/或聚对苯二甲酸亚烷基二醇酯(C.2),
D) 0.1 - 50重量份的中空陶瓷球,
E) 0.2 - 5.0重量份的至少一种聚有机硅氧烷,
F) 0 - 20重量份的至少一种含磷耐火剂,
G) 0 - 10重量份的至少一种其它添加剂,
其中所述的所有重量份为标准化的使得所述组合物中所有组分A+B+C+D+E+F+G的重量份之和为100,
并且其中所述聚有机硅氧烷(E)包含通式(IV)的单元:
RrSiO( 4-r)/2
(IV)
其中:
- R彼此独立地为取代或未取代的烃基,
- r是1、2或3,且
- r的平均数值为1.9至2.1。
2.根据权利要求1的组合物,其特征在于组分(D)与组分(E)的比率为2:1至10:1。
3.根据权利要求1的组合物,其特征在于R选自乙烯基、烯丙基、甲基烯丙基、1-丙烯基、1-丁烯基、1-戊烯基、5-己烯基、丁二烯基、己二烯基、环戊烯基、环戊二烯基、环己烯基、乙炔基、炔丙基、1-丙炔基、甲基、3-氯丙基、3,3,3-三氟丙基、全氟己基乙基、对氯苯基和对氯苄基。
4.根据权利要求1的组合物,其特征在于烷基键合到聚有机硅氧烷(E)中所含的至少70摩尔%的Si原子上。
5.根据权利要求1的组合物,其特征在于聚有机硅氧烷(E)具有50,000至1,000,000 mm2/s的在25℃下测得的粘度。
6.根据权利要求1的组合物,其特征在于所述中空陶瓷球具有5至25重量%的Al2O3含量。
7.根据权利要求1的组合物,其特征在于所述中空陶瓷球具有50 - 700 MPa的压缩强度。
8.根据权利要求1的组合物,其特征在于所述中空陶瓷球具有0.1 - 100.0微米的平均粒径d50。
9.根据权利要求1的组合物,其特征在于组分B的接枝基料具有0.05至10.00微米的平均粒度d50值。
10.根据权利要求1的组合物,其特征在于组分B的接枝基料选自二烯橡胶、EPM橡胶、EPDM橡胶、丙烯酸酯、聚氨酯、有机硅、氯丁二烯和乙烯/乙酸乙烯酯橡胶。
11.根据权利要求1的组合物,其特征在于所述接枝聚合物(B)由以下构成:
B.1) 43重量%的27重量%丙烯腈与73重量%苯乙烯的乳液聚合物,其在
B.2) 57重量%的以平均粒径d50为0.35微米的颗粒形式交联的聚丁二烯橡胶上。
12.根据权利要求1的组合物,其特征在于含磷耐火剂(F)是通式(V)的耐火剂,
其中:
R1、R2、R3和R4彼此独立地表示在每种情况下任选卤化的C1至C8-烷基,或者在每种情况下任选被烷基和/或卤素取代的C5至C6-环烷基、在每种情况下任选被烷基和/或卤素取代的C6至C20-芳基或在每种情况下任选被烷基和/或卤素取代的C7至C12-芳烷基,
n彼此独立地表示0或1,
q是指0.80至5.00,且
X是指具有6至30个C原子的单核或多核芳族基团或具有2至30个C原子的直链或支化的脂族基团,它们能够被OH取代并能够包含最多8个醚键。
13.根据权利要求1的组合物,包含至少一种选自防火协作剂、防滴落剂、润滑剂和脱模剂、成核剂、稳定剂、抗静电剂、染料、颜料和填料的添加剂作为组分G。
14.根据权利要求1的组合物,包含至少一种选自防火协作剂、防滴落剂、润滑剂和脱模剂、成核剂、稳定剂、抗静电剂、染料、颜料和增强物质的添加剂作为组分G。
15.根据权利要求1至7之一的组合物用于制造注射成型或热成型制品的用途。
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US8349926B2 (en) | 2013-01-08 |
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WO2011073289A1 (en) | 2011-06-23 |
EP2513217B1 (en) | 2016-02-17 |
CN102725340A (zh) | 2012-10-10 |
MX2012006973A (es) | 2012-10-15 |
JP2013514410A (ja) | 2013-04-25 |
KR101773637B1 (ko) | 2017-08-31 |
KR20120115970A (ko) | 2012-10-19 |
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