CN105899573A - 共聚碳酸酯及包含该共聚碳酸酯的组合物 - Google Patents
共聚碳酸酯及包含该共聚碳酸酯的组合物 Download PDFInfo
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- CN105899573A CN105899573A CN201580002721.9A CN201580002721A CN105899573A CN 105899573 A CN105899573 A CN 105899573A CN 201580002721 A CN201580002721 A CN 201580002721A CN 105899573 A CN105899573 A CN 105899573A
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- copolycarbonate
- double
- repetitive
- hydroxyphenyl
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Abstract
本发明涉及一种共聚碳酸酯以及一种包含该共聚碳酸酯的组合物。根据本发明的共聚碳酸酯具有在聚碳酸酯的主链中引入特殊的硅氧烷化合物的结构,并且室温下的冲击强度与低温下的冲击强度之间具有小的差异,从而表现出优异的抗冲击性。
Description
[相关申请的交叉引用]
本申请要求在韩国知识产权局于2014年12月04日提交的韩国专利申请号10-2014-0173005、于2015年07月27日提交的韩国专利申请号10-2015-0106021以及于2015年11月13日提交的韩国专利申请号10-2015-0159657的权益,通过引用将它们公开的内容全部并入本申请中。
技术领域
本发明涉及共聚碳酸酯以及包含该共聚碳酸酯的组合物,以及更具体地涉及共聚碳酸酯以及包含该共聚碳酸酯的组合物,所述共聚碳酸酯被经济地生产并且室温下的冲击强度与低温下的冲击强度之间具有小的差异。
背景技术
聚碳酸酯树脂通过芳香族二醇例如双酚A与碳酸酯前体例如光气的缩聚反应制备并且具有优异的冲击强度、尺寸稳定性、耐热性和透明度。因此,聚碳酸酯树脂在例如电子和电气产品的外部材料、汽车部件、建筑材料和光学元件中具有广泛的应用用途。
近来,为了将这些聚碳酸酯树脂应用至更多的不同领域中,已经进行了许多研究以通过将两种以上的具有彼此不同结构的芳香族二醇化合物共聚并且将具有不同结构的单元引入聚碳酸酯的主链中获得所需的物理性能。
特别地,已进行了将聚硅氧烷结构引入聚碳酸酯的主链中的研究,但是这些技术大部分有生产成本高,而且当耐化学性或冲击强度,特别是低温下的冲击强度增加时,熔融指数等降低的缺点。
鉴于上述情况,本发明人进行了深入的研究以克服现有技术中遇到的上述缺点并且开发一种室温下的冲击强度与低温下的冲击强度之间具有小的差异且因此表现出优异的抗冲击性的共聚碳酸酯,而且发现将特殊的硅氧烷化合物引入如下所述的聚碳酸酯的主链中的共聚碳酸酯满足上述性能。基于这些发现完成了本发明。
发明内容
技术问题
本发明的一个目的是提供一种共聚碳酸酯,该共聚碳酸酯的室温下的冲击强度与低温下的冲击强度之间具有小的差异,从而表现出优异的抗冲击性。
本发明的另一个目的是提供一种包含上述共聚碳酸酯的组合物。
技术方案
为了实现这些目的,本发明提供一种共聚碳酸酯,包含:芳香族聚碳酸酯类第一重复单元;以及一种或多种具有硅氧烷键的芳香族聚碳酸酯类第二重复单元,其中,根据ASTM D256(1/8英寸,缺口悬臂梁法)分别在23℃和-30℃下测定的室温下的冲击强度与低温下的冲击强度的比(室温下的冲击强度/低温下的冲击强度)为1.01至1.30,而且所述室温下的冲击强度为840J/m至1000J/m。
如上所述,根据本发明的共聚碳酸酯的特征在于室温下的冲击强度与低温下的冲击强度之间具有小的差异,从而表现出优异的抗冲击性。优选地,所述室温下的冲击强度与低温下的冲击强度的比(室温下的冲击强度/低温下的冲击强度)不大于1.29、不大于1.28、不大于1.27、不大于1.26、不大于1.25、不大于1.24、不大于1.23、不大于1.22、不大于1.21、不大于1.20、不大于1.19、不大于1.18、不大于1.17、不大于1.16、不大于1.15、不大于1.14、不大于1.13、不大于1.12、不大于1.11、不大于1.10、不大于1.09或不大于1.08;并且不小于1.02、不小于1.03或不小于1.04。
优选地,所述低温下的冲击强度不小于650J/m、不小于700J/m、不小于750J/m、不小于800J/m、不小于850J/m或不小于900J/m。此外,当所述值高时,在低温下的冲击强度优异,因此没有限制到任意上限值。但是,作为一个实例,所述低温下的冲击强度可以不大于990J/m、不大于980J/m、不大于970J/m、不大于960J/m或不大于950J/m。
此外,优选地,所述室温下的冲击强度不小于850J/m、不小于860J/m、不小于870J/m、不小于880J/m、不小于890J/m、不小于900J/m、不小于910J/m、不小于920J/m、不小于930J/m、不小于940J/m、不小于950J/m或不小于960J/m。此外,当所述值较高时,在室温下的冲击强度优异,因此没有限制到任意上限值。但是,作为一个实例,所述室温下的冲击强度可以不大于1000J/m、不大于990J/m、不大于980J/m或不大于970J/m。
此外,优选地,所述共聚碳酸酯根据ASTM D1238(300℃、1.2kg条件)测定的熔融指数为3g/10min至20g/10min。
此外,优选地,所述共聚碳酸酯根据ASTM D1925测定的YI(黄色指数)为2至6.5。优选地,YI(黄色指数)不小于2;并且不大于6.0、不大于5.5、不大于5.0、不大于4.5、不大于4.0、不大于3.5、不大于3.0或不大于2.5。
此外,根据本发明的共聚碳酸酯的重均分子量为1,000g/mol至100,000g/mol以及优选地15,000g/mol至35,000g/mol。更优选地,上述重均分子量不小于20,000g/mol、不小于21,000g/mol、不小于22,000g/mol、不小于23,000g/mol、不小于24,000g/mol、不小于25,000g/mol、不小于26,000g/mol、不小于27,000g/mol或不小于28,000g/mol。此外,上述重均分子量不大于34,000g/mol、不大于33,000g/mol或不大于32,000g/mol。
此外,优选地,所述共聚碳酸酯包含两种具有硅氧烷键的芳香族聚碳酸酯类第二重复单元。
此外,所述芳香族聚碳酸酯类第一重复单元与一种或多种具有硅氧烷键的芳香族聚碳酸酯类第二重复单元的摩尔比优选地是1:0.004至0.006,并且它们的重量比优选地是1:0.04至0.07。
具体地,所述芳香族聚碳酸酯类第一重复单元通过使芳香族二醇化合物与碳酸酯前体反应形成,而且其优选地由下面化学式1表示:
[化学式1]
在上面化学式1中,
R1、R2、R3和R4各自独立地是氢、C1-10烷基、C1-10烷氧基或卤素,
Z是未被取代的或被苯基取代的C1-10亚烷基、未被取代的或被C1-10烷基取代的C3-15亚环烷基、O、S、SO、SO2或CO。
优选地,R1、R2、R3和R4各自独立地是氢、甲基、氯或溴。
此外,Z优选地是未被取代的或被苯基取代的直链或支链C1-10亚烷基,以及更优选地是亚甲基、乙烷-1,1-二基、丙烷-2,2-二基、丁烷-2,2-二基、1苯乙烷-1,1-二基或二苯基亚甲基。此外,优选地,Z是环己烷-1,1-二基、O、S、SO、SO2或CO。
优选地,所述由化学式1表示的重复单元可以由选自双(4-羟苯基)甲烷、双(4-羟苯基)醚、双(4-羟苯基)砜、双(4-羟苯基)亚砜、双(4-羟苯基)硫醚、双(4-羟苯基)甲酮、1,1-双(4-羟苯基)乙烷、双酚A、2,2-双(4-羟苯基)丁烷、1,1-双(4-羟苯基)环己烷、2,2-双(4-羟基-3,5-二溴苯基)丙烷、2,2-双(4-羟基-3,5-二氯苯基)丙烷、2,2-双(4-羟基-3-溴苯基)丙烷、2,2-双(4-羟基-3-氯苯基)丙烷、2,2-双(4-羟基-3-甲基苯基)丙烷、2,2-双(4-羟基-3,5-二甲基苯基)丙烷、1,1-双(4-羟苯基)-1-苯乙烷、双(4-羟苯基)二苯基甲烷和α,ω-双[3-(邻羟苯基)丙基]聚二甲基硅氧烷中的一种或多种芳香族二醇化合物得到。
如此处所使用,“由芳香族二元醇化合物得到”是指芳香族二醇化合物的羟基与碳酸酯前体反应形成所述由化学式1表示的重复单元。
例如,当将芳香族二醇化合物双酚A与碳酸酯前体三光气聚合时,所述由化学式1表示的重复单元由下面化学式1-1表示:
[化学式1-1]
此处所使用的碳酸酯前体可以包括选自碳酸二甲酯、碳酸二乙酯、碳酸二丁酯、碳酸二环己酯、碳酸二苯酯、碳酸二甲苯酯、碳酸二(氯苯)酯、碳酸二间甲酚酯、碳酸二萘酯、碳酸二(联苯)酯、光气、三光气、双光气、溴光气以及二卤甲酸酯中的一种或多种。优选地,可以使用三光气或光气。
所述一种或多种具有硅氧烷键的芳香族聚碳酸酯类第二重复单元通过使一种或多种硅氧烷化合物与碳酸酯前体反应形成,并且其优选地包含由下面化学式2表示的重复单元和由下面化学式3表示的重复单元:
[化学式2]
在上面化学式2中,
各个X1独立地是C1-10亚烷基,
各个R5独立地是氢;未被取代的或被环氧乙烷基、环氧乙烷基取代的C1-10烷氧基或C6-20芳基取代的C1-15烷基;卤素;C1-10烷氧基;烯丙基;C1-10卤代烷基;或C6-20芳基,以及
n是10至200的整数,
[化学式3]
在上面化学式3中,
各个X2独立地是C1-10亚烷基,
各个Y1独立地是氢、C1-6烷基、卤素、羟基、C1-6烷氧基或C6-20芳基,
各个R6独立地是氢;未被取代的或被环氧乙烷基、环氧乙烷基取代的C1-10烷氧基或C6-20芳基取代的C1-15烷基;卤素;C1-10烷氧基;烯丙基;C1-10卤代烷基;或C6-20芳基,以及
m是10至200的整数。
在化学式2中,优选各个X1独立地是C2-10亚烷基,更优选C2-4亚烷基以及最优选丙烷-1,3-二基。
此外,优选地,各个R5独立地是氢、甲基、乙基、丙基、3-苯丙基、2-苯丙基、3-(环氧乙烷基甲氧基)丙基、氟、氯、溴、碘、甲氧基、乙氧基、丙氧基、烯丙基、2,2,2-三氟乙基、3,3,3-三氟丙基、苯基或萘基。此外,优选各个R5独立地是C1-10烷基、较优选C1-6烷基、更优选C1-3烷基以及最优选甲基。
此外,优选地,n是不小于10、不小于15、不小于20、不小于25、不小于30、不小于31或不小于32;并且不大于50、不大于45、不大于40、不大于39、不大于38或不大于37的整数。
在化学式3中,优选各个X2独立地是C2-10亚烷基、更优选C2-6亚烷基以及最优选异亚丁基。
此外,优选地,Y1是氢。
此外,优选地,各个R6独立地是氢、甲基、乙基、丙基、3-苯丙基、2-苯丙基、3-(环氧乙烷基甲氧基)丙基、氟、氯、溴、碘、甲氧基、乙氧基、丙氧基、烯丙基、2,2,2-三氟乙基、3,3,3-三氟丙基、苯基或萘基。此外,优选地,各个R6独立地是C1-10烷基、较优选C1-6烷基、更优选C1-3烷基以及最优选甲基。
优选地,m是不小于40、不小于45、不小于50、不小于55、不小于56、不小于57或不小于58;并且不大于80、不大于75、不大于70、不大于65、不大于64、不大于63或不大于62的整数。
所述由化学式2表示的重复单元和由化学式3表示的重复单元分别由由下面化学式2-1表示的硅氧烷化合物和由下面化学式3-1表示的硅氧烷化合物得到:
[化学式2-1]
在上面化学式2-1中,X1、R5和n与此前定义相同。
[化学式3-1]
在上面化学式3-1中,X2、Y1、R6和m与此前定义相同。
如此处所使用,“由硅氧烷化合物得到”是指各个硅氧烷化合物的羟基与碳酸酯前体反应形成由化学式2表示的重复单元和由化学式3表示的重复单元。此外,所述用于形成由化学式2和3表示的重复单元的碳酸酯前体与那些所述用于形成上述由化学式1表示的重复单元的碳酸酯前体相同。
所述用于制备由化学式2-1表示的硅氧烷化合物和由化学式3-1表示的硅氧烷化合物的方法由下面反应图示1和2表示:
[反应图示1]
在上面反应图示1中,
X1'是C2-10烯基,以及
X1、R5和n与此前定义相同。
[反应图示2]
在上面反应图示2中,
X2'是C2-10烯基,以及
X2、Y1、R6和m与此前定义相同。
在反应图示1和反应图示2中,所述反应优选在金属催化剂的存在下进行。作为所述金属催化剂,优选使用铂催化剂。此处所使用的铂催化剂可以包括选自Ashby催化剂、Karstedt催化剂、Lamoreaux催化剂、Speier催化剂、PtCl2(COD)、PtCl2(苄腈)2和H2PtBr6中的一种或多种。基于100重量份的由化学式7或9表示的化合物,所述金属催化剂的使用量可以是不小于0.001重量份、不小于0.005重量份或不小于0.01重量份;并且不大于1重量份、不大于0.1重量份或不大于0.05重量份。
此外,上述反应温度优选为80℃至100℃。此外,上述反应时间优选为1小时至5小时。
此外,所述由化学式7或9表示的化合物可以通过使有机二硅氧烷与有机环硅氧烷在酸性催化剂的存在下反应来制备,而且n和m可以通过调节反应物的使用量来调节。
所述反应温度优选为50℃至70℃。此外,所述反应时间优选为1小时至6小时。
上述有机二硅氧烷可以包括选自四甲基二硅氧烷、四苯基二硅氧烷、六甲基二硅氧烷和六苯基二硅氧烷中的一种或多种。此外,上述有机环硅氧烷可以包括例如有机环四硅氧烷。作为它的一个实例,可以包括八甲基环四硅氧烷和八苯基环四硅氧烷等。
基于100重量份的有机环硅氧烷,上述有机二硅氧烷的使用量可以是不小于0.1重量份或不小于2重量份;并且不大于10重量份或不大于8重量份。
可以在此处使用的上述酸性催化剂包括选自H2SO4、HClO4、AlCl3、SbCl5、SnCl4和酸性粘土(漂白土)中的一种或多种。此外,基于100重量份的所述有机环硅氧烷,所述酸性催化剂的使用量可以是不小于0.1重量份、不小于0.5重量份或不小于1重量份;并且不大于10重量份、不大于5重量份或不大于3重量份。
具体地,通过调节所述由化学式2表示的重复单元和由化学式3表示的重复单元的含量,可以同时提高共聚碳酸酯的低温下的冲击强度和熔融指数。优选地,所述重复单元之间的重量比可以是从1:99至99:1。优选地,所述重量比是从3:97至97:3、从5:95至95:5、从10:90至90:10或从15:85至85:15以及更优选地从20:80至80:20。上述重复单元的重量比对应于硅氧烷化合物例如由化学式2-1表示的硅氧烷化合物与由化学式3-1表示的硅氧烷化合物的重量比。
优选地,所述由化学式2表示的重复单元由下面化学式2-2表示:
[化学式2-2]
在上面化学式2-2中,R5和n与此前定义相同。优选地,R5是甲基。
此外,优选地,所述由化学式3表示的重复单元由下面化学式3-2表示:
[化学式3-2]
在上面化学式3-2中,R6和m与此前定义相同。优选地,R6是甲基。
此外,优选地,由化学式1-1表示的重复单元、由化学式2-2表示的重复单元和由化学式3-2表示的重复单元都包含在根据本发明的聚碳酸酯中。
此外,本发明提供一种制备共聚碳酸酯的方法,该方法包括使芳香族二醇化合物、碳酸酯前体以及一种或多种硅氧烷化合物聚合的步骤。
所述芳香族二醇化合物、碳酸酯前体以及一种或多种硅氧烷化合物与此前描述相同。
在所述聚合过程中,基于总计100重量%的所述芳香族二醇化合物、碳酸酯前体和一种或多种硅氧烷化合物,所述一种或多种硅氧烷化合物的使用量可以是不小于0.1重量%、不小于0.5重量%、不小于1重量%或不小于1.5重量%;并且不大于20重量%、不大于10重量%、不大于7重量%、不大于5重量%、不大于4重量%、不大于3重量%或不大于2重量%。此外,基于总计100重量%的所述芳香族二醇化合物、碳酸酯前体和一种或多种硅氧烷化合物,所述芳香族二醇化合物的使用量可以是不小于40重量%、不小于50重量%或不小于55重量%;并且不大于80重量%、不大于70重量%或不大于65重量%。基于总计100重量%的所述芳香族二醇化合物、碳酸酯前体和一种或多种硅氧烷化合物,所述碳酸酯前体的使用量可以是不小于10重量%、不小于20重量%或不小于30重量%;并且不大于60重量%、不大于50重量%或不大于40重量%。
此外,作为所述聚合方法,可以使用界面聚合法作为一个实例。在此情况下,有聚合反应能够在大气压、低温下进行而且分子量容易控制的效果。上述界面聚合优选地在酸结合剂和有机溶剂的存在下进行。此外,上述界面聚合可以包括例如进行预聚合然后加入偶联剂以及再进行聚合的步骤。在此情况下,可以获得具有高分子量的共聚碳酸酯。
在所述界面聚合中使用的物质没有特别限制,只要它们可以在聚碳酸酯的聚合中使用即可。其使用量可以根据需要控制。
所述酸结合剂可以包括例如,碱金属氢氧化物例如氢氧化钠或氢氧化钾,或胺类化合物例如吡啶。
所述有机溶剂没有特别限制,只要其是通常在聚碳酸酯的聚合中使用的溶剂即可。作为一个实例,可以使用卤代烃例如二氯甲烷或氯苯。
此外,在所述界面聚合过程中,还可以使用用于加速反应的反应加速剂,例如叔胺化合物例如三乙胺、四正丁基溴化铵和四正丁基溴化鏻或季铵化合物或季鏻化合物。
在所述界面聚合中,反应温度优选地从0℃至40℃以及反应时间优选地从10分钟至5小时。此外,在所述界面聚合反应中,pH优选地保持在9以上或11以上。
此外,所述界面聚合可以通过进一步地包含分子量调节剂来进行。所述分子量调节剂可以在聚合反应起始之前、聚合反应起始过程中或聚合反应起始之后加入。
作为上述分子量调节剂,可以使用单烷基苯酚。作为一个实例,所述单烷基苯酚是选自对叔丁基苯酚、对枯基苯酚、癸基苯酚、十二烷基苯酚、十四烷基苯酚、十六烷基苯酚、十八烷基苯酚、二十烷基苯酚、二十二烷基苯酚和三十烷基苯酚中的一种或多种,而且优选地为对叔丁基苯酚。在此情况下,调节分子量的效果巨大。
基于100重量份的所述芳香族二醇化合物,上述分子量调节剂的含量例如是不小于0.01重量份、不小于0.1重量份或不小于1重量份并且不大于10重量份、不大于6重量份或不大于5重量份。在此范围内,可以获得所需的分子量。
此外,本发明提供一种包含上述共聚碳酸酯和聚碳酸酯的聚碳酸酯组合物。
所述共聚碳酸酯可以单独使用,但也可以根据需要与聚碳酸酯一起使用以控制共聚碳酸酯的物理性能。
上述聚碳酸酯与根据本发明的共聚碳酸酯的区别在于未将聚硅氧烷结构引入聚碳酸酯的主链中。
优选地,上述聚碳酸酯包含由下面化学式4表示的重复单元:
[化学式4]
在上面化学式4中,
R'1、R'2、R'3和R'4各自独立地是氢、C1-10烷基、C1-10烷氧基或卤素,
Z'是未被取代的或被苯基取代的C1-10亚烷基、未被取代的或被C1-10烷基取代的C3-15亚环烷基、O、S、SO、SO2或CO。
此外,优选地,上述聚碳酸酯的重均分子量为15,000g/mol至35,000g/mol。更优选地,上述重均分子量(g/mol)不小于20,000、不小于21,000、不小于22,000、不小于23,000、不小于24,000、不小于25,000、不小于26,000、不小于27,000或不小于28,000。此外,上述重均分子量(g/mol)不大于34,000、不大于33,000或不大于32,000。
所述由化学式4表示的重复单元通过使芳香族二醇化合物与碳酸酯前体反应形成。此处可以使用的芳香族二醇化合物和碳酸酯前体与此前描述的由化学式1表示的重复单元使用的芳香族二醇化合物和碳酸酯前体相同。
优选地,化学式4中的R'1、R'2、R'3和R'4和Z'分别与此前描述的化学式1中R1、R2、R3、R4和Z相同。
此外,优选地,所述由化学式4表示的重复单元由下面化学式4-1表示:
[化学式4-1]
在所述聚碳酸酯组合物中,共聚碳酸酯与聚碳酸酯的重量比优选地从99:1至1:99、更优选地从90:10至50:50以及最优选地从80:20至60:40。
此外,本发明提供了一种包含上述共聚碳酸酯或聚碳酸酯组合物的制品。
优选地,上述制品是注射成型制品。此外,所述制品还可以包含例如选自抗氧化剂、热稳定剂、光稳定剂、塑化剂、抗静电剂、成核剂、阻燃剂、润滑剂、抗冲击增强剂、荧光增白剂、紫外线吸收剂、颜料和染料中的一种或多种。
制备所述制品的方法可以包括如下步骤:利用混合器混合根据本发明的共聚碳酸酯与添加剂例如抗氧化剂,用挤出机将所得混合物挤出成型以制备小球,干燥所述小球然后用注模机注射经干燥的小球。
有益效果
如前文所述,根据本发明,将特殊的硅氧烷化合物引入聚碳酸酯的主链中的共聚碳酸酯的室温下的冲击强度与低温下的冲击强度之间具有小的差异,且因此表现出优异的抗冲击性。
具体实施方式
下面,为了帮助理解本公开的内容,将提供优选实施方案。但是,提供这些实施例只是为了说明本发明,而且不应被解释为通过所述实施例限制本发明。
制备实施例1:AP-PDMS(n=34)的制备
混合47.60g(160mmol)的八甲基环四硅氧烷和2.40g(17.8mmol)的四甲基二硅氧烷。然后将混合物与1重量份(相对于100重量份的八甲基环四硅氧烷)的酸性粘土(DC-A3)一起放入3L的烧瓶中,然后在60℃下反应4小时。反应完成后,用乙酸乙酯稀释反应产物然后用硅藻土快速过滤。通过1H NMR确定由此制备的端基未改性的聚有机硅氧烷的重复单元(n)为34。
向所得到的端基未改性聚有机硅氧烷中加入4.81g(35.9mmol)的2-烯丙基苯酚和0.01g(50ppm)的Karstedt铂催化剂,然后在90℃下反应3小时。反应完成后,通过在120℃和1托的条件下进行蒸发去除未反应的硅氧烷。由此制备的端基改性聚有机硅氧烷称为AP-PDMS(n=34)。AP-PDMS是淡黄色油并且利用Varian 500MHz通过1H NMR确定重复单元为(n)为34,并且不需要进一步纯化。
制备实施例2:MBHB-PDMS(m=58)的制备
混合47.60g(160mmol)的八甲基环四硅氧烷和1.5g(11mmol)的四甲基二硅氧烷。然后将混合物与1重量份(相对于100重量份的八甲基环四硅氧烷)的酸性粘土(DC-A3)一起引入3L的烧瓶中,然后在60℃下反应4小时。反应完成后,用乙酸乙酯稀释反应产物然后用硅藻土快速过滤。通过1H NMR确定由此制备的端基未改性聚有机硅氧烷的重复单元(m)为58。
向所得到的端基未改性聚有机硅氧烷中加入6.13g(29.7mmol)的3-甲基-3-丁烯基4-羟基苯甲酸酯和0.01g(50ppm)的Karstedt铂催化剂,然后在90℃下反应3小时。反应完成后,通过在120℃和1托的条件下进行蒸发去除未反应的硅氧烷。由此制备的端基改性聚有机硅氧烷称为MBHB-PDMS(m=58)。MBHB-PDMS是淡黄色油并且利用Varian 500MHz通过1H NMR确定重复单元为(m)为58,并且不需要进一步纯化。
制备实施例3:丁香酚-PDMS
混合47.60g(160mmol)的八甲基环四硅氧烷和1.7g(13mmol)的四甲基二硅氧烷。然后将混合物与1重量份(相对于100重量份八甲基环四硅氧烷)的酸性粘土(DC-A3)一起放入3L的烧瓶中,然后在60℃下反应4小时。反应完成后,用乙酸乙酯稀释反应产物然后用硅藻土快速过滤。通过1H NMR确定由此制备的端基未改性的聚有机硅氧烷的重复单元(n)为50。
向所得到的端基未改性聚有机硅氧烷中加入6.13g(29.7mmol)的丁香酚和0.01g(50ppm)的Karstedt铂催化剂,然后在90℃下反应3小时。反应完成后,通过在120℃和1托的条件下进行蒸发去除未反应的硅氧烷。由此制备的端基改性聚有机硅氧烷称为丁香酚-PDMS。丁香酚-PDMS是淡黄色油并且利用Varian 500MHz通过1H NMR确定重复单元为(n)为50,并且不需要进一步纯化。
实施例1
向聚合反应器中加入1784g的水、385g的NaOH和232g的BPA(双酚A),然后在N2气氛下混合溶解。将4.3g的PTBP(对叔丁基苯酚)和5.91g的在制备实施例1中制备的AP-PDMS(n=34)与0.66g的在制备实施例2中制备的MBHB-PDMS(m=58)混合溶液(重量比为90:10)溶解在MC(二氯甲烷)中然后加入其中。然后。将128g的TPG(三光气)溶解在MC中,将溶解的TPG溶液加入其中,在将TPG溶液的pH保持在11以上的同时反应1小时。10分钟后,向其中加入46g的TEA(三乙胺)以进行偶联反应。在总反应时间为1小时以及20分钟后,pH降低至4以去除TEA,然后通过用蒸馏水清洗三次将所制备的聚合物的pH调节至6至7的中性pH。将由此获得的聚合物在甲醇和己烷的混合溶液中再沉淀,然后在120℃下干燥以获得最终共聚碳酸酯。
实施例2
除了AP-PDMS(n=34)与MBHB-PDMS(m=58)的重量比为95:5以外,以与实施例1中相同的方法制备共聚碳酸酯。
实施例3
除了AP-PDMS(n=34)与MBHB-PDMS(m=58)的重量比为97:3以外,以与实施例1中相同的方法制备共聚碳酸酯。
实施例4
除了AP-PDMS(n=34)与MBHB-PDMS(m=58)的重量比为99:1以外,以与实施例1中相同的方法制备共聚碳酸酯。
实施例5
除了AP-PDMS(n=34)与MBHB-PDMS(m=58)的重量比为95:5并且调节分子量调节剂PTBT(对叔丁基苯酚)的添加量以外,以与实施例1中相同的方法制备共聚碳酸酯。
对比实施例1
向聚合反应器中加入1784g的水、385g的NaOH和232g的BPA(双酚A),然后在N2气氛下混合溶解。将4.3g的PTBP(对叔丁基苯酚)和6.57g的在制备实施例3中制备的丁香酚-PDMS溶解在MC(二氯甲烷)中然后加入其中。然后,将128g的TPG(三光气)溶解在MC中,将溶解的TPG溶液加入其中,在将TPG溶液的pH保持在11以上的同时反应1小时。10分钟后,向其中加入46g的TEA(三乙胺)以进行偶联反应。在总反应时间为1小时以及20分钟后,pH降低至4以去除TEA,然后通过用蒸馏水清洗三次将所制备的聚合物的pH调节至6至7的中性pH。将由此获得的聚合物在甲醇和己烷的混合溶液中再沉淀,然后在120℃下干燥以获得最终共聚碳酸酯。
对比实施例2
除了使用AP-PDMS代替丁香酚-PDMS以外,以与对比实施例1中相同的方法制备共聚碳酸酯。
实验实施例:共聚碳酸酯的特性的确定
在实施例和对比实施例中制备的共聚碳酸酯的重均分子量通过GPC利用PC标准和Agilent 1200系列测定。
此外,相对于1重量份的在实施例和对比实施例中制备的各个共聚碳酸酯,向其中加入0.050重量份的三(2,4-二叔丁基苯基)亚磷酸酯、0.010重量份的十八烷基-3-(3,5-二叔丁基-4-羟苯基)丙酸酯和0.030重量份的季戊四醇四硬脂酸酯,然后利用配有通风口的Φ30mm双螺杆挤出机将所得混合物制成小球,然后利用JSW Co.,Ltd的N-20C注模机在300℃的料筒温度和80℃的模塑温度下注射成型以制备所需的试样。
以下面方式测定上述试样的特性,而且结果在下面表1中示出。
1)室温下的冲击强度:根据ASTM D256(1/8英寸,缺口悬臂梁法)在23℃下测定。
2)低温下的冲击强度:根据ASTM D256(1/8英寸,缺口悬臂梁法)在-30℃下测定。
3)YI(黄色指数):在300℃下将试样(宽度/长度/厚度=60mm/40mm/3mm)注射成型,然后根据ASTM D1925利用Color-Eye 7000A(X-rite Inc.)在下面条件下测定YI(黄色指数)。
-测定温度:室温(23℃)
-孔径尺寸:大孔径(large area of view)
-测定方法:在光谱范围(360nm至750nm)内测定透过率。
[表1]
如上面表1中所示,与对比实施例1和2相比,根据本发明的共聚碳酸酯具有优异的低温下的冲击强度和室温下的冲击强度。特别地,根据本发明的共聚碳酸酯的室温下的冲击强度与低温下的冲击强度之间具有小的差异,从而表现出优异的抗冲击性。
Claims (15)
1.一种共聚碳酸酯,包含:芳香族聚碳酸酯类第一重复单元;以及一种或多种具有硅氧烷键的芳香族聚碳酸酯类第二重复单元,
其中,根据ASTM D256(1/8英寸,缺口悬臂梁法)分别在23℃和-30℃下测定的室温下的冲击强度与低温下的冲击强度的比(室温下的冲击强度/低温下的冲击强度)为1.01至1.30,而且所述室温下的冲击强度为840J/m至1000J/m。
2.如权利要求1所述的共聚碳酸酯,其中,所述低温下的冲击强度为650J/m至950J/m。
3.如权利要求1所述的共聚碳酸酯,其中,根据ASTM D1238(300℃、1.2kg条件)测定的熔融指数为3g/10min至20g/10min。
4.如权利要求1所述的共聚碳酸酯,其中,所述共聚碳酸酯的重均分子量为1,000g/mol至100,000g/mol。
5.如权利要求1所述的共聚碳酸酯,其中,所述共聚碳酸酯包含两种具有硅氧烷键的芳香族聚碳酸酯类第二重复单元。
6.如权利要求1所述的共聚碳酸酯,其中,所述第一重复单元由下面化学式1表示:
[化学式1]
在上面化学式1中,
R1、R2、R3和R4各自独立地是氢、C1-10烷基、C1-10烷氧基或卤素,以及
Z是未被取代的或被苯基取代的C1-10亚烷基、未被取代的或被C1-10烷基取代的C3-15亚环烷基、O、S、SO、SO2或CO。
7.如权利要求6所述的共聚碳酸酯,其中,所述由化学式1表示的重复单元由选自双(4-羟苯基)甲烷、双(4-羟苯基)醚、双(4-羟苯基)砜、双(4-羟苯基)亚砜、双(4-羟苯基)硫醚、双(4-羟苯基)甲酮、1,1-双(4-羟苯基)乙烷、双酚A、2,2-双(4-羟苯基)丁烷、1,1-双(4-羟苯基)环己烷、2,2-双(4-羟基-3,5-二溴苯基)丙烷、2,2-双(4-羟基-3,5-二氯苯基)丙烷、2,2-双(4-羟基-3-溴苯基)丙烷、2,2-双(4-羟基-3-氯苯基)丙烷、2,2-双(4-羟基-3-甲基苯基)丙烷、2,2-双(4-羟基-3,5-二甲基苯基)丙烷、1,1-双(4-羟苯基)-1-苯乙烷、双(4-羟苯基)二苯基甲烷和α,ω-双[3-(邻羟苯基)丙基]聚二甲基硅氧烷中的一种或多种芳香族二醇化合物得到。
8.如权利要求6所述的共聚碳酸酯,其中,
所述化学式1由下面化学式1-1表示:
[化学式1-1]
9.如权利要求1所述的共聚碳酸酯,其中,所述第二重复单元包含由下面化学式2表示的重复单元和由下面化学式3表示的重复单元:
[化学式2]
在上面化学式2中,
各个X1独立地是C1-10亚烷基,
各个R5独立地是氢;未被取代的或被环氧乙烷基、环氧乙烷基取代的C1-10烷氧基或C6-20芳基取代的C1-15烷基;卤素;C1-10烷氧基;烯丙基;C1-10卤代烷基;或C6-20芳基,以及
n是10至200的整数,
[化学式3]
在上面化学式3中,
各个X2独立地是C1-10亚烷基,
各个Y1独立地是氢、C1-6烷基、卤素、羟基、C1-6烷氧基或C6-20芳基,
各个R6独立地是氢;未被取代的或被环氧乙烷基、环氧乙烷基取代的C1-10烷氧基或C6-20芳基取代的C1-15烷基;卤素;C1-10烷氧基;烯丙基;C1-10卤代烷基;或C6-20芳基,以及
m是10至200的整数。
10.如权利要求9所述的共聚碳酸酯,其中,所述由化学式2表示的重复单元与由化学式3表示的重复单元的的重量比为99:1至1:99。
11.如权利要求9所述的共聚碳酸酯,其中,所述由化学式2表示的重复单元由下面化学式2-2表示:
[化学式2-2]
12.如权利要求9所述的共聚碳酸酯,其中,所述由化学式3表示的重复单元由下面化学式3-2表示:
[化学式3-2]
13.一种聚碳酸酯组合物,包含权利要求1至12中任一项所述的共聚碳酸酯和聚碳酸酯。
14.如权利要求13所述的聚碳酸酯组合物,其中,在聚碳酸酯的主链中未引入聚硅氧烷结构。
15.如权利要求13所述的聚碳酸酯组合物,其中,所述聚碳酸酯包含由下面化学式4表示的重复单元:
[化学式4]
在上面化学式4中,
R'1、R'2、R'3和R'4各自独立地是氢、C1-10烷基、C1-10烷氧基或卤素,以及
Z'是未被取代的或被苯基取代的C1-10亚烷基、未被取代的或被C1-10烷基取代的C3-15亚环烷基、O、S、SO、SO2或CO。
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