CN105899576A - 共聚碳酸酯以及包含该共聚碳酸酯的组合物 - Google Patents
共聚碳酸酯以及包含该共聚碳酸酯的组合物 Download PDFInfo
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- CN105899576A CN105899576A CN201580002908.9A CN201580002908A CN105899576A CN 105899576 A CN105899576 A CN 105899576A CN 201580002908 A CN201580002908 A CN 201580002908A CN 105899576 A CN105899576 A CN 105899576A
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- copolycarbonate
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- YXFVVABEGXRONW-UHFFFAOYSA-N Cc1ccccc1 Chemical compound Cc1ccccc1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种共聚碳酸酯以及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其中将特殊的硅氧烷化合物引入聚碳酸酯的主链中的结构,从而同时表现出提高的耐化学性和冲击强度。
Description
[相关申请的交叉引用]
本申请要求向韩国知识产权局于2014年12月04日提交的韩国专利申请号10-2014-0173005、于2015年09月10日提交的韩国专利申请号10-2015-0128296以及于2015年11月13日提交的韩国专利申请号10-2015-0159658的权益,上述申请的全部公开内容通过引用的方式并入本申请中。
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同时具有提高的耐化学性和冲击强度。
背景技术
聚碳酸酯树脂通过芳香族二元醇例如双酚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,聚碳酸酯树脂可以应用于广泛的用途中,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。
近来,为了将这些聚碳酸酯树脂应用至更多的领域中,已经进行了各种研究以通过将两种或多种彼此具有不同结构的芳香族二元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来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的缺点,而且无法同时提高耐化学性和冲击强度。
考虑到上述情况,本发明人进行了深入的研究以解决现有技术中遇到的上述缺点并开发同时具有提高的耐化学性和冲击强度的共聚碳酸酯,而且发现如下所述的其中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
本发明的一个目的在于提供一种同时具有提高的耐化学性和冲击强度的共聚碳酸酯。
本发明的另一个目的在于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。
本发明的另一个目的在于提供一种包含上述共聚碳酸酯或上述聚碳酸酯组合物的制品。
技术方案
为了实现这些目的,本发明提供了一种共聚碳酸酯,该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,并且满足下面式1:
[式1]
TS/TS0≥0.80
在所述式1中,
TS0是根据ASTM D638测定的拉伸应力,以及
TS表示在根据ASTM D543(方法B)与乙酸乙酯接触168小时以后根据ASTM D638测定的拉伸应力。
如此处所使用,式1涉及根据本发明的共聚碳酸酯的耐化学性,表示共聚碳酸酯与特定溶剂接触特定时间段引起的拉伸应力的变化。如果式1中的TS/TS0为1,是指不管与特定溶剂的接触,共聚碳酸酯的拉伸应力没有变化。因此,这表示随着TS/TS0的值的增加,耐化学性优异。
具体地,根据本发明的共聚碳酸酯拉伸应力变化小,特别是当与乙酸乙酯接触时。具体地,在所述式1中,TS/TS0不小于0.81、不小于0.82、不小于0.83、不小于0.84、不小于0.85、不小于0.86、不小于0.87、不小于0.88、不小于0.89或者不小于0.90。此外,在所述式1中,TS/TS0可以例如不大于1或不大于0.99。
此外,根据本发明的共聚碳酸酯,除了乙酸乙酯以外,即使在与甲苯接触时也具有小的拉伸应力变化。具体地,根据本发明的共聚碳酸酯满足下面式2:
[式2]
TS/TS0≥0.50
在所述式2中,
TS0是根据ASTM D638测定的拉伸应力,以及
TS表示在根据ASTM D543(方法B)与甲苯接触168小时以后根据ASTMD638测定的拉伸应力。
具体地,在所述式2中,TS/TS0不小于0.51、不小于0.52、不小于0.53、不小于0.54或不小于0.55。此外,在所述公式2中,TS/TS0可以例如不大于1、不大于0.99、不大于0.98、不大于0.97、不大于0.96或不大于0.95。
根据本发明的共聚碳酸酯,除了乙酸乙酯和甲苯以外,即使在与盐酸、氢氧化钠或甲醇接触时也具有小的拉伸强度变化。当如式1或2中所示将TS/TS0应用至盐酸、氢氧化钠或甲醇中时,所述值不小于0.95且不大于1。
此外,除了上述优异的耐化学性以外,根据本发明的共聚碳酸酯具有优异的冲击强度例如低温冲击强度和室温冲击强度。
所述低温冲击强度在-30℃下根据ASTM D256(1/8英寸,缺口悬臂梁)测定。优选地,该低温冲击强度不小于600J/m、不小于650J/m、不小于700J/m、不小于710J/m、不小于720J/m、不小于730J/m、不小于740J/m或不小于750J/m。此外,当所述值越高时,低温冲击强度优异,且因此不限于任意上限值。但是,作为一个实施例,所述低温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、不大于950J/m、不大于940J/m、不大于930J/m、不大于920J/m或不大于910J/m。
所述室温冲击强度根据ASTM D256(1/8英寸,缺口悬臂梁)测定。优选地,所述室温冲击强度不小于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,当所述值越高时,室温下的冲击强度优异,且因此不限于任意上限值。但是,作为一个实施例,所述室温冲击强度可以不大于990J/m、不大于980J/m或不大于970J/m。
此外,根据本发明的共聚碳酸酯具有1,000g/mol至100,000g/mol以及优选地15,000g/mol至35,000g/mol的重均分子量。
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、不大于32,000g/mol或不大于31,000g/mol。
此外,优选地,根据本发明的共聚碳酸酯具有根据ASTM D1238(300℃及1.2kg的条件)测定的3至10的熔体指数。优选地,所述熔体指数不小于4、不小于5或不小于6;并且不大于9或不大于8。
此外,优选地,根据本发明的共聚碳酸酯可以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,在根据本发明的共聚碳酸酯中,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可以优选为1:0.001-0.006,和/或它们的重量比可以是1:0.01-0.03。
此外,在根据本发明的共聚碳酸酯中,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元醇化合物与碳酸酯前体反应形成,其可以优选地由下面化学式1表示:
[化学式1]
在所述化学式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是未被取代或被苯基取代的C1-10亚烷基、未被取代或被C1-10烷基取代的C3-15亚环烷基、O、S、SO、SO2或CO。
优选地,在化学式1中,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-苯基乙烷-1,1-二基或者二苯基亚甲基。此外,优选,Z为环己烷-1,1-二基、O、S、SO、SO2或者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-羟基苯基)甲烷、双(4-羟基苯基)醚、双(4-羟基苯基)砜、双(4-羟基苯基)亚砜、双(4-羟基苯基)硫醚、双(4-羟基苯基)甲酮、1,1-双(4-羟基苯基)乙烷、双酚A、2,2-双(4-羟基苯基)丁烷、1,1-双(4-羟基苯基)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-羟基苯基)-1-苯基乙烷、双(4-羟基苯基)二苯基甲烷和α,ω-双[3-(邻羟基苯基)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’是指芳香族二元醇化合物的羟基与碳酸酯前体反应以形成所述由化学式1表示的重复单元。
例如,当将为芳香族二元醇化合物的双酚A与为碳酸酯前体的三光气聚合时,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(bis(diphenyl)carbonate)、光气、三光气、二光气、溴光气以及二卤甲酸酯(bishalo formate)中的一种或多种。优选地,可以使用三光气或光气。
此外,在根据本发明的共聚碳酸酯中,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,并且它们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]
在所述化学式2中,
各个X1独立地是C1-10亚烷基,
各个R5独立地是氢;未取代或者被环氧乙烷基(oxiranyl)、被环氧乙烷基取代的C1-10烷氧基或被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]
在所述化学式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;未取代或者被环氧乙烷基(oxiranyl)、被环氧乙烷基取代的C1-10烷氧基或被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,各个X1独立地优选C2-10亚烷基,更优选C2-4亚烷基以及最优选为丙烷-1,3-二基。
此外,优选地,各个R5独立地是氢、甲基、乙基、丙基、3-苯基丙基、2-苯基丙基、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,各个R5独立地优选为C1-10烷基、更优选为C1-6烷基、还更优选为C1-3烷基以及最优选为甲基。
此外,优选地,n是不小于10的整数、不小于15的整数、不小于20的整数、不小于25的整数、不小于30的整数、不小于31的整数或不小于32的整数;并且不大于50的整数、不大于45的整数、不大于40的整数、不大于39的整数、不大于38的整数或不大于37的整数。
在化学式3中,各个X2独立地优选为C2-10亚烷基、更优选为C2-6亚烷基以及最优选为异亚丁基。
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-苯基丙基、2-苯基丙基、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、更优选为C1-6烷基、还更优选为C1-3烷基以及最优选为甲基。
优选地,m是不小于40的整数、不小于45的整数、不小于50的整数、不小于55的整数、不小于56的整数、不小于57的整数或不小于58的整数;并且不大于80的整数、不大于75的整数、不大于70的整数、不大于65的整数、不大于64的整数、不大于63的整数或不大于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]
在所述化学式2-1中,X1、R5和n与前面定义相同。
[化学式3-1]
在所述化学式3-1中,X2、Y1、R6和m与前面定义相同。
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以形成由化学式2表示的重复单元和由化学式3表示的重复单元。此外,所述可以用于形成由化学式2和3表示的重复单元的碳酸酯前体与所述可以用于形成由化学式1表示的重复单元的碳酸酯前体所描述的那些相同。
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分别由下面反应图示1和2表示:
[反应图示1]
在所述反应图示1中,
X1'是C2-10烯基,以及
X1、R5和n与前面定义相同。
[反应图示2]
在所述反应图示2中,
X2'是C2-10烯基,以及
X2、Y1、R6和m与前面定义相同
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Pt催化剂。此处所使用的Pt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(PtCl2(benzonitrile)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,可以使用不小于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重量份的金属催化剂。
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可以通过调节使用的反应物的量来调节。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。作为其中的一个实例,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重量份的有机环硅氧烷,可以使用不小于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重量份的酸性催化剂。
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耐化学性和冲击强度。优选地,上述重复单元之间的重量比可以是1:99至99:1。优选地,所述重量比是3:97至97:3、5:95至95:5、10:90至90:10或15:85至85:15,以及更优选地为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]
在所述化学式2-2中,R5和n与前面描述相同。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]
在所述化学式3-2中,R6和m与前面描述相同。优选地,R6是甲基。
此外,优选地,根据本发明的共聚碳酸酯包含由化学式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表示的重复单元三者。
此外,本发明提供了一种制备共聚碳酸酯的方法,该方法包括将芳香族二元醇化合物、碳酸酯前体以及一种或多种硅氧烷化合物聚合的步骤。
所述芳香族二元醇化合物、碳酸酯前体以及一种或多种硅氧烷化合物与前面描述相同。
在所述聚合的过程中,基于100重量%的全部芳香族二元醇化合物、碳酸酯前体和一种或多种硅氧烷化合物,可以使用不小于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%的一种或多种硅氧烷化合物。此外,基于100重量%的全部芳香族二元醇化合物、碳酸酯前体和一种或多种硅氧烷化合物,可以使用不小于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%的上述芳香族二元醇化合物。基于100重量%的全部芳香族二元醇化合物、碳酸酯前体和一种或多种硅氧烷化合物,可以使用不小于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%的上述碳酸酯前体。
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,有聚合反应能够在低温和大气压力下进行的效果,且因此分子量容易控制。上述界面聚合优选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。
在所述界面聚合物中使用的材料没有特别限制,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,只要其是通常可以用于聚碳酸酯的聚合的溶剂即可。作为一个实例,可以使用卤代烃例如二氯甲烷或氯苯。
此外,在所述界面聚合的过程中,还可以使用用于加速反应的反应加速剂,例如,例如三乙胺的叔胺化合物、四正丁基溴化铵和四正丁基溴化磷或季铵化合物或季磷化合物。
在所述界面聚合中,反应温度优选为0℃至40℃以及反应时间优选为10分钟至5小时。此外,在所述界面聚合反应中,pH优选保持在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引发之前、在聚合反应引发期间或者在聚合反应引发之后加入。
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,而且优选为对叔丁基苯酚。在此情况下,调节分子量的效果优异。
基于100重量份的所述芳香族二元醇化合物,包含例如不小于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重量份的上述分子量调节剂。在此范围内,可以获得所需的分子量。
此外,本发明提供了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来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聚硅氧烷结构没有引入该聚碳酸酯的主链中。
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]
在所述化学式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'是未被取代或被苯基取代的C1-10亚烷基、未被取代或被C1-10烷基取代的C3-15亚环烷基、O、S、SO、SO2或CO。
此外,优选地,上述聚碳酸酯具有15,000g/mol至35,000g/mol的重均分子量。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。
所述由化学式4表示的重复单元通过使芳香族二元醇化合物与碳酸酯前体反应而形成。此处可以使用的芳香族二元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中的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]
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、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颗粒,干燥该颗粒然后用注模机注射该经干燥的颗粒。
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同时具有提高的耐化学性和冲击强度的效果。
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,而且不应被解释由这些实施例限制本发明。
制备实施例1:AP-PDMS(n=34)
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。然后将混合物与相对于100重量份八甲基环四硅氧烷的1重量份的酸性粘土(DC-A3)一同放入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。由此制备的末端未改性的聚有机硅氧烷的重复单元(n)当通过1HNMR确定时为34。
向所得的末端未改性的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。由此制备的末端改性的聚有机硅氧烷称为AP-PDMS(n=34)。AP-PDMS是淡黄色油并且当利用Varian 500MHz通过1HNMR确认时重复单元为(n)为34,且不需要进一步的纯化。
制备实施例2:MBHB-PDMS(m=58)
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。然后将混合物与相对于100重量份八甲基环四硅氧烷的1重量份的酸性粘土(DC-A3)一同引入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并用硅藻土快速过滤。由此制备的末端未改性的聚有机硅氧烷的重复单元(m)当通过1HNMR确定时为58。
向所得的末端未改性的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。由此制备的末端改性的聚有机硅氧烷称为MBHB-PDMS(m=58)。MBHB-PDMS是淡黄色油并且当利用Varian 500MHz通过1HNMR确定时重复单元为(m)为58,且不需要进一步的纯化。
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。然后将混合物与相对于100重量份八甲基环四硅氧烷的1重量份的酸性粘土(DC-A3)一同放入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并用硅藻土快速过滤。由此制备的末端未改性的聚有机硅氧烷的重复单元(n)当通过1HNMR确定时为50。
向所得的末端未改性的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。由此制备的末端改性的聚有机硅氧烷称为丁香酚-PDMS。丁香酚-PDMS是淡黄色油并且当利用Varian 500MHz通过1HNMR确定时重复单元为(n)为50,且不需要进一步的纯化。
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气氛下利用混合溶解。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)的混合溶液(重量比为90:10)溶解在MC(二氯甲烷)中然后加入至其中。然后,将128g的TPG(三光气)溶解在MC中,将溶解的TPG溶液加入至其中,并在将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℃下干燥以获得最终的共聚碳酸酯。
实施例2
除了使用6.24g的在制备实施例1中制备的AP-PDMS(n=34)与0.33g的在制备实施例2中制备的MBHB-PDMS(m=58)的混合溶液(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。
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气氛下利用混合溶解。将4.3g的PTBP(对叔丁基苯酚)和6.57g的在制备实施例1中制备的AP-PDMS溶解在MC(二氯甲烷)中然后加入至其中。然后,将128g的TPG(三光气)溶解在MC中,将溶解的TPG溶液加入至其中,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℃下干燥以获得最终的共聚碳酸酯。
对比实施例2
除了使用在制备实施例3中制备的丁香酚-PDMS代替在制备实施例1中制备的AP-PDMS(n=34)以外,以与对比实施例1中相同的方法制备共聚碳酸酯。
对比实施例3
除了不使用在制备实施例1中制备的AP-PDMS(n=34)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采用安捷伦1200系列以PC标准由GPC测量。
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重量份的亚磷酸三(2,4-二叔丁基苯基)酯、0.010重量份的十八烷基-3-(3,5-二叔丁基-4-羟基苯基)丙酸酯和0.030重量份的季戊四醇四硬脂酸酯,然后利用Φ30mm的有孔的双螺杆挤出机将所得混合物制成颗粒,然后利用注模机N-20C(JSW,Ltd.)在300℃的料筒温度和80℃的模具温度下注射成型以制备所需的试样。
上述试样的特性按以下方式测定,而且结果在下面表1中示出。
1)耐化学性:拉伸应力(kg/cm2)根据ASTM D638(试样厚度:3.2mm)测定(TS0)。然后,在根据下面表1中所示选择溶剂之后,根据ASTM D543(方法B)基于JIG Strain R1.0进行实验。在室温(23℃)下将棉布(2cm×2cm)放置在各个试样的中心上。将溶剂滴至布上使其足以每天挥发,而且试样与溶剂接触168小时。实验完成后,用干净的布将试样上的溶剂完全去除,然后根据ASTM D638再次测定拉伸应力(TS)以计算TS/TS0。
2)室温冲击强度:根据ASTM D256在23℃下测定(1/8英寸,缺口悬臂梁)。
3)低温冲击强度:根据ASTM D256在-30℃下测定(1/8英寸,缺口悬臂梁)。
4)熔体指数(MI):根据ASTM D1238测定(条件为300℃和1.2kg)。
[表1]
如上面表1中所示,与对比实施例1至3相比,根据本发明(实施例1和2)的共聚碳酸酯表现出优异的耐化学性,以及具体地,当使用乙酸乙酯和甲苯作为溶剂时差异显著。此外,与对比实施例相比,实施例表现出优异的低温冲击强度和室温冲击强度。
因此,可以确定根据本发明的共聚碳酸酯同时表现出提高的耐化学性和冲击强度。
Claims (16)
1.一种共聚碳酸酯,该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,以及
所述共聚碳酸酯满足下面式1:
[式1]
TS/TS0≥0.80
在所述式1中,
TS0是根据ASTM D638测定的拉伸应力,以及
TS表示在根据ASTM D543(方法B)与乙酸乙酯接触168小时以后根据ASTM D638测定的拉伸应力。
2.如权利要求1所述的共聚碳酸酯,其中,所述共聚碳酸酯满足下面式2:
[式2]
TS/TS0≥0.50
在所述式2中,
TS0是根据ASTM D638测定的拉伸应力,以及
TS表示在根据ASTM D543(方法B)与甲苯接触168小时以后根据ASTMD638测定的拉伸应力。
3.如权利要求1所述的共聚碳酸酯,其中,所述共聚碳酸酯具有在-30℃下根据ASTM D256(1/8英寸,缺口悬臂梁)测定的600J/m至1000J/m的低温冲击强度。
4.如权利要求1所述的共聚碳酸酯,其中,所述共聚碳酸酯具有在23℃下根据ASTM D256(1/8英寸,缺口悬臂梁)测定的840J/m至1000J/m的室温冲击强度。
5.如权利要求1所述的共聚碳酸酯,其中,所述共聚碳酸酯具有1,000g/mol至100,000g/mol的重均分子量。
6.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。
7.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]
在所述化学式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是未被取代或被苯基取代的C1-10亚烷基、未被取代或被C1-10烷基取代的C3-15亚环烷基、O、S、SO、SO2或CO。
8.如权利要求7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-羟基苯基)甲烷、双(4-羟基苯基)醚、双(4-羟基苯基)砜、双(4-羟基苯基)亚砜、双(4-羟基苯基)硫醚、双(4-羟基苯基)甲酮、1,1-双(4-羟基苯基)乙烷、双酚A、2,2-双(4-羟基苯基)丁烷、1,1-双(4-羟基苯基)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-羟基苯基)-1-苯基乙烷、双(4-羟基苯基)二苯基甲烷和α,ω-双[3-(邻羟基苯基)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。
9.如权利要求7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]
10.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]
在所述化学式2中,
各个X1独立地是C1-10亚烷基,
各个R5独立地是氢;未取代或者被环氧乙烷基、被环氧乙烷基取代的C1-10烷氧基或被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]
在所述化学式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、C1-10烷氧基或C6-20芳基,
各个R6独立地是氢;未取代或者被环氧乙烷基、被环氧乙烷基取代的C1-10烷氧基或被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。
11.如权利要求10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1:99至99:1。
12.如权利要求10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]
13.如权利要求10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]
14.一种聚碳酸酯组合物,该聚碳酸酯组合物包含权利要求1至13中的任一项所述的共聚碳酸酯和聚碳酸酯。
15.如权利要求14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]
在所述化学式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'是未被取代或被苯基取代的C1-10亚烷基、未被取代或被C1-10烷基取代的C3-15亚环烷基、O、S、SO、SO2或CO。
16.如权利要求14所述的聚碳酸酯组合物,其中,未将聚硅氧烷结构引入所述聚碳酸酯的主链中。
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