CN105899575B - 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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- CN105899575B CN105899575B CN201580002907.4A CN201580002907A CN105899575B CN 105899575 B CN105899575 B CN 105899575B CN 201580002907 A CN201580002907 A CN 201580002907A CN 105899575 B CN105899575 B CN 105899575B
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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定的硅氧烷化合物的结构,因此,具有同时提供提高的低温冲击强度以及改善的YI(黄度指数)的特性。
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23日提交的韩国专利申请号10-2015-0104643以及于2015年11月13日提交的韩国专利申请号10-2015-0159660的权益,上述所公开的全部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,更具体地涉及被经济地生产并且同时具有相互矛盾的性能,即提高的低温冲击强度以及改善的YI(黄色指数)的共聚碳酸酯以及包含该共聚碳酸酯的组合物。
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,聚碳酸酯树脂大范围地应用于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的用途中。
近来,为了将这些聚碳酸酯树脂应用至更多样的领域中,已经进行了各种研究以通过将两种以上的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。
特别是,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,而且当耐化学性或冲击强度,特别是低温冲击强度增加时,YI(黄色指数)等降低。
考虑到上述情况,本发明人已进行了深入的研究以解决现有技术遇到的上述缺点并且开发同时具有提高的低温冲击强度和改善的YI(黄色指数)的共聚碳酸酯,并且发现如下所述的在聚碳酸酯的主链中引入特定的硅氧烷化合物的共聚碳酸酯满足上述性能。基于此发现完成了本发明。
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低温冲击强度和改善的YI(黄色指数)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的组合物。
技术方案
为了达到这些目的,本发明提供了如下描述的共聚碳酸酯:
(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,其中所述共聚碳酸酯根据ASTM D1925测定的YI(黄色指数)为2至6.5,以及根据ASTM D256(1/8英寸,缺口悬臂梁式)在-30℃下测定的低温冲击强度为600J/m至1000J/m。
优选地,所述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,优选地,所述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,优选地,当所述值高时低温冲击强度优异,因此不限于任一上限值。但是,作为一个实例,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。
(2)优选地,上面项(1)的共聚碳酸酯,其中,该共聚碳酸酯根据ASTM D256(1/8英寸,缺口悬臂梁式)在23℃下测定的室温冲击强度为840J/m至1000J/m。
更优选地,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,当所述值高时室温冲击强度优异,因此不限于任一上限值。但是,作为一个实例,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。
(3)此外,优选地,上面项(1)或(2)的共聚碳酸酯,其中,该共聚碳酸酯的重均分子量为1,000g/mol至100,000g/mol,更优选地为15,000g/mol至35,000g/mol。在此重均分子量的范围内,所述共聚碳酸酯具有提供优异的延展性和YI(黄色指数)的效果。
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。
(4)此外,优选地,上面项(1)至(3)中的任一项的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。
(5)此外,优选地,上面项(1)至(4)中的任一项的共聚碳酸酯,其中,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是1:0.001-0.006,和/或它们的重量比是1:0.01-0.03。
(6)此外,优选地,上面项(1)至(5)中的任一项的共聚碳酸酯,其中,特别地,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,优选地,由下面化学式1表示的共聚碳酸酯:
[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,
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,R1、R2、R3和R4各自独立地是氢、甲基、氯或溴。
更优选地,Z是未被取代或被苯基取代的直链或支链C1-10亚烷基,更优选地是亚甲基、1,1-亚乙基、2,2-亚丙基、2,2-亚丁基、1-苯乙烷-1,1-二基或二苯亚甲基。更优选地,Z是1,1-亚环己基、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来自于选自双(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元醇化合物。
如此处所使用,“来自于芳香族二元醇化合物”是指芳香族二元醇化合物的羟基与碳酸酯前体反应形成由化学式1表示的重复单元。
例如,当使芳香族二元醇化合物双酚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、碳酸双(氯苯基)酯、碳酸二间甲酚酯、碳酸二萘酯、碳酸双(联苯)酯、光气、三光气、双光气、溴光气以及双卤代甲酸酯中的一种或多种。优选地,可以使用三光气或光气。
(7)此外,优选地,上面项(1)至(6)中的任一项的共聚碳酸酯,其中,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,
X1各自独立地是C1-10亚烷基,
R5各自独立地是氢;未被取代或被环氧乙烷基、被环氧乙烷基取代的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,
n是10至200的整数,
[化学式3]
在所述化学式3中,
X2各自独立地是C1-10亚烷基,
Y1各自独立地是氢、C1-6烷基、卤素、羟基、C1-6烷氧基或C6-20芳基,
R6各自独立地是氢;未被取代或被环氧乙烷基、被环氧乙烷基取代的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,
m是10至200的整数。
在化学式2中,优选X1各自独立地是C2-10亚烷基,更优选C2-4亚烷基以及最优选1,3-亚丙基。
此外,优选地,R5各自独立地是氢、甲基、乙基、丙基、3-苯丙基、2-苯丙基、3-(环氧乙烷基甲氧)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R5各自独立地是C1-10烷基、更优选C1-6烷基、还更优选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X2各自独立地是C2-10亚烷基、更优选C2-6亚烷基以及最优选亚异丁基。
此外,优选地,Y1是氢。
此外,优选地,R6各自独立地是氢、甲基、乙基、丙基、3-苯丙基、2-苯丙基、3-(环氧乙烷基甲氧)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,R6各自独立地是C1-10烷基、更优选C1-6烷基、还更优选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来自于由下面化学式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:
[化学式2-1]
在所述化学式2-1中,X1、R5和n与此前定义相同。
[化学式3-1]
在所述化学式3-1中,X2、Y1、R6和m与此前定义相同。
如此处所使用的,“来自于硅氧烷化合物”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,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上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相同。
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解1和2表示:
[反应图解1]
在上面反应图解1中,
X1'是C2-10烯基,
X1、R5和n与此前定义相同。
[反应图解2]
在上面反应图解2中,
X2'是C2-10烯基,以及
X2、Y1、R6和m与此前定义相同。
在反应图解1和反应图解2中,所述反应优选地在金属催化剂的存在下进行。作为所述金属催化剂,优选地使用铂催化剂。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,由化学式7或9表示的化合物可以通过使有机二硅氧烷和有机环硅氧烷在酸性催化剂的存在下反应来制备,n和m可以通过调节反应物的量来调节。反应温度优选为50℃至70℃。另外,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。
特别是,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冲击强度和YI(黄色指数)。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]
在所述化学式2-2中。R5和n与此前描述相同。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与此前描述相同。优选地,R6是甲基。
(8)此外,本发明提供了一种共聚碳酸酯,该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。此外,提供了上述项(1)至(7)中的任一项所述的共聚碳酸酯,其中,所述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。
(9)此外,本发明提供了一种制备共聚碳酸酯的方法,该方法包括使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此前描述相同。
在所述聚合的过程中,基于共计100重量份的所述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,所述一种或多种硅氧烷化合物的使用量可以不小于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,基于共计100重量份的所述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,上述芳香族二元醇化合物的使用量可以不小于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%。基于共计100重量份的所述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,上述碳酸酯前体的使用量可以不小于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,作为一个实例,可以使用界面聚合法。在此情况下,有聚合反应可以在大气压力和低温下进行的效果,而且分子量容易控制。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。
在界面聚合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,只要其可以通常在聚碳酸酯的聚合中使用即可。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,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,反应温度优选地是从0℃至40℃以及反应时间优选地是从10分钟至5小时。此外,在所述界面聚合反应中,pH优选地保持在不小于9或不小于11。
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开始之前、聚合开始的过程中或聚合开始之后加入。
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,调节分子量的效果优异。
基于100重量份的所述芳香族二元醇化合物,上述分子量调节剂的含量为例如不小于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。在此范围内,可以获得所需的分子量。
(10)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以控制共聚碳酸酯的物理性能。
上述聚碳酸酯在聚碳酸酯的主链中未引入聚硅氧烷结构。就此而言,区别于根据本发明的共聚碳酸酯。
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,
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,所述重均分子量(g/mol)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,所述重均分子量(g/mol)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为从99:1至1:99、更优选地为从90:10至50:50,最优选地为从80:20至60:40。
(11)此外,本发明提供了一种包含上述共聚碳酸酯或共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,干燥颗粒然后用注模机注射干燥后的颗粒。
有益效果
如前文所述,根据本发明,提供了一种共聚碳酸酯,该共聚碳酸酯在聚碳酸酯的主链中引入特定的硅氧烷化合物,具有同时提供提高的低温冲击强度以及改善的YI(黄度指数)的特性。
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,而不应被解释为通过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1重量份的酸性粘土(DC-A3)(相对于100重量份八甲基环四硅氧烷)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赛力特硅藻土快速过滤。通过1HNMR确定由此制备的末端未改性的聚有机硅氧烷的重复单元(n)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铂催化剂并在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硅氧烷称为AP-PDMS(n=34)。AP-PDMS是淡黄色油,利用Varian 500MHz通过1HNMR确定重复单元为(n)为34,并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1重量份的酸性粘土(DC-A3)(相对于100重量份八甲基环四硅氧烷)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然后用赛力特硅藻土快速过滤。通过1HNMR确定由此制备的末端未改性的聚有机硅氧烷的重复单元(m)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硅氧烷称为MBHB-PDMS(m=58)。MBHB-PDMS是淡黄色油,利用Varian 500MHz通过1HNMR确定重复单元为(m)为58,并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1重量份的酸性粘土(DC-A3)(相对于100重量份八甲基环四硅氧烷)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赛力特硅藻土快速过滤。通过1HNMR确定由此制备的末端未改性的聚有机硅氧烷的重复单元(n)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硅氧烷称为丁香酚-PDMS。丁香酚-PDMS是淡黄色油,利用Varian 500MHz通过1HNMR确定重复单元为(n)为50,并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)中并加入至其中。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20分钟后,将pH降至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,获得最终的共聚碳酸酯。
实施例2
除了加入添加剂(抗氧化剂、润滑剂)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与MBHB-PDMS的比为95:5而不是90:10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
除了调节分子量调节剂(PTBT)的使用量以外,以与实施例3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)中并加入至其中。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20分钟后,将pH降至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,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1中制备的AP-PDMS(n=34)代替在制备实施例3中制备的丁香酚-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:共聚碳酸酯的性能的确定
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Agilent1200系列PC标准测定。
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,然后使用设置有通气孔的Φ30mm双螺杆挤出机对所得混合物进行造粒,然后使用JSW Co.,Ltd的N-20C注模机在300℃的料筒温度和80℃的模具温度下进行注射成型以制备所需的试样。
以下面方式测定上述试样的性能,结果在下面表1中示出。
1)室温冲击强度:根据ASTM D256在23℃下测定(1/8英寸,缺口悬臂梁式)。
2)低温冲击强度:根据ASTM D256在-30℃下测定(1/8英寸,缺口悬臂梁式)。
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,可以确定与对比实施例1和2相比,根据本发明(实施例1至4)的共聚碳酸酯表现出优异的低温冲击强度和室温冲击强度;与对比实施例1相比,实施例1和2在保持了低温冲击强度的同时具有改善的YI(黄色指数);与对比实施例2相比,实施例3和4在保持了低温冲击强度的同时具有改善的YI(黄色指数)。
因此,可以确定,根据本发明的共聚碳酸酯同时具有提高的低温冲击强度和改善的YI(黄色指数)。
Claims (5)
1.一种共聚碳酸酯,包含:由下面化学式1表示的芳香族聚碳酸酯类第一重复单元;以及由下面化学式2-2表示的具有硅氧烷键的芳香族聚碳酸酯类第二重复单元和由下面化学式3-2表示的具有硅氧烷键的芳香族聚碳酸酯类第二重复单元,
其中,所述共聚碳酸酯根据ASTM D1925测定的YI(黄色指数)为2至6.5,根据ASTM D256以1/8英寸、缺口悬臂梁式法在-30℃下测定的低温冲击强度为600J/m至1000J/m,并且根据ASTM D256以1/8英寸、缺口悬臂梁式法在23℃下测定的室温冲击强度为840J/m至1000J/m,
[化学式1]
在上述化学式1中,
R1、R2、R3和R4各自独立地是氢、C1-10烷基、或卤素,
Z是未被取代或被苯基取代的C1-10亚烷基、O、S、SO、SO2或CO,
[化学式2-2]
在所述化学式2-2中,
n是32至37的整数,
R5各自独立地是氢;C1-6烷基
[化学式3-2]
在所述化学式3-2中,
m是55至62的整数,
R6各自独立地是氢;C1-6烷基。
2.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15,000g/mol至35,000g/mol。
3.如权利要求1所述的共聚碳酸酯,其中,
所述由化学式1表示的重复单元来自于选自双(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、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-苯乙烷和双(4-羟苯基)二苯基甲烷中的一种或多种芳香族二元醇化合物。
4.如权利要求1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]
5.如权利要求1所述的共聚碳酸酯,其中,
所述由化学式2-2表示的重复单元与由化学式3-2表示的重复单元的重量比为1:99至99:1。
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