CN111875759B - 嵌段共聚物及其用途 - Google Patents
嵌段共聚物及其用途 Download PDFInfo
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- CN111875759B CN111875759B CN202010375138.5A CN202010375138A CN111875759B CN 111875759 B CN111875759 B CN 111875759B CN 202010375138 A CN202010375138 A CN 202010375138A CN 111875759 B CN111875759 B CN 111875759B
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Abstract
公开了一种聚合物组合物,其包含具有多个聚合物臂的星形支化共聚物。每个聚合物臂的分子量为1‑50kg/mol,且每个聚合物臂包括:得自包含自由基反应性基团的第一乙烯基芳族单体的聚合单元(i),其中大于10摩尔%至100摩尔%的聚合单元(i)未被氢化;任选地,聚合单元(ii),其包括:氢化和非氢化形式的得自高Tg单体的聚合单元(ii),和氢化形式的聚合单元(i)或氢化形式的聚合苯乙烯单元;和任选地,聚合单元(iii),其包括:(a)氢化形式的得自一个或多个无环共轭二烯的聚合单元,和(b)得自一种或多种第二乙烯基芳族单体的聚合单元,其中小于10重量%的(a)是未氢化的。
Description
技术领域
本公开内容涉及选择性氢化的共聚物,由其制备的可固化的组合物和固化的组合物,以及它们的用途,包括高温应用。
背景技术
与诸如电子和汽车应用的不同领域相关的技术的迅速发展导致对高性能材料的需求。大容量计算机系统和网络需要高频信号传输,电路基板适合于高频和高速传输。期望电路基板在高频和低传输损耗(例如介电损耗、导体损耗和辐射损耗)下操作信号。传输损耗会减弱电信号并破坏信号可靠性。
在许多商业领域,例如汽车工业、建筑、工具制造、粘合剂和密封剂中,都需要具有良好机械性能、在宽温度范围内的低损耗因数且结合具有良好加工能力的材料。一些主要应用要求在强度和足够的模量或硬度方面具有良好机械性能的材料。现有材料可能无法满足此类要求。
传统上,印刷电路板使用环氧树脂,该树脂具有较高的介电常数和介电损耗角正切值。环氧树脂可与酚类化合物、胺或酸酐固化剂结合使用以提高性能。这种树脂组合物仍然难以获得低损耗因数。聚苯醚树脂(称为聚氧化亚苯基树脂或PPO)由于其低耗散性能而被用于层压体中,但是在新的电子领域中使用高频信号需要甚至更低的介电常数和损耗因数。存在其他塑料解决方案,例如基于氟化聚合物的材料,具有较低的损耗因数,但它们缺乏易于加工性或有效的固化能力,无法抵抗高温或存在溶剂。
仍然需要具有适用于覆铜层压体和由其制成的印刷电路板的具有改善的性能(例如改善的机械性能、高温性能和/或改善的电性能)的改进的组合物。
发明内容
一方面,公开了一种聚合物组合物,其包含星形支化共聚物。所述星形支化共聚物具有多个聚合物臂,每个聚合物臂的分子量Mp为1-50kg/mol。每个聚合物臂包括聚合单元(i),任选地聚合单元(ii),和任选地聚合单元(iii)。聚合单元(i)得自包含自由基反应性基团的第一乙烯基芳族单体,其中大于10摩尔%至100摩尔%的聚合单元是未氢化的。聚合单元(ii)包括氢化和非氢化形式的得自高Tg单体的聚合单元,氢化形式的聚合单元(i)或氢化形式的聚合苯乙烯单元;和任选地,聚合单元(iii)。聚合单元(iii)包括(a)氢化形式的得自一种或多种无环共轭二烯的聚合单元,和(b)得自一种或多种第二乙烯基芳族单体的聚合单元,其中小于10重量%的单元(a)是未氢化的。所述共聚物包含大于10重量%的聚合单元(i),聚合单元(i)和(ii)一起占所述星形支化共聚物总重量的大于50重量%。所述共聚物的分子量Mp为15-500kg/mol,玻璃化转变温度高于100℃至250℃。
在其他方面,还公开了包含所述聚合物组合物的可固化的组合物,其中所述聚合物组合物包含星形支化共聚物,以及由所述可固化组合物制备的固化的组合物。
除非另有说明,否则“分子量”是指以kg/mol计的聚合物或嵌段共聚物的苯乙烯当量分子量。分子量可以使用聚苯乙烯校准标准物通过凝胶渗透色谱法(GPC)测定,例如根据ASTM 5296-19进行。色谱仪使用市售的聚苯乙烯分子量标准物进行校准。使用如此校准的GPC测定的聚合物的分子量是苯乙烯当量分子量。检测仪可以是紫外线和折射率检测仪的组合。在此表示的分子量是在GPC迹线的峰值处测定的,转换为真实分子量,通常称为“峰值分子量”,称为Mp。分子量是指苯乙烯当量峰值分子量。
损耗因数(Df)或tanδ定义为等效串联电阻(ESR)与电容电抗的比值。损耗因数也称为损耗角正切,通常以百分比表示。
介电常数(Dk)是电绝缘材料(电介质)的性能,其等于在真空中没有电介质材料的情况下填充有给定材料的电容器的电容与相同电容器的电容之比。
根据以下详细描述,本公开的前述方面以及其他特征和优点将是显而易见的。
聚合物组合物:所述聚合物组合物包含占所述聚合物组合物的大于80重量%的星形支化聚合物。在某些实施方案中,所述星形支化聚合物占所述聚合物组合物的85-100重量%,或90-95重量%,或95-100重量%。在另一个实施方案中,所述聚合物组合物基本上由星形支化共聚物组成。
所述星形支化共聚物具有多个聚合物臂。每个聚合物臂可具有1-50kg/mol的分子量。每个聚合物臂包括聚合单元(i)、任选的聚合单元(ii)和任选的聚合单元(iii)。所述星形支化共聚物结构的这些部分的每一个在下面详细讨论。
聚合单元(i)得自第一乙烯基芳族单体。第一乙烯基芳族单体具有包括自由基反应性基团的结构。自由基反应性基团是可形成或可被诱导形成自由基物质的化学基团。自由基物质可以通过任何已知的方式形成,包括加热方式、光化学方式和化学试剂。例如,具有至少一个氢取代基的苄基碳可以是自由基反应性基团。苄基碳基团也可以被取代,只要它具有一个苄基氢原子即可。自由基反应性基团的另一个实例是环丁烷环,其可以例如被光化学活化以形成自由基物质。自由基反应性基团的其他实例包括烯丙基,其可以形成烯丙基自由基。
在一个实施方案中,第一乙烯基芳族单体可以是式(I)的取代的苯乙烯、式(II)的乙烯基苯并环丁烯、式(III)的乙烯基二氢茚、式(IV)的乙烯基四氢萘、或其任何组合。
表1:各种第一乙烯基芳族单体的结构
在一个实施方案中,大于10摩尔%至100摩尔%的单元(i)是未氢化的。在另一个实施方案中,20-90摩尔%或30-80摩尔%或40-70摩尔%或50-60摩尔%的单元(i)是未氢化的。
式(I)的单体的实例包括邻甲基苯乙烯、对甲基苯乙烯、邻乙基苯乙烯、对乙基苯乙烯、邻异丙基苯乙烯、对异丙基苯乙烯、邻甲基-α-甲基苯乙烯、对甲基-α-甲基苯乙烯、邻乙基-α-甲基苯乙烯、对乙基-α-甲基苯乙烯、邻异丙基-α-甲基苯乙烯、对异丙基-α-甲基苯乙烯或它们的任何混合物。在一个实施方案中,第一乙烯基芳族单体包括对甲基苯乙烯、对甲基-α-甲基苯乙烯或其组合。在另一个实施方案中,第一乙烯基芳族单体包括对甲基苯乙烯。
聚合单元(ii)得自高Tg单体,例如当均聚或与其他共聚单体共聚时可形成高玻璃化转变温度(Tg)(例如最高300℃,或100-250℃,或110-200℃,或120-160℃)的阴离子可聚合单体。高Tg单体具有阴离子可聚合的乙烯基,且可以具有不同类型的结构。高Tg单体的非限制性实例包括选自以下的化合物:叔丁基苯乙烯、1,3-环己二烯、苯并富勒烯、1,1-二苯乙烯、乙烯基联苯、金刚烷基苯乙烯、乙烯基蒽、二乙烯基苯、双(乙烯基苯基)乙烷、及其组合。单体中的芳环也可以是双环,三环或多环的。可聚合的乙烯基也可以包含在环内,例如,茚或其取代的衍生物。
高Tg单体的其他实例包括共轭环二烯,例如1,3-环己二烯、1,3-环庚二烯、其取代的衍生物、或它们的组合。优选1,3-环己二烯,因为它相对更易得。
当使用共轭环二烯作为高Tg单体时,阴离子聚合可通过不同程度的1,4-加成机理和1,2-加成机理进行。比例不仅受单体结构的影响,而且还受聚合过程中存在的其他添加剂的影响。例如,可以使用添加剂来增强1,2-加成超过1,4-加成。在一个实施方案中,得自共轭环二烯的聚合单元,例如1,3-环己二烯或先前列出的任何高Tg单体,可以90:10-10:90或85:15-15:85或80:20-20:80或70:30-30:70或60:40-40:60或55:45-45:55的相对摩尔比包括1,2-和1,4-聚合单元。在一个具体的实施方案中,得自1,3-环己二烯的1,2-和1,4-聚合单元可以90:10-10:90的相对摩尔比变化。例如,已知诸如TMEDA的添加剂会以接近50/50含量的相对摩尔比产生1,2-和1,4-聚合单元。诸如DEP的改性剂可导致1,2-聚合单元与1,4-聚合单元的比率更接近30/70,而诸如DABCO的改性剂可提供1,2-聚合单元与1,4-聚合单元的比率更接近10/90。
在包含包括聚合单元(i)和(ii)的星形支化聚合物的聚合物组合物中,所述共聚物可包含大于10重量%的聚合单元(i),使得聚合单元(i)和(ii)一起占所述共聚物总重量的大于50重量%,或者大于60重量%,或者大于70重量%,或者大于80重量%,或者大于90重量%,或者基本上100重量%。
在另一个实施方案中,包含星形支化聚合物的聚合物组合物包括聚合单元(i)、(ii)和(iii),包含大于10重量%的聚合单元(i),使得聚合单元(i)和(ii)一起占所述共聚物总重量的大于50重量%,或者大于60重量%,或者大于70重量%,或者大于80重量%,或者大于90重量%。
包含得自包含表1中所列的自由基反应性基团的第一乙烯基芳族单体的聚合单元(i)的聚合物组合物表现出小于5000cP或者小于2000cP或者200-1800cP或者400-1500cP或者600-1200cP或者800-1000cP的溶液粘度,其根据在25℃于甲苯中25重量%的溶液测定。
在另一个实施方案中,所述星形支化共聚物的分子量大于30kg/mol,和溶液粘度小于2,000cP,所述粘度根据在25℃于甲苯中25重量%的共聚物含量测定。
在一些实施方案中,所述星形支化共聚物具有其中在氢化之前聚合单元(i)是聚合的对甲基苯乙烯单元的结构。在另一个实施方案中,所述共聚物具有其中第一乙烯基芳族单体是对甲基苯乙烯且聚合单元(ii)包括氢化形式的聚合的对甲基苯乙烯、聚合的二乙烯基苯、聚合的叔丁基苯乙烯或其组合的结构;且其中聚合单元(i)和(ii)一起占所述共聚物总重量的大于60重量%,或60-100重量%或70-95重量%,75-90重量%,或80-90重量%。在其他实施方案中,所述共聚物包含大于10重量%的聚合单元(i),使得当还存在聚合单元(ii)时,单元(i)和(ii)一起占所述共聚物总重量的大于50重量%。
所述星形支化共聚物还可以任选地包括聚合单元(iii),所述聚合单元(iii)包括(a)氢化形式的得自一种或多种无环共轭二烯的聚合单元,和(b)得自一种或多种第二乙烯基芳族单体的聚合单元,其中小于10重量%的(a)是未氢化的。在一个实施方案中,共轭二烯是无环1,3-二烯,其非限制性实例包括2,3-二甲基-1,3-丁二烯、丁二烯、异戊二烯、1,3-戊二烯、法呢烯、月桂烯、1,3-己二烯及其组合。第二乙烯基芳族单体可以是任何阴离子可聚合的芳族化合物,例如苯乙烯、取代的苯乙烯或其他乙烯基芳族化合物。当使用无环1,3-二烯时,它允许引入具有低玻璃化转变温度的聚合物嵌段,即在室温或在应用温度下的聚合物软嵌段。在某些实施方案中,得自第二乙烯基芳族单体和共轭二烯的聚合单元的相对比例可以100:0-0:100的摩尔比变化。不使用或使用少量(例如最多小于50摩尔%)的第二乙烯基芳族单体可用于制备具有较低Tg的软聚合物嵌段。
所述星形支化共聚物的分子量Mp为15-500kg/mol。在其他实施方案中,所述共聚物的分子量为30-400kg/mol,或者50-200kg/mol。所述共聚物的Tg为100-250℃。在一些实施方案中,Tg可以在110-225℃或150-200℃的范围内变化。
在另一个实施方案中,所述星形支化共聚物结构可以包括得自1,3-环己二烯的聚合单元(ii),且包括相对摩尔比为90:10-10:90的1,2-加成单元和1,4-加成单元。如前所述,通常可以使用某些类型的添加剂来控制二烯单体的1,2-加成与1,4-加成的比例。在另一个实施方案中,所述星形支化共聚物可具有其中大于50摩尔%或50-100摩尔%或60-90摩尔%或70-80摩尔%的聚合的1,3-环己二烯单元被氢化的结构。在又一个实施方案中,所述共聚物可以进一步包含聚合单元(iii),其中第二乙烯基芳族单体是苯乙烯,以及无环共轭二烯选自丁二烯、异戊二烯及其组合。
在一个实施方案中,所述星形支化共聚物可以是星形支化嵌段共聚物,其中多个聚合物臂中的每个可以包括一个或多个聚合物嵌段,所述聚合物嵌段包含如前所述的得自第一乙烯基芳族单体的聚合单元(i)、任选的聚合单元(ii)和任选的聚合单元(iii)。在一个特定的实施方案中,所述星形支化嵌段共聚物具有其中大于70重量%的一个或多个聚合物嵌段包括至少80重量%的聚合单元(i)和(ii)的组合的结构;且其中所述聚合物组合物具有根据ASTM D2240测定的大于80的肖氏A硬度。在其他实施方案中,所述嵌段共聚物具有其中75-100重量%或80-95重量%或85-90重量%的一个或多个聚合物嵌段包括至少80重量%的聚合单元(i)和(ii)的组合的结构,且所述聚合物组合物具有根据ASTM D2240测定的大于80的肖氏A硬度。
在其他实施方案中,所述嵌段共聚物具有其中大于70重量%的一个或多个聚合物嵌段包括85-100重量%或90-95重量%的聚合单元(i)和(ii)的组合的结构,且所述聚合物组合物具有根据ASTM D2240测定的大于80的肖氏A硬度。
在另一个实施方案中,所述聚合物组合物包含包括一个或多个聚合物嵌段D、任选的一个或多个聚合物嵌段E和任选的一个或多个聚合物嵌段F的星形支化共聚物,其中所述聚合物嵌段D包含聚合单元(i),聚合物嵌段E包含聚合单元(ii),聚合物嵌段F包含聚合单元(iii),其中聚合单元(i)和(iii)如前所述。
在一个实施方案中,所述星形支化的嵌段共聚物具有其中一个或多个嵌段D包括大于50重量%的聚合单元(i)、一个或多个嵌段E包括大于50重量%的聚合单元(ii)和一个或多个嵌段F包括大于50重量%的聚合单元(iii)的结构;其中所述聚合物组合物具有一种或多种选自以下的构型:(D-)nX,(D-E-)nX,(D-F-)nX,(E-D-)nX,(F-D-)nX,(D-E-D-)nX,(D-F-E-)nX,(D-E-F-)nX,(E-F-D-)nX和(E-D-F-)nX,其中n是2-50的整数,X是偶联剂残基。
在一个实施方案中,嵌段D包括氢化形式的聚合的对甲基苯乙烯单元。用于聚合单元(ii)的高Tg单体可以是1,3-环己二烯,因为它相对更易得。在另一个实施方案中,嵌段E可进一步包括得自无环1,3-二烯的聚合单元,所述无环1,3-二烯是例如2,3-二甲基-1,3-丁二烯、异戊二烯、丁二烯、1,3-戊二烯、法呢烯、月桂烯、1,3-己二烯、及其组合。
在另一个实施方案中,嵌段E包含氢化形式的得自高Tg单体1,3-环己二烯、对甲基苯乙烯或二乙烯基苯的聚合单元(ii)。
一个或多个聚合物嵌段F可以包括氢化形式的得自丁二烯或异戊二烯的聚合单元。如前所述,第二乙烯基芳族单体与无环共轭二烯的相对摩尔比可为100:0-0:100,或者90:10-10:90,或者80:20-20:80,或者70:30-30:70。
在一个实施方案中,具有一个或多个嵌段D、任选的一个或多个嵌段E和任选的一个或多个嵌段F的星形支化嵌段共聚物具有25-300kg/mol的总分子量,和聚合物臂的分子量为1-30kg/mol。在其他实施方案中,具有一个或多个嵌段D、任选的一个或多个嵌段E和任选的一个或多个嵌段F的共聚物的总分子量为50-250kg/mol,或100-200kg/mol,或125-150kg/mol。此外,聚合物臂的分子量可为3-25kg/mol,或6-20kg/mol,或10-18kg/mol。
上面讨论的星形支化共聚物可由也是星形支化的多种前体共聚物获得。表2中示出了前体共聚物的一些实例,其中使用了以下缩写和符号:X:用作偶联剂的二乙烯基苯(DVB)的残基;p-MeS:对甲基苯乙烯;DPE:1,1-二苯乙烯;CHD:1,3-环己二烯;p-tBuS:对叔丁基苯乙烯;p-AdS:对金刚烷基苯乙烯;S:苯乙烯;VBCB:4-乙烯基苯并环丁烯;BD:1,3-丁二烯;TMOS:四甲氧基硅烷。
表2:各种共聚物的结构和实例
可以对上述前体共聚物进行选择性氢化,以提供具有不同水平的氢化和未氢化形式的聚合单元(i)、任选地(ii)和任选地(iii)的所需的星形支化共聚物。在一个实施方案中,得自以上讨论的第一乙烯基单体的聚合单元可以被选择性地氢化,其中大于10摩尔%至100摩尔%或者20-90摩尔%或者30-70mol%或者40-60摩尔%的聚合单元为未氢化形式。在其中聚合单元(ii)得自1,3-环二烯的共聚物中,选择性氢化还可以导致其中聚合的环二烯单元中的一些或全部二烯双键被还原的结构。在其中包含聚合单元(iii)的共聚物中,选择性氢化可导致基本上所有的无环二烯双键的还原,和基本上不还原芳族双键,即不大于10摩尔%或者不大于5摩尔%或者不大于2摩尔%的芳族双键被氢化。当使用多于一种类型的乙烯基芳族单体来制备未氢化的共聚物时,在每种类型的聚合的乙烯基芳族单元中选择性氢化可以进行到不同程度。
可以从表2中列出的前体共聚物获得的选择性氢化的共聚物的实例在表3中示出。在表3中,选择性氢化形式的聚合单元由经历氢化的聚合单元的缩写之前的前缀“h”表示。例如,“hpMeS”是指选择性氢化形式的聚合的对甲基苯乙烯单元。
表3:由表2列出的共聚物制得的选择性氢化的星形支化共聚物
共聚物的制备:使用本领域已知的方法,通过阴离子聚合制备所述共聚物。聚合引发剂通常是有机金属化合物,例如有机锂化合物,例如乙基锂、丙基锂、异丙基锂、正丁基锂、仲丁基锂、叔丁基锂、苯基锂、己基联苯基锂、六亚甲基二基锂、丁二烯基锂、异戊二烯基锂、1,1-二苯基己基锂或聚苯乙烯基锂。所需引发剂的量基于要获得的分子量计算的,通常基于待聚合的单体的量为0.002-5摩尔%。合适的溶剂包括具有4-12个碳原子的脂族、脂环族或芳族烃,例如戊烷、己烷、庚烷、环戊烷、环己烷、甲基环己烷、萘烷、异辛烷、苯、烷基苯(例如甲苯、二甲苯或乙苯)或合适的混合物。使用阴离子猝灭剂(例如甲醇)或使用偶联剂进行聚合物链终止,其中所述偶联剂是例如双官能或多官能化合物,例如二乙烯基苯,脂族或芳脂族烃的卤化物,例如1,2-二溴乙烷、双(氯甲基)苯,或四氯化硅,二烷基或二芳基二氯化硅,烷基或芳基三氯化硅,四氯化锡,甲醇烷基硅盐,乙醇烷基硅盐,多官能醛,例如对苯二甲酸二醛,酮,酯,酸酐或环氧化物。优选多功能偶联剂,例如二乙烯基苯,因为它们会产生所需的星形支化共聚物结构。
如果需要,还可以使用影响聚合参数(例如1,2-加成与1,4-加成的相对比例)的路易斯碱添加剂。路易斯碱的实例包括二甲醚,二乙醚,乙二醇二甲醚,1,2-二乙氧基丙烷,二甘醇二甲醚,四氢呋喃,四氢糠基醚,例如四氢糠基甲基醚,和叔胺。
可以在受控条件下进行聚合单元中双键的氢化,以获得具有所需氢化百分比的选择性氢化的共聚物。在氢化步骤中使用基于镍、钴或钛的合适催化剂。可以通过在深真空和较高的温度下的溶剂蒸发以完全除去用于氢化的任何捕获的溶剂,来分离和回收氢化的聚合物。可以改变条件以获得上述任何选择性氢化的共聚物。在一个实施方案中,当包含二烯单体以制备共聚物时,可以进行氢化以使得聚合的二烯单元中的至少80摩尔%、至少90摩尔%或至少98摩尔%的双键被还原,和0-10摩尔%的芳烃双键被还原。类似地,当期望在聚合的乙烯基芳族单体中的芳族双键进行选择性氢化时,可以调节反应条件以产生选择性氢化的共聚物。
可固化的组合物:上述共聚物可用于生产可固化的组合物和由其制成的固化的组合物。所述可固化的组合物包含上述聚合物组合物、固化剂、共固化剂和任选地一种或多种添加剂。
可固化的组合物包含足够量的所述共聚物,以具有所需的性能,例如模量、韧性、粘度、玻璃化转变温度、凝胶含量、硬度、Dk、Df和阻燃性。所述量为1-99.5重量%或7-50重量%或0-25重量%的聚合物,基于可固化的组合物的总重量。基于所需的最终用途,可固化的组合物可进一步包含如下所述的不同组分。
固化剂/固化引发剂:所述可固化的组合物还包含至少一种固化剂/固化引发剂。实例包括但不限于叠氮化物、过氧化物、硫和硫衍生物。自由基引发剂特别优选作为固化引发剂。自由基引发剂的实例包括过氧化物、氢过氧化物和非过氧化物引发剂,例如2,3-二甲基-2,3-二苯基丁烷。过氧化物固化剂的实例包括过氧化二枯基、α,α-二(叔丁基过氧)-m,p-二异丙基苯、2,5-二甲基-2,5-二(叔丁基过氧)己烷、和2,5-二(叔丁基过氧)-2,5-二甲基-3-己炔以及包含一种或多种前述固化引发剂的混合物。
在某些实施方案中,相对于每100份可固化的组合物,固化引发剂的用量为0.1-10份,或0.3-7份,或1-5份,或0.1-5份。
如果需要,也可以使用共固化剂。实例包括苯乙烯,溴苯乙烯,二乙烯基苯,1,2-双(乙烯基苯基)乙烷,三烯丙基氰脲酸酯,三烯丙基异氰脲酸酯,乙烯基官能化的聚苯醚树脂,双马来酰亚胺树脂,液态或固态二烯基聚合物,丙烯酸酯例如三羟甲基丙烷三丙烯酸酯,邻苯二甲酸二烯丙酯,环氧树脂,二烯基聚合物组分,固态二烯基聚合物,苯乙烯-丁二烯二嵌段树脂和聚丁二烯树脂。
二烯基聚合物可以是例如二烯的均聚物,或不同的烯烃和/或二烯的共聚物(包括三嵌段共聚物),其在聚合物主链中具有双键。二烯基聚合物在室温下可以为液态或固态,包括用于介电基材的不饱和树脂,例如聚丁二烯聚合物,或丁二烯与苯乙烯或类似苯乙烯类单体的共聚物。
实例包括具有(甲基)丙烯酰基的聚丁二烯橡胶,具有(甲基)丙烯酰基的聚异戊二烯橡胶,具有(甲基)丙烯酰基的丁二烯与异戊二烯的共聚物橡胶,具有(甲基)丙烯酰基的丁二烯与正丁烯的共聚物橡胶等。在某些实施方案中,二烯基聚合物选自聚丁二烯,聚异戊二烯,丁二烯-苯乙烯共聚物,异戊二烯-苯乙烯共聚物,丁二烯-苯乙烯-甲基丙烯酸酯的三嵌段共聚物,丁二烯-苯乙烯-二乙烯基苯共聚物,丁二烯-苯乙烯-丙烯腈共聚物,丁二烯-苯乙烯-马来酸酐共聚物,及其任何组合。
液态丁二烯共聚物的例子是丁二烯-共-苯乙烯和丁二烯-共-丙烯腈。除了聚丁二烯或聚异戊二烯嵌段被氢化外,含不饱和丁二烯或异戊二烯的聚合物还可包含与第一嵌段共聚物相似的第二嵌段共聚物,从而形成聚乙烯嵌段(在聚丁二烯的情况下)或乙烯-丙烯共聚物(在聚异戊二烯的情况下)。
在某些实施方案中,二烯基树脂任选地包括官能化的液态聚丁二烯或聚异戊二烯树脂,例如,含有一种或多种酸官能化剂的残基(如环氧、马来酸酯、羟基、羧基和甲基丙烯酸酯)的未氢化的嵌段共聚物。
二烯基聚合物可以1-99重量%、30-70重量%、5-25重量%、7-20重量%或10-15重量%的量存在于所述可固化的组合物中,全部以干重计。
填料组分:所述可固化的组合物还包含至少一种无机和/或有机填料。无机填料可用于抑制热膨胀系数并提高层压的片材的韧性。可以使用有机填料来降低层压的片材的介电常数。具有低热膨胀系数的填料是优选的。
示例性的填料包括二氧化钛(金红石和锐钛矿),钛酸钡,钛酸锶,二氧化硅(包括熔融无定形二氧化硅),刚玉,硅灰石,芳族聚酰胺纤维,玻璃纤维,Ba2Ti9O20,玻璃球,石英,氮化硼,氮化铝,碳化硅,氧化铍,氧化铝,氧化镁,氢氧化镁,三聚氰胺多磷酸酯,三聚氰胺氰脲酸酯,蜜白胺,蜜胺(Melon),蜜勒胺,胍,磷氮烷,硅氮烷,DOPO(9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物),DOPO(10-5-二羟基苯基,10-H-9-氧代磷酰苯二酚(oxaphosphaphenanthrenelo)-氧化物),云母,滑石粉,纳米粘土,铝硅酸盐(天然和合成)和热解法二氧化硅,可单独使用或组合使用。
有机填料的实例包括氟基、聚苯乙烯基、二乙烯基苯基和聚酰亚胺基填料。氟基填料包括聚四氟乙烯(PTFE),聚全氟烷氧基树脂,聚氟乙烯-丙烯树脂,聚四氟乙烯-聚乙烯共聚物,聚偏二氟乙烯,聚氯三氟乙烯树脂等。
在某些实施方案中,可以用一种或多种偶联剂例如硅烷、锆酸酯或钛酸酯处理填料。可以对填料进行预处理,或者可以将偶联剂添加至可固化的组合物中。
填料的量为最高75重量%,或0-60重量%,或5-50重量%,或至少20重量%。
阻燃剂:在某些实施方案中,所述可固化的组合物包含选自含磷阻燃剂和溴化阻燃剂的阻燃剂。溴化阻燃剂的实例包括乙烯-双(四溴邻苯二甲酰亚胺),1,2-双(五溴苯基)乙烷和2,4,6-三(2,4,6-三溴苯氧基)-1,3,5-三嗪。含磷阻燃剂的实例包括双酚磷酸二苯酯,多磷酸铵,对苯二酚双(磷酸二苯酯),双酚A双(磷酸二苯酯),三(2-羧乙基)膦(TCEP),磷酸三(氯异丙基)酯,磷酸三甲酯(TMP),二甲基甲基膦酸酯(DMMP),间苯二酚双(二甲苯基磷酸酯),磷腈,三聚氰胺磷酸酯,9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)及其衍生物或树脂,三聚氰胺氰脲酸酯和三羟乙基异氰脲酸酯。在某些实施方案中,阻燃剂化合物可以是DOPO化合物,DOPO树脂(例如DOPO-HQ、DOPO-NQ、DOPO-PN和DOPO-BPN)和含DOPO的环氧树脂,其中DOPO-BPN可以是双酚酚醛清漆化合物,例如DOPO-BPAN,DOPO-BPFN和DOPO-BPSN。
在某些实施方案中,阻燃剂是非反应性阻燃剂,其在其化学结构中不包含反应性官能团。阻燃剂的量为2-30重量%,相对于所述可固化的组合物的总重量。
溶剂:在制备中,添加溶剂以改变所述可固化的组合物的固体含量并调节粘度。合适的溶剂包括例如,酮,例如甲基乙基酮等,醚,例如二丁基醚等,酯,例如乙酸乙酯等,酰胺,例如二甲基甲酰胺等,芳族烃,例如苯、甲苯、二甲苯等,和氯代烃,例如三氯乙烯等;可以单独使用每种溶剂或组合使用它们。
优选的溶剂选自甲醇、乙醇、乙二醇甲基醚、丙酮、甲基乙基酮、甲基异丁基酮、环己酮、甲苯、二甲苯、乙酸甲氧基乙酯、乙酸乙氧基乙酯、乙酸丙氧基乙酯、乙酸乙酯、二甲基甲酰胺、丙二醇甲基醚、γ-丁内酯(GBL)和二异丁基酮(DIBK)。
在一个实施方案中,可以使用合适的溶剂,例如甲苯、甲基乙基酮或酮,制备包含具有上述星形支化共聚物的可固化组合物的制剂。在另一个实施方案中,制剂具有10-60重量%或15-40重量%或20-30重量%的可固化组合物,且其中制剂具有小于5000cP或者小于2000cP或者200-1800cP或者400-1500cP或者600-1200cP或者800-1000cP的粘度,所述粘度在25℃下测定。随后可以将制剂转化为固化的组合物。所用溶剂的量取决于各组分的溶解度、填料量、施用方法和其他因素。
其他添加剂:在某些实施方案中,所述可固化的组合物可进一步包含以下添加剂中的至少一种:玻璃化转变温度为100-200℃的聚烯烃,芳族树脂,橡胶,抗氧化剂,紫外线稳定剂,紫外线自由基引发剂,抗收缩添加剂,粘合促进剂,着色剂,及其组合,增韧剂,粘合促进剂例如硅烷,抗收缩添加剂等。添加剂的选择取决于应用和期望的特性,选择以增强或基本上不负面影响电路子组件的电特性,例如介电常数、损耗因数、介电损耗和/或其他期望的特性。在某些实施方案中,所述聚合物组合物包含固化剂、共固化剂和一种或多种添加剂,其中共固化剂选自二乙烯基苯、1,2-双(乙烯基苯基)乙烷、三烯丙基氰脲酸酯、三烯丙基异氰脲酸酯、乙烯基官能化的聚苯醚树脂、双马来酰亚胺树脂、液态或固态二烯基聚合物;所述添加剂选自填料、阻燃剂、玻璃化温度为100-200℃的聚烯烃、芳族树脂、橡胶、抗氧化剂、紫外线稳定剂、紫外线自由基引发剂、抗收缩添加剂、粘合促进剂、着色剂、及其组合。
可以添加固化促进剂以提高所述可固化的组合物的反应速率。表面活性剂有助于确保无机填料在所述可固化的组合物中的均匀分布,并避免无机填料的聚集。增韧剂有助于提高所述可固化的组合物的韧性。
增韧剂可以是橡胶树脂、羧基封端的聚丁二烯丙烯腈和/或核-壳聚合物。示例性的抗氧化剂包括自由基清除剂和金属减活剂。可以存在偶联剂以促进形成或参与将金属表面或填料表面与聚合物连接的共价键的形成。示例性偶联剂包括3-巯基丙基甲基二甲氧基硅烷和3-巯基丙基三甲氧基硅烷和六亚甲基二硅氮烷。
所述可固化的组合物可包含催化剂,例如路易斯碱或路易斯酸。路易斯碱包括咪唑,三氟化硼胺络合物,乙基三苯基氯化鏻,2-甲基咪唑,2-苯基咪唑,2-乙基-4-甲基咪唑,三苯基膦和/或4-二甲基氨基吡啶。路易斯酸包含金属盐化合物,例如锰、铁、钴、镍、铜或锌金属盐化合物,优选金属催化剂,例如辛酸锌或辛酸钴。偶联剂可以是硅烷和/或硅氧烷化合物。优选地,偶联剂是氨基硅烷化合物、氨基硅氧烷化合物、苯乙烯基硅烷化合物、苯乙烯基硅氧烷化合物、丙烯酸硅烷化合物、丙烯酸硅氧烷化合物、甲基丙烯酸硅烷化合物、甲基丙烯酸硅氧烷化合物、烷基硅烷化合物和烷基硅氧烷化合物中的至少一种。
在某些实施方案中,任选的组分的量为0.01-5重量%,或0.001-0.1重量%,或5-10重量%,或小于20重量%。
固化的树脂组合物及其用途:可以将可固化的组合物加工、干燥并进一步固化成固化产物。固化产物具有所需的性能,例如固定的形状。对溶剂和温度的良好耐受性、高凝胶含量、低溶胀率和低Dk/Df。所述树脂组合物在覆铜层压体(CCL)、印刷电路板、LED、其他电子涂料、轮胎、纺织品、聚合物模塑胶料、医疗模塑胶料中具有价值。印刷电路板是通过用树脂浸渍支撑或增强材料(例如玻璃纤维、织造织物、交叉层压板)、然后使树脂部分或全部固化从而形成预浸料坯而生产的。然后将预浸料与在其间的铜箔一起层压,并在150-250℃的温度和25-70kg/cm2的压力下固化,从而形成电路基板。为了制造层压体,将一层或多层预浸料与一层或多层铜层压在一起。
性能和用途:上述聚合物组合物具有非常好的介电性能,这使其对于制备可固化的组合物和用于各种应用的固化的组合物很有价值。在一个实施方案中,所述组合物具有在1GHz下测定的小于3的介电常数Dk,在1GHz下测定的小于0.002的损耗因数Df。在其他实施方案中,所述组合物在1GHz下测定的Dk为0.5-4,或1-3,或1.5-2.5。在1GHz下测定的Df值为0.0005-0.002或0.001-0.0018。
适用于电子应用的可固化树脂组合物具有低粘度,并在溶剂如烃溶剂如环己烷、甲苯、二甲苯等中具有良好的溶解性。可固化的树脂可以快速固化和胶凝,以提供具有高Tg(例如大于100℃)和浸入溶剂中时低溶胀率的固化的树脂。
所述固化的组合物的特征在于具有低的介电损耗,特别是小于或等于0.03、小于或等于0.02或小于0.003的损耗因数,所有这些都在1GHz下测定。上述介电材料还具有小于或等于80ppm/℃、小于或等于60ppm/℃或小于或等于50ppm/℃的低CTE(热膨胀系数),所有在0-150℃范围内测定。
在某些实施方案中,所述固化的组合物具有下述性能:凝胶含量为80-100重量%,基于所述固化的组合物的总重量;溶胀比低于10,或1-5,或1.5-3;根据ASTM D2240测定的90-100的肖氏A硬度;在1GHz下测定的介电常数Dk小于4,或0.5-4,或1-3.7,或1.5-2.5;在1GHz下测定的损耗因数Df小于0.004,或0.0005-0.003或0.001-0.0018。在另一个实施方案中,膨胀比低于3。
所述固化的组合物还具有约0.2-0.7W/mK或0.3-0.5W/mK的良好导热性。
所述固化的组合物可进一步具有低吸湿性,这导致在使用中和储存期间对环境条件不那么敏感的包装基材。在一个实施方案中,在23℃浸入水中24小时后,吸湿率为0.05-0.3%。
所述固化的组合物具有良好的阻燃性。在一个实施方案中,所述组合物可以达到V-0的UL 94等级。在另一个实施方案中,在不存在溴化或氯化阻燃剂的情况下,所述组合物表现出V-0等级。
所述固化的组合物还具有较低的模量和高的伸长率。这对铜互连的可靠性特别有帮助,因为它可以防止零件热循环时在镀铜过孔的壁上施加过大的应力。在一个实施方案中,拉伸模量小于3000MPa。在另一个实施方案中,伸长率大于5%。
所述固化的组合物可用于多种应用,例如覆铜层压体、印刷电路板、LED、电子涂料、纺织品、聚合物模塑胶料和医疗模塑胶料。
也可以将所述可固化的树脂组合物与轮胎橡胶混合物混合并共固化以提供轮胎橡胶组合物。使用该组合物制得的轮胎部件具有良好的性能,例如良好的湿牵引性、干处理性、良好的防滑性、低滚动阻力等。
实施例
提供以下实施例以举例说明本发明,而不意图限制本发明的范围。
聚合物组合物1(实施例1):制备星形支化偶联的嵌段共聚物(PMeS)x DVB。
在玻璃压力容器中,加入400毫升纯化并干燥的环己烷溶剂,并加入7.1毫升仲丁基锂(0.0036摩尔),然后将混合物加热至50℃并加入25克纯化并干燥的对甲基苯乙烯。使反应进行2小时,并从溶液中收集第一少量样品用于GPC和NMR分析。NMR证实第一单体完全聚合。然后,加入1.5毫升二乙烯基苯,使反应进行1小时,然后用甲醇终止反应。通过在过量的醇中沉淀分离出聚合物,并在升高的温度下真空干燥。对于收集的样品,用聚苯乙烯校准的GPC得到最终产物的主峰值分子量Mp=6400g/mol和Mp=41690g/mol。
聚合物组合物2(实施例2):制备星形支化偶联的嵌段共聚物(PMeS-PCHE)x DVB。
在彻底清洁的玻璃压力瓶中,加入300毫升纯化和干燥的环己烷溶剂,并加入16毫升仲丁基锂(1.6摩尔),然后将混合物加热至50℃,并加入5.7克纯化和干燥的对甲基苯乙烯。使反应进行45分钟,并从溶液中收集第一少量样品用于GPC分析和NMR。NMR证实该第一单体完全聚合。然后冷却至30℃并加入0.4毫升1,2-二乙氧基丙烷,然后将18.7克纯化的1,3-环己二烯加入溶液中并使其聚合2小时。从溶液中收集了少量样品用于GPC和NMR分析。NMR证实第二单体几乎完全聚合。然后,加入5.5毫升二乙烯基苯,和使反应进行17小时,然后用4毫升的2-乙基己醇终止反应,得到最终样品。将聚合物溶液转移到氢化反应器中,在70℃下于48小时内,用均相的钴催化剂和氢,在40巴下,将其转化为40%的CHD烯烃物质。洗涤溶液以除去催化剂,并用抗氧化剂稳定,通过在过量的醇中沉淀分离样品,并在高温下真空干燥。对于三个分别收集的样品,用聚苯乙烯校准的GPC得到主峰值分子量Mp=420g/mol,Mp=1166g/mol和Mp=44520g/mol。
聚合物组合物3(实施例3):制备星形支化偶联的嵌段共聚物(PMeS-PCHE)x DVB
在彻底清洁的不锈钢反应器中,加入1升纯化和干燥的环己烷溶剂,并加入78毫升仲丁基锂(0.51摩尔),然后将混合物加热至50℃,并添加45克纯化并干燥的对甲基苯乙烯。使反应进行35分钟,并从溶液中收集第一少量样品用于GPC分析和NMR。NMR证实第一单体完全聚合。然后冷却至30℃并加入1.2毫升1,2-二乙氧基丙烷,然后将87克纯化的1,3-环己二烯加入溶液中并使其聚合3.5小时。从溶液中收集了少量样品用于GPC和NMR分析。NMR证实第二单体几乎完全聚合。然后,加入17毫升二乙烯基苯,将混合物加热至60℃,并使反应进行2.5小时,然后用5.5毫升2-乙基己醇终止反应。取样和将聚合物溶液转移到氢化反应器中,在15小时内,用均相钴催化剂和氢,在40巴下,将其转化为70%的CHD烯烃物质。洗涤溶液以除去催化剂,并用抗氧化剂稳定,并通过在过量的醇中沉淀分离样品,并在升高的温度下真空干燥。对于三个分别收集的样品,用聚苯乙烯校准的GPC得到主峰值分子量Mp=1103g/mol,Mp=4050g/mol和Mp=108800g/mol。
聚合物组合物4(实施例4):制备线性PCHE-PS
在干燥的不锈钢反应器中,将5.5升纯化和干燥的环己烷溶剂加入并加热至30℃,和加入7.3毫升1,2-二乙氧基丙烷,并加入700克纯化的1,3-环己二烯,然后加入383毫升0.91摩尔引发剂以引发反应并聚合2.5小时。从溶液中收集了少量样品用于GPC和NMR分析。NMR证实第二单体几乎完全聚合。然后,加入300克纯化和干燥的苯乙烯,和使反应进行35分钟,并收集第二个样品用于GPC和NMR分析。NMR证实第三单体几乎完全聚合。然后通过添加11克甲醇终止活性溶液。将所述聚合物溶液转移到氢化反应器中,在80℃下在2小时内,用均相钴催化剂和氢,在40巴下,将其转化为90%的CHD烯烃物质。洗涤溶液以除去催化剂,用抗氧化剂稳定,并通过在过量的醇中沉淀分离样品,并在升高的温度下真空干燥。对于三个分别收集的样品,用聚苯乙烯校准的GPC得到第一个嵌段的主峰值分子量Mp=2476g/mol,最后样品的Mp=4200g/mol。最终产物的NMR分析得到苯乙烯含量为30重量%。
聚合物组合物5(实施例5):制备线性PMeS聚合物
在不锈钢反应器中,加入1升纯化和干燥的环己烷溶剂,并加入15毫升仲丁基锂(0.3摩尔),然后将混合物加热至60℃并加入50克纯化和干燥的对甲基苯乙烯。使反应进行30分钟,并从溶液中收集少量样品用于GPC和NMR分析。NMR证实第一单体的完全聚合,然后用甲醇终止反应。稳定聚合物并在高温下真空干燥。用聚苯乙烯校准的GPC得到主峰值分子量为Mp=13200g/mol。
聚合物组合物6(实施例6):制备线性聚合物PMeS
在玻璃压力容器中,加入400毫升纯化和干燥的环己烷溶剂,并加入2.5毫升仲丁基锂(0.00125摩尔),然后将混合物加热至50℃,并加入25克纯化和干燥的对甲基苯乙烯。使反应进行2小时,并从溶液中收集第一少量样品用于GPC和NMR分析。NMR证实第一单体完全聚合。通过在过量的醇中沉淀分离出聚合物,并在升高的温度下真空干燥。对于收集的样品,用聚苯乙烯校准的GPC得到主峰值分子量Mp=22670g/mol。
将GPC嵌段分子量Mp或嵌段ΔMp计算为在所考虑的嵌段完成时测定的线性共聚物的GPC嵌段Mp与就在所考虑的聚合物聚合之前测定的相同线性聚合物的GPC峰值分子量之间的差。GPC用聚苯乙烯标准物校准,因此Mp值以聚苯乙烯当量分子量表示。
聚合物或固化材料的玻璃化转变温度(Tg)通过差示扫描量热法(DSC),在第二加热过程以+20℃/min的升温速率,根据ASTM D3418进行测定。DSC热循环如下:首先以+20℃/min从30℃升温到200℃进行第一次加热过程;在200℃下保持2分钟,然后以-20℃/min从200℃降温至20℃进行第一次冷却过程;在20℃下保持2分钟,然后以+20℃/min从20℃升温至250℃进行第二次加热过程。
基于共聚物的组合物根据下一工序混合。将共聚物和其他成分与甲苯混合,直至达到均匀可倾倒的溶液或清漆。将溶液倒入涂有防粘涂层的托盘中,使其缓慢蒸发过夜,以形成组合物的薄层。然后将蒸发的层在真空下于60℃进一步干燥4小时。样品可以在更高的真空温度下进一步干燥。选择较高的干燥温度和干燥时间以高于共聚物Tg,但不达到导致过早固化的条件。
使用真空平板硫化机(MDR)进行组合物固化。将样品引入预先设定为110℃(或共聚物Tg,如果这是更高的话)的机器模具中,以形成厚度为0.7mm的板。将模具在真空下关闭,并在该温度下保持2分钟。然后将模具温度提高到180℃。将样品在真空下于180℃固化30分钟。最后,将模具冷却以收集固化的组合物。在180℃的固化步骤中记录MDR最大扭矩值(以dN*m表示),该值对应于该固化期间重新编码的最大扭矩。达到最大扭矩值的90%所需的时间记录为tc90,以分钟和秒表示。
分析固化样品的凝胶含量和溶胀比。在将样品浸入大量甲苯中1天之前,测定固化样品的初始重量(Wi)。然后过滤包含样品的溶液,并记录过滤后的溶胀凝胶的重量(Ws)。然后将溶胀凝胶在真空下于60℃干燥,直到达到恒重,即干燥后的重量(Wd)。使用下式计算凝胶含量(凝胶%):凝胶%=100×Wd/Wi。溶胀比使用下式计算:溶胀比=Ws/Wd。
成分描述:DCP:过氧化二枯基;BIPB:双(叔丁基过氧异丙基)苯;TAC:三烯丙基氰脲酸酯;TAIC:三烯丙基异氰脲酸酯。
表4:聚合物组成和对比聚合物单体单元组成,实施例4的聚合物具有苯乙烯单元(iii),其中<10摩尔%的该单元被氢化,ND表示未检测到。
氢化单元在单元之前带有前缀h。pMeS是对甲基苯乙烯;DVB是二乙烯基苯;CHD为1,3-环己二烯;H2(CHD)为氢化的环己二烯;St是苯乙烯。
表5:聚合物组成和对比聚合物单体单元组成,实施例4聚合物具有30重量%的聚合单元(iii)和嵌段F含量
表6:聚合物组成以及对比聚合物结构和性能,()表示聚合物嵌段;[]表示聚合物臂,CE:偶联率
表7:可固化的组合物和固化的组合物的性能
在低的固化剂添加水平下和甚至在高的水平下,所述对比物都不会导致高凝胶含量。一个对比物导致高凝胶,但是尽管凝胶含量高,但是固化的组合物不能抵抗溶胀,固化溶胀比大于5。实施例10-14显示出即使在低的固化剂下具有良好的固化水平,和低的溶胀比显示出固化后良好的耐溶剂性。
Claims (15)
1.一种聚合物组合物,其包含具有多个聚合物臂的星形支化共聚物,其中每个聚合物臂的峰值分子量为1-50kg/mol,和每个聚合物臂包括:
得自包含自由基反应性基团的第一乙烯基芳族单体的聚合单元(i),其中大于10摩尔%至100摩尔%的聚合单元(i)是未氢化的;
聚合单元(ii),其包括:氢化或非氢化形式的得自高Tg单体的聚合单元,和氢化形式的得自包含自由基反应性基团的第一乙烯基芳族单体的聚合单元或氢化形式的聚合苯乙烯单元,其中所述高Tg单体选自叔丁基苯乙烯、1,3-环己二烯、1,3-环庚二烯、苯并富勒烯、1,1-二苯基乙烯、乙烯基联苯、金刚烷基苯乙烯、乙烯基蒽、二乙烯基苯、双(乙烯基苯基)乙烷、及其组合,和其中得自1,3-环己二烯的聚合单元包括相对摩尔比为90:10-10:90的1,2-加成单元和1,4-加成单元;和
任选地,聚合单元(iii),其包括:(a)得自一个或多个无环共轭二烯的聚合单元,和(b)得自一种或多种第二乙烯基芳族单体的聚合单元,其中小于10重量%的(a)是未氢化的;
其中所述共聚物包含大于10重量%的聚合单元(i),聚合单元(i)和(ii)一起占所述共聚物总重量的大于50重量%;
其中所述共聚物具有15-500kg/mol的峰值分子量和大于100℃至250℃的玻璃化转变温度。
2.权利要求1所述的聚合物组合物,其中所述第一乙烯基芳族单体选自:
式(I)的取代的苯乙烯
式(II)的乙烯基苯并环丁烯
式(III)的乙烯基二氢茚
式(IV)的四氢萘
其中R1是H或CH3,R2和R2’独立地为H或CH3;和
前述第一乙烯基芳族单体的组合;
其中所述聚合物组合物具有大于30kg/mol的分子量Mp和小于2,000cP的溶液粘度,其中所述粘度在25℃于甲苯中25重量%的聚合物组合物含量下测定;以及
其中所述星形支化共聚物占所述聚合物组合物总重量的大于80重量%。
3.权利要求1-2任一项所述的聚合物组合物,其包含大于1重量%的聚合单元(ii),相对于所述聚合物组合物的总重量。
4.权利要求2所述的聚合物组合物,其中所述星形支化共聚物是包括多个聚合物臂的星形支化嵌段共聚物,其中每个聚合物臂包括一个或多个聚合物嵌段;其中大于70重量%的一个或多个聚合物嵌段包括至少80重量%的聚合单元(i)和(ii)的组合;和其中所述聚合物组合物具有根据ASTM D2240测定的大于80的肖氏A的硬度。
5.权利要求1所述的聚合物组合物,其中,大于50摩尔%的聚合的1,3-环己二烯单元被氢化。
6.权利要求1所述的聚合物组合物,其中在聚合单元(i)中,第一乙烯基芳族单体是对甲基苯乙烯,聚合单元(ii)包括氢化形式的聚合的对甲基苯乙烯、聚合的二乙烯基苯、聚合的叔丁基苯乙烯、或其组合;和其中聚合单元(i)和(ii)一起占所述聚合物组合物总重量的大于60重量%。
7.权利要求1-2任一项所述的聚合物组合物,其包含聚合单元(iii),其中所述第二乙烯基芳族单体是苯乙烯,所述无环共轭二烯选自丁二烯、异戊二烯、及其组合。
8.权利要求4所述的聚合物组合物,其中所述星形支化嵌段共聚物包括一个或多个聚合物嵌段D,任选的一个或多个聚合物嵌段E和任选的一个或多个聚合物嵌段F;且其中一个或多个嵌段D包括大于50重量%的聚合单元(i),一个或多个嵌段E包括大于50重量%的聚合单元(ii),一个或多个嵌段F包括大于50重量%的聚合单元(iii);
其中所述聚合物组合物具有一种或多种选自以下的构型:(D-)nX,(D-E-)nX,(E-D-)nX,(D-E-D-)nX,(D-F-E-)nX,(D-E-F-)nX,(E-F-D-)nX和(E-D-F-)nX,其中n是大于2至50的整数,X是偶联剂残基;
其中所述星形支化嵌段共聚物的总峰值分子量为25-300kg/mol,和所述多个臂中的每一个的峰值分子量为1-30kg/mol。
9.权利要求8所述的聚合物组合物,其中所述一个或多个聚合物嵌段D包括聚合的对甲基苯乙烯单元。
10.权利要求8-9任一项所述的聚合物组合物,其包含一个或多个聚合物嵌段E,其中所述聚合单元(ii)包括氢化形式的得自1,3-环己二烯、对甲基苯乙烯或二乙烯基苯的聚合单元。
11.权利要求8-9任一项所述的聚合物组合物,其包含一个或多个聚合物嵌段F,其中所述聚合单元(iii)包括氢化形式的得自苯乙烯和丁二烯或异戊二烯的聚合单元。
12.权利要求1-2任一项所述的聚合物组合物,其中所述组合物具有小于3的在1GHz下测定的介电常数Dk和小于0.002的在1GHz下测定的损耗因数Df。
13.一种可固化的组合物,其包含权利要求1-12任一项所述的聚合物组合物、固化剂、共固化剂和一种或多种添加剂;
其中所述共固化剂选自二乙烯基苯、1,2-双(乙烯基苯基)乙烷、三烯丙基氰脲酸酯、三烯丙基异氰脲酸酯、乙烯基官能化的聚苯醚树脂、双马来酰亚胺树脂、液态或固态二烯基聚合物;
其中所述添加剂选自填料、阻燃剂、玻璃化转变温度为100-200℃的聚烯烃、芳族树脂、橡胶、抗氧化剂、UV稳定剂、UV自由基引发剂、抗收缩添加剂、粘合促进剂、着色剂、及其组合。
14.一种固化的组合物,其由权利要求13所述的可固化的组合物制备,其中所述固化的组合物具有:
80-100重量%的凝胶含量,基于所述固化的组合物的总重量;
低于5的溶胀比;
90-100的肖氏A硬度,根据ASTM D2240测定;
小于3.7的在1GHz下测定的介电常数Dk;和
小于0.003的在1GHz下测定的损耗因数Df。
15.权利要求14所述的固化的组合物,其中所述组合物用于覆铜层压体、印刷电路板、LED、电子涂料、纺织品、聚合物模塑胶料和医疗模塑胶料中。
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