CN114555701A - 用于无电镀中的聚合物组合物、无电镀的方法和通过无电镀制成的聚合物制品 - Google Patents
用于无电镀中的聚合物组合物、无电镀的方法和通过无电镀制成的聚合物制品 Download PDFInfo
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- CN114555701A CN114555701A CN202080072200.1A CN202080072200A CN114555701A CN 114555701 A CN114555701 A CN 114555701A CN 202080072200 A CN202080072200 A CN 202080072200A CN 114555701 A CN114555701 A CN 114555701A
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Classifications
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Abstract
一种用于无电镀的组合物,其包含:9至29重量%、9.7至29重量%、或10至29重量%的第一接枝橡胶共聚物,其包含聚合形式的至少一种共轭二烯单体和至少一种单乙烯基芳族单体;70至90重量%、优选70‑89.7重量%、更优选70至85重量%的未接枝苯乙烯类聚合物;0.1至10重量%的具有100至500纳米(nm)的粒度的基于二烯的核/壳橡胶;0.1至5重量%的总量的稳定剂和/或抗氧化剂中的一种或多种;0.1至2重量%的量的脂肪酸或脂肪酸的盐;0至5重量%的脱模剂;0至1重量%的金属氧化物;0至3重量%的润滑剂;和0至20重量%的聚碳酸酯;其中重量%和ppm是基于所述组合物的总重量。所述组合物可被成型为具有无电镀于所述组合物上的金属涂层的制品。
Description
发明背景
对塑料制品镀金属被用于各种领域中。例如,在电子领域中无电镀已被用于形成印刷电路板中的导电镀通孔。作为另一个实例,在汽车工业中聚合物部件的镀铬被用于制作各种汽车部件。在某些应用中,制成的制品在使用期间经受宽温度范围,在此期间涂层必须保持对基材良好的粘附。例如,当镀金属的聚合物汽车部件可被暴露于远低于0℃和远高于90℃的温度时。
当前无电镀面临的一个挑战是在金属镀层与聚合物基材之间存在适当粘附的情况下获得制品,甚至在重复的剧烈温度循环后也是如此。此外,当前无电镀面临的另一个挑战是提供一种允许制品成型(例如通过注塑)和随后无电镀(通常接着是电解电镀-即电镀另外的金属层)的合理宽的加工窗口、同时在最终制品中提供良好性质的组合物。制品的潜在重要性质的实例包括以下的一种或多种:在最终制品中的冲击强度、拉伸强度、拉伸模量、挠曲模量,热膨胀系数,一致的高反射外观,和金属涂层与聚合物基材之间良好的粘附。
发明内容
本文所公开的是一种用于无电镀的组合物,其包含:9至29重量%、优选9.7至29重量%、更优选10至29重量%的具有骨架的第一接枝橡胶共聚物,所述骨架包含至少一种聚合形式的共轭二烯单体,所述第一接枝橡胶共聚物具有接枝于骨架的聚合形式的至少一种选自单乙烯基芳族单体、丙烯酸类单体和它们的组合的单体;70至90重量%、优选70-89.7重量%、更优选70至85重量%的未接枝于聚合的共轭二烯橡胶的苯乙烯类聚合物;0.1至10重量%的具有100至500纳米(nm)粒度的基于二烯的核/壳橡胶,0.1至5重量%的总量的稳定剂和/或抗氧化剂中的一种或多种,0.1至2重量%的量的脂肪酸或脂肪酸的盐,0至5重量%的脱模剂,0至1重量%的金属氧化物,0至3重量%的润滑剂,和0至20重量%的聚碳酸酯,其中重量%和ppm是基于组合物的总重量。替代地,上文所表示组分的量可为重量份。
还公开了一种包含所述组合物的制品。制品可具有被无电镀于组合物上的金属涂层。
还公开了一种制作这种制品的方法,所述方法包括使组合物成型为所需形状,并且将一种或多种金属无电镀于成型的组合物上。无电镀方法可包括使用氧化性酸的蚀刻步骤。无电镀步骤可接着是电镀(例如电解电镀)一个或多个另外的金属层。
发明详述
尽管丙烯腈/丁二烯/苯乙烯接枝橡胶(ABS)组合物可被无电镀,但仍需要单独或组合地展示以下特性中的一种或多种的组合物:与无电镀和电解电镀于其上的金属涂层良好的粘附(特别是在热循环后),由组合物形成制品(例如通过注塑)的宽加工窗口,随后无电镀这类制品的宽加工窗口以提供金属涂层中无缺陷或缺陷很少的制品,和最终制品中诸如冲击强度、拉伸强度、拉伸模量、挠曲模量的良好力学性质。热膨胀系数可使得组合物可为在无电镀制品中有用的。
已提出了各种组合物。例如,WO 2013/116903提供了电镀组合物的实例,其包含聚碳酸酯(PC)、至少主要ABS冲击改性剂和化学上不同于主要冲击改性剂的次要冲击改性剂。WO2013/115903公开了当聚(苯乙烯丙烯腈)(SAN)也被包括在使用PC和两种不都是ABS的冲击改性剂的组合物中时,相比于包含单一ABS改性剂的组合物,电镀样品的粘附值减小。另外,WO2013/115903显示出将甲基丙烯酸酯丁二烯苯乙烯(MBS)作为次要冲击改性剂添加至ABS和PC的组合物在较低聚碳酸酯含量下使电镀样品的粘附值减小。意外地,鉴于WO2013/116903关于粘附减少的配方的教导,包含9至29重量%、优选9.7至29重量%、更优选10至29重量%的至少一种共轭二烯单体和至少一种单乙烯基芳族单体的接枝橡胶,70至90重量%、优选70-89.7重量%、更优选70至85重量%的未接枝苯乙烯类聚合物,0.1至10重量%的具有100至500nm粒度的基于二烯的核/壳橡胶,和0.1至2重量%的量的脂肪酸或脂肪酸的盐的本文所公开的组合物相比于不包括基于丁二烯的核/壳橡胶的类似组合物显示出更好的粘附(包括在热循环后)。在组合物中共轭二烯橡胶(例如第一接枝橡胶共聚物的骨架和基于二烯的核/壳橡胶的二烯橡胶核)的总量可为基于组合物的总重量计10至20重量%。替代地,上文所表示组分的量可为重量份。
第一接枝橡胶共聚物
诸如ABS的接枝橡胶共聚物含有两个或更多个化学键合的具有不同组成的聚合物部分。这类接枝橡胶共聚物可通过首先使共轭二烯诸如丁二烯或另外的共轭二烯、任选地与可与其共聚的单体诸如苯乙烯聚合,以提供聚合物骨架。在形成聚合物骨架后,在聚合物骨架的存在下使至少一种、且优选两种接枝单体聚合以获得接枝共聚物。这些树脂可通过本领域众所周知的方法、例如乳液或悬浮自由基聚合来制备。
聚合物骨架优选为共轭二烯聚合物,诸如聚丁二烯、聚异戊二烯,或共聚物,诸如丁二烯-苯乙烯、丁二烯-丙烯腈或类似物。
通常在制备接枝共聚物的聚合物骨架中利用的共轭二烯单体可由下式(I)描述:
其中Xb为氢、C1-C5烷基、氯、溴或类似物。可使用的共轭二烯单体的实例是丁二烯,异戊二烯,1,3-庚二烯,甲基-1,3-戊二烯,2,3-二甲基-1,3-丁二烯,2-乙基-1,3-戊二烯,1,3-和2,4-己二烯,氯和溴取代的丁二烯,诸如二氯丁二烯,溴代丁二烯,二溴丁二烯,包含前述共轭二烯单体中至少一种的混合物,和类似物。优选的共轭二烯单体是丁二烯。
可在聚合物骨架的存在下聚合的一种单体或单体的组是单乙烯基芳族烃。所利用的单乙烯基芳族单体可由下式(II)描述:
其中Xc为氢、C1-C12烷基(包括环烷基)、C6-C12芳基、C7-C12芳烷基、C7-C12烷芳基、C1-C12烷氧基、C6-C12芳氧基、氯、溴或类似物。单乙烯基芳族单体的实例包括苯乙烯,3-甲基苯乙烯,3,5-二乙基苯乙烯,4-正丙基苯乙烯,α-甲基苯乙烯,α-甲基乙烯基甲苯,α-氯代苯乙烯,α-溴代苯乙烯,二氯苯乙烯,二溴苯乙烯,四氯苯乙烯,包含前述化合物中至少一种的混合物,和类似物。优选的单乙烯基芳族单体是苯乙烯。
可在聚合物骨架的存在下聚合的第二组单体是丙烯酸类单体,诸如丙烯腈或取代的丙烯腈。
丙烯腈、取代的丙烯腈可由下式(III)描述:
其中Xb是如前文定义的,并且Y2是氰基或类似物。这类单体的实例包括丙烯腈,乙基丙烯腈,甲基丙烯腈,α-氯代丙烯腈,β-氯代丙烯腈,α-溴代丙烯腈,β-溴代丙烯腈,包含前述单体中至少一种的混合物,和类似物。优选的单体是丙烯腈。
在接枝共聚物的制备中,聚合物骨架(例如衍生自共轭二烯单体和任选的单乙烯基芳族共聚单体和/或丙烯酸系共聚单体)可占接枝共聚物组合物的总重量的至少15重量%或至少20重量%,至多65重量%或至多60重量%或至多50重量%。例如,接枝共聚物组合物可包含基于接枝共聚物组合物的总重量计15至65重量%、或15至60重量%或15至50重量%、或20至65重量%、或20至60重量%或20至50重量%的衍生自共轭二烯单体的聚合物骨架。由苯乙烯和丙烯腈例示的在聚合物骨架的存在下聚合的单体可占基于总接枝聚合物组合物的总重量计35重量%或40重量%或50重量%至85重量%或至80重量%。例如,接枝共聚物组合物可包含35至85重量%或40至90重量%的一种或多种选自单乙烯基芳族单体和丙烯酸类单体的共聚单体。接枝聚合物组合物的由丙烯腈例示的丙烯酸类单体可占总接枝共聚物组合物的5重量%至40重量%。由苯乙烯例示的单乙烯基芳族烃可占总接枝共聚物的10至70重量%。
然而,在制备接枝共聚物组合物的过程中,正常的是一定百分比的接枝于聚合物骨架上的聚合单体相互组合并且存在为游离共聚物。例如,如果苯乙烯被用作接枝单体中的一种且丙烯腈作为第二接枝单体,组合物的某一部分将共聚为游离、即未接枝的苯乙烯-丙烯腈共聚物。在用α-甲基苯乙烯(或其他单体)代替用于制备接枝聚合物的组合物中的苯乙烯的情况下,一定百分比的组合物可为α-甲基苯乙烯-丙烯腈共聚物。因此,接枝共聚物自身(不包括在骨架的存在下聚合的单体的游离聚合物或共聚物)可包含55或60至80或至75或至70重量%的包含共轭二烯单体的聚合形式的骨架,和20或25至50或至45或至40重量%的接枝于骨架的呈聚合形式的聚合单体。例如,接枝共聚物可包含55至75重量%或60至70重量%的衍生自共轭二烯单体的骨架和25至45重量%或30至40重量%的接枝于骨架上的一种或多种式II和/或III的单体的共聚物。
第一橡胶接枝共聚物组合物可为丙烯腈/丁二烯/苯乙烯。ABS共聚物组合物可包含基于ABS共聚物的总重量计20-65重量%的基于丁二烯的内含物(即,衍生自丁二烯单体)。基于苯乙烯的内含物(即,衍生自苯乙烯)与基于丙烯腈的内含物(即,衍生自丙烯腈)的重量比可为至少65:35。基于苯乙烯的内含物与基于丙烯腈的内含物的重量比可不超过80:20。然而,对于接枝共聚物自身(不包括未接枝于基于丁二烯的骨架的游离聚苯乙烯、游离丙烯腈或游离苯乙烯丙烯腈),基于丁二烯的内含物的重量%可为接枝共聚物的55或60至80或至75或至70重量%,并且接枝的苯乙烯丙烯腈可为基于接枝共聚物的总重量计20或25或30重量%至45或40重量%。接枝部分(即,接枝于丁二烯衍生的骨架的苯乙烯丙烯腈)可为基于骨架的重量计40-60重量%或45至55重量%。
第一橡胶接枝共聚物可具有至少50纳米或至少100纳米的粒度。第一橡胶接枝共聚物可具有至多1000纳米或800纳米的粒度。粒度可通过光散射UV-Vis光谱法、扫描电子显微术(SEM)、透射电子显微术(TEM)等来测量。平均粒度可根据ASTM D1417(2010)来测定。第一橡胶接枝共聚物可具有至少10%的凝胶含量。第一橡胶接枝共聚物可具有至多50%的凝胶含量。凝胶含量可通过D2765-16使用四氢呋喃(THF)或丙酮作为溶剂来测量。第一橡胶接枝共聚物可为具有如本文所述的粒度和/或凝胶含量的如本文所述的ABS。
第一橡胶接枝共聚物的量可为基于组合物的总重量计至少9重量%,优选至少9.7重量%,更优选至少10重量%,甚至更优选至少15重量%,和至多29或25重量%。第一橡胶接枝共聚物组合物(包括接枝于骨架的单体的未接枝聚合物)的量可为基于组合物的总重量计10至59重量%或至55重量%或至50重量%。例如,组合物可使用基于组合物的总重量计10至59重量%或20至55重量%、或30至55重量%、或35至50重量%的量的由ABS(包括游离未接枝的SAN)例示的第一橡胶接枝共聚物组合物制成。
基于二烯的核/壳橡胶
组合物还包含基于二烯的核-壳橡胶。基于二烯的核-壳橡胶在其化学组成、形态或两者上不同于第一橡胶接枝共聚物。
基于二烯的核壳橡胶的核包含诸如式(I)中的共轭二烯单体的聚合物或共聚物。例如,核可包含聚丁二烯、聚异戊二烯,或共聚物,诸如丁二烯-苯乙烯、丁二烯-丙烯腈或类似物。根据优选实施方案,核为聚丁二烯。核可为基于橡胶的总重量计基于二烯的核/壳橡胶的至少70重量%或至少80重量%。核可为基于橡胶的总重量计基于二烯的核/壳橡胶的至多95重量%或至多90重量%。例如,基于二烯的核/壳橡胶可包含基于基于二烯的核/壳橡胶的总重量计70至95重量%或80至95重量%或75至90重量%的量的如由聚丁二烯例示的核。
壳接枝于核。壳可包含根据式(II)的乙烯基芳族单体中的一种或多种和/或一种或多种如式(IV)中所示的丙烯酸类单体的聚合形式:
其中Xb是如前文定义的,并且Y2是氰基、C1-C12烷氧基羰基或类似物。这类单体的实例包括丙烯腈,乙基丙烯腈,甲基丙烯腈,α-氯代丙烯腈,β-氯代丙烯腈,α-溴代丙烯腈,β-溴代丙烯腈,丙烯酸甲酯,甲基丙烯酸甲酯,丙烯酸乙酯,丙烯酸丁酯,丙烯酸丙酯,丙烯酸异丙酯,包含前述单体中至少一种的混合物,和类似物。
这类丙烯酸类单体的实例包括丙烯腈、取代的丙烯腈和/或丙烯酸酯,由丙烯腈例示,和C1-C7烷基丙烯酸酯,诸如甲基丙烯酸甲酯,和类似物。优选丙烯酸酯,诸如甲基丙烯酸甲酯。
基于二烯的核/壳橡胶可包含至少5重量%或至少10重量%的基于一种或多种丙烯酸类单体的内含物。基于二烯的核/壳橡胶可包含基于橡胶的总重量计至多29或20重量%的基于一种或多种丙烯酸类单体的内含物。基于二烯的核/壳橡胶可包含基于基于二烯的核/壳橡胶的总重量计至少0.1重量%或至少0.5重量%或至少1重量%或至少2重量%的基于一种或多种单乙烯基芳族单体的内含物。基于二烯的核/壳橡胶可包含基于橡胶的总重量计至多10重量%或至多5重量%的基于一种或多种单乙烯基芳族单体的内含物。例如,基于二烯的核/壳橡胶可包含基于基于二烯的核/壳橡胶的总重量计5至29重量%或5至20重量%的由甲基丙烯酸甲酯例示的丙烯酸类单体,和0.1至10重量%的由苯乙烯例示的单乙烯基芳族单体。
优选地,基于二烯的核/壳橡胶是甲基丙烯酸甲酯/丁二烯/苯乙烯(MBS)。核/壳MBS橡胶可包含基于MBS的总重量计至少70重量%或至少80重量%的聚丁二烯核。核/壳MBS橡胶可包含基于MBS的总重量计至多95重量%或至多90重量%的聚丁二烯核。基于甲基丙烯酸甲酯的内含物的量可为基于MBS的总重量计至少5重量%或至少10重量%。基于甲基丙烯酸甲酯的内含物的量可为基于MBS的总重量计至多29重量%或至多20重量%。基于单乙烯基芳族(例如苯乙烯)的内含物的量可为基于MBS的总重量计至少0.1重量%或至少0.5重量%或至少1重量%或至少2重量%。基于单乙烯基芳族的内含物的量可为基于MBS的总重量计至多10重量%或至多5重量%。例如,基于二烯的核/壳橡胶可包含基于MBS的总重量计70至95重量%的聚丁二烯核,5至20重量%的作为壳的部分的基于甲基丙烯酸甲酯的内含物,和0.1至5重量%的基于苯乙烯的内含物。
基于二烯的核/壳橡胶的特征在于核-壳颗粒相对小的粒度。基于二烯的核/壳橡胶颗粒可具有至少100纳米(nm)的平均粒度。基于二烯的核/壳橡胶颗粒可具有至多500nm、或至多400nm、或至多300nm的平均粒度。例如,颗粒可具有100至500nm、或100至400nm的平均粒度。粒度可根据ASTM B822-17通过光散射来测量。
包括除第一接枝橡胶共聚物以外小的基于二烯的核/壳橡胶被认为有利于以下的一种或多种:改良或控制组合物在加工(例如注塑)期间的流变性,在作为无电镀过程的部分的蚀刻期间控制孔径,冲击强度(尤其是在低温下),和抗裂性。
基于二烯的核/壳橡胶的量为基于组合物的总重量计至少0.1重量%或至少0.5重量%或至少1重量%或至少2重量%或至少3重量%。基于二烯的核/壳橡胶的量为基于组合物的总重量计至多10重量%或至多9重量%或至多8重量%或至多7重量%或至多6重量%或至多5重量%。例如,组合物可包含基于组合物的总重量计0.1至10重量%、或0.5至9重量%、或1至8重量%、或1至7重量%、或2至6重量%或3至5重量%的量的基于二烯的核/壳橡胶。以较大颗粒ABS接枝橡胶为代价,配方中存在过多小粒度核壳橡胶可能导致非最优蚀刻和非最优孔径分布,金属镀层粘附减少。
未接枝苯乙烯类聚合物和共聚物
尽管第一接枝橡胶组合物可包括来自制作第一接枝橡胶组合物的过程的一些游离苯乙烯类聚合物残留物,但本文所公开的组合物具有以基于组合物的总重量计70至90重量%、优选70-89.7重量%、更优选70至85重量%的量存在的苯乙烯类聚合物。因此,一些未接枝苯乙烯类聚合物被加入第一接枝橡胶组合物和小粒度核壳橡胶。
本文中所使用的术语“苯乙烯类聚合物”(包括苯乙烯类共聚物)包括采用一种或多种式(II)的单乙烯基芳族烃,通过本领域已知的方法(包括本体、悬浮和乳液聚合)制备的聚合物。苯乙烯类共聚物可为无规或嵌段共聚物。单乙烯基芳族单体的实例包括苯乙烯,3-甲基苯乙烯,3,5-二乙基苯乙烯,4-正丙基苯乙烯,α-甲基苯乙烯,α-甲基乙烯基甲苯,α-氯代苯乙烯,α-溴代苯乙烯,二氯苯乙烯,二溴苯乙烯,四氯苯乙烯,包含前述化合物中至少一种的混合物,和类似物。优选的单乙烯基芳族单体是苯乙烯。
这些聚合物可含有共聚单体,诸如乙烯基单体,丙烯酸类单体(包括甲基丙烯酸类单体),马来酸酐和衍生物,和类似物,以及它们的组合。如本文所定义,乙烯基单体是具有一个或至少一个可聚合碳碳双键的脂族化合物。合适的乙烯基单体包括例如乙烯,丙烯,丁烯(包括1-丁烯、2-丁烯和异丁烯),戊烯,己烯,和类似物,以及它们的组合。
丙烯酸类单体包括例如丙烯腈,乙基丙烯腈,甲基丙烯腈,α-氯代丙烯腈,β-氯代丙烯腈,α-溴代丙烯腈,和β-溴代丙烯腈,丙烯酸甲酯,甲基丙烯酸甲酯,丙烯酸乙酯,丙烯酸丁酯,丙烯酸丙酯,丙烯酸异丙酯,和类似物,以及它们的混合物。丙烯腈腈类单体可在许多情况下赋予改进的抗溶剂性。
马来酸酐和其衍生物包括例如马来酸酐,马来酰亚胺,N-烷基马来酰亚胺,N-芳基马来酰亚胺,或者烷基或卤素取代的N-芳基马来酰亚胺,和类似物,以及它们的组合。丙烯腈是优选的共聚单体。
苯乙烯类共聚物中存在的一种或多种共聚单体的量可变化。共聚物可包含至少50重量%或至少60重量%或至少65重量%的衍生自单乙烯基芳族单体的内含物(例如聚合的苯乙烯单体的量)。共聚物可包含至多90重量%或至多85重量%或至多80重量%的衍生自诸如苯乙烯的单乙烯基芳族单体的内含物。共聚物可包含至少10重量%或至少15重量%或至少20重量%、至多40重量%或至多50重量%或至多35重量%的衍生自上文规定的共聚单体(例如取代或未取代的丙烯腈)的内含物。单体或单体衍生的内含物的重量%是基于苯乙烯类共聚物的总重量计。例如,苯乙烯类聚合物可包含基于苯乙烯类聚合物的总重量计50至90%含量的聚合的由苯乙烯例示的单乙烯基芳族单体,和10至50重量%聚合的由丙烯腈例示的共聚单体。
一种优选的聚苯乙烯类共聚物树脂是聚(苯乙烯丙烯腈),即SAN。SAN可具有如由ASTM D5296-11通过凝胶渗透色谱法(GPC)使用聚苯乙烯标准品测量的50,000至160,000g/mol的重均分子量。
在组合物中未接枝苯乙烯类聚合物的量(包括被提供为第一接枝橡胶共聚物组合物的一部分的任何量的未接枝苯乙烯类聚合物)为基于组合物的总重量计70至90重量%,优选70-89.7重量%,更优选70至85重量%。如果第一接枝橡胶共聚物组合物和/或核-壳具有高橡胶含量(例如对于第一接枝橡胶共聚物高含量的橡胶骨架),则可添加更多游离苯乙烯类以实现在组合物中基于组合物的总重量计10至20重量%的总橡胶含量。
脂肪酸或脂肪酸盐
组合物还包含一种或多种脂肪酸或脂肪酸的盐。脂肪酸是具有8至40个碳原子的有机酸。盐是这类酸的盐。因此,脂肪酸可具有式R-COOH且盐可具有式R-COOM,其中R为具有至少8个或至少碳原子、至多40个或至多36个或至多30个或至多24个或至多20个碳原子的烃,且M为金属离子。R可为饱和或不饱和烃,且可为直链或支链的,但常为直链的。R可为烷基。R可为烯基。如果碳原子数过少,则脂肪酸可能是过于挥发性的。如果碳原子数过多,则脂肪酸可能不足以相容于聚合物组合物中。可使用脂肪酸的混合物。合适的脂肪酸和它们的盐的实例包括肉豆蔻酸,亚油酸,棕榈酸,油酸,硬脂酸,反油酸,硬脂酸,和它们的盐,以及它们的任何组合。
优选脂肪酸碱金属盐。由于潜在的毒性和不利的环境影响,应避免脂肪酸的铅、汞、铊、镉、钡或锑盐。
脂肪酸或脂肪酸盐可协助二烯橡胶颗粒在组合物中的分散,并且还可提供金属释放效果。
所有脂肪酸和脂肪酸盐的总量为基于组合物的总重量计至少1000ppm或至少2000ppm或至少3000ppm。所有脂肪酸和脂肪酸盐的总量为基于组合物的总重量计不多于20,000ppm或不多于15,000ppm或不多于10,000ppm。例如,组合物可包含基于组合物的总重量计1000至20,000ppm、或2000至15,000ppm、或3000至10,000ppm的量的脂肪酸和脂肪酸盐。如果脂肪酸过多,在注塑过程中可能有压汁(或在模具上形成液体)的问题。
抗氧化剂和稳定剂
所公开的组合物还可包含一种或多种抗氧化剂。抗氧化剂的实例包括受阻酚,芳基仲胺,含磷化合物、诸如亚磷酸酯或膦酸酯,含硫化合物、诸如硫酯,或它们的任何组合。更具体的抗氧化添加剂包括例如:有机亚磷酸酯,诸如三(壬基苯基)亚磷酸酯,三(2,4-二-叔丁基苯基)亚磷酸酯,双(2,4-二-叔丁基苯基)季戊四醇二亚磷酸酯,二硬脂基季戊四醇二亚磷酸酯,或类似物;烷化单酚或多酚;多酚与二烯的烷化反应产物,诸如四[亚甲基(3,5-二-叔丁基-4-羟基氢化肉桂酸酯)]甲烷,或类似物;对甲酚或二聚环戊二烯的丁基化反应产物;烷化氢醌;羟基化硫代二苯醚;次烷基双酚;苄基化合物;β-(3,5-二-叔丁基-4-羟苯基)-丙酸与一羟基或多羟基醇的酯;β-(5-叔丁基-4-羟基-3-甲基苯基)-丙酸与一羟基或多羟基醇的酯;硫代烷基或硫代芳基化合物的酯,诸如二硬脂基硫代丙酸酯,二月桂基硫代丙酸酯,二(十三烷基)硫代二丙酸酯,十八烷基-3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯,季戊四醇基-四[3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯,或类似物;β-(3,5-二-叔丁基-4-羟苯基)-丙酸的酰胺,或类似物;或包含前述抗氧化剂中至少一种的组合。当使用时,抗氧化剂可以基于组合物的总重量计至少0.01重量%或至少0.05重量%或至少0.1重量%至5重量%或至3重量%或至1重量%的量被包括。例如,组合物可包含基于组合物的总重量计0.01至5重量%、或0.05至3重量%、或0.1至1重量%的量的抗氧化剂。
合适的稳定剂添加剂包括热或光稳定剂。
热稳定剂的实例包括:有机亚磷酸酯,诸如三苯基亚磷酸酯,三-(2,6-二甲基苯基)亚磷酸酯,三-(混合单和二壬基苯基)亚磷酸酯,或类似物;膦酸酯,诸如二甲基苯膦酸酯,或类似物;有机磷酸酯,诸如磷酸三甲酯;硫酯,诸如季戊四醇β月桂基硫代丙酸酯,和类似物;或包含前述热稳定剂中至少一种的组合。当使用时,热稳定剂可以基于组合物的总重量计至少0.01重量%或至少0.05重量%或至少0.1重量%、至多5重量%或至多3重量%或至多1重量%的量被包括。例如,组合物可包含基于组合物的总重量计0.01至5重量%、或0.05至3重量%、或0.1至1重量%的量的热稳定剂。
虽然电镀部件通常被保护免受光反应,但也可使用光稳定剂和/或紫外光(UV)吸收添加剂,尤其是在部件仅被部分电镀的情况下。合适的光稳定剂添加剂包括例如苯并三唑,诸如2-(2-羟基-5-甲基苯基)苯并三唑,2-(2-羟基-5-叔辛基苯基)-苯并三唑和2-羟基-4-正辛氧基二苯甲酮;受阻胺光稳定剂(HALS),或类似物;或包含前述光稳定剂中至少一种的组合。当使用时,光稳定剂可以基于组合物的总重量计至少0.01或至少0.05或至少0.1、至多10或至多5或至多3重量%的量被包括。例如,组合物可包含基于组合物的总重量计0.01至5重量%、或0.05至3重量%、或0.1至1重量%的量的光稳定剂。合适的UV吸收添加剂包括例如:羟基二苯甲酮,羟基苯并三唑,羟基苯并三嗪,氰基丙烯酸酯,草酰替苯胺,苯并噁嗪酮,2-(2H-苯并三唑-2-基)-4-(1,1,3,3-四甲基丁基)苯酚(CYASORBTM5411),2-羟基-4-正辛基氧基二苯甲酮(CYASORB*531),2-[4,6-双(2,4-二甲基苯基)-1,3,5-三嗪-2-基]-5-(辛氧基)苯酚(CYASORB*1164),2,2*-(1,4-亚苯基)双(4H-3,1-苯并噁嗪-4-酮)(CYASORB*UV-3638),1,3-双[(2-氰基-3,3-二苯基丙烯酰)氧基]-2,2-双[[(2-氰基-3,3-二苯基-丙烯酰基)氧基]甲基]丙烷(UVINUL*3030),2,2*-(1,4-亚苯基)双(4H-3,1-苯并噁嗪-4-酮),1,3-双[(2-氰基-3,3-二苯基丙烯酰)氧基]-2,2-双[[(2-氰基-3,3-二苯基-丙烯酰基)氧基]甲基]丙烷,或包含前述UV吸收剂中至少一种的组合。当使用时,UV吸收剂可以基于组合物的总重量计至少0.01重量%或至少0.05重量%或至少0.1重量%、至多5重量%或至多3重量%或至多1重量%的量被包括。例如,组合物可包含基于组合物的总重量计0.01至5重量%、或0.05至3重量%、或0.1至1重量%的量的UV吸收剂。
抗氧化剂和/或稳定剂的总组合重量可为基于组合物的总重量计0.1重量%或0.2重量%至5重量%或至3重量%。例如,组合物可包含0.1至3重量%的组合量的抗氧化剂和稳定剂。例如,组合物可包含基于组合物的总重量计0.01至5重量%、或0.05至3重量%、或0.1至1重量%的量的热稳定剂。例如,组合物可包含基于组合物的总重量计0.01至5重量%、或0.05至3重量%、或0.1至1重量%的量的抗氧剂。
其他添加剂
所公开的组合物还可任选地包含一种或多种添加剂,条件是添加剂不会不利影响组合物的所需性质。还可使用添加剂的混合物。这类添加剂可在组分混合形成组合物期间以合适的时间混合。
要注意一般应避免某些填料、特别是无机填料,诸如滑石、二氧化硅、TiO2、粘土、云母、纳米填料、玻璃纤维、玻璃片、玻璃球,因为它们可能在无电镀期间干扰组合物的蚀刻相。例如,在蚀刻过程中这种无机粒状物类从组合物中流失可能导致在蚀刻浴中沉积,从而降低浴寿命。因此,组合物可不含这类填料,或这类填料被减到最少并且以基于组合物的总重量计少于1000ppm或少于500ppm或少于200或少于100ppm(即,百万分之重量份)的量存在。
组合物还可包含一种或多种脱模剂。合适的脱模剂的实例包括脂肪酸酯,具有长碳链的酰胺、诸如亚乙基双硬脂酰胺,或四硬脂酸季戊四醇酯,甘油单、二或三硬脂酸酯,或聚烯烃,诸如矿物油、聚乙烯、聚丙烯,或它们的组合。这些材料可以基于组合物的总重量计0或0.1重量%至5重量%或至1重量%或至0.5重量%的总组合量使用。例如,脱模剂可以基于组合物的总重量计0.1至1重量%的量存在。
组合物还可包含一种或多种润滑剂或塑化剂。在这些类型的材料之中存在明显的重叠,包括例如:邻苯二甲酸酯,诸如二辛基-4,5-环氧-六氢邻苯二甲酸酯;三(八氧羰基乙基)异氰脲酸酯;三硬脂精;二或多官能芳族磷酸酯,诸如间苯二酚四苯基二磷酸酯(RDP),氢醌的双(二苯基)磷酸酯和双酚A的双(二苯基)磷酸酯;聚α-烯烃;环氧化大豆油;有机硅,包括硅油(例如具有至少1000g/mol的分子量),诸如聚二甲基硅氧烷(PDMS);硬脂酸甲酯与包含聚乙二醇聚合物、聚丙二醇聚合物和其共聚物的亲水和疏水非离子表面活性剂的混合物,例如在合适的溶剂中的硬脂酸甲酯和聚乙二醇-聚丙二醇共聚物;蜡,诸如蜂蜡、蒙丹蜡、石蜡,或类似物。这些材料可以基于组合物的总重量计0或0.05重量%至5重量%或至1重量%或至0.1重量%的量使用。例如,如由硅油例示的润滑剂/塑化剂的量可为基于组合物的总重量计0至5重量%,或0.1至1重量%。可使用某些金属氧化物来帮助使脂肪酸或其盐和某些其他润滑剂或塑化剂的压汁(即,在模具上沉积)减到最少。这类金属氧化物的实例包括氧化镁(MgO)、氧化钙(CaO)和氧化锌(ZnO)。金属氧化物颗粒可具有0.5至5微米的平均粒度。大于10微米、在其他情况下大于25微米的较大粒度可能导致电镀部件中不期望的凹陷和其他瑕疵。金属氧化物可具有基于金属氧化物的总重量计低于1重量%的氯含量。金属氧化物可以基于组合物的总重量计0或0.1重量%至1重量%或至0.5重量%、例如0.1至1重量%的量使用。金属氧化物与脂肪酸的摩尔比可为至少1:2或至少4:5、至多5:1或至多2:1或至多1.5:1。例如,金属氧化物与脂肪酸的摩尔比的范围可为1:2至5:1。
还可存在某些着色剂,诸如颜料和/或染料添加剂。颜料的实例包括例如:炭黑,某些金属氧化物(前提是它们在形成制品或无电镀的过程中不析出或造成问题);硫化物,诸如硫化锌,或类似物;铝酸盐;磺基硅酸硫酸钠,铬酸钠,或类似物;铁酸锌;群青;颜料棕24;颜料红101;颜料黄119;有机颜料,诸如偶氮,二偶氮,喹吖啶酮,苝,萘四羧酸,黄蒽酮,异吲哚啉酮,四氯异吲哚酮,蒽醌,蒽嵌蒽醌,二噁嗪,酞菁,和偶氮色淀;颜料蓝60,颜料红122,颜料红149,颜料红177,颜料红179,颜料红202,颜料紫29,颜料蓝15,颜料绿7,颜料黄147和颜料黄150,或包含前述颜料中至少一种的组合。炭黑是一种优选的颜料。颜料的量不应太高以至于在模塑或蚀刻中造成问题。例如,颜料的量可为基于组合物的总重量计0、或0.01至2、或至1或至0.5或至0.1重量%。例如,炭黑可以基于组合物的总重量计0.01至2、或0.01至1、或0.01至1重量%的量使用。
本文所公开的组合物可含有基于组合物的总重量计少于20或少于10或少于5或少于3或少于1重量%的聚碳酸酯。组合物可无聚碳酸酯(即,不含聚碳酸酯)。
本文所公开的组合物可由根据ISO 1133:2011在10kg和220℃下至少5、或至少10或至少15g/10分钟的熔体流动速率来表征。本文所公开的组合物由根据ISO1133在10kg和220℃下至多40或至多35或至多30g/10分钟的熔体流动速率来表征。
本文所公开的组合物可由根据ISO 180:2011至少15或至少20或至少25kJ/m2的Izod冲击强度来表征。本文所公开的组合物可由根据ISO 180至多50或至多40kJ/m2的Izod冲击强度来表征。
本文所公开的组合物可由至少1500或至少2000或至少2200MPa的拉伸模量来表征。本文所公开的组合物可由至多4000或至多3500MPa的拉伸模量来表征。本文所公开的组合物可由至少35或至少40MPa的屈服拉伸强度来表征。本文所公开的组合物可由至多60或至多55MPa的拉伸强度来表征。本文所公开的组合物可由至少10或至少20%的断裂伸长率来表征。本文所公开的组合物可由至多200或至多150%的断裂伸长率来表征。拉伸模量、屈服拉伸强度和断裂伸长率可由ISO 527-2012以50mm/分钟测量。
组合物可由至少50或至少60或至少65微米/m-℃的热膨胀系数来表征。组合物可由根据ASTM E831-14(即,2014)的至多90微米/m-℃的热膨胀系数来表征。
组合物可由根据ISO 75-2004在1.8MPa力下至少75℃的热变形温度(HDT)来表征。
组合物可由根据ISO 306:2004在50℃/分钟下至少90℃的Vicat C软化点来表征。
组合物可由如通过ISO 178:2010测量的2000至4000MPa的挠曲模量来表征。
组合物的制造
组合物可通过本领域中通常可用的方法来制造。例如,在一个实施方案中,在一种进行方式中,可首先在Henschel高速混合器或其他合适的混合器/共混器中共混组分。包括但不限于手动混合的其他低剪切法也可实现这种共混。然后,可经由料斗将共混物进料至双螺杆挤出机的喉道中。替代地,组分中的一种或多种可通过经侧填充机在喉部和/或下游直接进料至挤出机中而掺合入组合物。这类添加剂还可与所需聚合树脂一起被配混成母料,并且进料至挤出机中。挤出机可在高于引起组合物流动所需温度的温度下运行。挤出物可被立即淬灭(例如在水浴中)并粒化。丸粒可用于后续模塑、成形或成型。
制品和其制造
组合物可通过诸如像以下的各种方式被成型为可用的成形制品:注塑,增材制造,挤出,旋转模塑,压塑,吹塑,片材或膜挤出,型材挤出,气辅模塑,结构泡沫模塑,和热成型。本文所述的具有改进电镀粘附的热塑性组合物还可被制成膜和片材以及层压体系的组件。可通过用诸如聚碳酸酯、聚苯乙烯共混物、聚(甲基)丙烯酸酯和类似物的其他热塑塑料共成型、包覆成型或层压,使组合物成型为制品。
由组合物形成的制品可相对较薄,具有例如1或2或5mm至20或至15mm的厚度。制品可具有至少10的纵横比(长度和/或宽度比厚度)。
成型的热塑性制品可通过诸如无电镀的已知方法镀金属。例如,待镀表面可被表面处理。表面处理步骤可包括蚀刻、中和、活化和加速中的一种或多种。蚀刻可利用诸如三氧化铬和硫酸混合物的强氧化溶液来进行,以形成实现良好粘附的表面结构,和/或将疏水表面转换为亲水表面。在此步骤中,二烯橡胶可在表面和表面附近被选择性去除(蚀刻)。选择性去除可在助粘剂可附接的表面上形成承窝。在蚀刻后,可用诸如亚硫酸氢钠的中和溶液冲洗表面。诸如在酸溶液中的贵金属(例如钯)的活化剂(或助粘剂)可产生催化表面以实现有效电镀。活化的表面可随后暴露于无电镀溶液(例如在浴中)以使金属在催化表面上析出。电镀液可包含金属盐、还原剂、络合剂、稳定剂和缓冲剂。可通过在第一沉积金属涂层上重复电镀类似或不同的金属来施加另外的金属层。可使用例如在化学浴中的冲洗步骤,使表面处理步骤之间的化学性减到最少或避免污染。
在蚀刻后,诸如钯的助粘剂可机械附接至表面,其随后导电并且可在后续电镀期间与诸如镍或铜的金属结合。
在无电涂布期间,可将镍和/或铜涂布于基材上。在后续电镀期间,可添加包含诸如镍、铜、铬、钴、锌或它们的合金的金属的另外的金属层。可存在各种层,例如镍层、铜层、铬层。根据一种优选的结构,从聚合物组合物开始按顺序存在以下层:镍,铜,镍,铬。
任一金属层的厚度可为至少0.5或至少1或至少2微米。任一层的厚度可为至多50或至多40或至多30或至多25微米。例如,单一金属层可具有0.5至50微米的厚度。在电解电镀后金属层的总厚度可为至少2、至少5或至少10微米。金属层的总厚度可为至多150或至多120或至多100微米。例如,金属层的总厚度可为2至150微米。根据一个实例,金属涂层包含2微米的镍/20微米的铜/10-20微米的镍/0.2-5(或0.2至1)微米的铬。
可在顶部金属层上施加聚合物密封层。这类聚合物密封层的实例包括丙烯酸类和/或环氧涂层,聚氨酯涂层以及含有二氧化硅的硬涂层。
本文所公开的电镀制品可具有根据ASTM B533-85的至少8(1401N/m)或至少9(1576N/m)或至少10磅力/英寸(lbf/in)(1751N/m)的剥离强度。本文所公开的电镀制品可具有至多20lbf/in(3502N/m)的剥离强度。
本文所公开的电镀制品可展示明显的热循环耐性,而无失效的视觉迹象。失效的视觉迹象可为缺陷诸如分层、气泡、混浊、开裂或类似物。热循环试验涉及以下步骤:
1)检查样品缺陷,
2)将无缺陷样品置于-40℉(-40℃)环境中一小时,
3)从冷环境中移除并检查缺陷,
4)在从冷环境中移除2分钟内,将样品置于200℉(93℃)的热环境中一小时,
5)从热环境中移除并检查缺陷,
6)在从热环境中移除2分钟内,将样品置于-40℉的冷环境中一小时,
7)重复步骤3-6直至检测到缺陷。
电镀制品可耐受至少7、至少8、至少9、或至少10个循环而无缺陷。
镀金属制品可具有如通过ASTM C1503-08测量的至少99%的反射率。
镀金属制品可适合用于汽车或运输应用,因为它们具有良好的砾石碎片耐性和良好的耐化学性(例如通过了道路盐试验暴露标准)。
包含本文所公开的组合物的电镀制品可用于运输(例如汽车)、电子或管道工程应用或装置中。例如,运输或汽车应用的制品可为或可用于选自以下的制品中:仪表盘,顶置控制台,内部装饰件,中央控制台,面板,后围侧板,门槛板,装饰件,挡泥板,车门,后备箱盖,后车厢盖,引擎盖,发动机罩,车顶,保险杠,仪表板,格栅,小外罩,柱缝饰,包层,车侧饰条,轮罩,毂盖,门把手,阻流板,窗框,头灯边框,头灯,尾灯,尾灯外罩,尾灯边框,车牌外壳,车顶支架,踏脚板,无线电扬声器格栅,仪表盘边框,转向柱,滴水槽,能量吸收器,脚踢板,反射镜外罩,格栅开口加强框,台阶,舱口盖,旋钮,按钮,和操纵杆。
作为另一个实例,制品可为或可为例如以下的组件:计算机和商用机外罩,家用电器,托盘,板材,把手,头盔,管道工程零件、诸如龙头,或淋浴头。在各种另外的实例中,成型的制品包括但不限于:电动工具,食品服务用品,医疗器械,动物笼子,电连接器,电气设备的外壳,电动马达部件,配电设备,通信设备,计算机和类似物,包括具有模制于搭扣配合连接器中的装置。本发明的制品可包括外车身板件,和用于户外或受保护图形、诸如标志的部件,户外外壳,诸如电信和电气接线箱,和建筑应用,诸如屋顶部分、墙板和窗玻璃。
实施例
以下材料用于实施例中:
●苯乙烯/丙烯腈(SAN):72重量%苯乙烯/28重量%丙烯腈,重均分子量Mw 150,000g/mol,数均分子量Mn 70,000g/mol。可从Galata Chemicals作为BlendexTM 576商购获得。
●丙烯腈/丁二烯/苯乙烯(ABS)接枝橡胶组合物:21份丙烯腈,31份丁二烯,46份苯乙烯,2份甲基丙烯酸甲酯。ABS橡胶包含不溶性接枝橡胶部分和未接枝刚性SAN部分,接枝SAN/橡胶=接枝橡胶组合物的52重量%。未接枝(刚性可提取)SAN占ABS接枝橡胶组合物的48重量%,并且具有重均分子量(Mw)=120,000g/mol且数均分子量(Mn)=35,000g/mol。Mw和Mn通过GPC使用聚苯乙烯标准品测定。橡胶粒度为300nm,具有宽粒度分布。ABS接枝橡胶包含ABS橡胶的6300ppm重量的牛脂酸(TFA)。TFA是包含肉豆蔻酸、亚油酸、棕榈酸、油酸、反油酸和硬脂酸的饱和和不饱和羧酸的混合物。
●甲基丙烯酸甲酯/丁二烯/苯乙烯(MBS)核壳橡胶:13份甲基丙烯酸甲酯/68份丁二烯/17份苯乙烯,175nm粒度。可从Dow Chemical Co作为Paraloid EXL2961A商购获得。
●亚乙基双硬脂酰胺:MW 539g/mol,熔点(MP)145℃。
●硬脂酸镁:Mw 697g/mol,MP 155℃。
●季戊四醇二亚磷酸酯:作为稳定剂,MW 605g/mol,MP 175℃。可从Addivant Co作为Ultranox 626商购获得。
●受阻酚抗氧化剂:购自Omnova的Wingstay L,MW 650g/mol,MP 118℃。
●二甲基硅氧烷聚合物:粘度1000厘泊(Momentive)。
●氧化镁(MgO):390ppm,粒度小于1微米,表面积160至200平方米/克,99%的颗粒能通过325筛目。
●炭黑:颜料级,0.035重量%。
将成分在油漆摇动器中以下表1中所示的重量份的量组合,并随后在180至250℃下在同向旋转双螺杆挤出机上以约400rpm、施加真空挤出成丸粒。在220℃下评估组合物的丸粒的熔体流动速率(MFR)。试验部件在丸粒上注塑,在95℃下干燥2小时,并且在220至250℃下以25秒周期模制。根据上文规定的试验方法且在表2和3中,测量了Izod冲击、拉伸模量和强度(屈服时)、热变形温度(HDT)、热膨胀系数(CTE)。在测试前将样品在50%相对湿度、23℃下调节至少2天。
大致上根据以下过程,利用浴曝气和各化学浴之间主要用水部分冲洗,使制品被无电镀:
●在Trimax LSAC 349中浸洗10分钟,
●在159℉且pH<10下,硫酸铬蚀刻10分钟,
●Adhemax中和剂CR使六价铬还原1分钟,
●预活化以维持HCl浓度1分钟,
●Adhemax活化剂SF在塑料表面上形成Pd核4分钟,
●Adhemax加速剂加速Pd吸附2分钟,
●Adhemax EN使无电镍沉积10分钟,
●浸铜以增加无电铜层2分钟,
●电解预镀铜以增加2-3微米铜层,
●用于另外的金属层的标准电镀过程。
然后如上文所描述将注塑的三维样品板敷金属并且根据上文阐述的热循环试验测试热冲击。如上文所描述将注塑的扁平样品板敷金属。对于用于热循环试验的样品,通过电镀(即,电解涂布)增加了以下金属层:25-40微米铜,半光亮镍(10-15微米),光亮镍(8-15微米),微孔镍(0.5-3.0微米),和铬(0.25微米)。对于粘附测试,电镀(即,电解涂布)的金属是40-80微米铜层。粘附是通过剥离强度试验方法ASTM B533-85测定的。如表2中所见,相比于在6个循环时失效的仅具有一种类型橡胶的比较样品A,包括MBS核壳橡胶的样品1和2在失效前经受住约2倍(11和12个循环)的热冲击循环。
表1
表2
本发明进一步涵盖以下方面。
方面1.一种用于无电镀的组合物,其包含:9至29重量%、优选9.7至29重量%、更优选10至29重量%的具有骨架的第一接枝橡胶共聚物,所述骨架包含至少一种聚合形式的共轭二烯单体,所述第一接枝橡胶共聚物具有接枝于骨架的聚合形式的至少一种选自单乙烯基芳族单体、丙烯酸类单体和它们的组合的单体,优选其中第一接枝橡胶共聚物包含丙烯腈/丁二烯/苯乙烯橡胶;70至90重量%、优选70-89.7重量%、更优选70至85重量%的未接枝苯乙烯类聚合物,优选未接枝苯乙烯类聚合物包含聚(苯乙烯丙烯腈);0.1至10重量%的具有100至500nm粒度的基于二烯的核/壳橡胶;0.1至5重量%的总量的稳定剂和/或抗氧化剂中的一种或多种;0.1至2重量%的量的脂肪酸或脂肪酸的盐,优选其中脂肪酸或脂肪酸的盐包含8至36个碳原子;0至5重量%的脱模剂,优选具有8至80个碳原子的羧酸酰胺或羧酸酯;0至1重量%的金属氧化物,优选氧化镁、氧化锌或氧化钙,更优选氧化镁;0至3重量%的润滑剂,优选硅油;0至20重量%的聚碳酸酯,优选0至10重量%的聚碳酸酯,更优选0至5重量%的聚碳酸酯,且仍更优选0至1重量%的聚碳酸酯,且最优选0重量%聚碳酸酯;其中重量%和ppm是基于组合物的总重量。
方面2.如方面1所述的组合物,其中第一接枝橡胶共聚物包含丙烯腈/丁二烯/苯乙烯橡胶,并且其中丙烯腈/丁二烯/苯乙烯橡胶包含55至75重量%的衍生自丁二烯单体的骨架和25至45重量%的接枝于骨架上的苯乙烯和丙烯腈的共聚物。
方面3.如方面2所述的组合物,其中苯乙烯与丙烯腈的重量比为65:35至80:20。
方面4.如前述方面中任一项所述的组合物,其中未接枝苯乙烯类聚合物包含聚(苯乙烯丙烯腈),其具有20-35重量%丙烯腈和65-80重量%苯乙烯,和由ASTM D5296通过凝胶渗透色谱法使用聚苯乙烯标准品测量的50,000至160,000g/mol的重均分子量。
方面5.如前述方面中任一项所述的组合物,其中基于二烯的核-壳橡胶具有包含第二聚合共轭二烯单体的核和包含至少一种丙烯酸酯单体和至少一种单乙烯基芳族单体的聚合产物的壳,优选其中共轭二烯单体的量为70至95重量%,丙烯酸酯单体的量为5至29重量%,且单乙烯基芳族单体的量为0.1至5重量%,其中重量%是基于基于二烯的核-壳橡胶的总重量。
方面6.如方面5所述的组合物,其中共轭二烯单体是丁二烯,丙烯酸酯单体是甲基丙烯酸甲酯,并且单乙烯基芳族单体是苯乙烯。
方面7.如前述方面中任一项所述的组合物,其中稳定剂和/或抗氧化剂中的一种或多种选自受阻酚、含磷稳定剂、含硫稳定剂或它们的组合中的一种或多种,优选组合物不含铅、汞、铊、镉、钡或锑盐。
方面8.如前述方面中任一项所述的组合物,其中组合物包含少于1000ppm的以下材料中的任何者:二氧化钛,粘土,滑石,云母,铅稳定剂,镉稳定剂,纳米填料,玻璃。
方面9.如前述方面中任一项所述的组合物,其特征在于以下中的一种或多种:根据ISO1133在10kg和220℃下10至40g/10分钟的熔体流动速率,根据ISO180的20至50KJ/平方米的Izod冲击,根据ISO 527的2000至4000MPa的拉伸模量,根据ISO527的10-200%的断裂伸长率,通过ASTM E831-14的70至90um/(m-℃)的热膨胀系数(CTE)。
方面10.如前述方面中任一项所述的组合物,其中未接枝苯乙烯类聚合物的量为基于组合物的总重量计70-90重量%,优选70-89.7重量%,更优选70至85重量%。
方面11.根据前述方面中任何项所述的组合物,其包含:10至59重量%的丙烯腈/丁二烯/苯乙烯接枝橡胶组合物,40至60重量%的聚(苯乙烯丙烯腈),0.1至10重量%的甲基丙烯酸甲酯/丁二烯/苯乙烯核-壳橡胶,0.1至5重量%的稳定剂和/或抗氧化剂中的一种或多种,1000至20,000ppm的包含8至36个碳原子的脂肪酸或脂肪酸的盐,0至5重量%的脱模剂,0至1重量%的氧化镁、氧化锌或氧化钙,0至3重量%的硅油,0至5重量%的聚碳酸酯,其中重量%和ppm是基于组合物的总重量。
方面12.根据前述方面中任何项所述的组合物,其中衍生自共轭二烯单体的橡胶的总量为基于组合物的总重量计10至20重量%。
方面13.一种制作如方面1-11中任一项所述的组合物的方法,其包括提供包含(a)具有骨架的第一接枝橡胶共聚物和(b)至少一种选自单乙烯基芳族单体、丙烯酸类单体和它们的组合的单体的未接枝聚合物的接枝橡胶组合物,所述骨架包含至少一种聚合形式的共轭二烯单体,所述第一接枝橡胶共聚物具有接枝于骨架的聚合形式的至少一种选自单乙烯基芳族单体、丙烯酸类单体和它们的组合的单体;将第一接枝橡胶组合物与以下者共混:未接枝苯乙烯类聚合物,优选包含聚(苯乙烯丙烯腈)的未接枝苯乙烯类聚合物,0.1至10重量%的具有100至500nm粒度的基于二烯的核/壳橡胶,0.1至5重量%的总量的稳定剂和/或抗氧化剂中的一种或多种,0.1至2重量%的量的脂肪酸或脂肪酸的盐,优选其中脂肪酸或脂肪酸的盐包含8至36个碳原子,0至5重量%的脱模剂,优选具有8至80个碳原子的羧酸酰胺或羧酸酯,0至1重量%的金属氧化物,优选氧化镁、氧化锌或氧化钙,更优选氧化镁,0至3重量%的润滑剂,优选硅油,0至20重量%的聚碳酸酯,优选0至10重量%的聚碳酸酯,更优选0至5重量%的聚碳酸酯,且仍更优选0至1重量%的聚碳酸酯;其中重量%和ppm是基于组合物的总重量,其中未接枝苯乙烯类聚合物的量经选择使得接枝橡胶组合物中的未接枝聚合物的量加未接枝苯乙烯类聚合物的量占70至90重量%,其中所有重量%是基于组合物的总重量。
方面14.一种包含如方面1-11中任一项所述的组合物的制品,其被成型为具有表面的形状,其中将金属涂层无电镀于表面的至少一部分上。
方面15.如方面14所述的制品,其还具有至少一个在无电镀金属涂层之上电镀的金属涂层。
方面16.如方面15所述的制品,其中无电镀金属涂层是镍或铜,并且至少一个电镀金属涂层包含镍、铜、铬、钴、锌或它们的合金中的一种或多种。
方面17.如方面14或16所述的制品,其中金属涂层从组合物的表面开始按顺序包含镍层和铬层。
方面18.如方面14-17中任一项所述的制品,其中制品从聚合物组合物开始按顺序包含以下层:镍,铜,镍,铬。
方面19.如方面14-18中任一项所述的制品,其特征在于以下中的一种或多种:通过ASTM B533的8至20磅力/英寸(1401至3502N/m)的金属层剥离强度,制品经受住被置于-40℃环境中一小时并随后置于93℃环境中一小时、环境之间不超过2分钟的多于6个循环,而金属涂层没有可见的分层、气泡、开裂或缺陷。
方面20.如方面14-19中任一项所述的制品,其为汽车组件。
方面21.一种制作如方面14-20中任一项所述的制品的方法,其包括使组合物成型为形状,并且将一种或多种金属无电镀于成型并蚀刻的组合物的一部分上。
方面22.如方面21所述的方法,其进一步包括在无电镀金属之上电镀至少一个金属层。
方面23.如方面21或22所述的方法,其中组合物成型为所需形状包括注塑。
组合物、方法和制品可替代地包括、包含、由或基本上由本文中公开的任何适当材料、步骤或组分组成。另外或替代地,组合物、方法和制品可被配制为缺乏或大致上不含对实现组合物、方法和制品的功能或目的非必需的任何材料(或物类)、步骤或组分。
本文所公开的所有范围均包括端点,并且端点可独立地相互组合(例如“至多25重量%,或更明确而言5重量%至20重量%”的范围包括“5重量%至25重量%”的范围的端点和所有中间值,等)。此外,规定的上限和下限可被组合形成范围(例如“至少1或至少2重量%”和“至多10或5重量%”可被组合为“1至10重量%”或“1至5重量%”或“2至10重量%”或“2至5重量%”的范围)。“组合”包括了共混物、混合物、掺杂物、反应产物和类似物。术语“第一”、“第二”和类似物不表示任何次序、数量或重要性,而是用来将一个要素与另一个进行区分。除非本文中另外指出或明显与上下文矛盾,本文中术语“一种”、“一个”和“所述”不指示对数量的限制,并且被解释为涵盖单数和复数。除非另外清楚地规定,“或”意指“和/或”。在说明书各处提及“一些实施方案”、“一个实施方案”等等意指结合实施方案描述的具体要素被包括在本文所述的至少一个实施方案中,并且可存在或可不存在于其他实施方案中。另外,要理解所述要素可在各种实施方案中以任何合适的方式进行组合。“它们的组合”是开放的并且包括了包含所列举组分或性质、任选地连同未列举的类似或等效的组分或性质中的至少一种的任何组合。
除非本文中相反地规定,否则所有试验标准是截至本申请的申请日、或者出现试验标准的最早优先申请的申请日(在要求了优先权的情况下)生效的最新标准。
除非另外定义,否则本文中使用的技术和科学术语具有与本申请所属领域技术人员所通常理解的相同的含义。所有引用的专利、专利申请和其他参考文献都以引用的方式整体并入本文。然而,在本申请中的术语与所并入引用中的术语发生矛盾或冲突的情况下,本申请的术语优先于所并入引用的冲突术语。
使用标准命名法描述化合物。例如,未被任何指示基团取代的任何位置被理解为具有由如所指键或氢原子填充的其价数。未介于两个字母或符号之间的长划(“-”)用来指示取代基的连接点。例如,-CHO经由羰基的碳连接。
术语“烷基”意指支链或直链的不饱和的脂族烃基,例如甲基、乙基、正丙基、异丙基、正丁基、仲丁基、叔丁基、正戊基、仲戊基,以及正己基和仲己基。“烯基”意指直链或支链的具有至少一个碳碳双键的单价烃基(例如乙烯基(-HC=CH2))。“烷氧基”意指经由氧连接的烷基(即烷基-O-),例如甲氧基、乙氧基和仲丁氧基。“芳基”意指含有规定碳原子数的芳族烃基,诸如苯基、卓酮、茚满基或萘基。前缀“卤”意指基团或化合物包括氟、氯、溴或碘取代基中的一种或多种。可存在不同卤基(例如溴和氟)的组合,或仅氯基。前缀“杂”意指化合物或基团包括为杂原子的至少一个环成员(例如1、2或3个杂原子),其中一种或多种杂原子各自独立地为N、O、S、Si或P。“取代的”意指化合物或基团被至少一个(例如1、2、3或4个)取代基取代,取代基可各自独立地为替代氢的C1-9烷氧基,C1-9卤烷氧基,硝基(-NO2),氰基(-CN),C1-6烷基磺酰基(-S(=O)2-烷基),C6-12芳基磺酰基(-S(=O)2-芳基),巯基(-SH),氰硫基(-SCN),甲苯磺酰基(CH3C6H4SO2-),C3-12环烷基,C2-12烯基,C5-12环烯基,C6-12芳基,C7-13芳基亚烷基,C4-12杂环烷基,和C3-12杂芳基,前提是未超过取代的原子的正常价。基团中所指碳原子数不包括任何取代基。例如,-CH2CH2CN是被腈取代的C2烷基。
尽管已描述了具体的实施方案,但可由申请人或本领域其他技术人员提出当前未预见或可能未预见的替代方案、修改、变型、改进和实质等效物。因此,所提交和可能被修正的随附权利要求书意图包括所有这类替代方案、修改、变型、改进和实质等效物。
Claims (15)
1.用于无电镀的组合物,其包含:
9至29重量%、优选9.7至29重量%、更优选10至29重量%的具有骨架的第一接枝橡胶共聚物,所述骨架包含至少一种聚合形式的共轭二烯单体,所述第一接枝橡胶共聚物具有接枝于所述骨架的聚合形式的至少一种选自单乙烯基芳族单体、丙烯酸类单体和它们的组合的单体,优选其中所述第一接枝橡胶共聚物包含丙烯腈/丁二烯/苯乙烯橡胶,
70-90重量%、优选70-89.7重量%、更优选70至85重量%的未接枝苯乙烯类聚合物,优选所述未接枝苯乙烯类聚合物包含聚(苯乙烯丙烯腈),
0.1至10重量%的具有100至500nm的粒度的基于二烯的核/壳橡胶,
0.1至5重量%的总量的稳定剂和/或抗氧化剂中的一种或多种,
0.1至2重量%的量的脂肪酸或脂肪酸的盐,优选其中所述脂肪酸或脂肪酸的盐包含8至36个碳原子,
0至5重量%的脱模剂,优选具有8至80个碳原子的羧酸酰胺或羧酸酯,
0至1重量%的金属氧化物,优选氧化镁、氧化锌或氧化钙,更优选氧化镁,
0至3重量%的润滑剂,优选硅油,
0至20重量%的聚碳酸酯,优选0至10重量%的所述聚碳酸酯,更优选0至5重量%的所述聚碳酸酯,仍更优选0至1重量%的所述聚碳酸酯,且最优选0重量%聚碳酸酯,
其中重量%和ppm是基于所述组合物的总重量。
2.根据权利要求1所述的组合物,其中所述第一接枝橡胶共聚物包含丙烯腈/丁二烯/苯乙烯橡胶,并且其中所述丙烯腈/丁二烯/苯乙烯橡胶包含55至75重量%的衍生自丁二烯单体的骨架和25至45重量%的接枝于所述骨架上的苯乙烯和丙烯腈的共聚物。
3.根据权利要求1或2所述的组合物,其中所述未接枝苯乙烯类聚合物包含聚(苯乙烯丙烯腈),其具有20-35重量%丙烯腈衍生的内含物和65-80%苯乙烯衍生的内含物,和由ASTM D5296通过凝胶渗透色谱法使用聚苯乙烯标准品测量的50,000至160,000g/mol的重均分子量。
4.根据前述权利要求中任一项所述的组合物,其中所述基于二烯的核-壳橡胶具有包含第二聚合共轭二烯单体的核和包含至少一种丙烯酸酯单体和至少一种单乙烯基芳族单体的聚合产物的壳,优选其中所述共轭二烯单体的量为70至95重量%,所述丙烯酸酯单体的量为5至29重量%,且所述单乙烯基芳族单体的量为0.1至5重量%,其中重量%是基于所述基于二烯的核-壳橡胶的总重量。
5.根据权利要求4所述的组合物,其中所述第二共轭二烯单体是丁二烯,所述丙烯酸酯单体是甲基丙烯酸甲酯,并且所述单乙烯基芳族单体是苯乙烯。
6.根据前述权利要求中任一项所述的组合物,其中稳定剂和/或抗氧化剂中的一种或多种选自受阻酚、含磷稳定剂、含硫稳定剂或它们的组合中的一种或多种。
7.根据前述权利要求中任一项所述的组合物,其特征在于具有少于1000ppm的以下材料中的任何者:二氧化钛,粘土,滑石,云母,铅稳定剂,镉稳定剂,纳米填料,玻璃。
8.根据前述权利要求中任一项所述的组合物,其特征在于以下中的一种或多种:
根据ISO 1133在10kg和220℃下10至40g/10分钟的熔体流动速率,
根据ISO 180的20至50KJ/平方米的Izod冲击,
根据ISO 527的2000至4000MPa的拉伸模量,
根据ISO 527的10-200%的断裂伸长率,
通过ASTM E831-14的70至90um/(m-℃)的热膨胀系数(CTE)。
9.根据前述权利要求中任何项所述的组合物,其包含:9至29重量%、优选9.7至29重量%、优选10至29重量%的丙烯腈/丁二烯/苯乙烯接枝橡胶组合物,
70至90重量%、优选70至89.7重量%、更优选70至85重量%的聚(苯乙烯丙烯腈),
0.1至10重量%的甲基丙烯酸甲酯/丁二烯/苯乙烯核-壳橡胶,
0.1至5重量%的稳定剂和/或抗氧化剂中的一种或多种,
1000至20,000ppm的包含8至36个碳原子的脂肪酸或脂肪酸的盐,
0至5重量%的脱模剂和/或润滑剂,
0至1重量%的氧化镁、氧化锌或氧化钙,
0至3重量%的硅油,
0至5重量%的所述聚碳酸酯,
其中重量%和ppm是基于所述组合物的总重量。
10.包含根据权利要求1-9中任一项所述的组合物的制品,其被成型为具有表面的形状,其中将金属涂层无电镀于所述表面的一部分上。
11.根据权利要求10所述的制品,其特征在于以下中的一种或多种:
通过ASTM B533-85的1401至3502N/m的金属层剥离强度,
所述制品经受住被置于-40℃环境中一小时并随后被置于93℃环境中一小时、所述环境之间不超过2分钟的多于6个循环,而所述金属涂层没有可见的分层、气泡、开裂或缺陷。
12.根据权利要求10或11所述的制品,其中所述金属涂层从所述组合物的表面开始按顺序包含镍层和铬层。
13.根据权利要求10-12中任一项所述的制品,其为汽车组件。
14.制作根据权利要求10-12中任一项所述的制品的方法,所述方法包括使所述组合物成型为形状,用氧化性酸蚀刻所述形状,并且将一种或多种金属无电镀于成型并蚀刻的组合物的一部分上。
15.根据权利要求14所述的方法,其中所述组合物成型为所需形状包括注塑。
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