CN102459355A - 可热活化的自由基引发剂和包含磁性颗粒的复合材料 - Google Patents
可热活化的自由基引发剂和包含磁性颗粒的复合材料 Download PDFInfo
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- CN102459355A CN102459355A CN2010800284253A CN201080028425A CN102459355A CN 102459355 A CN102459355 A CN 102459355A CN 2010800284253 A CN2010800284253 A CN 2010800284253A CN 201080028425 A CN201080028425 A CN 201080028425A CN 102459355 A CN102459355 A CN 102459355A
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Abstract
本发明提供一种复合材料，其包含：选自有机过氧化物和/或含有不稳定的碳-碳键的引发剂的一种或多种可热活化的自由基引发剂，和具有核-壳结构的颗粒，并且所述核包含一种或多种磁性材料，同时所述壳包含二氧化硅。
Description
技术领域
本发明涉及复合材料，其包含可热活化的自由基引发剂和磁性颗粒。本发明还涉及制备此材料的方法，及其用途。
背景技术
可热活化的自由基引发剂用于聚合物的交联或固化是熟知的常规实践。有机过氧化物在此最重要。交联过程与热有关，其缺点是待交联的整个组合物必须被加热，导致能量输入不经济。此外，待交联的整个组合物经受热应力，这会不利地影响其性质。最后，还应提及过氧化物的敏感性质，这意味着在贮藏和交联过程中必须采取特别的预防措施。
因此，本发明的目的之一是提供能够更有效且破坏性较低地将热能导入待交联的组合物中的材料。另一个目的是提供制备该材料的方法。
发明内容
本发明提供复合材料，其包含
-选自有机过氧化物和/或含有不稳定的碳-碳键的引发剂(C-C引发剂)的一种或多种可热活化的自由基引发剂，和
-具有核-壳结构的颗粒，并且所述核包含一种或多种磁性材料，同时所述壳包含二氧化硅。
对于本发明，复合材料是所述组分的物理混合物。本发明所述的复合材料可采用粉末或糊状物、或者液体悬浮体或液体分散体的形式，或者可以是具有低至高粘度的可模塑的组合物。
本发明所述的复合材料的一个特征是已确保可热活化的引发剂的高稳定性。在长达1个月，优选长达6个月，特别优选长达12个月，非常特别优选2年或更久的时间内，所述可热活化的引发剂的浓度降低通常小于引发剂的用量的2％。这更加出人意料，因为所述颗粒包含磁性材料，而磁性材料的已知性质是例如它们一般使过氧化物瞬时分解或者在长时间内逐渐分解；所以，本领域技术人员不会考虑到可制备或贮藏包含磁性组分和过氧化物的复合材料。
对于本发明，可热活化是指通过热量形成自由基。聚合物交联时的温度通常为约50℃-250℃，随自由基引发剂和待交联的聚合物而改变。
对于本发明，具有核-壳结构的颗粒是如下所述的颗粒：
-被壳包围的孤立的个体颗粒，
-附着的核的聚集体，其中所述聚集体被壳包围和/或
-通过所述壳附着的聚集体。
聚集体是通过例如烧结颈而紧密附着的个体颗粒。
本发明所述的复合材料中所含的具有核-壳结构的颗粒的壳可以是包围所述核的一层或多层壳，其中这些壳中至少之一包含二氧化硅，或者基本上由其组成。若所述具有核-壳结构的颗粒具有多层壳，优选的是，外层是完全包围所述核的由二氧化硅组成的无孔壳。
相对接近于所述核的壳不必完全无孔。这些壳可包含例如，由所述壳材料中所含的元素和所述核材料中所含的元素组成的化合物。例如，若所述核包含铁或铁化合物，则壳材料可以是硅酸铁。
短语“基本上由其组成”是指在此类情况中所述壳还可包含典型的杂质。杂志的量，在每种情况中基于所述壳，通常小于1重量％，优选小于0.1重量％，特别优选小于0.01重量％。所述壳的二氧化硅主要或完全是非结晶的二氧化硅。
所述壳的厚度优选在纳米范围内。特别优选的厚度可以是2-500nm，非常特别优选的厚度可以是5-30nm。
所述壳优选为基本上无孔并且在表面上具有游离的羟基基团。
本发明所述的磁性材料是顺磁性、铁磁性、亚铁磁性或超顺磁性的材料，或者这些的混合物。可优选超顺磁性材料和仅具有少量剩余磁化强度的材料。
可优选具有核-壳结构并且表现出超顺磁性(Neel驰豫)和磁滞的颗粒。这些性质取决于例如化学组成、颗粒粒度分布、颗粒的形状及其可磁化性。
适合的核材料可以是，例如，纯金属例如Fe、Co和Ni，氧化物例如Fe3O4和γ-Fe2O3、尖晶石型铁磁性材料例如MgFe2O4、MnFe2O4和CoFe2O4，以及合金例如CoPt3和FePt。
在本发明的一个具体实施方案中，所述核材料包含或由选自赤铁矿、磁铁矿和磁赤铁矿的一种或多种铁氧化物组成，或者包含或由两种或三种这些铁氧化物的混合物组成。在本发明中感应加热复合材料的特别有利的性质是通过使用包含赤铁矿、磁铁矿和磁赤铁矿的核材料获得的，其中X-射线衍射图测得，在每种情况下基于所述核，赤铁矿的比例为1重量％-10重量％，磁铁矿的比例为20重量％-50重量％，磁赤铁矿的比例为40重量％-75重量％，并且这些比例总计为100重量％。在本发明的一个优选实施方案中，赤铁矿的比例为4重量％-8重量％，磁铁矿的比例为35重量％-40重量％，磁赤铁矿的比例为50重量％-60重量％。
核材料的比例和壳材料的比例可在宽范围内随着核材料、所述壳的厚度、孤立的或聚集的颗粒的结构而改变。所述核材料和所述壳材料的比例一般在每种情况中为10重量％-90重量％。可优选具有50重量％-90重量％的核材料比例和10重量％-50重量％的壳材料比例的核-壳颗粒。
所述核-壳颗粒的BET表面积可以为5-500m2/g，优选30-300m2/g，非常特别优选40-150m2/g。所述颗粒的平均直径优选5-100nm，特别优选30-80nm。本发明所述的颗粒的比例分布的90％的分散范围优选为5-60nm。
在本发明的一个具体实施方案中，所述具有核-壳结构的颗粒可以以表面改性的形式存在。对于本发明，表面改性是指位于所述粉末表面上的至少部分的羟基基团已与表面改性剂反应形成化学键。该化学键优选为共价键、离子键，或者在表面活性剂和所述颗粒之间形成络合物的配位键。配位键是指形成络合物。
所述表面改性剂可优选地为含有作为官能团的羧酸基团、酰氯基团、酯基团、腈基团、异腈基团、羟基基团、硫醇基团、环氧基团、酸酐基团、酰胺基团、氨基基团或硅醇基团的表面改性剂。
特别优选的表面改性剂是含有至少一个不可水解的基团或一个羟基基团的硅烷，特别是含有至少一个不可水解的基团的可水解的有机硅烷。
实例是通式为RaSiX4-a的硅烷，其中基团R相同或不同，并且是不可水解的基团，基团X相同或不同，并且是可水解的基团或羟基基团，且a为值1、2或3。a值优选为1。通式中的可水解基团X的实例是，其中这些X可以彼此相同或不同，
-氢或卤素，F、Cl、Br或I；
-烷氧基，特别是C1-C6-烷氧基，例如甲氧基、乙氧基、正丙氧基、异丙氧基和丁氧基；
-芳氧基，特别是C6-C10-芳氧基，例如苯氧基；
-酰氧基，特别是C1-C6-酰氧基，例如乙酰氧基或丙酰氧基；
-烷基羰基，特别是C2-C7-烷基羰基，例如乙酰基；
-氨基，特别是单烷基胺基或双烷基胺基，优选在每种情况中具有1-6个碳原子。
优选的可水解基团是卤素、烷氧基基团和酰氧基基团。特别优选的可水解基团是C1-C4-烷氧基基团，特别是甲氧基和乙氧基。
可彼此相同或不同的不可水解的基团R可以是含有或不含有官能团的不可水解的基团R。例如，不含有官能团的不可水解的基团R可以是
-烷基，特别是C1-C8-烷基，例如甲基、乙基、正丙基、异丙基、正丁基、仲丁基和叔丁基、戊基、己基、辛基或环己基；
-烯基，特别是C2-C6-烯基，例如乙烯基、1-丙烯基、2-丙烯基和丁烯基；
-炔基，特别是C2-C6-炔基，例如乙炔基和炔丙基；
-芳基，特别是C6-C10-芳基，例如苯基和萘基，以及相应的烷芳基基团，例如甲苯基、苄基和苯乙基。
可明确提及以下表面改性剂：CH3SiCl3、CH3Si(OC2H5)3、CH3Si(OCH3)3、C2H5SiCl3、C2H5Si(OC2H5)3、C2H5Si(OCH3)3、C3H7Si(OC2H5)3、(C2H5O)3SiC3H6Cl、(CH3)2SiCl2、(CH3)2Si(OC2H5)2、(CH3)2Si(OH)2、C6H5Si(OCH3)3、C6H5Si(OC2H5)3、C6H5CH2CH2Si(OCH3)3、(C6H5)2SiCl2、(C6H5)2Si(OC2H5)2、(iso-C3H7)3SiOH、CH2＝CHSi(OOCCH3)3、CH2＝CHSiCl3、CH2＝CH-Si(OC2H5)3、CH2＝CHSi(OC2H5)3、CH2＝CH-Si(OC2H4OCH3)3、CH2＝CH-CH2-Si(OC2H5)3、CH2＝CH-CH2-Si(OC2H5)3、CH2＝CH-CH2Si(OOOCH3)3、n-C6H13-CH2-CH2-Si(OC2H5)3、n-C8H17-CH2CH2-Si(OC2H5)3、(γ-缩水甘油基氧基丙基)三甲氧基甲硅烷、(γ-缩水甘油基氧基丙基)三乙氧基甲硅烷、(3-异氰酸基丙基)三乙氧基甲硅烷、(3-异氰酸基丙基)二甲基氯代甲硅烷、(3-氨基丙基)三甲氧基甲硅烷、(3-氨基丙基)三乙氧基甲硅烷、(N-(2-氨基乙基)-3-氨基丙基)三甲氧基甲硅烷、(N-[N’-(2’-氨基乙基)-2-氨基乙基]-3-氨基丙基)三甲氧基甲硅烷、羟甲基三乙氧基甲硅烷、(2-[甲氧基(聚亚乙基氧基)丙基])三甲氧基甲硅烷、(双(羟乙基)-3-氨基丙基)三乙氧基甲硅烷、(N-羟乙基-N-甲基氨基丙基)三乙氧基甲硅烷、(3-(甲基)丙烯酰氧基丙基)三乙氧基甲硅烷和(3-(甲基)丙烯酰氧基丙基)三甲氧基甲硅烷。
可优选用作表面改性剂的化合物是：辛基三甲氧基甲硅烷、辛基三乙氧基甲硅烷、六甲基二硅氮烷、(3-甲基丙烯酰氧基丙基)三甲氧基甲硅烷、(3-甲基丙烯酰氧基丙基)三乙氧基甲硅烷、二甲基聚硅氧烷、(缩水甘油基氧基丙基)三甲氧基甲硅烷、(缩水甘油基氧基丙基)三乙氧基甲硅烷、(九氟己基)三甲氧基甲硅烷、(十三氟辛基)三甲氧基甲硅烷、(十三氟辛基)三乙氧基甲硅烷和(氨基丙基)三乙氧基甲硅烷。特别优选辛基三甲氧基甲硅烷、辛基三乙氧基甲硅烷和二甲基聚硅氧烷。
在另一个具体的实施方案中，所述具有核-壳结构的颗粒是铁硅氧化物颗粒，其中
-所述颗粒的BET表面积为10-80m2/g，优选30-70m2/g，特别优选40-60m2/g；
-在每种情况中相对于包括它们的壳在内的颗粒，所述颗粒中铁氧化物的含量为60重量％-90重量％，优选75重量％-85重量％，二氧化硅的含量为10重量％-40重量％，优选15重量％-25重量％，其中相对于包括它们的壳在内的颗粒，铁、硅和氧的比例为至少99重量％，
-所述核是结晶体，并且所述铁氧化物包含赤铁矿、磁铁矿和磁赤铁矿；
-所述壳由非结晶的二氧化硅组成；
-在壳与核之间，至少部分地，存在一种或多种由元素硅、铁和氧组成的化合物，一般为硅酸铁；
-所述壳的厚度为5-20nm；
-所述颗粒的平均直径为5-100nm，优选30-80nm。
除了具有核-壳结构的颗粒之外，本发明所述的复合材料的第二基本组分是一种或多种有机过氧化物、C-C引发剂、或有机过氧化物的混合物和C-C引发剂的混合物。优选仅包含有机过氧化物的复合材料。
所述有机过氧化物优选地选自氢过氧化物、二烷基过氧化物、二芳基过氧化物、过氧羧酸、过氧羧酸酯、二酰基过氧化物、过氧碳酸酯、过氧化二碳酸酯、酮过氧化物、过氧化缩酮(perketal)和/或这些的混合物。具体可提及以下物质：
-氢过氧化物(R1-O-O-H)，例如叔丁基过氧化氢、异丙苯基过氧化氢、2，5-二甲基-2，5-二氢过氧己烷；
-二烷基(和/或二芳基)过氧化物(R1-O-O-R2)，例如二叔丁基过氧化物、2，5-二甲基己炔(3)-2，5-二叔丁基过氧化物、二(2-叔丁基过氧基异丙基)苯、叔丁基异丙苯基过氧化物、二异丙苯基过氧化物；
-过氧羧酸(R1-C(O)-O-OH)，例如过氧乙酸、过氧甲酸；
-过氧羧酸酯(R1-C(O)-O-O-R2)，例如叔丁基过氧新戊酸酯、叔丁基2-乙基过氧己酸酯、单叔丁基过氧马来酸酯、双(2-新癸酰基过氧基异丙基)苯；
-二酰基过氧化物(R1-C(O)-O-O-C-(O)-R2)，例如二苯甲酰基过氧化物、二(3，5，5-三甲基己酰基)过氧化物、2，4-二氯苯甲酰基过氧化物；
-过氧碳酸酯(R1-O-C(O)-O-O-R2)，例如叔丁基过氧基异丙基碳酸酯、叔丁基过氧基2-乙基己基碳酸酯；
-过氧二碳酸酯(R1-O-C(O)-O-O-C(O)-O-R2)，例如二(4-叔丁基环己基)过氧二碳酸酯、二(2-乙基己基)过氧二碳酸酯、二鲸蜡基过氧二碳酸酯；
-酮过氧化物，例如环己酮过氧化物、甲基异丁基酮过氧化物、甲乙酮过氧化物、3，3，5，7，7-五甲基-1，2，4-三氧杂环庚烷、3，6，9-三乙基-3，6，9-三甲基-1，2，4，5，7，8-六氧杂环壬烷；
-过氧化缩酮：2，2-双(叔丁基过氧基)丁烷、1，1-二叔丁基过氧基-3，3，5-三甲基环己烷、1，1-双(叔丁基过氧基)环己烷、3，3，6，6，9，9-六甲基-1，2，4，5-四氧杂环壬烷、3，3-二(叔丁基过氧基)丁酸乙酯；
-其它过氧化合物，例如3-叔丁基过氧基-3-苯基苯酞、叔丁基过氧基戊内酯。
就工业可得性而言，可特别提及：1，1，3，3-四甲基丁基过氧新癸酸酯、1，1-二(叔丁基过氧基)-3，3，5-三甲基环己烷、1，1-二(叔丁基过氧基)环己烷、2，2-二(叔丁基过氧基)丁烷、2，5-二甲基-2，5-二(叔丁基过氧基)己烷、2，5-二甲基-2，5-二(叔丁基过氧基)己-3-炔、乙酰丙酮过氧化物、异丙苯基过氧新癸酸酯、环己酮过氧化物、二(2，4-二氯苯甲酰基)过氧化物、二(2-乙基己基)过氧二碳酸酯、二(3，5，5-三甲基己酰基)过氧化物、二(4-甲基苯甲酰基)过氧化物、二(4-叔丁基环己基)过氧二碳酸酯、二(叔戊基)过氧化物、二(叔丁基)过氧化物、二苯甲酰基过氧化物、二鲸蜡基过氧二碳酸酯、二(异丙苯基)过氧化物、二月桂酰基过氧化物、二肉豆蔻基过氧二碳酸酯、二琥珀酰基过氧化物、甲乙酮过氧化物、甲基异丁基酮过氧化物、叔戊基2-乙基过氧己酸酯、叔戊基过氧基2-乙基己基碳酸酯、叔戊基过氧苯甲酸酯、叔戊基过氧新癸酸酯、叔戊基过氧新戊酸酯、叔丁基异丙苯基过氧化物、叔丁基过氧化氢、叔丁基2-乙基过氧己酸酯、叔丁基过氧基(2-乙基己基)碳酸酯、叔丁基3，5，5-三甲基过氧己酸酯、叔丁基过氧乙酸酯、叔丁基过氧苯甲酸酯、叔丁基过氧异丁酸酯、叔丁基过氧新癸酸酯、叔丁基过氧新庚酸酯和叔丁基过氧新戊酸酯。
所述有机过氧化物可以以不被稀释的固体形式或液体形式存在。它还可以以溶液形式、乳胶形式、悬浮液形式或糊状物形式与溶剂一起存在。在本发明的一个特别优选的实施方案中，所述有机过氧化物是液体过氧化物。
代替所述有机过氧化物或与其一起，本发明所述的复合材料可包含含有不稳定的碳-碳键(C-C引发剂)的引发剂，所述引发剂选自具有通式Ph-R4R3C-CR5R6-Ph的化合物，其中Ph是苯基基团或取代的苯基基团，并且R3、R4、R5和R6各彼此独立地为氢或烷基基团。典型的实例是3，4-二甲基-3，4-二苯基己烷、2，3-二甲基-2，3-二苯基丁烷、3，4-二甲基-3，4-二苯基己烷、2，3-二甲基-2，3-二苯基丁烷。可用作C-C引发剂的其它化合物是低聚1，1，2，2-四苯基-1，2-乙二醇甲硅烷基醚、单体或低聚的1，1，2，2-四苯基-1，2-乙二醇二甲硅烷基醚、1，1，2，2-四苯基-1，2-乙二醇二甲基醚、四苯基乙烷和四苯基乙烷二腈。
本发明所述的复合材料中所含的两种基本组分(具有核-壳结构的颗粒和可热活化的自由基引发剂)的比例，在各种情况中相对于所述复合材料，优选地，具有核-壳结构的颗粒的含量为0.1重量％-50重量％，所述可热活化的自由基引发剂的含量为0.1重量％-90重量％。本发明所述的复合材料可仅由这两种组分组成。
本发明所述的复合材料还可包含一种或多种待交联的聚合物或待固化的聚合物。例如，可提及聚烯烃，例如聚乙烯，特别是LLDPE、LDPE、HDPE、聚丙烯、聚丁烯，以及其共聚物；乙烯-乙酸乙烯基酯共聚物；橡胶，例如乙烯-丙烯-二烯橡胶、乙烯-丙烯橡胶、苯乙烯-丁二烯聚合物、丁腈橡胶、聚丁二烯、硅橡胶；热塑性弹性体，例如TPE-A、TPE-E、TPE-O、TPE-S、TPE-U、TPE-V；聚酯树脂，例如基于邻苯二甲酸和新戊二醇的聚酯树脂；二环戊二烯树脂、环氧树脂、乙烯基酯树脂、聚丙烯酸酯和聚甲基丙烯酸酯。
本发明所述的复合材料中聚合物的比例可优选地占所述复合材料的1重量％-99.8重量％。
具体地，有用的复合材料是可用作母料的那些，其中在各情况中相对于所述复合材料，核-壳颗粒的比例为1重量％-80重量％，可热活化的自由基引发剂的比例为1重量％-80重量％，聚合物的比例为1重量％-98重量％。特别优选的一个实施方案中，在各情况中相对于所述复合材料，其包含20重量％-80重量％的所述核-壳颗粒，20重量％-80重量％的可热活化的自由基引发剂和20重量％-80重量％的聚合物。
本发明所述的复合材料还可包含一种或多种增加交联度或固化度的物质。这些可以是，例如，多官能度的丙烯酸酯和甲基丙烯酸酯、N，N-间亚苯基二马来酰亚胺、2，4，6-三烯丙基氧基-1，3，5-三嗪和/或1，3，5-三烯丙基异氰尿酸酯。
本发明所述的复合材料还可包含一种或多种溶剂。这些可以是，例如，水、醇、二醇、硅油、C5-C10烷烃，和/或可以是芳香族化合物。
在本发明的一个具体实施方案中，所述复合材料由以下组成：
a)1重量％-90重量％，优选20重量％-80重量％的选自有机过氧化物和/或具有不稳定的碳-碳键的引发剂的一种或多种可热活化的自由基引发剂，
b)1重量％-90重量％，优选5重量％-50重量％的具有核-壳结构的颗粒，其中所述核包含一种或多种磁性材料，同时所述壳包含二氧化硅，
c)0重量％-99重量％，优选20重量％-80重量％的一种或多种待交联或待固化的聚合物，
d)0重量％-90重量％的一种或多种溶剂，
e)0重量％-90重量％的一种或多种增加交联度或固化度的物质，其中所有的百分比是相对于所述复合材料。
本发明还提供制备所述复合材料的方法，其中将
a)一种或多种有机过氧化物、一种或多种C-C引发剂，或者有机过氧化物和C-C引发剂的混合物，
b)具有核-壳结构的颗粒，
c)任选存在的待交联或待固化的聚合物，
d)任选存在的溶剂，和
e)任选存在的一种或多种增加交联度或固化度的物质混合。
在此有机过氧化物或C-C引发剂可采用液体、固体、溶解的、乳化的、或悬浮的形式。所述核-壳颗粒可以以未被稀释的固体形式或分散的形式被使用。
可使用本领域技术人员已知的设备，例如，辊磨机、捏合系统，例如内部混合机、共捏合机、Z-桨式混合机、单螺杆和多螺杆挤出机、粉末混合机，例如转筒式混合机和鼓式混合机和/或搅拌器。
本发明还提供本发明所述的复合材料用于聚合物的交联和固化的用途。所述聚合物与作为所述复合材料的可能组分所提及的那些相同。
在此感应加热所述混合物。感应加热是指使所述混合物暴露于交替的磁场或电磁场。适用于此的为在100Hz-100kHz的中频范围内或在10kHz-60MHz的高频范围内的常规的感应器。本发明所述的复合材料能够有效地被导入此能量。用于此的核-壳颗粒的壳抑制所述自由基引发剂提早分解，但不使其更难以导入能量。
具体实施方式
原料
核-壳颗粒：
实施例1：一股物流由包含0.49kg/h的SiCl4和0.05kg/h甲硅烷的蒸气形式的混合物组成，利用双流体喷嘴在室温(23℃)下获得的气溶胶形式的第二股物流由25重量％浓度的氯化亚铁(II)水溶液(相当于1.55kg/h的氯化亚铁(II))和5Nm3/h的作为喷雾气体的氮气组成，将这两股物流分别地导入反应器的混合区。此混合物在该反应器的燃烧区中在由点燃7.9Nm3/h的氢气和21Nm3/h的空气的混合物产生的火焰中反应。该反应混合物在燃烧区中的滞留时间为约40ms。
在该燃烧区之后的冷却区中，通过导入8kg/h的水使该反应混合物冷却至332℃。
所得的固体在过滤器上从气态物质中被分离。
实施例2与实施例1相同，除了改变四氯化硅、甲硅烷、氢气和空气的比例之外。
表1给出实施例1和2的反应参数，表2给出所得粉末的物理化学数据。
表1：反应参数
1)在进入混合区时；2)在燃烧区中；3)冷却后；
表2：粉末的物理化学数据
1)磁铁矿、赤铁矿±5％；磁赤铁矿±10％；
2)由于低比例的磁赤铁矿不能测定结晶大小。
过氧化物：
结晶形式的二异丙苯基过氧化物(DCUP，CAS 80-43-3)，视为工业纯的。
2，5-二甲基-2，5-二(叔丁基过氧基)己-3-炔(DYBP-85-WO，CAS1068-27-5)，以被减敏化的形式以75％的含量存在于白油中。
2，4-二氯苯甲酰基过氧化物(DCLBP-50-PSI，CAS 133-14-2)，在50％硅油中减敏的结晶过氧化物。
2，5-二甲基-2，5-二(叔丁基过氧基)己烷(DHBP，CAS 78-63-7)，液体形式的过氧化物视为工业纯的(约92％)。
叔丁基过氧苯甲酸酯(TBPB，CAS 614-45-9)，液体形式的过氧化物视为工业纯的(约96％)。
聚合物：
LDPE：Lupolen 1800Sp，Basell，注塑级，MFI 17-22；HDPE：Lupolen4261A，Basell，管材挤塑级，MFI 2-4；EVA：Elvax
PV1400，DuPont，光致电压应用的特级。
实施例3：将100g叔丁基过氧苯甲酸酯(液体组分)和100g来自实施例1的颗粒在桨式混合机(Beken捏合机)中混合20min得到干燥可流动的无尘的复合材料。
实施例4：将60g来自实施例2的颗粒和140g of叔丁基过氧苯甲酸酯(液体组分)在桨式混合机(Beken捏合机)中混合20min得到高粘度的糊状物。
实施例5：在25mm实验室用挤出机(Collin，热塑性螺杆)中，使用115℃的熔融温度通过线模(strand die)在70rpm下制备由以下物质组成的复合材料：LDPE(Lupolen 1800Sp)、以及基于LDPE，分别为2％、3％和10％的来自实施例1的颗粒，以及过氧化物含量分别为1％的二(异丙苯基)过氧化物(DCUP)和1％的2，5-二甲基-2，5-二(叔丁基过氧基)己-3-炔(DYBP-85-WO)。
在高频磁场中加热线材部分：将被预热至约75℃的来自挤塑实施例(实施例5，1％的DYBP-85-WO)的长3cm的线材部分置于高频磁场(直径约4cm的特斯拉线圈，HF发电机，在650kHz下额定功率25kW，Celes)中。该发电机以其额定功率的50％运行10秒，然后以其额定功率的3％运行50秒。在第一功率设定中线材样品的表面温度升至230℃，在第二功率设定中，它逐渐升至245℃。由此获得期望的高交联度。
实施例6：将100g2，4-二氯苯甲酰基过氧化物(糊状物形式)和100g来自实施例1的颗粒在桨式混合机(Beken捏合机)中混合20min得到干燥可流动的25％浓度的复合材料。
实施例7：测试从60-肖氏(Shore)硅橡胶和2重量％的来自实施例4的复合材料获得的复合材料的贮藏稳定性。2周和4周后的流变仪测定(Goettfert Viscoelastograph)表明，无显著的交联时间变化或交联效率降低。因贮藏所致的粘度的寻常略微增长使扭矩稍微增长：从1.80到1.87Nm。
二酰基过氧化物特别敏感。因此，此复合材料可视为最大可能贮藏难度的实例。
实施例8：将65份EVA PV1400(DuPont)、15份DHBP和20份来自实施例1的颗粒在凸轮式捏合机(Brabender，300cm3室)中在70℃下捏合获得无尘的似橡胶的复合材料。
Claims (14)
1.复合材料，其包含：
选自有机过氧化物和/或含有不稳定的碳-碳键的引发剂的一种或多种可热活化的自由基引发剂，和
具有核-壳结构的颗粒，所述核包含一种或多种磁性材料，同时所述壳包含二氧化硅。
2.权利要求1所述的复合材料，其特征在于所述壳的厚度为2-500nm。
3.权利要求1或2所述的复合材料，其特征在于所述壳包含铁氧化物或由铁氧化物组成。
4.权利要求1-3所述的复合材料，其特征在于所述核材料的比例为50重量％-90重量％，所述壳材料的比例为10重量％-50重量％。
5.权利要求1-4所述的复合材料，其特征在于所述核-壳颗粒已被表面改性。
6.权利要求1-5所述的复合材料，其特征在于所述有机过氧化物选自氢过氧化物、二烷基过氧化物、二芳基过氧化物、过氧羧酸、过氧羧酸酯、二酰基过氧化物、过氧碳酸酯、过氧二碳酸酯、酮过氧化物、过氧缩酮和/或这些的混合物。
7.权利要求1-6所述的复合材料，其特征在于所述含有不稳定的碳-碳键的引发剂选自具有通式Ph-R4R3C-CR5R6-Ph的化合物，其中Ph是苯基基团或者取代的苯基基团，并且R3、R4、R5和R6各彼此独立地为氢或烷基基团。
8.权利要求1-7所述的复合材料，其特征在于，在各情况中相对于所述复合材料，所述具有核-壳结构的颗粒的比例为0.1重量％-60重量％，所述可热活化的自由基引发剂的比例为0.1重量％-90重量％。
9.权利要求1-8所述的复合材料，其特征在于它总是包含一种或多种待交联的聚合物或待固化的聚合物。
10.权利要求1-9所述的复合材料，其特征在于，在每种情况中相对于所述复合材料，所述核-壳颗粒的比例为20重量％-80重量％，所述可热活化的自由基引发剂的比例为20重量％-80重量％，所述聚合物的比例为20重量％-80重量％。
11.权利要求1-10所述的复合材料，其特征在于它包含一种或多种增加交联度或固化度的物质。
12.权利要求1-11所述的复合材料，其特征在于它包含一种或多种溶剂。
13.制备权利要求1-12所述的复合材料的方法，其特征在于将
a)一种或多种有机过氧化物、一种或多种C-C引发剂、或有机过氧化物和C-C引发剂的混合物，
b)具有核-壳结构的颗粒，
c)任选存在的待交联或待固化的聚合物，
d)任选存在的溶剂，和
e)任选存在的一种或多种增加交联度或固化度的物质混合。
14.权利要求1-13所述的复合材料用于交联和固化聚合物的用途。
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| JP2012530822A (ja) | 2012-12-06 |
| EP2445938B1 (en) | 2013-09-04 |
| US8877835B2 (en) | 2014-11-04 |
| IL216797A0 (en) | 2012-02-29 |
| KR20120014931A (ko) | 2012-02-20 |
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