CN108137863A - 封装的稳定剂组合物 - Google Patents
封装的稳定剂组合物 Download PDFInfo
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- CN108137863A CN108137863A CN201680056552.1A CN201680056552A CN108137863A CN 108137863 A CN108137863 A CN 108137863A CN 201680056552 A CN201680056552 A CN 201680056552A CN 108137863 A CN108137863 A CN 108137863A
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- polymer
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- stabilizer
- outer layer
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Abstract
本发明提供了作为端封闭丸粒的树脂母料组合物,该端封闭丸粒具有芯和封装该芯的外层,其中该芯包含至少一种添加剂,并且该外层包含聚合物,其中该外层的厚度为从0.001mm至1cm。稳定化的组合物由待稳定化的有机材料和该树脂母料组合物制备。一种用于生产该树脂母料组合物的方法包括共挤出呈管状形式的由外层封装的芯材料以形成填充的管,其中该芯材料包含至少一种添加剂,并且该外层包含聚合物;将该填充的管送入密封装置中,该密封装置将该填充的管切割成多个不连续段密封件并且同时密封每个不连续段的每一端,从而形成端封闭丸粒;以及冷却该端封闭丸粒。
Description
发明背景
技术领域。本发明整体涉及用于提供保护从而使有机聚合物(塑料)免受空气(氧气)、残余催化剂、机械应力、热和光的有害影响的稳定剂组合物。更具体地,本发明涉及具有粘性、蜡质和/或粘稠性质的聚合物添加剂(稳定剂)浓缩物,该聚合物添加剂(稳定剂)浓缩物被封装在合成的热塑性聚合物基质中,并且在运输、处理、存储和加工中提供改进特性。
2.背景技术。本领域中已经开发出大量能够抑制因空气(氧气)、残余催化剂、机械应力、热和光的有害影响而产生的有机材料(诸如塑料和聚合物制品)的降解的聚合物添加剂稳定剂组合物,其中这些添加剂与有机材料混合。稳定剂包括若干不同类别的化合物,诸如抗氧化剂、抗臭氧剂、热稳定剂、紫外(UV)光稳定剂、紫外线吸收剂、表面活性剂、致密化助剂、分散剂、颜料、金属氧化物、硫酯、镍化合物、自由基抑制剂、抗静电剂、防雾剂和防腐剂。在许多情况下,为获得最佳保护,通常使用这些化合物的混合物,这些化合物各自经过特别地选择,从而最大程度防止某些类型的降解。
尽管可以在聚合工艺中添加某些此类稳定剂,但是这种方法可能证明对于引入其他添加剂不令人满意。例如,聚合工艺的效率可能受到稳定剂与聚合催化剂相互作用的不利影响,所考虑的聚合物稳定剂可能与聚合工艺中使用的其他添加剂表现出不相容性和/或聚合物的后续处理可能受到在此早期阶段结合的稳定剂的存在的限制。一种可单独使用的引入稳定剂的方法或者在包括预成形的稳定剂共混物的添加剂“体系”中引入稳定剂的方法是在后反应器挤出操作过程中与待稳定化的聚合物混合。为了便于共混操作,期望提供颗粒形式的稳定剂,因为许多稳定剂可能在进料斗中结块或形成鼠洞,和/或通过计量设备不均匀地进料。此外,通常用于制造聚合物的某些稳定剂在处理和共混操作过程中可能产生有害的飘尘。粉末添加剂难以在塑料工业中最常用的***中进行输送,并且在输送期间会发生显著的粉末损失。另外,粉末添加剂呈粉末状,可能发生粉尘***并且可能给吸入粉尘或皮肤接触粉尘的工人带来潜在的健康风险。此外,粉末难以精确计量。因此,加入100%单独的添加剂组分存在若干问题,例如,产生粉尘,需要用于多种添加剂的多个料斗/进料器,因设备高温熔融添加剂而引起的粘性,单独添加若干组分导致不均匀性,添加剂在聚合物中附聚/分散不佳,在存储过程中附聚和在运输过程中附聚。另一方面,虽然装入预成形的添加剂共混物改善了分散性,需要较少的进料***,但是一些问题仍未得到解决,例如,滚动时产生灰尘,由设备高温(料斗)引起的粘性,添加剂迁移出添加剂预成型件,在存储过程中附聚和在运输过程中附聚。
另一种方法是首先制备稳定剂浓缩物,该稳定剂浓缩物为稳定剂和热塑性聚合物的预混物,其中包含高水平的稳定剂,因此可用作母料或浓缩物。使用母料或浓缩物是一种通常优选的技术,尤其是含有液体添加剂或糊状添加剂,因为仅采用具有此类物理形式的添加剂经常导致投配问题,并且常常需要特殊的计量泵或其他昂贵的设备。然而,总体来讲,已发现难以获得添加剂浓度占母料重量超过约15重量%的聚合物添加剂浓缩物。此外,母料技术还存在添加剂迁移/泄漏和设备高温引起粘性的问题,尤其是在添加剂具有低熔点或呈糊状或蜡质时。因此,由于料斗中存在跨接,使用这些母料会导致低通量,最终延长加工时间。
为了克服母料中的低添加剂浓度问题,欧洲专利申请公开编号259,960A2披露了一种大大增加此类浓缩物中的聚合物添加剂的百分比的方法,该方法采用颗粒固体(优选地二氧化硅)作为液体、糊状或蜡质低浓度固体添加剂的吸收剂。这种装载的吸收剂在适当条件下与合适的聚合物中共混,使得形成包含从15-80重量%的此类添加剂的超级浓缩物。然而,虽然EP 259,960的聚合物添加剂浓缩物将提供大大增加液体、糊状或蜡质添加剂的负载量的母料,但此类浓缩物存在某些缺点。具体地,当此类浓缩物被向下料到被挤出成为透明膜的聚合物中时,二氧化硅(或其他颗粒填料)对最终膜的透明度产生不利影响。
最近,得自Addcomp Holland B.V.的SKIN TECHNOLOGYTM使用特征是添加剂内层和保护外层的双层方法来解决母料共混方法的一些问题。装入SKIN TECHNOLOGYTM稳定剂在一定程度上解决了母料共混物的迁移问题,并且它声称消除了丸粒附聚。然而,虽然存储、运输或使用过程中的泄漏减少,但是由于有开放/切割端,在很大程度上仍然存在泄漏。参考图1,其中示出了使用SKIN TECHNOLOGYTM制得的典型产品。对于在性质上为液体、糊状或蜡质的添加剂或者如果是固体的话具有低熔点的添加剂,尤其如此。此外,典型稳定剂的浓度为约25%。
因此,在高于现有技术所提供的浓度水平下实现多种聚合物添加剂稳定剂的均匀性(并因此在聚合物材料中提供改善的分散性和可加工性)并且减轻由于呈糊状、蜡质或具有低熔点的添加剂的迁移而引起的存储和运输附聚的母料递送***将是本领域中有用的进步,并且可在聚合物工业中得到迅速接受。
发明内容
现已发现一种在高于现有技术的***或方法所提供的浓度水平下实现多种稳定剂的均匀性(并因此在聚合物材料中提供改善的分散性和可加工性时间)并且减轻由于呈糊状、蜡质或具有低熔点的添加剂的迁移带来的粘性而引起的存储和运输附聚的母料递送***。本发明的一个有利特征是其能够提高通量,尤其是对于糊状或蜡质添加剂或具有低熔点的添加剂,因为本发明的母料递送***的添加剂经过封装,并且不迁移或导致母料变粘,因此不堵塞加工设备诸如料斗和挤出机。
因此,本发明在一个方面提供了封装的单独添加剂稳定剂或者纯添加剂稳定剂组合物的共混物,其无尘、无泄漏并且易于处理、存储和运输。此类封装的稳定剂易于进料至挤出机或其他装置,在其中它们被引入熔融聚合物流中。在该步骤中,将封装的稳定剂稀释到最终的最终用途水平,从而稳定或将适当的稳定剂功能引入至生产的聚合物树脂。此类封装的稳定剂共混物也可用于以下情况:直接进料至固体聚合物中时,以及在最终熔融、混合和制粒之前与基体聚合物物理共混时,或者同时进料至用于生产的聚合物树脂的最终熔融、混合和制粒装置中时。本发明的封装的稳定剂对最终用途或最终产品无有害影响,因为封装材料与聚合物树脂基本上相同,或者它在被引入树脂之后是惰性的和不迁移的。
在一个实施例中,本发明包括作为端封闭丸粒(“CEP”)提供的封装的母料稳定剂组合物,该端封闭丸粒具有芯和外层,该外层具有封装该芯的聚合物,其中该芯包含至少一种稳定剂。虽然构成封装芯的外层的材料主要包括聚合物,并且构成芯的材料主要包括稳定剂添加剂,但是在某些实施例中,预期外层还可包括稳定剂添加剂,和/或芯可包括聚合物材料。在某些实施例中,稳定剂添加剂在芯中和外层中可以是相同的。对于聚合物材料也可如此。在一些实施例中,聚合物材料在芯中和外层中可以是相同的。在此类实施例中,仅浓度不同。
在另一方面,本发明提供了用于制备端封闭丸粒组合物的方法,该方法包括:共挤出聚合物外层和芯母料稳定剂组合物以形成管,其中芯被外层封装,使填充的管穿过用于将管同时密封和切割成多个不连续段的装置,以及冷却这些不连续段,从而形成包含稳定剂组合物的多个封装的丸粒,其中丸粒在由丸粒制成的管的每一端(封闭端)处密封。本发明还设想由此类方法制备的产品(即,端封闭丸粒)。
在某些实施例中,端封闭丸粒组合物的直径和管壁的厚度可通过使用不同的挤出模头尺寸来改变。
在另一方面,本发明提供了端封闭丸粒稳定剂组合物的各种用途:用于模制/配混成聚合物制品;用于水性涂料或溶剂型涂料;制造太阳能电池板;和油墨中。
本发明的这些以及其他目的、特征和优点将从结合附图以及实例进行的本发明的不同方面的以下详细说明变得清楚。
附图说明
图1-使用SKIN TECHNOLOGYTM制得的圆柱形丸粒。
图2-根据本发明的端封闭丸粒(CEP)。
图2A-不同形式的吩噻嗪、粉末(左侧)、小球(配混到聚苯乙烯中,中间)和端封闭丸粒(具有聚苯乙烯封装剂,右侧)。
图2B-不同尺寸的聚苯乙烯封装的吩噻嗪(CEP)。
图3A-I-端封闭丸粒(CEP)对挤出机进料口跨接的影响。图3A-C:UV-3853S薄片母料,(A)开始;(B)在90-100°F下持续1小时后;(C)在旋转挤出机螺杆后。图3D-F: UV-3853 PP5圆柱形丸粒母料,(D)开始;(E)在90-100°F下持续1小时后;(F)在旋转挤出机螺杆后;图3G-I: UV-3853 70%CEP母料,(G)开始;(H)在90-100°F下持续1小时后;(I)在旋转挤出机螺杆后。
图4A-B-添加剂附聚的对比研究。图4A1-3:具有PP的 UV-3853CEP,(1)50% UV-3853;(2)60% UV-3853;和(3)70% UV-3853;图4B1-3:(1) UV-3853S薄片母料;(2) UV-3853PP5圆形丸粒;和(3) UV-3853PP5圆柱形丸粒。
图5A-I-运输过程中脆碎度的评估(摇动器测试)。图5A:含PP的50% UV-3853CEP;图5B:含PP的60% UV-3853CEP;图5C:含PP的70% UV-3853CEP;图5D:含PE的50% UV-3853CEP;图5E:含PE的70%3853CEP;图5F:含SAN的60% UV-3853CEP;图5G: UV-3853S薄片母料(在LDPE中包含50%活性物质);图5H:UV-3853PP5圆形丸粒(在PP中包含50%活性物质);图5I:3853PP5圆柱形丸粒(在PP中包含50%活性物质)。
图6-挤出头和形成根据本发明的端封闭丸粒的示意图。
具体实施方式
在一个方面,本发明提供了封装的添加剂的新型组合物。该封装的添加剂包含芯材料和完全包封芯材料的外层,该芯材料包含至少一种添加剂,并且该外层具有聚合物材料。封装聚合物优选地为热塑性聚合物,该热塑性聚合物包括以下项中的至少一种:聚烯烃,聚酯,聚醚,聚酮,聚酰胺,天然橡胶和合成橡胶,聚氨酯,聚苯乙烯,高-抗冲击聚苯乙烯,聚丙烯酸酯,聚甲基丙烯酸酯,聚缩醛,聚丙烯腈,聚丁二烯,聚苯乙烯,丙烯腈-丁二烯-苯乙烯三聚物,苯乙烯-丙烯腈共聚物,丙烯酸酯-苯乙烯-丙烯腈三聚物,纤维素乙酸丁酸酯,纤维素聚合物,聚酰亚胺,聚酰胺酰亚胺,聚醚酰亚胺,聚苯硫醚,聚苯醚,聚砜,聚醚砜,聚氯乙烯,聚碳酸酯,聚酮,脂肪族聚酮,乙烯乙酸乙烯酯共聚物,以及它们的混合物。包含芯材料的至少一种添加剂优选地选自由以下项组成的组:受阻胺光稳定剂(HALS),紫外线吸收剂,酚类抗氧化剂,受阻苯甲酸酯,3-芳基苯并呋喃酮,色烷类化合物,脂肪酸碱金属盐类,羟胺,氧化胺,表面活性剂,致密化助剂,分散剂,有机亚磷酸酯,颜料,金属氧化物,有机亚膦酸酯,硫酯,镍化合物,自由基抑制剂,抗静电剂,防腐剂,催化剂,金属萃取剂,光引发剂,交联剂;以及它们中的两种或更多种的混合物。
在另一方面,本发明提供了一种用于制备封装的稳定剂的方法,该封装的添加剂包含芯材料和完全包封该芯材料的外层,该芯材料包含至少一种稳定剂,并且该外层具有聚合物材料。该方法包括共同形成由聚合物材料组成并且填充有具有至少一种稳定剂添加剂的芯材料的管,通过以下步骤实现:将用于外层的聚合物同时进料至挤出机的一部分中,并且将芯材料进料至同一挤出机的另一部分中并且共挤出外层和芯,从而形成填充有芯材料的聚合物管。然后将填充的管送入用于密封的封闭装置(例如,齿轮),由此齿轮同时将填充有芯材料的聚合物管密封/焊接和切割成多个不连续段。然后冷却这些段,从而形成包含稳定剂组合物的多个封装的丸粒,其中丸粒在由丸粒制成的管的每一端(封闭端)处密封。然后使干燥的丸粒穿过分离器并且被包装。
在另一方面,本发明提供了一种将封装的稳定剂引入聚合物中的方法。可使用诸如压延机、混合器、捏合机、挤出机等装置将封装的稳定剂与聚合物混合。在另一方面,本发明提供了与待稳定化的聚合物混合的封装的稳定剂的新型组合物。
封装的CEP中的一种或多种稳定剂的量可为约20重量%至约95重量%,并且优选地为30重量%至约90重量%。这些封装的稳定剂可用于聚合物树脂生产工艺中,尤其是在聚合物的制造过程中,由此在聚合之后,将聚合物进料至挤出机或其他装置中,聚合物在这些装置中熔化以便将封装的稳定剂引入熔融聚合物流中。此类稳定剂对于保持和改善聚合物的特性以及增加所述聚合物的功能或其他性能特征必不可少。
本发明的端封闭丸粒(CEP)消除了丸粒的脆碎或磨耗性能。脆碎和磨耗通常是指同一现象,其中丸粒在其运输过程中在其容器内可产生细粉。抗脆碎或磨耗性是非常希望的,因为产生的细粒非常小。
在此更详细地描述了本发明的这些和其他方面。如贯穿本披露所采用的,提供以下术语和定义来帮助读者。除非另外定义,否则在此使用的所有专门术语、注释以及其他科学专有名词旨在具有化学领域的普通技术人员通常理解的含义。如在此和所附权利要求书中所使用的,单数形式包括复数指示物,除非上下文另外清楚地指出。此外,如在此以及在所附权利要求书中使用的,数量或浓度的任何范围的披露包括在给定范围中的任何量或值的披露。
缩写“MB”是指“母料”,它是添加剂与聚合物的浓缩共混物;“圆柱形丸粒”或“表层”是指部分封装的稳定剂,即用热塑性聚合物的圆柱形外壳封装但具有开口端的稳定剂,以得自Addcomp Holland B.V.的SKIN TECHNOLOGYTM而熟知;“CEP”是指“端封闭丸粒”或聚合物封装的稳定剂,其中每个管的两端被封闭;“PP”是指聚丙烯;“PPC”是指聚丙烯共聚物,“PE”是指聚乙烯,“LDPE”是指低密度聚乙烯;并且“SAN”是指苯乙烯-丙烯腈共聚物。所有百分比都是指重量/重量百分比(重量%),除非上下文另外指出。
贯穿本说明书,术语以及取代基保留它们的定义。有机化学家(即,本领域普通技术人员)使用的缩写的综合性列表出现在有机化学杂志(Journal of Organic Chemistry)的每卷的第一期中。该列表,其典型地以标题为“缩写标准列表(Standard List ofAbbreviations)”的表格呈现,通过引用结合在此。
术语“烃基”是具有全碳骨架并且由碳和氢原子组成的包括脂肪族、脂环族和芳香族基团的通用术语。在某些情况下,如在此定义的,构成碳骨架的一个或多个碳原子可以被特定的原子或原子的基团如被N、O、和/或S中的一个或多个杂原子替换或中断。烃基的实例包括烷基、环烷基、环烯基、碳环芳基、烯基、炔基、烷基环烷基、环烷基烷基、环烯基烷基以及碳环芳烷基、烷芳基、芳烯基和芳炔基。此类烃基还可以被如在此定义的一个或多个取代基任选地取代。因而,在说明书和权利要求书中讨论的化学基团或部分应理解为包括取代或未取代的形式。以下表示的实例和优选项也适用于具有在此描述的式的化合物的取代基的各种定义中所指的烃基取代基或含烃基的取代基中的每一种,除非上下文另外指出。
优选的非芳香族烃基为饱和基团,例如烷基和环烷基。总体上,并且作为举例,这些烃基可以具有最高达五十个碳原子,除非上下文另外要求。具有从1至30个碳原子的烃基是优选的。在具有1至30个碳原子的烃基的子集内,具体的实例是C1-20烃基,如C1-12烃基(例如C1-6烃基或C1-4烃基),特定实例是从C1到C30烃基中所选择的任何单独值或值的组合。
烷基旨在包括直链的、支链的、或环状的烃结构以及其组合。低级烷基是指具有从1至6个碳原子的烷基。低级烷基的实例包括甲基、乙基、丙基、异丙基、丁基、仲丁基和叔丁基等。优选的烷基是C30或低于C30的那些。
烷氧基或烷氧基烷基是指通过氧原子附接到母体结构上的直链的、支链的、环状的构型以及其组合的从1至20个碳原子的基团。实例包括甲氧基、乙氧基、丙氧基、异丙氧基、环丙氧基、环己氧基等。
酰基是指甲酰基并且是指通过羰基官能团附接到母体结构上的直链的、支链的、环状构型的,饱和的、不饱和的和芳香族以及其组合的1、2、3、4、5、6、7、8、9、10、11和12个碳原子的基团。实例包括乙酰基、苯甲酰基、丙酰基、异丁酰基、叔丁氧基羰基、苄氧基羰基等。低级酰基是指包含一至六个碳的基团。
提及如在此使用的“碳环的”或“环烷基”基团,除非上下文另外指出,否则应包括芳香族和非芳环体系二者。因此,例如,该术语在其范围内包括芳香族、非芳香族、不饱和的、部分饱和的和完全饱和的碳环体系。总体上,此类基团可以是单环的或二环的并且可以含有例如3至12个环成员、更通常是5至10个环成员。单环基团的实例是含有3、4、5、6、7、和8个环成员、更通常3至7、并且优选5或6个环成员的基团。二环基团的实例是含有8、9、10、11、和12个环成员、并且更通常9或10个环成员的那些。非芳香族碳环/环烷基的实例包括c-丙基、c-丁基、c-戊基、c-己基等。C7至C10多环烃的实例包括环体系,如降冰片基和金刚烷基。
芳基(碳环芳基)是指5元或6元的芳香族碳环,含有:双环的9元或10元的芳香族环体系;或三环的13元或14元的芳香族环体系。芳香族的6元至14元的碳环包括,例如,取代的或未取代的苯基、苯、萘、茚满、萘满、和芴。
取代的烃基、烷基、芳基、环烷基、烷氧基等是指特定的取代基,其中在每个残基中最高达三个H原子被烷基、卤素、卤烷基、羟基、烷氧基、羧基、烷氧碳酰基(也称为烷氧基羰基)、羧酰胺基(也称为烷基氨基羰基)、氰基、羰基、硝基、氨基、烷基氨基、二烷基氨基、巯基、烷硫基、亚砜、砜、酰氨基、脒基、苯基、苄基、卤代苄基、杂芳基、苯氧基、苄氧基、杂芳氧基、苯甲酰基、卤代苯甲酰基或低级烷羟基替代。
“(甲基)丙烯酸酯”是丙烯酸酯或甲基丙烯酸酯的缩略语。
一种作为端封闭丸粒提供的树脂母料组合物,该端封闭丸粒包括芯和封装该芯的外层,其中该芯包含至少一种添加剂,并且该外层包含聚合物,其特征在于该外层的厚度为从0.001mm至1cm。
用于封装芯的外层为聚合物。该聚合物可为热塑性聚合物、热固性聚合物、水溶性或水分散性聚合物、生物可降解聚合物或它们的组合。在一些实施例中,该聚合物为热塑性聚合物。在一些实施例中,该聚合物为热塑性聚合物,该热塑性聚合物包括以下项中的至少一种:聚烯烃,聚酯,聚醚,聚酮,聚酰胺,天然橡胶和合成橡胶,聚氨酯,聚苯乙烯,高-抗冲击聚苯乙烯,聚丙烯酸酯,聚甲基丙烯酸酯,聚缩醛,聚丙烯腈,聚丁二烯,丙烯腈-丁二烯-苯乙烯三聚物,苯乙烯-丙烯腈共聚物,丙烯酸酯-苯乙烯-丙烯腈三聚物,纤维素乙酸丁酸酯,纤维素聚合物,聚酰亚胺,聚酰胺酰亚胺,聚醚酰亚胺,聚苯硫醚,聚苯醚,聚砜,聚醚砜,聚氯乙烯,聚碳酸酯,以及乙烯-乙酸乙烯酯共聚物。
另外,热塑性“聚烯烃”聚合物可选自下组的成员,该组由以下各项组成:i)选自聚丙烯、聚异丁烯、聚丁-1-烯、聚-4-甲基戊-1-烯的单烯烃的聚合物;ii)选自聚异戊二烯或聚丁二烯的二烯;iii)选自环戊烯和降冰片烯的环烯烃的聚合物;iv)任选地选自交联的聚乙烯、高密度聚乙烯(HDPE)、高密度和高分子量聚乙烯(HDPE-HMW)、高密度和超高分子量聚乙烯(HDPE-UHMW)、中密度聚乙烯(MDPE)、低密度聚乙烯(LDPE)、线性低密度聚乙烯(LLDPE)、非常低密度聚乙烯(VLDPE)和超低密度聚乙烯(ULDPE)的聚乙烯;v)它们的共聚物;以及vi)它们的混合物。
该聚合物可为生物可降解聚合物。生物可降解聚合物的实例包括聚乳酸、聚羟基丁酸酯、聚琥珀酸丁二酯、聚己内酯、聚羟基己酸酯、脂肪族-芳香族共聚物、聚羟基戊酸酯、聚琥珀酸己二酸丁二酯、聚己二酸丁二酯/对苯二甲酸酯、聚对苯二甲酸乙二醇酯、聚亚甲基己二酸酯/对苯二酸酯、以及它们的混合物。
在一些实施例中,该聚合物为水溶性聚合物或水分散性聚合物。水溶性聚合物或水分散性聚合物的实例包括纤维素衍生物、聚环氧乙烷、聚环氧丙烷、羟丙基纤维素、瓜尔胶、聚乙烯吡咯烷酮、聚乙烯己内酰胺、聚丙烯酰胺、聚羟基甲基丙烯酸酯、聚乙烯基咪唑、聚乙烯醇、聚羟基乙基甲基丙烯酸酯、有机硅聚合物、以及它们的混合物。
在一些实施例中,聚合物包括聚乙烯、聚丙烯、聚丙烯共聚物、聚苯乙烯和苯乙烯-丙烯腈共聚物中的至少一者。在一些实施例中,热塑性聚合物为聚丙烯(PP)或聚丙烯共聚物(PPC)。聚丙烯共聚物可为丙烯和乙烯的共聚物,并且可为无规共聚物、嵌段共聚物或抗冲击共聚物。在一些实施例中,热塑性聚合物为聚苯乙烯。
包含聚合物的封装外层具有管状形式。外层的厚度为从0.001mm至1cm,优选地为从0.001mm至1mm。端封闭丸粒的尺寸为从0.1cm至5cm长,优选地为从0.2cm至5cm。芯材料在室温下可为固体、半固体、蜡质或液体,其中室温被定义为25℃。包含至少一种添加剂的芯材料为端封闭丸粒的总重量的从10重量%至95重量%、20重量%至95重量%、或30重量%至90重量%。优选地,芯材料为端封闭丸粒的总重量的从40重量%至80重量%。更优选地,芯材料为封装的组合物的总重量的从50重量%至75重量%。
芯材料的组合物包含至少一种添加剂。添加剂的实例包括受阻胺光稳定剂(HALS)、紫外线吸收剂、酚类抗氧化剂、受阻苯甲酸酯、3-芳基苯并呋喃酮、色烷、脂肪酸碱金属盐类、羟胺、氧化胺、表面活性剂、致密化助剂、分散剂、有机亚磷酸酯、颜料、金属氧化物、有机亚膦酸酯、硫酯、镍化合物、自由基聚合抑制剂、抗静电剂、防腐剂、催化剂、金属萃取剂、光引发剂、交联剂;以及它们中的两种或更多种的混合物。
在一些实施例中,该至少一种添加剂包含稳定剂。稳定剂可包括受阻胺光稳定剂(HALS)、有机亚磷酸酯或亚膦酸酯、受阻酚、色烷、紫外线(UV)吸收剂、受阻苯甲酸酯、羟胺、氧化叔胺和自由基聚合抑制剂中的至少一者。
“受阻胺光稳定剂(HALS)”是包含根据式(I)的分子片段的化合物
其中:
R62选自下组的成员,该组由以下各项组成:氢;OH;C1-C20烃基;-CH2CN;C1-C12酰基;和C1-C18烷氧基;
R65选自下组的成员,该组由以下各项组成:氢;以及C1-C8烃基;并且
R60、R61、R63和R64各自独立地选自C1-C20烃基,或者R60和R61和/或R63和R64与它们所附接的碳一起形成C5-C10环烷基;
或根据式(II)的分子片段的化合物
其中:
m是从1至2的整数;
R39选自下组的成员,该组由以下各项组成:氢;OH;C1-C20烃基;-CH2CN;C1-C12酰基;和C1-C18烷氧基;并且
G1-G4各自独立地选自C1-C20烃基。
受阻胺光稳定剂优选地选自下组的成员,该组由以下各项组成:双(2,2,6,6-四甲基哌啶-4-基)癸二酸酯;双(2,2,6,6-四甲基哌啶-4-基)丁二酸酯;双(1,2,2,6,6-五甲基哌啶-4-基)癸二酸酯;双(1-辛氧基-2,2,6,6-四甲基哌啶-4-基)癸二酸酯;双(1,2,2,6,6-五甲基哌啶-4-基)正丁基3,5-二-叔丁基-4-羟苄基丙二酸酯;1-(2-羟乙基)-2,2,6,6-四甲基-4-羟基哌啶和丁二酸的缩合物;2,2,6,6-四甲基哌啶-4-基硬脂酸酯;2,2,6,6-四甲基哌啶-4-基十二烷酸酯;1,2,2,6,6-五甲基哌啶-4-基硬脂酸酯;1,2,2,6,6-五甲基哌啶-4-基十二烷酸酯;N,N'-双(2,2,6,6-四甲基哌啶-4-基)六亚甲基二胺和4-叔辛基氨基-2,6-二氯-1,3,5-三嗪的缩合物;三(2,2,6,6-四甲基哌啶-4-基)次氮基三乙酸酯;四(2,2,6,6-四甲基哌啶-4-基)-1,2,3,4-丁烷四羧酸酯;4-苯甲酰基-2,2,6,6-四甲基哌啶;4-硬脂氧基-2,2,6,6-四甲基哌啶;双(1,2,2,6,6-五甲基哌啶基)-2-正丁基-2-(2-羟基-3,5-二-叔丁基苄基)丙二酸酯;3-正辛基-7,7,9,9-四甲基-1,3,8-三氮杂螺[4.5]癸-2,4-二酮;双(1-辛氧基-2,2,6,6-四甲基哌啶基)癸二酸酯;双(1-辛氧基-2,2,6,6-四甲基哌啶基)丁二酸酯;N,N'-双(2,2,6,6-四甲基哌啶-4-基)六亚甲基二胺和4-吗啉代-2,6-二氯-1,3,5-三嗪的缩合物( UV-3346);2-氯-4,6-双(4-正丁基氨基-2,2,6,6-四甲基哌啶基)-1,3,5-三嗪和1,2-双(3-氨基丙基氨基)乙烷的缩合物;2-氯-4,6-双(4-正丁基氨基-1,2,2,6,6-五甲基哌啶基)-1,3,5-三嗪和1,2-双(3-氨基丙基氨基)乙烷的缩合物;8-乙酰基-3-十二烷基-7,7,9,9-四甲基-1,3,8-三氮杂螺[4.5]癸-2,4-二酮;3-十二烷基-1-(2,2,6,6-四甲基哌啶-4-基)吡咯烷-2,5-二酮;3-十二烷基-1-(1-乙酰基-2,2,6,6-四甲基哌啶-4-基)吡咯烷-2,5-二酮;3-十二烷基-1-(1,2,2,6,6-五甲基哌啶-4-基)吡咯烷-2,5-二酮;4-十六烷氧基-和4-硬脂氧基-2,2,6,6-四甲基哌啶的混合物;N,N'-双(2,2,6,6-四甲基哌啶-4-基)六亚甲基二胺和4-环己基氨基-2,6-二氯-1,3,5-三嗪的缩合物;1,2-双(3-氨基丙基氨基)乙烷、2,4,6-三氯-1,3,5-三嗪和4-丁氨基-2,2,6,6-四甲基哌啶的缩合物;2-十一烷基-7,7,9,9-四甲基-1-氧杂-3,8-二氮杂-4-氧代螺[4.5]癸烷;氧代-哌嗪基-三嗪;7,7,9,9-四甲基-2-环十一烷基-1-氧杂-3,8-二氮杂-4-氧代螺[4.5]癸烷和表氯醇的反应产物;四(2,2,6,6-四甲基-4-哌啶基)丁烷-1,2,3,4-四羧酸酯;1,2,3,4-丁烷四羧酸,四(1,2,2,6,6-五甲基-4-哌啶基)酯;1,2,3,4-丁烷四羧酸,1,2,2,6,6-五甲基-4-哌啶基十三烷基酯;1,2,3,4-丁烷四羧酸,2,2,6,6-四甲基-4-哌啶基十三烷基酯;1,2,3,4-丁烷四羧酸,与2,2,6,6-四甲基-2,4,8,10-四氧杂螺[5.5]-十一烷-3,9-二乙醇,1,2,2,6,6-五甲基-4-哌啶基酯的聚合物;1,2,3,4-丁烷四羧酸,与2,2,6,6-四甲基-2,4,8,10-四氧杂螺[5.5]-十一烷-3,9-二乙醇,2,2,6,6-四甲基-4-哌啶基酯的聚合物;双(1-十一烷氧基-2,2,6,6-四甲基哌啶-4-基)碳酸酯;1-(2-羟基-2-甲基丙氧基)-2,2,6,6-四甲基-4-哌啶醇;1-(2-羟基-2-甲基丙氧基)-4-十八烷酰氧基-2,2,6,6-四甲基哌啶;1-(4-十八酰氧基-2,2,6,6-四甲基哌啶-1-基氧基)-2-十八酰氧基-2-甲基丙烷;1-(2-羟乙基)-2,2,6,6-四甲基-4-哌啶醇;1-(2-羟乙基)-2,2,6,6-四甲基-4-哌啶醇和琥珀酸二甲酯的反应产物;2,2,4,4-四甲基-7-氧杂-3,20-二氮杂二螺[5.1.11.2]二十一烷-21-酮;2,2,6,6-四甲基-4-哌啶醇与高级脂肪酸例如C12-21饱和脂肪酸和C18不饱和脂肪酸的酯( UV-3853);3-十二烷基-1-(2,2,6,6-四甲基-4-哌啶基)吡咯烷-2,5-二酮;1H-吡咯-2,5-二酮,1-十八烷基-,与(1-甲基乙烯基)苯和1-(2,2,6,6-四甲基-4-哌啶基)-1H-吡咯-2,5-二酮的聚合物;哌嗪酮,1,1',1”-[1,3,5-三嗪-2,4,6-三基三[(环己基亚氨基)-2,1-乙烷二基]]三[3,3,5,5-四甲基-;哌嗪酮,1,1',1”-[1,3,5-三嗪-2,4,6-三基三[(环己基亚氨基)-2,1-乙烷二基]]三[3,3,4,5,5-五甲基-;7,7,9,9-四甲基-2-环十一烷基-1-氧杂-3,8-二氮杂-4-氧代螺[4.5]癸烷和表氯醇的反应产物;N,N'-双(2,2,6,6-四甲基哌啶-4-基)六亚甲基二胺和4-环己基氨基-2,6-二氯-1,3,5-三嗪的缩合物;1,2-双(3-氨基丙基氨基)乙烷、2,4,6-三氯-1,3,5-三嗪和4-丁氨基-2,2,6,6-四甲基哌啶的缩合物;N,N'-双(2,2,6,6-四甲基哌啶-4-基)六亚甲基二胺和4-吗啉代-2,6-二氯-1,3,5-三嗪的缩合物;2-氯-4,6-双(4-正丁基氨基-2,2,6,6-四甲基哌啶基)-1,3,5-三嗪和1,2-双(3-氨基丙基氨基)乙烷的缩合物;2-氯-4,6-双(4-正丁基氨基-1,2,2,6,6-五甲基哌啶基)-1,3,5-三嗪和1,2-双(3-氨基丙基氨基)乙烷的缩合物;2-[(2-羟乙基)氨基]-4,6-双[N-(1-环己氧基-2,2,6,6-四甲基哌啶-4-基)丁氨基-1,3,5-三嗪;丙二酸,[(4-甲氧基苯基)-亚甲基]-双-(1,2,2,6,6-五甲基-4-哌啶基)酯;四(2,2,6,6-四甲基哌啶-4-基)-1,2,3,4-丁烷四羧酸酯;苯丙酸,3,5-双(1,1-二甲基乙基)-4-羟基-,1-[2-[3-[3,5-双(1,1-二甲基乙基)-4-羟基苯基]-1-氧代丙氧基]乙基]-2,2,6,6-四甲基-4-哌啶基酯;N-(1-辛氧基-2,2,6,6-四甲基哌啶-4-基)-N'-十二烷基草酰胺;三(2,2,6,6-四甲基哌啶-4-基)次氮基三乙酸酯;1,5-二氧杂螺{5,5}十一烷-3,3-二羧酸,双(1,2,2,6,6-五甲基-4-哌啶基):1,5-二氧杂螺{5,5}十一烷-3,3-二羧酸,双(2,2,6,6-四甲基-4-哌啶基);1-(2-羟乙基)-2,2,6,6-四甲基-4-羟基哌啶和丁二酸的缩合物;N,N'-双(2,2,6,6-四甲基哌啶-4-基)六亚甲基二胺和4-叔辛基氨基-2,6-二氯-1,3,5-三嗪的缩合物;1,2,3,4-丁烷四羧酸,1,2,2,6,6-五甲基-4-哌啶基十三烷基酯;四(2,2,6,6-四甲基哌啶-4-基)-1,2,3,4-丁烷四羧酸酯;1,2,3,4-丁烷四羧酸,2,2,6,6-四甲基-4-哌啶基十三烷基酯;四(1,2,2,6,6-五甲基哌啶-4-基)-1,2,3,4-丁烷四羧酸酯;2,2,4,4-四甲基-21-氧代-7-氧杂-3.20-二氮杂螺(5.1.11.2)-二十一烷-20-丙酸-十二烷基酯和2,2,4,4-四甲基-21-氧代-7-氧杂-3.20-二氮杂螺(5.1.11.2)-二十一烷-20-丙酸-十四烷基酯的混合物;1H,4H,5H,8H-2,3a,4a,6,7a,8a-六氮杂环戊[def]芴-4,8-二酮,六氢-2,6-双(2,2,6,6-四甲基-4-哌啶基)-;聚甲基[丙基-3-氧基(2',2',6',6'-四甲基-4,4'-哌啶基)]硅氧烷;聚甲基[丙基-3-氧基(1',2',2',6',6'-五甲基-4,4'-哌啶基)]硅氧烷;甲基丙烯酸甲酯与丙烯酸乙酯和2,2,6,6-四甲基哌啶-4-基丙烯酸酯的共聚物;混合的C20至C24α-烯烃和(2,2,6,6-四甲基哌啶-4-基)丁二酰亚胺的共聚物;1,2,3,4-丁烷四羧酸,与β,β,β',β'-四甲基-2,4,8,10-四氧杂螺[5.5]十一烷-3,9-二乙醇,1,2,2,6,6-五甲基-4-哌啶基酯的聚合物;1,2,3,4-丁烷四羧酸,与β,β,β',β'-四甲基-2,4,8,10-四氧杂螺[5.5]十一烷-3,9-二乙醇,2,2,6,6-四甲基-4-哌啶基酯共聚物的聚合物;1,3-苯二羧酰胺,N,N'-双(2,2,6,6-四甲基-4-哌啶基;1,1'-(1,10-二氧代-1,10-癸烷二基)-双(六氢-2,2,4,4,6-五甲基嘧啶;乙烷二酰胺,N-(1-乙酰基-2,2,6,6-四甲基哌啶基)-N'-十二烷基;甲酰胺,N,N'-1,6-己烷二基双[N-(2,2,6,6-四甲基-4-哌啶基);D-葡萄糖醇,1,3:2,4-双-O-(2,2,6,6-四甲基-4-亚哌啶基)-;2,2,4,4-四甲基-7-氧杂-3,20-二氮杂-21-氧代-二螺[5.1.11.2]二十一烷;丙酰胺,2-甲基-N-(2,2,6,6-四甲基-4-哌啶基)-2-[(2,2,6,6-四甲基-4-哌啶基)氨基]-;7-氧杂-3,20-二氮杂二螺[5.1.11.2]二十一烷-20-丙酸,2,2,4,4-四甲基-21-氧代-,十二烷基酯;N-(2,2,6,6-四甲基哌啶-4-基)-β-氨基丙酸十二烷基酯;N-(2,2,6,6-四甲基哌啶-4-基)-N'-氨基草酰胺;丙酰胺,N-(2,2,6,6-四甲基-4-哌啶基)-3-[(2,2,6,6-四甲基-4-哌啶基)氨基]-;4-十六烷氧基-和4-硬脂氧基-2,2,6,6-四甲基哌啶的混合物;3-十二烷基-1-(1,2,2,6,6-五甲基哌啶-4-基)吡咯烷-2,5-二酮;3-十二烷基-1-(1-乙酰基-2,2,6,6-五甲基哌啶-4-基)吡咯烷-2,5-二酮;双(2,2,6,6-四甲基哌啶-4-基)丁二酸酯;双(1,2,2,6,6-五甲基哌啶-4-基)正丁基3,5-二-叔丁基-4-羟苄基丙二酸酯;三(2,2,6,6-四甲基哌啶-4-基)次氮基三乙酸酯;1,1'-(1,2-乙烷二基)双(3,3,5,5-四甲基哌嗪酮);4-苯甲酰基-2,2,6,6-四甲基哌啶;4-硬脂氧基-2,2,6,6-四甲基哌啶;双(1,2,2,6,6-五甲基哌啶基)-2-正丁基-2-(2-羟基-3,5-二-叔丁基苄基)丙二酸酯;3-正辛基-7,7,9,9-四甲基-1,3,8-三氮杂螺[4.5]癸-2,4-二酮;双(1-辛氧基-2,2,6,6-四甲基哌啶基)癸二酸酯;双(1-辛氧基-2,2,6,6-四甲基哌啶基)丁二酸酯;8-乙酰基-3-十二烷基-7,7,9,9-四甲基-1,3,8-三氮杂螺[4.5]癸-2,4-二酮;3-十二烷基-1-(2,2,6,6-四甲基哌啶-4-基)吡咯烷-2,5-二酮;3-十二烷基-1-(1-乙酰基-2,2,6,6-四甲基哌啶-4-基)吡咯烷-2,5-二酮;3-十二烷基-1-(1,2,2,6,6-五甲基哌啶-4-基)吡咯烷-2,5-二酮;4-十六烷氧基-和4-硬脂氧基-2,2,6,6-四甲基哌啶的混合物;2-十一烷基-7,7,9,9-四甲基-1-氧杂-3,8-二氮杂-4-氧代螺[4.5]癸烷;1,5-二氧杂螺{5,5}十一烷-3,3-二羧酸,双(2,2,6,6-四甲基-4-哌啶基)和1,5-二氧杂螺{5,5}十一烷-3,3-二羧酸,双(1,2,2,6,6-五甲基-4-哌啶基);N1-(β-羟乙基)3,3-五亚甲基-5,5-二甲基哌嗪-2-酮;N1-叔辛基-3,3,5,5-四甲基-二氮杂卓-2-酮;N1-叔辛基-3,3-五亚甲基-5,5-六亚甲基-二氮杂卓-2-酮;N1-叔辛基-3,3-五亚甲基-5,5-二甲基哌嗪-2-酮;反式-1,2-环己烷-双-(N1-5,5-二甲基-3,3-五亚甲基-2-哌嗪酮;反式-1,2-环己烷-双-(N1-3,3,5,5-二螺五亚甲基-2-哌嗪酮);N1-异丙基-1,4-二氮杂二螺-(3,3,5,5)五亚甲基-2-哌嗪酮;N1-异丙基-1,4-二氮杂二螺-3,3-五亚甲基-5,5-四亚甲基-2-哌嗪酮;N1-异丙基-5,5-二甲基-3,3-五亚甲基-2-哌嗪酮;反式-1,2-环己烷-双-N1-(二甲基-3,3-五亚甲基-2-哌嗪酮);N1-辛基-5,5-二甲基-3,3-五亚甲基-1,4-二氮杂卓-2-酮;和N1-辛基-1,4-二氮杂二螺-(3,3,5,5)-五亚甲基-1,5-二氮杂卓-2-酮。
在一些实施例中,受阻胺光稳定剂包括2,2,6,6-四甲基-4-哌啶醇与C12-21饱和脂肪酸和C18不饱和脂肪酸的酯,以 UV-3853S(含LDPE的50重量%浓缩物)和 UV-3853PP5(含聚丙烯的50重量%浓缩物)购得。2,2,6,6-四甲基-4-哌啶醇与C12-21饱和脂肪酸和C18不饱和脂肪酸的酯还可作为与其他热塑性聚合物例如聚丙烯共聚物或苯乙烯-丙烯腈共聚物的浓缩物提供。在一些实施例中,受阻胺光稳定剂包括N,N'-双(2,2,6,6-四甲基哌啶-4-基)六亚甲基二胺和4-吗啉代-2,6-二氯-1,3,5-三嗪的缩合物(以 UV-3346购得)。在一些实施例中,可使用稳定剂的组合。例如,至少一种添加剂可为2,2,6,6-四甲基-4-哌啶醇与C12-21饱和脂肪酸和C18不饱和脂肪酸的酯和十六烷基3,5-二叔丁基-4-羟基苯甲酸酯的组合。
“有机亚磷酸酯或亚膦酸酯”选自:
根据式1-7的化合物
其中:
指数为整数,并且n为2、3或4;p是1或2;q是2或3;r是4至12;y是1、2或3;并且z是1至6;
A1(如果n是2)为C2-C18亚烷基;被氧、硫或-NR4-中断的C2-C12亚烷基;具有下式的基团
或亚苯基;
A1(如果n是3)为具有式-CrH2r-1-的基团;
A1(如果n是4)为
A2与A1的定义相同(如果n是2);
B是直接键、-CH2-、-CHR4-、-CR1R4-、硫、C5-C7环亚烷基、或亚环己基(其3、4和/或5位被1至4个C1-C4烷基取代);
D1(如果p是1)为C1-C4烷基,并且在p是2的情况下为-CH2OCH2-;
D2(如果p是1)为C1-C4烷基;
E(如果y是1)为C1-C18烷基、-OR1或卤素;
E(如果y是2)为-O-A2-O-,
E(如果y是3)为具有式R4C(CH2O-)3或N(CH2CH2O-3的基团;
Q为至少z价醇或酚的基团,该基团通过氧原子连接到磷原子;
R1、R2和R3彼此独立地为C1-C18烷基,其未被取代或被卤素、-COOR4、-CN或-CONR4R4取代;被氧、硫或-NR4-中断的C2-C18烷基;C7-C9苯基烷基;C5-C12环烷基、苯基、或萘基;被卤素、1至3个烷基或烷氧基(共具有1至18个碳原子)或被C7-C9苯基烷基取代的萘基或苯基;或具有式(III)的基团
其中m是在3至6的范围内的整数;
R4为氢、C1-C8烷基、C5-C12环烷基或C7-C9苯基烷基,
R5和R6彼此独立地为氢、C1-C8烷基或C5-C6环烷基,
R7和R8(如果q是2)彼此独立地为C1-C4烷基或者一起为2,3-去氢五亚甲基自由基;并且
R7和R8(如果q是3)是甲基;
R14是氢、C1-C9烷基或环己基,
R15是氢或甲基,并且如果存在两个或更多个自由基R14和R15,则这些自由基相同或不同,
X和Y各自为直接键或氧,
Z是直接键、亚甲基、-C(R16)2-或硫,并且
R16是C1-C8烷基;以及
根据式(8)的三芳基亚磷酸酯:
其中R17是取代基,该取代基在具有式(8)的芳香族部分的从0至5个位置处相同或不同并且独立地选自下组的成员,该组由以下各项组成:C1-C20烷基、C3-C20环烷基、C4-C20烷基环烷基、C6-C10芳基和C7-C20烷芳基;以及它们的组合。
优选地,有机亚磷酸酯或亚膦酸酯选自:亚磷酸三苯酯;亚磷酸二苯基烷基酯;亚磷酸苯基二烷基酯;亚磷酸三月桂酸酯;亚磷酸三(十八烷基)酯;亚磷酸二硬脂基季戊四醇酯;亚磷酸三-(2,4-二叔丁基苯基)酯;亚磷酸三(壬基苯基)酯;式(A)、(B)、(C)、(D)、(E)、(F)、(G)、(H)、(J)、(K)和(L)的化合物:
2-丁基-2-乙基-1,3-丙二醇2,4,6-三叔丁基苯酚亚磷酸酯,双(2,6-二叔丁基-4-甲基苯基)季戊四醇二亚磷酸酯,2-丁基-2-乙基-1,3-丙二醇2,4-二-枯基苯酚亚磷酸酯,2-丁基-2-乙基-1,3-丙二醇4-甲基-2,6-二叔丁基苯酚亚磷酸酯,和双(2,4,6-三叔丁基苯基)季戊四醇二亚磷酸酯。
更优选地,至少一种亚磷酸酯或亚膦酸酯选自三-(2,4-二叔丁基苯基)亚磷酸酯(168);双(2,4-二枯基苯基)季戊四醇二亚磷酸酯(S9228);和四(2,4-二叔丁基苯基)4,4'-亚联苯基-二亚磷酸酯( P-EPQ)。
该“受阻酚”化合物包含根据式(IVa)、(IVb)或(IVc)中的一个或多个的分子片段:
其中:
R18选自氢或C1-4烃基;
R19和R20各自独立地选自氢或C1-C20烃基;并且
R37选自C1-C12烃基。
优选的受阻酚为其中R18和R37各自独立地选自甲基或叔丁基。更优选地,至少一种受阻酚化合物选自下组的成员,该组由以下各项组成:(1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮;1,1,3-三(2'-甲基-4'-羟基-5'-叔丁基苯基)丁烷;三乙二醇双[3-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯];4,4'-硫代双(2-叔丁基-5-甲基苯酚);2,2'-硫代二亚乙基双[3-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯];十八烷基3-(3'-叔丁基-4'-羟基-5'-甲基苯基)丙酸酯;四亚甲基(3-叔丁基-4-羟基-5-甲基氢化肉桂酸酯)甲烷;N,N'-六亚甲基双[3-(3-叔丁基-4-羟基-5-甲基苯基)丙酰胺];二(4-叔丁基-3-羟基-2,6-二甲基苄基)硫代二丙酸酯;和十八烷基3,5-二-叔丁基-4-羟基氢化肉桂酸酯。
可用于本发明中的“色烷”选自具有式(V)的化合物:
其中:
R21选自-COR28或-Si(R29)3,其中R28选自H或C1-C20烃基;并且R29选自C1-C12烃基或烷氧基;
R22是取代基,该取代基在具有式V的芳香族部分的n=0至3位置处相同或不同并且独立地选自H或C1-C12烃基;
R23选自H或C1-C12烃基;
R24选自H或C1-C20烃基;
R25-R27各自独立地选自下组的成员,该组由以下各项组成:H;C1-C12烃基;和-OR30,其中R30选自H或C1-C12烃基;并且
R27是H,或与R26一起形成=O的键。
优选地,式(V)的化合物为生育酚,其选自由α-生育酚、β-生育酚、γ-生育酚、δ-生育酚、它们的异构体、相关的生育三烯酚以及它们的混合物组成的组中的成员。
另一种优选的色烷为根据式(VI)的维生素E乙酸酯:
或它们的异构体和/或混合物。
“紫外线(UV)吸收剂”选自下组的成员,该组由以下各项组成:2-羟基二苯甲酮、2-(2'-羟基苯基)苯并***、2-(2'-羟基苯基)-1,3,5-三嗪、苯并噁嗪酮、草酰胺、草酰替苯胺以及包含前述化合物中的至少一种的组合。
在一个优选的实施例中,根据式(VII)的紫外线吸收剂2-(2'-羟基苯基)-1,3,5-三嗪化合物:
其中:
R34和R35各自独立地选自下组的成员,该组由以下各项组成:任选取代的C6-C10芳基、C1-C10烃基取代的氨基、C1-C10酰基和C1-C10烷氧基;并且
R36是取代基,该取代基在具有式VII的苯氧基部分的从0至4个位置处相同或不同并且在每个实例中独立地选自由羟基、C1-C12烃基、C1-C12烷氧基、C1-C12烷氧基酯和C1-C12酰基组成的组中的成员。
优选地,2-(2'-羟基苯基)-1,3,5-三嗪化合物选自下组的成员,该组由以下各项组成:4,6-双(2,4-二甲基苯基)-2-(2-羟基-4-辛氧基苯基)-s-三嗪(1164,购自氰特公司(Cytec)(苏威基团(Solvay Group));4,6-双-(2,4-二甲基苯基)-2-(2,4-二羟基苯基)-s-三嗪;2,4-双(2,4-二羟基苯基)-6-(4-氯苯基)-s-三嗪;2,4-双[2-羟基-4-(2-羟基-乙氧基)苯基]-6-(4-氯苯基)-s-三嗪;2,4-双[2-羟基-4-(2-羟基-4-(2-羟基-乙氧基)苯基]-6-(2,4-二甲基苯基)-s-三嗪;2,4-双[2-羟基-4-(2-羟乙氧基)苯基]-6-(4-溴苯基)-s-三嗪;2,4-双[2-羟基-4-(2-乙酰氧基乙氧基)苯基]-6-(4-氯苯基)-s-三嗪;2,4-双(2,4-二羟基苯基)-6-(2,4-二甲基苯基)-s-三嗪;2,4-双(4-联苯基)-6-[2-羟基-4-[(辛氧基羰基)亚乙氧基]苯基]-s-三嗪;2,4-双(4-联苯基)-6-[2-羟基-4-(2-乙基己氧基)苯基]-s-三嗪;2-苯基-4-[2-羟基-4-(3-仲-丁氧基-2-羟丙氧基)苯基]-6-[2-羟基-4-(3-仲-戊氧基-2-羟丙氧基)苯基]-s-三嗪;2,4-双(2,4-二甲基苯基)-6-[2-羟基-4(-3-苄氧基-2-羟丙氧基)苯基]-s-三嗪;2,4-双(2-羟基-4-正丁氧基苯基)-6-(2,4-二-正丁氧基苯基)-s-三嗪;2,4-双(2,4-二甲基苯基)-6-[2-羟基-4-(3-壬氧基-2-羟丙氧基)-5-α-枯基苯基]-s-三嗪;亚甲基双-{2,4-双(2,4-二甲基苯基)-6-[2-羟基-4-(3-丁氧基-2-羟丙氧基)苯基]-s-三嗪};以5:4:1比率在3:5'、5:5'和3:3'位上桥联的亚甲基桥联的二聚物混合物;2,4,6-三(2-羟基-4-异辛氧基羰基异-亚丙氧基-苯基)-s-三嗪;2,4-双(2,4-二甲基苯基)-6-(2-羟基-4-己氧基-5-α-枯基苯基)-s-三嗪;2-(2,4,6-三甲基苯基)-4,6-双[2-羟基-4-(3-丁氧基-2-羟丙氧基)苯基]-s-三嗪;2,4,6-三[2-羟基-4-(3-仲-丁氧基-2-羟丙氧基)-苯基]-s-三嗪;4,6-双(2,4-二甲基苯基)-2-(2-羟基-4-(3-十二烷氧基-2-羟丙氧基)苯基)-s-三嗪和4,6-双(2,4-二甲基苯基)-2-(2-羟基-4-(3-十三烷氧基-2-羟丙氧基)苯基)-s-三嗪的400)的混合物(购自巴斯夫公司(BASF);4,6-双-(2,4-二甲基苯基)-2-(2-羟基-4(3-(2-乙基己氧基)-2-羟丙氧基)-苯基)-s-三嗪;4,6-二苯基-2-(4-己氧基-2-羟基苯基)-s-三嗪;以及它们的组合。
在另一个优选的实施例中,紫外线吸收剂2-(2'-羟基苯基)苯并***选自:2-(2'-羟基-5'-甲基苯基)-苯并***;2-(3',5'-二叔丁基-2'-羟基苯基)苯并***;2-(5'-叔丁基-2'-羟基苯基)苯并***;2-(2'-羟基-5'-(1,1,3,3-四甲基丁基)苯基)苯并***;2-(3',5'-二叔丁基-2'-羟基苯基)-5-氯-苯并***;2-(3'-叔丁基-2'-羟基-5'-甲基苯基)-5-氯-苯并***;2-(3'-仲丁基-5'-叔丁基-2'-羟基苯基)苯并***;2-(2'-羟基-4'-辛氧基苯基)苯并***;2-(3',5'-二叔戊基-2'-羟基苯基)苯并***;2-(3',5'-双(α,α-二甲基苄基)-2'-羟基苯基)苯并***;2-(3'-叔丁基-2'-羟基-5'-(2-辛氧基羰基乙基)苯基)-5-氯-苯并***;2-(3'-叔丁基-5'-[2-(2-乙基己氧基)-羰基乙基]-2'-羟基苯基)-5-氯-苯并***;2-(3'-叔丁基-2'-羟基-5'-(2-甲氧基羰基乙基)苯基)-5-氯-苯并***;2-(3'-叔丁基-2'-羟基-5'-(2-甲氧基羰基乙基)苯基)苯并***;2-(3'-叔丁基-2'-羟基-5'-(2-辛氧基羰基乙基)苯基)苯并***;2-(3'-叔丁基-5'-[2-(2-乙基己氧基)羰基]-2'-羟基苯基)苯并***;2-(3'-十二烷基-2'-羟基-5'-甲基苯基)苯并***;2-(3'-叔丁基-2'-羟基-5'-(2-异辛氧基羰基乙基)苯基苯并***;2,2'-亚甲基-双[4-(1,1,3,3-四甲基丁基)-6-苯并***-2-基苯酚];2-[3'-叔丁基-5'-(2-甲氧基羰基乙基)-2'-羟基苯基]-2H-苯并***与聚乙二醇300的酯交换产物;[R-CH2CH2-COO-CH2CH2]2,其中R是3'-叔丁基-4'-羟基-5'-2H-苯并***-2-基苯基;2-[2'-羟基-3'-(α,α-二甲基苄基)-5'-(1,1,3,3-四甲基丁基)-苯基]苯并***;2-[2'-羟基-3'-(1,1,3,3-四甲基丁基)-5'-(α,α-二甲基苄基)-苯基]苯并***;以及它们的混合物。
在另一方面,紫外线吸收剂2-羟基二苯甲酮选自2-羟基二苯甲酮的4-羟基、4-甲氧基、4-辛氧基、4-癸氧基、4-十二烷氧基、4-苄氧基、4,2',4'-三羟基和2'-羟基-4,4'-二甲氧基的衍生物;以及它们的混合物。
本发明中所用的“受阻苯甲酸酯”为选自以下项的化合物:4-叔丁基苯基水杨酸酯、水杨酸苯酯、水杨酸辛基苯基酯、二苯甲酰间苯二酚,双(4-叔丁基苯甲酰基)间苯二酚、苯甲酰间苯二酚、2,4-二叔丁基苯基3,5-二叔丁基-4-羟基苯甲酸酯、十六烷基3,5-二叔丁基-4-羟基苯甲酸酯、十八烷基3,5-二叔丁基-4-羟基苯甲酸酯、2-甲基-4,6-二叔丁基苯基3,5-二叔丁基-4-羟基苯甲酸酯以及它们的混合物。在一些实施例中,受阻苯甲酸酯包括十六烷基3,5-二叔丁基-4-羟基苯甲酸酯,以 UV-2908购自氰特公司(苏威基团)。
可用于本发明中的“羟胺”类稳定剂包括选自下组的成员,该组由以下各项组成的至少一种化合物:
根据式(VIII)的羟胺化合物
其中:
T1选自下组的成员,该组由以下各项组成:任选取代的C1-C36烃基、任选取代的C5-C12环烷基和任选取代的C7-C9芳烷基;并且
T2选自氢或T1;并且
根据式(IX)的氧化叔胺化合物
其中:
W1和W2各自独立地选自C6-C36烃基,该C6-C36烃基选自下组的成员,该组由以下各项组成:直链或支链C6-C36烷基、C6-C12芳基、C7-C36芳烷基、C7-C36烷芳基、C5-C36环烷基、C6-C36烷基环烷基(alkcycloalkyl);和C6-C36环烷基烷基;
W3选自C1-C36烃基,该C1-C36烃基选自下组的成员,该组由以下各项组成:直链或支链C1-C36烷基、C6-C12芳基、C7-C36芳烷基、C7-C36烷芳基、C5-C36环烷基、C6-C36烷基环烷基;和C6-C36环烷基烷基;
其前提是W1、W2和W3中的至少一者包含β碳氢键;
其中所述烷基、芳烷基、烷芳基、环烷基、烷基环烷基和环烷基烷基可被1至16个基团中断,这些基团选自由-O-、-S-、-SO-、-SO2-、COO、-OCO-、-CO-、NW4-、-CONW4-和-NW4CO-组成的组中的成员,或者其中所述烷基、芳烷基、烷芳基、环烷基、烷基环烷基和环烷基烯丙基可被1至16个基团取代,这些基团选自由-OW4、-SW4、-COOW4、-OCOW4、-COW4、-N(W4)2、-CON(W4)2、-NW4COW4以及包含-C(CH3)(CH2Rx)NL(CH2Rx)(CH3)C-基团的5元环和6元环组成的组中的成员,或者其中所述烷基、芳烷基、烷芳基、环烷基、烷基环烷基和环烷基烷基同时被上述基团中断和取代;
其中:
W4选自氢或C1-C8烷基;
Rx选自氢或甲基;并且
L选自C1-C30烷基;-C(O)R部分或-OR部分,其中R为C1-C30直链或支链烷基;并且
其中所述芳基可被选自下组的成员,该组由以下各项组成取代:一至三个卤素基团、C1-C8烷基、C1-C8烷氧基以及它们的组合。
根据式(VIII)的“羟胺”稳定剂组合物为N,N-二烃基羟胺,其中T1和T2各自独立地选自由苄基、乙基、辛基、月桂基、十二烷基、十四烷基、十六烷基、十七烷基和十八烷基组成的组中的成员;或者其中T1和T2各自为在于氢化牛脂胺中发现的烷基混合物。
更优选地,根据式(VIII)的化合物为N,N-二烃基羟胺,其选自下组的成员,该组由以下各项组成:N,N-二苄基羟胺;N,N-二乙基羟胺;N,N-二辛基羟胺;N,N-二月桂基羟胺;N,N-双十二烷基羟胺;N,N-双十四烷基羟胺;N,N-双十六烷基羟胺;N,N-双十八烷基羟胺;N-十六烷基-N-十四烷基羟胺;N-十六烷基-N-十七烷基羟胺;N-十六烷基-N-十八烷基羟胺;N-十七烷基-N-十八烷基羟胺;以及N,N-二(氢化牛脂)羟胺。
本发明的另一方面是提供包含自由基聚合抑制剂的树脂母料组合物。在烯键式不饱和单体的制造、蒸馏/纯化和存储/运输过程中,常见的做法是掺入单体稳定剂(即,自由基抑制剂)。这些抑制剂设计用于防止这些单体的过早聚合,从而使得单体在受控聚合条件下转化为有用的聚合物之前被制造、蒸馏、或以其他方式纯化和存储。烯键式不饱和单体的实例包括苯乙烯、丁二烯、α-甲基苯乙烯、乙烯基甲苯、乙烯基萘、乙烯、丙烯、乙酸乙烯酯、叔碳酸乙烯酯、氯乙烯、偏二氯乙烯、丙烯腈、甲基丙烯腈、(甲基)丙烯酰胺、(甲基)丙烯酸的各种C1-40烷基酯;例如,(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸正癸酯、(甲基)丙烯酸正十二烷基酯、(甲基)丙烯酸十四烷基酯、(甲基)丙烯酸月桂基酯、(甲基)丙烯酸油烯基酯、(甲基)丙烯酸棕榈基酯和(甲基)丙烯酸十八烷基酯;其他(甲基)丙烯酸酯,诸如(甲基)丙烯酸异冰片酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸苯酯、(甲基)丙烯酸2-溴乙酯、(甲基)丙烯酸2-苯乙基酯和(甲基)丙烯酸1-萘酯、(甲基)丙烯酸烷氧基烷基酯,诸如(甲基)丙烯酸乙氧基乙酯、烯键式不饱和二羧酸、三羧酸和酸酐的单烷基酯、二烷基酯和三烷基酯,诸如马来酸乙酯、富马酸二甲酯、乌头酸三甲酯和衣康酸乙酯;羧酸官能单体,诸如(甲基)丙烯酸、衣康酸、富马酸和马来酸,以及羧酸官能单体的酰氯衍生物,诸如(甲基)丙烯酰氯。烯键式不饱和单体还可包括磷酸酯-、次膦酸酯-或亚膦酸酯官能单体,例如(甲基)丙烯酸2-磷酸乙酯。烯键式不饱和单体还可为多烯键式不饱和单体。多烯键式不饱和单体的实例包括(甲基)丙烯酸烯丙酯、三丙二醇二(甲基)丙烯酸酯、二甘醇二(甲基)丙烯酸酯、乙二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、1,3-丁二醇二(甲基)丙烯酸酯、聚亚烷基二醇二(甲基)丙烯酸酯、邻苯二甲酸二烯丙酯、三羟甲基丙烷三(甲基)丙烯酸酯、二乙烯基苯、二乙烯基甲苯、三乙烯基苯和二乙烯基萘。在一些实施例中,烯键式不饱和单体包括(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己基酯、丙烯腈、乙酸乙烯酯、丙烯醛、丁二烯、苯乙烯和氯丁二烯中的至少一者。
聚合抑制剂在单体制造过程中单独使用或组合使用。在共混(即,混合)罐中,抑制剂溶解于合适的工艺溶剂或单体自身中。抑制剂以1重量%至50重量%的浓度溶解(取决于溶解度)以形成浓缩物。然后将浓缩物加入工艺流中以提供10ppm至10000ppm的最终使用浓度。
聚合抑制剂被分别装入混合罐中。因此,多种抑制剂可能需要多次添加。抑制剂以细粉、薄片、锭剂、小球或液体形式提供。在处理和添加固体形式以制造工艺流时,利用气动输送、螺杆式和台式加料器、螺旋输送机、回转阀或其他机械装置。利用这些装置可导致抑制剂磨耗、结块和团聚(clumping)。抑制剂也可能在其原始包装或储仓过程中结块和团聚。这些操作问题是生产效率下降的潜在原因。另外,将抑制剂装入混合***可能需要工人处理,这可能导致暴露于抑制剂化学品的潜在有害的化学效应下。呈细粉形式的抑制剂可能存在粉尘***危险。
因此,需要具有改进处理特性的聚合抑制剂,即不易发生产品磨耗、分解、结块或团聚的抑制剂。另外,在单一丸粒中提供抑制剂的组合而不是必须分别处理和添加到工艺流中,将简化单体生产和存储操作。
聚合抑制剂的实例包括吩噻嗪(PTZ)及其衍生物、二羟基苯(例如,氢醌(HQ)、间苯二酚、邻苯二酚)及其衍生物(例如,氢醌单甲醚(MEHQ)、叔丁基氢醌(TBHQ)、对苯醌(PBQ)、丁基化羟基茴香醚(BHA)、丁基化羟基甲苯(BHT)、叔丁基邻苯二酚(TBC))。其他聚合抑制剂包括二丁基二硫代氨基甲酸金属盐(例如,二丁基二硫代氨基甲酸铜、锰或银)、硝酰自由基(例如,TEMPO、4-羟基TEMPO、4-乙酰氨基TEMPO)、芳香族胺(例如,苯二胺、丁基二苯胺、辛基二苯胺、苯基-α-甲基萘胺)、羟胺(例如,二乙基羟胺)、亚硝胺(例如,对亚硝基酚)和受阻酚。羟胺和受阻酚如之前段落所详述。在一些实施例中,聚合抑制剂包括吩噻嗪、吩噻嗪衍生物、氢醌、氢醌单甲醚(MEHQ)和叔丁基邻苯二酚(TBC)中的至少一者。在一些实施例中,聚合抑制剂包括吩噻嗪(PTZ)。
本发明的另一方面是提供端封闭丸粒,其中芯包含至少一种金属萃取剂。
在一些实施例中,除稳定剂之外,芯还包含稀释剂聚合物。该稀释剂聚合物与外层中的聚合物相同或不同。在一些实施例中,除聚合物之外,外层还包含至少一种稳定剂。外层的至少一种稳定剂可与芯的至少一种稳定剂相同或不同。
一种用于生产树脂母料组合物的方法包括:共挤出呈管状形式的由外层封装的芯材料以形成填充的管,其中该芯材料包含至少一种添加剂,并且该外层包含聚合物;将该填充的管送入密封装置中,该密封装置将填充的管切割成多个不连续段密封件并且同时密封每个不连续段的每一端,从而形成端封闭丸粒;以及冷却该端封闭丸粒。该方法在下面的实例1中予以更详细地描述,其中包括对图6中示出的挤出头以及用于共挤出芯材料和外层的描述。在一些实施例中,至少两个填充的管同时挤出、切割、密封并且用同一装置冷却以形成至少两个端封闭丸粒的工艺流。
树脂母料组合物可有利地用于稳定多种有机材料。因此,稳定化的组合物由待稳定化的有机材料和树脂母料组合物制备。在一些实施例中,有机材料包括聚合物、涂料、模塑制品、纤维、纺织物、膜、烯属不饱和单体、蜡、有机化合物、照相胶片、纸张、化妆品、有机染料或油墨。涂料的实例包括溶剂型涂料、水性涂料和粉末涂料。
在一些实施例中,有机材料为聚合物。聚合物的实例包括聚烯烃、聚酯、聚醚、聚酮、聚酰胺、天然和合成的橡胶、聚氨酯、聚苯乙烯、高抗冲击聚苯乙烯、聚丙烯酸酯、聚甲基丙烯酸酯、聚缩醛、聚丙烯腈、聚丁二烯、聚苯乙烯、丙烯腈-丁二烯-苯乙烯三聚物、苯乙烯丙烯腈共聚物、丙烯酸酯-苯乙烯-丙烯腈三聚物、纤维素乙酸丁酸酯、纤维素聚合物、聚酰亚胺、聚酰胺酰亚胺、聚醚酰亚胺、聚苯硫醚、聚苯醚、聚砜、聚醚砜、聚氯乙烯、聚碳酸酯、热塑性烯烃、氨基树脂交联的聚丙烯酸酯和聚酯、多异氰酸酯交联的聚酯和聚丙烯酸酯、苯酚/甲醛、脲/甲醛和三聚氰胺/甲醛树脂、干燥和非干燥的醇酸树脂、醇酸树脂、聚酯树脂、用三聚氰胺树脂交联的丙烯酸酯树脂、脲树脂、异氰酸酯、异氰脲酸酯、氨基甲酸酯、环氧树脂、衍生自脂肪族、脂环族、杂环和芳香族的缩水甘油基化合物的交联的环氧树脂(用酸酐或胺交联得到)、聚硅氧烷、迈克尔加成聚合物、胺、具有活化的不饱和且亚甲基的化合物的封闭胺、具有活化的不饱和且亚甲基的化合物的酮亚胺、与不饱和的丙烯酸聚乙酰乙酸酯树脂组合的聚酮亚胺、与不饱和的丙烯酸树脂组合的聚酮亚胺、辐射可固化组合物、环氧三聚氰胺树脂、以及包含前述聚合物中的至少一者的组合。
在一些实施例中,该聚合物为聚烯烃。该聚烯烃可为:i)选自聚丙烯、聚异丁烯、聚丁-1-烯、聚-4-甲基戊-1-烯的单烯烃的聚合物;ii)选自聚异戊二烯或聚丁二烯的二烯;iii)选自环戊烯和降冰片烯的环烯烃的聚合物;iv)任选地选自交联的聚乙烯、高密度聚乙烯(HDPE)、高密度和高分子量聚乙烯(HDPE-HMW)、高密度和超高分子量聚乙烯(HDPE-UHMW)、中密度聚乙烯(MDPE)、低密度聚乙烯(LDPE)、线性低密度聚乙烯(LLDPE)、非常低密度聚乙烯(VLDPE)和超低密度聚乙烯(ULDPE)的聚乙烯;v)它们的共聚物;或vi)包含前述聚烯烃中的至少一者的混合物。
基于稳定剂组合物的总重量计,该稳定化的组合物包含从0.001重量%至75重量%的稳定剂。在该范围内,基于稳定化的组合物的总重量计,该稳定化的组合物可包含从0.01重量%至65重量%、从0.01重量%至50重量%、从0.01重量%至25重量%、从0.01重量%至15重量%、从0.05重量%至10重量%、或从0.05重量%至5重量%的稳定剂。
除待稳定化的有机材料和树脂母料组合物之外,该稳定化的组合物还可包含常规添加剂,这些添加剂包括但不限于金属减活化剂、硝酮、内酯、共稳定剂、成核剂、澄清剂、中和剂、金属硬脂酸盐、金属氧化物、水滑石、填充剂和增强剂、增塑剂、润滑剂、乳化剂、颜料、流变添加剂、催化剂、均化剂、光学增亮剂、阻燃剂、抗静电剂和发泡剂。
树脂母料组合物可用于提供稳定化的组合物。稳定化的组合物继而可用于各种制品中,包括但不限于汽车部件、土工膜、农用膜和太阳能电池板。土工膜的实例包括池塘衬垫、地面覆盖物、垫层、防水层、侵蚀控制膜等。稳定化的组合物还可用于可获益于热和/或紫外线稳定的任何其他制品。
本发明的另一方面是一种用于生产制品的方法,该方法包括将树脂母料组合物与聚合物熔融混合以形成稳定化的组合物;以及模塑该稳定化的组合物以形成该模塑制品。熔融混合可在捏合设备诸如单螺杆或双螺杆挤出机、班布里混合机或热轧辊中完成。模塑可为注塑、滚塑、吹塑、卷对卷模塑(reel-to-reel molding)、金属注塑、压缩模塑、传递模塑、浸渍模塑、气辅模塑、***注塑、微模塑(micro molding)、反应注塑和二次注塑。
本发明至少包括以下实施例。
实施例1.一种作为端封闭丸粒提供的树脂母料组合物,该端封闭丸粒包括芯和封装所述芯的外层,其中该芯包含至少一种添加剂,并且该外层包含聚合物,其特征在于该外层的厚度为从0.001mm至1cm。
实施例2.如实施例1所述的树脂母料组合物,其中该至少一种添加剂包括稳定剂。
实施例3.如实施例2所述的树脂母料组合物,其中该稳定剂包括受阻胺光稳定剂(HALS)、有机亚磷酸酯或亚膦酸酯、受阻酚、色烷、紫外线(UV)吸收剂、受阻苯甲酸酯、羟胺、氧化叔胺和自由基聚合抑制剂中的至少一者。
实施例4.如实施例2所述的树脂母料组合物,其中该稳定剂包括2,2,6,6-四甲基-4-哌啶醇与C12-21饱和脂肪酸和C18不饱和脂肪酸的酯。
实施例5.如实施例2所述的树脂母料组合物,其中该稳定剂包括吩噻嗪、吩噻嗪衍生物、氢醌和氢醌单甲醚(MEHQ)中的至少一者。
实施例6.如实施例1-5中任一项所述的树脂母料组合物,其中该聚合物为热塑性聚合物。
实施例7.如实施例6所述的树脂母料组合物,其中该热塑性聚合物包括以下项中的至少一种:聚烯烃,聚酯,聚醚,聚酮,聚酰胺,天然橡胶和合成橡胶,聚氨酯,聚苯乙烯,高抗冲击聚苯乙烯,聚丙烯酸酯,聚甲基丙烯酸酯,聚缩醛,聚丙烯腈,聚丁二烯,丙烯腈-丁二烯-苯乙烯三聚物,苯乙烯-丙烯腈共聚物,丙烯酸酯-苯乙烯-丙烯腈三聚物,纤维素乙酸丁酸酯,纤维素聚合物,聚酰亚胺,聚酰胺酰亚胺,聚醚酰亚胺,聚苯硫醚,聚苯醚,聚砜,聚醚砜,聚氯乙烯,聚碳酸酯,和乙烯-乙酸乙烯酯共聚物。
实施例8.如实施例6所述的树脂母料组合物,其中该热塑性聚合物包括聚乙烯、聚丙烯、聚丙烯共聚物、聚苯乙烯和苯乙烯-丙烯腈共聚物中的至少一者。
实施例9.如实施例6-8中任一项所述的树脂母料组合物,其中该芯还包含与该外层中的热塑性聚合物相同或不同的热塑性聚合物稀释剂。
实施例10.如实施例1-9中任一项所述的树脂母料组合物,其中该外层包含至少一种稳定剂。
实施例11.一种稳定化的组合物,该组合物由待稳定化的有机材料和如实施例1-10中任一项所述的树脂母料组合物制备。
实施例12.如实施例11所述的稳定化的组合物,其中该有机材料包括聚合物、涂料、模塑制品、纺织物、纤维、膜、烯属不饱和单体、蜡、有机化合物、照相胶片、纸张、化妆品、有机染料或油墨。
实施例13.如实施例1-10中任一项所述的树脂母料组合物用于提供稳定化的组合物的用途。
实施例14.一种用于生产如实施例1-10中任一项所述的树脂母料组合物的方法,该方法包括:共挤出呈管状形式的由外层封装的芯材料以形成填充的管,其中该芯材料包含至少一种添加剂,并且该外层包含聚合物;将该填充的管送入密封装置中,该密封装置将该填充的管切割成多个不连续段并且同时密封每个不连续段的每一端,从而形成端封闭丸粒;以及冷却该端封闭丸粒。
实施例15.如实施例14所述的方法,其中至少两个填充的管同时挤出、切割、密封并且用同一装置冷却以形成至少两个端封闭丸粒的工艺流。
实施例16.一种用于生产制品的方法,该方法包括将如实施例1-10中任一项所述的树脂母料组合物与聚合物熔融混合以形成稳定化的组合物;以及模塑该稳定化的组合物以形成该模塑制品。
实例.提供以下实例来帮助本领域的普通技术人员进一步理解某些实施例。这些实例旨在用于说明目的,不应被解释为限制本发明的范围。
实例1:用于制造封装的稳定剂(CEP)的方法。参考图6,其中示出了挤出头和形成根据本发明的端封闭丸粒的示意图。将作为聚合物(例如,聚丙烯、聚丙烯共聚物、聚乙烯或苯乙烯-丙烯腈共聚物)提供的外层装入挤出机(挤出头1的外部;挤出头5的内部),通过用于聚合物的挤出机的连接部4装入,并且进入用于聚合物熔体的通道2中。使用泵送***或另一挤出机通过连接部3,将作为稳定剂(例如, UV-3853或吩噻嗪)的芯材料装入挤出头1的另一部分中。在共挤出工艺中,挤出头1形成聚合物管7,其同时在模头开口6处向管内填充芯材料。然后将填充的管导入用于密封和切割的封闭装置8中。然后在管的每一端(封闭端)同时密封填充的管,并且将其切割成多个不连续段以形成多个端封闭丸粒。然后通过由水喷雾嘴9递送的水冷却丸粒。然后对端封闭丸粒进行干燥和包装。图2示出根据本发明的示例性端封闭丸粒。图2A示出不同形式的吩噻嗪、粉末(左侧)、小球(配混到聚苯乙烯中,中间)和CEP(具有聚苯乙烯封装剂,右侧)。图2B示出不同尺寸的聚苯乙烯封装的吩噻嗪(CEP)。标尺以厘米为单位来标记。
实例2:使用封装的稳定剂(CEP)对加工后的聚合物中稳定剂的分散性的影响。下列实验设计用于展示封装的稳定剂在聚合物稳定中的作用,并研究使用封装的稳定剂(CEP)对加工后聚合物中稳定剂的分散性的任何不利影响。在该实验中,研究了封装的稳定剂(CEP)的两个不同样品以及一个圆柱形丸粒的对比样品,如表1所示。
设备和材料:所用的设备:Davis-Standard(Killion);树脂类型:聚丙烯树脂(Pro-fax 6301);温度特征曲线范围:205-230℃。
方法描述:将挤出机保持在所需的加工温度(205-230℃)下一小时后,打开制粒机、鼓风机和挤出机。将挤出机马达速度和制粒机速度同步(即,设定在大致相同的速度下),使得材料均匀地流过浴而进入制粒器。挤出机速度保持在65rpm。将以聚合物中浓度为0.25%的目标配制的树脂(具有圆柱形丸粒和CEP的形式的稳定剂)倒入挤出机的漏斗中。几分钟后,清洁的材料流出模头。从模头中出来的材料流入冰水中,其中发生股线硬化。将股线进料至制粒机中,将挤出机螺杆速度调节到合适的转速(65rpm),并且将来自制粒机装置的丸粒收集到塑料袋中。
通过GC/FID分析PP丸粒中的稳定剂量,并且结果如表1所示,表明用本发明的CEP技术实现了目标浓度,与圆柱形丸粒的对比样品一样,并且未观察到不利影响。
表1:聚丙烯中的稳定剂分散性
实例3:使用封装的稳定剂(CEP)对挤出机进料口跨接的影响。在该实验中,模拟挤出机进料口跨接以研究对稳定剂沉积物形成的影响。从表2和图3I可以看出,CEP材料未留下任何沉积物,而薄片材料和表层MB材料在挤出机螺杆上表现出沉积物(分别为图3C和3F),因此表明了使用CEP技术的明显优点。
设备:Davis-Standard(Killion);温度:料斗中为90-100℃;保持时间:1h(在旋转螺杆之前);样品量:50-100g;母料:UV-3853S(在LDPE中包含50%活性物质,薄片),UV-3853PP5(在PP中包含50%活性物质,圆柱形丸粒),UV-3853PPC(在PPC中包含70%活性物质,CEP)。
将三种材料、薄片、圆柱形丸粒和CEP分别并且以相同的方式装入料斗中,并且在90-100℃的料斗中保持1h。然后打开挤出机螺杆,并且对料斗或挤出机螺杆中的任何残余物的沉积分配下列等级。从表2和图3A-I中可以清楚地看出,仅CEP未留下任何沉积物并且表现最佳。
等级评定***:1-料斗、挤出机进料口和挤出机螺杆中没有沉积物;2-料斗、挤出机进料口和挤出机螺杆中有极少沉积物;3-料斗、挤出机进料口和挤出机螺杆中有一些沉积物;4-料斗、挤出机进料口和挤出机螺杆中有大量沉积物。结果在下表2中示出。
表2.挤出机进料口跨接
实例4:添加剂的附聚(团聚和粘连)的对比研究。本实验旨在评估稳定剂粉末(及其他形式)在高于环境温度的温度下存储和处理过程中的团聚、粘连和脆碎度。一些添加剂的熔点相当低(25-40℃),从而导致在夏季出现团聚和处理问题。因此,已经开发出一种测试方法来测量存储在高于室温的条件下(在40-60℃的范围内)的添加剂或母料丸粒(聚合物载体包含20-60%添加剂)的相对团聚、粘连、脆碎度和流动性。团聚是指添加剂颗粒或母料丸粒附聚或粘到一起。粘连是指添加剂丸粒附聚而导致流动性降低,并且脆碎度是指易于碎裂或粉碎的添加剂颗粒或丸粒。
程序:稳定剂量提供在下表3中。对于CEP和圆柱形丸粒,封装剂为聚丙烯(PP)。将50克各种样品置于250mL烧杯中,在粉末或丸粒的顶部放置稍小的广口瓶,然后将500克砝码放在该较小广口瓶的顶部以施加恒定的压力。将样品置于40℃、50℃或60℃的鼓风烘箱(Blue M Oven)中处理24小时。(在每次温度暴露时采用新鲜样品。)在2小时内冷却至室温。使用下列等级评定***对样品的团聚、粘连、脆碎度和流动性进行评价:
1级-自由流动
2级-有一些团块,但是易于破碎(易碎)
3级-有大量团块,通过努力可将其破碎(在一定程度上易碎)
4级-有大量团块,无法破碎
5级-熔凝固体
在50℃下获得的结果列于下表3中。
表3.附聚的对比研究
图4A示出样品1-3的照片结果,并且图4B示出对比样品10-12的照片结果。
实例5:评估运输过程中的脆碎度:摇动器测试(Red Devil摇动器,型号#5400)。设计测试针对现有技术材料形式(即MB和表层MB)来评估本发明的CEP稳定剂。当一些稳定剂或稳定剂共混物在运输和装运过程中可能变脆时就会发生问题,产生大量细粒,其对于最终用户来说可能无法接受。
按照下列方法测试样品。用样品填充16盎司配衡的开口玻璃瓶,这样使其充满1/3。(约140克丸粒。)小心操作以免将粉末加入广口瓶中。用适当的盖封闭广口瓶。将广口瓶置于Red Devil摇动器(型号#5400)上,并通过向上旋拧底座以牢固地拧紧夹具,确保样品瓶在摇动过程中不发生意外松动。将样品摇动5分钟。通过35目(线直径0.011英寸-开口0.0175英寸)的筛网将广口瓶的内容物排空到箔托盘上。“细粒”的重量是托盘中的粉末与烧杯中的残余粉末的总重量。
表4:运输过程中由脆碎引起的稳定剂损耗百分比
实例7.芯中的聚合物稀释剂。端封闭丸粒用 UV-3853S(由50重量%UV-3853和50重量%LDPE组成)作为芯并且用PP作为封装芯的外层来制备。芯和外层分别占CEP的总重量的60重量%和40重量%。因此,CEP的总体组合物为30重量%UV-3853、30重量%LDPE和40重量%PP。
实例8.封装芯的外层中的稳定剂。端封闭丸粒用 UV-3853(具有100%活性)作为芯并且用50重量% UV-3346和50重量%PP的混合物作为封装芯的外层来制备。芯和外层分别占CEP的总重量的60重量%和40重量%。因此,CEP的总组成为60重量%UV-3853、20重量%UV-3346和20重量%PP。
实例9.不同形式的吩噻嗪在苯乙烯中的溶解时间比较。溶解时间定义为将吩噻嗪(2重量%)以及聚苯乙烯载体(对于小球)或封装剂(对于CEP)完全溶解在苯乙烯中以形成均匀溶液所需的时间。结果汇总于下表中,并且表明CEP形式的噻吩嗪易溶于苯乙烯单体中,实现完全溶解,并且溶解速度与小球形式一样快。聚苯乙烯聚合物完全溶解于苯乙烯单体中,最大程度减小了对任何后续生产操作(包括蒸馏)的任何不利影响。
表5.评估在苯乙烯中的溶解时间
粉末 | 小球 | CEP | |
溶解时间(min) | 7 | 21 | 21 |
平均粒径(μm) | 350 | 1000 | 10000 |
实例10.比较不同形式的吩噻嗪的脆碎度和完整性。将吩噻嗪粉末、聚苯乙烯中小球和CEP(封装在聚苯乙烯)样品置于广口瓶中并且剧烈摇动。在刚刚加入样品之后目视评估样品中形成的粉尘,并且在剧烈摇动之后再次评估。结果汇总于下表6中,其中粉化程度表征为“无”、“轻微”或“中等”。
表6.评估粉尘形成
这些结果表明CEP形式的噻吩嗪具有优异的产品完整性,并且甚至比小球形式更不易产生粉末和粉尘。基于这些结果,预计CEP形式在加工设备中更不易结块/团聚或跨接/堵塞,使工人无需直接暴露于吩噻嗪,并且最大程度减小了任何粉尘***危险。
也可以单独和组合来制备其他单体稳定剂(即,抑制剂)的CEP。本文所披露的其他热塑性聚合物可用作封装剂以制备CEP。热塑性聚合物的选择部分地取决于其在抑制的单体或溶剂中的溶剂速率。
贯穿本申请已经提及不同的专利和/或科学文献参考。这些出版物的披露内容以其全文通过引用结合在此,如同在此写出一样。鉴于以上说明和实例,本领域的普通技术人员将能够实施所要求的披露而无需过度实验。
虽然上述说明已经显示、描述并指出本传授内容的基本新颖特征,但应当理解,本领域技术人员可以进行以如所说明的设备以及其用途的细节的形式的各种省略、替换和改变,而不脱离本传授内容的范围。因此,本传授内容的范围不应被局限于前述讨论,而应由所附的权利要求书限定。
Claims (16)
1.一种作为端封闭丸粒提供的树脂母料组合物,该端封闭丸粒包括芯和封装所述芯的外层,其中该芯包含至少一种添加剂,并且该外层包含聚合物,其特征在于该外层的厚度为从0.001mm至1cm。
2.如权利要求1所述的树脂母料组合物,其中该至少一种添加剂包括稳定剂。
3.如权利要求2所述的树脂母料组合物,其中该稳定剂包括受阻胺光稳定剂(HALS)、有机亚磷酸酯或亚膦酸酯、受阻酚、色烷、紫外线(UV)吸收剂、受阻苯甲酸酯、羟胺、氧化叔胺和自由基聚合抑制剂中的至少一者。
4.如权利要求2所述的树脂母料组合物,其中该稳定剂包括2,2,6,6-四甲基-4-哌啶醇与C12-21饱和脂肪酸和C18不饱和脂肪酸的酯。
5.如权利要求2所述的树脂母料组合物,其中该稳定剂包括吩噻嗪、吩噻嗪衍生物、氢醌、氢醌单甲醚(MEHQ)和叔丁基邻苯二酚(TBC)中的至少一者。
6.如权利要求1-5中任一项所述的树脂母料组合物,其中该聚合物为热塑性聚合物。
7.如权利要求6所述的树脂母料组合物,其中该热塑性聚合物包括以下项中的至少一种:聚烯烃,聚酯,聚醚,聚酮,聚酰胺,天然橡胶和合成橡胶,聚氨酯,聚苯乙烯,高-抗冲击聚苯乙烯,聚丙烯酸酯,聚甲基丙烯酸酯,聚缩醛,聚丙烯腈,聚丁二烯,丙烯腈-丁二烯-苯乙烯三聚物,苯乙烯-丙烯腈共聚物,丙烯酸酯-苯乙烯-丙烯腈三聚物,纤维素乙酸丁酸酯,纤维素聚合物,聚酰亚胺,聚酰胺酰亚胺,聚醚酰亚胺,聚苯硫醚,聚苯醚,聚砜,聚醚砜,聚氯乙烯,聚碳酸酯,和乙烯-乙酸乙烯酯共聚物。
8.如权利要求6所述的树脂母料组合物,该热塑性聚合物包括聚乙烯、聚丙烯、聚丙烯共聚物、聚苯乙烯和苯乙烯-丙烯腈共聚物中的至少一者。
9.如权利要求6-8中任一项所述的树脂母料组合物,其中该芯还包含与该外层中的该热塑性聚合物相同或不同的热塑性聚合物稀释剂。
10.如权利要求1-9中任一项所述的树脂母料组合物,其中该外层包含至少一种稳定剂。
11.一种稳定化的组合物,该组合物由待稳定化的有机材料和如权利要求1-10中任一项所述的树脂母料组合物制备。
12.如权利要求11所述的稳定化的组合物,其中该有机材料包括聚合物、涂料、模塑制品、纺织物、纤维、膜、烯属不饱和单体、蜡、有机化合物、照相胶片、纸张、化妆品、有机染料或油墨。
13.如权利要求1-10中任一项所述的树脂母料组合物用于提供稳定化的组合物的用途。
14.一种用于生产如权利要求1-10中任一项所述的树脂母料组合物的方法,该方法包括:
共挤出呈管状形式的由外层封装的芯材料以形成填充的管,其中该芯材料包含至少一种添加剂,并且该外层包含聚合物;
将该填充的管送入密封装置中,该密封装置将该填充的管切割成多个不连续段并且同时密封每个不连续段的每一端,从而形成端封闭丸粒;以及
冷却该端封闭丸粒。
15.如权利要求14所述的方法,其中至少两个填充的管同时挤出、切割、密封并且用同一装置冷却以形成至少两个端封闭丸粒的工艺流。
16.一种用于生产制品的方法,该方法包括将如权利要求1-10中任一项所述的树脂母料组合物与聚合物熔融混合以形成稳定化的组合物;以及模塑该稳定化的组合物以形成该模塑制品。
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MX2018001168A (es) | 2018-07-06 |
SA518390842B1 (ar) | 2021-06-28 |
BR112018001961B1 (pt) | 2022-04-26 |
JP6872048B2 (ja) | 2021-05-19 |
JP2020062892A (ja) | 2020-04-23 |
KR20180036742A (ko) | 2018-04-09 |
JP2018523731A (ja) | 2018-08-23 |
RU2679252C1 (ru) | 2019-02-06 |
US20220048218A1 (en) | 2022-02-17 |
US20180222087A1 (en) | 2018-08-09 |
EP3328929B1 (en) | 2019-04-17 |
JP6850791B2 (ja) | 2021-03-31 |
PT3328929T (pt) | 2019-07-16 |
TR201910378T4 (tr) | 2019-08-21 |
ES2735148T3 (es) | 2019-12-16 |
US10974417B2 (en) | 2021-04-13 |
CA2993973C (en) | 2021-06-22 |
ZA201800568B (en) | 2023-07-26 |
BR112018001961A2 (pt) | 2019-05-14 |
EP3328929A1 (en) | 2018-06-06 |
PL3328929T3 (pl) | 2019-09-30 |
CN115627027A (zh) | 2023-01-20 |
WO2017023755A1 (en) | 2017-02-09 |
KR102641063B1 (ko) | 2024-02-27 |
CA2993973A1 (en) | 2017-02-09 |
HUE044832T2 (hu) | 2019-11-28 |
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