CN113597416A - 成型人造聚合物制品 - Google Patents
成型人造聚合物制品 Download PDFInfo
- Publication number
- CN113597416A CN113597416A CN202080019641.5A CN202080019641A CN113597416A CN 113597416 A CN113597416 A CN 113597416A CN 202080019641 A CN202080019641 A CN 202080019641A CN 113597416 A CN113597416 A CN 113597416A
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- China
- Prior art keywords
- metal oxide
- microspheres
- polymer
- tert
- butyl
- Prior art date
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- 229920001059 synthetic polymer Polymers 0.000 title claims description 12
- 229920000642 polymer Polymers 0.000 claims abstract description 129
- 239000004005 microsphere Substances 0.000 claims abstract description 101
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 86
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 86
- 238000000034 method Methods 0.000 claims abstract description 56
- 239000006185 dispersion Substances 0.000 claims abstract description 25
- 239000002077 nanosphere Substances 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 10
- 239000004611 light stabiliser Substances 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 63
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 45
- 239000011148 porous material Substances 0.000 claims description 35
- 239000006096 absorbing agent Substances 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 14
- 229920001194 natural rubber Polymers 0.000 claims description 12
- 229920003052 natural elastomer Polymers 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 150000001412 amines Chemical class 0.000 claims description 9
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- 150000001565 benzotriazoles Chemical class 0.000 claims description 8
- 239000000835 fiber Substances 0.000 claims description 8
- HJIAMFHSAAEUKR-UHFFFAOYSA-N (2-hydroxyphenyl)-phenylmethanone Chemical class OC1=CC=CC=C1C(=O)C1=CC=CC=C1 HJIAMFHSAAEUKR-UHFFFAOYSA-N 0.000 claims description 7
- HTTGVORJOBRXRJ-UHFFFAOYSA-N 2-(triazin-4-yl)phenol Chemical class OC1=CC=CC=C1C1=CC=NN=N1 HTTGVORJOBRXRJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 150000001558 benzoic acid derivatives Chemical class 0.000 claims description 5
- FTWUXYZHDFCGSV-UHFFFAOYSA-N n,n'-diphenyloxamide Chemical class C=1C=CC=CC=1NC(=O)C(=O)NC1=CC=CC=C1 FTWUXYZHDFCGSV-UHFFFAOYSA-N 0.000 claims description 5
- WBYWAXJHAXSJNI-UHFFFAOYSA-N cinnamic acid Chemical class OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 claims description 4
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 3
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- 229910000423 chromium oxide Inorganic materials 0.000 claims description 3
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
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- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 6
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Abstract
多孔金属氧化物微球作为用于成型人造聚合物制品的光稳定剂的用途,其中多孔金属氧化物微球通过如下方法制备,所述方法包括形成聚合物纳米粒子和金属氧化物的液体分散体;形成所述分散体的液滴;干燥所述液滴以提供包含聚合物纳米球的聚合物模板微球;和从模板微球中除去聚合物纳米球以提供多孔金属氧化物微球。
Description
本发明涉及特定的多孔金属氧化物球(例如微球)作为用于成型人造聚合物制品的光稳定剂的用途,以及相应的成型人造聚合物制品和相应的经挤出、浇铸、纺丝、模塑或压延的聚合物组合物。
现已发现某些多孔金属氧化物球对于稳定聚合物以防降解(特别是UV光引起的降解)特别有效。此外,已经发现,在与其它UV吸收剂的组合中,这些显示出关于这种稳定化的协同效应。
本发明尤其涉及多孔金属氧化物球作为用于成型人造聚合物制品的光稳定剂的用途,其中聚合物为合成聚合物和/或天然或合成弹性体且多孔金属氧化物球包含金属氧化物且例如通过如下方法制备,所述方法包括形成聚合物粒子(例如纳米粒子)和金属氧化物的液体分散体;形成所述分散体的液滴;干燥所述液滴以提供包含聚合物球(例如纳米球)和金属氧化物的聚合物模板球(例如微球);和从模板微球中除去聚合物球以提供多孔金属氧化物球,并且其中所述球具有例如0.5μm至100μm的平均直径、0.10至0.80的平均孔隙率和50nm至999nm的平均孔径。
附图简述
在附图中作为实例而非作为限制图示本文中描述的公开内容。为了图示的简单和清楚起见,图中所示的要素不一定按比例绘制。例如,为清楚起见一些要素的尺寸可能相对于其它要素放大。此外,当认为适当时,附图标记在附图之间重复以指示相应或类似的元件。
图1显示根据本发明的一个实施方案的用于制备多孔微球的一般概述。
图2是根据本发明的一个实施方案的聚合物模板微球的扫描电子显微镜(SEM)图像。
图3是根据本发明的一个实施方案的多孔二氧化硅微球的SEM图像。
图4是根据本发明的某些实施方案的喷雾干燥法的图示。
图5至12显示作为所示应用实施例的UV测量结果的透射曲线。
详述
本多孔金属氧化物球或光子球(photonic balls)可使用聚合牺牲模板制备。在一个实施方案中,制备含有聚合物粒子和金属氧化物的水性胶体分散体,聚合物粒子通常是纳米级的。例如能够在微流体装置内将水性胶体分散体与连续油相混合,以产生油包水乳液。制备乳液水性液滴,收集并干燥以形成含有聚合物粒子和金属氧化物的球(通常是微米级)。然后例如通过煅烧除去聚合物粒子(球),以提供含有高孔隙度和孔隙(通常是纳米级)的球形金属氧化物粒子(球)。所述球可含有均一孔径,这是聚合物粒子为球形和单分散的结果。
图1显示用于制备多孔微球的一般概述。将含有聚合物纳米球和金属氧化物的乳液液滴干燥以除去溶剂,以提供含有聚合物纳米球和在聚合物纳米球之间的间隙空间中的金属氧化物的组装微球(模板微球或“直接结构(direct structure)”)。聚合物纳米球划定间隙空间。煅烧导致除去聚合物,以提供具有高孔隙率或空隙体积的金属氧化物微球(反向结构(inverse structure))。
有利地,烧结多孔金属氧化物球,以产生热和机械稳定的连续固体结构。
在某些实施方案中,在微流体装置内进行液滴形成和收集。微流体装置是例如具有连接到收集储器的适合产生均一尺寸液滴的微米级液滴接头(junction)的窄通道装置。微流体装置例如含有具有大约10μm至大约100μm的通道宽度的液滴接头。该装置例如由聚二甲基硅氧烷(PDMS)制成并可例如通过软光刻法制备。可通过将水性分散相和油连续相以指定速率泵入该装置并在此发生混合以提供乳液液滴而在该装置内制备乳液。或者,可以使用水包油乳液。
在某些实施方案中,可以使用振动喷嘴技术。在这些技术中,制备液体分散体,形成液滴并投入连续相的浴中。然后将液滴干燥,接着除去聚合物。振动喷嘴设备可获自Büchi并包含例如注射器泵和脉动单元。振动喷嘴设备也可包含调压阀。
聚合物粒子例如具有大约50nm至大约999nm的平均直径并且是单分散的。
适用于所述球的模板聚合物包括热塑性聚合物。例如,模板聚合物选自聚(甲基)丙烯酸、聚(甲基)丙烯酸酯、聚苯乙烯类、聚丙烯酰胺、聚乙烯醇、聚乙酸乙烯酯、聚酯、聚氨酯、聚乙烯、聚丙烯、聚乳酸、聚丙烯腈、聚乙烯基醚、它们的衍生物、它们的盐、它们的共聚物及它们的组合。例如,聚合物选自聚甲基丙烯酸甲酯、聚甲基丙烯酸乙酯、聚(甲基丙烯酸正丁酯)、聚苯乙烯、聚(氯-苯乙烯)、聚(α-甲基苯乙烯)、聚(N-羟甲基丙烯酰胺)、苯乙烯/甲基丙烯酸甲酯共聚物、聚烷基化丙烯酸酯、聚羟基丙烯酸酯、聚氨基丙烯酸酯、聚氰基丙烯酸酯、聚氟化丙烯酸酯、聚(N-羟甲基丙烯酰胺)、聚丙烯酸、聚甲基丙烯酸、甲基丙烯酸甲酯/丙烯酸乙酯/丙烯酸共聚物、苯乙烯/甲基丙烯酸甲酯/丙烯酸共聚物、聚乙酸乙烯酯、聚乙烯基吡咯烷酮、聚乙烯基己内酯、聚乙烯基己内酰胺、它们的衍生物、它们的盐及它们的组合。
在某些实施方案中,聚合物模板包括聚苯乙烯类,包括聚苯乙烯和聚苯乙烯共聚物。聚苯乙烯共聚物包括具有水溶性单体的共聚物,例如聚苯乙烯/丙烯酸、聚苯乙烯/聚(乙二醇)甲基丙烯酸酯和聚苯乙烯/苯乙烯磺酸酯。
本金属氧化物包括过渡金属、类金属和稀土元素的氧化物,例如二氧化硅、二氧化钛、氧化铝、氧化锆、二氧化铈、铁氧化物、氧化锌、氧化铟、氧化锡、氧化铬、混合金属氧化物、它们的组合等。优选选自二氧化硅、二氧化钛、氧化铝及其组合的金属氧化物。
聚合物粒子与金属氧化物的wt/wt(重量/重量)比为例如0.1/1至10.0/1或0.5/1至10.0/1。
连续油相包含例如有机溶剂、硅油或氟化油。根据本发明,“油”是指与水不混溶的有机相。有机溶剂包括烃,例如庚烷、己烷、甲苯、二甲苯等,以及烷醇,如甲醇、乙醇、丙醇等。
将乳液液滴收集,干燥并除去聚合物。例如通过微波辐射、在热炉中、在真空下、在干燥剂存在下或其组合进行干燥。
可以例如通过煅烧、热解或用溶剂(溶剂脱除)进行聚合物脱除。煅烧在某些实施方案中在至少大约200℃、至少大约500℃、至少大约1000℃、大约200℃至大约1200℃或大约200℃至大约700℃的温度下进行。煅烧可持续合适的时间,例如大约0.1小时至大约12小时或大约1小时至大约8.0小时。在另某些实施方案中,煅烧可持续至少大约0.1小时、至少大约1小时、至少大约5小时或至少大约10小时。
或者,用油分散相和连续水相形成包含聚合物粒子和金属氧化物的液体分散体以形成水包油乳液。可如水性液滴那样收集和干燥油液滴。
或者,制备聚合物粒子(例如纳米例子)和金属氧化物的液体分散体并喷雾干燥以形成聚合物模板球(例如微球),而不形成液体-液体乳液。在喷雾干燥技术的某些实施方案中,将液体溶液或分散体进给(例如泵送)到与压缩气体入口关联的雾化喷嘴。将进料泵过雾化喷嘴以形成液滴。液滴在蒸发室中被预热气体包围,以致溶剂蒸发产生固体粒子。干燥的粒子被干燥气体携带经过旋风分离器并沉积在收集室中。气体包括氮气和/或空气。在喷雾干燥法的一个实施方案中,液体进料含有水或油相、聚合物粒子和金属氧化物。在喷雾干燥法的一个实施方案中,液体进料含有水或油相、聚合物粒子和任选金属氧化物。提供含有聚合物球和在聚合物球之间的间隙空间中的金属氧化物的聚合物模板球。聚合物球划定间隙空间。喷雾干燥技术包括喷墨喷雾干燥方法和设备。
在喷雾干燥技术中,空气可被视为连续相,具有分散的液相(液体-气体乳液)。在某些实施方案中,喷雾干燥包括大约100℃、大约105℃、大约110℃、大约115℃、大约120℃、大约130℃、大约140℃、大约150℃、大约160℃或大约170℃的任一个至大约180℃、大约190℃、大约200℃、大约210℃、大约215℃或大约220℃的任一个的入口温度。在某些实施方案中,使用大约1mL/min、大约2mL/min、大约5mL/min、大约6mL/min、大约8mL/min、大约10mL/min、大约12mL/min、大约14mL/min或大约16mL/min的任一个至大约18mL/min、大约20mL/min、大约22mL/min、大约24mL/min、大约26mL/min、大约28mL/min或大约30mL/min的任一个的泵速率(进料流量)。喷雾干燥技术公开在例如US2016/0170091中。
图4是根据本发明的某些实施方案的喷雾干燥法的图示。
在某些实施方案中,所述球是球形或类球形的,并且是微米级的,例如具有大约0.5微米(μm)至大约100μm的平均直径。用作模板的聚合物粒子也是球形的,在某些实施方案中是纳米级并且单分散的,具有例如大约50nm至大约999nm的平均直径。所用金属氧化物也可以是粒子形式,所述粒子可以是纳米级的。
分散体的金属氧化物可作为金属氧化物提供或可由金属氧化物前体例如通过溶胶-凝胶技术提供。
聚合物/金属氧化物液滴的干燥和接着聚合物的脱除提供具有均一空隙(孔隙)的球。一般而言,在本方法中,各液滴提供单个球。孔径取决于聚合物粒子的粒度。在聚合物脱除时可能发生一定的“收缩”或压实,以提供略小于原始聚合物粒度,例如比聚合物粒度小大约10%至大约40%的孔尺寸。如同聚合物粒子形状和粒度,孔径均一。
孔径在某些实施方案中可为大约50nm至大约999nm。
本金属氧化物球的平均孔隙率可相对较高。球的平均孔隙率是指作为整个球的体积的分数的总孔隙体积。平均孔隙率可被称为“体积分数”。
在某些实施方案中,多孔球可具有实心核(中心),其中孔隙率通常靠近球的外表面。在其它实施方案中,多孔球可具有空心核,其中孔隙率大部分靠近球的内部。在另某些实施方案中,孔隙率可遍布球体积。在其它实施方案中,孔隙率可作为梯度存在,较高孔隙率趋向球的外表面且较低孔隙率或无孔隙率(实心)趋向中心;或较低孔隙率趋向外表面且较高或完全孔隙率(空心)趋向中心。
对于任何多孔球,平均球直径优选大于平均孔径,例如,平均球直径为平均孔径的至少大约25倍、至少大约30倍、至少大约35倍或至少大约40倍。
在某些实施方案中,平均球直径与平均孔径的比率为例如大约40/1、大约50/1、大约60/1、大约70/1、大约80/1、大约90/1、大约100/1、大约110/1、大约120/1、大约130/1、大约140/1、大约150/1、大约160/1、大约170/1、大约180/1或大约190/1的任一个至大约200/1、大约210/1、大约220/1、大约230/1、大约240/1、大约250/1、大约260/1、大约270/1、大约280/1、大约290/1、大约300/1、大约310/1、大约320/1、大约330/1、大约340/1或大约350/1的任一个。
包含单分散聚合物球的聚合物模板球可在除去聚合物时提供具有通常类似孔径的孔隙的金属氧化物球。
球(例如微球)的平均直径可为0.5μm至100μm,或1μm至75μm或4.5μm至9.9μm。
球(例如微球)的平均孔隙率可以是0.10至0.90,或0.10至0.80或0.45至0.65。
球(例如微球)的平均孔径可以是50nm至999nm、50nm至800nm和220nm至300nm。
某些实施方案涉及多孔微球,其中所述微球具有0.5μm至100μm的平均直径、0.10至0.90或0.10至0.80的平均孔隙率和50nm至999nm的平均孔径。
其它实施方案涉及平均直径为1μm至75μm、平均孔隙率为0.45至0.65且平均孔径为50nm至800nm的多孔金属氧化物微球。
其它实施方案涉及平均直径为4.5μm至9.9μm、平均孔隙率为0.45至0.65且平均孔径为220nm至300nm的多孔金属氧化物微球。
不希望受制于理论,但相信,当孔隙率和/或球直径和/或孔径在一定范围内时,球的成批样品表现出吸收。
多孔球主要包含金属氧化物,即它们可基本由或由金属氧化物组成。基于微球的重量,微球中金属氧化物的量可为例如50重量%至99.9重量%。某些实施方案具有60重量%或70重量%或90重量%或95重量%的下限。
有利地,多孔球(例如微球)也可以是单分散的。
根据本发明,粒度与粒径同义并且例如通过扫描电子显微术(SEM)或透射电子显微术(TEM)测定。平均粒度与D50同义,其是指粒子数的一半位于该点以上,一半在其以下。粒度是指初级粒子。粒度可通过激光散射技术用分散体或干粉末测量。
使用汞孔隙率分析表征微球的孔隙率。汞孔隙率法向浸没在汞中的样品施加受控压力。施加外部压力以使汞渗入该材料的空隙/孔隙。侵入空隙/孔隙所需的压力量与空隙/孔隙的尺寸成反比。压汞仪由该仪器生成的压力vs侵入数据使用Washburn方程生成体积和孔尺寸分布。例如,含有平均尺寸为165nm的空隙/孔隙的多孔二氧化硅微球具有0.8的平均孔隙率。
术语“成批样品”是指一群球。例如,微球的成批样品简单地为成批的一群微球,例如≥0.1mg、≥0.2mg、≥0.3mg、≥0.4mg、≥0.5mg、≥0.7mg、≥1.0mg、≥2.5mg、≥5.0mg、≥10.0mg或≥25.0mg。球的成批样品可基本不含其它组分。术语“多孔球”或“多孔微球”可以是指成批样品。
术语“…的…”可以是指“包含…”,例如“…的液体分散体”可被解释为“包含…的液体分散体”。
本文中提到的术语“微球”、“纳米球”、“液滴”等可以是指例如多个它们、它们的集合、它们的群体、它们的样品或它们的成批样品。
术语“微米”或“微米级”是指大约0.5μm至大约999μm。术语“纳米”或“纳米级”是指大约1nm至大约999nm。
术语“球”和“粒子”可互换。
关于球群体或球的术语“单分散”是指具有大致均一的形状和大致均一的直径的粒子。单分散微球或纳米球群体例如可有按数量计90%、91%、92%、93%、94%、95%、96%、97%、98%或99%的粒子具有在该群体的平均直径的±7%、±6%、±5%、±4%、±3%、±2%或±1%内的直径。
聚合物球的单分散群体的脱除提供具有相应的孔隙群的多孔金属氧化物球,所述孔具有平均孔径。
术语“基本不含其它组分”是指例如含有按重量计≤5%、≤4%、≤3%、≤2%、≤1%或≤0.5%的其它组分。
冠词“a”和“an”在本文中是指一个或多于一个(例如至少一个)语法对象。本文中引用的任何范围都包括端点。通篇所用的术语“大约”用于描述和虑及小波动。例如,“大约”可以是指数值可被±5%、±4%、±3%、±2%、±1%、±0.5%、±0.4%、±0.3%、±0.2%、±0.1%或±0.05%修饰。被术语“大约”修饰的数值包括该具体指定值。例如“大约5.0”包括5.0。
除非另行指明,所有份数和百分比按重量计。如果没有另行指明,重量%(wt%)基于整个组合物计。
本发明的非限制性的实施方案组涉及制备多孔金属氧化物球的方法,包括:
在第一实施方案中,公开了一种制备包含金属氧化物的多孔金属氧化物微球的方法,所述方法包括形成聚合物纳米粒子和金属氧化物的液体分散体;形成所述分散体的液滴;干燥所述液滴以提供包含聚合物纳米球和金属氧化物的聚合物模板微球;和从模板微球中除去聚合物纳米球以提供多孔金属氧化物微球。
在第二实施方案中,根据第一实施方案的方法,其包括形成聚合物纳米粒子和金属氧化物的液体分散体,喷雾干燥所述液体分散体以提供聚合物模板微球和从模板微球中除去聚合物纳米球。
在第三实施方案中,根据第一实施方案的方法,其包括用振动喷嘴形成液滴。在第四实施方案中,根据实施方案1至3的方法,其中所述液滴是水性液滴。在第五实施方案中,根据实施方案1至3的方法,其中所述液滴是油液滴。
在第六实施方案中,根据实施方案1的方法,其包括提供连续相和将所述液体分散体与所述连续相混合以形成含有分散的液体分散体液滴的乳液。在第七实施方案中,根据实施方案6的方法,其包括提供连续油相和将水分散体与连续油相混合以形成含有水性液滴的油包水乳液。在第八实施方案中,根据实施方案6的方法,其包括提供连续水相和将油分散体与连续相混合以形成含有油液滴的水包油乳液。
在第九实施方案中,根据实施方案6至8的方法,其包括收集所述液滴。在第十实施方案中,根据实施方案9的方法,其包括干燥所述液滴以提供包含聚合物纳米球和金属氧化物的聚合物模板微球和从模板微球中除去聚合物纳米球。
在第十一实施方案中,根据实施方案6至10的方法,其中液滴干燥包括微波辐照、烘炉干燥、在真空下干燥、在干燥剂存在下干燥或其组合。
在第十二实施方案中,根据实施方案7至11的方法,其中所述油相或分散体包含烃、硅油或氟化油。在第十三实施方案中,根据实施方案6至12的方法,其中在微流体装置中进行液滴形成。在第十四实施方案中,根据实施方案6至13的方法,其中在微流体装置中进行液滴形成,所述微流体装置含有具有大约10μm、大约15μm、大约20μm、大约25μm、大约30μm、大约35μm、大约40μm或大约45μm的任一个至大约50μm、大约55μm、大约60μm、大约65μm、大约70μm、大约75μm、大约80μm、大约85μm、大约90μm、大约95μm或大约100μm的任一个的通道宽度的液滴接头。优选10μm至100μm的通道宽度。在第十五实施方案中,根据实施方案13或14的方法,其包括从微流体装置中收集所述液滴。
在第十六实施方案中,根据前述实施方案任一项的方法,其中聚合物粒子与金属氧化物的wt/wt比为大约0.1/1、大约0.5/1、大约1.0/1、大约1.5/1、大约2.0/1、大约2.5/1或大约3.0/1的任一个至大约3.5/1、大约4.0/1、大约5.0/1、大约5.5/1、大约6.0/1、大约6.5/1、大约7.0/1、大约8.0/1、大约9.0/1或大约10.0/1的任一个。优选0.1/1至10/1的比。
在第十七实施方案中,根据前述实施方案任一项的方法,其中所述聚合物纳米粒子具有大约50nm、大约75nm、大约100nm、大约130nm、大约160nm、大约190nm、大约210nm、大约240nm、大约270nm、大约300nm、大约330nm、大约360nm、大约390nm、大约410nm、大约440nm、大约470nm、大约500nm、大约530nm、大约560nm、大约590nm或大约620nm的任一个至大约650nm、大约680nm、大约710nm、大约740nm、大约770nm、大约800nm、大约830nm、大约860nm、大约890nm、大约910nm、大约940nm、大约970nm或大约990nm的任一个的平均直径。
在第十八实施方案中,根据前述实施方案任一项的方法,其中所述聚合物选自聚(甲基)丙烯酸、聚(甲基)丙烯酸酯、聚苯乙烯、聚丙烯酰胺、聚乙烯、聚丙烯、聚乳酸、聚丙烯腈、它们的衍生物、它们的盐、它们的共聚物及它们的组合。
在第十九实施方案中,根据前述实施方案任一项的方法,其中所述聚合物选自聚苯乙烯,例如聚苯乙烯共聚物,如聚苯乙烯/丙烯酸、聚苯乙烯/聚(乙二醇)甲基丙烯酸酯或聚苯乙烯/苯乙烯磺酸酯。在第二十实施方案中,根据前述实施方案任一项的方法,其中所述金属氧化物是二氧化硅、二氧化钛、氧化铝、氧化锆、二氧化铈、铁氧化物、氧化锌、氧化铟、氧化锡或氧化铬的一种或多种。
在第二十一实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球具有大约0.5μm至大约100μm的平均直径、大约0.10至大约0.90或大约0.10至大约0.80的平均孔隙率和大约50nm至大约999nm的平均孔径。
在第二十二实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球具有大约1μm至大约75μm、大约2μm至大约70μm、大约3μm至大约65μm、大约4μm至大约60μm、大约5μm至大约55μm或大约5μm至大约50μm;例如大约5μm、大约6μm、大约7μm、大约8μm、大约9μm、大约10μm、大约11μm、大约12μm、大约13μm、大约14μm或大约15μm的任一个至大约16μm、大约17μm、大约18μm、大约19μm、大约20μm、大约21μm、大约22μm、大约23μm、大约24μm或大约25μm的任一个的平均直径。
在第二十三实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球具有大约0.10、大约0.12、大约0.14、大约0.16、大约0.18、大约0.20、大约0.22、大约0.24、大约0.26、大约0.28、大约0.30、大约0.32、大约0.34、大约0.36、大约0.38、大约0.40、大约0.42、大约0.44、大约0.46、大约0.48大约0.50、大约0.52、大约0.54、大约0.56、大约0.58或大约0.60的任一个至大约0.62、大约0.64、大约0.66、大约0.68、大约0.70、大约0.72、大约0.74、大约0.76、大约0.78、大约0.80或大约0.90的任一个的平均孔隙率。
在第二十四实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球具有大约50nm、大约60nm、大约70nm、80nm、大约100nm、大约120nm、大约140nm、大约160nm、大约180nm、大约200nm、大约220nm、大约240nm、大约260nm、大约280nm、大约300nm、大约320nm、大约340nm、大约360nm、大约380nm、大约400nm、大约420nm或大约440nm的任一个至大约460nm、大约480nm、大约500nm、大约520nm、大约540nm、大约560nm、大约580nm、大约600nm、大约620nm、大约640nm、大约660nm、大约680nm、大约700nm、大约720nm、大约740nm、大约760nm、大约780nm或大约800nm的任一个的平均孔径。
在第二十五实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球具有大约4.5μm、大约4.8μm、大约5.1μm、大约5.4μm、大约5.7μm、大约6.0μm、大约6.3μm、大约6.6μm、大约6.9μm、大约7.2μm或大约7.5μm的任一个至大约7.8μm、大约8.1μm、大约8.4μm、大约8.7μm、大约9.0μm、大约9.3μm、大约9.6μm或大约9.9μm的任一个的平均直径。
在第二十六实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球具有大约0.45、大约0.47、大约0.49、大约0.51、大约0.53、大约0.55或大约0.57的任一个至大约0.59、大约0.61、大约0.63或大约0.65的任一个的平均孔隙率。
在第二十七实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球具有大约220nm、大约225nm、大约230nm、大约235nm、大约240nm、大约245nm或大约250nm的任一个至大约255nm、大约260nm、大约265nm、大约270nm、大约275nm、大约280nm、大约285nm、大约290nm、大约295nm或大约300nm的任一个的平均孔径。
在第二十八实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球具有大约4.5μm、大约4.8μm、大约5.1μm、大约5.4μm、大约5.7μm、大约6.0μm、大约6.3μm、大约6.6μm、大约6.9μm、大约7.2μm或大约7.5μm的任一个至大约7.8μm、大约8.1μm、大约8.4μm、大约8.7μm、大约9.0μm、大约9.3μm、大约9.6μm或大约9.9μm的任一个的平均直径;大约0.45、大约0.47、大约0.49、大约0.51、大约0.53、大约0.55或大约0.57的任一个至大约0.59、大约0.61、大约0.63或大约0.65的任一个的平均孔隙率;和大约220nm、大约225nm、大约230nm、大约235nm、大约240nm、大约245nm或大约250nm的任一个至大约255nm、大约260nm、大约265nm、大约270nm、大约275nm、大约280nm、大约285nm、大约290nm、大约295nm或大约300nm的任一个的平均孔径。
在第二十九实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球包含基于微球的总重量计大约60.0重量%至大约99.9重量%金属氧化物,例如包含大约60.0重量%、大约64.0重量%、大约67.0重量%、大约70.0重量%、大约73.0重量%、大约76.0重量%、大约79.0重量%、大约82.0重量%或大约85.0重量%的任一个至大约88.0重量%、大约91.0重量%、大约94.0重量%、大约97.0重量%、大约98.0重量%、大约99.0重量%或大约99.9重量%的任一个的金属氧化物。
在第三十实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球包含基于微球的总重量计大约0.1重量%至大约40.0重量%的一种或多种光吸收剂,例如包含大约0.1重量%、大约0.3重量%、大约0.5重量%、大约0.7重量%、大约0.9重量%、大约1.0重量%、大约1.5重量%、大约2.0重量%、大约2.5重量%、大约5.0重量%、大约7.5重量%、大约10.0重量%、大约13.0重量%、大约17.0重量%、大约20.0重量%或大约22.0重量%的任一个至大约24.0重量%、大约27.0重量%、大约29.0重量%、大约31.0重量%、大约33.0重量%、大约35.0重量%、大约37.0重量%、大约39.0重量%或大约40.0重量%的任一个的一种或多种光吸收剂。
在第三十一实施方案中,根据前述实施方案任一项的方法,其中所述多孔微球是单分散的。在第三十二实施方案中,根据前述实施方案中任一项的方法,其中所述多孔金属氧化物微球为微球的成批样品。
在第三十三实施方案中,根据前述实施方案任一项的方法,其中从模板微球中除去聚合物纳米球包括煅烧、热解或溶剂脱除。
在第三十四实施方案中,根据前述实施方案任一项的方法,其中除去聚合物纳米球包括在大约200℃、大约350℃、大约400℃、450℃、大约500℃或大约550℃的任一个至大约600℃、大约650℃、大约700℃或大约1200℃的任一个的温度下煅烧模板微球大约0.1h(小时)、1h、大约1.5h、大约2.0h、大约2.5h、大约3.0h、大约3.5h或大约4.0h的任一个至大约4.5h、大约5.0h、大约5.5h、大约6.0h、大约6.5h、大约7.0h、大约7.5h大约8.0h或大约12h的任一个的时间。或者,所述煅烧可在至少大约200℃、至少大约500℃或至少大约1000℃的温度下持续例如至少大约0.1小时、至少大约1小时、至少大约5小时或至少大约10小时的合适时间。
多孔金属氧化物球优选以基于成型人造聚合物制品的重量为0.01重量%至40.0重量%,或0.01重量%至20.0重量%的浓度使用。其它范围包括0.1重量%至20.0重量%,或0.1重量%至10.0重量%的浓度,或0.25重量%至10.0重量%,或0.5重量%至10.0重量%的浓度。
多孔金属氧化物微球可与一种或多种UV吸收剂组合使用,所述UV吸收剂选自2-羟基苯基三嗪类、苯并三唑类、2-羟基二苯甲酮类、N,N'-二苯基乙二酰胺类、肉桂酸酯类和苯甲酸酯类。
基于成型人造聚合物制品的重量,一种或多种UV吸收剂优选以0.01重量%至40.0重量%,尤其0.01重量%至20.0重量%的浓度使用。更优选的浓度为0.1重量%至20.0重量%,尤其是0.1重量%至10.0重量%。
与多孔金属氧化物微球组合的苯并三唑优选为式(Ia)的那些:
L1为二价基团,例如-(CH2)n-,其中n为1-8;
T2为氢、C1-C18烷基或被COOT5、C1-C18烷氧基、羟基、苯基或C2-C18酰氧基取代的C1-C18烷基;
T3为氢、卤素、C1-C18烷基、C1-C18烷氧基、C2-C18酰氧基、1-12个碳原子的全氟烷基如-CF3,或T3为苯基;
与多孔金属氧化物微球组合的2-羟基二苯甲酮优选为式(Ib)的那些:
其中
G1、G2和G3独立地为氢、羟基或C1-C18烷氧基。
与多孔金属氧化物微球组合的N,N'-二苯基乙二酰胺优选为式(Ic)的那些:
其中
G4、G5、G6和G7独立地为氢、C1-C12烷基或C1-C12烷氧基。
其实例是下面列表中给出的相应的UV吸收剂。
与多孔金属氧化物微球组合的肉桂酸酯优选为通式(Id)的那些:
其中
m为1-4的整数;
G15为氢或苯基;
如果m是1,G16为COO-G19;
如果m是2,G16为C2-C12链烷-二氧羰基;
如果m是3,G16为C3-C12链烷-三氧羰基;
如果m是4,G16为C4-C12链烷-四氧羰基;
G17为氢、CN或为COO-G19;
G18为氢或甲氧基;和
G19为C1-C18烷基。
与多孔金属氧化物微球组合的苯甲酸酯优选为式(Ie)的那些:
其中
k为1或2;
当k为1时,G20为C1-C18烷基、苯基或被C1-C12烷基取代的苯基,且G21为氢;
G22和G24独立地为氢或C1-C8烷基;和
G23为氢或羟基。
这类苯甲酸酯的实例是下面列表中给出的相应的UV吸收剂。
与多孔金属氧化物微球组合的2-羟基苯基三嗪优选为式(If)的那些:
其中
G8为C1-C18烷基或被COO或OCO或O间隔或者被O间隔且被OH取代的C4-C18烷基;
G9、G10、G11和G12独立地为氢、甲基、羟基或OG8;
或式(Ig)的那些:
其中R为C1-C12烷基、(CH2-CH2-O-)n-R2;-CH2-CH(OH)-CH2-O-R2;或-CH(R3)-CO-O-R4;n为0或1;R2为C1-C13烷基或C2-C20链烯基或C6-C12芳基或CO-C1-C18烷基;R3为H或C1-C8烷基;和R4为C1-C12烷基或C2-C12链烯基或C5-C6环烷基。
在所给定义的范围内,包括R2、R3或R4,烷基为例如支化或未支化的烷基,如甲基、乙基、丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基、2-乙基丁基、正戊基、异戊基、1-甲基戊基、1,3-二甲基丁基、正己基、1-甲基己基、正庚基、异庚基、1,1,3,3-四甲基丁基、1-甲基庚基、3-甲基庚基、正辛基、2-乙基己基、1,1,3-三甲基己基、1,1,3,3-四甲基戊基、壬基、癸基、十一烷基、1-甲基十一烷基、十二烷基、1,1,3,3,5,5-六甲基己基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基。
被一个以上O间隔的烷基是,例如聚氧化烯如聚乙二醇残基。
芳基通常是芳族烃基,例如苯基、联苯基或萘基。
在定义链烯基的上下文中,特别包括乙烯基、烯丙基、异丙烯基、2-丁烯基、3-丁烯基、异丁烯基、正戊-2,4-二烯基、3-甲基-丁-2-烯基、正辛-2-烯基、正十二-2-烯基、异十二烯基、正十二-2-烯基、正十八-4-烯基。
卤素主要是氟、氯、溴或碘,尤其是氯。
C5-C6环烷基主要是环戊基、环己基。
C2-C18酰氧基是,例如,烷酰氧基、苯甲酰氧基或链烯酰氧基如丙烯酰氧基或甲基丙烯酰氧基。
二价C2-C12链烷-二氧羰基的实例是-COO-CH2CH2-OCO-;
三价C3-C12链烷-三氧羰基的实例是-COO-CH2–CH(OCO-)CH2-OCO-;
四价C4-C12链烷-四氧羰基的实例是(-COO-CH2)4C。
优选地,用于与多孔金属氧化物微球组合的一种或多种UV吸收剂包含一种或多种选自(i)至(lv)的化合物:
i.2-(3',5'-二叔丁基-2'-羟基苯基)-5-氯苯并三唑,
ii.2-(3',5'-二叔戊基-2'-羟基苯基)苯并三唑,
iii.2-(3',5'-双(α,α-二甲基苄基)-2'-羟基苯基)苯并三唑,
iv.2-(3'-叔丁基-2'-羟基-5'-(2-辛氧基羰基乙基)苯基)苯并三唑,
v.2,2'-亚甲基-双[4-(1,1,3,3-四甲基丁基)-6-苯并三唑-2-基苯酚],
vi.2-[3'-叔丁基-5'-(2-甲氧基羰基乙基)-2'-羟基苯基]-2H-苯并三唑与聚乙二醇300的酯交换产物,
vii.2-[2'-羟基-3'-(α,α-二甲基苄基)-5'-(1,1,3,3-四甲基丁基)苯基]苯并三唑,
viii.5-三氟甲基-2-(2-羟基-3-α-异丙苯基-5-叔辛基苯基)-2H-苯并三唑,
ix.2-(2'-羟基-5'-(2-羟乙基)苯基)苯并三唑,
x.2-(2'-羟基-5'-(2-甲基丙烯酰氧基乙基)苯基)苯并三唑,
xi.2,4-双(2,4-二甲基苯基)-6-(2-羟基-4-烷氧基苯基)-1,3,5-三嗪,其中烷基是C8烷基的混合物(CAS号137759-38-7;85099-51-0;85099-50-9);
xii.2,4-双(2,4-二甲基苯基)-6-(2-羟基-4-辛氧基苯基)-1,3,5-三嗪(CAS号2725-22-6),
xiii.2,4-二苯基-6-(2-羟基-4-[α-乙基己酰氧基乙基]苯基)-1,3,5-三嗪,
xiv.2,4-双(2-羟基-4-丁氧基苯基)-6-(2,4-双丁氧基苯基)-1,3,5-三嗪,
xv.2,4,6-三(2-羟基-4-[1-乙氧基羰基乙氧基]苯基)-1,3,5-三嗪,
xvi.三(2,4-二羟基苯基)-1,3,5-三嗪与α-氯丙酯的混合物(由C7-C9醇的异构体混合物制得)的反应产物,
xvii.2-[4-(十二烷氧基/十三烷氧基-2-羟基丙氧基)-2-羟基苯基]-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪,
xviii.2-{2-羟基-4-[3-(2-乙基己基-1-氧基)-2-羟基丙氧基]苯基}-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪,
xix.2-(2-羟基-4-己氧基苯基)-4,6-二苯基-1,3,5-三嗪,
xx.2-(3'-叔丁基-5'-甲基-2'-羟基苯基)-5-氯-苯并三唑,
xxi.2-(3'-仲丁基-5'-叔丁基-2'-羟基苯基)-苯并三唑,
xxii.2-(3',5'-二叔丁基-2'-羟基苯基)-苯并三唑,
xxiii.2-(5'-叔辛基-2'-羟苯基)-苯并三唑,
xxiv.2-(3'-十二烷基-5'-甲基-2'-羟苯基)-苯并三唑,
xxv.2-(3'-叔丁基-5'-(2-辛氧基羰基乙基)-2'-羟基苯基)-5-氯-苯并三唑,
xxvi.2-(5'-甲基-2'-羟基苯基)-苯并三唑,
xxvii.2-(5'-叔丁基-2'-羟苯基)-苯并三唑,
xxxii.2-乙基己基-对甲氧基肉桂酸酯(CAS号5466-77-3),
xxxiii.2,4-二羟基二苯甲酮,
xxxiv.2-羟基-4-甲氧基二苯甲酮,
xxxv.2-羟基-4-十二烷氧基二苯甲酮,
xxxvi.2-羟基-4-辛氧基二苯甲酮,
xxxvii.2,2'-二羟基-4-甲氧基二苯甲酮,
xlvi.
lvi.十二烷二酸1,12-双[2-[4-(4,6-二苯基-1,3,5-三嗪-2-基)-3-羟基苯氧基]乙基]酯(CAS号1482217-03-7)
在一个实施方案中,优选UV吸收剂i-xx和xlvi。
在一个具体实施方案中,优选UV吸收剂i-iv、vi-xi、xiii-xviii、xx、xxiii-xxxix、xlvi;特别是ii、iii、iv、vi、vii、viii、xx、xxv、xxxvii、xlvi。
在另一实施方案中、优选i-x、xii、xiii、xix-xxiii、xxv-xxvii、xxx-xxxvi、xl-xlv和xlvi,特别是i、ii、iii、v、vi、viii、xii、xiii、xix、xx、xxii、xxiii、xxvi、xxx、xxxi、xxxiv、xxxvi、xl、xli、xlii、xliii、xliv、xlv、xlvi。
高度优选的2-羟基苯基三嗪是xii、xlviii和xlvi。
优选2-羟基苯基三嗪类、苯并三唑类、2-羟基二苯甲酮类和苯甲酸酯类,特别是2-羟基苯基三嗪类、苯并三唑类和2-羟基二苯甲酮类。更优选苯并三唑类和2-羟基二苯甲酮类,尤其是苯并三唑类。
用于成型人造聚合物制品的合成聚合物或天然或合成弹性体的具体实例为:
1.单烯烃和二烯烃的聚合物,例如聚丙烯、聚异丁烯、聚丁-1-烯、聚-4-甲基戊-1-烯、聚乙烯基环己烷、聚异戊二烯或聚丁二烯、聚己烯、聚辛烯,以及环烯烃如环戊烯、环己烯、环辛烯或降冰片烯的聚合物,聚乙烯(其任选可为交联的),例如高密度聚乙烯(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)、(VLDPE)和(ULDPE)。
聚烯烃,即前面段落中例举的单烯烃聚合物,优选聚乙烯和聚丙烯,可以通过不同方法制备,尤其通过下列方法制备:
a)自由基聚合(通常在高压和升高的温度下)。
b)使用通常含有一种或一种以上周期表第IVb、Vb、VIb或VIII族金属的催化剂的催化聚合。这些金属通常具有一个或一个以上配体,通常是可为π-或σ-配位的氧化物、卤化物、醇化物、酯、醚、胺、烷基、链烯基和/或芳基。这些金属配合物可为游离形式或固定在基材上,通常在活化氯化镁、氯化钛(III)、氧化铝或氧化硅上。这些催化剂可溶于或不溶于聚合介质中。所述催化剂本身可用于聚合或者可使用其他活化剂,通常为烷基金属、金属氢化物、金属烷基卤化物、金属烷基氧化物或金属烷基氧烷(alkyloxane),其中所述金属为周期表第Ia、IIa和/或IIIa族的元素。所述活化剂可方便地用其他酯、醚、胺或甲硅烷基醚基团改性。这些催化剂体系通常称为Philips、Standard Oil Indiana、齐格勒(-纳塔)、TNZ(杜邦)、茂金属或单中心催化剂(SSC)。
2.1)下提及的聚合物的混合物,例如聚丙烯与聚异丁烯、聚丙烯与聚乙烯的混合物(例如PP/HDPE、PP/LDPE)以及不同种类聚乙烯的混合物(例如LDPE/HDPE)。
3.单烯烃和二烯烃相互之间或与其他乙烯基单体的共聚物,例如乙烯/丙烯共聚物,线性低密度聚乙烯(LLDPE)及其与低密度聚乙烯(LDPE)的混合物,极低密度聚乙烯,丙烯/丁-1-烯共聚物,丙烯/异丁烯共聚物,乙烯/丁-1-烯共聚物,乙烯/己烯共聚物,乙烯/甲基戊烯共聚物,乙烯/庚烯共聚物,乙烯/辛烯共聚物,乙烯/乙烯基环己烷共聚物,乙烯/环烯烃共聚物(例如乙烯/降冰片烯,例如COC),乙烯/1-烯烃共聚物,其中1-烯烃原位产生,丙烯/丁二烯共聚物,异丁烯/异戊二烯共聚物,乙烯/乙烯基环己烯共聚物,乙烯/丙烯酸烷基酯共聚物,乙烯/甲基丙烯酸烷基酯共聚物,乙烯/乙酸乙烯酯共聚物或乙烯/丙烯酸共聚物及其盐(离聚物)以及乙烯与丙烯和二烯如己二烯、二环戊二烯或亚乙基-降冰片烯的三元共聚物,和这些共聚物相互之间及与上述1)下提及聚合物的混合物,例如聚丙烯/乙烯-丙烯共聚物、LDPE/乙烯-乙酸乙烯酯共聚物(EVA)、LDPE/乙烯-丙烯酸共聚物(EAA)、LLDPE/EVA、LLDPE/EAA和交替或无规聚烯烃/一氧化碳共聚物及其与其他聚合物如聚酰胺的混合物。
4.烃树脂(例如C5-C9),包括其氢化改性物(例如增粘剂)以及聚烯烃和淀粉的混合物。
来自1.)-4.)的均聚物和共聚物可以具有任何立体结构,包括间规、等规、半等规或无规立构;其中优选无规立构聚合物。还包括立构嵌段聚合物。来自1.)-4.)的共聚物可为无规或嵌段共聚物、均相或非均相或高结晶度均聚物。
5.聚苯乙烯、聚(对甲基苯乙烯)、聚(α-甲基苯乙烯)。
6.衍生于乙烯基芳族单体的芳族均聚物和共聚物,所述单体包括苯乙烯,α-甲基苯乙烯,乙烯基甲苯的所有异构体,尤其是对乙烯基甲苯,乙基苯乙烯、丙基苯乙烯、乙烯基联苯、乙烯基萘和乙烯基蒽的所有异构体及其混合物。均聚物和共聚物可具有任何立体结构,包括间规、等规、半等规或无规立构;其中优选无规立构聚合物。还包括立构嵌段聚合物。
6a.包括上述乙烯基芳族单体和选自乙烯、丙烯、二烯、腈、酸、马来酸酐、马来酰亚胺、乙酸乙烯酯和氯乙烯或丙烯酸衍生物及其混合物的共聚单体的共聚物,例如苯乙烯/丁二烯、苯乙烯/丙烯腈、苯乙烯/乙烯(共聚体)、苯乙烯/甲基丙烯酸烷基酯、苯乙烯/丁二烯/丙烯酸烷基酯、苯乙烯/丁二烯/甲基丙烯酸烷基酯、苯乙烯/马来酸酐、苯乙烯/丙烯腈/丙烯酸甲酯;高冲击强度的苯乙烯共聚物和其他聚合物如聚丙烯酸酯、二烯聚合物或乙烯/丙烯/二烯三元共聚物的混合物;苯乙烯的嵌段共聚物,例如苯乙烯/丁二烯/苯乙烯、苯乙烯/异戊二烯/苯乙烯、苯乙烯/异戊二烯/丁二烯/苯乙烯、苯乙烯/乙烯/丁烯/苯乙烯或苯乙烯/乙烯/丙烯/苯乙烯、HIPS、ABS、ASA、AES。
6b.衍生于6.)下所提到的聚合物的氢化的氢化芳族聚合物,尤其包括通过氢化无规立构聚苯乙烯得到的聚环己基乙烯(PCHE),也常称为聚乙烯基环己烷(PVCH)。
6c.衍生于6a.)下所提到的聚合物的氢化的氢化芳族聚合物。
均聚物和共聚物可以具有任何立体结构,包括间规、等规、半等规或无规立构;其中优选无规立构聚合物。还包括立构嵌段聚合物。
7.乙烯基芳族单体如苯乙烯或α-甲基苯乙烯的接枝共聚物,例如苯乙烯接枝聚丁二烯,苯乙烯接枝聚丁二烯-苯乙烯或聚丁二烯-丙烯腈共聚物;苯乙烯和丙烯腈(或甲基丙烯腈)接枝聚丁二烯;苯乙烯、丙烯腈和甲基丙烯酸甲酯接枝聚丁二烯;苯乙烯和马来酸酐接枝聚丁二烯;苯乙烯、丙烯腈和马来酸酐或马来酰亚胺接枝聚丁二烯;苯乙烯和马来酰亚胺接枝聚丁二烯;苯乙烯和丙烯酸烷基酯或甲基丙烯酸烷基酯接枝聚丁二烯;苯乙烯和丙烯腈接枝乙烯/丙烯/二烯三元共聚物;苯乙烯和丙烯腈接枝聚丙烯酸烷基酯或聚甲基丙烯酸烷基酯;苯乙烯和丙烯腈接枝丙烯酸酯/丁二烯共聚物,及其与6)下所列共聚物的混合物,例如称作ABS、MBS、ASA或AES聚合物的共聚物混合物。
8.含卤素的聚合物,例如聚氯丁二烯、氯化橡胶,异丁烯-异戊二烯的氯化和溴化共聚物(卤代丁基橡胶),氯化或磺基氯化的聚乙烯,乙烯和氯化乙烯的共聚物,表氯醇均聚物和共聚物,尤其是含卤素的乙烯基化合物的聚合物,例如聚氯乙烯、聚偏二氯乙烯、聚氟乙烯,聚偏二氟乙烯,以及它们的共聚物,例如氯乙烯/偏二氯乙烯,氯乙烯/乙酸乙烯酯或偏二氯乙烯/乙酸乙烯酯共聚物。聚氯乙烯可为刚性或柔性(增塑)的。
9.衍生于α,β-不饱和酸及其衍生物的聚合物,例如聚丙烯酸酯和聚甲基丙烯酸酯;用丙烯酸丁酯冲击改性的聚甲基丙烯酸甲酯、聚丙烯酰胺和聚丙烯腈。
10.9)下所提到的单体相互之间或与其他不饱和单体的共聚物,例如丙烯腈/丁二烯共聚物、丙烯腈/丙烯酸烷基酯共聚物、丙烯腈/丙烯酸烷氧基烷基酯或丙烯腈/卤乙烯共聚物或丙烯腈/甲基丙烯酸烷基酯/丁二烯三元共聚物。
11.衍生于不饱和醇和胺或其酰基衍生物或缩醛的聚合物,例如聚乙烯醇、聚乙酸乙烯酯、聚硬脂酸乙烯酯、聚苯甲酸乙烯酯、聚马来酸乙烯酯、聚乙烯醇缩丁醛、聚邻苯二甲酸烯丙基酯或聚烯丙基蜜胺;以及它们与上面1)中所提到的烯烃的共聚物。
12.环醚的均聚物和共聚物,如聚亚烷基二醇、聚氧乙烯、聚氧丙烯或其与二缩水甘油基醚的共聚物。
13.聚缩醛如聚甲醛和含有氧化乙烯作为共聚单体的那些聚甲醛;用热塑性聚氨酯、丙烯酸酯或MBS改性的聚缩醛。
14.聚苯醚和聚苯硫醚,以及聚苯醚与苯乙烯聚合物或聚酰胺的混合物。
15.一方面衍生自羟基封端的聚醚、聚酯或聚丁二烯且另一方面衍生自脂族或芳族多异氰酸酯的聚氨酯及其前体。聚氨酯由以下的反应形成:(1)二异氰酸酯与短链二醇(扩链剂)和(2)二异氰酸酯与长链二醇(热塑性聚氨酯,TPU)。
16.衍生于二胺和二羧酸和/或衍生于氨基羧酸或相应内酰胺的聚酰胺和共聚酰胺,例如聚酰胺4,聚酰胺6,聚酰胺6/6、6/10、6/9、6/12、4/6、12/12,聚酰胺11,聚酰胺12,来源于间苯二甲胺和己二酸的芳族聚酰胺;由六亚甲基二胺和间苯二甲酸或/和对苯二甲酸制备的聚酰胺(含或不含作为改性剂的弹性体),例如聚对苯二甲酰2,4,4,-三甲基六亚甲基二胺或聚间苯二甲酰间苯二胺;还有上述聚酰胺与聚烯烃、烯烃共聚物、离聚物或化学键合或接枝弹性体的嵌段共聚物;或与聚醚如聚乙二醇、聚丙二醇或聚四亚甲基二醇的嵌段共聚物;以及用EPDM或ABS改性的聚酰胺或共聚酰胺;以及在加工过程中缩合的聚酰胺(RIM聚酰胺体系)。聚酰胺可为无定型的。
17.聚脲、聚酰亚胺、聚酰胺-酰亚胺、聚醚酰亚胺、聚酯酰亚胺、聚乙内酰脲类和聚苯并咪唑类。
18.衍生自二羧酸和二醇和/或衍生于羟基羧酸或相应内酯或交酯的聚酯,例如聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚-1,4-二羟甲基环己烷对苯二甲酸酯、聚对苯二甲酸丙二醇酯、聚萘二甲酸亚烷基二醇酯和聚羟基苯甲酸酯以及衍生于羟基封端的聚醚的共聚醚酯,还有用聚碳酸酯或MBS改性的聚酯。共聚酯例如可以包括但不限于聚琥珀酸丁二醇酯/对苯二甲酸丁二醇酯、聚己二酸丁二醇酯/对苯二甲酸丁二醇酯、聚己二酸四亚甲基二醇酯/对苯二甲酸四亚甲基二醇酯、聚琥珀酸丁二醇酯/己二酸丁二醇酯、聚琥珀酸丁二醇酯/碳酸丁二醇酯、聚-3-羟基丁酸酯/辛酸酯共聚物、聚-3-羟基丁酸酯/己酸酯/癸酸酯三元共聚物。此外,脂族聚酯例如可以包括但不限于聚(羟基链烷酸酯)类,尤其是聚丙内酯、聚丁内酯、聚新戊内酯、聚戊内酯和聚己内酯,聚琥珀酸乙二醇酯、聚琥珀酸丙二醇酯、聚琥珀酸丁二醇酯、聚琥珀酸六亚甲基二醇酯、聚己二酸乙二醇酯、聚己二酸丙二醇酯、聚己二酸丁二醇酯、聚己二酸六亚甲基二醇酯、聚草酸乙二醇酯、聚草酸丙二醇酯、聚草酸丁二醇酯、聚草酸六亚甲基二醇酯、聚癸二酸乙二醇酯、聚癸二酸丙二醇酯、聚癸二酸丁二醇酯、聚呋喃酸乙二醇酯和聚乳酸(PLA)以及用聚碳酸酯或MBS改性的对应聚酯。术语“聚乳酸(PLA)”表示优选聚-L-交酯的均聚物以及其与其他聚合物的共混物或掺合聚合物;乳酸或交酯与其他单体如羟基羧酸,例如乙醇酸、3-羟基丁酸、4-羟基丁酸、4-羟基戊酸、5-羟基戊酸、6-羟基己酸及其环状形式的共聚物;术语“乳酸”或“丙交酯”包括L-乳酸、D-乳酸、其混合物和二聚体,即L-交酯、D-交酯、内消旋交酯及其任何混合物。优选的聚酯为PET、PET-G、PBT。
19.聚碳酸酯和聚酯碳酸酯。聚碳酸酯优选通过双酚化合物与碳酸化合物(尤其是光气或在熔体酯交换方法中碳酸二苯酯或碳酸二甲酯)反应来制备。尤其优选基于双酚A的均聚碳酸酯和基于单体双酚A和1,1-双(4-羟苯基)-3,3,5-三甲基环己烷(双酚TMC)的共聚碳酸酯。可用于聚碳酸酯合成的这些和其他双酚及二醇化合物尤其公开于WO08037364(第7页第21行至第10页第5行)、EP1582549([0018]至[0034])、WO02026862(第2页第23行至第5页第15行)、WO05113639(第2页第1行至第7页第20行)中。聚碳酸酯可为直链或支化的。还可使用支化和非支化聚碳酸酯的混合物。适用于聚碳酸酯的支化剂由文献已知且描述于例如专利说明书US4185009和DE2500092(根据本发明的3,3-双-(4-羟基芳基)羟吲哚,在每种情况下参见整个文献)、DE4240313(参见第3页第33-55行)、DE19943642(参见第5页第25-34行)和US5367044中以及其中所引用的文献中。所用聚碳酸酯可额外地本质上支化,其中在聚碳酸酯制备的上下文中未在此加入支化剂。内在支化的实例为所谓的Fries结构,如EP1506249中对熔融聚碳酸酯所公开。链终止剂可额外用于聚碳酸酯制备中。酚如苯酚;烷基酚如甲酚和4-叔丁基苯酚、氯苯酚、溴苯酚、异丙苯基苯酚或其混合物优选用作链终止剂。聚酯碳酸酯通过已提及的双酚、至少一种芳族二羧酸与任选地碳酸等效物的反应获得。合适芳族二羧酸为例如邻苯二甲酸、对苯二甲酸、间苯二甲酸、3,3'-二苯基二甲酸或4,4'-二苯基二甲酸和苯甲酮二甲酸。聚碳酸酯中碳酸酯基团的至多80mol-%,优选20-50mol-%部分可经芳族二羧酸酯基团替换。
20.聚酮。
21.聚砜、聚醚砜和聚醚酮。
22.一方面衍生于醛和另一方面衍生于酚、脲和蜜胺类的交联聚合物,例如苯酚/甲醛树脂、脲/甲醛树脂和蜜胺/甲醛树脂。
23.干性和不干性醇酸树脂。
24.衍生于饱和和不饱和二羧酸与多元醇的共聚酯和作为交联剂的乙烯基化合物的不饱和聚酯树脂,以及具有低可燃性的其含卤素改性物。
25.衍生于取代丙烯酸酯的可交联丙烯酸系树脂,例如环氧丙烯酸酯、尿烷丙烯酸酯或聚酯丙烯酸酯。
26.用蜜胺树脂、脲树脂、异氰酸酯、异氰脲酸酯、多异氰酸酯或环氧树脂交联的醇酸树脂、聚酯树脂和丙烯酸酯树脂。
27.衍生于脂族、脂环族、杂环或芳族缩水甘油基化合物的交联环氧树脂,例如双酚A、双酚E和双酚F的二缩水甘油醚的产物,它们用常规硬化剂如酸酐或胺交联,使用或不使用促进剂。
28.天然聚合物如纤维素、橡胶、明胶及其化学改性的同系衍生物,例如乙酸纤维素、丙酸纤维素和丁酸纤维素,或纤维素醚如甲基纤维素;以及松香及其衍生物。
29.上述聚合物的共混物(高分子共混物),例如PP/EPDM,聚酰胺/EPDM或ABS,PVC/EVA,PVC/ABS,PVC/MBS,PC/ABS,PBTP/ABS,PC/ASA,PC/PBT,PVC/CPE,PVC/丙烯酸酯,POM/热塑性PUR,PC/热塑性PUR,POM/丙烯酸酯,POM/MBS,PPO/HIPS,PPO/PA 6.6和共聚物,PA/HDPE,PA/PP,PA/PPO,PBT/PC/ABS或PBT/PET/PC。
30.为纯单体化合物或该类化合物的混合物的天然存在和合成有机材料,例如矿物油、动物和植物脂肪、油和蜡或基于合成酯(例如邻苯二甲酸酯、己二酸酯、磷酸酯或偏苯三酸酯)的油、脂肪和蜡以及任何重量比的合成酯与矿物油的混合物,通常为用作纺丝组合物的那些和该类材料的水性乳液。
31.天然或合成橡胶的含水乳液,例如羧化苯乙烯/丁二烯共聚物的天然胶乳。
32.粘合剂,例如嵌段共聚物如SIS、SBS、SEBS、SEPS(S代表苯乙烯,I代表异戊二烯,B代表聚丁二烯,EB代表乙烯/丁烯嵌段,EP代表聚乙烯/聚丙烯嵌段)。
33.橡胶,例如共轭二烯的聚合物,例如聚丁二烯或聚异戊二烯;单烯烃和二烯烃与彼此或与其他乙烯基单体的共聚物;苯乙烯或a-甲基苯乙烯与二烯或与丙烯酸衍生物的共聚物;氯化橡胶;天然橡胶。
34.弹性体,例如天然聚异戊二烯(顺式-1,4-聚异戊二烯天然橡胶(NR)和反式-1,4-聚异戊二烯古塔波胶(gutta-percha)),合成聚异戊二烯(IR表示异戊二烯橡胶),聚丁二烯(BR表示丁二烯橡胶),氯丁二烯橡胶(CR),聚氯丁二烯,氯丁橡胶(Neoprene),氯丁橡胶(Baypren)等;丁基橡胶(异丁烯与异戊二烯的共聚物,IIR),卤化丁基橡胶(氯丁基橡胶:CIIR;溴丁基橡胶:BIIR),苯乙烯-丁二烯橡胶(苯乙烯与丁二烯的共聚物,SBR);腈橡胶(丁二烯与丙烯腈的共聚物,NBR),还称为Buna N橡胶;经氢化的腈橡胶(HNBR)Therban和Zetpol;EPM(乙烯丙烯橡胶,乙烯与丙烯的共聚物)和EPDM橡胶(乙烯丙烯二烯橡胶,乙烯、丙烯与二烯组分的三元共聚物),表氯醇橡胶(ECO),聚丙烯酸系橡胶(ACM、ABR),聚硅氧烷橡胶(SI、Q、VMQ),氟硅橡胶(FVMQ),氟弹性体(FKM和FEPM)Viton、Tecnoflon、Fluorel、Aflas和Dai-El,全氟弹性体(FFKM)TecnoflonPFR、Kalrez、Chemraz、Perlast,聚醚嵌段酰胺(PEBA),氯磺化聚乙烯(CSM)、(Hypalon),乙烯-乙酸乙烯酯(EVA),热塑弹性体(TPE),用于织物产生中的节枝弹性蛋白和弹性蛋白、聚硫橡胶、Elastolefin、弹性纤维。
35.热塑弹性体,例如苯乙烯类嵌段共聚物(TPE-s)、热塑性烯烃(TPE-o)、弹性合金(TPE-v或TPV)、热塑性聚氨酯(TPU)、热塑性共聚酯、热塑性聚酰胺、反应器TPO(R-TPO)、聚烯烃塑料(POP)、聚烯烃弹性体(POE)。
最优选热塑性聚合物,如聚烯烃及其共聚物。
本发明的成型人造聚合物制品例如通过以下加工步骤之一制备:
注射吹塑、挤出、吹塑、旋转模塑、模内装饰(背部注射)、中空模塑、注塑、共注塑、吹塑、成型、压缩模塑、树脂转印模塑、按压、薄膜挤出(流延膜;吹塑膜)、纤维纺丝(织造、非织造)、拉伸(单轴、双轴)、退火、深拉伸、压延、机械转变、烧结、共挤出、层合、交联(辐射、过氧化物、硅烷)、气相沉积、焊接、胶接、硫化、热成型、管挤塑、型材挤塑、压片挤塑;压片浇铸、捆扎、发泡、再循环/返工、减粘(过氧化物、热)、纤维熔喷、纺粘、表面处理(电晕放电、火焰、等离子体)、灭菌(通过γ射线、电子束)、胶带挤塑、拉挤、SMC加工或增塑溶胶。
本发明的另一实施方案是成型人造聚合物制品,其中聚合物是合成聚合物和/或天然或合成弹性体,并且其中聚合物包含本文所定义的多孔金属氧化物微球。对于这类制品,应适用本文给出的定义和优选情形。
优选成型人造聚合物制品为经挤出、浇铸、纺丝、模塑或压延的成型人造聚合物制品。
根据本发明的制品的实例为:
I-1)漂浮装置、航海用具、浮筒、浮标、甲板用塑料木材、防波堤、船、皮艇、桨和海滩加固物。
I-2)汽车用具、内部用具、外部用具,特别是饰板、保险杠、仪表板、电池、后和前衬板、在引擎盖下的模塑品部分、帽架、车厢衬板、车内衬板、气囊包、配件(照明)用的电子模塑品、仪表板用的窗格、头灯玻璃、仪器板、车外衬板、车内装饰、汽车照明、头灯、边灯、尾灯、停车灯、车内外装饰;门板;油箱;前侧装配玻璃;后车窗;椅背、外板、电线绝缘物、密封用轮廓挤出物、覆盖层、支柱机盖、底盘零件、排气系统、燃料过滤器/填料、燃油泵、燃料箱、车身模塑品、可折叠顶盖、车外后视镜、外部装饰、固着/固定装置、前端模件、玻璃、铰链、车锁系统、行李/车顶架、冲压/模压部件、密封物、防侧撞梁、隔音装置/隔热装置和天窗,门图案、控制面板、仪表面板、座椅、框架、表皮、汽车应用加固、汽车应用纤维加固、具有填充聚合物的汽车应用、具有未填充聚合物的汽车应用。
I-3)道路交通装置,特别是信号标识杆、路标、车辆配件、警告三角架、急救箱、安全帽、轮胎。
I-4)用于运输或公共运输的装置。飞机、铁道、机动车(汽车、摩托车)、卡车、轻卡车、公共汽车、有轨电车、自行车用装置,包括装饰。
I-5)太空应用的装置,特别是火箭和卫星,例如重返防护罩。
I-6)建筑与设计用装置、采矿用具、静音体系、街道安全岛和庇护所。
II-1)在常规电器/电子设备(个人电脑、电话、移动电话、打印机、电视机、影音装置)中的器具、箱子和罩盖、花盆、卫星TV碗和面板装置。
II-2)用于其它材料如钢或织物的护套。
II-3)电子工业用装置,特别是插头用绝缘材料,尤其是电脑插头、电和电子零件用的箱子、印制板和用于电子数据储存的材料如晶片、提款卡或信用卡。
II-4)电器用具,特别是洗衣机、滚筒、烘箱(微波炉)、洗碗机、混合器和熨斗。
II-5)灯(例如街灯、台灯)罩。
II-6)在电线和电缆中的应用(半导体、绝缘体和电缆护套)。
II-7)用于冷凝器、冰箱、加热装置、空气调节机、电子封装、半导体、咖啡机和真空清洁器的箔片。
III-1)科技制品,例如嵌齿轮(齿轮)、滑动配件、垫片、螺丝、螺栓、把手和按钮。
III-2)旋转叶片、通风机和风车轮叶、太阳能装置、壁橱、衣柜、隔墙板、墙板、折叠墙、屋顶、百叶窗(例如卷帘)、配件、管子之间的连接机构、套管和输送带。
III-3)卫生制品,特别是移动厕所、淋浴隔间、马桶坐圈、马桶盖和水槽。III-4)卫生用品,特别是尿布(婴儿、成人失禁用)、女性卫生制品、浴帘、浴刷、浴毡、浴盆、移动厕所、牙刷和便盆。
III-5)水、废水和化学品用管道(交叉结合或未交叉结合)、电线与电缆保护用管道、气体、油和污水用管道、排水沟、下流管和排水系统。
III-6)任何几何(窗格)、包层和板壁的型材。
III-7)玻璃代用品,特别是挤出板材、用于建筑物(整体、双壁或多壁)、飞机、学校的装配玻璃、用于建筑装配玻璃、火车、运输和卫生物品的窗膜。
III-8)板(墙壁、砧板)、筒仓、木材代替物、塑料木材、木材复合物、墙壁、表面、家具、装潢箔、地板覆盖材料(内用和外用)、地板、沟槽板道和瓷砖。
III-9)进口和出口支管。
III-10)水泥-、混凝土-、复合物应用和盖、板壁和覆盖层、扶手、栏杆、厨房工作台、屋顶、屋面薄面板、瓷砖和防水布。
IV-1)板(墙壁和砧板)、盘子、人造草皮、阿斯特罗特夫尼龙草皮(astroturf)、用于体育馆圆形场地(运动)的人造覆盖物、用于体育馆圆形场地(运动)的人造地板和胶带。
IV-2)织物连续和定长纤维(地毯/卫生用品/土工织物/单长丝;过滤器;纸巾/帘(遮光物)/医学应用)、散纤维(应用如睡衣/保护服装)、网、粗绳、电缆、绳、粗线、线、安全带、服装、内衣、手套;长靴;雨靴、贴身内衣、衣服、泳衣、运动装、伞(阳伞、遮阳伞)、降落伞、飞行伞、帆、“气球-丝”、露营用品、帐篷、空气床、日光床、太空包和袋。
IV-3)用于屋顶、土工膜、隧道、垃圾场、池塘、墙壁屋顶薄膜、土工膜、游泳池、泳池衬里、水池衬里、池塘衬里、窗帘(遮光物)/太阳防护罩、遮阳篷、遮篷、壁纸、食物包装和包封(柔韧和坚固的)、医用包装(柔性和坚固的)、安全气囊/安全带、臂-和头靠、地毯、中心控制台、仪表板、座舱、门、头顶控制台组件、车门板、汽车顶蓬、内部照明、内部后视镜、包裹架、后行李盖、座位、转向柱、方向盘、纺织物和车厢装饰的膜、保温材料和密封件。
V-1)薄膜(包装膜、硬质包装膜、垃圾膜、层压膜、打包包装纸、游泳池
用膜、垃圾袋、壁纸、拉伸薄膜、酒椰纤维(raffia)、脱盐膜、电池和连接器。
V-2)农业膜(温室覆盖物、信道、多重信道、微信道、“斜顶型温室(raspayamagado)”、多跨度、低行走信道、高信道、护根物、青贮料、筒仓袋、筒仓延伸段、熏蒸、气泡纸、索套(keder)、索拉包装(solawrap)、热捆绑包装、拉伸捆绑包装、苗圃、膜管),尤其是在农用化学品的密集型应用存在下;其他农业应用(例如非织造土壤罩盖)、网(由条带、多长丝及其组合制成)、防水布。该农业用膜可为单层结构或多层结构,通常由3、5或7个层制成。这可产生膜结构如A-B-A、A-B-C、A-B-C-B-A、A-B-C-B-D、A-B-C-D-C-B-A、A-A-B-C-B-A-A。A、B、C、D代表不同聚合物和增粘剂。然而,相邻层还可经偶联使得最终膜制品可由偶数层制成,即2、4或6个层,例如A-A-B-A、A-A-B-B、A-A-B-A-A、A-B-B-A-A、A-A-B-C-B、A-A-B-C-A-A等。
V-3)条带
V-4)泡沫(密封、绝缘、阻挡层),运动和休闲垫。
V-5)密封剂
VI-1)食物包装和包装材料(柔韧和坚固型)、BOPP、BOPET、瓶。
VI-2)存储体系如箱(板条箱)、皮箱、盒、家用箱、垫板、容器、架子、轨道、螺丝盒、包装和罐子。
VI-3)药筒、注射器、医疗器具、用于任何运输的容器、垃圾篮和垃圾箱、垃圾袋、箱、垃圾箱、箱衬里、轮箱、常规容器、用于水/用后水/化学/气体/油/汽油/柴油的罐;槽衬层、箱、板条箱、电池箱、水槽、医学装置如活塞、眼科用具、诊断装置和药剂泡罩包装。
VII-1)任何种类的家庭用品(例如用具、热水瓶/衣架)、紧固系统如插头、电线和电线夹、拉链、密封盒、锁和按扣密封盒。
VII-2)支撑装置,休闲用品如运动和健身装置、体操垫、滑雪靴、直排轮鞋、滑雪板、大脚、运动表面(例如网球场地);用于瓶子和罐子的螺旋盖、盖和木塞。
VII-3)常规家具,泡沫制品(垫子、吸震器)、泡沫体、海绵、抹布、垫、花园椅、体育馆座位、桌子、长椅、玩具、建筑套具(板/外形/球)、剧场、滑梯和游戏车辆。
VII-4)用于光学和磁数据存储的材料。
VII-5)厨房用具(吃、喝、烹饪、储存)。
VII-6)用于CD、卡带和录影带的盒子;DVD电子物件、任何种类的办公用品(圆珠笔、图章和印泥、鼠标、架子、轨道)、任何体积和含量的瓶子(饮料、洗涤剂、包括香水的化妆品)和胶带。
VII-7)鞋类(鞋/鞋底)、鞋垫、护脚、粘合剂、结构粘着剂、食物(水果、蔬菜、肉、鱼)盒、合成纸、瓶用标签、长椅、人造关节(人类)、印刷版(苯胺印刷)、印刷电路板和显示技术。
VII-8)填充聚合物(滑石、粉笔、陶土(高岭土)、硅酸钙岩矿、颜料、炭黑、TiO2、云母、纳米复合材料、白云石、硅酸盐、玻璃、石棉)的装置。
优选作为膜、管、电缆、条带、薄片、容器、框架、纤维或单长丝的成型人造聚合物制品。
本发明的另一优选实施方案为薄膜,通常用吹塑挤塑技术获得。尤其关注单层膜或3、5或7个层的多层膜。薄塑料膜在农业中最重要的应用为作为用于温室和通道的覆盖物以在受保护环境中种植作物。
本发明的另一实施方案为经挤出、浇铸、纺丝、模塑或压延的聚合物组合物,其包含合成聚合物和/或天然或合成弹性体和本文所定义的多孔金属氧化物微球。对于这类组合物,应适用本文给出的定义和优选情形。
多孔金属氧化物球优选以基于组合物重量的0.01重量%至40.0重量%,尤其是0.01重量%至20.0重量%的量存在于经挤出、浇铸、纺丝、模塑或压延聚合物组合物中。更优选0.1重量%至20.0重量%,尤其是0.1重量%至10.0重量%的浓度。高度优选0.25重量%至10.0重量%,尤其是0.5重量%至10.0重量%的浓度。
经挤出、浇铸、纺丝、模塑或压延的聚合物组合物和成型人造聚合物制品可包含相对于经挤出、浇铸、纺丝、模塑或压延的聚合物组合物或制品的重量为0.001重量%至30重量%,优选0.005重量%至20重量%,尤其是0.005重量%至10重量%的量的至少一种其他添加剂。实例列于下文中:
1.抗氧化剂
1.1烷基化单酚,例如2,6-二叔丁基-4-甲基苯酚、2-叔丁基-4,6-二甲基苯酚、2,6-二叔丁基-4-乙基苯酚、2,6-二叔丁基-4-正丁基苯酚、2,6-二叔丁基-4-异丁基苯酚、2,6-二环戊基-4-甲基苯酚、2-(α-甲基环己基)-4,6-二甲基苯酚、2,6-二(十八烷基)-4-甲基苯酚、2,4,6-三环己基苯酚、2,6-二叔丁基-4-甲氧基甲基苯酚,侧链为直链或支化的壬基酚,例如2,6-二壬基-4-甲基苯酚、2,4-二甲基-6-(1'-甲基十一烷-1'-基)苯酚、2,4-二甲基-6-(1'-甲基十七烷-1'-基)苯酚、2,4-二甲基-6-(1'-甲基十三烷-1'-基)苯酚及其混合物。
1.2.烷硫基甲基苯酚,例如2,4-二辛硫基甲基-6-叔丁基苯酚、2,4-二辛硫基甲基-6-甲基苯酚、2,4-二辛硫基甲基-6-乙基苯酚、2,6-二(十二烷硫基)甲基-4-壬基苯酚。
1.3.氢醌类和烷基化氢醌类,例如2,6-二叔丁基-4-甲氧基苯酚、2,5-二叔丁基氢醌、2,5-二叔戊基氢醌、2,6-二苯基-4-十八烷氧基苯酚、2,6-二叔丁基氢醌、2,5-二叔丁基-4-羟基茴香醚、3,5-二叔丁基-4-羟基茴香醚、硬脂酸3,5-二叔丁基-4-羟基苯基酯、己二酸双(3,5-二叔丁基-4-羟基苯基)酯。
1.4.生育酚类,例如α-生育酚、β-生育酚、γ-生育酚、δ-生育酚及其混合物(维生素E)。
1.5.羟基化硫代二苯醚,例如2,2'-硫代双(6-叔丁基-4-甲基苯酚)、2,2'-硫代双(4-辛基苯酚)、4,4'-硫代双(6-叔丁基-3-甲基苯酚)、4,4'-硫代双(6-叔丁基-2-甲基苯酚)、4,4'-硫代双(3,6-二仲戊基苯酚)、4,4'-双(2,6-二甲基-4-羟基苯基)二硫醚。
1.6.亚烷基双酚,例如2,2'-亚甲基双(6-叔丁基-4-甲基苯酚)、2,2'-亚甲基双(6-叔丁基-4-乙基苯酚)、2,2'-亚甲基双[4-甲基-6-(α-甲基环己基)苯酚]、2,2'-亚甲基双(4-甲基-6-环己基苯酚)、2,2'-亚甲基双(6-壬基-4-甲基苯酚)、2,2'-亚甲基双(4,6-二叔丁基苯酚)、2,2'-亚乙基双(4,6-二叔丁基苯酚)、2,2'-亚乙基双(6-叔丁基-4-异丁基苯酚)、2,2'-亚甲基双[6-(α-甲基苄基)-4-壬基酚]、2,2'-亚甲基双[6-(α,α-二甲基苄基)-4-壬基酚]、4,4'-亚甲基双(2,6-二叔丁基苯酚)、4,4'-亚甲基双(6-叔丁基-2-甲基苯酚)、1,1-双(5-叔丁基-4-羟基-2-甲基苯基)丁烷、2,6-双(3-叔丁基-5-甲基-2-羟基苄基)-4-甲基苯酚、1,1,3-三(5-叔丁基-4-羟基-2-甲基苯基)丁烷、1,1-双(5-叔丁基-4-羟基-2-甲基苯基)-3-正十二烷基巯基丁烷、乙二醇双[3,3-双(3'-叔丁基-4'-羟基苯基)丁酸酯]、双(3-叔丁基-4-羟基-5-甲基苯基)二环戊二烯、双[2-(3'-叔丁基-2'-羟基-5'-甲基苄基)-6-叔丁基-4-甲基苯基]对苯二甲酸酯、1,1-双(3,5-二甲基-2-羟基苯基)丁烷、2,2-双(3,5-二叔丁基-4-羟基苯基)丙烷、2,2-双(5-叔丁基-4-羟基-2-甲基苯基)-4-正十二烷基巯基丁烷、1,1,5,5-四(5-叔丁基-4-羟基-2-甲基苯基)戊烷。
1.7.O-、N-和S-苄基化合物,例如3,5,3',5'-四叔丁基-4,4'-二羟基二苄基醚、4-羟基-3,5-二甲基苄基巯基乙酸十八烷基酯、4-羟基-3,5-二叔丁基苄基巯基乙酸十三烷基酯、三(3,5-二叔丁基-4-羟基苄基)胺、双(4-叔丁基-3-羟基-2,6-二甲基苄基)二硫代对苯二甲酸酯、双(3,5-二叔丁基-4-羟基苄基)硫化物、3,5-二叔丁基-4-羟基苄基巯基乙酸异辛基酯。
1.8.羟基苄基化丙二酸酯,例如2,2-双(3,5-二叔丁基-2-羟基苄基)丙二酸二(十八烷基)酯、2-(3-叔丁基-4-羟基-5-甲基苄基)丙二酸二(十八烷基)酯、2,2-双(3,5-二叔丁基-4-羟基苄基)丙二酸二(十二烷基巯基乙基)酯、2,2-双(3,5-二叔丁基-4-羟基苄基)丙二酸双[4-(1,1,3,3-四甲基丁基)苯基]酯。
1.9.芳族羟基苄基化合物,例如1,3,5-三(3,5-二叔丁基-4-羟基苄基)-2,4,6-三甲基苯、1,4-双(3,5-二叔丁基-4-羟基苄基)-2,3,5,6-四甲基苯、2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯酚。
1.10.三嗪化合物,例如2,4-双(辛基巯基)-6-(3,5-二叔丁基-4-羟基苯胺基)-1,3,5-三嗪、2-辛基巯基-4,6-双(3,5-二叔丁基-4-羟基苯胺基)-1,3,5-三嗪、2-辛基巯基-4,6-双(3,5-二叔丁基-4-羟基苯氧基)-1,3,5-三嗪、2,4,6-三(3,5-二叔丁基-4-羟基苯氧基)-1,2,3-三嗪、1,3,5-三(3,5-二叔丁基-4-羟基苄基)异氰脲酸酯、1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)异氰脲酸酯、2,4,6-三(3,5-二叔丁基-4-羟基苯基乙基)-1,3,5-三嗪、1,3,5-三(3,5-二叔丁基-4-羟基苯基丙酰基)-六氢-1,3,5-三嗪、1,3,5-三(3,5-二环己基-4-羟基苄基)异氰脲酸酯。
1.11.苄基膦酸酯,例如2,5-二叔丁基-4-羟基苄基膦酸二甲酯、3,5-二叔丁基-4-羟基苄基膦酸二乙酯、3,5-二叔丁基-4-羟基苄基膦酸二(十八烷基)酯、5-叔丁基-4-羟基-3-甲基苄基膦酸二(十八烷基)酯、3,5-二叔丁基-4-羟基苄基膦酸的单乙酯的钙盐。
1.12.酰氨基苯酚类,例如4-羟基月桂酰替苯胺、4-羟基硬脂酰替苯胺、N-(3,5-二叔丁基-4-羟基苯基)氨基甲酸辛酯。
1.13.β-(3,5-二叔丁基-4-羟基苯基)丙酸与一元醇或多元醇的酯,例如与甲醇、乙醇、正辛醇、异辛醇、十八烷醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二甘醇、二甘醇、三甘醇、四甘醇、季戊四醇、三(羟乙基)异氰脲酸酯、N,N'-双(羟乙基)草酰胺、3-硫杂十一烷醇、3-硫杂十五烷醇、三甲基己二醇、三羟甲基丙烷、4-羟基甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷的酯。
1.14.β-(5-叔丁基-4-羟基-3-甲基苯基)丙酸与一元醇或多元醇的酯,例如与甲醇、乙醇、正辛醇、异辛醇、十八烷醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二甘醇、二甘醇、三甘醇、季戊四醇、三(羟乙基)异氰脲酸酯、N,N'-双(羟乙基)草酰胺、3-硫杂十一烷醇、3-硫杂十五烷醇、三甲基己二醇、三羟甲基丙烷、4-羟基甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷、3,9-双[2-{3-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基}-1,1-二甲基乙基]-2,4,8,10-四氧杂螺[5.5]十一烷的酯。
1.15.β-(3,5-二环己基-4-羟基苯基)丙酸与一元醇或多元醇的酯,例如与甲醇、乙醇、辛醇、十八烷醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二甘醇、二甘醇、三甘醇、季戊四醇、三(羟乙基)异氰脲酸酯、N,N'-双(羟乙基)草酰胺、3-硫杂十一烷醇、3-硫杂十五烷醇、三甲基己二醇、三羟甲基丙烷、4-羟基甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷的酯。
1.16.3,5-二叔丁基-4-羟基苯基乙酸与一元醇或多元醇的酯,例如与甲醇、乙醇、辛醇、十八烷醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二甘醇、二甘醇、三甘醇、季戊四醇、三(羟乙基)异氰脲酸酯、N,N'-双(羟乙基)草酰胺、3-硫杂十一烷醇、3-硫杂十五烷醇、三甲基己二醇、三羟甲基丙烷、4-羟基甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷的酯。
1.17.β-(3,5-二叔丁基-4-羟基苯基)丙酸的酰胺,例如N,N'-双(3,5-二叔丁基-4-羟基苯基丙酰基)六亚甲基二胺、N,N'-双(3,5-二叔丁基-4-羟基苯基丙酰基)三亚甲基二胺、N,N'-双(3,5-二叔丁基-4-羟基苯基丙酰基)肼、N,N'-双[2-(3-[3,5-二叔丁基-4-羟基苯基]丙酰氧基)乙基]草酰胺(XL-1,由Uniroyal提供)。
1.18.抗坏血酸(维生素C)。
1.19.胺类抗氧化剂,例如N,N'-二异丙基对苯二胺、N,N'-二仲丁基对苯二胺、N,N'-双(1,4-二甲基戊基)对苯二胺、N,N'-双(1-乙基-3-甲基戊基)对苯二胺、N,N'-双(1-甲基庚基)对苯二胺、N,N'-二环己基对苯二胺、N,N'-二苯基对苯二胺、N,N'-双(2-萘基)对苯二胺、N-异丙基-N'-苯基对苯二胺、N-(1,3-二甲基丁基)-N'-苯基对苯二胺、N-(1-甲基庚基)-N'-苯基对苯二胺、N-环己基-N'-苯基对苯二胺、4-(对甲苯氨磺酰基)二苯基胺、N,N'-二甲基-N,N'-二仲丁基对苯二胺、二苯基胺、N-烯丙基二苯基胺、4-异丙氧基二苯基胺、N-苯基-1-萘基胺、N-(4-叔辛基苯基)-1-萘基胺、N-苯基-2-萘基胺、辛基化二苯基胺如p,p'-二叔辛基二苯基胺、4-正丁基氨基苯酚、4-丁酰基氨基苯酚、4-壬酰基氨基苯酚、4-十二烷酰基氨基苯酚、4-十八烷酰基氨基苯酚、双(4-甲氧基苯基)胺、2,6-二叔丁基-4-二甲基氨基甲基苯酚、2,4'-二氨基二苯基甲烷、4,4'-二氨基二苯基甲烷、N,N,N',N'-四甲基-4,4'-二氨基二苯基甲烷、1,2-双[(2-甲基苯基)氨基]乙烷、1,2-双(苯基氨基)丙烷、邻甲苯基双胍、双[4-(1',3'-二甲基丁基)苯基]胺、叔辛基化N-苯基-1-萘基胺、单-和二-烷基化叔丁基二苯基胺/叔辛基二苯基胺的混合物、单-和二-烷基化壬基二苯基胺的混合物、单-和二-烷基化十二烷基二苯基胺的混合物、单-和二-烷基化异丙基二苯基胺/异己基二苯基胺的混合物、单-和二-烷基化叔丁基二苯基胺的混合物、2,3-二氢-3,3-二甲基-4H-1,4-苯并噻嗪、吩噻嗪、单-和二-烷基化叔丁基吩噻嗪/叔辛基吩噻嗪的混合物、单-和二-烷基化叔辛基吩噻嗪的混合物、N-烯丙基吩噻嗪、N,N,N',N'-四苯基-1,4-二氨基丁-2-烯。
2.UV吸收剂和光稳定剂
2.1. 2-(2'-羟基苯基)苯并三唑类,例如2-(2'-羟基-5'-甲基苯基)苯并三唑、2-(3',5'-二叔丁基-2'-羟基苯基)苯并三唑、2-(5'-叔丁基-2'-羟基苯基)苯并三唑、2-(2'-羟基-5'-(1,1,3,3-四甲基丁基)苯基)苯并三唑、2-(3',5'-二叔丁基-2'-羟基苯基)-5-氯苯并三唑、2-(3'-叔丁基-2'-羟基-5'-甲基苯基)-5-氯苯并三唑、2-(3'-仲丁基-5'-叔丁基-2'-羟基苯基)苯并三唑、2-(2'-羟基-4'-辛氧基苯基)苯并三唑、2-(3',5'-二叔戊基-2'-羟基苯基)苯并三唑、2-(3',5'-双(α,α-二甲基苄基)-2'-羟基苯基)苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-辛氧基羰基乙基)苯基)-5-氯苯并三唑、2-(3'-叔丁基-5'-[2-(2-乙基己氧基)羰基乙基]-2'-羟基苯基)-5-氯苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-甲氧羰基乙基)苯基)-5-氯苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-甲氧羰基乙基)苯基)苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-辛氧基羰基乙基)苯基)苯并三唑、2-(3'-叔丁基-5'-[2-(2-乙基己氧基)羰基乙基]-2'-羟基苯基)苯并三唑、2-(3'-十二烷基-2'-羟基-5'-甲基苯基)苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-异辛氧基羰基乙基)苯基苯并三唑、2,2'-亚甲基双[4-(1,1,3,3-四甲基丁基)-6-苯并三唑-2-基苯酚];2-[3'-叔丁基-5'-(2-甲氧基羰基乙基)-2'-羟基苯基]-2H-苯并三唑与聚乙二醇300的酯交换产物;其中R=3'-叔丁基-4'-羟基-5'-2H-苯并三唑-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]苯并三唑;2-[2'-羟基-3'-(1,1,3,3-四甲基丁基)-5'-(α,α-二甲基苄基)苯基]苯并三唑。
2.2.2-羟基二苯甲酮类,例如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'-二甲氧基衍生物。
2.3.取代和未取代苯甲酸的酯,例如水杨酸4-叔丁基苯基酯、水杨酸苯基酯、水杨酸辛基苯基酯、二苯甲酰间苯二酚、双(4-叔丁基苯甲酰)间苯二酚、苯甲酰间苯二酚、3,5-二叔丁基-4-羟基苯甲酸2,4-二叔丁基苯基酯、3,5-二叔丁基-4-羟基苯甲酸十六烷基酯、3,5-二叔丁基-4-羟基苯甲酸十八烷基酯、3,5-二叔丁基-4-羟基苯甲酸2-甲基-4,6-二叔丁基苯基酯。
2.4.丙烯酸酯类,例如α-氰基-β,β-二苯基丙烯酸乙酯、α-氰基-β,β-二苯基丙烯酸异辛酯、α-甲酯基肉桂酸甲酯、α-氰基-β-甲基对甲氧基肉桂酸甲酯、α-氰基-β-甲基对甲氧基肉桂酸丁酯、α-甲酯基对甲氧基肉桂酸甲酯、N-(β-甲酯基-β-氰基乙烯基)-2-甲基二氢吲哚、四(α-氰基-β,β-二苯基丙烯酸新戊基酯。
2.5.镍化合物,例如2,2'-硫代双[4-(1,1,3,3-四甲基丁基)苯酚]的镍配合物,例如1:1或1:2配合物,其具有或不具有其他配体如正丁胺、三乙醇胺或N-环己基二乙醇胺,二丁基二硫代氨基甲酸镍,4-羟基-3,5-二叔丁基苄基膦酸的单烷基酯如甲酯或乙酯的镍盐,酮肟如2-羟基-4-甲基苯基十一烷基酮肟的镍配合物,1-苯基-4-月桂酰基-5-羟基吡唑的镍配合物,其具有或不具有其他配体。
2.6.位阻胺,例如碳酸双(1-十一烷氧基-2,2,6,6-四甲基-4-哌啶基)酯、双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(2,2,6,6-四甲基-4-哌啶基)琥珀酸酯、双(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯、双(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(1,2,2,6,6-五甲基-4-哌啶基)正丁基-3,5-二叔丁基-4-羟基苄基丙二酸酯、1-(2-羟乙基)-2,2,6,6-四甲基-4-羟基哌啶与琥珀酸的缩合物、N,N'-双(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺与4-叔辛基氨基-2,6-二氯-1,3,5-三嗪的线性或环状缩合物、三(2,2,6,6-四甲基-4-哌啶基)次氮基三乙酸酯、四(2,2,6,6-四甲基-4-哌啶基)-1,2,3,4-丁烷四甲酸酯、1,1'-(1,2-亚乙基)-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)琥珀酸酯、N,N'-双-(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺与4-吗啉基-2,6-二氯-1,3,5-三嗪的线性或环状缩合物、2-氯-4,6-双(4-正丁基氨基-2,2,6,6-四甲基哌啶基)-1,3,5-三嗪与1,2-双(3-氨基丙基氨基)乙烷的缩合物、2-氯-4,6-二(4-正丁基氨基-1,2,2,6,6-五甲基哌啶基)-1,3,5-三嗪与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]癸烷-2,4-二酮、3-十二烷基-1-(2,2,6,6-四甲基-4-哌啶基)吡咯烷-2,5-二酮、3-十二烷基-1-(1,2,2,6,6-五甲基-4-哌啶基)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-4-哌啶基)六亚甲基二胺与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)乙烷与2,4,6-三氯-1,3,5-三嗪以及4-丁基氨基-2,2,6,6-四甲基哌啶的缩合物(CAS登记号[136504-96-6]);1,6-己二胺与2,4,6-三氯-1,3,5-三嗪以及N,N-二丁胺与4-丁基氨基-2,2,6,6-四甲基哌啶的缩合物(CAS登记号[192268-64-7]);N-(2,2,6,6-四甲基-4-哌啶基)正十二烷基琥珀酰亚胺、N-(1,2,2,6,6-五甲基-4-哌啶基)正十二烷基琥珀酰亚胺、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、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]癸烷与表氯醇的反应产物、1,1-双(1,2,2,6,6-五甲基-4-哌啶基氧基羰基)-2-(4-甲氧基苯基)乙烯、N,N'-双甲酰基-N,N'-双(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺、4-甲氧基亚甲基丙二酸与1,2,2,6,6-五甲基-4-羟基哌啶的二酯、聚[甲基丙基-3-氧基-4-(2,2,6,6-四甲基-4-哌啶基)]硅氧烷、马来酸酐-α-烯烃共聚物与2,2,6,6-四甲基-4-氨基哌啶或1,2,2,6,6-五甲基-4-氨基哌啶的反应产物、2,4-双[N-(1-环己氧基-2,2,6,6-四甲基哌啶-4-基)-N-丁基氨基]-6-(2-羟乙基)氨基-1,3,5-三嗪、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、5-(2-乙基己酰基)氧基甲基-3,3,5-三甲基-2-吗啉酮、Sanduvor(Clariant;CAS登记号[106917-31-1])、5-(2-乙基己酰基)氧基甲基-3,3,5-三甲基-2-吗啉酮、2,4-双[(1-环己氧基-2,2,6,6-哌啶-4-基)丁基氨基]-6-氯-s-三嗪与N,N'-双(3-氨基丙基)乙二胺的反应产物、1,3,5-三(N-环己基-N-(2,2,6,6-四甲基哌嗪-3-酮-4-基)氨基)-s-三嗪、1,3,5-三(N-环己基-N-(1,2,2,6,6-五甲基哌嗪-3-酮-4-基)氨基)-s-三嗪,
N,N”'-1,6-己二基双[N',N”-二丁基-N,N',N”-三(2,2,6,6-四甲基-4-哌啶基)-1,3,5-三嗪-2,4,6-三胺与如下物质的反应产物:经氧化、经氢化的1,3,5-三嗪-2,4,6-三胺、N,N”'-1,6-己二基双[N',N”-二丁基-N,N',N”-三(2,2,6,6-四甲基-4-哌啶基)-3-溴-1-丙烯,4-哌啶醇,2,2,6,6-四甲基-1-(十一烷氧基)-,4,4'-碳酸酯,经氧化、经氢化的1,3,5-三嗪-2,4,6-三胺、N2,N2'-1,6-己二基双[N4,N6-二丁基-N2,N4,N6-三(2,2,6,6-四甲基-4-哌啶基)-N-烯丙基衍生物,及其组合。
2.7.草酰胺,例如4,4'-二辛氧基草酰二苯胺、2,2'-二乙氧基草酰二苯胺、2,2'-二辛氧基-5,5'-二叔丁基草酰二苯胺、2,2'-二(十二烷氧基)-5,5'-二叔丁基草酰二苯胺、2-乙氧基-2'-乙基草酰二苯胺、N,N'-双(3-二甲基氨基丙基)草酰胺、2-乙氧基-5-叔丁基-2'-乙基草酰二苯胺及其与2-乙氧基-2'-乙基-5,4'-二叔丁基草酰二苯胺的混合物、邻-和对-甲氧基二取代草酰二苯胺的混合物以及邻-和对-乙氧基二取代草酰二苯胺的混合物。
2.8. 2-(2-羟基苯基)-1,3,5-三嗪类,例如2,4,6-三(2-羟基-4-辛氧基苯基)-1,3,5-三嗪、2-(2-羟基-4-辛氧基苯基)-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2-(2,4-二羟基苯基)-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2,4-双(2-羟基-4-丙氧基苯基)-6-(2,4-二甲基苯基)-1,3,5-三嗪、2-(2-羟基-4-辛氧基苯基)-4,6-双(4-甲基苯基)-1,3,5-三嗪、2-(2-羟基-4-十二烷氧基苯基)-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2-(2-羟基-4-十三烷氧基苯基)-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2-[2-羟基-4-(2-羟基-3-丁氧基丙氧基)苯基]-4,6-双(2,4-二甲基)-1,3,5-三嗪、2-[2-羟基-4-(2-羟基-3-辛氧基丙氧基)苯基]-4,6-双(2,4-二甲基)-1,3,5-三嗪、2-[4-(十二烷氧基/十三烷氧基-2-羟基丙氧基)-2-羟基苯基]-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2-[2-羟基-4-(2-羟基-3-十二烷氧基丙氧基)苯基]-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2-(2-羟基-4-己氧基)苯基-4,6-二苯基-1,3,5-三嗪、2-(2-羟基-4-甲氧基苯基)-4,6-二苯基-1,3,5-三嗪、2,4,6-三[2-羟基-4-(3-丁氧基-2-羟基丙氧基)苯基]-1,3,5-三嗪、2-(2-羟基苯基)-4-(4-甲氧基苯基)-6-苯基-1,3,5-三嗪、2-{2-羟基-4-[3-(2-乙基己基-1-氧基)-2-羟基丙氧基]苯基}-4,6-双(2,4-二甲基苯基)-1,3,5-三嗪、2,4-双(4-[2-乙基己氧基]-2-羟基苯基)-6-(4-甲氧基苯基)-1,3,5-三嗪、2-(4,6-双-联苯-4-基-1,3,5-三嗪-2-基)-5-(2-乙基-(正)-己氧基)苯酚;十二烷二酸1,12-双[2-[4-(4,6-二苯基-1,3,5-三嗪-2-基)-3-羟基苯氧基]乙基]酯(CAS号1482217-03-7)。
3.金属减活剂,例如N,N'-二苯基草酰胺、N-水杨醛-N'-水杨酰肼、N,N'-双(水杨酰)肼、N,N'-双(3,5-二叔丁基-4-羟基苯基丙酰)肼、3-水杨酰氨基-1,2,4-三唑、双(亚苄基)草酰二肼、草酰二苯胺、间苯二甲酰二肼、癸二酰双苯基肼、N,N'-二乙酰己二酰二肼、N,N'-双(水杨酰)草酰二肼、N,N'-双(水杨酰)硫代丙酰二肼。
4.亚磷酸酯和亚膦酸酯,例如亚磷酸三苯基酯、亚磷酸二苯基烷基酯、亚磷酸苯基二烷基酯、亚磷酸三(壬基苯基)酯、亚磷酸三月桂基酯、亚磷酸三(十八烷基)酯、二硬脂基季戊四醇二亚磷酸酯、亚磷酸三(2,4-二叔丁基苯基)酯、二异癸基季戊四醇二亚磷酸酯、双(2,4-二叔丁基苯基)季戊四醇二亚磷酸酯、双(2,4-二枯基苯基)季戊四醇二亚磷酸酯、双(2,6-二叔丁基-4-甲基苯基)季戊四醇二亚磷酸酯、二异癸氧基季戊四醇二亚磷酸酯、双(2,4-二叔丁基-6-甲基苯基)季戊四醇二亚磷酸酯、双(2,4,6-三(叔丁基苯基)季戊四醇二亚磷酸酯、三硬脂酰基山梨糖醇三亚磷酸酯、四(2,4-二叔丁基苯基)4,4'-亚联苯基二亚膦酸酯、6-异辛氧基-2,4,8,10-四叔丁基-12H-二苯并[d,g]-1,3,2-二氧杂磷杂环辛烷(dioxaphosphocin)、亚磷酸双(2,4-二叔丁基-6-甲基苯基)甲基酯、亚磷酸双(2,4-二叔丁基-6-甲基苯基)乙基酯、6-氟-2,4,8,10-四叔丁基-12-甲基-二苯并[d,g]-1,3,2-二氧杂磷杂环辛烷、2,2',2”-次氮基[三乙基三(3,3',5,5'-四叔丁基-11'-联苯-2,2'-二基)亚磷酸酯]、亚磷酸2-乙基己基(3,3',5,5'-四叔丁基-11'-联苯-2,2'-二基)酯、5-丁基-5-乙基-2-(2,4,6-三叔丁基苯氧基)-1,3,2-二氧杂磷杂环丙烷(dioxaphosphirane)、亚磷酸、经混合的2,4-双(1,1-二甲基丙基)苯基和4-(1,1-二甲基)苯基三酯(CAS No.939402-02-5)、亚磷酸、三苯基酯、具有α-氢-ω-羟基聚[氧基(甲基-1,2-乙烷二基)]的聚合物、C10-16烷基酯(CAS No.1227937-46-3)。
尤其优选如下亚磷酸酯:
5.羟胺,例如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-二(十四烷基)羟胺、N,N-二(十六烷基)羟胺、N,N-二(十八烷基)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、衍生自氢化牛油胺的N,N-二烷基羟胺。
6.硝酮,例如N-苄基-α-苯基硝酮、N-乙基-α-甲基硝酮、N-辛基-α-庚基硝酮、N-月桂基-α-十一烷基硝酮、N-十四烷基-α-十三烷基硝酮、N-十六烷基-α-十五烷基硝酮、N-十八烷基-α-十七烷基硝酮、N-十六烷基-α-十七烷基硝酮、N-十八烷基-α-十五烷基硝酮、N-十七烷基-α-十七烷基硝酮、N-十八烷基-α-十六烷基硝酮、衍生自N,N-二烷基羟胺(衍生自氢化牛油胺)的硝酮。
7.硫增效剂,例如硫代二丙酸二月桂基酯、硫代二丙酸二肉豆蔻基酯、硫代二丙酸二硬脂基酯、季戊四醇四[3-(十二烷硫基)丙酸酯]或二硬脂基二硫化物。
8.过氧化物清除剂,例如β-硫代二丙酸的酯,例如月桂基酯、硬脂基酯、肉豆蔻基酯或十三烷基酯、巯基苯并咪唑或2-巯基苯并咪唑的锌盐、二丁基二硫代氨基甲酸锌、二(十八烷基)二硫化物、季戊四醇四(β-十二烷基巯基)丙酸酯。
9.聚酰胺稳定剂,例如与碘化物和/或磷化合物组合的铜盐和二价锰盐。
10.碱性共稳定剂,例如三聚氰胺、聚乙烯吡咯烷酮、双氰胺、氰脲酸三烯丙基酯、脲衍生物、肼衍生物、胺、聚酰胺、聚氨酯、高级脂肪酸的碱金属盐和碱土金属盐,例如硬脂酸钙、硬脂酸锌、山酸镁、硬脂酸镁、蓖麻醇酸钠和棕榈酸钾、焦儿茶酸锑或焦儿茶酸锌。
11.PVC热稳定剂,例如混合金属稳定剂(如钡/锌、钙/锌类型)、有机锡稳定剂(如有机锡巯基酯、有机锡羧酸酯、有机锡硫化物)、铅稳定剂(如三元硫酸铅、二元硬脂酸铅、二元邻苯二甲酸铅、二元磷酸铅、硬脂酸铅)、有机基稳定剂及其组合。
12.成核剂,例如无机物质如滑石,金属氧化物如二氧化钛或氧化镁,优选碱土金属的磷酸盐、碳酸盐或硫酸盐;有机化合物如单-或多羧酸及其盐,例如4-叔丁基苯甲酸、己二酸、二苯基乙酸、琥珀酸钠或苯甲酸钠;聚合化合物如离子共聚物(离聚物)。尤其优选1,3:2,4-双(3',4'-二甲基亚苄基)山梨糖醇、1,3:2,4-二(对甲基二亚苄基)山梨糖醇和1,3:2,4-二(亚苄基)山梨糖醇。
13.填料和增强剂,例如碳酸钙、硅酸盐、玻璃纤维、玻璃珠、石棉、滑石、高岭土、云母、硫酸钡、金属氧化物和氢氧化物、炭黑、石墨、木粉和面粉或其他天然产物的纤维、合成纤维。
14.增塑剂,其中所述增塑剂选自二(2-乙基己基)邻苯二甲酸酯、邻苯二甲酸二异壬酯、邻苯二甲酸二异癸酯、邻苯二甲酸二丙基庚酯、偏苯三酸三辛基酯、偏苯三酸三(异壬基)酯、环氧化大豆油、环己烷-1,2-二甲酸二(异壬基)酯、2,4,4-三甲基-1,3-戊二醇二异丁酸酯。
如根据本发明使用的增塑剂还可包含选自如下中的一个:邻苯二甲酸酯、偏苯三酸酯、脂族二元酯、聚酯、聚合物、环氧化物、磷酸酯。在一个优选实施方案中,所述增塑剂选自:邻苯二甲酸丁基苄基酯、邻苯二甲酸丁基2-乙基己基酯、邻苯二甲酸二异己基酯、邻苯二甲酸二异庚基酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二异辛基酯、邻苯二甲酸二正辛基酯、邻苯二甲酸二异壬基酯、邻苯二甲酸二异癸基酯、邻苯二甲酸二异十一基酯、邻苯二甲酸二异十三基酯、邻苯二甲酸二异(C11,C12,C13)酯、邻苯二甲酸二(正丁基)酯、邻苯二甲酸二(正C7,C9)酯、邻苯二甲酸二(正C6,C8,C10)酯、邻苯二甲酸二异(正壬基)酯、邻苯二甲酸二(正C7,C9,C11)酯、邻苯二甲酸二(正C9,C11)酯、邻苯二甲酸二(正十一基)酯、偏苯三酸三(正C8,C10)酯、偏苯三酸三(2-乙基己基)酯、偏苯三酸三(异辛基)酯、偏苯三酸三(异壬基)酯、己二酸二(正C7,C9)酯、己二酸二(2-乙基己基)酯、己二酸二(异辛基)酯、己二酸二(异壬基)酯、己二酸或戊二酸与丙二醇或丁二醇或2,2-二甲基-1,3-丙二醇的聚酯、环氧化油如环氧化大豆油、环氧化亚麻籽油、环氧化松油、环氧树脂酸辛基酯、环氧树脂酸2-乙基己基酯、磷酸异癸基二苯基酯、磷酸三(2-乙基己基)酯、磷酸三甲苯酯、对苯二甲酸二(2-乙基己基)酯、环己烷-1,2-二甲酸二(异壬基)酯及其组合。在一个尤其优选的实施方案中,所述增塑剂选自邻苯二甲酸二异己基酯、邻苯二甲酸二异庚基酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二异辛基酯、邻苯二甲酸二-正辛基酯、邻苯二甲酸二异壬基酯、邻苯二甲酸二异癸基酯、邻苯二甲酸二异十一基酯、邻苯二甲酸二异十三基酯、邻苯二甲酸二异(C11,C12,C13)酯、邻苯二甲酸二(正丁基)酯、邻苯二甲酸二(正C7,C9)酯、邻苯二甲酸二(正C6,C8,C10)酯、邻苯二甲酸二异(正壬基)酯、邻苯二甲酸二(正C7,C9,C11)酯、邻苯二甲酸二(正C9,C11)酯、邻苯二甲酸二(正十一基)酯、偏苯三酸三(正C8,C10)酯、偏苯三酸三(2-乙基己基)酯、偏苯三酸三(异辛基)酯、偏苯三酸三(异壬基)酯、己二酸二(正C7,C9)酯、己二酸二(2-乙基己基)酯、己二酸二(异辛基)酯、己二酸二(异壬基)酯、己二酸或戊二酸与丙二醇或丁二醇或2,2-二甲基-1,3-丙二醇的聚酯、环氧化油如环氧化大豆油、环己烷-1,2-二甲酸二(异壬基)酯及其组合。
15.其他添加剂,例如增塑剂、润滑剂、乳化剂、颜料、流变添加剂、催化剂、流动调节剂、荧光增白剂、阻燃剂、抗静电剂和发泡剂。
16.苯并呋喃酮和二氢吲哚酮,例如公开于U.S.4,325,863;U.S.4,338,244;U.S.5,175,312;U.S.5,216,052;U.S.5,252,643;DE-A-4316611;DE-A-4316622;DE-A-4316876;EP-A-0589839、EP-A-0591102;EP-A-1291384中的那些或3-[4-(2-乙酰氧基乙氧基)苯基]-5,7-二叔丁基苯并呋喃-2-酮、5,7-二叔丁基-3-[4-(2-硬脂酰氧基乙氧基)苯基]苯并呋喃-2-酮、3,3'-双[5,7-二叔丁基-3-(4-[2-羟基乙氧基]苯基)苯并呋喃-2-酮]、5,7-二叔丁基-3-(4-乙氧基苯基)苯并呋喃-2-酮、3-(4-乙酰氧基-3,5-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(3,5-二甲基-4-新戊基酰氧苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(3,4-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(2,3-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(2-乙酰基-5-异辛基苯基)-5-异辛基苯并呋喃-2-酮。
在某些实施方案中,本文所公开的具有UV吸收功能的光子材料可以涂布在基材上或结合到基材中,所述基材例如塑料、木材、纤维或织物、陶瓷、玻璃、金属及其复合产品。
本发明的范围和关注将基于以下实施例来更好地理解,该实施例意欲说明本发明的某些实施方案且为非限制性的。
实施例
应用实施例1至19的UV测量如下进行:
使用Varian 5000UV-Vis-NIR双光束分光光度计测量紫外透射光谱。将待测试板置于样品架中,通过光电检测器以200nm至800nm之间的1nm增量测量透射光。不使用参考光束。通过阻挡测量光束到达光电检测器来确定0%透射参考。通过允许光束无阻挡地到达光电检测器来确定100%透射参考。
合成实施例1:多孔二氧化硅微球
苯乙烯/丙烯酸共聚物如下制备:将230毫升去离子(DI)水添加到配有温度计、冷凝器、磁搅拌和氮气气氛的三颈反应烧瓶中。将水加热到80℃并在搅拌下加入10克苯乙烯,接着经注射器加入溶解在10毫升DI水中的100毫克丙烯酸。将100毫克过硫酸铵溶解在10毫升DI水中并经注射器添加到搅拌的混合物中。反应混合物在80℃下搅拌24小时。使聚合物胶体分散体冷却到室温并经离心提纯,以产生具有250nm的平均粒度的聚苯乙烯纳米球。
聚苯乙烯胶体水分散体用去离子水稀释到1重量%并加入1重量%二氧化硅纳米粒子,将混合物声处理以防止粒子附聚。连续油相含有在氟化油中的0.1重量%聚乙二醇/全氟聚醚表面活性剂。将胶体水分散体和油各自经由与泵关联的注射器注射到具有50μm液滴接头的微流体装置中。允许系统平衡直至产生单分散液滴。将单分散液滴收集在储器中。
收集的液滴在炉中在45℃下干燥4小时以提供单分散聚合物模板微球。聚合物模板微球如下煅烧:置于硅片上、经3小时从室温加热到500℃、在500℃下保持2小时和经3小时冷却回室温。提供具有15微米的平均直径的单分散二氧化硅微球。
图2和图3是以类似方式制备的聚合物模板微球和多孔二氧化硅微球的扫描电子显微镜(SEM)图像。
合成实施例2:干燥方法
重复实施例1,其中干燥步骤使用微波辐照、在真空下干燥和/或在干燥剂存在下干燥。
合成实施例3:通过喷雾干燥制备多孔二氧化硅微球
苯乙烯/丙烯酸共聚物如下制备:将230毫升去离子(DI)水添加到配有温度计、冷凝器、磁搅拌和氮气气氛的三颈反应烧瓶中。将水加热到80℃并在搅拌下加入10克苯乙烯,接着经注射器加入溶解在10毫升DI水中的100毫克丙烯酸。将100毫克过硫酸铵溶解在10毫升DI水中并经注射器添加到搅拌的混合物中。反应混合物在80℃下搅拌24小时。使聚合物胶体分散体冷却到室温并经离心提纯,以产生具有250nm的平均粒度的聚苯乙烯纳米球。
聚苯乙烯胶体水分散体用去离子水稀释到1重量%并加入1重量%二氧化硅纳米粒子,将混合物声处理以防止粒子附聚。将水分散体喷雾干燥以提供包含聚合物纳米球和二氧化硅的聚合物模板微球。微球如下煅烧:经3小时从室温加热到500℃、在500℃下保持2小时和经3小时冷却回室温。提供多孔二氧化硅微球。
合成实施例4:氧化锌多孔微球
根据实施例4的程序制备多孔氧化锌微球的样品,用氧化锌代替二氧化硅并且其中聚苯乙烯纳米球具有230nm的平均粒度和1:2的聚合物与氧化锌的wt/wt比。将0.5毫克多孔微球样品均匀布置在具有6cm2底面的10mL透明玻璃管瓶中。样品表现出对人眼而言明显的蓝色。
合成实施例5:二氧化硅/二氧化钛多孔微球
根据实施例1的方法制备含有二氧化硅和二氧化钛的多孔微球的样品,其中聚合物与总金属氧化物的wt/wt比为3:1。二氧化硅与二氧化钛的wt/wt比为9:1。
应用实施例1至3
在240ml杯中称重聚丙烯粉末(Profax 6301,12g/10min熔体流动速率)。称量抗氧化剂(Irganox B 215)和合成实施例3的多孔二氧化硅微球,并与粉末混合。每个样品的组分重量列于下表1中。
表1.组分的重量和浓度
应用实施例 | 聚丙烯,g | 抗氧化剂,g | 多孔二氧化硅微球,g |
1 | 49.95 | 0.05 | -- |
2 | 49.7 | 0.05 | 0.25 |
3 | 49.2 | 0.05 | 0.75 |
将聚合物混合物置于预热的210℃的C.W.Brabender Plasti-Corder中,并在50rpm下混合3分钟以获得均匀的熔融混合物。然后将熔融聚合物在218℃在低压条件下压缩模塑3分钟,随后在高压下压缩模塑3分钟,直至250μm的厚度。然后将模具在压缩模塑机中冷却3分钟。从该片上切下5cm×5cm的正方形用于UV-Vis测量。
应用实施例1至3的UV测量结果示于图5中。可以看出,多孔微球的加入导致透射的明显降低。
Irganox B 215是下式化合物的混合物:
应用实施例3至7
在240ml杯中称重聚丙烯粉末(Profax 6301,12g/10min熔体流动速率)。称量抗氧化剂(Irganox B 215)、紫外线吸收剂(PA 328)和合成实施例3的多孔二氧化硅微球,并与粉末混合。每个样品的组分重量列于下表2中。
表2.组分的重量和浓度
将聚合物混合物置于预热的210℃的C.W.Brabender Plasti-Corder中,并在50rpm下混合3分钟以获得均匀的熔融混合物。然后将熔融聚合物在218℃在低压条件下压缩模塑3分钟,随后在高压下压缩模塑3分钟,直至250μm的厚度。然后将模具在压缩模塑机中冷却3分钟。从该片上切下5cm×5cm的正方形用于UV-Vis测量。
应用实施例3至7的UV测量结果示于图6中。可以看出,使用多孔微球与紫外光吸收剂的混合物导致透射的显著降低,甚至可以在接近零的波长的特定范围内降低。
应用实施例8和9
在240ml杯中称重聚丙烯粉末(Profax 6301,12g/10min熔体流动速率)。称量抗氧化剂(Irganox B 215)、紫外线吸收剂和合成实施例3的多孔二氧化硅微球,并与粉末混合。每个样品的组分重量列于下表3中。
表3.组分的重量和浓度
样品编号 | 聚丙烯,g | 抗氧化剂,g | 紫外线吸收剂,g | 多孔二氧化硅微球,g |
8 | 49.9 | 0.05 | 0.05 | -- |
9 | 49.15 | 0.05 | 0.05 | 0.75 |
将聚合物混合物置于预热的210℃的C.W.Brabender Plasti-Corder中,并在50rpm下混合3分钟以获得均匀的熔融混合物。然后将熔融聚合物在218℃在低压条件下压缩模塑3分钟,随后在高压下压缩模塑3分钟,直至250μm的厚度。然后将模具在压缩模塑机中冷却3分钟。从该片上切下5cm×5cm的正方形用于UV-Vis测量。
应用实施例8和9的UV测量结果示于图7中。可以看出,使用多孔微球与紫外光吸收剂的混合物导致透射的显著降低,甚至可以在接近零的波长的特定范围内降低。
应用实施例10和11
在240ml杯中称重聚丙烯粉末(Profax 6301,12g/10min熔体流动速率)。称量抗氧化剂(Irganox B 215)、紫外线吸收剂和合成实施例3的多孔二氧化硅微球,并与粉末混合。每个样品的组分重量列于下表4中。
表4.组分的重量和浓度
样品编号 | 聚丙烯,g | 抗氧化剂,g | 紫外线吸收剂,g | 多孔二氧化硅微球,g |
10 | 49.9 | 0.05 | 0.05 | -- |
11 | 49.15 | 0.05 | 0.05 | 0.75 |
将聚合物混合物置于预热的210℃的C.W.Brabender Plasti-Corder中,并在50rpm下混合3分钟以获得均匀的熔融混合物。然后将熔融聚合物在218℃在低压条件下压缩模塑3分钟,随后在高压下压缩模塑3分钟,直至250μm的厚度。然后将模具在压缩模塑机中冷却3分钟。从该片上切下5cm×5cm的正方形用于UV-Vis测量。
应用实施例10和11的UV测量结果示于图8中。可以看出,使用多孔微球与紫外光吸收剂的混合物导致透射的显著降低,甚至可以在接近零的波长的特定范围内降低。
应用实施例12和13
在240ml杯中称重聚丙烯粉末(Profax 6301,12g/10min熔体流动速率)。称量抗氧化剂(Irganox B 215)、紫外线吸收剂(1577)和合成实施例3的多孔二氧化硅微球,并与粉末混合。每个样品的组分重量列于下表5中。
表5.组分的重量和浓度
样品编号 | 聚丙烯,g | 抗氧化剂,g | 紫外线吸收剂,g | 多孔二氧化硅微球,g |
12 | 49.9 | 0.05 | 0.05 | -- |
13 | 49.15 | 0.05 | 0.05 | 0.75 |
将聚合物混合物置于预热的210℃的C.W.Brabender Plasti-Corder中,并在50rpm下混合3分钟以获得均匀的熔融混合物。然后将熔融聚合物在218℃在低压条件下压缩模塑3分钟,随后在高压下压缩模塑3分钟,直至250μm的厚度。然后将模具在压缩模塑机中冷却3分钟。从该片上切下5cm×5cm的正方形用于UV-Vis测量。
应用实施例12和13的UV测量结果示于图9中。可以看出,使用多孔微球与紫外光吸收剂的混合物导致透射的显著降低,甚至可以在接近零的波长的特定范围内降低。
应用实施例14和15
在240ml杯中称重聚丙烯粉末(Profax 6301,12g/10min熔体流动速率)。称量抗氧化剂(Irganox B 215)、紫外线吸收剂(3035)和合成实施例3的多孔二氧化硅微球,并与粉末混合。每个样品的组分重量列于下表6中。
表6.组分的重量和浓度
样品编号 | 聚丙烯,g | 抗氧化剂,g | 紫外线吸收剂,g | 多孔二氧化硅微球,g |
14 | 49.9 | 0.05 | 0.05 | -- |
15 | 49.15 | 0.05 | 0.05 | 0.75 |
将聚合物混合物置于预热的210℃的C.W.Brabender Plasti-Corder中,并在50rpm下混合3分钟以获得均匀的熔融混合物。然后将熔融聚合物在218℃在低压条件下压缩模塑3分钟,随后在高压下压缩模塑3分钟,直至250μm的厚度。然后将模具在压缩模塑机中冷却3分钟。从该片上切下5cm×5cm的正方形用于UV-Vis测量。
应用实施例14和15的UV测量结果示于图10中。可以看出,使用多孔微球与紫外光吸收剂的混合物导致透射的显著降低,甚至可以在接近零的波长的特定范围内降低。
应用实施例16和17
在240 ml杯中称重聚乙烯粉末(Microthene MN 700 LDPE,20 g/10min熔体流动速率)。称量抗氧化剂(Irganox B 215)、紫外线吸收剂和合成实施例3的多孔二氧化硅微球,并与粉末混合。每个样品的组分重量列于下表7中。
表7.组分的重量和浓度
样品编号 | 聚乙烯,g | 抗氧化剂,g | 紫外线吸收剂,g | 多孔二氧化硅微球,g |
16 | 49.9 | 0.05 | 0.05 | -- |
17 | 49.15 | 0.05 | 0.05 | 0.75 |
将聚合物混合物置于预热的210℃的C.W.Brabender Plasti-Corder中,并在50rpm下混合3分钟以获得均匀的熔融混合物。然后将熔融聚合物在218℃在低压条件下压缩模塑3分钟,随后在高压下压缩模塑3分钟,直至250μm的厚度。然后将模具在压缩模塑机中冷却3分钟。从该片上切下5cm×5cm的正方形用于UV-Vis测量。
应用实施例16和17的UV测量结果示于图11中。可以看出,使用多孔微球与紫外光吸收剂的混合物导致透射的显著降低,甚至可以在接近零的波长的特定范围内降低。
应用实施例18和19
在240ml杯中称重聚乙烯粉末(Microthene MN 700LDPE,20g/10min熔体流动速率)。称量抗氧化剂(Irganox B 215)、紫外线吸收剂和合成实施例3的多孔二氧化硅微球,并与粉末混合。每个样品的组分重量列于下表8中。
表8.组分的重量和浓度
样品编号 | 聚乙烯,g | 抗氧化剂,g | 紫外线吸收剂,g | 多孔二氧化硅微球,g |
18 | 49.9 | 0.05 | 0.05 | -- |
19 | 49.15 | 0.05 | 0.05 | 0.75 |
将聚合物混合物置于预热的210℃的C.W.Brabender Plasti-Corder中,并在50rpm下混合3分钟以获得均匀的熔融混合物。然后将熔融聚合物在218℃在低压条件下压缩模塑3分钟,随后在高压下压缩模塑3分钟,直至250μm的厚度。然后将模具在压缩模塑机中冷却3分钟。从该片上切下5cm×5cm的正方形用于UV-Vis测量。
应用实施例18和19的UV测量结果示于图12中。可以看出,使用多孔微球与紫外光吸收剂的混合物导致透射的显著降低,甚至可以在接近零的波长的特定范围内降低。
断裂伸长率
Claims (16)
1.多孔金属氧化物微球作为用于成型人造聚合物制品的光稳定剂的用途,其中聚合物为合成聚合物和/或天然或合成弹性体且多孔金属氧化物微球包含金属氧化物且通过如下方法制备,所述方法包括
形成聚合物纳米粒子和金属氧化物的液体分散体;
形成所述分散体的液滴;
干燥所述液滴以提供包含聚合物纳米球和金属氧化物的聚合物模板微球;和
从模板微球中除去聚合物纳米球以提供多孔金属氧化物微球,并且
其中所述微球具有
0.5μm至100μm的平均直径,
0.10至0.80的平均孔隙率,和
50nm至999nm的平均孔径。
2.根据权利要求1所述的用途,其中所述金属氧化物选自二氧化硅、二氧化钛、氧化铝、氧化锆、二氧化铈、铁氧化物、氧化锌、氧化铟、氧化锡、氧化铬及它们的组合。
3.根据权利要求1或2所述的用途,其中所述多孔金属氧化物微球包含基于所述微球的总重量为50.0重量%至99.9重量%的金属氧化物。
4.根据权利要求1至3中任一项所述的用途,其中所述多孔金属氧化物微球具有1μm至75μm的平均直径。
5.根据权利要求1至4中任一项所述的用途,其中所述多孔金属氧化物微球具有0.45至0.65的平均孔隙率。
6.根据权利要求1至5中任一项所述的用途,其中所述多孔金属氧化物微球具有50nm至800nm的平均孔径。
7.根据权利要求1至3中任一项所述的用途,其中所述多孔金属氧化物微球具有
1μm至75μm的平均直径,
0.45至0.65的平均孔隙率,和
50nm至800nm的平均孔径。
8.根据权利要求1至3中任一项所述的用途,其中所述多孔金属氧化物微球具有
4.5μm至9.9μm的平均直径;
0.45至0.65的平均孔隙率;以及
220nm至300nm的平均孔径。
9.根据权利要求1至8中任一项所述的用途,其中所述多孔金属氧化物微球以基于所述成型人造聚合物制品的重量为0.01重量%至20.0重量%的浓度使用。
10.根据权利要求1至9中任一项所述的用途,其中所述多孔金属氧化物微球与一种或多种UV吸收剂组合使用,所述UV吸收剂选自2-羟基苯基三嗪类、苯并三唑类、2-羟基二苯甲酮类、N,N'-二苯基乙二酰胺类、肉桂酸酯类和苯甲酸酯类。
11.根据权利要求10所述的用途,其中所述一种或多种UV吸收剂以基于所述成型人造聚合物制品的重量为0.01重量%至20.0重量%的浓度使用。
12.根据权利要求1至11中任一项所述的用途,其中所述成型人造聚合物制品包含位阻胺光稳定剂(HALS)。
13.根据权利要求1至12中任一项所述的用途,其中所述成型人造聚合物制品是经挤出、浇铸、纺丝、模塑或压延的成型人造聚合物制品。
14.根据权利要求1至13中任一项所述的用途,其中所述成型人造聚合物制品是膜、管、电缆、条带、薄片、容器、框架、纤维或单长丝。
15.一种成型人造聚合物制品,其中所述聚合物是合成聚合物和/或天然或合成弹性体,并且其中所述聚合物包含如权利要求1所定义的多孔金属氧化物微球。
16.一种经挤出、浇铸、纺丝、模塑或压延的聚合物组合物,其中所述聚合物为合成聚合物和/或天然或合成弹性体,并且其中所述聚合物包含如权利要求1所定义的多孔金属氧化物微球。
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JP2022525061A (ja) | 2022-05-11 |
WO2020182709A1 (en) | 2020-09-17 |
SG11202109462UA (en) | 2021-09-29 |
AU2020239186A1 (en) | 2021-09-09 |
TW202041585A (zh) | 2020-11-16 |
US20220144712A1 (en) | 2022-05-12 |
EP3938334A1 (en) | 2022-01-19 |
BR112021017233A2 (pt) | 2021-11-09 |
MX2021010990A (es) | 2021-10-01 |
CA3133022A1 (en) | 2020-09-17 |
IL286206A (en) | 2021-10-31 |
KR20210137460A (ko) | 2021-11-17 |
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