CN110678510A - 成核剂、其制备方法和相关聚合物组合物 - Google Patents
成核剂、其制备方法和相关聚合物组合物 Download PDFInfo
- Publication number
- CN110678510A CN110678510A CN201880029214.8A CN201880029214A CN110678510A CN 110678510 A CN110678510 A CN 110678510A CN 201880029214 A CN201880029214 A CN 201880029214A CN 110678510 A CN110678510 A CN 110678510A
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- China
- Prior art keywords
- zinc
- tert
- zmg
- butyl
- bis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 238000000034 method Methods 0.000 title claims abstract description 35
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- 239000011701 zinc Substances 0.000 claims abstract description 47
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- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims abstract description 22
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- 229940049964 oleate Drugs 0.000 claims description 39
- LRGQZEKJTHEMOJ-UHFFFAOYSA-N propane-1,2,3-triol;zinc Chemical compound [Zn].OCC(O)CO LRGQZEKJTHEMOJ-UHFFFAOYSA-N 0.000 claims description 34
- 238000002425 crystallisation Methods 0.000 claims description 32
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- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 13
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- YQEMORVAKMFKLG-UHFFFAOYSA-N glycerine monostearate Natural products CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 claims description 8
- SVUQHVRAGMNPLW-UHFFFAOYSA-N glycerol monostearate Natural products CCCCCCCCCCCCCCCCC(=O)OCC(O)CO SVUQHVRAGMNPLW-UHFFFAOYSA-N 0.000 claims description 8
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- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 3
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- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims description 3
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- 239000000047 product Substances 0.000 description 22
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
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- 125000005591 trimellitate group Chemical group 0.000 description 7
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Abstract
本发明涉及一种制备含有并入的改性剂的单甘油酸锌的方法,和产物,其中该单甘油酸锌呈微晶附聚物形式,其中基于平均相干域长度的微晶尺寸由通过Scherrer等式经由粉末X射线衍射测定在<100>方向上不超过30nm,且在<011>方向上不超过60nm;且由<100>/<011>相干域长度计算的纵横比小于0.65,优选小于0.56,特别是小于0.44。还描述了含有该成核剂的聚合物及其制备方法。该单甘油酸锌可用作成核剂,且在低负载水平下在聚合物如聚丙烯中非常有效。
Description
领域
本发明涉及成核剂、其制备方法和含有成核剂的聚合物组合物。
发明背景
在通过注塑成型的聚烯烃的工业加工中,聚合物结晶程度通常通过使用适当水平的成核剂来控制。这些成核剂赋予聚合物以下优点:提升聚合物的结晶温度(Tc),提高结晶动力学,且因此减少完成用于注塑制品的各循环所需的时间(即循环时间),这又提高了注塑成型设备的输出。成核剂还可借助所得较高结晶度而赋予聚合物体改进的机械特性。
变得日益重要的一个特征为在低负载下的功效。在聚合物产物中成本考虑是重要的。若每千克聚合物所需的成核剂的成本高于获自相关的结晶温度升高或循环时间减少节省的成本,则无论成核剂的功效如何,成核剂在商业上并不成功。因此,重要的是持续寻求新的或改性的成核剂,相对于具有相同功效但在较高负载下的替代物,该成核剂在低负载下具有高功效。
已描述的成核剂或用于聚烯烃制备中的成核剂包括山梨糖醇基化合物、环状二羧酰胺(如N,N'-二环己基-2,6-萘二甲酰胺)、环状二羧酸盐、芳族杂环磷酸盐、丙二酸钙和二价金属丙烷三油酸酯(如单甘油酸锌)。
在商业聚烯烃制备中,单甘油酸锌(ZMG)为在低负载(例如500-1000ppm)下具有非常好的功效的现有高效成核剂。单甘油酸锌由Taylor等首次合成、表征和描述(参见Radoslovich,E.W.,Raupach,M.R.,Slade,P.G.,&Taylor,R.M.(1970).Crystallinecobalt,zinc,manganese,and iron alkoxides of glycerol.Australian Journal ofChemistry,23(10),1963-1971;Hambley,T.W.,&Snow,M.R.(1983)The crystal andmolecular structure of zinc(II)monoglycerolate.Australian Journal ofChemistry,36(6),1249-1253;和Slade,P.G.,Radoslovich,E.W.,&Raupach,M.(1971)Crystal and molecular structure of cobalt(II)monoglycerolate.ActaCrystallographica Section B:Structural Crystallography and Crystal Chemistry,27(12),2432-2436)。当前商业ZMG基于描述于发明人名称为Bos的US 5,475,123(1995)中的方法而制备,其在下文中称为“未改性ZMG”。ZMG的第二形式还由发明人名称也为Bos的专利文献US 7,074,949(2006)已知。在2006专利的方法中,单甘油酸锌由水锌矿(Zn5(CO3)2(OH)6)直接地或间接地合成。因此,该材料在下文中称为“水锌矿-ZMG”。
然而,随时间推移,聚合物制备的成本的压力增加,且研发新的或改性的成核剂是有利的,该成核剂在所需负载水平下的试剂成本与在含有该负载水平下的试剂的制备聚合物产物期间所获得的成本节省之间提供了甚至更有利的平衡。
本发明的目的为提供一种在低负载下具有改进成核效果的新的或改性的成核剂、含有成核剂的聚合物组合物和制备成核剂的相关方法。
概述
现已发现能够制备提供改进成核效果的改性形式的单甘油酸锌(尤其在与未改性单甘油酸锌相比时)。新的单甘油酸锌形式在下文中称为“GMS-ZMG”(以主要使用的甘油单硬脂酸酯(GMS)改性剂命名),且提供比用两倍的未改性单甘油酸锌的量实现的成核效果更好的成核效果。使用新的制备方法制备该产物(GMS-ZMG)。
根据一个实施方案,提供呈微晶附聚物形式的单甘油酸锌,其中基于平均相干域长度的微晶尺寸由通过Scherrer等式经由粉末X射线衍射测定在<100>方向上(即沿<100>晶带轴;下文通常称为<100>方向)不超过30nm,且在<011>方向上不超过60nm。产物还合适地具有小于0.65,例如小于0.60或小于0.56的纵横比(如<100>/<011>相干域长度所测量或计算)。优选的实施方案中的纵横比小于0.44。
通过本文所述的方法,申请人已制得含有并入的改性剂的单甘油酸锌(例如GMS-ZMG)形式,其使得形成微晶附聚物,其中微晶极小。附聚物含有多个微晶,且因此显著大于单个微晶。
申请人已通过提高结晶温度和/或加快完成聚合物结晶的时间周期对单甘油酸锌进行改性以改进结晶效率的方式进行了显著研究。
申请人努力多年后实现该结果,在该期间进行了一系列尝试以减小单甘油酸锌的微晶尺寸。
申请人现已成功地通过使用改性剂和通过控制单甘油酸锌的制备条件实现小的晶体尺寸的单甘油酸锌。与现有技术相比,关键革新是与水锌矿相反(如US 7,074,949中所述),能够使用易于商购且相对廉价的“间接法或法式方法(indirect or Frenchprocess)”氧化锌(例如如可获自Umicore Zinc Chemicals)作为起始点。对于用于氧化锌制备的“间接法或法式方法”的描述,参见Moezzi,A.,McDonagh,A.M.,&Cortie,M.B.(2012)Zinc oxide particles:Synthesis,properties and applications.ChemicalEngineering Journal,185,1-22。改性剂并不改变单甘油酸锌的基本化学结构。
根据一个实施方案,提供一种用于制备单甘油酸锌的方法,其包括使不同于水锌矿的锌化合物(即其为除水锌矿以外且不衍生自水锌矿的锌化合物)与甘油和改性剂在酸催化剂的存在下反应,其中:
-锌化合物选自由如下组成的组:氧化锌、碳酸锌、氢氧化锌、羧酸锌及其组合,或/和
-反应在基于反应组合物的总重量为小于10重量%的水的存在下进行。
在优选的实施方案中,两个条件均用于方法中。
本申请还描述用于在酸催化剂和改性剂的存在下由氧化锌和甘油制备单甘油酸锌以控制产物的微晶和附聚物尺寸的优选温度条件。
通过制备呈上文描述的指定改性形式的单甘油酸锌,申请人已能够制备含有单甘油酸锌(成核剂)(GMS-ZMG)的聚合物组合物,其中聚合物组合物在低单甘油酸锌负载下具有相对高的结晶温度。
因此,根据另一实施方案,提供一种包含有机聚合物和上文描述的单甘油酸锌的组合物。甘油酸锌可以0.01-20重量%聚合物组合物的量存在。
根据另一实施方案,提供一种包含有机聚合物和包含单甘油酸锌的成核剂的组合物,其中单甘油酸锌的基于平均相干域长度的微晶尺寸由通过Scherrer等式经由粉末X射线衍射测定在<100>方向上不超过30nm,且在<011>方向上不超过60nm;且上述相干域长度的比(其可称为纵横比)小于0.65,例如小于0.60或小于0.56,优选小于0.44。具有在该范围内的纵横比表明甘油锌片的堆积高度小于其板长度。
本申请提供上文描述的类型的单甘油酸锌(GMS-ZMG)作为成核剂的用途。还提供上文描述的类型的单甘油酸锌(GMS-ZMG)在改进(提高)有机聚合物的结晶温度中的用途。这可借助在低负载下(例如400ppm或更小)提高有机聚合物的结晶温度。
附图简述
图1显示根据本发明的实施方案的改性单甘油酸锌(GMS-ZMG)的XRD图。还显示未改性ZMG的XRD图。X轴显示2θ(以度计),且Y轴显示计数(峰值强度)。在2θ=10.9°处的峰值为单甘油酸锌的(100)峰值。两个XRD图均经标准化以使得(100)峰值具有相同强度。GMS-ZMG的(100)峰值比未改性ZMG的(100)峰值更宽,即GMS-ZMG微晶更小。
图2a和图2b显示出本发明的一个实施方案的未改性ZMG(图2a)和改性ZMG(图2b)的SEM图像。各图像中的比例尺为1μm。
图3a、图3b和图4为改性单甘油酸锌的额外SEM图像。各图像中的比例尺为100nm。
图5显示与GMS-ZMG(实施例1)的XRD曲线图相比的水锌矿-ZMG(对比例1)的XRD图。X轴为2θ轴(以度计),且Y轴为计数。在2θ=10.9°处的线为(100)峰值,且两个XRD图均经标准化以使得(100)峰值强度相同。GMS-ZMG的(100)峰值比水锌矿-ZMG的(100)峰值更宽,即GMS-ZMG微晶更小。
详述
下文描述根据本发明的特定实施方案的单甘油酸锌、制备方法、聚合物组合物和用途。
在概述改性单甘油酸锌的制备方法的细节之前,将描述改性单甘油酸锌的显著特征。改性单甘油酸锌适合用作成核剂。因此,对单甘油酸锌的提及可与“成核剂”互换地使用。
单甘油酸锌(GMS-ZMG)优选为至少90重量%的单甘油酸锌(化合物)。改性剂优选为不超过5mol%的单甘油酸锌含量。改性剂以使得其不简单为改性剂与预制备的未改性单甘油酸锌的混合物的方式并入。在制备单甘油酸锌期间加入改性剂。已发现改性材料为晶体结构ZMG(X射线衍射迹象)。在优选实施方案中,改性剂(甘油单硬脂酸酯)以5.47重量%的总GMS-ZMG质量使用。
改性剂为能够在制备期间改变单甘油酸锌的微晶尺寸的试剂。发现具有该类改性能力的合适类别的试剂为甘油羧酸酯。甘油羧酸酯优选为酸的单甘油酸酯或单酰基甘油。酸优选为饱和脂肪酸,且可为C6-C24饱和脂肪酸。根据优选实施方案,改性剂为甘油单硬脂酸酯(硬脂酸的酯)。应注意仅脂肪酸甘油三酯(例如椰子油)作为改性剂无效,因此甘油酯中优选存在两个羟基。
含有并入的改性剂的本申请的单甘油酸锌(GMS-ZMG)呈微晶附聚物形式。附聚物尺寸可通过扫描电子显微镜(SEM)测量。使用SEM,合适程序涉及将单甘油酸锌材料粘附至双侧碳带。将该带连接至SEM装置(且松散材料由压缩氮气吹离)。然后将所粘附的单甘油酸锌材料用金属(例如铂)溅射涂覆;且在不同放大倍数下在扫描电子显微镜(SEM)中获取图像。该技术确保单甘油酸锌材料的测量附聚物尺寸分布与松散产物的附聚物尺寸分布一致(即未在悬浮介质中进行进一步处理等)。计算图像区域内的可见附聚物的各颗粒的尺寸(作为直径)。附聚物尺寸在受处理条件影响下难以测量,且附聚物尺寸的概念过于模糊而不具普遍有效性。因此,用于本文中的附聚物尺寸未标准化地提供,而是作为表明成功合成(包含小微晶的松散的大附聚物)的描述给出。
附聚物包含多个微晶。显著地示于扫描电子显微镜(SEM)图像中的附聚物通常为5-50μm宽。具有附聚成微米尺寸的颗粒,特别是其中松散地结合附聚物的微米尺寸的颗粒的多个微晶是有利的。将材料呈现为离散的亚100纳米尺寸的颗粒引起材料的包装和运输方面的处理困难和问题。微米尺寸范围内的附聚物避免了这些问题。尽管附聚因此引人注目,但重要的是附聚物的性质不会导致单个微晶通过聚合物组合物分离和铺展的困难。据信本文所述用于制备GMS改性的单甘油酸锌(GMS-ZMG)的技术提供松散固持的附聚物。
本申请的单甘油酸锌(GMS-ZMG)具有极小微晶(由通过XRD测定),且因此每单位质量递送更多有效分散的微晶(即活性成核剂中心)。
本申请的单甘油酸锌(GMS-ZMG)即使在以少量使用时也提升结晶温度。
借助根据Bragg-Brentano(θ-2θ)几何结构设定的X射线衍射仪器,在所需2θ值之间扫描来获取XRD图。各峰值对应于一组由Miller指数(例如(100))所述的晶格面。对于给定峰值(例如(100)峰值),峰的宽度在晶带轴方向(即在该实例中的<100>)上对应于使用(100)峰值的半高全宽(FWHM)测量的平均相干域长度(即微晶尺寸)。然后可使用Scherrer等式计算微晶尺寸:
τ=Kλ/βcosθ;
其中τ为平均微晶尺寸(nm),K为无量纲形状因子(此处为0.9;相同β必须用于相互比较的所有数据),λ为所用X射线的波长(0.154nm(即Cu Kα辐射)),β为在FWHM下以弧度表示的线增宽,且θ为Bragg角度(以度表示;(峰值的2θ值)/2)。假设线增宽仅来自相干域长度变化。
可制得在<100>方向上(通过上述方法测定)为10-30nm、10-25nm或10-20nm的微晶尺寸的单甘油酸锌(GMS-ZMG)。平均微晶尺寸通常小于25nm、小于22nm或小于20nm。
可制得在<011>方向上(通过上述方法测定)为20-50nm、20-48nm或20-46nm的微晶尺寸的单甘油酸锌(GMS-ZMG)。
GMS-ZMG的微晶尺寸由通过Scherrer等式经由粉末X射线衍射测定在<100>方向上不超过30nm(即沿堆积方向的相干域长度),且在<011>方向上不超过60nm(即沿平面方向的相干域长度)。在<011>方向上的微晶尺寸优选小于60nm。合适地,上述相干域长度的比(纵横比)为约二分之一,或更精确地,小于0.65,例如小于0.60或小于0.56,优选小于0.44。
对于反应持续时间,温度优选保持低于120℃。然而,对于短持续时间,保持高于120℃的温度不应使得该类方法处于本申请的范围外。在此期间反应高于120℃的时间段优选不超过反应总持续时间的10%。优选在反应期间将温度提高至100-120℃的峰值。现有技术方法已涉及高于100℃的较高温度反应或更长时间段。作为在反应期间(至少部分)不同温度条件的结果,在现有技术条件下制备的产物的平均微晶尺寸大于对本申请的产物所示的范围。
锌化合物可选自由如下组成的组:氧化锌、碳酸锌、氢氧化锌、羧酸锌及其组合。然而,本发明的新颖性涉及其使用易于得到的间接法或法式方法氧化锌来制备高度分散性成核剂(比通过现有技术得到的更具分散性)的能力。此外,应注意,本文中所用氧化锌不包括已由水锌矿形成的氧化锌,且实际上不包括使用水锌矿本身(水锌矿-ZMG),这描述于Bos2006中。经由Bos 2006的规定方法,水锌矿的使用往往产生比本申请中指定的那些更大的微晶尺寸(特别是当与其他处理条件组合时),且因此优选不使用。
反应组合物中的甘油量优选为95-110mol%。该量优选为98-105mol%,且通常以化学计量量使用。
就改性剂量而言,该改性剂量优选为1.0-5.0mol%。使用较低量往往产生较大平均微晶尺寸,尽管其他因素还影响所得微晶尺寸。当以足够高的量并入时,改性剂促成较小平均微晶尺寸。该量优选为至少1.0mol%,更优选大于1.7mol%、1.9mol%、2.0mol%、2.1mol%、2.2mol%或2.3mol%。尤其适合的是2.0-5.0mol%。所用理想量可为约2.5mol%。还可使用较高量,然而发现当将量提高至处于/大于5.0mol%时无其他益处,且处于/大于该量的量还可能不利地影响加工性。
根据本发明的单甘油酸锌的一个优选制备方法包括将锌化合物、改性剂与75-95重量%的总甘油组合,混合,且随后加入其余甘油、乙酸和水的组合。
反应在酸催化剂的存在下进行。催化剂优选为酸或酸式盐,如低级烷基羧酸(例如C2至C6羧酸),如乙酸、戊酸;聚羧酸,如柠檬酸、苹果酸、马来酸、琥珀酸、丙二酸、马尿酸、酒石酸、草酸;中等/长链酸,如月桂酸、硬脂酸;任何其他酸,如乙酰丙酸、苯甲酸、硼酸、三氟乙酸;或其混合物。
催化剂还可为任何所述酸的锌盐,例如乙酸锌;但在优选实施方案中,将酸原位加入氧化锌。
所用催化剂的量相对于锌化合物优选为0.2-5mol%。
用于制备改性单甘油酸锌的方法中的一个关键优选特征为反应组合物中的水含量。优选水含量非常低。水含量优选不超过总反应组合物的10重量%,优选不超过8重量%、6重量%、4重量%或2重量%。酸催化剂组合物中可存在少量水,这由于通常可得酸水溶液。可容许水作为甘油中的杂质。在反应中产生水,但在开始时,仅反应组合物中存在显著量水似乎造成不希望的大的微晶尺寸。
本发明的另一方面涉及一种包含有机聚合物(至少一种)和0.001-20重量%,例如0.01-20重量%、0.001-10重量%、0.001-5重量%或0.01-1重量%(基于聚合物组合物)的如上文所述的单甘油酸锌(GMS-ZMG)的聚合物组合物。
有机聚合物的实例为:
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)、极低密度聚乙烯的混合物,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.)至4.)的共聚物可为无规或嵌段共聚物、均相或非均相的或高结晶均聚物。
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挠性的(塑化)。
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。聚氨酯通过使(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)反应形成。
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。聚碳酸酯优选通过使双酚化合物与碳酸化合物,特别是光气反应或在熔体转酯化方法中,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-羟基苯基)-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和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。聚碳酸酯的合适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至55行)、DE19943642(参见第5页第25至34行)和US5367044中并且描述于其中所引用的文献中。此外可将所用聚碳酸酯内部支化,在聚碳酸酯制备的上下文中未加入支化剂。内部支化的一个实例为所谓的Fries结构,如EP1506249中对熔融聚碳酸酯所公开。链终止剂可此外用于聚碳酸酯制备中。苯酚(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。通过使已提及的双酚、至少一种芳族二羧酸和任选地碳酸等同物反应来获得聚酯碳酸酯。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'-二苯基二羧酸或4,4'-二苯基二羧酸和二苯甲酮-二羧酸。至多80mol-%,优选20-50mol-%的聚碳酸酯中的碳酸酯基团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表示苯乙烯,I表示异戊二烯,B表示聚丁二烯,EB表示乙烯/丁烯嵌段,EP表示聚乙烯/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α-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)、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、Neoprene、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),还称为布纳N橡胶氢化的腈橡胶(HNBR)Therban和Zetpol,EPM(乙烯丙烯橡胶,乙烯与丙烯的共聚物)和EPDM橡胶(乙烯丙烯二烯烃橡胶,乙烯、丙烯与二烯组分的三元共聚物)、表氯醇橡胶(ECO)、聚丙烯酸橡胶(ACM、ABR)、聚硅氧烷橡胶(SI、Q、VMQ)、氟硅氧烷橡胶(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)、热塑性弹性体(TPE),用于织品制备中的节枝弹性蛋白和弹性蛋白、聚硫橡胶、Elastolefin、弹性纤维。
35.热塑性弹性体,例如苯乙烯类嵌段共聚物(TPE-s)、热塑性烯烃(TPE-o)、弹性掺杂物(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's(R-TPO's)、聚烯烃塑料(POP's)、聚烯烃弹性体(POE′s)。
优选的有机聚合物可选自聚烯烃(如聚乙烯、聚丙烯等)、聚氯乙烯、聚苯乙烯、聚丙烯酰胺、聚酯、其聚酰胺共聚物以及丙烯腈、丁二烯和苯乙烯中的一种或多种与彼此或与另外共聚单体的共聚物。优选聚烯烃,尤其优选聚丙烯。聚合物可加工成聚合制品,如纤维、膜、织物、包装或涂层。
含有并入的改性剂的单甘油酸锌(GMS-ZMG)通常以基于聚合物共混物的总重量为约0.01重量%至20重量%的量存在。在最终塑料产物中,浓度通常为0.01-2%,但用于制备该产物的母料组合物可含有至多20重量%。有机聚合物可以基于聚合物共混物的总重量为约80重量%至99.99重量%的量存在。
聚合物中的GMS改性的单甘油酸锌(GMS-ZMG)的量优选不超过400ppm,且甚至可为380ppm或更小、360ppm或更小、340ppm或更小、320ppm或更小或300ppm或更小。该量可低至100ppm或50ppm或更小。约200ppm+/-100ppm或+/-50ppm为合适的目的量。等规聚丙烯中的常规成核剂(例如未改性ZMG)的典型量通常为500ppm或更大,因此该减小的量表明显著的成本节省,同时对所实现的结晶时间无不利影响。
聚合物组合物相对于聚合物组合物的重量可进一步包括少量,例如0.001-20%,优选0.00-5%的常规配混成分。
常规配混成分的实例为:
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,
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)与3-溴-1-丙烯、经氧化氢化的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)和其组合的反应产物。
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。
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-(1,1-二甲基丙基)苯基三酯(CAS编号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编号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、山萮酸镁、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.塑化剂,其中该塑化剂选自二(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、偏苯三酸三辛酯、偏苯三酸三(异壬酯)、环氧化大豆油、环己烷-1,2-二甲酸二(异壬酯)、2,4,4-三甲基-1,3-戊二醇二异丁酸酯。
根据本发明使用的塑化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,该塑化剂选自邻苯二甲酸丁基苯甲基酯、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烷基酯、邻苯二甲酸二异十三烷基酯、二异(C11、C12、C13)邻苯二甲酸酯、邻苯二甲酸二(正丁基酯)、二(正C7、C9)邻苯二甲酸酯、二(正C6、C8、C10)邻苯二甲酸酯、邻苯二甲酸二异(正壬基酯)、二(正C7、C9、C11)邻苯二甲酸酯、二(正C9、C11)邻苯二甲酸酯、邻苯二甲酸二(正十一烷基酯)、三(正C8、C10)偏苯三酸酯、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)、二(正C7、C9)己二酸酯、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)、己二酸或戊二酸和丙二醇或丁二醇或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)、磷酸三甲苯基酯、对苯二甲酸二(2-乙基己基酯)、环己烷-1,2-二羧酸二(异壬基酯)及其组合。在一个尤其优选的实施方案中,该塑化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烷基酯、邻苯二甲酸二异十三烷基酯、二异(C11、C12、C13)邻苯二甲酸酯、邻苯二甲酸二(正丁基酯)、二(正C7、C9)邻苯二甲酸酯、二(正C6、C8、C10)邻苯二甲酸酯、邻苯二甲酸二异(正壬基酯)、二(正C7、C9、C11)邻苯二甲酸酯、二(正C9、C11)邻苯二甲酸酯、邻苯二甲酸二(正十一烷基酯)、三(正C8、C10)偏苯三酸酯、苯偏三酸三(2-乙基己基酯)、苯偏三酸三(异辛基酯)、苯偏三酸三(异壬基酯)、二(正C7、C9)己二酸酯、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)、己二酸或戊二酸和丙二醇或丁二醇或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-1,2-二羧酸二(异壬基酯)和其组合。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。
可将配混成分如颜料、着色剂、填料、增充剂、阻燃剂、抗臭氧剂、抗氧化剂、脱模剂、酸清除剂、塑化剂、稳定剂(如pH稳定剂)、乳化剂、硫化剂、聚合引发剂、敏化剂等并入聚合物组合物中。
本发明的另一实施方案为一种由本发明的聚合物组合物制成的成型制品。
合适成型制品的实例为:
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、内部应用、外部应用,特别是保险杠、仪表板、电池、后和前衬板、在引擎盖下的模制品部分、帽架、车厢衬板、车内衬板、气囊包、配件(照明)用的电子模制品、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、车身模制品、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、门雕饰板、控制面板、仪器板、座椅、框架、外皮、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。用于飞机、铁道、机动车(汽车、摩托车)、卡车、轻型卡车、公交车、有轨电车、自行车的装置,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,特别是移动式马桶、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、人工草皮、阿斯特罗特夫尼龙草皮(astroturf)、用于体育馆圆形场地(运动)的人工覆盖物、用于体育馆圆形场地(运动)的人工地板和胶带。
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、游泳池衬垫、池衬垫、池塘衬垫、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)农业薄膜(温室覆盖物、隧道、多隧道、微型隧道、“骨架结构(raspayamagado)”、多跨度、低行走隧道、高隧道、覆盖物、青贮料、仓袋、仓延伸段、熏蒸、气泡、keder、solawrap、热量、捆绑包装、拉伸捆绑包装、保育器、薄膜套管),尤其是在农用化学品的密集型应用存在下;其他农业应用(例如非织造土壤覆盖物)、网(由条带、多长丝及其组合制成)、防水布。该农业膜可为单层结构或多层结构,通常由3、5或7个层组成。这可得到薄膜结构如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表示不同聚合物和增粘剂。然而,相邻层还可经连接使得最终薄膜制品可由偶数个层组成,即2、4或6个层如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)泡沫剂(密封、绝缘、阻挡),运动和休闲垫。
V-5)封闭剂
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。
申请人已发现含有本文所述的微晶尺寸和/或根据本文所述的方法制备的单甘油酸锌提供了改进结晶特征。这些改进对于丙烯均聚物和共聚物和聚丙烯共混物尤其明显。这些改进包括以下:
1.较高Tc在较低成核剂负载下产生。在200ppm下加入等规聚丙烯(下文称为“iPP”-LyondellBasell,Moplen HP400N等规聚丙烯均聚物,MFI=11g/10min),甘油单硬脂酸酯改性的单甘油酸锌(GMS-ZMG)得到124.1℃的Tc,然而未改性ZMG得到仅120.6℃的Tc。为获得123.8℃的Tc(与200ppm下的GMS-ZMG大致相同),需要600ppm ZMG。HP400N的Tc(在无成核剂下)为117.0℃。
2.与未改性ZMG相比,在200ppm下使用本申请的改性ZMG显著改进(缩短)在140℃下实现50%聚合物结晶(t1/2)所需的时间:相对于ZMG的t1/2为14.6min,GMS-ZMG获得7.2min的t1/2。为仅使用未改性ZMG获得7.1min的t1/2,实际上需要600ppm的ZMG。HP400N本身在40min内不结晶。
与相同负载的未改性单甘油酸锌相比,改性单甘油酸锌(GMS-ZMG)提供在200ppm下等规聚丙烯中约3.4℃的Tc的增加。
在基于聚烯烃作为有机聚合物的组合物中,聚烯烃中以给定负载水平使用单甘油酸锌提供了比以在<100>方向上微晶尺寸大于30nm或在<011>方向上大于60nm,或通过<100>/<011>相干域长度计算的纵横比大于0.65的单甘油酸锌的相同负载水平所获得的结晶温度更高的聚烯烃结晶温度(即在与为未改性单甘油酸锌的单甘油酸锌或Bos形式的单甘油酸锌相比时)。在等规聚丙烯中,在等规聚丙烯中以给定负载水平使用本申请的改性单甘油酸锌提供的在140℃下实现50%聚合物结晶的时间(t1/2)比以相同负载实现的对比单甘油酸锌的时间少至少40%(即该对比单甘油酸锌在<100>方向上的微晶尺寸大于30nm,或在<011>方向上大于60nm,或通过<100>/<011>相干域长度计算的纵横比大于0.65)。
在权利要求和前述描述中,在本发明的各种实施方案中,除了由于明确的语言或必要的暗示上下文此外要求之外,措词“包含(comprise)”或变形(comprises或comprising)以包括性意义使用,即指定所述特征的存在但不排除存在或加入其他特征。
实施例
现将参照以下非限制性实施例进一步详细描述本发明。
程序
表征技术
XRD分析使用Phillips 1140衍射仪采用铜源(40kV,25mA)和石墨单色器或BrukerD2Phaser采用铜源(30kV,10mA)根据Bragg-Brentano(θ-2θ)几何结构设定进行。在所要2θ值(2θ=5-35°)之间扫描。例如,将“粉末样品”安放在标准样品固持器上(毫克-数克)。将聚合物样品在挤压机中挤压,且在金属板之间压制,以获得平坦零件,在水浴中冷却且切割以设定尺寸,以适用于可用样品固持器(<3mm厚度)中。
使用Scherrer等式,使用通过XRD(β)、X射线波长(λ)、布拉格角度(以度表示;(峰值的2θ值)/2)、无量纲形状因子(K,取成0.9;出于比较始终使用相同K)测量的测量半高全宽(FWHM)值来计算在<100>和(011)各方向上的平均微晶尺寸(平均相干域长度)。Scherrer等式为τ=Kλ/βcosθ。应注意,忽略由于仪器的线增宽,且假定线增宽仅来自相干结长度变化。
SEM显微法使用JEOL JSM-7001F扫描电子显微镜进行。将样品安放在碳带上且用Pt溅射涂覆。
如下制备结晶测试的样品:将半结晶等规聚丙烯(iPP)均聚物裸树脂(MoplenHP400N(来自LyondellBasell,Australia))用作iPP。通过使iPP与所需量的成核剂混合来制备不含成核剂(对照)或指定量的成核剂的iPP样品。首先进行彻底手动混合(粉末+iPP珠粒),然后挤压。制备1重量%或2000ppm母料(取决于该组对比实验)并挤压。将挤压线料粒化且以所要浓度(200ppm或600ppm)再次挤压。(在一种情况下,明确提及已挤压200ppm材料两次)。所用挤压机为CRD阻隔性单螺杆(直径=25mm;L/D=25)挤压机,由RauwendaalExtrusion Eng.Inc.制备,连接至Haake Rheocord90。将四个温度区分别设定为170℃、175℃、180℃和180℃(模具)。螺杆速度为100rpm。
实施例1-制备GMS改性的单甘油酸锌(GMS-ZMG)
在Z叶片混合器中将ZnO(656.4g)和GMS(72.3g)均化并加热。然后加入668.5g甘油。然后加入74.3g甘油+8.7g水+4.5g 90%乙酸,且进一步均化。使温度升至110℃。一旦完全反应,即细干燥粉末,则断开热。所达到的最高温度为约120℃,但反应期间的温度基本上在100-120℃范围内。在反应完成后在该温度范围内继续混合,在此期间形成附聚产物。将所得附聚(粉末)产物针磨。
然后进行XRD分析以测定平均微晶尺寸。XRD图显示于图1中。图1的XRD图中的线之一为实施例1的产物(标记的GMS-ZMG),且第二根线为未改性ZMG。在2θ=10.9°处的峰值是由于由(100)miller指数描述的平面组(卡片堆积)。与未改性ZMG样品的40nm相比,实施例1的GMS-ZMG在<100>方向上的相干域长度(微晶尺寸)经计算为17nm。2θ=17.2°处的峰值对应于由miller指数(011)描述的平面组(各卡片内的平面)。在此方向上GMS-ZMG和未改性ZMG二者的微晶尺寸均为45nm。
与未改性ZMG相比,对实施例1的附聚产物进行SEM成像。SEM图像显示于图2a和图2b中。各图像的比例尺为1μm。两种产物具有不同形态。图2a(A)的图像为未改性的ZMG。图2b(B)的图像为实施例1的GMS-ZMG产物。实施例1的产物显示出微晶的附聚集合。附聚微晶显示出“鱼鳞”样表面图案(对于单个颗粒),这表明小得多的微晶不完美地堆积,其中边缘暴露。
实施例1的GMS-ZMG产物的额外SEM图像显示于图3a、图3b和图4中。
制备含有200ppm未改性ZMG、600ppm未改性ZMG、200ppm实施例1的GMS-ZMG和无成核剂的对照组(“空白组”)的iPP(等规聚丙烯)的样品。使用差示扫描量热法(DSC)评估样品的结晶行为,由此相对于样品温度(℃)测量热量流动(样品内/外)(以mW为单位),以评估含有成核剂的聚丙烯样品的结晶温度。
下表以表格形式显示出结果:
样品 | Tc |
600ppm未改性ZMG | 123.8℃ |
200ppm未改性ZMG | 120.6℃ |
200ppm GMS-ZMG | 124.1℃ |
仅iPP(HP400N) | 117.0℃ |
上表显示出含有200ppm实施例1的GMS-ZMG的样品的Tc与含有600ppm(三倍量)未改性ZMG的样品的Tc大约相同。与相同量的未改性ZMG相比,在200ppm下实施例1的GMS-ZMG的Tc较高。
可以看出在140℃下等温t1/2的类似趋势:
样品 | t<sub>1/2</sub> |
600ppm未改性ZMG | 7.1min |
200ppm未改性ZMG | 14.6min |
200ppm GMS-ZMG | 7.2min |
仅iPP(HP400N) | 在40分钟内不结晶。 |
对比例
在sigma混合器中在混合下将湿润水锌矿(等同于50.0kg氧化锌)缓慢加入甘油(53.5kg)。在混合下缓慢加入甘油单硬脂酸酯(5.0kg),且将组合物混合成稀浆。混合物含有来自水锌矿的显著水-量经计算为所用水锌矿-水的浆液中70重量%水,或相对于反应组合物中的锌为1410mol%。将组合物加热至160℃并在该温度下保持16小时。制备干燥可流动粉末。
以上描述比Bos 2006的描述有效。由此制备的产物称为“水锌矿-ZMG”。
使用XRD(图5)来测量所制备的粉末(水锌矿-ZMG)的微晶尺寸,且结果,连同实施例1的产物(GMS-ZMG)和未改性ZMG的微晶尺寸测量值呈现于下表中。经计算的<100>/<011>纵横比值也包括于下表中:
实施例 | <100>尺寸 | <011>尺寸 | <100>/<011>纵横比 |
对比例的水锌矿-ZMG | 44nm | 57nm | 0.77 |
未改性ZMG | 40nm | 45nm | 0.89 |
实施例1的GMS-ZMG | 17nm | 45nm | 0.38 |
水锌矿-ZMG(对比例)在<100>方向上的微晶尺寸大致类似于未改性ZMG的微晶尺寸,但其显著高于实施例1的GMS-ZMG的微晶尺寸。值得注意的是,在所有三种情况下,在<011>方向上的微晶尺寸与GMS-ZMG的微晶尺寸具有相同数量级(尽管水锌矿-ZMG略微较长)。在GMS-ZMG(实施例1)中,尽管<011>微晶尺寸基本上保持相似(层尺寸),但<100>微晶尺寸(层堆积厚度)显著缩减。GMS-ZMG的<100>/<011>纵横比通常小于0.65,且通常小于0.44;在该情况下为0.38。显然地,这小于未改性ZMG和GMS-ZMG二者。换言之,与其他两个类型(未改性ZMG和水锌矿-ZMG)相比,根据本发明的ZMG的GMS改性形成ZMG层的较小堆积(其可更有效率地分散于聚合物中)。
实施例A:
制备含有100ppm、200ppm、600ppm或1200ppm未改性ZMG或GMS-ZMG和无成核剂的对照组(“空白组”)的iPP的样品(等规聚丙烯,均聚物,在230℃/2.16kg下熔融流动指数为8dg/min)。
使用XRD来测量未改性ZMG和GMS-ZMG的微晶尺寸且结果呈现于下表中。还包括经计算的<100>/<011>纵横比值:
实施例 | <100>尺寸 | <011>尺寸 | <100>/<011>纵横比 |
未改性ZMG | 40nm | 45nm | 0.89 |
GMS-ZMG | 25nm | 47nm | 0.53 |
使用差示扫描量热法(DSC)评估样品的结晶行为,由此相对于样品温度(℃)测量热量流动(样品内/外)(以mW为单位),以评估含有成核剂的聚丙烯样品的结晶温度。
下表以表格形式显示出结果:
样品 | Tc |
1200ppm未改性ZMG | 123.7℃ |
600ppm未改性ZMG | 126.7℃ |
200ppm未改性ZMG | 124.4℃ |
100ppm未改性ZMG | 122.1℃ |
1200ppm GMS-ZMG | 130.6℃ |
600ppm GMS-ZMG | 129.2℃ |
200ppm GMS-ZMG | 127.2℃ |
100ppm GMS-ZMG | 125.8℃ |
仅iPP(HD120MO) | 114.9℃ |
上表显示出含有100ppm GMS-ZMG的样品的Tc与含有600ppm(6倍量)未改性ZMG的样品的Tc大约相同。在该浓度扩展范围内的任何浓度下,与相同量的未改性ZMG的Tc相比,GMS-ZMG的Tc更高。
在用这些化合物制备的样品中,注入板材(2mm厚)。在熔体流动意义上模切具有根据ISO 527-2 5A(2012年)的形状的哑铃,且根据ISO 527(2012年)测试拉伸性能。结果(E-模量和屈服强度)呈现于下表中。对结晶温度观测到相同趋势。
(*)需要较高值
上表显示出含有200ppm GMS-ZMG的样品的E-模量和屈服强度显著高于含有600ppm(三倍量)未改性ZMG的样品的E-模量和屈服强度。在该浓度宽范围内的任何浓度下,与相同量的未改性ZMG的E-模量、屈服强度相比,GMS-ZMG的E-模量和屈服强度更高。
实施例B:
制备含有200ppm未改性ZMG、600ppm未改性ZMG、200ppm上述实施例的GMS-ZMG或600ppm上述实施例的GMS-ZMG和无成核剂的对照组(“空白组”)的iPP的样品(等规聚丙烯,均聚物,230℃/2.16kg下熔融流动指数为19dg/min)。使用差示扫描量热法(DSC)评估样品的结晶行为,由此相对于样品温度(℃)测量热量流动(样品内/外)(mW),以评估含有成核剂的聚丙烯样品的结晶温度。
下表以表格形式显示出结果:
样品 | Tc |
600ppm未改性ZMG | 126.0℃ |
200ppm未改性ZMG | 123.5℃ |
600ppm GMS-ZMG | 128.3℃ |
200ppm GMS-ZMG | 125.8℃ |
仅iPP(HF420FB) | 116.2℃ |
上表显示出含有200ppm GMS-ZMG的样品的Tc与含有600ppm(三倍量)未改性ZMG的样品的Tc大约相同。与相同量的未改性ZMG相比,在所有浓度下GMS-ZMG的Tc更高。
在用这些化合物制备的样品中,注入板材(2mm厚)。在熔体流动意义上模切具有根据ISO 527-2 5A(2012年)的形状的哑铃,且根据ISO 527(2012年)测试拉伸性能。结果(E-模量和屈服强度)呈现于下表中。对结晶温度观测到相同趋势。
(*)需要较高值
上表显示出含有200ppm GMS-ZMG的样品的E-模量和屈服强度显著高于含有600ppm(三倍量)未改性ZMG的样品的E-模量和屈服强度。在此浓度范围内的任何浓度下,与相同量的未改性ZMG的E-模量、屈服强度相比,GMS-ZMG的E-模量和屈服强度更高。
实施例C:
制备含有200ppm未改性ZMG或200ppm上述实施例的GMS-ZMG和无成核剂的对照组(“空白组”)的iPP raco的样品(等规聚丙烯,无规共聚物,在230℃/2.16kg下熔融流动指数为8dg/min)。使用差示扫描量热法(DSC)评估样品的结晶行为,由此相对于样品温度(℃)测量热量流动(样品内/外)(以mW为单位),以评估含有成核剂的聚丙烯样品的结晶温度。
下表以表格形式显示出结果:
样品 | Tc |
200ppm未改性ZMG | 116.2℃ |
200ppm GMS-ZMG | 118.4℃ |
仅iPP raco(RD204CF) | 114.2℃ |
上表显示出含有200ppm GMS-ZMG的样品的Tc显著高于在相同浓度下未改性ZMG的Tc。
在用这些化合物制备的样品中,注入板材(2mm厚)。在熔体流动意义上模切具有根据ISO 527-2 5A(2012年)的形状的哑铃,且根据ISO 527(2012年)测试拉伸性能。结果(E-模量和屈服强度)呈现于下表中。对结晶温度观测到相同趋势。
(*)需要较高值
上表显示出含有200ppm GMS-ZMG的样品的E-模量和屈服强度高于在相同浓度下未改性ZMG的样品的E-模量和屈服强度。
Claims (20)
1.一种微晶附聚物形式的单甘油酸锌,其中基于平均相干域长度的微晶尺寸通过Scherrer等式经由粉末X射线衍射测得在<100>方向上小于30nm(沿<100>晶带轴的尺寸),且在<011>方向上小于60nm(沿<100>晶带轴的尺寸);且通过<100>/<011>相干域长度计算的纵横比小于0.65,优选小于0.56。
2.根据权利要求1的单甘油酸锌,其含有改性剂。
3.根据权利要求2的单甘油酸锌,其中所述改性剂为甘油羧酸酯。
4.根据权利要求3的单甘油酸锌,其中所述甘油羧酸酯为甘油的饱和脂肪酸酯。
5.根据权利要求4的单甘油酸锌,其中所述甘油羧酸酯为甘油单硬脂酸酯。
6.根据权利要求2-5中任一项的单甘油酸锌,其中改性剂的量相对于所述单甘油酸锌为1.0-5.0mol%。
7.一种微晶附聚物形式的单甘油酸锌,含有1.0-5.0mol%的甘油羧酸酯。
8.一种用于制备根据权利要求1的单甘油酸锌的方法,包括使不同于水锌矿的锌化合物与甘油和改性剂在酸催化剂的存在下反应,其中:
-所述锌化合物选自由如下组成的组:氧化锌、碳酸锌、氢氧化锌、羧酸锌及其组合,或/和
-所述反应在基于所述反应组合物的总重量为小于10重量%的水的存在下进行。
9.根据权利要求8的方法,其中所述改性剂为甘油羧酸酯。
10.根据权利要求8或9的方法,其中所述甘油的量相对于所述锌化合物为90-110mol%。
11.根据权利要求8-10中任一项的方法,其中所述改性剂的量相对于所述锌化合物为1.0-5.0mol%。
12.根据权利要求8-11中任一项的方法,其中所述酸催化剂的量相对于所述锌化合物为0.2-5mol%。
13.一种单甘油酸锌,可通过根据权利要求8-12中任一项的方法获得。
14.一种组合物,包含有机聚合物和根据权利要求1-7中任一项的单甘油酸锌。
15.根据权利要求14的组合物,其中所述有机聚合物选自由如下组成的组:聚烯烃、聚氯乙烯、聚苯乙烯、聚丙烯酰胺、聚酯、聚酰胺及其共聚物,以及丙烯腈、丁二烯和苯乙烯中的一种或多种与彼此或与另外共聚单体的共聚物。
16.根据权利要求14或15的组合物,其中所述单甘油酸锌相对于所述有机聚合物的重量以0.001-20%、优选0.005-5%的量存在。
17.根据权利要求14的组合物,其中所述有机聚合物为聚烯烃,且在聚烯烃中呈给定负载水平的单甘油酸锌提供了比以在<100>方向上大于30nm或在<011>方向上大于60nm的微晶尺寸或通过<100>/<011>相干域长度计算的纵横比大于0.65的单甘油酸锌的相同负载水平所实现的结晶温度更高的聚烯烃结晶温度。
18.根据权利要求14的组合物,其中所述有机材料为等规聚丙烯,且在所述等规聚丙烯中呈给定负载水平的单甘油酸锌提供在140℃下实现50%聚合物结晶的时间(t1/2)比以相同负载水平的具有在<100>方向上大于30nm和/或在<011>方向上大于60nm的微晶尺寸或具有通过<100>/<011>相干域长度计算大于0.65的纵横比的单甘油酸锌所实现的时间少至少40%。
19.根据权利要求1-7中任一项的单甘油酸锌在提高有机聚合物的结晶温度或机械特性,优选E-模量或屈服强度中的用途。
20.根据权利要求1-7中任一项的单甘油酸锌作为有机聚合物中的成核剂的用途。
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SG11201910097PA (en) | 2019-11-28 |
AU2018263810A1 (en) | 2019-11-14 |
CN110678510B (zh) | 2022-03-29 |
BR112019022852A2 (pt) | 2020-05-26 |
JP2020518677A (ja) | 2020-06-25 |
CA3062107A1 (en) | 2018-11-08 |
TW201902864A (zh) | 2019-01-16 |
BR112019022852B1 (pt) | 2023-03-07 |
EP3619261B1 (en) | 2022-08-10 |
KR102550380B1 (ko) | 2023-07-04 |
PL3619261T3 (pl) | 2023-01-16 |
US20200079929A1 (en) | 2020-03-12 |
RU2019139027A3 (zh) | 2021-09-30 |
RU2019139027A (ru) | 2021-06-03 |
TWI788348B (zh) | 2023-01-01 |
EP3619261A1 (en) | 2020-03-11 |
US11414531B2 (en) | 2022-08-16 |
JP7184876B2 (ja) | 2022-12-06 |
AU2018263810B2 (en) | 2023-10-05 |
WO2018202707A1 (en) | 2018-11-08 |
ES2929776T3 (es) | 2022-12-01 |
KR20190140056A (ko) | 2019-12-18 |
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