CN107001503A - 用于提高减粘裂化效率的过氧化物和羟胺酯的协同减粘裂化组合物 - Google Patents
用于提高减粘裂化效率的过氧化物和羟胺酯的协同减粘裂化组合物 Download PDFInfo
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- CN107001503A CN107001503A CN201580066565.2A CN201580066565A CN107001503A CN 107001503 A CN107001503 A CN 107001503A CN 201580066565 A CN201580066565 A CN 201580066565A CN 107001503 A CN107001503 A CN 107001503A
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Abstract
用于提高聚丙烯聚合物在低于250℃的熔融挤出温度下的减粘裂化效率的过氧化物和羟胺酯的协同减粘裂化组合物和其在减粘裂化聚丙烯中的用途。本发明进一步地涉及该减粘裂化聚丙烯在制备具有改进的阻隔性的熔喷无纺布中的用途。
Description
技术领域
本发明涉及用于在低于250℃的熔融挤出温度下提高聚丙烯聚合物的减粘裂化效率的过氧化物和羟胺酯的协同减粘裂化组合物和其在减粘裂化聚丙烯中的用途。本发明还涉及此类减粘裂化聚丙烯聚合物在制备具有改进的阻隔性的熔喷无纺布中的用途。
背景技术
通过常规复合方法(例如通过挤出或注射成型)可控制备聚烯烃等级(具有不同摩尔质量、熔体粘度、密度、摩尔质量分布等的聚合物类型)是聚合物制造商和聚合物加工者/复合者采用的常规方法。
通过该聚合物工艺步骤设定的所需参数，例如熔体粘度，严重依赖于受控反应性和所用添加剂的作用方式。
使用自由基形成剂来改进聚烯烃类的熔体粘度(流变性)是一般已知的方法。其是否会导致分子量的降低(降解)或分子量的增加(交联)主要取决于聚烯烃的化学结构。
在聚合物加工过程中，聚丙烯类的聚合物与自由基形成剂的反应通常导致聚合物的降解，而聚乙烯类的聚合物倾向于交联。
聚丙烯(PP)的可控降解产生了具有较低分子量和较窄分子量分布的产物，这是商业上生产“可控流变性”聚丙烯(CR-PP)的重要方法。虽然通过合成方法或催化剂体系(茂金属催化剂、齐格勒催化剂)的优化可获得特定的PP等级(“反应器等级”)，但在加工技术中经常通过合成后的加工步骤改进标准PP等级。
已知的降解过程或是热降解(尤其在高于280℃的温度下)，或是在存在自由基发生剂的情况下进行。在加工技术中，自由基诱导过程在高于180℃的温度下在挤出机或注射成型机中进行。使用的自由基发生剂是在加工步骤中以稀释形式(PP Mastermix，在油中稀释，在无机载体上稳定)或直接作为液体加入的有机过氧化物。在给定的加工条件下，过氧化物分解成自由基，其引发链裂解反应并形成具有所需流变性能(熔体粘度)的聚合物。PP降解形成具有较低分子量(较高熔体流动速率(MFR))的产物，最重要的是，较低的熔体粘度通常表示为粘性裂化或减粘裂化过程。
CR-PP等级主要用于膜、纤维应用和注射成型应用，其中，低熔体粘度是经济加工的先决条件。现今，工艺技术需要各种的熔体粘度或分子量。
除了分子量之外，影响聚合物的加工性能的另一个参数是分子量分布(MWD)。虽然在纤维纺丝工艺中，在低拉伸速度(pull-off speed)下，具有宽MWD的聚合物等级显示出改进的聚合物链的取向性能，但是对于高拉伸速度和宽的MWD来说，情况恰恰相反。因此，为了在纺丝过程中实现改进的连续性，窄的MWD在高拉伸速度下是必不可少的。
除了过氧化物之外，其它自由基来源也是已知的，例如基于枯基体系的C-自由基发生剂，但它们只能在280℃以上的温度下使用。
也已知使用羟胺酯类作为自由基源。
WO 97/49737描述了使用所谓的NOR-HALS(HALS：受阻氨基光稳定剂)化合物在280℃以上的温度下降低聚合物分子量的方法，该NOR-HALS化合物包含以下基团：
其中G为氢或甲基，且G1和G2各自为氢、甲基或共同为含氧基(oxo)。这些已知的NOR-HALS化合物仅在280℃以上的温度下才能产生明显的聚合物降解。
WO 01/90113公开了降低聚丙烯、丙烯共聚物或聚丙烯共混物的分子量的方法，其中将下式的羟胺酯加入到待降解的聚丙烯聚合物中，并将混合物加热到低于280℃的温度：
其中，除了别的之外，Ra'是单酰基基团，R1-R4是烷基取代基。
根据WO 2007/126994，可以使用本领域已知的用于降低聚烯烃化合物、特别是丙烯聚合物的分子量或对聚烯烃化合物、特别是丙烯聚合物进行减粘裂化的任何羟胺酯。参考WO01/90113，其中大致描述了此类合适的羟胺酯。此外，其说明了优选的羟胺酯是由CibaSpecialty Chemicals Corporation(现由BASF)商售的CR76。将降解的聚丙烯用于无纺布过滤元件。
从Alexandros Psarreas在2006年提交给滑铁卢大学的有关Nitroxide-MediatedControlled Degradation of Polypropylene的论文中(例如第14页)，已知CR76在250℃的熔融挤出温度下显示出与过氧化物相当的减粘裂化性能。只有在较高的温度下，如从270℃起，特别是从280℃起，CR76的性能才会好于过氧化物的性能。
EP 1 282 630描述了羟胺酯用于聚丙烯的可控降解中的用途，其中羟胺酯具有下式
其中，
Ra'是单酰基或二酰基基团；R1-R4各自为C1-C6烷基；和
R5和R6各自彼此独立地为氢、C1-C6烷基或C6-C10芳基；或
R5和R6共同为氧。在EP 1 282 630中指出，在具体的实施方案中，除了羟胺酯(I)之外，可以将其它自由基来源，例如合适的双偶氮化合物、过氧化物或氢过氧化物加入待降解的聚合物中。在实施例中仅针对使用羟胺酯与DTBPH(2,5-双-叔丁基过氧-2,5-二甲基己烷)连续降解(2步挤出)聚丙烯示出了两种自由基源的用途。EP 1 282 630没有显示使用这种组合的任何效果。
EP 1 786 861公开了在WO 01/90113中所述的羟胺酯类(特别是下式的羟胺酯)
与硫化合物(如下式的硫代化合物1(“硫代-1”))在较低的熔融挤出温度(如250℃)下用于降解聚丙烯聚合物的用途。
如本发明的实验部分的比较例所示，这种组合没有协同效应。
虽然已知有许多用于降解PP以形成具有较低分子量(较高熔体流动速率(MFR))和最重要地较低的熔体粘度的产物的替代方案，但对于改进该减粘裂化过程，即找到特别是在低于250℃的熔融挤出温度下需要较少降解剂(即自由基发生剂)以实现相同的减粘裂化效率，并产生可以转化为具有改进的阻隔性能的熔喷无纺布的CR-PP等级的解决方案具有持续的需求。
令人惊奇的是，本发明人发现，可以使用过氧化物和羟胺酯的组合来达到上述目的。
发明内容
因此，本发明在第一方面涉及用于在低于250℃的熔融挤出温度下提高聚丙烯聚合物的减粘裂化效率的过氧化物和羟胺酯的协同减粘裂化组合物，其包括在1重量％(i)：99重量％(ii)至99重量％(i)：1重量％(ii)的范围内的过氧化物(i)和羟胺酯(ⅱ)，其中将过氧化物(i)和羟胺酯(ii)作为混合物或单独成分加入到待减粘裂化的聚丙烯中。
此外，本发明涉及包括过氧化物(i)和羟胺酯(ii)的该组合物用来提高聚丙烯聚合物在低于250℃的熔融挤出温度下根据ISO 1133测量的熔体流动速率MFR2(230℃/2.16kg)的用途。
另一方面，本发明涉及通过向待减粘裂化的聚丙烯聚合物中加入过氧化物(i)和羟胺酯(ⅱ)的协同减粘裂化组合物来提高聚丙烯聚合物在低于250℃的熔融挤出温度下的减粘裂化效率的方法。
另一方面，本发明涉及用协同减粘裂化组合物减粘裂化的聚丙烯聚合物在制备具有改进的阻隔性的熔喷无纺布中的用途。
在下文中，将更详细地描述本发明。
根据本发明的协同减粘裂化组合物包含过氧化物(i)和羟胺酯(ii)。
过氧化物(i)
典型的过氧化物减粘裂化剂是2,5-二甲基-2,5-双(叔丁基-过氧)己烷(DHBP)(例如以商品名Luperox 101和Trigonox 101出售的)、2,5-二甲基-2,5-双(叔丁基-过氧)己炔-3(DYBP)(例如以商品名Luperox 130和Trigonox 145出售的)、过氧化二异丙苯(DCUP)(例如以商品名Luperox DC和Perkadox BC出售的)、过氧化二叔丁基(DTBP)(例如以商品名Trigonox B和Luperox Di出售的)、过氧化叔丁基异丙苯(BCUP)(例如以商品名Trigonox T和Luperox 801出售的)和双(叔丁基过氧异丙基)苯(DIPP)(例如以商品名Perkadox 14S和Luperox DC出售的)。
优选的过氧化物是5-二甲基-2,5-双(叔丁基-过氧)己烷(DHBP)和过氧化叔丁基异丙苯(BCUP)。
使用一种特定的过氧化物或不同过氧化物的混合物均在本发明的范围内。
过氧化物可以是母料的一部分。
在本发明的意义上，“母料”是指丙烯聚合物与自由基形成剂(过氧化物)的浓缩预混物。
基于母料的总组成，过氧化物化合物可以以1至50重量％、例如5至40重量％的范围优选地包含在过氧化物母料组合物中。
羟胺酯(ii)
合适的羟胺酯选自现有技术中已知的羟胺酯类的组，如WO 01/90113中公开的那些。一种商售可得的合适的羟胺酯是例如由BASF商售的CR76。
优选的羟胺酯(ii)是下式的化合物
其中Ra表示酰基；
Rb和Rc之一表示氢，另一个表示取代基；或者
Rb和Rc都表示氢或相同或不同的取代基；或者
Rb和Rc共同表示氧；
R1-R4各自表示C1-C6烷基；和
R5和R6各自彼此独立地表示氢、C1-C6烷基或C6-C10芳基；
或R5和R6共同表示氧。
在羟胺酯(I)中，关于Ra中定义的术语酰基优选地表示选自由-C(＝O)-H、-C(＝O)-C1-C19烷基、-C(＝O)-C2-C19烯基、-C(＝O)-C2-C4烯基-C4-C10芳基、-C(＝O)-C6-C10芳基、-C(＝O)-O-C1-C6烷基、-C(＝O)-O-C6-C10芳基、-C(＝O)-NH-C1-C6烷基、-C(＝O)-NHC6-C10芳基和-C(＝O)-N(C1-C6烷基)2组成的组的酰基基团；
酰基基团Ra中的C1-C19烷基是例如C1-C6烷基(例如甲基、乙基、正丙基或异丙基或正、仲或叔丁基或直链或支链的戊基或己基)、或C7-C19烷基(例如直链或支链的庚基、辛基、异辛基、壬基、叔壬基、癸基或十一烷基)、或直链C11-C19烷基，其与-(C＝O)-基团形成具有偶数个C原子的C14-C20烷酰基(alkanoyl)，例如月桂酰(C12)、肉豆蔻酰(C14)、棕榈酰(C16)或硬脂酰(C18)。
C6-C10芳基是例如碳环单芳基或二芳基、优选单芳基，例如苯基，其可以被合适的取代基(例如C1-C4烷基(例如甲基、乙基或叔丁基)、C1-C4烷氧基(例如甲氧基或乙氧基)或卤素(例如氯))单取代或二取代。在二取代的情况下，优选2位和6位。
上述酰基基团Ra可以被合适的取代基(例如氟或氯)以自由价取代，并优选地是甲酰基、乙酰基、三氟乙酰基、新戊酰基、丙烯酰基、甲基丙烯酰基、油酰基、肉桂酰基、苯甲酰基、2,6-二甲苯酰基、叔丁氧基羰基、乙基氨基甲酰基或苯基氨基甲酰基。
作为R1-R4的C1-C6烷基优选为C1-C4烷基、特别是C1-C2烷基，例如甲基或乙基。
在优选的实施方案中，R1-R4是甲基或乙基。可选地，R1-R4中的一至三个取代基是乙基。其余的取代基是甲基。
R5和R6优选为氢。作为R5和R6的C1-C6烷基或C6-C10芳基优选为甲基或苯基。
羟胺酯(I)是已知的或可以通过已知方法制备的，例如在常规的酯化反应中，通过使用酸Ra-OH或其反应性官能衍生物(例如酰卤Ra-X(例如酰氯)或酸酐(如(Ra)2O))使相应的>N-OH化合物进行酰基化来制备，酸Ra-OH引入Ra基团并对应于选自例如由-C(＝O)-H、-C(＝O)-C1-C19烷基、-C(＝O)-C2-C19烯基、-C(＝O)-C2-C4烯基-C6-C10芳基、-C(＝O)-C6-C10芳基、-C(＝O)-O-C1-C6烷基、-C(＝O)-O-C6-C10芳基、-C(＝O)-NH-C1-C6烷基、-C(＝O)-NH-C6-C10芳基和-C(＝O)-N(C1-C6烷基)2组成的组的酰基。在WO 01/90113中描述了羟胺酯(I)及其制备方法。
优选的羟胺酯(I)选自由下式的空间位阻胺衍生物组成的组：
其中R1'和R2'彼此独立地表示氢或甲基；
Ra表示C1-C8烷酰基；和
Ra'表示C8-C22烷酰基。
根据更优选的实施方案，羟胺酯(I)选自由下式的空间位阻胺衍生物组成的组：
最优选的是上式的化合物，其中烷基是C17-基团。
这样的化合物是以商品名CR76商售可得的。
羟胺酯也可以以在聚合物基体中包含例如约1至50重量％、优选2至10重量％的浓度的这些化合物的母料的形式加入。
协同减粘裂化剂组合物
本发明的协同减粘裂化剂组合物包含1重量％(i)：99重量％(ii)至99重量％(i)：1重量％(ii)范围内、优选20重量％(i)：80重量％(ii)至95重量％(i)：5重量％(ii)范围内、更优选在25重量％(i)：75重量％(ii)至90重量％(i)：10重量％(ii)范围内、甚至更优选在30重量％(i)：70重量％(ii)至85重量％(i)：15重量％(ii)范围内且最优选在50重量％(i)：50重量％(ii)至85重量％(i)：15重量％(ii)范围内的过氧化物(i)和羟胺酯(ii)。
重量百分比与纯化合物(i)和(ii)有关。
过氧化物和羟胺酯可以直接作为混合物使用，也可以将组合物的两种成分分别加入到待减粘裂化的聚丙烯聚合物中。
优选地，将过氧化物和羟胺酯作为混合物直接加入到待减粘裂化的聚丙烯聚合物中。
优选地，羟胺酯以母料形式而过氧化物以纯的形式加入。
更优选地，以母料的形式加入过氧化物以及羟胺酯。
待减粘裂化的聚丙烯聚合物
待减粘裂化的聚丙烯聚合物可以包括丙烯均聚物、丙烯无规共聚物和聚丙烯共混物。
丙烯无规共聚物包括占共聚单体总量多达20重量％，优选多达10重量％的一种或两种(以各种比例)共聚单体。共聚单体的示例有：烯烃类(如1-烯烃类(例如乙烯、1-丁烯、1-戊烯、1-己烯、1-庚烯或1-辛烯)、异丁烯)、环烯烃类(例如环戊烯、环己烯、降冰片烯或亚乙基降冰片烯(ethylidenenorbome))、二烯类(如丁二烯、异戊二烯、1,4-己二烯、环戊二烯、二环戊二烯或降冰片二烯)；还有丙烯酸衍生物和不饱和羧酸酐，如马来酸酐。
优选的共聚单体是乙烯、1-丁烯、1-己烯和1-辛烯。
可以使用的聚丙烯共混物是聚丙烯与聚烯烃类的混合物，优选聚丙烯与聚丙烯基聚合物的混合物。
优选使用丙烯均聚物或丙烯无规共聚物作为原料，更优选仅使用丙烯均聚物。
聚丙烯、丙烯共聚物或聚丙烯共混物的加入可以在所有常规混合机中进行，其中聚合物被熔融并与添加剂混合。合适的机器是本领域技术人员已知的。它们主要是混合机、捏合机和挤出机。
优选在挤出机中在加工过程中通过引入协同减粘裂化剂组合物进行该方法。
特别优选的加工机器是单螺杆挤出机、反向旋转和同向旋转双螺杆挤出机、行星齿轮挤出机、环式挤出机或共捏合机。还可以使用设置有可以施加真空的至少一个除气室的加工机器。
在例如Handbuch der Kunststoffextrusion，第1卷Grundlagen，EditorsF.Hensen，W Knappe，H.Pentente，1989，第3-7页，ISBN：3-446-14339-4(第2卷Extrusionsanlagen 1986，ISBN 3-446-14329-7)中描述了合适的挤出机和捏合机。
基于待减粘裂化的聚合物的量，将浓度为约0.001至5.0重量％，特别是0.01至2.0重量％，特别优选地为0.02至1.0重量％的上述包括过氧化物(i)和羟胺酯(ii)的组合物加入到待减粘裂化的丙烯聚合物中。如上所述，该过氧化物(i)和羟胺酯(ii)可以作为单独的化合物或作为混合物加入到待减粘裂化的聚合物中。
除了协同减粘裂化剂组合物，基于聚丙烯聚合物，将所选的抗氧化剂、除酸剂和/或加工稳定剂或它们的混合物以至多3.0重量％、优选1.5重量％、更优选1.0重量％的少量加入到待减粘裂化的丙烯聚合物中。通常地我们加入总共最多1重量％的添加剂。
合适的抗氧化剂的示例是：
四(3-(3,5-二-叔丁基-4-羟基苯基)丙酸季戊四醇酯)(1010)、3-(3,5-二叔丁基-4-羟基苯基)丙酸十八烷基酯)(IRGANOX 1076)、3,3',3',5,5',5'-六叔丁基-α,α',α'-(均三甲苯-2,4,6-三基)三对甲酚(IRGANOX 1330)、二乙基双(((3,5-双(1,1-二甲基乙基)-4-羟基苯基)甲基)膦酸钙)(IRGANOX1425)、1,3,5-三(3,5-二叔丁基-4-羟基苄基)-1,3,5-三嗪-2,4,6(1H,3H,5H)三酮(IRGANOX 3114)、三(2,4-二叔丁基苯基)亚磷酸酯(168)、三(壬基苯基)亚磷酸酯、[1,1-联苯基]-4,4'-二基双亚膦酸四(2,4-二叔丁基苯基)酯(IRGANOX P-EPQ)、3,3'-硫代二丙酸双十二烷基酯(IRGANOX PS 800)、3,3'-硫代二丙酸二(十八烷基)酯(IRGANOX PS 802)；5,7-二叔丁基-3-(3,4-二甲基苯基-3H-苯并呋喃-2-酮(IRGANOX HP 136)和二硬脂酰羟胺(FS 042)。
适宜的除酸剂是例如由Patco提供的硬脂酸钙、硬脂酸锌、水滑石或乳酸钙或乳酰钙(calcium lactylate)。
聚丙烯聚合物是在升高的但仍比低于250℃的熔融挤出温度低的温度下、优选在160℃至低于250℃的熔融挤出温度下、更优选在200℃至245℃的温度下减粘裂化。
降解所需的时间可以根据温度、待降解的材料的量和所用的例如挤出机的类型而变化。
相较于在实验部分中所示的采用单独的组分，协同减粘裂化剂组合物增加了减粘裂化效率。显示出分子量降低效应高于预期，表明了两种自由基发生剂之间的协同作用。
因此，通过使用协同减粘裂化剂组合物，可以用较小量的减粘裂化剂达到所期望的结果。
因此，本发明的另一方面是包括过氧化物(i)和羟胺酯(ii)的此类组合物用于增加聚丙烯聚合物在低于250℃的熔体挤出温度下根据ISO 1133测量的熔体流动速率MFR2(230℃/2.16kg)的用途。
在另一个方面，本发明涉及通过向待减粘裂化的聚丙烯聚合物中加入过氧化物(i)和羟胺酯(ii)的协同减粘裂化组合物，增加在低于250℃的熔融挤出温度下的聚丙烯聚合物的减粘裂化效率的方法。
在另一方面，本发明涉及用协同减粘裂化组合物减粘裂化的聚丙烯聚合物在制备具有改进的阻隔性的熔喷无纺布中的用途。
由用协同减粘裂化组合物减粘裂化的聚丙烯聚合物制成的熔喷无纺布与通过单独使用过氧化物或单独使用羟胺酯而减粘裂化的聚丙烯聚合物相比，显示出了提高的阻隔性。
提高的阻隔性通过根据标准测试WSP 80.6(09)测量的较高静水压(hydrohead)值(第3次压降，cm H2O或毫巴)表示。
此外，本发明还涉及一种制品，该制品选自通常由过滤介质(过滤器)、尿布、卫生巾、内裤衬垫、成人失禁产品、防护服、手术单、手术长外衣和手术衣组成的组，基于制品总重量，该制品包括优选至少80.0重量％，更优选至少95.0重量％的量的熔喷无纺布。在本发明的一个实施方案中，制品由熔喷无纺布组成。
具体实施方式
实验部分
A.测试方法
除非另外定义，下述术语和测定方法的定义适用于包括权利要求书的本发明的上述一般描述以及适用于下面的实施例。
总的预计的MFR2的计算
在用过氧化物和羟胺减粘裂化的组合物的总的MFR遵循相加法则的条件下，总的MFR为MFR(过氧化物)+MFR(羟胺)的总和。
意思是，计算的MFR是已被测量的仅采用过氧化物减粘裂化的材料的MFR和仅采用羟胺酯减粘裂化的材料的MFR的总和(参见图1)
根据ISO 1133(230℃，2.16kg负荷)测量MFR2(230℃)。聚丙烯组合物的MFR2由材料的颗粒确定，而熔喷网的MFR2是在不高于200℃的温度下在热压机中由网制备的压塑板的裁片上测定的，所述裁片具有与颗粒尺寸相当的尺寸。
静水压
利用静水压测试确定的静水压或耐水性是根据在2009年12月发布的WSP(全球战略合作伙伴)标准测试WSP 80.6(09)来测定的。本工业标准又是基于ISO 811:1981并且使用100cm2的样品，在23℃下进行，其中用纯净水作为测试液体且水压的增加速率为10cm/min。该测试中X cm的H2O柱高度对应于X毫巴的压力差。
过滤效率
平板过滤介质的空气过滤效率是基于EN 1822-3，采用400cm2的测试过滤面积来测定的。颗粒截留利用癸二酸二乙基己基酯(DEHS)的常见气溶胶来测试，在0.1μm尺度的分级分析中计算直径为0.4微米级分的效率。利用16m3·h-1的气流，对应于0.11m·s-1的气流速度。
B.实施例
所用材料：
PP-均聚-1：HC001A-B1：密度为905kg/m3、MFR(2.16kg，230℃)为约3.7g/10min的丙烯均聚物。其由Borealis配给。
PP-均聚-2：HJ120UB：MFR2(2.16kg，230℃)为75g/10min、密度为0.905g/cm的Borealis的丙烯均聚物
PP-均聚-3：HD120MO：MFR2(2.16kg，230℃)为9g/10min、密度为0.905g/cm的Borealis的丙烯均聚物
抗氧化剂(AO)：由BASF提供的Irganox 1010(FF)
除酸剂(AS)：由Faci提供的硬脂酸钙。
纯POX：纯过氧化物：2,5-二甲基-2,5-二(叔丁基-过氧)己烷(DHBP)(CAS号78-63-7；由AkzoNobel，NL以商品名Trigonox 101出售)
过氧化物(POX PP5％ig)：PP中的母料5％：由United Initiators生产的DHBP-5-ICS。(在95％PP中的5％的2,5-二甲基-2,5-二(叔丁基-过氧)己烷(DHBP)
羟胺酯：CR 76，PP中的母料3.3重量％，由BASF提供(MB)
硫代化合物1：1-十八硫醇，CAS号2885-00-9，测定98％，购自Sigma Aldrich，原样使用。
实施例IE1至IE3+CE1至CE5
在240℃下，采用通过量为7kg/h的挤出机ZSK 18，将X重量％的PP-均聚-1与0.1重量％的Irganox 1010(FF)、0.05重量％的硬脂酸钙(CAS号1592-23-0)、y重量％过氧化物母料和z重量％的CR 76母料进行混合。
以重量％计的量示于表1。此外，MFR2(2.16kg，230℃)的值在表1中给出。
表1：
IE........本发明实施例
CE......比较例
表2显示了与实际MFR2(2.16kg，230℃)相比，预期的计算的MFR2(2.16kg，230℃)
表2：
图1显示了仅加入POX PP5％ig或仅加入MB的MFR2值
图2显示了1.6重量％的总减粘裂化剂减去所使用的重量％的POX(过氧化物)的计算出的MFR2值对实际MFR2值。
实施例IE4和CE6和CE7
将PP-均聚-2与0.1重量％Irganox 1010(FF)和0.05重量％硬脂酸钙(CAS号1592-23-0)混合。
通过在240℃下使用同向旋转双螺杆挤出机并使用1700ppm纯POX(Trigonox 101)对PP-均聚-2进行减粘裂化，以实现CE6的800g/10min的目标MFR2。
对于CE7，使用1.5重量％的CR76MB来实现800g/10min的目标MFR2。
对于IE4，使用1.1重量％的CR76MB和300ppm纯POX(Trigonox 101)来实现800g/10min的目标MFR2。
IE4、CE6和CE7的聚丙烯组合物在Reicofil MB250线上采用具有470个出口直径为0.4mm的孔且每英寸35个孔的喷丝头转化成熔喷无纺布网。在不同的熔体温度、通过量、DCD(模头到收集器距离)和空气体积下制备网。
熔喷网的加工条件和性能如表3和表4所示
表3：用于制备熔喷网的加工条件
表4:熔喷网的性能
从表4和图3可以看出，相比于比较例，采用用本发明的协同减粘裂化剂组合物减粘裂化的聚丙烯聚合物用于制备熔喷无纺布网得到具有较高的静水压值的网。
比较例8
对于该比较例，通过在250℃下使用挤出机ZSK 18，使用MB和/或硫代-1，将PP-均聚-3减粘裂化，通过量为7kg/h。
-结果见表5
表5:
从图4可以看出，使用与硫代-1组合，对于减粘裂化效率完全没有产生协同效应。
Claims (9)
1.一种过氧化物和羟胺酯的协同减粘裂化组合物，用于提高聚丙烯聚合物在低于250℃的熔融挤出温度下的减粘裂化效率，包括1重量％(i)：99重量％(ii)至99重量％(i)：1重量％(ii)范围内的过氧化物(i)和羟胺酯(ii)，其中将过氧化物(i)和羟胺酯(ii)作为混合物或单独成分加入到待减粘裂化的所述聚丙烯中。
2.根据权利要求1所述的协同减粘裂化组合物，其中所述羟胺酯选自由下式的空间位阻胺衍生物组成的组：
且所述过氧化物选自2,5-二甲基-2,5-双(叔丁基-过氧)己烷、2,5-二甲基-2,5-双(叔丁基-过氧)己炔-3、过氧化二异丙苯、过氧化二叔丁基、过氧化叔丁基异丙苯和双(叔丁基过氧-异丙基)苯。
3.根据权利要求1或2所述的协同减粘裂化组合物，包含20重量％(i)：80重量％(ii)至95重量％(i)：5重量％(ii)范围内、优选25重量％(i)：75重量％(ii)至90重量％(i)：10重量％(ii)范围内、更优选30重量％(i)：70重量％(ii)至85重量％(i)：15重量％(ii)范围内且最优选在50重量％(i)：50重量％(ii)至85重量％(i)：15重量％(ii)范围内的纯过氧化物(i)和纯羟胺酯(ii)。
4.根据前述权利要求中任一项所述的协同减粘裂化组合物，其中所述待减粘裂化的聚丙烯是丙烯均聚物或具有高达10重量％的选自乙烯、1-丁烯、1-己烯和1-辛烯的共聚单体的丙烯共聚物，优选丙烯均聚物。
5.根据权利要求1至4中任一项所述的包括过氧化物(i)和羟胺酯(ii)的组合物用于提高聚丙烯聚合物在低于250℃的熔融挤出温度下根据ISO 1133测量的熔体流动速率MFR2(230℃/2.16kg)中的用途。
6.一种通过将根据前述权利要求1至4中任一项所述的过氧化物(i)和羟胺酯(ii)的协同减粘裂化组合物加入到所述待减粘裂化的聚丙烯聚合物中来提高聚丙烯聚合物在低于250℃的熔融挤出温度下的减粘裂化效率的方法。
7.用根据前述权利要求1至4中任一项所述的协同减粘裂化组合物减粘裂化的聚丙烯聚合物用于制备具有改进的阻隔性的熔喷无纺布的用途。
8.一种包括用根据前述权利要求1至4中任一项所述的协同减粘裂化组合物减粘裂化的聚丙烯聚合物的熔喷无纺布。
9.一种制品，所述制品选自通常由过滤介质(过滤器)、尿布、卫生巾、内裤衬垫、成人失禁产品、防护服、手术单、手术长外衣和手术衣组成的组，所述制品包括根据权利要求8所述的熔喷无纺布。
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| PCT/EP2015/079530 WO2016096687A1 (en) | 2014-12-15 | 2015-12-14 | Synergistic visbreaking composition of peroxide and hydroxylamine ester for increasing the visbreaking efficiency |
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| US11993699B2 (en) * | 2018-09-14 | 2024-05-28 | Fina Technology, Inc. | Polyethylene and controlled rheology polypropylene polymer blends and methods of use |
| EP3670547B1 (en) | 2018-12-21 | 2023-06-07 | Borealis AG | Polypropylene composition for film sealing layer |
| CN114729482B (zh) * | 2019-12-04 | 2024-01-02 | 博里利斯股份公司 | 由具有改善的过滤性能的熔喷纤维制成的过滤介质 |
| WO2021170615A1 (en) * | 2020-02-26 | 2021-09-02 | Basf Se | Additive mixtures for rheology modification of polymers |
| EP4222183A1 (en) | 2020-09-30 | 2023-08-09 | Borealis AG | Process for recycling propylene-ethylene copolymers |
| EP4244285A1 (en) * | 2020-11-13 | 2023-09-20 | Braskem, S.A. | Processing of polyethylene-based compositions and products therefrom |
| CN116724153A (zh) * | 2020-12-08 | 2023-09-08 | Sabic环球技术有限责任公司 | 由聚丙烯制造的熔喷网 |
| CN112522859A (zh) * | 2020-12-30 | 2021-03-19 | 宿迁市美达净化科技有限公司 | 一种抗菌聚丙烯熔喷非织造材料的制备方法 |
| WO2024052176A1 (en) * | 2022-09-07 | 2024-03-14 | Basf Se | Rheology modifying of polymers with a radical initiator and thiourethane |
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| ES2710998T3 (es) | 2019-04-29 |
| KR101846805B1 (ko) | 2018-05-18 |
| BR112017011886B1 (pt) | 2022-03-15 |
| EP3034552B1 (en) | 2018-11-28 |
| KR20170077256A (ko) | 2017-07-05 |
| TWI606086B (zh) | 2017-11-21 |
| WO2016096687A1 (en) | 2016-06-23 |
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| EP3034552A1 (en) | 2016-06-22 |
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