CN102356191B - 聚乙烯纤维、其用途和其制备方法 - Google Patents

聚乙烯纤维、其用途和其制备方法 Download PDF

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CN102356191B
CN102356191B CN201080012358.6A CN201080012358A CN102356191B CN 102356191 B CN102356191 B CN 102356191B CN 201080012358 A CN201080012358 A CN 201080012358A CN 102356191 B CN102356191 B CN 102356191B
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I.纳克
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Baumhueter Extrusion GmbH
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Abstract

本发明涉及可通过将聚合物熔纺得到的新的聚乙烯聚合物纤维、该纤维的用途、制备该纤维的方法、和包含所述纤维的产物。

Description

聚乙烯纤维、其用途和其制备方法
本发明涉及可通过熔纺聚乙烯聚合物得到的聚乙烯聚合物纤维、该纤维的用途和制备该纤维的方法。而且,本发明涉及可热封的滤纸、双成分纤维和空气沉降(air laid)产物、水力缠结产物和非织造产物。
本领域已知合成木浆的用途，其用于代替木浆制备纸状底物,例如茶叶包或咖啡包,例如US4,049,493。特别是,茶叶包纸由约75%天然纤维和约25%合成材料组成，以提供使袋热封的可能性。
US5,173,154公开了茶叶包纸，其包含第一相的天然纤维，重量百分比为60%至85%,和第二相的可热封的合成纤维，其和剩余物一起的重量百分比为约15%至40%。公开的茶叶包纸据称可在特殊的高速自动茶叶包包装机上加工,这是由于袋子可热封的那侧的原因。
尽管多种制备合成木浆的方法是本领域已知的,例如从US4,049,492和US4,049,493，但制备合成木浆的典型方法是复杂的且包括在有机分散剂中精制固体聚烯烃纤条(fibrids)并用水代替分散剂的步骤，以形成聚烯烃纤条的基本上水性浆液。
因此,对合成聚合物材料仍然存在需要，其可以容易且经济的方式制备，且可用作木浆的代替,例如用于制备纸状底物,特别是可热封的滤纸。
聚乙烯纤维是本领域已知的用于许多领域，因为聚乙烯、其共聚物及聚合物掺合物的有利性质。聚乙烯为具有热塑性的聚合物,其显示优异的化学稳定性且具有相当低的价格。不同性质的聚合物纤维可通过熔纺聚乙烯聚合物而制备。然而,在熔纺方法中，必须考虑聚合物材料的具体性质。重要的熔纺方法参数(最终对于待制备纤维的性质来说重要的),为分子量、熔体流动指数和原料分子量分布。
通常可熔纺MFI低于5g/10分钟的聚合物。然而,必须施加高压力以熔纺这些高粘性聚合物,其为非常耗费的。而且相比于通过具有MFI为约5g/10分钟至约100g/10分钟,特别是MFI为约5g/10分钟至约40g/10分钟的聚合物可获得的速度，熔纺这些聚合物的最大速度显著减少。
另一方面,如果聚合物MFI值太高,聚合物的粘度变得太低，从而纤维不能从喷口拉出。因此没有连续纤维可通过熔纺低粘度聚合物得到。而且可通过熔纺具有高MFI(大于100g/10分钟)的聚合物得到的纤维片段显示低机械稳定性，且该纤维不适用于进一步加工,例如编织。
因此,由于熔纺方法，对关于聚合物熔体的流变性质的原料的质量有高需求。因此，适合用于通过熔纺制备纤维的聚合物的MFI值必须在大于5g/10分钟至约100g/10分钟的范围,特别是大于5g/10分钟至约40g/10分钟。
然而,已发现当由MFI大于5g/10分钟至约100g/10分钟的聚合物制备的聚乙烯纤维用于在可热封的滤纸中代替合成的木浆时,在制备滤纸的过程中,特别是在干燥设备中,以及在滤纸在茶叶袋机中热封的过程中，在机器零件上形成沉积。这些沉积不利地影响机器功能，从而使得已知的聚乙烯聚合物纤维不适合用于可热封的滤纸。
为克服现有技术的该问题，已出人意料地发现当已知聚乙烯纤维通过电离辐射(ionizing radiation)交联时,该交联聚合物纤维可优异地用作合成的木浆的代替,特别是用于可热封的滤纸。特别是,在制备滤纸的过程中没有在机器零件上形成沉积,特别是在干燥设备中,以及当滤纸在茶叶袋机中热封时。
因此,本发明涉及可通过将聚合物熔纺得到的聚合物纤维，其具有的MFI为大于5g/10分钟至约100g/10分钟,优选大于5g/10分钟至约40g/10分钟,特别是大于10g/10分钟至约40g/10分钟,其特征在于在熔纺步骤之后将纤维用电离辐射处理。交联纤维的MFI值为5g/10分钟或更少,优选约2g/10分钟或更少,如约1.5g/10分钟或更少,或甚至约1g/10分钟或更少。
适用于制备纤维的聚合物没有特别限制。可使用本领域技术人员已知且用于通过熔纺制备聚合物纤维的任何聚合物。该聚合物的实例为包括聚烯烃、聚酰胺、聚酯、热塑性弹性体和任意这些物质的混合物的聚合物。
制备本发明的纤维使用的聚合物为聚乙烯。该聚乙烯可为均聚物或共聚物,如聚乙烯均聚物,聚乙烯共聚物,如聚乙烯/聚丙烯共聚物,包含聚乙烯作为一种聚合物的聚合物掺合物,如聚乙烯/聚丙烯混合物或任意这些的混合物,包括聚乙烯-基热塑性弹性体(TPEs)。
在一个实施方案中，聚合物纤维中使用的聚合物基本上包括聚乙烯、或聚乙烯共聚物或包含聚乙烯作为一种聚合物的聚合物掺合物。所用的聚乙烯可为均聚物,或聚乙烯共聚物,或包含聚乙烯均聚物或聚乙烯共聚物作为一种聚合物的聚合物掺合物。优选共聚物或聚乙烯混合物为聚乙烯和α-烯烃(如丙烯和1-丁烯,优选丙烯)的共聚物或混合物。优选地,使用包含约1wt.-%至约15wt.-%,更优选约2wt.-%至约9wt.-%的α-烯烃(例如丙烯)的聚乙烯,作为共聚物或聚合物掺合物，且最优选具有熔体流动指数为约5g/10分钟至约20g/10分钟。特别是,使用乙烯和丙烯的无规共聚物、嵌段共聚物或聚合物掺合物。该聚乙烯均聚物、共聚物或聚合物掺合物可与丙烯聚合物如聚丙烯(例如具有熔体流动指数为约5g/10分钟至约20g/10分钟),和/或乙烯与聚合物如丙烯、乙酸乙烯酯、丙烯酸和丙烯酸乙酯的共聚物混合。聚乙烯均聚物或共聚物的量优选为聚合物的约70wt.-%至约100wt.-%,更优选约80wt.-%至约95wt.-%,如约85wt.-%至约90wt.-%。最优选地该聚合物为聚乙烯均聚物。
在一个优选实施方案中该聚合物为聚乙烯-基TPE(热塑性弹性体)，其有时在现有技术中称为"热塑性橡胶"。TPE为一类共聚物或聚合物掺合物，其由具有热塑性和弹性的材料组成。通常，TPEs为含橡胶的聚乙烯或聚丙烯混合物,如聚乙烯/EPDM混合物或聚丙烯/EPDM混合物(EPDM=乙烯丙烯二烯单体橡胶),其中该单体优选为M-级(是指ASDN标准D-1418中的分级)。典型EPDM橡胶为DCPD(二环戊二烯),ENB(亚乙基降冰片烯)和VNB(乙烯基降冰片烯)。聚乙烯/EPDM混合物中的典型聚乙烯含量为约50wt.-%至约95wt.-%,更优选约70wt.-%至约90wt.-%。EPDM橡胶中的典型乙烯含量为约45wt.-%至约75wt.-%,优选约55wt.-%至约70wt.-%。乙烯含量越高,聚合物的负载可能性越高,其导致更好的混合和挤压。二烯类,通常为聚合物掺合物的约2.5wt.-%至约12wt.-%,优选约5wt.-%至约10wt.-%,其作为交联键提供在最终使用时对不希望的粘性、打滑(creep)或漂浮(float)的抗性。
在更优选的实施方案中该聚乙烯为HDPE、LDPE、LLDPE,或其混合物。优选HDPE、LDPE或LLDPE在上述聚合物掺合物中使用。或者,该聚乙烯可为聚乙烯/EVA(乙烯乙酸乙烯酯)共聚物，其优选用于上述聚合物掺合物。通常,乙酸乙烯酯在EVA中的含量为约5wt.-%至约45wt.-%,优选约10wt.-%至约40wt.-%,且剩余部分优选为乙烯。基于EVA的共聚物具有有利的弹性,且可像其它热塑塑料一样加工。
本文所述的术语"基本上包括"是指各成分的量为至少80wt.-%,更优选至少90wt.-%,特别是至少95wt.-%,例如至少99wt.-%，基于各组合物的总重量。在一个优选实施方案中，用于聚合物纤维的聚合物分别由聚乙烯或其共聚物或聚合物掺合物组成,作为唯一聚合物成分。
使用聚乙烯、特别是上述本发明的纤维的另一优点为,聚乙烯通常具有更好的化学耐性,特别是更好的耐酸(如氢氟酸)性，相比于其它聚合物,特别是聚丙烯或聚酯。因此,相比于由其它聚合物制备的产物，聚乙烯纤维和由聚乙烯纤维制备的产物显示改善的化学耐性。因此，包含根据本发明的纤维(包含聚乙烯或上述各共聚物或聚合物掺合物，且经过电离辐射处理)的产物,都显示优异的耐温度耐性(辐射赋予)和化学耐性(聚乙烯材料赋予)。
制备本发明的纤维使用的聚合物可包含其它聚合物以及添加剂,如着色剂,助流剂,纺纱添加剂,功能共聚物,低分子量聚丙烯,聚丙烯蜡,无规聚丙烯,反应性成分,热稳定剂,UV稳定剂等等。添加剂可通过本领域技术人员根据熔纺方法的具体需求和最终纤维的预期用途而选择。
在一个实施方案中，该聚合物包含已知的金属活化剂,例如含氧化还原活性的过渡金属离子如Fe2+/Fe3+,Co2+/Co3+,Cu+/Cu2+,Cr2+/Cr3+,或Mn2+/Mn3+/Mn4+,如CuO的金属活化剂。典型地，该聚合物包含的金属活化剂的量为约0.001wt.-%至约1wt.-%,优选为约0.01wt.-%至约0.5wt.-%,基于聚合物的总重量。已发现当金属活化剂存在于聚合物中时，电离辐射的功效增加。因此,金属活化剂的存在是有利的，因为需要较少的辐射以提供足够的聚乙烯聚合物的交联。
在一个实施方案中，制备本发明的纤维使用的聚合物包括交联剂。与上述聚合物中的聚乙烯使用的交联剂通常为脂族多元醇的三丙烯酸酯或三甲基丙烯酸酯。适合作为交联剂的具体化合物包括,例如,三羟甲基丙烷三丙烯酸酯,三羟甲基丙烷三甲基丙烯酸酯,三羟甲基乙烷三丙烯酸酯和四羟甲基甲烷三丙烯酸酯。特别优选地为三羟甲基丙烷三丙烯酸酯和三羟甲基丙烷三甲基丙烯酸酯。交联剂通常存在的量为约0.5wt.-%至约4wt.-%,基于聚乙烯的重量。三羟甲基丙烷三丙烯酸酯和三羟甲基丙烷三甲基丙烯酸酯与聚乙烯高度相容且显示高交联作用。最优选地,交联剂的量的范围为约1.0wt.-%至约2.5wt.-%,基于聚乙烯的重量。可另外使用酚化合物的衍生物,如公开于US4,367,185的那些化合物,以增强交联作用。酚化合物衍生物的量通常在0.01wt.-%至5.0wt.-%，基于聚乙烯的重量。
在一个实施方案中，制备本发明的纤维使用的聚合物包括硅烷(-基)交联剂。典型硅烷交联剂是本领域已知的。合适的硅烷交联剂的非限制性实例包括不饱和硅烷，其包含烯式不饱和烃基,如乙烯基,烯丙基,异丙烯基,丁烯基,环己烯基或γ-(甲基)丙烯基氧基烯丙基,和可水解的基团如烃基氧基(hydrocarbyloxy),烃基氧基(hydrocarbonyloxy)和烃基氨基。在另一实施方案中所述硅烷为可接枝至聚合物上的不饱和烷氧基硅烷。合适的硅烷交联剂的实例为乙烯基三甲氧基硅烷,乙烯基三乙氧基硅烷,乙烯基三(2-甲氧基乙氧基)硅烷,乙烯基三乙酰氧基硅烷,乙烯基甲基二甲氧基硅烷,3-甲基丙烯酰基氧基丙基三甲氧基-硅烷,及其组合。硅烷交联剂的量通常为约0.1wt.-%至约1wt.-%,优选约0.5wt.-%至约1wt.-%,基于聚合物的总重量。尽管上述交联剂以及此处描述的基于聚硅氧烷的交联剂可优异地通过本文所述电离辐射交联结合在一起,已发现现有技术已知的通过过氧化物交联不能适用于制备交联聚乙烯纤维。
通过熔纺制备纤维是本领域技术人员已知的。该方法描述于,例如,B.von Falkai,Synthesefasern,Grundlagen,Technologie,Verarbeitung undAnwendung,Verlag Chemie,Weinheim1981。在熔纺方法中聚合物的性质通常没有显著改变。因此,例如该熔纺方法中获得的纤维的MFI值几乎与用作起始材料的聚合物颗粒的MFI值相同。因此,通过熔纺获得的聚合物纤维的MFI值与适合用于熔纺方法的那些聚合物的MFI值在相同范围,即MFI的范围为大于5g/10分钟至约100g/10分钟,特别是大于5g/10分钟至约40g/10分钟,例如约10g/10分钟至约40g/10分钟。
根据本发明，熔纺方法中得到的聚合物纤维的流变性质根据纤维的预期用途的需要通过用电离辐射处理纤维而定制。优选该电离辐射为γ或β辐射。
γ-和β-射线处理通过本领域已知的辐射过程进行。β-射线,也已知为电子束,通过本领域公知的电子加速器产生。工业领域使用的γ-射线通常在钴60(60Co)放射性转化为镍60(60Ni)的过程中产生。由此放射的γ-射线具有高穿透深度。尽管用β-射线辐射的时间通常为几秒,但用γ-射线辐射的时间可为几小时。施加于根据本发明的聚合物纤维的辐射剂量没有特别限制，但通常在约10kGy至约300kGy(kilo Gray),优选约30kGy至约160kGy的范围。
通过交联聚合物，即用电离辐射处理，聚合物纤维的性质改变。例如聚合物纤维的MFI值,取决于用于制备纤维的聚合物,被增加或降低。例如在聚丙烯的情况下，MFI由于聚合物链的键断裂而增加，而聚乙烯的情况下，MFI通过聚合物交联而降低。因此,聚合物纤维的其它性质,如聚合物的平均分子量和/或聚合物的分子量分布被改变。而且,通过辐射，聚乙烯的热塑性改变为热弹性。这可通过例如辐射后聚乙烯热收缩的丧失而看出。因此,聚乙烯纤维的性质可根据纤维的预期用途需要而定制。
本发明的聚合物纤维特别相关的为MFI(熔体流动指数(melt flow index))值,也称为熔体流速(melt flow rate)(MFR)。聚合物纤维的MFI值根据DINEN ISO1133测量。根据该定义，测量MFI的标准测量条件为对于聚乙烯190℃/2.16kg和对于聚丙烯230℃/2.16kg。MFI的单位为g/10分钟，其通过毛细管流变计测量,从而该材料,即聚合物,熔融为圆柱形且以一定压力通过限定的喷嘴压出。然后该形成的聚合物熔体物质以时间的函数检测。
用于制备根据本发明的聚合物纤维的方法的聚合物为聚乙烯均聚物、聚乙烯共聚物、包含聚乙烯作为一种聚合物的聚合物掺合物或其混合物。交联纤维的MFI值为约5g/10分钟或更少,优选约2g/10分钟或更少,如约1.5g/10分钟或更少,或甚至约1g/10分钟或更少。
本发明的聚合物纤维可通过制备聚合物纤维的方法获得，其包括将聚合物熔纺且随后用电离辐射处理纤维的步骤。本发明还涉及所述方法。在该方法中，纤维以连续丝条获得或该丝条被切成段。电离辐射的处理可在形成纤维后直接进行,例如在纤维被拉伸之前、之中或之后,但在其切成段之前或在其切成段之后。还可能在获得连续纤维丝条或切成的纤维段后,这些物质储存一段时间，且在稍后的时间进行电离辐射的处理步骤。
根据本发明的聚合物纤维的合适直径通常低于约170μm,优选低于约100μm,特别是低于约40μm,且优选在约5μm至约170μm,更优选约12μm至约50μm,且最优选纤维的直径为约20μm至约25μm,例如约23μm。
在通过电离辐射交联纤维前聚合物纤维的长度通常低于等于约20mm,优选低于约10mm,特别是低于约6mm,且优选约0.1mm至约40mm,如约2mm至约20mm,且特别为约2mm至约5mm,例如约2mm至约3mm。通过电离辐射交联纤维导致纤维的长度减少,取决于施加的总剂量，通常减少约辐射前长度的三分之一,。因此,优选该纤维在辐射前切割，因为较大的纤维切割物更有利,例如出于处理目的。
在一方面本发明涉及通过上述电离辐射交联的聚乙烯纤维在可热封的滤纸中的用途。
在一个优选方面，本发明提供上述聚合物纤维在可热封的滤纸中的用途以及含上述聚合物纤维的可热封的滤纸。在可热封的滤纸中，优选使用含聚乙烯均聚物、聚乙烯共聚物、包含聚乙烯作为一种聚合物的聚合物掺合物或其混合物的聚乙烯纤维。通过电离辐射处理，聚合物交联,其可通过MFI的减少进行检测,从而获得产物，该产物具有的熔融粘度高于由熔纺后但没用电离辐射处理的聚乙烯纤维制造的产物具有的熔融粘度。由于纤维交联，有利特性可赋予上述滤纸。
在一方面本发明涉及双成分纤维，其包含上述交联聚乙烯纤维作为一种成分。双组分聚合物纤维已知为并列纤维(side-by-side fiber)或皮芯型纤维(sheath-core fiber)。当MFI为大于5g/10分钟至约100g/10分钟的聚乙烯纤维作为双成分纤维的一种成分时,另一组分必须为在热封过程中提供足够稳定性的支持聚合物,如聚酯。通过交联聚乙烯，可获得具有优异的性质的双成分纤维,其中特别是该交联聚乙烯成分提供足够的支持,且另外使得纤维可热封。
在一个优选方面，本发明涉及包含交联聚乙烯纤维,特别是上述聚合物纤维的可热封的滤纸。根据本申请的可热封的滤纸可有利地用于茶叶包或咖啡包。因此,本发明优选还涉及包含根据本发明的可热封的滤纸的茶叶包或咖啡包,以及纤维在茶叶包或咖啡包中的各自用途。
根据本申请的可热封的滤纸通常包含已知来自滤纸的组分,例如天然纤维的重量百分比为约60%至约85%,剩余的约40wt.-%至约15wt.-%为合成纤维,如合成的木浆,其中合成纤维至少部分(特别是约20wt.-%至约100wt.-%,优选约50wt.-%至约100wt.-%)被根据本申请的交联聚乙烯纤维代替。
本发明另一方面为交联聚乙烯纤维,特别是上述聚合物纤维在空气沉降产物(air laid products)、水力缠结产物(hydroentangled products)和非织造产物(non-woven products)中的用途，以及包含交联聚乙烯纤维,特别是上述聚合物纤维的这些产物。由聚合物纤维制备这些产物是现有技术已知的。如上述通过辐射定制聚合物纤维的性质可以制备这些类型的新的和有利的产品。
本发明将通过实施例进一步阐述，其不构成限制。
实施例
聚乙烯(PE)纤维的β-辐射处理:
具有4分特克斯(相当于直径为约23μm)的和6mm长的PB EurofiberCUT F-2427类型的PE纤维样品(由baumhueter extrusion GmbH制造)用β-射线以35-160kGy的剂量处理。辐射后纤维的长度为约4.5mm。测量电离辐射处理之前和之后的MFI值。而且，具有4分特克斯(相当于直径为约23μm)的和2mm长的PB Eurofiber CUT F-2382类型的PE纤维样品(由baumhueter extrusion GmbH制造)用β-射线以50kGy的剂量处理。辐射后纤维的长度为约1.5mm。测量电离辐射处理之前和之后的MFI值。MFI测量根据DIN EN ISO1133在标准条件,即190℃/2.16kg进行。测试辐射交联前和后的包含纤维F-2382的滤纸的热封性能。结果示于下表。
表1
*高度交联的,不再可熔。
1)没有交联，由于干燥设备中的问题纤维不可在造纸机上加工,这是由于纤维的轻易熔化导致的。
2)制备茶叶包纸且没有任何问题。该纸成功在茶叶袋机上测试。
上述结果证实根据本发明经辐射的PE纤维可用于可热封的纸,而未处理的纤维则不能使用。而且在制备滤纸的过程中在茶叶袋机中当包含经辐射的PE纤维的滤纸被热封时将不会在机器零件上检测到聚合物沉积。

Claims (12)

1.聚合物纤维，其可通过将聚合物熔纺得到，所述聚合物具有的MFI为大于5g/10分钟至100g/10分钟,其特征在于在熔纺步骤之后将该纤维用电离辐射处理进行交联,其中所述聚合物为聚乙烯均聚物、聚乙烯共聚物、包含聚乙烯作为一种聚合物的聚合物掺合物、或其混合物，以及其中所述交联后的所述聚合物纤维具有的MFI为5g/10分钟或更少，其中MFI测量根据DIN EN ISO1133在标准条件,即190℃/2.16kg进行，其中所述聚合物纤维在电离辐射交联该纤维前的长度小于等于20mm，其中辐射剂量为30kGy至160kGy。
2.根据权利要求1的聚合物纤维,其中所述交联后的所述聚合物纤维具有的MFI为2g/10分钟或更少。
3.根据权利要求1或2的聚合物纤维，其中所述聚合物纤维在电离辐射处理前切割成长度小于20mm。
4.根据权利要求1或2的聚合物纤维，其中所述聚合物纤维在交联该纤维前的长度为2mm至20mm。
5.根据权利要求1的聚合物纤维，其中所述纤维为交联聚乙烯纤维。
6.制备聚合物纤维的方法，其包括将聚合物熔纺的步骤,其中所述聚合物为MFI大于5g/10分钟至100g/10分钟的聚乙烯均聚物、聚乙烯共聚物、包含聚乙烯作为一种聚合物的聚合物掺合物、或其混合物,以及随后用电离辐射处理纤维的步骤,以得到MFI为5g/10分钟或更少的交联聚合物纤维，其中MFI测量根据DIN EN ISO1133在标准条件,即190℃/2.16kg进行，所述聚合物纤维在电离辐射交联该纤维前的长度小于等于20mm，其中辐射剂量为30kGy至160kGy。
7.根据权利要求6的方法，其中所述聚合物纤维在电离辐射处理前切割成小于20mm的纤维长度。
8.根据权利要求6的方法，其中所述纤维在辐射前切割成2mm至20mm的纤维长度。
9.权利要求1-5中任一项的聚合物纤维在可热封的滤纸中的用途。
10.权利要求1-5中任一项的聚合物纤维在空气沉降产物中的用途。
11.可热封的滤纸，其包含根据权利要求1至5任一项的聚合物纤维。
12.空气沉降产物，其包含根据权利要求1至5任一项的聚合物纤维。
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