CN102356187B - 聚合物纤维、其用途及其制造方法 - Google Patents

聚合物纤维、其用途及其制造方法 Download PDF

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CN102356187B
CN102356187B CN2010800123571A CN201080012357A CN102356187B CN 102356187 B CN102356187 B CN 102356187B CN 2010800123571 A CN2010800123571 A CN 2010800123571A CN 201080012357 A CN201080012357 A CN 201080012357A CN 102356187 B CN102356187 B CN 102356187B
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I.纳克
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Abstract

本发明涉及聚合物纤维，其可通过将聚合物熔纺得到，且随后用电离辐射处理该纤维，其中所述聚合物为聚丙烯均聚物、聚丙烯共聚物或其混合物，所述聚合物纤维具有的长度范围为0.1至40mm，直径范围为5至170μm，且MFI大于500g/10分钟。本发明涉及所处理的聚合物纤维改善混凝土、灰浆、石膏、水泥或耐火材料的耐火性的用途。

Description

聚合物纤维、其用途及其制造方法
本发明涉及可通过熔纺聚合物得到的聚合物纤维、该纤维的用途和制备该纤维的方法。
聚合物纤维作为水泥、石膏、灰浆、混凝土等的加强物的用途是本领域众所周知的，例如EP-A-0 225 404，EP-A-0 235 577和EP-A-0 448 577。水泥糊剂、灰浆或混凝土这些材料，尽管有极大的压缩强度，但拉伸强度低，具有低破裂应变且通常非常脆。因此纤维被引入以克服这些弱点中的一些，且开发出不可能的产品。聚合物纤维在这些应用中证明是特别合适的，因为它们具有良好的化学耐性，不受湿气影响，具有高抗拉强度和断裂伸长，具有低比重，且可容易处理。
混凝土的耐火性是非常重要的，尤其在隧道建筑领域。如果由于例如车祸在隧道内发生起火，温度快速升至1000℃以上。因此隧道内的壁的外层温度升高。因为混凝土包含水，水在短时间内开始蒸发。然而，该气流无法足够快地从混凝土结构内逃逸，因此压力剧烈增加。如果混凝土内的压力超过混凝土的抗拉强度，外层将开始掉块且热可更快地传递至混凝土的最内部。如果热量达到钢加强物，其稳定性也损失非常快。通过这种方式，隧道有很高的坍塌风险。由于混凝土掉块部分引起的损坏的程度根据混凝土中的水含量相应增加。混凝土致密且压实的结构进一步阻止气流逃逸。材料的掉块是耐火性工业中众所周知的问题。类似问题出现在耐火材料如烤箱器皿中。因为混凝土的结构显著被混凝土表面部分的爆发性掉块所削弱，必须避免掉块以尽可能减少损坏发生。
尽管已知聚合物纤维加强物可增加混凝土、水泥等的耐火性，仍然存在需求以进一步改善产物，特别是改善耐火性。
出人意料地发现，如果聚合物纤维的熔体流动指数(MFI)增加，水泥、灰浆、混凝土或其它耐火材料的产物的耐火性进一步增加。不希望束缚于任何理论，认为这可通过当聚丙烯纤维由于升高温度而熔化时混凝土中毛细管网或多孔系统的形成而解释。结果，混凝土变得可使水流透过，且混凝土内的压力减少以降低或避免掉块。
如果聚合物纤维的MFI值增加，则形成低粘液聚合物熔体，其更易被混凝土基质吸收，且导致通过成形毛细管(forming capillars)的更早和更高的渗透性。
聚合物纤维的另一应用为可热封的滤纸(hot sealable filter paper)。对于该应用，低MFI值的聚合物纤维是有利的，因为纤维在高温和高压下保持可密封的，但低MFI值的纤维减少聚合物熔体由于其高粘度沉积于机器零件上从而不利地影响机器功能的风险。
两种聚合物纤维(用于加强应用和用于制备可热封的滤纸)都通过熔纺常规制备。然而，在熔纺方法中聚合物材料的具体特性必须加以考虑。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。特别是，如果聚合物的MFI太低，其粘度变得对熔纺方法太高。另一方面，如果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，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40g/10分钟的较小范围内。
另一方面，对于许多应用，如用于增强水泥、灰浆、混凝土、石膏等的添加剂或用于上述可热封的滤纸的添加剂，期望使用的聚合物纤维的MFI值高于或低于用于熔纺方法的聚合物的MFI值。
为克服现有技术的这种和其它上述问题，出人意料地发现通过熔纺得到的聚合物纤维的性质通过用电离辐射(ionizing radiation)处理熔纺纤维而适用于各种应用进行定制。
因此，本发明涉及可通过将聚合物熔纺得到的聚合物纤维，其特征在于在熔纺步骤之后该纤维用电离辐射处理。
制备本发明的纤维使用的聚合物没有特别限制。本领域技术人员已知且可通过熔纺用于制备聚合物纤维的任何聚合物可以使用。该聚合物的实例为包含聚烯烃、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。在一优选的实施方案中所述聚合物为聚烯烃，如聚丙烯或聚乙烯。这些聚合物的每一个可为均聚物或共聚物，如聚丙烯均聚物、聚丙烯共聚物、聚乙烯均聚物、聚乙烯共聚物、聚丙烯/聚乙烯共聚物或任意这些物质的混合物.
制备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(glidents)，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。添加剂可通过本领域技术人员根据熔纺方法的具体需求以及最终纤维预期用途而选择。
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，Weinheim 1981。在熔纺过程中聚合物的性质通常没有改变。因此，例如该方法得到的纤维的MFI值与用作起始材料的聚合物颗粒的MFI值相同。因此，通过熔纺得到的聚合物的MFI值必然与适用于熔纺方法的那些聚合物的MFI值在相同的范围，即该MFI在大于5g/10分钟至约40g/10分钟的范围。
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。
通过用电离辐射处理，聚合物纤维的流变性质改变。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，因此，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)值，也称为熔体流速(MFR)。聚合物纤维的MFI值根据DIN EN ISO 1133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。因为聚合物纤维被熔融以测定其MFI值，聚合物纤维的MFI等于纤维聚合物的MFI，即包括任何添加剂或与其它聚合物的混合物(如果存在的话)的聚合物。
由聚丙烯制备(无论均聚物或共聚物或其混合物)的根据本发明的聚合物纤维的优选的MFI值高于约50g/10分钟，更优选高于约100g/10分钟，如高于约500g/10分钟，特别是高于约1000g/10分钟。
如果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、聚乙烯共聚物或其混合物，该MFI值优选低于约5g/10分钟，更优选低于约2g/10分钟，如低于约1.5g/10min或甚至低于约1g/10分钟。
本发明进一步提供可通过熔纺得到的聚丙烯纤维，其特征在于该纤维具有的MFI大于约50g/10分钟，优选大于约100g/10分钟，如大于约500g/10分钟或甚至大于约1000g/10分钟。该纤维可从上述含聚丙烯的聚合物制备。该聚丙烯例如可为均聚物或共聚物或其混合物。熔纺步骤后，所得纤维的MFI如上所述通过用电离辐射处理而增加。或者，MFI可通过本领域技术人员已知的其它手段增加，如通过与过氧化物反应而部分分解聚合物。
本发明另一方面提供制备聚合物纤维的方法，其包括将聚合物熔纺且随后用电离辐射处理纤维的步骤。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。
在本发明另一方面，该聚合物纤维用作混凝土、灰浆、石膏、水泥或耐火材料中的添加剂。通过用电离辐射处理聚合物纤维，特别是本发明的聚丙烯纤维，它们的熔融粘度可显著降低。因此，当用作水泥等的添加剂时，它们促进上述毛细管体系的早期形成(当水泥被加热，例如在火中)，因此水流在较低温度和压力就可逃逸。结果，相比于使用未处理的聚丙烯纤维作为添加剂，掉块显著减少，且水泥或混凝土产物如隧道的稳定性可保持更长的时间。
在实验中，使用根据本发明的纤维证明了显著改善的耐火性效果。在耐火试验中比较根据本发明的纤维与标准聚丙烯纤维，其使用相同量的相同几何形状的纤维作为混凝土样品中的添加剂。结果，相比包含不用电离辐射处理的标准聚丙烯纤维的样品，包含根据本发明的纤维的样品显示显著较少的掉块。
而且，MFI大于约50g/10分钟，优选大于约100g/10分钟，特别是大于约500g/10分钟，如大于约1000g/10分钟的聚丙烯纤维用作混凝土、灰浆、石膏、水泥或耐火材料中的添加剂。该聚丙烯纤维可为上述纤维。或者，该纤维可例如通过其它方法制备，如熔喷具有所需范围的MFI的聚合物。
本发明还提供包含聚合物纤维的混凝土、灰浆、石膏、水泥或耐火材料，特别是上述聚丙烯纤维。
用于混凝土等的根据本发明的聚合物纤维的直径的合适范围根据本发明为约5μm至约170μm，更优选约12μm至约50μm且最优选约15μm。
用于混凝土等的根据本发明的聚合物纤维的长度根据本发明优选为约0.1mm至约40mm，如约2mm至约20mm，更优选约4mm至约8mm且最优选约6mm。
在混凝土等中，根据本发明，优选少于约2kg的根据本发明的聚合物纤维存在于1m3混凝土等中。1m3混凝土使用的根据本发明的聚合物纤维的量的优选范围为约0.1kg至约1.5kg，更优选约0.1kg至约1.0kg。高于约2kg聚合物纤维的量不利地影响混凝土的稳定性。然而，不仅混凝土中聚合物纤维的量是重要的，而且纤维的直径和长度也是重要的。给定量的不同直径的聚合物纤维导致不同数量的聚合物纤维存在于混凝土中，其影响混凝土的性质。因此，需要参数的合适组合。
在另一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上述含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、聚乙烯共聚物或其混合物的聚乙烯纤维。通过用电离辐射处理，聚乙烯的MFI降低，从而得到具有较高熔融粘度的产物，相比于熔纺后但没用电离辐射处理的聚乙烯纤维得到的产物。由于该纤维较高的熔融粘度，可将有利特性赋予上述滤纸。
本发明另一方面为上述聚合物纤维在空气沉降(air laid)产物、水力缠结式非织物(hydroentangled products)和非织造产物(non-woven products)中的用途，以及含上述聚合物纤维的这些产品。通过定制聚合物纤维的性质，可制备这些类型的新的和有利的产品。例如如果聚合物熔体的粘度增加，该纤维更易于热封。
本发明将通过实施例进一步阐述，其不构成限制。
实施例
聚丙烯(PP)纤维的β-射线处理：
具有1.7分特克斯(相当于直径为约15μm)的PB Eurofiber CUT F-1763类型的PP纤维样品(由baumhueter extrusion GmbH制造)用β-射线以132kGy的剂量处理。然后测量其MFI值。在β-射线处理前，MFI值为40g/10分钟(在实验中以下标记为“U”的未处理的纤维样品用作对照样品)。处理后，MFI值>1200g/10分钟(处理的纤维样品在以下标记为“T”)。MFI测量根据DIN ENISO 1133在标准条件，即230℃/2.16kg进行。
耐火试验：
对于两种纤维样品，制备混凝土样品且进行耐火试验。使用隧道建筑的典型混凝土组合物制备混凝土样品。以下量对于35L的体积计算：
水：           6.3kg
砂：           19.5kg
劈离料(Split)：43kg
水泥：         11.2kg
烟道灰：       2.8kg
测试样品从所得混凝土混合物使用不同量的PP纤维制备，且填充为具有10cm边长的立方钢形式(cubic steel form)。该混凝土样品以钢形式固化1天，然后在水中储存7天，然后进行耐火试验。在耐火试验中将样品放入1100℃炉中5分钟。冷却后，测量掉下的(chipped off)块的体积。结果总结于以下表1：
表1
Figure BDA0000092192820000071
上述结果证实含根据本发明的辐射的PP纤维(T)的混凝土的掉下的块的量显著小于未处理的PP纤维(U)。可见，根据本发明的混凝土样品的掉下的块的量为含现有技术的纤维的混凝土样品的掉下的块的量的约1/2至1/4。

Claims (9)

1.聚合物纤维，其可通过将聚合物熔纺得到，且随后用电离辐射处理该纤维,其中所述聚合物为聚丙烯均聚物、聚丙烯共聚物或其混合物,所述聚合物纤维具有的长度范围为0.1至40mm,直径范围为5至170μm，且MFI大于500g/10分钟,根据DIN EN ISO 1133在230℃和2.16kg测量。
2.根据权利要求1的聚合物纤维，其中所述辐射的剂量为10kGy至300kGy。
3.根据权利要求1的聚合物纤维，其中所述辐射的剂量为30kGy至160kGy。
4.制备根据权利要求1的聚合物纤维的方法，其包括将聚合物熔纺且随后用电离辐射处理纤维的步骤。
5.根据权利要求4的方法，其中所述辐射的剂量为10kGy至300kGy。
6.根据权利要求4的方法，其中所述辐射的剂量为30kGy至160kGy。
7.根据权利要求1-3中任一项的聚合物纤维在混凝土、灰浆、石膏、水泥或耐火材料中作为添加剂的用途。
8.根据权利要求1-3中任一项的聚合物纤维在改善混凝土、灰浆、石膏、水泥或耐火材料的耐火性中的用途。
9.混凝土、灰浆、石膏、水泥或耐火材料，其包含根据权利要求1-3中任一项的聚合物纤维。 
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AU2010225025B2 (en) 2013-11-28
IL214863A (en) 2014-09-30
EP2408959A1 (en) 2012-01-25
CA2754878C (en) 2016-10-11
JP5859422B2 (ja) 2016-02-10
BRPI1009493A2 (pt) 2016-03-15
CN102356187A (zh) 2012-02-15
KR20110133478A (ko) 2011-12-12
RU2011141887A (ru) 2013-04-27
KR101698619B1 (ko) 2017-01-20
EP2230350B1 (en) 2011-04-13
AU2010225025A1 (en) 2011-08-25
RU2543176C2 (ru) 2015-02-27
DK2408959T3 (en) 2018-12-10
PL2230350T3 (pl) 2011-08-31
CA2754878A1 (en) 2010-09-23
WO2010105980A1 (en) 2010-09-23
SI2230350T1 (sl) 2011-07-29
US20120071589A1 (en) 2012-03-22

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