CN108100460A - 抗菌聚合物材料的复合材料、其制备方法及用途 - Google Patents

抗菌聚合物材料的复合材料、其制备方法及用途 Download PDF

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Publication number
CN108100460A
CN108100460A CN201711202428.4A CN201711202428A CN108100460A CN 108100460 A CN108100460 A CN 108100460A CN 201711202428 A CN201711202428 A CN 201711202428A CN 108100460 A CN108100460 A CN 108100460A
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China
Prior art keywords
composite material
fluoropolymer
material according
polymer material
polymer
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CN201711202428.4A
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CN108100460B (zh
Inventor
伊拉里亚·洛坎托雷
温琴佐·瓜尔涅里
切萨雷·洛巴肖
埃马努埃莱·科隆博
马西莫·维拉诺
贾科莫·西莫尼
露西娅·格里扎菲
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Alcari LLC
Gu Arnie Furlong Joint-Stock Co
Thales Alenia Space Italia SpA
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Alcari LLC
Gu Arnie Furlong Joint-Stock Co
Thales Alenia Space Italia SpA
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Publication of CN108100460A publication Critical patent/CN108100460A/zh
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Abstract

本发明涉及一种无孔复合材料，其包括用第一含氟聚合物浸渍的纺织基材和用多孔硅酸盐粒子填充的包含至少一种第二含氟聚合物的聚合物材料的膜，所述多孔硅酸盐粒子具有小于或等于5μm的粒度尺寸d50和30至60体积％的孔隙率并且负载有选自由银、铜、锌和镍组成的组中的至少一种金属的抗菌离子。本发明还涉及用于制备所述复合材料的方法，以及利用所述复合材料制备的用于流体、优选水的容纳和/或运输元件。

Description

抗菌聚合物材料的复合材料、其制备方法及用途
技术领域
本发明涉及无孔(非多孔，non-porous)且抗菌的复合材料及其例如在航空航天领域中用于容纳和/或运输流体的用途。
背景技术
已知的是，在航空航天领域，流体，例如饮用水的运输面临许多困难。特别地，已知的是，由FEP制成的容器在太空航行期间用于饮用水的保存和运输。这些容器与由其他聚合物制成的容器相比较少受到细菌侵袭。然而，它们需要在每次使用后消毒。备选地，使用金属容器和管，但是这些需要非常昂贵的预处理以使有利于微生物生长的表面粗糙度最小化。此外，它们特别重。
最后，定期地将消毒剂，例如胶体银或碘加入到所运输的液体。银的使用是非常昂贵的，并且已经证实具有随着时间不稳定的杀生物活性。而碘的使用需要借助于过滤器系统在消耗之前移除水，这明显地减少空间单元中的可用空间并且需要全体人员维护。
因此，正在进行对于避免使用化学品并且廉价和轻量的用于制造流体的容纳元件和/或运输元件的新材料。
发明内容
因此，本发明的目的是提供解决上述问题的新材料。
所述目的通过与根据权利要求1的复合材料、根据权利要求12的其制备方法和根据权利要求14的容纳和/或运输元件相关的本发明实现。
具体实施方式
特别地，提供了一种无孔复合材料，其包括用第一含氟聚合物浸渍的纺织基材(textile substrate)和至少一个用多孔硅酸盐粒子(硅酸盐的多孔粒子，porousparticles of a silicate)填充的包含至少一种第二含氟聚合物的聚合物材料的膜，所述多孔硅酸盐粒子负载有选自由银、铜、锌和镍组成的组中的至少一种金属的抗菌离子。
第二含氟聚合物可以是聚四氟乙烯或四氟乙烯(TFE)的共聚物。所述聚合物的实例可以是四氟乙烯(TFE)-全氟烷基乙烯基醚(FVE)的共聚物，其中FVE的碳原子数为1至5，或者TFE-六氟丙烯(HPF)-FVE共聚物。在一个实施方案中，所使用的共聚物是TFE-全氟丙基乙烯基醚(PPVE)的共聚物，其中基于TFE的总重量，PPVE含量为低于1重量％的量，更优选为0.05至0.5重量％的量。
TFE共聚物的分子量为PTFE的分子量的五分之一。这种改性导致具有改善的熔融性能的聚合物，显著有助于该聚合物的改善的可加工性。
此外，有利地，PPVE的使用抑制结晶，从而提高无定形物含量并且因此保持含氟聚合物特有的机械性质。此外，PPVE确保微晶(雏晶，crystallite)在无定形基体中的改善的分布，显著地减少冷流(冷裂，cold flow)。
由此改性的含氟聚合物因此具有改善的可焊接性，在负荷下的较低变形性，具有较少空隙的较致密的聚合物结构，较低的可渗透性，改善的压缩应力后弛豫，较大的透明度，改善的可成膜性和改善的表面可加工性。
在本发明的另一实施方案中，含氟聚合物是聚四氟乙烯(PTFE-四氟乙烯TFE的均聚物)。
PTFE的主要性质是极度的化学惰性，对热和老化的优异抗性，优异的介电性质，自润滑性质和最小的摩擦系数。PTFE仅在高压和高温下受金属形式的碱金属、氯三氟化物和单质氟侵袭。
PTFE具有低的传热因子并且因此可以被认为是隔热材料。其还具有阻燃性质并且在高达260℃长期稳定。
PTFE还在宽范围的温度和频率内具有优异的介电性质。
由于其不吸收水，因此其也在长期暴露于大气试剂(atmospheric agents)后保持所述性质。电阻不受操作温度影响。此外，对于电弧形成的抗性非常高并且火花不产生碳残留物而仅产生不导电的蒸气。其他介电性质(例如介电常数，表面电阻率，体积电阻率和功率因数)具有极大关注价值。
在机械性质方面，在宽范围的操作温度内，对预定义变形的抗压缩性是PTFE的最佳特性之一。抗弯强度、弹性记忆和硬度是辨别PTFE的其他特性。另外，其摩擦学性质，具体地非常低的摩擦系数，使PTFE成为一种独特的材料。
此外，第二含氟聚合物可以用一种或多种无机和/或有机添加剂，如例如玻璃纤维、碳、石墨、二硫化钼、青铜、钢、陶瓷粉末及其混合物填充。所述添加剂的使用改善该含氟聚合物的性能，例如它们提高其抗压强度、硬度和耐磨性，降低热膨胀系数以及表面和体积电阻率。
聚合物材料中存在的多孔粒子优选为玻璃多孔粒子。多孔粒子具有低于或等于5μm的粒度尺寸d50。
通过术语“粒度尺寸d50”，其意指粒度分布的中值直径或平均值，并且其是在累积分布的50％处的粒子的直径的值。
多孔粒子具有以体积计30至60％的孔隙率，优选50％的孔隙率(表示为空穴体积与总体积之间的百分比)。
聚合物材料可以利用本领域已知的方法制备。例如，将粉末形式的PTFE在模具中压制以在环境温度获得预成型件。在从模具中移出后，将预成型件在炉中加热至高于其熔融温度并且烧结。这些粒子在烧结期间的固结被称为聚结，并且产生均匀的抗性结构。
根据本发明，在混合器中将含氟聚合物在0℃与负载有抗菌离子的多孔硅酸盐粒子混合。PTFE的低温度促进混合，防止混合物免于过热。
将由此获得的混合物在压机(模制机，press)中以圆筒形形状(圆柱形形状，cylindrical shape)预成型并且随后烧结。热循环包括达到烧结温度的斜坡，处于烧结温度的平台和冷却阶段。然后将由此获得的圆筒状物借助于如本领域已知的剥落工艺转化为无孔膜，所述剥落工艺利用例如具有受控进料和刀片的水平车床，其以受控方式剥落具有均匀厚度的膜。
基于聚合物材料的总重量，获得的聚合物材料的膜可以包含95至99重量％的第二含氟聚合物和1至5重量％的多孔硅酸盐粒子。获得的膜具有等于或小于100微米的厚度。
本发明的复合材料的纺织基材可以由选自由玻璃纤维、芳族聚酸胺纤维和碳纤维组成的组中的纤维制成。芳族聚酸胺纤维例如是Nomex纤维和Kevlar纤维。在本发明的复合材料的制备期间，将纺织基材用第一含氟聚合物浸渍以允许纺织基材与聚合物材料的膜的偶联。
基于复合材料的总重量，含氟聚合物(理解为第一和第二含氟聚合物的总和)在该复合材料中以高于50重量％的量存在。
本发明的复合材料有利地可以储存长时间期；其允许制造不可渗透的柔性袋以及管道或其他容器和表面覆层(涂层，coating)。
除了PTFE的机械强度、化学惰性和对极端温度(-200°至+260°)的适用性之外，本发明的复合材料由于抗菌粒子的存在而允许容器和表面的再利用以及因此在成本、体积和占据空间方面的节省。
本发明的复合材料经由以下步骤制备：
a)将至少一种第二含氟聚合物与多孔硅酸盐粒子混合以获得聚合物材料，所述多孔硅酸盐粒子具有低于或等于5μm的粒度尺寸d50和30至60体积％的孔隙率并且负载有选自由银、铜、锌和镍组成的组中的至少一种金属的抗菌离子；
b)将从步骤a)获得的所述聚合物材料在压机中以圆筒形形状预成型并且随后进行烧结以获得聚合物材料的圆筒状物；
c)将步骤b)中获得的所述聚合物材料的圆筒状物剥落以获得具有均匀厚度的聚合物材料的膜；
d)将纺织基材通过在至少400℃烧结用水分散体形式(作为水分散液，in aqueousdispersion)的第一含氟聚合物浸渍，使得所述第一含氟聚合物渗透到所述纺织基材的纤维之间；
e)借助于热层压并且在压力下将至少一个从步骤c)获得的聚合物材料的膜施加至用所述第一含氟聚合物浸渍的所述纺织基材。
优选地，步骤b)在至少255℃的温度并且施加至少4巴的压力下进行。
利用其进行浸渍纺织基材的步骤a)的第一含氟聚合物选自由以下各项组成的组：聚四氟乙烯，四氟乙烯-六氟丙烯共聚物，以及四氟乙烯-全氟烷基乙烯基醚的共聚物，其中FVE的碳原子数为1至5，并且基于复合材料的总重量，以大于30重量％的量存在。
从步骤d)获得的经浸渍的纺织基材可以具有小于或等于1100微米的厚度。
在一个实施方案中，本发明的复合材料包括在两侧上都层压有如上所述的聚合物材料的膜的纺织基材。
本发明的复合材料具有优异的柔性，保持良好的机械强度。其还是不可渗透的，无孔的，重量轻的，耐宽温度范围(-73℃至260℃)的，化学惰性的，并且具有抗菌性质。
根据本发明的复合材料可以用于制造用于流体、优选水的容纳和/或运输元件。本发明的复合材料因此可以用于制造用于运输和储存流体的柔性袋，而且可以用于制造食品容器或用于管道，例如在航空航天领域中。
其还可以用于制造抗菌覆层面板。
本发明的其他特征根据以下对一些仅仅是示例性而非限制性的实例的描述将变得明显。
实施例1
聚合物材料的抗菌性质
在实验室中，利用标准方法(混合，预成型和烧结)来制备三个具有不同百分比的负载有银离子的硅酸盐粒子的根据本发明的聚合物材料(TFE-全氟丙基乙烯基醚(PPVE)的共聚物，其中相对于TFE含量，PPVE含量为大约0.3重量％的量)的棒状物(直径：60mm，高度80mm)。
根据ISO 22196：2007标准程序：“塑料一塑料表面上的抗菌活性的测量(Plastics-Measurement of antibacterial activity on plastics surfaces)”，利用金黄色葡萄球菌(Staphylococcus aureus)ATCC 6538和肺炎克雷伯菌(Klebsiellapneumonia)ATCC 4352来测试三个样品的抗菌活性。
实验条件为：
-微生物：肺炎克雷伯菌(Klebsiella pneumoniae)ATCC 4352和金黄色葡萄球菌ATCC 6538。
-接种物：0.4mL的细菌悬浮液，在营养肉汤培养基和盐水溶液中以1/500比例稀释的6x 105UFC/mL。
-接触时间：24小时，在37℃。
-中和溶液：10ml(30g/l卵磷脂，30g/lTween 80，5g/l硫代硫酸钠，1g/lL-组氨酸，0.68g/l KH2PO4，(在7.2+/-0.2的pH))。
-样品的消毒：是，在121℃的20分钟。
-膜施加：是(40mm x 40mm)。
活菌数量的计算：
N＝(100x C x D x V)/A，其中：
N＝每个试管每cm2回收的活菌的数量。
C＝计数的菌落的平均数量。
D＝计数的菌落的稀释因子。
V＝加入的中和溶液的体积，以ml计。
A＝膜的面积(1600mm2)，以mm2计。
样品的抗菌活性R如下计算：
R＝(Ut-U0)-(At-U0)＝Ut-At
其中：
U0＝在接种后立即从参考样品回收的细菌数量的对数的平均值，以细胞/cm2计。
Ut＝在24小时接触后从参考样品回收的细菌数量的对数的平均值，以细胞/cm2计。
At＝在24小时接触后从样品回收的细菌数量的对数的平均值，以细胞/cm2计。
R＝抗微生物活性。
结果在表1中给出。
表1
重复相同的测试以研究真菌生长。同样，在这种情况下未观察到真菌生长。
实施例2
借助于上述方法，将抗菌含氟聚合物的无孔膜层压在经浸渍的玻璃纤维织物的两侧上，所制备的本发明的复合材料具有在表2中给出的机械性质。
表2

Claims (14)

1.一种无孔复合材料，所述无孔复合材料包括用第一含氟聚合物浸渍的纺织基材和用多孔硅酸盐粒子填充的包含至少一种第二含氟聚合物的聚合物材料的膜，所述多孔硅酸盐粒子具有小于或等于5μm的粒度尺寸d50和30至60体积％的孔隙率并且负载有选自由银、铜、锌和镍组成的组中的至少一种金属的抗菌离子。
2.根据权利要求1所述的复合材料，其特征在于，所述纺织基材利用选自由玻璃纤维、芳族聚酸胺纤维和碳纤维组成的组中的纤维制备。
3.根据权利要求1所述的复合材料，其特征在于，所述第一含氟聚合物和所述第二含氟聚合物在所述复合材料中的总量大于所述复合材料的总重量的50重量％。
4.根据权利要求1所述的复合材料，其特征在于，所述第二含氟聚合物选自由以下各项组成的组：聚四氟乙烯，四氟乙烯-六氟丙烯共聚物，以及四氟乙烯-全氟烷基乙烯基醚的共聚物，其中所述FVE的碳原子数为1至5。
5.根据权利要求4所述的复合材料，其特征在于，所述第二含氟聚合物是四氟乙烯-全氟烷基乙烯基醚的共聚物，其中所述全氟丙基乙烯基醚以低于所述四氟乙烯的总重量的1重量％的量存在。
6.根据权利要求5所述的复合材料，其特征在于，所述全氟丙基乙烯基醚以所述四氟乙烯的总重量的0.05至0.5重量％的量存在。
7.根据权利要求4所述的复合材料，其特征在于，所述第二含氟聚合物是聚四氟乙烯。
8.根据权利要求1所述的复合材料，其特征在于，所述第二含氟聚合物用至少一种无机和/或有机添加剂填充，所述无机和/或有机添加剂优选地选自由玻璃纤维、碳、石墨、二硫化钼、青铜、钢、陶瓷粉末及其混合物组成的组。
9.根据权利要求1所述的复合材料，其特征在于，所述多孔硅酸盐粒子是多孔玻璃粒子。
10.根据权利要求1所述的复合材料，其特征在于，基于所述聚合物材料的总重量，所述聚合物材料包含95至99重量％的所述第二含氟聚合物和1至5重量％的所述多孔硅酸盐粒子。
11.根据权利要求1所述的复合材料，其特征在于，所述基材用选自由以下各项组成的组中的第一含氟聚合物浸渍：聚四氟乙烯，四氟乙烯-六氟丙烯共聚物，以及四氟乙烯-全氟烷基乙烯基醚的共聚物，其中所述FVE的碳原子数为1至5。
12.一种用于制备根据权利要求1的复合材料的方法，所述方法包括以下步骤：
a)将至少一种第二含氟聚合物与多孔硅酸盐粒子混合以获得聚合物材料，所述多孔硅酸盐粒子具有低于或等于5μm的粒度尺寸d50和30至60体积％的孔隙率并且负载有选自由银、铜、锌和镍组成的组中的至少一种金属的抗菌离子；
b)将从步骤a)获得的所述聚合物材料在压机中以圆筒形形状预成型并且随后烧结，以获得聚合物材料的圆筒状物；
c)将步骤b)中获得的所述聚合物材料的圆筒状物剥落以获得具有均匀厚度的聚合物材料的膜；
d)通过在至少400℃烧结将纺织基材用水分散体形式的第一含氟聚合物浸渍，使得所述第一含氟聚合物渗透到所述纺织基材的纤维之间；
e)借助于热层压并且在压力下将至少一个从步骤c)获得的聚合物材料的膜施加至用所述第一含氟聚合物浸渍的所述纺织基材。
13.根据权利要求12所述的方法，其特征在于，所述步骤e)在至少255℃的温度且施加至少4巴的压力下进行。
14.一种用于流体、优选水的容纳和/或运输元件，所述元件利用根据权利要求1所述的复合材料制成。
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