CN1222883A - 柔韧的防水复合材料 - Google Patents

柔韧的防水复合材料 Download PDF

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CN1222883A
CN1222883A CN97195772A CN97195772A CN1222883A CN 1222883 A CN1222883 A CN 1222883A CN 97195772 A CN97195772 A CN 97195772A CN 97195772 A CN97195772 A CN 97195772A CN 1222883 A CN1222883 A CN 1222883A
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W·策恩德
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W L Core & Associates GmbH
WL Gore and Associates GmbH
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Abstract

本发明提供不透气的防水透水汽的复合材料,该复合材料具有提高的透水汽的性能。该复合材料包括:一层微孔聚合物,该聚合物是可透水汽且防水的。该层与不透气、防水可透水汽分子的聚合物层接触。第三层为微孔的透水汽的亲水性聚合物,该聚合物在不透气的聚合物层的另一面上。

Description

柔韧的防水复合材料
发明领域
本发明涉及柔韧的层压复合材料，它们特别适用于防水但透水汽的纺织材料，或由这些材料制成的服装。
发明背景
用于雨衣的材料是已知的，它们具有一层发泡微孔聚四氟乙烯(ePTFE)或多孔聚丙烯，参见Gore等的美国专利4,194,041或Henn的美国专利4,969,998。在Gore的美国专利3,953,566中揭示的发泡微孔防水聚四氟乙烯材料特别适用于此用途。它是防水的，但能使汗水通过。聚氨酯类和其它聚合物也可用于此用途。为了使用于织物方面(textile sector)的材料具有良好的柔韧性，所述微孔层应制得尽可能薄。然而，膜比较薄通常会导致性能降低，而且涂层薄具有防水性下降的危险。
美国专利4,194,041提到了在微孔聚合物上使用另外的涂层，该涂层是基于薄的不透气涂层，它由聚醚聚氨酯或聚全氟磺酸组成，通过扩散运送水汽分子。使用该薄的涂层以减少表面活性剂和污染物透过聚合物。由于聚合物的化学结构，在微孔结构上的这种单一涂层显示出高的运送水分子通过聚合物材料的能力(高的透水汽性)。该薄膜应制得尽可能薄，以不影响柔韧性，并向复合材料提供充分的保护。而且，对于较厚的单一薄膜，透水汽性大大降低。
美国专利4,969,998中揭示了一类复合膜。在该膜中，内层材料部分渗入微孔外层的孔中。作为微孔外层的材料，提到了微孔发泡聚四氟乙烯。作为内层，提到了聚醚-聚硫醚。后一材料在一定程度上填入微孔层的孔中，但始终是密封的、无定形的和无孔的。据报道，该复合材料的透湿气率高于上述层压材料的透湿气率。然而，当该复合材料用作雨衣的纺织层压材料时，发现在极大的运动负荷下形成大量汗液，后者并不总能消散在环境中而没有残留物。残留在服装内的汗液对于良好的触觉和穿着舒适有不良的影响。
发明的综述
本发明的目的在于提供柔韧的防水透水汽的复合材料，该材料具有提高的透湿气率。
所述复合材料为：
(a)一层微孔聚合物，该聚合物是可透水汽且防水的，所述层粘附于，
(b)不透气聚合物层，该层可透水汽，所述层(b)粘附在层(a)对面一侧的，
(c)一层微孔聚合物，它是可透水汽的且亲水的。
微孔聚合物具有穿透内部结构的孔隙，形成从一面到另一面的相互连接的连续的气体通路。
现已发现，当服装中使用含有层(c)的复合材料且该层在最里面时，从里到外的透湿气率出人意料地大于其它不含亲水层的三层复合材料之一的透湿气率。这一令人吃惊的现象可能是由于当界面上存在水时，中间层(b)的透湿气率以过量比例增加的缘故。具有亲水性能的微孔内层的作用就象海绵类，吸收形成的汗液，并将其散布于较大的表面积上，使边界层至内部扩散层上的单个水分子容易通过，或者以较高的浓度进入溶液，因此更快地迁移或扩散至外侧，
微孔层(c)可以是本来就具有亲水性的，或者是使用已知的方法赋予其亲水性的，例如使用美国专利5,209,850中所述的方法。在美国专利5,352,511和5,354,587中提到了赋予微孔聚合物亲水性的方法。DE-A 4243955也是关于初始赋予氟聚合物类防水层亲水性，其它的处理方法如下所述。
较好的是所述微孔聚合物层的实例为多孔发泡聚四氟乙烯(ePTFE)薄膜。
发明详述
定义
“柔韧的”是指容易弯曲，即柔软的。
“防水的”是指在13.8kN/M2的水压下材料是防水的，
“微孔的”是指材料具有穿透内部结构的非常小的细微孔隙，形成从一面至另一面相互连接的连续的气体通路。
“不透气的”是指经下述的Gurley试验测定至少两分钟观察不到气流。
“可透水汽”是指MVTR或者每24小时至少1000g/m2，较好为每24小时2000g/m2。
“亲水性”材料是指多孔材料，当遇到液态水而不加压时，其孔隙中充满液态水。
“粘附于”是指层与层表面接触或层(b)全部或部分浸入层(a)的孔中，以及通过使用粘合剂进行粘合。
适宜的用于层(a)和层(c)的微孔聚合物包括氟聚合物，如聚四氟乙烯或聚偏氟乙烯；聚烯烃，如聚乙烯或聚丙烯；聚酰胺；聚酯；聚砜、聚醚砜及其混合物，聚碳酸酯，聚氨酯。为了获得柔韧性，这些层应是薄的。
如果层(c)的微孔聚合物不是天然具有亲水性的，则可对它进行处理，使它具有亲水性。可用于处理该微孔聚合物使它具有亲水性的材料包括：四氟乙烯和乙酸乙烯酯的共聚物、聚丙烯酸及其共聚物、聚丙烯酰胺及其共聚物、聚乙酸乙烯酯(PVA)、聚苯乙烯磺酸盐；聚乙二醇或聚丙二醇(PEG,PPG)、亲水性聚硅氧烷；阴离子、阳离子、非离子或两性表面活性剂或混合物以及上述物质的复合体的水溶液、醇溶液或水/醇溶液。
用亲水性材料进行处理是通过将该材料以液态(如该材料的熔体，或者溶液或乳胶分散体)施用(如将表面浸渍在所述液体中，或将所述液体涂抹、喷涂、辊涂或刷涂在表面)而完成的。施用一直进行到该微孔结构的内表面被涂覆，但孔中未充填该液体，因为否则的话将破坏或大大降低该层的透水汽性能。因此，亲水性材料的存在对孔隙度几乎没有影响；这就是说，限定微孔聚合物中孔隙的壁最好仅带有很薄的所述材料涂层。该材料的施用可在各种溶液或分散体浓度、固体含量和/或在各种温度或压力下进行，
用多种方法中的任何一种方法将不透气的聚合物层(b)与聚合物层(a)和(c)复合。不透气的聚合物可以液体混合物的液态施用，或者可以固态薄片形式施用。如果该聚合物是以薄片的形式，则可通过使这些薄片通过夹辊或施用可吸入的粘合剂将它层压于疏油性膜片。适宜的用于层(b)的聚合物有透水汽但不透空气的聚氨酯，例如Hypol2000(W.R.Grace & Co.)。它可进行预交联或施用之后进行交联。微孔层(c)可进行预处理，使它具有亲水性。这可在层(b)固定之前或之后进行。
在一种制造三层复合材料的方法中，使用辊涂机将预交联的聚氨酯树脂与固化剂一起施用于第一片ePTFE薄膜，该涂层重量可为，例如，10克/平方米。然后施用另一片微孔ePTFE层，将用此方法接合的层送入两个压辊之间的狭缝，使尚未完全交联的树脂被压制到一定的程度进入微孔结构并渗入孔中。然而，如DE-PS2925318中所述，该聚氨酯树脂可作为成品薄膜首先粘附于一层。然后经上述处理，使一微孔薄膜层(层(c))具有亲水性。
所用的ePTFE层的厚度、密度和孔径可根据用途而不同。
本发明的复合材料可层压于织物的一面或两面，所得到的材料可用于制造防水但可透水汽的服装。
该复合材料可用于雨衣和运动服装。当然该复合材料也可用于其它工业领域，它可用于从溶液、蒸馏液、污水浓缩液、浓缩汁或生物体系中去除低分子量的分子，也可用于渗析领域。该应用的先决条件是中间层具有选择性扩散的性能，该中间层对于通过分子的溶解度必须高于对于欲浓缩的混合物中其它分子的溶解度。
该复合材料的另一个优点是存在气孔但不导致泄漏。从里面(即面对穿着者身体的一面)通过孔渗入的水份将首先形成水滴。然而，该水滴通过毛细管力重新被送入该内层，并送入中间层(b)。在该表面，水分布在表面并“转变”成水汽排出。
测试方法
透气性/不透气性-Gurley数测定
用下述方法获得Gurley数：
用W. & L.E.Gurley & Sons制造的Gurley透气度测定仪(ASTM D726-58)测定样品耐空气流动性。根据Gurley数报告结果，该结果为在水的压降为1.215千牛/平方米时，100立方厘米的空气流经6.54平方厘米试验样品所用的时间(秒)。如果在120秒内没有观察到气体流过，则该材料是不透气的。
湿汽透过率测试(MVTR)
在本方法中，将约70毫升由35重量份乙酸钾和15重量份蒸馏水组成的溶液放入内径为6.5厘米的133毫升聚丙烯杯中。用授予Crosby的美国专利4,862,730中所述方法使用乙酸钾测得每24小时的最小MVTR约为60000克/平方米的发泡聚四氟乙烯(PTFE)薄膜(可从特拉华州Newark的W.L.Gore &Associates,Inc.购得)热密封含该溶液的杯口，以形成绷紧的防漏的微孔隔膜。使用控温辊(temperature controlled roll)和循环水浴，将水浴装置的温度控制在23℃±0.2℃。在测定之前，使待测样品处于23℃的温度和50％的相对湿度下。放置样品，使待测微孔聚合物薄膜与水浴表面接触，在放入杯组件中之前，对有织物的层压材料至少平衡15分钟，对薄膜复合材料至少平衡10分钟。将该杯组件称重精确到1/1000克，并倒置在测试样品的中间部位。通过水浴中的水和饱和盐溶液之间的推动力，在该方向扩散提供水流而输送水。样品测定15分钟，然后取出该杯组件并重新称重。由杯组件重量增加量计算MVTR，并以每24小时每平方米样品面积水的克数表示。
实施例1
将两片由W.L.Gore & Associates,Inc.提供的发泡微孔聚四氟乙烯(PTFE)薄膜层压在一起制备复合材料。这两片PTFE薄膜的标称孔径为0.25微米，重量约为20克/平方米，厚度为40微米。为了层压透水汽的(可吸入的)聚氨酯(PUR)，施用美国专利4,942,214中所述的MDI预聚物和烯化氧，并施用辊涂覆装置使其部分渗入第一片薄膜的微孔结构，然后用PUR作为两个夹辊之间的粘合剂层压第二片薄膜。在室温下湿固化PUR之后，将上述层压膜的一面涂覆美国专利No.5,209,850中所述的聚合物溶液，使微孔PTFE具有亲水性(沉积=4克/平方米)。干燥之后，所得到的复合材料的一面在浸入水中之后变成透明的。
首先使隔膜的未经处理的一面面对水，然后使隔膜的亲水性一面面对水，测定该复合材料的湿汽透过率。
对于未经处理的一面，每24小时测得的MVTR为28000克/平方米，而对于面对水的亲水性一面，每24小时测得的MVTR为75000克/平方米。
实施例2
在施用亲水性涂层之前，采用逐点粘合的方法(spot wise adhesion process)将实施例1的复合材料层压在120克/平方米聚酯织物的一面。用该方法之后，未层压于织物的一面是用美国专利No.5,209,850中所述的聚合物赋予亲水性的亲水性PUR涂层(沉积=4克/平方米)。
对于面对水的织物一面，每24小时测得的MVTR为7600克/平方米，而对于面对水的亲水性薄膜一面，每24小时测得的MVTR为23000克/平方米。
实施例3
用与实施例1一样的方法制得复合材料，不同的是亲水性处理是将市售的防雾喷剂(Nigrin Anti Fogging Spray,Inter-Union Technohandel Landau)施用于一面。对于未经处理的一面，每24小时测得的MVTR为28000克/平方米，而对于面对水的亲水性一面，每24小时测得的MVTR为79000克/平方米。

Claims (9)

1．一种柔韧的防水透水汽的复合材料，它包括：
(a)一层微孔聚合物薄膜，该聚合物是可透水汽且防水的，所述层粘附于
(b)不透气聚合物层，该层可透水汽，所述层(b)粘附在层(a)对面一侧的，
(c)一层微孔聚合物薄膜，它是可透水汽的且亲水的。
2．如权利要求1所述的复合材料，其特征在于它层压于织物层的一面或两面。
3．如权利要求1所述的复合材料，其特征在于所述层(a)膜为发泡聚四氟乙烯。
4．如权利要求3所述的复合材料，其特征在于它层压于织物层的一面或两面。
5．如权利要求3所述的复合材料，其特征在于层(b)为聚氨酯，而层(c)为已被赋予亲水性的发泡聚四氟乙烯。
6．如权利要求5所述的复合材料，其特征在于它层压于织物层的一面或两面。
7．用于形成复合材料的方法，它包括以下步骤：
(1)形成可透水汽但防水的微孔聚合物薄膜；
(2)形成不透气但可透水汽的聚合物；
(3)形成可透水汽且亲水性的微孔聚合物薄膜；
(4)将这些聚合物粘合在一起形成三层的层压材料。
8．用于形成复合材料的方法，它包括以下步骤：
(1)形成可透水汽但防水的微孔聚合物薄膜；
(2)形成不透气但可透水汽的聚合物；
(3)形成可透水汽且经亲水性材料处理的微孔聚合物薄膜；
(4)将这些聚合物粘合在一起形成三层的层压材料。
9．含有如权利要求1所述的复合材料的服装。
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US6235662B1 (en) 2001-05-22
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DE69703694D1 (de) 2001-01-18
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