CN1111476C - 透气的薄膜/无纺布层合物及其制法和包含所述材料的制品 - Google Patents

透气的薄膜/无纺布层合物及其制法和包含所述材料的制品 Download PDF

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CN1111476C
CN1111476C CN94194968A CN94194968A CN1111476C CN 1111476 C CN1111476 C CN 1111476C CN 94194968 A CN94194968 A CN 94194968A CN 94194968 A CN94194968 A CN 94194968A CN 1111476 C CN1111476 C CN 1111476C
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nonwoven
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fiber
polyolefin
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A·L·麦科马克
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Kimberly Clark Worldwide Inc
Kimberly Clark Corp
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Abstract

这里公开的是一种透气的薄膜(12)和用透气薄膜制成的透气的布样薄膜/无纺布复合体(10)，该薄膜是经过拉伸制薄并粘结到纤维聚烯烃无纺布(14)上去的。某些热塑性薄膜例如线型低密度聚乙烯薄膜，是难于热粘结到例如聚丙烯无纺布上去的，因为这两种聚合物是不相容的。本发明将粘结剂加到两层中的一层内或两层内都加，从而使两层较易粘结在一起。还公开了制造各种复合体的方法。

Description

透气的薄膜/无纺布层合物及其制法和包含所述材料的制品
                            发明领域
本发明的目标是提供透气薄膜和透气的布样薄膜/无纺布复合体以及它们的制造方法。更具体而言，本发明的目标是提供一种透气的薄膜/无纺布层压物，它包括一层薄的按各别点层压到增强的布样纤维无纺布上的透气膜。本发明在要求结实、舒适、透气和不透水的广阔多样的领域有其实用性。两个具体的应用领域包括：人身护理吸收物品和与保键有关的项目包括帘幕、长服和其他外科用品。人身护理吸收物品的例子包括尿布、卫生巾、大小便失禁服、训练便溺的裤子、绷带等。本发明的材料还可用于制作一件衣服的全部或一部分。
                            发明背景
现在的许多产品都包含有人造的、合成的成分，人身护理吸收物品如尿布只是其中的一个例子。现在的尿布，典型地是包括用一层合成纤维无纺布作为贴身衬垫材料来贴近婴儿的皮肤。尿布内部为吸收芯子，它可用天然木浆纤维配合合成纤维和超级吸收剂制成。尿布的背面或外罩传统上是用塑料薄膜制作，这是考虑价格问题，同时也是因为塑料薄膜具有不透液体的性质。
尽管塑料薄膜在使用中能有效地包容液体和其它废物，但是这同一种塑料薄膜却有着一定的缺点：接触它时感到不舒服，还不易透过水蒸气，从穿戴舒服的立埸来看，塑料薄膜易于引起皮肤的水合作用，从而使婴儿更易罹患尿布皮疹。曾有一种解决办法是用透气的塑料薄膜代替普通的无孔塑料薄膜做尿布的背面材料。有多种方法可使薄膜透气，包括打孔和使用填充剂时。当使用填充剂时，常将薄膜在辊子间挤压以使填充剂破裂，或拉伸以使在聚合物和嵌入聚合物中的粒子之间产生出小的间隙。这样可在薄膜的一面与另一面之间形成曲折的通道，使薄膜在起到液体(如水和尿)阻挡层作用的同时还能提供散发水蒸气的通道。聚烯烃薄膜常被用来制造透气薄膜。做这种用途的一种特别有用的薄膜是用含有有机填充剂和/或无机填充剂的线型聚烯烃制造的。这种加有填充剂的聚烯烃薄膜能提供很好的水蒸气传输能力，从而使尿布对穿戴者来说更舒适。因此，依靠使用透气材料可使尿布或其他产品内部的相对湿度和温度降低。尽管如此，这样的透气薄膜还是有冰凉和滑腻的缺点，因为透气薄膜能往产品外面透出水气，这些水气在薄膜表面易于凝结。结果，就有试着用无纺布做尿布背面材料的另一种解决方法。
当用纤维无纺布做尿布的背面材料时可减轻上述的薄膜问题，但是，这样的纤维无纺布通常对液体包括尿液的通过只能提供很差的阻挡层作用。因此，多数无纺布单靠他们自己是不适于用做背面材料的。某些纤维无纺布在排拒液体上优于其它品种，特别是当它们包括一层细纤维无纺材料如一层熔融吹制物时是如此。熔融吹制纤维布是用一种细纤维制成的，这种细纤维是将熔融的热塑性塑料挤压穿过精细拉丝模的毛细管而形成熔融的线或细丝，然后用高速气体把它吹细而制成的。制得的纤维其直径通常非常小，约在10微米或其以下，并堆集在成形台上成为纤维无纺絮的形态，其孔隙结构非常小，趋于能阻止液流。参见Buntin等的美国专利No.3,849,241的例子。但是，即使是使用熔融吹制物层的纤维无纺材料也常证明是不完全适于用作人身护理产品的背面材料的。
鉴于薄膜和纤维无纺材料两者的上述缺陷，曾有人做过把两种材料结合起来的尝试，以图能依赖一种材料的优势来克服另一材料的弱点。将透气薄膜和纤维无纺材料的最好特性结合起来的例子，是加有填充剂的线型聚烯烃薄膜和聚丙烯或聚丙烯共聚物短纤捻合布的结合物。为了使这两种材料得以协调工作，必须将它们以某种方式联结在一起。有多种联结薄膜和无纺布的方法，包括加热和超声粘结、胶合、针穿和缝合。如果目的是要保持液体阻挡层的作用，针穿和缝合通常是不合用的。因为这些方法所造成的孔洞较大，因而会泄漏液体。粘结和胶合由于它们本身包括堵塞薄膜孔隙和使整个层合物变硬的缺点也不合适。薄膜和无纺布之间的层压应较全面地进行。照例，要想用粘合剂把薄膜和无纺布层压好，就必须在两种材料的整个接合面都喷一层薄而均匀的粘合剂，或者必须在分隔开的间距上局部使用更多数量的粘合剂。均匀使用粘合剂常常会堵塞薄膜一个面上的孔隙，从而使原先是有孔的薄膜变成无孔的。这种方法不合适。在较局部的面积上使用更多数量的粘合剂会减少薄膜被堵塞的面积，但由于集中使用粘合剂又会带来使薄膜/无纺布层合物变硬的缺点。由此可见，更合乎需要的是使用热层压技术。
热层压可通过加热和加压来实现，例如用加热的型样辊子或用超声波。当薄膜和无纺布都是用同一种聚合物制造时，这两种技术都很适合用来把它们结合在一起。但有时用来制造薄膜的聚合物与用来制造纤维无纺布的聚合物并不相同。这可能是既有价格上的原因也有物理性能上的原因。线型低密度聚乙烯(LLDPE)薄膜和聚丙烯无纺布就是一个例子。这两种聚合物在热性能上是互相不相容的，它们不能热层压在一起而具有至少5克的粘合力。还有一种情况，就是做两层材料的聚合物虽是同样的，因此也是相容的，但实行热层压时必须使用那么多的热量和压力，以致最终在薄膜上形成了孔洞，并常使层合物过分坚硬。因此，需要有一种热层合方法，它能把这样的不相容的和相容的材料粘结起来，而又能使两种材料的优点和热层合法的优点得以发挥。也需要这样制得的产品。由下面的详细说明可知，本发明已满足了这些需要。
                            发明概述
本发明的方法已经克服了前述的各种缺点。在这里公开的是一种透气薄膜和一种用透气薄膜热粘结到纤维聚烯烃无纺布上做成的透气的布样薄膜/无纺布复合体。上述材料的制造方法也已公开。
按理想来说，层压薄膜和无纺布的最符合需要的方法之一是热粘结。热粘结要求两种材料在热性能上相容。通常是，薄膜和无纺布各自用能提供该特定材料所需的性能的聚合物来制作，但各材料相互间不易热粘结起来，或根本不能热粘结。本发明在薄膜内加进了粘结剂，它只要求能与纤维无纺布的聚烯烃聚合物成分相相容，在层压过程中，它起着对热和压力敏感的粘结剂的作用。另一种办法是，可把粘结剂加到纤维无纺布的纤维中去，以在薄膜与无纺布层压时起帮助作用。重要的是，把两层材料粘结在一起所用的温度要低于薄膜或纤维的聚烯烃聚合物的熔点，以便保持薄膜或纤维的完整性，从而降低在层压过程中形成孔洞和失去强度的危险。因此，对本发明来说很重要的一点是，作为一个整体，薄膜或纤维不允许达到它们的总熔点，从而兼顾成品复合体的完整性和挡水特性。依靠粘结添加剂而实现“局部化”热粘结并采用一种不连续粘结的形式，就提供了一种能以通气膜孔隙特性损失最小的办法来保证粘结，同时还能保持复合体或层合物总体上的良好韧性。
本发明的一个实施方案是，透气的薄膜/无纺布层合物是这样做成的：第一步，用一种混合物制造薄膜，混合物内包括，以其干重为基础按薄膜总重计，为：约10-68％的以线型为主体的聚烯烃聚合物，约30-80％的填充剂，其平均粒径约为0.5-5微米，以及约2-20％的粘结剂。然后将薄膜在辊子之间拉伸或挤压变为透气的。薄膜一旦制成，就至少应有每平方米每24小时100克的水蒸气传输率。其后将纤维聚烯烃无纺布热层压到薄膜上而做成层合物或复合体。要求层合物应具有用5克的负荷才能把两层互相分拆开的强度。
制造薄膜层的合适的原料包括但不限于以线型为主体的聚烯烃聚合物，如线型低密度聚乙烯；以及填充剂，如碳酸钙。制造纤维无纺布的合适的原料包括但不限于聚丙烯，聚丙烯纤维和线型低密度聚乙烯纤维这样的聚烯烃混合物，以及以聚烯烃成分组成纤维外表面的双组份纤维。
制造方法包括，第一步先做预挤压成形的上述聚合物的混合物，然后把该混合物挤压成薄膜。薄膜制成后，就在低于薄膜中以线型为主体的聚合物组份的熔点温度下进行拉伸，更符合需要的是还要在低于粘结剂软化点温度下拉伸。依靠拉伸，使薄膜变薄、变得有孔隙而透气。薄膜经拉伸后，应至少有每平方米每24小时100克的水蒸气传输率。此后，在低于薄膜中以线型为主体的聚合物组份熔点的温度下把薄膜粘结到纤维聚烯烃无纺布上而做成层合物。另外，如果需要的话，可以在薄膜粘结到无纺布上以后让它回缩，从而使整个复合体收缩，这就可做成波浪形的表面和膨松的复合体。
所做成的透气的、布样薄膜/无纺布复合体，有着多种多样的用途，决不止是只用作人身护理吸收物品的外罩而已。这样的物品典型的是包括体侧的内衬和一个其中设置一个吸收剂芯的外罩。本发明的材料可以用作外罩，以其纤维无纺布层朝外作产品的外表面，而以薄膜层临近吸收剂芯。
如果需要热粘结，但用以制造薄膜和支持层的全部或一部分聚合物在热性能上是不相容时，作为一种替代办法，可在纤维无纺布支持层上加入粘结剂以取代或补充在薄膜上加入粘结剂。粘结剂可以加在制造纤维的聚合物混合物内。当纤维是单组份纤维时，粘结剂可加到整个纤维内。除单组份纤维外，也有可能以全部或部分地用多组份纤维，如双组份纤维来制成纤维无纺布支持层。双组份纤维的例子包括但不限于皮/芯纤维、并排纤维和海/岛纤维。此外，双组份纤维也可用来制作纤维无纺布支持层。对所有这些纤维外形不说，粘结剂必须存在于纤维的那一部分内，使之至少成为纤维外表面的一部分，以便粘结剂能接触到并与薄膜层的一部分粘结起来。纤维无纺布支持层做成后，它就能热、压力、热和压力和/或超声波使之热粘结到薄膜层上。
附图简述
图1是本发明的透气的、布样薄膜/无纺布复合体的横断面图。
图2是本发明的透气的、布样薄膜/无纺布复合体制造方法示意图。
发明详述
本发明的目标是制造出改进的薄膜/无纺布层合物，它是用一种薄膜热粘结到以聚烯烃为基本材料的纤维无纺布上而成，这种薄膜由以线型为主体的聚烯烃聚合物、填充剂和粘结剂组成。举例来说，传统的线型低密度聚乙烯薄膜是不能热粘结到以聚丙烯为基本材料的无纺布上去的，这是因为这两种聚合物不相容，制造薄膜和无纺布的熔点也不一致。本发明提供一种透气的薄膜，由于它独一无二的成分和工艺条件，它可以热粘结到以聚丙烯为基本材料的无纺布上。在一个具体的实施方案中，一种利用线型低密度聚乙烯和粘结剂的混合物制成的透气薄膜被热粘结到了聚丙烯无纺布上。做成的层合物表现出的性状包括：外表面有柔软、布一样的感觉，在起到阻挡液体流通的作用的同时，还有良好的水蒸气通透能力。此外，由于线型低密度聚乙烯薄膜经过高度的拉伸和加入填充剂，薄膜是透气的、触觉非常柔软，“噪声”或“卡嗒声”很小很小。因此，这种层合物有着广泛的用途，下面指出的专门用途并不意味着限制它用于别的埸合。它的专门用途是作人身护理吸收产品的背面材料，这些产品包括尿布、卫生巾、训练便溺的裤子、大小便失禁服、绷带等。本发明的材料还可用于制作一件衣服的全部或一部分。此外，本发明的材料还可用于制作医院用品的全部或一部分，例如外科帘幕、长服、擦布、鞋罩、面罩和帽子。因此，这些用途和其它用途都被认为是在本发明的范围之内的。
在另一个实施方案中，可以把粘结剂加到纤维无纺布中，特别是加到制造无纺布纤维的聚合物混合物中，使之成为多数纤维外表面的至少一部分。因此，可提供另一种手段，使得两层本来热性能不相容的材料能够热粘结或热层压在一起。所制得的层合物也能适用于上述的各种用途。
在图1中，本发明的复合体或层合物10，其最基本的形态是包括薄膜层12和纤维聚烯烃无纺布舒适支持层14，这两者是互相热粘结在一起的。尽管这是本发明的最基本的形态，但若有需要，即可在复合体10内加入额外的材料层以构成多层复合体。例如，可在薄膜层12对着第一层纤维聚烯烃无纺布14的薄膜一面粘结上第二层纤维聚烯烃无纺布(图中未示出)。
薄膜层12包括三种基本成分，第一种以线型为主体的聚烯烃聚合物，如线型低密度聚乙烯，第二种是填充剂，第三种是粘结剂或增粘剂。这三种成分一起搅和加热，然后挤压成薄膜，所用的压制方法可以多种多样，包括浇注和吹制。这对具备正常薄膜技术技能的人员来说都是熟知的。在薄膜中也可加入其它的添加剂和配料，条件是所加之物要在不干扰薄膜的透气能力，不影响与纤维聚烯烃无纺布舒适层14进行热粘结。一般来说，以其干重为基础按薄膜总重计，薄膜层中将包括：约10-68％以线型为主体的热塑性塑料聚合物，约2-20％的粘结剂和约30-80％的填充剂。在更具体的实施方案中，除上述外还可包括0-68％的其它聚烯烃，如聚丙烯。
线型低密度聚乙烯(LLDPE)，当它混合有适当数量的粘结剂时，能做成很好的薄膜基础层。但是，相信本发明也能使用任何以线型为主体的聚烯烃聚合物。这里所用的“线型低密度聚乙烯”术语意为包括乙烯聚合物和更高的α-烯烃共聚用单体，如C3-C12及其结合。“以线型为主体”意为主要的聚合物链是线型的，每1000个乙烯单元带有的长链分枝小于约5个。长链分枝可能包括大于C12的碳链。对因掺杂有共聚用单体而无弹性、有短链分枝C3-C12的以线型为主体的聚烯烃聚合物来说，典型地是被在1000个聚乙烯单元中将短链限制为20个以下，有弹性的聚合物在20个或以上。以线型为主体的聚烯烃聚合物的例子包括但不限于：线型聚烯烃如乙烯、丙烯、1-丁烯、4-甲基-戊烯、1-己烷、1-辛烯和更高级的烯烃，以及上述化合物的共聚物。此外，乙烯和其它烯烃包括戊烯、己烷、庚烯、辛烯、癸烯等的共聚物，也是以线型为主体的热塑性塑料聚合物的例子。
本发明的一个主要目的是提供一种热粘结方法，能把用这样一些以线型为主体的聚烯烃聚合物制成的可透气薄膜，粘结到纤维聚烯烃无纺布上去，而不会破坏各层的完整性，特别是薄膜层的完整性。依靠在薄膜聚合物混合物中加入规定数量范围的粘结剂，就可使薄膜和无纺布在较低的温度和/或压力下、以较低百分数的总粘结面积粘结在一起。此外，不相容的薄膜和无纺布，如LLDPE和聚丙烯无纺布现已能有效地层压在一起。做成的层合物仍然非常柔软而且通常没有因想得到良好的层合而过分粘结所引起的不慎穿孔现象。
对能使之相容的LLDPE薄膜和聚丙烯无纺布来说，理想的是要能在等于或低于LLDPE薄膜的熔点温度下，用15％或其左右的总粘结面积把这两层材料热粘结起来，并使粘结好的层合物有足够的强度，需用至少5克的负荷才能使两层分拆开，所用的粘结强度测试法将在后面说明。依靠在薄膜聚合物混合物中加入粘结剂，就可做到这一点。“粘结剂”在这里是指一种添加剂当被加入到薄膜聚合物混合物中以后，就可使薄膜在比薄膜聚合物混合物中首要的以线型为主体的热塑性塑料聚合物组分的熔点至少低5°F的温度下与无纺布粘结-在这里，“首要的”聚合物就是线型低密度聚乙烯。此外，层合物的粘结强度或剥离强度应至少为5克。
粘结剂也可称为增粘树脂，在Kieffer等的美国专利No.4,789,699中进行了讨论，在此引入它的全部内容作为参考。本发明使用粘结剂的目的是使得薄膜和无纺布粘结能在  较低温度下进行。粘结剂的例子包括氢化烃树脂，如REGALREZ系列增粘剂和ARKON P系列增粘剂。REGALREZ增粘剂可从Hercules,Incorporated of Wilmington，Delaware获得。REGALREZ增粘剂是高度稳定、浅色、低分子量的非极性树脂。级号3102是指它的软化点为102R & B℃，它在21℃时的比重为1.04，在149℃时的熔融粘度为100poise，玻璃转化温度Tg为51℃。REGALREZ1094增粘剂是指它的软化点94℃，它在21℃时的比重为0.99，它在126℃时的熔融粘度为100poise，它的玻璃转化温度Tg为33℃。级号1126是指它的软化温度为126℃，它在21℃时的比重为0.97，它在159℃时的熔融粘度为100poise，玻璃转化温度Tg为65℃。
ARKON P系列树脂是Arakawa Chemical(U.S.A.)Incorporated ofChicago，Illinois用石油烃树脂制造的合成增粘树脂。例如级号P-70，其软化点为70℃，而P-100的软化点则为100℃，P-125的软化点为125℃。
ZONATEC501 lite树脂是另一类增粘剂，它是一种萜烯烃，软化点为105℃，是由Arizona Chemical Company of Panama City，Florida制造的。EASTMAN1023 PL树脂是一种无定形的聚丙烯增粘剂，其软化点为150-155℃，可从Eastman Chemical Company Longview，Texas获得。
粘结剂的其他例子通常包括但不限于：聚酰胺类；乙烯共聚物如乙烯乙酸乙烯酯(EVA)、乙烯丙烯酸乙酯(EEA)、乙烯丙烯酸(EAA)、乙烯丙烯酸丁酯(EMA)和乙烯正丙烯酸丁酯(ENBA)；木松香及其衍生物；烃树脂；多萜烯烃树脂；无规立构的聚丙烯以及无定形的聚丙烯。还包括无定形为主体的乙烯丙烯共聚物，通常称之为乙烯-丙烯橡胶(EPR)，和一大类称为韧化聚丙烯(TPP)的材料，以及烯烃热塑性聚合物，其中EPR是通过反应器内多级聚合作用而机械地分散或分子态分散在聚丙烯或聚丙烯/聚乙烯混合物中的。
必须说明，上述粘结剂或助粘剂只是作为例证而不意味着限制本发明的范围。任何粘结剂，只要它可以与其他薄膜和/或纤维聚合物掺合；只要它有能力使薄膜层与无纺层的粘结温度比薄膜或纤维混合物中首要的以线型为主体的热塑性聚合物组分的熔点至少低5℃；以及只要它能使两层之间的粘结至少需要5克的负荷才能把粘结的两层材料分拆开，就可认为是符合本发明的目的的粘结剂。通常粘结剂的含量约为薄膜总重的2-20％。尽管可用超出该重量百分数范围的粘结剂，但在较高的百分数下，薄膜的透气能力会受到损害，对人身护理吸收物品的结构来说，这样是不合适的。
在薄膜层中，除包含以线型为主体的聚烯烃聚合物和粘结剂外，还包含填充剂。这里所说的“填充剂”，是指能加到薄膜聚合物挤压混合物中去而不会在化学上干扰或对被挤压的薄膜产生负面影响，并能在整个薄膜上均匀分布的颗粒状或其它形状的材料。通常填充剂都是颗粒状的，并常常多少是圆形的。平均颗粒直径的范围为约0.1至7微米。不管是有机的还是无机的填充剂，只要它不干扰薄膜的制造过程，不干扰成品薄膜的透气能力和粘到纤维聚烯烃无纺布或舒适层上去的能力，就认为是属于本发明的范围之内的。填充剂的例子包括：碳酸钙(CaCO3)、多种粘土、氧化硅(SiO2)、氧化铝、硫酸钡、碳酸钠、滑石、硫酸镁、二氧化钛、沸石、硫酸铝、纤维素型粉末、硅藻土、硫酸镁、碳酸镁、碳酸钡、高岭土、云母、碳、氧化钙、氧化镁、氢氧化铝、纸浆粉、木粉、纤维素衍生物、几丁质以及几丁质衍生物。
前面已经说过，薄膜可用熟悉薄膜生产人员所知道的任何一种传统方法来制造。先把以线型为主体的聚烯烃聚合物、粘结剂和填充剂按上文给出的适当比例范围掺和好，然后加热并挤压成薄膜。为了提供均匀的透气能力，填充剂必须在整个聚合物混合物内均匀分布，从而也在整个薄膜内均匀分布。透气能力可用薄膜的水蒸气传输率来反映。从本发明的目的来看，如薄膜用后面实施例中的测试方法来计算，能具有至少100g/m2/24h的水蒸气传输率，这薄膜就是“透气的”。通常，制成的薄膜其单位面积重量约小于每平方米100g，在拉伸和变薄后其单位面积重量将会小于约每平方米35g，而更理想的是小于约每平方米18g。
下面的实施例中使用的薄膜是吹制薄膜，但是，其它类型的薄膜，只要它的制造技术与加填充剂的薄膜相适应，也被认为是在本发明的范围之内。通常初步形成的薄膜都太厚，噪声太大，当摇振时会发出“卡嗒”声，这时的薄膜如用水蒸气传输率衡量还没有具备足够程度的透气能力。因此，要把薄膜的温度加热到低于以线型为主体的热塑性聚合物熔点至少5℃，然后拉伸到原来长度的至少2.5倍以使之变薄并产生气孔。更理想的是，拉伸时薄膜加热到的温度还要低于粘结剂的软化点。对于某些粘结剂，其软化点有一个范围。因此，“加热到低于软化点”将可能是指低于给定范围中最高温度的温度。
在制薄过程中另一个情况是薄膜的不透明度有所改变。薄膜刚制成时是相对透明的，但拉伸后却变得不透明了。此外，当薄膜在拉伸过程中变为定向排列时，它也变得更软了，而且也没有拉伸前那么利害的“卡嗒声”了。考虑所有这些因素，并考虑需要有至少每平方米每24小时100克的水蒸气传输率，薄膜应制薄到的程度是，对用于人身护理吸收物品来说，它的单位面积重量应小于约每平方米35g，而更理想的是应小于约每平方米18g。
纤维无纺布舒适层14是用聚烯烃纤维如聚丙烯制成的。在实施例中，无纺布是聚丙烯捻合布，但也可用其它聚烯烃纤维。纤维混合物或掺合物也可能包括不同的聚烯烃纤维和聚烯烃与非聚烯烃纤维的混合物，例如聚乙烯皮/聚丙烯芯双组份纤维以及聚酯纤维。天然纤维也可包括在纤维无纺布内。具体的纤维类型包括单组份纤维和多组份纤维，例如并排、皮/芯和海/岛双组份纤维。纤维可以是直的或弯皱的、中空的或实心的。通常这些纤维的横截面是圆形的或非圆形的，包括二裂片的、三裂片的和“X”型截面的。纤维长度可以象短纤维那样是短的，也可以象纺捻纤维和熔喷纤维那样是长的。纤维的粗细取决于要求的性能。细纤维可生产出较软的无纺布，而较粗的纤维可以提供更大的强度和弹力。替代的办法是，可用多种纤维直径的混合物。对用于人身护理吸收物品来说，纤维直径具有代表性的是在1到5登尼尔之间。就本发明的目的而言，“以聚烯烃为基本材料的纤维无纺布”和“纤维聚烯烃无纺布”总起来称为纤维无纺布，其中至少要有约50％的纤维表面积是由聚烯烃构成的。
对本发明来说，可采用多种制造无纺布的方法。制造方法的例子包括但不限于：空气和湿法铺放、短纤维梳理和粘结、溶液纺丝、熔融吹制以及捻合等方法。所有这些方法均系本领域正常技术人员所熟知。对本发明来说，捻合的聚丙烯无纺布的作用是特别好的。捻合无纺布可按照Appel的普通转让美国专利No4,340,563中所讲述的来制造，在此全部引入该专利作为参考。捻合材料的制作方法是，将熔融的热塑性塑料材料通过喷丝帽上的多根毛细管挤压成细丝，然后再把挤压出的细丝的直径利用众所周知的离析拉丝等捻合机制来变小。
制成的纤维无纺布舒适层14可进行预粘结以增加其强度和整体性。在实施例中使用的聚丙烯捻合无纺布是用一种点粘模式预粘结过的，其表面粘结面积约为15％，粘结密度为约每平方英寸100到300个粘结点。大于或小于这一范围的粘结密度也可使用，这是因为比密度是取决于各粘结点的大小的。
制作本发明的透气的、布样薄膜/无纺布复合体10时，把薄膜层12和纤维聚烯烃无纺布14互相接触，然后用图2中所示的粘结工具把它们热粘结在一起。一般薄膜都是已挤压、拉伸和制薄过并随后卷到辊子20上，然后再粘合到复合体上。替代的办法是，薄膜可在未经拉伸的状态下卷到辊子上，然后在送去粘结的过程中加以拉伸和制薄。还有进一步的替代办法，就是薄膜可在流水线上制成并拉伸。
纤维无纺布也可预先制成并从供料辊子22上退卷开而进入粘结过程。作为替代办法，它也可以在流水线上制造。如果薄膜12和无纺布14以相同的速度被送入粘结机16，就会制成相对是二维的复合体。替代的办法是，可将复合体设法回缩借此生产出波浪形的、较厚的、更加三维的结构。引起回缩的一个方法是在粘结过程中用加速和/或减速两层中的一层的办法使两层中的一层处于拉紧状态，而使之拉伸或膨胀。在完成粘结后就取消拉伸或制动力，这时复合体就回缩并因此形成波浪形。另一种方法是利用薄膜层内部定向排列的线型聚烯烃分子的受力状态。当往薄膜层12加热时，其结果常常是薄膜要回缩。因此，如果收卷辊子18以低于复合体在粘结机16处的速度收卷复合体10，薄膜就会放松，从而就会生成波浪形。
两层材料热粘结在一起至少可用两种方法来完成。一种是利用加热加压，例如用带图案的加热粘结辊子。两个辊子可以都刻图案，也可以一个刻图案，一个是平滑的。可以给一个或两个辊子加热，或者可用辅助的热源。如果加工条件有规定，两辊子中的一个可以加以冷却。在任何情况下，加热必须进行调节，以使薄膜中的粘结剂发粘而把两层材料粘结在一起，与此同时仍能保持比薄膜中首要的以线型为主体的聚烯烃聚合物的熔点至少低5℃的温度。“首要的”的意思是指在薄膜总重中占最高重量百分数的那种以线型为主体的聚烯烃聚合物，如果在薄膜聚合物混合物中有一种以上的以线型为主体的聚烯烃聚合物的话。
粘结的图案和面积可根据具体的最终用途而变化。适当的粘结图案可包括：点粘结、连续线条、装饰性图案和三者的结合。粘结面积取决于要求的层压程度。对用于人身护理吸收物品上而言，粘结后需达到至少要用5克的负荷才能把两层分拆开的强度。
粘结的第二种方法是超声粘结，这对本领域中具有正常技能的人员来说也是熟知的。同样地，用超声粘结时，砧辊可设计成带有上述任一种粘结图案的。
复合体制成后，有着多种多样的用途，决不止是只用作人身护理物品的外罩而已。人身护理物品典型的是包括体侧的内衬、一个吸收芯子和一个背面层或称外罩。本发明的材料可以用作外罩，把纤维无纺布层朝外作物品的外表面，而把薄膜层对着吸收芯子。很多时候外罩和体侧的内衬是互相连结的，以便封住吸收芯子。人体一侧的内衬也常用纤维聚烯烃无纺布来制造。因此，由于有粘结剂存在，薄膜层和体侧内衬层可以用象本发明组合材料的两层相同的方式把它们热封在一起。
在前面的讨论中，是把粘结剂加到薄膜层12中去以使它与纤维无纺布舒适支持层14相容。但是，也可以把粘结剂加到支持层14的纤维中去。
前已述及，组成无纺布层14的纤维可以是短的短纤维，也可以是更长更连续的纤维，例如纺捻无纺布和熔喷无纺布的情形。在所有情况下，都可用单种聚合物来制造纤维，就象直的聚烯烃纤维那样；也可用多组份的纤维如双组份纤维来制造。对两种类型的纤维来说，必须使粘结剂存在于纤维的外表面上，以便薄膜能成功地与无纺布层相粘结。对直纤维如聚乙烯纤维来说，可把粘结剂加入到聚乙烯预混合料中并挤压成为纤维。对双组份纤维来说，必须把粘结剂加到最终形成纤维暴露表面的聚合物之一中去。在皮/芯纤维的情况下，这就指的是皮的部分，而对并排纤维来说，就可把粘结剂或是加到一种聚合物中或是两种聚合物中都加，因为它们两者都可能作为纤维的外表面而暴露出来。
一般说来，粘结剂的含量，以用来制作纤维部分的混合物或掺合物中聚合物总重量为基础，应占掺粘结剂的聚烯烃纤维聚合物的约2-20％。因此，在直的聚乙烯纤维中，聚合物掺合物内将含有2-20％(重量)的粘结剂和约80-98％(重量)的聚乙烯，在它的纤维聚合物掺合物内不存在任何添加材料。对双组份或多组份纤维来说，百分数的基础将是那一专用部分掺合物的总重量。此外，举例说，如果纤维是并排的聚乙烯/聚丙烯纤维，则可在两种聚烯烃成分内都加入粘结剂，并各占每一成分的相同的重量百分比范围，也就是说，各占每种纤维聚合物部分总重的约2-20重量百分数。
由于在同一无纺布内可以混有不同类型和组分的纤维，因此，只要能把薄膜和无纺布充分粘结好，达到至少要用5克的负荷才能把两层材料互相分拆开或剥离开，那么就不一定要求所有的纤维在它的外表面内存在有粘结剂。如果在纤维无纺布中至少有50％的纤维照上述情况使用了粘结剂，就肯定可以这样办。最后，在选择粘结剂和粘结条件时，凡是能以低于薄膜层中聚烯烃熔点的温度进行粘结的粘结剂，就可以被选用。
为了展示本发明的热粘结性能，制备了几个样品，下文将会列述。许多样品测试过两层之间的粘结强度，还测试过薄膜的水蒸气传输率(WVTR)，在实施例4中还测试了复合体。算出WVTR和粘结强度的试验方法将在下面列述。
                    水蒸气传输率
样品材料的水蒸气传输率(WVTR)是按照ASTM标准E96-80进行计算的。从每种试验材料上切下直径3英寸的圆形样品，对照品是一块Hoechst Celanese Corporation of Sommerville，New Jersey生产的CELGUARD2500薄膜。CELGUARD2500薄膜是带微气孔的聚丙烯薄膜。每种材料准备出5个样品。测试器皿是Thwing-Albert InstrumentCompany of Philadelphia，Pennsylvannia销售的60-1号Vapometer皿。在每个Vapometer皿中倒入100毫米的水并把各块试验材料的样品和对照材料的样品扣在各个皿的开口端上。旋紧法兰盘使沿皿边密封起来，使相关的试验材料或对照材料向周围大气暴露出6.5厘米直径的圆形，暴露面积约33.17平方厘米。把测试皿放入有强制空气循环的烘箱内在100°F(32℃)下平衡1小时。烘箱是恒温烘箱，有外部空气穿过它循环，以防止内部积聚水蒸气。适用的烘箱举例说有：BlueM Electric Company of Blue Island，Illinois销售的Blue M Power-O-Matic 60烘箱。平衡完毕后，把测试皿从烘箱中取出，称重后立刻再放回烘箱。经24小时后，把测试皿取出并再次称重。按下式计算出初步的水蒸气传输率实测值：
实测WVTR＝24小时重量损失克数× 315.5g/m2/24 h
烘箱内相对湿度不进行特别控制。
在预定的100°F(32℃)和环境相对湿度的设定条件下，CELGUARD2500对照品的WVTR已经测定为每平方米每24小时5000g。因此，对照样品每次测试都参与进行，因此初步的实测值可用下式修正为设定条件下的值：WVTR＝(实测WVTR/对照WVTR)×5000g/m2/24h)(g/m2/24h)
                     粘结强度
为测试薄膜层与纤维无纺布舒适支持层之间粘结的强度，对各种材料的样品进行了剥离试验。从材料上切下2英寸×约6英寸的样品，然后在短边的一端人工拆解开二个边，以便放入Sintech/2计算机整体测试系统的夹爪内，该系统是由MTS Systems Corporation ofEden Prairie，MN生产的。夹爪的间隙设定在100mm的跨距，要保留足够的材料处于层合状态，以便夹爪可以运行65mm。样品应这样放入夹爪，以使夹爪在张开10mm以前样品就开始剥离。十字头的速度是设定在每分钟300mm，在10mm的起点与65mm终点之间记录数据。所记录的数据指示出剥离强度或把两层分拆所需负荷的克数，标准的克数指标分为最大、最小和平均值。
                            实施例
实施例1
制备并评价了三种透气的薄膜/无纺布层合物来确定加入粘结剂对薄膜的水蒸气传输率和整个复合体粘结强度的影响。首先，制备了三种具有不同的聚合物混合物的薄膜，然后把每块薄膜粘结到大约2登尼尔每平方码0.5盎司(17克/m2)的聚丙烯捻合无纺布材料上，该材料预粘结了15％的粘结面积。每种薄膜的配方中包括了以总重的百分数计为65％的English China Supercoat碳酸钙(CaCO3)，平均颗粒直径为1微米，顶切(top cut)为7微米。这种碳酸钙是从一个EECInternational的分部、ECCA Calisium Products，Inc.in Sylacauga，Alabama那里获得的。碳酸钙与15-25％(重量)的线型低密度聚乙烯相混合。该线型低密度聚乙烯是由Dowlex2517线型低密度聚乙烯与Dowlex2532线型聚乙烯以重量比1∶4混合而成，以使混合物的熔融指数为10M.I.(/在190°F下10分钟)。该Dowlex聚合物可从Dow Chemical U.S.A.，Midland，Michigan购得。配剂中余下的10-20％的重量包括Himont KSO51P以聚丙烯为基本成分的聚合物，这是Himont，USA of Wilmington，Delaware生产的。KSO51P聚合物是一种烯属的热塑性弹性体或者是TPO多级反应器产物，其中有无定形的乙烯丙烯无规共聚物分子态地分布在半晶质为主体的高聚丙烯单体/低乙烯单体的连续基体中。无定形成分起着助粘剂或粘结剂的作用，因为它在约55℃就开始软化。如下面的表I所示，样品1含有65％的碳酸钙、10％的KSO51P聚合物和25％的线型低密度聚乙烯。样品2含有65％的碳酸钙、15％的KSO51P聚合物和20％的线型低密度聚乙烯。样品3含有65％的碳酸钙、20％的KSO51P聚合物和15％的线型低密度聚乙烯。三种配剂都在熔融温度357°F(191℃)下制成薄膜，吹胀比大约为1.7，制成未拉伸厚度大约为1.25密尔(50g/m2)的薄膜。每种薄膜随后都在机械方向定向单元(MDO)上拉伸，拉伸比为3X，拉伸温度140°F(60℃)。制成的薄膜是透气的，这从下面表I中所列的水蒸气传输率数据可以得知，薄膜的基本重量大约每平方米14克。
                                 表I样品    CaCO3    LLDPE     KSO51P      WVTR       粘结强度   薄膜   MDO
    (重量％)  (重量％)  (重量％)    g/m2/24h    (g)      加工   拉伸1     65        25        10          4530          24      良好   尚可2     65        20        15          4300          27      良好   良好3     65        15        20          3710          26      良好   特优
从表I可以看出，随着粘结剂数量的增加，水蒸气传输率就减小。粘结剂数量增加时Himont KSO51P聚合物中的无定形乙烯丙烯共聚物部分的数量也增加，这些无定形共聚物是在约55℃时就开始软化。相反地，随着助粘剂或粘结剂的增加，样品就显示出粘结强度增大，因此对剥离具有更大的抗力。给定了粘结剂加入量后，对薄膜加工的难易和在机械方向拉伸的能力进行了目测。表I中示出了薄膜加工是良好的，与加入薄膜预挤压混合物中的粘结剂百分数无关，但与相反的是，随着薄膜中粘结剂数量的增加，观察到了它的拉伸能力也呈直线增大。样品1的薄膜在机械方向的拉伸能力为“尚可”，而样品3的拉伸能力为“特优”。每种薄膜都层压到17g/m2(0.5盎司/码2)的聚丙烯捻合无纺布上，走料速度为每分钟100英尺(30.5m/min)，咬合压力为每平方英寸20磅(1.41kg/cm2)，用的是不连续的粘结图案，粘结面积大约为15％。图案辊子保持在250°F(121℃)而平滑的砧辊则保持160°F(71℃)，平滑砧辊是与薄膜直接接触。
表I中的数据证明，本发明的三种样品全都具有特优的水蒸气传输率和特优的粘结强度。样品要用24至27克之间的负荷才能把两层剥离，而两层之间的粘结面积只用了15％。此外，薄膜层上没有出现穿孔，因此当把本材料用于做人身护理吸收物品的外罩时，薄膜还兼具阻挡层的性能。
实施例2
在本实施例中，用实施例1中样品1的薄膜配剂来估量拉伸温度的效果。设想KSO51P聚合物中的无定形成分的逐步软化使它变得象粘胶似的，会对聚合物混合物在树脂基体和碳酸钙颗粒表面的接合面上形成全面破裂产生干扰。为了确认这一点，把薄膜样品拉伸3X，即把1米长的样品拉伸成3米，温度在146°F(63℃)和186°F(86℃)之间变化。随着拉伸温度的提高，水蒸气传输率就降低，最可能是因为在薄膜上围绕碳酸钙颗粒所形成的气孔较少和/或较小。如表II所示，增高拉伸温度肯定地使线型低密度聚乙烯的分子具有更大的流动性，借此使拉伸更加容易。随着温度从146°F(63℃)增高到186°F(86℃)，拉伸的容易性也增加。在177°F(81℃)和186°F(86℃)时，薄膜中的分子显现出了过分定向，薄膜上出现了较多的裂口，出现了在机械方向上撕裂的倾向。因此可以看出，WVTR、加工能力和薄膜机械特性之间的平衡，可用选择适当的拉伸温度的办法来加以最优化。最佳的拉伸和最佳的透气能力只有当拉伸在低于薄膜中首要的、以线型为主体的聚烯烃聚合物熔点的温度下，以及在粘结剂软化点左右的温度下进行时才能得到。
                      表II
          拉伸温度    WVTR        MDO
          °F/℃      g/m2/24h   拉伸
          146/63      4300        尚可
          157/69      4100        良好
          167/75      3960        良好
          177/81      3730        裂口
          186/86      3515        更多裂口
实施例3
在实施例1和2中，所有样品以干重计含有：65％的碳酸钙、15-25％的线型低密度聚乙烯和10-20％的Himont KSO51P以聚丙烯为基本成分的聚合物树脂，它含有无定形的乙烯丙烯无规共聚物用作助粘剂或粘结剂。在实施例3中，系将65％重量的碳酸钙和30％重量的低密度聚乙烯相混合。如表III所示，在该基础混合物中加入了一系列的公认的助粘剂或粘结剂，其数量为5％(重量)。粘结剂包括：Regalrez1094、3102和1126粘结剂，还有Zonatac501L和Eastman1023PL粘结剂。此外，照实施例1中样品2的配剂做成了同一式样的薄膜。每块薄膜都以吹胀比为1.7来吹制，厚度大约为1.5密尔(60g/m2)。这些薄膜都在146°F(63℃)下在机械方向拉伸到它们原有长度的三倍(3X)。这一拉伸温度低于以线型为主体的聚烯烃聚合物的熔点(235°F/113℃)。随后这些薄膜样品被层压到与实施例1中同样的聚丙烯无纺布上去，粘结的条件也相同，总的粘结面积约为15％。图案辊子的温度保持在250°F(121℃)，而直接与薄膜接触的光滑砧辊的温度则调节在160°F(71℃)、175°F(79℃)、185°F(85℃)和195°F(91℃)等四种温度。对每块薄膜/无纺布复合体在每一温度下的粘结强度进行了测量。此外，还测量了每块薄膜的水蒸气传输率，目测了薄膜加工和拉伸的难易程度。测试结果列于下表III内。
                                表III粘结剂      WT   CaCO3  LLDPE   WVTR    粘结强度(克)               薄膜加工     MDO拉伸
        ％   WT％    WT％    g/m2
                             /24h 160°F 175°F 185°F 195°FKS050       15％ 65％    20％    4300   41      *      *      *         良好       尚可Regalrez1094        5％ 65％     30％    2300    3      5      6      10        特优       特优Regalrez3102        5％ 65％     30％    3840    3      3      7      5         特优       特优Regalrez1126        5％ 65％     30％    3198    3      3      5      7         良好       良好Zonatac501L        5％ 65％     30％    2990    4      4      10     9         特优       特优Eastman1023PL     5％ 65％      30％    4900    8      7      10     7         良好       良好
*不能分拆(粘结很好)
Himont KS050粘结剂使两层之间的粘结强度最高，但请注意它占薄膜的重量百分数是15，而其它粘结剂所占的重量百分数只有5。大多数粘结剂显示出粘结强度随着粘结温度升高而加大，但有几种粘结剂在185°F时达到高峰，然后在195°F时开始降低其粘结强度。所有粘结剂的加工能力都“良好”到“特优”，但使用Himont KSO50粘结剂的机械方向拉伸能力只是“尚可”。所有薄膜都显示出有良好的水蒸气传输率。
实施例4
在实施例4中进行了一次临床研究，以确定使用本发明的透气的、布样薄膜/无纺布复合体代替普通的聚乙烯薄膜(对照)作为尿布外罩时对减轻皮肤水合作用的效果。用对照外罩和实施例1中的样品2的薄膜/无纺布复合体做成了多块尿布。复合体中的薄膜的水蒸气传输率(WVTR)为4300g/m2/24h，而复合体的WVTR为4100g/m2/24h。对照尿布中单层1.2密尔厚的聚乙烯薄膜的WVTR为40-50g/m2/24h。
每块尿布都隔离着60毫升的合成尿，然后绕参试人员的前臂包紧。在预定的时间间隔中测定水分损失以确定皮肤水合作用的程度。根据试验结果，可确定使用本发明的复合体做的尿布的人，其尿布下皮肤的水合作用要比对照尿布有明显的降低，从而就宣告了在取得层间有效粘结的同时，仍能保持透气性并减轻皮肤的水合作用。
由上述实施例可以看出，本发明的材料提供了一种层间粘结良好的透气的、布样薄膜/无纺布复合体。当复合体用作人身护理吸收物品如尿布的外罩时，无纺布层起着增强透气薄膜层的作用，无纺布层可帮助克服透气薄膜的冰凉滑腻的不良特性。此外，由于在薄膜和/或纤维聚合物混合物中掺入了粘结剂，就可能使本来不相容的聚合物/材料层互相层压在一起。
本发明经过这样详述以后，已可很清楚地看出，本发明能作多种多样的变更和变化，而不会脱离下述权利要求的精神和范围。

Claims (15)

1.一种透气的薄膜/无纺布层合物，它包括：
一层由下述混合物制成的薄膜，该混合物以其干重计，以薄膜的总重为基础，包括有约10-68％的以线型为主体的聚烯烃聚合物，约30-80％的填充剂，以及约2-20％的粘结剂，该薄膜的水蒸气传输率至少为100g/m2/24h，以及
一层直接粘合到该薄膜上面构成层合物的纤维聚烯烃无纺布，该层合物的剥离强度至少为24克。
2.权利要求1的层合物，其中所说的以线型为主体的聚烯烃聚合物为线型低密度聚乙烯。
3.权利要求1的层合物，其中所说的填充剂为碳酸钙。
4.权利要求1的层合物，其中所说的薄膜是拉伸过的薄膜，其单位面积重量小于35g/m2。
5.权利要求1的层合物，其中所说的薄膜是拉伸过的薄膜，其单位面积重量小于18g/m2。
6.权利要求1的层合物，其中所说的纤维聚烯烃无纺布是聚丙烯无纺布。
7.权利要求1的层合物，其中所说的纤维聚烯烃无纺布包含有双组分的纤维，其组分之一是聚烯烃。
8.权利要求3的层合物，其中在所说的薄膜相对于所说的纤维聚烯烃无纺布的一面粘结有第二层纤维聚烯烃无纺布。
9.一种薄膜/无纺布层合物，它包括：
一层由下述混合物制成的薄膜，该混合物以其干重计，以薄膜的总重为基础，包括有约10-68％的以线型为主体的聚烯烃聚合物，约30-80％的填充剂，以及约2-20％的粘结剂，该薄膜的水蒸气传输率至少为100g/m2/24h，以及
一层纤维无纺布，该无纺布由其内的多根纤维直接粘结到该薄膜层上，所述无纺布包含一种聚烯烃聚合物和一种粘结剂，所述聚烯烃聚合物和粘结剂形成所述纤维外表面的至少一部分，并在该薄膜层和纤维无纺布之间形成至少24克的剥离强度。
10.一种人身护理吸收物品，包括：
体侧的内衬和外罩，及两层之间放入的吸收剂芯，
该外罩包括一层薄膜，该薄膜由一种混合物制成，该混合物所包括的成分，以干重计，以薄膜的总重量为基础，为：约10-68％的以线型为主体的聚烯烃聚合物，约30-80％的填充剂和约2-20％的粘结剂，该薄膜的水蒸气传输率至少为100g/m2/24h，以及
一层直接粘结到上述薄膜上构成层合物的纤维聚烯烃无纺布，该层合物的剥离强度至少为24克。
11.一种包括有透气的薄膜/无纺布层合物的服装和衣着用品，该层合物包括：
一层由一种混合物制成的薄膜，该混合物所包括的成分，以干重计，以薄膜的总重为基础，为：约10-68％的以线型为主体的聚烯烃聚合物，约30-80％的填充剂和约2-20％的粘结剂，该薄膜的水蒸气传输率至少为100g/m2/24h，以及
一层直接粘结到上述薄膜上构成层合物的纤维聚烯烃无纺布，该层合物的剥离强度至少为24克。
12.一种制造透气的薄膜/无纺布层合物的方法，它包括：
配制预挤压的混合物，该混合物所包括的成分，以干重计，以薄膜的总重为基础，为：约10-68％以线型为主体的聚烯烃聚合物，约30-80％的填充剂和约2-20％的粘结剂，
用上述预挤压混合物制造薄膜，
在低于以线型为主体的热塑性聚合物熔点的温度下拉伸该薄膜，以及
将所说的薄膜在低于薄膜中的以线型为主体的热塑性聚合物熔点的温度下，直接粘结到纤维聚烯烃无纺布上，构成剥离强度至少为24克的层合物。
13.权利要求12的方法，它包括进一步使得所述层合物回缩以使该层合物产生波浪形的表面。
14.权利要求12的方法，其中的拉伸步骤是也在同时等于或低于粘结剂的软化点的温度下进行。
15.一种制造薄膜/无纺布层合物的方法，它包括：
制造一种薄膜层，该薄膜层中包括以干重为基础计，占薄膜总重约30-80％的填充剂和约20-70％的聚烯烃聚合物，
拉伸该薄膜层，
用纤维无纺布内的多根纤维把纤维无纺布直接粘结到该薄膜层上，该纤维无纺布含有聚烯烃聚合物和粘结剂，该聚烯烃聚合物和粘结剂存在于该纤维外表面的至少一部分上，其间具有的剥离强度至少为24克。
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WO2018192006A1 (zh) 2017-04-20 2018-10-25 佛山金万达科技股份有限公司 一种透汽阻隔型功能薄膜层合物
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CA2116081A1 (en) 1995-06-18
RU2140855C1 (ru) 1999-11-10
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GB2285408B (en) 1998-01-07
FR2713983A1 (fr) 1995-06-23
GB2285408A (en) 1995-07-12
EG20760A (en) 2000-01-31
ES2131800T5 (es) 2005-09-16
CO4290498A1 (es) 1996-04-17
EP0734321B2 (en) 2005-05-25
US5695868A (en) 1997-12-09
CA2116081C (en) 2005-07-26
MY113303A (en) 2002-01-31
RO116364B1 (ro) 2001-01-30
BR9408329A (pt) 1997-08-19
AU687967B2 (en) 1998-03-05
DE69417258T2 (de) 1999-07-08
EP0734321A1 (en) 1996-10-02
JPH09506656A (ja) 1997-06-30
GB9425471D0 (en) 1995-02-15
ES2131800T3 (es) 1999-08-01
CN1142798A (zh) 1997-02-12
ZA9410026B (en) 1995-08-22
US5855999A (en) 1999-01-05
CR5094A (es) 1995-07-17
MY121155A (en) 2005-12-30
UA26938C2 (uk) 1999-12-29
FR2713983B1 (fr) 1997-07-18
PL315183A1 (en) 1996-10-14
DE69417258T3 (de) 2005-10-06
UY23876A1 (es) 1995-06-07
EP0734321B1 (en) 1999-03-17
JP3373211B2 (ja) 2003-02-04
WO1995016562A1 (en) 1995-06-22
JP2003175575A (ja) 2003-06-24
AU1335395A (en) 1995-07-03
DE9422432U1 (de) 2002-01-24
FR2717737A1 (fr) 1995-09-29
FR2717737B1 (zh) 1997-02-21
DE69417258D1 (de) 1999-04-22
PE13096A1 (es) 1996-04-27

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