CN1665879A - 辐射可固化低应力弛豫弹性体材料 - Google Patents
辐射可固化低应力弛豫弹性体材料 Download PDFInfo
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- CN1665879A CN1665879A CN038155826A CN03815582A CN1665879A CN 1665879 A CN1665879 A CN 1665879A CN 038155826 A CN038155826 A CN 038155826A CN 03815582 A CN03815582 A CN 03815582A CN 1665879 A CN1665879 A CN 1665879A
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Images
Classifications
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- A—HUMAN NECESSITIES
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Abstract
一种辐射固化的低应力弛豫弹性材料，其具有改进的弹性和机械性质。该弹性材料可被单独或与表层一起使用以形成弹性薄膜、层压材料和包含它们的产品。
Description
发明领域
本发明涉及低应力弛豫弹性体组合物和由该组合物制造的产品。一方面，本发明涉及弹性体组合物的选择***联，使用官能化大分子交联剂以提供改善的机械和弹性性能。另一方面，本发明涉及将熔融可加工和辐射可固化的弹性体组合物制成产品的方法，所述产品如基本平面的薄膜；宏观扩展的三维网；有孔网；薄膜或网的层压材料；以及吸收制品，该制品具有由薄膜、网或层压材料制成的组分。
发明背景
弹性体嵌段共聚物具有乙烯芳烃聚合物嵌段和烯属和/或双烯聚合物嵌段，典型地显示具有两相形态，相似的嵌段聚在一起形成一相，与由其它的嵌段形成的第二相区分开。所述的嵌段共聚物形成三维的、缠绕的(即物理交联)网状结构。聚合链能来回移动并从这些物理交联中解脱出来，导致弹性和机械性能的丧失。低分子量的交联剂已经被用于在聚合链之间形成化学交联以改善性能。然而，已知对于两相共聚物中的两个相来说，小分子在热力学上相容性更好，因此选择性也就越差。因此，低分子量交联剂与共聚物的两相都均匀混合，并在两相中没有区别地交联。所得的材料可能变得更加难以加工且在使用时更易碎。选择性地交联一相的方法也是已知的。包含一般和选择***联剂的弹性体组合物公开于美国专利4,133,731(Hansen等人)、4,556,464(St.Claire)、5,073,611(Rehmer等人)、5,407,971(Everaerts等人)、6,294,698(Nohr等人)、6,369,123(Stark等人)和6,384,139(Ho等人)。
继续需要可固化的弹性体组合物，该组合物能够选择性地交联以提供改善的弹性和机械性能，并能够仍然保持热塑性的加工性能。
健康护理或个人卫生制品的弹性化部分可以对人体适形，并在产品下面产生相对闭合的环境。由于在这些产品中使用的材料具有较大的弹性，对人体提供了较好的贴合性，因此减少了流向皮肤的空气流和来自闭合面的蒸汽流。透气性(尤其是蒸汽渗透性)成为皮肤健康的重要因素。使弹性体材料更多孔、更透气的几种方法，如模冲、切口、热穿孔是本领域已知的。生产更好的多孔薄膜或网如宏观扩展的三维网的改善的方法公开于美国专利3,929,135(Thompson)、4,342,314(Radel等人)、5,733,628(Pelkie)、6,303,208(Pelkie)和PCT Publication WO 98/37266(Curro等人)。
由于弹性体材料固有的发粘和拉伸特性，在加工和处理弹性体材料时存在相当大的困难。弹性体材料有粘在加工设备上的倾向，难以从辊上除去或裁剪成恰当的尺寸以组成成品。此外，期望弹性体材料可以连接在非弹性体基质上，如非弹性无纺材料，这意味着赋予所得层压材料弹性。赋予弹性的不同方法公开于美国专利4,153,664(Sabee)；5,143,679(Weber等人)、5,156,793(Buell等人)、5,167,897(Weber等人)、5,518,801(Chappell等人)、5,628,097(Benson等人)、5,650,214(Anderson等人)。然而，据知，使用上述方法或它们的组合，各种不同的弹性体材料会有缺陷，如针孔、鱼眼或类似物。这些在弹性体材料中的缺陷在使用时可充当应力集中器，加剧材料的撕裂引发、撕裂扩大和灾难性故障。
因此，继续需要弹性体材料提供弹性(包括低应力弛豫)和透气性及其可加工性。
期望有熔融可加工的弹性体组合物，该组合物可以优先地在所述组合物的选择相里交联。
进一步期望有大分子交联剂能够优先地在所述组合物的选择相里交联，并且有助于改善所得弹性体组合物的机械和弹性特性。
还期望有弹性体组合物，该组合物适于形成弹性体产品，如开孔的或宏观扩展的三维弹性体网，或吸收产品的组分(包括健康护理产品或个人卫生制品)或可拉伸的衣服。吸收产品可以包括胶带/扣紧的尿布、套穿尿布、训练裤、失禁衣服、卫生巾、短裤护垫、擦拭物、伤口敷料、绷带、消毒盖布和包裹物。
发明概述
本发明涉及辐射可固化、低应力弛豫弹性体组合物，该组合物具有改善的机械和弹性特性。该组合物可包含：
a)约20％至约80％重量的热塑性弹性体(TPE)，该弹性体是嵌段共聚物，其具有至少一个包含乙烯芳烃的刚性嵌段和至少一个包含双烯的柔性嵌段；
b)约5％至约60％重量的加工油；和
c)约1％至约60％重量的大分子光引发剂；
其中，在固化后，所述材料在室温下伸长200％后应力弛豫低于约20％，在37.7℃(100°F)下伸长50％约10小时后应力弛豫低于约45％。
本发明进一步涉及由弹性体组合物制备的弹性体薄膜、网和层压材料，以及包含这些薄膜、网或层压材料的制品。
所有引用文献的相关部分均引入本文以供参考，任何文献的引用不可解释为是对其作为本发明的现有技术的认可。
附图简述
虽然本说明书以由特别指出和清楚地要求保护本发明主旨的权利要求书作为结论，但据信通过以下结合附图的描述可更好地理解本发明，
图中相同的参考数字标示相同的元件，其中：
图1是本发明的弹性体纤网实施方案的局部分段的放大透视图，所述弹性体纤网具有两层聚合物薄膜，其中至少一层是弹性体的；
图2是通常如图1所示类型的纤网进一步放大的局部视图，但此视图仅仅为更详细图示说明本发明可供选择的弹性体纤网的纤网结构；
图3为一次性衣服的局部分段透视图，其中至少一部分包含本发明的弹性体材料；
图4为实施例1交联前和交联后的所承受的负载力弛豫图；以及
图5为实施例2交联前和交联后的所承受的负载力驰豫图。
发明详述
本文所用术语“包含”是指各种组分、成分或步骤可联合用于实施本发明。相应地，术语“包含”包括更具限制性的术语“由...组成”和“基本上由...组成”。
本文所用术语“弹性的”或“弹性体的”是指在外力下能够拉伸或变形的任何材料，并且在外力解除后能够基本恢复其原来的尺寸或形状，仅有很小的永久变形(典型地不超过约20％)。术语“弹性体”是指任何显示具有本文上述的弹性特性的材料。
本文所用术语“热塑性”是指任何能够熔融和再凝固，而物理属性(假定氧化降解为最小值)只有很小或没有变化的材料。
本文所用术语“可拉伸的层压材料”是指多层薄膜、三维宏观扩展网或由所述薄膜制备的有孔网，其中薄膜或网至少一层包含本发明所述的弹性体材料。本文所用术语“复合层压材料”是指前述薄膜/网与纤维无纺材料的组合以及单层薄膜与纤维无纺材料的组合，所述单层薄膜包含本发明所述的弹性体材料。
除非另外指明，本发明中所用的所有百分数、比率和比例均按重量计。
本发明涉及辐射可固化低应力弛豫弹性体材料，所述弹性体材料显示具有改善的弹性和机械特性，如抗拉模量、极限伸长和应力弛豫特性。所述弹性体材料可以用于具有表层的单层薄膜或多层薄膜。所述弹性体薄膜可以形成有孔网或宏观扩展的三维弹性体网。此外，所述弹性体薄膜或网可以连接到无纺纤网，并递增拉伸(即活性的)以形成弹性体层压材料。所述弹性体薄膜、网或层压材料适用于弹性化的或一次性吸收制品的贴体部分，如侧片、腰带、护腕或卫生保健产品，如伤口敷料、绷带和包裹物。本发明所述多孔可延展聚合网或层压材料可以用于吸收制品中其它需要可拉伸或透气材料的部分，如顶片或底片。
本发明的弹性体组合物包含弹性体嵌段共聚物(该共聚物具有至少一个刚性嵌段和至少一个柔性嵌段)、大分子光引发剂、加工油，而且可任选地，热塑性聚合物和/或交联剂。
可用于本文的合适的嵌段共聚物可包括至少一个“刚性”聚合物嵌段和至少一个“柔性”聚合物嵌段。典型地，所述刚性嵌段(或A嵌段)可以是无定形的，而且二级转变温度或玻璃化转变温度在室温以上，或者是结晶的，具有结晶片断(该片断可以在主链中、在侧链中、或者在侧基中)，而且一级转变温度或晶体融化温度在室温以上。这些相变的定义可见于“Principles of Polymer Chemistry”，Flory著，Cornell University Press(1953)。
典型地，所述柔性嵌段(或B嵌段)具有室温以下的玻璃化转变温度。柔性嵌段在室温下能相对运动。刚性嵌段和柔性嵌段趋于彼此分开形成单独的相。通常，这些共聚物被称为热塑性弹性体(TPE)，其中所述刚性嵌段充分显示热塑性特征，所述柔性嵌段充分显示弹性体特征。
所述刚性嵌段可以包含聚乙烯芳烃，聚乙烯芳烃衍生自如下单体，如苯乙烯、α-甲基苯乙烯、对甲基苯乙烯、其它烷基苯乙烯衍生物，或它们的混合物。刚性嵌段还可以是任意共聚物，该共聚物衍生自乙烯芳烃单体和短的C2-C6烯属单体，如乙烯、丙稀，丁烯，C4-C6双烯单体，如异戊二烯、丁二烯，或双烯/烯烃单体的混合物。在优选的实施方案中，按所述刚性嵌段的重量计，TPE的刚性嵌段包含约1％至20％的不饱和或部分饱和的双烯。
所述刚性嵌段期望具有的数均分子量为约1,000至约200,000，优选约2,000至约100,000，更优选约5,000至约60,000。所述刚性嵌段可占嵌段共聚物总重量的约10％至约80％，优选约20％至约50％，更优选约25％至35％。
柔性嵌段可以是双烯聚合物，该聚合物衍生自不饱和或部分饱和的约4至约6个碳的双烯单体。合适的双烯单体可包括丁二烯、异戊二烯等。所述柔性嵌段还可以是烯属聚合物，该聚合物衍生自直链或支链的约2至约6个碳的烯烃单体。合适的烯烃单体可包括乙烯、丙稀、丁烯等。所述柔性嵌段还可包括上述单体的组合物，如乙烯/丙稀聚合物、乙烯/丁烯聚合物等。
所述柔性嵌段的数均分子量可为约1,000至约300,000，优选约10,000至约200,000，且更优选约20,000至约100,000。所述柔性嵌段可占共聚物总重量的约20％至约90％，优选约50％至约80％，更优选约65％至约75％。
可用于本文的合适嵌段共聚物可包含至少一个柔性(即基本弹性体的)嵌段部分B和至少一个刚性(即基本热塑性的)嵌段部分A。所述嵌段共聚物可具有多个嵌段，如A-B-A三嵌段共聚物，A-B-A-B四嵌段共聚物，或A-B-A-B-A五嵌段共聚物等。
可用于本发明的嵌段共聚物还可具有一个以上的A嵌段和/或一个以上的B嵌段，其中每一个A嵌段可衍生自相同或不同的乙烯芳烃单体，每个B嵌段可衍生自相同或不同的双烯或烯属单体。例如，三嵌段共聚物可具有一个弹性体中间嵌段B和两个热塑性末端嵌段A和A’，其中A和A’可衍生自不同的乙烯芳烃单体。
在一些实施方案中，所述烯属嵌段至少占所述嵌段共聚物重量的约50％。如果需要，双烯单体的不饱和部分可选择地氢化，以降低对氧化降解的敏感度并可能导致改善弹性和机械特性。例如，聚异戊二烯嵌段可以选择性地还原形成乙烯-丙稀嵌段。在其它实施方案中，所述乙烯芳烃嵌段至少占所述嵌段共聚物重量的约10％。较高的乙烯芳烃含量提供低的应力弛豫和高的弹性/拉伸特性。
示例性嵌段共聚物可包括苯乙烯-双烯-苯乙烯或苯乙烯-烯烃-苯乙烯三嵌段共聚物，如苯乙烯-丁二烯-苯乙烯(S-B-S)、苯乙烯-乙烯/丁烯-苯乙烯(S-EB-S)、苯乙烯-乙烯/丙稀-苯乙烯(S-EP-S)、苯乙烯-异戊二烯-苯乙烯(S-I-S)、氢化聚苯乙烯-异戊二烯/丁二烯-苯乙烯(S-IB-S)以及他们的混合物。市售嵌段共聚物包括购自Shell Chemical Company(Houston，TX)的KRATON，Kuraray America，Inc.(New York，NY)的SEPTON，和购自Dexco Chemical Company(Houston，TX)的VECTOR。
所述嵌段共聚物还可以是辐射状的，有三个或更多个悬臂(arm)，每个悬臂都是具有B-A，B-A-B-A或类似结构的共聚物，B嵌段处在或靠近辐射状聚合物的中心部分。
所述嵌段共聚物可用于弹性体组合物中，以有效含量使用以获得期望的特性，如伸展性、弹性和应力弛豫以及其它机械性能。嵌段共聚物通常存在于弹性体组合物中，在组合物中含量典型地为约20％至约80％重量，优选约25％至约75％重量，更优选约30％至约70％重量。
在本发明中使用的所述嵌段共聚物可以是端基改性的。所谓端基改性，是指聚合物在嵌段共聚物的一个或两个末端包含官能团，如丙烯酸酯、烷基丙烯酸酯、马来酸酯、反丁烯二酸酯、衣康酸酯、柠康酸酯、乙烯醚、乙烯酯、肉桂酸酯、γ-酮丙烯酸酯、马来酰亚胺、羟基、伯胺、仲胺和叔胺、羧基、环氧基和硫醇。一个端基嵌段共聚物合成的实施例描述于PCT专利出版物WO99/64931，转让给Dow Chemical并公布于1999年12月16日。
优选的端基改性聚合物一般形式为：
A-B-A-R
A-B-R
R-A-B-A-R
R’-A-B-A-R
其中A为苯乙烯聚合物嵌段，B为乙烯/丙稀、乙烯/丁烯、丁二烯和/或异戊二烯聚合物嵌段，R和R’为如上所述的端基。
所述光引发剂可以是包含紫外(UV)响应取代基的官能化的大分子，当暴露在紫外辐射中时倾向于产生自由基。所得自由基可以从TPE中的不饱和部分吸收质子以形成自由基，这可导致在TPE之间发生化学交联。这些化学交联增强了物理缠结，使TPE基质的三维网状结构增强，并改善了弹性和机械性能。另外，以自由基形式的光引发剂还可彼此发生反应，形成与TPE网互相贯穿的网络，这进一步增强了所得组合物的弹性和机械特性。
此外，由于它们的大分子结构，大分子光引发剂(在下文中为“大分子光引发剂”)可显示具有聚合材料的弹性和机械性能。因而，当大分子光引发剂与热塑性弹性体混合时，它们可增强混合组合物的弹性和机械性能，这样不需要额外的热塑性材料就可以达到期望的性能。所述大分子光引发剂可存在于所述组合物中，在组合物中的含量在约1％至约60％重量、优选约5％至约50％重量，更优选约10％至约40％重量的范围内。
在TPE所期望的相里目标交联，相容性是需要考虑的因素。尽管低分子量分子通常能够在TPE的两相中都混合良好，但是高分子量聚合材料可以优先地移动到包含相容性更好的聚合嵌段的一相中。分子量和化学结构是影响聚合物之间相容性的因素。本发明合适的大分子光引发剂数均分子量为约5,000至约300,000，优选约10,000至约200,000，且更优选约25,000至约150,000。结构上，包含芳烃或乙烯芳烃单体单元的大分子光引发剂与TPE的刚性相更相容，包含脂肪族或烯属单体单元的大分子光引发剂与TPE的柔性相更相容。
此外，大分子光引发剂包含取代的单体，该单体含有UV响应取代基。为了产生足够数量的交联，以改善弹性和机械性能，至少约5％，优选至少约7％，且更优选至少约10％的大分子光引发剂单体单元为取代的单体。所述取代单体具有一般结构：
其中R1可为乙烯基、乙烯芳烃、丙烯酸酯或甲基丙烯酸酯单体，R2可为烷基、芳基、烷基芳基、烷氧基、取代烷基、卤素、烷基磺酸盐、烷基铵磺酸盐、过酸酯、肉桂酸酯和叔胺。大分子光引发剂在聚合物骨架中可包括取代的单体，所述单体具有，但不限于，下列示例性结构：
在一个实施方案中，大分子光引发剂可以是取代的聚苯乙烯，在苯乙烯的芳族或脂族碳上包含苯乙酮或二苯酮官能团，并且至少约5％的单体是取代的。
在另一个实施方案中，大分子光引发剂可以通过把UV活性基团接枝到聚合物主链中制备，该聚合物主链可以购自National Starch&Chemicals，Bridgewater，NJ，这里所述的聚合物主链可以是具有剩余不饱和重复单元的任何聚合物。有用的聚合物包括但不限于苯乙烯-丁二烯-苯乙烯(S-B-S)、苯乙烯-异戊二烯-苯乙烯(S-I-S)、聚苯乙烯-异戊二烯/丁二烯-苯乙烯(S-IB-S)、苯乙烯-丁二烯橡胶(SBR)、乙烯-丙稀-二环戊二烯(EPDM)、丙烯腈-丁二烯-苯乙烯(ABS)、聚丁二烯(PBD)、聚异戊二烯(PI)以及他们的混合物。
可任选地，交联剂还可用来加速交联反应。所述交联剂可包含多个自由基接受官能度(典型地具有可吸收质子)，与来自所述光引发剂和/或其它交联剂的自由基反应。因此，交联剂的多个官能度可与所述TPE发生多重化学交联，以改善可固化弹性体组合物的特性。所述交联剂的分子量可以低，典型地小于约700。示例的交联剂可以是硫醇，如三羟甲基丙烷三(3-巯基丙酸酯)；二或三丙烯酸酯，如三羟甲基丙烷三丙烯酸酯；或者二或三(甲基丙烯酸酯)，如三羟甲基丙烷三甲基丙烯酸脂，都可购自Sigma-AldrichChemicals。在优选的实施方案中，低分子量交联剂存在的量按组合物的重量计为约0.5％至约10％重量，更优选约1％至约8％重量，且最优选为约1.5％至约5％重量。
同时包含所述UV响应取代基和自由基接受官能度的大分子也可适用于本文。这些大分子可以作为光引发剂，也可以作为交联剂。例如，大分子光引发剂可在主链或取代基中包含不饱和C＝C，取代基包含可引起额外化学交联的吸收质子。
另外，可加入加工油或增塑油，如烃油，以使粘度降低并增强弹性体组合物的加工性。然而，加工油趋于对所述组合物的弹性、应力弛豫和伸展特性有负面影响。本发明弹性体组合物中所述加工油的典型浓度范围为所述弹性体组合物重量的5％至约60％，优选约10％至约50％，更优选约15％至约45％。
典型地，加工油与所述组合物相容，并在加工温度下基本不降解。适用于本文的烃油为脂族(包括直链、支链或环状)或芳族。所述油可以是矿物油以及其它石油衍生的油和蜡，如石蜡油、环烷油、石油、微晶蜡、石蜡或异链烷烃蜡。合成蜡(例如Fischer-Tropsch蜡)，天然蜡(例如鲸蜡、巴西棕榈蜡、地蜡、蜂蜡、小烛树蜡、石蜡、纯地蜡、西班牙草蜡、小冠椰子蜡、rezowax)，和其它已知的矿物蜡，也适用于本发明。烯属低聚物和低分子量聚合物也可用于本发明。烯属低聚物可以是重均分子量在约350至约8000之间的聚丙烯、聚丁烯、氢化聚异戊二烯、氢化聚丁二烯或类似物。
在一个典型的实施方案中，加工油为白色矿物油，商品名称BRITOL，购自Witco Company，Greenwich，CT。在另外一个典型的实施方案中，加工油为另外的矿物油，商品名称DRAKEOL，购自Pennzoil CompanyPenrenco Division，Karns City，PA。
可选择地，各种不同的热塑性聚合物或热塑性聚合物组合物可用于本发明的弹性体组合物中。在一些实施方案中，热塑性聚合物可优先与嵌段共聚物的刚性嵌段相连，并合并到刚性相的缠绕的三维网络结构中。不受理论的约束，据信这种缠绕的网络结构能改善伸展性、弹性和应力弛豫特性。热塑性聚合物，如由单体衍生的聚苯醚、乙烯芳烃聚合物，所述单体包括苯乙烯、α-甲基苯乙烯、对甲基苯乙烯、其它烷基苯乙烯衍生物、乙烯基甲苯，以及它们的混合物，可用于本发明。因为它们通常被认为与嵌段共聚物的苯乙烯刚性嵌段化学相容。相容的组分可以更容易地混合并且合并到缠绕的三维网络结构中，而且它们从网络结构中物理分离(即解脱)的趋势较低。
使用具有高玻璃化转变温度的聚合物，作为本发明的弹性体组合物的可选择组分是有利的。由于玻璃化转变温度(Tg)比弹性体材料的使用温度高，这些聚合物在使用温度下相对稳定，帮助“锁进”三维网络结构并提供期望的弹性和机械特性。由于使用温度和玻璃化转变温度之间的差距缩小，这些聚合物变得更易流动。运动的聚合物链可从网络结构中解脱出来，产生弱的网络结构和退化的弹性和机械特性。应力弛豫特性对这种效应尤其敏感。
此外，对于可贴着人体并长时间穿着的体温应用品(如吸收制品、绷带、包裹物、伤口敷料等)，把具有高玻璃化转变温度的聚合物(如聚苯醚或乙烯芳烃聚合物)掺入到弹性体组合物是有利的。然而，熔融加工性和加工温度也是要考虑的因素。前者涉及弹性体材料的易加工性和不同加工方法的适用性。后者涉及把弹性体材料连接或应用于其它具有低热降解温度(如聚乙烯)或精细结构(如无纺织网)的基质或组分。作为任选的组分，可用于本发明的乙烯芳烃聚合物玻璃化转变温度范围典型地为约58℃至约180℃，更优选为约70℃至约150℃，更优选为约90℃至约130℃。
作为任选的组分，可用于本发明的热塑性聚合物具有的平均分子量要足够高，以提供高玻璃化转变温度、伸展性和弹性特性。此外，这些热塑性聚合物的平均分子量与弹性体嵌段共聚物没有显著的差异，以实现与刚性嵌段的相容。可用于本发明的合适的乙烯芳烃聚合物，其数均分子量典型地为约600至约200,000，更优选约5,000至约150,000，且最优选约10,000至约100,000。合适的乙烯芳烃聚合物的分子量分布在约1至约4范围内。在一个典型的实施方案中，乙烯芳烃为数均分子量在约40,000至约60,000的聚苯乙烯，如购自Nova Chemicals，Inc.，Monaca，PA的NOVACORPS 3900系列。
所述热塑性聚合物或组合物，当存在时，其含量按本发明使用的低应力弛豫弹性体组合物的重量计为约1％至约60％重量，优选约5％至约40％重量，且更优选约10％至约30％重量。
本发明的弹性体组合物还可包含其它添加剂，如抗氧化剂或稳定剂、防粘剂或增滑剂。典型的抗氧化剂为受阻酚(即那些具有空间位阻基团的，如在酚羟基附近有叔丁基)或多官能化酚(即含有硫或磷)。受阻酚抗氧化剂IRGANOX1010购自Ciba-Geigy Company，Hawthorn，New York。其它添加剂也可包括在弹性体组合物中，包括但不限于颜料、染料、紫外吸收剂、气味控制剂、香料、填充剂和干燥剂。每种添加剂可存在的含量少于约10％重量，优选少于5％重量，且更优选少于1％重量。
本发明还涉及包含上述弹性体组合物的薄膜。进一步，所述弹性体薄膜可在它的反面包含一个或更多表层，以改善薄膜的加工性和处理性。
典型的表层可包含聚合物，该聚合物与弹性体嵌段共聚物的组分至少部分地相容或相混，以在弹性体层和表层之间提供足够的粘性，以便进一步加工和处理。
适用作本文表层的热塑性聚合物可以是聚烯烃，衍生自单体如乙烯、丙稀、丁烯；α-烯烃包括1-丁烯、1-己烯、1-辛烯等；聚二烯，衍生自单体如异戊二烯、丁二烯、1，3-戊二烯等；以及这些单体的混合物；乙烯共聚物如乙烯-乙酸乙烯酯共聚物(EVA)，乙烯-甲基丙烯酸酯共聚物(EMA)，以及乙烯-丙烯酸共聚物；聚乙烯芳烃如聚苯乙烯，聚(α-甲基苯乙烯)，苯乙烯的无规嵌段共聚物(如INDEX共聚体，购自Dow Chemicals，Midland，MI)；聚苯醚；以及它们的混合物。
用于表层的材料可具有熔融流动特性，尤其适用于和上述弹性体组合物同时处理表面材料，以形成多层膜。生产多层聚合物膜的典型方法是共挤出法。在一个实施方案中，弹性体组合物和热塑性聚合物共挤出，在两个表层之间提供弹性体中心层，每个面基本都与中心层的反面相连接。所述两个表层可以具有相同或不同的组合物。
此外，粘合剂和/或联结层可被用来促进中心弹性体层和热塑性表层间的粘附。当使用时，每个联结层可占整个薄膜厚度的约5％至10％。
典型地，弹性体层本身能够在室温下作为一个完整无孔的薄膜承受50％至1200％的伸长率。弹性体层可包括纯弹性体或弹性组合物。本发明的弹性材料在室温下在200％伸长率时的应力弛豫可小于约20％，更优选地小于约30％，以及最优选地小于约40％。本发明弹性材料在体温下(约37.7℃(100°F))保持10小时后在50％伸长率时的应力弛豫小于约45％，优选地小于约50％，以及更优选地小于约55％。
本发明的表层优选地较薄且弹性比弹性体层小很多。在一些实施方案中，表层甚至可没有弹性。当表层和弹性体层一起使用时，所得的薄膜或纤网可具有与单弹性体层不同的修改的弹性特性。如果采用了多于一层的表层，则各表层可具有相同或不同的材料特性。
在一个多层薄膜中，弹性体层可占薄膜总厚度的约20％至约95％，每个表层可占薄膜总厚度的约1％至约40％。典型地，弹性薄膜(单层或多层)的厚度为约1.27μM(0.5MILS)至508μM(20MILS)，优选地为约25.4μM(1.0MIL)至约127μM(5.0MILS)。每个表层的厚度典型地为约1.27μM(0.05MIL)至约127μM(5MILS)，以及优选地为约2.54μM(0.1MIL)至约38.1μM(1.5MILS)。在一个有代表性的实施方案中，弹性体层的厚度为约81.28μM(3.2MILS)，每个表层的厚度为约3.81μM(0.15MIL)。在另一个有代表性的实施方案中，弹性体层的厚度为约81.28至76.2μM(3.2至3.0MILS)，每个表层的厚度为约3.048至2.54μM(0.12至0.10MIL)。
同样，在本发明的范围内为一个由诸如本文所描述的那些材料之类的多层弹性薄膜制成的宏观扩展的三维纤网。这样的纤网的详细说明被公开于美国专利3,929,135(THOMPSON)；4,342,314(RADEL等人)；5,733,628(PELKIE)；6,303,208(PELKIE)和PCT(专利合作条约)出版物WO 98/37266(CURRO等人)中。这样的三维纤网显示具有高孔隙度和高弹性以及可靠性和高强度的优点。
图1为本发明的宏观扩展的三维纤网80的代表性实施方案。纤网80显示具有多个主孔71，其通过例如彼此互连的构件91、92、93、94、95的互连构件的连续网络在第一表面90的平面102上被形成。主孔71投影在第一表面90的平面上的形状优选地呈规则或无规则图案排列的多边形形式，例如，正方形、六边形等。在另一个有代表性的实施方案中，每个互连构件包括一个位于平面102上的基底部分81，并且每个基底部分具有一个连接到其每个边缘上的侧壁部分83。侧壁部分83大致在纤网的第二表面85的方向上延伸并与毗连互连构件的侧壁相交。相交的侧壁部分彼此互连起纤网的第一和第二表面的中间体作用，并且基本上彼此同时终止形成第二表面85的平面106上的辅孔72。
图2为一般类似于图1的纤网80类型的一个纤网的进一步放大的局部视图。仅仅图示说明根据本发明的一个可供选择的纤网结构。纤网80的多层弹性有孔薄膜120优选地由至少一个弹性体层101和至少一个表层103构成。尽管图2显示了一个表层103靠近第一表面90的两层实施方案，据信有孔薄膜120的分层次序不受此限制。如图2所示，尽管在一些实施方案中，弹性体层基本上同时终止于第二表面平面上，应理解的是，它们不是必需这样，即，一层或多层可比其余的层朝第二表面延伸的更多。
本发明的弹性薄膜或纤网可被用于一次性吸收制品或卫生护理产品。应理解的是，甚至诸如内衣、长袜、绑腿、游泳衣和其它运动服装之类的可拉伸的衣服可得益于本发明的弹性薄膜或纤网的多孔、可拉伸特性。
图3中以处于平展状态(即，在被放置在穿着者身上之前)的呈尿布400形式显示了包含由本弹性组合物制成的弹性薄膜或纤网的一次性吸收制品的有代表性的实施方案。本文中使用的术语“尿布”是指通常由婴儿或失禁患者在躯干下部穿用的衣服。示例性的尿布构形一般被描述于美国专利3,860,003(BUELL)；5,151,092(BUELL等人)；5,221,274(BUELL等人)；5,554,145(ROE等人)；5,569,234(BUELL等人)；5,580,411(NEASE等人)和美国专利申请序列号08/915,471中。
图3为其中顶片404和底片402的延伸区域相同并且长度和宽度尺寸大于吸收芯406的那些尺寸的尿布400的代表性实施方案。顶片404与底片402连接到一起并上叠在底片402上以形成尿布400的周边。周边限定了尿布400的外周长或边缘。周边包括端边401和纵边403。
在一个实施方案中，尿布可包括一对弹性侧片420，其呈伸出的构型从尿布400的端边401中横向伸出来。在一个可供选择的实施方案中，可将衣服的相对侧424缝合或接合起来以形成一个短裤。这使该制品能够被用作套穿尿布或训练短裤。具有弹性侧片的示例性尿布被公开于美国专利4,857,067(WOOD等人)；4,381,781(SCIARAFFA等人)；4,938,753(VAN GOMPEL等人)；5,151,092(BUELL)；5,221,274(BUELL)；5,246,433(HASSE等人)；5,464,401(HASSE等人)；5,669,897(LAVON等人)；5,897,545(KLINE等人)；6,120,487(ASHTON)和美国专利申请序列号08/155,048(ROBLE等人)中。
弹性侧片420可包括本发明的弹性薄膜或纤网。在其它实施方案中，当将本发明的薄膜或纤网用作侧片时，其可通过在其一侧或两侧上粘结纤维性无纺材料来形成一个分层被进一步加工形成复合层压材料。
本发明的弹性薄膜或纤网也可被用于包括邻近尿布400周边的诸如腰部和腿部开口之类的弹性构件、弹性顶片或底片在内的尿布其它部分。
本发明的多层薄膜120可采用在传统共挤出制膜设备上生产多层薄膜的传统方法进行加工。一般而言，聚合物可采用或是注塑或是吹塑薄膜挤出法被熔化加工成薄膜，这两种方法被描述于ALLANA.GRIFF所著的“PLASTICS EXTRUSION TECHNOLOGY”，第二版(VAN NOSTRANDREINHOLD，1976)。共挤出法也被描述于均授予CLOEREN的美国专利4,152,387；4,197,069；4,533,308中。
在已经共挤出多层弹性薄膜后，将其优选地提供给用来成孔的成形工序，导致一个本发明的宏观扩展的三维弹性纤网。这样的工序可包括液压成形、真空成形并被描述于美国专利3,929,135；4,342,314；4,154,240；4,695,422；4,552,709；4,878,825；4,741,877；5,733,628(PELKIE)和PCT(专利合作条约)出版物WO 98/37266(CURRO等人)中。使平面的无孔弹性薄膜成孔的其它方法也为本领域所知，例如模具冲孔、铣切孔和热针熔化成孔。可采用这些方法将包括本发明弹性组合物的单层或多层薄膜制成有孔纤网。
薄膜或纤网可通过采用本领域已知的方法例如粘合剂、加热、加压或超声粘结在其一侧或两侧上与纤维性无纺材料粘结来形成一个分层被进一步加工形成一个复合层压材料。在粘结纤维性无纺材料后，由于所粘结的无纺材料相对没有弹性，该复合层压材料的弹性可比单独的弹性薄膜或纤网小。要使无纺材料弹性更大并使复合层压材料恢复弹性，复合层压材料可通过一种增量拉伸工序借助于用于使“零应变”层压材料具有弹性的方法和装置进行加工，如前面提到的美国专利5,143,679(WEBER等人)；5,156,793(BUELL等人)和5,167,897(WEBER等人)中所述。当用于吸收制品或其它个人/卫生护理制品时，所得的经过弹性处理的“零应变”复合层压材料具有一种柔软顺滑的布状感觉以及一种舒适暖和的贴合性。
辐射交联可用波长范围为250至400NM的紫外辐射来进行，并且剂量在约0.1至约10J/CM2之间，优选地在约0.5至约8J/cm2之间以及更优选地在约1至约5J/cm2的范围内变化。可用于本文的设备可为购自马里兰州Fredrick的INPRO Technologies的型号为LC-6B的台式输送机。辐射交联步骤典型地在共挤出和/或成孔步骤之后进行。
试验方法
A.拉伸强度和断裂伸长率
由该方法所确定的性质可与弹性薄膜的拉伸性有关。这些性质与选择适于用作穿上时被明显拉伸的吸收制品，尤其是套穿尿布、训练短裤、带扣件的一次性尿布或成人用的其它吸收性衣服的弹性部件材料有关。
可使用购自马里兰州Canton的Instron Engineering Corp.或明尼苏达州Eden Prairie的SINTECH-MTS Systems Corporation的市售拉伸测试仪来进行该试验。将薄膜切成MD(薄膜的纵向)2.54cm(1″)宽乘以CD(与MD成90°角的横向)5.08cm(2″)长的试样。将该仪器与用于控制试验速度和其它试验参数以及用于收集、计算和报告数据的计算机连接。薄膜的拉伸应力-应变特性根据ASTM Method D882-83进行确定。这些拉伸特性在室温下(约20℃)进行测定。步骤如下：
(1) 选择试验用的适当夹具和测力传感器；夹具应该足够宽以与试样吻合，典型地采用2.54cm(1″)宽的夹具；选择测力传感器以使从所测试的试样中得到的拉伸特性曲线将会在测力传感器的能力或所采用的载荷范围25％和75％之间，典型地采用22.7kg(50lb)的测力传感器；
(2) 根据厂商的说明书校准仪器；
(3) 将标距设定为2.54cm(1″)；
(4) 根据厂商的说明书将试样放在夹具的平直表面上；
(5) 将十字头速度设为0.254米/分钟(10″/分钟)的恒定速度；
(6) 开始试验并同时采集数据；和
(7) 计算并记录包括断裂伸长率、在100％、200％和300％伸长率时的载荷在内的拉伸特性。记录下三个试样的平均结果。
B.持续载荷应力弛豫试验
由本方法所确定的特性可与穿着具有诸如侧片、腰带等等之类的弹性部件的产品时穿着者所受的弹力、具体地讲在其已经被穿着一段时间后产品在体温下的贴合性有关。由本方法所确定的特性与选择在体温(约37.7℃(100°F))在持续载荷下抵抗应力弛豫、因此在长期穿着吸收制品的时间范围内提供不变的贴合性的材料有关。
仪器和试样与上述的试验方法A相同。持续载荷应力弛豫在37.7℃(100°F)(约为人体温度)下进行测定。步骤如下：
(1) 选择试验用的适当夹具和测力传感器；夹具应该足够宽以适应试样，典型地采用2.54cm(1″)宽的夹具；选择测力传感器以使从所测试的试样中得到的特性曲线将在测力传感器的能力或所采用的载荷范围25％和75％之间，典型地采用22.7kg(50lb)的测力传感器；
(2) 根据生产商的说明书校准仪器；
(3) 根据厂商的说明书将标距设定为2.54cm(1″)并将试样放在仪器中；
(4) 将十字头速度设为0.254米/分钟(10″/分钟)的恒定速度；
(5) 将试样预应变到500％的伸长率并马上(即，无需保持时间)回到0％伸长率；
(6) 重新夹住预应变的试样以除去任何弛豫并保持2.54cm(1″)的标距；
(7) 开始持续载荷应力弛豫试验并同时收集数据，持续载荷应力弛豫试验具有下列步骤：
a)以0.254米/分钟(10″/分钟)的速率达到200％伸长率；
b)原位置保持30秒；
c)以0.254米/分钟(10″/分钟)的速率回到0％的伸长率；
d)原位置保持60秒；
e)以0.254米/分钟(10″/分钟)的速率达到50％伸长率；
f)原位置保持10小时；和
g)回到0％拉伸率；和
h)计算作为初始载荷和在步骤7(f)的时间t处的载荷间损失率的50％伸长率时的应力弛豫如下：
纪录下三个试样的平均结果。
C.滞后或应力弛豫试验
由本方法所确定的特性可与穿着者从加入了弹性部件的产品上经受的力有关。第一循环为一个预应变步骤，其模拟最初将产品伸长以便将产品穿在穿着者身上或调整产品贴合该穿着者时的状况。第二循环测量由该预应变步骤产生的弹力的降低(即，应力弛豫)。
仪器和试样与上述的试验方法A相同。除了下列改变之外，试验步骤类似于上述的试验方法B。(1)在室温下(约20C)作本试验；(2)试验在步骤7(c)后终止；和(3)计算在200％伸长率时的应力弛豫作为在初始载荷和步骤7(b)的最终载荷的损失率。记录下在步骤7(c)期间在50％和30％时的卸载应力。
尽管已说明和描述了本发明的具体实施方案，但对于本领域的技术人员显而易见的是，在不背离本发明的精神和保护范围的情况下可作出各种其它变化和修改。因此有意识地在附加的权利要求书中包括本发明范围内的所有这些变化和修改。
实施例
实施例1至4
通过混合各种量的诸如购自德克萨斯州休斯顿市的Dexco Company的Vector 4211、Vector 8505系列之类的苯乙烯系弹性共聚物、购自德克萨斯州休斯顿市的Dexco Company的S-B-S/甲基丙烯酸酯改性S-B(SB-MA)的70/30混合物、诸如购自宾西法尼亚州Monaca的NovaChemical，Inc.的聚苯乙烯PS3900之类的乙烯芳烃树脂、购自新泽西州Bridgewater的National Starch and Chemicals的大分子光引发剂和诸如购自宾西法尼亚州Kams City的Pennzoil Co.，Penrenco Div.的Drakeol之类的矿物油来制备制剂，以形成一种弹性混合物。
通过将聚合组分和油干混至少24小时来制备混合制剂。将一个Haake间歇式搅拌器混合机预热到150℃并将干混合制剂缓慢地加入混合机中。有时，某些组分呈粘稠液体的形式，在混合步骤期间直接借助于吸移管将其加入聚合组分和油中。
表1显示了可用于本文的弹性组合物的实施例。每种组分的量用弹性组分的重量百分比表示。添加剂，具体地讲抗氧化剂，其仅有少量，未被显示于表1的组分中。典型地，用于本发明的弹性组分包括约0.5％的抗氧化剂和约0.3％的抗光剂。
表1
弹性组分(重量百分比)
| 实施例 | 1 | 2 | 3 | 4 |
| S-I-S | 43 | 72 | 43 | 0 |
| S-B-S | 0 | 0 | 29 | 72 |
| SBS/SB-MA | 28 | 0 | 0 | 0 |
| 聚苯乙烯PS3900 | 15 | 15 | 15 | 15 |
| 矿物油 | 10 | 8 | 8 | 8 |
| 大分子光引发剂 | 4 | 5 | 5 | 5 |
在暴露于紫外辐射之前和之后确定压制薄膜(模压的)的物理特性。
薄膜通过称重约12g的混合制剂进行制备。通过将预先称好的制剂置于在两片PTFE(Teflon)薄膜(254μm(0.010in)厚)之间模压该制剂，然后将其置于被装入型号为3853-0的Carver压力机中的预热的铝板间，铝板的预热温度设定为约168℃。将制剂加热3分钟，然后将其在施加了17.2MPa(2500psi)压力的平板间进行压缩。使制剂能够在压力下流动30秒。然后将所得的薄膜急冷至室温并随后切成三个相等的部分。将每部分放在PTFE薄膜和预热的铝板之间并在施加13.7MPa(2,000psi)压力之前使其在Carver压力机中加热到168℃保温1分钟。使制剂能够在该压力下流动30秒。卸掉压力并将试样旋转90°并装回到压力机中并马上施加20.6MPa(3,000psi)的压力。使制剂能够再次流动30秒。卸掉压力并将试样翻转装回到压力机中并马上施加27.57MPa(4,000psi)的压力。使制剂能够再次流动30秒。卸掉压力并将试样旋转90°，装回到压力机中并马上施加34.5MPa(5,000psi)的压力。使制剂能够再次流动30秒。在最后压缩之后，将薄膜急冷至室温。所得的薄膜厚度在101.6μm(4mils)至254μm(10mils)之间。根据上文所述的试验方法将薄膜切成合适的试样大小。
采用一个购自马里兰州Fredrick的INPRO Technologies，Inc.的型号为LC-6B的台式输送机来紫外辐射用来交联研究的切膜并与对应的不交联薄膜相比较。紫外交联通过在紫外源下将薄膜放在以约16.4米/分钟(54英尺/分钟)的速度移动的传送带上来进行。重复这个步骤4次以达到约1.4至2.5J/cm2的紫外剂量。
表2和3中公开了实施例1和2在紫外辐射之前或之后的物理特性。
表2
拉伸强度数据
| 实施例 | 100％时的应力(MPa) | 200％时的应力(MPa) | 300％时的应力(MPa) | 断裂伸长率(％) |
| 1a | 0.43 | 0.57 | 0.76 | 818 |
| 1b(紫外交联) | 0.89 | 1.75 | 3.21 | 830 |
| 2a | 1.37 | 1.89 | 2.80 | 780 |
| 2b(紫外交联) | 2.10 | 3.69 | 5.36 | 900 |
表3
滞后和持续载荷力弛豫数据
| 实施例 | 50％时的应力(MPa) | 200％时的应力(MPa) | 200％时的力弛豫(％) | 50％时的应力(卸载)(MPa) | 30％时的应力(卸载)(MPa) | 100F下50％时的10小时应力弛豫(％) |
| 1a | 0.35 | 0.58 | 9.4 | 0.21 | 0.13 | 56 |
| 1b(紫外交联) | 0.60 | 1.33 | 12.8 | 0.41 | 0.27 | 34 |
| 2a | 0.54 | 1.02 | 9.1 | 0.36 | 0.26 | 51 |
| 2b(紫外交联) | 0.78 | 1.97 | 13.4 | 0.41 | 0.25 | 29 |
如表2和3所示，尽管与实施例1和2的未交联试样相比，这些实施例的持续载荷应力弛豫显著降低，但紫外辐射的实施例1和2的拉伸强度和滞后提高了。
尽管已说明和描述了本发明的具体实施方案，但对于本领域的技术人员显而易见的是，在不背离本发明的精神和保护范围的情况下可作出许多其它的变化和修改。因此有意识地在附加的权利要求书中包括本发明范围内的所有这些变化和修改。
Claims (14)
1.辐射可固化材料，所述辐射可固化材料包括：
a)20％至80％重量的热塑性弹性体(TPE)，所述弹性体为嵌段共聚物，其具有至少一个包含乙烯芳烃的刚性嵌段和至少一个包含双烯的柔性嵌段；
b)5％至60％重量的加工油；和
c)至60％重量的大分子光引发剂；
d)可任选地，0.5％至10％重量的交联剂；和
e)可任选地，1％至60％重量的热塑性聚合物的组合物，所述聚合物包含聚乙烯芳烃；
其中，在固化后，所述材料在室温下伸长200％后的应力弛豫低于20％，在100°F下伸长50％10小时后的应力弛豫低于45％。
2.如权利要求1所述的辐射可固化材料，其中所述大分子光引发剂包含选自乙烯芳烃、不饱和双烯、部分饱和双烯以及它们的混合物的单体。
3.如前述任一项权利要求所述的辐射可固化材料，其中所述大分子光引发剂的单体单元的至少5％为具有反应性取代基的取代单体，所述取代单体具有下式结构
其中R1为乙烯基、乙烯芳烃、丙烯酸酯或甲基丙烯酸酯单体，并且R2为烷基、芳基、烷基芳基、烷氧基、取代的烷基、卤素、烷基磺酸盐、烷基铵磺酸盐、过酸酯、肉桂酸酯或叔胺。
4.如前述任一项权利要求所述的辐射可固化材料，其中所述刚性嵌段的1％至20％包含不饱和或部分饱和的双烯。
5.如前述任一项权利要求所述的辐射可固化材料，其中所述加工油选自烃油、石油衍生的油和蜡、合成蜡、天然蜡、矿物蜡、烯属低聚物以及它们的混合物；并且所述交联剂为硫醇、二丙烯酸酯、三丙烯酸酯、二(甲基丙烯酸酯)或三(甲基丙烯酸酯)。
6.共挤出的紫外可固化弹性体薄膜，所述薄膜包含弹性体层和至少一个连接到所述弹性体层的热塑性表层，所述弹性体层包含如前述任一项权利要求所述的辐射可固化材料。
7.贴着人体穿着的制品，所述制品的至少一部分包括可拉伸层压材料，所述层压材料包括具有相对的第一和第二表面的弹性体层，并且至少第一表层连接到所述弹性体层的第一表面，
其中所述弹性体层包括如前述任一项权利要求所述的辐射可固化材料。
8.如前述任一项权利要求所述的制品，其中所述可拉伸层压材料还包括连接到弹性体层的第二表面的第二表层。
9.如前述任一项权利要求所述的制品，其中所述第一和所述第二表层相同或不同并包含热塑性聚合物，所述热塑性聚合物选自聚烯烃、α-烯烃聚合物、聚二烯、乙烯共聚物、聚乙烯芳烃、聚苯醚，以及它们的混合物。
10.如前述任一项权利要求所述的制品，其中所述可拉伸层压材料为多层膜、三维宏观扩展纤网或有孔纤网。
11.如前述任一项权利要求所述的制品，其中所述可拉伸层压材料连接到第一表层的开放表面上的纤维无纺材料上，以形成复合层压材料。
12.如前述任一项权利要求所述的制品，其中所述制品的一部分选自侧片、腿部弹性构件、腰部弹性构件、弹性顶片、弹性底片以及它们的组合。
13.如前述任一项权利要求所述的制品，其中所述制品为系牢/扣紧的尿布、套穿尿布、训练裤、失禁衣服、卫生巾、短裤护垫、擦拭物、伤口敷料、绷带、消毒盖布、包裹物、游泳衣、运动服、长袜、绑腿或内衣。
14.生产可拉伸层压材料的方法，所述方法包括以下步骤：
共挤出如权利要求1至5所述的弹性体材料和热塑性聚合物以形成可拉伸层压材料，所述层压材料包括一个弹性体芯层和至少一个热塑性表层；
辐射交联所述可拉伸层压材料以完成足够量的交联来改善所述弹性体薄膜的应力弛豫特性；
在所述可拉伸层压材料上开孔；
可任选地，将所述表层的自由面连接到纤维无纺材料上，以形成复合层压材料；和
可任选地，递增拉伸所述复合层压材料的至少一部分以永久伸长被拉伸部分中的纤维无纺材料。
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2003
- 2003-07-01 DE DE60326845T patent/DE60326845D1/de not_active Expired - Lifetime
- 2003-07-01 MX MXPA05000090A patent/MXPA05000090A/es unknown
- 2003-07-01 JP JP2004519722A patent/JP2005530030A/ja active Pending
- 2003-07-01 CN CNB038155826A patent/CN1324081C/zh not_active Expired - Fee Related
- 2003-07-01 AU AU2003253769A patent/AU2003253769A1/en not_active Abandoned
- 2003-07-01 AT AT03763076T patent/ATE426639T1/de not_active IP Right Cessation
- 2003-07-01 CA CA002489168A patent/CA2489168A1/en not_active Abandoned
- 2003-07-01 WO PCT/US2003/020692 patent/WO2004005398A1/en active Application Filing
- 2003-07-01 EP EP03763076A patent/EP1517958B1/en not_active Expired - Lifetime
- 2003-07-01 US US10/610,605 patent/US7445831B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103522682A (zh) * | 2013-04-09 | 2014-01-22 | 林志平 | 一种双层复合弹性打孔膜及其生产方法 |
| CN103522682B (zh) * | 2013-04-09 | 2016-11-30 | 林志平 | 一种双层复合弹性打孔膜及其生产方法 |
| CN108603079A (zh) * | 2016-02-01 | 2018-09-28 | 3M创新有限公司 | 可适形的、可剥离的粘合剂制品 |
Also Published As
| Publication number | Publication date |
|---|---|
| AU2003253769A1 (en) | 2004-01-23 |
| US7445831B2 (en) | 2008-11-04 |
| EP1517958A1 (en) | 2005-03-30 |
| DE60326845D1 (de) | 2009-05-07 |
| CA2489168A1 (en) | 2004-01-15 |
| US20040049836A1 (en) | 2004-03-18 |
| ATE426639T1 (de) | 2009-04-15 |
| WO2004005398A1 (en) | 2004-01-15 |
| MXPA05000090A (es) | 2005-04-08 |
| JP2005530030A (ja) | 2005-10-06 |
| CN1324081C (zh) | 2007-07-04 |
| EP1517958B1 (en) | 2009-03-25 |
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