CN1233209A - 改善滞后性的弹性层合制品 - Google Patents
改善滞后性的弹性层合制品 Download PDFInfo
- Publication number
- CN1233209A CN1233209A CN97198735A CN97198735A CN1233209A CN 1233209 A CN1233209 A CN 1233209A CN 97198735 A CN97198735 A CN 97198735A CN 97198735 A CN97198735 A CN 97198735A CN 1233209 A CN1233209 A CN 1233209A
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- Prior art keywords
- laminate
- elastomer
- blend
- polymer
- elastomeric
- Prior art date
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Classifications
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Abstract
提供一种改善滞后性的复合弹性材料(40),其包含在至少一个侧面上粘合到非弹性材料层(12)上的弹性材料层。弹性材料层(32)是由窄多分散性数值的聚合物和常规弹性体的共混物制备的,该共混物基本不含低分子量聚乙烯加工助剂。复合弹性材料层合制品(40)的滞后性,比不具有窄多分散性数值的弹性体而具有加工助剂制成的相似层合制品,好至少15%。
Description
发明背景
概括地说,本发明涉及包含至少一层弹性层的,由纤维、薄膜、纤维排列等形成的非织造织物或纤网层合制品,这类材料由热塑性树脂制造。
将热塑性树脂挤出成形为纤维、织物和薄膜等已有多年历史。用于这种用途的最普通的热塑性树脂是聚烯烃,特别是聚丙烯。诸如聚酯、聚醚酯、聚酰胺和聚氨酯等其他材料也应用于制造这些层状物。
例如,非织造织物广泛地用于诸如尿布、妇女卫生用品、毛巾、休闲或防护织物以及土工布和过滤介质之类的各种应用之中。在这些应用中使用的非织造纤网可以是单纯的纺粘织物,但是经常取非织造织物层合制品的形式,例如纺粘/纺粘(SS)层合制品、纺粘/熔喷/纺粘(SMS)层合制品和纺粘/薄膜/纺粘层合制品(SFS)。
非织造纤网的许多用途要求具有若干弹性度。例如,诸如尿布之类制品的用途,需要材料能随婴幼儿的正常运动而伸展和缩回。尿布缺乏这种弹性会限制运动,或者由于弯曲或伸展而产生渗漏。
提供可伸展的弹性层合制品的工作以前主要集中在弹性足以在这种应用中很好起作用的苯乙烯类共聚物上。Wisneski等的美国专利4663220,已被共同转让,是这类发明的好例子。已经证明,这些聚合物多少有些昂贵,在今天消费者需要的产品市场中并不完全令人满意。因此,需要经济的这类化合物的替换物。还需要比现在所使用者具有更好的滞后性的弹性材料。
发明概述
采用具有改善滞后性的复合弹性材料达到了本发明的目的,该材料包含至少在一面上被粘合到非弹性材料层上的弹性材料层。该弹性材料层由窄的多分散性数值聚合物和通用弹性体的共混物制造,该共混物基本不含低分子量聚乙烯加工助剂,但可以含有增粘剂。复合弹性材料层合制品的滞后性,比不含窄多分散性数值弹性体而含加工助剂而制造的相似层合制品,至少好15%。
附图简述
所附图示意说明了复合弹性颈缩-粘合材料的制造方法。
定义
本文所使用的术语“非织造织物或纤网”意指结构为单根纤维或丝交互铺置的,而不是象针织物或机织物那样以一种可看作是相同的方式铺置的纤网。非织造织物或纤网现已能用许多方法制成,例如熔喷法、纺粘法和机梳纤网粘合法。非织造织物的单位重量通常以每平方码材料的盎司数(osy)或以每平方米的克数(gsm)表示,有效纤维直径通常以微米表示。(注:从osy换算成gsm的方法为osy×33.91)。
本文使用的术语“微纤维”意指平均直径不大于约75微米的小直径纤维。例如:平均直径为约0.5~约50微米,或者更具体地说,微纤维的平均直径可为约2~约40微米。另一种常常用于表示纤维直径的词是“旦”,其定义是每9000米纤维的克数,其可以按下述计算,即,以微米为单位的纤维直径的平方,乘以以克/厘米3为单位的聚合物密度,再乘以0.00707。旦数越低表示纤维越细,而旦数越高表示纤维越粗或越重。例如,给定15微米的聚丙烯纤维直径可以通过下述方法转化成旦数,即,将该直径数值平方、再将所得结果乘以0.89克/厘米3,再乘以0.00707。这样,15微米的聚丙烯纤维的旦数为约1.42(152×0.89×0.00707=1.415)。除了美国之外,计量单位通常更多使用的是“特”,其定义为每一千米纤维的克数。特数可以按旦数/9计算出。
本文所使用的术语“纺粘纤维”指的是小直径纤维,其成型方法包括:将熔融热塑性材料,从纺丝板的许多细的通常为圆形的毛细纺丝孔中以长丝的形式挤压出来,然后挤出的长丝直径迅速按以下专利所述方法变小。所述专利例如Appel等人的美国专利4340563、Dorschner等人的美国专利3692618、Matsuki等人的美国专利3802817、Kinney的美国专利3338992和3341394、Hartman的美国专利3502763和Dobo等人的美国专利3542615。当沉积在凝聚面上时,纺粘纤维一般是不发粘的。纺粘纤维一般是连续的,并且平均直径(自至少10根纤维的样品)大于7微米,更具体地说,为约10~20微米。
本文所使用的术语“熔喷纤维”意指按如下方法形成的纤维,将熔融热塑性材料经许多细的、通常为圆形的压出板毛细纺丝孔,以熔融纤维或长丝的形式挤出到通常为热的会聚高速气流(例如空气)中,该气流使熔融热塑材料的丝变细来减少其直径,可以达到微纤维直径。此后,高速气流携带熔喷纤维,纤维被沉积于凝聚面上,形成无规分布的熔喷纤网。这种方法公开于,例如,Butin等的美国专利3849241中。熔喷纤维是微纤维,可以是连续的或者不连续的,其平均直径一般小于10微米;在将其置于凝聚面上时,它通常是发粘的。
本文所使用的术语“长丝排列”意指基本平行的长丝的丝束,可以是,例如,美国专利5385775和5366793中所公开者。
本文所使用的术语“共成型”意指下述方法,在该方法中,将至少一个熔喷模头安装在溜槽附近,其他材料通过溜槽加入到正在成型的纤网中。这些其他材料可以是,例如纸浆、超吸收颗粒、纤维素或短纤维。共成型方法见于已经共同转让的Lau的美国专利4818464和Anderson等人的4100324中。通过共成型方法制造的纤网一般称为共成型材料。
本文所使用的术语“多层层合制品”意指一些层是纺粘的而一些层是熔喷的的层合制品,例如纺粘/熔喷/纺粘(SMS)层合制品等,其他的公开在下述专利中:Brock等人的美国专利4041203、Collier等人的美国专利5169706、Potts等人的美国专利5145727、Perkins等人的美国专利5178931和Timmons等人的美国专利5188885。这样的层合制品可以通过如下方法制造,在移动的成型输送带上顺序沉积先是纺粘织物层、然后是熔喷织物层、最后是另一纺粘层;再用下述方法将该层合制品粘合在一起。或者用另一种方法,可以单独制造各织物层,再将其收集成布卷,再在单独的粘合步骤中结合在一起。这类织物的单位重量通常为约0.1~12osy(6~400gsm),或者,更具体地说,为约0.5~约3osy。多层层合制品也可以按许多不同的构型含有不同数目的熔喷层或多层纺粘层,还可以包含其他诸如薄膜(F)之类的材料或共成型材料,例如SMMS、SM、SFS等。
本文所使用的术语“复合弹性材料”指的是下述弹性材料,它可以是多组分材料或多层材料,后者的其中一层是有弹性的。这些材料可以是,例如,“颈缩粘合”层合制品、“拉伸粘合”层合制品、“颈缩拉伸粘合”层合制品和“零应变”层合制品。复合弹性材料也可用下述成型方法来制造,此法包括:按美国专利申请08/730511所述,在未拉伸条件下将各层结合起来,然后颈缩。该申请与本发明同一天提交美国专利和商标局,并转让相同受让人,题目为“具有改善的横向延伸性的层合织物及其生产方法”,在此引入作为参考。
“颈缩粘合”指的是这样一种方法,在该方法中,仅仅非弹性部被延伸或颈缩,以便减小其在垂直于延伸的方向的尺寸,这时,将弹性部件粘合到非弹性部件上。“颈缩粘合层合制品”指的是按颈缩粘合方法制造的复合弹性材料,即,当仅仅非弹性层处在延伸状态下时,将各层结合在一起。这样的层合制品通常在横向具有拉伸性能。颈缩粘合层合制品的实例见述于Morman的美国专利5226992、4981747、4965122和5336545以及Haffner等人的美国专利5514470中。
通常,“拉伸粘合”指的是这样一种方法,在该方法中,当仅仅将弹性部件延伸其松驰长度的至少约25%时,将弹性部件粘合到其他部件上。“拉伸粘合层合制品”指的是按照拉伸粘合方法制造的复合弹性材料,即,当仅仅弹性层处在延伸状态下时,将各层结合在一起,如此,靠着松弛各层,使非弹性层收拢。这样的层合制品通常在纵向上具有拉伸性能,其后,该层合制品可以拉伸到在粘合位置之间收拢的非弹性材料使弹性材料伸长的程度。一种拉伸粘合层合制品公开在,例如,Vander Wielen等的美国专利4720415中,其中使用了从复排挤出机生产的相同聚合物的多个层。其他的复合弹性材料公开在Kieffer等人的美国专利4789699、Taylor的美国专利4781966和Morman的美国专利4657802和4652487以及Morman等人的4655760中。
“颈缩拉伸粘合”一般指的是这样一种方法,在该方法中,当弹性部件被延伸其松驰长度的至少约25%时,将弹性部件粘合到另一部件上;而另一层是颈缩非弹性层。“颈缩拉伸层合制品”指的是按照颈缩拉伸粘合法制造的复合弹性材料,即,在两层均处于延伸状态下时将各层结合在一起,然后使其松驰。这种层合制品通常具有无定向拉伸性能。
“零应变”拉伸粘合通常指的是这样一种方法,在该方法中,至少两层在未受张力(因此为零应变)状态下彼此粘合,并且,在其中,一层是可拉伸的而且是弹性体的,而另一层是可拉伸的但未必是弹性体的。然后,通过使用减少纤网经受的应变速率的一对或多对啮合沟槽辊,将层合制品递增地拉伸。“零应变拉伸层合制品”指的是按照零应变拉伸粘合方法制造的复合弹性材料,即,弹性层和非弹性层均处于非延伸状态时彼此结合在一起。第二层,随着层合制品的拉伸,将至少在某种程度上被永久伸长了,这样,层合制品不会因除去拉伸力而回转到其原来的未变形的状态。这导致了层合制品的Z-向隆起,以及随之而来的至少直至初始拉伸点的初始拉伸方向上的弹性延伸性。这样的层合制品及其生产方法的实例可见述于美国专利5143679、5151092、5167897和5196000。
本文所使用的术语“颈缩”或“颈缩拉伸”通用,均指一种将非织造织物通常在纵向上拉长的方法,以便将其幅宽以控制的方式减少到所需要的数值。该控制拉伸可以在冷却、室温或较高温度下进行,将它限制在拉伸方向上的总尺寸的增加最高可达到使织物断裂所需要的伸长,在许多情况下,该伸长约为1.2~1.4倍。当松驰时,纤网朝着其原尺寸方向收缩。这种方法已公开在,例如,Meitner和Notheis的美国专利4443513、Morman的美国专利4965122、4981747和5114781以及Hassenboehler Jr.等人的美国专利5244482中。
本文所使用的术语“颈缩软化”意指,当材料在纵向上进行拉伸时,在不加热的条件下,即在室温下,对材料进行的颈缩拉伸。在颈缩拉伸或颈缩软化中,所指的织物,例如,被拉伸20%。这意指织物在纵向上拉伸一直到其长度为其未拉伸的原长度的120%。
本文所使用的术语“可颈缩材料”意指任何能被颈缩的材料。
本文所使用的术语“颈缩材料”指的是任何通过诸如拉伸或收拢的方法在至少一维方向上已被收缩的材料。
本文所使用的术语“弹性”和“弹性体”,当针对纤维、薄膜或织物时,意指一种材料,该材料因受到位移力的作用可拉伸到拉伸的位移的长度,该长度至少为其松弛的未拉伸长度的约150%或一倍半,当除去拉伸位移力时,材料回复其伸长的至少50%。
本文所使用的术语“回复”指的是,在通过施加位移力拉伸某材料后,因位移力终止而产生的被拉伸材料的收缩。例如:假如松弛的未位移的1英寸长的材料通过拉伸到1.5英寸长,即被拉伸50%,那未该材料所具有的拉伸长度为松弛长度的150%。假如该示范拉伸材料在除去位移和拉伸力之后,收缩即回复到1.1英寸长,那未材料回复了其伸长的80%(0.4英寸)。
本文所使用术语的“未颈缩”(“un-necking”)意指应用于可逆颈缩材料的方法,通过施加方向为大体上垂直于原拉伸力方向的拉伸力使其延伸到至少其原来的预颈缩尺寸,该拉伸力在其除去时导致材料回复到其可逆颈缩尺寸的至少约50%范围之内。
本文所使用的术语“聚合物”通常包括,但并不限于:均聚物、共聚物例如嵌段、接枝、无规和交替共聚物、三元共聚物等以及其共混物和改性物。此外,除非另外专门限制,术语“聚合物”包括材料所有可能的分子几何构型。这些构型包括,但并不限于,等规、间规和无规对称构型。
本文所使用术语“单组分”纤维指的是使用仅仅一种聚合物由一台或一台以上挤出机制造的纤维。这不意味着排除由一种聚合物制造,但为色泽、抗静电性、润滑性和亲水性等而加入少量添加剂的纤维。这些添加剂,例如用于着色的二氧化钛,一般用量为5%(重量)以下,更典型的为约2%(重量)。
本文所使用的术语“共轭纤维”指的是由至少两种聚合物经各自独立的挤出机挤出但是纺在一起形成一根纤维所制造的纤维。共轭纤维有时也称为多组分纤维或双组分纤维。一般聚合物是彼此不同的,尽管共轭纤维也可以是单组分纤维。聚合物在共轭纤维横断面上排列在位置基本恒定的不同区域,并沿着共轭纤维的长度连续延伸。这样的共轭纤维的排列可以是,例如一种聚合物围绕着另一种聚合物的皮/芯排列,或者可以是并列排列、盘形排列或者“海岛”排列。共轭纤维见述于Kaneko等人的美国专利5108820、Krueger等人的美国专利4795668和Strack等人的美国专利5336552。共轭纤维也述于Pike等人的美国专利5382400,其可以用于在纤维中产生卷曲,方法包括两种(或多种)聚合物以不同速率伸长和收缩。卷曲纤维也可以采用机械方法和通过德国专利DT2513251A1的方法生产。对于两种组分的纤维来说,聚合物的存在比例可以为75/25、50/50、25/75或者任何其他需要的比例。纤维也可以具有如Hogle等人的美国专利5277976、Hills的美国专利5466410和Largman等人的美国专利5069970和5057368所述的形状,这些专利叙述了具有非常规形状的纤维。
本文所使用的术语“双成分纤维”指的是从同一台挤出机以共混物的形式挤出的至少两种聚合物形成的纤维。术语“共混物”的定义见下述。双成分纤维没有以相对稳定地定位在纤维横截面中不同区域的方式排列的各种聚合物组分,各种聚合物沿着纤维全长通常是不连续的,而是通常形成无规开始和结束的原纤维或原生纤维。双成分纤维有时也称为多成分纤维。这种通用型纤维,例如,在Gessner的美国专利5108827和5294482中,已有详述。详述双组分纤维和双成分纤维的文献还有,作者为John A.Manson和Leslie H.Sperling的教科书《聚合物共混物和复合材料》(Polymer Blends and Composites),纽约的PlenumPublishing Corposation的分部,Plenum Press,1976版权,IBSN0-306-30831-2,第273页至277页。
本文所使用的术语“共混物”意指两种或两种以上聚合物的混合物,而术语“合金”意指共混物的一个子类,其中各组分不溶混,但是已被相容。
术语“相似的纤网或层合制品”意指,作为发明材料,使用了基本相同的工艺条件的纤网或层合制品,但是其中聚合物稍有变化。按照“Webster′s New Collegiate Dictionary”(1980),“相似”意指:1)具有共同的特性,十分类似;2)在材料上或实质上相似;一致。采用“相似”这个词的普遍被接受的含义,这个术语意指,除了所述的条件外,所有其他条件均基本相同。应当指出,在不同聚合物之间并不是所有条件均完全相同,因为组分本身的变化使工艺变化,例如,所需要的最佳温度的变化。
本文使用的术语“衣服”意指任何类型的非医用可以穿着的有关服装。其包括诸如衣裤相连的工作服之类的工业工作服、内衣、裤子、衬衣、夹克、手套和短袜等。
本文使用的术语“防感染用品”意指有关医用物品,例如:外科用手术服和消毒档帷,面罩,诸如膨松帽、外科用帽和头巾之类的头部覆盖物,诸如鞋套、靴套和拖鞋之类的鞋袜、绷带、绷带、杀菌包、楷布、诸如实验外套之类的衣服、衣裤相连的工作服、围裙和短外衣、病员床上用品、担架和摇篮用的被单等。
本文所用的术语“个人护理用品”意指尿布、运动裤、吸湿衬裤、成人失禁用品和妇女卫生用品。
试验方法
熔体流动速率:熔体流动速率(MFR)是聚合物粘度的一种度量。MFR以在规定负荷或切变速率下在测定时间内从已知尺寸的毛细管流出的物料重量表示;按照,例如:ASTM试验1238-90b,在设定温度和负荷下进行测量,以g/10min为单位表示。
循环试验:循环试验采用Sintech2计算机化材料试验装置进行,该装置由Sintech公司(Stoughton,MA)提供。
在伸长或拉伸至停止的试验中,将3英寸×6英寸(76mm×152mm)的、其较长尺寸为纵向的样品置于Sintech2机的夹头中,所使用的夹头间隙为50mm。然后,以约500mm/min的十字头速度将试样拉伸到停止负荷为2000g。此时相对于未拉伸长度计的伸长率%是拉伸到停止的数值。
停止试验伸长也产生截距伸长值。截距伸长是当材料弹性不起作用、样品拉伸强度占优势时的负荷,以克为单位。用截距伸长值的75%确定样品在随后循环试验中拉伸的最大百分数。
在循环试验中,使材料达到相当截距伸长的75%的固定伸长五次,使其回到原来尺寸(如果能作到的话)。所进行的测量是伸长负荷、滞后损耗和回复负荷。可以使用这些数据,作出表示该结果的图,Y轴为负荷,X轴为伸长率。该图得到一条曲线,在其下面的区域称为吸收总能量或“TEA”。样品多次循环的TEA曲线的比值是与材料、单位重量和试样宽度无关的数值,其可以与其他样品进行比较。
详述
弹性层合制品广泛应用于许多用途,例如在服装,防感染用品和个人护理用品中。这类材料能使这些物品更舒服地适应用途和更耐用。
测定弹性材料性能如何的一种方法是测定其滞后性。滞后性是弹性材料经多次拉伸是否或如何优良地维持其弹性的一种度量,理想的是,材料经多次拉伸循环,其滞后损耗应当很小。循环试验用来测定材料的滞后,上文对该试验已作说明。
没有滞后损耗的材料应当显示为,在第二次循环收缩过程中伸长率30%时所测定的力与第一次循环过程中在伸长率为30%时的伸长力相同。第一次循环的伸长力除以第二次循环的收缩力(两者伸长率都为30%)表明,该材料滞后为1.0。具有某些滞后损耗的材料该数值应当大于1.0,比值越小越好。
借助于选择弹性层的材料,本发明的复合弹性材料在伸长率为30%下的滞后比,与以前已知的弹性层合制品相比,至少改善15%。优选弹性材料层由常规弹性体和窄多分散性数值的聚烯烃弹性体的共混物制造,例如多分散性为4或4以下。多分散性数值有时称为多分散性指数,其定义是重均分子量除以数均分子量。
参见图,其中以10示意说明复合弹性颈缩粘合材料的制造方法。
按照本发明的一个实施方案,可颈缩的非弹性材料12从供料辊14退绕下来,随着供料辊14按与其相关的箭头方向的转动,非弹性体材料按与其相关的箭头所示的方向行进。可颈缩的材料12通过由传动辊20和22所形成的传动辊装置18的辊隙16。
非弹性材料12可以在制成后,直接通过辊隙16,而不先贮存在供料辊上。
弹性材料32从供料辊34退绕下来,随着供料辊34按其相关的箭头方向的转动,弹性材料按与其相关的箭头所示的方向行进。弹性材料32通过由粘合辊28和30所形成的粘合辊装置26的辊隙24。弹性材料32可以在制成后,直接通过辊隙24,而不先贮存在供料辊上。
非弹性材料12通过S-辊装置18的辊隙16,其路径为反-S形,如与辊组20和22相关的转动箭头方向所示。从S-辊装置18出来的非弹性材料12通过由粘合辊装置26所形成的加压辊隙24。因为S-辊装置18的辊的周边线速度被控制小于粘合辊装置26的辊的周边线速度,所以非弹性材料12在S-辊装置18和粘合辊装置26的加压辊隙之间受到拉伸。通过调节辊的速度差,非弹性材料12受到拉伸,以使其颈缩所需要的量,并保持在这样的拉伸的颈缩状态下,同时弹性材料32,在它们通过粘合辊装置26的过程中,结合到颈缩非弹性材料12上,形成复合弹性颈缩粘合层合制品40。
也可以使用其他方法拉伸可颈缩的非弹性材料12,例如,拉幅机或其他与纵向交叉的方向伸幅器设备,这些设备在其他方向上使非弹性材料12扩展,例如在与纵向交叉的方向上,结果,在非弹性材料12粘合到弹性材料32上以后,所得的复合弹性颈缩粘合材料40在平行于颈缩方向的方向上,即纵向,是具有弹性的。
本发明中使用的非弹性材料12可以是微纤维纤网,例如由纺粘和熔喷工艺所生产者,微纤维可以是卷曲的或非卷曲的。非弹性材料12也可以是长丝排列、泡沫体、粘合机梳纤网(bonded carded web)和共成型纤网。
非弹性材料12可以由诸如聚烯烃之类的成纤聚合物制造。典型的聚烯烃包括一种或多种聚丙烯、聚乙烯、乙烯共聚物、丙烯共聚物和丁烯共聚物。实用的聚丙烯包括,例如,Montell公司出品的聚丙烯,商品名PC-973;Exxon化学公司出品的聚丙烯,商品名Exxon 3445;Shell化学公司出品的聚丙烯,商品名DX 5A09。
非弹性材料12可以是含有下述的多层材料,含有,例如,至少一层纺粘纤网,该纤网接合到熔喷纤网、粘合机梳纤网或其他适宜的材料的至少一层上。例如:非弹性材料12可以是,包含第一层单位重量为约0.2~约8osy的纺粘聚丙烯层,和第二层单位重量为约0.2~约8osy的纺粘聚丙烯层的多层材料。替代地,非弹性材料12可以是单层材料,例如,单位重量为约0.2~约10osy的纺粘纤网,或者单位重量为约0.2~约8osy的熔喷纤网。
非弹性材料12也可以是两种或多种不同纤维的混合物制造的复合材料,或者纤维和粒子的混合物制造的复合材料,如共成型纤网。这类混合物可以通过把纤维和/或粒子加到携带熔喷纤维的气流中制得;这样,在熔喷纤维被收集到收集设备上之前,熔喷纤维和其他材料进行了充分的缠结混合;所述其他材料例如木浆、短纤维和粒子,如普通称为超吸收材料的水解胶体(水凝胶)颗粒;这样形成了熔喷纤维和其他材料无规分散的粘结纤网,例如公开在美国专利4100324中的纤网。
如果非弹性材料12是纤维的非织造纤网,那末纤维应通过纤维间粘合而结合形成能够经受颈缩的粘附纤网结构。纤维间粘合可以通过单根熔喷纤维之间缠结而产生。纤维缠结是熔喷工艺所固有的,但是通过诸如水力缠结或针刺工艺的方法可以产生或增加。替代和/或附加,可以使用粘合剂,以便增加所需要的粘合。
本发明所使用的弹性材料可以是微纤维纤网,例如,通过纺粘和熔喷工艺制造的非织造纤网,微纤维可以是卷曲的或没有卷曲的。弹性材料也可以是长丝排列、薄膜和泡沫体。
非织造工艺一般使用挤出机将熔融的热塑性聚合物供应到喷丝板,在喷丝板将聚合物纤维化,得到可以切成短纤长度或较长的纤维。然后将纤维拉伸,通常采用气动方法,再将其沉积于运动着的有小孔的垫或运输带上,形成非织造织物。在纺粘和熔喷工艺中所生产的纤维是上文所定义的微纤维。
弹性材料层优选由常规弹性体和窄的多分散性的聚烯烃弹性体的共混物制造,例如多分散性为4或更小。优选,弹性材料层由约62%~约80%(重量)的常规弹性体和约10%~约30%(重量)窄多分散性的聚烯烃弹性体的共混物制造。
完全由窄的多分散性数值的聚合物制造的弹性层也是能使用的,但这不是本发明的主题。
在本发明实践中使用的常规弹性体热塑性聚合物可以是由下述制的弹性体,即,嵌段共聚物如聚氨酯、共聚醚酯、聚酰胺聚醚嵌段共聚物、乙烯醋酸乙烯酯(EVA)、通式为A-B-A′或A-B的嵌段共聚物如共聚(苯乙烯/乙烯-丁烯)、苯乙烯-聚(乙烯-丙烯)-苯乙烯、苯乙烯-聚(乙烯-丁烯)-苯乙烯、(聚苯乙烯/聚(乙烯-丁烯)/聚苯乙烯和聚(苯乙烯/乙烯-丁烯/苯乙烯)等。
有用的弹性体树脂包括通式为A-B-A′或A-B的嵌段共聚物,式中A和A′分别是热塑性聚合物端嵌段,其包含诸如聚(乙烯基芳烃)的苯乙烯部分,式中B是弹性体聚合物的中嵌段,如共轭二烯或低级链烯聚合物。A-B-A′型嵌段共聚物,对于A和A′嵌段来说,能够含有不同的或相同的热塑性嵌段聚合物;本嵌段共聚物是用来包含线性、支链和放射状嵌段共聚物。在这方面,放射状嵌段共聚物可以表示为(A-B)m-X,式中X是多官能原子或分子,其中每一个(A-B)m-以A是端嵌段的方式从X向各方伸展出。在放射状嵌段共聚物中,X可以是有机或无机多官能原子或分子,m是数值与原来存在于X中的官能基个数相同的整数。其通常至少为3,常常为4或5,但不限于此。因此,在本发明中,词“嵌段共聚物”、和特别是“A-B-A′”和“A-B”嵌段共聚物,是用来包含能够挤出的(例如,通过熔喷)所有的前文详述的具有橡胶态嵌段和热塑性嵌段的嵌段共聚物,而对嵌段数目没有限制。弹性体非织物纤网可以由,例如弹性体(聚苯乙烯/聚(乙烯-丁烯)/聚苯乙烯)嵌段共聚物制造。这类弹性体共聚物的商用例子是,例如,Shell化学公司(得克萨斯州、休斯敦)出品的称为KRATON材料。KRATON嵌段共聚物能以几种不同的配方供货,许多配方可见于美国专利4663220和5304599,在此引入作为参考。
在实施本发明中,也可以使用由弹性体A-B-A-B四嵌段共聚物组成的聚合物。这类聚合物详述在Taylor等的美国专利5332613中。在这类聚合物中A是热塑性聚合物嵌段,B是氢化至基本是聚(乙烯-丙烯)单体单元的异戊二烯单体单元。这种四嵌段共聚物的实例是苯乙烯-聚(乙烯-丙烯)-苯乙烯-聚(乙烯-丙烯)或SEPSEP弹性体嵌段共聚物,由Shell化学公司(得克萨斯州,休斯敦)出品,商品名为KRATON。
可以使用的其他典型的弹性体材料包括聚氨酯弹性体材料,例如B.F.Goodrich & Co出品的商标名为ESTANE者、或Morton Thiokol公司出品的MORTHANE;聚酯弹性体材料,例如杜邦公司出品的商品名为HYTREL者、和AKZO Plastics(Amhem,荷兰)以前出品的而由DSM(Sittard,荷兰)现在出品的ARNITEL者。
式中:n是正整数,PA代表聚酰胺聚合物链段、PE代表聚醚聚合物链段。尤其是,聚醚嵌段酰胺共聚物的熔点为约150℃~约170℃,按ASTM D-789测定;熔体指数为约6克/10分钟~约25克/10分钟,按ASTM D-1238、条件Q(235℃/1kg负荷)测定;挠曲弹性模量为约20Mpa~约200Mpa,按ASTM D-790测定;断裂拉伸强度为约29Mpa~约33Mpa,按ASTM D-638测定;以及极限断裂伸长为约500%~约700%,按ASTM D-638测定。聚醚嵌段酰胺共聚物的具体实施方案,熔点为约152℃,按ASTM D-789测定;熔体指数为约7克/10分钟,按ASTM-D-1238条件Q(235℃/1kg负荷)测定;挠曲弹性模量为约29.50Mpa,按ASTM D-790测定;断裂拉伸强度为约29Mpa,按ASTM D-639测定,断裂伸长为约650%,按ASTMD-638测定。这类材料能以各种级别得自Atochem公司聚合物分部(RILSAN)(Glen Rock,新泽西州),商品名为PEBAX。这类聚合物的应用实例可见述于Killian等人的转让给本发明相同受让人的美国专利4724184、4820572和4923742,在此引入作为参考。
弹性体聚合物也包括乙烯和至少一种诸如醋酸乙烯酯、不饱和脂族单羧酸以及这类单羧酸的酯之类的乙烯基单体的共聚物。弹性体共聚物和从这些弹性体共聚物制造弹性体非织造纤网的方法公开在,例如,美国专利4803117。
热塑性共聚物弹性体包括具有下述通式的共聚醚酯:式中,“G”选自聚(氧乙烯)-α,ω-二醇、聚(氧丙烯)-α,ω-二醇、聚(氧四亚甲基)-α,ω-二醇;“a”和“b”为正整数,包括2、4和6;m、n为包括1~20的正整数。这些材料一般具有,断裂伸长约600%~750%,按ASTM D-638测定,熔点约350°F~约400°F(176~205℃)、按ASTM D-2117测定。这类共聚酯材料的市售实例是,例如,以前由Akzo Plastics(Amhem,荷兰)出品的、现在由DSM(Sittard,荷兰)出品的称为ARNITEL者,杜邦公司(特拉华州、威尔明顿)出品的称为HYTREL者。以聚酯弹性体材料制造弹性体非织造纤网的方法公开在,例如,Morman等的美国专利4741949和Boggs的美国专利4707398中,特此引入作为参考。
用于薄膜和纤维生产的上述常规弹性体是非聚烯烃类,同时还需要将加工助剂加到弹性体聚合物中。例如,可以将聚烯烃加工助剂与弹性体共聚物(例如:弹性体嵌段共聚物)共混,以便改善组合物的加工性能。聚烯烃必须是,在共混并经受适宜组合的高压高温条件时,能以与弹性体聚合物共混物的形式挤出者。有用的共混用聚烯烃材料包括,例如,聚乙烯、聚丙烯和聚丁烯,包括乙烯共聚物、丙烯共聚物和丁烯共聚物。特别有用的聚乙烯可以得自U.S.I化学公司,商品名为Petrothene NA601(本文也称为PE NA601或聚乙烯NA601)。可以使用两种或多种聚烯烃。弹性体聚合物和聚烯烃的可挤出的共混物公开在,例如,美国专利4663220中。为了从前述非聚烯烃弹性体成功地生产薄膜和熔喷纤维,至今仍需要加工助剂。不幸的是,诸如NA601的加工助剂对底基弹性体的滞后性有不良影响。
本发明者发现,通过除去本领域技术人员以前认为必需的加工助剂,而加入其他种类的聚合物或弹性体,可以达到滞后性的大幅度改善。新一类弹性体的多分散性数值很低或很窄,例如:Mw/Mn为4或更低,其可以通过采用称为茂金属工艺的方法制备。这类聚合物有时称为茂金属催化聚合物。
茂金属聚合法一般使用由共催化剂活化即离子化的催化剂。
茂金属法催化剂包括二氯化双(正丁基环戊二烯基)合钛、二氯化双(正-丁基环戊二烯基)合锆、氯化双(环戊二烯基)合钪、二氯化双(茚基)合锆、二氯化双(甲基环戊二烯基)合钛、二氯化双(甲基环戊二烯基)合锆、二茂钴、三氯化环戊二烯基钛、二茂铁、二氯化二茂铪、二氯化异丙基(环戊二烯基,-1-芴)合锆、二氯化二茂钼、二茂镍、二氯化二茂铌、二茂钌、二氯化二茂钛、氯化氢化二茂锆、二氯化二茂锆,等。这类化合物的更详尽的一览表包括在Rosen等的、转让给Dow化学公司的美国专利5374696中。Stevens等的也转让给Dow的美国专利5064802也详述了这类化合物。
茂金属聚合方法,特别是催化剂和催化剂载体系统是许多专利的主题。Kaminsky等的美国专利4542199叙述了一种生产过程,其中,将MAO加到甲苯中,加入通式为(环茂二烯基)2Me RHal的茂金属方法催化剂,其中Me是过渡金属元素,Hal是卤素,R是环戊二烯基或C1~C6烷基或卤素,然后加入乙烯形成聚乙烯。LaPointe等的转让给Dow化学公司的美国专利5189192叙述了一种经金属中心氧化作用制备加聚反应催化剂的方法。Exxon Chemical Patents的美国专利5352749叙述了一种在流化床中使单体聚合的方法。美国专利5349100叙述了手性茂金属化合物及其制备,该法包括:由异构对映选择性氢化物转移而形成手性中心。
共催化剂是诸如最普通的甲基铝氧烷(MAO)等材料,还有其他烷基铝和含硼化合物如三(五氟苯基)硼、锂四(五氟苯基)硼、和二甲基苯铵四(五氟苯基)硼。因为加工和产品污染问题,正继续进行关于其他共催化剂体系或减少甚至去除烷基铝的可能性的研究工作。重要的是将茂金属催化剂活化或离子化成阳离子的形式,以便与聚合单体进行反应而聚合。
采用茂金属方法生产聚合物的独特优点是其分子量范围很窄。茂金属所生产的聚合物多分散性数值(Mw/Mn)能够为4以下,甚至在2以下。与其他的齐格勒-纳塔生产的相似类型聚合物比较,这些聚合物还具有受控短链支化分布。
还能够做到的是,当使用立构有择催化剂时,采用茂金属方法催化剂体系能够相当精密地控制聚合物的全同立构规整度。事实上所生产的聚合物的全同立构规整度已经超过了99%。还能够采用该体系生产间同立构高的聚丙烯。
控制聚合物全同立构规整度,结果也能生产在整个聚合物链长中交替含有全同立构嵌段和无规立构嵌段材料的聚合物。这种结构借助于无规立构部分得到了弹性聚合物。这种聚合物的合成详述于科学(Science)杂志,第267卷(1995年1月13日),第191页,K.B.Wagner的论文中。Wagner,在讨论Coates和Waymouth的工作时,解释了催化剂在各个立体化学结构之间摆动,结果,聚合物链具有连接到无规立构中心的连续长度(running length)上的全同立构规整中心的连续长度。全同立构占优势被减少产生弹性。Geoffrey W.Coates和Robert M.Waymouth,在与上述相同期刊中第217页发表的论文题为“摆动立构控制:合成热塑性弹性体聚丙烯的关键”中,讨论了他们的工作,在工作中,他们使用了在甲基铝氧烷(MAO)存在下的二氯化茂金属双(2-苯基茚基)-锆,通过改变反应器的压力和温度,使聚合物结构在全同立构和无规立构之间摆动。
通过茂金属方法大规模生产聚合物多少受到限制,但正在增长。这类聚合物可得自Exxon化学公司(得克萨斯州、贝敦),聚丙烯基聚合物商品名为ACHIEVETM,聚乙烯基聚合物商品名为EXACTTM和EXCEEDTM。Dow化学公司(密歇安州、米德兰)的市售聚合物商品名为AFFINITYTM和ENGAGETM。Exxon一般称他们的茂金属催化剂工艺为“单一点”(Single Site)催化剂,而Dow称其为“受限构型”(constrained geometry)催化剂,名为INSIGHTTM,以便将其与具有多个反应点的齐格勒-纳塔催化剂相区分。其他生产商,如Fina Oil、BASF、Amoco、Hoechst和Mobil,在本领域中的活动活跃,相信,今后十年按照该工艺生产的聚合物的可得性将大大增长。在实施本发明中,优选诸如聚丙烯和聚乙烯之类的弹性聚烯烃。
关于以茂金属方法为基础的弹性体聚合物,Kaminsky等的美国专利5204429叙述了一种使用立构刚性手性二茂过渡金属化合物和铝氧烷催化剂可以从环烯和直链烯烃生产弹性共聚物的方法。聚合反应在诸如脂肪族或脂环族烃如甲苯的惰性溶剂中进行。也可以应用待聚合的单体作溶剂在气相中进行反应。均为Lai等人的并转让Dow化学公司的美国专利5278272和5272236,题目“基本为线型的烯烃弹性聚合物”,叙述了具有特殊弹性的聚合物。
另外,可以将相容的增粘树脂加入到上述可挤出的组合物中,以便提供自动粘合的粘性材料。当将各层结合成层合制品时增粘剂也助于粘合,这样改善了层合制品和由这些层合制品制造的产品在使用期间的耐久性。能够应用任何与聚合物相容的可经受高加工(例如挤出)温度的增粘剂。如果聚合物与加工助剂共混,例如聚烯烃或增量油,增粘剂树脂也应与这些加工助剂相容。一般,优选氢化烃类树脂作增粘剂,因为它们具有较好的温度稳定性。氢化烃树脂的实例是REGALREZ和ARKONP系列增粘剂。萜烯烃的实例是ZONATAC501lite。REGALREZ烃类树脂由Hercules公司出品。ARKONP系列树脂由Arakawa化学公司(美国)出品。诸如美国专利4787699公开的增粘树脂是适用的,特此引入作为参考。也能够使用与组合物的其他组合相容的、能经受高加工温度的其他增粘树脂。
也能将少量其他物质与按照本发明生产纤维层所使用的聚合物共混;例如提高化学防护性的氟代烃,其可以是,例如美国专利5178931所述的任何物质;阻燃剂、改进耐紫外辐射的化学品和赋予各层相同或不同颜色的颜料。纺粘和熔喷热塑性聚合物用的阻燃剂和颜料是本领域已知的,并且它们是内添加剂。颜料,例如TiO2,如果使用,一般存在量为该层的5%(重量)以下,而其他物质累积存在量为25%(重量)以下。
改进耐紫外辐射的化学品可以是,例如,受阻胺和其他市售的化合物。受阻胺详述在Hudson的美国专利5200443,这类胺的实例是American Hoescht公司(新泽西州,萨默维尔)出品的Hostavin TMN20、Ciba-Geigy公司(纽约州、霍索恩)出品的Chimassorb944FL、Amcrieam Cyanamid公司(新泽西州,韦恩)出品的Cyasorb UV-3668以及Enichem Americas公司(纽约)出品的Uvasil-299。
本发明的织物也可以含有施加其上的后处理剂,以赋予更特殊的功能。这些后处理剂及其施加方法在本领域中是已知的,包括,例如,斥醇处理剂、抗静电剂等,施加方法包括喷洒、浸渍等。这类后处理的实例是施加Zelec抗静电剂(由特拉华州威尔明顿的杜邦公司出品)。
为了测定可归因于窄多分散性聚合物共混物的改善滞后的情况,对于许多含有和不含有窄多分散性聚合物的层合物进行了试验。实例1不是本发明的实例,而实例2和3是。
实例1
将弹性体聚合物的共混物的熔融薄膜夹在两层颈缩纺粘织物中间,纺粘织物由Shell化学公司(得克萨斯州、休斯敦)出品的名为E5D47的聚丙烯聚合物制造,其单位重量为1.2osy(41gsm)。纺粘层均从其未拉伸长度延伸约22%。
薄膜由包含下述物质(以重量计)的共混物制造,包括63%Shell化学公司的KratonG-1659、17%Regalrez1126增粘剂、20%NA601低分子量聚乙烯加工助剂、0.15%Ciba-Geigy公司出品的称为B900的抗氧剂,以及5000ppm Quantum化学公司(Cincinnati,OH)出品的称为Microthene FA-709的隔离剂。薄膜的单位重量为1.65osy(56gsm)。薄膜挤出温度为约440°F(227℃)。
将三层层合制品经具有固定辊隙为0.030英寸(0.76mm)的夹辊之间拉出,以便随着薄膜冷却和固化,使薄膜接触并粘合到纺粘层上。
测试30%伸长下的层合制品的滞后性,其结果示于表中。
实例2
将弹性体聚合物共混物的熔融薄膜夹在两层颈缩纺粘织物中间。纺粘织物由与实例1相同的聚合物制造,纺粘层均从其未拉伸长度延伸与实例1大约相同的数值。
薄膜由包含下述物质(按重量计)的共混物制造,包括69%Shell化学公司的KratonG-1659,14%Regalrez1126增粘剂、17%Exxon的EXACT4038高分子量茂金属催化的线型低密度聚乙烯、0.15%抗氧剂、5000ppm Microthene FA-709隔离剂。薄膜的单位重量为1.4~1.55osy(47~53gsm)。在不同的薄膜层合温度下,约440°F(227)和约460°F(238),制造该材料的两个样品。
将三层层合制品经具有固定辊隙为0.030英寸的夹辊之间拉出,以便随着薄膜的冷却和固化,使薄膜接触并粘合到纺粘层上。
测试30%伸长下的层合制品的滞后性,其结果示于表中。
实例3
将弹性体聚合物共混物的熔融薄膜夹在两层颈缩纺粘织物中间。纺粘织物由与实例1相同的聚合物制造,纺粘层均从其未拉伸长度延伸与实例1大约相同的数值。
薄膜由包含下述物质(按重量计)的共混物制造,包括69%Shell化学公司的KratonG-1659,17%Regalrez1126增粘剂,20%Dow的AFFINITYPL1880高分子量茂金属催化的线型低密度聚乙烯、0.15%抗氧剂、和5000ppm Microthene隔离剂。薄膜的单位重量为1.4~1.55osy。在不同的薄膜层合温度下,约440°F(227℃)和约460°F(238℃),制造该材料的两个样品。
将三层层合制品经具有固定辊隙为0.030英寸的夹辊之间拉出,以便随着薄膜的冷却和固化,使薄膜接触并粘合到纺粘层上。
测试30%伸长下的层合制品的滞后性,其结果示于表中。
表
实例1 实例2 实例3温度 440°F 440°F 460°F 440°F 460°F比例 4.25 3.22 3.57 3.89 3.54改善,% - 32 19 9 24
于是,可见,去除低分子量聚乙烯加工助剂,而使用高分子量窄分散性的聚烯烃弹性体能够大幅度改善滞后性。除实例3,440°F之外均显示出,与使用加工助剂的相似层合制品比较,滞后改善15%以上,尽管是这大概是由于440°F不是最佳加工温度。
按照本发明制造的复合弹性材料可以用于衣服、防感染制品和个人护理用品。具体地说,可以将这类材料用作这类需要弹性性能的物品的部件。这些部件包括,例如,手术服和工作服的肘部和裤脚管;腰部分和腕带或袖口;尿布、运动裤、吸湿内裤和成人失禁用品的“弹性耳”(Stretch ears)、外罩、侧嵌片和密闭折翼;和床上用品等。
虽然上文详述了本发明的几个典型实施方案,但是对本领域技术人员来说,显而易见,在实质上不脱离本发明的新颖内容和优点的条件下,能够对典型实施方案进行许多变换。因此,所有这些变换均包括在以下权利要求所限定的本发明范围之中。在权利要求书中,方法和功能方面的权利要求是意在用来包括本文所述的完成所列功能的结构,不仅包括结构等价物,而且也包括等价结构。例如虽然钉子和螺钉不是结构等价物,因为钉子利用圆柱表面把木质零件固定在一起,而螺钉利用螺旋表面进行固定,但就固定木质零件而言,钉子和螺钉是等价结构。
Claims (20)
1.一种具有改善的滞后性的复合弹性材料层合制品,其包含至少在一面上被粘合到非弹性材料层上的弹性材料层;其中所述弹性材料层包含窄多分散性数值的聚合物和常规弹性体的共混物;和其中所述共混物基本不含低分子量聚乙烯加工助剂。
2.权利要求1的复合材料,其中所述复合弹性材料层合制品的滞后性,比不含所述窄多分散性数值的弹性体、而含有所述加工助剂制成的相似层合制品,好至少15%。
3.权利要求1的材料,其中所述共混物还包含增粘剂。
4.权利要求1的材料,其中所述非弹性材料选自微纤维、长丝排列、泡沫体、粘合机梳纤网和共成型纤网。
5.权利要求1的材料,其中所述弹性材料选自微纤维、长丝排列、泡沫体和薄膜。
6.权利要求1的材料,其中所述的窄多分散性的弹性体是聚乙烯。
7.权利要求1的材料,其中所述常规聚合物选自聚氨酯、共聚醚酯、聚酰胺聚醚嵌段共聚物、乙烯醋酸乙烯酯(EVA)、通式为A-BA′或A-B的嵌段共聚物如共聚(苯乙烯/乙烯-丁烯)、苯乙烯-聚(乙烯-丙烯)-苯乙烯、苯乙烯-聚(乙烯-丁烯)-苯乙烯、(聚苯乙烯/聚(乙烯-丁烯)/聚苯乙烯和聚(苯乙烯/乙烯-丁烯/苯乙烯)。
8.权利要求1的层合制品,其是由选自颈缩粘合、拉伸粘合、颈缩拉伸粘合和零应变拉伸粘合的方法制备的。
9.包含权利要求1的层合制品的衣服。
10.包含权利要求1的层合制品的防感染用品。
11.包含权利要求1的层合制品的用于个人护理用品的外罩。
12.包含权利要求1的层合制品的用于个人护理用品的袖口。
13.包含权利要求1的层合制品的用于个人护理用品的弹性耳。
14.包含权利要求1的层合制品的用于个人护理用品的侧嵌片。
15.包含粘合同时颈缩到弹性材料层上的非弹性材料的层合制品,所述弹性材料层包含约62%~约80%(重量)常规弹性体和约10%~约30%(重量)的窄多分散性数值的聚烯烃弹性体的共混物,其中所述共混物基本不含低分子量聚乙烯加工助剂,并且其中,所述层合制品的滞后性,比不具有所述窄多分散性数值的聚烯烃弹性体而具有所述加工助剂制成的相似层合制品,好至少15%。
16.权利要求16的材料,其中所述非弹性材料选自微纤维、长丝排列、泡沫体、粘合机梳纤网和共成型纤网。
17.权利要求16的材料,其中所述弹性材料选自微纤维、长丝排列、泡沫体和薄膜。
18.权利要求16的材料,其中所述窄多分散性弹性体是聚乙烯。
19.一种颈缩粘合层合制品,其包含粘合同时颈缩到弹性薄膜层上的非弹性微纤维纤网材料层,所述薄膜包含约62%~约80%(重量)常规弹性体和约10%~约30%(重量)的窄多分散性数值的聚烯烃弹性体的共混物,其中所述共混物基本不含低分子量聚乙烯加工助剂。
20.权利要求19的层合制品,其中,所述层合制品的滞后性,比不具有所述窄多分散性数值的聚烯烃弹性体而具有所述加工助剂制成的相似层合制品,好至少15%。
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-
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- 1997-09-04 CN CN97198735A patent/CN1096933C/zh not_active Expired - Lifetime
- 1997-09-04 CA CA002264669A patent/CA2264669C/en not_active Expired - Lifetime
- 1997-09-04 DE DE69727147T patent/DE69727147T2/de not_active Expired - Lifetime
- 1997-09-04 EP EP97940792A patent/EP0930967B1/en not_active Expired - Lifetime
- 1997-09-04 WO PCT/US1997/015539 patent/WO1998016379A1/en active IP Right Grant
- 1997-09-04 AU AU42490/97A patent/AU712783B2/en not_active Expired
- 1997-09-04 KR KR10-1999-7003110A patent/KR100451880B1/ko not_active IP Right Cessation
- 1997-09-30 CO CO97056945A patent/CO5040243A1/es unknown
- 1997-10-09 AR ARP970104672A patent/AR011249A1/es active IP Right Grant
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1950555B (zh) * | 2004-04-30 | 2010-05-05 | 金伯利-克拉克环球有限公司 | 弹性层压材料及其制备方法 |
Also Published As
Publication number | Publication date |
---|---|
BR9712229A (pt) | 1999-08-31 |
AU712783B2 (en) | 1999-11-18 |
AU4249097A (en) | 1998-05-11 |
KR20000049041A (ko) | 2000-07-25 |
EP0930967A1 (en) | 1999-07-28 |
WO1998016379A1 (en) | 1998-04-23 |
DE69727147D1 (de) | 2004-02-12 |
EP0930967B1 (en) | 2004-01-07 |
US5853881A (en) | 1998-12-29 |
CO5040243A1 (es) | 2001-05-29 |
AR011249A1 (es) | 2000-08-16 |
DE69727147T2 (de) | 2004-11-25 |
KR100451880B1 (ko) | 2004-10-08 |
CN1096933C (zh) | 2002-12-25 |
CA2264669C (en) | 2006-11-21 |
CA2264669A1 (en) | 1998-04-23 |
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