CN1117904C - 柔软吸收性薄纸产品 - Google Patents
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- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
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Abstract
胺-改性聚硅氧烷被施涂到薄纸产品的彼此相对外表面,如3-层搽面纸的2个外表面上,从而改善该表面的柔软和疏水程度,以防止使用期间液体湿透。然而,疏水程度通过胺-改性聚硅氧烷的化学结构和/或胺-改性聚硅氧烷与较为亲水的改性聚硅氧烷的掺混予以控制,以便使液体仍旧能够在合理短的时间内进入薄纸结构从而被中间层吸收,但该吸水性与其他外表面疏水性的联合作用却大大延缓了液体完全透过薄纸产品的进程。
Description
发明背景
在包括搽面纸及浴巾纸的薄纸产品制造中,为改善触觉特性业内人士已做了相当大的努力来满足消费者对“柔软”薄纸的需求。借助化学添加剂改善薄纸的柔软度有2种主要方法。第1,有一类化学柔软剂,可在成形前加入到配料中以降低原纸(base sheet)的挺度和/或提供改善的表面触觉特性。第2,有一类化学品,可在纸页成形之后施涂到薄纸表面以提供改善的表面感觉。
然而,除了柔软之外,还希望搽面纸和浴巾纸具有的另一项属性是使用期间使手受到保护的能力。鉴于柔软和手保护功能都是薄纸消费品应具备的消费者要求的重要品质,因此需要一种能提供这2种属性的单一化学体系。
发明概述
现已发现,以1种或多种适当胺-改性聚硅氧烷局部处理的多层薄纸原纸,依靠改善表面感觉和降低原纸挺度这2种机理,可生产出更为柔软的纸,同时通过控制疏水与吸水性,又使之足以提供使用期间的手保护。胺-改性聚硅氧烷优选位于施涂该改性聚硅氧烷的薄纸层的外表面,从而依靠氢键键合或静电吸引或者其他化学相互作用为该表面提供柔软的优点并提供一定程度疏水或疏液性。然而,当液体一旦透入薄纸的外表面,该液体将很快被居中的、未处理的薄纸部分所吸收并沿薄纸的x-y平面芯吸散开(wick away)。与此同时,胺-改性聚硅氧烷在背面的存在,延缓了液体朝薄纸以外的进一步渗透,从而将该液体基本上围困在薄纸的中心层内。此种“单向阀”效应在正常使用期间可保护使用者的手免遭打湿,与此同时,提供柔软的优点。此种柔软、抗液性和吸水性的组合是独特和有利于消费者的。
然而,并非所有胺-改性聚硅氧烷都适合本发明的目的。必须赋予薄纸表面以亲水性与疏水性之间恰当的平衡,方能既充分延缓液体的渗透,又允许其足够快地透入以便薄纸内层部分将液体吸收。所要求的平衡可通过改变1项或多项下列因素以提高或降低疏水性来达到:(1)可提高胺-改性聚硅氧烷的分子量以提高疏水性,而降低,则提高亲水性;(2)可改变胺-改性聚硅氧烷中胺官能团的摩尔百分数,以提高或降低疏水性;(3)可提高施涂到薄纸表面的胺-改性聚硅氧烷的施涂量,以提高疏水性;以及(4)可将胺-改性聚硅氧烷与较为亲水的材料,例如像聚醚-改性聚硅氧烷之类的改性聚硅氧烷,彼此掺混以降低疏水性。通过对这些因素的权衡,化学技术专业人员将能够获得满足本发明薄纸性能的胺-改性聚硅氧烷及改性聚硅氧烷的共混物。
因此,本发明一方面在于一种有2或更多层的柔软薄纸产品,所述薄纸产品的MD模量(定义见下文)为约30kg或更低;浸润面积(WetOut Area)(定义见下文),约2平方英寸或更高;且湿透时间(WetThrough Time)(定义见下文),约15s或更长。此种薄纸具备柔软度(按MD模量衡量)与吸水性(按湿透时间及浸润面积衡量)之间的恰当平衡,从而可保护使用者以使其在使用期间手不接触液体。
更具体地说,本发明在于一种有2或更多层且2个朝外表面经过以胺-改性聚硅氧烷局部处理的柔软薄纸产品,所述薄纸产品的MD模量为约30kg或更低;浸润面积,约2平方英寸或更高,且湿透时间,约15s或更长。
更具体地说,浸润面积可为约3平方英寸或更高,更具体地说约4平方英寸或更高,进一步具体地说约2平方英寸~6平方英寸。还有,更具体地说,湿透时间可为约20s或更长,更具体地说约30s或更长,更具体地说约45s或更长,进一步具体地说约15s~60s。再者,更具体地说,MD模量可为约20kg或更低,更具体地说约5~约20kg。
本发明另一方面在于一种制造柔软、吸水性受控、多层薄纸产品的方法,包括:a)制备造纸纤维的水悬浮体;b)将纤维水悬浮体沉积到成形织物上以形成纸幅;c)干燥该纸幅以形成薄纸纸页;d)将该薄纸纸页与1层或多层类似的薄纸纸页合并成一个具有2个外表面的多层薄纸原纸以及(e)以胺-改性聚硅氧烷的水悬浮液体对薄纸表面的2个外表面进行局部处理以制成薄纸产品,使所述薄纸产品的浸润面积为约2平方英寸或更高,且湿透时间为约15s或更长。
本文所使用的术语“MD模量”是薄纸片材柔软性的度量,它是样品在70~157g载荷与相对伸长百分率的各点之间“最小二乘法直线”的斜率。MD模量数值系采用传统抗张强度试验仪(例如,Sintech/2电脑一体化测试系统)获得的。以模切机将单层搽面纸沿纵向裁成3英寸宽。试样长度应超出夹持长度(抗张试验机2个夹具之间的距离)至少2英寸。试样不应有任何撕裂或皱褶并应具有清晰、平行的边缘。打开抗张试验机夹具并将试样放在夹具之间,捋直并对中。合上夹具以将试样夹牢并按试验设定值进行仪器的初始化。样品以1/3正常试验速度(10英寸每分钟)接受拉伸。当试验载荷达到满载荷量程的0.5%时测量伸长值,以此作为对试样中可能存在任何松懈的校正。此刻,滑动横梁改变速度,并以正常速度继续拉伸。收集数据,直至达到峰值载荷以及载荷降低到该峰值载荷65%时。合适的抗张试验机可由Sintech公司(P.O.Box 14226,科研三角园区,NC 27709-4226)获得。
下面,将结合附图详细说明“湿透时间”及“浸润面积”的测定方法。
本发明薄纸产品可具有2层、3层、4层或更多层。优选3层的产品,因为这样,2个外层每个的朝外表面便于按照本发明以改性聚硅氧烷分别处理。所形成的3-层产品具有2个柔软、疏液外表面和一个内部吸收剂层。这使得液体不仅被内部层吸收,而且被围困在层间的空间内,从而进一步减少使用期间使用者遭遇薄纸湿透的可能。特别合适的薄纸产品包括搽面纸、浴巾纸、厨房毛巾(Kitchen towels)之类。该产品宜于采用传统造纸纤维制造。各单独层可以是层合的或均质的,湿压榨或穿透干燥的。
适合用于本发明目的的胺-改性聚硅氧烷材料具有下列通式:
其中x和y是大于0的整数。x对(x+y)的摩尔比可介于0.005%-约25%。R1-R9部分可以是C1或更高级烷基取代基。另外,R2和R5可以是羟基或者C1或更高级烷基醇取代基。优选的R1-R9部分包括C1-C4。R10部分可包括任何与胺有关的官能团或者诸如胺、亚胺和/或酰胺之类的基团。
例如,胺-改性聚硅氧烷可以是这样的聚硅氧烷,其中R10部分包含1个胺基团每个取代基,或者2或更多个胶基团每个取代基,其间由等于或大于C1的线形或支链烷基链隔开。
其中x和y是大于0的整数。x对(x+y)的摩尔比可介于0.005%-约25%。R1-R9部分可以是C1或更高级烷基取代基。另外,R2和R5可以是羟基或C1或更高级烷基醇取代基。优选的R1-R9部分包括C1-C4。R11是包含1种或多种选自醚、聚醚、酯、胺、亚胺、酰胺的官能团及此类官能团的烷基及链烯基类似物的C1或更高级烷基链。
作为例子,R11部分可以是通式为-R12-(R13-O)a-(R14-O)b-R15的聚醚官能团,其中R12、R13及R14是C1或更高级烷基链,R15可以是氢或C1-C4烷基基团,“a”和“b”可以是1-100,尤其是10-30的整数。
胺-改性聚硅氧烷的粘度范围,作为其分子量的标示,可介于约25cp-约2,000,000cp或更高,更具体地说约100-约1,000,000cP。
适合用于将改性聚硅氧烷施涂到薄纸表面上的方法包括喷涂、印剧成涂布。优选凹印法,因为它可提供对薄纸表面上施涂量的控制。改性聚硅氧烷在薄纸表面上的施涂量将取决于具体使用的改性聚硅氧烷。然而,合适的施涂量,以薄纸产品的干重为基准介于约0.1-约5wt%,更具体地说约0.5~约3wt%,进一步具体地说约0.7~约2wt%。优选的是,首先以合适的表面活性剂将改性聚硅氧烷乳化在水中,然后再将乳液施涂到薄纸表面上。尽管改性聚硅氧烷择优地留在它施涂上去的薄纸表面上,但聚硅氧烷固有的迁移性将使得就连3-层薄纸产品的中间层也可能包含一定的硅氧烷材料。但是,该数量远低于薄纸外表面上的数量,因此中间层依旧保持为基本亲水并可芯吸或吸收液体。
为进一步优化及平衡改性聚硅氧烷处理的柔软、手保护与吸水性,可在薄纸表面施涂2或更多种改性聚硅氧烷材料的共混物。在一种具体实施例中,可采用疏水胺-改性聚硅氧烷与亲水聚醚-改性聚硅氧烷的共混物来调节最终薄纸产品的湿透时间。胺-改性聚硅氧烷对聚醚-改性聚硅氧烷的比例可介于100%~约10%,更具体地说100%~约50%。
熟悉聚合物技术的人将懂得,可改变--每一种改性聚硅氧烷种类的分子量(粘度)、取代度、各R基团具体选择的种类及其链长,“X”与“Y”成分之间的摩尔比,乃至2或更多种改性聚硅氧烷种类之间的掺混--以影响准备施涂到薄纸表面上的改性聚硅氧烷的疏水性,从而达到本发明要求的湿透时间及浸润面积。
附图简述
图1是,如下文所述,用于测定湿透时间及浸润面积的设备示意图。
图2是图1所示样品盖板的平面视图。
图3是表示本发明薄纸与某些其他薄纸的湿透时间比较的直方图。
图4是表示本发明薄纸与图3其他薄纸的浸润面积比较的直方图。
附图详述
参照附图,下面将说明湿透时间和浸润面积的测定方法。大致地说,该方法涉及将计量数量的染色液放在薄纸样品的上表面,并测量液体透过样品从而将位于薄纸底下的湿敏传感器激活所需要的时间。该时间便是湿透时间。此刻,将观察到,染色液已沿薄纸的x-y方向芯吸达及的范围呈圆形或椭圆斑。该斑点的面积即为浸润面积。
图1示意地表示用于实施上述程序的设备配置。图中可见到湿敏传感器1,坐落在平坦表面上并连接到受潮指示灯2上。(具体的湿敏传感器是Cole-Parmer液体敏感控制器77096-00,由Barnant公司(Barrington,伊利诺斯)制造及Cole-Parmer Liqui-Sense Sensor77095-00)。根据制造商说明,将湿敏传感器的灵敏度标定到对应于0.2mL试验液(如下面所述)。薄纸样品3,已对折并放在湿敏传感器上面,以2个exan侧向重物4和5夹牢在湿敏传感器的2个侧面。每个侧向重物的断面尺寸为3/4英寸×1/4英寸,长4英寸。放置这2个重物时,应使得折叠薄纸样品平展地抵住湿敏传感器的表面但不受张力。在样品的上表面放置4英寸×4英寸×1/2英寸exan样品压盖6,如图2更详细的表示的。样品压盖带有贯通中心的锥形孔7,其上表面直径为3/8英寸,下表面直径为1/16英寸。由于湿敏传感器的厚度略薄于侧向重物的1/4英寸厚度,故而样品夹具基本上坐落在侧向重物上。
位于样品压盖上方的是摄像机8(JVC TK-1070U彩色摄像机,日本JVC制造)。摄像机的输出连接到盒式录像机9(松下AG-1960Proline,松下工业公司(Secaucus,新泽西)总经销)以及彩色监视器10上。调整摄像机在三角架上的位置,以便将受潮指示灯2纳入摄像机视野以内。
试验所使用的试验液是Hercules Size Tester Green Dye,由Hercules公司(Wilmington,特拉华)供应。在22℃下测定的试验液性质如下:粘度,10cp,测定时采用Brookfield Synchro-lectric粘度计,型号RVT,1号转子,速度50rpm;表面张力,60.5dyn/cm,测定采用duNouy圆环张力仪(Fisher科学表面张力仪20);pH,7.3;比电导,18μS/cm。
为实施测定湿透时间和浸润面积的试验,图像被调节到使样品盖板在监视器上的影像为6英寸X6英寸的大小。液敏控制器装置被放在,从监视器屏幕能清楚地看到报警灯(受潮指示灯)的位置。待测薄纸产品的样品,对折后放在湿敏传感器上表面,以侧向重物夹牢,并盖上样品盖板,如上面图示和说明那样。启动盒式磁带录像机。采用微型吸移管,将0.5mL试验液置于样品压盖的孔5中,并开始试验计时。到潮湿监视器报警灯激活时所经过的时间,以秒计,即为该样品的湿透时间。此后,停下盒式磁带录像机。利用断续慢放功能,将图像调节到报警灯启动报警的那一帧,于是该帧图像显示出染色液形成的斑点大小。此刻屏幕上染色图像的面积,以平方英寸为单位,即为浸润面积。由于染色图像通常呈椭圆形,该面积可通过测量椭圆的长、短轴并计算面积来确定。然而,如果希望获得更高精确度,不难看出,也可采用更为高级的图像分析技术来计算面积。
图3和4是表示下列实施例中制备的薄纸,及若干市售薄纸的湿透时间及浸润面积的直方图。如图所示,本发明的薄纸具有高拒水(湿透时间测定值较高)和高吸水性(浸润面积测定值较高)的独特组合。
实施例
实例1(对比例)。成品定量为22.7磅每2880平方英尺、配料由65%硬木和35%软木纤维组成的3-层薄纸幅,通过“同时轮转凹印法”在2面印刷上改性聚硅氧烷水乳液(FTS-226,Witco公司(Greenwich,CT)制造)。该改性聚硅氧烷水乳液包含约20wt%胺-改性聚硅氧烷、约20wt%聚醚-改性聚硅氧烷、约57wt%水、约2wt%乳化剂、约0.75wt%杀菌剂包(package)及将最终乳液pH调节到6.5~7.5范围内的少量缓冲剂。胺-改性聚硅氧烷的百分含量对聚醚-改性聚硅氧烷的百分含量之比是50/50。
凹印辊筒为铜辊筒基底,上面有电子雕刻的铬表面层,由Southern Graphics System(Louisville,肯塔基)供应。辊筒具有由360个着墨孔每线性英寸组成的线条网屏,容积为1.5千兆μm3(BCM)每平方英寸辊筒面积。该辊筒的典型着墨孔尺寸是65μm长、110μm宽及13μm深。橡胶涂墨砧辊为75 Shore A肖氏硬度的铸造聚氨酯,由美国辊筒公司(Union Grove,Wisconsin)供应。印刷过程被调整如下状态:凹印辊与橡胶砧辊的公盈(interference)为0.375英寸;2个彼此面对的砧辊之间的间隙为0.003英寸。该同时凹版胶印/胶印机以2000英尺每分钟的速度运转。该过程产生的总施涂量,以薄纸重量为基准为1.0wt%。
所获得的柔软薄纸产品具有2.4s的湿透时间和0.9平方英寸的浸润面积。MD模量为约16.54kg。
实例2(本发明)。按实例1所述制备薄纸产品,不同的是,改性聚硅氧烷水乳液(Y-14344硅氧烷乳液,来自Witco公司)为第1改性聚硅氧烷水乳液(Y-14264硅氧烷乳液,来自Witco公司)与第2改性聚硅氧烷水乳液(Y-14275硅氧烷乳液,来自Witco公司)的1∶1混合物。更具体地说,第1改性聚硅氧烷水乳液包含约32wt%胺-改性聚硅氧烷、约63.2wt%水、约3.2wt%乳化剂包、约0.75wt%杀菌剂包、约0.8wt%冻融稳定剂和将pH调节到6.5~7.5范围内的缓冲剂。第2改性聚硅氧烷水乳液含约24wt%胺-改性聚硅氧烷、约11wt%2种聚醚-改性聚硅氧烷的共混物、约61.2wt%水、约2.4wt%乳化剂包、约0.75wt%杀菌剂包、约0.6wt%冻融稳定剂和足以将pH调节到6.5~7.5范围内的缓冲剂。胺-改性聚硅氧烷的百分含量对聚醚-改性聚硅氧烷百分含量之比为84/16。
所获得的柔软薄纸产品具有22.8s的湿透时间和3.8平方英寸的浸润面积。MD模量为约14.18kg。
实例3(本发明)。按实例1所述制备薄纸产品,不同的是,改性聚硅氧烷水乳液(Y-14316硅氧烷乳液,来自Witco公司)为第1改性聚硅氧烷水乳液(Y-14264硅氧烷乳液,来自Witco公司)与第2改性聚硅氧烷水乳液(Y-14275硅氧烷乳液,来自Witco公司)的9∶1混合物。更具体地说,第1改性聚硅氧烷水乳液包含约32wt%胺-改性聚硅氧烷、约63.2wt%水、约3.2wt%乳化剂包、约0.75wt%杀菌剂包、约0.8wt%冻融稳定剂和将pH调节到6.5~7.5范围内的缓冲剂。第2改性聚硅氧烷水乳液含约24wt%胺-改性聚硅氧烷、约11wt%2种聚醚-改性聚硅氧烷的共混物、约61.2wt%水、约2.4wt%乳化剂包、约0.75wt%杀菌剂包、约0.6wt%冻融稳定剂和足以将pH调节到6.5~7.5范围内的缓冲剂。胺-改性聚硅氧烷的百分含量对聚醚-改性聚硅氧烷百分含量之比为97/3。
所获得的柔软薄纸产品具有31.7s的湿透时间和5.3平方英寸的浸润面积。MD模量为约17.24kg。
实例4(本发明)。按实例1所述制备薄纸产品,不同的是,改性聚硅氧烷水乳液包含约32wt%胺-改性聚硅氧烷、约63.8wt%水、约3.2wt%乳化剂包、约0.2wt%杀菌剂包、约0.8wt%冻融稳定剂。(Y-14240硅氧烷乳液,来自Witco公司)。胺-改性聚硅氧烷的百分含量对聚醚-改性聚硅氧烷百分含量之比为100/0。
所获得的柔软薄纸产品具有53.4s的湿透时间和4.6平方英寸的浸润面积。MD模量为约11.65kg。
实例5(市售薄纸)。按如上所述对Kleenex搽面纸(Kimberly-Clark公司)的样品进行试验。该薄纸的湿透时间为2.0s,浸润面积为1.1平方英寸。
实例6(市售薄纸)。按如上所述对KleenexCold Care带洗剂的搽面纸(3-层)样品进行试验。该薄纸的湿透时间为15.1s,浸润面积为1.3平方英寸。
实例7(市售薄纸)。按如上所述对Puffs柔软而结实的搽面纸样品进行试验。该薄纸的湿透时间为8.1s,浸润面积为1.0平方英寸。
实例8(市售薄纸)。按如上所述对Puffs高级超强搽面纸的样品进行试验。该薄纸的湿透时间为2.2s,浸润面积为1.2平方英寸。
实例9(市售薄纸)。按如上所述对Puffs Plus搽面纸的样品进行试验。该薄纸的湿透时间为6.8s,浸润面积为0.9平方英寸。
实例10(市售薄纸)。按如上所述对Scotties搽面纸(3-层)的样品进行试验。该薄纸的湿透时间为1.2s,浸润面积为0.8平方英寸。
应当指出,给出以上实施例的目的在于举例说明,不应构成对本发明范围的限制,本发明范围由后面的权利要求及其等价物规定。
Claims (14)
1、一种具有2或更多层的柔软薄纸产品,所述薄纸产品的MD模量为30kg或更低;浸润面积,2平方英寸或更高;湿透时间,15s或更长。
2、权利要求1的薄纸产品,还包含中间层。
3、权利要求1的薄纸产品,其中浸润面积为3平方英寸或更高。
4、权利要求1的薄纸产品,其中浸润面积为4平方英寸或更高。
5、权利要求1的薄纸产品,其中浸润面积为2-6平方英寸。
6、权利要求1的薄纸产品,其中湿透时间为20s或更长。
7、权利要求1的薄纸产品,其中湿透时间为30s或更长。
8、权利要求1的薄纸产品,其中湿透时间为45s或更长。
9、权利要求1的薄纸产品,其中湿透时间为15-60s。
11、权利要求10的薄纸产品,其中R10包含1个或多个胺基基团,其间由C1或更高级烷基链隔开。
13、权利要求12的薄纸产品,其中,R11具有通式 -R12-(R13-O)a-(R14-O)b-R15,其中R12、R13及R14是C1或更高级烷基链,R15是氢或C1-C4烷基基团,“a”和“b”是1-100的整数。
14、一种制造柔软、吸水性受控、多层薄纸产品的方法,包括:a)制备造纸纤维的水悬浮体;b)将纤维水悬浮体沉积到成形织物上以形成纸幅;c)干燥该纸幅以形成薄纸纸页;d)将该薄纸纸页与1层或多层的薄纸纸页合并成一个具有2个外表面的多层薄纸原纸;以及e)以胺-改性聚硅氧烷的水乳液对薄纸表面的2个外表面进行局部处理从而形成薄纸产品,使所述薄纸产品的浸润面积为2平方英寸或更高,且湿透时间为15s或更长。
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Application Number | Priority Date | Filing Date | Title |
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US09/012588 | 1998-01-23 | ||
US09/012,588 US6054020A (en) | 1998-01-23 | 1998-01-23 | Soft absorbent tissue products having delayed moisture penetration |
US09/012,588 | 1998-01-23 |
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CN1288497A CN1288497A (zh) | 2001-03-21 |
CN1117904C true CN1117904C (zh) | 2003-08-13 |
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CN99802297A Expired - Fee Related CN1117904C (zh) | 1998-01-23 | 1999-01-19 | 柔软吸收性薄纸产品 |
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US (1) | US6054020A (zh) |
EP (1) | EP1047838B1 (zh) |
JP (1) | JP2002501132A (zh) |
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CN (1) | CN1117904C (zh) |
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DE (1) | DE69932802T2 (zh) |
ES (1) | ES2270579T3 (zh) |
IL (1) | IL136311A (zh) |
PL (1) | PL341515A1 (zh) |
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- 1999-01-11 ZA ZA9900165A patent/ZA99165B/xx unknown
- 1999-01-15 TW TW088100559A patent/TW589428B/zh not_active IP Right Cessation
- 1999-01-19 WO PCT/US1999/001059 patent/WO1999037860A1/en active IP Right Grant
- 1999-01-19 BR BRPI9907182-7A patent/BR9907182B1/pt not_active IP Right Cessation
- 1999-01-19 AU AU22356/99A patent/AU737728B2/en not_active Ceased
- 1999-01-19 DE DE69932802T patent/DE69932802T2/de not_active Expired - Lifetime
- 1999-01-19 CN CN99802297A patent/CN1117904C/zh not_active Expired - Fee Related
- 1999-01-19 ES ES99902355T patent/ES2270579T3/es not_active Expired - Lifetime
- 1999-01-19 JP JP2000528758A patent/JP2002501132A/ja active Pending
- 1999-01-19 EP EP99902355A patent/EP1047838B1/en not_active Expired - Lifetime
- 1999-01-19 KR KR1020007008043A patent/KR100592004B1/ko not_active IP Right Cessation
- 1999-01-19 IL IL13631199A patent/IL136311A/en active IP Right Grant
- 1999-01-19 TR TR2000/02098T patent/TR200002098T2/xx unknown
- 1999-01-19 PL PL99341515A patent/PL341515A1/xx unknown
- 1999-01-20 CO CO99002864A patent/CO5040188A1/es unknown
- 1999-01-20 AR ARP990100217A patent/AR017229A1/es active IP Right Grant
- 1999-01-22 SV SV1999000005A patent/SV1999000005A/es unknown
- 1999-01-25 CR CR5958A patent/CR5958A/es not_active Application Discontinuation
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Also Published As
Publication number | Publication date |
---|---|
US6054020A (en) | 2000-04-25 |
DE69932802T2 (de) | 2007-01-18 |
KR100592004B1 (ko) | 2006-06-22 |
PL341515A1 (en) | 2001-04-23 |
CO5040188A1 (es) | 2001-05-29 |
IL136311A0 (en) | 2001-05-20 |
EP1047838B1 (en) | 2006-08-16 |
BR9907182B1 (pt) | 2010-02-23 |
IL136311A (en) | 2004-09-27 |
SV1999000005A (es) | 1999-08-18 |
ES2270579T3 (es) | 2007-04-01 |
TR200002098T2 (tr) | 2000-12-21 |
CR5958A (es) | 1999-11-18 |
AU2235699A (en) | 1999-08-09 |
TW589428B (en) | 2004-06-01 |
JP2002501132A (ja) | 2002-01-15 |
WO1999037860A1 (en) | 1999-07-29 |
AR017229A1 (es) | 2001-08-22 |
EP1047838A1 (en) | 2000-11-02 |
AU737728B2 (en) | 2001-08-30 |
BR9907182A (pt) | 2000-11-14 |
CN1288497A (zh) | 2001-03-21 |
KR20010034320A (ko) | 2001-04-25 |
DE69932802D1 (de) | 2006-09-28 |
ZA99165B (en) | 1999-07-12 |
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