CN101638561A - 用于结合印版的压敏胶带和提供它们的方法 - Google Patents
用于结合印版的压敏胶带和提供它们的方法 Download PDFInfo
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Abstract
本发明涉及压敏粘合剂在用于柔性印版和印刷辊筒或印刷套筒的结合的胶带中的用途,该压敏粘合剂包括至少一种树脂-聚合物共混物,其组成如下:至少50%重量的包括基于乙烯基芳族化合物的聚合物嵌段和基于1,3-二烯的聚合物嵌段的一种或多种嵌段共聚物,和不大于50%重量的至少一种增粘树脂。
Description
技术领域
本发明涉及制备压敏胶带,和这种压敏胶带(PSA带)结合印版的用途,所述压敏胶带包括至少一层压敏粘合剂(PSA),该压敏粘合剂在极性表面上具有非常低的剥离增加(peel increase)水平,易于重新定位,以及与印刷辊筒(printing cylinder)结合之后,表现出低的印版、固定剂版的胶带/印版组装件的边缘上翘(edge lifting)水平。
背景技术
在印刷产业中,已知有大量技术用于将图案例如通过印刷原件转印到纸上。一种可行的方法称为柔性版印刷。柔性版印刷的一种实施方式进而使用具有柔性下部结构(substructure)的多层光聚合物印版,这类印刷在相当一段时间已经成为现有技术的一部分。这些印版由多层各自具有特定功能的不同聚合物材料构成。例如,来自Flint Group公司的“Nyloflex ACE”印版具有至少两层,即光敏缓冲层(relief layer)和它下面的稳定化膜。
在柔性版印刷法中,柔性印版和印刷辊筒结合。这种粘结通常使用双面压敏胶带(PSA带)进行,对该胶带的有非常严格的要求。对于该印刷法,要求PSA带不仅具有一定硬度,而且还具有一定弹性。这些性质必须非常精确地设定,从而得到的印刷图像产生符合要求的期望的结果。对PSA还有一些其它严格的要求,其中结合强度必须同样足够高,以至于印版不与双面PSA带分开,或者PSA带不与筒体分开。即使在40~60℃的高温和相对高的印刷速度下也必须如此。然而,除了该性质之外,PSA还要求具有可逆的粘合性质,因为该印版通常多次使用,所以常常需要结合印版,然后将它们再次分开以便重新定位。即使对于相当长时间(高达6个月)后的粘结,这种可分开能力也应该存在;这里,印版应该能够毫无破坏地再次移去。此外,在印版或辊筒上应该没有残留物。
总之,对适合该应用的双面PSA带有非常严格的要求。
US 4,380,956描述了用于固定柔性版印刷法的印版的方法。该方法也使用PSA,但没有进行任何更详细的说明。
GB 1,533,431要求保护一种包括弹性体层的双面PSA带,所述弹性体层又通过易破的空气泡发泡。在柔性版印刷应用中该空气泡在压力下被破坏。
US 4,574,697要求保护一种双面PSA带,包括作为其载体材料固定到PET(聚对苯二甲酸乙二醇酯)膜的柔性聚氨酯泡沫。外层由PSA构成。据说所述PSA带为可逆的并且可以从印刷辊筒和印版移除。在EP0206760中描述了类似的产品结构。此处所用的柔性泡沫载体为聚乙烯泡沫。
类似于US 4,574,697,US 4,574,712描述了相似的PSA带结构。此处对PSA有限制,从而使得与印版和与印刷辊筒的结合强度应低于与载体膜和与载体泡沫的结合强度。
US 3,983,287描述了一种层合体,它的载体材料包括不可压缩的弹性体。可压缩性是通过在压力下被破坏并因此产生弹性的珠粒获得的。
US 5,613,942描述了特别适合在湿表面上结合的PSA带。另外据说该PSA带适于结合印版。
US 5,476,712同样描述了用于柔性版印刷法中的双面PSA带。该PSA带进而包括热塑性弹性体,在这种情况存在的结构是通过微粒膨胀产生的多孔结构(cellular structure)。
在上面提到的例子中,使用了大量不同的PSA。天然橡胶粘合剂在室温具有良好的粘性但剪切强度不大,并且由于在聚合物中存在的双键发生降解而老化。
为了结合印版(下文也称为版)和印刷辊筒,通常使用基于丙烯酸酯的粘合剂。这些粘合剂的优点是它们具有高的初始粘性且可以容易地再次卸下。然而,这些粘合剂的边缘上翘趋势增大。
在市场上,对于该应用还有基于苯乙烯嵌段共聚物的胶带,但这些胶带也表现出严重的边缘上翘,特别在使用厚度为2.54mm的厚版时尤其如此,具体地如长期印刷操作中遇到的情形。随着印版的厚度和硬度增加,边缘上翘增大。
边缘上翘的现象是实际上所有现有市售印版胶带已知存在的问题,且起因于柔性印版在与印刷辊筒的结合操作之后-和在该操作中不可避免地存在的变形-表现恢复至平坦面的倾向的事实。边缘上翘的倾向取决于一些参数,包括辊筒直径,印版的厚度和特性,印版边缘的存在,该印版边缘不用于印刷(并且其在此情况下是较薄的并表现出较低的恢复力);取决于在所述版边缘的印刷设计(如果印版在整个区域上印刷,则它通常具有最高恢复力);取决于固定到辊筒之前印版背面的清洁度(cleaning);取决于在结合过程中施加到印版的压力,以及取决于其它参数。
在同时使用两块或更多块印版时,对印版之间的间隙(通常是无缝结合)的要求变得更高,特别在将要制备其中看不到过渡变化的大规格印刷品时。柔性版印刷(即,使用印版的印刷)与诸如凹版印刷的其它方法的竞争加剧,因此前述要求变得更为重要。除了间隙必须变得更小(对于印刷图像更加不明显)的事实之外,还不再存在留下非印刷边缘的可能性。
印刷机试图通过采用两个或更多个工序(workstep)实施印刷过程来克服现有的这些问题,但这带来了相当的不便和额外的成本。
发明内容
本发明的目的是解决这种状况,提供的胶带即使在稍高温度下长期存放之后也不表现边缘上翘,可以容易地再次移除,而且还理想地允许具有有效的重新定位能力。
该目的令人惊讶地如以下用途所实现,该用途为压敏粘合剂在用于柔性印版和印刷辊筒或印刷套筒的结合的胶带中的用途,所述压敏粘合剂包括:至少一种树脂-聚合物共混物,其组成如下:至少50%重量的包括基于乙烯基芳族化合物的聚合物嵌段和基于1,3-二烯的聚合物嵌段的一种或多种嵌段共聚物,和不大于50%重量的至少一种增粘树脂。
附图说明:
图1示出了本发明PSA带的结构。
具体实施方式
使用包括聚合物-树脂共混物的粘合剂,该共混物具有高分率的嵌段共聚物(特别是大于50%重量)和低分率的树脂,所述嵌段共聚物是基于乙烯基芳族化合物的共聚物。
在最简单的形式下,该粘合剂可以仅由所述聚合物-树脂共混物获得;然而,在本发明粘合剂的拓展中,还可以加入其他添加剂和辅助剂。
这些胶粘剂仅具有中等结合强度,但没有显示与基板的剥离增加的倾向,因此容易重新定位。令人惊讶的是,配置本发明粘合剂的胶带展示出非常小的边缘上翘或根本没有边缘上翘。
使用的压敏粘合剂是基于嵌段共聚物的那些,该嵌段共聚物包含由乙烯基芳族化合物形成的聚合物嵌段(A嵌段),乙烯基芳族化合物如苯乙烯,以及由1,3-二烯的聚合形成的嵌段(B嵌段),1,3-二烯如丁二烯和异戊二烯或者丁二烯和异戊二烯的共聚物。优选还可以使用不同嵌段共聚物的混合物。进一步优选可以使用部分或全部氢化的产物。
使用的嵌段共聚物特别是可以具有线型A-B-A结构。也可以使用放射状的嵌段共聚物,还有星型嵌段共聚物和线型多嵌段共聚物。可以使用A-B二嵌段共聚物作为其他组分。根据本发明,使用不同结构的嵌段共聚物的混合物也具有出色的效果。
优选使用聚乙烯基芳族化合物含量至少为20%重量的那些嵌段共聚物。
作为本发明所用的压敏粘合剂的聚合物组分,能够使用并获得特别出色的效果的是苯乙烯-异戊二烯-苯乙烯嵌段共聚物(SIS)和/或苯乙烯-丁二烯-苯乙烯嵌段共聚物。
所用的增粘剂是与所述乙烯基芳族化合物嵌段共聚物的弹性体嵌段相容的增粘树脂。合适的增粘树脂包括基于松香和松香衍生物的非氢化、部分氢化或全部氢化的树脂,二环戊二烯的氢化或非氢化聚合物,基于C-5、C-5/C-9或C-9单体流的非氢化或部分、选择性或完全氢化的烃树脂,和/或基于α-蒎烯和/或β-蒎烯和/或δ-苧烯的氢化或非氢化聚萜烯树脂。可以单独使用或以混合物的形式使用上述增粘树脂。
嵌段共聚物的使用浓度在50%重量以上至75%,更具体地介于55%重量和65%重量之间的范围内,每种情况均基于树脂-聚合物共混物。相应有利的是,优选选择树脂的分率为25%~50%重量,非常优选分率为35%~45%重量。
特别是,可以用于所述压敏粘合剂并具有出色效果的其他添加剂为以下化合物:
·主抗氧化剂,如位阻酚
·辅助抗氧化剂,如亚磷酸酯或硫酯
·过程稳定剂(in-process stabilizer),如C-自由基清除剂
·光稳定剂,如UV吸收剂或位阻胺
·加工助剂
·端部封闭的增强剂树脂和
·在需要时,优选具有弹性体特性的其他聚合物,其中,相应有用的弹性体包括基于纯烃的那些,例如不饱和聚二烯,如天然或合成的聚异戊二烯或聚丁二烯;基本上化学饱和的弹性体,例如饱和的乙烯-丙烯共聚物、α-烯烃共聚物、聚异丁烯、丁基橡胶、乙丙橡胶,以及化学官能化的烃,例如,含卤素的、含丙烯酸酯的或含乙烯基醚的聚烯烃,上面仅仅是部分列举。
·无机填料,如白垩和/或硅酸盐。
本发明的压敏粘合剂体系的特征在于,它们满足所述的条件要求且特别具有以下优点:
·PSA带可多次反复使用的能力(重新定位能力),
·在不同表面上的可逆性,
·无残留地与基底可再分开的能力,
·甚至在极性表面上具有低的剥离增加,
·在结合到印刷辊筒上之后,具有最小化的边缘上翘,或者根本没有边缘上翘。
在本发明胶带的一种优选实施方式中,所述带至少包括载体层和在该载体层两面的每个面上的一个压敏粘合剂层。
特别是,本发明胶带的载体是膜,泡沫,或者两层或更多层膜的复合体,两层或更多层泡沫的复合体或至少一层膜和至少一层泡沫的复合体,带有双面自粘合涂层的相应载体或组装件,并且至少面对印版的那面配置了本发明的PSA。本发明的PSA可以优选用于两个PSA层。
根据本发明特别合适的是下面的双面胶带,它包括泡沫载体、在泡沫载体的一个面上的聚合物膜,在胶带两个面每个的上面的PSA层,至少一个PSA外层为本发明的交联的PSA,但更特别地两个PSA层均为本发明的PSA。
当使用至少一层膜和至少一层泡沫材料(“泡沫”)的复合体作为载体时,在一种优选方案中,这些载体层可以通过用粘合剂层合在一起以获得载体组装件。在另一实施方式中,可以通过热封将各层彼此相连接。为了得到载体组装件,一种可选的可行方案是使用本领域已知的其他方法,将具体为聚合物的两个层大范围(extensively)相连接。
在PSA带面对印刷辊筒的那个面上,可以优选使用本发明的PSA,但原则上可以使用本领域技术人员已知的其他PSA。因此,例如,橡胶类PSA、合成橡胶PSA,基于聚硅氧烷、聚氨酯、聚烯烃或聚丙烯酸酯的PSA都是合适的。
对于膜类载体,可以使用本领域技术人员熟悉的那些材料,特别是聚酯、聚对苯二甲酸乙二醇酯(PET)、聚乙烯(FE)、聚丙烯(PP)、双轴取向的聚丙烯(BOPP)、聚氯乙烯(PVC)等。此列举应理解为是非穷举性的。特别优选使用聚对苯二甲酸乙二醇酯膜。
适合的泡沫载体特别优选为聚合物泡沫,例如,该载体泡沫由聚烯烃(更具体为聚乙烯或聚丙烯)、聚氨酯或聚氯乙烯构成。
当使用泡沫作为载体材料时,特别优选还在所述泡沫载体至少一面上提供至少一种稳定化载体,以得到上述的载体组装件。更具体地,稳定化载体可以为纸或膜,特别是聚酯、聚对苯二甲酸乙二醇酯、聚乙烯、聚丙烯、双轴取向聚丙烯或聚氯乙烯的膜。优选可以在泡沫载体的两个面均提供稳定化载体。
通常,通过使载体材料粗糙化可以改进PSA的锚固。粗糙化和化学改性聚合物结构的一种方式是通过湿式化学刻蚀载体材料。除了刻蚀之外,还可以以其他方式进行预处理。
例如,为了改进锚固,载体材料可以进行化学和物理预处理。对于物理处理,优选将膜通过火焰或电晕或等离子体进行处理。对于化学预处理,对载体材料配置底漆涂层(prime coat),在一种特别优选的实施方式中,使用反应性底漆涂层。适宜的底漆涂层材料包括例如反应性底漆。
为了用作结合印版的双面压敏胶带,在本发明的一个特别优选的实施方式中,该PSA带具有图1中的产品结构。
使用所述胶带来结合由PET-膜2和光聚合物层1构成的印版。
层3-9形成固定版的双面胶带,由于其泡沫载体8,其是可压缩的和弹性的。
从结合所述版的那面开始,该胶带由以下单独部分构成:
3用于锚固版的PSA
4PET膜5的粗糙上表面
5聚对苯二甲酸乙二醇酯(PET)膜
6PET膜5的粗糙底表面
7将泡沫载体8锚固在聚对苯二甲酸乙二醇酯(PET)膜5上的PSA
8泡沫载体
9用于在印刷辊筒上锚固的PSA
在印刷业中特别重要的是此处使用的胶带具有高柔性,即,在施加压力时,能够在一定程度改变它们的厚度,并且当移去载荷时能够恢复到它们原来的形状。
此外,优选泡沫载体8是由聚烯烃、聚氯乙烯(PVC)或聚氨酯(PU)构成。一种特别优选的实施方式使用发泡的聚乙烯和聚丙烯。还优选泡沫载体的表面已经是物理预处理过的,更具体地是电晕预处理过的。
还优选聚对苯二甲酸乙二醇酯(PET)膜的厚度为5μm~500μm,优选5μm~60μm。
另外,本发明的胶带可以在一面或两面配置纸衬里或相应的膜衬里,更具体地为双面硅化的纸衬里或双面硅化的膜或有机硅膜衬里,以确保长期存放和在使用过程中方便处理。
由于其特定的性质,本发明的双面胶带可以出色用于将印版,特别是多层光聚合物印版固定到印刷辊筒或套筒上。
由于其特殊的构造,特别是具有与印版匹配的结合强度,本发明的胶带特别适合用于印版和印刷辊筒的结合。一方面,在开始印刷前可以将印版多次重新定位,而另一方面,确保印刷操作期间版的牢固结合。
使用配置有本发明PSA的PSA带所结合的印版可以毫无破坏地从PSA带中移去,特别是还可以毫无残留地移去。
不出现版的载体层的剥离或者在移去时在版中形成的不必要的折痕。在胶带从印刷辊筒除去之后也不留下任何残留物。
本发明的胶带还特别适合柔性印版和印刷套筒的结合。
实验
下面在多个实验中描述本发明胶带的优点。使用如下测试方法评估制得的PSA的技术性质。
测试方法
结合强度:
根据PSTC-1测试剥离强度(结合强度)。将30g/m2的PSA层施用到23μm厚的PET膜上。
将此2cm宽的样本(specimen)条结合到钢板上并使用2kg辊来回滚三次。在张力试验机中,将该板夹紧,将PSA条以180°的剥离角和300mm/min的速度从它的自由端剥离。
在该步骤过程中,一种情况在结合后直接测量结合强度,另一种情况在室温存放72h后测量。如下确定在聚乙烯上的结合强度:所用的规定的基板(结合强度板)是聚乙烯板,它是由Basell Hostalen GC7260HDPE粒料通过注塑制备为测试板。在测量前,用乙醇清洗该板。作为考察的样品,在厚度为23μm的标准聚酯载体的一面涂布相应的自粘性粘合剂(自粘性粘合剂的涂布重量:50g/m2)。在载荷(2kg)下将宽20mm的涂布的标准聚酯载体条压到基板上。之后在室温下立即以180°的角度和300mm/min的速度将胶带从基底剥去,测量完成它所需要的力。获得的测量值(以N/cm计)为三个单次测量的平均值。为了校准测量方法,用该测量方法考察市售的用于测试非粘合剂涂层的测试胶带(型号为“tesa 7475”,得自tesa AG;根据规格书,与钢的结合强度为:31.25N/25mm);此时与聚乙烯测试板的结合强度为4.5N/cm。
边缘上翘
钢印刷辊筒配置了与图1结构一致的双面胶带,所用的稳定化膜是23μm的刻蚀过的PET膜,所用的泡沫是密度为270kg/m3的500μm的PE-EVA泡沫(聚乙烯-乙烯-乙酸乙烯酯)。
两个面,即对着钢筒和印版两者的面均使用粘合剂,厚度为30g/m2,该粘合剂是得自实施例B1~B5及C6和C7的各自的组合物。
除去防粘纸之后,与施用到钢筒的胶带外部的本发明的粘合剂层(图1中的附图标记3)结合的是厚度为2.54mm的DuPont Cyrel HOS印版,通过图1中的粘合剂9结合该胶带和印刷辊筒。
将样本以结合状态在室温静置3天。随后测量边缘上翘,以mm计。
可分开能力:
在3天剥离增加时间(peel increase time)之后,用手移除上述结合的印版,并主观观察可分开能力;该可分开能力分类为容易、可接受的、困难和非常困难。
样品的准备
可以由溶液、由分散体和由熔体进行PSA的制备和加工。优选的制备和加工方法是由溶液和由熔体进行的方法。
样本的制备
将组分溶于甲苯和汽油(benzine)的50∶50混合物中,得到40%的固体含量。然后将样本涂布到23μm厚的蚀刻过的PET膜上,并在100℃干燥,得到每单位面积重量为30g/cm2的粘合剂。
各实施例的组成参见表1(所有量以%重量计)。
表1:
所用原料的性质:
Kraton polymers
Kraton polymers
Kraton polymers
Kraton polymers,分子量比Kraton D 1102高
Exxon Mobil
A 15 α-蒎烯树脂,软化温度:约115℃,DRT
A 10 液体烃树脂,Eastman
10 液体烃树脂,Goodyear
根据DIN EN 1427:2007方法使用测试树脂代替沥青测量软化点。
实施例C7
向常规用于自由基聚合反应的2升玻璃反应器中装入8g丙烯酸、372g丙烯酸2-乙基己酯、20g丙烯酸异冰片酯和170g丙酮∶特定沸点石油溶剂油60/95(1∶1)。在搅拌下使氮气通过该反应器45分钟之后,将反应器加热至58℃,并添加0.2g偶氮异丁腈(AIBN,64,DuPont)于10g丙酮中的溶液。随后将外部热浴加热至75℃,并在此外部温度下持续进行反应。在1小时反应时间之后,添加另外的0.2g AIBN在10g丙酮中的溶液。反应5小时之后,添加0.8g二(4-叔丁基环己基)过氧化二碳酸酯[16;Akzo Nobel]于10g丙酮中的溶液。6小时之后,用100g特定沸点石油溶剂油60/95稀释该批料。反应7小时之后,添加0.8g二(4-叔丁基环己基)过氧化二碳酸酯(16;Akzo Nobel)于10g丙酮中的溶液。
10小时之后,用150g特定沸点石油溶剂油60/95稀释该批料。在反应24小时之后,中止反应并将批料冷却至室温。之后,将聚丙烯酸酯与0.6%重量的乙酰丙酮铝(3%浓度溶液,于丙酮中)共混,并用特定沸点石油溶剂油60/95稀释该共混物至固体含量为30%,然后由溶液涂布到PET膜上。在120℃干燥30分钟后,涂布重量为30g/m2。
测得例示的PSA条具有以下技术数据:
PSA实施例号 | 和钢的结合强度,瞬间,以N/cm计 | 和钢的结合强度,72h后,以N/cm计 | 和PE的结合强度,以N/cm计 | 室温下的保持力,以分钟计 | 边缘上翘,以mm计 | 可分开能力 |
B1 | 5.8 | 6.3 | 4.1 | >10000 | 0 | 可接受的 |
B2 | 6.2 | 6.5 | 3.8 | >10000 | 0 | 容易-可接受的 |
B3 | 5.3 | 5.7 | 3.4 | >10000 | 0 | 容易-可接受的 |
B4 | 5.9 | 6.5 | 3.8 | >10000 | 0 | 容易 |
B5 | 4.8 | 5.2 | 3.1 | >10000 | 0 | 容易 |
C6 | 8.2 | 9.3 | 4.9 | >10000 | 0 | 非常难 |
C7 | 2.2 | 3.1 | 55 | 容易 |
注意到基于丙烯酸酯的粘合剂(C7)尽管容易分开,但表现出严重的边缘上翘。
含有少量乙烯基芳族化合物嵌段共聚物的粘合剂(C6)具有高的结合强度且显示无边缘上翘,但不仅非常难分开,而且在较大印版的情况下根本无法分开。
具有高分率的弹性体(乙烯基芳族化合物嵌段共聚物)时,特别是大于50%重量时(基于树脂-嵌段共聚物混合物),同样没有边缘上翘,但移除印版容易得多,在使用之后没有残留物,在这一点上,本发明的实施例B1~B5相当。
Claims (9)
1.压敏粘合剂在用于柔性印版和印刷辊筒或印刷套筒的结合的胶带中的用途,所述压敏粘合剂包括:
至少一种树脂-聚合物共混物,其组成如下:至少50%重量的包括基于乙烯基芳族化合物的聚合物嵌段和基于1,3-二烯的聚合物嵌段的一种或多种嵌段共聚物,和不大于50%重量的至少一种增粘树脂。
2.双面胶带,包括至少一层发泡载体,在该发泡载体的一面上的至少一层聚合物膜和在所述胶带两个面各自上面的一层压敏粘合剂,其特征在于,外层压敏粘合剂中的至少一种是包含以下物质的组合物:
至少一种树脂-聚合物共混物,其组成如下:至少50%重量的包括基于乙烯基芳族化合物的聚合物嵌段和基于1,3-二烯的聚合物嵌段的一种或多种嵌段共聚物,
和不大于50%重量的至少一种增粘树脂。
3.权利要求2的胶带,其特征在于,所述树脂-聚合物共混物中的嵌段共聚物分率为55%~65%重量。
4.权利要求2和3任一项的胶带,其特征在于,所述树脂-聚合物共混物的树脂分率为35%~45%重量。
5.权利要求2-4任一项的胶带,其特征在于:
所述树脂是基于以下物质的树脂:松香和松香的衍生物,二环戊二烯的氢化或非氢化聚合物;基于C-5、C-5/C-9或C-9单体流的非氢化的烃树脂或部分氢化的烃树脂、选择性氢化的烃树脂或完全氢化的烃树脂;基于α-蒎烯和/或β-蒎烯和/或δ-苧烯的氢化或非氢化聚萜烯树脂。
6.权利要求2-5任一项的胶带,其特征在于,所述嵌段共聚物的聚乙烯基芳族化合物的含量为至少20%重量。
7.权利要求2-6任一项的胶带,其特征在于,苯乙烯用作乙烯基芳族化合物。
8.权利要求2-7任一项的胶带,其特征在于,丁二烯和/或异戊二烯用作1,3-二烯。
9.权利要求2-8任一项的胶带用于柔性印版和印刷辊筒或印刷套筒的结合的用途。
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CN103589388A (zh) * | 2012-07-23 | 2014-02-19 | 德莎欧洲公司 | 用于胶带的压敏粘合剂以及其在胶带中的应用 |
CN104169384A (zh) * | 2012-03-30 | 2014-11-26 | Lg化学株式会社 | 粘合胶带 |
CN105283318A (zh) * | 2013-06-12 | 2016-01-27 | 株式会社金阳社 | 柔版印刷用版材 |
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- 2008-05-15 DE DE200810023741 patent/DE102008023741A1/de not_active Withdrawn
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2009
- 2009-04-17 CA CA 2663208 patent/CA2663208A1/en not_active Abandoned
- 2009-04-22 EP EP20090158444 patent/EP2130885A1/de not_active Withdrawn
- 2009-05-04 US US12/434,707 patent/US20090277561A1/en not_active Abandoned
- 2009-05-08 JP JP2009113110A patent/JP2009270110A/ja not_active Withdrawn
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CA2663208A1 (en) | 2009-11-09 |
JP2009270110A (ja) | 2009-11-19 |
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