CN101815767B - 具有层间层压透明模压聚合物全息图的安全层压材料 - Google Patents
具有层间层压透明模压聚合物全息图的安全层压材料 Download PDFInfo
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Abstract
本发明涉及一种层间层压透明模压全息图的方法,所述透明模压全息图包括具有两个侧面的载体,两个侧面的至少一个侧面自身被模压或在上面具有模压层;和邻接模压侧面或模压层的HRI材料层,所述方法包括以下步骤:a)用至少一种有机液体调节无机HRI材料层的最外表面;b)使无机HRI材料层的最外表面干燥,从而提供无机HRI材料层的经调节最外表面;c)将粘合剂层施加到经调节最外表面;和d)使无机HRI材料的最外表面层压到任选透明薄膜,其中至少一种有机液体选自酮、醚、杂环醚、内酰胺、酰胺、卤代脂族化合物、腈和酯;其中载体和薄膜的至少一个是透明的;并且其中HRI材料为具有高于模压材料至少0.3的折光指数的材料。本发明还公开可用所述方法得到的层压材料和包含层压材料的身份证件。
Description
发明领域
本发明涉及具有含有无机HRI材料涂层的层间层压透明模压聚合物全息图的安全层压材料和得到所述材料的方法。
发明背景
安全层压材料传统上用于保护文件或包装,以通过包含鉴定特征保证位于下面的项目不被改变,使它们难以伪造。安全层压材料特别用在身份证件上,如驾驶证、身份证和护照,也用在其他重要文件上,如产权证。安全层压材料也可在药物、录像带和光盘上用作防篡改密封。在制造和使用安全层压材料时,有5个特征特别重要。第一,一旦施加到制品上,层压材料难以去掉,以保证位于下面的项目不被变动或篡改就很重要。第二,合乎需要的层压材料难以被伪造者复制,如果不是不可能。第三,如果出现篡改,则快速精确地识别改动或伪造层压材料很重要。第四,层压材料的制造成本不惊人地昂贵很重要。第五,在用于制品上时,如身份证件,层压材料具有足够耐久性经受严酷处理很重要。
由于产生和复制困难,全息图已成为诸如***、驾驶证和出入证(access card)等物品上的一般鉴定特征。全息图也已在高端产品上用作安全标记,使伪造这些产品更加困难。
全息摄影术的主要进展出现在1968年,这一年,A.Benton发明了白光透射全息术。此类型全息图可在从组成白光的七种颜色产生“彩虹”图像的普通白光中看到。Benton的发明使得用模压技术大量产生全息图成为可能。利用此技术,可使全息信息从光敏玻璃板转移到镍模压垫片上。通过使干涉图案模压到塑料上,可“印刷”全息图像。虽然主垫片辊需要定期更换,但得到的全息图可廉价地复制数百万次。因此,模压全息图现在正由出版业、广告业、金融业和安全业使用。产生和复制全息图的困难使它们成为诸如***、驾驶证和出入(身份)证等安全物品上的一般鉴定特征。透明全息图通常用于安全应用,如身份或出入证,在此需要位于全息图后的信息保持对肉眼可见。
产生全息图的最一般方法是在表面中产生光栅图案,以便在光栅中光线衍射时具体结构变得可见。US 3,578,845描述如何一般性产生衍射光栅。一般将衍射图案模压入可热成形的基片,如可模压的聚合物薄膜。通过将加热的由硬材料制成的印模下压,以将来自印模接触表面的所需光栅刻印在可模压的基片上,可进行此过程。
衍射需要制成光栅的介质和邻接光栅的介质具有折光指数差。折光指数差越大,衍射显得越鲜明。为了在透明全息图中产生最高衍射,用具有高折光指数(HRI)的透明材料的薄膜涂覆光栅。
虽然光栅可用印模压入基片材料,但更一般的经济方法是使用连续模压***。此类模压***描述于例如US 4,913,858和5,164,227。在这些方法中,光栅结构刻入辊的表面,辊的表面将其表面图案连续压入在模压辊和背面辊之间通过的卷(web)类型的基片。为了在基片的表面中得到光栅,加热在此表面上的可热成形层。这可通过将基片预热到所需温度达到,或者加热模压辊。
WO 2007/027619A2公开一种半透明全息薄膜,所述全息薄膜包括:粘合剂层、模压层,所述模压层包括模压侧,模压侧限定具有指向粘合剂层的峰的脊。
一般通过使用真空蒸发技术,以用透明HRI涂层涂覆模压的聚合物,可产生透明全息图。另外,为了防止篡改,通常通过在复合身份证件内层压包埋得到的全息图。这不仅需要全息图的载体/基底粘合到组成身份证件的复合***内的邻接薄膜或层,而且需要HRI层的最外表面也粘合到组成身份证件的复合***内的邻接薄膜或层。
另外,HRI层的最外表面粘合到邻接薄膜、层或卡应在无全息图亮度基本损失下进行,以防止对比度损失。
用无机HRI材料涂覆的市售透明模压全息图不适合在组成复合身份证件的复合***中防篡改层间层压。
发明方面
因此,本发明的一个方面是提供在组成身份证件的复合***内层压用无机HRI材料涂覆的透明模压聚合物全息图,而不基本损失亮度的防篡改方法。
因此,本发明的另一个方面是提供一种复合身份证件,所述复合身份证件包含用无机HRI材料涂覆的层间层压防篡改模压聚合物全息图。
通过以下说明,本发明的其他方面将变得显而易见。
发明概述
用无机HRI材料涂覆的市售透明模压全息图不适合在组成复合身份证件的复合***中防篡改层间层压。通过在载体上涂覆可模压聚合物层,随后局部模压所述层,并使HRI层真空蒸发在可模压聚合物层的整个表面上,一般可制备此模压全息图。已发现,使用标准粘合剂不可能使HRI层(例如ZnS或TiO2层)的最外表面充分粘合到聚乙烯薄膜,从而避免整体脱层。意外的是,已发现,用某些有机液体处理用无机HRI材料涂覆的市售透明模压全息图的无机HRI层的最外表面,以便调节无机HRI材料的最外表面,可用粘合剂达到对聚乙烯、聚对苯二甲酸乙二酯、PET、PVC或聚碳酸酯薄膜的良好粘合。此外,以充分低的浓度组合使用这类有机液体与具体粘合剂能够得到良好的粘合,从而减少实现层间层压所需的方法步骤的数目。此粘合改进以亮度为代价,显示表面粗糙化,但用保护性水可释放/可溶解薄膜掩蔽或部分覆盖使此问题能够通过达到与被保护区域相邻的粘合作用克服。
本发明的各方面已通过权利要求1中定义的层间层压透明模压全息图的方法实现。
本发明的各方面也已通过可由上述方法得到的安全层压材料实现。
本发明的各方面还已通过包括上述安全层压材料的身份文件实现。
从属权利要求公开了优选的实施方案。
发明详述
定义
一般在本领域区分“软模压”和“硬模压”。“软模压”描述在施加高反射(reflective)指数(HRI)层之前进行模压的过程。“硬模压”由通过HRI层产生光栅进行。虽然硬模压对用“软”金属涂覆的基片进行,如铝、铜或金,但一般不通过半透明反射增强HRI层进行,如ZnS或TiO2。
本发明所用术语“层间层压”是指在两层薄膜之间层压箔、标签或其他基本平的物体。
本发明所用术语“薄膜”是指自支承聚合物基片,这种片可具有数微米厚(例如,在热升华印刷(TSP)和制造复合身份证件中使用的箔)至数毫米厚的不同厚度。
本发明所用术语“透明全息图”是指与透明HRI材料邻接的全息图。
本发明所用术语“不透明全息图”是指与不透明HRI材料(例如金属)邻接的全息图。
本发明所用术语“高折光指数(HRI)材料”是指具有高于被模压材料至少0.3,优选高于被模压材料至少0.6的折光指数的材料。
层间层压透明模压全息图的方法
本发明的方面已通过层间层压透明模压全息图的方法达到,所述透明模压全息图包括具有两个侧面的任选透明载体,两个侧面的至少一个侧面自身被模压或在上面具有模压层;和邻接模压侧面或模压层的HRI材料层,所述方法包括以下步骤:用至少一种有机液体调节无机HRI材料层的最外表面;使无机HRI材料层的最外表面干燥,从而提供无机HRI材料层的经调节最外表面;将粘合剂层施加到经调节最外表面;和使无机HRI材料的最外表面层压到任选透明薄膜,其中至少一种有机液体选自酮、醚、杂环醚、内酰胺、酰胺、卤代脂族化合物、腈和酯,其中载体和薄膜的至少一个是透明的。
使用溶剂调节HRI层最外表面可以通过使用涂敷技术或印刷技术如凹版印刷和丝网印刷,随后干燥来实现。
本发明方法的一个实施方案中,模压层具有在载体折光指数0.2内的折光指数。
在本发明的方法的优选实施方案中,层压到HRI材料层的最外表面的聚合物薄膜为聚合物箔,所述聚合物箔优选具有约5μm至约120μm,更优选约10μm至约60μm,最优选约10μm至约30μm的厚度。
在本发明的方法的一个实施方案中,HRI层的剥离强度为根据ISO Norm 10373-1-1978测定至少6N/cm。如果箔在剥离强度试验期间断开,则剥离强度高于剥离强度值的可测量范围。
在本发明的方法的一个实施方案中,透明箔对HRI层的最外表面的层压具有根据ISO Norm 10373-1-1978测定至少6N/cm的剥离强度。如果箔在剥离强度试验期间断开,则剥离强度高于剥离强度值的可测量范围。
在本发明的方法的一个实施方案中,所述方法进一步包括以下步骤:将粘合剂层施加到不在模压层上具有HRI层的载体侧面上的最外表面,并且使透明薄膜层压到粘合剂层,以便粘合剂至少围绕透明模压全息图提供密封。
在本发明的方法的一个实施方案中,载体对聚合物薄膜的层压具有根据ISO Norm 10373-1-1978测定至少6N/cm的剥离强度。如果聚合物薄膜在剥离强度试验期间断开,则剥离强度高于剥离强度值的可测量范围。
在本发明的方法的一个实施方案中,经调节最外层对聚合物薄膜的层压具有根据ISO Norm 10373-1-1978测定至少6N/cm的剥离强度。如果聚合物薄膜在剥离强度试验期间断开,则剥离强度高于剥离强度值的可测量范围。
在本发明的方法的一个实施方案中,载体是透明的。
在本发明的方法的一个实施方案中,载体具有边界,并且任选作为图案存在的高折光指数材料位于边界内侧。高折光指数材料的水分驱使腐蚀一般从层压片的边缘开始。在层压材料边缘没有腐蚀敏感性高折光指数涂层的区域提供改善的水分屏障,并且减小高折光指数材料的腐蚀和退化。
在本发明的方法的一个实施方案中,透明的模压全息图进一步包括基层和使基层粘合到载体的粘合剂层。
在本发明的方法的一个实施方案中,载体的表面用均匀的光栅(一般称为“彩虹”光栅)模压,并且在光栅顶上在限定的图案中施加透明的高折光指数材料。利用此实施方案,后续处理,如施加热敏或压敏粘合剂,覆盖完全区域,包括用高折光指数涂层涂覆的那些区域和不用高折光指数涂层涂覆的那些区域。粘合剂的折光指数优选差不多与经模压基片相同,这导致消除不用高折光指数涂层涂覆的那些区域中的衍射效应。
在本发明的方法的一个实施方案中,经模压层或经模压载体经表面处理。表面处理活化全息图侧,用于沉积透明的HRI层。使可模压的多层薄膜的表面暴露于电离气体(即等离子)或电晕放电是一种优选的表面处理。
在本发明的方法的一个实施方案中,在真空涂覆前进行模压,从而使载体的层或表面暴露于模压过程的另外的热和压力,如此更大地除去残留的水分和溶剂。
可模压层
可模压层优选由与载体相同种类的低结晶聚合物制成。可模压层优选由具有低于载体的相关聚合物至少约10℃(但优选至少约20℃)的熔点的聚合物制成。
可模压层的厚度优选为约1μm至约10μm,更优选约2μm至约8μm,最优选约3μm至约7μm。太薄的层可导致模压的图像品质差。太厚的层则无效。
适用于可模压低结晶层的聚合物包括聚对苯二甲酸乙二酯(PET)、聚氯乙烯、聚偏二氯乙烯、聚乙烯、聚丙烯、聚碳酸酯、玻璃纸、乙酸酯、尼龙、聚乙烯醇、聚酰胺、聚酰胺酰亚胺、乙烯-乙烯醇共聚物、聚甲基丙烯酸甲酯、聚醚砜或聚醚醚酮及其混合物。
优选可模压层包括选自以下聚合物组的基片薄膜的聚合物低结晶变种:聚对苯二甲酸乙二酯(PET)、聚氯乙烯、聚偏二氯乙烯、聚乙烯、聚丙烯、聚碳酸酯、玻璃纸、乙酸酯、尼龙、聚乙烯醇、聚酰胺、聚酰胺酰亚胺、乙烯-乙烯醇共聚物、聚甲基丙烯酸甲酯、聚醚砜或聚醚醚酮。低结晶聚合物在低于芯聚合物的温度***。
在载体上产生可模压层(如可模压聚(对苯二甲酸乙二酯)(PET)或聚丙烯(PP))的一般方法是将可热成形可模压涂层施加到载体的至少一个表面上。此方法离线进行,即在制造载体之后进行。一般使用在本领域熟知的涂覆***,如辊涂、凹版涂覆、气刀涂覆和棒涂,作为水基或溶剂基溶液施加可模压涂层。
通过将在其表面包埋所需光栅的垫片压在可模压基片上,并且HRI涂层和可模压层面对模压垫片,可进行模压。关于模压过程,可将薄膜预热,以允许可模压层聚合物在模压垫片下柔软,或者垫片自身被加热,并使热转移到可模压层,使其柔软。
载体
适合的载体为任何聚合物薄膜。优选的载体薄膜包括聚对苯二甲酸乙二酯(PET)、聚氯乙烯、聚偏二氯乙烯、聚乙烯、聚丙烯、聚碳酸酯、玻璃纸、乙酸酯、尼龙、聚酰胺、聚酰胺酰亚胺、聚甲基丙烯酸甲酯、聚醚砜和聚醚醚酮薄膜。
载体应足够厚,以便为自支承,但也应足够薄,以便弯曲、折叠或起皱而不破裂。优选基片薄膜具有约7μm至约120μm,更优选约10μm至约60μm,最优选约10μm至约30μm厚度。
无机HRI材料
透明无机HRI涂层施加到可模压表面或层的顶部上。为了得到足够的反射率,经模压材料和HRI涂层的折光指数差优选为至少0.3,更优选大于0.6。
在一个优选的实施方案中,HRI材料的折光指数为至少2.0,更优选至少2.2。
适合的透明高折光指数(HRI)材料包括硫化锌(ZnS)、硫化锑(III)、氧化铁(III)(Fe2O3)、氧化铅(II)(PbO)、硒化锌(ZnSe)、硫化镉(CdS)、二氧化钛(TiO2)、氯化铅(II)(PbCl2)、氧化铈(IV)(CeO2)、氧化钽(Ta2O5)、氧化锌(ZnO)、氧化镉(CdO)、氧化钕(Nd2O3)和氧化铝(Al2O3)。目前,在透明全息图中用ZnS作为透明反射增强层是最广泛使用的技术。也可使用材料的混合物。US 5,513,019公开用于全息图的硫化锌(ZnS)和氧化钨(WO3)的混合物。
可通过标准沉积技术使透明的无机HRI材料沉积于其中已或将用全息垫片模压的层或载体表面上,如蒸发、反应或非反应性真空蒸气沉积、物理蒸气沉积(PVD)、化学蒸气沉积(CVD)、溅射、电子束沉积和离子束辅助沉积。
透明HRI涂层的厚度优选厚得足以提供优良折射(折光)性质,但不要太厚,以免抑制其透明性质。优选透明HRI材料以约20至约250nm厚度沉积,约5至约150nm厚度特别优选,约5至约100nm厚度尤其优选,10nm至80nm厚度最尤其优选。在沉积之前模压的情况下,沉积的HRI材料追随模压分布。
在蒸气沉积技术中,涂料在升高温度在低压蒸发,一般在1×10-3Pa范围。由使基片通过蒸气,蒸发的材料凝结在经模压的基片表面上,产生反射增强材料薄层。沉积层的厚度取决于多个因素,例如蒸发速率、蒸气压和基片在蒸气云中的停留时间。
沉积技术可导致化学计量损失(化学计量损失造成据以产生效应的折光指数差减小)、透明度损失和亮度损失。
硫化锌倾向为软多孔涂层,但可在金属化速度沉积(100’s m/min)。另外,ZnS可从跨整个卷宽度的槽源热蒸发。另外,ZnS可很容易离解并重新化合,因此,化学计量一般不是问题。也可通过ZnS模压入聚合物,仍得到良好的全息图,并且ZnS的优点是对全息垫片的磨损小于较硬材料,如二氧化钛。操作人员可能对这种材料不太满意,因为在***排放时由于残余硫散发气味。
二氧化钛倾向于较为致密,较硬,通常由较慢技术沉积(1-10’sm/min)。如果需要耐磨损最高品质的全息图,则二氧化钛大概会是优选的材料。沉积二氧化钛的部分问题是使化学计量合适。从钛靶溅射并使涂层与氧反应产生二氧化钛不一定容易。不能选择性控制氧达到生长涂层,也不达到溅射阴极,因此阴极中毒。二氧化钛的溅射速率比金属慢20倍,因此,此过程倾向于骤然从氧化物靶缓慢溅射。对此失控过程有纠正方法,但它们均提高沉积成本。理想的是,如果要通过溅射双阴极沉积涂层,优选利用AC电源,包括电弧控制。可从电子束沉积源沉积二氧化钛,但得到一致的化学计量却不简单。通常另外的氧等离子用于使涂层致密,使其更象是溅射的涂层,但也作为一种减少使金属转化成二氧化钛所需的过量氧的方法。
HRI涂层的均匀性也可能是个问题。溅射具有朝向阴极端衰减的沉积速率,因此,跨整个卷宽度得到高均匀性需要宽于卷宽度的阴极长度。关于电子束源,它取决于是否你拥有具有跨宽度成一体的沉积通量的一系列单独的源,或者取决于是否有利用跨卷宽度的单一熔缸(crucible)的单一扫描电子束。
对所有真空沉积技术的关键是泵抽***在***中的位置和在氧气中进料的方法。理想的是泵抽围绕卷中心线对称(包括任何低温泵),如果不是这样,得到均匀性中有另外的问题。来自卷的水分可以是对涂层的氧和加入以控制过程的氧的氧源。如果有不对称泵抽,则就会有跨卷的压力梯度,因此输送足够氧变得困难,并且不再达到溅射阴极的所有部分或来自电子束源的蒸气通量。任何不平衡都会产生非化学计量涂层。
可用等离子后处理清洁最外HRI层表面,以除去表面污染物。功率、时间和气体组成的选择均可影响任何等离子处理的效率。氩等离子可使表面粗糙化并且有效溅射,但没有使烃转化成可泵抽掉的气体物质的机制,因此,从表面溅射的任何物质都可完全落回,并且仍为表面上的污染物,尽管已经过等离子处理。因此,用氧/氩混合物等离子处理通常优选。然而,如果表面过度处理,就会由于太多聚合物断链在表面上产生弱的边界层。
有机液体
在本发明的方法中使用的至少一种有机液体选自酮、醚、杂环醚、内酰胺、酰胺、卤代脂族化合物、腈和酯。
合适的酮包括丙酮、甲基乙基酮和环己酮。
合适的醚包括二甘醇二甲醚(2-甲氧基乙基醚)、四氢呋喃和二氧杂环己烷。
合适的杂环醚包括四氢呋喃和二氧杂环己烷。
合适的内酰胺包括2-吡咯烷酮、N-甲基-2-吡咯烷酮和己内酰胺。
合适的酰胺包括甲酰胺、乙酰胺、N-甲基甲酰胺和二乙基乙酰胺。
合适的卤代脂族化合物包括氯脂族化合物、溴脂族化合物、氟脂族化合物、氯-溴脂族化合物和氯-氟脂族化合物。
合适的氯脂族化合物包括二氯甲烷、氯仿、二氯乙烷、三氯乙烷、四氯乙烷和三氯乙烯。
合适的腈包括乙腈和丁腈。
合适的酯包括脂族酯、芳族酯和杂环酯。
合适的脂族酯包括乙酸甲酯、乙酸乙酯、乙酸丙酯和乙酸丁酯。
合适的芳族酯包括苯甲酸甲酯、苯甲酸乙酯、苯二甲酸二甲酯、苯二甲酸二乙酯、苯二甲酸二丁酯和二-(2-乙基己基)苯二甲酸酯。
合适的杂环酯包括γ-丁内酯、β-丁内酯、γ-己内酯和ε-己内酯。
粘合剂
在本发明的方法中用于施加粘合剂层的粘合剂组合物包含具有多个羟基的聚合物和选自聚异氰酸酯、聚环氧化物和水解聚烷氧基硅烷(例如原硅酸四烷基酯)的固化剂。
在本发明的方法的一个实施方案中,粘合剂为离子自固化粘合剂。
在本发明的方法的一个实施方案中,粘合剂为热固化粘合剂。
在本发明的方法的一个实施方案中,粘合剂为通过释放水自固化的粘合剂。
在本发明的方法的一个实施方案中,粘合剂为在环境条件下自固化的粘合剂。
在本发明的方法的一个实施方案中,粘合剂为在低于100℃温度(优选低于80℃,特别优选低于50℃)自固化的粘合剂。
具有多个羟基的适合聚合物包括羟基氨基甲酸酯预聚物、聚乙烯醇、部分水解的聚乙酸乙烯酯和明胶。
适合的聚异氰酸酯化合物包括芳族和脂族聚异氰酸酯或聚氰酸酯前体,参见公开聚异氰酸酯和聚异氰酸酯前体的部分。
固化反应主要基于异氰酸酯基或热产生的异氰酸酯基和含多个羟基的聚合物的游离羟基之间的反应,但也基于在树脂中已生成的氨基甲酸酯基与聚异氰酸酯的异氰酸酯基的反应中生成脲基甲酸酯基[D.H.Solomon“The Chemistry of Organic Film Formers”(有机薄膜前体化学)-John Wiley&Sons,Inc.New York(1967)p.203]。
适合的聚烷氧基硅烷包括原硅酸四烷基酯,例如原硅酸四甲酯和原硅酸四乙酯。
适用于聚氨酯粘合剂的成分为:
Liofol UK 3640=聚氨酯溶剂(乙酸乙酯)粘合剂,购自Henkel
Liofol UK 6800=坚膜剂,购自Henkel,与Liofol UK 3640一起使用
Liofol UR 7750=具有异氰酸酯基的聚氨酯预聚物,购自Henkel
Liofol UR 6071=羟基坚膜剂,购自Henkel,与Liofol UR 7750一起使用
Liofol UR 7780=具有异氰酸酯基的聚氨酯预聚物,购自Henkel
Liofol UR 6080=坚膜剂,购自Henkel,与Liofol UR 7780一起使用
聚异氰酸酯
能够在本发明的方法中使用的粘合剂中使用的聚异氰酸酯交联剂为脂族聚异氰酸酯,如1,6-己二异氰酸酯衍生物(HDI)(包括1,6-己二异氰酸酯衍生物(HDI))、环己烷二异氰酸酯(CHDI)和异佛尔酮二异氰酸酯(IPDI);和芳族聚异氰酸酯,如4,4′-二异氰酸基二苯基甲烷(MDI)、2,4-甲苯二异氰酸酯(2,4-TDI)、2,6-甲苯二异氰酸酯(2,6-TDI)和甲苯(2,4/2,6)-二异氰酸酯衍生物(TDI)、萘-1,5-二异氰酸酯(NDI)、对苯二异氰酸酯(PPDI)、三苯基甲烷三异氰酸酯(例如,DESMODURTM R)、三苯基甲烷-p,p′,p″-三苯甲基三异氰酸酯和硫代磷酸三(p-异氰酸基苯基酯)。
得自BAYER MATERIAL SCIENCE的适合聚异氰酸酯包括:
DESMODUR H | 基于1,6-己二异氰酸酯(HDI)的单体脂族二异氰酸酯 |
DESMODUR HL BA | 基于甲苯二异氰酸酯(TDI)和1,6-己二异氰酸酯(HDI)的脂族/芳族聚异氰酸酯共聚物 |
DESMODUR I | 基于IPDI的单体脂环族二异氰酸酯共聚物 |
DESMODUR IL | TDI-异氰脲酸酯 |
DESMODUR IL BA | 基于甲苯二异氰酸酯(TDI)的芳族聚异氰酸酯 |
DESMODUR IL 1351 | TDI-异氰脲酸酯 |
DESMODUR IL 1451 | 基于甲苯二异氰酸酯(TDI)的芳族聚异氰酸酯,用于双组分聚氨酯涂料 |
DESMODUR L 67 BA | 基于甲苯二异氰酸酯(TDI)的芳族聚异氰酸酯 |
DESMODUR L 67 MPA/X | 基于甲苯二异氰酸酯(TDI)的芳族聚异氰酸酯 |
DESMODUR L 75 | 芳族聚异氰酸酯,为甲苯二异氰酸酯(TDI)和三羟甲基丙烷的反应产物的75%溶液 |
DESMODUR N 75 BA | 基于1,6-己二异氰酸酯(HDI)的脂族聚异氰酸酯树脂,缩二脲HDI的75%溶液 |
DESMODUR N 75BA/X | 基于1,6-己二异氰酸酯(HDI)的脂族聚异氰酸酯树脂,HDI缩二脲的75%溶液 |
DESMODUR N 100 | 基于1,6-己二异氰酸酯(HDI)的无溶剂脂族聚异氰酸酯树脂,HDI缩二脲 |
DESMODUR N 300 | HDI异氰脲酸酯 |
DESMODUR N 3200 | 基于1,6-己二异氰酸酯(HDI)的无溶剂脂族聚异氰酸酯树脂,具有低于DESMODUR N100的粘度的HDI缩二脲 |
DESMODUR N 3300A | 基于1,6-己二异氰酸酯(HDI)的无溶剂脂族聚异氰酸酯树脂,HDI三聚体 |
DESMODUR N 3390ABA/SN | 基于1,6-己二异氰酸酯(HDI)的脂族聚异氰酸酯树脂,HDI三聚体,HDI异氰脲酸酯的90%溶液 |
DESMODUR N 3400 | 基于1,6-己二异氰酸酯(HDI)的无溶剂脂族聚异氰酸酯树脂,低粘度HDI三聚体 |
DESMODUR N 3600 | 基于1,6-己二异氰酸酯(HDI)的无溶剂多官能脂族聚异氰酸酯树脂,低粘度HDI三聚体 |
DESMODUR N 3790BA | 基于1,6-己二异氰酸酯(HDI)的脂族聚异氰酸酯树脂,HDI三聚体 |
DESMODUR N 3800 | 基于1,6-己二异氰酸酯(HDI)的无溶剂增韧脂族聚异氰酸酯树脂,HDI三聚体 |
DESMODUR NZ 1 | 基于1,6-己二异氰酸酯(HDI)和异佛尔酮二异氰酸酯(IPDI)的无溶剂脂族聚异氰酸酯树脂 |
DESMODUR VL | 基于二苯基甲烷二异氰酸酯(MDI)的芳族聚异氰酸酯 |
DESMODUR W | 液体脂环族二异氰酸酯 |
DESMODUR XO 672 | 基于4,4′-二苯基甲烷二异氰酸酯(MDI)的无溶剂芳族聚异氰酸酯,用于含水聚合物分散体的水分散***联剂,如聚氨酯、聚乙酸乙烯酯及其共聚物、聚氯丁二烯、反应性丙烯酸类等 |
DESMODUR XP 2410 | (研发产物)低粘度HDI三聚体,基于1,6-己二异氰酸酯(HDI)的脂族聚异氰酸酯树脂 |
DESMODUR XP 2580 | (研发产物)基于1,6-己二异氰酸酯(HDI)的脂族聚异氰酸酯 |
DESMODUR XP 2619 | 基于二苯基甲烷二异氰酸酯(MDI)的芳族异氰酸酯,用于无溶剂双组分聚氨酯涂料 |
DESMODUR XP 7144 | 基于二苯基甲烷二异氰酸酯(MDI)的芳族聚异氰酸酯预聚物,用于1K和2K聚氨酯涂料和密封剂 |
DESMODUR Z 4470 BA | 基于异佛尔酮二异氰酸酯(IPDI)的脂族聚异氰酸酯 |
DESMODUR Z 4470MPA/X | 基于异佛尔酮二异氰酸酯(IPDI)的脂族聚异氰酸酯 |
DESMODUR Z 4470SN | 基于异佛尔酮二异氰酸酯(IPDI)的脂族聚异氰酸酯 |
DESMODUR Z 4470SN/BA | 基于异佛尔酮二异氰酸酯(IPDI)的脂族聚异氰酸酯 |
聚异氰酸酯前体
在用于本发明的方法和层压材料的粘合剂中可使用聚异氰酸酯前体,如具有封端基团以防止在室温反应的聚异氰酸酯,封端基团在解封时与多羟基粘合剂和多羟基粘合剂反应。
聚异氰酸酯用H酸性组分热可逆“封端”。“封端剂”的适当选择决定反应性,即封端聚异氰酸酯的***温度,并因此决定此脂族单组分热固性聚氨酯***的固化条件。以下封端剂可以购得,并且在技术上有利,更重要的是2-丁酮肟(甲基·乙基酮肟,MEKO)、ε-己内酰胺,和有限扩展3,5-二甲基吡唑。在具体领域,尤其是在粉末涂料中,用异氰酸酯二聚体/二聚体结构使异氰酸酯基热可逆地去活化,而不使用封端剂。
120至250℃温度对释放封端基是必要的,封端基通常从涂料挥发。得到的聚异氰酸酯可与其他活性含氢化合物反应形成更热稳定的氨基甲酸酯或脲键。封端聚异氰酸酯的不稳定键的离解温度取决于所用聚异氰酸酯和封端基团的结构。基于芳族聚异氰酸酯的封端聚异氰酸酯在低于基于脂族聚异氰酸酯的温度离解。基于商业利用封端剂的封端聚异氰酸酯的离解温度按以下顺序降低:醇>ε-己内酰胺>酚>甲基·乙基酮肟>活性亚甲基化合物。
可用封端聚异氰酸酯使溶剂性树脂和水性树脂两者交联。封端聚异氰酸酯提供宽制剂范围。可将它们加入到树脂共反应剂,从而提供具有极佳保存期限的单组分涂料。这些组合在合理固化周期内得到交联薄膜。得到的涂层显示具有高硬度和优良柔韧性的独特组合的高性能。基于水分散性封端聚异氰酸酯交联剂和适合水性聚合物的涂料接近以前只由溶剂性涂料得到的性能水平。
由BAYER MATERIAL SCIENCE提供的适合聚异氰酸酯前体包括:
*Nippon Polyurethane Industries
#Mitsubishi Kasei Corp.
聚合物薄膜
在本发明的方法中使用的聚合物薄膜优选为聚乙烯、聚对苯二甲酸乙二酯、PET、PVC或聚碳酸酯薄膜。
在本发明的方法中使用的聚合物薄膜优选为聚合物箔。聚合物箔优选具有约5μm至约120μm,更优选约10μm至约60μm,最优选约10μm至约30μm厚度。
被层压的适合聚合物薄膜和箔包括乙酸丙酸纤维素或乙酸丁酸纤维素、聚酯(如聚对苯二甲酸乙二酯和聚萘二甲酸乙二酯)、聚酰胺、聚碳酸酯、聚酰亚胺、聚烯烃、聚(乙烯醇缩醛)、聚醚和聚磺酰胺。
在本发明的安全文件的一个优选实施方案中,聚合物薄膜为聚氯乙烯、聚碳酸酯或聚酯。聚酯优选为聚对苯二甲酸乙二酯(PET)或对苯二甲酸乙二酯二醇共聚物(PETG)。
安全文件
本发明的安全文件优选为选自身份证、安全卡、驾驶证、社会安全卡、会员卡、时间记录卡、银行卡、工资卡和***的身份证件。在一个优选实施方案中,本发明的安全文件为个人身份证。
工业应用
本发明的方法可用于制备安全层压材料,这种安全层压材料可用在身份证件上,如驾驶证、身份证和护照,也用在其他重要文件上,如产权证。安全层压材料也可在药物、录像带和光盘上用作防篡改密封。
本发明由以下比较性实施例和发明实施例说明。除非另外指明,这些实施例中给出的百分比和比率均以重量计。
MEK=甲基乙基酮
THF=四氢呋喃
在比较性实施例和发明实施例中使用的全息图购自CentroGrafico、FASVER和OVD,全息图由用模压的约5μm厚可模压层涂覆的12μm或23μm厚聚对苯二甲酸乙二酯载体组成,所述可模压层用约100nm厚硫化锌层真空涂覆,硫化锌为HRI材料,以产生相应于模压的全息图。通过真空技术(如真空蒸发或溅射)施加的约100nm厚硫化锌材料层为非晶形,并且多孔。
发明实施例1至4和比较性实施例1
在发明实施例1至4和比较性实施例2和3中,将上述全息图固定在23μm厚聚(对苯二甲酸乙二酯)载体上。约100nm的蒸发的硫化锌层最外表面通过如下步骤调节,使用具有绕线棒的涂覆装置将不同有机液体铺展于其上,接触时间为200s,随后液体在60℃蒸发并干燥5分钟,在比较性实施例1中不进行调节。
通过混合50g Liofol UK 3640(一种聚氨酯溶剂(乙酸乙酯)粘合剂)与1g坚膜剂Liofol UK 6800层,制备粘合剂组合物,此组合物用Braive涂覆装置利用10μm绕线棒施加到用不同有机液体调节的发明实施例1至4的箔的最外表面、没有调节的比较性实施例1的箔的最外表面和用本发明范围之外的有机液体在载体的硫化锌涂覆侧调节的比较性实施例1和2的箔的最外表面,并在50℃干燥5分钟。
然后利用EXECELAM 655Q层压机(购自GMP Co.Ltd,Korea)在160℃温度在速度位置1,将箔的粘合剂层涂覆侧层压到身份证模拟透明层压材料的聚乙烯侧,层压材料由已用12μm明胶层层压到35μm厚聚乙烯箔的500μm PETG片组成。
发明实施例1至4和比较性实施例1至3的所得层压材料的抗脱层用Instron根据ISO/IEC 7810:1995按照剥离强度干燥评价。测定层压材料的干燥剥离强度值,数值在表1中给出。
也评价溶剂调节和粘合剂层对全息图亮度的影响。评价全息图亮度没有标准技术,因此,与未涂覆的全息图比较视觉检查是唯一的选择。亮度根据以下标准通过裁定计分评价:
5=亮度增加超过未涂覆的全息图
4=亮度可比于未涂覆的全息图
3=亮度显著低于未涂覆的全息图
2=亮度相当大地低于未涂覆的全息图
1=全息图消失
发明实施例1至4和比较性实施例1至3的层压材料的计分在表1中给出。
表1:
全息图用甲基乙基酮、乙酸乙酯、四氢呋喃或丙酮调节的发明实施例1至4的层压材料的剥离强度对于身份证件超过≥6N/cm的目标值,但具有未涂覆全息图的比较性实施例1的层压材料和用甲苯和甲醇的比较性实施例2至3的层压材料显示剥离强度完全低于≥6N/cm的目标值(在ISO 10373-1制定的标准为≥3.5N/cm)。发明实施例1至4的经湿润层压材料的剥离强度对于身份证件也满足≥6N/cm的目标值。
观察到的低亮度主要是由于调节溶剂的亮度降低效应和长接触时间。这种效应可以通过减少接触时间来降低,如通过用凹版辊施加3μm厚溶剂层,亮度增加到3,不损失粘合力,或者调节溶剂可以与非调节溶剂混合,如醇或芳族溶剂,从而减少HRI层对亮度降低甲基乙基酮的暴露。
Claims (12)
1.一种层间层压透明模压全息图的方法,所述透明模压全息图包括具有两个侧面的载体,两个侧面的至少一个侧面自身被模压或在上面具有模压层;和邻接模压侧面或模压层的HRI材料层,所述方法包括以下步骤:
a)用至少一种有机液体调节无机HRI材料层的最外表面;
b)使无机HRI材料层的最外表面干燥,从而提供无机HRI材料层的经调节最外表面;
c)将粘合剂层施加到经调节最外表面;和
d)使无机HRI材料的最外表面层压到任选透明聚合物薄膜,
其中至少一种有机液体选自酮、醚、酰胺、卤代脂族化合物、腈和酯;
其中载体和聚合物薄膜的至少一个是透明的;并且
其中HRI材料为具有高于模压材料至少0.3的折光指数的材料。
2.权利要求1的方法,其中载体是透明的。
3.权利要求1或2的方法,其中聚合物薄膜是聚乙烯、聚对苯二甲酸乙二酯、PVC或聚碳酸酯薄膜。
4.权利要求1或2的方法,其中聚合物薄膜为具有5μm至120μm厚度的聚合物箔。
5.权利要求1或2的方法,其中粘合剂包含具有多个羟基的聚合物和选自聚异氰酸酯、聚环氧化物和水解聚烷氧基硅烷的固化剂。
6.权利要求1或2的方法,其中模压层具有在载体折光指数0.2倍内的折光指数。
7.权利要求1或2的方法,其中载体和聚合物薄膜之间的粘合剂层具有在模压层0.2倍内的折光指数。
8.权利要求1或2的方法,其中所述方法还包括将粘合剂层施加到不在模压层上具有HRI层的载体侧面上的最外表面,并且使透明薄膜层压到粘合剂层,以便粘合剂至少围绕透明模压全息图提供密封的步骤。
9.权利要求1或2的方法,其中载体对聚合物薄膜的层压具有根据ISO Norm10373-1-1978测定至少6N/cm的强度。
10.权利要求1或2的方法,其中无机HRI材料层的经调节最外表面对聚合物薄膜的层压具有根据ISO Norm10373-1-1978测定至少6N/cm的强度。
11.一种层压材料,所述层压材料可通过前述权利要求中任一项的方法获得。
12.一种安全文件,所述安全文件包括权利要求11的层压材料。
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EP07116829A EP2042576A1 (en) | 2007-09-20 | 2007-09-20 | Security laminates with interlaminated transparent embossed polymer hologram. |
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CN200880107882A Pending CN101821346A (zh) | 2007-09-20 | 2008-09-19 | 具有插于层间的透明的压纹聚合物全息图的安全层压物 |
CN200880108736.3A Expired - Fee Related CN101815767B (zh) | 2007-09-20 | 2008-09-19 | 具有层间层压透明模压聚合物全息图的安全层压材料 |
Family Applications Before (1)
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CN200880107882A Pending CN101821346A (zh) | 2007-09-20 | 2008-09-19 | 具有插于层间的透明的压纹聚合物全息图的安全层压物 |
Country Status (4)
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US (2) | US8435725B2 (zh) |
EP (2) | EP2042576A1 (zh) |
CN (2) | CN101821346A (zh) |
WO (2) | WO2009037334A1 (zh) |
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- 2008-09-19 WO PCT/EP2008/062495 patent/WO2009037330A1/en active Application Filing
- 2008-09-19 US US12/672,964 patent/US20110266788A1/en not_active Abandoned
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Also Published As
Publication number | Publication date |
---|---|
US8435725B2 (en) | 2013-05-07 |
EP2042576A1 (en) | 2009-04-01 |
WO2009037334A1 (en) | 2009-03-26 |
US20110266788A1 (en) | 2011-11-03 |
CN101815767A (zh) | 2010-08-25 |
US20110204616A1 (en) | 2011-08-25 |
WO2009037330A1 (en) | 2009-03-26 |
EP2203533A1 (en) | 2010-07-07 |
CN101821346A (zh) | 2010-09-01 |
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