CN102124067A - 剥离材料 - Google Patents

剥离材料 Download PDF

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CN102124067A
CN102124067A CN2009801319454A CN200980131945A CN102124067A CN 102124067 A CN102124067 A CN 102124067A CN 2009801319454 A CN2009801319454 A CN 2009801319454A CN 200980131945 A CN200980131945 A CN 200980131945A CN 102124067 A CN102124067 A CN 102124067A
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adhesive article
article according
block copolymer
film
polyolefin block
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CN102124067B (zh
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杰弗里·O·埃姆斯兰德尔
乔治·J·克莱门茨
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3M Innovative Properties Co
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3M Innovative Properties Co
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Abstract

本专利申请涉及一种粘合剂制品，所述粘合剂制品包含压敏粘合剂层和与所述压敏粘合剂层接触的剥离层。所述剥离层包含聚烯烃嵌段共聚物。一般来讲，所述聚烯烃嵌段共聚物的密度不大于0.9g/cc。

Description

剥离材料
技术领域
本发明涉及剥离材料。例如，可用作压敏粘合胶带的剥离衬垫的材料。
背景技术
剥离表面在例如压敏粘合胶带行业中是熟知的，所提供的剥离表面可使得胶带从胶带卷退绕而不会使粘合剂粘在胶带背面。还可将剥离涂层涂覆到衬垫上，该衬垫充当压敏粘合转移胶带或双面胶带的载体，这两种胶带的两面都具有粘性。剥离表面还可用作供压敏粘合膜使用的剥离衬垫。
通常用于剥离表面和涂层的材料是有机硅组合物，因为这些组合物可以配制成提供从“高”剥离(即，用以退绕胶带的力非常低)到“低粘合性背胶”剥离(通常需要更大的力来退绕)的各种剥离水平。
有机硅剥离涂层的主要缺点是可能存在与之相关的污染。当工人操作带有机硅剥离涂层的胶带或衬垫时，有机硅可转移到他们的手部、工作手套或衣服上。有机硅还可从其手部转移到待喷漆的表面，从而引起诸如油漆对污染表面的粘合较弱以及有机硅所在表面区域的油漆不润湿之类的问题。另外，电子器件制造商通常不使用有机硅以避免制造过程中出现污染。此外，有机硅剥离材料往往较昂贵，并且带有机硅涂层的材料难以回收。另外，通常有机硅涂层需要额外的工序，例如通常在第二步将其涂覆在现有基底上。因而增加了制造成本。
聚乙烯也已被用作剥离材料，并可涂覆在牛皮纸上形成剥离衬垫，或者可用作单层膜，或者可用作具有与基层共挤出或层合的聚乙烯(例如高密度聚乙烯等)的多层膜。更高密度的聚乙烯只限于在某些粘合剂中使用，并已发现其不适合极强力的压敏粘合剂，因为聚乙烯和粘合剂之间的粘合力很强，以致难以开始对衬垫的去除。当试图将粘合剂从衬垫分离时，由于剥离力较高，粘合剂和/或衬垫可能还会被损坏。
一些聚烯烃聚合物和无规聚烯烃共聚物也被用作剥离材料。另外，这些共聚物共混有聚乙烯。将聚乙烯添加到这些聚烯烃共聚物中导致产生增高的并且不期望的剥离值。一直需要一种受控剥离衬垫，以用于不具有有机硅剥离层的压敏粘合剂。
发明内容
本专利申请涉及一种粘合剂制品，其包含压敏粘合剂层和与压敏粘合剂层接触的剥离层。该剥离层包含聚烯烃嵌段共聚物。一般来讲，聚烯烃嵌段共聚物的密度不大于0.9g/cc。
具体实施方式
在本专利申请中，可用于剥离层的材料为烯烃嵌段共聚物。合适的α-烯烃包括1-丁烯、1-己烯、1-辛烯以及它们的组合。一般来讲，乙烯和1-辛烯的共聚物用作剥离层，适用于例如丙烯酸酯类压敏粘合剂。通常将这些共聚物描述为烯烃嵌段共聚物。一般来讲，共聚物的密度不大于0.90克/立方厘米(g/cc)。具体共聚物的密度不大于0.89g/cc，例如不大于0.88g/cc。在一些实施例中，共聚物的密度大于0.85g/cc，例如大于0.86g/cc。此类烯烃嵌段共聚物还导致减少了制品中静电的积聚和放电，其中烯烃嵌段共聚物布置在邻近压敏粘合剂的位置。
该共聚物通常具有高熔点。一些共聚物的熔点为约118℃至约122℃，例如约120℃。
已发现共聚物密度越低，则提供的剥离值也越低，并且可通过混合不同类型的共聚物来改变剥离值。合适的共聚物可以商品名INFUSE从Dow Chemical Company(Midland，Michigan)商购获得。
剥离层可包含100％的共聚物。在其他实施例中，剥离层包含共聚物与另外的聚合物的共混物。在一些实施例中，剥离层包含至少10重量％的共聚物，例如20重量％、50重量％的共聚物。可用于与共聚物共混的合适聚合物包括非嵌段聚烯烃共聚物，例如可以商品名EXACT从Exxon商购获得的那些。其他可用于该共混物的聚合物包括有机硅共聚物(例如美国专利申请No.2007-0148474中所述的聚二有机硅氧烷-聚乙二酰胺嵌段共聚物)以及有机硅聚脲聚合物(例如美国专利No.6919405中所述的那些)，所述专利以引用方式并入本文。
如本文所用，术语“剥离衬垫”、“衬垫”和“剥离膜”可互换使用。本文所述的剥离层是剥离膜的一部分。通过将共聚物挤出为不存在第二层的单个自支承膜，可制备剥离膜。膜厚度可在约0.1毫米至约0.4毫米的范围内，但厚度通常取决于诸如以下的因素：剥离衬垫中所需的强度、膜的易操作性、衬垫所需的柔韧性等。
还可通过将共聚物挤出到基材上或者通过将共聚物与一种或多种其他聚合物共挤出形成多层膜以提供额外的强度和/或硬度，从而制备剥离膜。合适基材的例子包括纤维素材料(例如纸张、织造/非织造织物)、膜(例如尼龙、聚酯、聚烯烃、丙烯腈丁二烯苯乙烯)、以及由诸如金属、陶瓷或塑料之类的材料制成的片状材料。还可使用合适的层合粘合剂将共聚物膜附连到基材。基材还可以是适用于热成形或真空成形的片状材料，使得可形成具有剥离表面的托盘，以固定带压敏粘合剂涂层的部分。
基层上共聚物膜的厚度应足以提供所需的剥离力，并且可小于自支承片材的厚度。
通常使用吹塑薄膜工艺或注塑薄膜工艺将膜挤出到冷却辊上，该冷却辊具有各种表面(例如糙面精整面或光面精整面)，从而在剥离衬垫上形成哑光表面或光亮表面。然后可按照以下的详细描述将膜结构化。可用材料处理或涂覆冷却辊，以防止挤出物粘在辊表面上，例如采用特氟隆或等离子体涂层。硅橡胶辊也可用于此用途。还可将该挤出膜挤出到冷却辊和平滑聚酯膜之间，以在一侧上形成光亮表面，在另一侧上形成哑光表面；或者将其挤出到两个聚酯衬垫之间，以形成两个光亮表面。另外，注塑薄膜工艺可包括取向步骤，例如拉幅处理。
可通过已知的共挤出工艺制备多层膜。可与共聚物共挤出的其他聚合物包括聚烯烃(例如聚丙烯、聚乙烯、聚丁烯以及它们的混合物)、尼龙材料和聚酯。与聚烯烃的共挤出尤其可用于制备可回收或可重复使用的衬垫。
在多层膜构造中，可对聚合物和共聚物进行选择，以呈现出有差别的剥离，即压敏粘合剂从一侧剥离所需的力显著低于另一侧。
在制备压敏粘合剂转移胶带的典型方法中，将粘合剂组合物涂覆在剥离衬垫上。然后将粘合剂固化以在衬垫上形成凝胶膜，并将带有粘合剂的剥离衬垫卷成一个大胶带卷。或者，可将粘合剂涂覆并固化在一个衬垫上，然后在转换加工前将其转移到另一个衬垫上。在一些实施例中，粘合剂不需要在涂覆后进行任何固化。于是，通过以下方式将涂覆有粘合剂的片材加工成窄胶带卷：切割大胶带卷并将窄幅胶带缠绕在胶带芯上供顾客使用。
在另一个实施例中，剥离衬垫可用于大幅形式的膜，例如图形膜。多种基底采用图形膜进行广告和促销展示。基底可包含聚合物片状材料，例如含丙烯酸类的膜、含聚(氯乙烯)的膜、含聚(氟乙烯)的膜、含氨基甲酸酯的膜、含三聚氰胺的膜、含聚乙烯醇缩丁醛的膜、含聚烯烃的膜、含聚酯的膜以及含聚碳酸酯的膜。对于图形膜而言，希望具有适应基底表面上的曲面、凹陷或凸起的膜，使得该膜可以围绕曲面或凸起进行拉伸或者可以向下压入到凹陷中同时不会使膜破裂或脱层(具有适形能力)。还希望具有可施加到不规则和/或不平表面上并且之后不会从基底表面脱层或剥离(起泡)的膜。此外，希望图形膜可成像(即具有印刷接收表面和/或图形)并且在户外应用时表现出优良的耐候性。粘合剂层位于图形膜上，而剥离衬垫位于与图形膜相对的粘合剂上。
粘合剂的例子包括在施加时对压力敏感的压敏粘合剂、热熔融或热活化粘合剂，例如在Handbook of Pressure-Sensitive Adhesives，Ed.D.Satas，2ndEdition，Von Nostrand Reinhold，New York，1989(《压敏粘合剂手册(第二版)》，D.Satas编辑，1989年)中公开的压敏粘合剂和任何其他类型的PSA。尤其可用于本发明的丙烯酸酯类PSA包括美国专利No.4,181,752(Clemens等人)和4,418,120(Kealy等人)、WO 95/13331以及Handbook of Pressure-Sensitive Adhesives，Ed.D.Satas，2nd Edition(《压敏粘合剂手册(第二版)》，D.Satas编辑)中描述的那些。
一般来讲，粘合剂层以一定剥离强度从剥离衬垫剥离，例如对于“高剥离”而言，需要剥离衬垫的膜可能要求在90英寸/分钟速度下的180°剥离强度小于30克/英寸。通常其他应用需要高于30克/英寸的剥离强度。例如，用于胶带的低粘合力背胶。其他实施例需要低剥离值，例如小于20克/英寸。
在一些实施例中，粘合剂为(甲基)丙烯酸粘合剂，其包含(甲基)丙烯酸酯和加固共聚单体。合适的丙烯酸酯单体包括丙烯酸-2-乙基己酯、丙烯酸异辛酯、丙烯酸异壬酯、丙烯酸正丁酯、丙烯酸癸酯、丙烯酸十二烷基酯、以及它们的混合物。优选的单体包括丙烯酸异辛酯、丙烯酸正丁酯、丙烯酸十八烷基酯、以及它们的混合物。
可用的加固共聚单体包括丙烯酸、甲基丙烯酸、衣康酸、丙烯酰胺、取代的丙烯酰胺、N-乙烯基吡咯烷酮。N-乙烯基己内酰胺、丙烯酸异冰片酯、乙酸乙烯酯和丙烯酸环己酯。优选的共聚单体包括N-乙烯基己内酰胺、取代的丙烯酰胺(例如N，N-二甲基丙烯酰胺)和丙烯酸异丁酯。
在实践本发明的过程中，使用合适的引发剂制备压敏粘合剂。所用引发剂的类型和数量适于进行所用类型的聚合反应，例如光引发剂(例如苯偶酰二甲基缩酮)的用量可为每100份紫外光固化粘合剂单体含约0.1至约5份，而用于溶液聚合的2，2′-二偶氮异丁腈的含量可为每100份单体含约0.1份至约2份。
压敏粘合剂还可包含添加剂，例如交联剂、增粘剂、增塑剂、填料、气体、发泡剂、玻璃或聚合物微球、二氧化硅、碳酸钙纤维、表面活性剂等等。所包含的添加剂的量应足以实现所需性质。
压敏粘合剂还可以包含热固性树脂，例如环氧树脂和氨基甲酸酯，它们可以在压敏粘合胶带施加到表面后被加热固化以形成热固性粘合剂。
压敏粘合剂可以通过本行业已知的方法制备，包括溶液聚合、辐射聚合(采用诸如电子束、γ辐射和紫外线辐射之类的方式)、乳液聚合等等。制备压敏粘合剂的方法在例如美国专利No.Re 24,906(Ulrich)中有所公开。
在多个实施例中，剥离衬垫被结构化，并且剥离衬垫上的结构可用来在粘合剂上形成结构的反相，从而得到结构化粘合剂。例如，对于粘合剂中的每一个凹槽而言，所述剥离衬垫都具有一个相对应的脊。这些脊突出于衬垫的参考平面，其中该衬垫的参考平面由各脊底部的衬垫表面来限定。每个脊的尺寸与粘合剂中每个凹槽的期望尺寸一致。例如，参考平面内的凹槽宽度与衬垫参考平面内的脊宽度一致。在包含突出于粘合剂结构化表面上的参考平面或真实壁的凸起的实施例中，剥离衬垫将包含相应的凹陷。剥离衬垫上的结构可以采用已为人们所知的数种方法来形成，这些方法包括：对衬垫进行压花以形成结构化表面，或在表面上印刷出某种结构。
可以通过将粘合剂与剥离衬垫的结构化表面相接触，来制成结构化的粘合剂层，从而形成粘合剂制品。粘合剂可以通过例如涂覆组合物(如溶液中的粘合剂组合物、分散体形式的组合物或热熔融组合物)或层合现有粘合剂层的方式接触结构化表面。在衬垫涂覆有剥离涂层的实施例中，粘合剂层位于所有剥离涂层之上。剥离衬垫上的结构向粘合剂层的一个主表面赋予某种结构。
剥离层可以涂覆在基层上，以形成剥离衬垫。例子包括纸张和聚合物膜(包括塑料)。衬垫基材可以是单层或者多层的。衬垫基材的具体实例包括，聚酯(例如聚对苯二甲酸乙二醇酯)、聚乙烯、聚丙烯(包括流延和双轴取向的聚丙烯)和纸(包括涂瓷土纸)。
通常，粘合剂的结构化表面与背衬相背。背衬可以是任何材料，这取决于粘合剂制品的预期用途。例如，在粘合剂制品用于大幅面图形(如宽度大于32英寸)的实施例中，背衬可以为适用于接纳图像的材料(如乙烯基背衬或聚烯烃背衬，其具有与粘合剂层相对的油墨接收层)。
在本专利申请中，可通过将粘合剂粘附到基底的方法来使用该粘合剂制品。在这类实施例中，将粘合剂的结构化表面施加到被粘基底上。粘合剂层的结构化表面发生变形，使得第一凹槽真实壁的绝大部分接触该基底，同时第二凹槽真实壁的绝大部分不接触该基底。就本专利申请的目的而言，当包含凹槽壁的粘合剂表面有超过50％的面积与被粘基底接触时，即认为壁的绝大部分与被粘基底接触。
可采用附加手段来将粘合剂制品施加到被粘基底上，这些附加手段例如为升高温度、施压、以及将粘合剂老化以使其流动。在一些实施例中，在第一凹槽的绝大部分接触到基底之后，第二凹槽壁的绝大部分也与该基底接触。
在一些实施例中，粘合剂制品的结构化表面上可具有附加结构，该附加结构叠加在本文所述的结构之上。这些附加结构的例子可见于(例如)美国专利No.5,141,790。附加结构可包括结构化粘合剂表面上的粘性或非粘性凸起，例如突出于参考平面或突出于粘合剂真实壁的那些凸起。
实例
这些实例仅用于示例性目的，并且无意于限制所附权利要求的范围。除非另外指明，实例中的所有份数、百分数、比率等均按重量计。
下面的聚合物用于实例中：
聚合物A：以商品名Exact 5181出售的非嵌段聚烯烃共聚物
聚合物B：以商品名Dow Infuse 9530.05出售的聚烯烃嵌段共聚物(密度＝0.887)
聚合物C：如美国专利申请No.2007-0148474所述的聚二有机硅氧烷-聚乙二酰胺嵌段共聚物。
聚合物D：以商品名Dow Infuse 9500.05出售的聚烯烃嵌段共聚物(密度＝0.877)
聚合物E：以商品名Dow Infuse 9507.15出售的聚烯烃嵌段共聚物(密度＝0.866)
聚合物F：以商品名Exxon 129.24出售的低密度聚乙烯
使用具有混合螺杆的3/4英寸Brabender实验室挤出机和表1所述材料制备膜。将这些实例熔化并迫使其通过6英寸的挤出流延膜平模头，从而形成熔融膜。然后使该熔融膜通过冷却辊层叠件，以使树脂冷却并固化成最终的成品膜。再将这些膜样品层合到具有丙烯酸类粘合剂的2密耳PVC膜上，此PVC膜可以商品名3M Scotchcal 7725-13从3M公司商购获得。
表1
 实例   组成
 比较例A   100％聚合物A
 1   90％聚合物A/10％聚合物B
 2   80％聚合物A/20％聚合物B
 3   70％聚合物A/30％聚合物B
 4   50％聚合物A/50％聚合物B
 5   50％聚合物A/45％聚合物B/5％聚合物C
 6   100％聚合物B
 7   95％聚合物B/5％聚合物C
  8   95％聚合物D/5％聚合物C
  9   100％聚合物D
  10   90％聚合物A/10％聚合物D
  11   80％聚合物A/20％聚合物D
  12   70％聚合物A/30％聚合物D
  13   50％聚合物A/50％聚合物D
  14   50％聚合物A/45％聚合物D/5％聚合物C
  15   95％聚合物E/5％聚合物C
  16   100％聚合物E
  17   90％聚合物A/10％聚合物E
  18   80％聚合物A/20％聚合物E
  19   70％聚合物A/30％聚合物E
  20   50％聚合物A/50％聚合物E
  21   50％聚合物A/45％聚合物E/5％聚合物C
然后在以下两个条件下测试该膜的粘合性：1)停留5分钟和2)在150℉烘箱中老化5天。使用180度剥离力以90英寸/分钟的速度在I-Mass测试装置上进行剥离测试。结果示于表2中。
表2
Figure BPA00001311115900081
Figure BPA00001311115900091
使用具有混合螺杆的3/4英寸Brabender实验室挤出机和表3所述材料制备膜。将这些实例熔化并迫使其通过6英寸的挤出流延膜平模头，从而形成熔融膜。然后使该熔融膜通过冷却辊层叠件，以使树脂冷却并固化成最终的成品膜。再将这些膜样品层合到具有2.5密耳厚聚乙烯背衬和0.8密耳厚粘合剂层的粘合膜上，该粘合剂层包含15.45％丙烯酸丁酯、64.25％丙烯酸异辛酯、16.8％丙烯酸十八烷基酯、2％丙烯酸和1.5％取代的二苯甲酮。在紫外线辐射下使该粘合剂交联。
 实例   组成
 比较例B   100％聚合物A
 22   50％聚合物A/50％聚合物B
 23   50％聚合物A/45％聚合物B/5％聚合物C
 24   100％聚合物B
 25   95％聚合物B/5％聚合物C
 26   95％聚合物D/5％聚合物C
 27   100％聚合物D
 28   50％聚合物A/50％聚合物D
 29   50％聚合物A/45％聚合物D/5％聚合物C
 30   95％聚合物E/5％聚合物C
 31   100％聚合物E
 32   50％聚合物A/50％聚合物E
 33   50％聚合物A/45％聚合物E/5％聚合物C
然后在以下三个条件下测试该膜的粘合性：1)在室温(25℃)下停留小于5分钟的时间，2)在120℉下停留10天以及3)在90℉和90％湿度下停留2周。结果示于表4中。
表4
Figure BPA00001311115900101
使用表5中详述的组成，按照与比较例A相同的方法制备比较例C和D。
表5
 实例   组成
 比较例C   60％聚合物A/40％聚合物F
 比较例D   80％聚合物A/20％聚合物F
将比较例C和D在室温(25℃)下老化24小时。使用180度剥离力以90英寸/分钟的速度在I-Mass测试装置上进行剥离测试。结果示于表6中。
表6
 实例   室温/24小时条件下的剥离力(克/英寸)
 比较例C   58
 比较例D   47
压印实例
使用以商品名Dow Infuse 9100出售的聚烯烃嵌段共聚物(密度＝0.877g/cm3)的剥离表面制备剥离衬垫。该衬垫采用3层吹塑薄膜共挤出生产线制备，其中气泡膜的外层为含有3％ Polyfil ABC5000防粘化合物的聚烯烃嵌段共聚物；芯层包含聚丙烯树脂(商品名Phillips Sumika HHC007)与线性低密度树脂(商品名Chevron D-143)的80/20共混物；气泡膜的内层包含PP/LLDPE与4％ Polyfil ABC5000防粘浓缩物的80/20共混物。压印所得剥离衬垫以在剥离表面中形成图案。然后用压敏粘合剂涂覆剥离表面。再将粘合剂从剥离衬垫去除。剥离衬垫上的图案劣化程度最低。粘合剂表面还保留了剥离衬垫的反相结构。
使用以商品名Exact 8201出售的非嵌段聚烯烃共聚物的剥离表面制备用作比较的剥离衬垫。该衬垫采用3层吹塑薄膜共挤出生产线制备，其中气泡膜的外层为含有3％ Polyfil ABC5000防粘化合物的非嵌段聚烯烃共聚物；芯层包含聚丙烯树脂(商品名Phillips Sumika HHC007)与线性低密度树脂(商品名Chevron D-143)的80/20共混物；气泡膜的内层包含PP/LLDPE与4％Polyfil ABC5000防粘浓缩物的80/20共混物。压印所得剥离衬垫以在剥离表面中形成图案。然后用压敏粘合剂涂覆剥离表面。再将粘合剂从剥离衬垫去除。剥离衬垫上的图案出现劣化。另外，由于剥离衬垫结构的劣化，粘合剂表面也出现劣化。
在不脱离本发明的范围和精神的前提下，本发明的各种修改和更改对本领域的技术人员而言将是显而易见的。应当理解，本发明并非意图受本文提出的示例性实施例和实例的不当限制，并且这种实例和实施例仅以举例的方式提出，本发明的范围旨在仅受下文提出的权利要求书的限制。

Claims (16)

1.一种粘合剂制品，包括：
压敏粘合剂层，
与所述压敏粘合剂层接触的剥离层，所述剥离层包含聚烯烃嵌段共聚物。
2.根据权利要求1所述的粘合剂制品，其中所述聚烯烃嵌段共聚物的密度不大于0.9g/cc。
3.根据权利要求1所述的粘合剂制品，其中所述聚烯烃嵌段共聚物的密度不大于0.89g/cc。
4.根据权利要求1所述的粘合剂制品，其中所述聚烯烃嵌段共聚物的密度大于0.85g/cc。
5.根据权利要求1所述的粘合剂制品，其中所述聚烯烃嵌段共聚物的密度大于0.86g/cc。
6.根据权利要求1所述的粘合剂制品，其中所述剥离层还包含聚二有机硅氧烷-聚乙二酰胺线性嵌段共聚物。
7.根据权利要求1所述的粘合剂制品，其中所述剥离层还包含密度不大于0.9的第二聚烯烃聚合物。
8.根据权利要求1所述的粘合剂制品，其中所述剥离层包含至少10重量％的所述聚烯烃嵌段共聚物。
9.根据权利要求1所述的粘合剂制品，其中所述剥离层包含至少20重量％的所述聚烯烃嵌段共聚物。
10.根据权利要求1所述的粘合剂制品，其中所述剥离层包含至少30重量％的所述聚烯烃嵌段共聚物。
11.根据权利要求1所述的粘合剂制品，其中所述剥离层包含至少50重量％的所述聚烯烃嵌段共聚物。
12.根据权利要求1所述的粘合剂制品，其中所述粘合剂层与所述剥离层之间的界面为结构化界面。
13.根据权利要求1所述的粘合剂制品，其中所述粘合剂为丙烯酸类粘合剂。
14.根据权利要求13所述的粘合剂制品，其中所述粘合剂包含丙烯酸十八烷基酯。
15.根据权利要求1所述的粘合剂制品，其中所述聚烯烃嵌段共聚物的熔点为约120℃。
16.一种制备剥离衬垫的方法，包括：
提供在第一表面上具有聚烯烃嵌段共聚物的剥离衬垫，以及
将所述剥离衬垫的所述第一表面结构化。
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