CN102015780B - 用水性2k涂料组合物涂布的基材和制品 - Google Patents

用水性2k涂料组合物涂布的基材和制品 Download PDF

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Publication number
CN102015780B
CN102015780B CN200980115969.0A CN200980115969A CN102015780B CN 102015780 B CN102015780 B CN 102015780B CN 200980115969 A CN200980115969 A CN 200980115969A CN 102015780 B CN102015780 B CN 102015780B
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base material
water dispersible
carbodiimide
coating
goods
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CN102015780A (zh
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R·R·阿穆布罗斯
A·M·沙瑟尔
M·A·M·福瑞
周宏英
G·J·麦克拉姆
I·G·施温德曼
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PPG Industries Ohio Inc
PPG Industries Inc
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PPG Industries Inc
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Abstract

公开了至少部分地用水性涂料组合物涂覆的可压缩基材，所述组合物包含至少一种碱中和的含活性氢的成膜树脂和能够与所述成膜树脂反应以形成交联膜的水分散性碳二亚胺交联剂。另外公开了具有至少部分地用上述涂料涂覆的至少两个不同挠性基材的制品。

Description

用水性2K涂料组合物涂布的基材和制品
交叉引用
这是2002年9月17日提交的美国专利申请10/245,028；2004年12月23日提交的美国专利申请11/020,921；2005年7月1日提交的美国专利申请11/172,718和2006年8月2日提交的美国专利申请11/461,844的部分继续申请。 
发明领域
本发明涉及至少部分地用具有碳二亚胺交联剂的碱中和的水性涂料组合物涂覆的基材和制品。 
发明背景 
诸如织物、热塑性聚氨酯、乙烯-乙酸乙烯酯泡沫和皮革之类的许多基材具有相当大的挠性。往往希望用涂料涂覆这些基材以改善外观、耐水性、耐化学品性、耐划伤性、耐紫外光性和/或耐久性。还可能希望涂覆或者“装饰”这些基材以提供改善的外观、施加图案等等。改善这些性能的许多涂料为适合用于硬性基材上的硬性涂料。当将硬性涂料、例如丙烯酸类涂料施涂于挠性基材上时，所述涂料经常会裂开以及当基材被弯曲时从基材上剥落。因此，希望适合用于挠性基材上的挠性涂料。 
此外，一种或多种挠性基材常常被作为制品中的不同部件组合。经常希望在这些不同的部件之间保持颜色均一性。然而，当由不同种类的材料制成所述部件时，可能难以在组装所述部件时提供制品的均一视觉外观。 
例如，鞋类如运动鞋经常包含不同种类的材料，其包括天然皮革、合成皮革、乙烯基树脂、织物、泡沫和/或橡胶。常规地将不同的涂料 组合物施涂于每一类基材上。例如，可能将一类涂料施涂至鞋的天然皮革鞋面部件，和可能将另一类涂料施涂至该鞋的合成皮革鞋面部件。此外，通常将颜料引入所述鞋的泡沫夹层以便为该夹层赋予颜色和/或在鞋的鞋面部件和夹层之间提供均一性和/或颜色协调。这样使用多种专门的涂料和颜料可能造成相对复杂且昂贵的制造工艺、库存问题以及还可能产生对不同涂料的“颜色匹配”的需要。 
颜色匹配是使多于一种涂料的视觉特性“匹配”以使得两种或更多种涂料产生相同或基本上相同的外观的过程。当例如用两种不同涂料涂覆同一制品上的两种不同基材时，可能期望颜色匹配。当试图确定与预先涂覆的制品或部件匹配的涂料时也可能期望颜色匹配。例如，机动车车身车间常常用经选择而匹配原始车身漆的颜色的涂料组合物为车身的修补部分上漆；这些经颜色匹配的涂料往往具有与原始涂料不同的组成，并且可能包含明显不同种类的涂料，例如空气固化的涂料vs.热固化的涂料。 
虽然在一些观察和照明条件下经颜色匹配的部件可能具有基本上相同的外观，但是当改变观察角度时、当改变光源的光谱分布时和/或当涂层已老化时，它们可能不会保持相同的外观。例如，一些经颜色匹配的部件可能在日光条件下具有相同的外观，但是可能在荧光和/或白炽灯照明下不匹配。当颜色匹配依赖于照明或观察条件时，这种匹配称为有条件的或“条件配色(metameric)的”。 
将期望提供能够涂覆制品的各种不同种类的基材并同时消除进行颜色匹配的需要的涂料组合物。 
发明概述 
本发明涉及至少部分地用水性涂料组合物涂覆的可压缩基材，所述组合物包含：a)至少一种碱中和的含活性氢的成膜树脂；和b)能够与所述成膜树脂反应以形成交联膜的水分散性碳二亚胺交联剂。 
本发明进一步涉及制品，其包括：a)包含第一挠性材料的第一基材；和b)包含与所述第一挠性材料不同的第二挠性材料的第二基材， 其中所述第一基材的至少一部分和所述第二基材的至少一部分用水性涂料组合物涂覆，所述组合物包含：i)至少一种碱中和的含活性氢的成膜树脂；和ii)能够与所述成膜树脂反应以形成交联膜的水分散性碳二亚胺交联剂。 
发明详述 
本发明涉及至少部分地用水性涂料组合物涂覆的可压缩基材。本发明所用的水性涂料组合物包含至少一种碱中和的含活性氢的成膜树脂。“碱中和的”以及类似术语表明将碱用于中和所述含活性氢的成膜树脂的至少一部分。合适的碱包括胺类和无机碱例如氢氧化锂和氢氧化钾。合适的胺类包括氨以及任何伯胺、仲胺和叔胺。叔胺是特别合适的。 
碱可以以将所述含活性氢的成膜树脂中和60-170％所需的量存在于所述水性涂料组合物中。100％中和意味着碱与酸的摩尔比为1∶1，70％中和意味着碱与酸的摩尔比为7∶10。 
“含活性氢的”以及类似术语表明所述成膜树脂具有能够与碳二亚胺基团反应的基团，例如羧基、醇羟基、酚羟基和/或硫醇。合适的含活性氢的成膜树脂包括聚酯、聚氨酯、(甲基)丙烯酸类聚合物、聚酰胺、聚碳酸酯和/或聚醚。在本发明中用作成膜树脂的聚合物可以经制备具有未反应的羧酸基团以赋予酸官能性。 
合适的(甲基)丙烯酸类聚合物包括含羧酸基以及硫和磷的酸基团的共聚物。这些(甲基)丙烯酸类聚合物和制备它们的方法是本领域公知的。例如，可以由酸单体和一种或多种(甲基)丙烯酸烷基酯合成这些(甲基)丙烯酸类聚合物。合适的酸单体包括：(甲基)丙烯酸、马来酸、富马酸、巴豆酸、衣康酸、甲基丙烯酸2-磺基乙基酯、2-丙烯酰胺基-2-甲基-1-丙烷磺酸、(甲基)丙烯酰胺基甲基膦酸和(甲基)丙烯酸2-磷酰乙基酯。在碱中和性化合物的存在下，这些酸基团的存在促进将所述丙烯酸类聚合物分散在水中。还可以将马来酸的单烷基酯、富马酸的单烷基酯和衣康酸的单烷基酯用于合成所述丙烯酸类聚合 物。如同本领域技术人员将会意识到的并且对它们而言常规的那样，(甲基)丙烯酸包括丙烯酸和对等的甲基丙烯酸两者；对于具有前缀“(甲基)”的其它化合物而言也是如此。 
合适的(甲基)丙烯酸烷基酯包括在烷基中含有1-30个碳原子、例如在烷基中含有4-18个碳原子的脂族或环脂族烷基酯。(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己基酯和(甲基)丙烯酸羟基乙基酯均为合适的(甲基)丙烯酸烷基酯的实例。 
合适的(甲基)丙烯酸类聚合物另外包括由上述单体中的一种与下列可聚合的烯键式不饱和单体中的一种或多种合成的共聚物：乙烯基芳族化合物如苯乙烯和乙烯基甲苯；腈类如(甲基)丙烯腈；酰胺类如(甲基)丙烯酰胺；卤代乙烯和偏二卤乙烯如氯乙烯；和偏二氯乙烯以及乙烯基酯类如乙酸乙烯酯。 
可以在本发明中用作成膜树脂的聚酯和醇酸树脂以及制备它们的方法是本领域公知的。例如，可以经由多元醇和多元羧酸的缩合制备聚酯。合适的多元醇包括乙二醇、丙二醇、丁二醇、1，6-己二醇、新戊二醇、二甘醇、甘油、三羟甲基丙烷和季戊四醇。合适的多元羧酸包括琥珀酸、己二酸、壬二酸、癸二酸、马来酸、富马酸、邻苯二甲酸、四氢化邻苯二甲酸、六氢化邻苯二甲酸和偏苯三酸。 
还可以由硫和/或磷的酸形成聚酯和醇酸树脂，如同本领域公知的。合适的硫和磷的酸包括2-膦酰基丁烷-1，2，4-三羧酸和5-磺基间苯二甲酸。 
可以用于本发明成膜树脂中的聚氨酯以及制备它们的方法是本领域公知的。例如，可以如下制备聚氨酯：使聚酯多元醇、聚碳酸酯多元醇、聚醚多元醇或丙烯酸类多元醇与多异氰酸酯和酸官能的多元醇反应以使得OH/NCO比例大于1∶1，用胺将其中和，然后分散入水中。作为选择，可以如下制备聚氨酯：使所述多元醇、异氰酸酯和酸官能的多元醇与异氰酸酯反应以使得OH/NCO当量比小于1∶1，将预聚物分散在含有异氰酸酯扩链剂和中和性胺的水中。以这种方式制备的聚氨 酯一般由于其固有的挠性而是优选的。合适的多异氰酸酯包括脂族多异氰酸酯、芳族多异氰酸酯以及它们的混合物。 
用于本发明的含活性氢的成膜树脂可以具有大于1,000的重均分子量和大于500的数均分子量，二者都由采用聚苯乙烯标准物的凝胶渗透色谱法测定。本发明所用的含活性氢的成膜树脂可以具有5mgKOH/g-738mg KOH/g、例如10mg KOH/g-200mg KOH/g、或10mgKOH/g-45mg KOH/g的酸值或者在任何这些范围任内的数值的任何其它组合。 
所述含活性氢的成膜树脂可以以10-100wt％、例如45-85wt％存在于所述水性涂料组合物中，其中所述重量百分比由所述含活性氢的成膜树脂中的树脂固体与所述组合物的全部树脂固体之比确定。 
用于本发明的水性涂料组合物还包含水分散性碳二亚胺交联剂。“水分散性的”以及类似术语在连同碳二亚胺一起使用时，是指溶解或分散于水相中的碳二亚胺。为了在本发明中使用某些碳二亚胺，可能必须改性所述碳二亚胺以使它们成为水分散性的。用于改性碳二亚胺以使它们成为水分散性的技术是本领域公知的。 
合适的水分散性碳二亚胺交联剂包括具有如下一般结构的碳酸的脂族和/或芳族二氮类似物：RN＝C＝NR1，其中R和R1独立地是氢、脂族或芳族基团。所述脂族基团包括烷基链以及可以包括诸如二环己基碳二亚胺之类的碳二亚胺。还可以使用低聚或聚合的碳二亚胺交联剂。 
水分散性碳二亚胺交联剂的制备是本领域公知的。可以通过将少量的胺例如二甲基氨基丙胺、和烷基磺酸盐或硫酸盐引入碳二亚胺结构而制备合适的水分散性碳二亚胺交联剂。还可以通过将聚环氧乙烷或聚环氧丙烷引入碳二亚胺结构而制备合适的水分散性碳二亚胺。 
合适的水分散性碳二亚胺可商购获得。例如，可从Union Carbide购得的UCARLINK XL-29SE、XL-20和可从Nisshinbo Industries，Inc.购得的CARBODILITE VO2-L2可以用于本发明。 
水性介质中分散的碳二亚胺的量可以是基于该水性分散体的重量至少1wt％，例如基于该水性分散体的重量2-60wt％。 
在用于本发明的水性涂料组合物中，所述水分散性碳二亚胺交联剂可以基于全部树脂固体以5-50、例如10-35或15-25wt％树脂固体存在。 
任选地，用于本发明的水性涂料组合物包含水分散性多异氰酸酯。“水分散性”以及类似术语在连同多异氰酸酯一起使用时，是指溶解或分散于水相中的多异氰酸酯。为了在本发明中使用某些多异氰酸酯，可能必需改性所述多异氰酸酯以使它们成为水分散性的。用于改性多异氰酸酯以使它们成为水分散性的技术是本领域公知的。 
合适的水分散性多异氰酸酯包括多官能异氰酸酯和二异氰酸酯。合适的多官能异氰酸酯包括众多单体和低聚的多官能异氰酸酯。实例包括3分子二异氰酸酯的缩二脲加合物、至少三官能多元醇与每羟基当量1分子二异氰酸酯的加合物、含异氰脲酸酯基的化合物、1，3，5-三异氰酸基苯、2，4，6-三异氰酸基甲苯、和异氰酸酯二聚体(uretdione)。 
本发明的水性涂料可以进一步包含一种或多种在本领域中典型地添加的添加剂。所述添加剂可以包括着色剂、增塑剂、抗氧化剂、受阻胺光稳定剂、UV光吸收剂和稳定剂、表面活性剂、流动控制剂、触变剂、填料、有机助溶剂、反应性稀释剂、催化剂、研磨载体、和其它常规辅料。 
本文使用的术语“着色剂”是指任何赋予所述组合物颜色和/或其它不透明性和/或其它视觉效果的物质。着色剂可以以任何合适的形式加入到所述涂料中，例如离散颗粒、分散体、溶液和/或薄片。可以在本发明的涂料中使用单一着色剂或者两种或更多种着色剂的混合物。 
着色剂的实例包括颜料、染料和调色料(tints)，例如在涂料工业中使用和/或在Dry Color Manufacturers Association(DCMA)中列出的那些，以及特殊效果组合物。着色剂可以包括例如在使用条件下不可溶但可润湿的细粒状固体粉末。着色剂可以是有机或无机的并且可以是聚集或非聚集的。可以通过研磨或简单混合将着色剂引入涂料中。可以通过利用研磨载体例如丙烯酸类研磨载体将着色剂引入 涂料中，所述研磨载体的使用是本领域技术人员熟知的。 
颜料和/或颜料组合物的实例包括，但不限于，咔唑二 嗪粗颜料、偶氮、单偶氮、双偶氮、萘酚AS、盐型(色淀)、苯并咪唑酮、缩合物、金属络合物、异二氢吲哚酮、异二氢吲哚和多环酞菁、喹吖啶酮、苝、紫环酮、二酮吡咯并吡咯、硫靛、蒽醌、靛蒽醌、蒽嘧啶、黄烷士酮、皮蒽酮、蒽嵌蒽醌、二 嗪、三芳基碳 、喹酞酮颜料、二酮吡咯并吡咯红(“DPPBO红”)、二氧化钛、炭黑、碳纤维、石墨、其它导电颜料和/或填料、和它们的混合物。术语“颜料”和“着色填料”可互换地使用。 
染料的实例包括但不限于溶剂基和/或水性的那些，例如酸性染料、偶氮染料、碱性染料、直接染料、分散染料、活性染料、溶剂染料、硫化染料、媒介染料，例如钒酸铋、蒽醌、苝铝、喹吖啶酮、噻唑、噻嗪、偶氮、靛类、硝基、亚硝基、噁嗪、酞菁、喹啉、茋和三苯基甲烷。 
调色料的实例包括，但不限于，分散在水基或可水混溶的载体中的颜料例如可从Degussa，Inc.商购获得的AQUA-CHEM 896和可从Accurate Dispersions division of Eastman Chemical，Inc.商购获得的CHARISMA COLORANTS和MAXITONER INDUSTRIAL COLORANTS。 
如上所述，着色剂可以呈分散体形式，包括但不限于呈纳米颗粒分散体形式。纳米颗粒分散体可以包括一种或多种高度分散的纳米颗粒着色剂和/或着色剂颗粒，其产生所需的可见颜色和/或不透明性和/或视觉效果。纳米颗粒分散体可以包括粒径小于150nm例如小于70nm或小于30nm的着色剂例如颜料或染料。可以通过将原料有机或无机颜料与粒径小于0.5mm的研磨介质一起碾磨而产生纳米颗粒。纳米颗粒分散体实例和它们的制造方法在美国专利号6,875,800B2中进行了描述，该文献通过引用并入本文。纳米颗粒分散体也可以通过结晶、沉淀、气相冷凝和化学磨损(即，部分溶解)产生。为了使纳米颗粒在涂料中的再聚集最小化，可以使用树脂涂覆的纳米颗粒的分散体。本文所使用的“树脂涂覆的纳米颗粒的分散体”是指其中分散了离散 “复合微粒”的连续相，该“复合微粒”包含纳米颗粒和在该纳米颗粒上的树脂涂层。树脂涂覆的纳米颗粒的分散体实例和它们的制造方法在2004年6月24日提交的美国专利申请公开2005-0287348 A1和2003年6月24日提交的美国临时申请号60/482,167以及2006年1月20日提交的美国专利申请号11/337,062中进行了描述，所述文献通过引用并入本文。着色剂还包括透明颜料例如可从Clariant购得的那些。 
可以使用的特殊效果组合物的实例包括产生一种或多种外观效应例如反射、珠光、金属光泽、磷光、荧光、光致变色、感光性、热致变色、随角异色(goniochromism)和/或颜色变化的颜料和/或组合物。另外的特殊效果组合物可以提供其它可察觉性能例如不透明性或纹理。在非限制性实施方案中，特殊效果组合物可以产生色移，以致当在不同角度观察涂层时涂层的颜色改变。颜色效果组合物的实例描述于美国专利No.6,894,086中，其通过引用并入本文。另外的颜色效果组合物可以包括透明涂覆的云母和/或合成云母、涂覆的二氧化硅、涂覆的氧化铝、透明液晶颜料、液晶涂料和/或其中干涉由材料内的折射指数差异引起而不归因于材料表面和空气之间的折射指数差异的任何组合物。 
在某些非限制性实施方案中，可以将当暴露于一种或多种光源时可逆地改变其颜色的光敏组合物和/或光致变色组合物用于本发明的涂料中。可以通过暴露于特定波长的辐射而使光致变色和/或光敏组合物活化。当组合物受到激发时，分子结构被改变并且该改变的结构显示与该组合物的原始颜色不同的新颜色。当除去对辐射的暴露时，该光致变色和/或光敏组合物可以恢复到静态，其中恢复组合物的原始颜色。在一种非限制性实施方案中，光致变色和/或光敏组合物可以在非激发态下是无色的而在激发态下显示颜色。完全的变色可以在数毫秒至若干分钟内出现，例如20秒至60秒。光致变色和/或光敏组合物的实例包括光致变色染料。 
在一种非限制性实施方案中，可以使光敏组合物和/或光致变色 组合物与聚合物和/或可聚合组分的聚合材料关联和/或至少部分地结合，例如通过共价键合。与其中光敏组合物可能迁移出涂料并且结晶到基材中的一些涂料相反，根据本发明的非限制性实施方案与聚合物和/或可聚合组分关联和/或至少部分地结合的光敏组合物和/或光致变色组合物具有最小程度的迁移出涂料的作用。光敏组合物和/或光致变色组合物的实例及其制备方法描述于2004年7月16日提交的美国申请No.10/892,919中，其通过引用并入本文。 
一般而言，着色剂可以以足以赋予期望的视觉和/或颜色效果的任何量存在。着色剂可以占本发明组合物的1-65wt％，例如3-40wt％或5-35wt％，其中重量百分比基于所述组合物的总重量。 
其它合适的涂料组分包括一种或多种改善表面触感和/或提高涂料的耐沾污性的质地增强剂(texture-enhancer)。在一种非限制性实施方案中，质地增强剂赋予涂层柔软触感。本文使用的术语“柔软触感”是指涂覆的基材在被触摸时显示出改变的触觉性质例如仿天鹅绒或皮革触感。质地增强剂可以是能够加入到涂料组合物中的添加剂，例如二氧化硅整平剂和/或蜡添加剂。二氧化硅整平剂的实例可以包括可从Degussa，Inc.购得的ACEMATT OK 412和ACEMATT TS 100。蜡添加剂的实例可以包括聚氧化四亚乙基(polytetraethylene oxide)、氟化蜡、聚乙烯蜡和天然蜡、例如石蜡和/或巴西棕榈蜡。在另一非限制性实施方案中，可以将质地增强剂引入聚氨酯树脂本身中。例如，可以使用将赋予聚氨酯更大的“软链段”的组分。实例包括可从Invista，Inc.以商品名TERATHANE 2000购得的聚四亚甲基醚二醇。 
如上所述，本发明涉及至少部分地用本文所述的水性涂料组合物中的一种或多种涂覆的可压缩基材。“可压缩基材”和类似术语是指能够经历压缩变形并且一旦停止压缩变形时恢复基本上相同形状的基材。术语“压缩变形”和类似术语是指在至少一个方向上至少暂时减小基材的体积的机械应力。可压缩基材是例如压缩应变为50％或更大、如70％、75％或80％或更大的基材。可压缩基材的具体实例包括含有泡沫以及填充有空气、液体和/或等离子体的聚合物囊的那些基材。“泡 沫”可以是包含开孔泡沫和/或闭孔泡沫的聚合物或天然材料。“开孔泡沫”是指包含多个互连气室的泡沫；“闭孔泡沫”是指包含离散的封闭孔的泡沫。泡沫的实例包括但不限于聚苯乙烯泡沫、聚乙酸乙烯酯和/或共聚物、聚氯乙烯和/或共聚物、聚(甲基)丙烯酰亚胺泡沫、聚氯乙烯泡沫、聚氨酯泡沫、热塑性聚氨酯泡沫、以及聚烯烃类泡沫和聚烯烃共混物。聚烯烃类泡沫包括但不限于聚丙烯泡沫、聚乙烯泡沫和乙烯-乙酸乙烯酯(“EVA”)泡沫。EVA泡沫可以包括平坦片材或板材或模制EVA泡沫，例如鞋底夹层。不同类型的EVA泡沫可以具有不同类型的表面孔隙率。模制EVA可以包含致密的表面或“外皮”，而平坦片材或板材可以显示出多孔表面。 
本发明进一步涉及制品，其包含：a)包含第一挠性材料的第一基材；和b)包含与所述第一挠性材料不同的第二挠性材料的第二基材，其中所述第一基材的至少一部分和所述第二基材的至少一部分用水性涂料组合物涂覆，所述组合物包含：i)至少一种碱中和的含活性氢的成膜树脂；和ii)能够与所述成膜树脂反应以形成交联膜的水分散性碳二亚胺交联剂。所述水性涂料组合物可以是上述组合物中的任一种。 
术语“挠性基材”是指能够经受机械应力例如弯曲、拉伸等而没有显著的不可逆变化的基材。在某些实施方案中，挠性基材为如上所述的可压缩基材。其它挠性基材包括非刚性基材，例如织造和非织造的玻璃纤维、织造和非织造的玻璃、织造和非织造的聚酯、热塑性聚氨酯(TPU)、合成皮革、天然皮革、整饰过的天然皮革、整饰过的合成皮革、橡胶、聚氨酯弹性体、合成织物和天然织物。“织物”可以包括天然和/或合成织物如布(fabric)、乙烯基树脂和聚氨酯涂覆的布(fabrics)、网状物、网织品、软线(cord)、纱线等等，并且可以例如由帆布、棉、聚酯、KEVLAR、聚合物纤维、聚酰胺如尼龙等、聚酯如聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯等、聚烯烃如聚乙烯和聚丙烯等、人造丝、聚乙烯基聚合物如聚丙烯腈等、其它纤维材料、纤维素类材料等构成。 
在本发明的一种非限制性实施方案中，所述制品包括鞋类。本文 使用的术语“鞋类”包括体育和运动用鞋、礼服男鞋和女鞋、休闲男鞋和女鞋、童鞋、凉鞋、人字拖、靴子、工装靴、户外鞋类、矫形鞋、拖鞋等。鞋类部件的实例包括鞋底、夹层、鞋面材料和衬里。作为具体的非限制性实例，运动鞋可能包含天然皮革、合成皮革和/或织物鞋面，以及EVA泡沫夹层。 
本文使用的术语“涂料”是指在基材上形成基本上连续的层或膜的材料。可以将涂料以任何期望的厚度、例如适合实现期望的机械和/或视觉效果的厚度施涂于包括但不限于织物的挠性基材上。在一种非限制性实施方案中，当将涂料保持在挠性基材的外表面上的同时，涂料可能渗入挠性基材的表面的一部分。在某些实施方案中挠性基材的外表面被全部或部分涂覆。“外表面”是指当所述挠性基材组装入成品时至少部分地被暴露的表面。与织物使用相关的实例包括服装的外表面或地板覆盖材料的外表面。与鞋类相关的实例包括鞋底夹层的那部分或成品鞋中(也就是当将所有鞋部件组装时)可见的其它鞋部件。因而外表面不是被另一部件覆盖并由此隐藏的表面，除该表面的至少一部分保持未被隐藏和/或在成品的外部或外侧上可见之外。 
本发明所用的涂料组合物适合于制备任何类型的涂料，并且特别适合作为基材上的面涂层。在一种实施方案中，本发明的涂料可以用作单一施涂涂层或单层涂层。在另一实施方案中，所述涂料可以用作多层涂层中的一层或多层，其中每一涂层可以含有相同或不同的添加剂。本发明的涂料可以单独或者与其它涂料组合使用。在某些实施方案中，可能期望在待涂覆的基材上使用附着促进层。在某些实施方案中，可能期望以某种设计或图案向基材施涂一种或多种上述涂料。所述设计和/或图案可以使用一种颜色、或者两种或更多种颜色的上述涂料。在某些实施方案中可能期望向基本上全部的基材施涂一种或多种涂料。如此，可以赋予基材一种或多种颜色。 
可以用任何已知的方式例如刷涂、喷涂、辊轧、辊涂、狭缝式涂布和/或浸涂，将根据本发明使用的涂料组合物施涂于包括织物在内的挠性基材上。还可以通过任何已知的染色、印刷或着色方式，例如丝 网印刷、喷墨印刷、喷射染色、射流注射染色(jet injection dying)、转印等，施涂所述涂料。上述方式可以是计算机控制的，如同本领域技术人员所理解的那样，而且可以包括按像素对基材施加颜色，例如在美国专利6,792,329和6,854,146中讨论的，这两篇专利都通过引用整体并入。“像素”是图案中或者基材上的能够以给定的颜色单独地分配或寻址的最小区域或位置。例如，可以将上述方式用于印刷图案和/或颜色至基材上；基材上的“图案”可以意味着通过向基材施加着色剂(典型地以预定方式)，该基材已经被着色，例如逐个像素地着色。在用于染色、印刷或者其它赋予基材颜色的各种方法中，可以使用计算机和数字设计软件以产生输入到数控染色、印刷或着色设备中的数字设计；上述设备可商购获得并且可以按照厂商说明书使用。 
这些涂料的固化可以包括在环境温度或升高的温度下闪蒸，接着热烘焙，以便获得最佳的性能。本发明的涂料被典型地沉积在挠性基材上至0.1-3密尔的厚度。在一种实施方案中，涂料被沉积至0.5-1.0密尔的厚度。 
用于本文时，除非另有明确说明，所有数字例如表示值、范围、量或百分比的那些可以像前面有措辞“约”一样来理解，即使该术语没有明确出现也一样。另外，本文列出的任何数值范围希望包括其中所含的所有子范围。单数形式包括复数形式，反之亦然。例如，尽管本文中提及“一种”可压缩基材、“一种”碱中和的含活性氢的成膜树脂和“一种”碳二亚胺，但是可以使用这些以及任何其它组分各自中的一种或多种的混合物。本文使用的术语“聚合物”是指低聚物以及均聚物和共聚物，前缀“聚”是指二或更多。包括以及类似的术语是指包括但不限于。 
实施例
将通过下列非限制性实施例进一步说明本发明。表1包含本发明的水性涂料组合物的配方数据。表2描述了在示例性的涂料体系中使用的交联剂体系。表3列出各种交联的水性涂料体系的适用期。 
示例性的本发明涂料组合物通过取100g市售的底涂剂组合物然后加入一定量的碱而制备。采用胺作为示例性组合物中的碱。然后将底涂剂与胺混合以形成本发明的涂料组合物。实施例的具体组成信息在下面示于表1。 
表1.本发明的水性涂料组合物 
  实施例   T408Black BC1   二甲基乙醇胺2   ％中和的5   近似pH6
  1   100g   无   77.1   7.24
  2   100g   0.10g   93.2   8.28
  3   100g   0.20g   109.2   8.58
  4   100g   0.25g   117.2   8.76
  5   100g   0.30g   125.2   8.92
  6   100g   0.35g   133.3   9.04
  7   100g   0.40g   141.3   9.10
  8   100g   0.50g   157.3   9.24
    T413Blue BC3      
  9   100g   无   95.2   7.71
  10   100g   0.20g   122.0   8.70
  11   100g   0.50g   162.0   9.17
    T400White BC4      
  12   100g   无   90.9   8.25
  13   100g   0.20g   113.6   8.74
  14   100g   0.50g   147.6   9.25
1T408 黑色底涂剂，可购自PPG Industries，Inc. 
2二甲基乙醇胺为可购自Huntsman Petrochemicals.的羟基胺 
3T413 蓝色底涂剂，可购自PPG Industries，Inc. 
4T400 白色底涂剂，可购自PPG Industries，Inc. 
5底涂剂中的酸当量除以胺当量乘以100 
6用T408 黑色底涂剂形成不同的两组试样。所述pH值仅用于一组数据。不同组试样中pH值之间的最大偏差为±0.27。 
表2.用于示例性涂料体系的交联剂体系 
将下列组分混合在一起以形成用于示例性涂料体系的交联剂体系。 
1可购自Bayer Corporation的多异氰酸酯产品 
2可购自Eastman Chemical Company的溶剂 
3可购自Union Carbide Corporation的碳二亚胺产品 
表3.示例性的水性涂料体系 
1由下列方法测定适用期。一开始，在容器中合并底涂剂和交联剂体系(时间＝0)。然后在不同的时间间隔(例如10分钟、25分钟、40分钟等)将容器翻倒以检验液体流动。将容器翻倒并且液体不再流动的时间记录作为适用期。 
结论
本发明提供具有良好适用期的水性涂料组合物。如上表3所示，本发明的交联水性涂料组合物的适用期可以通过提高水性涂料组合物的％中和而增加。 
实施例A 
如下制备水性聚碳二亚胺树脂“A”： 
表4
 成分     重量份
    进料#1  
 Desmodur W1     16.68
 环磷烯氧化物(Phospholene oxide)     0.25
    进料#2  
 二月桂酸二丁基锡     0.0015
    进料#3  
 N-甲基吡咯烷酮     10.13
 乙二醇     0.62
    进料#4  
 Jeffamine M1000(XTJ-506)2     18.22
    进料#5  
 去离子水     51.84
 Abex 20053     2.25
1Desmodur W为出自Bayer Materials Science，LLC的亚甲基-双-(4-环己基二异氰酸酯) 
2Jeffamine M1000为出自Huntsman的聚醚胺(EO/PO摩尔比＝6.3，MW＝1000) 
3Abex 2005为出自Rhodia的专利阴离子表面活性剂 
将进料#1加入到2升四颈烧瓶中，该烧瓶配备电机驱动的不锈钢搅拌叶片、水冷式冷凝器、氮气入口以及具有通过温度反馈控制装置连接的温度计的加热套。将烧瓶内容物加热到140℃并且保持在该温度直至通过滴定测量异氰酸酯当量＞350eq/g为止。然后将温度降至95℃并且加入进料#2。用10分钟加入进料#3并且将反应混合物保持在90-100℃直至NCO当量停在约1300eq/g为止。加入进料#4并且将混合物保持在90-100℃直至IR光谱表明不存在NCO特征谱带。将批料冷却至60-65℃，在保持温度低于65℃的同时用20分钟向反应烧瓶中加入已经预热到60-65℃的进料#5。 
聚碳二亚胺分散体的试样在120°F加温室内放置4周，树脂保持分散。 
实施例15 
制备热固性水性组合物，其包括含羧酸基的聚氨酯和实施例A的聚碳二亚胺。由下列成分制备该组合物。 
1如下制备聚氨酯分散体：在甲乙酮(MEK)溶剂中使异佛尔酮二异氰酸酯与聚醚二醇(POLYMEG 2000)和二羟甲基丙酸反应(2.85∶0.95∶1.27当量比)，从而产生NCO当量为2663且酸值为21.1的NCO-预聚物。在水中用己二酸二酰肼使NCO预聚物扩链并且用二甲基乙醇胺部分中和以及真空气提MEK，从而产生34.66wt％树脂固体的分散体。 
2出自Dayglo Color Corp.的橙色颜料 
3出自Goldschmidt Chemical的硅流动添加剂 
4出自BYK Chemie的流变剂 
5出自BYK Chemie的脱气剂 
如下提及的将所述热固性组合物喷涂于基材上，在170℃固化20分钟以得到膜厚约1密尔的固化涂层。测试该涂覆的基材的挠性和耐压缩性。测试结果在下面报道： 
  实施例   压缩1   挠性2
  15   合格   大于40,000
1压缩试验为NIKE公司设计的试验(KIM压缩)，其模拟压缩运动鞋的震动支柱(shok column)的上下跑步动作测量重复压缩。将如上所述涂覆的、大约2.5平方厘米且厚2.5厘米的挠性聚氨酯基材放在固定器中，该固定器正上方的板冲击试样至材料被压缩其原始高度50％的程度。压缩后的尺寸因此将是大约2.5×2.5×1.75cm。冲击/压缩重复每秒5-10次并且持续直到涂层不合格或者计数达到100,000次循环为止。一次循环是一次压缩/一次松弛，两次循环为两次压缩/两次松弛。 
2挠性试验也是NIKE公司设计的使用Bally挠度仪的试验。在试验中，将如上所述涂覆的、大约2.5平方厘米且厚2.5厘米的挠性聚氨酯基材放在夹具中，折叠90度(涂层侧在外)以模拟当用于跑步时运动鞋的鞋面所经受的弯曲。将试样进行20,000次折叠，检查涂层中的裂纹。如果没有显示裂纹，将试样再进行20,000次折叠并且再次检查涂层中的裂纹。继续测试直至涂层裂开为止。 

Claims (21)

1.至少部分地用水性涂料组合物涂覆的可压缩基材，所述组合物包含：
a.至少一种碱中和的含活性氢的成膜树脂，其包含通过如下制备的聚氨酯分散体：
(i)使多元醇、异氰酸酯和酸官能的多元醇与异氰酸酯以小于1∶1的0H／NCO当量比反应，由此形成异氰酸酯官能的预聚物；和
(ii)使所述异氰酸酯官能的预聚物分散在包含异氰酸酯扩链剂和中和性胺的水中，由此，形成所述聚氨酯分散体；
b.能够与所述成膜树脂反应以形成交联膜的水分散性碳二亚胺交联剂，其中所述水分散性碳二亚胺为水分散性低聚碳二亚胺和／或水分散性的聚合碳二亚胺，其中所述水分散性碳二亚胺交联剂是通过引入少量的胺而制备的；
c.流动控制剂；和
d.水分散性多异氰酸酯。
2.权利要求1的基材，其中所述碱中和的含活性氢的成膜树脂的总中和值为100—200。
3.权利要求1的基材，其中所述含活性氢的成膜树脂具有大于500的数均分子量，这是采用聚苯乙烯标准物通过凝胶渗透色谱法测定的。
4.权利要求1的基材，其中所述基材包括泡沫。
5.权利要求4的基材，其中所述泡沫包括乙烯-乙酸乙烯酯泡沫。
6.权利要求4的基材，其中所述泡沫包括热塑性聚氨酯泡沫。
7.权利要求1的基材，其中所述基材包括织物。
8.权利要求1的基材，其中所述基材包括填充有空气的聚合物囊。
9.包括权利要求4的基材的鞋类。
10.制品，其包含：
a)包含第一挠性材料的第一基材；和
b)包含与所述第一挠性材料不同的第二挠性材料的第二基材，
其中所述第一基材的至少一部分和所述第二基材的至少一部分用水性涂料组合物涂覆，所述组合物包含：
i)至少一种碱中和的含活性氢的成膜树脂，其包含通过如下制备的聚氨酯分散体：
使多元醇、异氰酸酯和酸官能的多元醇与异氰酸酯以小于1∶1的OH／NCO当量比反应，由此，形成异氰酸酯官能的预聚物；和
使所述异氰酸酯官能的预聚物分散在包含异氰酸酯扩链剂和中和性胺的水中，由此，形成所述聚氨酯分散体；
i i)能够与所述成膜树脂反应以形成交联膜的水分散性碳二亚胺交联剂，其中所述水分散性碳二亚胺为水分散性低聚碳二亚胺和／或水分散性聚合的碳二亚胺，其中所述水分散性碳二亚胺交联剂是通过引入少量的胺而制备的，和
iii)流动控制剂；和
iv)水分散性多异氰酸酯。
11.权利要求10的制品，其中所述第一和第二基材独立地包括天然皮革、合成皮革、乙烯基树脂、尼龙、热塑性聚氨酯、布、泡沫和／或橡胶。
12.权利要求10的制品，其中所述第一基材包括泡沫以及第二基材包括合成和／或天然皮革。
13.权利要求10的制品，其中所述涂料进一步包含着色剂。
14.权利要求10的制品，其中所述制品为鞋类。
15.权利要求14的制品，其中所述鞋类为运动鞋。
16.权利要求10的制品，其中所述第一和／或第二基材包括填充有空气的聚合物囊。
17.包括权利要求8的基材的鞋类。
18.权利要求1的可压缩基材，其中所述水分散性多异氰酸酯选自3分子二异氰酸酯的缩二脲加合物、至少三官能多元醇与每羟基当量1分子二异氰酸酯的加合物、含异氰脲酸酯基的化合物、1，3，5-三异氰酸基苯、2，4，6-三异氰酸基甲苯、和异氰酸酯二聚体。
19.权利要求10的制品，其中所述水分散性多异氰酸酯选自3分子二异氰酸酯的缩二脲加合物、至少三官能多元醇与每羟基当量1分子二异氰酸酯的加合物、含异氰脲酸酯基的化合物、1，3，5-三异氰酸基苯、2，4，6-三异氰酸基甲苯、和异氰酸酯二聚体。
20.权利要求1的可压缩基材，其中在所述水分散性碳二亚胺交联剂的制备期间加入的所述胺是二甲基氨基丙胺。
21.权利要求10的制品，其中在所述水分散性碳二亚胺交联剂的制备期间加入的所述胺是二甲基氨基丙胺。
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EP2260064A1 (en) 2010-12-15
KR20100125455A (ko) 2010-11-30
TW200946615A (en) 2009-11-16
WO2009120560A1 (en) 2009-10-01
US20130122223A1 (en) 2013-05-16
TWI441877B (zh) 2014-06-21
US8389113B2 (en) 2013-03-05
US9534141B2 (en) 2017-01-03
US20080176061A1 (en) 2008-07-24
US9688876B2 (en) 2017-06-27
KR101201637B1 (ko) 2012-11-15
US20130122229A1 (en) 2013-05-16
MX2010010577A (es) 2010-12-15
BRPI0906335A2 (pt) 2015-07-07

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