CN105283519B - 涂料组合物和通过其涂覆得到的涂膜 - Google Patents
涂料组合物和通过其涂覆得到的涂膜 Download PDFInfo
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- CN105283519B CN105283519B CN201480033423.1A CN201480033423A CN105283519B CN 105283519 B CN105283519 B CN 105283519B CN 201480033423 A CN201480033423 A CN 201480033423A CN 105283519 B CN105283519 B CN 105283519B
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Abstract
本发明为提供用于在预涂覆钢板的下面提供尤其在其抗压痕性、涂膜附着力和可弯性方面显著的涂膜的涂料组合物;以及通过涂覆该涂料组合物得到的涂膜。本发明涉及包含涂膜形成树脂(A)、交联剂(B)和树脂珠粒(C)的涂料组合物,其中借助微型抗压试验机测量在各树脂珠粒10%加压变形时树脂珠粒(C)的压缩强度为0.1MPa至20MPa,此外,借助微型抗压试验机测量在各树脂珠粒90%加压变形以后树脂珠粒(C)的恢复率为至少80%。
Description
[技术领域]
本发明涉及作为生产预涂覆钢板中的背面涂层(下面)涂料,特别是在其抗压痕性方面显著的涂料组合物。
[背景技术]
与其中涂覆在首先以目标制造产品的形式制造以后进行的后涂覆相反,预涂覆钢板为在其制造以前预先经受涂覆的金属板(切片或卷),并且它广泛用于建筑材料如屋顶和墙壁,以及用于音频设备、冰箱、隔离物等的外壳,因为与后涂覆相比,在成本、能量节约和材料节约方面存在优点。
预涂覆钢板的涂覆通常在其上面和下面上进行,其中上面为在制造以后形成产品的外面的区域,所以在其上施涂在涂膜外观、物理性能(硬度、附着力、耐刮擦性、可弯性等)、耐腐蚀性和耐气侯性等方面显著的涂料,并且为此采用的涂覆方法为使用底漆和顶涂层涂料的双涂双烘体系,或者使用底漆、中间涂层涂料和顶涂层涂料的三涂三烘体系。另一方面,由于下面在制造以后位于产品的内部,不需要与上面的情况下相同等级的涂膜外观和耐气侯性,从成本的观点看,其涂覆通常通过仅使用背面涂层涂料的一涂一烘体系进行,但在尤其需要耐腐蚀性的应用中,采用使用底漆和背面涂层涂料的双涂双烘体系。
尽管预涂覆钢的上面和下面理想地具有相同的外观(光泽度、色调),由于预涂覆钢的下面在制造以后形成加工产品的内部,它几乎永远不能看见,所以不需要高水平的设计,通常仅提供两类涂料作为背面涂层涂料,即高光泽度背面涂层涂料和低光泽度背面涂层涂料,使得在上面光泽度相当高的情况下,将高光泽度背面涂层涂料施涂于下面上,而在上面光泽度相当低的情况下,将低光泽度背面涂层涂料施涂于下面上,这样,所用涂料产品的数量降低且成本改善。
在这些中,低光泽度背面涂层涂料迄今为止通过引入具有光泽度降低效果的无机粉末如二氧化硅制备,但产生问题,例如由粘度提高导致的可涂覆性降低或者可弯性降低,以及由差抗压痕性导致的光泽转移等。此处,由差抗压痕性导致的光泽转移指这一现象:在上面具有与下面不同的光泽度的预涂覆钢板为卷形状并施加强压力,同时上面与下面接触的情况下,高光泽度面的光泽度降低,同时相反,低光泽度面的光泽度提高,且这作为光泽从高光泽度面向低光泽度面的表观转移被感知。该现象被认为是由于具有微小凸起和压痕的低光泽度面挤压相对光滑的高光泽度面,使得低光泽度面上的微小凸起和压痕咬入高光泽度面的表面中并降低其光滑性,同时低光泽度面上的细凸起和压痕挤压光滑的高光泽度面并由此变光滑而发生。当发生该现象时,预涂覆钢板表面光泽度改变,同时保存卷曲状态,并且在存在局部负载应用的区域中还尤其存在光泽度的明显变化,因此产生光泽转移变化,其中光泽转移均匀地显现,所以存在不能提供均匀的最终产品的问题。
在专利文件1中,公开了背面涂层涂料组合物,其包含选自聚酰胺树脂、聚丙烯腈树脂和丙烯酸系树脂的至少一类细树脂颗粒。
然而,其中存在的问题是取决于所用细树脂颗粒的类型,它在抗压痕性试验中失效,并且发生细粒本身的脱落。
在专利文件2中,描述了通过使用软氨基甲酸酯珠粒增强钢板的耐刮擦性的方法,但当预涂覆钢板经受高压时,珠粒本身变形,并且不能维持预期的性能。
在专利文件3中,描述了反应性氨基甲酸酯珠粒。这些珠粒的特性特征是它们在表面上具有反应性封端异氰酸酯,但实际上,在进行抗压痕性试验时没有显示良好的结果。为此的原因认为是尽管珠粒由于摩擦等导致的脱落实际上由于反应性氨基甲酸酯珠粒与基体树脂的化学结合而被抑制,当珠粒经受变形压力时,它们不会然后恢复其原始状态。
[现有技术文献]
[专利文献]
[专利文件1]JP-A-2006-219731
[专利文件2]日本专利4448511
[专利文件3]JP-A-2009-197067
[发明概要]
[本发明待解决的问题]
本发明的目的是提供在预涂覆钢板的下面上提供特别是在其抗压痕性、涂膜附着力和可弯性方面显著的涂膜的涂料组合物,以及提供通过施涂该涂料组合物得到的涂膜。
[解决问题的方法]
作为关于解决上述问题的艰辛研究的结果,本发明人发现在树脂珠粒在10%加压变形时的压缩强度限于指定范围的情况下,以及此外在90%加压变形以后的恢复率限于指定范围的情况下,得到可形成显示出在抗压痕性、涂膜附着力和可弯性方面良好评估结果的背面涂膜的涂料组合物,并基于该发现完成本发明。
此外,它们发现通过将树脂珠粒的含量基于质量限于指定范围,以及通过将平均粒径限于指定范围,得到在抗压痕性、涂膜附着力和可弯性方面甚至更好的评估结果。
具体而言,本发明涉及包含涂膜形成树脂(A)、交联剂(B)和树脂珠粒(C) 的涂料组合物,其中借助微型抗压试验机测量在各树脂珠粒10%加压变形时所述树脂珠粒(C)的压缩强度为0.1MPa至20Mpa,此外,借助微型抗压试验机测量在各树脂珠粒90%加压变形以后树脂珠粒(C)的恢复率为至少 80%。
此外,本发明提供涂料组合物,其中在上述涂料组合物中,上述树脂珠粒(C)的质量含量根据上述涂膜形成树脂(A)和上述交联剂(B)的质量计总固体含量为0.5-20质量%。
此外,本发明提供涂料组合物,其中在上述10%加压变形时的压缩强度为0.2MPa至1.5Mpa,此外,上述树脂珠粒(C)的质量含量根据上述涂膜形成树脂(A)和上述交联剂(B)的质量计总固体含量为0.8-15质量%。
本发明还提供涂料组合物,其中在上述组合物中,上述树脂珠粒(C) 通过氨基甲酸酯反应制备。
本发明还提供涂料组合物,其中上述树脂珠粒(C)通过氨基甲酸酯反应制备,且原料异氰酸酯为二官能的。
另外,通过施涂本发明涂料组合物而提供在其抗压痕性、涂膜附着力和可弯性方面显著的涂膜。
[发明效果]
通过将本发明涂料组合物施涂于下面上,可得到在抗压痕性、涂膜附着力和可弯性方面显著的涂膜。
[实施本发明的模式]
用于本发明涂料组合物中的涂膜形成树脂(A)不特别受限,条件是它为具有涂膜形成能力,此外具有可与交联剂(B)反应的官能团的树脂,但根据可弯性和紧密附着力,它优选为至少一种选自环氧树脂和聚酯树脂的涂膜形成树脂。这类涂膜形成树脂可单独使用,或者可使用两类或更多类的组合。
在环氧树脂用作涂膜形成树脂(A)的情况下,环氧树脂的实例为由双酚 A和表氯醇合成的双酚A类环氧树脂,以及由双酚F和表氯醇合成的双酚 F类环氧树脂,但根据耐腐蚀性,优选双酚A类环氧树脂。
当环氧树脂用作涂膜形成树脂(A)时,从可弯性、耐腐蚀性和涂覆效率等的观点看,环氧树脂的数均分子量优选为400-10,000,优选2,000-8,000。在本发明中,数均分子量的值为借助凝胶渗透色谱(GPC)使用聚苯乙烯标准作为标准材料测定的。
如果环氧树脂用作涂膜形成树脂(A),则该环氧树脂中的所有或一些环氧基团或羟基可通过与改性剂反应而改性。环氧树脂改性剂的实例为聚酯、链烷醇胺、己酸内酯、异氰酸酯化合物、磷酸化合物、酸酐等。这些改性剂可单独使用,或者可使用其两类或更多类的组合。
在聚酯树脂用作涂膜形成树脂(A)的情况下,该聚酯树脂可通过已知的方法使用多元醇与多元酸之间的反应得到。
多元醇的实例为二醇,以及三元或更高级多元醇。二醇的实例包括乙二醇、丙二醇、二甘醇、三甘醇、四甘醇、二丙二醇、聚乙二醇、聚丙二醇、新戊二醇、己二醇、1,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、2-丁基-2-乙基-1,3-丙二醇、甲基丙二醇、环己烷二甲醇、3,3-二乙基-1,5- 戊二醇等。三元醇或更高级多元醇的实例包括甘油、三羟甲基乙烷、三羟甲基丙烷、季戊四醇、二季戊四醇等。这些多元醇可单独使用,或者可使用其两种或更多种的组合。
通常,聚羧酸用作多元酸,但是如果需要的话,也可联合使用一元脂族酸等。聚羧酸的实例包括邻苯二甲酸、对苯二甲酸、六氢邻苯二甲酸、 4-甲基六氢邻苯二甲酸、二环[2,2,1]庚烷-2,3-二羧酸、偏苯三酸、己二酸、癸二酸、琥珀酸、壬二酸、富马酸、马来酸、衣康酸、均苯四酸、二聚酸等及酐,以及1,4-环己烷二羧酸、间苯二甲酸、四氢间苯二甲酸、六氢间苯二甲酸、六氢对苯二甲酸等。这些多元酸可单独使用,或者可使用其两种或更多种的组合。
当聚酯树脂用作涂膜形成树脂(A)时,从耐溶剂性和可弯性等的观点看,优选聚酯树脂的羟值为5-200mgKOH/g。
此外,当聚酯树脂用作涂膜形成树脂(A)时,从耐溶剂性和可弯性等的观点看,优选所述聚酯树脂的数均分子量为500-20,000。
本发明中所用交联剂(B)与涂膜形成树脂(A)反应以形成固化涂膜。交联剂(B)的实例包括氨基树脂、多异氰酸酯化合物和封端多异氰酸酯化合物等,但从可弯性和普遍适用性的观点看,优选三聚氰胺树脂和封端多异氰酸酯化合物。这些交联剂可单独使用,或者它们可以以其两种或更多种的组合使用。
‘氨基树脂’指通过甲醛与具有氨基的化合物加成和缩合而得到的树脂,所述具有氨基的化合物的具体实例为三聚氰胺树脂、脲树脂和三聚氰二胺树脂等。在这些中,优选三聚氰胺树脂。三聚氰胺树脂的实例包括通过三聚氰胺与甲醛之间反应得到的部分或完全羟甲基化三聚氰胺树脂,通过使用醇组分将羟甲基化三聚氰胺树脂中的羟甲基部分或完全醚化而得到的部分或完全烷基醚型三聚氰胺树脂,含亚氨基的三聚氰胺树脂和包含这些的混合物的三聚氰胺树脂。烷基醚型三聚氰胺树脂的实例包括甲基化三聚氰胺树脂、丁基化三聚氰胺树脂和甲基/丁基混合烷基型三聚氰胺树脂等。
多异氰酸酯化合物的实例包括六亚甲基二异氰酸酯、三甲基六亚甲基二异氰酸酯、二聚酸二异氰酸酯和其它这类脂族二异氰酸酯,异佛尔酮二异氰酸酯、二甲苯二异氰酸酯(XDI)、间-二甲苯二异氰酸酯、氢化XDI、氢化TDI、氢化MDI和其它这类脂环族二异氰酸酯,甲苯二异氰酸酯 (TDI)、4,4-二苯基甲烷二异氰酸酯(MDI)和其它这类芳族二异氰酸酯,以及其加合物、缩二脲、异氰尿酸酯等。这些多异氰酸酯化合物可单独使用,或者可使用其两种或更多种的组合。
封端多异氰酸酯化合物的实例为其中多异氰酸酯化合物中的异氰酸酯基团用例如醇如丁醇、肟如甲基乙基酮肟、内酰胺如ε-己内酰胺、二酮如乙酰乙酸二酯、咪唑如咪唑本身或2-乙基咪唑和苯酚如间甲酚封端的化合物。
从耐腐蚀性和可弯性的观点看,优选本发明涂料组合物中交联剂(B) 的固体组分质量含量根据涂膜形成树脂(A)为3-60质量%。如果它小于3 质量%,则涂膜强度可能降低,而如果它大于60质量%,则可弯性可能降低。
在本发明涂料组合物中,除上述组分外,还可任选包含常用于涂料领域中的各种已知组分。这些的具体实例为均染剂、消泡剂和其它类型的表面调节剂,分散剂、防沉降剂、UV吸收剂、光稳定剂和各种其它类型的添加剂,有色颜料、体质颜料和各种其它类型的颜料,闪光材料、固化催化剂、有机溶剂等。
用于本发明中的树脂珠粒(C)借助微型抗压试验机测量在各树脂珠粒 10%加压变形时具有0.1MPa至20MPa,优选0.15MPa至10Mpa,更优选0.2MPa至1.5Mpa的压缩强度。此外,借助微型抗压试验机测量在各树脂珠粒90%加压变形以后树脂珠粒(C)的恢复率为至少80%,优选至少 90%,且这贡献于固化涂膜的抗粘结性能。
本发明中各树脂珠粒10%加压变形时树脂珠粒(C)的压缩强度及其在 90%加压变形以后的恢复率为借助微型抗压试验机(“MCT-510”,由the Shimadzu Corporation生产)测量的值。具体而言,将单一珠粒设定在试验机的下部压力板上,并且在降低上部压力板时,单一珠粒经受压缩变形,在此期间进行负载的测量,并且将树脂珠粒直径降低10%时的负载视为 10%加压变形时的压缩强度。此外,单一珠粒经受压缩变形并在珠粒直径降低90%时停止负载。将施加负载以前的树脂珠粒直径视为di(mm),且在负载终止以后消逝60秒以后树脂珠粒的直径视为dt(mm),可借助以下等式(1)计算由90%加压变形的恢复率。
由90%加压变形的恢复率=dt/di…等式(1)
甚至在其中树脂珠粒(C)的上述压缩强度为0.1-20Mpa的情况下,如果借助微型抗压试验机测量各树脂珠粒由90%加压变形的恢复率小于80%,则涂膜的抗压痕性是不足的。
树脂珠粒(C)的质量含量根据上述涂膜形成树脂(A)和上述交联剂(B) 的质量计总固体含量优选为0.5-20质量%,更优选0.8-15质量%,仍更优选1.0-15质量%。如果它小于0.5质量%,则抗压痕性可能降低。另一方面,如果它大于20质量%,则可能存在可弯性的降低。
树脂珠粒(C)的平均粒径优选为5-30μm。如果平均粒径小于5μm,则涂膜抗压痕性的增强是不足的,而如果它超过30μm,则除外观不令人满意外,还存在由于树脂珠粒脱落导致的抗压痕性降低。
接着描述树脂珠粒制备方法。
<第一阶段:氨基甲酸酯原料的制备>
在第一阶段中,将原料异氰酸酯和多元醇混合在一起。将二官能或三官能异氰酸酯和多元醇预先在用于随后悬浮聚合的制剂中混合在一起。当使用二官能异氰酸酯和多元醇时,可得到高弹性树脂珠粒。当使用三官能异氰酸酯和多元醇时,形成刚性树脂珠粒。因此,这些适合一起用于调整性能。根据异氰酸酯类型,可使用经历泛黄的类型或非泛黄类型。
通常,所用多元醇与异氰酸酯以等摩尔比例混合。异氰酸酯和多元醇的比例根据所用多元醇的分子量改变。如果存在太少多元醇组分,则得到硬颗粒,而如果存在太多多元醇组分,则倾向于得到软得多的颗粒。
多元醇组分可以为聚酯-、聚醚-或丙烯酸-多元醇等。此外,这些也可联合使用。
如果悬浮液的粘度为高的且处置变得困难,则优选将稀释溶剂与珠粒原料混合。稀释溶剂的实例为溶解包含封端异氰酸酯基团的多异氰酸酯预聚物且不抑制聚合反应的那些。
将上述珠粒原料加入含有悬浮稳定剂的水中。该含有悬浮稳定剂的水通过将悬浮稳定剂溶于或分散于水中而制备。
悬浮稳定剂不特别受限,条件是它是常用于悬浮聚合中的类型,且它可以为有机或无机类型。悬浮稳定剂的具体实例包括甲基纤维素、羟乙基纤维素、羟丙基甲基纤维素、三甲基纤维素和其它类型的纤维素基水溶性树脂,聚乙烯醇、聚丙烯酸酯、聚乙二醇、聚乙烯吡咯烷酮、聚丙烯酰胺、三磷酸等。这些中的一种可单独使用,或者一起使用两种或更多种。
此外,表面活性剂可与悬浮稳定剂联合使用。与悬浮稳定剂联合使用的表面活性剂可以为阴离子表面活性剂、阳离子表面活性剂、非离子表面活性剂或两性表面活性剂。
每100质量份包含封端异氰酸酯基团的异氰酸酯预聚物加入的悬浮稳定剂的根据所用类型而不同,但优选1-10质量份。当悬浮稳定剂的加入量在该范围内时,珠粒的平均粒径倾向于在5-30μm范围内,其适用作填料。
如果悬浮稳定剂的量大于10质量份,则平均粒径倾向于小于5μm,此外,悬浮液的粘度倾向于提高,使得固体/液体分离和洗涤步骤变得更困难。另一方面,用小于1质量份的悬浮稳定剂,颗粒倾向于聚集,此外,存在粒径提高至30μm以上的倾向。
分散稳定剂溶于或分散于其中的水的量优选为100-300质量份每100 质量份包含封端异氰酸酯基团的多异氰酸酯预聚物。
<第二阶段:悬浮聚合>
在将珠粒原料加入包含悬浮稳定剂的水中以后,通常采用搅拌方法以产生颗粒形式的其分散体。此时优选适当地调整搅拌速率使得在第一阶段中制备的氨基甲酸酯原料采取指定的粒径。
完全调整包含封端异氰酸酯基团的多异氰酸酯预聚物的分散颗粒的粒径以后,将温度提高至30-90℃,并进行悬浮聚合1-6小时,使得得到悬浮液。
<第三阶段:后处理>
将如过滤或离心的方法用于后处理步骤中的固体/液体分离。
在洗涤步骤中,将分离且回收的反应性聚氨酯珠粒用水等进一步洗涤,使得除去保留在聚氨酯珠粒上的任何悬浮稳定剂。对于干燥,使用热干燥方法、空气基干燥方法、真空干燥方法、红外线干燥方法等。例如,在使用热干燥方法的情况下,优选干燥温度设置为40-110℃,且干燥时间为2-40 小时。
当使悬浮液经受固体/液体分离和洗涤时,还将悬浮液用例如酶如纤维素分解酶或聚乙烯醇分解酶或者试剂如次氯酸盐处理以将悬浮稳定剂分解。通过这样处理,可降低悬浮液的粘度,由此,促进固体/液体分离,除此之外还促进洗涤。
作为使用本发明涂料组合物的材料的实例,存在热浸镀锌钢板、电镀锌钢板、合金镀锌钢板、铝-锌涂覆钢板、镍-锌涂覆钢板、镁-铝-锌涂覆钢板、镁-铝-二氧化硅-锌涂覆钢板和各种其它类型的镀锌钢板,不锈钢板和铝板等,其已经受用无铬或铬酸盐基化学处理剂等处理。
在预涂覆钢板的生产中,一般而言,将顶涂层涂料施涂在底漆的涂膜上。通过施涂顶涂层涂料,可赋予预涂覆钢板吸引力,还可增强预涂覆钢板的各种所需性能,例如可弯性、耐气侯性、耐化学品性、防污染性、防水性和耐腐蚀性等。
本发明涂料组合物的用途不特别受限,但它优选作为背面涂层涂料用于生产预涂覆钢板。
关于用于本发明涂料组合物的涂覆方法,可使用常用于生产预涂覆钢板的任何方法,例如滚涂机涂覆、帘幕式淋涂机涂覆等。
生产预涂覆钢板中的常用涂覆条件可用作在本发明涂料组合物的情况下的涂覆条件。生产预涂覆钢板中的底漆涂料的涂膜厚度为例如1-30μm,且用于底漆涂膜的热固化条件为例如150-300℃的最大获得板温度和 15-150秒的固化时间。生产预涂覆钢板中的顶涂层涂料的涂膜厚度为例如 10-25μm,且用于顶涂膜的热固化条件为例如190-250℃的最大获得板温度和20-180秒的硬化时间。
[工作实施例]
下文通过提供工作实施例进一步详细地解释本发明,但本发明不限于所述实施例。除非另外说明,实施例中对份、百分数(%)和比的体积分别表示质量份、质量%和质量比。
<树脂珠粒合成实施例C-1至C-14和对比合成实施例RC-1至RC-3>
将表1所示原料(用于第一烧瓶)以表1所示量引入装配有搅拌器的2L 烧瓶中,然后在80℃下进行反应4小时,同时搅拌,以产生氨基甲酸酯预聚物。接着将表1所示材料(用于第二烧瓶)以表1所示量引入分开的装配有搅拌器的2L烧瓶中,然后在搅拌时将在第一烧瓶中制备的氨基甲酸酯预聚物分散于其中,并在60℃下进行反应2小时。将通过反应得到的树脂珠粒使用金属网过滤并用纯水洗涤,其后在热空气干燥器中在80℃下进行干燥3小时,这样分别得到树脂珠粒C-1至C-14和RC-1至RC-3。
表1中所用原料的详情如下。
六亚甲基二异氰酸酯三聚物:Sumidur N3200(由the Sumika Bayer UrethaneCo.生产)
六亚甲基二异氰酸酯二聚物:Sumidur N3400(由the Sumika Bayer UrethaneCo.生产)
二苯基甲烷二异氰酸酯聚合物:Millionate MR200(由the Nippon PolyurethaneIndustry Co.生产)
甲苯二异氰酸酯单体:Cosmonate T100(由the Mitsui Chemicals Co. 生产)
聚己酸内酯多元醇:Placcel 303(由the Daicel Corporation生产)
聚乙烯醇:Poval 220(由the Kuraray Co.生产)
<测量平均粒径的方法>
合成树脂珠粒的平均粒径使用激光衍射型粒度分布测量装置 (“SALD-2300”,由the Shimadzu Corporation生产)测量。结果显示于表1 中。
<树脂珠粒的压缩强度和恢复率的测量>
合成树脂珠粒在10%加压变形时的压缩强度和在90%加压变形以后的恢复率通过使用微型抗压试验机(“MCT-510”,由the Shimadzu Corporation生产)进行的测量测定。结果一起显示于表1中。
<制备实施例1(背面涂层涂料基料E-1的制备)>
使用装配有搅拌器、冷凝器和温度计的烧瓶,将80份环氧树脂(商品名“jER1009”;双酚A类环氧树脂,由the Mitsubishi Chemical Co.生产) 加热并溶于120份混合溶剂(芳族溶剂(商品名“Solvesso 100”,由the Exxon Mobil Chemical Co.生产)/环己酮/正丁醇=55/27/18(质量比))中以得到用于提供涂膜形成树脂(A)的环氧树脂溶液。接着将30份环己酮和30份芳族溶剂(商品名“Solvesso 150”,由the Exxon Mobil ChemicalCo.生产)加入200 份该环氧树脂溶液中,然后引入70份二氧化钛(商品名“JR701”由theTayca Corporation生产)、1份炭黑颜料、20份防腐蚀性颜料(商品名“Shieldex C303”,由W.R.Grace&Co.生产)和8份沉淀硫酸钡,其后使用砂磨机进行分散至5-10μm的粒度,得到研磨基料。作为交联剂(B),将21 份封端多异氰酸酯化合物(商品名“Desmodur BL-3175”,(固体含量75%),由the Sumika Bayer Urethane Co.生产)和1.2份二月桂酸二丁锡(DBTDL)加入该研磨基料中并进行均匀地混合以得到背面涂层涂料基料E-1(固体含量51%)。
<制备实施例2(背面涂层涂料基料E-2的制备)>
加入160份的the Evonik Degussa Co.产品Dynapol LH822(固体含量 55%,数均分子量5000,羟值50mg/g)、30份环己酮和30份芳族溶剂(商品名“Solvesso 150”,由theExxon Mobil Chemical Co.生产),然后引入70 份二氧化钛(商品名“JR701”,由the TaycaCorporation生产)、1份炭黑颜料、20份防腐蚀性颜料(商品名“Shieldex C303”,由W.R.Grace&Co.生产)和15份沉淀硫酸钡,其后使用砂磨机进行分散至5-10μm的粒度,得到研磨基料。将40份正丁基化三聚氰胺树脂(由the Mitsui Chemicals Co.生产;U-Van 122(固体含量60%))作为交联剂(B)加入该研磨基料中并进行均匀地混合以得到背面涂层涂料基料E-2(固体含量60%)。
<制备实施例3(底漆涂料P-1的制备)>
使用装配有搅拌器、冷凝器和温度计的烧瓶,将80份环氧树脂(商品名“jER1009”;双酚A类环氧树脂,由the Mitsubishi Chemical Co.生产) 加热并溶于120份混合溶剂(芳族溶剂(商品名“Solvesso 100”,由the Exxon Mobil Chemical Co.生产)/环己酮/正丁醇=55/27/18(质量比))中以得到用于提供涂膜形成树脂(A)的环氧树脂溶液。接着将30份环己酮和30份芳族溶剂(商品名“Solvesso 150”,由the Exxon Mobil Chemical Co.生产)加入200 份该环氧树脂溶液中,然后引入30份防腐蚀性颜料(商品名“Shieldex C303”,由W.R.Grace&Co.生产),其后使用砂磨机进行分散至20-25μm 的粒度,得到研磨基料。作为交联剂(B),将21份封端多异氰酸酯化合物(商品名“Desmodur BL-3175”,由the SumikaBayer Urethane Co.生产)和1.2 份二月桂酸二丁锡(DBTDL)加入该研磨基料中并进行均匀地混合以得到底漆涂料P-1。
<工作实施例CB-1至CB-18、对比例RCB-1至RCB-3(背面涂层涂料的制备)>
将表2和3中所示树脂珠粒(C)以表2和3中所示量加入3-400份的制备实施例1中所得背面涂层涂料基料E-1中,然后加入细二氧化硅粉末(商品名“Nipsil E-200A”,由theTosoh Silica Corporation生产)并进行调整使得60°镜面光泽度为10,这样得到背面涂层涂料CB-1至CB-18和RCB-1 至RCB-3。每400质量份背面涂层涂料基料E-1中所含涂膜形成树脂(A) 和交联剂(B)的结合总量为100质量份。
<工作实施例CB-31至CB-48、对比例RCB-31至RCB-33(背面涂层涂料的制备)>
将表4和5中所示树脂珠粒(C)以表4和5中所示量加入327份的制备实施例2中所得背面涂层涂料基料E-2中,然后加入细二氧化硅粉末(商品名“Nipsil E-200A”,由theTosoh Silica Corporation生产),并进行调整使得60°镜面光泽度为10,这样得到背面涂层涂料CB-31至CB-48和RCB-31 至RCB-33。每327质量份背面涂层涂料基料E-2中所含涂膜形成树脂(A) 和交联剂(B)的结合总量为100质量份。
<试片的制备>
制备涂有背面涂层涂料的板
使用涂布棒将背面涂层涂料CB-1至CB-48和RCB1至RCB33分别施涂于板厚度为0.35mm的化学处理铝/锌合金基涂覆钢板(Al 55%)的一面上以得到8μm的干膜厚度,然后将这些板各自在热空气干燥器中在220℃的最大获得板温度下烘烤40秒以形成背面涂层涂膜。
制备涂有上面(前面)涂料的板
使用涂布棒将底漆涂料P-1涂覆于未用背面涂层涂覆的厚度为 0.35mm的化学处理铝/锌合金基涂覆钢板(Al 55%)的该表面上以得到5μm 的干膜厚度,然后将这些板各自在热空气干燥器中在210℃的最大获得板温度下烘烤40秒以形成底漆涂膜。
接着,使用涂布棒将该底漆涂膜用聚酯树脂基顶涂层涂料(商品名“PrecolorHD0030”;由BASF Japan生产,褐色)涂覆以得到15μm的干膜厚度,然后将各个板在热空气干燥器中在220℃的最大获得板温度下烘烤 40秒以形成试片。
以下对涂膜性能的评估在所得试片的下面上进行,且结果显示于表2-5 中。
<抗压痕性>
从制备的涂覆钢板上切下尺寸为10cm×10cm的试片,然后将前面和后面叠加,并将这些在50℃大气中以施加5MPa/cm2的压力的状态保持24 小时。随后,使温度恢复室温并释放压力,其后将叠加的试片分离并进行对表面压痕的观察。
表面外观在试验以前和以后未改变
O:表面外观仅轻微地改变,在第一眼时没有注意到的程度
Δ:表面外观仅轻微地改变,足以在第一眼时注意到
×:外观相当大地变化
<涂膜附着力>
使用绞刀,在试片的涂膜中形成具有100个尺寸为1mm×1mm的正方形的十字交叉图案。接着,使用Erichsen试验机,用冲压器将形成十字交叉图案时的区域中的漆膜从试片的底面上伸展开,使得从冲压器尖端到试片挤压面的距离为6mm。最后,将赛璐玢带紧紧地粘附在漆膜的伸展开的十字交叉区域上,然后以45°角将带端突然剥离,并观察十字交叉图案的状态,其后如下进行评估。
没有注意到涂膜的剥离
O:不多于5%的涂膜剥离面积
Δ:不多于20%的涂膜剥离面积
×:多于20%的涂膜剥离面积
<可弯性>
将试片用与插入其间的试片相同的片材弯曲180°。所用名称基于与这样插入的试片相同的片材数目为0T、2T等。例如,0T为试片未用与插入试片相同的片材弯曲的情况,且2T为试片用与插入试片相同的两个片材弯曲的情况。在评估本发明涂膜的性能中,进行2T和3T试验,并且在这样弯曲以后,将赛璐玢带紧紧地粘附在冠顶区域上,然后以45°角将带端突然剥离,并如下评估涂膜的剥离状态。
在2T或3T情况下没有注意到涂膜的剥离
O:在3T试验中没有注意到涂膜的剥离,但在2T情况下观察到轻微的剥离
Δ:在3T情况下注意到轻微的剥离
×:在3T情况下注意到明显的剥离
<讨论>
通过使用其中在10%加压变形时的压缩强度为0.1MPa至20MPa且在90%加压变形以后的恢复率为至少80%的树脂珠粒,在评估抗压痕性、涂膜附着力和可弯性中,在所有工作实施例中得到优异的结果。
此外,在CB-1至CB-14和CB-31至CB-44的情况下,通过使用平均粒径为5-30μm的树脂珠粒(C)且其中所述树脂珠粒(C)的质量含量根据涂膜形成树脂(A)和交联剂(B)的质量计总固体含量为0.5-20质量%,在评估抗压痕性、涂膜附着力和可弯性中得到更加显著的结果。此外,在CB-2 至CB-7和CB-32至CB-37中,其中所述树脂珠粒(C)在10%加压变形时的压缩强度为0.2MPa至1.5MPa,且其中所述树脂珠粒(C)的含量为0.8-15 质量%,得到的甚至更好的评估结果。
Claims (6)
1.包含涂膜形成树脂(A)、交联剂(B)和树脂珠粒(C)的涂料组合物,其中借助微型抗压试验机测量所述树脂珠粒(C)进行10%加压变形时所述树脂珠粒(C)的压缩强度为0.1MPa至20MPa,此外,借助微型抗压试验机测量所述树脂珠粒(C)进行90%加压变形以后树脂珠粒(C)的恢复率为至少80%,
其中,交联剂(B)的固体组分质量含量根据涂膜形成树脂(A)为3-60质量%,
树脂珠粒(C)的质量含量根据上述涂膜形成树脂(A)和上述交联剂(B)的质量计总固体含量为0.5-20质量%,
上述树脂珠粒(C)通过氨基甲酸酯反应制备。
2.根据权利要求1的涂料组合物,其中上述树脂珠粒(C)的平均粒径为5-30μm。
3.根据权利要求1或2的涂料组合物,其中在上述10%加压变形时的压缩强度为0.2MPa至1.5MPa,此外,上述树脂珠粒(C)的质量含量根据上述涂膜形成树脂(A)和上述交联剂(B)的质量计总固体含量为0.8-15质量%。
4.根据权利要求1或2的涂料组合物,上述树脂珠粒(C)通过氨基甲酸酯反应制备,此外,原料异氰酸酯为二官能的。
5.根据权利要求3的涂料组合物,上述树脂珠粒(C)通过氨基甲酸酯反应制备,此外,原料异氰酸酯为二官能的。
6.通过施涂根据权利要求1-5中任一项的涂料组合物得到的涂膜。
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