CN113874209A - 装饰片 - Google Patents

装饰片 Download PDF

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Publication number
CN113874209A
CN113874209A CN202080038042.8A CN202080038042A CN113874209A CN 113874209 A CN113874209 A CN 113874209A CN 202080038042 A CN202080038042 A CN 202080038042A CN 113874209 A CN113874209 A CN 113874209A
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China
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decorative sheet
layer
resin
sheet according
bisphenol
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CN113874209B (zh
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大久保透
村田大辅
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Toppan Inc
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Toppan Printing Co Ltd
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
    • C08G18/4269—Lactones
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    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Laminated Bodies (AREA)

Abstract

本发明提供一种粘接性和耐湿热性均优异的装饰片。其主旨在于，本实施方式涉及的装饰片(10)至少依次层叠有基材层(11)、粘接层(13)以及透明树脂层(14)，粘接层(13)包含聚酯树脂和双酚A型环氧树脂，聚酯树脂包含苯二甲酸、直链二羧酸以及亚烷基二醇作为构成要素，以质量比计，聚酯树脂和双酚A型环氧树脂的含量在(聚酯树脂/双酚A型环氧树脂)＝50/50～90/10的范围内。

Description

装饰片
技术领域
本发明涉及装饰片。
背景技术
在建筑物外部装饰和浴室等应用中，有时要求装饰片具有对高温多湿的耐久性(耐湿热性)。装饰片通常为在基材上经由粘接层而层叠有透明树脂层的构成。以往，作为粘接层的材料，多使用粘接性通常为优异的聚酯树脂(专利文献1)。然而，聚酯树脂容易水解且耐湿热性不足，有时会成为在基材与透明树脂层之间产生剥离的原因。
现有技术文献
专利文献
专利文献1：日本专利第4281403号公报
发明内容
发明所要解决的课题
针对上述问题，本发明的目的在于提供一种粘接性和对高温多湿的耐久性(耐湿热性)均优异的装饰片。
用于解决课题的方案
为了实现上述目的，本发明的一个方式涉及的装饰片的要旨在于，至少依次层叠有基材层、粘接层以及透明树脂层，所述粘接层包含聚酯树脂和双酚A型环氧树脂，所述聚酯树脂包含苯二甲酸、直链二羧酸以及亚烷基二醇作为构成要素，以质量比计，所述聚酯树脂和所述双酚A型环氧树脂的含量在(聚酯树脂/双酚A型环氧树脂)＝50/50～90/10的范围内。
发明效果
根据本发明，可以提供一种粘接性和耐湿热性均优异的装饰片。
附图说明
[图1]为示出本发明的实施方式涉及的装饰片的构成的示意性剖面图。
具体实施方式
下面，参照附图对本发明涉及的实施方式进行说明。在以下附图的记载中，对相同或类似的部分标注相同或类似的符号。但是，应当注意，附图是示意性的，厚度与平面尺寸的关系、各层的厚度比等与实际情况不同。因此，具体的厚度和尺寸应参考以下说明来判断。此外，显而易见的是，即使在附图彼此之间也包含相互尺寸的关系和比率不同的部分。
此外，以下所示的实施方式例示了用于将本发明的技术思想具体化的装置和方法，本发明的技术思想并不限于下述描述的构成部件的材质、形状、结构、配置等。本发明的技术思想可以在权利要求书所记载的权利要求项规定的技术范围内进行各种变更。
[装饰片的构成]
如图1所示，本发明涉及的实施方式(以下简称为“本实施方式”)的装饰片10依次层叠有基材层11、图案层12、粘接层13、透明树脂层14以及表面保护层15。
[基材层]
基材层11优选使用聚烯烃或聚酯，可以从聚乙烯、聚丙烯、聚丁烯、聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚萘二甲酸乙二醇酯等现有材料中任意选择。
为了补充基材层11与相邻层的密合性，可以对基材层11进行电晕处理、等离子体处理、臭氧处理、电子束处理、紫外线处理、重铬酸处理等表面处理。
[粘接层]
粘接层13含有聚酯树脂和双酚A型环氧树脂，该聚酯树脂包含苯二甲酸、直链二羧酸以及亚烷基二醇作为构成要素。此外，该聚酯树脂可以通过已知的技术(例如，二羧酸与二醇的缩聚反应)进行制备。
通过将双酚A型环氧树脂混合在上述聚酯树脂中，本实施方式的粘接层13在装饰片中在实际应用上可以表现出充分的耐湿热性。双酚A型环氧树脂可以根据通常可获得的分子量和环氧当量不同的各种等级进行适当地选择并使用。从兼顾耐湿热性和粘接性的观点出发，双酚A型环氧树脂的分子量(质均分子量MW)优选在1,000以上4,000以下的范围内，特别优选在1,000以上2,000以下的范围内。
从兼顾耐湿热性和粘接性的观点出发，以质量比计，双酚A型环氧树脂的混合量优选在(聚酯树脂/双酚A型环氧树脂)＝50/50～90/10的范围内。当双酚A型环氧树脂的混合比过少时，耐湿热性不足，而当其过大时，粘接性有时不足。
作为该聚酯树脂的构成要素的苯二甲酸(在本实施方式中为邻苯二甲酸和对苯二甲酸的统称)用于强化粘接层的耐湿热性。以物质的量的比(摩尔比)计，苯二甲酸的含量优选在(苯二甲酸/直链二羧酸)＝45/55～85/15的范围内。当苯二甲酸含量过大时，粘接层容易变硬变脆，从而有时会对粘接性产生不利影响。此外，当其过少时，由于粘接层的凝聚力不足，从而有时粘接力不足。
对作为该聚酯树脂的构成要素的直链二羧酸没有特别地限定，例如可以从琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸等中适当地选择并使用。
作为该聚酯树脂的构成要素的亚烷基二醇，例如可以使用(聚)乙二醇、(聚)丙二醇、(聚)丁二醇、(聚)己二醇等，但是从耐湿热性方面来看，优选与新戊二醇一起使用。
以物质的量的比计，亚烷基二醇的含量优选在{亚烷基二醇/(苯二甲酸+直链二羧酸)}＝40/60～60/40的范围内。由于在该数值范围以外的聚酯树脂的分子量小，因此粘接性和耐热性可能不足。
粘接层13的形成方法可以应用(例如)凹版涂布、微凹版涂布、逗号涂布、刮刀涂布、模涂等通常的涂布方法。
[图案层]
图案层12是通过使用油墨对基材层11进行图案印刷而得到的。图案层12的形成中所使用的油墨含有粘合剂树脂，作为粘合剂树脂，例如可以从硝化棉、纤维素、氯乙烯-乙酸乙烯酯共聚物、聚乙烯醇缩丁醛、聚氨酯、丙烯酸类、聚酯类等中单独地或者从各个改性物中适当地选择并使用。此外，它们可以是水性、溶剂型、乳液型中的任意一者，此外也可以是1液型或者使用了固化剂的2液型。
从相对于基材层11的密合性和耐湿热性的观点来看，本实施方式的图案层12的粘合剂树脂优选为至少包含特定的构成要素，即聚己内酯多元醇、聚亚烷基二醇以及多异氰酸酯的氨基甲酸酯树脂。
构成本实施方式的氨基甲酸酯树脂的聚己内酯多元醇是由ε-己内酯的开环聚合所得到的材料，在其内部具有酯键。因此，与基材层11的密合性、即基材密合性得以提高。例如，与由己二酸等二羧酸和二元醇的缩聚而获得的通用聚酯多元醇相比，上述聚己内酯多元醇通常具有优异的耐水解性。
构成本实施方式的氨基甲酸酯树脂的聚亚烷基二醇具有聚醚结构，与上述聚己内酯多元醇相比，耐水解性优异，但是耐热性和基材密合性倾向于劣化。在本实施方式中，通过与聚己内酯多元醇一起使用聚亚烷基二醇，可以兼顾基材密合性和耐湿热性。
上述聚亚烷基二醇可以使用(例如)聚乙二醇、聚丙二醇、聚丁二醇等，从耐湿热性的观点来看，优选疏水性大的聚丁二醇。
本实施方式的氨基甲酸酯树脂优选进一步包含新戊二醇作为构成要素。由于含有新戊二醇，从而耐湿热性得以提高。
从分子量和官能团数(每分子中的羟基数)等观点来看，本实施方式的聚己内酯多元醇和聚亚烷基二醇可以从市售的各种材料中适当地选择并使用。此外，多异氰酸酯可以使用(例如)六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、二甲苯二异氰酸酯等二异氰酸酯及其氢化物等，在耐湿热性这一方面上，优选异佛尔酮二异氰酸酯。
对本实施方式的氨基甲酸酯树脂的组成没有特别地限定，但是考虑到通常通过印刷而形成的图案层12的印刷适性和装饰片10的各种性能，当将下述结构式所示的氨基甲酸酯树脂的各部位(己内酯单元(CL)、亚烷基二醇单元(AG)、二异氰酸酯单元(I)、新戊二醇(NPG))的物质的量分别设为X、Y、Z、N时，优选满足以下关系式(1)～(3)。
[化学式1]
CL单元(X):-C(＝O)C5H10O-
AG单元(Y)(在为聚丁二醇的情况下):-C4H8O
I单元(Z)(在为异佛尔酮二异氰酸酯的情况下):
Figure BDA0003367747250000051
NPG单元(N):-OCH2C(CH3)2CH2O-
3＜(X+Y+N)/Z＜50 (式1)
0.1＜X/Y＜10 (式2)
N/(X+Y+X+N)＜0.2 (式3)
若在上述数值范围内，则可以容易地提高印刷适性。
对本实施方式的氨基甲酸酯树脂的分子量没有特别地限定，例如，考虑到通常由印刷形成的图案层12的印刷适性和装饰片10的各种性能，质均分子量(MW)优选在5,000以上100,000以下的范围内。
若在上述数值范围内，则可以容易地提高印刷适性。
对本实施方式的氨基甲酸酯树脂的固化所使用的固化剂没有特别地限定，例如，可以从市售的固化剂中适当地选择并使用，该市售的固化剂包括：六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、甲苯二异氰酸酯、二甲苯二异氰酸酯及其氢化产物、或二苯甲烷二异氰酸酯及其氢化产物等。
通常，图案层12是将使用上述氨基甲酸酯树脂作为粘合剂树脂的图案油墨印刷在基材层11上而形成的，但是根据需要也可以添加其他的树脂成分。
作为除了图案油墨的粘合剂树脂以外的成分，例如可以使用颜料、染料等着色剂、体质颜料、溶剂、光稳定剂等各种添加剂等。作为颜料，例如可列举出：缩合偶氮、不溶性偶氮、喹吖啶酮、异吲哚啉、蒽醌、咪唑酮、钴、酞菁、碳、氧化钛、氧化铁、云母等珠光颜料等。
对设置图案层12的方法没有特别地限定，例如可以使用：凹版印刷、胶版印刷、丝网印刷、柔性版印刷、喷墨印刷等通常的印刷方法。
[透明树脂层]
透明树脂层14优选使用聚烯烃，例如可以使用：聚丙烯、聚乙烯、聚丁烯、各种α-烯烃共聚物(丙烯、1-丁烯、1-戊烯、1-己烯、1-辛烯等的共聚物)。
根据需要，可以在透明树脂层14中混合(例如)紫外线吸收剂、热稳定剂、光稳定剂、防粘连剂、催化剂捕捉剂、着色剂、光散射剂以及光泽调节剂等各种添加剂。
对透明树脂层14的形成方法没有特别地限定，可以使用压延成膜或挤出成膜等通常的方法。
在透明树脂层14上也可以设置表面凹凸以赋予其设计性。作为设置凹凸的方法，例如存在如下方法：将透明树脂层14挤出成形之后进行热压花加工的方法；在挤出形成时，使用设置了凹凸的冷却辊进行挤出成形并同时进行压花加工的方法。
[表面保护层]
表面保护层15是为了赋予装饰片10以耐候性、耐伤性、耐污染性、设计性等功能而设置的层。对构成表面保护层15的材料没有特别地限定，例如，可以从氨基甲酸酯类、丙烯酸类、丙烯酸有机硅类、氟类、环氧类等树脂材料中适当地选择并使用。
根据需要，表面保护层15也可以混合(例如)紫外线吸收剂、热稳定剂、光稳定剂、防粘连剂、催化剂捕捉剂、着色剂、光散射剂以及光泽调节剂等各种添加剂。
对表面保护层15的形成方法没有特别地限定，例如，通过凹版涂布、微凹版涂布、逗号涂布、刮刀涂布、模涂等通常的方法将由上述材料制成的涂布液进行涂布，然后使用热固化、紫外线固化等适合于材料的方法使其固化而形成。
表面保护层15可以在设置在基材层11上的图案层12上经由粘接层13而与透明树脂层14接合之后再进行设置。
接下来，对构成本实施方式的装饰片10的各层的厚度进行描述。
考虑到印刷操作性、成本等，优选的是，基材层11在20μm以上150μm以下的范围内，图案层12在0.5μm以上10μm以下的范围内，粘接层13在1μm以上20μm以下的范围内，透明树脂层14在20μm以上200μm以下的范围内，表面保护层15在3μm以上20μm以下的范围内。此外，装饰片10的总厚度优选在45μm以上250μm以下的范围内。
接下来，示出实施例和比较例的装饰片并对本发明进行更具体的说明。
＜实施例1＞
[印刷原材的制作]
使用聚己内酯二元醇、聚丁二醇以及新戊二醇作为多元醇，并使用异佛尔酮二异氰酸酯作为多异氰酸酯，通过已知的加成聚合法合成了数均分子量为2×104的羟基封端的氨基甲酸酯树脂。将酞菁铜类颜料以颜料/氨基甲酸酯树脂＝20/80的质量比分散在该氨基甲酸酯树脂中，从而制备了图案油墨。
使用上述图案油墨，在具有隐蔽性的聚乙烯原材(厚度t＝70μm)上凹版印刷木纹图案以在基材层11上形成了图案层12(厚度t＝3μm)，从而制作了印刷原材。
[粘接剂的制备]
使用间苯二甲酸(IP)和己二酸(AD)作为二元羧酸、乙二醇和己二醇作为二元醇，合成了聚酯二醇(聚酯树脂)P(IP/AD＝90/10(摩尔比)、数均分子量：1×104、固形物羟值：10mg KOH/g)。
将双酚A型环氧树脂EP(jER 1004AF，三菱化学(株))以P/EP＝70/30的固形物质量比混合在聚酯二醇(聚酯树脂)P中，然后再加入异氰酸酯固化剂和稀释剂，从而制备了粘接剂。
[装饰片的制作]
使用上述粘接剂将透明聚烯烃树脂干式层压在上述印刷原材上，然后再涂布形成由丙烯酸多元醇(甲基丙烯酸甲酯和2-羟基甲基丙烯酸酯的共聚物)和固化剂(六亚甲基二异氰酸酯的脲酸酯体)构成的2液固化型聚氨酯树脂层，从而得到了形成有粘接层13(厚度t＝1μm)、透明树脂层14(厚度t＝70μm)以及表面保护层15(厚度t＝8μm)的实施例1的装饰片10。
＜实施例2＞
在实施例1中设为P/EP＝80/20(固形物质量比)，除此以外，以与实施例1相同的方法得到了实施例2的装饰片10。
＜实施例3＞
在实施例1中设为P/EP＝60/40(固形物质量比)，除此以外，以与实施例1相同的方法得到了实施例3的装饰片10。
＜实施例4＞
在实施例1中设为IP/AD＝65/35(摩尔比)，除此以外，以与实施例1相同的方法得到了实施例4的装饰片10。
＜实施例5＞
在实施例4中使用乙二醇、己二醇以及新戊二醇作为二元醇，除此以外，以与实施例4相同的方法得到了实施例5的装饰片10。
＜比较例1＞
在实施例5中将双酚A型环氧树脂的混合量设为P/EP＝100/0，除此以外，以与实施例5相同的方法得到了比较例1的装饰片10。
＜比较例2＞
在实施例5中将双酚A型环氧树脂的混合量设为P/EP＝40/60，除此以外，以与实施例5相同的方法得到了比较例2的装饰片10。
＜评价＞
使用以下方法，对在上述实施例和比较例中所得到的装饰片进行了粘接性和耐湿热性的评价。评价结果示于表1。
(a)粘接性
在制作装饰片之后，对于在室温环境下保存了24小时的试样，测定透明树脂层与基材层之间的T字剥离强度(试样宽度：25mm，拉伸速度：50mm/min)。
[评价基准]
◎：基材断裂而未形成剥离界面
○：在基材层发生变形的同时生成剥离面
△：产生剥离面而基材层没有变形
×：在处理试样时发生剥离，无法测定
需要说明的是，在本实施例中，若评价为“◎”或“○”，则为合格。
(b)耐湿热性
在制作装饰片之后，使用HAST室，对在室温环境下保存了24小时的试样进行压力锅测试(PCT)(105℃、100％RH，96小时)，然后测定了透明树脂层与基材层之间的T字剥离强度(试样宽度：25mm、拉伸速度：50mm/min)。
[评价基准]
◎：基材断裂而未形成剥离界面
○：在基材层发生变形的同时生成剥离面
△：产生剥离面而基材层没有变形
×：在处理试样时发生剥离，无法测定
需要说明的是，在本实施例中，若评价为“◎”或“○”，则为合格。
[表1]
Figure BDA0003367747250000101
*IP(间苯二甲酸),AD(己二酸),NPG(新戊二醇),
P(聚酯树脂),EP(双酚A型环氧树脂)
从表1中可以看出，实施例1～5所示的装饰片10通过将粘接层13的聚酯树脂设为特定的组成、并且以特定的比率混合双酚A型环氧树脂，从而具有优异的粘接性和耐湿热性。特别是，与实施例4相比，在作为聚酯树脂的构成要素的二元醇中并用了新戊二醇的实施例5显示出耐湿热性优异的结果。
符号说明
10 装饰片
11 基材层
12 图案层
13 粘接层
14 透明树脂层
15 表面保护层

Claims (10)

1.一种装饰片，至少依次层叠有基材层、粘接层以及透明树脂层，其特征在于，
所述粘接层包含聚酯树脂和双酚A型环氧树脂，
所述聚酯树脂包含苯二甲酸、直链二羧酸以及亚烷基二醇作为构成要素，
以质量比计，所述聚酯树脂和所述双酚A型环氧树脂的含量在(聚酯树脂/双酚A型环氧树脂)＝50/50～90/10的范围内。
2.根据权利要求1所述的装饰片，其特征在于，
以摩尔比计，所述苯二甲酸和所述直链二羧酸的含量在(苯二甲酸/直链二羧酸)＝45/55～85/15的范围内。
3.根据权利要求1或2所述的装饰片，其特征在于，
所述亚烷基二醇包含新戊二醇。
4.根据权利要求1至3中任一项所述的装饰片，其特征在于，
在所述基材层与所述粘接层之间形成有图案层。
5.根据权利要求4所述的装饰片，其特征在于，
所述图案层含有氨基甲酸酯树脂作为粘合剂树脂，所述氨基甲酸酯树脂包含聚己内酯多元醇、聚亚烷基二醇以及多异氰酸酯作为构成要素。
6.根据权利要求5所述的装饰片，其特征在于，
作为所述氨基甲酸酯树脂的构成要素，还包含新戊二醇。
7.根据权利要求5或6所述的装饰片，其特征在于，
所述聚亚烷基二醇为聚丁二醇。
8.根据权利要求5至7中任一项所述的装饰片，其特征在于，
所述多异氰酸酯为异佛尔酮二异氰酸酯。
9.根据权利要求1至8中任一项所述的装饰片，其特征在于，
所述透明树脂层由聚烯烃树脂形成。
10.根据权利要求1至9中任一项所述的装饰片，其特征在于，
在所述透明树脂层上层叠有表面保护层。
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