CN109715581A - 中间膜用树脂组合物、中间膜用膜材以及夹层玻璃的制造方法 - Google Patents
中间膜用树脂组合物、中间膜用膜材以及夹层玻璃的制造方法 Download PDFInfo
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- CN109715581A CN109715581A CN201680089408.8A CN201680089408A CN109715581A CN 109715581 A CN109715581 A CN 109715581A CN 201680089408 A CN201680089408 A CN 201680089408A CN 109715581 A CN109715581 A CN 109715581A
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- methyl
- intermediate coat
- acrylate
- resin layer
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Abstract
本发明涉及一种中间膜用树脂组合物,其包含单体混合物的共聚物,所述单体混合物含有(甲基)丙烯酰基化合物和硅氧烷化合物,所述硅氧烷化合物具有烯键式不饱和基团且烯键式不饱和基团的当量为2000~20000g/mol。
Description
技术领域
本发明涉及中间膜用树脂组合物、中间膜用膜材以及夹层玻璃的制造方法。
背景技术
目前,作为汽车这样的车辆的窗户、天窗、内饰板等的玻璃,夹层玻璃被广泛使用,因为夹层玻璃即使受到外部冲击而破损,玻璃的碎片也很少飞散,是安全的。夹层玻璃也用于电车、航空器、建设机械、建筑物等的窗户。
作为夹层玻璃的一个例子,可以列举出:将由通过增塑剂增塑化后的聚乙烯醇缩丁醛树脂等聚乙烯醇缩醛树脂形成的夹层玻璃用中间膜夹在至少一对玻璃板之间、使其一体化而得到的夹层玻璃(例如,参考专利文献1~3)。
现有技术文献
专利文献
专利文献1:日本特开昭62-100463号公报
专利文献2:日本特开2005-206445号公报
专利文献3:国际公开第2012/091117号
发明内容
发明所要解决的问题
以往的夹层玻璃多数与同等厚度的玻璃相比具有同程度的防裂性,但正在要求对于从外部施加的冲击更加难以破裂、防裂性高的夹层玻璃。
另外,为了夹层玻璃的轻量化,正在研究使用透明塑料基板代替玻璃板。但是,在以往的隔着中间膜将玻璃板与透明塑料基板一体化或者将透明塑料基板彼此之间一体化的情况下,在高温或高温高湿条件下有时在透明塑料基板与中间膜之间产生气泡。
因此,本发明的目的在于,提供能够制作防裂性优良的夹层玻璃并且在使用了透明塑料基板的情况下能够形成耐发泡性优良的中间膜的中间膜用树脂组合物、中间膜用膜材以及夹层玻璃的制造方法。
用于解决问题的手段
本发明提供一种中间膜用树脂组合物,其包含单体混合物的共聚物,所述单体混合物含有(甲基)丙烯酰基化合物和硅氧烷化合物,所述硅氧烷化合物具有烯键式不饱和基团且烯键式不饱和基团的当量为2000~20000g/mol。
上述(甲基)丙烯酰基化合物可以含有(甲基)丙烯酸烷基酯和具有羟基的(甲基)丙烯酸酯。另外,上述单体混合物可以含有50~90质量份(甲基)丙烯酸烷基酯、5~30质量份具有羟基的(甲基)丙烯酸酯以及5~20质量份硅氧烷化合物。另外,本发明的树脂组合物还可以含有热交联剂。
本发明还提供一种中间膜用膜材,其具有基材和设置在基材上的树脂层,树脂层为由上述中间膜用树脂组合物形成的层。上述树脂层的雾度可以为5%以下。
本发明还提供一种夹层玻璃的制造方法,所述夹层玻璃具有对置的两片被粘体和夹持在两片被粘体之间的中间膜,所述制造方法包括:隔着上述中间膜用膜材所具有的树脂层来使上述两片被粘体粘贴而得到层叠体的工序;和在30~150℃以及0.3~1.5MPa的条件下对上述层叠体进行加热加压处理的工序,其中上述两片被粘体之中的至少一个为玻璃板。可以是:上述两片被粘体之中的一个为玻璃板,另一个为透明塑料基板。
发明效果
根据本发明,可以提供能够制作防裂性优良的夹层玻璃并且在使用了透明塑料基板的情况下能够形成耐发泡性优良的中间膜的中间膜用树脂组合物、中间膜用膜材以及夹层玻璃的制造方法。
附图说明
图1是表示中间膜用膜材的一个实施方式的示意截面图。
图2是表示夹层玻璃的一个实施方式的示意截面图。
具体实施方式
以下,根据情况,参照附图对本发明的优选实施方式进行说明,但本发明根本不限于以下实施方式。
本说明书中,“(甲基)丙烯酸酯”是指“丙烯酸酯”以及与其对应的“甲基丙烯酸酯”中的至少一个。关于(甲基)丙烯酰基等其他类似表现也是同样的。
<中间膜用树脂组合物>
本实施方式的中间膜用树脂组合物(以下,有时简单称为“树脂组合物”)包含单体混合物的共聚物,所述单体混合物含有(甲基)丙烯酰基化合物和硅氧烷化合物,所述硅氧烷化合物具有烯键式不饱和基团且烯键式不饱和基团的当量为2000~20000g/mol。
本实施方式的树脂组合物通过含有特定的共聚物从而使向玻璃等被粘体表面上的密合性提高,所制作的层叠体的强韧性提高,由此能够显示出夹层玻璃的高防裂性。另外,该树脂组合物具有高凝聚性,能够形成耐发泡性优良的中间膜。
(共聚物)
本实施方式的共聚物包含:基于具有(甲基)丙烯酰基的化合物(其中不具有硅作为构成原子)的结构单元;和基于具有烯键式不饱和基团且烯键式不饱和基团的当量为2000~20000g/mol的硅氧烷化合物的结构单元。
作为具有1个(甲基)丙烯酰基的化合物,可以列举出:例如,(甲基)丙烯酸、(甲基)丙烯酰胺、(甲基)丙烯酰胺衍生物、(甲基)丙烯酸烷基酯、具有亚烷基二醇链的(甲基)丙烯酸酯、具有羟基的(甲基)丙烯酸酯、具有芳香环的(甲基)丙烯酸酯、具有脂环式基团的(甲基)丙烯酸酯、(甲基)丙烯酰基吗啉、(甲基)丙烯酸四氢糠酯以及具有异氰酸酯基的(甲基)丙烯酸酯。
作为(甲基)丙烯酸烷基酯,可以列举出:例如,(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸正戊酯、(甲基)丙烯酸正己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸异癸酯、(甲基)丙烯酸十二酯以及(甲基)丙烯酸十八酯等具有碳原子数为1~18的烷基的(甲基)丙烯酸烷基酯。其中,作为(甲基)丙烯酸烷基酯,优选为(甲基)丙烯酸正丁酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸2-乙基己酯以及(甲基)丙烯酸正辛酯,更优选为(甲基)丙烯酸2-乙基己酯。另外,与甲基丙烯酸烷基酯相比优选丙烯酸烷基酯。(甲基)丙烯酸烷基酯可以单独使用或者组合使用2种以上。
作为具有羟基的(甲基)丙烯酸酯,可以列举出:例如,(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸1-羟基乙酯、(甲基)丙烯酸2-羟基丙酯、(甲基)丙烯酸3-羟基丙酯、(甲基)丙烯酸1-羟基丙酯、(甲基)丙烯酸4-羟基丁酯、(甲基)丙烯酸3-羟基丁酯、(甲基)丙烯酸2-羟基丁酯以及(甲基)丙烯酸1-羟基丁酯。
作为具有亚烷基二醇链的(甲基)丙烯酸酯,可以列举出:例如,二乙二醇单(甲基)丙烯酸酯、三乙二醇单(甲基)丙烯酸酯、四乙二醇单(甲基)丙烯酸酯、六乙二醇单(甲基)丙烯酸酯等聚乙二醇单(甲基)丙烯酸酯;二丙二醇单(甲基)丙烯酸酯、三丙二醇单(甲基)丙烯酸酯、八丙二醇单(甲基)丙烯酸酯等聚丙二醇单(甲基)丙烯酸酯;二丁二醇单(甲基)丙烯酸酯、三丁二醇单(甲基)丙烯酸酯等聚丁二醇单(甲基)丙烯酸酯;甲氧基三乙二醇(甲基)丙烯酸酯、甲氧基四乙二醇(甲基)丙烯酸酯、甲氧基六乙二醇(甲基)丙烯酸酯、甲氧基八乙二醇(甲基)丙烯酸酯、甲氧基九乙二醇(甲基)丙烯酸酯、甲氧基聚乙二醇(甲基)丙烯酸酯、甲氧基七丙二醇(甲基)丙烯酸酯、乙氧基四乙二醇(甲基)丙烯酸酯、丁氧基乙二醇(甲基)丙烯酸酯、丁氧基二乙二醇(甲基)丙烯酸酯等烷氧基聚亚烷基二醇(甲基)丙烯酸酯。另外,这些含有亚烷基二醇链的(甲基)丙烯酸酯可以单独使用,或者组合使用2种以上。
作为具有芳香环的(甲基)丙烯酸酯,可以列举出:例如,(甲基)丙烯酸苄酯以及(甲基)丙烯酸苯氧基乙酯。作为具有脂环式基团的(甲基)丙烯酸酯,可以列举出:例如,(甲基)丙烯酸环己酯、(甲基)丙烯酸异冰片酯以及(甲基)丙烯酸二环戊酯。作为(甲基)丙烯酰胺衍生物,可以列举出:例如,N,N-二甲基氨基乙基(甲基)丙烯酸酯、N,N-二甲基氨基丙基(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺、N-异丙基(甲基)丙烯酰胺、N,N-二乙基(甲基)丙烯酰胺以及N-羟基乙基(甲基)丙烯酰胺。作为具有异氰酸酯基的(甲基)丙烯酸酯,可以列举出:例如,2-(2-甲基丙烯酰氧乙基氧基)乙基异氰酸酯以及2-(甲基)丙烯酰氧基乙基异氰酸酯。
本实施方式的共聚物优选包含基于(甲基)丙烯酸烷基酯的结构单元。(甲基)丙烯酸烷基酯的共聚比例是相对于共聚物的总质量优选为50~90质量%,更优选为50~85质量%。(甲基)丙烯酸烷基酯的共聚比例如果在这样的范围内,则树脂层与被粘体的密合性能够提高。这样的共聚物可以通过使以与上述共聚比例相同的含有比例含有(甲基)丙烯酸烷基酯的单体混合物共聚而得到。另外,聚合率更优选基本上接近100质量%。
本实施方式的共聚物优选包含基于具有羟基的(甲基)丙烯酸酯的结构单元。具有羟基的(甲基)丙烯酸酯的共聚比例是相对于共聚物的总质量优选为5~30质量%,更优选为10~30质量%。具有羟基的(甲基)丙烯酸酯的共聚比例如果在这样的范围内,则在夹层玻璃的可靠性试验(加热加湿条件)中,能够显示出雾度为5.0%以下的透明性。
雾度(Haze)是表示浊度的值(%),用灯进行照射,由透过试样中的光的总透射率Tt和在试样中被扩散且散射的光的透过率Td以(Td/Tt)×100的形式求出。它们被JIS K7136规定,可以通过市售的浊度计例如日本电色工业株式会社制NDH-5000容易地测定。
本实施方式的(甲基)丙烯酰基化合物优选含有(甲基)丙烯酸烷基酯、和具有羟基的(甲基)丙烯酸酯。
(甲基)丙烯酰基化合物可以还含有下述化合物,该化合物具有:(甲基)丙烯酰基;和吗啉基、氨基、羧基、氰基、羰基、硝基、来自亚烷基二醇的基团等极性基团。通过含有具有极性基团的(甲基)丙烯酸酯,树脂层与被粘体的密合性容易提高。
作为本实施方式的硅氧烷化合物,只要是具有下述基团并且烯键式不饱和基团的当量在2000~20000的范围内的化合物就行,没有特别限定,所述基团具有(甲基)丙烯酰基、苯乙烯基、肉桂酸酯基、乙烯基、烯丙基等不饱和基团。硅氧烷化合物可以单独使用或者组合使用2种以上。作为本实施方式的硅氧烷化合物,可以列举出例如由下述式(a)或(b)表示的化合物。
式中,R1表示氢原子或甲基,R2、R3、R4、R5、R6以及R7分别独立地表示氢原子或甲基,R8表示1价烃基,L1表示氧原子可以介于其中的2价烃基或单键,m表示1以上的整数。从烯键式不饱和基团的当量在2000~20000g/mol的范围的观点出发,m优选为10~300。
式中,R1表示氢原子或甲基,R2、R3、R4、R5、R6以及R7分别独立地表示氢原子或甲基,L1以及L2分别独立地表示氧原子可以介于其中的2价烃基或单键,n表示1以上的整数。从烯键式不饱和基团的当量在2000~20000g/mol的范围的观点出发,n优选为10~300。
作为1价烃基,可以列举出例如碳原子数为1~6的烷基或苯基。作为2价烃基,可以列举出例如碳原子数为1~20的亚烷基。
硅氧烷化合物的烯键式不饱和基团的当量可以为3000~18000g/mol、4000~15000g/mol或4500~13000g/mol。硅氧烷化合物的烯键式不饱和基团的当量如果在这样的范围内,则中间膜用树脂组合物具有高凝聚性,可以形成耐发泡性更加优良的中间膜。
本实施方式的共聚物中,基于硅氧烷化合物的单体单元的共聚比例是相对于共聚物的总质量优选为5~20质量%,更优选为10~20质量%。硅氧烷化合物的共聚比例如果在这样的范围内,则树脂层与被粘体的密合性提高,层叠体的强韧性提高,由此夹层玻璃的防裂性更进一步提高。
从进一步提高夹层玻璃的防裂性以及中间膜的透明性的观点出发,单体混合物可以含有50~90质量份(甲基)丙烯酸烷基酯、5~30质量份具有羟基的(甲基)丙烯酸酯以及5~20质量份硅氧烷化合物,也可以含有50~85质量份(甲基)丙烯酸烷基酯、10~30质量份具有羟基的(甲基)丙烯酸酯以及5~20质量份硅氧烷化合物。
单体混合物可以含有具有2个以上(甲基)丙烯酰基的化合物、具有(甲基)丙烯酰基以外的聚合性基团的化合物,只要是在不损害本发明的效果的范围内就行。作为具有(甲基)丙烯酰基以外的聚合性基团的化合物,可以列举出:例如,丙烯腈、苯乙烯、乙酸乙烯酯、乙烯、丙烯以及二乙烯基苯。
关于共聚物的重均分子量(Mw),通过凝胶渗透色谱(GPC)法使用标准聚苯乙烯的标准曲线换算而得到的值优选为80000~1000000,更优选为100000~900000,进一步优选为200000~800000。共聚物的Mw为80000以上时,容易得到对于被粘体具有密合性的树脂层,为1000000以下时,树脂组合物的粘度不会变得过高,形成树脂层时的加工性变得良好。
本实施方式的共聚物可以使用例如溶液聚合、乳化聚合、悬浮聚合、本体聚合等已知的聚合方法进行合成。
作为合成共聚物时的聚合引发剂,可以使用通过热产生自由基的化合物。作为聚合引发剂,可以列举出:例如,过氧化苯甲酰、过氧化月桂酰等有机过氧化物;2,2’-偶氮二异丁腈、2,2’-偶氮二(2-甲基丁腈)等偶氮系化合物。
(其他添加剂)
在树脂组合物中根据需要可以与上述共聚物一起含有各种添加剂。
作为添加剂,例如,为了提高树脂组合物的凝聚力,可以使用交联剂。作为交联剂的具体例子,可以列举出光交联剂以及热交联剂。
作为光交联剂,可以列举出:例如,具有碳原子数为1~20的亚烷基的亚烷基二醇二(甲基)丙烯酸酯;聚乙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯等亚烷基二醇二(甲基)丙烯酸酯;乙氧基化双酚A二(甲基)丙烯酸酯、乙氧基化双酚F二(甲基)丙烯酸酯、双酚A型环氧(甲基)丙烯酸酯等双酚型二(甲基)丙烯酸酯;以及具有氨基甲酸乙酯键的氨基甲酸乙酯二(甲基)丙烯酸酯。
从与其他成分的相容性良好的观点出发,具有氨基甲酸乙酯键的氨基甲酸乙酯二(甲基)丙烯酸酯可以具有聚亚烷基二醇链,从确保透明性的观点出发,可以具有脂环式结构。在光交联剂与共聚物的相容性低的情况下,由树脂组合物形成的树脂膜有可能发生白浊。
从能够进一步抑制高温或高温高湿下的气泡以及剥离发生的观点出发,光交联剂的Mw优选为100000以下,更优选为300~100000,进一步优选为500~80000。
在使用光交联剂时光交联剂的含量相对于共聚物的总质量优选为15质量%以下,更优选为10质量%以下,进一步优选为7质量%以下。如果在这样的范围,则可以得到具有充分的密合性的树脂层。关于光交联剂的含量的下限没有特别限制,但从使膜形成性变良好的观点出发,光交联剂的含量优选为0.1质量%以上,更优选为2质量%以上,进一步优选为3质量%以上。
作为热交联剂,可以使用例如异氰酸酯化合物、三聚氰胺化合物、环氧化合物等热交联剂。作为热交联剂,为了形成在树脂层中缓慢扩张的网眼状结构,更优选为3官能、4官能这样的多官能的热交联剂。
从反应性的观点出发,作为热交联剂,优选为异氰酸酯化合物,更优选为聚异氰酸酯化合物。作为聚异氰酸酯化合物,可以列举出:例如,己二异氰酸酯的三聚物、三羟甲基丙烷等的三醇、二醇或单官能醇、与己二异氰酸酯的反应产物即多官能性己二异氰酸酯化合物。
在使用热交联剂时热交联剂的含量相对于共聚物的总质量优选为5质量%以下,更优选为2质量%以下,进一步优选为1质量%以下。如果在这样的范围,则可以得到具有充分的密合性的树脂层。关于热交联剂的含量的下限没有特别限制,但从使膜形成性变良好的观点出发,热交联剂的含量优选为0.01质量%以上。
在共聚物或交联剂中的任意一种为利用活性能量射线的固化系的情况下,需要光聚合引发剂。光聚合引发剂通过活性能量射线的照射促进固化反应。活性能量射线是指紫外线、电子射线、α射线、β射线、γ射线等。
作为光聚合引发剂,没有特别限定,可以使用二苯甲酮化合物、蒽醌化合物、苯甲酰化合物、锍盐、重氮盐、鎓盐等公知的材料。
作为光聚合引发剂,可以列举出:例如,二苯甲酮、N,N,N’,N’-四甲基-4,4’-二氨基二苯甲酮(米勒酮)、N,N,N’,N’-四乙基-4,4’-二氨基二苯甲酮、4-甲氧基-4’-二甲基氨基二苯甲酮、α-羟基异丁酰苯、2-乙基蒽醌、叔丁基蒽醌、1,4-二甲基蒽醌、1-氯蒽醌、2,3-二氯蒽醌、3-氯-2-甲基蒽醌、1,2-苯并蒽醌、2-苯基蒽醌、1,4-萘醌、9,10-菲醌、噻吨酮、2-氯噻吨酮、1-羟基环己基苯基酮、2,2-二甲氧基-1,2-二苯基乙烷-1-酮、2-羟基-2-甲基-1-苯基丙烷-1-酮、2,2-二乙氧基苯乙酮等芳香族酮化合物;苯偶姻、甲基苯偶姻、乙基苯偶姻等苯偶姻化合物;苯偶姻甲基醚、苯偶姻乙基醚、苯偶姻异丁基醚、苯偶姻苯基醚等苯偶姻醚化合物;苄基、苄基二甲基缩酮等苄基化合物;β-(吖啶-9-基)(甲基)丙烯酸等酯化合物;9-苯基吖啶、9-吡啶基吖啶、1,7-二吖啶基庚烷等吖啶化合物;2-(邻氯苯基)-4,5-二苯基咪唑二聚物、2-(邻氯苯基)-4,5-二(间甲氧基苯基)咪唑二聚物、2-(邻氟苯基)-4,5-二苯基咪唑二聚物、2-(邻甲氧基苯基)-4,5-二苯基咪唑二聚物、2-(对甲氧基苯基)-4,5-二苯基咪唑二聚物、2,4-二(对甲氧基苯基)5-苯基咪唑二聚物、2-(2,4-二甲氧基苯基)-4,5-二苯基咪唑二聚物、2-(对甲基巯基苯基)-4,5-二苯基咪唑二聚物等2,4,5-三芳基咪唑二聚物;2-苄基-2-二甲基氨基-1-(4-吗啉代苯基)-1-丁酮;2-甲基-1-[4-(甲硫基)苯基]-2-吗啉代-1-丙烷;双(2,4,6-三甲基苯甲酰)-苯基氧化膦;低聚(2-羟基-2-甲基-1-(4-(1-甲基乙烯基)苯基)丙酮)。这些化合物可以组合使用多种。
作为不会使树脂组合物着色的光聚合引发剂,可以列举出:例如,1-羟基环己基苯基酮、2-羟基-2-甲基-1-苯基-丙烷-1-酮、1-[4-(2-羟基乙氧基)-苯基]-2-羟基-2-甲基-1-丙烷-1-酮等α-羟基烷基酰苯化合物;双(2,4,6-三甲基苯甲酰)-苯基氧化膦、双(2,6-二甲氧基苯甲酰)-2,4,4-三甲基-戊基氧化膦、2,4,6-三甲基苯甲酰-二苯基氧化膦等酰基氧化膦化合物;低聚(2-羟基-2-甲基-1-(4-(1-甲基乙烯基)苯基)丙酮)。
特别是为了形成厚树脂层,光聚合引发剂可以含有例如双(2,4,6-三甲基苯甲酰)-苯基氧化膦、双(2,6-二甲氧基苯甲酰)-2,4,4-三甲基-戊基氧化膦、2,4,6-三甲基苯甲酰-二苯基氧化膦等酰基氧化膦化合物。
光聚合引发剂的含量相对于树脂组合物的总质量优选为0.05~5质量%,更优选为0.1~3质量%,进一步优选为0.1~0.5质量%。通过使含量为5质量%以下,可以得到透过率高、而且色调也不会带有黄色感、透明性优良的中间膜。
在树脂组合物中根据需要还可以含有交联剂之外的添加剂。作为添加剂,可以列举出:例如,为了提高树脂组合物的保存稳定性而添加的对甲氧基苯酚等阻聚剂、为了提高使树脂组合物光固化而得到的中间膜的耐热性而添加的三苯基亚磷酸酯等抗氧化剂、为了提高树脂组合物对紫外线等光的耐性而添加的HALS(Hindered Amine Light Stabilizer)等光稳定化剂、为了提高树脂组合物对玻璃的密合性而添加的硅烷偶联剂。
<中间膜用膜材>
本实施方式的中间膜用膜材具有基材和设置在基材上的树脂层。树脂层是由上述中间膜用树脂组合物形成的层。
如图1所示,本实施方式的中间膜用膜材可以具有:树脂层11;和以夹着树脂层11的方式层叠的一个基材10和另一个基材12。
作为基材10,优选使用比基材12更轻剥离性的基材。作为基材10,可以列举出:例如,聚对苯二甲酸乙二醇酯、聚丙烯、聚乙烯等聚合物膜,其中,优选为聚对苯二甲酸乙二醇酯膜(以下,也有时称为“PET膜”)。从作业性的观点出发,基材10的厚度优选为25~150μm,更优选为30~100μm,进一步优选为40~80μm。
优选的是基材10的平面形状比树脂层11的平面形状大、且基材10的外缘向树脂层11的外缘的更外侧伸出。关于基材10的外缘向树脂层11的外缘进一步伸出的宽度,从能够进一步降低处理容易性、剥离容易性、灰尘等的附着的观点出发,优选为2~20mm,更优选为4~10mm。在树脂层11以及基材10的平面形状为大致长方形等大致矩形状的情况下,关于基材10的外缘向树脂层11的外缘进一步伸出的宽度,优选的是在至少1个边中为2~20mm,更优选的是在至少1个边中为4~10mm,进一步优选的是在全部边中为2~20mm,特别优选的是在全部边中为4~10mm。
作为基材12,优选使用比基材10更重剥离性的基材。作为基材12,可以列举出:例如,聚对苯二甲酸乙二醇酯、聚丙烯、聚乙烯等聚合物膜,其中,优选为PET膜。从作业性的观点出发,基材12的厚度优选为50~200μm,更优选为60~150μm,进一步优选为70~130μm。
优选的是基材12的平面形状大于树脂层11的平面形状,且基材12的外缘向树脂层11的外缘的更外侧伸出。从能够进一步降低处理容易性、剥离容易性、灰尘等的附着的观点出发,基材12的外缘向树脂层11的外缘进一步伸出的宽度优选为2~20mm,更优选为4~10mm。在树脂层11以及基材12的平面形状为大致长方形等大致矩形状的情况下,基材12的外缘向树脂层11的外缘进一步伸出的宽度优选的是在至少1个边中为2~20mm,更优选的是在至少1个边中为4~10mm,进一步优选的是在全部边中为2~20mm,特别优选的是在全部边中为4~10mm。
基材10与树脂层11之间的剥离强度优选低于基材12与树脂层11之间的剥离强度。由此,基材12与基材10相比难以从树脂层11上剥离。剥离强度可以通过例如实施基材12以及基材10的表面处理来调节。作为表面处理方法,可以列举出:例如,通过硅系化合物或氟系化合物对基材进行脱模处理。
作为形成树脂层11的方法,可以使用公知的技术。例如,首先,将本实施方式的树脂组合物用2-丁酮、环己酮、甲乙酮、乙酸乙酯、甲苯等挥发性溶剂稀释来制备涂液。接着,将上述涂液涂布在基材12上,通过干燥而除去溶剂,可以形成具有任意厚度的树脂层。在制备上述涂液时,可以在配合各成分后用溶剂稀释,也可以在各成分的配合前预先用溶剂稀释。作为涂布方法,可以使用例如流涂法、辊涂法、凹版涂布法、绕线棒涂布法、唇模涂布法等公知的方法。
在基材12上形成树脂层11后,在树脂层11上层叠基材10,由此制作本实施方式的中间膜用膜材。形成下述构成:树脂层11被基材10以及基材12夹持。为了控制树脂层11与基材10以及基材12的剥离性,可以在树脂组合物中含有聚二甲基硅氧烷系表面活性剂、氟系表面活性剂等表面活性剂。
树脂层11的厚度会根据使用用途以及方法来适当调节,所以没有特别限定,可以为10~5000μm、25~200μm、25~180μm或者25~150μm。在该范围内使用的情况下,可得到对于从外部施加的冲击而言防裂性更加优良的夹层玻璃用中间膜。
树脂层11对于可见光区域(波长:380nm~780nm)的光线的透光率优选为80%以上,更优选为90%以上,进一步优选为95%以上。
树脂层11的雾度优选为5%以下,更优选为3%以下,进一步优选为1%以下。
根据本实施方式的中间膜用膜材,能够使保管以及搬运变容易而不会使树脂层11损坏。
树脂层11可以作为用于使被粘体彼此之间粘贴的中间膜使用,能够使例如玻璃彼此之间、玻璃与透明塑料基板、或者透明塑料基板彼此之间粘贴。在被粘体的至少一个中使用透明塑料基板时,树脂层11可以形成耐发泡性优良的中间膜。
<夹层玻璃>
本实施方式的中间膜用膜材可以适用于玻璃、透明塑料基板等被粘体的粘贴。
本实施方式的夹层玻璃具有对置的两片被粘体和夹持在两片被粘体之间的中间膜,两片被粘体之中的至少一个为玻璃板。上述夹层玻璃中,可以是被粘体中的一个为玻璃板,另一个为透明塑料基板。
作为玻璃,可以列举出:例如,浮法玻璃、风冷强化玻璃、化学强化玻璃以及多层玻璃。玻璃的厚度例如可以为0.1~50mm、0.5~30mm、1~20mm或2~10mm。
作为透明塑料基板,可以列举出:例如,丙烯酸树脂基板、聚碳酸酯基板、环烯烃聚合物基板以及聚酯基板。透明塑料基板的厚度可以为例如0.1~10mm、0.5~5mm或1~5mm。
本实施方式的夹层玻璃的制造方法包括:隔着上述中间膜用膜材所具有的树脂层来使被粘体之间粘贴而得到层叠体的工序;和在30~150℃以及0.3~1.5MPa的条件下对上述层叠体进行加热加压处理的工序。
图2是示意地表示夹层玻璃的一个实施方式的截面图。图2所示的夹层玻璃依次层叠有浮法玻璃20(第一被粘体)、中间膜21、浮法玻璃22(第二被粘体)。图2所示的夹层玻璃可以通过例如下述的方法制造。
首先,将中间膜用膜材中的基材10从树脂层11上剥离,使树脂层11的表面露出。接着,将成为中间膜21的树脂层11的表面粘贴到作为第一被粘体的浮法玻璃20上,用辊等按压后,将基材12从树脂层11上剥离,使表面露出。接着,将树脂层11的表面粘贴到作为第二被粘体的浮法玻璃22上,进行加热加压处理(压热处理),制作隔着中间膜21(树脂层11)粘贴浮法玻璃20以及21而成的夹层玻璃。
通过使用树脂层11,可以没有褶皱地使被粘体彼此之间容易地粘贴,另外,还可以在低温短时间内进行加热加压处理的工序。通过使用树脂层11,能够维持夹层玻璃的稳定的透明性而不会使中间膜21白化。
关于加热加压处理的条件,温度为30~150℃,压力为0.3~1.5MPa,但从能够进一步除去卷入气泡的观点出发,可以为50~70℃、0.3~0.5MPa。另外,处理时间优选为5~60分钟,更优选为10~30分钟。
需要说明的是,上述方案中,作为第二被粘体使用了浮法玻璃,但第二被粘体可以为透明塑料基板。
本实施方式的中间膜可以用于组合夹层玻璃的防反射层、防污层、色素层、硬涂层等具有功能性的功能层后进行粘贴。
防反射层只要是具有可见光反射率达到5%以下的防反射性的层即可。作为防反射层,可以使用通过已知的防反射方法对透明的塑料膜等透明基材进行处理后的层。
防污层是用于使表面难以污染的层。作为防污层,可以使用为了降低表面张力而由氟系树脂或硅系树脂等构成的已知的层。
色素层是用于提高色纯度的层,用于降低在夹层玻璃中透过的不需要的波长的光。色素层可以通过使吸收不需要的波长的光的色素在树脂中溶解、在聚乙烯膜、聚酯膜等基材膜上制膜或层叠而得到。
硬涂层用于提高表面硬度。作为硬涂层,可以使用例如:氨基甲酸乙酯丙烯酸酯、环氧丙烯酸酯等丙烯酸树脂;环氧树脂等在聚乙烯膜等基材膜上制膜或层叠而成的层。同样地,为了提高表面硬度,可以使用在玻璃、丙烯酸树脂、聚碳酸酯等透明保护板上制膜或层叠而成的硬涂层。
在得到这样的层叠体的情况下,树脂层11可以使用层压辊、真空粘贴机或单张粘贴机进行层叠。
通过本实施方式的夹层玻璃的制造方法,能够制作对于从外部施加的冲击而言防裂性优良的夹层玻璃。另外,通过上述方法,在被粘体的一方使用透明塑料基板的情况下,能够制作在被粘体与中间膜之间不会发生剥离或气泡的夹层玻璃。
实施例
以下,通过实施例对本发明进行说明。需要说明的是,本发明不限于以下的实施例。
制造例中所制作的共聚物的重均分子量(Mw)是根据GPC法使用由标准聚苯乙烯制作的标准曲线、使用下述的GPC测定装置以及测定条件进行测定。
RI检测器:L-3350(株式会社日立制作所、制品名)
洗脱液:THF
色谱柱:Gelpac GL-R420+R430+R440(日立化成株式会社、制品名)
柱温:40℃
流量:2.0mL/分钟
制造例1
在具有冷却管、温度计、搅拌装置、滴液漏斗以及氮气导入管的反应容器中,加入丙烯酸2-乙基己酯85.0g、丙烯酸2-羟基乙酯10.0g、单末端甲基丙烯酰基改性聚硅氧烷化合物(信越化学工业株式会社制、制品名“X-22-2426”、烯键式不饱和基团的当量:12000g/mol)5.0g以及乙酸乙酯145.0g,在用100mL/分钟的风量进行氮气置换的同时,用15分钟从常温(25℃)加热至65℃。接着,在保持为65℃的同时,投入在乙酸乙酯5.0g中溶解过氧化月桂酰0.1g而成的溶液,使其反应8小时,得到固体成分浓度为40%的共聚物A-1(Mw700000)的溶液。
制造例2
在反应容器中加入丙烯酸2-乙基己酯70.0g、丙烯酸2-羟基乙酯10.0g、单末端甲基丙烯酰基改性聚硅氧烷化合物(烯键式不饱和基团的当量:12000g/mol)20.0g以及乙酸乙酯145.0g,除此以外,与制造例1同样地操作,得到固体成分浓度为40%的共聚物A-2(Mw700000)的溶液。
制造例3
在反应容器中加入丙烯酸2-乙基己酯80.0g、丙烯酸2-羟基乙酯10.0g、单末端甲基丙烯酰基改性聚硅氧烷化合物(信越化学工业株式会社、制品名“KF-2012”、烯键式不饱和基团的当量:4600g/mol)10.0g以及乙酸乙酯145.0g,除此以外,与制造例1同样地操作,得到固体成分浓度为40%的共聚物A-3(Mw700000)的溶液。
制造例4
在反应容器中加入丙烯酸2-乙基己酯70.0g、丙烯酸2-羟基乙酯10.0g、丙烯酰基吗啉10.0g、单末端甲基丙烯酰基改性聚硅氧烷化合物(烯键式不饱和基团的当量:12000g/mol)10.0g以及乙酸乙酯145.0g,除此以外,与制造例1同样地操作,得到固体成分浓度为40%的共聚物A-4(Mw700000)的溶液。
制造例5
加入丙烯酸2-乙基己酯90.0g、丙烯酸2-羟基乙酯10.0g以及乙酸乙酯145.0g,除此以外,与制造例1同样地操作,得到固体成分浓度为40%的共聚物A-5(Mw700000)的溶液。
制造例6
在反应容器中加入丙烯酸2-乙基己酯80.0g、丙烯酸4-羟基丁酯10.0g、单末端甲基丙烯酰基改性聚硅氧烷化合物(信越化学工业株式会社、制品名“X-22-174ASX”(烯键式不饱和基团的当量:900g/mol)10.0g以及乙酸乙酯145.0g,除此以外,与制造例1同样地操作,得到固体成分浓度为40%的共聚物A-6(Mw700000)的溶液。
<中间膜用树脂组合物的制备以及中间膜用膜材的制作>
实施例1
向制造例1中得到的共聚物A-1溶液的共聚物100质量份中混合作为热交联剂的聚异氰酸酯化合物(东曹株式会社、制品名“CORONATE HL”)0.2质量份,从而制备树脂组合物的涂液。
接着,在对表面脱模处理后的厚度为75μm的PET膜(基材12)上,使用棒涂机涂布上述树脂组合物的涂液以使得干燥后的厚度达到100μm,在100℃下加热干燥10分钟,形成树脂层。然后,在树脂层上被覆脱模处理后的厚度为75μm的PET膜(基材10),用1.0kgf的手压辊粘贴,制作中间膜用膜材。
实施例2
除了使用制造例2中得到的共聚物A-2的溶液以外,与实施例1同样地操作,得到树脂组合物的涂液以及中间膜用膜材。
实施例3
除了使用制造例3中得到的共聚物A-3的溶液以外,与实施例1同样地操作,得到树脂组合物的涂液以及中间膜用膜材。
实施例4
除了使用制造例4中得到的共聚物A-4的溶液以外,与实施例1同样地操作,得到树脂组合物的涂液以及中间膜用膜材。
比较例1
除了使用制造例5中得到的共聚物A-5的溶液以外,与实施例1同样地操作,得到树脂组合物的涂液以及中间膜用膜材。
比较例2
除了使用制造例6中得到的共聚物A-6的溶液以外,与实施例1同样地操作,得到树脂组合物的涂液以及中间膜用膜材。
比较例3
将测定红外吸收光谱时得到的与羟基对应的色谱峰的半峰宽为245cm-1的聚乙烯醇缩丁醛树脂(缩醛化度为68.0摩尔%、乙酸乙烯酯成分的比例为0.6摩尔%)100质量份、与作为增塑剂的三乙二醇双(2-乙基己酸酯)38质量份混合,用混合辊充分地熔融混炼后,通过压制成形机在150℃下压制成形30分钟,得到厚度为380μm的树脂膜,将其作为夹层玻璃用中间膜。
<评价>
关于各实施例以及比较例中得到的中间膜用膜材或树脂膜,通过以下的方法进行评价。将结果示于表1。
1.雾度的测定
将实施例以及比较例1和2的中间膜用膜材切割成50mm×50mm的尺寸,在85℃、85%RH的条件下放置24小时后,取出,剥离基材10,使树脂层的表面露出后,将树脂层的表面粘贴到纵为50mm、横为50mm、厚度为2.7mm的浮法玻璃上,用辊按压。将基材12从树脂层上剥离,使树脂层的表面露出,使用真空层叠机,在真空状态下将树脂层的表面粘贴到纵为50mm、横为50mm、厚度为2.7mm的浮法玻璃上,制作层叠体。然后,将层叠体在温度为50℃、压力为0.5MPa下保持30分钟的条件下进行加热加压处理(压热处理),得到夹层玻璃。另外,比较例3中,将树脂膜切割成50mm×50mm的尺寸,在85℃、85%RH的条件下放置24小时后,取出,用上述浮法玻璃夹着,在温度为135℃、压力为118N/cm2MPa、20分钟的条件下进行压热处理,得到夹层玻璃。
关于所得的夹层玻璃,使用浊度计(日本电色工业株式会社制、NDH-5000)测定雾度。
2.夹层玻璃的制作
实施例以及比较例1以及2中,从制作的中间膜用膜材上剥离基材10,使树脂层的表面露出后,将树脂层的表面粘贴到作为第一被粘体的纵为110mm、横为110mm、厚度为2.7mm的浮法玻璃上,用辊按压。接着,将基材12从树脂层上剥离,使树脂层的表面露出,使用真空层叠机,在真空状态下将树脂层的表面粘贴到作为第二被粘体的纵为110mm、横为110mm、厚度为2.7mm的浮法玻璃上,从而制作层叠体。然后,将层叠体在温度为50℃、压力为0.5MPa下保持30分钟的条件下进行加热加压处理(压热处理),得到夹层玻璃。
另外,比较例3中,将树脂膜用上述浮法玻璃夹着,在温度为135℃、压力为118N/cm2MPa、20分钟的条件下进行压热处理,从而得到夹层玻璃。
3.耐冲击试验
在距所制作的纵为110mm、横为110mm见方的夹层玻璃(周边支撑)的中心点为25mm以内的位置上使质量为约1040g、直径为63.5mm的钢球从5cm~100cm之中每隔5cm的高度依次落下,记录玻璃破裂时的高度。对6片由各个中间膜形成的夹层玻璃进行试验,计算出其平均高度,值越大,作为防裂性越高的夹层玻璃。
5.耐发泡性的评价
将第一被粘体变更为纵为70mm、横为50mm、厚度为2mm的浮法玻璃,将第二被粘体变更为纵为70mm、横为50mm、厚度为2mm的聚碳酸酯板,除此以外,与上述2.夹层玻璃的制作同样地进行,将玻璃板与透明塑料基板粘贴,制作耐发泡性的评价用样品。评价是通过下述方式来进行:对样品在下述条件下分别进行处理,然后取出,目视确认有无剥离以及发泡。表1中,“A”表示在任意处理条件下样品中都没有发生剥离以及气泡的情况,“B”表示在某一处理条件下样品中出现剥离以及气泡的情况。
(处理条件)
(1)高温高湿试验
将样品在85℃、85%RH的条件下放置24小时。
(2)高温试验
将样品在85℃的条件下放置24小时。
(3)热循环试验
实施将样品在-30℃气氛中放置30分钟、在85℃气氛中放置30分钟的热循环20次。
表1
符号说明
10,12 基材、11 树脂层、20,22 浮法玻璃、21 中间膜。
Claims (8)
1.一种中间膜用树脂组合物,其包含单体混合物的共聚物,所述单体混合物含有(甲基)丙烯酰基化合物和硅氧烷化合物,所述硅氧烷化合物具有烯键式不饱和基团且烯键式不饱和基团的当量为2000~20000g/mol。
2.根据权利要求1所述的中间膜用树脂组合物,其中,所述(甲基)丙烯酰基化合物含有(甲基)丙烯酸烷基酯和具有羟基的(甲基)丙烯酸酯。
3.根据权利要求2所述的中间膜用树脂组合物,其中,所述单体混合物含有50~90质量份所述(甲基)丙烯酸烷基酯、5~30质量份所述具有羟基的(甲基)丙烯酸酯以及5~20质量份所述硅氧烷化合物。
4.根据权利要求1~3中任一项所述的中间膜用树脂组合物,其还含有热交联剂。
5.一种中间膜用膜材,其具有基材和设置在所述基材上的树脂层,所述树脂层为由权利要求1~4中任一项所述的中间膜用树脂组合物形成的层。
6.根据权利要求5所述的中间膜用膜材,其中,所述树脂层的雾度为5%以下。
7.一种夹层玻璃的制造方法,所述夹层玻璃具有对置的两片被粘体和夹持在所述两片被粘体之间的中间膜,所述制造方法包括下述工序:
隔着权利要求5或6所述的中间膜用膜材所具有的所述树脂层来使所述两片被粘体粘贴而得到层叠体的工序;和
在30~150℃以及0.3~1.5MPa的条件下对所述层叠体进行加热加压处理的工序,
其中,所述两片被粘体之中的至少一个为玻璃板。
8.根据权利要求7所述的方法,其中,所述两片被粘体之中的一个为玻璃板,另一个为透明塑料基板。
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JP2011073943A (ja) * | 2009-09-30 | 2011-04-14 | Dainippon Printing Co Ltd | 合わせガラスの製造方法 |
CN106082713B (zh) | 2010-12-28 | 2019-04-12 | 积水化学工业株式会社 | 夹层玻璃用中间膜及夹层玻璃 |
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US20200047467A1 (en) | 2020-02-13 |
KR20190078556A (ko) | 2019-07-04 |
JPWO2018078873A1 (ja) | 2019-09-12 |
JP6733740B2 (ja) | 2020-08-05 |
TW201821520A (zh) | 2018-06-16 |
WO2018078873A1 (ja) | 2018-05-03 |
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