CN116034022A - 夹层玻璃用中间膜、夹层玻璃和夹层玻璃用层叠体 - Google Patents
夹层玻璃用中间膜、夹层玻璃和夹层玻璃用层叠体 Download PDFInfo
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- CN116034022A CN116034022A CN202180054255.4A CN202180054255A CN116034022A CN 116034022 A CN116034022 A CN 116034022A CN 202180054255 A CN202180054255 A CN 202180054255A CN 116034022 A CN116034022 A CN 116034022A
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- Prior art keywords
- resin layer
- laminated glass
- resin
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- interlayer film
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Abstract
夹层玻璃用中间膜10,具备第一树脂层11、第二树脂层12和配置在第一树脂层11和第二树脂层12之间的塑料层13,第一树脂层11含有热塑性树脂,第一树脂层的厚度为900μm以下且镁元素浓度小于25ppm,第二树脂层12含有热塑性树脂,第二树脂层中的镁元素和钾元素合计浓度为25ppm以上,在将2片2.5mm厚的玻璃板介隔夹层玻璃用中间膜10贴合后依照JIS R 3212:2015进行的落球试验中,在夹层玻璃用中间膜的含水率为0.4%和2.0%的任一种情况下都满足落球高度(MBH)为5m以上的要件。
Description
技术领域
本发明涉和夹层玻璃用中间膜、夹层玻璃和用于形成夹层玻璃用中间膜的夹层玻璃用层叠体。
背景技术
夹层玻璃即使受到外部冲击而破损,玻璃碎片也很少飞散,是安全的,因此作为汽车等车辆的前玻璃、侧玻璃、后玻璃、棚顶玻璃、飞机、建筑物等的窗玻璃等被广泛使用。作为夹层玻璃,在一对玻璃之间夹设含有聚乙烯醇缩醛树脂等树脂成分的夹层玻璃用中间膜而一体化的夹层玻璃已经被广为人知。
夹层玻璃用中间膜可为多层以赋予各种功能。例如,在专利文献1中公开了一种夹层玻璃用中间膜,该夹层玻璃用中间膜具有杨氏模量为1GPa以上的塑料层和层叠在塑料层的两个表面上的第一树脂层和第二树脂层。在专利文献1中,通过上述结构,可以提高夹层玻璃中间膜的操作性和耐击穿性等,进而可以减小破损后的碎片等。
另外,在专利文献2~4中,作为能够兼顾高隔热性和高可见光线透过率的夹层玻璃用中间膜,公开了具备红外线反射层和分别配置在红外线反射层的两面的第一树脂层和第二树脂层,且在第二树脂层中配合有金属氧化物粒子等的中间膜。
现有技术文献
专利文献
专利文献1:国际公开2014/021407号
专利文献2:国际公开2014/021406号
专利文献3:日本特开2015-196612号公报
专利文献4:国际公开2015/115626号
发明内容
发明要解决的课题
但是,夹层玻璃用中间膜一般如专利文献4所公开的那样,配合钾盐、镁盐等粘接力调节剂来进行与玻璃的粘接力的调整。另一方面,夹层玻璃用中间膜在各种环境中使用,不仅在低湿环境下使用,有时也在高湿环境下使用。
但是,钾盐和镁盐具有很好地吸附水的性质,配合了钾盐或镁盐的夹层玻璃用中间膜通过在高湿环境下使用,有含水率变高、粘接力变高的倾向。因此,在高湿环境下难以控制粘接力,有可能产生耐击穿性能降低等不良情况。
因此,本发明的目的在于,使具有3层以上的层的多层夹层玻璃用中间膜无论在高湿下还是低湿下都耐击穿性能良好。
解决课题手段
本发明人等进行了深入研究,结果发现,在具有第一树脂层和第二树脂层和配置在它们间的塑料层的夹层玻璃用中间膜中,通过使树脂层的厚度、和各树脂层中的镁元素的浓度、或镁元素和钾元素的合计浓度在规定的范围内,能够解决上述课题,完成了以下的本发明。即,本发明提供以下的[1]~[31]。
[1].一种夹层玻璃用中间膜,具备第一树脂层、第二树脂层和配置在所述第一树脂层和第二树脂层之间的塑料层,
所述第一树脂层含有热塑性树脂,所述第一树脂层的厚度为900μm以下且镁元素浓度小于25ppm,
所述第二树脂层含有热塑性树脂,所述第二树脂层中的镁元素和钾元素合计浓度为25ppm以上,
在将2片2.5mm厚的玻璃板介隔所述夹层玻璃用中间膜贴合后依照JIS R 3212:2015进行的落球试验中,在所述夹层玻璃用中间膜的含水率为0.4%和2.0%的任一种情况下,都满足落球高度MBH为5m以上的要件。
[2].根据[1]所述的夹层玻璃用中间膜,所述第一树脂层中的镁元素和钾元素的合计浓度小于25ppm。
[3].根据[2]所述的夹层玻璃用中间膜,所述第一树脂层的厚度为800μm以下,且所述合计浓度为20ppm以下。
[4].根据[1]~[3]中任一项所述的夹层玻璃用中间膜,所述第二树脂层的厚度为900μm以下。
[5].根据[1]~[4]中任一项所述的夹层玻璃用中间膜,所述第二树脂层的厚度为100μm以上。
[6].根据[1]~[5]中任一项所述的夹层玻璃用中间膜,所述第二树脂层的厚度为350μm以上,且所述合计浓度为30ppm以上。
[7].根据[1]~[6]中任一项所述的夹层玻璃用中间膜,所述塑料层的厚度为30μm以上且200μm以下。
[8].根据[1]~[7]中任一项所述的夹层玻璃用中间膜,所述第一树脂层含有具有对苯二甲酸酯结构的发光材料。
[9].根据[1]~[8]中任一项所述的夹层玻璃用中间膜,所述第一树脂层含有磷酸酯化合物。
[10].根据[1]~[9]中任一项所述的夹层玻璃用中间膜,所述第一树脂层含有隔热粒子。
[11]根据[10]所述的夹层玻璃用中间膜,其中,所述隔热粒子为选自金属氧化物粒子和六硼化镧粒子中的至少一种。
[12].根据[1]~[11]中任一项所述的夹层玻璃用中间膜,第一树脂层的所述合计浓度与所述第二树脂层的所述合计浓度之差为10ppm以上且300ppm以下。
[13].根据[1]~[12]中任一项所述的夹层玻璃用中间膜,上述第一树脂层和第二树脂层中含有热塑性树脂分别为选自聚乙烯醇缩醛树脂、乙烯-乙酸乙烯酯共聚物树脂、离聚物树脂、聚氨酯树脂和热塑性弹性体中的至少一种。
[14].根据[1]~[13]中任一项所述的夹层玻璃用中间膜,所述第一树脂层和第二树脂层中含有的热塑性树脂为聚乙烯醇缩醛树脂。
[15]根据上述[1]~[14]中任一项所述的夹层玻璃用中间膜,其中,所述塑料层含有选自聚酯树脂膜和丙烯酸树脂膜中的至少一种。
[16]根据上述[1]~[15]中任一项所述的夹层玻璃用中间膜,其中,所述塑料层含有聚对苯二甲酸乙二醇酯膜。
[17]根据上述[1]~[16]中任一项所述的夹层玻璃用中间膜,其中,在所述第二树脂层中,镁元素的含有比例高于钾元素的含有比例。
[18]根据上述[1]~[17]中任一项所述的夹层玻璃用中间膜,所述第一树脂层的厚度为100μm以上。
[19]如上述[1]~[18]中任一项所述的夹层玻璃用中间膜,其中,所述第二树脂层含有粘接力调节剂。
[20]根据上述[19]所述的夹层玻璃用中间膜,其中,所述粘接力调节剂是选自钾盐和镁盐中的至少一种金属盐。
[21]根据上述[1]~[20]中任一项所述的夹层玻璃用中间膜,其中,所述第一树脂层不含有粘接力调节剂,或者相对于100质量份热塑性树脂,含有小于0.005质量份。
[22]根据上述[1]-21]中任一项所述的夹层玻璃用中间膜,其中,所述第一树脂层含有发光材料。
[23]根据上述[1]~[22]中任一项所述的夹层玻璃用中间膜,其中,所述第二树脂层实质上不含有具有对苯二甲酸酯结构的发光材料。
[24]根据上述[1]~[23]中任一项所述的夹层玻璃用中间膜,其中,所述第二树脂层实质上不含有磷酸酯化合物。
[25]根据上述[1]~[24]中任一项所述的夹层玻璃用中间膜,其中,所述第一树脂层和第二树脂层均含有增塑剂。
[26]根据上述[1]-25]中任一项所述的夹层玻璃用中间膜,其中,所述塑料层实质上不含有增塑剂。
[27]一种夹层玻璃,其具有上述[1]~[26]中任一项所述的夹层玻璃用中间膜、第一玻璃板和第二玻璃板,所述夹层玻璃用中间膜配置在所述第一玻璃板和所述第二玻璃板之间。
[28]一种夹层玻璃用层叠体,其用于与第一树脂层重叠而形成夹层玻璃用中间膜,
所述夹层玻璃用层叠体具备塑料层和层叠在所述塑料层一个面上的第二树脂层,
所述第一树脂层含有热塑性树脂,所述第一树脂层的厚度为900μm以下且镁元素浓度小于25ppm,
所述第二树脂层含有热塑性树脂,所述第二树脂层中的镁元素和钾元素的合计浓度为25ppm以上,
将夹层玻璃用层叠体以使所述塑料层配置在所述第一树脂层和第二树脂层之间的方式与所述第一树脂层重合而形成夹层玻璃用中间膜,介隔所述夹层玻璃用中间膜将2片2.5mm厚的玻璃板进行贴合、并依照JIS R3212:2015进行落球试验,在该试验中、在所述夹层玻璃用中间膜的含水率为0.4%和2.0%的任一种情况下都满足落球高度MBH为5m以上的要件。
[29]一种组件,具有上述[28]所述的上述夹层玻璃用层叠体和上述第一树脂层。
[30].一种夹层玻璃用层叠体,其用于与第二树脂层重叠而形成夹层玻璃用中间膜,
所述夹层玻璃用层叠体具备塑料层和层叠在所述塑料层一个面上的第一树脂层,
所述第一树脂层含有热塑性树脂,所述第一树脂层的厚度为900μm以下且镁元素浓度小于25ppm,
所述第二树脂层含有热塑性树脂,所述第二树脂层中的镁元素和钾元素的合计浓度为25ppm以上,
将夹层玻璃用层叠体以使所述塑料层配置在所述第一树脂层和第二树脂层之间的方式与所述第二树脂层重合而形成夹层玻璃用中间膜,介隔所述夹层玻璃用中间膜将2片2.5mm厚的玻璃板进行贴合、并依照JIS R3212:2015进行落球试验,在该试验中、在所述夹层玻璃用中间膜的含水率为0.4%和2.0%的任一种情况下都满足落球高度MBH为5m以上的要件。
[31]一种组件,具有上述[30]所述的上述夹层玻璃用层叠体和上述第二树脂层。
发明效果
根据本发明,具有3层以上的层的多层夹层玻璃用中间膜在高湿下和低湿下的任一种都能够良好地实现耐击穿性能。
附图说明
图1是表示本发明的一个实施方式的夹层玻璃用中间膜的剖面图。
图2是表示本发明的一个实施方式的夹层玻璃的剖面图。
具体实施方式
<夹层玻璃用中间膜>
以下,对本发明进行详细说明。
本发明的夹层玻璃用中间膜(以下有时简称为“中间膜”)是具有3层以上的中间膜。如图1所示,本发明的中间膜10包括含有热塑性树脂的第一树脂层11、含有热塑性树脂的第二树脂层12、以及配置在它们之间的塑料层13。第一树脂层和第二树脂层11、12分别可以直接层叠在塑料层13上,也可以隔着粘接层等其他层层叠在塑料层13上。
[镁元素和钾元素的合计浓度]
在本发明中,第一树脂层的镁元素浓度小于25ppm,并且第二树脂层的镁元素和钾元素的合计浓度(以下有时简称为“合计金属浓度”)为25ppm以上。本发明的夹层玻璃用中间膜通过具有以上的结构,在后述的落球试验中,即使在含水率为0.4%、2.0%的任一种情况下,都能够满足落球高度(MBH)为5m以上的条件,在高湿下和低湿环境下的任一种情况下都能够提高耐击穿性能。其原理虽然不确定,但推测如下。
树脂层在低湿环境下含水率变低,镁元素和钾元素的合计浓度高时,由于这些金属元素的作用,对玻璃板的粘接力变低。因此,本发明的夹层玻璃用中间膜在低湿环境下,通过第二树脂层的合计金属浓度为25ppm以上,由此能够使得夹层玻璃对另一玻璃板的粘接力调整得较低。其结果,本发明的中间膜对两块玻璃板的粘接力维持在适当的大小,提高了低湿环境下的耐击穿性。
另一方面,在高湿环境下含水率变高时,上述合计金属浓度高的第二树脂层对玻璃板的粘接力变高。但是,第一树脂层通过镁元素的浓度低,能够降低对高湿环境下的玻璃板的粘接力,因此本发明的中间膜即使在高湿环境下,也能够防止对2片玻璃板的粘接力过高,能够得到良好的耐击穿性。
在高湿环境下,从防止中间膜对玻璃板粘接力过高、提高耐击穿性的观点出发,第一树脂层中镁元素的浓度优选为20ppm以下,更优选为15ppm以下,进一步优选为10ppm以下、更优选5ppm以下。另外,关于下限值,第一树脂层中的镁元素的浓度没有特别限定,只要为0ppm以上即可,但考虑不可避免地混入的金属量,通常为0.1ppm以上,另外,也可以为0.5ppm以上。
从在高湿环境下可靠地降低第一树脂层对玻璃板粘接力的观点出发,在第一树脂层中,镁元素和钾元素的合计浓度(合计金属浓度)优选小于25ppm,更优选20ppm以下,进一步优选15ppm以下、更优选10ppm以下,特别优选5ppm以下。另外,关于下限值,第一树脂层中的合计金属浓度没有特别限定,只要为0ppm以上即可,但考虑不可避免地混入的金属量,通常为0.1ppm以上,另外,也可以为0.5ppm以上。
另外,从在低湿下适当地降低第二树脂层对玻璃板粘接力,同时在高湿下适当地增大第二树脂层对玻璃板的粘接力的观点出发,第二树脂层中的上述合计金属浓度优选为25ppm以上,更优选为30ppm以上、更优选35ppm以上,更优选40ppm以上。另外,从耐湿性等观点出发,第二树脂层中的上述合计金属浓度优选为300ppm以下,更优选为250ppm以下,进一步优选为200ppm以下,进一步优选为150pm以下。
另外,第一树脂层的合计金属浓度与第二树脂层的合计金属浓度之差优选为10ppm以上300ppm以下。若将合计金属浓度的差设为10ppm以上,则在高湿和低湿环境下的任何一种情况下,都容易使对两块玻璃板的粘接力均衡地成为适当的大小,从而容易维持较高的耐击穿性。另外,若将合计金属浓度的差设为300ppm以下,则能够防止第二树脂层的合计金属浓度变大到必要以上,提高耐湿性等。
上述合计金属浓度之差更优选为15ppm以上,进一步优选为20ppm以上,进一步优选为25ppm以上,进一步优选为30ppm以上,另外,更优选为200ppm以下、更优选150ppm以下,进而更优选100ppm以下。
另外,镁元素的浓度和钾元素的浓度是通过ICP发射光谱分析法测定的各树脂层中含有的镁(Mg)元素、钾(K)元素的含量(质量)浓度。另外,合计金属浓度是各树脂层中的镁(Mg)元素的浓度和钾(K)元素的浓度的合计量。
第二树脂层优选含有来自后述的粘接力调节剂的镁元素和钾元素中的至少一种。但是,在第二树脂层中使用的热塑性树脂、添加剂、制造过程中使用的各种溶剂等中,通常作为微量的杂质含有镁元素和钾元素。因此,第二树脂层不仅可以含有来自粘接力调节剂的物质,还可以含有来自粘接力调节剂以外的镁元素、钾元素或这两者。
第一树脂层可以含有或不含有后述的粘接力调节剂,因此,可以含有或不含有来自粘接力调节剂的镁元素和钾元素中的至少一种。但是,与第二树脂层同样,第一树脂层通常可以含有来自粘接力调节剂以外的镁元素、钾元素或这两者。
另外,如上所述,第二树脂层也可以含有镁元素和钾元素这两者。此时,在第二树脂层中,镁元素的含有比例可以高于钾元素的含有比例,钾元素的含有比例可以高于镁元素的含有比例,两者的含有比例也可以相同。但是,第二树脂层优选镁元素的含有比例比钾元素的含有比例高。
同样,第一树脂层可以含有镁元素和钾元素两者,此时,在第一树脂层中,镁元素含有比例可以高于钾元素的含有比例,钾元素的含有比例可以高于镁元素的含有比例两者的含有比例、也可以相同。
耐击穿性
本发明的中间膜隔着该中间膜贴合2片2.5mm厚的玻璃板,在依照JIS R 3212:2015进行的各落球试验中,在中间膜的含水率为0.4%和2.0%的情况下都满足落球高度(MBH)为5m以上的要件。本发明的中间膜在上述落球试验中,在含水率为0.4%或2.0%的情况下,即使MBH为5m,夹层玻璃也不会击穿,因此在高湿和低湿环境下的任一种中,耐击穿性都优异。
[各层的厚度]
在本发明中间膜中,第一树脂层的厚度为900μm以下。第一树脂层的厚度大于900μm时,中间膜的厚度大于需要,实用性降低。另外,厚度为大于900μm时,即使不如上所述调整第一树脂层和第二树脂层的合计金属浓度,也容易使耐击穿性良好。因此,难以发挥将第一树脂层的镁浓度以及第一树脂层和第二树脂层的合计金属浓度调整到规定的范围内的效果。
从这些观点出发,第一树脂层的厚度优选为800μm以下,更优选700μm以下,更优选600μm以下。另外,第一树脂层的厚度为800μm以下且合计金属浓度为20ppm以下时,能够更有效地发挥本发明的效果。
另外,从确保耐击穿性、耐冲击性、与玻璃粘接性等观点出发,第一树脂层的厚度为100μm以上是优选,200μm以上更优选,350μm以上进而更优选。
在本发明中间膜中,第二树脂层的厚度例如为900μm以下。第二树脂层的厚度为900μm以下时,可以防止中间膜的厚度大于需要。另外,厚度为900μm以下时,通过如上调整各树脂层的镁浓度和合计金属浓度,容易发挥耐击穿性良好的效果。
从这些观点出发,第二树脂层的厚度优选为850μm以下,更优选800μm以下,进而更优选780μm以下。
另外,从确保耐击穿性、耐冲击性、与玻璃粘接性等观点出发,第二树脂层的厚度为100μm以上是优选,200μm以上更优选,350μm以上进而更优选。另外,第二树脂层的厚度为350μm以上且合计金属浓度为30ppm以上时,能够更有效地提高耐击穿性。
塑料层的厚度优选为30μm以上200μm以下。30μm以上,容易使中间膜的耐击穿性良好。另外,容易使塑料层的阻挡性能良好。另外,通过为200μm以下,容易确保中间膜的柔软性,耐冲击性等良好。从这些观点出发,塑料层的厚度为40μm以上更优选,45μm以上进而更优选,另外,150μm以下更优选,120μm以下更进而优选。
另外,从确保中间膜的柔软性、耐冲击性等的观点出发,塑料层的厚度优选比第一树脂层和第二树脂层的任一厚度都小。
中间膜整体厚度例如为400μm以上2000μm以下。通过使中间膜整体厚度为400μm以上,容易使对玻璃板的粘接性、耐击穿性等良好。另外,通过设为2000μm以下,在实用上容易用于夹层玻璃。从这些观点出发,中间膜整体厚度优选为500μm以上1700μm以下,更优选600μm以上1400μm以下,更优选700μm以上1250μm以下。
[热塑性树脂]
第一树脂层包括热塑性树脂。第二树脂层包括热塑性树脂。第一树脂层和第二树脂层通过含有热塑性树脂,容易起到作为粘接层的功能,与玻璃板或塑料层的粘接性良好。
作为可以在第一树脂层和第二树脂层中使用的热塑性树脂,没有特别限定,例如可以列举出聚乙烯醇缩醛树脂、乙烯-乙酸乙烯酯共聚物树脂、离聚物树脂、聚氨酯树脂、热塑性弹性体等。通过使用这些树脂,容易确保与玻璃板的粘接性。
在各树脂层中,热塑性树脂可以单独使用1种,也可以并用2种以上。
上述热塑性树脂中,优选选自聚乙烯醇缩醛树脂和乙烯-乙酸乙烯酯共聚物树脂中的至少一种。热塑性树脂在与增塑剂并用时,从对玻璃发挥优异的粘接性的观点出发,更优选聚乙烯醇缩醛树脂。如后所述,聚乙烯醇缩醛树脂优选聚乙烯醇缩丁醛树脂。
第一树脂层中的热塑性树脂和第二树脂层中的热塑性树脂可以使用彼此相同种类的树脂,也可以使用不同的树脂,但从制造容易性等观点出发,优选使用相同种类的树脂。
因此,第一树脂层和第二树脂层中的热塑性树脂均优选聚乙烯醇缩醛树脂或乙烯-乙酸乙烯酯共聚物树脂,均更优选聚乙烯醇缩醛树脂,其中均更优选聚乙烯醇缩醛树脂。
(聚乙烯醇缩醛树脂)
在第一树脂层和第二树脂层中均使用的聚乙烯醇缩醛树脂是将聚乙烯醇用醛缩醛化而得到的。聚乙烯醇例如通过皂化聚乙酸乙烯酯等聚乙烯酯而得到。聚乙烯醇缩醛树脂可以单独使用1种,也可以并用2种以上。
用于缩醛化的醛没有特别限定,优选使用碳原子数为1~10的醛,更优选碳原子数为2~6的醛,进一步优选碳原子数为4的醛。
上述碳原子数为1~10的醛没有特别限定,例如可以列举出正丁醛、异丁醛、正戊醛、2-乙基丁醛、正己醛、正辛醛、正壬醛、正癸醛、甲醛、乙醛、苯甲醛等。其中,优选正丁醛、正己醛、正戊醛,更优选正丁醛。这些醛可以单独使用,也可以并用2种以上。
另外,作为聚乙烯醇,一般使用皂化度80~99.8摩尔%的聚乙烯醇。为了将聚乙烯醇缩醛树脂的平均聚合度调整到所希望的范围内,聚乙烯醇的平均聚合度优选为500以上,另外,优选为4000以下。聚乙烯醇的平均聚合度更优选为1000以上,另外更优选为3600以下。聚乙烯醇的平均聚合度通过依据JIS K6726“聚乙烯醇试验方法”的方法求出。
聚乙烯醇缩醛树脂中所含的缩醛基的碳原子数没有特别限定,优选为1~10,更优选为2~6,进一步优选为4。作为缩醛基,具体而言特别优选丁醛基,因此,作为聚乙烯醇缩醛树脂,优选聚乙烯醇缩丁醛树脂。
聚乙烯醇缩醛树脂的缩醛化度优选为40摩尔%以上,另外优选为85摩尔%以下。另外,缩醛化度更优选为60摩尔%以上,另外,更优选为75摩尔%以下。另外,缩醛化度是指缩醛基为丁醛基,聚乙烯醇缩醛树脂为聚乙烯醇缩丁醛树脂时,是指丁醛化度。
聚乙烯醇缩醛树脂的羟基量优选为15摩尔%以上,另外优选为35摩尔%以下。通过使羟基量为15摩尔%以上,与玻璃板等的粘接性容易变得良好,容易使夹层玻璃的耐击穿性等变得良好。另外,通过使羟基量为35摩尔%以下,可以防止夹层玻璃变得过硬。聚乙烯醇缩醛树脂的羟基量更优选为20摩尔%以上,另外更优选为33摩尔%以下。
聚乙烯醇缩醛树脂的酰化度(酰基量)优选为0.1摩尔%以上,另外优选为20摩尔%以下。通过使酰化度为上述下限值以上,容易与增塑剂等的相容性良好。另外,通过设为上述上限值以下,各树脂层的耐湿性变高。从这些观点出发,酰化度更优选为0.3摩尔%以上,进一步优选为0.5摩尔%以上,另外,更优选为10摩尔%以下,进一步优选为5摩尔%以下。
另外,羟基量、缩醛化度(丁醛化度)和酰化度可以根据JIS K6728“聚乙烯醇缩丁醛试验方法”的方法测定的结果来计算。
聚乙烯醇缩醛树脂的平均聚合度优选为500以上,另外优选为4000以下。通过使平均聚合度为500以上,夹层玻璃的耐击穿性变得良好。另外,通过使平均聚合度为4000以下,夹层玻璃容易成型。聚合度更优选为1000以上,另外更优选为3600以下。另外,聚乙烯醇缩醛树脂的平均聚合度与作为原料的聚乙烯醇的平均聚合度相同,可以通过聚乙烯醇的平均聚合度求出。
(乙烯-乙酸乙烯酯共聚物树脂)
作为乙烯-乙酸乙烯酯共聚物树脂,可以是非交联型的乙烯-乙酸乙烯酯共聚物树脂,另外,也可以是高温交联型的乙烯-乙酸乙烯酯共聚物树脂。作为乙烯-乙酸乙烯酯共聚物树脂,也可以使用乙烯-乙酸乙烯酯共聚物皂化物、乙烯-乙酸乙烯酯的水解物等乙烯-乙酸乙烯酯改性体树脂。
乙烯-乙酸乙烯酯共聚物树脂,依据JIS K 6730“乙烯·乙酸乙烯酯树脂试验方法”或JIS K 6924-2:1997测定的乙酸乙烯酯含量优选为10质量%以上50质量%以下,更优选20质量%以上40质量%以下。通过使乙酸乙烯酯含量为这些下限值以上,对玻璃的粘接性变高,另外,在夹层玻璃中使用时夹层玻璃的耐击穿性容易变好。另外,通过使乙酸乙烯酯含量为这些上限值以下,树脂层的断裂强度变高,夹层玻璃的耐冲击性变好。
(离聚物树脂)
作为离聚物树脂,没有特别限定,可以使用各种离聚物树脂。具体而言,可以列举出乙烯系离聚物、苯乙烯系离聚物、全氟碳系离聚物、遥爪离聚物、聚氨酯离聚物等。其中,从后述的夹层玻璃的机械强度、耐久性、透明性等良好的方面、对玻璃的粘接性优异的方面考虑,优选乙烯系离聚物。
作为乙烯系离聚物,由于乙烯·不饱和羧酸共聚物的离聚物的透明性和强韧性优异,因此优选使用。乙烯-不饱和羧酸共聚物是至少具有来自乙烯的结构单元和来自不饱和羧酸的结构单元的共聚物,也可以具有来自其他单体的结构单元。
作为不饱和羧酸,可以列举出丙烯酸、甲基丙烯酸、马来酸等,优选丙烯酸、甲基丙烯酸,特别优选甲基丙烯酸。另外,作为其他单体,可以列举出丙烯酸酯、甲基丙烯酸酯、1-丁烯等。
作为乙烯·不饱和羧酸共聚物,如果将该共聚物具有的全部构成单元设为100摩尔%,则优选具有75~99摩尔%的来自乙烯的构成单元,优选具有1~25摩尔%的来自不饱和羧酸的构成单元。
乙烯·不饱和羧酸共聚物的离聚物是通过用金属离子中和或交联乙烯·不饱和羧酸共聚物所具有的羧基的至少一部分而得到的离聚物树脂,但该羧基的中和度通常为1~90%、优选为5~85%。
作为离聚物树脂中的离子源,可以列举出锂、钠、钾、铷、铯等碱金属,镁、钙、锌等多价金属,优选钠、锌。
作为离聚物树脂的制造方法没有特别限定,可以通过以往公知的制造方法制造。例如,作为离聚物树脂使用乙烯·不饱和羧酸共聚物的离聚物时,例如,在高温、高压下使乙烯和不饱和羧酸进行自由基共聚,制造乙烯·不饱和羧酸共聚物。然后,通过使该乙烯·不饱和羧酸共聚物与含有上述离子源的金属化合物反应,能够制造乙烯·不饱和羧酸共聚物的离聚物。
(聚氨酯树脂)
作为聚氨酯树脂,可以列举出使异氰酸酯化合物与二醇化合物反应而得到的聚氨酯、异氰酸酯化合物与二醇化合物、进而与多胺等链长延长剂反应而得到的聚氨酯等。另外,聚氨酯树脂也可以含有硫原子。在这种情况下,上述二醇的一部分或全部可以选自多元硫醇和含硫多元醇。聚氨酯树脂可以使与有机玻璃的粘接性良好。因此,优选在玻璃板为有机玻璃的情况下使用。
(热塑性弹性体)
作为热塑性弹性体,可以列举出苯乙烯系热塑性弹性体、脂肪族聚烯烃。作为苯乙烯系热塑性弹性体,没有特别限定,可以使用公知的热塑性弹性体。苯乙烯系热塑性弹性体一般具有成为硬链段的苯乙烯单体聚合物嵌段、成为软链段的共轭二烯化合物聚合物嵌段或其氢化嵌段。作为苯乙烯系热塑性弹性体具体例,可以列举出苯乙烯-异戊二烯二嵌段共聚物、苯乙烯-丁二烯二嵌段共聚物、苯乙烯-异戊二烯-苯乙烯三嵌段共聚物、苯乙烯-丁二烯/异戊二烯-苯乙烯三嵌段共聚物、苯乙烯-丁二烯-苯乙烯三嵌段共聚物和其氢化物。
上述脂肪族聚烯烃可以是饱和脂肪族聚烯烃,也可以是不饱和脂肪族聚烯烃。上述脂肪族聚烯烃可以是以链状烯烃为单体的聚烯烃,也可以是以环状烯烃为单体的聚烯烃。从有效地提高树脂层的保存稳定性等的观点出发,上述脂肪族聚烯烃优选为饱和脂肪族聚烯烃。
作为上述脂肪族聚烯烃材料,可以列举出乙烯、丙烯、1-丁烯、反式-2-丁烯、顺式-2-丁烯、1-戊烯、反式-2-戊烯、顺式-2-戊烯、1-己烯、反式-2-己烯、顺式-2-己烯、反式-3-己烯、顺式-3-己烯、1-庚烯、反式-2-庚烯、顺式-2-庚烯、反式-3-庚烯、顺式-3-庚烯、1-辛烯、反式-2-辛烯、顺式-2-辛烯、反式-3-辛烯、顺式-3-辛烯、反式-4-辛烯、顺式-4-辛烯、1-壬烯、反式-2-壬烯、顺式-2-壬烯、反式-3-壬烯、顺式-3-壬烯、反式-4-壬烯、顺式-4-壬烯、1-癸烯、反式-2-癸烯、顺式-2-癸烯、反式-3-癸烯、顺式-3-癸烯、顺式-3-癸烯、反式-4-癸烯、顺式-4-癸烯、反式-5-癸烯、顺式-5-癸烯、4-甲基-1-戊烯和乙烯基环己烷等。
〔粘接力调节剂〕
如上所述,第二树脂层的镁元素和钾元素的合计金属浓度为一定量以上,但为了使合计金属浓度为一定量以上,优选含有粘接力调节剂。
作为粘接力调节剂,优选为选自钾盐和镁盐中的至少一种金属盐,其中优选镁盐。上述金属盐更优选为碳原子数为2~16的有机酸的钾盐或碳原子数为2~16的有机酸的镁盐。金属盐更优选为碳原子数为2~16的羧酸的镁盐或碳原子数为2~16的羧酸的钾盐。
作为金属盐,没有特别限定,例如可以列举出乙酸镁、乙酸钾、丙酸镁、丙酸钾、2-乙基丁酸镁、2-乙基丁酸钾、2-乙基丁酸镁、2-乙基丁酸钾、2-乙基丁酸钾、2-乙基己酸镁和2-乙基己酸钾等。作为粘接力调节剂,也可以使用它们的水合物。粘接力调节剂可以单独使用1种,也可以并用2种以上。
第二树脂层中粘接力调节剂的配合量可以调整为镁元素和钾元素的合计金属浓度为25ppm以上,相对于热塑性树脂100质量份,例如为0.01质量份以上0.15质量份以下,优选0.012质量份以上0.08质量份以下。
第一树脂层可以含有粘接力调节剂,但优选不含有粘接力调节剂。在含有粘接力调节剂的情况下,第一树脂层中的粘接力调节剂的配合量可以是微量,相对于100质量份热塑性树脂,例如可以小于0.005质量份,优选小于0.002质量份左右。
[发光材料]
第一树脂层和第二树脂层可以至少任一种含有发光材料,但优选第一树脂层含有发光材料。中间膜可以是通过第一树脂层和第二树脂层中的至少任一层含有发光材料而成为照射激发光而发光的发光中间膜。
作为发光材料,只要是通过照射激发光而发光的材料即可,例如可以使用镧系络合物、具有对苯二甲酸酯结构的发光材料、具有萘二甲酰亚胺骨架的发光材料、具有香豆素骨架的发光材料、具有喹啉骨架的发光材料等。发光材料可以单独使用1种,也可以并用2种以上。通过组合发光波长不同的多个发光材料,不仅可以显示单色的图像,还可以显示组合了各种颜色的图像。
在上述发光材料中,优选具有对苯二甲酸酯结构的发光材料,更优选第一树脂层含有具有对苯二甲酸酯结构的发光材料。在树脂层中,具有对苯二甲酸酯结构的发光材料与一定量以上的镁元素、钾元素等金属元素、特别是镁元素并存时,有时会使树脂层变黄或使雾度值上升。但是,如上所述,第一树脂层的镁元素含量少,优选镁元素和钾元素的合计量也少。因此,即使在第一树脂层中含有具有对苯二甲酸酯结构的发光材料,也能够防止黄变或雾度值的上升。
另外,由于在第一树脂层和第二树脂层之间配置有塑料层,所以能够防止发光材料从第一树脂层向第二树脂层的转移。因此,即使第一树脂层含有具有对苯二甲酸酯结构的发光材料,也能够防止该发光材料向第二树脂层转移,因此也能够防止第二树脂层中的黄变或雾度值的上升。进而,还可以防止镁元素和钾元素从第二树脂层向第一树脂层的转移,由此,还可以防止第一树脂层中的黄变和雾度值上升的发生。
各树脂层中的发光材料的含量可以根据发光材料的种类、所希望的发光强度等适当调整,没有特别限定,例如相对于100质量份热塑性树脂,为0.01质量份以上2.0质量份以下,优选为0.1质量份以上1.0质量份以下。
如上所述,在本发明中,优选第一树脂层含有具有对苯二甲酸酯结构的发光材料。在第一树脂层中,相对于100质量份热塑性树脂,具有对苯二甲酸酯结构的发光材料的含量优选为2.0质量份以下,更优选为1.5质量份以下,进一步优选为1.2质量份以下,更优选为1质量份以下。通过使含量为这些上限值以下,中间膜的透明性提高,可见光透过率变高,另外,还可以防止因发光材料的影响而雾度值变高。
另外,相对于第一树脂层中热塑性树脂100质量份,第一树脂层中的具有对苯二甲酸酯结构的发光材料的含量优选为0.01质量份以上,更优选为0.1质量份以上,进一步优选为0.15质量份以上、更优选0.2质量份以上。通过使发光材料的含量为这些下限值以上,通过激发光的照射能够以良好的可视性显示所希望的图像等。
另外,从防止基于发光材料的黄变和雾度值的上升的观点出发,第二树脂层优选实质上不含有具有对苯二甲酸酯结构的发光材料。另外,实质上不含有具有对苯二甲酸酯结构的发光材料是指,在不因含有发光材料而发生黄变和雾度值的上升的程度上,也可以有无意中不可避免地混入的该发光材料含有在第二树脂层中。例如,相对于第二树脂层中的热塑性树脂100质量份,只要不到0.01质量份左右即可,优选为0质量份。
上述具有对苯二甲酸酯结构的发光材料只要是通过照射激发光而发光的材料即可。具有对苯二甲酸酯结构的发光材料例如可以列举出具有下述通式(1)表示的结构的化合物或具有下述通式(2)表示的结构的化合物。
它们可以单独使用,也可以使用2种以上。
在上述通式(1)中,R1表示有机基团,x为1、2、3或4。
从提高中间膜的可见光透射率的观点出发,x优选为1或2,x更优选为2。另外,更优选苯环的2位或5位具有羟基,进一步优选苯环的2位和5位具有羟基。
上述R1的有机基团优选为烃基,更优选为碳原子数为1~10的烃基,进一步优选为碳原子数为1~5的烃基,特别优选为碳原子数为1~3的烃基。当所述烃基的碳原子数为10以下时,可以容易地将具有所述对苯二甲酸酯结构的发光材料分散在树脂层中。上述烃基优选为烷基。
作为具有上述通式(1)表示的结构的化合物,例如可以列举出2,5-二羟基对苯二甲酸二乙酯、2,5-二羟基对苯二甲酸二甲酯等。其中,具有上述通式(1)表示的结构的化合物优选为2,5-二羟基对苯二甲酸二乙酯。
在上述通式(2)中,R2表示有机基团,R3和R4表示氢原子或有机基团,y为1、2、3或4。
上述R2的有机基团优选为烃基,更优选为碳原子数为1~10的烃基,进一步优选为碳原子数为1~5的烃基,特别优选为碳原子数为1~3的烃基。当上述烃基的碳原子数为上述上限以下时,可以容易地使具有上述对苯二甲酸酯结构的发光材料分散在树脂层中。上述烃基优选为烷基。
在上述通式(2)中,R3和R4的有机基团例如为碳原子数为1~10的烃基,作为有机基团,优选为碳原子数为1~5的烃基,更优选为碳原子数为1~3的烃基,作为烃基优选为烷基。另外,R3和R4都优选为氢原子。y优选为1或2,更优选为2。另外,更优选苯环的2位或5位具有NR3R4,进一步优选苯环的2位和5位具有NR3R4。
作为具有上述通式(2)表示的结构的化合物,优选2,5-二氨基对苯二甲酸二乙酯。
[隔热粒子]
第一树脂层和第二树脂层中,至少任一种可以含有隔热粒子,其中,优选第一树脂层含有隔热粒子。通过第一树脂层和第二树脂层中的至少任一层含有隔热粒子,可以提高中间膜的隔热性。
第一树脂层和第二树脂层可以分别含有发光材料,但第一树脂层和第二树脂层除了发光材料以外,还可以分别含有隔热粒子。当然,第一树脂层和第二树脂层各自可以仅含有发光材料或隔热粒子中的一方,也可以两方都不含有。
隔热粒子是能够吸收波长为780nm以上的红外线即热线的材料。隔热粒子由无机材料构成,作为其具体例,可以列举出金属氧化物粒子、六硼化镧(LaB6)粒子等金属氧化物粒子以外的粒子。作为金属氧化物粒子,可以列举出铝掺杂氧化锡粒子、铟掺杂氧化锡粒子、锑掺杂氧化锡粒子(ATO粒子)等氧化锡粒子、镓掺杂氧化锌粒子(GZO粒子)、铟掺杂氧化锌粒子(IZO粒子)、铝掺杂氧化锌粒子(AZO粒子)、锡掺杂氧化锌粒子和硅掺杂氧化锌粒子等氧化锌粒子、铌掺杂氧化钛粒子等氧化钛粒子、锡掺杂氧化铟粒子(ITO粒子)等氧化铟粒子、钠掺杂氧化钨粒子、铯掺杂氧化钨粒子(CWO粒子)、铊掺杂氧化钨粒子、铷掺杂氧化钨粒子等氧化钨粒子。另外,也可以使用这些以外的隔热粒子。隔热粒子可以单独使用一种,也可以并用两种以上。
其中,由于热线的遮蔽功能高,所以优选金属氧化物粒子,更优选使用选自ATO粒子、GZO粒子、ITO粒子和CWO粒子中的至少一种,进一步优选ITO粒子。
隔热粒子的平均粒径的优选下限为10nm,更优选下限为20nm,优选上限为100nm,更优选上限为80nm,进一步优选上限为50nm。如果平均粒径为上述优选的下限以上,则能够充分提高热线的遮蔽性。另外,如果平均粒径在上述优选的上限以下,则难以利用隔热粒子遮蔽可见光线,容易提高中间膜的可见光透过率。
另外,“平均粒径”表示体积平均粒径。平均粒径可以使用粒度分布测定装置(日机装公司制造的“UPA-EX150”)等进行测定。
另外,第一树脂层含有隔热粒子时,第一树脂层中的隔热粒子的含量优选为0.005质量%以上2.0质量%以下,更优选为0.01质量%以上1.5质量%以下,进一步优选为0.04质量%以上1.0质量%以下。通过使隔热粒子的含量在这些范围内,能够在不降低可见光透射率等的情况下提高中间膜的隔热性。
在第二树脂层含有隔热粒子的情况下,第二树脂层中的隔热粒子的含量与上述第一树脂层中所示的同样,但第二树脂层也可以实质上不含有隔热粒子。另外,实质上不含有隔热粒子是指在第二树脂层中可以以不经意地不可避免地混入的程度含有隔热粒子,例如在第二树脂层中,隔热粒子只要不到0.005质量%左右即可,优选为0质量%。
[磷酸酯化合物]
第一树脂层和第二树脂层中的至少一种可以含有磷酸酯化合物,其中,优选第一树脂层含有磷酸酯化合物。
在树脂层中,镁元素和钾元素即使配合一定量以上,若与磷酸酯化合物并存,则即使在低湿环境下,粘接力也变高,有时难以得到提高耐击穿性能的效果,但第一树脂层如上所述,镁元素的含量、优选镁元素和钾元素的总含量少。因此,即使在第一树脂层中含有磷酸酯化合物,也能够防止由于磷酸酯化合物的影响导致玻璃板的粘接力上升,不会降低耐击穿性能。
磷酸酯化合物作为分散剂使用,具体而言,用于分散上述隔热粒子、后述的颜料、染料等着色剂。使用磷酸酯化合物时,隔热粒子、着色剂等可以分散在增塑剂中,然后配合在热塑性树脂中。例如,可以在增塑剂中加入隔热粒子、着色剂等,再加入分散剂等,分散在增塑剂中,然后与热塑性树脂混合。
作为磷酸酯化合物,可以列举例如:磷酸三辛酯、磷酸三异丙酯、磷酸三丁氧基乙酯、磷酸三甲苯基酯、磷酸异癸基苯基酯、聚氧化乙烯壬基苯基醚磷酸酯、聚氧乙烯辛基苯基醚磷酸酯、以及聚氧乙烯烷基苯基醚磷酸酯等聚氧亚烷基烷基苯基醚磷酸酯、聚氧乙烯烷基醚磷酸酯、烷基醚磷酸酯等。它们可以单独使用1种,也可以并用2种以上。
当第一树脂层含有磷酸酯化合物时,第一树脂层中的磷酸酯化合物的含量例如为0.0001质量%以上且1质量%以下,优选为0.0005质量%以上且0.5质量%以下,更优选为0.001质量%以上且0.1质量%以下。通过将含量设为上述范围内,不需要过度使用磷酸酯化合物,容易使隔热粒子等分散在第一树脂层中。另外,第一树脂层在含有磷酸酯化合物时,更优选含有隔热粒子。
另外,如上所述,第二树脂层可以含有磷酸酯化合物,但优选实质上不含有。第二树脂层通过实质上不含有磷酸酯化合物,防止在低湿环境下对玻璃板的粘接力变高,在低湿和高湿环境下的任一种环境中都容易提高耐击穿性能。
另外,实质上不含有磷酸酯化合物是指,可以以在低湿和高湿环境下耐击穿性能不降低的程度、无意中不可避免地在第二树脂层中含有磷酸酯化合物,因此,例如在第二树脂层中如果磷酸酯化合物小于0.01质量%左右、优选小于0.001质量%、更优选小于0.0005质量%、进一步优选小于0.0001质量%,则可以含有。但是,第二树脂层中的磷酸酯化合物的含量更优选为0质量%。
〔增塑剂〕
本发明的第一树脂层可以含有增塑剂。另外,第二树脂层也可以含有增塑剂。第一树脂层和第二树脂层通过含有增塑剂而变得柔软,其结果,能够提高中间膜的柔软性,提高夹层玻璃的耐击穿性和耐冲击性等。进而,也可以发挥对玻璃的高粘接性。
当使用聚乙烯醇缩醛树脂作为热塑性树脂时,含有增塑剂特别有效。因此,第一树脂层和第二树脂层分别地、在含有聚乙烯醇缩醛树脂时优选进一步含有增塑剂。
作为增塑剂,例如可以列举出一元有机酸酯和多元有机酸酯等有机酯增塑剂等。
作为一元有机酸酯,可以列举出二醇和一元有机酸的酯。作为二醇,可以列举出各亚烷基单元为碳原子数2~4、优选碳原子数2或3、亚烷基单元的重复数为2~10、优选为2~4的聚亚烷基二醇。另外,作为二醇,也可以是碳原子数为2~4、优选碳原子数为2或3、重复单元为1的单亚烷基二醇。
作为二醇,具体而言,可以列举出乙二醇、二乙二醇、三乙二醇、四乙二醇、丙二醇、二丙二醇、三丙二醇、四丙二醇、丁二醇等。
作为一元有机酸,可以列举出碳原子数为3~10的有机酸,具体而言,可以列举出丁酸、异丁酸、己酸、2-乙基丁酸、2-乙基戊酸、庚酸、正辛酸、2-乙基己酸、正壬酸和癸酸等。
作为具体的一元有机酸酯,可以列举出:三乙二醇二-2-乙基丁酸酯、三乙二醇二-2-乙基己酸酯、三乙二醇二己酸酯、三乙二醇二正辛酸酯、三乙二醇二正庚酸酯、四乙二醇二正庚酸酯、四乙二醇二-2-乙基己酸酯、二乙二醇二-2-乙基丁酸酯、二乙二醇二-2-乙基己酸酯、二丙二醇二-2-乙基丁酸酯、三乙二醇二-2-乙基戊酸酯、四乙二醇二-2-乙基丁酸酯、二乙二醇二辛酸酯、三乙二醇二正庚酸酯、四乙二醇二正庚酸酯、三乙二醇二-2-乙基丁酸酯、乙二醇二-2-乙基丁酸酯、1,2-丙二醇二-2-乙基丁酸酯、1,3-丙二醇二-2-乙基丁酸酯、1,4-丁二醇二-2-乙基丁酸酯、1,2-丁二醇二-2-乙基丁酸酯等。
另外,作为多元性有机酸酯,例如可以列举出己二酸、癸二酸、壬二酸等碳原子数为4~12的二元性有机酸与碳原子数为4~10的醇的酯化合物。碳原子数为4~10的醇可以是直链,也可以具有支链结构,也可以具有环状结构。
具体而言,可以列举出癸二酸二丁酯、壬二酸二辛酯、己二酸二己酯、己二酸二辛酯、己二酸己基环己酯、己二酸二异壬酯、己二酸庚基壬基酯、二丁基卡必醇己二酸酯、混合型己二酸酯等。另外,也可以是油改性癸二酸醇酸等。作为混合型己二酸酯,可以列举出由选自碳原子数4~9的烷基醇和碳原子数4~9的环状醇中的2种以上的醇制作的己二酸酯。
增塑剂可以单独使用1种,也可以并用2种以上。
作为增塑剂,在上述之中,优选二醇与一元有机酸的酯,特别优选使用三乙二醇-2-乙基己酸酯(3GO)。
在第一树脂层和第二树脂层中,增塑剂的含量没有特别限定,相对于热塑性树脂100质量份,优选为20质量份以上80质量份以下。当增塑剂的含量为20质量份以上时,夹层玻璃变得适度柔软,耐击穿性等变得良好。另外,如果增塑剂的含量为80质量份以下,则可以防止增塑剂从各树脂层分离。增塑剂的含量更优选为30质量份以上,进一步优选为35质量份以上,另外,更优选为70质量份以下,进一步优选为63质量份以下。
另外,在第一树脂层和第二树脂层中均为:以热塑性树脂或热塑性树脂和增塑剂为主要成分,热塑性树脂和增塑剂的合计量以各树脂层总量为基准,通常为70质量%以上,优选为80质量%以上,进一步优选为90质量%以上且小于100质量%。
[其他的添加剂]
根据需要,第一树脂层和第二树脂层还可以分别含有染料、颜料等着色剂、紫外线吸收剂、抗氧化剂、光稳定剂、荧光增白剂、结晶成核剂等添加剂。
[塑料层]
如上所述,本发明的中间膜在第一树脂层和第二树脂层之间含有塑料层。中间膜通过含有塑料层,机械强度提高,耐击穿性能提高。
另外,塑料层还起到防止一个树脂层中含有的添加剂转移到另一个树脂层的阻挡层的作用。例如,在第一树脂层中含有发光材料、隔热粒子和磷酸酯化合物中的至少一种的情况下,可以防止它们转移到第二树脂层。进而,还可以防止第二树脂层中含有的镁元素和钾元素转移到第一树脂层,能够可靠且长时间地使耐击穿性优异。
塑料层可以由各种树脂膜构成,可以列举出聚酯树脂膜、丙烯酸树脂膜等。
丙烯酸树脂膜是树脂由丙烯酸树脂构成树脂膜,作为丙烯酸树脂,优选含有来自含羟基(甲基)丙烯酸酯的构成单元的丙烯酸系聚合物,具体而言,优选聚甲基丙烯酸羟基丙基酯(HPMA树脂)、聚甲基丙烯酸羟基乙基酯(HEMA树脂)等是优选的。另外,聚酯树脂膜优选树脂由聚酯树脂构成的树脂膜,使用的聚酯树脂为聚对苯二甲酸乙二醇酯(PET)的PET膜。
作为树脂膜,在上述中,优选PET膜。另外,PET薄膜中使用的聚对苯二甲酸乙二醇酯也可以是改性PET,例如优选环己烷二亚甲基改性PET(PETG)等。
构成塑料层的树脂膜可以仅由上述树脂构成,但只要不阻碍其功能,也可以配合添加剂。作为添加剂,可以列举出紫外线吸收剂、抗氧化剂、光稳定剂、荧光增白剂、结晶成核剂等。
另外,塑料层优选实质上不含有增塑剂。塑料层通过不含有增塑剂,容易发挥作为阻挡层的功能,能够更有效地防止发光材料、磷酸酯化合物、隔热粒子等添加剂、镁元素和钾元素等金属元素从一个树脂层转移到另一个树脂层。特别是,如果第一树脂层和第二树脂层两者都含有增塑剂,则容易产生添加剂、金属元素的转移,因此优选第一树脂层和第二树脂层两者都含有增塑剂,另一方面,塑料层实质上不含有增塑剂。
另外,所谓实质上不含有增塑剂是指,可以以不损害塑料层的功能的量含有增塑剂,例如也可以无意中含有不可避免地混入的增塑剂。相对于100质量份热塑性树脂,塑料层中的增塑剂的含量可以小于2质量份,优选小于1质量份,进一步优选小于0.5质量份,最优选为0质量份。
另外,塑料层可以由树脂膜单层构成,也可以由多个树脂膜构成,但在任何情况下,塑料层都优选含有聚酯树脂膜和丙烯酸树脂膜中至少一种,更优选含有PET膜塑料层,更优选仅由PET薄膜构成。
另外,在塑料层中可以适当层叠金属箔或金属酸化合物层等,在中间膜中,在塑料层上层叠有金属箔或金属酸化合物层等的层叠体也可以配置在第一树脂层和第二树脂层之间。作为构成金属箔的金属,可以列举出铝、铜、银、金、钯以及含有它们的合金等。
另外,在本发明的中间膜中,第一树脂层、塑料层和第二树脂层只要相互重合就没有特别限定。例如,中间膜也可以是第一树脂层、塑料层和第二树脂层层叠而成为一体的层叠膜。另外,中间膜也可以以第一树脂层、塑料层和第二树脂层能够相互分离的程度重合。当然,中间膜如后所述,也可以配置在两片夹层玻璃之间。
[夹层玻璃]
在本发明中,如图2所示,夹层玻璃20具有第一玻璃板21、第二玻璃板22、配置在第一玻璃板21和第二玻璃板22之间的中间膜10。夹层玻璃通过中间膜10粘接第一玻璃板21和第二玻璃板22。此时,第一树脂层11以与第一玻璃板21接触的方式配置,第二树脂层12以与第二玻璃板22接触的方式配置较好。
作为夹层玻璃中使用的第一和第二玻璃板,可以是无机玻璃、有机玻璃中的任一种。作为无机玻璃,没有特别限定,可以列举出透明玻璃、浮法玻璃、抛光玻璃、压花玻璃、嵌丝玻璃、嵌线玻璃、绿色玻璃等。
另外,作为有机玻璃,一般使用被称为树脂玻璃的有机玻璃,没有特别限定,可以列举出由聚碳酸酯、丙烯酸树脂、丙烯酸共聚物树脂、聚酯等树脂构成的有机玻璃。
两块玻璃板可以由彼此相同的材质构成,也可以由其他材质构成。例如,一方可以是无机玻璃,另一方可以是有机玻璃,但优选两块玻璃板两者都为无机玻璃,或者都为有机玻璃,在本发明中,更优选两块玻璃板都为无机玻璃。
另外,各玻璃板的厚度没有特别限定,例如为0.1~15mm左右,优选为0.5~5mm。各玻璃板的厚度可以彼此相同,也可以不同,但优选相同。
[夹层玻璃的用途]
本发明的夹层玻璃例如作为窗玻璃使用,更具体地说,可以用于汽车、电车、船舶、飞机等各种交通工具、大楼、公寓、别墅、会馆、体育馆等各种建筑物等的窗玻璃。
夹层玻璃优选用于交通工具窗玻璃,特别是汽车用窗玻璃。另外,在夹层玻璃含有发光材料的情况下,例如通过从室内侧(汽车中为车内侧)向中间膜照射激发光,能够通过中间膜的发光显示各种图像。
汽车用窗玻璃可以是前玻璃、后玻璃、侧玻璃、车顶玻璃中的任一种,但优选用于前玻璃。将具有发光材料的夹层玻璃用于前玻璃,可适用于HUD应用。
[中间膜和夹层玻璃的制造方法]
第一树脂层和第二树脂层例如可以由热塑性树脂、以及根据需要添加的发光材料、增塑剂、隔热粒子、磷酸酯化合物、粘接力调节剂、和其他添加剂等构成各树脂层的材料构成的树脂组合物形成。第一树脂层和第二树脂层可以将各自的构成材料混炼而得到的树脂组合物进行挤出成形、冲压成形等而形成。塑料层也可以通过将构成塑料层的树脂挤出成形、冲压成形等来形成。
本发明的中间膜可以通过准备第一树脂层、塑料层和第二树脂层,将它们重合,进行热压接等来制造。另外,也可以通过准备2个以上的挤出机,在多个挤出机的前端安装多层用进料块并共挤出的方法来制造。
夹层玻璃可以通过在两块玻璃板之间层叠构成中间膜的各层并进行热压接等来制造。另外,可以通过将预先制作的中间膜配置在2片玻璃板之间进行热压接等来制造。
进而,中间膜也可以预先层叠在一方的玻璃板上,将层叠有该中间膜的玻璃板与另一方的玻璃板重叠,然后进行热压接等来制造。
[夹层玻璃用层叠体]
另外,在本发明中,也可以预先准备具有第一树脂层、塑料层和第二树脂层这3层中的2层的夹层玻璃用层叠体,将该夹层玻璃用层叠体与剩余的1层重叠,形成中间膜。以下,对在这样的用途中使用的夹层玻璃用层叠体进行详细说明。
作为夹层玻璃用层叠体,可以列举出具有塑料层和层叠在塑料层的一个面上的第二树脂层的夹层玻璃用层叠体(以下,也简称为层叠体(X))。层叠体(X)用于与第一树脂层重合而形成中间膜。
这里,层叠体(X)中的第二树脂层含有热塑性树脂,镁元素和钾元素的合计金属浓度为25ppm以上,其详细情况如上所述。另外,用于与层叠体(X)重合的第一树脂层含有热塑性树脂,厚度为900μm以下,且镁元素的浓度小于25ppm,优选镁元素和钾元素的合计金属浓度小于25ppm,其详细情况如上所述。
层压体(X)用于以使得塑料层配置在第一树脂层和第二树脂层之间的方式在第一树脂层上重叠形成中间膜。在本发明中,这样形成的中间膜通过隔着该中间膜贴合2片2.5mm厚的玻璃板,在依照JIS R 3212:2015进行的各落球试验中,在中间膜的含水率为0.4%和2.0%的任一种情况下满足落球高度(MBH)为5m以上的条件。
另外,作为夹层玻璃用层叠体,可以列举出具有塑料层和层叠在塑料层的一个面上的第一树脂层的夹层玻璃用层叠体(以下,也简称为层叠体(Y))。层叠体(Y)用于与第二树脂层重合而形成中间膜。
这里,层叠体(Y)中第一树脂层含有热塑性树脂,厚度为900μm以下,且镁元素的浓度小于25ppm,优选镁元素和钾元素的合计金属浓度小于25ppm,其详细情况如上所述。另外,用于与层叠体(Y)重合的第二树脂层含有热塑性树脂,镁元素和钾元素的合计金属浓度为25ppm以上,其详细情况如上所述。
叠层体(Y)用于以塑料层配置在第一树脂层和第二树脂层之间的方式与第二树脂层重合而形成中间膜。在本发明中,这样形成的中间膜通过隔着该中间膜贴合2片2.5mm厚的玻璃板,在依照JIS R 3212:2015进行的各落球试验中,在中间膜的含水率为0.4%和2.0%的任一种情况下满足落球高度(MBH)为5m以上的条件。
层叠体(X)可以重叠在第一树脂层上,并且配置在第一和第二玻璃板之间,通过热压接等来制造夹层玻璃。同样,层叠体(Y)可以重叠在第二树脂层上,并且配置在第一和第二玻璃板之间,通过热压接等来制造夹层玻璃。
层叠体(X)、(Y)也可以层叠在构成夹层玻璃的一方的玻璃板上。当层叠体(X)、(Y)层叠在玻璃板上时,通过将层叠有该层叠体的玻璃板与第一树脂层或第二树脂层和另一玻璃板重叠,然后进行热压接等,可以制造夹层玻璃。通过这样的结构,夹层玻璃的制造变得容易。此时,用于与层叠体(X)重合的第一树脂层或用于与层叠体(Y)重合的第二树脂层也可以层叠在另一玻璃板上。
当然,层叠体(X)或层叠体(Y)也可以不预先层叠在玻璃板上。此时,可以将用于与层叠体(X)重合的第一树脂层或用于与层叠体(Y)重合的第二树脂层层叠在另一玻璃板上,也可以不层叠。
实施例
通过实施例更详细地说明本发明,但本发明不受这些例子的任何限定。
[金属浓度]
分别采集0.3g第一树脂层和第二树脂层,加入6mL硝酸使其溶解,溶解后用超纯水定容为50mL,通过ICP发射光谱分析测定各树脂层中所含的镁元素和钾元素各自的浓度(质量ppm)。这些合计浓度为镁元素和钾元素的合计浓度。另外,ICP发射光谱分析的测定条件如下。
<测定条件>
测量装置:株式会社岛津制作所制“ICPE-9000”
高频输出:1.2kW等离子气体流量:10L/分
辅助气体流量:0.6L/分载气流量:0.7L/分
[落球试验]
将各实施例、比较例中得到的中间膜在23±2℃的恒温槽中保持1小时以上,使含水率为0.4质量%。
之后,准备2片透明玻璃板(纵300mm×横300mm×厚2.5mm、以JISR 3211(1998)为准),在2片透明玻璃板之间配置中间膜,形成层叠体。将得到的层叠体转移到橡胶袋内,将橡胶袋与吸引减压体系连接,在外部空气加热温度下加热,同时在-600mmHg(绝对压力160mmHg)的减压下保持10分钟,加热成层叠体的温度(预压接温度)分别为60℃后,返回大气压进行临时压接。将临时压接的层叠体在高压釜内,在温度140℃、压力1.3MPa的条件下保持10分钟后,将温度降低至50℃并返回大气压,由此结束正式压接,得到夹层玻璃。
在根据JIS R 3212:2015进行所得夹层玻璃的落球试验中,将落球高度(MBH)设为5m,确认夹层玻璃是否被击穿。将夹层玻璃未击穿的情况评价为“A”,将击穿的情况评价为“B”。
另外,将各实施例、比较例中得到的中间膜以含水率为2.0质量%的方式,在50℃、相对湿度95%的恒温槽中保持40分钟。之后,立即与上述同样地制作夹层玻璃,对制作的夹层玻璃进行落球试验并进行评价。
另外,用以下的方法确认了含水率。
(含水率)
将称量瓶用恒温干燥机干燥3小时。在干燥器内放置30分钟后,用天平测量称量瓶的重量X。然后,将中间膜放入称重瓶中,测量装有中间膜的称重瓶的重量A。然后,将装有中间膜的称重瓶整个在50℃、减压度700mm/ng的真空干燥机中减压干燥2小时,在干燥器内放冷20分钟。放冷后,用天平测量装有中间膜的称量瓶的重量B。根据重量A和重量B,代入式:含水率=(A-B)/(A-X)×100,求出含水率。
[YI值]
使用分光光度计(日立ハイテク公司生产的“U-4100”),根据JIS Z8722测定得到的中间膜的YI值(黄色度、黄色指数)。将YI值为10以下评价为“A”,将YI值超过10的情况评价为“B”。
在实施例、比较例中使用了以下的成分、原材料。
(树脂)
PVB:聚乙烯醇缩丁醛树脂、缩醛化度68.5摩尔%、羟基量30.5摩尔%、酰化度1.0摩尔%、平均聚合度1700
(增塑剂)
3GO:三乙二醇二-2-乙基己酸酯
(发光材料)
对苯二甲酸酯:2,5-二羟基对苯二甲酸二乙基酯
(隔热粒子)
ITO:锡掺杂氧化铟粒子(ITO粒子),平均粒径30nm
(磷酸酯)
第一工业制药公司制造
(粘接力调节剂)
粘接力调节剂(1):乙酸镁
粘接力调节剂(2):乙酸钾
(塑料层)
PET:PET薄膜、商品名“ルミラー100-U34”、东丽株式会社制
[实施例1]
将100质量份聚乙烯醇缩丁醛树脂和40质量份增塑剂混合,利用双轴各向异性挤出机将所得到树脂组合物挤出成形,制造厚度380μm的第一树脂层。另外,将100质量份聚乙烯醇缩丁醛树脂、40质量份增塑剂和0.032质量份粘接剂调节剂(1)混合,利用双轴各向异性挤出机将得到的树脂组合物挤出成形,制造第二树脂层中的合计金属浓度为50ppm的厚度380μm的第二树脂层。进而,准备厚度50μm的作为塑料层的PET薄膜。将第一树脂层、PET薄膜和第二树脂层重合而制作中间膜。
[实施例2]
通过将第二树脂层中粘接力调节剂(1)的配合量变更为0.019质量份,调整为第二树脂层中的合计金属浓度为30ppm,且将第二树脂层的厚度调整为760μm,除此以外,与实施例1同样地实施。
[实施例3]
除了使塑料层的厚度为100μm以外,与实施例1同样地实施。
[实施例4]
除了将第二树脂层中的粘接力调节剂变更为粘接力调节剂(2),并且将其配合量变更为0.065质量份,从而将第二树脂层中的合计金属浓度调整为100ppm以外,与实施例3同样地实施。
[实施例5]
除了使塑料层的厚度为200μm以外,与实施例1同样地实施。
[实施例6]
除了使将第二树脂层的厚度设为500μm以外,与实施例1同样地实施。
[实施例7]
除了在用于构成第一树脂层的树脂组合物中进一步添加0.5质量份的发光材料以外,与实施例1同样地实施。
[实施例8]
在40质量份增塑剂中,以按照第一树脂层总量基准为0.2质量%的方式添加隔热粒子和为0.1质量%的方式添加磷酸酯化合物,然后用水平型的微珠磨机混合,得到混合液。然后,在搅拌下向混合液中添加0.1质量份乙酰丙酮,制作分散液。接着,相对于100质量份聚乙烯醇缩丁醛树脂,添加得到分散液总量,用混合辊充分熔融混炼后,使用挤出机挤出,得到厚度380μm的第一树脂层。之后,与实施例1同样地实施,得到中间膜。
[比较例1]
与实施例1的第一树脂层同样地制作树脂层,将该树脂层作为中间膜。
[比较例2]
除了变更厚度为800μm以外,与比较例1同样地实施。
[比较例3]
除了变更厚度为800μm以外,与实施例1的第二树脂层同样地制作树脂层,将该树脂层作为中间膜。
[比较例4]
制作2片与实施例1的第一树脂层相同的树脂层,将该2片树脂层重合而得到中间膜。
[比较例5]
除了省略塑料层以外,与实施例1同样地制作中间膜。
[比较例6]
制作2片与实施例1的第一树脂层相同的树脂层,依次重叠树脂层、作为塑料层的PET薄膜和树脂层,得到中间膜。
[比较例7]
制作2片与实施例1的第二树脂层相同的树脂层,将树脂层、作为塑料层的PET薄膜和树脂层重合而得到中间膜。
[比较例8]
除了在用于构成一个树脂层的树脂组合物中进一步添加0.5质量份的发光材料以外,与比较例7同样地实施。
[比较例9]
在40质量份增塑剂中,以树脂层总量为基准为0.2质量%的方式添加隔热粒子和以成为0.1质量%的方式添加磷酸酯化合物后,用水平型的微珠磨机混合,得到混合液。然后,在搅拌下向混合液中添加0.1质量份乙酰丙酮,制作分散液。接着,相对于100质量份聚乙烯醇缩丁醛树脂,添加所得到的分散液总量和0.032质量份粘接力调节剂(1),用混合辊充分熔融混炼后,使用挤出机挤出,得到厚度800μm的树脂层,将该树脂层作为中间膜。
※表1中的质量份是相对于树脂(PVB)100质量份的质量份,质量%是各树脂层中的质量%。
※表1中的“2>”表示2ppm以下。
如以上实施例所示,通过中间膜具备第一树脂层和第二树脂层和配置在其间的塑料层,第一树脂层的厚度为900μm以下、镁浓度小于25ppm,且第二树脂层的合计金属浓度为25ppm以上,由此在低湿和高湿下的任一种中落球试验的结果都良好,耐击穿性优异。另外,在实施例7、8中,中间膜含有具有对苯二甲酸酯结构的发光材料或磷酸酯化合物,但都含有在镁浓度甚至合计金属浓度都低的第一树脂层中,通过这样,不会在中间膜产生黄变或耐击穿性降低。
与此相对,在比较例1~3、9中,中间膜为单层结构,另外,在比较例4中,由于2个树脂层为相同的组成,所以不能设置镁浓度小于25ppm的第一树脂层和合计金属浓度为25ppm以上的第二树脂层。因此,在低湿和高湿环境下,不能使落球试验成为优异的结果,耐击穿性不好。
另外,在比较例9中,由于含有磷酸酯化合物,因此尽管合计金属浓度高,但不仅高湿,而且低湿下的耐击穿性也降低。这被认为是因为调整镁元素的粘接力的功能被磷酸酯化合物阻碍了。
另外,在比较例5中,设置了镁浓度小于25ppm的第一树脂层和合计金属浓度为25ppm以上的第二树脂层,但由于没有塑料层,因此无法防止镁元素、钾元素从第二树脂层向第一树脂层的转移。因此,在夹层玻璃中,在第一树脂层中也存在一定量以上的镁元素等金属元素,在低湿和高湿下两者中都不能良好地实现耐击穿性。另外,在比较例6~8中设置了塑料层,但由于不具有镁浓度小于25ppm的树脂层和合计金属浓度为25ppm以上的树脂层两者,因此在低湿和高湿下两者中都不能良好地进行耐击穿性。另外,在比较例8中,在合计金属浓度为25ppm以上的树脂层中含有发光材料,因此产生黄变,YI值变高。
符号说明
10 中间膜
11 第一树脂层
12 第二树脂层
13 塑料层
20 合玻璃
21 第一玻璃板
22 第二玻璃板
Claims (16)
1.一种夹层玻璃用中间膜,具备第一树脂层、第二树脂层和配置在所述第一树脂层和第二树脂层之间的塑料层,
所述第一树脂层含有热塑性树脂,所述第一树脂层的厚度为900μm以下且镁元素浓度小于25ppm,
所述第二树脂层含有热塑性树脂,所述第二树脂层中的镁元素和钾元素的合计浓度为25ppm以上,
在将2片2.5mm厚的玻璃板介隔所述夹层玻璃用中间膜贴合后依照JIS R 3212:2015进行的落球试验中,在所述夹层玻璃用中间膜的含水率为0.4%和2.0%的任一种情况下,都满足落球高度MBH为5m以上的要件。
2.根据权利要求1所述的夹层玻璃用中间膜,所述第一树脂层中的镁元素和钾元素的合计浓度小于25ppm。
3.根据权利要求2所述的夹层玻璃用中间膜,所述第一树脂层的厚度为800μm以下,且所述合计浓度为20ppm以下。
4.根据权利要求1~3中任一项所述的夹层玻璃用中间膜,所述第二树脂层的厚度为900μm以下。
5.根据权利要求1~4中任一项所述的夹层玻璃用中间膜,所述第二树脂层的厚度为100μm以上。
6.根据权利要求1~5中任一项所述的夹层玻璃用中间膜,所述第二树脂层的厚度为350μm以上,且所述合计浓度为30ppm以上。
7.根据权利要求1~6中任一项所述的夹层玻璃用中间膜,所述塑料层的厚度为30μm以上且200μm以下。
8.根据权利要求1~7中任一项所述的夹层玻璃用中间膜,所述第一树脂层含有具有对苯二甲酸酯结构的发光材料。
9.根据权利要求1~8中任一项所述的夹层玻璃用中间膜,所述第一树脂层含有磷酸酯化合物。
10.根据权利要求1~9中任一项所述的夹层玻璃用中间膜,所述第一树脂层含有隔热粒子。
11.根据权利要求1~10中任一项所述的夹层玻璃用中间膜,第一树脂层的所述合计浓度与所述第二树脂层的所述合计浓度之差为10ppm以上且300ppm以下。
12.根据权利要求1~11中任一项所述的夹层玻璃用中间膜,所述第一树脂层和第二树脂层中含有的热塑性树脂为聚乙烯醇缩醛树脂。
13.根据权利要求1~12中任一项所述的夹层玻璃用中间膜,所述塑料层含有聚对苯二甲酸乙二醇酯膜。
14.一种夹层玻璃,具有权利要求1~13中任一项所述的夹层玻璃用中间膜、第一玻璃板和第二玻璃板,所述夹层玻璃用中间膜配置在所述第一玻璃板和所述第二玻璃板之间。
15.一种夹层玻璃用层叠体,其用于与第一树脂层重叠而形成夹层玻璃用中间膜,
所述夹层玻璃用层叠体具备塑料层和层叠在所述塑料层一个面上的第二树脂层,
所述第一树脂层含有热塑性树脂,所述第一树脂层的厚度为900μm以下且镁元素浓度小于25ppm,
所述第二树脂层含有热塑性树脂,所述第二树脂层中的镁元素和钾元素的合计浓度为25ppm以上,
将夹层玻璃用层叠体以使所述塑料层配置在所述第一树脂层和第二树脂层之间的方式与所述第一树脂层重合而形成夹层玻璃用中间膜,介隔所述夹层玻璃用中间膜将2片2.5mm厚的玻璃板进行贴合、并依照JIS R3212:2015进行落球试验,在该试验中、在所述夹层玻璃用中间膜的含水率为0.4%和2.0%的任一种情况下都满足落球高度MBH为5m以上的要件。
16.一种夹层玻璃用层叠体,其用于与第二树脂层重叠而形成夹层玻璃用中间膜,
所述夹层玻璃用层叠体具备塑料层和层叠在所述塑料层一个面上的第一树脂层,
所述第一树脂层含有热塑性树脂,所述第一树脂层的厚度为900μm以下且镁元素浓度小于25ppm,
所述第二树脂层含有热塑性树脂,所述第二树脂层中的镁元素和钾元素的合计浓度为25ppm以上,
将夹层玻璃用层叠体以使所述塑料层配置在所述第一树脂层和第二树脂层之间的方式与所述第二树脂层重合而形成夹层玻璃用中间膜,介隔所述夹层玻璃用中间膜将2片2.5mm厚的玻璃板进行贴合、并依照JIS R3212:2015进行落球试验,在该试验中、在所述夹层玻璃用中间膜的含水率为0.4%和2.0%的任一种情况下都满足落球高度MBH为5m以上的要件。
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