CN112739754B - 聚乙烯醇缩醛树脂薄膜和其薄膜卷以及层叠体 - Google Patents
聚乙烯醇缩醛树脂薄膜和其薄膜卷以及层叠体 Download PDFInfo
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- CN112739754B CN112739754B CN201980061255.XA CN201980061255A CN112739754B CN 112739754 B CN112739754 B CN 112739754B CN 201980061255 A CN201980061255 A CN 201980061255A CN 112739754 B CN112739754 B CN 112739754B
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- polyvinyl acetal
- acetal resin
- resin film
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- roll
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- C08L29/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
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- B29C48/25—Component parts, details or accessories; Auxiliary operations
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- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal 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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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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Abstract
本发明涉及一种聚乙烯醇缩醛树脂薄膜,其由聚乙烯醇缩醛树脂材料构成,所述聚乙烯醇缩醛树脂薄膜的厚度为5~350μm,将一个面与另一个面相比,将表面较粗糙的面A的十点平均粗糙度的平均值设为Rz1(a)μm、较平滑的面B的十点平均粗糙度的平均值设为Rz2(a)μm时,满足式(1)和式(2):Rz1(a)>1.1×Rz2(a)(1)3>Rz2(a)(2),且面A的十点平均粗糙度的标准偏差除以Rz1(a)而得到的值和面B的十点平均粗糙度的标准偏差除以Rz2(a)而得到的值分别为0~0.30,前述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型(B型)粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇=1/1(质量比)溶液的粘度为100~1000mPa·s,聚乙烯醇缩醛树脂薄膜中的增塑剂的量基于聚乙烯醇缩醛树脂薄膜的总质量为0~20质量%。
Description
技术领域
本发明涉及聚乙烯醇缩醛树脂薄膜和其薄膜卷、以及包含前述聚乙烯醇缩醛树脂薄膜的层叠体。
背景技术
由聚乙烯醇缩醛树脂构成的薄膜由于透明性、柔软性、冲击吸收性、与玻璃的粘接性等优异,因此,被广泛用作各种车辆、建筑用的夹层玻璃用中间膜。这种薄膜通常从其操作性的观点出发,大多在以卷状卷绕于芯材上的状态下被保管,但存在在保管中相邻的薄膜彼此强烈密合,薄膜彼此容易经时地自粘合的问题。为了防止这种薄膜卷中的自粘合,例如提出了一种夹层玻璃用中间膜,其是由通过压花加工等对两面赋予了微细的凹凸的增塑化聚乙烯醇缩醛树脂层、片构成的夹层玻璃用中间膜(专利文献1)。
现有技术文献
专利文献
专利文献1:日本特开2000-290046号公报
发明内容
发明要解决的问题
然而,即使为如专利文献1中记载的那种在两面形成有微细凹凸的树脂薄膜,由于两面具有相同的表面形状,因此在将该树脂薄膜以卷状卷绕时彼此接触的树脂薄膜的一个面的凹凸与另一个面的凹凸变得容易嵌合。因此,结局有树脂薄膜彼此的密合性变强的倾向,产生卷出时薄膜变得容易破裂、或卷出时在薄膜的表面产生凹凸等薄膜表面变得不均匀的问题,作为保管时的自粘合的抑制效果,未必满足。特别是,容易成为高温环境下的薄膜卷的保管时、输送、搬运时自粘合变得容易产生,因此,要求在宽的温度域、尤其是高温环境下抑制自粘合的效果也优异的树脂薄膜。
因此,本发明的目的在于,提供:以卷状卷绕时不易产生经时的薄膜卷的自粘合、特别是被暴露于高温环境的情况下自粘合抑制效果也优异、从卷卷出时具有均匀的表面的、聚乙烯醇缩醛树脂薄膜。
用于解决问题的方案
本发明人等为了解决上述课题而进行了深入研究,结果完成了本发明。即,本发明提供以下的适合的方式。
[1]一种聚乙烯醇缩醛树脂薄膜,其由聚乙烯醇缩醛树脂材料构成,所述聚乙烯醇缩醛树脂薄膜的厚度为5~350μm,将一个面与另一个面相比,将表面较粗糙的面A的十点平均粗糙度的平均值设为Rz1(a)μm、较平滑的面B的十点平均粗糙度的平均值设为Rz2(a)μm时,满足式(1)和式(2):
Rz1(a)>1.1×Rz2(a) (1)
3>Rz2(a) (2),
且面A的十点平均粗糙度的标准偏差除以Rz1(a)而得到的值和面B的十点平均粗糙度的标准偏差除以Rz2(a)而得到的值分别为0~0.30,
前述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型(B型)粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇=1/1(质量比)溶液的粘度为100~1000mPa·s,聚乙烯醇缩醛树脂薄膜中的增塑剂的量基于聚乙烯醇缩醛树脂薄膜的总质量为0~20质量%。
[2]根据前述[1]所述的聚乙烯醇缩醛树脂薄膜,其进一步满足式(3):
Rz1(a)<5 (3)。
[3]根据前述[1]或[2]所述的聚乙烯醇缩醛树脂薄膜,其中,将以50℃保持了30分钟后的、面A的十点平均粗糙度的平均值设为Rz1(b)μm、面B的十点平均粗糙度的平均值设为Rz2(b)μm时,满足式(4)、式(5)和式(6):
0.7×Rz1(a)≤Rz1(b)≤1.3×Rz1(a) (4)
0.7×Rz2(a)≤Rz2(b)≤1.3×Rz2(a) (5)
Rz1(b)>Rz2(b) (6)。
[4]根据前述[1]~[3]中任一项所述的聚乙烯醇缩醛树脂薄膜,其中,前述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型(B型)粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇=1/1(质量比)溶液的粘度为300mPa·s以下。
[5]根据前述[1]~[4]中任一项所述的聚乙烯醇缩醛树脂薄膜,其中,前述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型(B型)粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇=1/1(质量比)溶液的粘度大于200mPa·s。
[6]根据前述[1]~[5]中任一项所述的聚乙烯醇缩醛树脂薄膜,其中,前述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的分子量分布为2.7以上。
[7]根据前述[1]~[6]中任一项所述的聚乙烯醇缩醛树脂薄膜,其中,前述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂为粘均聚合度不同的至少2种聚乙烯醇缩醛树脂的混合物、或粘均聚合度不同的至少2种聚乙烯醇系树脂的混合物的缩醛化物。
[8]一种聚乙烯醇缩醛树脂薄膜卷,其是以前述[1]~[7]中任一项所述的聚乙烯醇缩醛树脂薄膜的面A侧成为内侧的方式进行卷绕而成的。
[9]一种聚乙烯醇缩醛树脂薄膜卷,其是以前述[1]~[7]中任一项所述的聚乙烯醇缩醛树脂薄膜的面A侧成为外侧的方式进行卷绕而成的。
[10]一种聚乙烯醇缩醛树脂薄膜卷的保管方法,其包括如下步骤:将前述[8]或[9]所述的聚乙烯醇缩醛树脂薄膜卷在-20℃~60℃的温度下进行保管。
[11]一种带功能性层的聚乙烯醇缩醛树脂薄膜,其在前述[1]~[7]中任一项所述的聚乙烯醇缩醛树脂薄膜的至少一个面具有功能性层。
[12]根据前述[11]所述的带功能性层的聚乙烯醇缩醛树脂薄膜,其中,前述功能性层为导电层。
[13]根据前述[12]所述的带功能性层的聚乙烯醇缩醛树脂薄膜,其中,形成前述导电层的材料包含银或铜。
[14]根据前述[12]或[13]所述的带功能性层的聚乙烯醇缩醛树脂薄膜,其中,前述导电层由线宽1~30μm的多个线状导电性材料构成。
[15]一种前述[11]~[14]中任一项所述的带功能性层的聚乙烯醇缩醛树脂薄膜的制造方法,其包括如下步骤:在聚乙烯醇缩醛树脂薄膜的至少一个面涂布、印刷或层压构成功能性层的材料。
[16]一种层叠体,其包含:透明基材;和,前述[1]~[7]中任一项所述的聚乙烯醇缩醛树脂薄膜或前述[11]~[15]中任一项所述的带功能性层的聚乙烯醇缩醛树脂薄膜。
[17]一种层叠体,其是在多个透明基材之间夹持前述[1]~[7]中任一项所述的聚乙烯醇缩醛树脂薄膜或前述[11]~[15]中任一项所述的带功能性层的聚乙烯醇缩醛树脂薄膜而成的。
[18]根据前述[16]或[17]所述的层叠体,其还包含增塑化聚乙烯醇缩醛树脂层。
[19]根据前述[16]~[18]中任一项所述的层叠体,其中,前述透明基材为玻璃。
[20]一种交通工具用玻璃,其是由前述[16]~[19]中任一项所述的层叠体形成的。
发明的效果
根据本发明,可以提供一种聚乙烯醇缩醛树脂薄膜,其以卷状卷绕时不易产生经时的薄膜卷的自粘合、特别是被暴露于高温环境的情况下自粘合抑制效果也优异、从卷卷出时具有均匀的表面。
具体实施方式
以下,对本发明的实施方式详细地进行说明,但本发明不限定于这些。
<聚乙烯醇缩醛树脂薄膜>
本发明的聚乙烯醇缩醛树脂薄膜如下:将一个面与另一个面相比,将表面较粗糙的面A的十点平均粗糙度的平均值设为Rz1(a)μm、较平滑的面B的十点平均粗糙度的平均值设为Rz2(a)μm时,满足式(1)和式(2):
Rz1(a)>1.1×Rz2(a) (1)
3>Rz2(a) (2),
且面A的十点平均粗糙度的标准偏差除以Rz1(a)而得到的值和面B的十点平均粗糙度的标准偏差除以Rz2(a)而得到的值分别为0~0.30。夹层玻璃用中间膜中使用的以往的聚乙烯醇缩醛树脂薄膜通常其两表面具有相同的表面形状,但本发明的聚乙烯醇缩醛树脂薄膜的一个面与另一个面具有彼此不同的表面形状。由此,将制膜后的长尺寸的薄膜卷绕为卷状时相邻的树脂薄膜的一个面与另一个面之间产生微细的孔隙,薄膜彼此的密合性适度降低,因此,可以抑制经时的自粘合。另外,可以抑制薄膜彼此的自粘合、卷入空气所导致的卷褶皱的发生,卷出时可以得到具有均匀的表面的薄膜卷。进而,如果在将树脂薄膜卷绕为卷状时重叠的薄膜彼此的表面,部分地存在有具有相同的形状(同等程度的粗糙度)的部位,则在上述部分变得容易产生自粘合,因此,本发明的树脂薄膜中,通过使各表面的表面形状为均匀,从而即使暴露于较容易产生自粘合的高温环境的情况下,也可以得到具有高的自粘合抑制效果的聚乙烯醇缩醛树脂薄膜。
本发明的聚乙烯醇缩醛树脂薄膜中,上述“十点平均粗糙度的平均值”是指,以在各表面测定的朝向彼此成为平行、且测定的间隔彼此距离3cm以上的方式选择的任意5处的十点平均粗糙度的平均值。特别是在本发明的聚乙烯醇缩醛树脂薄膜以挤出成型等连续工序生产的情况下,测定十点平均粗糙度的朝向与挤出成型等的成型朝向(薄膜的长度方向)相同,进而在聚乙烯醇缩醛树脂薄膜的宽度超过50cm的情况下,测定是在从聚乙烯醇缩醛树脂薄膜的宽度方向的一个端部开始测定宽度的17±2%的位置、宽度的34±2%的位置、宽度的50±2%的位置、宽度的67±2%的位置和宽度的83±2%的位置这5处而得到的十点平均粗糙度的平均值。需要说明的是,树脂薄膜表面的十点平均粗糙度可以使用表面粗糙度计或激光显微镜依据JIS B0601-1994而测定。优选利用接触式的表面粗糙度计的测定。具体而言,可以通过后述的实施例中记载的方法而测定。
本发明的聚乙烯醇缩醛树脂薄膜中,Rz1(a)与Rz2(a)满足式(1):
Rz1(a)>1.1×Rz2(a) (1)。
在Rz1(a)为1.1×Rz2(a)以下的情况下,树脂薄膜的一个面与另一个面成为彼此类似的表面形状,将该树脂薄膜卷绕为卷状时相邻的薄膜表面之间难以产生适度的孔隙,变得难以抑制自粘合,可能成为将树脂薄膜卷出时产生不均匀的薄膜表面的因素之一。薄膜表面如果不均匀,则例如在树脂薄膜上设置导电层等功能性层等的情况下,在该工序中或层叠后变得容易引起功能性层的变形、破坏。本发明中,Rz1(a)优选1.3×Rz2(a)以上、更优选1.5×Rz2(a)以上、进一步优选1.8×Rz2(a)以上、特别优选2×Rz2(a)以上。从抑制自粘合的观点出发,Rz1(a)与Rz2(a)相比,只要大于1.1倍即可,因此,上述关系中的系数的上限没有特别限定,Rz1(a)与Rz2(a)之差只要成为不超过聚乙烯醇缩醛树脂薄膜的厚度的关系即可,Rz2(a)大于0μm的情况下,通常Rz1(a)为1000×Rz2(a)以下。需要说明的是,Rz1(a)和Rz2(a)的测定温度为室温。
本发明的聚乙烯醇缩醛树脂薄膜满足式(2):
3>Rz2(a) (2)。
即,本发明的聚乙烯醇缩醛树脂薄膜的表面中、较平滑的面B的十点平均粗糙度的平均值低于3μm。较平滑的面B的表面粗糙度如果为3μm以上,则树脂薄膜的两表面成为较粗糙的面,例如在树脂薄膜上设置导电层等功能性层等的情况下,在该工序中或层叠后变得容易引起功能性层的变形、破坏。Rz2(a)优选低于2.5μm、更优选低于2μm、进一步优选低于1.5μm、特别优选低于1μm。Rz2(a)如果为上述上限以下,则容易得到高的自粘合抑制效果。另外,以具有这种十点平均粗糙度的平均值的面B侧成为卷的外侧的方式将树脂薄膜卷绕,从而灰尘、尘埃等异物在保管中、输送、搬运中等变得不易附着,另一方面,以该面B成为卷的内侧的方式将树脂薄膜卷绕,从而即使灰尘、尘埃等异物附着于树脂薄膜上也可以容易去除。因此,本发明的聚乙烯醇缩醛树脂薄膜根据薄膜卷所暴露的环境等而选择卷的卷绕方向,从而在能改善作业效率的方面也是有利的。需要说明的是,例如在树脂薄膜上设置导电层等功能性层等的情况下,通过层叠于更平滑的面B侧,从而从变得容易抑制该变形、破坏的观点出发,Rz2(a)的下限没有特别限定,可以为0μm。
本发明的聚乙烯醇缩醛树脂薄膜优选满足式(3):
Rz1(a)<5 (3)。
即,本发明的聚乙烯醇缩醛树脂薄膜的表面中、较粗糙的面A的十点平均粗糙度的平均值Rz1(a)优选低于5μm。Rz1(a)的上限如果低于5μm,则面A的表面粗糙度不过度变得粗糙,与较平滑的面B接触时容易产生适度的孔隙,容易得到高的自粘合抑制效果。另外,例如在树脂薄膜上层叠玻璃等透明基材而得到层叠体的情况下,通过在作为较粗糙面的面A侧上层叠透明基材,从而还有容易有效地抑制在层叠体中起泡的优点。Rz1(a)更优选4.5μm以下、进一步优选4μm以下。另外,Rz1(a)优选0.8μm以上、更优选1μm以上、进一步优选1.5μm以上、特别优选2μm以上。较粗糙的面A的表面粗糙度如果为上述下限以上,则与较平滑的面B接触时容易产生适度的孔隙,容易得到高的自粘合抑制效果。进而,以具有这种十点平均粗糙度的平均值的面A侧成为卷的内侧的方式将树脂薄膜卷绕,从而灰尘、尘埃等异物在保管中、输送、搬运中等变得不易附着,另一方面,以该面A成为卷的外侧的方式将树脂薄膜卷绕,从而即使灰尘、尘埃等异物附着于树脂薄膜上,也可以容易去除。因此,本发明的聚乙烯醇缩醛树脂薄膜根据薄膜卷所暴露的环境等而选择卷的卷绕方向,从而在能改善作业效率的方面也是有利的。
本发明的聚乙烯醇缩醛树脂薄膜中,面A的十点平均粗糙度的标准偏差除以Rz1(a)而得到的值和面B的十点平均粗糙度的标准偏差除以Rz2(a)而得到的值分别为0~0.30。各面的十点平均粗糙度的标准偏差除以Rz1(a)或Rz2(a)而得到的值能成为表示各表面的表面粗糙度的均匀性的一个指标,它们分别处于上述范围的情况下,有树脂薄膜的各表面具有均匀的表面形状的倾向。上述情况下,在将树脂薄膜卷绕为卷状时重叠的薄膜彼此的表面,部分地存在有具有相同的形状(同等程度的粗糙度)的部位的可能性变低,可以防止在上述部分具有类似的形状的面A的凹凸与面B的凹凸嵌合而产生的自粘合。本发明的聚乙烯醇缩醛树脂薄膜如此控制各表面的表面形状的均匀性,从而即使暴露于较容易产生自粘合的高温环境的情况下,也可以得到高的自粘合抑制效果。面A的十点平均粗糙度的标准偏差除以Rz1(a)而得到的值和面B的十点平均粗糙度的标准偏差除以Rz2(a)而得到的值分别优选0.25以下、更优选0.2以下,其下限的理想值为0,但例如可以为0.01以上。
本发明中,聚乙烯醇缩醛树脂薄膜的十点平均粗糙度的平均值Rz1(a)和Rz2(a)分别例如可以通过如下方法而调整:控制通过熔融挤出法将聚乙烯醇缩醛树脂材料制膜时使用的卷的表面形状、卷的材质;控制熔融挤出成型时的加压压力;控制压花加工的条件(树脂薄膜温度和卷表面温度等);等。另外,各面的十点平均粗糙度的标准偏差除以Rz1(a)或Rz2(a)而得到的值可以如下进行调整:控制通过熔融挤出法将聚乙烯醇缩醛树脂材料制膜时使用的卷的表面形状、卷的材质;控制熔融挤出成型时的加压压力;控制压花加工的条件(树脂薄膜温度和卷表面温度等);等。
本发明的聚乙烯醇缩醛树脂薄膜优选的是,将以50℃保持了30分钟后的、面A的十点平均粗糙度的平均值设为Rz1(b)μm、面B的十点平均粗糙度的平均值设为Rz2(b)μm时,满足式(4)、式(5)和式(6):
0.7×Rz1(a)≤Rz1(b)≤1.3×Rz1(a) (4)
0.7×Rz2(a)≤Rz2(b)≤1.3×Rz2(a) (5)
Rz1(b)>Rz2(b) (6)。
通过满足上述式(4)、(5)和(6),从而即使暴露于较容易产生自粘合的高温环境的情况下,也可以得到高的自粘合抑制效果。Rz1(b)和Rz2(b)分别优选的是,与作为加热前(室温下)的表面粗糙度的平均值Rz1(a)和Rz2(a)相比,变化小者,
更优选满足:
0.8×Rz1(a)≤Rz1(b)≤1.2×Rz1(a) (7)
0.8×Rz2(a)≤Rz2(b)≤1.2×Rz2(a) (8)。
进而,本发明中聚乙烯醇缩醛树脂薄膜优选的是,在宽的温度域中,与作为室温下的表面粗糙度的平均值Rz1(a)和Rz2(a)相比,加热后的变化小者,例如优选将以60℃保持了30分钟后的、面A的十点平均粗糙度的平均值设为Rz1(c)μm、面B的十点平均粗糙度的平均值设为Rz2(c)μm时,满足式(9)、式(10)和式(11):
0.7×Rz1(a)≤Rz1(c)≤1.3×Rz1(a) (9)
0.7×Rz2(a)≤Rz2(c)≤1.3×Rz2(a) (10)
Rz1(c)>Rz2(c) (11)。
本发明中,通过如下方法,从而可以得到满足上述式(4)~(11)的聚乙烯醇缩醛树脂薄膜:控制各表面的表面粗糙度、其均匀性,调整构成聚乙烯醇缩醛树脂薄膜的聚乙烯醇缩醛树脂材料的组成,控制熔融挤出成型时的加压压力,控制压花加工的条件(树脂薄膜温度和卷表面温度等)等。
本发明的聚乙烯醇缩醛树脂薄膜的厚度为5~350μm。厚度如果低于5μm,则变得容易产生聚乙烯醇缩醛树脂薄膜的收缩、变形。另外,厚度如果大于350μm,则与本发明的聚乙烯醇缩醛树脂薄膜相邻并贴合增塑化聚乙烯醇缩醛树脂层的情况下,增塑剂从该增塑化聚乙烯醇缩醛树脂层向本发明的聚乙烯醇缩醛树脂薄膜的迁移量变多,层叠体的耐贯通性变得容易降低,例如变得不易充分得到使用该层叠体作为交通工具用玻璃时的碰撞时的头部冲击的降低效果。聚乙烯醇缩醛树脂薄膜的厚度优选10μm以上、更优选20μm以上、进一步优选30μm以上,另外,优选330μm以下、更优选295μm以下、进一步优选270μm以下、特别优选250μm以下、进一步更优选150μm以下、特别是更优选120μm以下、最优选低于100μm。聚乙烯醇缩醛树脂薄膜的厚度如果为前述下限值以上且前述上限值以下,则不易产生上述问题,且容易得到良好的制膜性。
需要说明的是,聚乙烯醇缩醛树脂薄膜的厚度例如可以使用厚度计或激光显微镜等而测定。
(聚乙烯醇缩醛树脂)
本发明的聚乙烯醇缩醛树脂薄膜由包含聚乙烯醇缩醛树脂的聚乙烯醇缩醛树脂材料构成。聚乙烯醇缩醛树脂是通过聚乙烯醇或乙烯乙烯醇共聚物等聚乙烯醇系树脂的缩醛化而制造的树脂。需要说明的是,本发明中“聚乙烯醇缩醛树脂材料”中,包括由聚乙烯醇缩醛树脂构成者、和由包含聚乙烯醇缩醛树脂的树脂组合物构成者中的任意者。
本发明中的聚乙烯醇缩醛树脂薄膜中所含的聚乙烯醇缩醛树脂可以为1种聚乙烯醇缩醛树脂,或为粘均聚合度、缩醛化度、乙酸乙烯酯单元含量、乙烯醇单元含量、乙烯单元含量、缩醛化中使用的醛的分子量和链长中的任1者以上分别不同的2种以上的聚乙烯醇缩醛树脂。在聚乙烯醇缩醛树脂薄膜包含2种以上不同的聚乙烯醇缩醛树脂的情况下,从熔融成型的容易性观点、以及容易防止在夹层玻璃上设置功能性层等时的变形和夹层玻璃使用时的玻璃的错位等的观点出发,聚乙烯醇缩醛树脂优选为粘均聚合度不同的至少2种聚乙烯醇缩醛树脂的混合物、或粘均聚合度不同的至少2种聚乙烯醇系树脂的混合物的缩醛化物。
本发明中使用的聚乙烯醇缩醛树脂的缩醛化度优选40摩尔%以上、更优选45摩尔%以上、进一步优选50摩尔%以上、进一步更优选60摩尔%以上、特别优选68摩尔%以上,且优选86摩尔%以下、更优选84摩尔%以下、进一步优选82摩尔%以下。缩醛化度是指,将作为聚乙烯醇缩醛树脂的制造原料的聚乙烯醇系树脂中的主链的包含2个碳的单元(例如乙烯醇单元、乙酸乙烯酯单元、乙烯单元等)为一个重复单元,且以该一个重复单元为基准形成缩醛的上述单元的量。缩醛化度如果为前述下限值与上限值的范围内,则得到的聚乙烯醇缩醛树脂薄膜的力学强度容易变得充分,聚乙烯醇缩醛树脂与增塑剂的相溶性容易变得良好,故优选。在聚乙烯醇缩醛树脂薄膜包含2种以上不同的聚乙烯醇缩醛树脂的情况下,优选至少1种聚乙烯醇缩醛树脂的缩醛化度处于前述下限值与上限值的范围内。另外,从耐水性的观点出发,聚乙烯醇缩醛树脂的缩醛化度优选65摩尔%以上。缩醛化度可以通过调整缩醛化反应中的醛的用量而调整。
聚乙烯醇缩醛树脂的乙酸乙烯酯单元含量优选0.1摩尔%以上、更优选0.3摩尔%以上、进一步优选0.5摩尔%以上,且优选30摩尔%以下、更优选20摩尔%以下、特别优选0.5~3摩尔%或5~8摩尔%。乙酸乙烯酯单元的含量是指,将作为聚乙烯醇缩醛树脂的制造原料的聚乙烯醇系树脂中的主链的包含2个碳的单元(例如乙烯醇单元、乙酸乙烯酯单元、乙烯单元等)为一个重复单元,且以该一个重复单元为基准的乙酸乙烯酯单元的量。乙酸乙烯酯单元含量能对聚乙烯醇缩醛树脂的极性产生影响,据此,聚乙烯醇缩醛树脂薄膜的增塑剂相溶性或机械强度有可能会变化。乙酸乙烯酯单元含量如果处于前述下限值与上限值的范围内,则与根据情况相邻并层叠的增塑化聚乙烯醇缩醛树脂层的良好接合以及光学畸变的降低等容易达成。在聚乙烯醇缩醛树脂薄膜包含2种以上不同的聚乙烯醇缩醛树脂的情况下,优选至少1种聚乙烯醇缩醛树脂的乙酸乙烯酯单元含量处于前述范围内。乙酸乙烯酯单元的含量可以通过适宜调整原料的聚乙烯醇系树脂的皂化度而调整。
聚乙烯醇缩醛树脂的乙烯醇单元含量优选9~36摩尔%、更优选18~34摩尔%、进一步优选22~34摩尔%、进一步更优选26~34摩尔%、特别优选26~31摩尔%、特别是更优选26~30摩尔%。乙烯醇单元含量是指,将作为聚乙烯醇缩醛树脂的制造原料的聚乙烯醇系树脂中的主链的包含2个碳的单元(例如乙烯醇单元、乙酸乙烯酯单元、乙烯单元等)为一个重复单元,且以该一个重复单元为基准的乙烯醇单元的量。乙烯醇单元含量如果处于前述范围内,则与根据情况相邻并层叠的增塑化聚乙烯醇缩醛树脂薄膜的折射率差变小,容易得到光学不均少的夹层玻璃。另一方面,进一步为了也赋予隔音性能,优选的乙烯醇单元含量为9~29摩尔%、更优选12~26摩尔%、进一步优选15~23摩尔%、特别优选16~20摩尔%。在聚乙烯醇缩醛树脂薄膜包含2种以上不同的聚乙烯醇缩醛树脂的情况下,优选至少1种聚乙烯醇缩醛树脂的乙烯醇单元含量处于前述范围内。乙烯醇单元含量可以通过调整缩醛化反应中的醛的用量而调整为前述范围内。
聚乙烯醇缩醛树脂通常由形成缩醛的单元、乙烯醇单元和乙酸乙烯酯单元构成,这些各单元量例如通过JIS K6728“聚乙烯醇缩丁醛试验方法”或核磁共振法(NMR)而测定。
构成本发明的聚乙烯醇缩醛树脂薄膜的聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型(B型)粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇=1/1(质量比)溶液的粘度为100~1000mPa·s。前述粘度如果小于100mPa·s,则使用聚乙烯醇缩醛树脂薄膜作为夹层玻璃时不易确保充分的耐热性,如果大于1000mPa·s,则不易得到良好的制膜性。
本发明的一方式中,聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型(B型)粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇=1/1(质量比)溶液的粘度优选300mPa·s以下、更优选250mPa·s以下、进一步优选200mPa·s以下、特别优选180mPa·s以下。前述粘度如果为前述上限值以下,则使用该聚乙烯醇缩醛树脂薄膜制作夹层玻璃时容易使加热温度或加热时间为期望的范围,聚乙烯醇缩醛树脂的未熔融部变得不易残留,因此,不易引起聚乙烯醇缩醛树脂薄膜的黄变。作为上述粘度适合的具体例,可以举出:在聚乙烯醇缩醛树脂薄膜与增塑化聚乙烯醇缩醛树脂层之间的基本整面形成有无机物层、或不易使增塑剂渗透的树脂层、例如包含聚酯树脂或聚烯烃系树脂等而成的功能性层的情况等。从容易得到无聚乙烯醇缩醛树脂的未熔融部的夹层玻璃的观点出发,上述方式中的上述粘度的下限值优选100mPa·s以上、更优选120mPa·s以上、特别优选150mPa·s以上。
另外,本发明的另一方式中,聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型(B型)粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇=1/1(质量比)溶液的粘度优选大于200mPa·s、更优选210mPa·s以上、进一步优选220mPa·s以上、进一步更优选230mPa·s以上、特别优选240mPa·s以上、进一步更优选250mPa·s以上、特别是更优选265mPa·s以上。聚乙烯醇缩醛树脂的前述粘度如果为前述下限值以上,则即使成为高温,也容易得到玻璃不易错位的夹层玻璃,例如层叠功能性层、导电体等结构体时,也可以充分抑制这些变形和破坏。从容易得到良好的制膜性的观点出发,上述方式中的上述粘度的上限值通常为1000mPa·s以下、优选800mPa·s以下、更优选500mPa·s以下、进一步优选450mPa·s以下、特别优选400mPa·s以下。
前述粘度通过使用或并用使用粘均聚合度高的聚乙烯醇系树脂作为原料或原料的一部分而制造的聚乙烯醇缩醛树脂而调整。用于构成聚乙烯醇缩醛树脂薄膜的聚乙烯醇缩醛树脂由多个树脂的混合物构成的情况下,前述粘度为这种混合物的粘度。
前述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的峰顶分子量优选115000~200000、更优选120000~160000、特别优选130000~150000。聚乙烯醇缩醛树脂的峰顶分子量如果处于前述范围内,则容易得到适合的薄膜制膜性和适合的薄膜物性(例如层压适合性、耐蠕变性和断裂强度)。前述峰顶分子量通过使用或并用使用粘均聚合度高的聚乙烯醇系树脂作为原料或原料的一部分而制造的聚乙烯醇缩醛树脂而调整。
前述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的分子量分布、即、重均分子量(Mw)与数均分子量(Mn)之比(Mw/Mn)优选2.7以上、更优选2.8以上、特别优选2.9以上。聚乙烯醇缩醛树脂的分子量分布如果为前述下限值以上,则容易兼顾制膜性和适合的薄膜物性(例如层压适合性、耐蠕变性和断裂强度)。前述分子量分布可以通过将粘均聚合度不同的聚乙烯醇系树脂的混合物缩醛化、或将粘均聚合度不同的聚乙烯醇系树脂的缩醛化物混合而调整。分子量分布的上限值没有特别限定,从制膜容易性的观点出发,通常为10以下、优选5以下。
在前述聚乙烯醇缩醛树脂材料包含2种以上不同的聚乙烯醇缩醛树脂的情况下,优选至少1种聚乙烯醇缩醛树脂的峰顶分子量和分子量分布处于上述范围内。
需要说明的是,峰顶分子量和分子量分布例如用凝胶渗透色谱法(GPC)、以分子量已知的聚苯乙烯为标准而求出。
本发明中使用的聚乙烯醇缩醛树脂可以通过以往公知的方法而制造,代表性地,可以通过将聚乙烯醇系树脂(例如聚乙烯醇树脂或乙烯乙烯醇共聚物)利用醛缩醛化而制造。没有限定,具体而言例如,将浓度3~30质量%的聚乙烯醇或乙烯乙烯醇共聚物的水溶液保持为80~100℃的温度范围内后,用10~60分钟缓慢地冷却,温度降低至-10~30℃后,添加醛和酸催化剂,边将温度保持为恒定边进行30~300分钟的缩醛化反应。接着,将反应液用30~200分钟升温至20~80℃的温度,保持30~300分钟后,将反应液根据需要进行过滤后,添加碱等中和剂进行中和,将树脂过滤、水洗和干燥,从而可以制造本发明中能使用的聚乙烯醇缩醛树脂。
缩醛化反应中使用的酸催化剂没有特别限定,可以使用有机酸和无机酸,均可。作为这种酸催化剂的例子,可以举出乙酸、对甲苯磺酸、硝酸、硫酸和盐酸等。其中,从酸的强度和清洗时的去除容易性的观点出发,优选使用盐酸、硫酸和硝酸。
从容易得到具有适合的断裂能的聚乙烯醇缩醛树脂的观点出发,聚乙烯醇缩醛树脂的制造中使用的醛或酮化合物优选具有2~10个碳原子的直链状、支链状或环状化合物,更优选直链状或支链状化合物。由此,也可以带来相应的直链状或支链状的缩醛基。另外,本发明中使用的聚乙烯醇缩醛树脂可以为通过多个醛或酮化合物的混合物将聚乙烯醇或乙烯乙烯醇共聚物缩醛化而得到的缩醛化物。
本发明中使用的聚乙烯醇缩醛树脂优选通过至少1种聚乙烯醇系树脂与具有2~10个碳原子的1个以上脂肪族非支链的醛的反应而产生。作为这种醛,从容易得到具有适合的断裂能的聚乙烯醇缩醛树脂的观点出发,优选正丁醛。缩醛化中使用的醛中的正丁醛的含量优选50质量%以上、更优选80质量%以上、进一步优选95质量%以上、特别优选99质量%以上,可以为100质量%。本发明的优选一方式中,聚乙烯醇缩醛树脂为聚乙烯醇缩丁醛树脂。
用于制造聚乙烯醇缩醛树脂的聚乙烯醇系树脂可以为单独,或可以为粘均聚合度或水解度等不同的聚乙烯醇系树脂的混合物。
成为聚乙烯醇缩醛树脂的原料的聚乙烯醇系树脂的粘均聚合度优选100以上、更优选300以上、进一步优选400以上、进一步更优选600以上、特别优选700以上、特别是更优选750以上。聚乙烯醇系树脂的粘均聚合度如果为前述下限值以上,则制作夹层玻璃时容易抑制功能性层的变形和破坏,能防止得到的夹层玻璃中由于热而玻璃错位的现象。另外,聚乙烯醇系树脂的粘均聚合度优选5000以下、更优选3000以下、进一步优选2500以下、特别优选2300以下、特别是更优选2000以下。聚乙烯醇系树脂的粘均聚合度如果为前述上限值以下,则容易得到良好的制膜性。
需要说明的是,聚乙烯醇缩醛树脂的优选的粘均聚合度的值与上述聚乙烯醇系树脂的优选的粘均聚合度的值相同。在聚乙烯醇缩醛树脂薄膜包含2种以上不同的聚乙烯醇缩醛树脂的情况下,优选至少1种聚乙烯醇缩醛树脂的粘均聚合度为前述下限值以上且前述上限值以下。聚乙烯醇系树脂的粘均聚合度可以基于JIS K 6726“聚乙烯醇试验方法”而测定。
从容易得到良好的制膜性的观点出发,聚乙烯醇缩醛树脂薄膜优选包含未交联的聚乙烯醇缩醛。聚乙烯醇缩醛树脂薄膜也可以包含经交联的聚乙烯醇缩醛。用于使聚乙烯醇缩醛交联的方法例如记载于EP 1527107B1和WO 2004/063231 A1(含羧基的聚乙烯醇缩醛的热自交联)、EP 1606325 A1(利用聚醛交联了的聚乙烯醇缩醛)、和WO 2003/020776 A1(利用乙醛酸交联了的聚乙烯醇缩醛)。另外,通过适宜调整缩醛化反应条件,从而控制生成的分子间缩醛键量、或控制残留羟基的封端化度也是有用的方法。
(增塑剂)
本发明中,聚乙烯醇缩醛树脂薄膜中的增塑剂的量基于聚乙烯醇缩醛树脂薄膜的总质量为0~20质量%。前述增塑剂量如果超过20质量%,则变得不易得到良好的制膜性。另外,特别是在高温环境下树脂薄膜变得容易自粘合,有变得难以得到均匀的表面、或变得容易产生变形的倾向,因此,例如在层叠功能性层来制作夹层玻璃的情况下,变得无法发挥良好的功能性。虽然通过减少增塑剂量或不配混增塑剂,聚乙烯醇缩醛树脂薄膜有成膜性和操作性优异的倾向,但同时在低增塑或无增塑的聚乙烯醇缩醛树脂薄膜中,有变得容易产生卷褶皱的倾向。本发明的聚乙烯醇缩醛树脂薄膜中,通过精确地控制树脂薄膜的两表面的十点平均粗糙度和其均匀性,从而树脂薄膜的一个面与另一个面具有不同的表面形状,且各表面整体具有均匀的表面粗糙度。因此,即使为源自增塑剂量少而原本容易产生卷褶皱的树脂薄膜,在相邻的树脂薄膜间也产生适度的孔隙,可以有效地抑制卷褶皱的发生,将薄膜卷出时容易得到均匀的薄膜表面。因此,通过在较平滑的面(面B)层叠功能性层等,从而可以得到不易产生功能性层的经时的变形和破坏的夹层玻璃,本发明的聚乙烯醇缩醛树脂薄膜能适合作为具有功能性层等的夹层玻璃用的树脂薄膜使用。
前述增塑剂量基于聚乙烯醇缩醛树脂薄膜的总质量优选0~19质量%、更优选0~15质量%、进一步优选0~10质量%、特别优选0~5质量%。聚乙烯醇缩醛树脂薄膜中的增塑剂的量如果处于前述范围内,则有聚乙烯醇缩醛树脂薄膜的制膜性和操作性优异的倾向,另外,成为能适合用于制作具有功能性层等的夹层玻璃的树脂薄膜。
聚乙烯醇缩醛树脂薄膜中包含增塑剂的情况下,作为增塑剂,优选使用下述组的1个或多个化合物。
·多元的脂肪族或芳香族酸的酯。例如可以举出己二酸二烷基酯(例如己二酸二己酯、己二酸二-2-乙基丁酯、己二酸二辛酯、己二酸二-2-乙基己酯、己二酸己基环己酯、己二酸二庚酯、己二酸二壬酯、己二酸二异壬酯、己二酸庚基壬酯);己二酸与包含醇或醚化合物的醇的酯(例如己二酸二(丁氧基乙基)酯、己二酸二(丁氧基乙氧基乙基)酯);癸二酸二烷基酯(例如癸二酸二丁酯);癸二酸与包含脂环式或醚化合物的醇的酯;邻苯二甲酸的酯(例如邻苯二甲酸丁基苄酯、邻苯二甲酸双-2-丁氧基乙酯);和脂环式多元羧酸与脂肪族醇的酯(例如1,2-环己烷二羧酸二异壬基酯)。
·多元的脂肪族或芳香族醇或具有1个以上的脂肪族或芳香族取代基的低聚醚甘醇的酯或醚。例如可以举出甘油、二甘醇、三甘醇、四甘醇等与直链状或支链状的脂肪族或脂环式羧酸的酯。具体而言,可以举出二甘醇-双-(2-乙基己酸酯)、三甘醇-双-(2-乙基己酸酯)(以下中,也有时称为“3GO”)、三甘醇-双-(2-乙基丁酸酯)、四甘醇-双-正庚酸酯、三甘醇-双-正庚酸酯、三甘醇-双-正己酸酯、四甘醇二甲醚、和二丙二醇二苯甲酸酯。
·脂肪族或芳香族醇的磷酸酯。例如可以举出磷酸三(2-乙基己基)酯、磷酸三乙酯、磷酸二苯基-2-乙基己酯、和磷酸三甲苯酯。
·柠檬酸、琥珀酸和/或富马酸的酯。
另外,也可以使用由多元醇与多元羧酸构成的聚酯或低聚酯、它们的末端酯化物或醚化物、由内酯或羟基羧酸构成的聚酯或低聚酯、或它们的末端酯化物或醚化物等作为增塑剂。
聚乙烯醇缩醛树脂薄膜中包含增塑剂的情况下,从抑制伴有增塑剂在该聚乙烯醇缩醛树脂薄膜与能层叠的增塑化聚乙烯醇缩醛树脂层之间迁移的问题(例如经时的物性变化等问题)的观点出发,优选使用:与层叠的增塑化聚乙烯醇缩醛树脂层中所含者相同的增塑剂、或不有损该增塑化聚乙烯醇缩醛树脂层的物性(例如耐热性、耐光性、透明性和增塑化效率)的增塑剂。从这种观点出发,作为增塑剂,优选包含三甘醇-双-(2-乙基己酸酯)、三甘醇-双(2-乙基丁酸酯)、四甘醇-双-(2-乙基己酸酯)、四甘醇-双庚酸酯,特别优选包含三甘醇-双-(2-乙基己酸酯)。
进而,本发明的聚乙烯醇缩醛树脂薄膜可以包含其他添加剂。作为这种添加剂,例如可以举出水、紫外线吸收剂、抗氧化剂、粘接调节剂、增白剂或荧光增白剂、稳定剂、色素、加工助剂、耐冲击性改良剂、流动性改良剂、交联剂、颜料、发光材料、折射率调节剂、隔热材料、有机或无机纳米颗粒、焙烧硅酸和表面活性剂等。
通过减少聚乙烯醇缩醛树脂薄膜中的凝胶的量,从而变得不易在聚乙烯醇缩醛树脂薄膜上产生凸状缺陷,变得容易将Rz值控制为较低的范围。为了减少聚乙烯醇缩醛树脂薄膜中的凝胶的量,有用的是,抑制聚乙烯醇缩醛树脂的粒料化时、制膜时的凝胶的生成,为此,有用的是,在构成聚乙烯醇缩醛树脂薄膜的聚乙烯醇缩醛树脂材料中添加抗氧化剂等稳定剂。
作为抗氧化剂,例如可以举出酚系抗氧化剂、磷系抗氧化剂和硫系抗氧化剂等,其中,优选酚系抗氧化剂,特别优选烷基取代酚系抗氧化剂。
作为酚系抗氧化剂的例子,可以举出:丙烯酸2-叔丁基-6-(3-叔丁基-2-羟基-5-甲基苄基)-4-甲基苯酯、和丙烯酸2,4-二叔戊基-6-(1-(3,5-二叔戊基-2-羟基苯基)乙基)苯酯等丙烯酸酯系化合物、2,6-二叔丁基-4-甲基苯酚、2,6-二叔丁基-4-乙基苯酚、十八烷基-3-(3,5-)二叔丁基-4-羟基苯基)丙酸酯、2,2’-亚甲基-双(4-甲基-6-叔丁基苯酚)、4,4’-丁叉基-双(4-甲基-6-叔丁基苯酚)、4,4’-丁叉基-双(6-叔丁基-间甲酚)、4,4’-硫代双(3-甲基-6-叔丁基苯酚)、双(3-环己基-2-羟基-5-甲基苯基)甲烷、3,9-双(2-(3-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基)-1,1-二甲基乙基)-2,4,8,10-四氧杂螺[5,5]十一烷、1,1,3-三(2-甲基-4-羟基-5-叔丁基苯基)丁烷、1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯、四(亚甲基-3-(3’,5’-二叔丁基-4’-羟基苯基)丙酸酯)甲烷、和三甘醇双(3-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯)等烷基取代酚系化合物、6-(4-羟基-3,5-二叔丁基苯胺基)-2,4-双-辛基硫代-1,3,5-三嗪、6-(4-羟基-3,5-二甲基苯胺基)-2,4-双-辛基硫代-1,3,5-三嗪、6-(4-羟基-3-甲基-5-叔丁基苯胺基)-2,4-双-辛基硫代-1,3,5-三嗪、和2-辛基硫代-4,6-双-(3,5-二叔丁基-4-氧苯胺基)-1,3,5-三嗪等含三嗪基酚系化合物等。
作为磷系抗氧化剂,例如可以举出:亚磷酸三苯酯、亚磷酸二苯基异癸酯、亚磷酸苯基二异癸酯、亚磷酸三(壬基苯基)酯、亚磷酸三(二壬基苯基)酯、亚磷酸三(2-叔丁基-4-甲基苯基)酯、亚磷酸三(环己基苯基)酯、亚磷酸2,2-亚甲基双(4,6-二叔丁基苯基)辛酯、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、10-(3,5-二叔丁基-4-羟基苄基)-9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、和10-癸氧基-9,10-二氢-9-氧杂-10-磷杂菲等单亚磷酸酯系化合物、4,4’-丁叉基-双(3-甲基-6-叔丁基苯基-二-十三烷基亚磷酸酯)、4,4’-异丙叉基-双(苯基-二-烷基(C12~C15)亚磷酸酯)、4,4’-异丙叉基-双(二苯基单烷基(C12~C15)亚磷酸酯)、1,1,3-三(2-甲基-4-二-十三烷基亚磷酸酯-5-叔丁基苯基)丁烷、和四(2,4-二叔丁基苯基)-4,4’-亚联苯基亚磷酸酯等二亚磷酸酯系化合物等。其中,优选单亚磷酸酯系化合物。
作为硫系抗氧化剂,例如可以举出:二月桂基3,3’-硫代二丙酸酯、二硬脂基3,3-硫代二丙酸酯、月桂基硬脂基3,3’-硫代二丙酸酯、季戊四醇-四-(β-月桂基-硫代丙酸酯)、和3,9-双(2-十二烷基硫代乙基)-2,4,8,10-四氧杂螺[5.5]十一烷等。
这些抗氧化剂可以单独使用,或组合2种以上而使用。抗氧化剂的添加量相对于聚乙烯醇缩醛树脂100质量份,优选0.001质量份以上、更优选0.01质量份以上。抗氧化剂的量如果为前述下限值以上,则容易有效地抑制聚乙烯醇缩醛树脂的分解等所产生的凝胶的生成。另外,抗氧化剂的添加量相对于聚乙烯醇缩醛树脂100质量份,通常为5质量份以下、优选1质量份以下、更优选0.1质量份以下。抗氧化剂的添加量可以多于5质量份,但无法期望关于凝胶生成抑制的额外的效果。
另外,为了防止聚乙烯醇缩醛树脂的氧化劣化,还优选在氮气气氛下进行聚乙烯醇缩醛树脂薄膜的制造工序的至少一部分,例如使用挤出机制造聚乙烯醇缩醛树脂薄膜时将进料口和排出口附近进行氮气置换。
作为其他稳定剂,可以举出紫外线吸收剂、紫外线屏蔽剂和光稳定剂等。
作为紫外线吸收剂,可以举出2-(5-甲基-2-羟基苯基)苯并***、2-[2-羟基-3,5-双(α,α’-二甲基苄基)苯基]-2H-苯并***、2-(3,5-二叔丁基-2-羟基苯基)苯并***、2-(3-叔丁基-5-甲基-2-羟基苯基)-5-氯苯并***、2-(3,5-二叔丁基-5-甲基-2-羟基苯基)-5-氯苯并***、2-(3,5-二叔戊基-2-羟基苯基)苯并***、和2-(2’-羟基-5’-叔辛基苯基)苯并***等苯并***系紫外线吸收剂、2,2,6,6-四甲基-4-哌啶基苯甲酸酯、双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(1,2,2,6,6-五甲基-4-哌啶基)-2-(3,5-二叔丁基-4-羟基苄基)-2-正丁基丙二酸酯、和4-(3-(3,5-二叔丁基-4-羟基苯基)丙酰氧基)-1-(2-(3-(3,5-二叔丁基-4-羟基苯基)丙酰氧基)乙基)-2,2,6,6-四甲基哌啶等受阻胺系紫外线吸收剂、2,4-二叔丁基苯基-3,5-二叔丁基-4-羟基苯甲酸酯、和十六烷基-3,5-二叔丁基-4-羟基苯甲酸酯等苯甲酸酯系紫外线吸收剂、和丙二酸酯系紫外线吸收剂等。
作为丙二酸酯系紫外线吸收剂,可以举出2-(对甲氧基苄叉基)丙二酸二甲酯、四乙基-2,2-(1,4-亚苯基二甲叉基)双丙二酸酯、和2-(对甲氧基苄叉基)-双(1,2,2,6,6-五甲基4-哌啶基)丙二酸酯等。也可以使用市售的丙二酸酯系紫外线吸收剂,作为其例子,可以举出Hostavin B-CAP、Hostavin PR-25、和Hostavin PR-31(均为Clariant公司制)。
作为紫外线屏蔽剂,可以举出草酰苯胺化合物、例如N-(2-乙基苯基)-N’-(2-乙氧基-5-叔丁基苯基)草酸二酰胺、N-(2-乙基苯基)-N’-(2-乙氧基-苯基)草酸二酰胺、和2-乙基-2’-乙氧基-氧基酰替苯胺(Oxyanilide)(Clariant公司制“SanduvorVSU”)等在氮原子上具有取代了的芳基等的草酸二酰胺类等。
紫外线吸收剂或紫外线屏蔽剂的添加量相对于聚乙烯醇缩醛树脂薄膜中所含的聚乙烯醇缩醛树脂,以质量基准计优选10ppm以上、更优选100ppm以上。紫外线吸收剂或紫外线屏蔽剂的添加量如果为前述下限值以上,则容易发挥充分的效果。另外,紫外线吸收剂或紫外线屏蔽剂的添加量相对于聚乙烯醇缩醛树脂薄膜中所含的聚乙烯醇缩醛树脂,以质量基准计通常为50000ppm以下、优选10000ppm以下。可以使紫外线吸收剂或紫外线屏蔽剂的添加量多于50000ppm,但无法期望关于凝胶生成抑制的额外的效果。
紫外线吸收剂或紫外线屏蔽剂可以单独使用,或组合2种以上而使用。
作为光稳定剂,可以使用受阻胺系光稳定剂,作为其市售品的例子,可以举出株式会社ADEKA制“ADECASTAB LA-57(商品名)”。
本发明的聚乙烯醇缩醛树脂薄膜中的聚乙烯醇缩醛树脂的量基于聚乙烯醇缩醛树脂薄膜的总质量,优选75质量%以上、更优选80质量%以上、进一步优选85质量%以上、更优选90质量%以上、特别优选95质量%以上。聚乙烯醇缩醛树脂薄膜中的聚乙烯醇缩醛树脂的量如果处于前述范围内,则容易制造透明性、制膜性和操作性优异的聚乙烯醇缩醛树脂薄膜,另外,成为能适合用于制作具有功能性层等的夹层玻璃的树脂薄膜。
本发明的聚乙烯醇缩醛树脂薄膜可以具有基于多成分的层分离结构,但层分离结构的岛成分的平均粒径优选低于100nm、更优选低于80nm,特别优选不示出海岛的层分离结构。不示出海岛的层分离结构,或示出充分细的粒径,从而可以确保也能用于车的挡风玻璃等的透明性。
<聚乙烯醇缩醛树脂薄膜的制造方法>
聚乙烯醇缩醛树脂薄膜的制造方法没有特别限定。将前述聚乙烯醇缩醛树脂、根据情况的规定量的增塑剂、和根据需要的其他添加剂配混,将其均匀地混炼后,通过挤出法、压延法、加压法、浇铸法、吹胀法等公知的制膜方法,成型为薄膜状,从而能制作。
公知的制膜方法中,特别适合采用使用挤出机制造薄膜的方法。挤出时的树脂温度优选150~250℃、更优选170~230℃。树脂温度如果过度变高,则引起聚乙烯醇缩醛树脂分解,挥发性物质的含量变多。另一方面,温度过低的情况下,挥发性物质的含量也变多。为了有效地去除挥发性物质,优选从挤出机的排气口通过减压去除挥发性物质。
熔融挤出中,使用表面形状、材质不同的冷却辊,从而可以将树脂薄膜表面的十点平均粗糙度和其均匀性(各表面的十点平均粗糙度的标准偏差/Rz1(a)或Rz2(a)的值)控制为特定的范围。例如,为了形成平滑的面,可以使用以金属弹性辊和金属刚体辊等镜面金属冷却辊为代表的平滑的(镜面)冷却辊,为了形成粗糙的面,可以使用对应于期望的表面形状(表面粗糙度)的金属弹性辊、橡胶弹性辊、压花辊。为了控制树脂薄膜的两表面的表面形状使得树脂薄膜的各表面的十点平均粗糙度和其均匀性成为上述特定范围,优选的是,适宜选择这些辊,将从T模头挤出的树脂材料制膜。例如,使夹住挤出的树脂材料的辊对的一者为镜面辊、另一者为适于形成凹凸的压花辊等,从而可以得到具有平滑的面和较粗糙的面的树脂薄膜。这种成型中,选择压花辊的表面形状的波动小者,或选择挤出成型时的宽度方向上的、压花形状的赋型率成为相同的成型条件,从而可以将各表面的十点平均粗糙度的标准偏差/Rz1(a)、或Rz2(a)控制为本发明的适合的范围。
从容易控制聚乙烯醇缩醛树脂薄膜的两表面的表面形状、容易得到上述特定的十点平均粗糙度和其均匀性的观点出发,优选制膜时的辊对的至少一者使用选自金属辊、橡胶辊中的辊,更优选使用金属辊。另外,从同样的观点出发,与聚乙烯醇缩醛树脂薄膜中所含的聚乙烯醇缩醛树脂的玻璃化转变温度相比,从冷却辊剥离时的聚乙烯醇缩醛树脂薄膜的温度优选低5℃以上、更优选低10℃以上、进一步优选低15℃以上、特别优选低20℃以上。从冷却辊剥离时的聚乙烯醇缩醛树脂薄膜的温度与上述玻璃化转变温度如果满足上述关系,则容易减少由于从冷却辊剥离时的聚乙烯醇缩醛树脂薄膜的粘合性所导致的表面粗糙、或由于薄膜的收缩等所导致的厚度不均。需要说明的是,在聚乙烯醇缩醛树脂薄膜中所含的聚乙烯醇缩醛树脂为2种以上不同的聚乙烯醇缩醛树脂的情况下,优选至少1种聚乙烯醇缩醛树脂的玻璃化转变温度与冷却辊的剥离点处的聚乙烯醇缩醛树脂薄膜的温度满足上述关系。
本发明中,聚乙烯醇缩醛树脂薄膜的表面的十点平均粗糙度和其均匀性(各表面的十点平均粗糙度的标准偏差/Rz1(a)或Rz2(a)的值)均受到薄膜的表面形状的影响,但十点平均粗糙度和其均匀性均未必处于恒定的相关关系。因此,本发明的聚乙烯醇缩醛树脂薄膜中,重要的是,将各表面的十点平均粗糙度与各表面的十点平均粗糙度的标准偏差/Rz1(a)或Rz2(a)的值分别控制为上述规定的范围。
<聚乙烯醇缩醛树脂薄膜卷>
本发明的聚乙烯醇缩醛树脂薄膜的一个面与另一个面具有彼此不同的表面形状,且各表面整体中的表面粗糙度均匀,因此,该将树脂薄膜卷绕为卷状时的自粘合抑制效果优异,且以具有较粗糙的面的面A侧成为卷的内侧的方式将树脂薄膜卷绕,从而灰尘、尘埃等异物在保管中、输送、搬运中等变得不易附着,另一方面,以该面A成为卷的外侧的方式将树脂薄膜卷绕,从而即使灰尘、尘埃等异物附着于树脂薄膜上,也可以容易去除。分别在能改善利用该薄膜卷时的作业效率的方面,异物不易附着、或异物容易去除也是有利的。因此,本发明中,也将以本发明的聚乙烯醇缩醛树脂薄膜的面A侧成为内侧的方式卷绕而成的聚乙烯醇缩醛树脂薄膜卷、和以本发明的聚乙烯醇缩醛树脂薄膜的面A侧成为外侧的方式卷绕而成的聚乙烯醇缩醛树脂薄膜卷作为对象。
本发明的聚乙烯醇缩醛树脂薄膜卷可以使用公知的方法和装置/设备而制造,例如,可以在适当的卷芯上卷绕长尺寸的本发明的聚乙烯醇缩醛树脂薄膜使得任意的面成为内侧或外侧。作为构成卷芯的材料,例如可以举出聚乙烯树脂、聚丙烯树脂、聚氯乙烯树脂、聚酯树脂、环氧树脂、酚醛树脂、三聚氰胺树脂、硅树脂、聚氨酯树脂、聚碳酸酯树脂、ABS树脂等合成树脂;铝等金属;纤维增强塑料;纸等。卷芯通常呈圆筒状或圆柱状等形状,其直径例如可以为20~200mm。另外,薄膜卷的直径(卷取后的直径)没有特别限定,通常为30~800mm。
树脂薄膜卷绕时的张力、卷取速度、温度等可以根据聚乙烯醇缩醛树脂薄膜的组成、宽度、厚度等而适宜选择。
<聚乙烯醇缩醛树脂薄膜卷的保管方法>
本发明的聚乙烯醇缩醛树脂薄膜在包含高温环境的广泛的温度域内具有高的自粘合抑制效果。因此,本发明还涉及一种聚乙烯醇缩醛树脂薄膜卷的保管方法,其包括如下步骤:将本发明的聚乙烯醇缩醛树脂薄膜卷在-20℃~60℃的温度下进行保管。特别是,通常,与将聚乙烯醇缩醛树脂薄膜在低温(例如20℃以下)下进行保管的情况相比,在能成为30℃以上的高温、特别是50℃以上的高温环境下进行保管的情况下,保管中有时发生自粘合,但通过适当控制树脂薄膜的两表面的表面形状和其均匀性,从而即使在历经长期间地保管的情况下,薄膜彼此的自粘合也变得不易产生。因此,本发明的保管方法中,特别是在50℃以上的温度下进行保管的情况下也可以得到优异的自粘合抑制效果。需要说明的是,本发明的保管方法中,“在~℃(以上)的温度下进行保管”通常是指在被管理为该温度以上的特定温度的环境下保管的情况,例如还包括在室温下保管而包含在该特定温度以上的温度下保管的时间的情况。另外,在保管中,上述温度以外的条件没有特别限制,例如,聚乙烯醇缩醛树脂薄膜卷可以为静置的状态,也可以为供于输送等接受振动的状态。
聚乙烯醇缩醛树脂薄膜卷的保管条件可以根据聚乙烯醇缩醛树脂薄膜的组成等而适宜确定。
<带功能性层的聚乙烯醇缩醛树脂薄膜>
本发明的聚乙烯醇缩醛树脂薄膜的自粘合抑制效果优异,且不易产生经时的变形,从卷卷出时的表面均匀性高,因此,适合作为用于层叠功能性层的树脂薄膜。因此,本发明也将在本发明的聚乙烯醇缩醛树脂薄膜的至少一个面具有功能性层的带功能性层的聚乙烯醇缩醛树脂薄膜作为对象。本发明中功能性层是指,对夹层玻璃等层叠体赋予特定的功能的层。功能性层可以为1层或多层。聚乙烯醇缩醛树脂薄膜具有多个功能性层的情况下,各自的功能性层的种类可以相同也可以不同。
设置功能性层的情况下,优选在本发明的聚乙烯醇缩醛树脂薄膜的表面中作为更平滑面的面B设置功能性层。通过在面B设置功能性层,从而聚乙烯醇缩醛树脂薄膜与功能性层的密合性改善,变得不易产生功能性层的经时的变形、破坏。带功能性层的聚乙烯醇缩醛树脂薄膜具有多个功能性层的情况下,可以根据功能性层的种类、目的而适宜选择层叠的面,但形成后述的层叠体(夹层玻璃)时,通过使本发明的聚乙烯醇缩醛树脂薄膜的较粗糙面的面A与透明基材贴合,从而可以有效地抑制夹层玻璃等中的发泡,因此,优选多个功能性层均设置于面B侧。
在聚乙烯醇缩醛树脂薄膜的具有功能性层的面,聚乙烯醇缩醛树脂薄膜可以在其面的整面具有功能性层,也可以在其面的一部分具有功能性层。将后述的增塑化聚乙烯醇缩醛树脂层层叠于聚乙烯醇缩醛树脂薄膜而制作层叠体的情况下,优选聚乙烯醇缩醛树脂薄膜在其面的一部分具有功能性层使得增塑化聚乙烯醇缩醛树脂层中的增塑剂可以向聚乙烯醇缩醛树脂薄膜迁移。但是,只要功能性层不妨碍增塑剂从增塑化聚乙烯醇缩醛树脂层向聚乙烯醇缩醛树脂薄膜的迁移,就不限定于此。
功能性层优选为选自由导电层、红外线反射层或紫外线反射层那样的特定波长电磁波反射层、色彩校正层、红外线吸收层、紫外线吸收层、荧光/发光层、隔音层、电致变色层、光致变色层、热致变色层、设计性层和高弹性模量层组成的组中的1者以上。
本发明的聚乙烯醇缩醛树脂薄膜的增塑剂含量较少,因此,不易产生树脂薄膜的变形等,且以树脂薄膜的两面具有上述特定的表面粗糙度的方式构成,因此,通过适当选择层叠功能性层的面,从而可以得到对功能性层的经时的变形和破坏的高的抑制效果。因此,本发明的聚乙烯醇缩醛树脂薄膜特别适合于制造在以往的聚乙烯醇缩醛树脂薄膜中包含容易产生变形、断裂的导电层的树脂薄膜。因此,本发明的一方式中,功能性层优选为导电层。
从电阻和制造的容易性等的观点出发,导电层的厚度优选1~30μm、更优选2~15μm、特别优选3~10μm。导电层的厚度用厚度计或激光显微镜等而测定。
从电阻、放热性能、电磁波吸收性和光学特性等的观点出发,导电层优选具有线状、格子状或网状的形状。此处,作为线状的例子,可以举出直线状、波浪线状和Z字形状等。1个导电层中,可以为单一的形状,也可以混合存在多个形状。
某一方式、例如通过印刷法形成导电层,例如在前方可视性的确保不重要的区域中,将层叠体(夹层玻璃)部分地加热、或用作传感器或天线的方式中,从充分的放热量或作为传感器或天线的功能性的确保和制造容易性的观点出发,导电层优选由线宽0.001~5mm的多个线状导电性材料构成。即,构成前述线状、格子状或网状的形状的线状导电性材料(布线)的线宽优选0.001~5mm。前述线宽更优选0.01~2mm、特别优选0.03~1mm。
另一方式、例如将层叠体整面地加热的方式中,从容易确保充分的放热量和良好的前方可视性这两者的观点出发,导电层优选由线宽1~30μm的多个线状导电性材料构成。即,构成前述线状、格子状或网状的形状的线状导电性材料的线宽优选1~30μm。前述线宽更优选2~15μm、特别优选3~12μm。
从电阻或放热量的确保的容易性、和制造容易性的观点出发,构成导电层的导电性材料优选包含银或铜,更优选仅由银或铜构成。另外,从经济的观点出发,构成导电层的导电性材料更优选包含铜,更优选仅由铜构成。
导电层基于金属箔的方式中,优选导电层的至少一面进行低反射率处理,更优选导电层的两面进行低反射率处理。本发明中“进行低反射率处理”是指,进行处理使得依据JIS R 3106而测定的可见光反射率成为30%以下。从前方可视性的观点出发,更优选进行处理使得可见光反射率成为10%以下。可见光反射率如果为前述上限值以下,则使用具有导电层的聚乙烯醇缩醛树脂薄膜制作层叠体时,容易得到期望的可见光反射率,使用层叠体作为交通工具用夹层玻璃的情况下等,有前方可视性优异的倾向。
作为低反射率处理的方法,例如可以举出黑化处理(暗色化处理)、褐色化处理和镀覆处理等。从工序通过性的观点出发,低反射率处理优选为黑化处理。因此,从良好的前方可视性的观点出发,特别优选对导电层的单面、两面或整面进行黑化处理使得可见光反射率成为10%以下。黑化处理具体而言使用碱系黑化液等而进行。
<带功能性层的聚乙烯醇缩醛树脂薄膜的制造方法>
带功能性层的聚乙烯醇缩醛树脂薄膜的制造方法没有特别限制,例如,可以通过包括如下步骤的方法而制造:在设有功能性层的聚乙烯醇缩醛树脂薄膜的表面涂布、印刷或层压构成功能性层的材料。
前述涂布、印刷或层压构成功能性层的材料的方法没有特别限定。
作为涂布的方法,例如可以举出如下方法:将构成聚乙烯醇缩醛树脂薄膜的树脂材料的熔融物涂布于功能性层的方法(例如在功能性层上熔融挤出前述树脂材料的方法、或在功能性层上通过刮刀涂布等涂布前述树脂材料的方法);在聚乙烯醇缩醛树脂薄膜上通过蒸镀、溅射或电气蒸镀赋予功能性层的方法;功能性层由树脂材料构成的情况下,将构成聚乙烯醇缩醛树脂薄膜的树脂材料与构成功能性层的树脂材料同时挤出的方法;或使聚乙烯醇缩醛树脂薄膜浸渍于构成功能性层的树脂材料的溶液中的方法。
作为印刷的方法,例如可以举出丝网印刷、柔性印刷、或凹版印刷。该印刷的方法中,可以使用在层叠具有功能性层的聚乙烯醇缩醛树脂薄膜之前进行干燥或通过热或光进行固化的墨。
作为层压的(贴合)方法,例如可以举出如下方法:将功能性层与聚乙烯醇缩醛树脂薄膜重叠并进行热压接的方法;将溶剂、或包含构成聚乙烯醇缩醛树脂薄膜的树脂和溶剂的树脂材料(组合物)的溶液涂布于功能性层和聚乙烯醇缩醛树脂薄膜的一者或两者,或注入至功能性层与聚乙烯醇缩醛树脂薄膜之间,使功能性层与聚乙烯醇缩醛树脂薄膜接合的方法;用粘接剂使功能性层与聚乙烯醇缩醛树脂薄膜接合的方法。作为使用粘接剂接合的方法中能使用的粘接剂,可以使用本技术领域中通常使用的粘接剂,可以举出丙烯酸酯系粘接剂、氨基甲酸酯系粘接剂、环氧系粘接剂和热熔粘接剂。光学上要求优异的特性的方式中,从不产生源自粘接剂的雾度的观点出发,优选不使用粘接剂地将功能性层与聚乙烯醇缩醛树脂薄膜接合的方法。
功能性层为导电层的方式中,印刷法中使用的墨通常包含导电性颗粒和/或导电性纤维。导电性颗粒或导电性纤维没有特别限定,例如可以举出金属颗粒(例如金、银、铜、锌、铁或铝的颗粒);用金属覆盖了的颗粒或纤维(例如镀银的玻璃纤维或玻璃小球);或导电性炭黑、碳纳米管、石墨或石墨烯的颗粒或纤维等。进而,导电性颗粒可以为导电性金属氧化物的颗粒等半导体的颗粒、例如铟掺杂氧化锡、铟掺杂氧化锌或锑掺杂氧化锡的颗粒。从导电性的观点出发,前述墨优选包含银颗粒、铜颗粒和/或碳纳米管,更优选包含银颗粒或铜颗粒,从经济的观点出发,特别优选包含铜颗粒。
本发明的优选一方式中,导电层(导电性结构体)为金属箔的蚀刻结构体。从赋予导电性结构体时的生产效率高的观点和黑化处理容易性的观点出发,优选该方式。使金属箔与聚乙烯醇缩醛树脂薄膜接合的工序例如可以以下述方法(I)~(III)中的任意者进行。
(I)将聚乙烯醇缩醛树脂薄膜与金属箔重叠并热压接的方法、
(II)在金属箔上覆盖构成聚乙烯醇缩醛树脂薄膜的树脂材料的熔融物并接合的方法、例如在金属箔上熔融挤出前述树脂材料的方法、或将前述树脂材料通过刮刀涂布等涂布在金属箔上的方法、或
(III)将溶剂、或包含构成聚乙烯醇缩醛树脂薄膜的树脂和溶剂的树脂材料(组合物)的溶液或分散液涂布于金属箔和聚乙烯醇缩醛树脂薄膜的一者或两者,或注入至金属箔与聚乙烯醇缩醛树脂薄膜之间,使金属箔与聚乙烯醇缩醛树脂薄膜接合的方法。
上述方法(I)中的将金属箔与聚乙烯醇缩醛树脂薄膜热压接时的接合温度取决于构成聚乙烯醇缩醛树脂薄膜的树脂的种类,通常为90~170℃、优选100~160℃、更优选105~155℃、进一步优选105~150℃。接合温度如果为上述范围内,则容易得到良好的接合强度。
从降低聚乙烯醇缩醛树脂薄膜中的挥发性物质的含量的观点出发,上述方法(II)中的挤出时的树脂温度优选150~250℃、更优选170~230℃。
作为上述方法(III)中的溶剂,优选使用聚乙烯醇缩醛树脂中通常使用的增塑剂。
由得到的带金属箔的聚乙烯醇缩醛树脂薄膜形成导电层的期望的形状的工序可以利用公知的光刻法的手法而进行。前述工序例如如后述的实施例中记载,首先,在带金属箔的聚乙烯醇缩醛树脂薄膜的金属箔上层压干膜抗蚀剂后,利用光刻法的手法,形成耐蚀刻图案,接着,使赋予了耐蚀刻图案的聚乙烯醇缩醛树脂薄膜浸渍于蚀刻液以形成导电层的形状后,通过公知的方法,将残留的光致抗蚀层去除,从而可以进行。
<层叠体>
本发明涉及一种层叠体,其包含:透明基材;和,本发明的聚乙烯醇缩醛树脂薄膜或带功能性层的聚乙烯醇缩醛树脂薄膜。本发明还涉及一种层叠体,其在多个透明基材之间包含本发明的聚乙烯醇缩醛树脂薄膜或带功能性层的聚乙烯醇缩醛树脂薄膜。
从透明性、耐气候性和力学强度的观点出发,前述透明基材优选为无机玻璃(以下,也有时简称为玻璃)、或甲基丙烯酸类树脂片、聚碳酸酯树脂片、聚苯乙烯系树脂片、聚酯系树脂片、聚酰亚胺系树脂片、或聚环烯烃系树脂片等有机玻璃,更优选为无机玻璃、甲基丙烯酸类树脂片或聚碳酸酯树脂片,特别优选为无机玻璃。作为无机玻璃,没有特别限制,可以举出浮法玻璃、强化玻璃、半强化玻璃、化学强化玻璃、绿玻璃或石英玻璃等。另外,对使用的透明基材的形状没有特别限制,可以为单纯的平面状的透明基材,也可以为具有曲率的透明基材。
包含带功能性层的聚乙烯醇缩醛树脂薄膜的层叠体中,前述聚乙烯醇缩醛树脂薄膜中的功能性层可以与透明基材接触,也可以与后述的增塑化聚乙烯醇缩醛树脂层等其他层接触。
包含导电层作为功能性层的情况下,导电层的各布线通常与母线连接。作为母线,使用本技术领域中通常使用的母线,作为其例子,可以举出金属箔带、带导电性粘合剂的金属箔带和导电性糊剂等。另外,形成导电层时的同时,通过残留金属箔的一部分作为母线,从而可以形成母线。在母线上分别连接供电线,各供电线连接于电源,因此,向导电性结构体供给电流。
本发明中,层叠体可以还包含增塑化聚乙烯醇缩醛树脂层。增塑化聚乙烯醇缩醛树脂层含有聚乙烯醇缩醛树脂和增塑剂。作为增塑化聚乙烯醇缩醛树脂层中所含的聚乙烯醇缩醛树脂和增塑剂,可以使用与作为能构成本发明的聚乙烯醇缩醛树脂薄膜者的上述示例的物质同样的物质。
对于增塑化聚乙烯醇缩醛树脂层中的增塑剂的含量,在层叠层前的初始状态下,基于增塑化聚乙烯醇缩醛树脂层的总质量,优选16.0质量%以上、更优选16.1~36.0质量%、进一步优选22.0~32.0质量%、特别优选26.0~30.0质量%。前述增塑剂含量如果处于前述范围内,则容易得到耐冲击性优异的夹层玻璃。另外,作为增塑化聚乙烯醇缩醛树脂层,也可以使用具有隔音功能的增塑化聚乙烯醇缩醛树脂层。此时,对于增塑剂的含量,在层叠层前的初始状态下,基于增塑化聚乙烯醇缩醛树脂层的总质量,优选30质量%以上、更优选30~50质量%、进一步优选31~40质量%、特别优选32~35质量%。
增塑化聚乙烯醇缩醛树脂层根据需要可以含有作为构成本发明的聚乙烯醇缩醛树脂薄膜的添加剂示例的添加剂。另外,增塑化聚乙烯醇缩醛树脂层可以通过与本发明的聚乙烯醇缩醛树脂薄膜同样的方法而制造。
增塑化聚乙烯醇缩醛树脂层的厚度优选100~1600μm、更优选350~1200μm、进一步优选700~900μm。增塑化聚乙烯醇缩醛树脂层的厚度如果处于前述范围内,则容易得到优异的耐贯通性。上述厚度用厚度计或激光显微镜等而测定。
层叠体具有增塑化聚乙烯醇缩醛树脂层的情况下,构成本发明的聚乙烯醇缩醛树脂薄膜的聚乙烯醇缩醛树脂的乙烯醇单元的量、与构成前述增塑化聚乙烯醇缩醛树脂层的聚乙烯醇缩醛树脂的乙烯醇单元的量之差优选5摩尔%以下、更优选3摩尔%以下、特别优选1摩尔%以下。构成本发明的聚乙烯醇缩醛树脂薄膜的聚乙烯醇缩醛树脂或构成增塑化聚乙烯醇缩醛树脂层的聚乙烯醇缩醛树脂由多个树脂的混合物构成的情况下,构成本发明的聚乙烯醇缩醛树脂层的聚乙烯醇缩醛树脂的平均乙烯醇单元的量与增塑化聚乙烯醇缩醛树脂层的聚乙烯醇缩醛树脂的平均乙烯醇单元的量优选满足前述关系。前述差如果为前述上限值以下,则层叠体中增塑剂迁移后的平衡状态下的聚乙烯醇缩醛树脂薄膜与增塑化聚乙烯醇缩醛树脂层的折射率差变小,因此,使用彼此尺寸不同的增塑化聚乙烯醇缩醛树脂层与聚乙烯醇缩醛树脂薄膜的情况下,不易可视其边界,故优选。
另一方面,对构成本发明的聚乙烯醇缩醛树脂薄膜的聚乙烯醇缩醛树脂的乙烯醇单元的量、与构成前述增塑化聚乙烯醇缩醛树脂层的聚乙烯醇缩醛树脂的乙烯醇单元的量赋予差,从而在增塑剂迁移后的平衡状态下,也可以对聚乙烯醇缩醛树脂薄膜中的增塑剂量与增塑化聚乙烯醇缩醛树脂层中的增塑剂量之间赋予差,得到隔音性能优异的层叠体。上述情况下,前述乙烯醇单元的量之差优选5摩尔%以上、更优选8摩尔%以上。
增塑化聚乙烯醇缩醛树脂层可以为市售的增塑化聚乙烯醇缩丁醛片,也可以为分散有具有红外线吸收能力或反射能力的纳米颗粒的增塑化聚乙烯醇缩醛树脂层、经着色的增塑化聚乙烯醇缩醛树脂层、或具有隔音功能的增塑化聚乙烯醇缩醛树脂层。
<层叠体的制造方法>
层叠体可以以对本领域技术人员来说公知的方法而制造。例如,在透明基材上以任意的顺序重叠并配置任意的张数的本发明的聚乙烯醇缩醛树脂薄膜或带功能性层的聚乙烯醇缩醛树脂薄膜和根据情况的增塑化聚乙烯醇缩醛树脂层,进一步重叠另一张透明基材,对于其,作为预压接工序,提高温度以使聚乙烯醇缩醛树脂薄膜和根据情况的增塑化聚乙烯醇缩醛树脂层整面或局部地熔接于透明基材,接着,在高压釜中进行处理,从而可以制造层叠体。另外,将本发明的聚乙烯醇缩醛树脂薄膜或带功能性层的聚乙烯醇缩醛树脂薄膜以及根据情况的增塑化聚乙烯醇缩醛树脂层等的、构成层叠体的透明基材以外的层预先进行预粘接后,配置于2张透明基材之间,在高温下彼此熔接,从而可以制造层叠体。
此时,与透明基材接触的本发明的聚乙烯醇缩醛树脂薄膜的表面优选为较粗糙面的面A。面A与透明基材接触,从而使透明基材与聚乙烯醇缩醛树脂薄膜贴合时变得容易脱气,可以抑制层叠体(夹层玻璃)中的发泡。
本发明的层叠体可以作为建筑物或交通工具中使用的夹层玻璃使用。因此,本发明还涉及作为交通工具用夹层玻璃的层叠体。交通工具用夹层玻璃是指,用于火车、电车、汽车、船舶或航空机的交通工具的、挡风玻璃、后玻璃、顶玻璃或侧窗玻璃等。
本发明中,在层叠体包含相邻或接近于聚乙烯醇缩醛树脂薄膜的增塑化聚乙烯醇缩醛树脂层的情况下,通常,增塑化聚乙烯醇缩醛树脂层中所含的增塑剂随着时间经过而向聚乙烯醇缩醛树脂薄膜的层迁移,增塑化聚乙烯醇缩醛树脂层中所含的增塑剂量与聚乙烯醇缩醛树脂薄膜的层中所含的增塑剂量成为同等程度。本发明中,该平均增塑剂量优选18~35质量%、更优选20~30质量%、特别优选25~29质量%。平均增塑剂量如果处于前述范围内,则容易得到例如可以缓和碰撞时的对乘车人物的头部的冲击等的、夹层玻璃的期望的特性。通过调整增塑化聚乙烯醇缩醛树脂层中所含的增塑剂的量、增塑化聚乙烯醇缩醛树脂层的厚度、聚乙烯醇缩醛树脂薄膜中所含的增塑剂的量、和聚乙烯醇缩醛树脂薄膜的厚度,从而平均增塑剂量可以调整为前述范围内。
实施例
以下,根据实施例和比较例,对本发明具体地进行说明,但本发明不限定于这些实施例。需要说明的是,以下的实施例中,“%”只要没有特别限定就是指“质量%”。
(1)聚乙烯醇缩醛树脂材料
将各实施例和比较例中使用的聚乙烯醇缩醛树脂的组成和物性示于表1。
[表1]
表1中记载的聚乙烯醇缩醛树脂A和B的粘度依据以下的方法而测定。
在甲苯/乙醇=1/1的混合溶液中以成为浓度10质量%的方式分别加入并溶解聚乙烯醇缩醛树脂A和B。使用Brookfield型(B型)粘度计,在20℃、30rpm下测定得到的溶液的粘度。
[实施例1]
将表1中记载的聚乙烯醇缩醛树脂A和B以表2所示的质量比共混,得到聚乙烯醇缩醛树脂材料。通过与上述聚乙烯醇缩醛树脂A和B的粘度同样的方法测定得到的聚乙烯醇缩醛树脂材料的、浓度10质量%的甲苯/乙醇=1/1(质量比)溶液的粘度。另外,依据下述的方法测定峰顶分子量和分子量分布并算出。
<聚乙烯醇缩醛树脂材料的峰顶分子量和分子量分布的测定>
通过GPC分析用于构成得到的聚乙烯醇缩醛树脂薄膜的树脂。GPC分析中,使用Viscotek制GPCmaxTDA305和RI检测器作为分析装置,作为柱,使用连接有Shodex制GPC KF-806L和GPC KF-806L 2根、另行在前端连接有作为保护柱的Shodex制KF-G的柱,使用THF溶剂和标准聚苯乙烯(Agilent Technologies公司制Easical GPC/SEC CalibrationStandards PS-1),作为解析软件,使用OmniSE、C4.7。在40℃、注入量100μL下进行测定,求出前述树脂的峰顶分子量和分子量分布。将结果示于表2。
将共混聚乙烯醇缩醛树脂A和B得到的聚乙烯醇缩醛树脂材料进行熔融混炼以股线状挤出并粒料化。使用单螺杆挤出机和T模头,将得到的粒料在230℃下熔融挤出。使用金属弹性辊和金属镜面辊进行制膜,得到厚度45μm的聚乙烯醇缩醛树脂薄膜1(以下,有时简称为“树脂薄膜1”)。
(2)聚乙烯醇缩醛树脂薄膜的物性/特性的评价
依据以下的方法测定得到的聚乙烯醇缩醛树脂薄膜的表面物性。
<十点平均粗糙度的平均值Rz的测定和标准偏差的算出>
树脂薄膜1的十点平均粗糙度使用Mitutoyo Co.,Ltd.制Surf test SJ-310(测定力:0.75mN、尖笔形状:前端半径2μmR/前端角度60°),依据JIS B0601-1994而测定。
具体而言,对于树脂薄膜1的任意的面、任意部位,测定第1次的十点平均粗糙度。在距离其测定处5cm的部位,测定第2次的十点平均粗糙度使得测定方向与第1次的测定成为平行。接着,在距离第2次的测定处5cm、且与第1次的测定处朝向相反地偏离的部位,测定第3次的十点平均粗糙度使得测定方向与第2次的测定成为平行。同样地测定第4次、第5次的十点平均粗糙度,求出它们的平均值和标准偏差。同样地,在树脂薄膜1的另一个面测定十点平均粗糙度,求出它们的平均值、标准偏差。
将算出的2个十点平均粗糙度的平均值中、大的一者作为Rz1(a),将该面的十点平均粗糙度的标准偏差作为SD1,算出SD1除以Rz1(a)而得到的值。另外,将十点平均粗糙度的平均值小的一者作为Rz2(a),将该面的十点平均粗糙度的标准偏差作为SD2,算出SD2除以Rz2(a)而得到的值。将Rz1(a)、Rz2(a)、SD1/Rz1(a)和SD2/Rz2(a)分别示于表2。
<加热后的树脂薄膜的十点平均粗糙度的平均值Rz的测定和标准偏差的算出>
将切成30cm×30cm的树脂薄膜1放置于平的PET片上,用带固定其4个角。将该PET片放入加热至50℃的恒温槽中,放置30分钟后,从恒温槽取出。用与上述同样的方法测定十点平均粗糙度,将热处理前的十点平均粗糙度的平均值为Rz1(a)的一面的十点平均粗糙度的平均值作为Rz1(b)、标准偏差作为SD3、热处理前的十点平均粗糙度的平均值为Rz2(a)的面的十点平均粗糙度的平均值作为Rz2(b)、标准偏差作为SD4。将Rz1(b)、Rz2(b)、SD3/Rz1(b)、SD4/Rz2(b)、Rz1(a)/Rz1(b)和Rz2(a)/Rz2(b)分别示于表2。
[实施例2]
不使用聚乙烯醇缩醛树脂B作为聚乙烯醇缩醛树脂,除此之外,与实施例1同样地制膜,得到聚乙烯醇缩醛树脂薄膜2。对于得到的树脂薄膜2,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[实施例3]
相对于聚乙烯醇缩醛树脂总计100质量份,添加作为增塑剂的三甘醇二2-乙基己酸酯7.5质量份(PVB树脂与增塑剂的总计量的7%),除此之外,与实施例1同样地制膜,得到聚乙烯醇缩醛树脂薄膜3。对于得到的树脂薄膜3,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[实施例4~6]
使片的厚度分别为22μm、120μm和240μm,除此之外,与实施例1同样地制膜,分别得到聚乙烯醇缩醛树脂薄膜4、5和6。对于得到的树脂薄膜4~6,分别通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[实施例7]
将金属弹性辊变更为橡胶弹性辊,除此之外,与实施例1同样地制膜,得到聚乙烯醇缩醛树脂薄膜7。对于得到的树脂薄膜7,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[实施例8]
将金属弹性辊变更为压花1辊,除此之外,与实施例1同样地制膜,得到聚乙烯醇缩醛树脂薄膜8。对于得到的树脂薄膜8,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
需要说明的是,实施例8~10和比较例2~5中使用的压花1辊~压花6辊分别为表面凹凸的平均值和波动不同的压花辊。
[实施例9]
将金属弹性辊变更为压花2辊,除此之外,与实施例1同样地制膜,得到聚乙烯醇缩醛树脂薄膜9。对于得到的树脂薄膜9,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[实施例10]
将金属镜面辊变更为压花3辊,除此之外,与实施例9同样地制膜,得到聚乙烯醇缩醛树脂薄膜10。对于得到的树脂薄膜10,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[实施例11]
相对于聚乙烯醇缩醛树脂总计100质量份,添加作为增塑剂的三甘醇二2-乙基己酸酯8.7质量份(PVB树脂与增塑剂的总计量的8%),除此之外,与实施例2同样地制膜,得到聚乙烯醇缩醛树脂薄膜11。对于得到的树脂薄膜11,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[比较例1]
将金属弹性辊变更为金属镜面辊,除此之外,与实施例1同样地制膜,得到比较聚乙烯醇缩醛树脂薄膜1。对于得到的比较树脂薄膜1,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[比较例2]
将金属弹性辊和金属镜面辊这两者变更为压花2辊,除此之外,与实施例1同样地制膜,得到比较聚乙烯醇缩醛树脂薄膜2。对于得到的比较树脂薄膜2,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[比较例3]
将金属弹性辊变更为压花4辊,除此之外,与实施例1同样地制膜,得到比较聚乙烯醇缩醛树脂薄膜3。对于得到的比较树脂薄膜3,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[比较例4]
将金属弹性辊变更为压花5辊,除此之外,与实施例1同样地制膜,得到比较聚乙烯醇缩醛树脂薄膜4。对于得到的比较树脂薄膜4,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[比较例5]
将金属镜面辊变更为压花6辊,除此之外,与比较例3同样地制膜,得到比较聚乙烯醇缩醛树脂薄膜5。对于得到的比较树脂薄膜5,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[比较例6]
将金属弹性辊变更为橡胶弹性辊,将金属镜面辊变更为橡胶弹性辊,除此之外,与实施例1同样地制膜,得到比较树脂薄膜6。对于得到的比较树脂薄膜6,通过与实施例1同样的方法,测定各表面的物性。将结果示于表2。
[表2]
(3)聚乙烯醇缩醛树脂薄膜卷的特性评价
依据以下的方法评价将上述实施例1~11和比较例1~6的聚乙烯醇缩醛树脂薄膜卷绕为卷状时(层叠时)的自粘合性、以及实施例1~11的聚乙烯醇缩醛树脂薄膜的卷中的灰尘的附着性和去除性。
<自粘合性的评价>
制作将10m的树脂薄膜以具有Rz1(a)的十点平均粗糙度的平均值的面成为内侧的方式、以张力50N缠绕于外径6英寸的芯材的卷。将得到的卷以50℃保持6小时后,在23℃50%RH下静置24小时。从前述卷将树脂薄膜卷出10转,将卷出的部分切断、废弃后,从残留的卷切出长10cm×宽3cm的试验片(树脂薄膜重叠2张的层叠体),用手剥离,从而评价自粘合性。评价基准如下述。将结果示于表3。
A:未自粘合
B:自粘合、但用手能剥离
C:自粘合,用手无法剥离,或剥离时可见树脂薄膜的变形、断裂
<树脂薄膜卷中的灰尘附着性和灰尘去除性的评价>
制作将10m的树脂薄膜以具有Rz1(a)的十点平均粗糙度的平均值的面成为内侧的方式、以张力50N缠绕于外径6英寸的芯材的卷(卷A)。另外,制作将10m的树脂薄膜以具有Rz1(a)的十点平均粗糙度的平均值的面成为外侧的方式、以张力50N缠绕于外径6英寸的芯材的卷(卷B)。
(灰尘附着性)
将卷A和卷B分别在JIS B9920(2002)中规定的清洁度等级为6等级的房间中保管24小时。取样存在于保管后的卷的最外侧部分的树脂薄膜,用手振荡样品后,用扫描型电子显微镜拍摄将其表面(卷中为外侧的面)的任意5处的1mm×1mm见方的区域纵横分别放大至100倍的照片。计数各照片中能以目视确认的灰尘的数量,求出5处的平均值(平均值1)。评价基准如下述。将结果示于表3。
A:平均值1低于2个
B:平均值1为2个以上且低于5个
C:平均值1为5个以上
(灰尘去除性)
另外,取样存在于前述保管后的卷的最外侧的树脂薄膜,用手振荡样品后,进一步吹气,用扫描型电子显微镜拍摄将其表面(卷中为外侧的面)的任意5处的1mm×1mm见方的区域纵横分别放大至100倍的照片。计数各照片中能以目视确认的灰尘的数量,求出5处的平均值(平均值2)。评价基准如下述。将结果示于表3。
A:平均值2除以平均值1而得到的值低于0.2
B:平均值2除以平均值1而得到的值为0.2以上且低于0.5
C:平均值2除以平均值1而得到的值为0.5以上
[表3]
本发明的实施例1~11的聚乙烯醇缩醛树脂薄膜中,以卷状卷绕并保管时的自粘合抑制效果优异。另一方面,不满足本发明的限定的比较例1~6的聚乙烯醇缩醛树脂薄膜中,确认了保管时的自粘合抑制效果均差。
Claims (10)
1.一种聚乙烯醇缩醛树脂薄膜,其由聚乙烯醇缩醛树脂材料构成,所述聚乙烯醇缩醛树脂薄膜的厚度为5~350μm,将一个面与另一个面相比,将表面较粗糙的面A的十点平均粗糙度的平均值设为Rz1(a)μm、较平滑的面B的十点平均粗糙度的平均值设为Rz2(a)μm时,满足式(1)和式(2):
Rz1(a)>1.1×Rz2(a) (1)
3>Rz2(a) (2),
且面A的十点平均粗糙度的标准偏差除以Rz1(a)而得到的值和面B的十点平均粗糙度的标准偏差除以Rz2(a)而得到的值分别为0~0.30,
所述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇的质量比=1/1的溶液的粘度为100~1000mPa·s,聚乙烯醇缩醛树脂薄膜中的增塑剂的量基于聚乙烯醇缩醛树脂薄膜的总质量为0~20质量%。
2.根据权利要求1所述的聚乙烯醇缩醛树脂薄膜,其进一步满足式(3):
Rz1(a)<5 (3)。
3.根据权利要求1或2所述的聚乙烯醇缩醛树脂薄膜,其中,将以50℃保持了30分钟后的、面A的十点平均粗糙度的平均值设为Rz1(b)μm、面B的十点平均粗糙度的平均值设为Rz2(b)μm时,满足式(4)、式(5)和式(6):
0.7×Rz1(a)≤Rz1(b)≤1.3×Rz1(a) (4)
0.7×Rz2(a)≤Rz2(b)≤1.3×Rz2(a) (5)
Rz1(b)>Rz2(b) (6)。
4.根据权利要求1或2所述的聚乙烯醇缩醛树脂薄膜,其中,所述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇的质量比=1/1的溶液的粘度为300mPa·s以下。
5.根据权利要求1或2所述的聚乙烯醇缩醛树脂薄膜,其中,所述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的、使用Brookfield型粘度计以20℃、30rpm测得的、浓度10质量%的甲苯/乙醇的质量比=1/1的溶液的粘度大于200mPa·s。
6.根据权利要求1或2所述的聚乙烯醇缩醛树脂薄膜,其中,所述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂的分子量分布为2.7以上。
7.根据权利要求1或2所述的聚乙烯醇缩醛树脂薄膜,其中,所述聚乙烯醇缩醛树脂材料中的聚乙烯醇缩醛树脂为粘均聚合度不同的至少2种聚乙烯醇缩醛树脂的混合物、或粘均聚合度不同的至少2种聚乙烯醇系树脂的混合物的缩醛化物。
8.一种聚乙烯醇缩醛树脂薄膜卷,其是以权利要求1~7中任一项所述的聚乙烯醇缩醛树脂薄膜的面A侧成为内侧的方式进行卷绕而成的。
9.一种聚乙烯醇缩醛树脂薄膜卷,其是以权利要求1~7中任一项所述的聚乙烯醇缩醛树脂薄膜的面A侧成为外侧的方式进行卷绕而成的。
10.一种聚乙烯醇缩醛树脂薄膜卷的保管方法,其包括如下步骤:将权利要求8或9所述的聚乙烯醇缩醛树脂薄膜卷在-20℃~60℃的温度下进行保管。
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