CN103648762A - 绝热叠层体 - Google Patents
绝热叠层体 Download PDFInfo
- Publication number
- CN103648762A CN103648762A CN201280033296.6A CN201280033296A CN103648762A CN 103648762 A CN103648762 A CN 103648762A CN 201280033296 A CN201280033296 A CN 201280033296A CN 103648762 A CN103648762 A CN 103648762A
- Authority
- CN
- China
- Prior art keywords
- layer
- laminated body
- adiabatic
- adiabatic laminated
- photocatalyst
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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Abstract
本发明提供一种高的绝热性和可视光透过率兼备,有防污性,且耐伤性优良的绝热叠层体。绝热叠层体,具有光触媒层4;二枚的透明基板1·1之间挟持由纤维集合体2以及无机粒子3形成的复合材料的透明绝热层10;以及粘着材料层5。光触媒层4为所述绝热叠层体的一个面的最外层,粘着材料层5为另一个面的最外层。光触媒层4和透明绝热层10之间以及透明绝热层10和粘着材料层5之间,至少一方可以具有硬涂布层。
Description
技术领域
本发明涉及在建筑物以及汽车的窗玻璃上贴合,在保持对可视光的透明性的同时,又可以带来绝热效果的绝热叠层体。
背景技术
为了在寒冷时对从窗的热损失进行防止的同时,在温暖时对从窗来的热的侵入进行防止,并且为了对视界进行确保,将多层玻璃,热线反射薄膜,透明绝热薄膜用于建筑物,车辆等的玻璃窗。为了节能而贴附于窗玻璃的透明绝热薄膜已经商品化。但是,现状是市售的透明绝热薄膜还没有达到用于宽敞的住宅,大楼,汽车等水平。
本来,透明性和绝热性能是两个相反的特性,所以,实际状况,是不可能有即保持必要的透明性即可视光透过率,又具有充分的绝热性能的窗用透明绝热薄膜。例如可以在汽车的窗上使用的市售的透明绝热薄膜,如确保可视光透过率为70%以上,绝热性能即使最高,太阳辐射屏蔽系数也就是0.7以上。如重视绝热性能,将太阳辐射屏蔽系数压在0.6附近的制品的可视光透过率达不到70%。
另外,所谓太阳辐射屏蔽系数,为表示对日照的屏蔽效果的指标。如将3mm厚的透明玻璃的太阳辐射屏蔽系数作为1,6mm厚透明玻璃在贴附薄膜的场合,进入室内的太阳照射量的比例就被称为薄膜的太阳辐射屏蔽系数。
透明绝热薄膜以外也有绝热叠层体,对此已有很多的建议。在专利文献1中,公开了一种其基本构造为具有氧化钛层/银层/氧化钛层3层构造的透明绝热叠层体。在专利文献2中,公开了一种在银层的前后设置镍层,使银层变薄,提高了透明层的构造。进一步,专利文献3中,公开了2层的银层被电介体氧化铟层挟持的氧化铟层/银层/氧化铟层/银层/氧化铟层的5层构造的透明绝热叠层体。专利文献4中,提示了作为光补赏层,代替以往的透明电介体层,使用从氧化铟锡(ITO)等的金属氧化物形成的透明导电层的透明绝热叠层体。
先行技术文献
专利文献
【专利文献1】米国专利第4337990号说明书
【专利文献2】米国专利第3682528号说明书
【专利文献3】日本专利第2901676号公报
【专利文献4】日本特开2006-334787号公报
所述的以往的透明绝热薄膜,或者绝热叠层体,没有能在必要的透明性被确保的同时,又得到由于所期望的由绝热效果而得来的节能。本发明,为兼备高的绝热性和可视光透过率,被赋予防污性,耐伤性优良的绝热叠层体。
发明内容
本发明的目的可以以下来达成:
1.一种绝热叠层体,其特征在于:包括光触媒层;2枚的透明基板之间挟有纤维集合体;以及由无机粒子形成的复合材料的透明绝热层以及粘着材料层,所述光触媒层为所述绝热叠层体的一个面的最外层,所述粘着材料层为另一个面的最外层。
2.上述1所述的绝热叠层体,在所述光触媒层和所述透明绝热层之间以及在所述透明绝热层和所述粘着材料层之间,至少一方具有硬涂布层。
3.上述1或者2的绝热叠层体,其特征在于:所述透明基板包括聚乙烯醇缩丁醛。
4.上述1或者2所述的绝热叠层体,其特征在于:所述纤维集合体的纤维径最大为700nm。
5.上述1或者2所述的绝热叠层体,其特征在于:所述纤维集合体,是由用电场纺丝法纺丝而形成的连续或者非连续的石英纤维形成的。
6.上述1或者2所述的绝热叠层体,其特征在于:所述无机粒子为硅胶中空粒子。
7.上述1或者2所述的绝热叠层体,其特征在于:所述光触媒层是用含有光触媒粒子和水溶性粘合剂的涂布液涂布而形成的。
8.上述7所述的绝热叠层体,其特征在于:所述光触媒粒子为,在具有n型半导体性的金属氧化物的结晶微粒子上,承载从由钒,锰,铁,钴,镍,铜,锌,铌,钼,钌,铑,银,锡,钨,铂,金形成的群选出的金属,金属的氧化物,或者/以及金属的化合物的光触媒粒子。
9.上述7所述的绝热叠层体,其特征在于:所述水溶性粘合剂含有水解性硅化合物,在水,碱性化合物以及极性溶媒的混合溶剂中水解了的化合物。
10.上述1或者2记载的绝热叠层体,其特征在于:所述粘着材料层是由硅酮类粘着材料形成的。
11.上述2所述的绝热叠层体,其特征在于:所述硬涂布层是由硅酮类硬涂布材料形成的。
12.上述11所述的绝热叠层体,其特征在于:所述硅酮类硬涂布材料为光固化性硅酮类硬涂布材料
13.一种绝热叠层体,其特征在于:上述1至12的任一项所述的绝热叠层体的全光透过率为60%以上。
14.一种透明绝热薄膜,其特征在于:具有上述1至13的任一项所述的绝热叠层体。
发明的效果
本发明的绝热叠层体为,在全光透过率高的同时,绝热性也优良。另外,由于最外层具有光触媒层,防污性也优良。另一个最外层设置粘着材料层,以便在窗等上容易贴附。进一步由于具有硬涂布层的构造,由此可以得到表面不易受伤的绝热叠层体,绝热薄膜。
另外,所谓全光线,包括可视光的波长范围。本发明的绝热叠层体的全光透过率高,意味著可视光线的透明性优良。
附图说明
【图1】适用本发明的绝热叠层体的一例的示意截面图。
【图2】适用本发明的绝热叠层体的另一例的示意截面图。
【图3】适用本发明的绝热叠层体的另一个例子的示意截面图。
【图4】适用本发明的绝热叠层体的另一个例子的示意截面图。
符号的说明
1:透明基板
2:纤维集合体
3:无机粒子
4:光触媒层
5:粘着材料层
6:硬涂布层
10:透明绝热层
具体实施方式
以下,对本发明的绝热叠层体,绝热薄膜,边列举实施方式边进行详细说明。但是,这些实施方式,仅为本发明的适宜的适用例,并不对本发明进行限定。另外,该说明书中所谓“树脂”,指高分子化合物。
本发明的第1实施方式的图1中,表示了透明绝热层10的一个面上叠层有光触媒层4,另一个面上,为粘着材料层5叠层的绝热叠层体。透明绝热层10为在2枚的透明基板1·1之间挟持有由纤维集合体2以及无机粒子3形成的复合材料而成。
本发明的第2个实施方式的图2中,表示了在透明绝热层10的两面有硬涂布层6·6叠层,进一步在其最外面叠层有光触媒层4,另一个的最外面叠层有粘着材料层5的叠层绝热叠层体。
本发明的第3的实施方式图3中,表示了在透明绝热层10的一个面上有硬涂布层6叠层,进一步其最表面有光触媒层4叠层,在透明绝热层10的另一个面有粘着材料层5叠层的绝热叠层体。
在本发明的第4实施方式的图4中,表示了在透明绝热层10的一个面上有硬涂布层6叠层,进一步其最表面有粘着材料层5叠层,透明绝热层10的另一个面有光触媒层4叠层的绝热叠层体。
(1:透明基板)
透明基板,对可视光(波长400~700nm)透明,可以耐受叠层的层的形成时的条件(溶媒,温度等),较佳为尺寸安定性优良之物。较佳的透明基板,可以为聚烯,丙烯酸树脂(含有聚甲基丙烯酸甲酯),聚酯树脂(含有聚对苯二甲酸乙二醇酯),聚碳酸酯树脂,聚酰亚胺树脂,乙烯-乙酸乙烯基酯共聚合体(EVA),聚乙烯醇缩丁醛(PVB),离子键聚合物树脂等。从透明性,耐久性等的观点,特别是聚乙烯基缩丁醛(PVB)为特佳。作为光学用途的聚乙烯醇缩丁醛(PVB)可以使用公知之物。
透明基板的聚乙烯醇缩丁醛(PVB)的基板,对制膜方法没有限定,以溶液刮刀涂布法为佳。用溶液刮刀涂布法将含有聚乙烯醇缩丁醛树脂的低粘度流体覆盖在PET薄膜等的基板上,在例如100℃烤箱中进行加热而进行薄膜状成形。低粘度流体由聚乙烯醇缩丁醛树脂和有机溶剂形成。有机溶剂,可以例举氯化溶媒(二氯甲烷以及1,2-二氯乙烷),醇(甲醇,乙醇,n-丙醇,异丙醇,n-丁醇,异丁醇,异戊醇),酮(丙酮,甲乙酮,甲基异丁基酮以及环己酮,二丙酮醇),酯(乙酸甲酯,乙酸乙酯,乙酸n-丙酯,乙酸异丙酯,乙酸异丁基酯以及乙酸n-丁基酯),芳香族化合物(甲苯以及二甲苯)以及醚(1,3-二氧戊环以及四氢呋喃)。聚乙烯基醇丁醛溶液与所述的溶媒进行混合调制即可。在聚乙烯醇缩丁醛形成中较佳的一次溶媒,可以例举甲乙酮,二氯甲烷,乙酸乙酯以及甲苯。
聚乙烯醇缩丁醛的基板的厚度,可以根据目的进行任意选择,作为绝热叠层体,或者透明绝热薄膜用途时,以150μm以上为佳。更佳为200μm以上。进一步在绝热叠层体的刚性有要求的使用方式中以250μm以上为佳。另外,绝热叠层体,或者透明绝热薄膜,比其他的层(硬涂布层,光触媒层,粘着材料层)的任一个层都要厚。
(2:纤维集合体)
透明绝热层中的纤维集合体的纤维径以700nm以下为佳。更佳为500nm以下,进一步较佳为400nm以下。如比700nm大,得到的透明绝热层变为不透明,有全光透过率变低的可能。纤维集合体的纤维长,从如过小,补强效果差的观点,较佳为5μm以上。没有特别的上限。
纤维集合体,可以采用各种的无纺布,或者纺织布。材料质,可以为石英纤维,玻璃纤维,或者可以确保透明性的聚丙烯酸酯纤维,聚苯乙烯纤维等,以石英纤维为较佳。
作为石英纤维的纺丝方法,没有特别的限制,可以使用电场纺丝法,蒸汽喷射法,APEX(注册商标)技术(PolymerGroup.Inc.)法等,这些之中,电场纺丝法可以得到均一的纤维,所以较佳。
电场纺丝法,作为用电力的纤维化方法是公知的。目标基板和喷口之间,以直流电源在原料侧为正,在目标侧为负施加直流电压,由此向着目标将原料材料放出,在目标上形成纤维的堆叠层。将原料从石墨等的导电性材料形成的喷口以一定速度运送,在火炎的中先端先溶融,软化。该喷口和不锈钢材料等的金属目标基板之间施加1kV~50kV的高压直流电压。从溶融的喷口先端以直径1μm以下的纳米纤维通过静电力堆积在金属目标基板上,纳米纤维的外径可以通过玻璃材料的运送速度,火炎温度,施加电压等的调整来进行控制。金属目标基板为圆筒状一边回转,一边以在回转轴方向上进行往复移动的方法或者,在XY台子上进行二维移动,从而使形成的纤维以平面状进行堆积,形成纤维集合体的堆叠层(石英纤维层)。纤维集合体堆积中或者其后,进行桨纱材料涂布,来维持强度。另外,可以通过添加粘合剂来进行强化,通过该过程,纤维径为数十~数百纳米程度的均一形成的纤维堆叠层(石英纤维层)在为目标基板上形成。
为了用静电纺丝得到玻璃纤维,将由直径为0.1~2mm的玻璃柱或者玻璃纤维形成的玻璃材料的先端从变为电极的喷口送出,被加热装置溶融,软化,在该喷口和目标基板之间施加高电压,用静电力使玻璃丝在基板上堆积。由此,形成石英纤维的无纺布。
作为该玻璃纤维的材料,可以例举电气用的低碱玻璃的E玻璃,低电介率玻璃的D玻璃等的配线基板用的玻璃以及石英玻璃。从光学的特性等的观点,以石英玻璃较佳。
(3:无机粒子)
纤维集合体,特别是在石英纤维,玻璃纤维中混合的无机粒子,以硅胶中空粒子适宜。硅胶中空粒子的制造方法没有限定,以以下的方法较佳。
在75容量%以上的水中,将胶体状碳酸钙,烷氧硅,以及碱触媒投入混合,在胶体状碳酸钙表面,由烷氧硅的加水分解反应生成的硅胶析出。其后,用酸处理,使硅胶层内部的碳酸钙溶解。其结果,可以制造具有约10nm至约300nm的范围的外径的硅胶中空粒子。
无机粒子的外径为,以约10nm至约300nm的范围为适宜。外径太小,制造困难,另外即使可以制造,也易于凝集。
无机粒子为硅胶中空粒子的场合,根据实验的结果,以30nm~130nm较佳,更佳为50nm~100nm,具有该外径的硅胶中空粒子最易于制造,难于凝集,可以使硅胶中空粒子的优点得以充分发挥。
对石英纤维的硅胶中空粒子的添加量,以对100质量份的石英纤维,添加1质量份以上100质量份以下为较佳,更佳为5质量份以上80质量份以下。如硅胶中空粒子的添加量在该范围中,透明绝热层的绝热性和光透过率的两方都好。如添加量为1质量份以下,不能充分得到透明绝热层的绝热性,如100质量份以上,在透明绝热层的光透过率不能充分得到的同时,层会变得非常脆弱。
(4:光触媒层)
本发明的绝热叠层体,作为绝热薄膜中的光触媒层,以将光触媒粒子和水溶性粘合剂形成的光触媒涂布液涂布,干燥固化而得到的光触媒膜为宜。可以给绝热叠层体,绝热薄膜带来防污效果。
作为光触媒粒子,可以使用现在市售的氧化钛类,氧化钨类,氧化锌类,氧化铌类等,n型半导体的金属氧化物的结晶微粒子。例如,可以使用锐钛型的二氧化钛(TiO2),金红石型的二氧化钛(TiO2),三氧化钨(WO3),氧化锌(ZnO),Ga搀杂氧化锌(GZO),氧化铌(Nb2O5)等。其中,作为可视光活性高之物,是在这些金属氧化物的结晶内将氮,硫黄,磷,碳等搀杂之物,或者在表面使铜,铁,镍,金,银,铂,碳等被承载之物加以适宜地使用。进一步详细地说,有承载铂的金红石型氧化钛,承载铁的金红石型氧化钛,承载铜的金红石型氧化钛,承载氢氧化铜的金红石型氧化钛,承载金的锐钛型氧化钛,承载铂的三氧化钨等。进一步,该微粒子的一次粒子径微细之物,即一次粒径为1~100nm的范围,较佳为1~50nm的范围之物可以适宜地使用。如一次粒径比100nm大,涂膜的透明度变低,有损外观。
这样,作为可视光活性高的光触媒微粒子,可能例举MPT-623(可视光响应光触媒,粉体状,承载铂的金红石型二氧化钛;石原产业公司制),MPT-625(可视光响应光触媒,粉体状,承载铁的金红石型二氧化钛;石原产业公司制)等。
光触媒涂布液的水溶性粘合剂可以在水,碱性化合物,以及极性溶媒中,使以下述式(1)表示的硅烷氧化合物,或者其缩合物进行加水分解的手法适宜地得到。
Si(OR)X(OH)4-X···(1)
式(1)中R,独立地为氢原子或者官能基。R可以相互同一或不同。作为官能基R,具体地说可以例举氢原子(H),甲基(CH3),乙基(CH2CH3),丙基(CH2CH2CH3),异丙基(CH2(CH3)CH3),丁基(CH2CH2CH2CH3),烷氧硅基(Si(OCH2CH2)3)等。
这些之中,以四甲氧基硅烷(上述R全为甲基),四乙氧基硅烷(上述R全为乙基)为特佳。
作为在光触媒涂布液的水溶性粘合剂中含有的,硅氧烷化合物的加水分解中使用的碱性化合物,由下述式(2)表示。
RX-NH4-X···(2)
式(2)中R独立表示氢原子或者官能基。R可以相互同一或不同。作为官能基R的具体例子,可以例举氢原子(H),甲基(CH3),乙基(CH2CH3),丙基(CH2CH2CH3),异丙基(CH2(CH3)CH3),丁基(CH2CH2CH2CH3),甲醇基(CH2OH),乙醇基(CH2CH2OH)。另外,可以为被氢原子以外的官能基取代的,下述式(3)表示的季胺的方式。
R4N+X-···(3)
也可以为以式(3)表示的X-的阴离子的盐类。具体地说,作为X可以为羟基(OH),卤素(F,Cl,Br,I)等。这些之中,四甲铵羟化物可以适宜地使用。
作为水溶性粘合剂的一部分,可以在与硅化合物,碱性化合物一同供给反应的极性溶媒,可以例举水,醇类(例如,甲醇,乙醇,异丙醇),多元醇类(例如,甘油,甲基溶纤剂,乙基溶纤剂,丙基溶纤剂,或者这些的乙酸酯类),酮类(例如,丙酮,二丙酮醇,乙酰丙酮,甲乙酮)。上述极性溶媒,可以1种单独或者2种以上并用。在它们之中,丙酮适宜使用。
硅化合物,碱性化合物,极性溶媒,水混合·搅拌,使得到的生成物在水或者醇中溶解,以酸添加或者离子交换使pH=5~8,将此作为粘合剂液使用,进行硅烷氧化合物的加水分解。
光触媒涂布液为,由光触媒粒子分散,并且在上述条件下调制的加水分解硅酸酯溶解或者分散而得到。预先调制在溶媒中使光触媒粒子分散的光触媒分散液,混合搅拌而得到。这样的光触媒涂布液,具体地说有信越化学工业公司制TA-801-G,TA-802-G,TA-803-G等。
光触媒涂布液中的光触媒固体成分浓度为0.01~10质量%,较佳为0.1~5质量%。光触媒固体成分浓度如比0.01质量%少,光触媒的防污活性变低,如比10质量%多,透明性变低,有损外观。另外,涂布液中的光触媒和加水分解硅酸酯的固体成分浓度为,光触媒固体成分质量与硅酸酯固体成分质量比,为0.05:99.5~99.5:0.05,较佳为5:95~95:5。如光触媒质量比为5少,不能得到充分的由亲水基.氧化分解而形成的防污活性,另外如比95多,膜的强度变低,会发生剥离,断裂。
光触媒涂布液涂布的基材,只要薄膜可以形成,就没有特别的限制。将光触媒涂布液在基材上涂布时,可以使用以往公知的方法来进行涂布。具体可以例举浸渍涂布法,旋涂布法,喷雾涂布法,毛刷涂布法,浸入涂布法,辊涂布法,线涂布法,模具涂布法,凹板印刷涂布法,喷墨法等。用此可以在基材上形成涂膜。
形成的涂膜的膜厚,以1~500nm,特别是,以50~300nm的范围为较佳。膜厚过薄,强度低,另外过厚,有发生断裂的场合。
将光触媒涂布液进行涂布,使涂膜干燥固化时,以在50~200℃的温度范围进行1~120分处理为较佳,特别是,以60~110℃的温度范围进行5~60分处理为较佳。
(5:粘着材料层)
作为绝热叠层体,绝热薄膜中的粘着材料层,以硅酮粘着材料层为适宜。作为硅酮粘着材料,可以使用一般使用的加热固化型的链状的有机聚硅氧烷和,固体状的硅酮树脂形成的粘着材料。作为加热固化型的硅酮粘着材料,有有机过氧化物固化型和铂附加固化型,但是,作为基材使用拉伸性的聚乙烯薄膜,聚丙烯薄膜的场合,由于会发生热变形,所以以使用在比较低的温度固化的铂附加固化型的硅酮粘着材料为特佳。
有机过氧化物固化型的硅酮粘着材料包括,链状的有机聚硅氧烷以及由(R3SiO1/2)单位和(SiO2)单位(R为取代或者非取代的一价烃基)形成的有机聚硅氧烷共聚合体树脂((R3SiO1/2)单位与(SiO2)单位之比为0.5~1.5)的有机聚硅氧烷混合物,以及含有作为交联固化剂的苯甲酰过氧化物,双(4-甲苯甲酰)过氧化物,2,5-二甲基-2,5-双(t-丁基过氧)己烷等的有机过氧化物。铂附加固化型的硅酮粘着材料包括链状的含乙烯基的有机聚硅氧烷,所述有机聚硅氧烷共聚合体树脂,以及含有作为交联固化剂的硅键合氢原子的有机氢聚硅氧烷,作为触媒的氯化铂酸,醇改性氯化铂酸,铂的烯配位体,铂与乙烯基聚硅氧烷的配位体等的铂族金属类触媒之物。
作为这样的硅酮类粘着材料,可以例举信越化学工业制X-40-3270/CAT-PL-50T=100/0.5,X-40-3229/CAT-PL-50T=100/0.5,X-40-3323/CAT-PL-50T=100/0.25等。
硅酮粘着材料层的厚度,以5~100μm为较佳,更佳为10~50μm。作为固化条件,通常为80~150℃。
(6:硬涂布层)
作为硬涂布层,以硅酮类硬涂布材料为较佳。硅酮类硬涂布层,没有特别的限制,光固化性硬涂布材料从作业性的观点来看,是适宜的。由含有光反应性基的硅氧烷化合物,(甲基)丙烯酸基含有化合物,自由基类光聚合引发剂形成。具体地说,可以例举信越化学工业公司的KP-1001,X-12-2437等。将该涂布液在聚乙烯醇缩丁醛树脂形成的绝热叠层体,绝热薄膜上涂布,用UV灯照射固化,得到硬涂布层。
硬涂布层的形成方法没有特别的限制,可以根据目的从公知的涂布机中进行适宜选择涂布即可。例如,可以例举逆转辊涂布机,线棍涂布机,帘式涂布机。形成的覆盖膜的膜厚为0.1~50μm,特别是以0.5~30μm的范围为较佳。膜厚过薄,耐摩耗性变低,另外过厚,耐破裂性变低。
作为使硬涂布层固化的光源,通常,使用含有200~450nm的波长的光的光源,例如高压水银灯,超高压水银灯,金属卤化物灯,氙灯,碳弧灯等。照射量没有特别的限制,为10~5,000mJ/cm2,特别是以20~2,000mJ/cm2为较佳。固化时间,通常为0.5秒~2分,较佳为1秒~1分。
本发明的绝热叠层体,绝热薄膜,在不要求耐伤性的场合,没有硬涂布层也可以。本发明的第2实施方式的图2中的绝热叠层体,绝热薄膜,没有硬涂布层。
绝热叠层体,绝热薄膜可以进一步含有添加剂。添加剂可以含在构成绝热叠层体,绝热薄膜的任何层中。进一步可以设另一个层,使添加剂含在该层中。另外,添加剂在多个的层含有也可以。其中,以在透明基板聚乙烯醇缩丁醛树脂中含有为较佳。通过在比其他的层要厚的聚乙烯醇缩丁醛树脂中含有,即使添加剂浓度低,也可以得到充分的效果。例如作为添加剂,使用下述的那样紫外线吸收剂的场合,通过使紫外线吸收剂含在聚乙烯醇缩丁醛树脂中,即使紫外线吸收剂的浓度低,也可以得到充分的紫外线吸收效果。
作为第1添加剂,紫外线吸收剂,可以例举共同药品制Visorb110,Ciba Specialty Chemicals公司制Tinuvin328,BASF制Uvinul Aplus等。作为第2添加剂,有可以防止由光以及热产生的氧化的氧化防止剂以及HALS(位阻胺光安定剂,HinderdAmine LightStabilizer)。第1添加剂和第2添加剂可以被含在相互不同的层中,也可以含在同一层中。
实施例
以下,例举实施例进行具体的说明,但是些实施例并不对本发名进行限制。可以在在本发明的精神下进行适宜的变更,这都包括在本发明的范围内。
另外,在实施例中采用的测定·评价方法如下。另外,实施例中“份”在没有特别说明的场合,是指“质量份”,「%」在没有特别的声明时,是指“质量%”。
1.热传导率的测定
是按JISR2618记载的非固定热丝法(探针法),用热传导测定计(QTM-500:京都电子工业公司)对热传导率进行测定。测定,在向尺寸为100×50×1mm的绝热叠层体试样持续施加一定电力的同时,对加热器的温度上升进行记录,从其温度倾斜度测定试样的热传导率。
2.透过光的扩散度的测定
用自动变角光度计(GP-200:村上色彩研究所制)进行测定。求取在透过测定方式,光线入射角:60°,受光角度:-90°~90°,灵敏度:150,HIGHVOLTON:500,过滤器:ND10使用,光圈:10.5mm(VS-13.0),受光光圈:9.1mm(VS-34.0)以及变角间隔0.1度的条件下测定透过峰的上升开始角度到下降终了角度的角度宽(度)以及峰高。角度宽为扩散度,峰高为透过度。
3.全光线透过率
用日本电色工业公司制雾度测定器「NDH-2000」,按JISK7105-1981进行测定。该全光线透过率与可视光透过率大略一致。
4.薄膜外观
对薄膜的表面进行目视观察,对是否有蜿蜒状模样等的外观不良进行判定。没有该外观不良的为良,有该外观不良者为不良。
5.平均纤维径,平均粒子径
用扫描型电子显微镜(日立制作所制,商品名:S-4700II),对得到的石英纤维,硅胶中空粒子的表面进行摄影,得到照片。从照片任选20个地方,对直径进行测定。求取所有的测定结果(n=20)的平均值,作为石英纤维,硅胶中空粒子的平均纤维径(直径),平均粒子径。
6.防污性的确认
防污性的确认为,用10μmol/L的甲基蓝水溶液,在5cm×5cm的扩散薄膜上展开1mL,用LED的光,以在试样表面的光量为10,000勒克司的光量进行3时间照射,青色消色的为好(用○表示),无变化的为不好(用×表示)。
(实施例1)
透明基板的制作
向聚乙烯醇缩丁醛树脂(积水化学公司制,S-LECSV-05)100重量份中加入二氯甲烷500重量份溶解。得到的树脂溶液用间隙尺寸1mm的涂布机(横山制作所公司制,刮刀涂布机)进行,在厚度100μm的聚酯薄膜上以溶液刮刀涂布法成膜,100℃,20分干燥,得到厚度200μm的透明绝热层用的透明基板。
石英纤维集合体的制作
将直径0.3mm的石英玻璃纤维用输送辊向石墨制喷口供给,从与该运送方向垂直的方向由氢氧火炎将先端溶融,软化。在与其相对的150mm的位置上设置可以XY2方向移动的装置,使不锈钢基板被保持。该喷口和不锈钢基板之间施加20kV的高压直流电压,从溶融的玻璃先端将直径约300nm的石英纤维用静电力在不锈钢基板上堆积。
硅胶中空粒子的制作
使结晶成长,使碳酸钙的外径成为8nm~85nm,老化脱水。制成干燥状态的固体微粉末状的碳酸钙微粒子后,在乙醇中分散。然后,通过添加硅氧烷以及铵,用溶胶凝胶法在碳酸钙(CaCO3)微粒子上进行硅胶(SiO2)涂布。作为硅氧烷,使用四乙氧基硅烷(TEOS)(信越化学工业公司制,KBE-04),作为铵,使用28重量%的氨水。
将如此制作的硅胶涂布粒子洗净后,在水中分散,添加盐酸使内部的碳酸钙溶解流出,形成有流出孔的立方体状的硅胶中空粒子。最后,干燥后,在加热工程中400℃加热,溶解的碳酸钙堵塞流出孔,由此制得硅胶中空粒子。该硅胶中空粒子的粒子径为80nm。
透明绝热层的作成
上述石英纤维集合体100重量份与上述硅胶中空粒子10重量份混合。将其用厚度200μm的所述聚乙烯醇缩丁醛基板2枚进行挟持,100℃,10分钟加热,得到透明绝热层。
绝热叠层体的作成
在透明绝热层的一个面上用线棍法将光触媒粒子在溶媒中分散,并且将含有水溶性硅酸酯粘合剂的光触媒涂布液(信越化学工业公司制,TA-801-G)涂布,100℃的烤箱中30分热处理,得到厚度200nm的光触媒层。在透明绝热层的另一个面上,用线棍法将硅酮类粘着材料(信越化学工业公司制,X-40-3270/CAT-PL-50T=100/0.5)涂布,130℃的烤箱中2分热处理,得到厚度30μm的粘着材料层。
如此得到的实施例1的绝热叠层体的测定值,特性列于表1。
(实施例2)
代替实施例1的石英纤维集合体的制作中的石英玻璃纤维,使用由高硼硅酸玻璃得到的直径约300nm的玻璃纤维,除此之外,进行与实施例1同样的操作,得到绝热叠层体。
该实施例2的绝热叠层体的测定值,特性表示于表1。
(实施例3)
在实施例1中制作的透明绝热层的两面上,用线棍法将光固化型硅酮类硬涂布材料(信越化学工业公司,KP-1001)涂布,用高压水银灯,375nm的波长的光进行1200mJ/cm2,1分照射,得到厚度3μm的硬涂布层。在一个硬涂布层的面上用线棍法将具有在溶媒中分散的光触媒粒子,并且含有水溶性硅酸基粘合剂的光触媒涂布液(信越化学工业公司制,TA-801-G)涂布。在100℃的烤箱中进行30分热处理,得到厚度200nm的光触媒层。另一个硬涂布层的面上,用线棍法将硅酮类粘着材料(信越化学工业公司制,X-40-3270/CAT-PL-50T=100/0.5)涂布,在130℃的烤箱中进行2分热处理,得到厚度30μm的粘着材料层。
如此得到的实施例3的绝热叠层体的测定值,特性列于表1。
(比较例1)
除了将硅胶中空粒子,变为气相二氧化硅(日本AEROSIL公司制,AEROSILRY50:一次粒子径40nm)以外,以与实施例1同样的方法得到透明绝热层。该透明绝热层与实施例1同样,形成光触媒层以及粘着材料层,得到比较例1的绝热叠层体。该比较例1的绝热叠层体的特性列于表1。
(比较例2)
除了将石英纤维集合体的直径变为800nm以外,与实施例1同样得到透明绝热层。从该透明绝热层与实施例1同样,形成光触媒层以及粘着材料层,得到比较例2的绝热叠层体。该比较例2的绝热叠层体的特性表示于表1。
(比较例3)
在相当于透明基板的厚度200μm的聚乙烯醇缩丁醛薄膜的一个面上,将由聚苯乙烯类聚合物珠形成的微粒子层进行涂布叠层,得到比较例3的绝热叠层体。该比较例3的绝热叠层体的特性列于表1。
(比较例4)
在相当于透明基板的厚度200μm的聚乙烯醇缩丁醛薄膜的一个面上将由丙烯酸类树脂形成的微粒子层进行涂布叠层,而得到比较例4的绝热叠层体。该比较例4的绝热叠层体的特性列于表1中。
表1
Claims (14)
1.一种绝热叠层体,其特征在于:包括光触媒层;2枚的透明基板之间挟有纤维集合体以及由无机粒子形成的复合材料的透明绝热层;以及粘着材料层,所述光触媒层为所述绝热叠层体的一个面的最外层,所述粘着材料层为另一个面的最外层。
2.权利要求1所述的绝热叠层体,在所述光触媒层和所述透明绝热层之间以及在所述透明绝热层和所述粘着材料层之间,至少一方具有硬涂布层。
3.权利要求1或者2的绝热叠层体,其特征在于:所述透明基板包括聚乙烯醇缩丁醛。
4.权利要求1或者2所述的绝热叠层体,其特征在于:所述纤维集合体的纤维径最大为700nm。
5.权利要求1或者2所述的绝热叠层体,其特征在于:所述纤维集合体,是由用电场纺丝法纺丝而形成的连续或者非连续的石英纤维形成的。
6.权利要求1或者2所述的绝热叠层体,其特征在于:所述无机粒子为硅胶中空粒子。
7.权利要求1或者2所述的绝热叠层体,其特征在于:所述光触媒层是用含有光触媒粒子和水溶性粘合剂的涂布液涂布而形成的。
8.权利要求7所述的绝热叠层体,其特征在于:所述光触媒粒子为,在具有n型半导体性的金属氧化物的结晶微粒子上,承载从由钒,锰,铁,钴,镍,铜,锌,铌,钼,钌,铑,银,锡,钨,铂,金形成的群选出的金属,金属的氧化物,或者/以及金属的化合物的光触媒粒子。
9.权利要求7所述的绝热叠层体,其特征在于:所述水溶性粘合剂为含有水解性硅化合物,在水,碱性化合物以及极性溶媒的混合溶剂中水解了的化合物。
10.权利要求1或者2所述的绝热叠层体,其特征在于:所述粘着材料层是由硅酮类粘着材料形成的。
11.权利要求2所述的绝热叠层体,其特征在于:所述硬涂布层是由硅酮类硬涂布材料形成的。
12.权利要求11所述的绝热叠层体,其特征在于:所述硅酮类硬涂布材料为光固化性硅酮类硬涂布材料
13.一种绝热叠层体,其特征在于:权利要求1至12的任一项所述的绝热叠层体的全光透过率为60%以上。
14.一种透明绝热薄膜,其特征在于:具有权利要求1至13的任一项所述的绝热叠层体。
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CN104805599A (zh) * | 2015-04-28 | 2015-07-29 | 武汉纺织大学 | 一种静电纺制备功能性乙烯基聚硅氧烷纳米纤维膜的方法 |
CN111954778A (zh) * | 2018-03-29 | 2020-11-17 | 大日本印刷株式会社 | 真空绝热材料用外包装材料、真空绝热材料和带有真空绝热材料的物品 |
CN110183107A (zh) * | 2019-05-30 | 2019-08-30 | 张学新 | 一种高硼硅耐热玻璃表面插丝的生产工艺 |
CN110183107B (zh) * | 2019-05-30 | 2021-10-01 | 张学新 | 一种高硼硅耐热玻璃表面插丝的生产工艺 |
Also Published As
Publication number | Publication date |
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JP5753453B2 (ja) | 2015-07-22 |
WO2013005711A1 (ja) | 2013-01-10 |
JP2013014108A (ja) | 2013-01-24 |
TW201315605A (zh) | 2013-04-16 |
US20140120794A1 (en) | 2014-05-01 |
TWI490123B (zh) | 2015-07-01 |
KR20140033464A (ko) | 2014-03-18 |
US9512953B2 (en) | 2016-12-06 |
CN103648762B (zh) | 2015-11-25 |
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