CN104812578A - 复合体 - Google Patents

复合体 Download PDF

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Publication number
CN104812578A
CN104812578A CN201380057121.3A CN201380057121A CN104812578A CN 104812578 A CN104812578 A CN 104812578A CN 201380057121 A CN201380057121 A CN 201380057121A CN 104812578 A CN104812578 A CN 104812578A
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weight
complex
tfe
cotton cloth
silica
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CN104812578B (zh
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田村成教
山口雄斗
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CHUKI CHEMICAL INDUSTRIES Co Ltd
Chukoh Chemical Industries Ltd
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CHUKI CHEMICAL INDUSTRIES Co Ltd
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    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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    • D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
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    • B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
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  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

复合体1包括基材2和形成在基材2上的透光性树脂层3。基材2包括织布4、和形成在织布4上的含有四氟乙烯树脂以及二氧化硅的组合物层5。

Description

复合体
技术领域
本发明涉及一种复合体。
背景技术
作为具有高透光性的复合材料，在织布或无纺布上层叠了树脂膜的片用于广泛的领域。织布或无纺布使用由玻璃等构成的纤维，为了保持形状而实施各种填缝处理。在该处理中，广泛使用热塑性树脂。此外，在建筑用途中所使用的层叠片中，作为树脂膜广泛使用耐候性、耐污染性、耐水性等优良的氟树脂膜。
例如，专利文献1中记载了层叠了由用粘合剂粘合的玻璃纤维构成的织布或无纺布和含氟树脂膜的层叠片，粘合剂使用所谓的熔融型氟树脂。
但是，以往的层叠片在对弯折应力的强度、树脂层之间的粘合性、处理上存在问题。
现有技术文献
专利文献
专利文献1：WO2008/105298A1国际公开公报
发明的概要
发明所要解决的技术问题
本发明所要解決的技术问题是提供一种对弯折应力的强度、树脂层之间的粘合性、处理上优良的复合体。
解决技术问题所采用的技术方案
本发明的复合体是包括基材和形成在上述基材上的透光性树脂层的复合体，其中，上述基材包括织布、和形成在上述织布上的含有四氟乙烯树脂以及二氧化硅的组合物层。
发明的效果
本发明可提供一种对弯折应力的强度、树脂层之间的粘合性、处理上优良的复合体。
附图说明
图1是表示实施方式的复合体的剖视图。
图2是表示实施例以及比较例的复合体的弯折次数和拉伸断裂强度保持率的关系的图。
具体实施方式
以下，对本发明的实施方式进行详细说明。
复合体包括基材和形成在基材上的透光性树脂层。基材包括织布、和形成在织布上的含有四氟乙烯树脂以及二氧化硅的组合物层。如果采用这样的复合体，则可提高基材的柔软性。因此，即使在进行曲率半径小的弯折加工的情况下，也可减少组合物层由于弯曲(kink)而导致产生裂纹的情况。其结果是，由于能够缓和对构成织布的纤维的应力集中，因此可推迟反复施加弯曲应力的情况下的单纤维的强度下降。因此，如果采用实施方式的复合体，则可提高对弯折应力的强度。
此外，组合物层中含有的二氧化硅可提高组合物层和透光性树脂层的粘合性。
而且，在提高复合体的对弯折应力的强度以及树脂层间的粘合性之外，还改善了柔软性。因此，复合体容易操作、搬运、施行，处理性也优良。
与此相对，如果用熔融型氟树脂层代替含有四氟乙烯树脂以及二氧化硅的组合物层来形成织布，则基材变得具有刚性。因而，在进行曲率半径小的弯折加工、或反复施加弯曲应力的情况下，熔融型氟树脂层由于弯曲而树脂层本身产生裂纹。此外，还由于构成织布的单纤维上应力被集中，发生单纤维的强度下降和断裂。
以下，对实施方式的复合体的基材以及透光性树脂层进行说明。
构成基材的织布例如由通过单纤维束构成的线形成。单纤维的材质例如可例举选自玻璃、芳香族聚酰胺、碳以及氧化铝的至少1种。所使用的纤维的种类可以是1种或2种以上。优选含有玻璃纤维的纤维。
对单纤维的线径，理想的是设在3μm以上9μm以下的范围。此外，对由单纤维束构成的线，理想的是设在10特克斯(tex)以上300特克斯以下的范围。藉此，可进一步提高织布的柔软性和强度。
织布的纺织组织可以是平织、斜纹织、缎纹织(日文：朱子織)、纱罗织(日文：からみ織)、或模纱织(日文：摸紗織)。
织布的纺织组织的开口率用以下的方法进行测定。将长100mm、宽100mm的尺寸的织布(用四氟乙烯树脂被覆的状态的织布)作为样品，用显微镜(型号VHX-1000的株式会社基恩士公司(株式会社キーエンス)制或与其具有相同性能的显微镜)测定样品的开口部分面积，由以下算式算出。
X＝(S1/S2)×100
其中，X为织布开口率(％)，S1为织布开口部分面积(mm2)，S2为织布面积(mm2)。
织布开口率理想的是设在10％以上30％以下的范围。通过设置在该范围内，可得到具有所希望的透光率的复合体。透光率用以JIS R 3106为基准的方法进行测定。
复合体的透光率理想的是设在30％以上、95％以下。藉此，可得到所希望的复合体强度和最适于空间的亮度。进一步优选的范围是50％以上90％以下。
形成在织布上的组合物层含有四氟乙烯树脂以及二氧化硅。四氟乙烯树脂的粒子可分散在组合物层的一部分或整体中，但考虑到复合体的对弯折应力的强度，理想的是被覆织布。另一方面，二氧化硅的粒子可分散在组合物层的一部分或整体中，但考虑到树脂层间的粘合，理想的是在组合物层的表面上露出，与透光性树脂层接触。
组合物层中，可根据需要添加熔融流动性氟树脂。熔融流动性氟树脂可进一步提高组合物层和透光性树脂层的熔接性。熔融流动性氟树脂的粒子可分散在组合物层的一部分或整体中。具体而言，熔融流动性氟树脂的粒子可保持在织布中，或存在于组合物层的表面上。
四氟乙烯树脂在组合物层中作为四氟乙烯树脂粒子的烧结体存在。四氟乙烯树脂粒子理想的是平均一次粒径在0.02μm以上0.5μm以下的范围内。更优选的范围为0.1μm以上0.3μm以下。
基材重量中的四氟乙烯树脂重量％理想的是在5重量％以上40重量％以下的范围内。这基于以下理由。通过将四氟乙烯树脂重量％设为5重量％以上，能够抑制由于施行时的外部应力等而导致的构成基材的织布的变形。但是，如果四氟乙烯树脂量变多，则在不能确保与透光性树脂层的充分熔接性的同时，产品成本本身也变高。熔接性下降的问题在用后述的方法制作复合体的情况下容易产生。在后述的方法中，在织布上形成四氟乙烯树脂层后，将该织布含浸在使二氧化硅粒子混合在熔融流动性氟树脂粒子的水系分散液中而成的分散液中。如果四氟乙烯树脂量变多，则由于该分散液而成的层难以在四氟乙烯树脂表面形成，而不能确保与透光性树脂层的足够的熔接性。此外，如果四氟乙烯树脂量变多，则由于产品重量增加，需要将建筑物设为高强度而建筑成本变高。因此，四氟乙烯树脂重量％理想的是设在40重量％以下。更优选的范围是10重量％以上25重量％以下。
二氧化硅(SiO2)优选非晶质二氧化硅。非晶质二氧化硅更优选亲水性非晶质二氧化硅。
二氧化硅的粒子根据Brunauer、Emmett、Teller(BET)的吸附等温式的比表面积优选10m2/g以上。通过将比表面积设为10m2/g以上，可提高透光性树脂层和组合物层的密合性。更优选的范围为50m2/g以上400m2/g以下。
二氧化硅的粒子优选平均一次粒径为5nm以上80nm以下的范围。更优选的范围是7nm以上40nm以下。
四氟乙烯树脂粒子、二氧化硅粒子的平均一次粒径能够通过透射型电子显微镜进行测定。
组合物层重量中的二氧化硅重量％优选0.5重量％以上30重量％以下的范围。通过将二氧化硅重量％设为0.5重量％以上，可提高透光性树脂层和组合物层的密合性。二氧化硅量多则透光性树脂层与组合物层的密合性变高，但基材的柔软性有可能变低。通过将二氧化硅重量％设为30重量％以下，能够在基材中得到优良的柔软性。更优选的范围是5重量％以上20重量％以下。
在熔融流动性氟树脂的例子中，包括四氟乙烯-乙烯共聚树脂(ETFE)、四氟乙烯全氟烷基乙烯基醚共聚树脂(PFA)、以及四氟乙烯-六氟丙烯共聚树脂(FEP)。使用的树脂的种类可以是1种或2种以上。
透光性树脂层理想的是含有熔融流动性氟树脂。在熔融流动性氟树脂的例子中，包括四氟乙烯-乙烯共聚树脂(ETFE)、四氟乙烯全氟烷基乙烯基醚共聚树脂(PFA)、以及四氟乙烯-六氟丙烯共聚树脂(FEP)、偏氟乙烯树脂(PVDF)。所使用的树脂的种类可以是1种或2种以上。
复合体理想的是拉伸断裂强度在300N/15mm以上，拉伸断裂伸长率在35％以下。拉伸断裂强度以及拉伸断裂伸长率可用以JIS L1096的条状法(日文：ストリップ法)为基准的方法(切割条(日文：カットストリップ)，拉伸速度；200mm/分钟，试验片宽；30mm)进行测定。
复合体例如用以下的方法进行制作。
通过使织布含浸在四氟乙烯树脂粒子的水系分散液(以下称第1分散液)的方式进行涂布，在100℃以上200℃以下进行干燥后，在气氛温度330℃以上400℃以下进行烧成。通过多次重复涂布、干燥以及烧成的一系列工序，在织布上形成四氟乙烯树脂层。接着，准备将二氧化硅粒子混合在熔融流动性氟树脂粒子的水系分散液中而成的分散液(以下称第2分散液)，通过使形成了四氟乙烯树脂层的织布含浸在分散液的方式进行涂布，在100℃以上200℃以下进行干燥后，在气氛温度330℃以上400℃以下进行烧成。通过多次重复涂布、干燥以及烧成的一系列工序，在织布上形成含有四氟乙烯树脂、熔融流动性氟树脂以及二氧化硅的组合物层，得到基材。在基材的两面上配置透光性树脂膜后，通过加热加压压接进行热压接后，通过冷却加压压接实施冷却，得到复合体。
另外，可以在第1分散液中添加熔融流动性氟树脂粒子。此外，上述的方法中，进行第1分散液的涂布、干燥以及烧成的一系列工序后，进行第2分散液的涂布、干燥以及烧成的一系列工序，但第1分散液的涂布、干燥以及烧成的一系列工序和第2分散液的涂布、干燥以及烧成的一系列工序也可以相互重复。
采用上述方法进行制作的情况下，通过将四氟乙烯树脂粒子的平均一次粒径设为0.02μm以上0.5μm以下的范围，可提高第1分散液中的四氟乙烯树脂粒子的分散性。此外，提高将二氧化硅粒子的平均一次粒径设为5nm以上80nm以下的范围，可提高第2分散液中的二氧化硅粒子的分散性。因此，通过重复分别将均匀分散了四氟乙烯树脂粒子的分散液、均匀分散了二氧化硅粒子的分散液涂布在织布，干燥，烧成的工序制得组合物层，因此可实现几乎原样维持了分散液中的四氟乙烯树脂粒子和二氧化硅粒子的分散性的组合物层。
复合体的一例的大致剖面示于图1。如图1所例示，复合体1具有基材2、和形成在基材2的两面上的透光性树脂层3。基材2具有织布4、和形成在织布4的两面上的组合物层5。组合物层5含有四氟乙烯树脂以及二氧化硅。图1中，为了说明各层是如何进行层叠的，在织布4和组合物层5和透光性树脂层3之间为了方便起见设置了界面6，但在上述制造方法中，由于通过重复第1、第2分散液的涂布、干燥以及烧成的工序来得到组合物层，因此在组合物层中、组合物层和织布之间都不存在明确的界面。
在复合体中，允许含有基材、透光性树脂层以外的层(例如，光扩散层、防污层)。
复合体的用途例如可例举大规模温室和中庭等的屋檐材料、运动设施的外壁、屋檐材料、中大型帐篷、农业用温室的被覆材料等膜结构物。
实施例
以下，对实施例进行说明。
(实施例)
对作为耐热性织布的厚度为580μm、370g/m2目、纺织组织为纱罗织(日文：絡み織)的玻璃纤维织物(日东纺织株式会社(日東紡績)制)，通过含浸由平均一次粒径为0.2μm的四氟乙烯树脂(PTFE)粒子成分为60重量％、非离子表面活性剂为6重量％以及水为34重量％构成的四氟乙烯树脂微粒子水系分散液(大金工业株式会社(ダイキン工業)制)进行涂布，在将气氛温度调整为100℃的密封炉中干燥5分钟，去除水分后，在将气氛温度调整至360℃的密封炉中烧成5分钟。通过多次重复该含浸、干燥以及烧成的一系列的工序，得到厚度50μm的四氟乙烯树脂层。被四氟乙烯树脂层所被覆的织布的开口率为60％。
接着，对1kg四氟乙烯-六氟丙烯共聚物树脂(FEP)粒子水系分散液(三井杜邦氟化学株式会社(三井デュポンフロロケミカル株式会社)制)混合搅拌0.1kg亲水性非晶质二氧化硅粒子(日本阿尔洛希尔株式会社(日本アエロジル)制，利用Brunauer、Emmett、Teller(BET)的吸附等温式而得的比表面积为50m2/g，平均一次粒径为30nm)，由此对四氟乙烯-六氟丙烯共聚物树脂粒子水系分散液进行了调整。通过使形成了四氟乙烯树脂层的玻璃纤维织物含浸在该分散液的方式进行涂布，在将气氛温度调整至100℃的密封炉钟干燥5分钟，去除水分后，在将气氛温度调整至360℃的密封炉中烧成5分钟。通过多次重复该含浸、干燥以及烧成的一系列工序，在四氟乙烯树脂层上形成厚度为20μm的四氟乙烯-六氟丙烯共聚物树脂层，得到PTFE树脂量为85g/m2、FEP树脂量为30g/m2的组合物层。
在如上制作的基材的两面上分别以温度300℃、压力3.4kgf/cm2的条件将100μm的ETFE膜进行3分钟热压接。接着，通过在温度约25℃、压力1kgf/cm2下进行20秒钟的冷却压接，使ETFE膜熔接在基材上，得到实施例的复合体。
在实施例的复合体中，基材重量中的四氟乙烯树脂的重量％为17.5重量％，组合物层重量中的亲水性非晶质二氧化硅的重量％为3.9重量％，基材重量中的四氟乙烯-六氟丙烯共聚物的重量％为6.2重量％。
(比较例)
对与实施例相同的玻璃纤维织物(日东纺织株式会社制)，通过使其含浸在四氟乙烯-六氟丙烯共聚物粒子成分为60重量％的四氟乙烯-六氟丙烯共聚物树脂粒子水系分散液(三井杜邦氟化学株式会社制)进行涂布，在将气氛温度调整为100℃的密封炉中干燥5分钟，去除水分后，在将气氛温度调整至360℃的密封炉中烧成5分钟。通过多次重复该含浸、干燥以及烧成的一系列的工序，得到厚度为50μm的四氟乙烯-六氟丙烯共聚物树脂层。
在得到的纤维基布的两面上层叠100μm的ETFE膜，通过与实施例相同条件的热压接以及冷却压接使ETFE膜熔接在基材上，得到比较例的复合体。
对实施例以及比较例的复合体用以下的试验方法测定弯折次数和拉伸断裂强度的关系，其结果示于下述表1。
试验通过以(社团法人)日本膜结构协会实验法标准的膜材料的品质以及性能试验方法(MSAJ/M-03-2003)为基准的方法进行。即，使用MIT试验机，在荷重1kg/1.5cm、弯曲角175°、R＝1以及R＝3的条件下求出将试验片重复弯折规定次数时的拉伸断裂强度。弯折次数变化为100、200、500、1000次。拉伸断裂强度以JIS L1096的条状法为基准的方法(切割条，拉伸速度；200mm/分钟，试验片宽；30mm)进行测定。此外，将进行100、200、500、1000次弯曲后的拉伸断裂强度，以将进行弯曲前的试验片(弯折次数)的拉伸断裂强度表示为100％计而得的值作为断裂强度保持率。分别进行0、100、200、500、1000次弯曲后的拉伸断裂强度以及断裂强度保持率示于表1，分别进行0、100、200、500、1000次弯曲后的断裂强度保持率示于图2。
[表1]
由表1以及图2可知，实施例的复合体在R＝3的条件下重复弯曲试验片时的拉伸断裂强度保持率在弯折次数100、200、500、1000次中均高于比较例。此外，在弯折条件比R＝3更严苛的R＝1的情况下，弯折次数为100、200、500、1000次的各自拉伸断裂强度保持率也高于比较例。因此，实施例的复合体由于拉伸断裂强度优于比较例的复合体，是对弯折应力的强度、树脂层间的粘合性、处理上优良的复合体。
符号说明
1···复合体，2···基材，3···透光性树脂层，4···织布，5···组合物层，6···界面。

Claims (8)

1.一种复合体，它是包括基材和形成在所述基材上的透光性树脂层的复合体，其特征在于，所述基材包括织布、和形成在所述织布上的含有四氟乙烯树脂以及二氧化硅的组合物层。
2.如权利要求1所述的复合体，其特征在于，所述四氟乙烯树脂的平均一次粒径在0.02μm以上0.5μm以下的范围内。
3.如权利要求1或2所述的复合体，其特征在于，所述二氧化硅为亲水性非晶质二氧化硅。
4.如权利要求1～3中任一项所述的复合体，其特征在于，所述二氧化硅根据Brunauer、Emmett、Teller(BET)的吸附等温式的比表面积在10m2/g以上。
5.如权利要求1～4中任一项所述的复合体，其特征在于，所述二氧化硅的平均一次粒径在5nm以上80nm以下的范围内。
6.如权利要求1～5中任一项所述的复合体，其特征在于，所述基材的重量中的所述四氟乙烯树脂的重量％在5重量％以上40重量％以下的范围内。
7.如权利要求1～6中任一项所述的复合体，其特征在于，所述组合物的重量中的所述二氧化硅的重量％在0.5重量％以上30重量％以下的范围内。
8.如权利要求1～7中任一项所述的复合体，其特征在于，所述透光性树脂层含有选自四氟乙烯-乙烯共聚树脂、四氟乙烯全氟烷基乙烯基醚共聚树脂、四氟乙烯-六氟丙烯共聚树脂以及偏氟乙烯树脂的至少一种。
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