CN106660330B - 层叠体和轮胎 - Google Patents
层叠体和轮胎 Download PDFInfo
- Publication number
- CN106660330B CN106660330B CN201580032409.4A CN201580032409A CN106660330B CN 106660330 B CN106660330 B CN 106660330B CN 201580032409 A CN201580032409 A CN 201580032409A CN 106660330 B CN106660330 B CN 106660330B
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- CN
- China
- Prior art keywords
- laminated body
- rubber
- functional group
- modified polyvinylalcohol
- overlay film
- 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.)
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Abstract
本发明的目的是提供展示出优异的挠性和耐疲劳性同时具有高的耐臭氧龟裂性的层叠体。该层叠体的特征在于包括：包含接枝了分子量为20至10,000的直链状、脂环族、分枝状或芳族的官能团的改性聚乙烯醇的覆膜(12)；与所述覆膜(12)接触配设的橡胶层(11)。
Description
技术领域
本公开涉及层叠体和轮胎。
背景技术
臭氧龟裂(ozone cracking)是导致轮胎劣化的因素之一。臭氧龟裂是橡胶的主链由于空气中的臭氧而断裂且由此出现裂纹的现象。臭氧龟裂在如聚丁二烯、聚异戊二烯和苯乙烯-丁二烯等的二烯系聚合物中频繁发现。因为聚合物主链的断裂在产品中作为可见的裂纹出现，臭氧龟裂在轮胎耐久性方面是重大的问题。
传统上已开发了一些技术来保护橡胶表面不受到由臭氧导致的这样的劣化。例如，专利文献(PTL)1公开了一种组合物，其包含苯乙烯-聚丙烯酸酯共聚物作为主要组分并且进一步包含二氧化硅微粒。
然而，PTL 1中公开的组合物不具有充分的对臭氧气体的阻隔功能，并且当施加动态输入或伸长率为20％以上时不能抑制由臭氧气体导致的龟裂。
如聚酰胺树脂、纤维素系树脂、聚乙烯醇和乙烯-聚乙烯醇等具有氢键的阻隔性材料能够提供反映主链间分子间相互作用的强度的优异的气体阻隔性。
然而，这样的阻隔性树脂在用于各种工业产品时在挠性、耐疲劳性和对其它材料的粘接力方面不足。例如，在由例如轮胎代表的其中阻隔性材料在橡胶基材上经历很多循环变形的用途中，阻隔性材料的疲劳强度和阻隔性材料对橡胶的粘接力是有问题的。迄今已经试图改善这些性能。
作为改善阻隔性材料的挠性的技术，例如，PTL 1公开了一种多层结构体，其通过将由阻隔性材料制成的层和挠性的弹性体层交替层叠形成，以同时实现气体阻隔性和挠性。
作为用于改善阻隔性材料的粘接性的技术，例如，PTL 2公开了包含乙烯-乙烯醇共聚物、热塑性聚酯树脂、具有碳-碳双键的热塑性树脂和过渡金属盐来改善气体阻隔性和层间粘接性的树脂组合物。
引用列表
专利文献
PTL 1：JP H08-245852 A
PTL 2：JP 2013-71968 A
发明内容
发明要解决的问题
然而，PTL 2中的技术具有由于重复弯曲而强度下降的问题(差的耐疲劳性)，这是因为组合物中相分离的域(domains)之间的不足的界面强度。除此以外，对于作为轮胎部件的使用，期望挠性的进一步改善。
因此可有助于提供具有高的耐臭氧龟裂性(ozone crack resistance)且在挠性和耐疲劳性方面优异的层叠体，和使用该层叠体且由此具有优异的耐臭氧龟裂性、挠性、粘接性和耐疲劳性的轮胎。
用于解决问题的方案
作为对于包括橡胶层和覆膜的层叠体的深入研究的结果，我们发现以下情况：包含通过将作为接枝链的具有特定的结构和分子量的官能团接枝至具有优异的气体阻隔性的聚乙烯醇的主链获得的改性聚乙烯醇的覆膜具有如共混阻隔性树脂和合成橡胶的情况一样优异的挠性的效果。此外，因为阻隔性树脂与该官能团之间的键合通过接枝反应来形成，微域(microdomain)间的界面强度与共混体系相比更高，这有助于进一步改善耐疲劳性。
本公开基于这些发现。我们由此提供以下：
一种层叠体，其包括：包含由直链状、脂环族、分枝状或芳族的、分子量为20至10000的官能团接枝的改性聚乙烯醇的覆膜；和与所述覆膜接触配设的橡胶层。
这样的层叠体具有优异的耐臭氧龟裂性、挠性和耐疲劳性。
优选地，用于接枝改性的官能团的碳数为3至20。这确保更优异的挠性和耐疲劳性。
优选地，用于接枝改性的官能团的引入比例相对于改性聚乙烯醇的主链中的乙烯醇单元为0.5mol％至50mol％。这同时确保优异的耐臭氧龟裂性和优异的挠性和耐疲劳性。
优选地，改性聚乙烯醇进一步接枝有含丙烯酰基的低聚硅烷醇基，并且所述含丙烯酰基的低聚硅烷醇基的引入比例相对于改性聚乙烯醇的主链中的乙烯醇单元为0.5mol％至10mol％。这确保更优异的层间粘接性。
优选地，改性聚乙烯醇的主链的分子量为10000以上。这确保更优异的耐臭氧龟裂性。
优选地，所述层叠体进一步包括：在所述覆膜上方或下方的有色层。期望的设计特性可以以此方式来实现。
一种轮胎，其使用前述层叠体。
这样的轮胎具有优异的耐臭氧龟裂性、挠性和耐疲劳性。
发明的效果
由此可以提供具有高的耐臭氧龟裂性且在挠性和耐疲劳性方面优异的层叠体，和使用该层叠体且由此具有优异的耐臭氧龟裂性、挠性和耐疲劳性的轮胎。
附图说明
在附图中：
图1是示意性示出根据一个公开的实施方案的层叠体的结构的图。
具体实施方式
以下详细地描述公开的实施方案。
<层叠体>
如图1中示出的，层叠体10包括覆膜12和与该覆膜接触的橡胶层11。
(覆膜)
包括在根据本公开的层叠体中的覆膜包含由直链状、脂环族、分枝状或芳族的、分子量为20至10000的官能团接枝的改性聚乙烯醇。
这样的结构可以改善耐臭氧龟裂性、挠性和耐疲劳性。
构成改性聚乙烯醇的聚乙烯醇的主链与直链状、脂环族、分枝状或芳族的、分子量为20至10000的官能团(下文中酌情称为“官能团”或“根据本公开的官能团”)的一个或多个接枝链在堆积状态(bulk state)下不相容。因此，获得的改性聚乙烯醇形成了由聚乙烯醇和形成所述官能团的分子量为20至10000的直链状、脂环族、分枝状或芳族化合物所形成的微相分离结构(micro phase separation structure)。例如，在作为主链的树脂具有较高的体积分率的情况下，形成了其中树脂部分对应于海并且分子量为20至10000的化合物部分对应于岛的海-岛结构。在作为主链的树脂具有较低的体积分率的情况下，形成的海-岛结构与以上在主链具有较高的体积分率的情况下的海-岛结构相反。
在形成了前述微相分离结构的情况下，实现与将两种组分共混的情况相同的有利效果。具体地，气体阻隔性和耐臭氧龟裂性通过聚乙烯醇的效果来改善，并且挠性通过分子量为20至10000的化合物部分(根据本公开的官能团)的效果来改善。
此外，在获得的改性聚乙烯醇中，聚乙烯醇的主链和由根据本公开的官能团形成的接枝链化学地形成键，这有助于使微域间的界面强度比共混体系的高。因此，与例如聚乙烯醇树脂和弹性体材料的传统共混物相比，可以改善耐疲劳性。
根据本公开的官能团对聚乙烯醇的主链的接枝点(反应点)优选为末端部分。这可以维持或增加溶剂可溶性。例如，当在橡胶层上形成根据本公开的覆膜时，加工可以以涂料状态来进行。
为了改善挠性和耐疲劳性同时维持优异的耐臭氧龟裂性，用于接枝的官能团的引入比例相对于主链的乙烯醇单元优选为0.5mol％至50mol％。如果官能团的引入比例小于0.5mol％，则官能团的量不足，所以存在不能实现期望的挠性和耐疲劳性的可能性。如果官能团的引入比例大于50mol％，则源自聚乙烯醇的羟基的量不足，所以存在不能实现期望的耐臭氧龟裂性的可能性。
聚乙烯醇没有特别限制，并且可以为仅由乙烯醇单元构成的均聚物，或由乙烯醇和与乙烯醇可共聚的单体构成的共聚物(下文中也称为“PVA共聚物”)。可以使用单一种类的这些聚乙烯醇树脂，或可以以组合使用其两种以上。聚乙烯醇树脂的制造方法没有特别限制。例如，聚乙烯醇树脂可以通过将如聚乙酸乙烯酯等乙烯基酯聚合物皂化来获得。用于形成乙烯基酯单元的乙烯基酯单体的实例包括甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、戊酸乙烯酯、癸酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯、苯甲酸乙烯酯、新戊酸乙烯酯和叔碳酸乙烯酯(vinyl versatate)。其中，因为可以以良好的生产性获得PVA，乙酸乙烯酯是优选的。
PVA共聚物中可共聚的单体的实例包括：如乙烯、丙烯、1-丁烯、异丁烯和1-己烯等α-烯烃类；丙烯酸和其盐；如丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯和丙烯酸异丙酯等丙烯酸酯类；甲基丙烯酸和其盐；如甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丙酯和甲基丙烯酸异丙酯等甲基丙烯酸酯类；如丙烯酰胺、N-甲基丙烯酰胺和N-乙基丙烯酰胺等丙烯酰胺衍生物；如甲基丙烯酰胺、N-甲基甲基丙烯酰胺和N-乙基甲基丙烯酰胺等甲基丙烯酰胺衍生物；如甲基乙烯基醚、乙基乙烯基醚、正丙基乙烯基醚、异丙基乙烯基醚和正丁基乙烯基醚等乙烯基醚类；如乙二醇乙烯基醚、1,3-丙二醇乙烯基醚和1,4-丁二醇乙烯基醚等含羟基的乙烯基醚类；如乙酸烯丙酯、丙基烯丙基醚、丁基烯丙基醚和己基烯丙基醚等烯丙基醚类；具有如聚氧乙烯基、聚氧丙烯基和聚氧丁烯基等的氧化烯基的单体；如乙烯基三甲氧基硅烷等乙烯基硅烷类；如乙酸异丙烯酯、3-丁烯-1-醇、4-戊烯-1-醇、5-己烯-1-醇、7-辛烯-1-醇、9-癸烯-1-醇和3-甲基-3-丁烯-1-醇等含羟基的α-烯烃类，或其酯；如N-乙烯基甲酰胺、N-乙烯基乙酰胺和N-乙烯基吡咯烷酮等N-乙烯基酰胺类；具有来源自富马酸、马来酸、衣康酸、马来酸酐、邻苯二甲酸酐、偏苯三酸酐或衣康酸酐等的羧基的单体；具有来源自亚乙基二磺酸、烯丙基磺酸、甲代烯丙基磺酸和2-丙烯酰胺基-2-甲基丙烷磺酸等的磺酸基的单体；和具有来源自乙烯氧基乙基三甲基氯化铵、乙烯氧基丁基三甲基氯化铵、乙烯氧基乙基二甲基胺、乙烯氧基甲基二乙基胺、N-丙烯酰胺甲基三甲基氯化铵、N-丙烯酰胺乙基三甲基氯化铵、N-丙烯酰胺二甲基胺、烯丙基三甲基氯化铵、甲代烯丙基三甲基氯化铵、二甲基烯丙基胺或烯丙基乙基胺等的阳离子基团的单体。
这些可共聚的单体单元(下文中也称为“共聚用单体单元”)的含量在100mol％构成PVA共聚物的全部单体单元中优选为20mol％以下，更优选10mol％以下。为了展示出共聚的优势，共聚用单体单元的含量优选为0.01mol％以上。
聚乙烯醇可以完全皂化或部分皂化，即，部分皂化的聚乙烯醇树脂。鉴于色相、鱼眼的减少、由该组合物制成的成形品和膜的表面平滑性，皂化度优选为60mol％以上，更优选95mol％以上，进一步优选99mol％以上，并且特别优选99.5mol％以上。
聚乙烯醇的分子量优选为10000以上，并且更优选100000以上，从而在用作覆膜时确保强度和防止臭氧气体侵入。
在改性聚乙烯醇中的直链状、脂环族、分枝状或芳族的、分子量为20至10000的官能团在作为接枝链引入时将挠性和耐疲劳性赋予根据本公开的覆膜。
用于接枝的官能团的碳数优选为3至20，并且更优选4至18，从而赋予更优异的挠性和耐疲劳性。
具体地，官能团优选地包含丁基缩水甘油基、硬脂酰基、己酰基(caproyl group)、己酰基(hexanoyl group)、月桂基、棕榈基、异戊酰基和环己烷羰基。
改性聚乙烯醇可以进一步具有除了前述官能团(直链状、脂环族、分枝状或芳族的、分子量为20至10000的官能团)以外的接枝基团。
例如，优选进一步使含丙烯酰基的低聚硅烷醇基接枝至聚乙烯醇的主链上，以致含丙烯酰基的低聚硅烷醇基的引入比例相对于主链的乙烯醇单元为0.5mol％至10mol％，以进一步改善层间粘接性。
对于形成根据本公开的覆膜的改性聚乙烯醇，将直链状、脂环族、分枝状或芳族的、分子量为20至10000的官能团接枝至聚乙烯醇的主链上的接枝反应方法没有特别限制，并且可以是如酯化反应、环氧开环反应或酸酐反应等已知的有机化学反应。
作为接枝反应方法的实例，选择具有羧基的化合物作为接枝化合物，并且使用酯化剂来进行与主链的聚乙烯醇羟基的酯化反应。
包括在根据本公开的层叠体中的覆膜可以包含除了前述改性聚乙烯醇以外的各种填料。
例如，填料包括二氧化硅、炭黑和粘土。
这些填料中，二氧化硅是优选的，因为预期其改善加强效果。通过透射电子显微镜(TEM)测量的二氧化硅的平均一次粒径优选为30nm至120nm，并且更优选40nm至100nm。
炭黑也优选用作填料，因为其产生良好的加强作用。炭黑的种类的实例包括N660、N772、N762和N754。具有以下胶体特征的炭黑是更优选的：碘吸收量(IA)优选为40mg/g以下，并且更优选约35mg/g至20mg/g，并且邻苯二甲酸二丁酯吸油量(DBP)优选为100ml/100g以下，并且更优选在70ml/100g至30ml/100g的范围内。在该胶体特征中，根据ASTM D1510-95来测量IA，并且根据ASTM D2414-97来测量DBP。
(橡胶层)
包括在根据本公开的层叠体中的橡胶层是与覆膜接触的部件。
橡胶层优选地通过使用包含在主链中具有不饱和碳键的橡胶组分的橡胶组合物来形成，以确保对覆膜的密合性。
在主链中具有不饱和碳键的橡胶组分例如是天然橡胶或合成橡胶。合成橡胶的实例包括如合成聚异戊二烯橡胶、丁苯橡胶和聚丁二烯橡胶等二烯系橡胶，以及丁基系橡胶。可以使用单一种类的这些橡胶组分，或可以以组合使用其两种以上。
在形成橡胶层的橡胶组合物中，橡胶组分的15质量％以上优选为非二烯系橡胶。在橡胶组分的15质量％以上为非二烯系橡胶的情况下，显著改善橡胶层的耐候性。
在形成橡胶层的橡胶组合物中作为任选组分的防老剂的含量相对于100质量份橡胶组分(A)优选为0质量份至1.5质量份，并且更优选小于1.0质量份。如果防老剂的含量相对于100质量份橡胶组分(A)为大于1.5质量份，则防老剂向表面侧的移动增加，这会阻碍适合用于形成覆膜的紫外线固化型涂料的紫外线固化并且降低覆膜与橡胶层之间的密合性。如果防老剂的含量相对于100质量份橡胶组分(A)为小于1.0质量份，则特别良好地进行紫外线固化型涂料的紫外线固化，同时可以进一步改善覆膜与橡胶层之间的密合性。
防老剂的实例包括N-苯基-N’-(1,3-二甲基丁基)-对苯二胺(6PPD)、2,2,4-三甲基-1,2-二氢喹啉聚合物(TMDQ)、6-乙氧基-2,2,4-三甲基-1,2-二氢喹啉(AW)、N,N’-二苯基-对苯二胺(DPPD)、N,N’-二仲丁基-对苯二胺和N-苯基-N’-(甲基庚基)-对苯二胺。
除了前述橡胶组分和防老剂以外，在不妨碍本公开的目的的范围内，形成橡胶层的橡胶组合物可以酌情选择地包含典型地用于橡胶工业的配混剂，例如，如炭黑等填料、如硫磺等硫化剂、硫化促进剂、加工油、防焦烧剂、氧化锌和硬脂酸。市售品可以适当地用作这些配混剂。
橡胶组合物可以通过将橡胶组分与酌情选择的配混剂一起混炼、加温、挤出等来制造。
(有色层)
如图1中示出的，根据本公开的层叠体优选地进一步包括在覆膜12上方或下方(图1中为在覆膜12上方)的有色层13。层叠体可以由此提供有期望的装饰或可视性。
有色层没有特别限制，只要其能够着色即可。例如，有色层通过在作为基体的橡胶组分、多硫醇化合物、或UV-固化型墨等中包含任意的各种着色剂来形成。
着色剂可以是有机或无机颜料或染料。无机颜料例如是氧化钛。白色着色剂的实例包括氧化钛、锑白、硫化锌。红色着色剂的实例包括红色氧化铁、镉红、铅丹、硫化汞、镉、永固红4R、立索红、吡唑啉酮红、华琼红(watching red)、钙盐、色淀红D、亮胭脂红6B、曙红色淀、若丹明色淀B、茜素色淀、亮胭脂红3B、C.I.颜料红2。蓝色着色剂的实例包括C.I.颜料蓝15:3、C.I.颜料蓝15、普鲁士蓝、钴蓝、碱性蓝色淀、维多利亚蓝色淀、酞菁蓝、无金属酞菁蓝、部分氯化酞菁蓝、坚牢天蓝、阴丹士林蓝BC。黄色着色剂的实例包括铬黄、锌黄、镉黄、黄色氧化铁、矿物坚牢黄、镍钛黄、拿浦黄(navel yellow)、萘酚黄S、汉撒黄G、汉撒黄10G、联苯胺黄G、联苯胺黄GR、喹啉黄色淀、永固黄NCG、酒石黄色淀、C.I.颜料黄12。
(轮胎)
根据本公开的轮胎使用根据本公开的层叠体。
例如，在充气轮胎中，该层叠体可以用于胎侧部的表面部，所述充气轮胎包括：一对胎圈部；一对胎侧部；与两个胎侧部连续的胎面部；在埋设在各胎圈部中的胎圈芯之间环状延伸的胎体；以及在胎体的冠部的轮胎半径外侧配置的带束部。
根据本公开的轮胎可以不仅使用根据本公开的层叠体作为胎侧部，也使用其作为例如轮胎的气密层。
实施例
使用实施例在以下更详细地描述本公开的技术，然而本公开不限于这些实施例。
(实施例1至9)
将1g的PVA颗粒(Poval PVA117，Kuraray Co.,Ltd.制)在30mL的DMSO(二甲亚砜)中加热溶解。之后，以表1中示出的量(官能团化合物添加量(g))添加丁基缩水甘油醚，添加0.01g的三(五氟苯基)硼，并且将混合物在80℃下搅拌6小时。将反应溶液进行在500mL甲醇中的再沉淀和过滤两次，将固体回收并干燥，从而获得各实施例的改性聚乙烯醇的样品。改性聚乙烯醇的主链的分子量(×103)和改性聚乙烯醇的官能团引入率(mol％)也在表1中示出。
将改性聚乙烯醇的样品作为膜厚度为100μm的膜层叠在厚度为1mm的NR/BR硫化橡胶的表面上，从而制造各实施例的试验片。
实施例1至9中的形成硫化橡胶的橡胶组合物由以下组分制成：
天然橡胶：50质量份；
丁二烯橡胶：50质量份；
石蜡油(“A/O MIX”，JX Nippon Oil&Energy Corporation制)：3质量份；
炭黑(“Asahi NPG”，Asahi Carbon Co.,Ltd.制)：50质量份；
茴香胺(“RAC-23”，J&K Scientific Ltd.制，3-甲氧基苯胺)：3质量份；
硬脂酸(“MXST-L”，Miyoshi Oil&Fat Co.,Ltd.制)：2质量份；
氧化锌(“HakusuiTech”，Kyushu Hakusui Corporation制)：3质量份；
硫化促进剂(“Sanceler CM-G”，Sanshin Chemical Industry Co.,Ltd.制)：0.2质量份；和
不溶性硫磺(“Mu-cron OT-20”，Shikoku Chemicals Corporation制)：3质量份。
(实施例10)
将1g的PVA颗粒(Poval PVA117，Kuraray Co.,Ltd.制)在30mL的DMSO(二甲亚砜)中加热溶解。之后，以表1中示出的量(官能团化合物添加量(g))添加己酸，添加0.3g的1-乙基-3-(3-二甲基氨丙基)碳二亚胺盐酸盐，并且将混合物在40℃下搅拌6小时。将反应溶液进行在500mL甲醇中的再沉淀和过滤两次，将固体回收并干燥，从而获得实施例10的改性聚乙烯醇的样品。改性聚乙烯醇的主链的分子量(×103)和改性聚乙烯醇的官能团引入率(mol％)也在表1中示出。
将改性聚乙烯醇的样品作为膜厚度为100μm的膜层叠在厚度为1mm的NR/BR硫化橡胶的表面上，从而制造实施例10的试验片。形成硫化橡胶的橡胶组合物与用于实施例1至9的相同。
(比较例1和2)
对于比较例1，如表1中示出的，将聚苯乙烯-丙烯酸丁酯制备为样品。
对于比较例2，如表1中示出的，将PVA(“Poval PVA117”，Kuraray Co.,Ltd.制)制备为样品。
将改性聚乙烯醇的样品作为膜厚度为100μm的膜层叠在厚度为1mm的NR/BR硫化橡胶的表面上，从而制造各比较例的试验片。形成硫化橡胶的橡胶组合物与用于实施例1至9的相同。
(比较例3)
将1g的PVA颗粒(“Poval PVA117”，Kuraray Co.,Ltd.制)在30mL的DMSO(二甲亚砜)中加热溶解。之后，以表1中示出的量(官能团化合物添加量(g))添加丙酸，添加0.3g的1-乙基-3-(3-二甲基氨丙基)碳二亚胺盐酸盐，并且将混合物在40℃下搅拌6小时。将反应溶液进行在500mL甲醇中的再沉淀和过滤两次，将固体回收并干燥，从而获得比较例3的改性聚乙烯醇的样品。改性聚乙烯醇的主链的分子量(×103)和改性聚乙烯醇的官能团引入率(mol％)也在表1中示出。
将改性聚乙烯醇的样品作为膜厚度为100μm的膜层叠在厚度为1mm的NR/BR硫化橡胶的表面上，从而制造比较例3的试验片。形成硫化橡胶的橡胶组合物与用于实施例1至9的相同。
(比较例4)
将1g的PVA颗粒(Poval PVA117，Kuraray Co.,Ltd.制)在30mL的DMSO(二甲亚砜)中加热溶解。之后，以表1中示出的量(官能团化合物添加量(g))添加二十二烷酸，添加0.9g的1-乙基-3-(3-二甲基氨丙基)碳二亚胺盐酸盐，并且将混合物在40℃下搅拌6小时。将反应溶液进行在500mL甲醇中的再沉淀和过滤两次，将固体回收并干燥，从而获得比较例4的改性聚乙烯醇的样品。
二十二烷酸的添加量(g)、改性聚乙烯醇的主链的分子量(×103)和改性聚乙烯醇的官能团引入率(mol％)也在表1中示出。
(比较例5)
将由实施例1至9的改性聚乙烯醇制成的膜厚度为100μm的膜制造为比较例5的样品。
[表1]
(评价)
(1)气体阻隔性(透氧率)
将各实施例和比较例的样品加工为厚度为1.1mm且直径为50mm的圆盘形状，并且使用由Modern Controls,Inc.制造的OX-TRAN型号2/20在湿度0％和温度25℃的条件下测量氧透过度。测量结果在表3中示出。透氧率越低表示结果越好。
(2)挠性-1(断裂伸长率)
对于各实施例和比较例的样品，制造了厚度为1.1mm的试验片，并且基于JIS 7161测量断裂伸长率(Eb)。具体地，测量当将试验片以50mm/min的速度牵引时的断裂伸长率(％)。测量结果在表3中示出。断裂伸长率的值越高表示结果越好。
(3)挠性-2(拉伸强度)
对于各实施例和比较例的样品，制造了厚度为1.1mm的试验片，并且基于JIS K6251测量拉伸强度(Tb)。具体地，哑铃状试验片(No.3)使用拉伸试验装置以规定的速度(50±2.5mm/min)牵引至断裂，并且测量使试验片断裂所需要的最大张力。测量结果在表3中示出。拉伸强度的值越高表示结果越好。
(4)静态臭氧龟裂试验
将各实施例和比较例的样品在温度40℃和臭氧浓度50pphm的环境下以牵引25％的状态固定，并且目测检查在1天后、在2天后、和在3天后是否出现龟裂。结果(有无裂纹)在表3中示出。裂纹越少表示结果越好。
(5)动态臭氧龟裂试验
将各实施例和比较例的样品在温度40℃和臭氧浓度50pphm的环境下重复伸缩±10％(频率为1Hz)，并且目测检查在1天后、在2天后、和在3天后是否出现龟裂以及龟裂的状态。结果在表3中示出。裂纹越少表示结果越好。基于以下标准(表2)来评价龟裂的状态。
[表2]
(6)耐疲劳性(弯曲次数)
将各实施例和比较例的样品切割为21cm×30cm的50个膜，并且将各切割的膜在0℃下湿度控制7天。然后依照ASTM F392-74，使用由Rigaku Kogyo Co.,Ltd.制造的Gelvo型屈挠-龟裂试验机，将切割的膜弯曲50次、75次、100次、125次、150次、175次、200次、225次、250次、300次、400次、500次、600次、700次、800次、1000次和1500次，并且测量针孔数。对于各弯曲次数，进行5次测量，并且将其平均值设定为针孔数。在横轴表示弯曲次数(P)且纵轴表示针孔数(N)的情况下，绘制测量结果的图，并且当针孔数为1时的弯曲次数(Np1)通过外推来算出并且四舍五入为两个有效数字。对于在1500次弯曲后没有观察到针孔的各个膜，将弯曲次数随后以500次为单位地增加，并且将观察到针孔的弯曲次数设定为Np1。
基于比较例1的弯曲次数为100的指数进行评价。指数越高表示弯曲次数越多和耐疲劳性越高。
[表3]
从表3显示出以下情况。
对于气体阻隔性和挠性，比较例1中的聚苯乙烯-丙烯酸丁酯具有适当的挠性，但透氧率高，所以预期臭氧透过性高。比较例2至5和实施例1至10的样品全部示出高的氧气阻隔性，所以预期它们的臭氧透过性低。此外，实施例1至10的样品具有改善的断裂伸长率同时维持氧气阻隔性。这可能是因为，在侧链中引入的官能团起到使主链的氢键网络适当地(但没有显著地损害阻隔性)缓和的作用，从而增加韧性而没有脆性的断裂。另外，如从实施例6至9可见的，随着官能团的引入量增加，阻隔性下降。进一步，如从实施例4和10可见的，如果碳数(分子量)等同，则接枝的官能团的种类不显著影响结果。
在静态臭氧龟裂试验中，与比较例1中具有丙烯酸酯骨架的聚合物相比，PVA衍生物(比较例2至4和实施例1至10)示出高的耐龟裂性。另一方面，对于动态耐臭氧龟裂性，比较例2至4的样品龟裂。这可能是因为，由于比较例2至4的样品缺乏挠性，促进了微小的断裂在膜中出现和臭氧分子透过膜。与此同时，实施例1至10具有与静态臭氧龟裂试验中相同的结果。
对于耐疲劳性，实施例1至10的树脂组合物的样品具有与比较例2至5的样品相比更高的耐疲劳性，显示赋予了挠性而导致改善的耐疲劳性。
产业上的可利用性
由此可以提供具有高的耐臭氧龟裂性且在挠性和耐疲劳性方面优异的层叠体，和使用该层叠体且由此具有优异的耐臭氧龟裂性、挠性和耐疲劳性的轮胎。
Claims (5)
1.一种层叠体，其特征在于包括：
包含由直链状、脂环族、分枝状或芳族的、分子量为20至10000的官能团接枝的改性聚乙烯醇的覆膜；和
与所述覆膜接触配设的橡胶层，
其中所述改性聚乙烯醇的主链的分子量为10000以上，
其中所述改性聚乙烯醇进一步接枝有含丙烯酰基的低聚硅烷醇基，并且所述含丙烯酰基的低聚硅烷醇基的引入比例相对于所述改性聚乙烯醇的主链中的乙烯醇单元为0.5mol％至10mol％。
2.根据权利要求1所述的层叠体，
其中用于所述接枝改性的官能团的碳数为3至20。
3.根据权利要求1或2所述的层叠体，
其中用于所述接枝改性的官能团的引入比例相对于所述改性聚乙烯醇的主链中的乙烯醇单元为0.5mol％至50mol％。
4.根据权利要求1所述的层叠体，其进一步包括：
在所述覆膜上方或下方的有色层。
5.一种轮胎，其使用根据权利要求1至4任一项所述的层叠体。
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| JP6162920B2 (ja) * | 2011-05-31 | 2017-07-12 | 株式会社ブリヂストン | ランフラットタイヤ |
| JP5803329B2 (ja) * | 2011-06-27 | 2015-11-04 | 横浜ゴム株式会社 | ポリアミド系樹脂フィルムとゴムの積層体およびタイヤ |
| EP3159378B1 (en) * | 2014-06-17 | 2020-07-08 | Bridgestone Corporation | Modified polyvinyl alcohol resin composition, film, and tire |
-
2014
- 2014-06-17 JP JP2014124722A patent/JP6616063B2/ja not_active Expired - Fee Related
-
2015
- 2015-05-01 US US15/317,031 patent/US20170121477A1/en not_active Abandoned
- 2015-05-01 CN CN201580032409.4A patent/CN106660330B/zh active Active
- 2015-05-01 EP EP15809976.2A patent/EP3159160B1/en active Active
- 2015-05-01 WO PCT/JP2015/002309 patent/WO2015194085A1/ja active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007026935A1 (ja) * | 2005-08-31 | 2007-03-08 | Tohcello Co., Ltd. | ガスバリア性膜、ガスバリア性積層体及びその製造方法 |
| CN102712181A (zh) * | 2009-12-01 | 2012-10-03 | 可乐丽股份有限公司 | 充气轮胎用内衬及其制造方法 |
| WO2013001313A1 (en) * | 2011-06-29 | 2013-01-03 | Revolymer Limited | Vinyl alcohol polymers with silane side chains |
| CN106459422A (zh) * | 2014-06-12 | 2017-02-22 | 株式会社普利司通 | 接枝共聚物、树脂组合物、覆膜、层叠体和轮胎 |
Also Published As
| Publication number | Publication date |
|---|---|
| JP6616063B2 (ja) | 2019-12-04 |
| WO2015194085A1 (ja) | 2015-12-23 |
| EP3159160A1 (en) | 2017-04-26 |
| CN106660330A (zh) | 2017-05-10 |
| EP3159160B1 (en) | 2018-07-04 |
| JP2016002716A (ja) | 2016-01-12 |
| EP3159160A4 (en) | 2017-08-09 |
| US20170121477A1 (en) | 2017-05-04 |
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