CN111836853A - 丙烯腈-丁二烯橡胶组合物及包含该组合物层的层叠体 - Google Patents
丙烯腈-丁二烯橡胶组合物及包含该组合物层的层叠体 Download PDFInfo
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- CN111836853A CN111836853A CN201980017963.3A CN201980017963A CN111836853A CN 111836853 A CN111836853 A CN 111836853A CN 201980017963 A CN201980017963 A CN 201980017963A CN 111836853 A CN111836853 A CN 111836853A
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- vinyl acetate
- ethylene
- acetate copolymer
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- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
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Classifications
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Abstract
本发明的课题在于开发与乙烯‑乙酸乙烯酯共聚物皂化物层的粘接强度优异的NBR组合物、以及NBR层与乙烯‑乙酸乙烯酯共聚物皂化物层的粘接强度优异的层叠体;本发明涉及一种丙烯腈‑丁二烯橡胶组合物,其特征在于,包含丙烯腈‑丁二烯橡胶以及相对于该丙烯腈‑丁二烯橡胶100质量份为0~50质量份的硅烷改性乙烯‑乙酸乙烯酯共聚物;本发明还涉及一种层叠体,其特征在于,包含所述丙烯腈‑丁二烯橡胶组合物的丙烯腈‑丁二烯橡胶层与乙烯‑乙酸乙烯酯共聚物皂化物层隔着乙烯‑乙酸乙烯酯共聚物层而层叠。
Description
技术领域
本发明涉及与乙烯-乙酸乙烯酯共聚物皂化物层的粘接强度得到改善的丙烯腈-丁二烯橡胶(NBR)组合物以及该组合物层与乙烯-乙酸乙烯酯共聚物皂化物层的层叠体。
背景技术
在汽车、产业机械、建筑机械、摩托车、农业机械等中,安装有用于冷却发动机的散热器软管、散热器溢流箱用排水软管、室内取暖器用加热器软管、空调排水软管、刮水器送水软管、顶棚排水软管、保护软管等各种软管。这些软管使用了耐油性、耐热性、耐气体透过性良好的NBR。
然而,根据用途的不同,有时NBR单层的耐气体透过性不充分,因此例如,提出了将NBR层与阻气性更优异的乙烯-乙烯醇共聚物层进行层叠的方案(专利文献1)。
然而,尽管尝试了简单地将NBR层与乙烯-乙烯醇共聚物层层叠,但是可知粘接强度仍不充分。
现有技术文献
专利文献
专利文献1:日本特开2009-006575号公报
发明内容
发明所要解决的课题
本发明的课题在于开发与乙烯-乙酸乙烯酯共聚物皂化物层的粘接强度优异的NBR组合物、以及NBR层与乙烯-乙酸乙烯酯共聚物皂化物层的粘接强度优异的层叠体。
用于解决课题的方法
本发明涉及以下的[1]~[6]。
[1]一种丙烯腈-丁二烯橡胶组合物,其特征在于,包含丙烯腈-丁二烯橡胶、以及相对于该丙烯腈-丁二烯橡胶100质量份为0~50质量份的硅烷改性乙烯-乙酸乙烯酯共聚物。
[2]一种层叠体,其特征在于,包含项[1]所述的组合物的丙烯腈-丁二烯橡胶层与乙烯-乙酸乙烯酯共聚物皂化物层隔着乙烯-乙酸乙烯酯共聚物层而层叠。
[3]根据项[2]所述的层叠体,其特征在于,所述乙烯-乙酸乙烯酯共聚物层包含硅烷改性乙烯-乙酸乙烯酯共聚物。
[4]根据项[1]所述的丙烯腈-丁二烯橡胶组合物,其特征在于,包含丙烯腈-丁二烯橡胶、以及相对于该丙烯腈-丁二烯橡胶100质量份为2~50质量份的硅烷改性乙烯-乙酸乙烯酯共聚物。
[5]根据项[1]或项[4]所述的丙烯腈-丁二烯橡胶组合物,其特征在于,进一步包含1.7~20质量份的过氧化二枯基。
[6]一种层叠体,其特征在于,包含项[4]或项[5]所述的丙烯腈-丁二烯橡胶组合物的层与乙烯-乙酸乙烯酯共聚物皂化物层层叠。
发明的效果
本发明的包含硅烷改性乙烯-乙酸乙烯酯共聚物的丙烯腈-丁二烯橡胶组合物由于在与乙烯-乙酸乙烯酯共聚物皂化物层层叠的情况下的粘接强度优异,因此可以适合用于需要耐油性、耐热性、耐气体透过性的各种用途。
此外,在丙烯腈-丁二烯橡胶层与乙烯-乙酸乙烯酯共聚物皂化物层之间具有乙烯-乙酸乙烯酯共聚物层的层叠体的层间粘接强度优异,可以适合用于需要耐油性、耐热性、耐气体透过性的各种用途。
具体实施方式
《丙烯腈-丁二烯橡胶》
构成本发明的层叠体的丙烯腈-丁二烯橡胶(NBR)层(以下,有时简称为“NBR层”。)、以及构成丙烯腈-丁二烯橡胶组合物(以下,有时简称为“NBR组合物”。)的丙烯腈-丁二烯橡胶(NBR)为将丙烯腈与丁二烯进行乳液聚合而获得的二烯系合成橡胶。NBR通常根据丙烯腈的结合量而被分类成极高(43%以上)、高(36~42%)、中高(31~35%)、中(25~30%)、低(24%以下)这5个等级,中高为通用类型。
《硅烷改性乙烯-乙酸乙烯酯共聚物》
在本发明涉及的NBR中配合的硅烷改性乙烯-乙酸乙烯酯共聚物为将不饱和硅烷化合物与乙烯-乙酸乙烯酯共聚物进行接枝改性而得的改性共聚物。不饱和硅烷化合物的接枝量通常为0.01~5重量%,优选为0.02~3重量%。
本发明涉及的硅烷改性乙烯-乙酸乙烯酯共聚物的熔体流动速率(MFR)为按照JISK7210〔190℃、2.16kg载荷〕测定得到的值通常为1.6~6.4g/10分钟,优选处于1.6~4.6g/10分钟的范围内。
被硅烷改性的乙烯-乙酸乙烯酯共聚物中,共聚物中所存在的乙酸乙烯酯含量通常为5~50重量%,优选处于5~40重量%的范围内。
本发明涉及的乙烯-乙酸乙烯酯共聚物的熔体流动速率(MFR)按照JIS K7210〔190℃、2.16kg载荷〕测定得到的值通常为1.6~6.4g/10分钟,优选处于1.6~4.6g/10分钟的范围内。
将不饱和硅烷化合物对于乙烯-乙酸乙烯酯共聚物进行接枝改性的方法能够采用各种公知的改性方法,例如,能够在自由基引发剂的存在下或不存在的情况下进行接枝改性。此时,如果在自由基引发剂的存在下进行接枝改性,则能够将上述不饱和硅烷化合物效率良好地接枝改性。
作为这样的自由基引发剂,使用有机过氧化物、偶氮化合物等。作为这样的自由基引发剂,具体而言,可举出过氧化苯甲酰、过氧化二氯苯甲酰、过氧化二枯基、过氧化二叔丁基、2,5-二甲基-2,5-二(过氧化苯甲酸酯)己炔-3、1,4-双(叔丁基过氧化异丙基)苯、过氧化月桂酰、叔丁基过氧化乙酸酯、2,5-二甲基-2,5-二(叔丁基过氧化)己炔-3、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、叔丁基过氧化苯甲酸酯、叔丁基过氧化苯基乙酸酯、叔丁基过氧化异丁酸酯、叔丁基过氧化仲辛酸酯、叔丁基过氧化新戊酸酯、枯基过氧化新戊酸酯、叔丁基过氧化二乙基乙酸酯;偶氮二异丁腈、二甲基偶氮异丁酸酯等。
其中,优选使用过氧化二枯基、过氧化二叔丁基、2,5-二甲基-2,5-二(叔丁基过氧化)己炔-3、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、1,4-双(叔丁基过氧化异丙基)苯等二烷基过氧化物。
〈不饱和硅烷化合物〉
作为接枝于乙烯-乙酸乙烯酯共聚物的不饱和硅烷化合物,可举出各种公知的化合物,例如,乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基(β-甲氧基乙氧基)硅烷、乙烯基三乙酰氧基硅烷等乙烯基硅烷类、丙烯酰氧基丙基三甲氧基硅烷、甲基丙烯酰氧基丙基三甲氧基硅烷等丙烯酸系硅烷类等。
《NBR组合物》
本发明的NBR组合物为相对于上述NBR:100质量份,包含上述硅烷改性乙烯-乙酸乙烯酯共聚物0~50质量份、优选为2~50质量份、更优选为5~20质量份的组合物。
当本发明的NBR组合物中,除了上述硅烷改性乙烯-乙酸乙烯酯共聚物以外还包含过氧化二枯基1.7~20质量份、更优选为3.4~10.2质量份时,与由乙烯-乙酸乙烯酯共聚物皂化物形成的层的粘接强度进一步得以改善。
本发明涉及的NBR中,根据所期望的目的,除了上述硅烷改性乙烯-乙酸乙烯酯共聚物和过氧化二枯基以外,能够在不损害本发明的效果的范围内配合其它成分。作为其它成分,可以含有例如,选自填料、交联助剂、硫化促进剂、硫化助剂、软化剂、防老剂、加工助剂、活性剂、耐热稳定剂、耐候稳定剂、抗静电剂、着色剂、润滑剂、增稠剂、发泡剂和发泡助剂中的至少1种。此外,各个添加剂可以单独使用1种,也可以并用2种以上。
〈填料〉
在本发明涉及的NBR中配合的填料为与NBR配合的公知的橡胶增强剂,通常为炭黑、被称为无机增强剂的无机物。
作为本发明涉及的填料,具体而言,可举出旭#55G、旭#60G(以上为旭Carbon(株)制)、Seast(SRF、GPF、FEF、MAF、HAF、ISAF、SAF、FT、MT等)的炭黑(东海Carbon(株)制)、将这些炭黑用硅烷偶联剂等进行了表面处理而得到的产物、以及二氧化硅、活化碳酸钙、微粉滑石、微粉硅酸、轻质碳酸钙、重质碳酸钙、滑石、粘土等。
这些填料可以为单独的,也可以为两种以上的混合物。
作为本发明涉及的填料,优选使用亲水性二氧化硅、疏水性二氧化硅等二氧化硅、炭黑、轻质碳酸钙、重质碳酸钙、滑石、粘土等。
在本发明涉及的NBR包含填料的情况下,相对于上述NBR100质量份,通常以100~300质量份、优选以100~250质量份的范围进行配合即可。
〈交联助剂、硫化促进剂和硫化助剂〉
在使用过氧化二枯基作为交联剂的情况下,可以并用交联助剂。作为交联助剂,可举出例如,硫;对醌二肟等醌二肟系交联助剂;乙二醇二甲基丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯等丙烯酸系交联助剂;邻苯二甲酸二烯丙酯、异氰脲酸三烯丙酯等烯丙基系交联助剂;马来酰亚胺系交联助剂;二乙烯基苯;氧化锌(例如,ZnO#1·氧化锌2种(JIS标准(K-1410))、HakusuiTech(株)制)、氧化镁、锌白〔例如,“META-Z102”(商品名;井上石灰工业(株)制)等氧化锌〕、活性锌白等金属氧化物。
在使用交联助剂的情况下,NBR中的交联助剂的配合量相对于过氧化二枯基1摩尔,通常为0.5~10摩尔,优选为0.5~7摩尔,更优选为1~6摩尔。
作为本发明涉及的硫化促进剂,可举出例如,N-环己基-2-苯并噻唑亚磺酰胺、N-氧基二亚乙基-2-苯并噻唑亚磺酰胺、N,N’-二异丙基-2-苯并噻唑亚磺酰胺、2-巯基苯并噻唑(例如,Sanceler M(商品名;三新化学工业公司制))、2-(4-吗啉代二硫代)苯并噻唑(例如,Nocceler MDB-P(商品名;大内新兴化学工业公司制))、2-(2,4-二硝基苯基)巯基苯并噻唑、2-(2,6-二乙基-4-吗啉代硫代)苯并噻唑和二苯并噻唑基二硫化物(例如,SancelerDM(商品名;三新化学工业公司制))等噻唑系硫化促进剂;二苯基胍、三苯基胍和二邻甲苯基胍等胍系硫化促进剂;乙醛-苯胺缩合物和丁醛-苯胺缩合物等醛胺系硫化促进剂;2-巯基咪唑啉等咪唑啉系硫化促进剂;单硫化四甲基秋兰姆(例如,Sanceler TS(商品名;三新化学工业公司制))、二硫化四甲基秋兰姆(例如,Sanceler TT(商品名;三新化学工业公司制))、二硫化四乙基秋兰姆(例如,Sanceler TET(商品名;三新化学工业公司制))、二硫化四丁基秋兰姆(例如,Sanceler TBT(商品名;三新化学工业公司制))和四硫化双五亚甲基秋兰姆(例如,Sanceler TRA(商品名;三新化学工业公司制))等秋兰姆系硫化促进剂;二甲基二硫代氨基甲酸锌、二乙基二硫代氨基甲酸锌、二丁基二硫代氨基甲酸锌(例如,Sanceler PZ、Sanceler BZ和Sanceler EZ(商品名;三新化学工业公司制))和二乙基二硫代氨基甲酸碲等二硫代酸盐系硫化促进剂;亚乙基硫脲(例如,Sanceler BUR(商品名;三新化学工业公司制)、Sanceler 22-C(商品名;三新化学工业公司制))、N,N’-二乙基硫脲和N,N’-二丁基硫脲等硫代脲系硫化促进剂;二丁基黄原酸锌等黄原酸盐系硫化促进剂。
在使用硫化促进剂的情况下,NBR中的这些硫化促进剂的配合量相对于NBR100质量份,一般为0.1~20质量份,优选为0.2~15质量份,进一步优选为0.5~10质量份。如果硫化促进剂的配合量在上述范围内,则在所得的层叠体的表面上不会起霜,NBR显示优异的交联特性。在使用硫系化合物作为交联剂的情况下,能够并用硫化助剂。
作为本发明涉及的硫化助剂,可举出例如,氧化锌(例如,ZnO#1·氧化锌2种,HakusuiTech(株)制)、氧化镁、锌白(例如,“META-Z102”(商品名;井上石灰工业(株)制)等的氧化锌)。
在使用硫化助剂的情况下,NBR组合物中的硫化助剂的配合量相对于NBR100质量份,通常为1~20质量份。
〈软化剂〉
作为本发明涉及的软化剂,可举出例如,工艺油、润滑油、石蜡油、液体石蜡、石油沥青、凡士林等石油系软化剂;煤焦油等煤焦油系软化剂;蓖麻油、亚麻籽油、菜籽油、豆油、椰子油等脂肪油系软化剂;蜜蜡、巴西棕榈蜡等蜡类;环烷酸、松油、松香或其衍生物;萜烯树脂、石油树脂、香豆酮茚树脂等合成高分子物质;邻苯二甲酸二辛酯、己二酸二辛酯等酯系软化剂;以及微晶蜡、液态聚丁二烯、改性液态聚丁二烯、烃系合成润滑油、妥尔油、硫化油膏(油膏),其中,优选为石油系软化剂,特别优选为工艺油。
在本发明涉及的NBR含有软化剂的情况下,软化剂的配合量相对于NBR100质量份,一般为2~100质量份,优选为10~100质量份。
〈防老剂(稳定剂)〉
通过在本发明涉及的NBR中配合防老剂(稳定剂),从而能够延长由其形成的密封衬垫的寿命。作为这样的防老剂,有以往公知的防老剂,例如,胺系防老剂、酚系防老剂、硫系防老剂等。
作为本发明涉及的防老剂,例如,有苯基丁基胺、N,N-二-2-萘基-对苯二胺等芳香族仲胺系防老剂;二丁基羟基甲苯、四[亚甲基(3,5-二叔丁基-4-羟基)氢化肉桂酸酯]甲烷等酚系防老剂;双[2-甲基-4-(3-正烷基硫代丙酰氧基)-5-叔丁基苯基]硫醚等硫醚系防老剂;二丁基二硫代氨基甲酸镍等二硫代氨基甲酸盐系防老剂;2-巯基苯甲酰咪唑、2-巯基苯并咪唑、2-巯基苯并咪唑的锌盐、硫代二丙酸二月桂酯、硫代二丙酸二硬脂酯等硫系防老剂等。
在本发明涉及的NBR含有防老剂的情况下,防老剂的配合量相对于NBR100质量份,通常为0.3~10质量份,优选为0.5~7.0质量份。如果防老剂的配合量在上述范围内,则所得的层叠体的表面不会起霜,进一步能够抑制硫化阻碍的发生。
〈加工助剂〉
作为本发明涉及的加工助剂,一般而言,作为加工助剂,能够广泛使用橡胶中所配合的加工助剂。具体而言,可举出蓖麻油酸、硬脂酸、棕榈酸、月桂酸、硬脂酸钡、硬脂酸锌、硬脂酸钙、月桂酸锌或酯类等。其中,优选为硬脂酸。
在本发明涉及的NBR含有加工助剂的情况下,能够以相对于NBR100质量份,通常为1~3质量份的量来适当配合。如果加工助剂的配合量在上述范围内,则混炼加工性、挤出加工性、注射成型性等加工性优异,因此是适合的。
上述加工助剂可以为单独1种,也可以为2种以上。
〈活性剂〉
作为本发明涉及的活性剂,可举出例如,二正丁基胺、二环己基胺、单乙醇胺等胺类;二甘醇、聚乙二醇、卵磷脂、1,2,4-苯三甲酸三烯丙酯(triallyl trimellitate)、脂肪族羧酸或芳香族羧酸的锌化合物等活性剂;过氧化锌调整物;十八烷基三甲基溴化铵、合成水滑石、特殊季铵化合物。
在本发明涉及的NBR含有活性剂的情况下,活性剂的配合量相对于NBR100质量份,通常为0.2~10质量份,优选为0.3~5质量份。
〈发泡剂和发泡助剂〉
使用本发明涉及的NBR来形成的层叠体可以为非发泡体,也可以为发泡体。在层叠体为发泡体的情况下,优选NBR组合物中包含发泡剂。
作为本发明涉及的发泡剂,市售的发泡剂都适合使用。作为这样的发泡剂,可举出例如,碳酸氢钠、碳酸钠、碳酸氢铵、碳酸铵、亚硝酸铵等无机系发泡剂;N,N’-二亚硝基对苯二甲酰胺、N,N’-二亚硝基五亚甲基四胺等亚硝基化合物;偶氮二碳酰胺、偶氮二异丁腈、偶氮环己基腈、偶氮二氨基苯、偶氮二甲酸钡等偶氮化合物;苯磺酰肼、甲苯磺酰肼、对,对’-氧基双(苯磺酰肼)二苯基砜-3,3’-二磺酰肼等磺酰肼化合物;叠氮化钙、4,4’-二苯基二磺酰叠氮化物、对甲苯磺酰叠氮等叠氮化合物。其中,优选使用偶氮化合物、磺酰肼化合物、叠氮化合物。
在本发明涉及的NBR含有发泡剂的情况下,发泡剂的配合量可根据由NBR制造的层叠体所要求的性能来适当选择,相对于NBR100质量份,通常以0.5~30质量份、优选以1~20质量份的比例来使用。
此外,也可以根据需要与发泡剂一起并用发泡助剂。发泡助剂的添加对于发泡剂的分解温度的调节、气泡的均匀化等具有效果。作为发泡助剂,具体而言,可举出水杨酸、邻苯二甲酸、硬脂酸、草酸等有机酸、脲及其衍生物等。
在本发明涉及的NBR含有发泡助剂的情况下,发泡助剂的配合量相对于发泡剂100质量份,通常以1~100质量份、优选以2~80质量份的比例来使用。
<乙烯-乙酸乙烯酯共聚物皂化物>
构成本发明的层叠体的乙烯-乙酸乙烯酯共聚物皂化物是乙烯与乙烯醇的共聚物,也被称为乙烯-乙烯醇共聚物。
本发明涉及的乙烯-乙酸乙烯酯共聚物皂化物不受特别限定,通常,乙烯含有率为20~50摩尔%,优选处于24~35摩尔%的范围内。另外,本发明涉及的乙烯-乙酸乙烯酯共聚物皂化物只要具有熔融挤出成型性,MFR(载荷:2160g、测定温度:190℃)就不受特别限定,通常处于1.6~6.4g/10分钟的范围内。
关于本发明涉及的乙烯-乙酸乙烯酯共聚物皂化物,具体而言,由株式会社可乐丽以Eval的商品名,以及由日本合成化学以Soarnol的商品名分别制造销售。
《乙烯-乙酸乙烯酯共聚物》
构成本发明的层叠体的乙烯-乙酸乙烯酯共聚物为乙烯与乙酸乙烯酯的共聚物,共聚物中存在的乙酸乙烯酯含量通常,共聚物中存在的乙酸乙烯酯含量通常为5~50重量%,优选处于5~40重量%的范围内。
本发明涉及的乙烯-乙酸乙烯酯共聚物的熔体流动速率(MFR)按照JIS K7210〔190℃、2.16kg载荷〕测定得到的值通常为1.6~6.4g/10分钟,优选处于1.6~4.6g/10分钟的范围内。
本发明涉及的乙烯-乙酸乙烯酯共聚物可以为将不饱和硅烷化合物进行接枝改性而成的改性共聚物。该情况下的不饱和硅烷化合物的接枝量通常为0.01~5重量%,优选处于0.02~3重量%的范围内。
本发明涉及的改性共聚物为利用各种公知的改性方法,例如,例如,在自由基引发剂的存在下或不存在的情况下,将乙烯-乙酸乙烯酯共聚物进行接枝改性而获得。此时,如果在自由基引发剂的存在下进行接枝改性,则能够将上述不饱和硅烷化合物效率良好地接枝改性。
作为这样的自由基引发剂,使用有机过氧化物、偶氮化合物等。作为这样的自由基引发剂,具体而言,可举出过氧化苯甲酰、过氧化二氯苯甲酰、过氧化二枯基、过氧化二叔丁基、2,5-二甲基-2,5-二(过氧化苯甲酸酯)己炔-3、1,4-双(叔丁基过氧化异丙基)苯、过氧化月桂酰、叔丁基过氧化乙酸酯、2,5-二甲基-2,5-二(叔丁基过氧化)己炔-3、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、叔丁基过氧化苯甲酸酯、叔丁基过氧化苯基乙酸酯、叔丁基过氧化异丁酸酯、叔丁基过氧化-仲辛酸酯、叔丁基过氧化新戊酸酯、枯基过氧化新戊酸酯、叔丁基过氧化二乙基乙酸酯;偶氮二异丁腈、二甲基偶氮异丁酸酯等。
其中,优选使用过氧化二枯基、过氧化二叔丁基、2,5-二甲基-2,5-二(叔丁基过氧化)己炔-3、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、1,4-双(叔丁基过氧化异丙基)苯等二烷基过氧化物。
〈不饱和硅烷化合物〉
作为接枝于乙烯-乙酸乙烯酯共聚物的不饱和硅烷化合物,可举出各种公知的化合物,例如,乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基(β-甲氧基乙氧基)硅烷、乙烯基三乙酰氧基硅烷等乙烯基硅烷类、丙烯酰氧基丙基三甲氧基硅烷、甲基丙烯酰氧基丙基三甲氧基硅烷等丙烯酸系硅烷类等。
<层叠体>
本发明的层叠体为上述NBR组合物层与上述乙烯-乙酸乙烯酯共聚物皂化物层层叠而成的层叠体。
作为构成本发明的层叠体的上述NBR组合物层与上述乙烯-乙酸乙烯酯共聚物皂化物层的厚度,没有特别限定,NBR组合物层通常为0.1~30mm,优选为1~5mm,乙烯-乙酸乙烯酯共聚物皂化物层通常为0.1~30mm,优选为1~5mm。此外,作为层叠体整体的厚度,没有特别限定,通常为1~31mm,优选为5~20mm。
此外,本发明的层叠体为上述NBR层与上述乙烯-乙酸乙烯酯共聚物皂化物层隔着上述乙烯-乙酸乙烯酯共聚物层层叠而成的层叠体。
构成上述层叠体的上述NBR层包含上述NBR组合物层。
作为构成本发明的层叠体的上述NBR层与上述乙烯-乙酸乙烯酯共聚物皂化物层的厚度,没有特别限定,NBR层通常为0.1~30mm,优选为1~5mm,乙烯-乙酸乙烯酯共聚物皂化物层通常为0.1~30mm,优选为1~5mm。
此外,上述乙烯-乙酸乙烯酯共聚物层的厚度没有特别限定,通常为30~300μm,优选处于30~250μm的范围内。
此外,作为层叠体整体的厚度,没有特别限定,通常为1~31mm,优选为5~20mm。
本发明的层叠体能够通过各种公知的成型加工方法来制成层叠体,具体而言,例如,将NBR与乙烯-乙酸乙烯酯共聚物皂化物以乙烯-乙酸乙烯酯共聚物作为中间层进行共挤出成型而制成层叠体的方法;将NBR、乙烯-乙酸乙烯酯共聚物和乙烯-乙酸乙烯酯共聚物皂化物分别挤出成型或压制成型后,将NBR层与乙烯-乙酸乙烯酯共聚物皂化物层隔着乙烯-乙酸乙烯酯共聚物层进行层叠的方法;将乙烯-乙酸乙烯酯共聚物层挤出至NBR层或乙烯-乙酸乙烯酯共聚物皂化物层上并层压后,贴合乙烯-乙酸乙烯酯共聚物皂化物层或NBR层的方法;或者注射成型、压延成型、中空成型等各种成型加工方法。
此外,本发明的层叠体例如,能够通过将NBR组合物与乙烯-乙酸乙烯酯共聚物皂化物进行共挤出成型而制成层叠体的方法;将NBR和乙烯-乙酸乙烯酯共聚物皂化物分别挤出成型或压制成型后,将NBR组合物层与乙烯-乙酸乙烯酯共聚物皂化物层进行层叠的方法;或者注射成型、压延成型、中空成型等各种成型加工方法来制成层叠体。
本发明的层叠体适合用作需要耐油性、耐热性、耐气体透过性的各种用途,例如,汽车燃料配管用管或软管、汽车冷却系统配管用管或软管、汽车散热器软管、制动软管、空调软管、电线被覆材、光纤被覆材等的管、软管类、农业用膜、衬里(lining)、建筑用内装材(壁纸等)、层压钢板等的膜、片类、汽车散热器罐、药液瓶、药液罐、药液容器、汽油罐等罐类。本发明的层叠结构体由于燃料透过性低,因此作为汽车燃料配管用管或软管是特别有用的。
实施例
以下,通过实施例来进一步详细地说明本发明,但本发明并不限定于这些实施例。
以下示出实施例和比较例所使用的聚合物等。
(1)NBR:商品名Nipol 1042,结合丙烯腈(AN)量:33.5%,ML(1+4)100℃:77.5,非污染性,比重:0.98[日本瑞翁(株)制]
(2)乙烯-乙酸乙烯酯共聚物
(2-1)乙烯-乙酸乙烯酯共聚物
作为乙烯-乙酸乙烯酯共聚物(EVA-1),使用了商品名EVAFLEX品牌EVA150 MFR:30g/10分钟,VA含量:33重量%和密度:960kg/m3三井-杜邦聚合化学株式会社制。
(2-2)硅烷改性乙烯-乙酸乙烯酯共聚物
实施例所使用的硅烷改性乙烯-乙酸乙烯酯共聚物(改性EVA)由以下制造例1来制造。
〔制造例1〕
将乙烯-乙酸乙烯酯共聚物〔商品名EVAFLEX品牌EV260(MFR:6g/10分钟,密度:950kg/m3,乙酸乙烯酯含量:28重量%三井-杜邦聚合化学制)100质量份、乙烯基三甲氧基硅烷:1.7质量份、过氧化二枯基:0.15质量份、以及十二烷基硫醇:0.03质量份进行混合,供给至的多轴挤出机,在挤出温度200℃以上进行熔融混炼并挤出后,冷却制粒,获得了硅烷改性乙烯-乙酸乙烯酯共聚物(改性EVA)。
(3)乙烯-乙酸乙烯酯共聚物皂化物
作为由乙烯-乙酸乙烯酯共聚物皂化物构成的膜,使用了EVOH商品名F101B[(株)可乐丽公司制]熔点:180℃,厚度:100μm的膜(EVOH膜)。
在与NBR层叠之前将该EVOH膜以100℃×3小时进行减压干燥,保存于封装容器中。
[实施例1]
(NBR组合物的调制)
作为第一阶段,使用BB-2型班伯里密炼机(神户制钢所制),将上述NBR塑炼30秒,接着在其中,将相对于NBR:100质量份为5质量份的氧化锌(井上石灰工业(株)制)、40质量份的FEF炭黑(旭#60UG,旭Carbon(株)公司制)和1质量份的硬脂酸在140℃混炼2分钟。然后,使活塞上升,进行清扫,进一步,进行1分钟混炼,在约150℃排出,获得了第一阶段的配合物。
接下来,作为第二阶段,将由第一阶段获得的配合物卷缠于8英寸辊(日本Roll(株)公司制,前辊的表面温度50℃,后辊的表面温度50℃,前辊的转速16rpm,后辊的转速18rpm),在其中添加0.7质量份的N-叔丁基-2-苯并噻唑基亚磺酰胺(Nocceler NS-P,大内新兴(株)制)和1.5质量份的硫,混炼10分钟,获得了未交联的NBR组合物(NBR配合物)。
(层叠体的制作、评价)
(T字型剥离试验用的层叠体的制作)
将在上述NBR组合物的调制中获得的NBR组合物压成片状。接下来,将压片后的NBR组合物片50g利用拉伸聚对苯二甲酸乙二醇酯膜(东丽制商品名:lumirror)从上下夹持共聚物组合物片。使用50吨压制成型机,将上下被lumirror膜夹持的NBR组合物片在120℃压制2分钟,制作出t(厚度)=1mm、20cm见方的NBR组合物片。
将进行了上述压制后的NBR组合物片(层1)裁切成正式压制尺寸(15cm×15cm×t=1mm)。裁切后剥离上下的lumirror膜。
将在110℃以真空状态干燥处理3小时后的EVOH膜(层3)裁切成正式压制尺寸(15cm×15cm×t=1mm)。
使用改性EVA,准备厚度250μm的膜(层2)。
接下来,将各个片(层1)、膜(层3)和膜(层2)以层(2)作为中间层进行重叠。
重叠时,在层间的一部分(宽度3cm,长度15cm:剥离试验时的夹持端头)插入lumirror膜(t=0.2mm),在该状态下,将层(1)、层(2)和层(3)进行重叠,接着,使用100吨压制成型机,将在上述一部分夹入有lumirror膜的、重叠的片与膜在180℃压制(正式压制)10分钟,将NBR片进行交联,获得了厚度2mm的层叠体。
从获得的层叠体除去lumirror膜,用手剥离NBR组合物片〔层(1)〕与改性EVA层、或EVA-1层〔层(2)〕的层间,改性EVA层或EVA-1层〔层(2)〕与EVOH层〔层(3)〕的界面,对于其剥离性(粘接性),将没有粘接设为1,将牢固地粘接而用手无法剥离的状态设为5,按照1~5的5个等级进行评价,并且观察EVOH层的状态。
将评价结果示于表1中。
[实施例2]
除了替代实施例1所使用的改性EVA而使用EVA-1以外,与实施例1同样地进行,获得了层叠体。将评价结果示于表1中。
[比较例1]
在实施例1中,没有使用用于中间层的改性EVA,而将片(层1)与膜(层3)直接层叠而获得了层叠体。将评价结果示于表1中。
[实施例3]
除了替代实施例1所使用的Nocceler NS-P和硫而使用过氧化二枯基40%母料(DCP-40C,日油(株)制)以外,与实施例1同样地进行,获得了层叠体。将评价结果示于表1中。
[实施例4]
除了替代实施例3所使用的改性EVA而使用EVA-1以外,与实施例3同样地进行,获得了层叠体。将评价结果示于表1中。
[比较例2]
在实施例3中,没有使用用于中间层的改性EVA,而将片(层1)与膜(层3)直接层叠而获得了层叠体。将评价结果示于表1中。
[表1]
[实施例5]
(NBR组合物的调制)
作为第一阶段,使用BB-2型班伯里密炼机(神户制钢所制),将上述NBR塑炼30秒,接着在其中,将相对于NBR:100质量份为10质量份的硅烷改性EVA、5质量份的氧化锌(井上石灰工业(株)制)、40质量份的FEF炭黑(旭#60UG,旭Carbon(株)公司制)和1质量份的硬脂酸在140℃混炼2分钟。然后,使活塞上升,进行清扫,进一步,进行1分钟混炼,在约150℃排出,获得了第一阶段的配合物。
接下来,作为第二阶段,将由第一阶段获得的配合物卷缠于8英寸辊(日本Roll(株)公司制,前辊的表面温度50℃,后辊的表面温度50℃,前辊的转速16rpm,后辊的转速18rpm),在其中添加0.7质量份的N-叔丁基-2-苯并噻唑基亚磺酰胺(Nocceler NS-P,大内新兴(株)制)和1.5质量份的硫,混炼10分钟,获得了未交联的NBR组合物(NBR配合物)。
(层叠体的制作、评价)
(T字型剥离试验用的层叠体的制作)
将在上述NBR组合物的调制中获得的NBR组合物压成片状。接下来,将压片后的NBR组合物片50g利用拉伸聚对苯二甲酸乙二醇酯膜(东丽制商品名:lumirror)从上下夹持共聚物组合物片。使用50吨压制成型机,将上下被lumirror膜夹持的NBR组合物片在120℃压制2分钟,制作出t(厚度)=1mm、20cm见方的NBR组合物片。
接下来,将进行了上述压制后的NBR组合物片(层1)裁切成正式压制尺寸(15cm×15cm×t=1mm)。裁切后剥离上下的lumirror膜。
接下来,将在110℃以真空状态干燥处理3小时后的EVOH膜(层2)裁切成正式压制尺寸(15cm×15cm×t=1mm)。接下来,将各个片(层1)和膜(层2)进行重叠。重叠时,在NBR组合物片的一部分(宽度3cm,长度15cm:剥离试验时的夹持端头)插入lumirror膜(t=0.2mm),在该状态下,将片与膜重叠,接着,使用100吨压制成型机,将在上述一部分夹入有lumirror膜的、重叠的片与膜在180℃压制(正式压制)10分钟,将NBR片进行交联,获得了厚度2mm的层叠体。
从获得的层叠体除去lumirror膜,用手剥离NBR组合物片与EVOH膜的界面,对于其剥离性(粘接性),将没有粘接设为1,将牢固地粘接而用手无法剥离的状态设为5,以按照1~5的5个等级进行评价,并且观察EVOH膜的状态。
将评价结果示于表2中。
[实施例6]
除了替代实施例5所使用的Nocceler NS-P和硫而使用过氧化二枯基40%母料(DCP-40C,日油(株)制)以外,与实施例5同样地进行,获得了NBR组合物和层叠体。
将评价结果示于表2中。
[比较例3]
除了替代实施例5所使用的NBR组合物而使用没有配合硅烷改性EVA的NBR组合物以外,与实施例5同样地进行,获得了NBR组合物及其层叠体。
将评价结果示于表2中。
[比较例4]
除了替代实施例6所使用的NBR组合物而使用没有配合硅烷改性EVA的NBR组合物以外,与实施例6同样地进行,获得了NBR组合物及其层叠体。
将评价结果示于表2中。
[表2]
Claims (6)
1.一种丙烯腈-丁二烯橡胶组合物,其特征在于,包含丙烯腈-丁二烯橡胶、以及相对于该丙烯腈-丁二烯橡胶100质量份为0~50质量份的硅烷改性乙烯-乙酸乙烯酯共聚物。
2.一种层叠体,其特征在于,包含权利要求1所述的组合物的丙烯腈-丁二烯橡胶层与乙烯-乙酸乙烯酯共聚物皂化物层隔着乙烯-乙酸乙烯酯共聚物层而层叠。
3.根据权利要求2所述的层叠体,其特征在于,所述乙烯-乙酸乙烯酯共聚物层包含硅烷改性乙烯-乙酸乙烯酯共聚物。
4.根据权利要求1所述的丙烯腈-丁二烯橡胶组合物,其特征在于,包含丙烯腈-丁二烯橡胶、以及相对于该丙烯腈-丁二烯橡胶100质量份为2~50质量份的硅烷改性乙烯-乙酸乙烯酯共聚物。
5.根据权利要求1或4所述的丙烯腈-丁二烯橡胶组合物,其特征在于,进一步包含1.7~20质量份的过氧化二枯基。
6.一种层叠体,其特征在于,包含权利要求4或5所述的丙烯腈-丁二烯橡胶组合物的层与乙烯-乙酸乙烯酯共聚物皂化物层层叠。
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