TWI788539B - 丙烯腈-丁二烯橡膠組成物及含有該組成物層之積層體 - Google Patents
丙烯腈-丁二烯橡膠組成物及含有該組成物層之積層體 Download PDFInfo
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- TWI788539B TWI788539B TW108108682A TW108108682A TWI788539B TW I788539 B TWI788539 B TW I788539B TW 108108682 A TW108108682 A TW 108108682A TW 108108682 A TW108108682 A TW 108108682A TW I788539 B TWI788539 B TW I788539B
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- Prior art keywords
- vinyl acetate
- ethylene
- layer
- acetate copolymer
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Abstract
本發明之課題在於開發出與乙烯-醋酸乙烯酯共聚合體皂化物層間之接著強度優異的NBR組成物,以及NBR層與乙烯-醋酸乙烯酯共聚合體皂化物層間之接著強度優異的積層體。本發明的丙烯腈-丁二烯橡膠組成物,係含有:丙烯腈-丁二烯橡膠以及矽烷改質乙烯-醋酸乙烯酯共聚合體;相對於該丙烯腈-丁二烯橡膠100質量份,矽烷改質乙烯-醋酸乙烯酯共聚合體為0~50質量份。本發明的積層體,係由含有該組成物的丙烯腈-丁二烯橡膠層、與乙烯-醋酸乙烯酯共聚合體皂化物層,隔著乙烯-醋酸乙烯酯共聚合體層進行積層。
Description
本發明係關於與乙烯-醋酸乙烯酯共聚合體皂化物層間之接著強度獲改善的丙烯腈-丁二烯橡膠(NBR)組成物、以及該組成物層與乙烯-醋酸乙烯酯共聚合體皂化物層的積層體。
例如汽車、產業機械、建築機械、摩托車、農業機械等均裝設有供冷卻引擎用的散熱器軟管、散熱器溢流排水用軟管、室內暖房用加熱器軟管、冷氣機排水軟管、雨刷水管、屋頂排水管、排水蛇腹軟管等各種軟管。該等軟管係使用耐油性、耐熱性、耐氣體穿透性佳的NBR。
然而,依照用途,因為NBR單層會有耐氣體穿透性不足之情形,因而有提案例如由NBR層、與阻氣性更優異的乙烯-乙烯醇共聚合體層進行積層(專利文獻1)。
然而,得知即便嘗試僅NBR層與乙烯-乙烯醇共聚合體層的積層,接著強度仍嫌不足。
專利文獻1:日本專利特開2009-006575號公報
本發明課題在於開發出與乙烯-醋酸乙烯酯共聚合體皂化物層間之接著強度優異的NBR組成物,以及NBR層與乙烯-醋酸乙烯酯共聚合體皂化物層間之接著強度優異的積層體。
本發明係關於以下[1]~[6]。
[1]一種丙烯腈-丁二烯橡膠組成物,係含有:丙烯腈-丁二烯橡膠以及矽烷改質乙烯-醋酸乙烯酯共聚合體;相對於該丙烯腈-丁二烯橡膠100質量份、矽烷改質乙烯-醋酸乙烯酯共聚合體為0~50質量份。
[2]一種積層體,係含有第[1]項所記載之組成物的丙烯腈-丁二烯橡膠層、與乙烯-醋酸乙烯酯共聚合體皂化物層,隔著乙烯-醋酸乙烯酯共聚合體層進行積層。
[3]如第[2]項所記載的積層體,其中,上述乙烯-醋酸乙烯酯共聚合體層係含有矽烷改質乙烯-醋酸乙烯酯共聚合體。
[4]如第[1]項所記載的丙烯腈-丁二烯橡膠組成物,其中,含有:丙烯腈-丁二烯橡膠以及矽烷改質乙烯-醋酸乙烯酯共聚合體;相對於該丙烯腈-丁二烯橡膠100質量份,矽烷改質乙烯-醋酸乙烯酯共聚合體為2~50質量份。
[5]如第[1]項或第[4]項所記載的丙烯腈-丁二烯橡膠組成物,其中,更進一步含有過氧化二異丙苯1.7~20質量份。
[6]一種積層體,係由:由第[4]項或第[5]項所記載之丙烯腈-丁二烯橡膠組成物構成的層、與乙烯-醋酸乙烯酯共聚合體皂化物層進行積層而成。
本發明含有矽烷改質乙烯-醋酸乙烯酯共聚合體的丙烯腈-丁二烯橡膠組成物,係當與乙烯-醋酸乙烯酯共聚合體皂化物層進行積層時的接著強度優異,因而頗適用於需要耐油性、耐熱性、耐氣體穿透性的各種用途。
再者,丙烯腈-丁二烯橡膠層與乙烯-醋酸乙烯酯共聚合體皂化物層間,設有乙烯-醋酸乙烯酯共聚合體層的積層體,係層間接著強度優異,頗適用於需要耐油性、耐熱性及耐氣體穿透性的各種用途。
構成本發明積層體的丙烯腈-丁二烯橡膠(NBR)層(以下亦簡稱為「NBR層」)、及丙烯腈-丁二烯橡膠組成物(以下亦簡稱「NBR組成物」)的丙烯腈-丁二烯橡膠(NBR),係由丙烯腈與丁二烯進行乳化聚合而獲得的二烯系合成橡膠。NBR一般依照丙烯腈的鍵結量,分類為極高(43%以上)、高(36~42%)、中高(31~35%)、中(25~30%)、低(24%以下)等5階段,而中高係屬於通用形式。
本發明在NBR中所摻合的矽烷改質乙烯-醋酸乙烯酯共聚合體,係由乙烯-醋酸乙烯酯共聚合體利用不飽和矽烷化合物進行接
枝改質而成的改質共聚合體。不飽和矽烷化合物的接枝量通常係0.01~5重量%、較佳係0.02~3重量%。
本發明之矽烷改質乙烯-醋酸乙烯酯共聚合體的熔體流動速率(MFR),根據JIS K7210[190℃、2.16kg荷重]所測定的值,通常係1.6~6.4g/10分、較佳係1.6~4.6g/10分的範圍。
被矽烷改質的乙烯-醋酸乙烯酯共聚合體,在共聚合體中存在的醋酸乙烯酯含量通常係5~50重量%、較佳係5~40重量%範圍。
本發明之乙烯-醋酸乙烯酯共聚合體的熔體流動速率(MFR),根據JIS K7210[190℃、2.16kg荷重]所測定的值,通常係1.6~6.4g/10分、較佳係1.6~4.6g/10分的範圍。
乙烯-醋酸乙烯酯共聚合體利用不飽和矽烷化合物進行接枝改質的方法,可利用各種公知之改質方法實施,例如在自由基起始劑存在下(或不存在下)進行接枝改質。此時,若在自由基起始劑存在下進行接枝改質,則上述不飽和矽烷化合物可效率佳地進行接枝改質。
此種自由基起始劑係使用有機過氧化物、偶氮化合物等。此種自由基起始劑具體係可舉例如:過氧化對苯甲醯、二氯過氧化苯甲醯、過氧化二異丙苯、過氧化二第三丁基、2,5-二甲基-2,5-二(過氧化苯甲酸酯)-3-己炔、1,4-雙(過氧化第三丁基異丙基)苯、過氧化月桂醯、過氧化醋酸第三丁酯、2,5-二甲基-2,5-二(過氧化第三丁基)-3-己炔、2,5-二甲基-2,5-二(過氧化第三丁基)己烷、過氧化苯甲酸第三丁酯、過氧化苯基醋酸第三丁酯、過氧化異丁酸第三丁酯、過氧化第二辛酸第三丁酯、過氧化三甲基乙酸第三丁酯、過氧
化三甲基乙酸異丙苯酯、過氧化二乙基醋酸第三丁酯;偶氮雙異丁腈、二甲基偶氮異丁酸酯等。
該等之中,較佳係使用過氧化二異丙苯、過氧化二第三丁基、2,5-二甲基-2,5-二(過氧化第三丁基)-3-己炔、2,5-二甲基-2,5-二(過氧化第三丁基)己烷、1,4-雙(過氧化第三丁基異丙基)苯等二烷基過氧化物。
乙烯-醋酸乙烯酯共聚合體所接枝的不飽和矽烷化合物係可例如各種公知之化合物,例如:乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、乙烯基(β-甲氧基乙氧基)矽烷、乙烯基三乙醯氧基矽烷等烯基矽烷類;丙烯醯氧丙基三甲氧基矽烷、甲基丙烯醯氧丙基三甲氧基矽烷等丙烯酸系矽烷類等。
本發明的NBR組成物係相對於上述NBR:100質量份,含有上述矽烷改質乙烯-醋酸乙烯酯共聚合體0~50質量份、較佳2~50質量份、更佳係5~20質量份的組成物。
本發明的NBR組成物係除上述矽烷改質乙烯-醋酸乙烯酯共聚合體之外,若尚含有1.7~20質量份、更佳3.4~10.2質量份之過氧化二異丙苯,則與由乙烯-醋酸乙烯酯共聚合體皂化物所構成層之間的接著強度,將可獲更進一步之改善。
在本發明的NBR中,配合所需目的,除上述矽烷改質乙烯-醋酸乙烯酯共聚合體與過氧化二異丙苯之外,在不致損及
本發明效果之範圍內,尚亦可摻合其他成分。其他成分係亦可含有例如從填料、交聯助劑、硫化促進劑、硫化助劑、軟化劑、抗老化劑、加工助劑、活性劑、耐熱安定劑、耐候安定劑、抗靜電劑、著色劑、滑劑、增黏劑、發泡劑及發泡助劑中選擇之至少1種。又,各個添加劑係可單獨使用1種、亦可併用2種以上。
在本發明NBR中所摻合的填料,係在NBR中所摻合的公知橡膠補強劑,通常係碳黑、通稱「無機補強劑」的無機物。
本發明的填料具體係可舉例如:旭#55G、旭#60G(以上均為Asahi Carbon(股)製);Seast(SRF、GPF、FEF、MAF、HAF、ISAF、SAF、FT、MT等)碳黑(Tokai Carbon(股)製);該等碳黑經矽烷偶合劑等施行表面處理者,以及二氧化矽、活性碳酸鈣、微粉滑石、微粉矽酸、輕質碳酸鈣、重質碳酸鈣、滑石、黏土等。
該等填料係可單獨使用、亦可為二種以上的混合物。
本發明的填料較佳係使用親水性二氧化矽、疏水性二氧化矽等二氧化矽;碳黑、輕質碳酸鈣、重質碳酸鈣、滑石、黏土等。
當本發明的NBR係含有填料時,相對於上述NBR:100質量份,通常依100~300質量份、較佳係100~250質量份範圍摻合。
當交聯劑係使用過氧化二異丙苯的情況,亦可併用交聯助劑。
交聯助劑係可舉例如:硫;對醌二肟等醌二肟系交聯助劑;乙二醇二(甲基丙烯酸酯)、三(甲基丙烯酸)三羥甲基丙酯等丙烯酸系交聯助劑;酞酸異二烯丙酯、異三聚氰酸三烯丙酯等烯丙系交聯助劑;順丁烯二醯亞胺系交聯助劑;二乙烯苯;氧化鋅[例如:ZnO#1-氧化鋅2種(JIS規格(K-1410))、HakusuiTech(股)製]、氧化鎂、鋅華[例如:「META-Z102」(商品名;井上石灰工業(股)製)等氧化鋅]、活性鋅華等金屬氧化物。
當使用交聯助劑的情況,相對於過氧化二異丙苯1莫耳,NBR中的交聯助劑摻合量通常係0.5~10莫耳、較佳係0.5~7莫耳、更佳係1~6莫耳。
本發明的硫化促進劑係可舉例如:N-環己基-2-苯并噻唑基亞磺醯胺、N-氧二伸乙基2-苯并噻唑基亞磺醯胺、N,N'-二異丙基-2-苯并噻唑基亞磺醯胺、2-巰基苯并噻唑(例如SANCELERM(商品名,三新化學工業公司製))、2-(4-啉二硫基)苯并噻唑(例如Nocceler MDB-P(商品名,大內新興化學工業公司製))、2-(2,4-二硝苯基)巰基苯并噻唑、2-(2,6-二乙基-4-啉硫基)苯并噻唑、及二硫化二苯并噻唑(例如SANCELER DM(商品名,三新化學工業公司製))等噻唑系硫化促進劑;二苯胍、三苯胍及二鄰甲苯胍等胍系硫化促進劑;乙醛-苯胺縮合物及丁醛-苯胺縮合物等醛胺系硫化促進劑;2-巰基咪唑啉等咪唑啉系硫化促進劑;單硫化四甲胺硫甲醯(例如SANCELER TS(商品名,三新化學工業公司製))、二硫化四甲基秋蘭姆(例如SANCELER TT(商品名,三新化學工業公司製))、二硫化四乙基秋蘭姆(例如SANCELER TET(商品名,三新化學工業公司製))、二硫化四丁基秋蘭姆(例如SANCELER TBT(商品名,三
新化學工業公司製))及四硫化雙(五甲基)秋蘭姆(例如、SANCELER TRA(商品名;三新化學工業公司製))等秋蘭姆系硫化促進劑;二甲基二硫胺甲酸鋅、二乙基二硫胺甲酸鋅、二丁基二硫胺甲酸鋅(例如SANCELER PZ、SANCELER BZ、及SANCELER EZ(商品名,三新化學工業公司製))、及二乙基二硫胺甲酸碲等二硫代酸鹽系硫化促進劑;乙烯硫脲(例如SANCELER BUR(商品名,三新化學工業公司製)、SANCELER 22-C(商品名,三新化學工業公司製))、N,N'-二乙基硫脲及N,N'-二丁基硫脲等硫脲系硫化促進劑;二丁基黃原酸鋅等黃原酸酯系硫化促進劑。
當使用硫化促進劑的情況,相對於NBR:100質量份,在NBR中的該等硫化促進劑摻合量一般係0.1~20質量份、較佳係0.2~15質量份、更佳係0.5~10質量份。若硫化促進劑的摻合量在上述範圍內,則不會於所獲得積層體的表面暈開,NBR呈現優異的交聯特性。若交聯劑係使用硫系化合物時,亦可併用硫化助劑。
本發明的硫化助劑係可舉例如:氧化鋅(例如ZnO#1-氧化鋅2種、HakusuiTech(股)製)、氧化鎂、鋅華(例如「META-Z102」(商品名,井上石灰工業(股)製)等氧化鋅)。
當使用硫化助劑的情況,相對於NBR:100質量份,在NBR組成物中的硫化助劑摻合量通常係1~20質量份。
本發明的軟化劑係可舉例如:加工處理油、潤滑油、石蠟油、液態石蠟、石油瀝青、凡士林等石油系軟化劑;煤焦油等煤焦油系軟化劑;篦麻油、亞麻仁油、菜籽油、大豆油、椰子油等脂肪油系
軟化劑;蜜蠟、棕櫚蠟等蠟類;環烷酸、松油、松脂或其衍生物;萜烯樹脂、石油樹脂、香豆酮-茚樹脂等合成高分子物質;酞酸二辛酯、己二酸二辛酯等酯系軟化劑;其他尚可例如:微晶蠟、液狀聚丁二烯、改質液狀聚丁二烯、烴系合成潤滑油、松脂油、油膏(硫化油膏),該等之中,較佳係石油系軟化劑、更佳係加工處理油。
當本發明的NBR係含有軟化劑時,相對於NBR:100質量份,軟化劑的摻合量一般係2~100質量份、較佳係10~100質量份。
藉由在本發明的NBR中摻合抗老化劑(安定劑),便可延長由其所形成之密封迫緊的壽命。此種抗老化劑係有如習知公知的抗老化劑,例如:胺系抗老化劑、酚系抗老化劑、硫系抗老化劑等。
本發明的抗老化劑係可例如:苯基丁胺、N,N-二-2-萘基-對伸苯二胺等芳香族二級胺系抗老化劑;二丁基羥甲苯、四[亞甲基(3,5-二第三丁基-4-羥)氫化肉桂酸酯]甲烷等酚系抗老化劑;雙[2-甲基-4-(3-正烷硫基丙醯氧基)-5-第三丁基苯基]硫醚等硫醚系抗老化劑;二丁基二硫胺甲酸鎳等二硫胺甲酸鹽系抗老化劑;2-巰基苯甲醯咪唑、2-巰基苯并咪唑、2-巰基苯并咪唑的鋅鹽、二硫代二丙酸二月桂酯、硫代二丙酸二硬脂酯等硫系抗老化劑等。
當本發明的NBR係含有抗老化劑時,相對於NBR:100質量份,抗老化劑的摻合量通常係0.3~10質量份、較佳係0.5~7.0質量份。若抗老化劑的摻合量係在上述範圍內,則所獲得之積層體的表面不會出現暈開之情形,更可抑制阻礙硫化之現象的
發生。
本發明之加工助劑係可廣泛使用一般當作加工助劑摻合於橡膠中者。具體係可舉例如:蓖麻油酸、硬脂酸、棕櫚酸、月桂酸、硬脂酸鋇、硬脂酸鋅、硬脂酸鈣、月桂酸鋅或酯類等。該等之中,較佳係硬脂酸。
當本發明的NBR係含有加工助劑時,相對於NBR:100質量份,通常可依1~3質量份的量適當摻合。若加工助劑的摻合量在上述範圍內,便可使混練加工性、擠出加工性、射出成形性等加工性優異,故較佳。
上述加工助劑係可單獨1種、亦可為2種以上。
本發明的活性劑係可舉例如:二正丁胺、二環己胺、單乙醇胺等胺類;二乙二醇、聚乙二醇、卵磷脂、1,2,4-苯三酸三烯丙酯、脂肪族羧酸或芳香族羧酸的鋅化合物等活性劑;過氧化鋅調製物;十八烷基三甲基溴化銨、合成水滑石、特殊四級銨化合物。
當本發明的NBR係含有活性劑的情況,相對於NBR:100質量份,活性劑的摻合量通常係0.2~10質量份、較佳係0.3~5質量份。
使用本發明的NBR所形成之積層體,係可為非發泡體、亦可
為發泡體。當積層體係發泡體的情況,較佳為在NBR組成物中含有發泡劑。
本發明的發泡劑係任一市售發泡劑均頗適用。此種發泡劑係可舉例如:重碳酸鈉、碳酸鈉、重碳酸銨、碳酸銨、亞硝酸銨等無機系發泡劑;N,N'-二亞硝基對苯二甲醯胺、N,N'-二亞硝基五亞甲基四胺等亞硝基化合物;偶氮二羧醯胺、偶氮雙異丁腈、偶氮環己腈、偶氮二胺基苯、偶氮二羧酸鋇等偶氮化合物;苯磺醯基醯肼、甲苯磺醯基醯肼、p,p'-氧雙(苯磺醯基醯肼)二苯碸-3,3'-二磺醯基醯肼等磺醯基醯肼化合物;疊氮化鈣、疊氮化-4,4'-二苯基二磺醯、疊氮化對甲苯丙二醯等疊氮化合物。其中,較佳係使用偶氮化合物、磺醯基醯肼化合物、疊氮化合物。
當本發明的NBR係含有發泡劑的情況,發泡劑的摻合量係依照對由NBR所製造之積層體要求的性能再行適當選擇,相對於NBR:100質量份,通常係依0.5~30質量份、較佳係1~20質量份的比例使用。
再者,視需要亦可併用發泡劑與發泡助劑。發泡助劑的添加係具有發泡劑分解溫度調節、氣泡均勻化等效果。發泡助劑具體係可舉例如:水楊酸、酞酸、硬脂酸、草酸等有機酸;脲及其衍生物等。
當本發明的NBR係含有發泡助劑的情況,相對於發泡劑100質量份,發泡助劑的摻合量通常係依1~100質量份、較佳係2~80質量份的比例使用。
構成本發明之積層體的乙烯-醋酸乙烯酯共聚合體皂化物,係亦稱為「乙烯-乙烯醇共聚合體」之乙烯與乙烯醇的共聚合體。
本發明的乙烯-醋酸乙烯酯共聚合體皂化物並無特別的限定,通常乙烯含有率係20~50莫耳%、較佳24~35莫耳%的範圍。又,本發明的乙烯-醋酸乙烯酯共聚合體皂化物,在具有熔融擠出成形性的前提下,MFR(荷重:2160g、測定溫度:190℃)並無特別的限定,通常係1.6~6.4g/10分的範圍。
本發明的乙烯-醋酸乙烯酯共聚合體皂化物,具體已分別有由KURARAY股份有限公司依商品名EVAL、以及由日本合成化學依商品名SoarnoL製造販售。
構成本發明之積層體的乙烯-醋酸乙烯酯共聚合體,係乙烯與醋酸乙烯酯的共聚合體,在共聚合體中存在的醋酸乙烯酯含量通常係5~50重量%、較佳係5~40重量%的範圍。
本發明的乙烯-醋酸乙烯酯共聚合體之熔體流動速率(MFR),根據JIS K7210[190℃、2.16kg荷重]所測定的值,通常係1.6~6.4g/10分、較佳係1.6~4.6g/10分的範圍。
本發明的乙烯-醋酸乙烯酯共聚合體,亦可由將不飽和矽烷化合物施行接枝改質而成的改質共聚合體。此情況的不飽和矽烷化合物接枝量,通常係0.01~5重量%、較佳係0.02~3重量%的範圍。
本發明的改質共聚合體係可利用各種公知改質方法
實施,例如在自由基起始劑存在下或不存在下,將乙烯-醋酸乙烯酯共聚合體進行接枝改質而獲得。此時,若在自由基起始劑存在下進行接枝改質,則上述不飽和矽烷化合物可效率佳地進行接枝改質。
此種自由基起始劑係可使用有機過氧化物、偶氮化合物等。此種自由基起始劑具體係可舉例如:過氧化對苯甲醯、二氯過氧化苯甲醯、過氧化二異丙苯、過氧化二第三丁基、2,5-二甲基-2,5-二(過氧化苯甲酸酯)-3-己炔、1,4-雙(過氧化第三丁基異丙基)苯、過氧化月桂醯、過氧化醋酸第三丁酯、2,5-二甲基-2,5-二(過氧化第三丁基)-3-己炔、2,5-二甲基-2,5-二(過氧化第三丁基)己烷、過氧化苯甲酸第三丁酯、過氧化苯基醋酸第三丁酯、過氧化異丁酸第三丁酯、過氧化第二辛酸第三丁酯、過氧化三甲基乙酸第三丁酯、過氧化三甲基乙酸異丙苯酯、過氧化二乙基醋酸第三丁酯;偶氮雙異丁腈、二甲基偶氮異丁酸酯等。
該等之中,較佳係使用過氧化二異丙苯、過氧化二第三丁基、2,5-二甲基-2,5-二(過氧化第三丁基)-3-己炔、2,5-二甲基-2,5-二(過氧化第三丁基)己烷、1,4-雙(過氧化第三丁基異丙基)苯等二烷基過氧化物。
乙烯-醋酸乙烯酯共聚合體所接枝的不飽和矽烷化合物係可例如各種公知之化合物,例如:乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、乙烯基(β-甲氧基乙氧基)矽烷、乙烯基三乙醯氧基矽烷等乙烯基矽烷類;丙烯醯氧丙基三甲氧基矽烷、甲基丙烯醯氧丙基
三甲氧基矽烷等丙烯酸系矽烷類等。
本發明的積層體係由上述NBR組成物層與上述乙烯-醋酸乙烯酯共聚合體皂化物層進行積層的積層體。
構成本發明積層體的上述NBR組成物層與上述乙烯-醋酸乙烯酯共聚合體皂化物層的厚度,並無特別的限定,NBR組成物層通常係0.1~30mm、較佳係1~5mm,乙烯-醋酸乙烯酯共聚合體皂化物層通常係0.1~30mm、較佳係1~5mm。又,積層體全體的厚度並無特別的限定,通常係1~31mm、較佳係5~20mm。
再者,本發明的積層體,係由上述NBR層、與上述乙烯-醋酸乙烯酯共聚合體皂化物層,隔著上述乙烯-醋酸乙烯酯共聚合體層進行積層的積層體。
構成上述積層體的上述NBR層係含有上述NBR組成物層。
構成本發明積層體的上述NBR層與上述乙烯-醋酸乙烯酯共聚合體皂化物層之厚度並無特別的限定,NBR層通常係0.1~30mm、較佳係1~5mm、乙烯-醋酸乙烯酯共聚合體皂化物層通常係0.1~30mm、較佳係1~5mm。
再者,上述乙烯-醋酸乙烯酯共聚合體層的厚度並無特別的限定,通常係30~300μm、較佳係30~250μm的範圍。
再者,積層體全體的厚度並無特別的限定,通常係1~31mm、較佳係5~20mm。
本發明的積層體係可採用各種公知之成形加工方
法,具體係例如:將NBR與乙烯-醋酸乙烯酯共聚合體皂化物,以乙烯-醋酸乙烯酯共聚合體為中間層,進行共擠出成形而形成積層體的方法;分別將NBR、乙烯-醋酸乙烯酯共聚合體及乙烯-醋酸乙烯酯共聚合體皂化物施行擠出成形、或壓合成形後,再將NBR層與乙烯-醋酸乙烯酯共聚合體皂化物層介隔著乙烯-醋酸乙烯酯共聚合體層進行積層的方法;在NBR層或乙烯-醋酸乙烯酯共聚合體皂化物層上,擠出形成乙烯-醋酸乙烯酯共聚合體層後,再貼合乙烯-醋酸乙烯酯共聚合體皂化物層或NBR層的方法;或者利用射出成形、軋延成形、中空成形等各種成形加工方法便可形成積層體。
再者,本發明的積層體係例如:將NBR組成物與乙烯-醋酸乙烯酯共聚合體皂化物施行共擠出成形,而形成積層體的方法;分別將NBR與乙烯-醋酸乙烯酯共聚合體皂化物施行擠出成形、或壓合成形後,再將NBR組成物層與乙烯-醋酸乙烯酯共聚合體皂化物層進行積層的方法;或者利用射出成形、軋延成形、中空成形等各種成形加工方法便可形成積層體。
本發明的積層體係頗適用為需求耐油性、耐熱性、耐氣體穿透性的各種用途,例如:汽車燃料配管用硬管或軟管、汽車冷卻系配管用硬管或軟管、汽車散熱器軟管、煞車軟管、冷氣機軟管、電線被覆材、光纖被覆材等硬管、軟管類;農業用薄膜、內襯底、建築用內裝材(壁紙等)、積層鋼板等薄膜、薄片類;汽車散熱水箱、藥液瓶、藥液槽、藥液容器、汽油槽等槽類。因為本發明積層構造體的燃料穿透性低,因而作為汽車燃料配管用硬管或軟管係特別有用。
以下,針對本發明利用實施例進行更詳細說明,惟本發明並不僅侷限於該等實施例。
實施例及比較例所使用的聚合體等,係如下示:
(1)NBR:商品名Nipol 1042、鍵結丙烯腈(AN)量:33.5%、ML(1+4)100℃:77.5、非污染性、比重:0.98[日本ZEON(股)製]
(2)乙烯-醋酸乙烯酯共聚合體
(2-1)乙烯-醋酸乙烯酯共聚合體
乙烯-醋酸乙烯酯共聚合體(EVA-1)係使用商品名EVAFLEX產品名稱EVA150 MFR:30g/10分、VA含有量:33重量%及密度:960kg/m3三井-杜邦高分子化學股份有限公司製。
(2-2)矽烷改質乙烯-醋酸乙烯酯共聚合體
實施例所使用的矽烷改質乙烯-醋酸乙烯酯共聚合體(改質EVA),係由以下製造例1所製造。
將乙烯-醋酸乙烯酯共聚合體[商品名EVAFLEX產品名稱EV260(MFR:6g/10分、密度:950kg/m3、醋酸乙烯酯含有量:28重量%三井-杜邦高分子化學製)]100質量份、乙烯基三甲氧基矽烷:1.7質量份、過氧化二異丙苯:0.15質量份、及十二烷基硫醇:0.03質量份予以混合,供應給65mm之多螺桿擠出機,依擠出溫度200℃以上施行熔融混練並擠出後,施行冷卻顆粒化,獲得矽烷改質乙烯-醋酸乙烯酯共聚合體(改質EVA)。
由乙烯-醋酸乙烯酯共聚合體皂化物形成的薄膜,係使用EVOH商品名F101B[KURARAY公司(股)製]熔點:180℃、厚度:100μm的薄膜(EVOH薄膜)。
該EVOH薄膜在與NBR進行積層前,先施行100℃×3小時的減壓乾燥,並保管於密封容器中。
第一階段係使用BB-2型班布瑞混合機(神戸製鋼所製),將上述NBR施行30秒之素練,接著相對於NBR:100質量份,將5質量份的氧化鋅(井上石灰工業(股)製)、40質量份的FEF碳黑(旭#60UG、Asahi Carbon(股)公司製)及1質量份的硬脂酸,依140℃施行2分鐘混練。然後,使上頂栓上升施行清掃,更進一步施行1分鐘混練,在約150℃下排出,獲得第一階段的摻合物。
其次,第二階段係將第一階段所獲得之摻合物,捲繞於8吋輥(Nippon Roll(股)公司製、前輥表面溫度50℃、後輥表面溫度50℃、前輥轉數16rpm、後輥轉數18rpm)上,在其中添加0.7質量份的N-第三丁基-2-苯并噻唑基亞磺醯胺(Nocceler NS-P、大內新興(股)製)及1.5質量份的硫,混練10分鐘,獲得未交聯的NBR組成物(NBR摻合物)。
將上述NBR組成物製備所獲得的NBR組成物呈薄片狀擠出。接著將所擠出的NBR組成物薄片50g,利用延伸聚對苯二甲酸乙二酯薄膜(Toray製 商品名:LUMIRROR)夾置共聚合體組成物薄片的上下。將由LUMIRROR膜上下夾置的NBR組成物薄片,使用50噸壓合成形機,依120℃施行2分鐘壓合,而製得t(厚度)=1mm、正方形邊長為20cm的NBR組成物薄片。
其次,經施行上述壓合後,將NBR組成物薄片(層1)裁剪為主壓合尺寸(15cm×15cm×t=1mm)。經裁剪後剝離上下的LUMIRROR膜。
將經依110℃、真空狀態施行3小時乾燥處理的EVOH薄膜(層3),裁剪為主壓合尺寸(15cm×15cm×t=1mm)。
使用改質EVA,準備厚度250μm的薄膜(層2)。
接著,使各薄片(層1)、薄膜(層3)及薄膜(層2),以層(2)為中間層進行重疊。
重疊時,依在層間其中一部分(寬3cm、長15cm:剝離測試時的抓持份),被LUMIRROR膜夾置(t=0.2mm)的狀態下,使層(1)、層(2)及層(3)重疊,接著,將上述一部分被LUMIRROR膜夾置重疊的薄片與薄膜,使用100噸壓合成形機,依180℃施行10分鐘壓合(主壓合),而使NBR薄片進行交聯,獲得厚度2mm的積層體。
從所獲得之積層體中去除LUMIRROR膜,利用手撕開NBR組成物薄片[層(1)]與改質EVA層、或與EVA-1層[層(2)]的層間,改質EVA層或EVA-1層[層(2)]與EVOH層[層(3)]的界面,針對其剝離性(接著性),將沒有接著者評為1,將牢固接著無法用
手撕開的狀態評為5,依1~5的5階段施行評價,並觀察EVOH層的狀態。
評價結果如表1所示。
除取代實施例1所使用的改質EVA,改為使用EVA-1之外,其餘均與實施例1同樣地實施,獲得積層體。評價結果如表1所示。
除在實施例1中,未使用當作中間層用的改質EVA,而是將薄片(層1)與薄膜(層3)直接積層獲得積層體。評價結果如表1所示。
除取代實施例1所使用的Nocceler NS-P及硫,改為使用過氧化二異丙苯40%母料(DCP-40C、日油(股)製)之外,其餘均與實施例1同樣地實施,獲得積層體。評價結果如表1所示。
除取代實施例3所使用的改質EVA,改為使用EVA-1之外,其餘均與實施例3同樣地實施,獲得積層體。評價結果如表1所示。
未使用在實施例3中當作中間層用的改質EVA,而是將薄片(層1)與薄膜(層3)直接積層獲得積層體。評價結果如表1所示。
第一階段係使用BB-2型班布瑞混合機(神戸製鋼所製),將上述NBR施行30秒素練,接著相對於NBR:100質量份,將10質量份的矽烷改質EVA、5質量份的氧化鋅(井上石灰工業(股)製)、40質量份的FEF碳黑(旭#60UG、Asahi Carbon(股)公司製)及1質量份的硬脂酸,依140℃施行2分鐘混練。然後,使上頂栓上升施行清掃,更進一步施行1分鐘混練,在約150℃下排出,獲得第一階段的摻合物。
其次,第二階段係將第一階段所獲得之摻合物,捲繞於8吋輥(Nippon Roll(股)公司製、前輥表面溫度50℃、後輥表面溫度50℃、前輥轉數16rpm、後輥轉數18rpm)上,在其中添加0.7質量份的N-第三丁基-2-苯并噻唑基亞磺醯胺(Nocceler NS-P、大內新興(股)製)及1.5質量份的硫,混練10分鐘,獲得未交聯的NBR組成物(NBR摻合物)。
將上述NBR組成物製備所獲得的NBR組成物呈薄片狀擠出。接著將所擠出的NBR組成物薄片50g,利用延伸聚對苯二甲酸乙二酯薄膜(Toray製 商品名:LUMIRROR)夾置共聚合體組成物薄片的上下。將由LUMIRROR膜上下夾置的NBR組成物薄片,使用50噸壓合成形機,依120℃施行2分鐘壓合,而製得t(厚度)=1mm、正方形邊長為20cm的NBR組成物薄片。
其次,經施行上述壓合後,將NBR組成物薄片(層1)裁剪為主壓合尺寸(15cm×15cm×t=1mm)。經裁剪後剝離上下的LUMIRROR膜。
其次,將經依110℃、真空狀態施行3小時乾燥處理的EVOH薄膜(層2),裁剪為主壓合尺寸(15cm×15cm×t=1mm)。接著,使各薄片(層1)及薄膜(層2)重疊。重疊時,依在NBR組成物其中一部分(寬3cm、長15cm:剝離測試時的抓持份),被LUMIRROR膜夾置(t=0.2mm)的狀態下,使薄片與薄膜重疊;接著,將上述一部分被LUMIRROR膜夾置重疊的薄片與薄膜,使用100噸壓合成形機,依180℃施行10分鐘壓合(主壓合),而使NBR薄片進行交聯,獲得厚度2mm的積層體。
從所獲得積層體中去除LUMIRROR膜,利用手撕開NBR組成物薄片與EVOH薄膜的界面,針對其剝離性(接著性),將沒有接著者評為1,將牢固接著無法用手撕開的狀態評為5,依1~5的5階段施行評價,並觀察EVOH薄膜的狀態。
評價結果如表2所示。
除取代實施例5所使用的Nocceler NS-P與硫,改為使用過氧化二異丙苯40%母料(DCP-40C、日油(股)製)之外,其餘均與實施例5同樣地實施,獲得NBR組成物與積層體。
評價結果如表2所示。
除取代實施例5所使用的NBR組成物,改為使用未摻合矽烷改質EVA的NBR組成物之外,其餘均與實施例5同樣地實施,獲得NBR組成物與其積層體。
評價結果如表2所示。
除取代實施例6所使用的NBR組成物,改為使用未摻合矽烷改質EVA的NBR組成物之外,其餘均與實施例6同樣地實施,獲得NBR組成物與其積層體。
評價結果如表2所示。
Claims (5)
- 一種積層體,其係使含有下述丙烯腈-丁二烯橡膠組成物的丙烯腈-丁二烯橡膠層、與乙烯-醋酸乙烯酯共聚合體皂化物層,隔著乙烯-醋酸乙烯酯共聚合體層進行積層;含丙烯腈-丁二烯橡膠但不包含矽烷改質乙烯-醋酸乙烯酯共聚合體之丙烯腈-丁二烯橡膠組成物,或含丙烯腈-丁二烯橡膠及相對於該丙烯腈-丁二烯橡膠100質量份,矽烷改質乙烯-醋酸乙烯酯共聚合體為超過0質量份且為50質量份以下之丙烯腈-丁二烯橡膠組成物。
- 如請求項1之積層體,其中,上述乙烯-醋酸乙烯酯共聚合體層係含有矽烷改質乙烯-醋酸乙烯酯共聚合體。
- 一種丙烯腈-丁二烯橡膠組成物,其含有:丙烯腈-丁二烯橡膠以及矽烷改質乙烯-醋酸乙烯酯共聚合體;相對於該丙烯腈-丁二烯橡膠100質量份,矽烷改質乙烯-醋酸乙烯酯共聚合體為2~50質量份。
- 如請求項3之丙烯腈-丁二烯橡膠組成物,其中,更進一步含有過氧化二異丙苯1.7~20質量份。
- 一種積層體,其係:由請求項3或4之丙烯腈-丁二烯橡膠組成物構成的層、與乙烯-醋酸乙烯酯共聚合體皂化物層進行積層而成。
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