CN110023406A - 层叠体用组合物 - Google Patents
层叠体用组合物 Download PDFInfo
- Publication number
- CN110023406A CN110023406A CN201880004635.5A CN201880004635A CN110023406A CN 110023406 A CN110023406 A CN 110023406A CN 201880004635 A CN201880004635 A CN 201880004635A CN 110023406 A CN110023406 A CN 110023406A
- Authority
- CN
- China
- Prior art keywords
- laminated body
- acid
- weight
- vulcanizing agent
- diazabicyclo
- 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
Links
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Abstract
本发明涉及一种层叠体用组合物以及使用层叠体用组合物而成的层叠体、由层叠体构成的管状体或软管体;其中所述层叠体用组合物的特征在于包含:环氧氯丙烷类聚合物(a),二硫代氨基甲酸锌盐(b),选自由1,8‑二氮杂双环(5.4.0)十一烯‑7盐、1,5‑二氮杂双环(4.3.0)‑壬烯‑5盐、1,8‑二氮杂双环(5.4.0)十一烯‑7和1,5‑二氮杂双环(4.3.0)‑壬烯‑5所构成的组中的至少一种化合物(c),以及金属盐水合物(d)。
Description
技术领域
本发明涉及一种层叠体用组合物。
背景技术
近年来,对于汽车尾气的排放规章趋于非常严苛,作为其中之一的汽油挥发规章得到以美国为中心的日益强化。对于这些严苛的要求,在汽车燃油软管体方面,也正在开发兼备耐热老化性、耐候性、耐劣化汽油性、耐含醇汽油性、汽油不渗透性等的燃油软管体。作为该燃油软管体材料之一,可列举含氟的聚合物。但是,由于价高且在耐寒性方面也有问题,经常使用在内层使用含氟的聚合物、在外层使用环氧氯丙烷类橡胶的层叠体。
但是,在由上述这种多相聚合物组合物所构成的层叠软管体的情况下,该软管体间的粘结性就变得最为重要。众所周知,含氟的聚合物与其它种类聚合物之间的粘结性较差,因此,通常采用在聚合物组合物中配合某种添加剂等方法。在由含氟的聚合物层和环氧氯丙烷类橡胶层构成的层叠体的情况下,能够通过采用专利文献1~3中记载的方式使含氟的聚合物层与环氧氯丙烷类橡胶层进行粘结。但是,近年来,通过更少的维护来延长寿命、通过优化适应部件来进行材料变更及统一化,也需要牢固粘结有其它各种橡胶和各种低透气性材料而成的层叠体。
作为用于层叠体的组合物,本申请人公开了专利文献4,但针对汽车用燃油软管体需要更牢固的粘结性。另外,针对蒸气硫化时的粘结性仍需改善,需要进一步探讨。
现有技术文献
专利文献
专利文献1:日本特开昭64-11180号公报
专利文献2:日本特开平9-85898号公报
专利文献3:日本特开2006-306053号公报
专利文献4:日本特许第5818169号
发明内容
发明所要解决的技术问题
本发明的目的在于提供一种用于硫化粘结时的粘结性更加优异的层叠体的层叠体用组合物、及使用层叠体用组合物而成的层叠体、由层叠体构成的管状体或软管体。
用于解决问题的技术方案
本发明的层叠体用组合物的特征在于,其包含:环氧氯丙烷类聚合物(a),二硫代氨基甲酸锌盐(b),选自由1,8-二氮杂双环(5.4.0)十一烯-7盐、1,5-二氮杂双环(4.3.0)-壬烯-5盐、1,8-二氮杂双环(5.4.0)十一烯-7和1,5-二氮杂双环(4.3.0)-壬烯-5所构成的组中的至少一种化合物(c),以及金属盐水合物(d)。
另外,本发明可以采用下述技术方案。
项1一种层叠体用组合物,其特征在于,其包含:环氧氯丙烷类聚合物(a),二硫代氨基甲酸锌盐(b),选自由1,8-二氮杂双环(5.4.0)十一烯-7盐、1,5-二氮杂双环(4.3.0)-壬烯-5盐、1,8-二氮杂双环(5.4.0)十一烯-7和1,5-二氮杂双环(4.3.0)-壬烯-5所构成的组中的至少一种化合物(c),以及金属盐水合物(d)。
项2如项1所述的层叠体用组合物,其特征在于,还包含具有乙烯基的化合物(e)。
项3如权利要求1或2中任一项所述的层叠体用组合物,其中,相对于100重量份的所述环氧氯丙烷类聚合物(a),所述金属盐水合物(d)为0.1重量份~80重量份。
项4如项1至3中任一项所述的层叠体用组合物,其中,还包含环氧树脂(f)。
项5如项1至4中任一项所述的层叠体用组合物,其中,还包含铜盐(g)。
项6如项1至5中任一项所述的层叠体用组合物,其中,还包含硫化剂(h)。
项7如项6所述的层叠体用组合物,其中,所述硫化剂(h)包含选自喹喔啉类硫化剂、硫脲类硫化剂、巯基三嗪类硫化剂、双酚类硫化剂、硫类硫化剂、过氧化物类硫化剂中的至少一种硫化剂。
项8如项1至7中任一项所述的层叠体用组合物,其中,相对于100重量份的所述环氧氯丙烷类聚合物,所述化合物(c)为0.3重量份~3.0重量份。
项9一种层叠体,其是使用上述项1至8中任一项所述的层叠体用组合物而成的。
项10一种管状体或软管体,其包含项9所述的层叠体。
项11一种汽车燃油管道,其包含项10所述的管状体或软管体。
发明效果
采用本发明的层叠体用组合物得到的层叠体在进行硫化粘结时的粘结性优异,并且在蒸气粘结时的粘结性优异。由本发明的层叠体构成的管状体或软管体能够有效地用作汽车燃油管道。
具体实施方式
本发明的层叠体用组合物至少包含:环氧氯丙烷类聚合物(a),二硫代氨基甲酸锌盐(b),选自由1,8-二氮杂双环(5.4.0)十一烯-7盐、1,5-二氮杂双环(4.3.0)-壬烯-5盐、1,8-二氮杂双环(5.4.0)十一烯-7和1,5-二氮杂双环(4.3.0)-壬烯-5所构成的组中的至少一种化合物(c),以及金属盐水合物(d)。
作为用于本发明的层叠体用组合物的环氧氯丙烷类聚合物(a)而言,具有作为来自环氧氯丙烷的结构单元[-CH2-CH(CH2Cl)-O-]的开环聚合物;具体而言,其为环氧氯丙烷的开环聚合物、环氧氯丙烷和能够与环氧氯丙烷进行共聚的单体之间的开环聚合物;可以举出环氧氯丙烷-环氧烷烃类的开环聚合物、环氧氯丙烷-缩水甘油基类的开环聚合物、环氧氯丙烷-环氧烷烃类-缩水甘油基类的开环聚合物,也可记作环氧氯丙烷橡胶。作为能够与环氧氯丙烷进行共聚的单体,可以举出环氧烷烃类(例如环氧乙烷、环氧丙烷、环氧正丁烷等)、缩水甘油基类(例如甲基缩水甘油醚、乙基缩水甘油醚、正缩水甘油醚、烯丙基缩水甘油醚、苯基缩水甘油醚等)。具体地,可列举:环氧氯丙烷均聚物、环氧氯丙烷-环氧乙烷共聚物、环氧氯丙烷-环氧丙烷共聚物、环氧氯丙烷-环氧乙烷-烯丙基缩水甘油醚三元共聚物、环氧氯丙烷-环氧乙烷-环氧丙烷-烯丙基缩水甘油醚四元共聚物等。其中优选为环氧氯丙烷均聚物、环氧氯丙烷-环氧乙烷共聚物、环氧氯丙烷-环氧乙烷-烯丙基缩水甘油醚三元共聚物。对于这些均聚物或共聚物的分子量没有特别限制,通常,以门尼粘度表示为ML1+4(100℃)=30~150左右。对这些均聚物或共聚物能够使用一种或并用两种以上。对这些均聚物或共聚物能够使用一种或并用两种以上。
从耐热性的观点出发,作为环氧氯丙烷类聚合物(a),优选含有基于环氧氯丙烷的聚合单元10mol%以上,更优选含有20mol%以上,特别优选含有25mol%以上。关于基于环氧氯丙烷的聚合单元,能够根据氯含量等来计算。氯含量能够按照JIS K7229中记载的方法,通过电位差滴定法而求得。
当使用环氧氯丙烷-环氧乙烷共聚物时,对基于环氧氯丙烷的聚合单元而言,其下限优选为10mol%以上、更优选为20mol%以上、特别优选为25mol%以上;其上限优选为95mol%以下、更优选为75mol%以下、特别优选为65mol%以下。对基于环氧乙烷的聚合单元而言,其下限优选为5mol%以上、更优选为25mol%以上、特别优选为35mol%以上;其上限优选为90mol%以下、更优选为80mol%以下、特别优选为75mol%以下。
当使用环氧氯丙烷-环氧乙烷-烯丙基缩水甘油醚三元共聚物时,对基于环氧氯丙烷的聚合单元而言,其下限优选为10mol%以上、更优选为20mol%以上、特别优选为25mol%以上;其上限优选为95mol%以下、更优选为75mol%以下、特别优选为65mol%以下。对基于环氧乙烷的聚合单元而言,其下限优选为4mol%以上、更优选为24mol%以上、特别优选为34mol%以上;其上限优选为89mol%以下、更优选为79mol%以下、特别优选为74mol%以下。对基于烯丙基缩水甘油醚的聚合单元而言,其下限优选为1mol%以上;其上限优选为10mol%以下、更优选为8mol%以下、特别优选为7mol%以下。
关于环氧氯丙烷-环氧乙烷共聚物、环氧氯丙烷-环氧乙烷-烯丙基缩水甘油醚三元共聚物的共聚组成,根据氯含量、碘值来求得。
氯含量可依据JIS K7229中记载的方法,通过电位差滴定法来进行测定。根据所得到的氯含量算出基于环氧氯丙烷的结构单元的摩尔分数。
碘值通过依据JIS K6235的方法来进行测定。根据所得到的碘值算出基于烯丙基缩水甘油醚的结构单元的摩尔分数。
基于环氧乙烷的结构单元的摩尔分数,根据基于环氧氯丙烷的结构单元的摩尔分数、基于烯丙基缩水甘油醚的结构单元的摩尔分数来算出。
作为本发明的层叠体用组合物中使用的二硫代氨基甲酸锌盐(b)的示例,可以举出N-五亚甲基二硫代氨基甲酸锌、二苄基二硫代氨基甲酸锌、N-乙基-N-苯基二硫代氨基甲酸锌、二甲基二硫代氨基甲酸锌、二乙基二硫代氨基甲酸锌、双(二甲基二硫代氨基甲酰基)亚乙基双二硫代氨基甲酸锌、二丁基二硫代氨基甲酸锌以及二戊基二硫代氨基甲酸锌,并且从提高粘结性的观点出发,更优选化合物(b)为N-五亚甲基二硫代氨基甲酸锌。
在本发明的层叠体用组合物中使用的化合物(b)的配合量,相对于100重量份的环氧氯丙烷类聚合物(a),优选为0.1重量份~4重量份,更优选为0.5重量份~3重量份,特别优选为1重量份~2重量份。
本发明的层叠体用组合物包含化合物(c),所述化合物(c)选自由1,8-二氮杂双环(5.4.0)十一烯-7盐、1,5-二氮杂双环(4.3.0)-壬烯-5盐、1,8-二氮杂双环(5.4.0)十一烯-7(在本申请中也记作DBU)和1,5-二氮杂双环(4.3.0)-壬烯-5(在本申请中也记作DBN)所构成的组中的至少一种。
作为化合物(c)的示例,可以举出:1,8-二氮杂双环(5.4.0)十一烯-7的对甲苯磺酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的苯酚盐,1,8-二氮杂双环(5.4.0)十一烯-7的酚醛树脂盐,1,8-二氮杂双环(5.4.0)十一烯-7的邻苯二甲酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的甲酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的辛酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的碳酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的硬脂酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的2-乙基己酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的苯甲酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的水杨酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的3-羟基-2-萘甲酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的2-巯基苯并咪唑盐,1,5-二氮杂双环(4.3.0)-壬烯-5的对甲苯磺酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的苯酚盐,1,5-二氮杂双环(4.3.0)-壬烯-5的酚醛树脂盐,1,5-二氮杂双环(4.3.0)-壬烯-5的邻苯二甲酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的甲酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的辛酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的碳酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的硬脂酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的2-乙基己酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的苯甲酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的水杨酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的3-羟基-2-萘甲酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的2-巯基苯并咪唑盐,1,8-二氮杂双环(5.4.0)十一烯-7,以及1,5-二氮杂双环(4.3.0)-壬烯-5等。
优选化合物(c)选自如下化合物所构成的组中的至少一种:1,8-二氮杂双环(5.4.0)十一烯-7的对甲苯磺酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的苯酚盐,1,8-二氮杂双环(5.4.0)十一烯-7的酚醛树脂盐,1,8-二氮杂双环(5.4.0)十一烯-7的邻苯二甲酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的甲酸盐,1,8-二氮杂双环(5.4.0)十一烯-7的辛酸盐,,5-二氮杂双环(4.3.0)-壬烯-5的对甲苯磺酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的苯酚盐,1,5-二氮杂双环(4.3.0)-壬烯-5的酚醛树脂盐,1,5-二氮杂双环(4.3.0)-壬烯-5的邻苯二甲酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的甲酸盐,1,5-二氮杂双环(4.3.0)-壬烯-5的辛酸盐,1,8-二氮杂双环(5.4.0)十一烯-7,以及1,5-二氮杂双环(4.3.0)-壬烯-5。
从提高粘结性的观点出发,更优选化合物(c)为1,8-二氮杂双环(5.4.0)十一烯-7的苯酚盐。
在本发明的层叠体用组合物中,相对于100重量份的(a)环氧氯丙烷类聚合物,优选化合物(c)的配合量为0.3~3.0重量份,更优选为0.5~2.0重量份,特别优选为0.5~1.5重量份。
本发明的层叠体用组合物中的金属盐水合物(d)包括:金属(钠、铝、钙、锌、锰、镧、钛、锆、铁、钴、镍、镁、铜等)的诸如硅酸、硼酸、磷酸、硫酸、硝酸和碳酸等的无机酸盐水合物,以及诸如苯甲酸、邻苯二甲酸、马来酸、琥珀酸、水杨酸、柠檬酸等羧酸的有机酸盐水合物。优选为选自金属(钠、铝、钙、锌、锰、镧、钛、锆、铁、钴、镍、镁、铜等)的乙酸盐和硫酸盐水合物,更优选为选自钠、钙、镁和铜的金属的硫酸盐和/或乙酸盐的水合物,特别优选为半水硫酸钙、二水硫酸钙和十水硫酸钠、五水硫酸铜(II)和十水硫酸镁。
在本发明的层叠体用组合物中,相对于100重量份的(a)环氧氯丙烷类聚合物,金属盐水合物(d)的配合量为0.1重量份~80重量份,优选为0.5重量份~70重量份,更优选为1重量份~50重量份,特别优选为1重量份~20重量份。在这些范围内,可获得足够的粘结效果且不损害机械物性,因此优选。
作为本发明的层叠体用组合物中使用的具有乙烯基的化合物(e),只要是具有乙烯基的化合物即可,可以是具有烯丙基的化合物、具有(甲基)丙烯酰基的化合物。作为具有乙烯基的化合物(e),优选在分子中具有两个以上的乙烯基(烯丙基、(甲基)丙烯酰基),更优选具有2至5个乙烯基(烯丙基、(甲基)丙烯酰基),特别优选具有2至4个乙烯基(烯丙基、(甲基)丙烯酰基)。另外,上述“(甲基)丙烯酰基”的意思是指“丙烯酰基”和/或“甲基丙烯酰基”。
作为具有乙烯基的化合物的示例,可以举出:诸如烷基乙烯基醚(例如甲基乙烯基醚、乙基乙烯基醚、正丙基乙烯基醚等)、烷氧基烷基乙烯基醚(例如乙氧基乙基乙烯基醚、2-甲氧基乙基乙烯基醚、2-乙氧基乙基乙烯基醚、2-丁氧基乙基乙烯基醚等)、羟烷基乙烯基醚(例如3-羟基丙基乙烯基醚、4-羟基丁基乙烯基醚等)等的单乙烯基醚化合物,诸如二乙烯基醚、乙二醇二乙烯基醚、二甘醇二乙烯基醚、三甘醇二乙烯基醚等二乙烯基醚化合物,诸如三羟甲基丙烷三乙烯基醚、季戊四醇三乙烯基醚等三乙烯基醚化合物,诸如季戊四醇四乙烯基醚、双三羟甲基丙烷四乙烯基醚等四乙烯基醚化合物等。
作为具有烯丙基的化合物,优选为烯丙酯、烯丙基醚、烯丙基胺、氰尿酸烯丙酯、异氰尿酸烯丙酯、烯丙基硫醚、烯丙基鎓,更优选为在同一分子中具有两个以上的烯丙基的化合物的多官能烯丙酯、多官能烯丙基醚、多官能烯丙基胺、多官能氰尿酸酯、多官能异氰尿酸酯、多官能烯丙基硫醚,特别优选多官能烯丙酯、多官能氰尿酸酯、多官能异氰尿酸酯。
作为多官能烯丙酯,使用选自脂肪族多官能烯丙酯、脂环族多官能烯丙酯以及芳香族多官能烯丙酯中的多官能烯丙酯。作为选自脂肪族多官能烯丙酯、脂环族多官能烯丙酯以及芳香族多官能烯丙酯中的烯丙酯,可以是其中一种或者组合其中两种以上而成。在此,所述多官能烯丙酯是指具有两个以上的烯丙酯基(-COOCH2-CH=CH2基)的化合物,所述脂肪族多官能烯丙酯是指具有脂肪烃基和两个以上的烯丙酯基的化合物,所述脂环族多官能烯丙酯是指具有脂环烃基和两个以上烯丙酯基的化合物,所述芳香族多官能烯丙酯是指具有芳烃基和两个以上的烯丙酯基的化合物。另外,在本说明书中,脂肪族多官能烯丙酯是包括两个烯丙酯基直接键合的草酸二烯丙酯的概念。
脂肪族多官能烯丙酯的具体示例可以举出:草酸二烯丙酯,丙二酸二烯丙酯,琥珀酸二烯丙酯,戊二酸二烯丙酯,己二酸二烯丙酯,庚二烯二烯丙酯,辛二酸二烯丙酯,壬二酸二烯丙酯,癸二酸二烯丙酯,富马酸二烯丙酯,马来酸二烯丙酯,柠檬酸三烯丙酯,衣康酸二烯丙酯和1,2,3,4-丁烷四甲酸四烯丙酯。
作为脂环族多官能烯丙酯的具体示例,可以举出:环丁烷二甲酸二烯丙酯,环庚烷二甲酸二烯丙酯,环己烷二甲酸二烯丙酯(六氢邻苯二甲酸二烯丙酯),降冰片烷二甲酸二烯丙酯,环丁烯二甲酸二烯丙酯,环庚烯二甲酸二烯丙酯,环己烯二甲酸二烯丙酯(四氢邻苯二甲酸二烯丙酯),降冰片烯二甲酸二烯丙酯,3-甲基-六氢-1,2-邻苯二甲酸二烯丙酯,4-甲基-六氢-1,2-邻苯二甲酸二烯丙酯,3-甲基-1,2,3,6-四氢-1,2-邻苯二甲酸二烯丙酯,4-甲基-1,2,3,6-四氢-1,2-邻苯二甲酸二烯丙酯,3,6-内亚甲基-3 1,2,3,6-四氢-1,2-邻苯二甲酸二烯丙酯,3,6-内亚甲基-4-甲基-1,2,3,6-四氢-1,2-邻苯二甲酸二烯丙酯,4-环己烯-1,2-二甲酸二烯丙酯,2-环己烯-1,2-二甲酸二烯丙酯以及1,2,3,4-丁烷四甲酸四烯丙酯等。其中,优选为1,2-环己烷二甲酸二烯丙酯、1,3-环己烷二甲酸二烯丙酯、1,4-环己烷二甲酸二烯丙酯以及降冰片烷二甲酸二烯丙酯。
作为芳香族多官能烯丙酯的示例,可以举出苯二甲酸二烯丙酯(邻苯二甲酸二烯丙酯、间苯二甲酸二烯丙酯、对苯二甲酸二烯丙酯)、苯均三酸三烯丙酯、偏苯三酸三烯丙酯、苯均四酸四烯丙酯、苯六酸六烯丙酯、苯六甲酸六烯丙酯、1,3,5,7-四烯丙基萘,其中,优选均苯三酸三烯丙酯、苯二甲酸二烯丙酯。
作为多官能烯丙基醚是指具有两个以上的烯丙基醚基(-O-CH2-CH=CH2基)的化合物,作为示例可以举出乙二醇二烯丙基醚、二甘醇二烯丙基醚、聚乙二醇二烯丙基醚、丙二醇二烯丙基醚、丁二醇二烯丙基醚、己二醇二烯丙基醚、双酚A烯化氧二乙烯基醚、双酚F的烯化氧二乙烯基醚、三羟甲基丙烷三烯丙基醚、三羟甲基丙烷四烯丙基醚、甘油三烯丙基醚、季戊四醇四烯丙基醚、二季戊四醇五烯丙基醚、二季戊四醇六烯丙基醚、聚乙二醇二烯丙基醚、季戊四醇二烯丙基醚、季戊四醇三烯丙基醚、季戊四醇四烯丙基醚、1,4-二烯丙基氧基甲基苯、环氧乙烷加成的三羟甲基丙烷三烯丙基醚、环氧乙烷加成的三羟甲基丙烷四烯丙基醚、环氧乙烷加成的季戊四醇四烯丙基醚、环氧乙烷加成的二季戊四醇六烯丙基醚,优选为聚乙二醇二烯丙基醚。
作为多官能烯丙基胺是指具有两个以上的烯丙基(-CH2-CH=CH2基)的胺,优选以具有-NH-CO-NH-的脂环族或二脂环族化合物为骨架且具有两个以上的烯丙基(-CH2-CH=CH2基)的胺,更优选为具有甘脲骨架且具有两个以上的烯丙基(-CH2-CH=CH2基)的胺。作为多官能烯丙胺的示例可以举出二烯丙基胺、二烯丙基甲胺、二烯丙基乙胺、三烯丙基胺以及1,3,4,6-四丙烯基甘脲。
多官能氰尿酸烯丙酯是具有烯丙基和氰尿酸骨架的化合物,可以列举氰尿酸烯丙酯、氰尿酸二烯丙酯、氰尿酸三烯丙酯等。
多官能异氰尿酸烯丙酯是具有烯丙基和异氰尿酸骨架的化合物,可以列举异氰尿酸烯丙酯、异氰尿酸二烯丙酯和异氰尿酸三烯丙酯。
作为多官能烯丙基硫醚是具有两个以上的烯丙基(-CH2-CH=CH2基)和硫醚结构的化合物,可以例举出亚烷基二醇二烯丙基硫醚。
作为烯丙基鎓可以例示:单官能烯丙基鎓和多官能烯丙基鎓,单烯丙基三烷基铵盐、二烯丙基二烷基铵盐、三烯丙基单烷基铵盐等,以及它们的氯化物、溴化物和碘化物等。
作为具有烯丙基的化合物,可以优选:对苯二甲酸二烯丙酯、二烯丙基邻苯二甲酸酯、间苯二甲酸二烯丙酯、对苯二甲酸二烯丙酯、三羟甲基丙烷二烯丙基醚、季戊四醇二烯丙基醚、双酚A二烯丙基醚、双酚F二烯丙基醚、丙二醇二烯丙基醚、甘油二烯丙基醚、1,2-环己烷二甲酸二烯丙酯、1,3-环己烷二甲酸二烯丙酯、1,4-环己烷二甲酸二烯丙酯等二烯丙基化合物,氰尿酸三烯丙酯、异氰尿酸三烯丙酯、偏苯三酸三烯丙酯、均苯三酸三烯丙酯、三羟甲基丙烷三烯丙基醚、季戊四醇三烯丙基醚等三烯丙基化合物等。
作为具有(甲基)丙烯酰基的化合物,例如,可以举出:(甲基)丙烯酸丁酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸十八烷基酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸四氢糠酯、(甲基)丙烯酸羟乙酯等(甲基)丙烯酸烷基酯,甲氧基丙二醇(甲基)丙烯酸酯、乙氧基二乙二醇(甲基)丙烯酸酯等烷氧基亚烷基二醇(甲基)丙烯酸酯等单(甲基)丙烯酸酯;新戊二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯等亚烷基二醇二(甲基)丙烯酸酯,二丙二醇二(甲基)丙烯酸酯、三丙二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯等烷二醇二(甲基)丙烯酸酯等的二官能(甲基)丙烯酸酯;三羟甲基丙烷三(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、环氧乙烷/环氧丙烷改性三羟甲基丙烷三丙烯酸酯等三官能(甲基)丙烯酸酯;季戊四醇四(甲基)丙烯酸酯、双三羟甲基丙烷四(甲基)丙烯酸酯等四官能(甲基)丙烯酸酯。
在本发明的层叠体用组合物中的化合物(e)的配合量,相对于100重量份的环氧氯丙烷类聚合物(a),优选为1重量份~20重量份,更优选为2重量份~15重量份,特别优选为3重量份~10重量份。
本发明的粘结用组合物,包含环氧氯丙烷类聚合物(a)、化合物(b)、化合物(c)和金属盐水合物(d)作为必要组分,进而还可以包含环氧树脂(f)作为任选组分。
作为环氧树脂(f),例如优选为选自由双酚A型环氧树脂、双酚F型环氧树脂、苯酚酚醛清漆型环氧树脂、邻甲酚酚醛清漆型环氧树脂、胺型环氧树脂、氢化双酚A型环氧树脂以及多官能环氧树脂所组成的组中的至少一种树脂。其中,从耐化学性和粘结性良好的观点出发,优选双酚A型环氧树脂,并且,特别优选下列式(1)所示的环氧树脂。
其中,式(1)中,n为平均值,优选为0.1~3,更优选为0.1~0.5,进一步优选为0.1~0.3。
相对于100重量份的环氧氯丙烷类聚合物(a),优选环氧树脂(f)为0.1重量份~5重量份的范围,更优选为0.3重量份~3重量份。
另外,在本发明的层叠体用组合物中,相对于100重量份的环氧氯丙烷类聚合物(a),化合物(c)与环氧树脂(f)的总量超过2.0重量份也是优选形式之一。
从提高粘结性的观点出发,优选层叠体用组合物还含有铜盐(g)。
作为铜盐(g),优选有机铜盐。作为有机铜盐,可以举出:饱和羧酸(例如甲酸、乙酸、丁酸和硬脂酸等)的铜盐,不饱和羧酸(例如油酸和亚油酸等)的铜盐,芳族羧酸(例如水杨酸、苯甲酸和邻苯二甲酸等)的铜盐,二羧酸(例如草酸、琥珀酸、己二酸、马来酸和富马酸等)的铜盐,羟基酸(例如乳酸和柠檬酸等)的铜盐,氨基甲酸的铜盐,硫代氨基甲酸以及磺酸等的铜盐(例如二甲基二硫代氨基甲酸铜、二乙基二硫代氨基甲酸铜、二丁基二硫代氨基甲酸铜、N-乙基-N-苯基二硫代氨基甲酸铜、N-五亚甲基二硫代氨基甲酸铜和二苄基二硫代氨基甲酸铜)。作为有机铜盐,优选饱和羧酸的铜盐、不饱和羧酸的铜盐、芳族羧酸的铜盐、硫代氨基甲酸的铜盐,更优选硬脂酸铜、二甲基二硫代氨基甲酸铜、二乙基二硫代氨基甲酸铜、二丁基二硫代氨基甲酸铜。
从提高粘结性的观点出发,相对于100重量份的环氧氯丙烷类聚合物(a),铜盐(g)的配合量为0.01重量份~5重量份,优选为0.05重量份~3重量份。进一步优选为0.1重量份~2重量份。在这些范围内,可获得足够的粘结效果且不损害硫化产品的机械物性,因此优选。
本发明的层叠体用组合物含有硫化剂(h)。作为硫化剂(h),能够使用以往公知的硫化剂。
作为硫化剂(h),可以举出利用氯原子反应性的公知硫化剂,例如多胺类硫化剂、硫脲类硫化剂、噻二唑类硫化剂、巯基三嗪类硫化剂、吡嗪类硫化剂、喹喔啉类硫化剂、双酚类硫化剂等。
对于利用氯原子反应性的公知的硫化剂(h)的示例而言,作为多胺类硫化剂,可列举乙二胺、六亚甲基二胺、二亚乙基三胺、三亚乙基四胺、六亚甲基四胺、对苯二胺、异丙基苯二胺(cumene diamine)、N,N'-双肉桂醛缩-1,6-己二胺、乙二胺氨基甲酸酯、六亚甲基二胺氨基甲酸酯等。
作为硫脲类硫化剂,可列举:亚乙基硫脲、1,3-二乙基硫脲、1,3-二丁基硫脲、三甲基硫脲等。
作为噻二唑类硫化剂,可列举:2,5-二巯基-1,3,4-噻二唑、2-巯基-1,3,4-噻二唑-5-硫代苯甲酸酯等。
作为巯基三嗪类硫化剂,可列举2,4,6-三巯基-1,3,5-三嗪、2-甲氧基-4,6-二巯基三嗪、2-己基氨基-4,6-二巯基三嗪、2-二乙基氨基-4,6-二巯基三嗪、2-环己烷氨基-4,6-二巯基三嗪、2-二丁基氨基-4,6-二巯基三嗪、2-苯胺基-4,6-二巯基三嗪、2-苯基氨基-4,6-二巯基三嗪等。
作为吡嗪类硫化剂可以举出2,3-二巯基吡嗪衍生物等;并且,作为2,3-二巯基吡嗪衍生物的示例可以举出:吡嗪-2,3-二硫代碳酸酯、5-甲基-2,3-二巯基吡嗪、5-乙基吡嗪-2,3-二硫代碳酸酯、5,6-二甲基-2,3-二巯基吡嗪以及5,6-二甲基吡嗪-2,3-二硫代碳酸酯等。
作为喹喔啉类硫化剂的示例可以举出2,3-二巯基喹喔啉衍生物等;并且,作为2,3-二巯基喹喔啉衍生物的示例可以举出喹喔啉-2,3-二硫代碳酸酯、6-甲基喹喔啉-2,3-二硫代碳酸酯、6-乙基-2,3-二巯基喹喔啉、6-异丙基喹喔啉-2,3-二硫代碳酸酯、5,8-二甲基喹喔啉-2,3-二硫代碳酸酯等。
作为双酚类硫化剂可以例示4,4'-二羟基二苯基亚砜、4,4'-二羟基二苯基砜(双酚S)、1,1-亚环己基-双(4-羟基苯)、2-氯-1,4-亚环己基-双(4-羟基苯)、2,2-异亚丙基-双(4-羟基苯)(双酚A)、六氟异亚丙基-双(4-羟基苯)(双酚AF)和2-氟-1,4-亚苯基-双(4-羟基苯)等。
本发明中,可将公知的硫化促进剂和延迟剂与硫化剂(h)一起用于本发明的层叠体用组合物中。作为与利用氯原子反应性的已知硫化剂(h)组合使用的硫化促进剂可举出:伯胺、仲胺和叔胺,这些胺的有机酸盐或它们的加合物,胍类促进剂,秋兰姆类促进剂,二硫代氨基甲酸类促进剂等。另外,作为延迟剂,可列举N-环己基硫代邻苯二甲酰亚胺等。
作为硫化促进剂,作为伯胺、仲胺和叔胺,特别优选具有5个至20个碳原子的脂族或环状脂肪酸的伯胺、仲胺或叔胺;这种胺的代表示例是正己胺、辛胺、二丁胺、三丁胺、六亚甲基二胺等。
作为与胺形成盐的有机酸的示例可举出羧酸、氨基甲酸、2-巯基苯并噻唑、二硫代磷酸等。此外,作为与所述胺形成加合物的物质可例示出醇类、肟类等。作为胺的有机酸盐或加合物的具体示例,可举出正丁胺·乙酸盐、六亚甲基二胺·氨基甲酸盐和2-巯基苯并噻唑的二环己胺盐。
作为胍促进剂的示例可举出二苯基胍、二甲苯基胍等。
作为秋兰姆类硫化促进剂的具体示例可举出:二硫化四甲基秋兰姆、一硫化四甲基秋兰姆、二硫化四乙基秋兰姆、二硫化四丁基秋兰姆、四硫化二十四烷基秋兰姆物。
作为与利用氯原子的反应性的已知硫化剂(h)组合使用的硫化促进剂或延迟剂的配合量,相对于100重量份的环氧氯丙烷类聚合物(a),优选为0重量份~10重量份,更优选为0.1重量份~5重量份。
此外,当环氧氯丙烷类聚合物(a)是具有双键的聚合物(例如,环氧氯丙烷-烯丙基缩水甘油醚共聚物、环氧氯丙烷-环氧乙烷-烯丙基缩水甘油醚三元共聚物等)时,可以举出公知的通常用于丁腈橡胶的硫化的硫化剂,如硫类硫化剂、过氧化物类硫化剂、树脂类硫化剂、醌二肟类硫化剂等。
作为硫类硫化剂可举出硫、二硫化吗啉、二硫化四甲基秋兰姆、二硫化四乙基秋兰姆、二硫化四丁基秋兰姆、N,N'-二甲基-N,N’-二硫化二苯基秋兰姆、四硫化二十烷基二硫化秋兰姆、四硫化二亚甲基秋兰姆和六硫化二亚甲基秋兰姆。
作为过氧化物硫化剂,可列举叔丁基过氧化氢、对萜烷过氧化氢、过氧化二异丙苯、过氧化叔丁基、1,3-二(叔丁基过氧基异丙基)苯、2,5-二甲基-2,5-二(叔丁基过氧基)己烷、过氧化苯甲酰、叔丁基过氧化苯甲酸酯。
作为树脂类硫化剂可举出烷基酚甲醛树脂。
作为醌二肟类硫化剂可举出对醌二肟和对-对-二苯甲酰基醌二肟。
作为与硫类硫化剂、过氧化物类硫化剂、树脂类硫化剂、醌二肟类硫化剂组合使用的硫化促进剂、硫化延迟剂,硫化促进助剂、交联助剂,例如可举出:醛氨类促进剂、醛胺类促进剂、硫脲类促进剂、胍类促进剂、噻唑类促进剂、次磺酰胺类促进剂、秋兰姆类促进剂、二硫代氨基甲酸盐类促进剂、黄原酸盐类促进剂等的各种硫化促进剂,N-亚硝基二苯胺、邻苯二甲酸酐、N-环己基硫代邻苯二甲酰亚胺等硫化延迟剂,锌华、硬脂酸、硬脂酸锌等硫化促进助剂,醌二肟类交联助剂,甲基丙烯酸酯类交联助剂,烯丙基类交联助剂,马来酰亚胺类交联助剂等。
作为与硫类硫化剂、过氧化物类硫化剂、树脂类硫化剂、醌二肟类硫化剂组合使用的硫化促进剂、硫化延迟剂、硫化促进助剂、交联助剂的配合量,相对于100重量份的环氧氯丙烷类聚合物(a),优选为0重量份至10重量份,更优选为0.1重量份至5重量份。
本发明的层叠体用组合物中,优选为选自由硫脲类硫化剂、喹喔啉类硫化剂、硫类硫化剂、过氧化物类硫化剂、巯基三嗪类硫化剂以及双酚类硫化剂所构成的组中的至少一种硫化剂,更优选为选自由硫脲类硫化剂、喹喔啉类硫化剂和双酚类硫化剂中的至少一种硫化剂,特别优选为喹喔啉类硫化剂。对这些硫化剂(h)可以单独使用或混合两种以上使用。
在本发明的层叠体用组合物中,相对于100重量份的(a)环氧氯丙烷类聚合物、优选含有硫化剂(h)为0.1重量份~10重量份。更优选为0.5重量份~5重量份。
在本发明的层叠体用组合物中,可含有丙烯腈-丁二烯橡胶(NBR)、氢化NBR(H-NBR)、丙烯酸橡胶(ACM)、乙烯丙烯酸酯橡胶(AEM)、氟橡胶(FKM)、氯丁二烯橡胶(CR)、氯磺化聚乙烯(CSM)、氯化聚乙烯(CPE)、乙丙橡胶(EPM、EPDM)等任何橡胶。在该情况下,相对于100重量份的环氧氯丙烷类聚合物(a),优选橡胶的配合量为1重量份~50重量份。
在本发明的层叠体用组合物中,可以进一步含有除了环氧树脂之外的其它树脂。作为树脂,例如可举出聚甲基丙烯酸甲酯(PMMA)树脂、聚苯乙烯(PS)树脂、聚氨酯(PUR)树脂、聚氯乙烯(PVC)树脂、乙烯-乙酸乙烯酯(EVA)树脂、苯乙烯-丙烯腈(AS)树脂和聚乙烯(PE)树脂。
在该情况下,相对于100重量份的环氧氯丙烷类聚合物(a),优选树脂的配合量为1重量份~50重量份。
另外,在本发明中,可以根据目的或需要,在不损害本发明的效果的范围内,配合普通橡胶组合物中所配合的普通添加物,例如,填充剂、加工助剂、增塑剂、缚酸剂、软化剂、抗老化剂、着色剂、稳定剂、粘结助剂、脱模剂、导电性赋予剂、导热性赋予剂、表面非粘合剂、粘合赋予剂、柔软性赋予剂、耐热性改良剂、阻燃剂、紫外线吸收剂、耐油性改进剂、发泡剂、防焦剂、润滑剂等各种添加剂。另外,也可以配合一种或两种以上与上述物质不同的常用硫化剂及硫化促进剂。
作为填充剂,可列举:二硫化钼、硫化铁、硫化铜等金属硫化物;硅藻土、石棉、立德粉(硫化锌/硫化钡)、石墨、炭黑、氟化碳、氟化钙、焦炭、石英微粉、滑石、云母粉、硅灰石、碳纤维、芳纶纤维、各种晶须、玻璃纤维、有机增强剂、有机填充剂等。
作为加工助剂,可列举:硬脂酸、油酸、棕榈酸、月桂酸等高级脂肪酸;硬脂酸钠、硬脂酸锌等高级脂肪酸盐;硬脂酸酰胺、油酸酰胺等高级脂肪酸酰胺;油酸乙酯等高级脂肪酸酯、十八烷基胺、油胺等高级脂肪族胺;巴西棕榈蜡、地蜡等石油类蜡;乙二醇、甘油、二乙二醇等聚乙二醇;凡士林、石蜡等脂肪族烃;硅油、有机硅类聚合物、低分子量聚乙烯、苯二甲酸酯类、磷酸酯类、松香、(卤化)二烷基胺、(卤化)二烷基砜、表面活性剂等。
作为增塑剂,例如,可列举苯二甲酸衍生物及癸二酸衍生物;作为软化剂,例如,可列举润滑油、工艺油、煤焦油、蓖麻油、硬脂酸钙;作为抗老化剂,例如,可列举苯二胺类、磷酸盐类、喹啉类、甲酚类、苯酚类、二硫代氨基甲酸酯金属盐等。
本发明的层叠体用组合物,通过将前述环氧氯丙烷类聚合物(a)、前述化合物(b)、前述化合物(c)、前述金属盐水合物(d)以及根据需要使用的化合物(e)、环氧树脂(f)、铜盐(g)、硫化剂(h)和其它添加剂进行混炼而制备。
混炼能够在100℃以下的温度下使用开口辊、密炼机、加压捏合机等来进行。
通过使用本发明的层叠体用组合物,能够形成与其它种类聚合物组合物的层叠体。作为层叠体的制造方法,可例示如下方法:将层叠体用组合物与其它种类的聚合物组合物进行层叠,并使其加热硫化且粘结。加热温度为100℃~200℃,硫化时间根据温度的不同而异,通常在0.5分钟~300分钟之间进行。作为加热方法,能够使用任意方法,例如,利用模具压缩成型、注塑成型且利用蒸气、紫外线或微波来进行加热等。
当制造上述层叠体时,无需特别复杂的工序,由于硫化时能够获得牢固的化学粘结,因此能够提供即使在暴露于恶劣的条件的情况下,也具有充分粘结力的层叠体。另外,关于成型性,能够在低成本下成型且成型也很容易。另外,由于能够通过挤压成型等普通方法成型,因此可实现薄膜化,且在柔软性方面也得到改善。
作为其它种类的聚合物层,可例示低透气性聚合物层,作为低透气性聚合物层,优选为含氟的聚合物层。
作为用于低透气性聚合物层的聚合物,可列举:偏二氟乙烯-六氟丙烯二元共聚物、四氟乙烯-六氟丙烯二元共聚物、偏二氟乙烯-六氟丙烯-四氟乙烯三元共聚物、偏二氟乙烯-全氟烷基乙烯基醚-四氟乙烯三元共聚物、四氟乙烯-全氟乙基乙烯基醚共聚物、四氟乙烯-全氟丙基乙烯基醚共聚物、四氟乙烯-全氟烷基乙烯基醚-三氟氯乙烯三元共聚物、四氟乙烯-丙烯二元共聚物、偏二氟乙烯-四氟乙烯-四氟乙烯三元共聚物、乙烯-四氟乙烯二元共聚物、聚偏二氟乙烯、聚四氟乙烯、聚氯三氟乙烯(PCTFE)、氯三氟乙烯(CTFE)共聚物、聚偏二氯乙烯树脂、聚乙烯基醇树脂、乙烯-乙烯基醇共聚物树脂、尼龙树脂、聚丙烯腈树脂、聚酯树脂等;优选为偏二氟乙烯-六氟丙烯二元共聚物、四氟乙烯-六氟丙烯二元共聚物、偏二氟乙烯-六氟丙烯-四氟乙烯三元共聚物、偏二氟乙烯-全氟烷基乙烯基醚-四氟乙烯三元共聚物、四氟乙烯-全氟乙基乙烯基醚共聚物、四氟乙烯-全氟丙基乙烯基醚共聚物、四氟乙烯-全氟烷基乙烯基醚-三氟氯乙烯三元共聚物、四氟乙烯-丙烯二元共聚物、偏二氟乙烯-四氟乙烯-四氟乙烯三元共聚物、乙烯-四氟乙烯二元共聚物、聚偏二氟乙烯、聚四氟乙烯、氯三氟乙烯(CTFE)、聚氯三氟乙烯(PCTFE)、共聚物;特别优选为氯三氟乙烯(CTFE)共聚物。
作为CTFE共聚物,优选包括:来自CTFE的共聚单元(CTFE单元);以及,来自选自由四氟乙烯(TFE)、六氟丙烯(HFP)、全氟(烷基乙烯基醚)(PAVE)、偏二氟乙烯(VdF)、氟乙烯、六氟异丁烯、式CH2=CX1(CF2)nX2(式中、X1为H或F,X2为H、F或Cl,n为1~10的整数)所示的单体、乙烯、丙烯、1-丁烯、2-丁烯、氯乙烯及偏二氯乙烯构成的组中的至少一种单体的共聚单元。另外,作为CTFE共聚物,更优选为全卤聚合物。
作为CTFE共聚物,更优选包含CTFE单元和来自选自由TFE、HFP及PAVE构成的组中的至少一种单体的共聚单元,进一步优选实质上仅由这些共聚单元构成。另外,从低燃油浸透性的观点考虑,优选包含乙烯、偏二氟乙烯、氟乙烯等具有CH键的单体。通常,全卤聚合物难以与橡胶粘结,但根据本发明的配置,即使氟树脂层是由全卤聚合物构成的层,氟树脂层和橡胶层的层之间也能够牢固地粘结。
CTFE共聚物优选具有全部单体单元的10摩尔%~90摩尔%的CTFE单元。
作为CTFE共聚物,特别优选包含CTFE单元、TFE单元、以及可与它们共聚的单体(α)来源的单体(α)单元的共聚物。
在CTFE共聚物的分子结构上,“CTFE单元”和“TFE单元”分别为来自CTFE的部分(-CFCl-CF2-)、来自TFE的部分(-CF2-CF2-),在CTFE类共聚物的分子结构上,所述“单体(α)单元”同样为单体(α)加成而成的部分。
作为单体(α),只要是能够与CTFE和TFE进行共聚的单体即可,没有特别限定,可列举:乙烯(Et)、偏二氟乙烯(VdF)、CF2=CF-ORf1(式中,Rf1为碳原子数1~8的全氟烷基)所表示的全氟(烷基乙烯基醚)(PAVE)、CX3X4=CX5(CF2)nX6(式中,X3、X4及X5相同或不同,为氢原子或氟原子;X6为氢原子、氟原子或氯原子;n为1~10的整数)所表示的乙烯基单体、CF2=CF-OCH2-Rf2(式中,Rf2为碳原子数1~5的全氟烷基)所表示的烷基全氟乙烯基醚衍生物等,其中,优选为选自由PAVE、上述乙烯基单体及烷基全氟乙烯基醚衍生物构成的组中的至少一种,更优选为由PAVE及HFP构成的组中的至少一种。
作为烷基全氟乙烯基醚衍生物,优选为Rf2为碳原子数1~3的全氟烷基的物质,更优选为CF2=CF-OCH2-CF2CF3。
在CTFE共聚物中,作为CTFE单元和TFE单元的比率,CTFE单元为15摩尔%~90摩尔%,TFE单元为85摩尔%~10摩尔%,更优选地,CTFE单元为20摩尔%~90摩尔%,TFE单元为80摩尔%~10摩尔%。另外,更优选由15摩尔%~25摩尔%CTFE单元和85摩尔%~75摩尔%TFE单元构成的物质。
CTFE共聚物优选为CTFE单元和TFE单元的合计为90摩尔%~99.9摩尔%、单体(α)单元为0.1摩尔%~10摩尔%的物质。若单体(α)单元低于0.1摩尔%,则成型性、耐环境应力开裂性及耐燃油开裂性容易变差;若超过10摩尔%,则存在低燃油浸透性、耐热性、机械性能变差的倾向。
氟聚合物(b1)最优选为PCTFE或CTFE-TFE-PAVE共聚物。上述CTFE-TFE-PAVE共聚物是实质上仅由CTFE、TFE及PAVE构成的共聚物。PCTFE及CTFE-TFE-PAVE共聚物中不存在直接键合在构成主链的碳原子上的氢原子,不会产生脱氟氢化反应。因此,利用通过脱氟氢化反应在氟聚合物中所形成的不饱和键的现有粘结性改善方法并不适用。
作为PAVE,可列举:全氟(甲基乙烯基醚)(PMVE)、全氟(乙基乙烯基醚)(PEVE)、全氟(丙基乙烯基醚)(PPVE)、全氟(丁基乙烯基醚)等,其中,优选为选自由PMVE、PEVE及PPVE构成的组中的至少一种。
PAVE单元优选为全部单体单元的0.5摩尔%以上且5摩尔%以下。
CTFE单元等的结构单元是通过进行19F-NMR分析而得到的值。
氟聚合物(b1)可以是在聚合物的主链末端和/或侧链上导入有选自由羰基、羟基、杂环基及氨基构成的组中的至少一种反应性官能团的物质。
在本说明书中,“羰基”是由碳-氧双键构成的碳二价基团,以-C(=O)-表示的基团为代表。作为包含所述羰基的反应性官能团,没有特别限定,可列举包含羰基作为化学结构上的一部分的基团,例如碳酸酯基、羧酸卤化物基(卤代甲酰基)、甲酰基、羧基、酯键(-C(=O)O-)、酸酐键(-C(=O)O-C(=O)-)、异氰酸酯基、酰胺基、酰亚胺基(-C(=O)-NH-C(=O)-)、氨酯键(-NH-C(=O)O-)、氨基甲酰基(NH2-C(=O)-)、氨基甲酰氧基(NH2-C(=O)O-)、脲基(NH2-C(=O)-NH-)、氨基乙二酰基(NH2-C(=O)-C(=O)-)等。
在酰胺基、酰亚胺基、氨酯键、氨基甲酰基、氨基甲酰氧基、脲基、氨基乙二酰基等中,与其氮原子键合的氢原子可以被例如烷基等烃基取代。
作为反应性官能团,从容易导入方面以及氟聚合物(b1)具有适当的耐热性和较低温度下的良好粘结性的方面考虑,优选酰胺基、氨基甲酰基、羟基、羧基、碳酸酯基、羧酸卤化物基、酸酐键,进一步优选酰胺基、氨基甲酰基、羟基、碳酸酯基、羧酸卤化物基、酸酐键。
根据目的,向与层叠体用组合物层叠的聚合物层中添加公知的配合剂,例如,交联剂(硫化剂)、硫化促进剂、稳定剂、着色剂、增塑剂、增强剂等。
作为将本发明的层叠体用于燃料油系统的软管体时的形式,作为代表,可列举:在软管体的内层配设有含氟的聚合物、其外层配设有环氧氯丙烷类聚合物的双层软管体、且在双层软管体的外侧配置编织强化层的三层软管体;或者,进一步在三层软管体的外侧配设橡胶层的四层结构的软管体等。作为用于上述三层软管体或四层软管体的编织材料,通常使用聚酯纤维、聚酰胺纤维、玻璃纤维、维纶纤维、棉花等的编织物。另外,作为用于上述四层软管体的最外层的材料,除环氧氯丙烷类聚合物之外,通常使用乙烯-丙烯酸酯橡胶、氯丁橡胶、氯化聚乙烯橡胶、氯磺化聚乙烯等具有耐热老化性、耐候性以及耐油性等的合成橡胶。
下面,作为实施例,将列举代表性的示例,但本发明不限定于此。
实施例、比较例
按照表1所示的配合方式,将各材料使用捏合机和开口辊进行混炼,得到厚度2mm~2.5mm的片状层叠体用组合物(i)。
(加压硫化粘结层叠体)
将上述片材(i)与厚度0.3mm~0.5mm的低透气性聚合物层(ii)进行贴合,在160℃、20kg/cm2~25kg/cm2下对贴合体加压30分钟,得到厚度2.0mm~2.5mm的橡胶-树脂层叠体。
(蒸气硫化粘结层叠体)
将上述片材(i)与厚度0.3mm~0.5mm的低透气性聚合物层(ii)进行贴合,在160℃、20kg/cm2~25kg/cm2下对贴合体加压4分钟,得到厚度2.0mm~2.5mm的片材(iii)。
将上述片材(iii)在硫化罐中在0.52kPa(160℃)下硫化30分钟,得到厚度为2.0mm至2.5mm的橡胶-树脂层叠体。
作为低透气性聚合物层(ii),使用CTFE/TFE/PPVE[21.3/76.3/2.4(mol%)]共聚物的氟树脂。
(90℃剥离试验粘结评价)
将上述加压硫化粘结层叠体、蒸气硫化粘结层叠体切割为1.0cm×10cm的条带状,制成粘结试验用试件,在25℃下以50mm/min的拉伸速度进行90℃剥离试验,并通过目测观察剥离状态。将剥离试验的结果示于表2。
(180°弯曲粘结评价)
针对上述条带状粘结试验用的试验片的低透气性聚合物层(ii)用切刀切割并弯曲180°,通过目视观察切割部分的剥离状态。将剥离试验的结果示于表2。
90°剥离试验(剥离状态评价)
○:牢固地粘结,层间产生了橡胶破坏;
△:材料未破坏但彼此粘结;
×:完全未粘结,界面产生剥离。
180°弯曲试验(剥离状态评价)
○:整个切口牢固粘结。
△:切口部位的一部分剥离。
×:整个切口剥离。
下面示出了实施例和比较例中所用的配合剂。
*1株式会社大阪曹达制造的“EPICHLOMER CG”
*2东海碳素株式会社制造的“SEAST 3”
*3东海碳素株式会社制造的“SEAST SO”
*4Burgess Pigment公司制造的“BURGESS#30”
*5株式会社ADEKA制造的“ADEKACIZER RS-107”
*6花王株式会社制造的“SPLENDER R-300”
*7大内新兴化学株式会社制造的“NOCRAC NBC”
*8大内新兴化学株式会社制造的“NOCCELER TTCu”
*9协和化学工业株式会社制造的“Kyowamag#150”
*10协和化学工业株式会社制造的“DHT-4A”
*11三菱化学株式会社制造的“JER828”
*12大内新兴化学株式会社制造的“NOCTIZER SS”
*13San-Apro株式会社制造的“U-CAT SA-1”
*14大内新兴化学株式会社制造的“RETARDER CTP”
*15株式会社大阪曹达制造的“DAISONET XL21-S”
表1
配合(单位:重量份) | 实施例1 | 实施例2 | 比较例1 | 比较例2 |
环氧氯丙烷类聚合物*1 | 100 | 100 | 100 | 100 |
HAF碳*2(填充剂) | 25 | 25 | 30 | 25 |
FEF碳*3(填充剂) | 30 | 30 | 30 | 30 |
硬质粘土*4 | 15 | 15 | 15 | 15 |
己二酸二(丁氧基乙氧基)乙酯*5 | 10 | 10 | 10 | 10 |
山梨醇酐单硬酸酯*6 | 3 | 3 | 3 | 3 |
二丁基二硫代氨基甲酸镍*7 | 1 | 1 | 1 | 1 |
二甲基二硫代氨基甲酸铜*8 | 0.5 | 0.5 | 0.5 | 0.5 |
氧化镁*9 | 3 | 3 | 3 | 3 |
合成水滑石*10 | 3 | 3 | 3 | 3 |
环氧树脂*11 | 1.5 | 1.5 | 1.5 | 1.5 |
2,2-二苯甲酰氨基二苯二硫*12 | 1 | 1 | 1 | 1 |
异氰尿酸三烯丙脂 | 5 | 5 | 5 | 5 |
DBU的酚盐*13 | 1 | 1 | 1 | 1 |
半水硫酸钙 | 5 | 5 | 5 | 5 |
亚乙基硫脲 | 0.5 | 0.5 | 0.5 | 0.5 |
N-五亚甲基二硫代氨基甲酸锌 | 1 | 2 | ||
异丙基黄原酸锌 | 1 | |||
N-环己基硫代邻苯二甲酰亚胺*14 | 1 | 1 | 1 | 1 |
喹喔啉类硫化剂*15 | 1.7 | 1.7 | 1.7 | 1.7 |
表2
实施例1 | 实施例2 | 比较例1 | 比较例2 | |
90°剥离试验(加压) | ○ | ○ | ○ | × |
180°弯曲试验(加压) | ○ | ○ | △ | × |
90°剥离试验(蒸气) | ○ | ○ | △ | × |
180°弯曲试验(蒸气) | ○ | ○ | × | × |
如表2所示,通过使用实施例的层叠体用组合物的层叠体与使用比较例的层叠体用组合物的层叠体进行比较,能够确认在90°剥离试验、180°弯曲试验中有牢固的粘结性。
工业实用性
本发明能够提高所得到的硫化物与其它物质(例如,其它种类聚合物)的粘结性优异的层叠体用组合物,能够应用于例如与含氟的聚合物的层叠体等。
Claims (11)
1.一种层叠体用组合物,其特征在于,其包含:
环氧氯丙烷类聚合物(a),二硫代氨基甲酸锌盐(b),选自由1,8-二氮杂双环(5.4.0)十一烯-7盐、1,5-二氮杂双环(4.3.0)-壬烯-5盐、1,8-二氮杂双环(5.4.0)十一烯-7和1,5-二氮杂双环(4.3.0)-壬烯-5所构成的组中的至少一种化合物(c),以及金属盐水合物(d)。
2.如权利要求1所述的层叠体用组合物,其特征在于,还包含具有乙烯基的化合物(e)。
3.如权利要求1或2中任一项所述的层叠体用组合物,其中,
相对于100重量份的所述环氧氯丙烷类聚合物(a),所述金属盐水合物(d)为0.1重量份~80重量份。
4.如权利要求1至3中任一项所述的层叠体用组合物,其中,
还包含环氧树脂(f)。
5.如权利要求1至4中任一项所述的层叠体用组合物,其中,
还包含铜盐(g)。
6.如权利要求1至5中任一项所述的层叠体用组合物,其中,
还包含硫化剂(h)。
7.如权利要求6所述的层叠体用组合物,其中,
所述硫化剂(h)包含选自喹喔啉类硫化剂、硫脲类硫化剂、巯基三嗪类硫化剂、双酚类硫化剂、硫类硫化剂、过氧化物类硫化剂中的至少一种硫化剂。
8.如权利要求1至7中任一项所述的层叠体用组合物,其中,
相对于100重量份的所述环氧氯丙烷类聚合物,所述化合物(c)为0.3重量份~3.0重量份。
9.一种层叠体,其是使用权利要求1至8中任一项所述的层叠体用组合物而成的。
10.一种管状体或软管体,其包含权利要求9所述的层叠体。
11.一种汽车燃油管道,其包含权利要求10所述的管状体或软管体。
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JP2003253112A (ja) * | 2002-03-01 | 2003-09-10 | Daiso Co Ltd | 加硫用ゴム組成物およびその加硫物 |
CN101046265A (zh) * | 2006-03-28 | 2007-10-03 | 东海橡胶工业株式会社 | 燃料胶管 |
JP2008266558A (ja) * | 2007-03-27 | 2008-11-06 | Tokai Rubber Ind Ltd | ヒドリンゴム組成物 |
JP2013043400A (ja) * | 2011-08-25 | 2013-03-04 | Daiso Co Ltd | 積層体及びその製造方法 |
CN103249794A (zh) * | 2010-11-12 | 2013-08-14 | 大曹株式会社 | 加硫粘结用组合物 |
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DE3127081C2 (de) | 1981-07-09 | 1985-01-24 | Degussa Ag, 6000 Frankfurt | Vorrichtung zur Messung der Strömungsgeschwindigkeit von Gasen und Flüssigkeiten |
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JP3106925B2 (ja) | 1995-09-21 | 2000-11-06 | ダイソー株式会社 | 加硫ゴム積層体 |
EP1704994B1 (en) | 2005-03-25 | 2008-12-31 | Daiso Co., Ltd. | Vulcanized rubber laminate |
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JP2003253112A (ja) * | 2002-03-01 | 2003-09-10 | Daiso Co Ltd | 加硫用ゴム組成物およびその加硫物 |
CN101046265A (zh) * | 2006-03-28 | 2007-10-03 | 东海橡胶工业株式会社 | 燃料胶管 |
JP2008266558A (ja) * | 2007-03-27 | 2008-11-06 | Tokai Rubber Ind Ltd | ヒドリンゴム組成物 |
CN103249794A (zh) * | 2010-11-12 | 2013-08-14 | 大曹株式会社 | 加硫粘结用组合物 |
JP2013043400A (ja) * | 2011-08-25 | 2013-03-04 | Daiso Co Ltd | 積層体及びその製造方法 |
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JP7205231B2 (ja) | 2023-01-17 |
WO2018135367A1 (ja) | 2018-07-26 |
EP3572464A1 (en) | 2019-11-27 |
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