CN109689820A - 氯丁橡胶胶乳粘接剂组合物 - Google Patents
氯丁橡胶胶乳粘接剂组合物 Download PDFInfo
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- CN109689820A CN109689820A CN201780053828.5A CN201780053828A CN109689820A CN 109689820 A CN109689820 A CN 109689820A CN 201780053828 A CN201780053828 A CN 201780053828A CN 109689820 A CN109689820 A CN 109689820A
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- chloroprene
- carboxy
- solid component
- based polymer
- emulsion
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Abstract
提供初始粘接强度、常态粘接强度优异、与被粘物的抗热蠕变性优异的氯丁橡胶胶乳粘接剂组合物。氯丁橡胶胶乳粘接剂组合物含有:羧基改性氯丁二烯系共聚物胶乳(A)、氯丁二烯系聚合物胶乳(B)及氯化聚烯烃树脂乳液(C),所述羧基改性氯丁二烯系共聚物胶乳(A)含有:氯丁二烯单体与烯属不饱和羧酸的共聚物、和聚乙烯醇,所述氯丁二烯系聚合物胶乳(B)含有氯丁二烯均聚物或氯丁二烯单体与其他单体的共聚物且含有松香酸金属盐,前述羧基改性氯丁二烯系共聚物胶乳(A)与前述氯丁二烯系聚合物胶乳(B)的含量以固体成分换算比计为80:20~20:80。
Description
技术领域
本发明涉及氯丁橡胶胶乳粘接剂组合物。
背景技术
氯丁橡胶胶乳在土木建筑、胶合板、家具、鞋、潜水服等的水系粘接剂、劳动作业用手套、实验用手套、医疗用手套、橡胶丝、气球等浸渍成形品、土木、建筑中的防水用涂膜等各种领域中被利用。水系粘接剂由于是水系的,因此有安全性高、具有接触性、初始粘接强度优异的特征。特别是将聚乙烯醇(PVA)用于乳化剂而制造的氯丁橡胶胶乳的配混稳定性、粘合性优异,因此常常作为水系粘接剂而利用。
但是,即使为这样适应范围广的氯丁橡胶胶乳粘接剂,对于表面不存在极性基团的聚烯烃这样的极化性小的物质,粘接也非常困难。聚烯烃树脂具有耐水性、耐化学药品性,并且坚韧,因此被广泛用作电绝缘材料、日用杂货等各种成形品的材料,因此若无法实现聚烯烃树脂的粘接,则制品的制造工序非常受限、不便。特别是对要求抗热蠕变性的用途的适应的难度高,针对近年来要求的进一步的高耐热化,正在研究使用了氯丁橡胶胶乳粘接剂的一些改良。
例如,专利文献1中,公开了通过使用特定凝胶含有率的氯丁橡胶胶乳提高了抗热蠕变性的粘接剂组合物。
另外,专利文献2中公开了通过将凝胶含有率不同的氯丁橡胶胶乳共混,并且添加碳二亚胺交联剂从而进一步提高了粘接物性的配混粘接剂组合物。
现有技术文献
专利文献
专利文献1:日本特开2002-275442号公报
专利文献2:日本特开2011-063672号公报
发明内容
发明要解决的问题
本发明提供初始粘接强度、常态粘接强度优异、与被粘物的抗热蠕变性也优异的氯丁橡胶胶乳粘接剂组合物。
用于解决问题的方案
即本发明提供一种氯丁橡胶胶乳粘接剂组合物,其含有:羧基改性氯丁二烯系共聚物胶乳(A)、氯丁二烯系聚合物胶乳(B)及氯化聚烯烃树脂乳液(C),
所述羧基改性氯丁二烯系共聚物胶乳(A)含有:氯丁二烯单体与烯属不饱和羧酸的共聚物、和作为非离子系表面活性剂的聚乙烯醇,
所述氯丁二烯系聚合物胶乳(B)含有氯丁二烯均聚物或氯丁二烯单体与其他单体的共聚物且含有松香酸金属盐,
前述羧基改性氯丁二烯系共聚物胶乳(A)与前述氯丁二烯系聚合物胶乳(B)的含量以固体成分换算比计为80:20~20:80。
本技术的氯丁橡胶胶乳粘接剂组合物中,可以相对于前述羧基改性氯丁二烯系共聚物胶乳(A)及前述氯丁二烯系聚合物胶乳(B)的以固体成分换算计的合计100质量份,含有以固体成分换算计为1~50质量份的前述氯化聚烯烃树脂乳液(C)。
另外,本技术的氯丁橡胶胶乳粘接剂组合物中,可以相对于前述羧基改性氯丁二烯系共聚物胶乳(A)及前述氯丁二烯系聚合物胶乳(B)的以固体成分换算计的合计100质量份,含有以固体成分换算计为1~100质量份的增粘树脂、及以固体成分换算计为0.5~10质量份的锌白。
作为可以使用本技术的氯丁橡胶胶乳粘接剂组合物的被粘物,可列举出聚烯烃。
发明的效果
根据本发明,能够提供初始粘接强度、常态粘接强度优异、与被粘物的抗热蠕变性优异的氯丁橡胶胶乳粘接剂组合物。
具体实施方式
以下,对用于实施本发明的适宜的方式进行说明。需要说明的是,以下说明的实施方式示出了本发明的代表性的实施方式的一例,并不由此对本发明的范围狭义地进行解释。
本实施方式的氯丁橡胶胶乳粘接剂组合物至少含有羧基改性氯丁二烯系共聚物胶乳(A)、氯丁二烯系聚合物胶乳(B)、和氯化聚烯烃树脂乳液(C)。另外,根据需要,也可以含有增粘树脂、锌白等。以下,详细地对各成分进行说明。
氯丁橡胶胶乳(也称为“氯丁二烯系聚合物胶乳”)是指使聚氯丁二烯分散于水中而得到的胶乳(乳液)。氯丁橡胶是指2-氯-1,3-丁二烯(以下,记为氯丁二烯)的均聚物、或氯丁二烯及可与氯丁二烯共聚的单体的共聚物。
作为可与氯丁二烯共聚的单体,例如,有2,3-二氯-1,3-丁二烯、1-氯-1,3-丁二烯、硫、丁二烯、异戊二烯、苯乙烯、甲基丙烯酸及其酯类、丙烯酸及其酯类,根据需要可以使用2种以上。
<羧基改性氯丁二烯系共聚物胶乳(A)>
对于本实施方式的氯丁橡胶胶乳粘接剂组合物中使用的羧基改性氯丁二烯系共聚物胶乳(A),氯丁二烯系聚合物为氯丁二烯单体与烯属不饱和羧酸的共聚物。若使含羧基的乙烯基单体共聚,则在粘接剂中配混有锌白、氧化镁等金属氧化物时,会发生2价金属离子与羧基的交联,能够提高抗热蠕变性、耐溶剂性等粘接性能。
作为烯属不饱和羧酸,只要不损害本发明的效果,可以自由选择使用1种或2种以上公知的烯属不饱和羧酸。本实施方式中,优选甲基丙烯酸和/或丙烯酸。
对于烯属不饱和羧酸的投入量,只要不损害本发明的效果,没有特别限定,可以自由设定。本实施方式中,在与氯丁二烯单体的合计100质量%中,烯属不饱和羧酸的投入量优选0.5~10质量%、更优选1~4质量%。通过将烯属不饱和羧酸的投入量设为0.5质量%以上,从而能够提高作为水系粘接剂时的抗热蠕变性。另外,通过将烯属不饱和羧酸的投入量设为10质量%以下,从而能够防止胶乳组合物的贮藏稳定性受损。
对于羧基改性氯丁二烯系共聚物胶乳(A)的烯属不饱和羧酸量,可以通过对标准曲线中预先使用了烯属不饱和羧酸的键合量已知的试样的气相色谱进行测定来求出。
为了得到羧基改性氯丁二烯系共聚物胶乳(A),使用聚合引发剂、链转移剂,使单独的氯丁二烯、或使氯丁二烯及可与氯丁二烯共聚的单体在聚乙烯醇(以下,也称为“PVA”)的存在下进行乳液聚合,在达到规定的聚合率时添加聚合终止剂来停止聚合即可。
对于本实施方式的氯丁橡胶胶乳粘接剂组合物中使用的羧基改性氯丁二烯系共聚物胶乳(A),作为氯丁二烯的乳液聚合中使用的乳化剂,将聚乙烯醇(PVA)作为必需成分。该PVA为非离子系表面活性剂,是通过使乙烯基酯单体的均聚物、或乙烯基酯单体及可与其共聚的单体的共聚物皂化而得到的聚合物。
聚乙烯醇的聚合度没有特别限定,从氯丁橡胶胶乳的稳定性的观点出发,聚合率优选为150~3000、进一步优选为200~700。
对于聚乙烯醇的含量,可以将经冷冻干燥的氯丁橡胶胶乳进行裁切,放入附属有冷凝器的茄形烧瓶,进行热水提取,对提取到的成分进行NMR测定来求出。
对于以上说明的羧基改性氯丁二烯系共聚物胶乳(A)的制造方法,只要不损害本发明的效果,就没有限定,可以使用公知的方法来制造。例如,可以依据日本特开2013-159741号记载的方法来合成。
<氯丁二烯系聚合物胶乳(B)>
本实施方式的氯丁橡胶胶乳粘接剂组合物中使用的氯丁二烯系聚合物胶乳(B)含有氯丁二烯均聚物或氯丁二烯单体与其他单体的共聚物且含有松香酸金属盐。
为了得到氯丁二烯系聚合物胶乳(B),使用聚合引发剂、链转移剂,使单独的氯丁二烯、或使氯丁二烯及可与氯丁二烯共聚的单体在松香酸金属盐的存在下进行乳液聚合,在达到规定的聚合率时添加聚合终止剂来停止聚合即可。
对于本实施方式的氯丁橡胶胶乳粘接剂组合物中使用的氯丁二烯系聚合物胶乳(B),通过气相色谱测定的松香酸金属盐的含量优选为0.5~8质量%、更优选为1.5~5质量%。通过将松香酸金属盐的含量设为0.5质量%以上,从而防止乳液聚合时的保护胶体不足,能够提高聚合稳定性。另外,通过将松香酸金属盐的含量设为8质量%以下,从而能够防止聚合反应体系的粘度的上升,进行均匀的搅拌。
对于松香酸金属盐的含量,可以将经冷冻干燥的氯丁橡胶胶乳进行裁切,放入附属有冷凝器的茄形烧瓶,进行ETA提取,由通过气相色谱对提取到的成分进行测定而得到的松香成分的峰面积来求出。
对于氯丁二烯系聚合物胶乳(B)的制造方法,只要不损害本发明的效果,就没有限定,可以使用公知的方法来制造。例如,可以依据日本特开昭48-84891号、日本特开平11-158327号、日本特开2013-159741号记载的公知的方法来合成。
另外,对于氯丁二烯系聚合物胶乳(B)的凝胶含有率,只要不损害本发明的效果,就没有特别限定。需要说明的是,对于氯丁二烯系聚合物胶乳的凝胶含有率,通过以下的方法来测定。将氯丁二烯系聚合物胶乳冷冻干燥,得到聚集物,将其在甲苯中浸渍2天,通过200目(开口0.075mm)的筛网,将残留于筛网上的物质进行真空干燥,由此将甲苯去除,得到凝胶。由凝胶的重量与聚集物的重量之比求出凝胶含有率。
本实施方式的氯丁橡胶胶乳粘接剂组合物的特征在于,含有前述具有不同特征的2种氯丁橡胶胶乳。为了平衡良好地兼顾初始粘接强度、常态粘接强度、及与被粘物的抗热蠕变性的各性能,前述羧基改性氯丁二烯系共聚物胶乳(A)与前述氯丁二烯系聚合物胶乳(B)的含量设为以固体成分换算比计为80:20~20:80。若前述羧基改性氯丁二烯系共聚物胶乳(A)超过80质量%,则抗热蠕变性降低,若不足20质量%,则初始粘接强度、常态粘接强度降低。
<氯化聚烯烃树脂乳液(C)>
氯化聚烯烃树脂乳液(C)为使聚烯烃氯化、或酸改性而成的树脂乳液。氯化聚烯烃树脂乳液(C)为用于对氯丁橡胶胶乳粘接剂组合物的聚烯烃系树脂赋予粘附性的成分。
对于氯化聚烯烃树脂乳液(C)的含量,只要不损害本发明的效果,就没有特别限定,可以自由设定。本实施方式中,相对于氯丁橡胶胶乳的以固体成分换算计的100质量份,优选使用以固体成分换算计为1~50质量份的氯化聚烯烃树脂乳液(C),更优选使用以固体成分换算计5~40质量份。若不添加氯化聚烯烃树脂乳液,则得不到对聚烯烃系树脂的良好的粘接性,若添加量过多,则有时抗热蠕变性会降低,而且不能避免成本增加。
作为氯化聚烯烃树脂乳液(C)的原料,只要不损害本发明的效果,可以自由选择使用公知的可成为氯化聚烯烃树脂乳液的原料的物质。例如,可列举出结晶化聚丙烯、非结晶性聚丙烯、聚丁烯-1、低密度或高密度聚乙烯、乙烯-丙烯共聚物、乙烯-丙烯-二烯共聚物等。
氯化聚烯烃树脂乳液(C)优选为将选自α,β-不饱和羧酸及其酸酐中的至少一种单体接枝聚合而成的酸改性氯化聚烯烃树脂乳液。作为此处使用的α,β-不饱和羧酸及其酸酐,可列举出马来酸、衣康酸、柠康酸、富马酸、中康酸、乌头酸、马来酸酐、衣康酸酐、柠康酸酐、乌头酸酐等。若对氯化聚烯烃树脂乳液(C)进行酸改性,则在粘接剂中配混有锌白、氧化镁等金属氧化物时,会发生2价金属离子与羧基的交联,能够提高抗热蠕变性、耐溶剂性等粘接性能。
前述氯化聚烯烃树脂乳液的氯含有率没有特别限定,优选为10~40%。通过将氯含有率设为10%以上,从而能够提高与聚氯丁二烯胶乳的相容性。另外,通过使氯含有率不足40%,从而能够防止与聚烯烃基材等被粘物的密合性的降低。
对于前述氯化聚烯烃树脂乳液(C)中使用的表面活性剂,只要不损害本发明的效果,就没有特别限定,例如,可列举出非离子性表面活性剂、阴离子性表面活性剂、阳离子性表面活性剂、两性表面活性剂。本技术中,从粘接剂组合物的贮藏稳定性的观点出发,优选使用非离子性表面活性剂。
对于可用作氯化聚烯烃树脂乳液(C)的市售品,有东洋纺株式会社制EW-5303、EH-801等。
<增粘树脂>
本实施方式的氯丁橡胶胶乳粘接剂组合物中,除了前述羧基改性氯丁二烯系共聚物胶乳(A)、前述氯丁二烯系聚合物胶乳(B)、及前述氯化聚烯烃树脂乳液(C)以外,还可以使用增粘树脂。
增粘树脂是为了提高氯丁橡胶胶乳粘接剂组合物的初始粘接强度而添加的。特别是能够提高使用聚烯烃作为被粘物时的密合性。
对于增粘树脂,相对于氯丁橡胶胶乳的以固体成分换算计的100质量份,优选使用以固体成分换算计1~100质量份、更优选使用以固体成分换算计20~70质量份。通过将增粘树脂的添加量设为1质量份以上,从而能够提高初始粘接强度。另外,通过将增粘树脂的添加量设为100质量份以下,从而能够防止与被粘物的抗热蠕变性的降低。
对增粘树脂的种类没有特别限定,可列举出脂松香、浮油松香、木松香、歧化松香、聚合松香、这些松香的甘油酯、季戊四醇酯、它们的氢化物等松香系树脂、萜烯酚树脂的氢化物等萜烯酚系树脂、脂肪族系石油树脂、脂环族系石油树脂、芳香族系石油树脂、共聚系石油树脂、二环戊二烯系石油树脂、纯单体系石油树脂、它们的氢化物等石油系树脂、苯乙烯系树脂、香豆酮茚系树脂、烷基酚系树脂、二甲苯树脂、达玛树脂(dammar)、柯巴脂(copal)、虫胶等。
作为本实施方式中可以使用的增粘树脂的市售品,有作为萜烯酚树脂乳液的荒川化学工业株式会社制TAMANOL E-100、TAMANOL E-200NT等。
<锌白>
本实施方式的氯丁橡胶胶乳粘接剂组合物中,除了前述羧基改性氯丁二烯系共聚物胶乳(A)、前述氯丁二烯系聚合物胶乳(B)、及前述氯化聚烯烃树脂乳液(C)以外,还可以使用锌白。
锌白是为了提高粘接剂组合物的粘接强度、抗热蠕变性而添加的。特别是若粘接剂组合物内含有羧基,则会发生2价金属离子与羧基的交联,因此能够进一步提高抗热蠕变性。另外,能够提高使用聚烯烃作为被粘物时的密合性。
对于锌白,相对于氯丁橡胶胶乳的以固体成分换算计的100质量份,优选使用以固体成分换算计0.5~10质量份、更优选使用以固体成分换算计1~5质量份。通过将锌白的添加量设为0.5质量份以上,从而能够提高抗热蠕变性。另外,通过将锌白的添加量设为10质量份以下,从而能够防止初始粘接强度的降低,而且能够降低成本。
作为本实施方式中使用的锌白,没有特别限定,可以使用公知的锌白,锌白的数均粒径特别优选0.1~0.3μm。锌白的数均粒径为在水中进行超声波分散后自然干燥而得到的锌白粉末的、通过SEM装置(FE-SEMSU6600:Hitachi High-Technologies Corporation制)得到的200个观察图像的定向切线直径(Feret径)的数均值。通过使用数均粒径为0.1μm以上的锌白,由此能够防止锌白彼此的聚集,从而在氯丁橡胶胶乳粘接剂组合物中均匀地分散,另外,能够防止锌白自身的飞散,从而提高处理性能。另外,通过使用数均粒径为0.3μm以下的锌白,从而能够可靠地提高粘接强度。
另外,本实施方式中使用的锌白的比表面积也没有特别限定,优选为15~25m2/g。此处锌白的比表面积为,将使锌白在水中进行超声波分散后自然干燥而得到的粉末作为样品,使用比表面积测定装置(MONOSORB:QUANTACHROME INSTRUMENTS公司制),依据JIS-Z8830,通过以氮气为吸附质的BET法测定的值。通过使用比表面积为15m2/g以上的锌白,从而能够促进氯丁橡胶胶乳、氯化聚烯烃树脂乳液的交联,能够提高得到的氯丁橡胶胶乳粘接剂组合物的粘接强度。另一方面,比表面积为25m2/g以下的锌白的吸湿性低,因此能够防止锌白自身的品质的劣化,可以适宜地用于工业上的生产。
作为满足前述数均粒径及比表面积的条件的锌白,例如可例示出使包含无机锌盐水溶液和碱水溶液的反应液在搅拌反应槽内反应而得到的基于湿式制造法的锌白分散液。需要说明的是,为了容易将锌白均匀混合,也可以在添加至氯丁橡胶胶乳前预先使其分散于水中。作为用于使锌白分散于水中的乳化剂,可以使用通常的阴离子系乳化剂,例如有DarvanNo.1(商品名、R.T.Verderbilt Company,Inc制)等市售品。
作为本实施方式中可以使用的锌白的市售品,有大崎工业株式会社制AZ-SW、井上石灰株式会社META-Z等。
<其他>
此外,本实施方式的氯丁橡胶胶乳粘接剂组合物中可以适宜配混碳酸钙、二氧化硅等无机填充材料、防老化剂、硫化促进剂、表面活性剂、防腐剂、消泡剂、分散剂、流平剂、冷冻稳定剂等。
以上说明的本实施方式的氯丁橡胶胶乳可以用于各种被粘物,特别是可以适宜地用于以聚烯烃为被粘物的情况。因此,作为至少一方的被粘物为聚烯烃、要求高抗热蠕变性的粘接用途、例如用作汽车内饰材料的聚烯烃基材与聚氨酯泡沫、聚烯烃基材与织物等的粘接用途,是有用的。
实施例
以下,基于实施例更详细地对本发明进行说明。需要说明的是,以下说明的实施例示出本发明的代表性的实施例的一例,并不由此对本发明的范围狭义地进行解释。
<制备例1>
[羧基改性氯丁二烯系共聚物胶乳(A)-1的制造]
使用内容积3升的反应器,在氮气气流下、投入纯水100质量份、聚乙烯醇(商品名“UHR-20H”、皂化度79mol%、聚合度380、Unitika Ltd.制)4.0质量份,溶解后,边搅拌边添加氯丁二烯系单体98质量份、甲基丙烯酸2质量份、及辛基硫醇0.3质量份。边将其保持为45℃边使用过硫酸钾和亚硫酸钠作为引发剂来进行聚合,得到羧基改性氯丁二烯系共聚物胶乳(A)-1。
<制备例2>
[氯丁二烯系聚合物胶乳(B)-1的制造]
使用内容积3升的反应器,在氮气气流下、投入纯水100质量份、松香酸的钾盐(荒川化学工业株式会社制、商品名“RONDIS”(注册商标))4.0质量份、氢氧化钾1.0质量份、β-萘磺酸钠盐(花王株式会社制、商品名“DEMOL NL”(注册商标))0.8质量份,溶解后,边搅拌边添加氯丁二烯系单体90质量份、2,3-二氯1,3-丁二烯10质量份、十二烷基硫醇0.03质量份。边将其保持为40℃边使用过硫酸钾和亚硫酸钠作为引发剂来进行聚合,在聚合率达到90%时加入吩噻嗪的乳浊液,使聚合停止。在减压下将未反应单体去除,得到氯丁二烯系聚合物胶乳(B)-1。氯丁二烯系聚合物胶乳(B)-1的凝胶含有率为90%。
<制备例3>
[氯丁二烯系聚合物胶乳(B)-2的制造]
使用内容积3升的反应器,在氮气气流下、投入纯水100质量份、松香酸的钾盐(荒川化学工业株式会社制、商品名“RONDIS”(注册商标))4.0质量份、氢氧化钾1.0质量份、β-萘磺酸钠盐(花王株式会社制、商品名“DEMOL NL”(注册商标))0.8质量份,溶解后,边搅拌边添加氯丁二烯系单体100质量份、十二烷基硫醇0.1质量份。边将其保持为10℃边使用过硫酸钾和亚硫酸钠作为引发剂来进行聚合,在聚合率达到90%时加入吩噻嗪的乳浊液,使聚合停止。在减压下将未反应单体去除,得到氯丁二烯系聚合物胶乳(B)-2。氯丁二烯系聚合物胶乳(B)-2的凝胶含有率为8%。
<实施例1>
添加以固体成分换算计为50质量份的作为羧基改性氯丁二烯系共聚物胶乳(A)的羧基改性氯丁二烯系共聚物胶乳(A)-1、以固体成分换算计为50质量份的作为氯丁二烯系聚合物胶乳(B)的氯丁二烯系聚合物胶乳(B)-1、以固体成分换算计为15质量份的作为氯化聚烯烃树脂乳液(C)的EW-5303(东洋纺株式会社制)、以固体成分换算计为50质量份的作为增粘树脂的TAMANOL E-100(荒川化学工业制)、以固体成分换算计为1质量份的作为锌白的AZ-SW(大崎工业株式会社制),得到实施例1的氯丁橡胶胶乳粘接剂组合物。
<实施例2>
在表1所示的条件下、添加氯丁二烯系聚合物胶乳(B)-2来代替作为氯丁二烯系聚合物胶乳(B)的氯丁二烯系聚合物胶乳(B)-1,对于除此以外的其他条件,利用与实施例1同样的条件,得到实施例2的氯丁橡胶胶乳粘接剂组合物。
<实施例3>
在表1所示的条件下、添加EH-801(东洋纺株式会社制)来代替作为氯化聚烯烃树脂乳液(C)的EW-5303,对于除此以外的其他条件,利用与实施例1同样的条件,得到实施例3的氯丁橡胶胶乳粘接剂组合物。
<实施例4及5>
在表1所示的条件下、变更羧基改性氯丁二烯系共聚物胶乳(A)-1和氯丁二烯系聚合物胶乳(B)-1的添加量,对于除此以外的其他条件,利用与实施例1同样的条件,得到实施例4及5的氯丁橡胶胶乳粘接剂组合物。
<实施例6及7>
在表1所示的条件下、变更氯化聚烯烃树脂乳液(C)的添加量,对于除此以外的其他条件,利用与实施例1同样的条件,得到实施例6及7的氯丁橡胶胶乳粘接剂组合物。
<实施例8及9>
在表1所示的条件下、变更增粘树脂的添加量,对于除此以外的其他条件,利用与实施例1同样的条件,得到实施例8及9的氯丁橡胶胶乳粘接剂组合物。
<实施例10>
在表1所示的条件下、变更锌白的添加量,对于除此以外的其他条件,利用与实施例1同样的条件,得到实施例10的氯丁橡胶胶乳粘接剂组合物。
<比较例1~比较例12>
在表2所示的条件下、分别进行粘接剂组合物的制备,对于其他条件,利用与实施例1同样的条件,得到氯丁橡胶胶乳粘接剂组合物。
对以上得到的各氯丁橡胶胶乳粘接剂组合物,如下地制作样品,进行粘接强度的评价。需要说明的是,表1及2的配混处方分别是以固体成分换算计的质量份。
<样品的制作>
分别用刷毛在帆布(25×70mm)上涂布300g(固体成分)/m2的各粘接剂组合物(实施例1~10、比较例1~12),在聚丙烯板(25×70mm)上涂布150g(固体成分)/m2的各粘接剂组合物,在80℃气氛下干燥9分钟。然后,在室温下放置1分钟后粘贴涂布面,用手压辊进行压接,得到粘接体。
<评价>
(1)初始粘接强度
辊压接10分钟后,使用拉伸试验机,以拉伸速度200mm/分钟测定180°剥离强度。
(2)常态粘接强度
使粘接体在23℃气氛下熟化5天后,使用拉伸试验机,以拉伸速度200mm/分钟测定180°剥离强度。
(3)抗热蠕变
使粘接体在23℃气氛下熟化5天后,在80℃气氛下沿180°方向施加100g/25mm的载荷,测定24小时后的剥离长度。
<结果>
将结果示于下述的表1及2。
[表1]
[表2]
如表1所示,含有羧基改性氯丁二烯系共聚物胶乳(A)、氯丁二烯系聚合物胶乳(B)、氯化聚烯烃树脂乳液(C),且羧基改性氯丁二烯系共聚物胶乳(A)与氯丁二烯系聚合物胶乳(B)的含量以固体成分换算比计为80:20~20:80的各实施例的氯丁橡胶胶乳粘接剂组合物的初始粘接强度、常态粘接强度、抗热蠕变性均良好。
另一方面,如表2所示,对于不含有羧基改性氯丁二烯系共聚物胶乳(A)、氯丁二烯系聚合物胶乳(B)、氯化聚烯烃树脂乳液(C)中任一者的比较例1~4及7、羧基改性氯丁二烯系共聚物胶乳(A)与氯丁二烯系聚合物胶乳(B)的含量以固体成分换算比计为80:20~20:80的范围外的比较例5及6,得不到初始粘接强度、常态粘接强度、抗热蠕变性全部得到满足的结果。
若在实施例中进行比较,则对于在以固体成分换算计为1~50质量份的范围内含有氯化聚烯烃树脂乳液(C)的实施例1、6及7,与含有以固体成分换算计超过50质量份的氯化聚烯烃树脂乳液(C)的实施例11相比,抗热蠕变的评价结果良好。根据该结果可知,相对于羧基改性氯丁二烯系共聚物胶乳(A)及氯丁二烯系聚合物胶乳(B)的以固体成分换算计的合计100质量份,氯化聚烯烃树脂乳液(C)的优选的含量为1~50质量份。
另外,对于在以固体成分换算计为1~100质量份的范围内含有增粘树脂的实施例1及8,与不含增粘树脂的实施例12相比,粘接强度为良好的结果。另外,对于在以固体成分换算计为1~100质量份的范围内含有增粘树脂的实施例1及9,与含有以固体成分换算计超过100质量份的增粘树脂的实施例13相比,抗热蠕变的评价结果良好。根据该结果可知,相对于羧基改性氯丁二烯系共聚物胶乳(A)及氯丁二烯系聚合物胶乳(B)的以固体成分换算计的合计100质量份,增粘树脂的优选的含量为1~100质量份。
进而,对于在以固体成分换算计为0.5~10质量份的范围内含有锌白的实施例1,与不含锌白的实施例14相比,粘接强度及抗热蠕变性中的任一评价结果均良好。另外,对于在以固体成分换算计为0.5~10质量份的范围内含有锌白的实施例1及10,与含有以固体成分换算计超过10质量份的锌白的实施例15相比,粘接强度良好。根据该结果可知,相对于羧基改性氯丁二烯系共聚物胶乳(A)及氯丁二烯系聚合物胶乳(B)的以固体成分换算计的合计100质量份,锌白的优选的含量为1~10质量份。
Claims (4)
1.一种氯丁橡胶胶乳粘接剂组合物,其含有:羧基改性氯丁二烯系共聚物胶乳(A)、氯丁二烯系聚合物胶乳(B)及氯化聚烯烃树脂乳液(C),
所述羧基改性氯丁二烯系共聚物胶乳(A)含有:氯丁二烯单体与烯属不饱和羧酸的共聚物、和聚乙烯醇,
所述氯丁二烯系聚合物胶乳(B)含有氯丁二烯均聚物或氯丁二烯单体与其他单体的共聚物且含有松香酸金属盐,
所述羧基改性氯丁二烯系共聚物胶乳(A)与所述氯丁二烯系聚合物胶乳(B)的含量以固体成分换算比计为80:20~20:80。
2.根据权利要求1所述的氯丁橡胶胶乳粘接剂组合物,其中,相对于所述羧基改性氯丁二烯系共聚物胶乳(A)及所述氯丁二烯系聚合物胶乳(B)的以固体成分换算计的合计100质量份,
含有以固体成分换算计为1~50质量份的所述氯化聚烯烃树脂乳液(C)。
3.根据权利要求1或2所述的氯丁橡胶胶乳粘接剂组合物,其中,相对于所述羧基改性氯丁二烯系共聚物胶乳(A)及所述氯丁二烯系聚合物胶乳(B)的以固体成分换算计的合计100质量份,
含有以固体成分换算计为1~100质量份的增粘树脂及以固体成分换算计为0.5~10质量份的锌白。
4.根据权利要求1~3中任一项所述的氯丁橡胶胶乳粘接剂组合物,其中,至少一方的被粘物为聚烯烃。
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