CN108290373A - 发泡性板件补强材料、其制造方法和板件的补强方法 - Google Patents
发泡性板件补强材料、其制造方法和板件的补强方法 Download PDFInfo
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Abstract
提供了一种发泡性板件补强材料,其包括:发泡性组合物层,和层压于所述发泡性组合物层上的片状纤维层,所述发泡性组合物层至少包含具有固化性的、交联高分子基体的可塑组分,所述可塑组分的固化剂,所述可塑组分的固化促进剂,交联高分子基体,填料,和分解温度为T℃的热分解型发泡剂,其中,所述发泡性组合物层示出的由动态粘弹性测量装置测量[其中测量温度为(T‑10)℃]的储能弹性模量(G’)为1×101至1×104Pa。
Description
技术领域
本发明涉及发泡性板件(panel)补强材料、其制造方法和板件的补强方法。更具体地,本发明涉及用于提高输送机器和金属外壳等用的板件例如碳纤维增强树脂板、钢板和铝合板等的弯曲强度同时实现轻量化的发泡性板件补强材料、其制造方法和板件的补强方法。
背景技术
用于输送机器(例如车体)和金属外壳等的例如碳纤维增强树脂板、钢板和铝合板等板件倾向于薄以实现轻量化,并且近年来,主要使用厚度为约0.6至0.8mm的板件。出于该原因,存在以下问题,板件变得易于在弱的力下变形和屈曲(buckled),并且产生应变以使外观劣化。进一步,在薄的板件中,因为刚性和耐冲击性下降,在运输机器的车体中会损害应对冲击的乘客的安全性。出于该原因,在假定冲击的部位中,要求板件的刚性再更进一步提高。
以往,要求刚性的板件的部位的补强已经通过将片状补强材料贴附至内侧以使其与板件一体化的方法来进行。作为补强材料,通过以下获得的补强材料是已知的:在醇酸树脂、环氧树脂、丙烯酸系树脂、聚氨酯树脂或尿素树脂等中配混液态橡胶、固体橡胶、固化剂、填料、发泡剂和各种添加剂,将它们用压延辊(calendar roll)混炼,将混炼产物加压为片材,并将该片材加工为预定厚度。该补强材料通过贴附至板件并且将此借由加热来固化而补强板件。
作为补强材料,例如,在专利文献1(日本特开2005-139218号公报)中,已经提出了如玻璃布等拘束层和由加热发泡固化性树脂组合物构成的片状树脂层的层压体。这里的树脂组合物包含NBR橡胶、SBR橡胶、填料、发泡剂、环氧系树脂和其固化剂。
现有技术文献
专利文献
专利文献1:日本特开2005-139218号公报
发明内容
发明要解决的问题
因为在记载于专利文献1中的补强材料中,难以增加发泡倍率,所以已经需要提供可以给予高的发泡倍率的补强材料。
用于解决问题的方案
本发明鉴于这样的情况而做出,其目的是提供一种发泡性板件补强材料,所述材料可以通过固化而提供高发泡倍率,并且可以将强固的粘接性、弯曲强度和韧性赋予至固化后的板件,同时由于固化前的适度的压敏粘合性而示出充分的对板件的暂时粘着力(temporary adhesive force)。本发明人深入地进行了研究以解决上述问题,结果发现,上述问题可以通过使发泡性组合物层具有特定的储能弹性模量(G’)来解决,所述发泡性组合物层至少包含具有固化性的、交联高分子基体的可塑组分,所述可塑组分的固化剂,所述可塑组分的固化促进剂,交联高分子基体,填料,和分解温度为T℃的热分解型发泡剂,导致完成了本发明。另外,在本发明的补强材料中,可塑组分主要有助于表现压敏粘合性,可塑组分、固化剂和固化促进剂主要有助于表现对板件的粘接性,填料和分解型发泡剂有助于表现发泡性,交联高分子基体主要有助于补强材料的形状保持性。
因而,根据本发明,提供了一种发泡性板件补强材料,其包括:发泡性组合物层,和层压于所述发泡性组合物层上的片状纤维层,所述发泡性组合物层至少包含具有固化性的、交联高分子基体的可塑组分,所述可塑组分的固化剂,所述可塑组分的固化促进剂,交联高分子基体,填料,和分解温度为T℃的热分解型发泡剂,其中当将储能弹性模量(G’)用动态粘弹性测量装置来测量[条件是测量温度为(T-10)℃]时,所述发泡性组合物层展现的储能弹性模量(G’)为1×101至1×104Pa。
根据本发明,还提供了一种所述发泡性板件补强材料的制造方法,所述方法包括:通过将具有一个聚合性官能团的单官能性单体和具有两个以上的聚合性官能团的多官能性单体使用聚合引发剂聚合来获得所述交联高分子基体,其中所述聚合在所述可塑组分、所述固化剂、所述固化促进剂、所述填料和所述热分解型发泡剂的存在下进行。
根据本发明,进一步提供了一种板件的补强方法,所述方法包括以下步骤:将所述发泡性板件补强材料贴附至板件,从而将所述发泡性板件补强材料和所述板件暂时固定;和使所述发泡性板件补强材料进行在T℃以上的加热发泡和固化。
发明的效果
根据本发明,可以提供一种发泡性板件补强材料,其确保了由于发泡倍率增加得到的轻量性以及弯曲强度,可以将由断裂应变增加得到的韧性赋予至板件,同时由于初始状态的压敏粘合性而示出充分的对板件的暂时粘着力。
依照以下任何之一或其组合,还可以提供一种发泡性板件补强材料,其具有更加改善的暂时粘着力、更加改善的轻量性和更加改善的弯曲强度,并且可以更加将韧性赋予至板件。
(1)所述热分解型发泡剂选自偶氮二甲酰胺、偶氮二异丁腈、偶氮二甲酸钡、硝基二胍、N,N’-二亚硝基五亚甲基四胺、N,N’-二甲基-N,N’-二亚硝基对苯二甲酰胺、P,P’-氧双(苯磺酰肼)、亚肼基二甲酰胺(hydrazodicarbonamide)、对甲苯磺酰肼、二苯砜-3,3’-二磺酰肼、烯丙基双(磺酰肼)、对甲代亚苯基磺酰氨基脲(p-toluylenesulfonylsemicarbazide)、4,4’-氧双(苯磺酰氨基脲)、5-苯基-1,2,3,4-四唑、碳酸氢钠、碳酸铵和无水硝酸钠,其含量相对于100重量份的所述发泡性组合物层为0.1至10重量份。
(2)当进行在(T+20)℃下20分钟的加热发泡和固化时,所述发泡性板件补强材料展现1.5至10倍的发泡倍率。
(3)当所述发泡性板件补强材料通过将所述发泡性板件补强材料贴着至厚度为0.8mm的冷轧钢板且使所述发泡性板件补强材料进行在(T+20)℃下20分钟的加热发泡和固化而形成为补强板件时,所述补强板件使所述冷轧钢板展现以下性质:
在以100mm的跨度(span)测量三点弯曲(three-point bending)时,
(i)1mm位移时的强度为25N以上,
(ii)2mm位移时的强度为50N以上,和
(iii)直至断裂点的应变能量为0.5N·m以上。
(4)所述发泡性板件补强材料展现0.01至0.5N/mm2的压敏粘合力。
(5)所述片状纤维层为无机纤维或有机纤维的织布或单向性布(unidirectionally cloth)并且位于所述发泡性板件补强材料的一侧表层上。
(6)所述交联高分子基体为具有一个聚合性官能团的单官能性单体和具有两个以上的聚合性官能团的多官能性单体的共聚物。
(7)所述可塑组分为在25℃的温度下展现500至30,000mPa·s范围内的粘度的液态环氧系树脂,所述液态环氧系树脂包含至少一种具有苯骨架的组分。
(8)所述固化剂至少包含双氰胺(dicyanodiamide)。
(9)所述固化促进剂为胺系或咪唑系固化促进剂。
(10)当进行在(T+20)℃下20分钟的加热发泡和固化时,所述发泡性板件补强材料提供了具有平均泡孔直径为10至500μm的闭孔结构的发泡体。
(11)所述发泡性板件补强材料用于补强厚度为3mm以下的板件,所述板件选自碳纤维增强树脂板、钢板和铝板。
(12)所述发泡性组合物层进一步包含橡胶或含有橡胶组分的化合物,所述橡胶或含有橡胶组分的化合物在所述交联高分子基体的可塑组分中相分离为海-岛结构的岛部分,和
所述发泡性板件补强材料展现如下的物性:在-40℃、23℃和80℃的温度环境下以100mm的跨度通过三点弯曲测量补强板件而得的最大点强度中,-40℃和80℃下的最大点强度相对于23℃下的最大点强度的变化率为25%以下,所述补强板件通过将所述发泡性板件补强材料贴着至厚度为0.8mm的冷轧钢板且使所述发泡性板件补强材料和所述冷轧钢板在180℃下加热一体化而获得。
(13)所述岛部分包括相分离尺度(phase separation scale)为10至1,000nm的特定岛部分,在使用电子显微镜得到的加热发泡固化后的板件补强材料的截面照片中,所述特定岛部分以在3,000nm×3,000nm的范围内为10个以上的数量存在。
进一步,根据使用发泡性板件补强材料的板件的补强方法,对于板件的轻量性和刚性的确保、以及由断裂应变增加得到的韧性的赋予可以简单地进行。
附图说明
图1为实施例1的发泡性板件补强材料的加热发泡固化物的截面SEM照片。
图2为实施例6的发泡性板件补强材料的加热发泡固化物的截面TEM照片。
图3为实施例8的发泡性板件补强材料的加热发泡固化物的截面TEM照片。
图4为实施例10的发泡性板件补强材料的加热发泡固化物的截面TEM照片。
具体实施方式
以下将详细地说明本发明的板件补强材料和板件的补强方法。本发明不限于以下说明,但可以在其主旨范围内多方面地改变。
(发泡性板件补强材料)
发泡性板件补强材料(下文中,也简称为补强材料)包括:发泡性组合物层,和层压于所述发泡性组合物层上的片状纤维层,所述发泡性组合物层至少包含具有固化性的、交联高分子基体的可塑组分,所述可塑组分的固化剂,所述可塑组分的固化促进剂,交联高分子基体,填料,和分解温度为T℃的热分解型发泡剂。
另外,当将储能弹性模量(G’)用动态粘弹性测量装置来测量[条件是测量温度为(T-10)℃]时,发泡性组合物层展现的储能弹性模量(G’)为1×101至1×104Pa。当储能弹性模量小于1×101Pa时,气泡变得粗大,断裂点位移会变得太小。当储能弹性模量大于1×104Pa时,不能产生充分的发泡。储能弹性模量可以取1×101Pa、5×101Pa、1×102Pa、5×102Pa、1×103Pa、5×103Pa和1×104Pa。储能弹性模量优选为1×102至5×103Pa。储能弹性模量的上限可以为1×103Pa。
当进行在(T+20)℃下20分钟的加热发泡和固化时,优选的是,补强材料展现1.5至10倍的发泡倍率。当发泡倍率小于1.5倍时,轻量化会变得不充分。当发泡倍率大于10倍时,断裂点位移会变小,这样的应力的吸收能会变得小。发泡倍率可以取1.5倍、2倍、3倍、4倍、6倍、8倍和10倍。发泡倍率优选为1.5至6倍,更优选2至4倍。
当补强材料通过将补强材料贴着至厚度为0.8mm的冷轧钢板且使补强材料进行在(T+20)℃下20分钟的加热发泡和固化而形成为补强板件时,优选的是,补强板件使冷轧钢板展现以下性质:
在以100mm的跨度测量三点弯曲时,
(i)1mm位移时的强度(在发泡体层位移1mm时的弯曲强度)为25N以上,
(ii)2mm位移时的强度(在发泡体层位移2mm时的弯曲强度)为50N以上,和
(iii)直至断裂点的应变能量(通过在从应变0至断裂点应变的范围内积分而计算出的面积值)为0.5N·m以上。
当1mm位移时的强度小于25N时,补强板件的刚性会劣化。1mm位移时的强度可以取25N、30N、50N、60N、70N、80N、90N、和100N。1mm位移时的强度没有特别限制,但更优选30N以上,进一步优选50N以上。
当2mm位移时的强度小于50N时,补强板件的刚性会劣化。2mm位移时的强度可以取50N、60N、70N、80N、90N、100N、110N、120N、130N、140N、150N、160N、和170N。2mm位移时的强度没有特别限制,但更优选80N以上。
当直至断裂点的应变能量小于0.5N·m时,补强板件的冲击吸收性会劣化。应变能量可以取0.5N·m、1.0N·m、1.5N·m、2.0N·m、和2.5N·m。应变能量没有特别限制,但为了获得实际使用时充分的冲击吸收性,应变能量更优选为1.0N·m以上,进一步优选1.5N·m以上。
优选的是,补强材料展现0.01至0.5N/mm2的压敏粘合力。当压敏粘合力小于0.01N/mm2时,对板件的压敏粘合力会不足。当压敏粘合力高于0.5N/mm2时,压敏粘合力会太强以致降低操作性。压敏粘合力可以取0.01N/mm2、0.02N/mm2、0.05N/mm2、0.1N/mm2、0.3N/mm2、0.4N/mm2和0.5N/mm2。更优选的压敏粘合力为0.05至0.3N/mm2。
补强材料的厚度没有特别限制,只要其为可以在操作时保持补强材料的形状的厚度即可。例如,厚度为0.1至5mm。
当进行在(T+20)℃下20分钟的加热发泡和固化时,优选的是,补强材料提供了具有平均泡孔直径为10至500μm的闭孔结构的发泡体。当平均泡孔直径小于10μm时,膜厚度的增加会变得困难。当平均泡孔直径大于500μm时,由于容易开裂(cracking),断裂点位移会变小并且应变能量会变小。平均泡孔直径可以取10μm、50μm、100μm、200μm、300μm、400μm、和500μm。更优选的平均泡孔直径为50至300μm。
(1)可塑组分
可塑组分没有特别限制,只要其将塑性赋予至交联高分子基体即可,并且其本身具有固化性。其实例包括通常用于环氧树脂粘接剂的已知的环氧树脂。
环氧树脂的实例包括:如双酚F型和双酚A型等双酚型环氧树脂、酚醛清漆树脂型环氧树脂、联苯型环氧树脂、二环戊二烯型环氧树脂、萘型环氧树脂、环己烷型环氧树脂、氢化双酚A型环氧树脂、环氧环己烷(cyclohexeneoxide)型环氧树脂、和缩水甘油胺(glycidylamine)型环氧树脂等。尤其,如双酚F型和双酚A型等双酚型环氧树脂和酚醛清漆树脂型环氧树脂是优选的,这是因为如粘接强度、耐久性、耐冲击性和耐热性等性能与成本之间的平衡是优异的。优选的是,环氧系树脂为在25℃的温度下的粘度在500至30,000mPa·s的范围内的液态材料。另外,环氧系树脂的粘度为依照JIS K 7117-1:1999使用Brookfield型旋转粘度计在25℃的试验温度下测量的值。粘度可以取500mPa·s、1,000mPa·s、3,000mPa·s、5,000mPa·s、10,000mPa·s、20,000mPa·s、和30,000mPa·s。
(2)固化剂
固化剂没有特别限制,只要其具有与上述可塑组分的反应性即可。固化剂的实例包括胺型固化剂、酸酐类、酚醛清漆树脂、酚类、硫醇类、路易斯酸胺配合物、鎓盐、和咪唑类等。胺型固化剂的实例包括如二氨基二苯基甲烷和二氨基二苯砜等芳香族胺、脂肪族胺、咪唑衍生物、双氰胺、四甲基胍、和硫脲加成胺等;其同分异构体和改性体;等。除了胺型以外的固化剂包括4,4-二氨基二苯砜、如2-正十七烷基咪唑等咪唑衍生物、间苯二甲酸二酰肼、N,N-二烷基脲衍生物、N,N-二烷基硫脲衍生物、如四氢化邻苯二甲酸酐等酸酐、异弗尔酮二胺、间苯二胺、N-氨乙基哌嗪、三聚氰胺、胍胺、三氟化硼配合物、三-二甲基氨基甲基-苯酚、和多硫醇(polythiol)等。其中,胺型固化剂是特别优选的,并且双氰胺是特别优选的。固化剂可以单独使用,或两种以上可以通过组合它们来使用。
固化剂的含量没有特别限制,但最佳的量可以根据固化剂的种类而不同。例如,固化剂可以优选以预先已知的对于每种固化剂都最佳的量使用。作为该最佳的量,可以采用记载于例如“General Review of Epoxy Resins Basic Edition”(The Japan Society ofEpoxy Resin Technology,出版于2003年)的第三章中的量。
(3)固化促进剂
固化促进剂为用于促进补强材料的固化的缩合催化剂。固化促进剂的实例包括胺系固化促进剂、咪唑系固化促进剂和其衍生物。具体地,其实例包括:脲衍生物例如1,1’-(4-甲基-1,3-亚苯基)双(3,3-二甲基脲)、苯基-二甲基脲、亚甲基-二苯基-双二甲基脲、3-苯基-1,1-二甲基脲、3-(3,4-二氯苯基)-N,N-二甲基脲(DCMU)和3-(3-氯-4-甲基苯基)-1,1-二甲基脲;叔胺;咪唑衍生物例如2-十一烷基咪唑(C11Z)、2-十七烷基咪唑(C17Z)、2-苯基咪唑(2PZ)、和1,2-二甲基咪唑(1,2DMZ);脲化合物例如苯基二甲基脲(PDMU);三氟化单乙基胺;胺配合物例如三氯化胺配合物;等。
当其中,双氰胺用作固化剂时,适合地使用胺系固化促进剂和具有作为交联胺和促进催化剂的功能的咪唑系固化促进剂、和其衍生物。胺系固化促进剂的实例包括3-(3,4-二氯苯基)-N,N-二甲基脲(DCMU),并且咪唑系固化促进剂的实例包括2-十七烷基咪唑(C17Z)。
作为固化促进剂,DCMU是特别优选的。
相对于100重量份可塑组分,固化促进剂的含量优选为0.1至15重量份,并且进一步优选1至10重量份。
(4)交联高分子基体
交联高分子基体优选为具有一个聚合性官能团的单官能性单体和具有两个以上的聚合性官能团的多官能性单体的共聚物,并且优选由(甲基)丙烯酸系树脂组成。(甲基)丙烯酸系树脂没有特别限制,只要其为构成高分子基体的并可以在基体中包括可塑组分、固化剂和固化促进剂的树脂即可。(甲基)丙烯酸系树脂优选为具有苯骨架的树脂。(甲基)丙烯酸系树脂的实例包括源自单官能(甲基)丙烯酸系单体和多官能(甲基)丙烯酸系单体的共聚物的树脂。
单官能(甲基)丙烯酸系单体是指其中在一分子中包含一个(甲基)丙烯酰基的单体。例如,其为通过使在分子中具有至少一个羟基的芳香族或脂肪族醇、和其环氧烷加合物(alkylene oxide adduct)与(甲基)丙烯酸反应获得的(甲基)丙烯酸酯、(甲基)丙烯酰胺或(甲基)丙烯酰胺衍生物。
(甲基)丙烯酸酯的实例具体包括:脂肪族(甲基)丙烯酸系单体,例如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸异冰片酯、(甲基)丙烯酸四氢化糠酯、(甲基)丙烯酸4-羟基丁酯、(甲基)丙烯酸4-羟基丁酯、(甲基)丙烯酸2-羟基乙酯、1,10-癸二醇(甲基)丙烯酸酯和1,9-壬二醇(甲基)丙烯酸酯;具有苯骨架的(甲基)丙烯酸系单体,例如(甲基)丙烯酸苄酯、(甲基)丙烯酸苯氧基乙酯、苯基二甘醇(甲基)丙烯酸酯、(甲基)丙烯酸2-羟基-3-苯氧基丙酯、(甲基)丙烯酸甲基苯氧基乙酯、和乙氧基化邻苯基苯酚(甲基)丙烯酸酯;具有环氧基的(甲基)丙烯酸系单体,例如(甲基)丙烯酸缩水甘油酯和4-羟基丁基(甲基)丙烯酸酯缩水甘油醚;等。
(甲基)丙烯酰胺或(甲基)丙烯酰胺衍生物的实例具体包括叔丁基丙烯酰胺磺酸(TBAS)、叔丁基丙烯酰胺磺酸酯、N,N-二甲基氨乙基丙烯酰胺(DMAEAA)盐酸盐、N,N-二甲基氨丙基丙烯酰胺(DMAPAA)盐酸盐、(甲基)丙烯酰胺、N-甲基(甲基)丙烯酰胺、N-乙基(甲基)丙烯酰胺、N-丙基(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺、N,N-二乙基(甲基)丙烯酰胺、和丙烯酰基吗啉等。
多官能(甲基)丙烯酸系单体是指其中在一分子中包含两个以上的(甲基)丙烯酰基的(甲基)丙烯酸酯。其实例包括环己烷二甲醇二(甲基)丙烯酸酯、环己烷二甲醇(甲基)丙烯酸酯、二羟甲基三环癸烷二(甲基)丙烯酸酯、乙二醇二(甲基)丙烯酸酯、丙二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、己二醇二(甲基)丙烯酸酯、二甘醇二(甲基)丙烯酸酯、乙二醇二(甲基)丙烯酸酯、丙二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、己二醇二(甲基)丙烯酸酯、和二甘醇二(甲基)丙烯酸酯等。
另外,作为多官能(甲基)丙烯酸系单体,可以适合地使用聚氨酯系(甲基)丙烯酸酯(urethane-based(meth)acrylate)、聚酯系(甲基)丙烯酸酯、聚醚系(甲基)丙烯酸酯、环氧系(甲基)丙烯酸酯、和二烯聚合物系(甲基)丙烯酸酯等。
聚氨酯系(甲基)丙烯酸酯是指例如在分子中具有氨基甲酸酯键的(甲基)丙烯酸酯。聚氨酯系(甲基)丙烯酸酯可以通过将聚丁二烯二醇、聚醚多元醇、聚酯多元醇、或聚碳酸酯二醇等与多异氰酸酯之间的反应而得的聚氨酯用(甲基)丙烯酸酯化来获得。通过将聚丁二烯用(甲基)丙烯酰基改性获得的聚丁二烯改性的聚氨酯系(甲基)丙烯酸酯也包括在聚氨酯系(甲基)丙烯酸酯中。通过将氢化聚丁二烯用(甲基)丙烯酰基改性获得的氢化聚丁二烯改性的聚氨酯系(甲基)丙烯酸酯也包括在聚氨酯系(甲基)丙烯酸酯中。聚氨酯系(甲基)丙烯酸酯的实例包括1,2-聚丁二烯改性的聚氨酯系(甲基)丙烯酸酯、聚酯聚氨酯系(甲基)丙烯酸酯、二丁二醇聚氨酯系(甲基)丙烯酸酯、聚碳酸酯聚氨酯系(甲基)丙烯酸酯、和聚醚聚氨酯系(甲基)丙烯酸酯等。
聚酯系(甲基)丙烯酸酯通过例如将借由多元羧酸和多元醇的缩合获得的在两端具有羟基的聚酯的羟基用(甲基)丙烯酸酯化,或将借由将环氧烷加合至多元羧酸获得的末端羟基用(甲基)丙烯酸酯化来获得。
聚醚系(甲基)丙烯酸酯可以通过例如将聚醚多元醇的羟基用(甲基)丙烯酸酯化来获得。
环氧系(甲基)丙烯酸酯可以通过例如具有相对低的分子量的双酚型环氧树脂或酚醛清漆型环氧树脂环氧乙烷环(oxirane ring)与(甲基)丙烯酸反应从而使树脂酯化来获得。选择性地,还可以使用通过将该环氧系(甲基)丙烯酸酯用二元羧酸酐部分地改性获得的羧基改性的环氧(甲基)丙烯酸酯。
二烯聚合物系(甲基)丙烯酸酯的实例包括:通过将液态苯乙烯-丁二烯共聚物用(甲基)丙烯酰基改性获得的SBR二(甲基)丙烯酸酯、和通过将聚异戊二烯用(甲基)丙烯酰基改性获得的聚异戊二烯二(甲基)丙烯酸酯等。
优选的是,单官能(甲基)丙烯酸系单体和多官能(甲基)丙烯酸系单体的至少之一具有环氧基。通过在丙烯酰基凝胶骨架中存在环氧基,在使环氧树脂固化时,增塑剂和丙烯酰基凝胶骨架化学键合,并且可以获得更强的粘接强度。
相对于单官能(甲基)丙烯酸系单体和多官能(甲基)丙烯酸系单体的混合物,多官能(甲基)丙烯酸系单体的添加量优选在0.01至1.0重量%的范围内,更优选在0.1至0.5重量%的范围内。
“可塑组分”与“单官能(甲基)丙烯酸系单体和多官能(甲基)丙烯酸系单体的混合物”之间的重量比优选在30:70至70:30的范围内,更优选在40:60至60:40的范围内。
上述单官能(甲基)丙烯酸系单体和上述多官能(甲基)丙烯酸系单体的聚合方法没有特别限制,但其实例包括本体聚合、溶液聚合、悬浮聚合、和乳液聚合等。上述共聚方法中的聚合反应没有特别限制,但其实例包括自由基聚合反应、活性自由基聚合反应、和活性阴离子聚合反应等。上述聚合反应可以通过例如赋予例如热、紫外线和电子束等能量来引发。选择性地,在上述聚合反应中,反应引发剂可以在聚合时使用。
(5)热分解型发泡剂
作为热分解型发泡剂,可以广泛地使用已知的热分解型化学发泡剂和热膨胀胶囊。热分解型化学发泡剂的实例包括:有机系化学发泡剂例如偶氮二甲酰胺(ADCA)、偶氮二异丁腈、偶氮二甲酸钡、硝基二胍、N,N’-二亚硝基五亚甲基四胺、N,N’-二甲基-N,N’-二亚硝基对苯二甲酰胺、P,P’-氧双(苯磺酰肼)(OBSH)、亚肼基二甲酰胺、对甲苯磺酰肼、二苯砜-3,3’-二磺酰肼、烯丙基双(磺酰肼)、对甲代亚苯基磺酰氨基脲、4,4’-氧双(苯磺酰氨基脲)、5-苯基-1,2,3,4-四唑和有机酸金属盐;和无机系化学发泡剂例如碳酸氢钠、碳酸铵和无水硝酸钠。热分解型发泡剂可以单独使用,或两种以上可以通过混合它们来使用。
热膨胀胶囊为具有具气体阻隔性的热塑性树脂的壳且低沸点物质(热膨胀剂)容纳在该壳中的微胶囊。通过加热热膨胀胶囊,壳的热塑性树脂软化,并且伴随着由于低沸点物质的蒸发导致的体积增加,胶囊膨胀从而变为中空球状颗粒。因为热塑性树脂具有气体阻隔性,即使当加热和膨胀时,低沸点物质也可以保持在颗粒内。构成壳的热塑性树脂的实例包括偏二氯乙烯、丙烯腈、聚苯乙烯、聚甲基丙烯酸酯、和聚乙烯醇等。要容纳在壳内的低沸点物质的实例包括低沸点液态烃。尤其,实例包括容易蒸发的异戊烷和正戊烷等。
热膨胀胶囊的市售品的实例包括Expancel(Japan Fillite Co.,Ltd.制造)、Matsumoto Microsphere(Matsumoto Yushi-Seiyaku Co.,Ltd.制造)、和Microsphere(KUREHA CORPORATION制造)等。这些热膨胀胶囊可以单独使用,或两种以上可以通过混合它们来使用。
作为热分解型发泡剂,分解温度T为160℃的OBSH是优选的。
热分解型发泡剂的添加量可以为用于获得期望的发泡倍率的适当必要量。例如,优选的是,0.1至10重量份包含于100重量份发泡性组合物层中。
(6)填料
通过添加填料,可以赋予增粘性、发泡性和低固化收缩性。填料没有特别限制,但其实例包括由以下物质组成的无机填料:微细粉碎的二氧化硅、氧化铝、碳酸钙、氧化镁、氢氧化镁、粘土矿物、层状双氢氧化物、和中空微球等。这些可以单独使用,或两种以上可以同时使用。另外,上述填料的表面可以用表面处理剂例如硅烷偶联材料来处理。
微细粉碎的二氧化硅的实例包括:借由干式法粉碎获得的二氧化硅微粉末(例如,产品名:Aerosil 300,NIPPON AEROSIL CO.,LTD.制造)、通过将二氧化硅微粉末用六甲基二硅氮烷改性获得的微粉末(例如,产品名:Aerosil RX300,NIPPON AEROSIL CO.,LTD.制造)、通过将二氧化硅微粉末用聚二甲基硅氧烷获得的微粉末(例如,产品名:AerosilRY300,NIPPON AEROSIL CO.,LTD.制造)、和通过将微粉末二氧化硅用二甲基二氯硅烷处理获得的疏水性微粉末二氧化硅(产品名:Aerosil R972,NIPPON AEROSIL CO.,LTD.制造)等。
碳酸钙的实例具体包括由SHIRAISHI CALCIUM KAISHA,LTD.制造的Hakuenka CC、Hakuenka CCR、Hakuenka DD、Vigot10、Vigot15和Hakuenka U,等。
氧化镁的实例具体包括由Ube Materials Industries制造的UC95S、UC95M和UC95H,等。
氢氧化镁的实例具体包括由Ube Materials Industries制造的UD-650-1和UD-653,等。
无机填料的平均粒径优选为1,000μm以下,更优选200μm以下,进一步优选100μm以下,特别优选75μm以下,最优选20μm以下。另一方面,平均粒径优选为5nm以上,更优选10nm以上。上述平均粒径可以使用光散射法用粒径分析仪来测量。
中空微球的实例包括:由玻璃制成的中空球,例如中空玻璃球;由金属化合物制成的中空球,例如中空氧化铝球;由瓷(porcelain)制成的中空球,例如中空陶瓷球;等。
中空微球的比重优选为0.01g/cm3以上,更优选0.05g/cm3以上,进一步优选0.1g/cm3以上。另外,比重优选为0.8g/cm3以下,更优选0.6g/cm3以下,进一步优选0.5g/cm3以下。
无机填料的颗粒的形状的实例包括微粉末状、粉末状、粒状(particulateshape)、颗粒状(granular shape)、鳞片状、多面体状、棒状、含曲面的形状、和中空状等。另外,平均粒径在上述范围内的颗粒,除了将颗粒用球磨机等粉碎,将所得粗颗粒在分散剂中分散为期望的粒径,接着浓缩的方法,和将粗颗粒用筛子等筛分从而选择粒径的方法以外,可以通过使在生产颗粒的阶段的制备条件最优化,并且获得期望粒径的(纳米)颗粒的方法等来生产。
无机填料的比表面积优选为0.01m2/g以上,更优选0.5m2/g以上。另外,比表面积优选为500m2/g以下。比表面积可以通过氮吸附BET法等用比表面积测量装置来测量。
相对于100体积%的发泡性组合物层,无机填料的比例优选为0.1体积%以上,更优选1体积%以上,进一步优选5体积%以上,再优选10体积%以上,并且特别优选30体积%以上。另一方面,无机填料的比例优选为99.9体积%以下,更优选90体积%以下,进一步优选80体积%以下,再优选60体积%以下,并且特别优选50体积%以下。
(7)片状纤维基材
作为片状纤维基材,可以使用已知的那些,并且其实例具体包括通过将如玻璃纤维和碳纤维等无机纤维或如聚酯纤维、聚酰胺纤维、芳族聚酰胺纤维、维尼纶(vinylon)纤维和聚烯烃纤维等有机纤维编织或原纤化(fibrillating)获得的织布、无纺布、或单向性布等。优选的是,板件补强材料通过层压从上述已知的片状纤维基材选择的不同的两种以上的片状纤维基材来构成,并且进一步优选的是,至少一种为无机纤维或有机纤维的织布或单向性布,并且位于板件补强材料的一侧表层上。
位于板件补强材料的一侧表层上的无机纤维的织布或单向性布将韧性赋予至固化后的树脂层(下文中,固化体层),并且优选为片状,并且由轻的材料形成,并且可以与固化体层紧密接触且一体化,并且作为这样的材料,例如,使用具有刚性的碳纤维的织布、玻璃纤维的织布(玻璃布)、或单向性增强布。
玻璃布为由玻璃纤维制成的布,更具体地,其实例包括其中将多根玻璃丝的玻璃纤维束编织而成的已知的玻璃布。玻璃布中的编织结构通常为常见的平纹组织,但不限于此,例如,可以为如方平组织和重平组织等变化的平纹组织(modified plain weave)、斜纹组织、或缎纹组织等。优选的是平纹组织。另外,关于玻璃纤维束的纤维支数,进行打麻以使用树脂覆盖处理前的玻璃布的重量(基重)为150至300g/m2,并且优选为180至260g/m2。另外,玻璃布的重量可以通过依照JIS R3420:2013 7.2的测量方法来计算。另外,在由此编织的玻璃布中,通常,厚度为100至300μm,并且透气度为2至20cm3/cm2/sec。另外,透气度可以通过依照JIS R3420:2013 7.13的测量方法来计算。
作为玻璃布,更具体地,例如,可以使用玻璃纤维束的纱线支数为5至250tex(特数(tex count))、玻璃丝直径(glass filament diameter)为3至13μm、束数(bundle number)为100至800、玻璃纤维束的捻数为0.1至5.0次/25mm、玻璃纤维束的纤维支数为30至80根/25mm的玻璃布。另外,为了提高环氧树脂的纤维含浸性,玻璃布可以用硅烷偶联剂来处理。作为这样的硅烷偶联剂,具体地,例如,使用乙烯基三氯硅烷、乙烯基三乙氧基硅烷、乙烯基三(β-甲氧基乙氧基)硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-苯胺基丙基三甲氧基硅烷、N-β-氨乙基-γ-氨丙基三甲氧基硅烷、N-乙烯基苄基-氨乙基-γ-氨丙基三甲氧基硅烷(盐酸盐)、γ-环氧丙氧基丙基三甲氧基硅烷、β-(3,4-环氧环己基)乙基三甲氧基硅烷、γ-巯丙基三甲氧基硅烷、和γ-氯丙基三甲氧基硅烷等。这些硅烷偶联剂可以单独使用,或可以同时使用。其中,优选地,使用γ-环氧丙氧基丙基三甲氧基硅烷。该硅烷偶联剂对于玻璃布的附着量为例如基于玻璃布的0.01至2重量%,并且优选0.05至0.5重量%。
进一步,也可以使用通过以下方法的已经网眼堵塞(weather-stripped)至一定程度的经开纤处理(opening-treated)的玻璃布:编织玻璃纤维束以获得玻璃布(包括已经用施胶剂附着处理的玻璃布和已经用硅烷偶联剂附着处理的玻璃布),进行开纤处理例如用高压水流或在液体中的超声波处理,从而扩宽玻璃纤维束的经线和纬线。
(8)橡胶或含有橡胶组分的化合物
要求贴附至用于输送机器的车体的金属板件的补强材料具有耐寒性和耐热性。在冬季,在寒冷地区,车体外部板件的温度会由于车外环境而下降至约-20至-10℃。出于该原因,除非发泡性板件补强材料具有耐寒性,在这样的低温环境下,树脂的脆性变高,并且不会获得充分的弯曲强度。另外,在夏季,车体外部板件的温度会由于车外环境而升高至约60至70℃。出于该原因,除非发泡性板件补强材料具有耐热性,在这样的高温环境下,树脂软化,刚性降低,并且像在低温环境下一样,不会获得充分的弯曲强度。
期望提供其中在这样的高温环境和低温环境下的两种弯曲强度具有与在常温(15至25℃)环境下相比较低的变化率的发泡性板件补强材料。为了解决上述问题,本发明人发现,通过使发泡性组合物层进一步包含橡胶或含有橡胶组分的化合物(下文中,也称为橡胶化合物),可以提供如下的发泡性板件补强材料:当将发泡性板件补强材料贴着至厚度为0.8mm的冷轧钢板且将其在180℃下加热一体化以得到补强板件时,在-40℃、23℃和80℃的温度环境下以100mm的跨度测量的三点弯曲中,补强板件的-40℃和80℃下的最大点强度相对于23℃下的最大点强度的变化率为25%以下。在该发泡性板件补强材料中,在高温环境下和在低温环境下都可以期望更稳定的强度保持。变化率可以取1%、2%、5%、8%、10%、15%、20%、和25%。
作为橡胶化合物,可以使用如下的化合物:(i)在发泡性组合物层中的交联高分子基体的可塑组分中相分离为海-岛结构的岛部分,和(ii)可以展现如下物性:在-40℃、23℃和80℃的温度环境下以100mm的跨度通过三点弯曲测量补强板件而得的最大点强度中,-40℃和80℃下的最大点强度相对于23℃下的最大点强度的变化率为25%以下,所述补强板件通过将发泡性板件补强材料贴着至厚度为0.8mm的冷轧钢板且使发泡性板件补强材料和冷轧钢板在180℃下加热一体化而获得。
橡胶化合物可以在海-岛结构的界面处与交联高分子基体的可塑组分化学键合。另外,在上述化合物中,橡胶组分可以在其化学结构内化学键合。
橡胶化合物的实例包括:丁二烯橡胶颗粒、丙烯酸系橡胶颗粒、硅橡胶颗粒和橡胶聚合物颗粒的环氧树脂分散体,CTBN改性的环氧树脂,硅酮改性的环氧树脂,环氧化聚丁二烯,SBR,NBR,和聚丁烯橡胶等。上述橡胶组分或含有橡胶组分的化合物可以为固体、半固体和液体中的任一者。
特别地,优选使用丁二烯橡胶颗粒和/或丙烯酸系橡胶颗粒。
橡胶颗粒的平均粒径优选为0.01至5μm,更优选0.05至1μm。当考虑由于溶胀导致的粘度变化时,核壳型橡胶颗粒是最优选的。通过添加丁二烯橡胶颗粒和/或丙烯酸系橡胶颗粒,橡胶组分与交联高分子基体的可塑组分不相容,并且采用相分离结构,因此,树脂层的耐热性不降低,并且耐寒性可以得到改善。进一步,可以期望由于韧性的改善或粘接强度的改善导致的耐冲击性的改善。
还可以使用已经预先分散在环氧树脂中的橡胶颗粒。具体地,已经用例如超级混合机和均质机等混合搅拌装置分散在环氧树脂中的橡胶颗粒以及已经在环氧树脂中通过乳液聚合合成的橡胶颗粒对应于此。已经通过乳液聚合的过程最终形成的橡胶颗粒的平均粒径优选为0.05至5μm。通过使用已经预先分散在环氧树脂中的橡胶颗粒,存在以下优势:在生产树脂组合物时,组分的处理变得简单。另外,因为环氧树脂与橡胶颗粒充分相容,时间流逝时的粘度变化趋于小。
上述丁二烯橡胶颗粒的实例包括由MITSUBISHI RAYON CO.,LTD.制造的Metablene E系列和Metablene C系列,等。上述丙烯酸系橡胶颗粒的实例包括由SokenChemical&Engineering Co.,Ltd.制造的MX系列、由MITSUBISHI RAYON CO.,LTD.制造的Metablene W系列、和由ZEON KASEI Co.,Ltd.制造的ZEFIAC系列等。其中已经预先分散了橡胶颗粒的环氧树脂的实例包括由Resinous Kasei Co.,Ltd.制造的RKB系列、和由KanekaCorporation制造的Kane Ace系列、和丁二烯橡胶颗粒等,但不限于它们。
相对于100重量份发泡性组合物层,橡胶化合物的添加量优选为1至50重量份。当添加量大于50重量份时,刚性趋于降低,并且当添加量小于5重量份时,效果趋于不显示。最优选地,添加量为5至30重量份。
进一步,优选的是,在观察使用电子显微镜得到的加热发泡固化后的板件补强材料的截面时,分离尺度为10至1,000nm的源自橡胶的特定岛部分以在树脂部分中在3,000nm×3,000nm的范围内为10个以上的数量存在。特定岛部分的数量可以取10个、20个、30个、40个、50个、60个、70个、和100个。
(9)其它
本领域中已知的添加剂,例如硅烷偶联剂、稳定剂、润滑剂、着色剂、紫外线吸收剂、抗氧化剂、防老剂、和耐候稳定剂可以按需要包含于补强材料中。
(补强材料的制造方法)
对于补强材料,交联高分子基体通过将具有一个聚合性官能团的单官能性单体和具有两个以上的聚合性官能团的多官能性单体使用聚合引发剂聚合来获得。这里,聚合在可塑组分、固化剂、固化促进剂、填料、热分解型发泡剂和任选的橡胶化合物的存在下进行。
作为聚合引发剂,可以使用取决于例如热、紫外线和电子束等能量的已知聚合引发剂。另外,特别地,可以通过例如紫外线和电子束等能量引发聚合反应的光聚合引发剂是优选的。聚合引发剂可以单独使用,或两种以上可以通过组合它们来使用。
光聚合引发剂的实例包括肟酯系光聚合引发剂、烷基苯某酮系(alkylphenone-based)光聚合引发剂、酰基氧化膦系光聚合引发剂和二茂钛系(titanocene-based)光聚合引发剂。
相对于100重量份的具有一个聚合性官能团的单官能性单体和具有两个以上的聚合性官能团的多官能性单体的混合物,光聚合引发剂的添加量优选为0.1至2.0重量份。
作为市售品,肟酯系光聚合引发剂的实例包括由BASF Japan Ltd.制造的CGI-325、Irgacure OXE01和Irgacure OXE02,和由ADEKA CORPORATION制造的N-1919等。
烷基苯某酮系光聚合引发剂的实例包括:苄基二甲基缩酮系光聚合引发剂例如2,2-二甲氧基-1,2-二苯基乙-1-酮;α-羟基烷基苯某酮系光聚合引发剂例如1-羟基环己基苯基酮、2-羟基-2-甲基-1-苯基-丙-1-酮、1-[4-(2-羟基乙氧基)-苯基]-2-羟基-2-甲基-1-丙-1-酮和2-羟基-1-{4-[4-(2-羟基-2-甲基-丙酰基)-苄基]苯基}-2-甲基-丙-1-酮;α-氨基苯乙酮系光聚合引发剂例如2-甲基-1-[4-(甲硫基)苯基]-2-吗啉基丙酮-1,2-苄基-2-二甲基氨基-1-(4-吗啉基苯基)-丁-1-酮、2-(二甲基氨基)-2-[(4-甲基苯基)甲基]-1-[4-(4-吗啉基)苯基]-1-丁酮、和N,N-二甲基氨基苯乙酮。苄基二甲基缩酮系光聚合引发剂的市售品的实例包括由BASF Japan Ltd.制造的Irgacure 651,等。
α-羟基烷基苯某酮系光聚合引发剂的市售品的实例包括由BASF Japan Ltd.制造的Irgacure 184、DAROCUR 1173、Irgacure 2959和Irgacure 127,等。α-氨基苯乙酮系光聚合引发剂的市售品的实例包括由BASF Japan Ltd.制造的Irgacure 907、Irgacure 369和Irgacure 379,等。
酰基氧化膦系光聚合引发剂的实例包括2,4,6-三甲基苯甲酰基二苯基氧化膦、双(2,4,6-三甲基苯甲酰基)-苯基氧化膦、和双(2,6-二甲氧基苯甲酰基)-2,4,4-三甲基-戊基氧化膦等。市售品的实例包括由BASF Japan Ltd.制造的Lucirin TPO和Irgacure 819,等。
二茂钛系光聚合引发剂的实例包括双(环戊二烯基)-二苯基钛、双(环戊二烯基)-二氯钛、双(环戊二烯基)-双(2,3,4,5,6-五氟苯基)钛、和双(环戊二烯基)-双(2,6-二氟-3-(吡咯-1-基)苯基)钛等。市售品的实例包括由BASF Japan Ltd.制造的Irgacure 784,等。
具体地,补强材料可以通过经过将聚合性组合物成形为期望形状的步骤(成形步骤),和将聚合性组合物中的单体混合物用聚合引发剂聚合的步骤(聚合步骤)来生产,所述聚合性组合物包括用于形成交联高分子基体的包含单官能性单体和多官能性单体的单体混合物,以及聚合引发剂、可塑组分、固化剂、固化促进剂、填料和热分解型发泡剂。
(a)成形步骤
成形为补强材料没有特别限制,但可以采用已知方法。其实例包括使聚合性组合物铸入具有期望形状的模具的方法。其它方法的实例包括在两个由树脂膜组成的保护膜之间铸造聚合性组合物,并且将其保持在恒定厚度的方法。
例如,如下,片状纤维层可以包含于补强材料中。实例包括在将聚合性组合物在成形步骤中铸入模具中时,在铸造之前、期间和之后,将片状纤维层配置在模具中的方法。另外,实例也包括将片状纤维层放置在补强材料上,并且在其上放置另一补强材料,由此将片状纤维层用一对补强材料夹持的方法。
(b)聚合步骤
成形的聚合性组合物通过使在其中的单体混合物聚合而变为补强材料。聚合的实例包括自由基聚合反应、活性自由基聚合反应、和活性阴离子聚合反应等。上述聚合反应可以通过例如赋予例如热、紫外线和电子束等能量来引发。
(板件的补强方法)
补强方法包括:将上述补强材料贴附至板件,从而将补强材料和板件暂时固定的步骤(暂时固定步骤);和使补强材料在压敏粘合之前和之后通过加热补强材料进行固化从而固定补强材料和板件(固定步骤)。暂时固定步骤利用补强材料的压敏粘合力,并且固定步骤利用粘接力。即使当不特别除去通常存在于板件的表面上的防锈剂时,该暂时固定步骤也是可行的。补强材料的加热没有特别限制,只要其在不使树脂热分解的范围内即可,并且温度为发泡剂的分解温度T℃以上。当加热温度低于T℃时,发泡会不充分。
另外,板件没有特别限制,只要期望通过薄化而补强即可。其实例包括输送机器(例如,如门和屋顶等汽车用外部材料,车辆(例如,新干线)用地板下侧封闭板和地板下下部封闭板),机器人构件(例如,手臂、和供给杆等)、房屋构造材料(外壁贴砖),金属壳等内的碳纤维增强树脂板、钢板、和铝夹板,等。该补强方法可用于厚度为3mm以下的板件。另外,因为由补强板件构成的输送机器等与由展现与补强板件同等的弯曲强度的非补强板件构成的机器等相比重量减小,可以降低驱动和输送所需的能量。
实施例
本发明将通过实施例和比较例的方式具体地说明,但本发明不受限于这些实施例。首先,将说明实施例和比较例中的测量方法。
(分解温度T)
热分解型发泡剂的分解温度通过依照JIS K0064:1992的方法来获得。
(发泡性组合物层的150℃((分解温度T)-10℃)下的储能弹性模量G’(Pa))
动态粘弹性用粘弹性测量设备PHYSICA MCR301(AntonPaar制造)和温度控制***CTD450来测量。将固化前的直径为25mm(±1mm)且厚度为1mm(±0.1mm)的圆盘状补强材料保持在设定为测量初始温度的粘弹性测量设备的板之间,并且在法向力0.03至0.1N下调节至测量位置。进一步,在测量初始温度±1℃保持5分钟之后,应变设定为1%,频率在23℃至180℃的温度范围内以对数升降从10Hz改变至1Hz,并且动态粘弹性在温度升高速度为15℃/min、氮气环境、测量间隔为30秒且恒定法向力为0N的条件下在23℃至180℃的范围内测量,从而测量储能弹性模量G’。另外,作为板,使用一次性平行盘和一次性盘。
(发泡倍率)
根据下式,从加热发泡固化前后的补强材料的密度的测量结果来获得发泡倍率。
(发泡倍率)=(加热发泡固化前的补强材料的密度)/(加热发泡固化后的补强材料的密度)
(压敏粘合力)
将补强材料切割为2×2cm,在与其上存在有位于测量用补强材料的表层上的织布基材的表面相反的表面朝上的情况下,使用双面胶带(No.5486,Sliontec Ltd.制造),将凝胶片的另一表面贴附至双面胶带(No.5486,Sliontec Ltd.制造)固定的SUS板。探针粘性试验使用质地分析仪TX-AT(EKO Instruments制造)来进行。作为探针,使用由直径为10mm的SUS制成的探针。在将负荷500g施加至探针的压敏粘合面10秒之后,测量将探针以1mm/sec的速度剥离时的最大负荷(N)。压敏粘合力定义为通过最大负荷(N)除以压敏粘合面的面积获得的值(N/mm2)。
(弯曲强度和应变能量)
将各实施例和各比较例的各发泡性板件补强材料的剥离纸剥离,将各发泡性板件补强材料在20℃的环境下分别贴着至25mm宽×150mm长×0.8mm厚的油面冷轧钢板(SPCC-SD)(Nippon Testpanel Co.,Ltd.制造),并且将此在180℃下加热20分钟从而使增塑剂组分固化,从而制备试验片。
之后,在钢板变得向上的状态下,将各试验片以100mm的跨度支承,在沿其长度方向的中央,将试验用棒以5mm/min的压缩速度从垂直方向上侧降落,在与钢板接触之后,测量发泡体层的1mm位移时的弯曲强度(N)和弯曲强度的最大点(N)。另外,仅使用厚度为0.8mm的油面冷轧钢板(SPCC-SD),相似地进行三点弯曲强度试验,在与钢板接触之后,测量1mm位移时和2mm位移时的弯曲强度(N)、和断裂(最大)点强度(N)。
另外,从三点弯曲强度试验中获得的应力-应变曲线,在应变0(mm)至断裂点应变(mm)的积分范围内通过积分计算的面积值定义为应变能量(N·m)。
(补强材料基重)
将各实施例和各比较例的各板件补强材料切割为宽25mm和长150mm,并且将其重量用电子天平测量,并且转化为每1m2的重量,由此计算补强材料基重(g/m2)。
(用透射电子显微镜(TEM)观察橡胶化合物的相分离结构和特定岛部分的个数)
从发泡性板件补强材料的加热发泡固化后的样品切出树脂层的切片,将切片固定在样品台上,之后,使用由Leica Microsystems制造的“LEICA ULTRACUT UCT”超薄切片机来制备超薄切片(厚度70nm)。然后,将超薄切片的树脂层截面用由Hitachi High-Technologies Incorporation制造的“H-7600”透射电子显微镜通过由AMT Incorporated制造的“ER-B”CCD照相机***来拍摄,并且观察橡胶组分的相分离结构(海-岛结构)。从截面照片中计数每3,000nm×3,000nm面积中存在的相分离尺度为10至1,000nm的源自橡胶组分的岛部分(特定岛部分)。作为制备超薄切片时的染色剂,使用四氧化锇。
(实施例1至4)
溶解多官能性单体、单官能性单体和光聚合引发剂Irgacure 819从而制备单体混合物。然后,将环氧树脂、固化剂、固化促进剂、填料(微粉碎的二氧化硅、碳酸钙)和热分解型发泡剂添加至单体混合物从而获得用于生产板件补强材料的聚合用树脂组合物。多官能性单体、单官能性单体、光聚合引发剂、环氧树脂、固化剂、固化促进剂、填料和热分解型发泡剂的种类和量(重量份)在表1中示出。
然后,将模具放置在硅酮涂覆的剥离膜(100μm厚的PET)上。将树脂组合物铸入模具中,其上放置经填隙处理(filling-treated)的平织组织玻璃布(产品编号(stocknumber):EH2101-CKU,MOLYMER SSP Co.,Ltd.),进一步,放置硅酮涂覆的剥离膜(100μm厚的PET),并且均匀地铺展树脂组合物。之后,用小型UV聚合机器(J-cure1500,JATEC Co.,Ltd.制造,金属卤化物灯型号MJ-1500L)照射UV,以致在300至390nm的波长下的积分光量变为约5,000mJ/cm2,由此,获得补强材料。
(比较例1和2)
将环氧树脂、丙烯腈·丁二烯橡胶、苯乙烯·丁二烯橡胶、聚丁烯橡胶、和填料(滑石、碳酸钙和炭黑)根据表2的基于重量份的配方而混合,并且在120℃下用混炼机混炼1小时,将混料机温度降低至70℃,并且添加固化剂、固化促进剂和发泡剂,进一步混炼1小时。丙烯腈·丁二烯橡胶、苯乙烯·丁二烯橡胶、聚丁烯橡胶、滑石、碳酸钙、炭黑、固化剂、固化促进剂和发泡剂的种类和量在表2中示出。将混炼产物取出,并且用加压机加压从而将其成形为片材。将经填隙处理的平织组织玻璃布(产品编号:EH2101-CKU,MOLYMER SSP Co.,Ltd.制造)贴附至片材的一侧,并且将此用加压机进一步成形从而获得补强材料。
另外,以下示出表1和2中的缩写等的说明。
·jER828:双酚A型环氧树脂,产品名“jER828”,环氧当量180g/eqiv.,粘度13,500mPa·s,Mitsubishi Chemical Corporation制造
·DICY:双氰胺,产品名“DICY7”,Mitsubishi Chemical Corporation制造
·DCMU:3-(3,4-二氯苯基)-N,N-二甲基脲,产品名“DCMU99”,HODOGAYA CHEMICALCO.,LTD.制造
·DMAAm:N,N-二甲基丙烯酰胺,Tg=约120℃,KJ Chemicals Corporation制造
·P2HA:苯氧基二甘醇丙烯酸酯,产品名“Light acrylate P2HA”,Tg=约-20℃,KYOEISHA CHEMICAL Co.,Ltd.制造
·1.6HDDA:1,6-己二醇二丙烯酸酯,产品名“A-HD-N”,SHIN-NAKAMURA CHEMICALCO.,LTD.制造
·IRGACURE 819:双(2,4,6-三甲基苯甲酰基)-苯基氧化膦,BASF制造
·Aerosil R972:疏水性气相二氧化硅,比表面积110±20(m2/g),产品名“Aerosil R972”,EVONIK制造
·Hakuenka CC:碳酸钙,产品名“Hakuenka CC”,SHIRAISHI KOGYO KAISHA,LTD.制造
·OBSH:4,4’-氧双(苯磺酰肼),分解温度160℃,产品名“Celmike SX”,SANKYOKASEI Co.,Ltd.制造
·NBR橡胶:丙烯腈·丁二烯橡胶,产品名“Nipol1042”,丙烯腈含量33.5重量%,门尼粘度77.5(ML1+4,100℃),ZEON CORPORATION制造
·SBR橡胶:苯乙烯·丁二烯橡胶,产品名“Asaprene T-411”,苯乙烯含量30%,Asahi Kasei Corporation制造
·HV-300:聚丁烯橡胶,产品名“Nisseki Polybutene HV-300”,数均分子量1,400,JX Nikko Nisseki Energy Co.,Ltd.制造
·炭黑#3050B:炉黑,产品名“#3050B”,平均一次粒径为约0.04至0.05μm,比表面积50m2/g(BET法),Mitsubishi Chemical Corporation制造
[表1]
[表2]
从表1和2中,可见的是,实施例1至4确保轻量性和弯曲强度,具有大的断裂应变,并且可以将韧性通过加热固化赋予至板件,同时示出由于初始状态的压敏粘合性导致的充分的暂时粘着力。进一步,可见的是,即使当不从钢板除去防锈油时,实施例1至4的用补强材料的钢板的补强也是可行的。
记载于实施例1中的发泡性板件补强材料的所得加热发泡固化物的截面SEM照片(扫描电子显微镜)在图1中示出。从图1可知,在实施例1中,获得了具有泡孔直径为200至300μm(平均泡孔直径248μm)的闭孔结构的发泡体。
另外,通过以下过程测量平均泡孔直径。
关于发泡性板件补强材料的加热发泡固化物的平均泡孔直径,从加热发泡固化物层切出块状样品,样品截面的照片在10至400的放大倍率下用扫描电子显微镜(HitachiHigh-Technologies Corporation制造,型号“S-3400N”)拍摄,测量20个以上的闭孔的泡孔直径,并将其算术平均值表示为平均泡孔直径。
从图1中,因为泡孔为其中相邻泡孔之间不存在贯通的泡孔并且泡孔部分与固相部分之间的边界为包含其泡孔部分内部的封闭曲面,可以说该泡孔部分为不与隔热外侧的空间连通的闭孔。
(实施例5)
根据与实施例1相同的方式,获得了补强材料。除了使用所得补强材料,并且油面冷轧钢板改变为25mm宽×150mm长×0.6mm厚的油面冷轧钢板(SPCC-SD)(TP Giken Co.,Ltd.制造)以外,进行记载于上述“(弯曲强度和应变能量)”中的条件下的试验片的制备,以及1mm位移时和2mm位移时的弯曲强度(N)和试验片的断裂点处的弯曲强度(N)的测量。另外,还在实施例5中进行补强材料对于钢板的贴着,而不除去防锈剂。
另外,将试验片的重量用电子天平测量,并且将测量值转化为每1m2的重量,由此,计算试验片基重(g/m2)。
(比较例3)
除了不使用补强材料,并且试验片改变为25mm宽×150mm长×1.6mm厚的油面冷轧钢板(SPCC-SD)(TP Giken Co.,Ltd.制造)以外,进行记载于上述“(弯曲强度和应变能量)”中的条件下的试验片的1mm位移时和2mm位移时的弯曲强度(N)的测量。另外,因为试验片屈曲但不断裂,不能测量断裂点。出于该原因,将屈曲时弯曲强度(N)作为位移的最大点来测量。
另外,将试验片的重量用电子天平测量,并且将测量值转化为每1m2的重量,由此,计算试验片基重(g/m2)。
[表3]
从表3可知,实施例5的用补强材料补强的试验片的基重为展现与实施例5的试验片的断裂点的最大点相同的程度的比较例3的未补强的试验片的基重的约一半。该结果显示实施例5的补强材料确保了由金属板件构成的构件的重量的显著降低,而不降低弯曲强度(同时抑制了挠曲)。
(实施例6至10)
溶解多官能性单体、单官能性单体和光聚合引发剂Irgacure 819从而制备单体混合物。然后,将环氧树脂、固化剂、固化促进剂、橡胶化合物、填料(微粉碎的二氧化硅、碳酸钙)和热分解型发泡剂添加至单体混合物从而获得用于生产板件补强材料的聚合用树脂组合物。多官能性单体、单官能性单体、光聚合引发剂、环氧树脂、固化剂、固化促进剂、填料和热分解型发泡剂的种类和重量(重量份)在表4中示出。
然后,将模具放置在硅酮涂覆的剥离膜(100μm厚的PET)上。将聚合用树脂组合物铸入模具中,其上放置经填隙处理的平织组织玻璃布(产品编号:EH2101-CKU,MOLYMER SSPCo.,Ltd.),进一步,放置硅酮涂覆的剥离膜(100μm厚的PET),并且均匀地铺展树脂组合物。然后,将在300至390nm的波长下的积分光量变为5,000mJ/cm2的条件下的紫外线用由Fusion Co.,Ltd.制造的固化设备使用无极放电灯照射至聚合用组合物,由此,获得板件补强材料。
所得板件补强材料的各种物性在表4中示出。
(比较例4)
将环氧树脂、丙烯腈和丁二烯橡胶、苯乙烯和丁二烯橡胶、聚丁烯橡胶、填料(滑石、碳酸钙和炭黑)和润滑剂(硬脂酸锌)根据表5的基于重量份的配方而混合,并且在120℃下用混炼机混炼1小时,将混料机温度降低至70℃,并且添加固化剂、固化促进剂和发泡剂,进一步混炼1小时。丙烯腈和丁二烯橡胶、苯乙烯和丁二烯橡胶、聚丁烯橡胶、滑石、碳酸钙、炭黑、硬脂酸锌、固化剂、固化促进剂和发泡剂的种类和量在表5中示出。将混炼产物取出,并且用加压机加压从而将其成形为片材。将经填隙处理的平织组织玻璃布(产品编号:EH2101-CKU,MOLYMER SSP Co.,Ltd.制造)贴附至片材的一个表面,并且将此用加压机进一步成形从而获得板件补强材料。
另外,以下示出表4和5中的缩写等的说明。除了以下记载的那些以外的缩写等记载于表1和2的缩写等的说明部分。
·EPU1395:聚氨酯改性的环氧树脂(“ADEKA RESIN EPU1395”,ADEKACORPORATION制造)
·EPR-2000:NBR改性的环氧树脂,(“ADEKA RESIN EPR2000”,ADEKA CORPORATION制造)
·BPA328:丙烯酸系橡胶微颗粒分散的双酚A型环氧树脂(“ACRYSET BPA-328”,NIPPON SHOKUBAI CO.,LTD.制造)
·MX-154,257:丁二烯橡胶微颗粒分散的双酚A型环氧树脂(“Kane Ace MX-154”,Kaneka Corporation制造)
·Nipol1042:丙烯腈和丁二烯橡胶,产品名“Nipol1042”,丙烯腈含量33.5重量%,门尼粘度77.5(ML1+4,100℃),ZEON CORPORATION制造
·R972:疏水性气相二氧化硅,比表面积110±20(m2/g),产品名“Aerosil R972”,EVONIK制造
·QCEL5020:中空硼硅酸钠玻璃珠,平均粒径60μm,Potters Ballotini Co.,Ltd.制造
[表4]
[表5]
从表4和5可知,实施例6至10确保轻量性和弯曲强度,具有大的断裂应变,并且可以将韧性通过加热固化赋予至板件,同时示出由初始状态的压敏粘合性导致的充分的暂时粘着力。进一步可知,实施例6至10的补强材料具有充分的耐寒性和耐热性。
记载于实施例6、8、10中的加热发泡固化后的所得发泡性板件补强材料的截面TEM照片在图2至4中示出。从这些图中可知,实施例6、8和10包含相分离尺度为10至1,000nm的特定岛部分,并且在使用电子显微镜得到的加热发泡固化后的板件补强材料的截面照片中特定岛部分以在3,000nm×3,000nm的范围内为10个以上的数量存在。
实施例和比较例中获得的上述补强材料切割为100mm宽×100mm长,贴附至100mm宽×100mm长×0.8mm厚的油面冷轧钢板(SPCC-SD)(TP Giken Co.,Ltd.制造),并且进行在记载于上述“(弯曲强度)”中的条件下的试验片的制备。使用落锤型冲击试验装置CEAST9350(Tiast制造)作为试验装置,将冲击施加至作为打击面的试验片的钢板侧。试验速度设定为3.96m/sec,落锤负荷设定为4.3kg,使用的击打头设定为并且试验温度设定为室温。另外,在试验片在JIS K 7100:1999的记号“23/50”(温度23℃,相对湿度50%)、2级的标准环境下经过24小时以上调整状态之后,在相同的标准环境下进行测量(下文中,位移测量法)。将打击后的试验片的变形最大的点与试验片的四个角的各个点各自之间在垂直方向上的高度的差(mm)用由KEYENCECORPORATION制造的3D形状测量机VR-3200测量,并且打击后的试验片的变形最大的点与试验片的四个角的各个点之间在垂直方向上的高度的差(mm)的算术平均值定义为冲击位移(mm)。
相对于未贴附补强材料的100mm宽×100mm长×0.8mm厚的单独的油面冷轧钢板(SPCC-SD)的冲击位移(mm),用板件补强材料补强的试验片的冲击位移作为冲击时的位移抑制效果示出。
[表6]
从表6中的结果可知,在实施例11至13的板件补强材料中,板件的耐冲击性得以改善。
Claims (16)
1.一种发泡性板件补强材料,其包括:发泡性组合物层,和层压于所述发泡性组合物层上的片状纤维层,所述发泡性组合物层至少包含具有固化性的、交联高分子基体的可塑组分,所述可塑组分的固化剂,所述可塑组分的固化促进剂,交联高分子基体,填料,和分解温度为T℃的热分解型发泡剂;其中
当将储能弹性模量(G’)用动态粘弹性测量装置来测量、条件是测量温度为(T-10)℃时,所述发泡性组合物层展现的储能弹性模量(G’)为1×101至1×104Pa。
2.根据权利要求1所述的发泡性板件补强材料,其中所述热分解型发泡剂选自偶氮二甲酰胺、偶氮二异丁腈、偶氮二甲酸钡、硝基二胍、N,N’-二亚硝基五亚甲基四胺、N,N’-二甲基-N,N’-二亚硝基对苯二甲酰胺、P,P’-氧双(苯磺酰肼)、亚肼基二甲酰胺、对甲苯磺酰肼、二苯砜-3,3’-二磺酰肼、烯丙基双(磺酰肼)、对甲代亚苯基磺酰氨基脲、4,4’-氧双(苯磺酰氨基脲)、5-苯基-1,2,3,4-四唑、碳酸氢钠、碳酸铵和无水硝酸钠,其含量相对于100重量份的所述发泡性组合物层为0.1至10重量份。
3.根据权利要求1所述的发泡性板件补强材料,其中当进行在(T+20)℃下20分钟的加热发泡和固化时,所述发泡性板件补强材料展现1.5至10倍的发泡倍率。
4.根据权利要求1所述的发泡性板件补强材料,其中当所述发泡性板件补强材料通过将所述发泡性板件补强材料贴着至厚度为0.8mm的冷轧钢板且使所述发泡性板件补强材料进行在(T+20)℃下20分钟的加热发泡和固化而形成为补强板件时,所述补强板件使所述冷轧钢板展现以下性质:
在以100mm的跨度测量三点弯曲时,
(i)1mm位移时的强度为25N以上,
(ii)2mm位移时的强度为50N以上,和
(iii)直至断裂点的应变能量为0.5N·m以上。
5.根据权利要求1所述的发泡性板件补强材料,其中所述发泡性板件补强材料展现0.01至0.5N/mm2的压敏粘合力。
6.根据权利要求1所述的发泡性板件补强材料,其中所述片状纤维层为无机纤维或有机纤维的织布或单向性布并且位于所述发泡性板件补强材料的一侧表层上。
7.根据权利要求1所述的发泡性板件补强材料,其中所述交联高分子基体为具有一个聚合性官能团的单官能性单体和具有两个以上的聚合性官能团的多官能性单体的共聚物。
8.根据权利要求1所述的发泡性板件补强材料,其中所述可塑组分为在25℃的温度下展现500至30,000mPa·s范围内的粘度的液态环氧系树脂,所述液态环氧系树脂包含至少一种具有苯骨架的组分。
9.根据权利要求1所述的发泡性板件补强材料,其中所述固化剂至少包含双氰胺。
10.根据权利要求1所述的发泡性板件补强材料,其中所述固化促进剂为胺系或咪唑系固化促进剂。
11.根据权利要求1所述的发泡性板件补强材料,其中当进行在(T+20)℃下20分钟的加热发泡和固化时,所述发泡性板件补强材料提供了具有平均泡孔直径为10至500μm的闭孔结构的发泡体。
12.根据权利要求1所述的发泡性板件补强材料,其中所述发泡性板件补强材料用于补强厚度为3mm以下的板件,所述板件选自碳纤维增强树脂板、钢板和铝板。
13.根据权利要求1所述的发泡性板件补强材料,其中
所述发泡性组合物层进一步包含橡胶或含有橡胶组分的化合物,所述橡胶或含有橡胶组分的化合物在所述交联高分子基体的可塑组分中相分离为海-岛结构的岛部分,和
所述发泡性板件补强材料展现如下的物性:在-40℃、23℃和80℃的温度环境下以100mm的跨度通过三点弯曲测量补强板件而得的最大点强度中,-40℃和80℃下的最大点强度相对于23℃下的最大点强度的变化率为25%以下,所述补强板件通过将所述发泡性板件补强材料贴着至厚度为0.8mm的冷轧钢板且使所述发泡性板件补强材料和所述冷轧钢板在180℃下加热一体化而获得。
14.根据权利要求13所述的发泡性板件补强材料,其中所述岛部分包括相分离尺度为10至1,000nm的特定岛部分,在使用电子显微镜得到的加热发泡固化后的板件补强材料的截面照片中,所述特定岛部分以在3,000nm×3,000nm的范围内为10个以上的数量存在。
15.一种根据权利要求1所述的发泡性板件补强材料的制造方法,所述方法包括:通过将具有一个聚合性官能团的单官能性单体和具有两个以上的聚合性官能团的多官能性单体使用聚合引发剂聚合来获得所述交联高分子基体,其中
所述聚合在所述可塑组分、所述固化剂、所述固化促进剂、所述填料和所述热分解型发泡剂的存在下进行。
16.一种板件的补强方法,所述方法包括以下步骤:
将根据权利要求1所述的发泡性板件补强材料贴附至板件,从而将所述发泡性板件补强材料和所述板件暂时固定;和
使所述发泡性板件补强材料进行在T℃以上的加热发泡和固化。
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PCT/JP2016/084623 WO2017090618A1 (ja) | 2015-11-27 | 2016-11-22 | 発泡性パネル補強材、その製造方法及びパネルの補強方法 |
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JPH06170997A (ja) * | 1992-12-08 | 1994-06-21 | Nippon Zeon Co Ltd | 車両用制振補強構造体 |
CN1626578A (zh) * | 2003-11-04 | 2005-06-15 | 日东电工株式会社 | 钢板增强用树脂组合物、钢板增强片和钢板的增强方法 |
CN103087663A (zh) * | 2011-10-31 | 2013-05-08 | 比亚迪股份有限公司 | 一种补强胶片基体组合物及其制备方法、一种补强胶片及钢板复合材料 |
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JPH06170997A (ja) * | 1992-12-08 | 1994-06-21 | Nippon Zeon Co Ltd | 車両用制振補強構造体 |
CN1626578A (zh) * | 2003-11-04 | 2005-06-15 | 日东电工株式会社 | 钢板增强用树脂组合物、钢板增强片和钢板的增强方法 |
CN103087663A (zh) * | 2011-10-31 | 2013-05-08 | 比亚迪股份有限公司 | 一种补强胶片基体组合物及其制备方法、一种补强胶片及钢板复合材料 |
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