CN116997460A - 结构物的加强、修补方法以及结构物 - Google Patents
结构物的加强、修补方法以及结构物 Download PDFInfo
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- CN116997460A CN116997460A CN202280022044.7A CN202280022044A CN116997460A CN 116997460 A CN116997460 A CN 116997460A CN 202280022044 A CN202280022044 A CN 202280022044A CN 116997460 A CN116997460 A CN 116997460A
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- acrylate
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Landscapes
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Abstract
本发明提供一种结构物的加强、修补方法,其特征在于,在结构物的加强、修补方法中,包括:a)将预浸渍体与所述结构物的表面的形状一致地进行层叠、赋形的工序;b)将进行了所述层叠、赋形的所述预浸渍体真空加压的工序;c)将进行了所述真空加压的所述预浸渍体加热固化,制造所述预浸渍体的固化物的工序;以及d)将所述固化物粘接于所述结构物的所述表面的工序,所述预浸渍体含有树脂组合物及强化纤维(C),所述树脂组合物包含含有烯属不饱和基团的树脂(A)及聚合引发剂(B),所述聚合引发剂(B)的10小时半衰期温度为60~75℃。该结构物的加强、修补方法可以获得作业性优异、具有优异的机械强度的结构物,因此可以用于汽车构件、铁道车辆构件、航空航天器构件、船舶构件、住宅设备构件、运动构件、轻型车辆构件、建筑土木构件、OA设备等的壳体等。
Description
技术领域
本发明涉及结构物的加强、修补方法、以及利用上述结构物的加强、修补方法得到的结构物。
背景技术
利用碳纤维、玻璃纤维等强化纤维强化了的强化纤维复合材料因其在轻质的同时耐热性、机械强度优异的特征而受到关注,以汽车、航空器的壳体或各种构件为代表,在各种各样的结构体用途中的利用、在土木、建筑材料的修补用途中的需求正在扩大。
作为强化纤维复合材料的成形方法,使用如下的方法,即,使用向强化纤维浸渗热固性树脂而得的被称作预浸渍体的中间材料,利用高压釜成形、压制成形来使之固化、成形。
另外,在土木、建筑材料的修补用途中,使用将碳纤维片粘贴于修补部位后浸渗常温固化的树脂的手工铺叠成形、将成形了的强化纤维复合材料的成形板用粘接材料粘贴于修补部位的成形方法。
作为上述预浸渍体用的树脂,通常需要为兼具常温下的稳定性和基于加热等的固化性的树脂,因此一般多用以环氧树脂组合物为代表的热固性树脂。然而,使用了环氧树脂的预浸渍体由于固化反应慢,因此需要高的成形温度,并且由于在常温下也慢慢地进行固化,因此为了延迟固化需要进行冷藏保管。因而,正在推进能够实现高生产率和常温下的稳定性的自由基聚合性树脂组合物的开发。
另外,作为已有或新设的结构物的加强、修补方法,在其表面粘贴、卷绕浸渗热固性树脂而成的加强纤维片后,进行常温固化,由此来进行结构物的加强、修补(参照专利文献1)。
另外,近年来,在粘贴、卷绕强化纤维片后一边浸渗环氧树脂等粘接浸渗树脂一边进行加强、修补的工艺也得到实用化,然而要充分地加强结构物需要重叠多层地粘贴强化纤维片,在工期方面需要较长时间。另外,由于在施工现场向强化纤维片浸渗树脂,因此根据作业者的熟练度等的不同,产生树脂的浸渗情况不同等无法稳定地获得加强、修补效果的课题。
另外,也有将未固化的基质树脂连续地向纤维束浸渗、并在粘接所得的纤维片后使之固化的工艺,然而该工艺存在如下等课题,即,在使基质树脂热固化时,需要高温下的固化、或者低温下长时间的固化,若为高温,则需要加热装置、高温保持,因此现场施工困难,若为低温固化,则工期方面需要较长时间。
此外,为了省略现场的树脂的浸渗,还开发出了将工厂生产的板状的纤维强化塑料材料使用油灰状粘接树脂进行粘接的FRP板粘接工艺。然而,这些工艺中由于使用板状的纤维强化塑料材料,因此存在有无法应对具有凹凸、曲面的结构物的加强、修补的课题。
现有技术文献
专利文献
专利文献1:日本特开平9-296615号公报
发明内容
发明所要解决的课题
本发明所要解决的课题在于,提供一种工期的缩短、作业性的提高优异的结构物的加强、修补方法、以及使用上述结构物的加强、修补方法得到的机械强度优异的结构物。
用于解决课题的手段
本发明人等发现如下的结构物的加强、修补方法,即,针对结构物,将特定条件下使特定的预浸渍体固化而得的固化物与上述结构物粘接,由此实现基于预浸渍体的快速固化性(短时间固化性)、低温固化性的工期的缩短、作业性的提高,此外将上述固化物粘接于上述结构物的表面并进行一体化,由此得到具有加强、修补所必需的机械强度的结构物,从而完成了本发明。
即,本发明涉及一种结构物的加强、修补方法,其特征在于,在结构物的加强、修补方法中,包括:
a)将预浸渍体与上述结构物的表面的形状一致地层叠、赋形的工序;
b)将进行了上述层叠、赋形的上述预浸渍体真空加压的工序;
c)将进行了上述真空加压的上述预浸渍体加热固化,制造上述预浸渍体的固化物的工序;以及
d)将上述固化物粘接于上述结构物的上述表面的工序,
上述预浸渍体含有树脂组合物及强化纤维(C),上述树脂组合物包含含有烯属不饱和基团的树脂(A)及聚合引发剂(B),
上述聚合引发剂(B)的10小时半衰期温度为60~75℃。
本发明的结构物的加强、修补方法中,上述含有烯属不饱和基团的树脂(A)优选为氨基甲酸酯(甲基)丙烯酸酯和/或环氧(甲基)丙烯酸酯。
本发明的结构物的加强、修补方法中,上述氨基甲酸酯(甲基)丙烯酸酯优选为多异氰酸酯化合物与含有具有羟基及(甲基)丙烯酰基的化合物的具有羟基的化合物的反应产物。
本发明的结构物的加强、修补方法中,上述多异氰酸酯化合物优选为选自2,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯的碳二亚胺改性物以及多亚甲基多苯基多异氰酸酯中的至少1种以上的多异氰酸酯。
本发明的结构物的加强、修补方法中,上述预浸渍体的凝胶时间(100℃)优选为50~350秒。
本发明的结构物的加强、修补方法中,上述预浸渍体优选在120℃以下、并且在15分钟以内固化。
本发明的结构物的加强、修补方法中,上述树脂组合物的熔融粘度(100℃)在升温速度15℃/分钟以及频率1Hz的条件下的动态粘弹性测定中优选为0.4~900Pa·s。
本发明涉及一种结构物,其特征在于,是利用上述结构物的加强、修补方法得到的。
发明效果
本发明的结构物的加强、修补方法中,对结构物使用特定的预浸渍体,在特定条件下,使上述结构物与使用上述预浸渍体得到的固化物一体化,由此获得取得作业性的提高、以及加强、修补所必需的机械强度的结构物,因而有用。
具体实施方式
[预浸渍体]
本发明中使用的预浸渍体的特征在于,含有树脂组合物及强化纤维(C),上述树脂组合物包含含有烯属不饱和基团的树脂(A)及聚合引发剂(B),上述聚合引发剂(B)的10小时半衰期温度为60~75℃。上述预浸渍体使用强化纤维(C),由此使利用上述预浸渍体得到的固化物与结构物一体化,得到优异的机械强度,另外,树脂组合物中含有的聚合引发剂(B)的半衰期温度为上述范围内,由此能够实现有利于施工的低温固化性和快速固化性(短时间固化性),因而有用。
[含有烯属不饱和基团的树脂(A)]
上述含有烯属不饱和基团的树脂(A)没有特别限制,可以为聚合物,也可以为单体,但例如优选为氨基甲酸酯(甲基)丙烯酸酯和/或环氧(甲基)丙烯酸酯,此外,可以在含有上述氨基甲酸酯(甲基)丙烯酸酯、环氧(甲基)丙烯酸酯的同时,还含有苯乙烯化合物、单官能(甲基)丙烯酸酯化合物、含有羟基的(甲基)丙烯酸酯化合物、二(甲基)丙烯酸酯化合物以及不饱和聚酯等,它们可以单独使用,也可以并用2种以上。通过使用这些含有烯属不饱和基团的树脂(A),所得的预浸渍体的作业性及成形性优异,可以获得耐热性等各种物性优异的成形品,因此优选。
[环氧(甲基)丙烯酸酯]
作为上述环氧(甲基)丙烯酸酯,可以使环氧树脂与(甲基)丙烯酸和/或(甲基)丙烯酸酐反应而得到。通过使用上述环氧(甲基)丙烯酸酯,所得的预浸渍体的作业性及成形性优异,可以获得耐热性等各种物性优异的成形品,因此优选。作为上述环氧(甲基)丙烯酸酯中使用的环氧树脂,可以举出双酚型环氧树脂、线型酚醛型环氧树脂以及噁唑烷酮改性环氧树脂等。
[氨基甲酸酯(甲基)丙烯酸酯]
上述氨基甲酸酯(甲基)丙烯酸酯优选为多异氰酸酯化合物与含有具有羟基及(甲基)丙烯酰基的化合物的具有羟基的化合物的反应产物。通过使用上述氨基甲酸酯(甲基)丙烯酸酯,所得的预浸渍体的作业性及成形性优异,可以获得耐热性等各种物性优异的成形品,因此优选。作为上述氨基甲酸酯(甲基)丙烯酸酯,从获得耐热性等各种物性优异的成形品的观点出发,例如可以举出由多亚甲基多苯基多异氰酸酯、4,4-二苯基甲烷二异氰酸酯、羟基烷基(甲基)丙烯酸酯和双酚A的环氧烷烃加成物形成的氨基甲酸酯(甲基)丙烯酸酯等。
作为上述多异氰酸酯化合物,优选为选自2,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯的碳二亚胺改性物以及多亚甲基多苯基多异氰酸酯中的至少1种以上的多异氰酸酯。通过使用上述多异氰酸酯,所得的氨基甲酸酯(甲基)丙烯酸酯可以获得耐热性等各种物性优异的成形品,因此优选。另外,在上述多异氰酸酯化合物中,通过使用上述多亚甲基多苯基多异氰酸酯,利用与上述强化纤维(C)的表面亲和性高的多亚甲基多苯基多异氰酸酯的芳香环多核体结构,可以获得提高了与强化纤维(C)的密合性的预浸渍体、以及使用了上述预浸渍体的固化物。
上述多亚甲基多苯基多异氰酸酯为下述通式(1)所示的化合物。需要说明的是,这些多亚甲基多苯基多异氰酸酯可以单独使用,也可以并用2种以上。
[化1]
(式中,n为1以上的整数。)
作为能够用作包含上述多亚甲基多苯基多异氰酸酯的多异氰酸酯化合物的市售品,可以举出TOSOH株式会社制的“MILLIONATE MR-100”、“MILLIONATE MR-200”、万华JAPAN株式会社制的“WANNATE PM-200”、“WANNATE PM-400”、三井化学株式会社制的“COSMONATEM-1500”、DOW CHEMICAL株式会社制的“VORANATE M-595”等。
作为上述多异氰酸酯化合物,可以在含有上述多亚甲基多苯基多异氰酸酯以外,还含有二苯基甲烷二异氰酸酯(MDI)。通过使用上述二苯基甲烷二异氰酸酯(MDI),可以调整所得的氨基甲酸酯(甲基)丙烯酸酯的交联密度,获得韧性优异的固化物,因而优选。
作为上述二苯基甲烷二异氰酸酯(MDI),优选为选自2,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯以及4,4’-二苯基甲烷二异氰酸酯的碳二亚胺改性物中的至少1种。
另外,在上述多亚甲基多苯基多异氰酸酯以及上述二苯基甲烷二异氰酸酯以外,还可以使用上述二苯基甲烷二异氰酸酯的脲酸酯改性物、缩二脲改性物、氨基甲酸酯亚胺改性物、利用二乙二醇、二丙二醇等数均分子量1000以下的多元醇改性了的多元醇改性物等二苯基甲烷二异氰酸酯改性物、甲苯二异氰酸酯(TDI)、联甲苯胺二异氰酸酯、多亚甲基多苯基多异氰酸酯、苯二亚甲基二异氰酸酯、1,5-萘二异氰酸酯、四甲基二甲苯二异氰酸酯等芳香族多异氰酸酯;异佛尔酮二异氰酸酯(IPDI)、氢化二苯基甲烷二异氰酸酯、氢化苯二亚甲基二异氰酸酯、降冰片烯二异氰酸酯等脂环式多异氰酸酯;六亚甲基二异氰酸酯、六亚甲基二异氰酸酯的脲酸酯改性物、缩二脲改性物、加合物、二聚酸二异氰酸酯等脂肪族多异氰酸酯等。
上述具有羟基的化合物优选含有具有羟基及(甲基)丙烯酰基的化合物。通过使用上述具有羟基及(甲基)丙烯酰基的化合物,所得的氨基甲酸酯(甲基)丙烯酸酯的作业性及成形性优异,耐热性等各种物性优异,因而有用。
作为上述具有羟基及(甲基)丙烯酰基的化合物,例如可以举出(甲基)丙烯酸羟基烷基酯等。需要说明的是,这些具有羟基及(甲基)丙烯酰基的化合物可以单独使用,也可以并用2种以上。
作为上述(甲基)丙烯酸羟基烷基酯,例如可以举出(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸3-羟基丙酯、(甲基)丙烯酸4-羟基-正丁酯、(甲基)丙烯酸2-羟基丙酯、(甲基)丙烯酸2-羟基-正丁酯、(甲基)丙烯酸3-羟基-正丁酯等,然而优选(甲基)丙烯酸2-羟基乙酯。需要说明的是,这些(甲基)丙烯酸羟基烷基酯可以单独使用,也可以并用2种以上。
从耐热性的观点出发,上述具有羟基及(甲基)丙烯酰基的化合物在上述具有羟基的化合物中优选为35~75质量%的范围,更优选为40~70质量%。
从耐热性的观点出发,上述具有羟基的化合物在本发明的预浸渍体中使用的树脂组合物(固体成分)中优选为30~80质量%的范围,更优选为35~75质量%。
另外,作为上述具有羟基的化合物,从所得的固化物的韧性等进一步提高的方面出发,优选并用上述具有羟基及(甲基)丙烯酰基的化合物以外的其他多元醇。
作为上述其他多元醇,没有特别限定,例如可以使用双酚A的环氧烷烃加成物、芳香族二醇的环氧烷烃加成物、聚酯多元醇、丙烯酸类多元醇、聚醚多元醇、聚碳酸酯多元醇、聚亚烷基多元醇等。这些多元醇可以单独使用,也可以并用2种以上。
从预浸渍体的硬度的稳定性的观点出发,成为上述氨基甲酸酯(甲基)丙烯酸酯的原料的、上述多异氰酸酯化合物的异氰酸酯基(NCO)与上述具有羟基的化合物的羟基(OH)的摩尔比(NCO/OH)优选为0.7~1.2,更优选为0.9~1.0。
[其他含有烯属不饱和基团的树脂(A)]
作为能够与上述氨基甲酸酯(甲基)丙烯酸酯、环氧(甲基)丙烯酸酯一起含有(使用)的其他作为含有烯属不饱和基团的树脂(A)的上述苯乙烯化合物,可以举出苯乙烯、甲基苯乙烯、卤代苯乙烯、二乙烯基苯等,作为上述单官能(甲基)丙烯酸酯化合物,可以举出(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸异冰片酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸甲基苄酯、(甲基)丙烯酸苯氧基乙酯、(甲基)丙烯酸甲基苯氧基乙酯、(甲基)丙烯酸吗啉酯、丙烯酸苯基苯氧基乙酯、(甲基)丙烯酸苯基苄酯、甲基丙烯酸苯酯、(甲基)丙烯酸二环戊烯酯、(甲基)丙烯酸二环戊烯基氧乙酯、甲基丙烯酸二环戊酯等,作为上述含有羟基的(甲基)丙烯酸酯化合物,可以举出(甲基)丙烯酸羟基乙酯、(甲基)丙烯酸羟基丙酯、(甲基)丙烯酸羟基丁酯等,作为上述二(甲基)丙烯酸酯化合物,可以举出双酚A的环氧乙烷加成物的二甲基丙烯酸酯、三环癸烷二甲醇二甲基丙烯酸酯、1,12-十二烷二醇二甲基丙烯酸酯、氢化双酚A二甲基丙烯酸酯、聚1,4-丁二醇二甲基丙烯酸酯、9,9-双[4-(2-甲基丙烯酰氧基乙氧基)苯基]芴、异山梨醇的环氧乙烷加成物的二甲基丙烯酸酯、氢化双酚A的环氧乙烷加成物的二甲基丙烯酸酯、三羟甲基丙烷的环氧乙烷加成物的三甲基丙烯酸酯、季戊四醇的环氧乙烷加成物的四甲基丙烯酸酯、二季戊四醇的环氧乙烷加成物的六甲基丙烯酸酯、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、1,6-己二醇二(甲基)丙烯酸酯、双酚二(甲基)丙烯酸酯、1,4-环己烷二甲醇二(甲基)丙烯酸酯等,作为上述不饱和聚酯,是利用包含α,β-不饱和二元酸的二元酸成分与多元醇成分、单醇类的脱水缩合反应等以公知的方法合成、得到的化合物,可以优选使用数均分子量(Mn)为400~5000的范围的化合物。
作为制备上述不饱和聚酯时使用的上述α,β-不饱和二元酸,例如可以举出马来酸、马来酸酐、富马酸、衣康酸、衣康酸酐等。作为饱和二元酸,例如可以举出邻苯二甲酸、邻苯二甲酸酐、卤代邻苯二甲酸酐、间苯二甲酸、对苯二甲酸、四氯邻苯二甲酸、四氯邻苯二甲酸酐、二聚酸、2,6-萘二甲酸、2,7-萘二甲酸、2,3-萘二甲酸、2,3-萘二甲酸酐、4,4’-联苯二甲酸、以及它们的二烷基酯等芳香族二元酸、卤代饱和二元酸等。上述饱和二元酸可以单独使用,也可以并用2种以上地使用,另外,优选在全部二元酸中,不饱和二元酸成分为70~100摩尔%,而饱和二元酸为0~30摩尔%。作为多元醇,例如可以举出乙二醇、二乙二醇、三乙二醇、聚乙二醇、丙二醇、二丙二醇、聚丙二醇、1,3-丙二醇、1,3-丁二醇、新戊二醇、氢化双酚A、1,4-丁二醇、2-甲基-1,4-丁二醇、2-乙基-1,4-丁二醇、1,5-戊二醇、环己烷二甲醇、2,2,4-三甲基-1,3-戊二醇、1,6-己二醇、以双酚A、双酚F、双酚S、四溴双酚A等为代表的二元酚与以环氧丙烷或环氧乙烷为代表的环氧烷烃的加成物、1,2,3,4-四羟基丁烷、甘油、三羟甲基丙烷、季戊四醇、1,2-环己二醇、1,3-环己二醇、1,4-环己二醇、1,4-环己烷二甲醇、对二甲苯二醇、二环己基-4,4’-二醇、2,6-十氢化萘二醇、2,7-十氢化萘二醇、2-乙基-2-丁基-1,3-丙二醇、2-甲基-1,3-丙二醇、3-甲基-1,5-戊二醇等。上述多元醇优选并用2种以上地使用。
[聚合引发剂(B)]
作为上述聚合引发剂(B),10小时半衰期温度为60~75℃,优选为60~70℃。若为上述聚合引发剂(B),则没有特别限制,然而例如从常温(23℃)下的稳定性、利用含有上述聚合引发剂(B)的预浸渍体得到的固化物的低温固化性、成形时间缩短(快速固化性)的观点出发,优选有机过氧化物。
作为上述有机过氧化物,例如可以举出二酰基过氧化物化合物、过氧化酯化合物、氢过氧化物化合物、酮过氧化物化合物、烷基过酸酯化合物、过碳酸酯化合物、过氧化缩酮等,可以根据成形条件恰当地选择。需要说明的是,这些聚合引发剂(B)可以单独使用,也可以并用2种以上。
若上述有机过氧化物的10小时半衰期温度为60~75℃的范围内,则预浸渍体的常温下的贮存期(日文:ライフ)长,另外可以通过加热在短时间(15分钟以内)固化(快速固化性),施工时具有有利的低温固化性,因此优选,通过使用本发明的预浸渍体,固化性和成形性更加优异。作为此种聚合引发剂,例如可以举出过氧化2-乙基己酸1,1,3,3-四甲基丁酯、过氧化2-乙基己酸叔丁酯、过氧化异丁酸叔丁酯、过氧化异丁酸叔戊酯、过氧化2-乙基己酸叔戊酯、过氧化二异壬酰、过氧化二月桂酰、过氧化二苯甲酰、过氧化二琥珀酸、2,5-二甲基-2,5-己烷二基=双(2-乙基过氧化己酸酯)(日文:2,5-ジメチル-2,5-ヘキサンジイル=ビス(2-工チルペル才キシヘキサノァ一卜))、过氧化2-乙基己酸叔己酯、过氧化二乙基乙酸叔丁酯等,它们当中,优选过氧化2-乙基己酸1,1,3,3-四甲基丁酯、过氧化二月桂酰、过氧化二琥珀酸、2,5-二甲基-2,5-己烷二基=双(2-乙基过氧化己酸酯)、过氧化2-乙基己酸叔己酯等10小时半衰期温度为60~70℃的有机过氧化物,特别优选过氧化2-乙基己酸1,1,3,3-四甲基丁酯。
作为上述聚合引发剂(B)的含量,从固化特性和保存稳定性均优异的方面出发,在本发明的预浸渍体中使用的树脂组合物(固体成分)中,优选为0.3~3质量%的范围,更优选为0.5~2.5质量%。
[树脂组合物]
作为本发明的预浸渍体中使用的树脂组合物的熔融粘度(100℃),在使用粘弹性测定装置(MCR302、株式会社Anton Paar Japan制、测定夹具直径25mm)在升温速度15℃/分钟以及频率1Hz的条件下进行的动态粘弹性测定中,优选为0.4~900Pa·s,更优选为1~450Pa·s。通过使上述熔融粘度为上述范围内,在向上述强化纤维(C)涂布、浸渗上述树脂组合物时,产品单位面积重量(质量)稳定,所得的预浸渍体的产品的品质稳定(产品稳定性),因而有用。
[强化纤维(C)]
作为上述强化纤维(C),没有特别限制,然而从机械强度、耐久性的观点出发,优选碳纤维,从获得高强度的碳纤维的方面出发,可以更优选使用聚丙烯腈系、沥青系、人造丝系等各种强化纤维,其中,从容易地获得高强度的碳纤维的方面出发,优选聚丙烯腈系的强化纤维。
作为上述强化纤维(C)的形状没有特别限制,可以举出使强化纤维丝收束而得的强化纤维束、将强化纤维束沿一个方向并丝而得的单向材料、进行了织造的织物或包含裁短了的强化纤维的无纺布等,通过使用单向材料作为强化纤维并使之层叠、进行成形,可以获得高的机械物性,因此优选。
在织物的情况下,可以举出以平纹织物、斜纹织物、缎纹织物、或无卷曲织物为代表的将纤维束沿一个方向并丝而得的片材、将改变角度地层叠的片材以不松解的方式缝合而得的缝合片材等。
关于本发明的预浸渍体中的上述强化纤维(C)的含有率,从所得的固化物的机械强度进一步提高的方面出发,优选为35~85质量%的范围,更优选为45~75质量%的范围。
作为本发明的预浸渍体的成分,也可以使用上述的以外的化合物,例如可以含有热固性树脂、热塑性树脂、阻聚剂、固化促进剂、填充剂、低收缩剂、脱模剂、增稠剂、减稠剂、颜料、抗氧化剂、增塑剂、阻燃剂、抗菌剂、紫外线稳定剂、增强材料、光固化剂等。
[预浸渍体]
本发明的预浸渍体是通过使上述树脂组合物反应后使用而以未固化或半固化的状态形成的材料,通过使用本发明的预浸渍体,所得的固化物可以实现低温固化性、快速固化性(短时间固化性)等,得到工期的缩短、作业性优异的预浸渍体,因此优选。
[预浸渍体的制造方法]
作为上述预浸渍体的制造方法,没有特别限制,可以使用公知的方法,例如可以利用如下的工序1和接下来的工序2得到预浸渍体,即,在使用行星式混合机、液体混合装置等公知的混合机混合上述含有烯属不饱和基团的树脂(A)(例如作为多异氰酸酯化合物与含有具有羟基及(甲基)丙烯酰基的化合物的具有羟基的化合物的反应产物的氨基甲酸酯(甲基)丙烯酸酯)、聚合引发剂(B)(例如有机过氧化物)以及其他成分(例如相当于上述具有羟基的化合物的多元醇)而得的树脂组合物(溶液)中,浸渗强化纤维(C)(例如碳纤维),继而,从上面用脱模纸或脱模膜夹入,利用压延机进行压延,得到片材的工序(工序1);使上述多异氰酸酯化合物所具有的异氰酸酯基与上述具有羟基的化合物(例如(甲基)丙烯酸羟基烷基酯、以及上述多元醇等)所具有的羟基反应的工序(工序2)。作为上述反应条件,反应温度为40~80℃左右,反应时间为1~30分钟左右。另外,在工序1中,也可以在不妨碍对强化纤维(C)的浸渗性的范围中,使用使上述多异氰酸酯、上述具有羟基的化合物预先进行部分反应而得的化合物。继而,将用脱模纸等夹入的预浸渍体在10~50℃熟化(aging)12小时~48小时(工序3),可以得到固化物的制备中使用的预浸渍体。
作为本发明的预浸渍体的厚度,优选为15~1000μm,更优选为20~500μm。通过制备为上述厚度,在层叠预浸渍体时,操作变得容易,树脂组合物的浸渗变得良好,因此优选。
作为上述预浸渍体,优选为在加热温度为120℃以下、并且加热时间为15分钟以内固化的预浸渍体,更优选为在115℃以下并且在12分钟以内固化的预浸渍体。通过使上述固化中的加热温度及加热时间为上述范围内,可以实现低温固化性、快速固化性(短时间固化性)等,得到工期的缩短、作业性优异的预浸渍体,因此优选。
作为上述预浸渍体的凝胶时间(100℃),优选为50~350秒,更优选为70~320秒。通过使上述凝胶时间为上述范围内,得到作业性、成形性优异的预浸渍体,因此优选。
[结构物]
本发明涉及一种结构物,其特征在于,是利用上述结构物的加强、修补方法得到的。通过上述预浸渍体的固化物进行一体化,上述结构物的机械强度、耐久性优异,因此优选。
[结构物的加强、修补方法]
本发明涉及一种结构物的加强、修补方法,其特征在于,在结构物的加强、修补方法中,包括:
a)将预浸渍体与上述结构物的表面的形状一致地层叠、赋形的工序;
b)将进行了上述层叠、赋形的上述预浸渍体真空加压的工序;
c)将进行了上述真空加压的上述预浸渍体加热固化,制造上述预浸渍体的固化物的工序;以及
d)将上述固化物粘接于上述结构物的上述表面的工序。
作为上述结构物的加强、修补方法,若更具体地进行说明,则首先将包含强化纤维的上述预浸渍体与结构物的表面的形状一致地进行层叠或赋形,由此制备与上述表面的形状匹配的预浸渍体(工序a))。
接下来,将与上述表面的形状匹配的预浸渍体放入真空包装等中,进行真空加压,由此在维持预浸渍体的形状的同时,制备经过真空包装的预浸渍体(工序b))。
将进行了上述真空加压的预浸渍体加热,由此促进固化反应,制备上述预浸渍体的固化物(工序c))。
由于所得的上述固化物存在于真空包装内,因此从真空包装中取出上述固化物。需要说明的是,通过进行真空包装、并使之固化,可以得到与上述表面形状匹配的固化物。
此后,在需要进行加强、修补的结构物的上述表面,使用粘接剂粘接(接合)与上述表面的形状匹配的固化物,将结构物与固化物一体化(工序d))。
利用包括上述工序a)~d)的结构物的加强、修补方法,例如与缺陷、缺损部位的表面形状一致地粘接固化物,由此可以进行结构物的加强、修补,机械强度优异,因而有用。
另外,由于无需像以往那样在粘贴、卷绕强化纤维片后浸渗环氧树脂等粘接浸渗树脂,因此作业性优异而可以缩短工期,另外,由于使用已经浸渗有树脂的预浸渍体,因此可以获得稳定化的加强、修补效果,因而有用。
[粘接剂]
作为上述粘接剂,可以使用公知的粘接剂,例如可以使用采用了环氧树脂等的双组分型的粘接剂。作为上述粘接剂,具体而言,可以举出Three Bond制的常温固化型双组分型环氧粘接剂、KONISHI制的以环氧树脂和硅聚合物作为主成分的双组分混合型常温固化粘接剂等。
[固化物的制作]
作为使用上述预浸渍体进行最终固化而制备固化物的方法,使用多片预浸渍体,与结构物的表面的形状一致地进行层叠或赋形,对其进行真空包装,将与上述表面的形状匹配的预浸渍体与真空包装一起加热,进行最终固化,由此可以使多片预浸渍体密合,可以制备与上述表面的形状匹配的固化物(层叠体)。另外,真空包装的真空到达度优选为-50kPa以下,更优选为一90kPa以下。
作为使用上述预浸渍体得到固化物的方法,具体而言,可以使用如下的方法等,即,将上述预浸渍体层叠2~30片后,在-50kPa~-90kPa下进行真空包装,将加热烘箱等预先加热到100℃~160℃,向上述加热烘箱等中投入上述进行了真空包装的层叠了的预浸渍体,加热、保持1~15分钟,由此使与上述表面的形状匹配的预浸渍体固化,可以得到固化物。其后,从真空包装内中取出固化物,得到与上述表面的形状匹配的固化物。
实施例
以下举出具体的实施例,对本发明进一步详细说明。
[羟基当量]
所使用的多元醇等的羟基当量(g/eq)的测定使用以依照JIS K0070(1992)中规定的中和滴定法的方法测定的值。需要说明的是,作为上述多元醇等的羟基当量,从耐热性的观点出发,优选为50~400g/eq,更优选为90~300g/eq。
[树脂组合物的熔融粘度(100℃)]
作为本发明中使用的树脂组合物的100℃时的熔融粘度,使用粘弹性测定装置(MCR302、株式会社Anton Paar Japan制、测定夹具直径25mm),利用动态粘弹性测定来进行评价。需要说明的是,作为上述动态粘弹性测定的测定条件,在以下的条件下进行。
温度条件:室温(23℃)~150℃,
升温速度:15℃/分钟,
频率:1Hz。
作为上述树脂组合物的熔融粘度(100℃),优选为0.4~900Pa·s,更优选为1~450Pa·s。
[凝胶时间的评价]
从预浸渍体的两面剥离脱模膜,对于剥离了脱模膜的预浸渍体的凝胶时间,在100℃和110℃,分别利用依照JASO M 406-87中规定的固化特性试验的方法,将以5cm×5cm切出的样品层叠24片,使用层叠了的预浸渍体,测定出凝胶时间(秒)。
作为100℃时的凝胶时间,优选为50~350秒,更优选为70~320秒。
作为110℃时的凝胶时间,优选为20~300秒,更优选为30~200秒。
[成形性的评价]
在将预浸渍体层叠20片后,使用真空包装装置进行真空包装,分别放入预先加热到100℃和110℃的烘箱中10分钟,对分别得到的固化物的表面基于下述的基准进行确认,评价成形性。
○:没有鼓起及未固化部分,
×:有鼓起、或未固化部分。
[层间剪切强度的评价]
从上文中得到的固化物中,切出宽度10mm、长度22mm的试验片,对该试验片依照JIS K7078测定层间剪切强度(MPa),基于下述的基准,评价固化物的层间的粘接性。
○:50MPa以上,
×:小于50MPa。
[实施例1]
(预浸渍体用树脂组合物(1)的制备)
将多亚甲基多苯基多异氰酸酯与4,4’-二苯基甲烷二异氰酸酯的混合物(TOSOH株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、甲基丙烯酸2-羟基乙酯(HEMA)66质量份、NEWPOL BPE-20(三洋化成株式会社制:双酚A的EO加成物、羟基当量:164g/eq)25质量份、NEWPOL BPE-40(三洋化成株式会社制:双酚A的EO加成物、羟基当量:204g/eq)31质量份及聚合引发剂(Kayaku Nouryon株式会社“KAYAESTERTMPO-70”、过氧化2-乙基己酸1,1,3,3-四甲基丁酯、10小时半衰期温度65℃)3质量份在室温(23℃)下混合,放入聚乙烯制袋中,在45℃熟化24小时,由此得到预浸渍体用树脂组合物(1)(100℃时的熔融粘度:370Pa·s)。
(预浸渍体(1)的制作及评价)
将多亚甲基多苯基多异氰酸酯与4,4’-二苯基甲烷二异氰酸酯的混合物(TOSOH株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、甲基丙烯酸2-羟基乙酯(HEMA)66质量份、NEWPOL BPE-20(三洋化成株式会社制:双酚A的EO加成物、羟基当量:164g/eq)25质量份、NEWPOL BPE-40(三洋化成株式会社制:双酚A的EO加成物、羟基当量:204g/eq)31质量份及聚合引发剂(Kayaku Nouryon株式会社“KAYAESTERTMPO-70”、过氧化2-乙基己酸1,1,3,3-四甲基丁酯、10小时半衰期温度65℃)3质量份在室温(23℃)下混合,涂布于进行了脱模处理的聚对苯二甲酸乙二醇酯膜(NIPPA公司制、50μm、硅脱模处理)的一面后,利用手工铺叠法(日文:ハンドレイアップ法)浸渗碳纤维(三菱化学公司制“TRK979PQRW”),使得碳纤维含量为50质量%,盖上相同的膜后,在25℃1周的条件下进行熟化,由此制作出预浸渍体(1)。该预浸渍体(1)的凝胶时间在100℃时为90秒,在110℃时为30秒。
(固化物的制成及评价)
将上述预浸渍体(1)层叠20片后,使用真空包装装置以真空到达度-90kPa进行真空包装,放入预先分别加热到100℃和110℃的烘箱中10分钟,并进行保持,由此使预浸渍体固化,得到固化物后,评价基于各个温度的固化物的成形性。
[实施例2]
(预浸渍体用树脂组合物(2)的制备)
将多亚甲基多苯基多异氰酸酯与4,4’-二苯基甲烷二异氰酸酯的混合物(TOSOH株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、甲基丙烯酸2-羟基乙酯(HEMA)66质量份、NEWPOL BPE-20(三洋化成株式会社制:双酚A的EO加成物、羟基当量:164g/eq)25质量份、NEWPOL BPE-40(三洋化成株式会社制:双酚A的EO加成物、羟基当量:204g/eq)31质量份及聚合引发剂(Kayaku Nouryon株式会社“KAYAESTER O”、过氧化2-乙基己酸叔丁酯、10小时半衰期温度72℃)3质量份在室温(23℃)下混合,放入聚乙烯制袋中,在45℃熟化24小时,由此得到预浸渍体用树脂组合物(2)(100℃时的熔融粘度:375Pa·s)。
(预浸渍体(2)的制作及评价)
将多亚甲基多苯基多异氰酸酯与4,4’-二苯基甲烷二异氰酸酯的混合物(TOSOH株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、甲基丙烯酸2-羟基乙酯(HEMA)66质量份、NEWPOL BPE-20(三洋化成株式会社制:双酚A的EO加成物、羟基当量:164g/eq)25质量份、NEWPOL BPE-40(三洋化成株式会社制:双酚A的EO加成物、羟基当量:204g/eq)31质量份及聚合引发剂(Kayaku Nouryon株式会社“KAYAESTER O”、过氧化2-乙基己酸叔丁酯、10小时半衰期温度72℃)3质量份在室温(23℃)下混合,涂布于进行了脱模处理的聚对苯二甲酸乙二醇酯膜(NIPPA公司制、50μm、硅脱模处理)的一面后,利用手工铺叠法浸渗碳纤维(三菱化学公司制“TRK979PQRW”),使得碳纤维含量为50质量%,盖上相同的膜后,在25℃1周的条件下进行熟化,由此制作出预浸渍体(2)。该预浸渍体(2)的凝胶时间在100℃时为300秒,在110℃时为110秒。
(固化物的制成及评价)
将预浸渍体(2)层叠20片后,使用真空包装装置以真空到达度-90kPa进行真空包装,放入预先分别加热到100℃和110℃的烘箱中10分钟,并进行保持,由此使预浸渍体固化,得到固化物后,评价基于各个温度的固化物的成形性。
[比较例1]
(固化物的制成及评价)
将上述预浸渍体(1)层叠20片后,粘贴于玻璃板,放入预先分别加热到100℃和110℃的烘箱中10分钟,并进行保持,由此使预浸渍体固化,得到固化物后,评价基于各个温度的固化物的成形性。
[比较例2]
(固化物的制成及评价)
将上述预浸渍体(2)层叠20片后,粘贴于玻璃板,放入预先分别加热到100℃和110℃的烘箱中10分钟,并进行保持,由此使预浸渍体固化,得到固化物后,评价基于各个温度的固化物的成形性。
[比较例3]
(预浸渍体用树脂组合物(R1)的制备)
将多亚甲基多苯基多异氰酸酯与4,4’-二苯基甲烷二异氰酸酯的混合物(TOSOH株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、甲基丙烯酸2-羟基乙酯(HEMA)66质量份、NEWPOL BPE-20(三洋化成株式会社制:双酚A的EO加成物、羟基当量:164g/eq)25质量份、NEWPOL BPE-40(三洋化成株式会社制:双酚A的EO加成物、羟基当量:204g/eq)31质量份及聚合引发剂(Kayaku Nouryon株式会社“TRIGONOX 122-80C”、1,1-二(叔戊基过氧化)环己烷、10小时半衰期温度87℃)3质量份在室温(23℃)下混合,放入聚乙烯制袋中,在45℃熟化24小时,由此得到预浸渍体用树脂组合物(R1)(100℃时的熔融粘度:375Pa·s)。
(预浸渍体(R1)的制作及评价)
将多亚甲基多苯基多异氰酸酯与4,4’-二苯基甲烷二异氰酸酯的混合物(TOSOH株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、甲基丙烯酸2-羟基乙酯(HEMA)66质量份、NEWPOL BPE-20(三洋化成株式会社制:双酚A的EO加成物、羟基当量:164g/eq)25质量份、NEWPOL BPE-40(三洋化成株式会社制:双酚A的EO加成物、羟基当量:204g/eq)31质量份及聚合引发剂(Kayaku Nouryon株式会社“TRIGONOX 122-80C”、1,1-二(叔戊基过氧化)环己烷、10小时半衰期温度87℃)3质量份在室温(23℃)下混合,涂布于进行了脱模处理的聚对苯二甲酸乙二醇酯膜(NIPPA公司制、50μm、硅脱模处理)的一面后,利用手工铺叠法浸渗碳纤维(三菱化学公司制“TRK979PQRW”),使得碳纤维含量为50质量%,盖上相同的膜后,在25℃1周的条件下进行熟化,由此制作出预浸渍体(R1)。关于该预浸渍体(R1)的凝胶时间,由于在100℃及110℃未固化,无法进行测定、评价,因此进一步升温到120℃、130℃以及140℃,其结果是,在120℃依然未固化,130℃时的凝胶时间为80秒,140℃时的凝胶时间为50秒。
(固化物的制成及评价)
将预浸渍体(R1)层叠20片后,使用真空包装装置以真空到达度-90kPa进行真空包装,放入预先分别加热到100℃和110℃的烘箱中10分钟,并进行保持,由此使预浸渍体固化,得到固化物后,评价基于各个温度的固化物的成形性。
[表1]
根据上述评价结果可以确认,在实施例1中,通过使用所期望的预浸渍体,经过在100℃进行真空加压的工序,可以得到固化物的成形性、层间剪切强度优异的固化物。另外可以确认,在实施例2中,通过使用所期望的预浸渍体,经过在与有机过氧化物的分解温度对应的110℃进行真空加压的工序,可以得到固化物的成形性、层间剪切强度优异的固化物。
另一方面可以确认,比较例1及比较例2虽然分别使用了与实施例1及实施例2相同的预浸渍体,然而没有进行真空加压的工序,因此固化物的成形性差,层间剪切强度差。实施例2和比较例2中,虽然尝试将预浸渍体在100℃加热来得到固化物(固化板),然而由于有机过氧化物的10小时半衰期温度比实施例1高,因此低温固化性差,无法得到固化物本身。
另外,比较例3中,制造预浸渍体时使用的聚合引发剂(B)的10小时半衰期温度不包含于所期望的范围中,而是使用了显示出高的温度的聚合引发剂,因此若为120℃以下的固化温度,则导致有机过氧化物的性能不足,无法测定凝胶时间,另外,无法得到固化物本身。
产业上的可利用性
本发明中,将使特定的预浸渍体在特定条件下固化而得的固化物与上述结构物粘接,由此实现基于预浸渍体的快速固化性(短时间固化性)、低温固化性的工期的缩短、作业性的提高,并且将上述固化物粘接于上述结构物的表面而使之一体化,由此得到具有加强、修补所必需的机械强度的结构物,因此可以用于汽车构件、铁道车辆构件、航空航天器构件、船舶构件、住宅设备构件、运动构件、轻型车辆构件、建筑土木构件、OA设备等的壳体等,特别是适于住宅设备构件、建筑土木构件等的使用。
Claims (8)
1.一种结构物的加强、修补方法,其特征在于,在结构物的加强、修补方法中,包括:
a)将预浸渍体与所述结构物的表面的形状一致地层叠、赋形的工序;
b)将进行了所述层叠、赋形的所述预浸渍体真空加压的工序;
c)将进行了所述真空加压的所述预浸渍体加热固化,制造所述预浸渍体的固化物的工序;以及
d)将所述固化物粘接于所述结构物的所述表面的工序,
所述预浸渍体含有树脂组合物及强化纤维(C),所述树脂组合物包含含有烯属不饱和基团的树脂(A)及聚合引发剂(B),
所述聚合引发剂(B)的10小时半衰期温度为60℃~75℃。
2.根据权利要求1所述的结构物的加强、修补方法,其特征在于,
所述含有烯属不饱和基团的树脂(A)为氨基甲酸酯(甲基)丙烯酸酯和/或环氧(甲基)丙烯酸酯。
3.根据权利要求2所述的结构物的加强、修补方法,其特征在于,
所述氨基甲酸酯(甲基)丙烯酸酯为多异氰酸酯化合物与含有具有羟基及(甲基)丙烯酰基的化合物的具有羟基的化合物的反应产物。
4.根据权利要求3所述的结构物的加强、修补方法,其特征在于,
所述多异氰酸酯化合物为选自2,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯的碳二亚胺改性物以及多亚甲基多苯基多异氰酸酯中的至少1种以上的多异氰酸酯。
5.根据权利要求1~4中任一项所述的结构物的加强、修补方法,其特征在于,
所述预浸渍体在120℃以下、在15分钟以内固化。
6.根据权利要求1~5中任一项所述的结构物的加强、修补方法,其特征在于,
所述预浸渍体的100℃时的凝胶时间为50秒~350秒。
7.根据权利要求1~6中任一项所述的结构物的加强、修补方法,其特征在于,
所述树脂组合物的100℃时的熔融粘度在升温速度15℃/分钟以及频率1Hz的条件下的动态粘弹性测定中为0.4Pa·s~900Pa·s。
8.一种结构物,其特征在于,是利用权利要求1~7中任一项所述的结构物的加强、修补方法获得的。
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