CN111133040B - 预浸渍体用树脂组合物、预浸渍体及成型品 - Google Patents
预浸渍体用树脂组合物、预浸渍体及成型品 Download PDFInfo
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- CN111133040B CN111133040B CN201880062790.2A CN201880062790A CN111133040B CN 111133040 B CN111133040 B CN 111133040B CN 201880062790 A CN201880062790 A CN 201880062790A CN 111133040 B CN111133040 B CN 111133040B
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Abstract
提供一种预浸渍体用树脂组合物,其特征在于,其为以氨基甲酸酯(甲基)丙烯酸酯(A)及聚合引发剂(B)为必需成分的预浸渍体用树脂组合物,上述氨基甲酸酯(甲基)丙烯酸酯(A)为多异氰酸酯(a1)、多元醇(a2)与(甲基)丙烯酸羟烷基酯(a3)的反应物,上述多异氰酸酯(a1)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、及多亚甲基多苯基多异氰酸酯中的1种以上多异氰酸酯,上述多元醇(a2)具有芳香环及氧化烯结构。本发明的预浸渍体用树脂组合物的操作性及成型性优异,可得到外观、耐热性等各种物性优异的成型品,因此可以适宜用于预浸渍体及其成型品。
Description
技术领域
本发明涉及操作性及成型性优异、可得到耐热性等各种物性优异的成型品的预浸渍体用树脂组合物、预浸渍体及其成型品。
背景技术
经碳纤维、玻璃纤维等强化纤维强化后的纤维强化树脂复合材料由于轻质且耐热性、机械强度优异的特征而受到关注,在以汽车、航空器的壳体或各种构件为代表的各种结构体用途中的应用正大扩大。作为该纤维强化树脂复合材料的成型方法,使用例如下述方法:使用在强化纤维中浸渗有热固化性树脂的被称为预浸渍体的中间材料,通过高压釜成型、冲压成型而使其固化、成型的方法。
作为预浸渍体用树脂,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,因此通常大多使用以环氧树脂组合物为代表的热固化性树脂。但是,使用环氧树脂的预浸渍体会在常温下进行固化,因此有需要冷藏保管的问题。
为了解决该问题,正在进行可以实现高生产率和常温下的稳定性的成型材料的开发(例如,参照专利文献1。)。该成型材料虽然包含具有特定结构的氨基甲酸酯(甲基)丙烯酸酯化合物和强化纤维,但是有预浸渍体所需的操作性(粘性)及成型性不充分的问题。
因此,需要具有优异的操作性及成型性且可得到耐热性等各种物性优异的成型品的材料。
现有技术文献
专利文献
专利文献1:日本特开2016-29133号公报
发明内容
发明要解决的课题
本发明所要解决的课题是提供:熔融粘度低、操作性及成型性优异且可得到耐热性、层间剪切强度等各种物性优异的成型品的预浸渍体用树脂组合物;预浸渍体;及其成型品。
用于解决课题的方案
本发明人等发现,就以特定的氨基甲酸酯(甲基)丙烯酸酯、聚合引发剂及强化纤维为必需原料的预浸渍体用树脂组合物及预浸渍体而言,其操作性及成型性优异,可得到耐热性、层间剪切强度等各种物性优异的成型品,从而完成了本发明。
即,涉及预浸渍体用树脂组合物、预浸渍体及其成型品,所述预浸渍体用树脂组合物的特征在于,其为以氨基甲酸酯(甲基)丙烯酸酯(A)及聚合引发剂(B)为必需成分的预浸渍体用树脂组合物,上述氨基甲酸酯(甲基)丙烯酸酯(A)为多异氰酸酯(a1)、多元醇(a2)与(甲基)丙烯酸羟烷基酯(a3)的反应物,上述多异氰酸酯(a1)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、及多亚甲基多苯基多异氰酸酯中的1种以上多异氰酸酯,上述多元醇(a2)具有芳香环及氧化烯结构。
发明效果
由本发明的预浸渍体用树脂组合物及预浸渍体得到的成型品的耐热性、层间剪切强度等优异,因此可以适宜用于汽车构件、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。
具体实施方式
本发明的预浸渍体用树脂组合物为以氨基甲酸酯(甲基)丙烯酸酯(A)、聚合引发剂(B)及强化纤维(C)为必需成分的预浸渍体,上述氨基甲酸酯(甲基)丙烯酸酯(A)为多异氰酸酯(a1)、多元醇(a2)与(甲基)丙烯酸羟烷基酯(a3)的反应物,上述多异氰酸酯(a1)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、及多亚甲基多苯基多异氰酸酯中的1种以上多异氰酸酯,上述多元醇(a2)具有芳香环及氧化烯结构。
上述氨基甲酸酯(甲基)丙烯酸酯(A)为多异氰酸酯(a1)、多元醇(a2)与(甲基)丙烯酸羟烷基酯(a3)的反应物。
上述多异氰酸酯(a1)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及多亚甲基多苯基多异氰酸酯中的1种以上多异氰酸酯,从进一步提高成型品的耐热性的角度出发,优选包含多亚甲基多苯基多异氰酸酯。
作为上述氨基甲酸酯(甲基)丙烯酸酯(A)的异氰酸酯原料,可以组合使用上述多异氰酸酯(a1)以外的其他多异氰酸酯。作为其他多异氰酸酯,可以使用例如: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1,000以下的多元醇改性的多元醇改性物、甲苯二异氰酸酯(TDI)、二甲基联苯二异氰酸酯、苯二亚甲基二异氰酸酯、1,5-萘二异氰酸酯、四甲基间苯二亚甲基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。
上述多异氰酸酯(a1)在上述氨基甲酸酯(甲基)丙烯酸酯(A)的异氰酸酯原料中优选为20质量%以上,更优选为50质量%以上。
上述多元醇(a2)具有芳香环及氧化烯结构,从耐热性进一步提高的角度出发,羟基当量优选为90~300g/eq。
上述多元醇(a2)可列举例如:双酚A的环氧烷加成物、双酚S的环氧烷加成物、及双酚F的环氧烷加成物等双酚化合物的环氧烷加成物;1,3-双(2-羟基乙氧基)苯、1,4-双(2-羟基乙氧基)苯等二羟基苯化合物的环氧烷加成物;2’-[(1,1’-联苯基-4,4’-二基)双氧]双乙醇等联苯酚化合物的环氧烷加成物;二羟基萘化合物的环氧烷加成物、9,9-双[4-(2-羟基乙氧基)苯基]芴等。这些之中,优选双酚A的环氧烷加成物、二羟基苯化合物的环氧烷加成物。这些多元醇(a2)可以单独使用,也可以将两种以上组合使用。
另外,根据需要,作为上述氨基甲酸酯(甲基)丙烯酸酯(A)的原料,也可以组合使用上述多元醇(a2)以外的多元醇。作为上述多元醇(a2)以外的其他多元醇,可以使用聚酯多元醇、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。
作为上述(甲基)丙烯酸羟烷基酯(a3),可列举例如:(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸3-羟丙酯、(甲基)丙烯酸4-羟基-正丁酯、(甲基)丙烯酸2-羟丙酯、(甲基)丙烯酸2-羟基-正丁酯、(甲基)丙烯酸3-羟基-正丁酯等,优选(甲基)丙烯酸2-羟乙酯。需要说明的是,这些(甲基)丙烯酸羟烷基酯(a3)可以单独使用,也可以将两种以上组合使用。
上述(甲基)丙烯酸羟烷基酯(a3)在预浸渍体用树脂组合物中优选为5~50质量%的范围。
成为上述氨基甲酸酯(甲基)丙烯酸酯(A)的原料的、异氰酸酯化合物的异氰酸酯基(NCO)与具有羟基的化合物的羟基(OH)的摩尔比(NCO/OH)优选为0.7~1.5,更优选为0.8~1.3,进一步优选为0.8~1.0。
作为上述聚合引发剂(B),没有特别限定,优选有机过氧化物,可列举例如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(日文:アルキルパーエステル)化合物、过碳酸酯(日文:パーカーボネート)化合物、过氧化缩酮等,可以根据成型条件适宜选择。需要说明的是,这些聚合引发剂(B)可以单独使用,也可以将两种以上组合使用。
另外,为了缩短成型时间,这些之中,优选使用用于得到10小时半衰期的温度为70℃以上且100℃以下的聚合引发剂。若为70℃以上且100℃以下,则预浸渍体的常温下的贮存期长,另外通过加热可以在短时间(5分钟以内)固化,因此优选,通过与本发明的预浸渍体组合,从而固化性和成型性更优异。作为这类聚合引发剂,可列举例如:1,6-双(叔丁基过氧化羰氧基)己烷、1,1-双(叔丁基过氧化)环己烷、1,1-双(叔戊基过氧化)环己烷、1,1-双(叔己基过氧化)环己烷、过氧化二乙基乙酸叔丁酯、过氧化异丙基碳酸叔丁酯、过氧化异丙基碳酸叔戊酯、过氧化异丙基碳酸叔己酯、过氧化六氢对苯二甲酸二叔丁酯、过氧化三甲基己酸叔戊酯、过氧化-2-乙基己酸叔己酯等。
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角度出发,在预浸渍体用树脂组合物中优选为0.3~3质量%的范围。
另外,作为本发明的预浸渍体用树脂组合物的原料,可以根据需要使用烯属不饱和单体。作为这些烯属不饱和单体,可列举例如:苯乙烯、甲基苯乙烯、卤代苯乙烯、二乙烯基苯等苯乙烯化合物;(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(日文:モルホリン(メタ)アクリレート)、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)丙烯酸二环戊二烯酯、(甲基)丙烯酸二环戊二烯氧基乙酯、甲基丙烯酸二环戊基酯等单官能(甲基)丙烯酸酯化合物;(甲基)丙烯酸羟乙酯、(甲基)丙烯酸羟丙酯、(甲基)丙烯酸羟丁酯等含羟基的(甲基)丙烯酸酯化合物;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)丙烯酸酯等二(甲基)丙烯酸酯化合物等。这些可以单独使用,也可以将两种以上组合使用。
这些之中,从操作环境时的臭气及危险物的处理上、成型体的机械强度及耐热性出发,优选分子量150~250的单官能(甲基)丙烯酸酯,更优选(甲基)丙烯酸苯氧基乙酯、(甲基)丙烯酸甲基苯氧基乙酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸甲基苄酯,进一步优选(甲基)丙烯酸苯氧基乙酯、(甲基)丙烯酸苄酯。
从操作性(粘性)与耐热性、固化性的平衡出发,本发明的预浸渍体用树脂组合物中的上述烯属不饱和单体优选为50质量%以下,更优选为30质量%以下。
作为本发明的预浸渍体用树脂组合物的成分,也可以使用上述成分以外的成分,例如可以含有热固化性树脂、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、减粘剂、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。
作为上述热固化性树脂,可列举例如乙烯基酯树脂、不饱和聚酯树脂、酚树脂、三聚氰胺树脂、呋喃树脂等。另外,这些热固化性树脂可以单独使用,也可以将两种以上组合使用。
作为上述热塑性树脂,可列举例如:聚酰胺树脂、聚对苯二甲酸乙二醇酯树脂、聚对苯二甲酸丁二醇酯树脂、聚碳酸酯树脂、氨基甲酸酯树脂、聚丙烯树脂、聚乙烯树脂、聚苯乙烯树脂、丙烯酸类树脂、聚丁二烯树脂、聚异戊二烯树脂及通过共聚等对这些进行改性而得的树脂。这些之中,优选聚酰胺树脂、氨基甲酸酯树脂。另外,这些热塑性树脂可以单独使用,也可以将两种以上组合使用。另外,热增塑树脂可以以粒子状来添加并使用,也可以熔融混合后使用。在使用粒子状的热塑性树脂的情况下,从在纤维中的分散性的观点出发,粒径优选为30μm以下,更优选为20μm。
作为上述阻聚剂,可列举例如:氢醌、三甲基氢醌、对叔丁基儿茶酚、叔丁基氢醌、甲苯氢醌(日文:トルハイドロキノン)、对苯醌、萘醌、氢醌单甲醚、吩噻嗪、环烷酸铜、氯化铜等。这些阻聚剂可以单独使用,也可以将两种以上组合使用。
作为上述固化促进剂,可列举例如:环烷酸钴、辛烯酸钴、辛烯酸氧钒、环烷酸铜、环烷酸钡等金属皂类;乙酰乙酸氧钒(日文:バナジルアセチルアセテート)、乙酰乙酸钴、乙酰丙酮铁等金属螯合物。另外,作为胺类,可列举:N,N-二甲基氨基-对苯甲醛、N,N-二甲基苯胺、N,N-二乙基苯胺、N,N-二甲基-对甲苯胺、N-乙基-间甲苯胺、三乙醇胺、间甲苯胺、二亚乙基三胺、吡啶、苯基吗啉、哌啶、二乙醇苯胺等。这些固化促进剂可以单独使用,也可以将两种以上组合使用。
作为上述填充剂,有无机化合物、有机化合物,可以用于调整成型品的强度、弹性模量、抗冲强度、疲劳耐久性等物性。
作为上述无机化合物,可列举例如:碳酸钙、碳酸镁、硫酸钡、云母、滑石、高岭土、粘土、硅藻土、石棉、重晶石(日文:バーライト)、氧化钡、二氧化硅、硅砂、白云石、石灰石、石膏、铝微粉、中空球、氧化铝、玻璃粉、氢氧化铝、寒水石、氧化锆、三氧化锑、氧化钛、二氧化钼、铁粉等。
作为上述有机化合物,有纤维素、几丁质等天然多糖类粉末、合成树脂粉末等,作为合成树脂粉末,可以使用:由硬质树脂、软质橡胶、弹性体或聚合物(共聚物)等构成的有机物的粉体、具有芯壳型等多层结构的粒子。具体而言,可列举:丙烯酸类粒子、聚酰胺粒子、丁二烯橡胶和/或丙烯酸类橡胶、聚氨酯橡胶、硅橡胶等所构成的粒子、聚酰亚胺树脂粉末、氟树脂粉末、酚树脂粉末等。这些填充剂可以单独使用,也可以将两种以上组合使用。
作为上述脱模剂,可列举例如:硬脂酸锌、硬脂酸钙、石蜡、聚乙烯蜡、巴西棕榈蜡等。优选列举石蜡、聚乙烯蜡、巴西棕榈蜡等。这些脱模剂可以单独使用,也可以将两种以上组合使用。
作为上述增稠剂,可列举例如:氧化镁、氢氧化镁、氧化钙、氢氧化钙等金属氧化物或金属氢氧化物等;丙烯酸类树脂系微粒等,可以根据本发明的预浸渍体的处理性而适宜选择。这些增稠剂可以单独使用,也可以将两种以上组合使用。
从成型性及所得到的成型品的外观进一步提高的角度出发,本发明的预浸渍体用树脂组合物中的120℃下的熔融粘度优选为300~30000mPa·s,更优选为300~15000mPa·s,进一步优选为300~3000mPa·s。
本发明的预浸渍体含有上述预浸渍体用树脂组合物及上述强化纤维(C),作为上述强化纤维(C),可列举:碳纤维、玻璃纤维、碳化硅纤维、氧化铝纤维、硼纤维、金属纤维、芳族聚酰胺纤维、维尼纶纤维、蒂托轮纤维等有机纤维等,从得到更高强度、更高弹性的成型品的角度出发,优选碳纤维或玻璃纤维,更优选碳纤维。这些强化纤维(C)可以单独使用,也可以将两种以上组合使用。
作为上述碳纤维,可以使用聚丙烯腈系、沥青系、人造丝系等各种碳纤维,这些之中,从容易得到高强度的碳纤维的角度出发,优选聚丙烯腈系碳纤维。
作为上述强化纤维(C)的形状,没有特别限定,可列举: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、织造的织物或裁短的强化纤维、或者、包含裁短的强化纤维的无纺布或纸等,通过使用单向材料作为强化纤维并使其层叠、进行成形,从而可得到高机械物性,因此优选。
在使用裁短的强化纤维的情况下,从成型时在模具内的流动性、成型品的外观进一步改善的角度出发,优选使用切成2.5~50mm的碳纤维。
为织物的情况下,可列举:以平纹织物、斜纹织物、缎纹织物或非绉纹织物(日文:ノン·クリンプト·ファブリック)为代表的将纤维束沿一个方向并丝而得的片材、将改变角度而层叠后的这种片材以不松解的方式缝合而得的缝合片材等。
作为强化纤维的基重(每1m2纤维的重量),没有特别限制,优选为10g/m2~650g/m2。若达到10g/m2以上的基重,则纤维宽度不均变少且机械物性变得良好,因此优选。若为650g/m2以下的基重,则树脂的浸渗变得良好,因此优选。该基重进一步更优选为50~500g/m2,特别优选为50~300g/m2。
从得到的成型品的机械强度进一步提高的角度出发,本发明的预浸渍体中的、上述强化纤维(C)的含有率优选为20~85质量%的范围,更优选为40~80质量%的范围。
本发明的预浸渍体例如可以通过下述的工序1和工序2而得到,工序1:在使用行星式混合机、捏合机等公知的混合机将上述多异氰酸酯(a1)、上述多元醇(a2)、(甲基)丙烯酸羟烷基酯(a3)及聚合引发剂(B)混合而成的树脂溶液中,浸渗上述强化纤维(C),再从上表面用脱模PET膜夹住,用压延机进行压延而得到片;工序2:将其在常温~50℃下静置,使上述多异氰酸酯(a1)所具有的异氰酸酯基、与上述多元醇(a2)及上述(甲基)丙烯酸羟烷基酯(a3)所具有的羟基反应。另外,在工序1中,也可以在不损害对纤维的浸渗性的范围内,使用使上述多异氰酸酯(a1)、上述多元醇(a2)与(甲基)丙烯酸羟烷基酯(a3)预先部分地进行了反应的反应产物。
本发明的预浸渍体的厚度优选为0.02~1.0mm。若为0.02mm以上的厚度,则层叠处理变得容易,因此优选,若为1mm以下的厚度,则树脂的浸渗变得良好,因此优选。另外,更优选为0.05~0.5mm。
作为由上述所得到的预浸渍体来得到成型品的方法,可以使用例如下述方法:从预浸渍体剥离上述脱模PET膜,将8~16片预浸渍体层叠,之后放入预先加热到110℃~160℃的模具中,用压缩成型机进行合模而对预浸渍体赋形,保持0.1~10MPa的成型压力而使预浸渍体固化,之后取出成型品而得到成型品。这种情况下,优选如下制造方法:在具有剪刃(日文:シェアエッジ)的模具内,在模具温度120℃~160℃下,以每1mm的成型品厚度为1~2分钟的规定时间,保持1~8MPa的成型压力,进行加热压缩成型的制造方法。
由本发明的预浸渍体得到的成型品由于耐热性、层间剪切强度等优异,因此可以适宜用于汽车构件、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。
实施例
以下列举具体实施例更详细地说明本发明。
(实施例1:预浸渍体用树脂组合物(1)的制造及评价)
将多亚甲基多苯基多异氰酸酯与二苯基甲烷二异氰酸酯的混合物(东曹株式会社制“MILLIONATE MR-200”)100质量份、甲基丙烯酸羟乙酯(以下简单记作“HEMA”。)95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)6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)7质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox122-C80”、有机过氧化物)3质量份混合,得到预浸渍体用树脂组合物(1)。
另外,将多亚甲基多苯基多异氰酸酯与二苯基甲烷二异氰酸酯的混合物(东曹株式会社制“MILLIONATE MR-200”)100质量份、HEMA 95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)6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)7质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(1)。该预浸渍体(1)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为0.92。另外,厚度为0.25mm。
[熔融粘度的评价]
用锥板式粘度计(MST Engineering株式会社制、CONE PLATE VISCOMETER、型号CV-1S)测定上述得到的预浸渍体用树脂组合物(1)的熔融粘度,按照下述基准评价。
◎:小于3000mPa·s
○:3000mPa·s以上且小于15000mPa·s
△:15000mPa·s以上
×:不熔融
[操作性(粘性)的评价]
按照下述基准评价在室温下将上述得到的预浸渍体(1)从脱模膜(SP-PET)剥离时的操作性。
○:脱模膜上无树脂附着
×:脱模膜上有树脂附着
[成型品的制作]
将8片上述得到的预浸渍体(1)层叠,使用300mm×300mm×3mm的板状模具在模具温度140℃、合模压力0.98MPa的条件下进行5分钟加热加压成型,从而得到成型品(1)。
[成型性的评价]
测定预浸渍体(1)的碳纤维含有率与上述得到的成型品(1)的碳纤维含有率之差,按照下述基准评价成型性。
○:碳纤维含有率之差小于5%
△:碳纤维含有率之差为5%以上且小于10%
×:碳纤维含有率之差为10%以上
[耐热性]
从上述得到的成型品(1)切出宽5mm、长55mm的试验片,对于该试验片,使用SIINanotechnology公司制造的“DMS6100”对测定频率1Hz、升温速度3℃/分钟、基于固化物的两端弯曲的动态粘弹性进行测定。将得到的储能模量图中的玻璃区域的近似直线与转变区域的切线的交点作为玻璃化转变温度,按照下述基准评价耐热性。
◎:玻璃化转变温度为140℃以上
○:玻璃化转变温度为120℃以上且低于140℃
△:玻璃化转变温度为100℃以上且低于120℃
×:玻璃化转变温度低于100℃
[成型品的层间剪切强度]
从上述得到的成型品(1)切出宽10mm、长度22mm的试验片,对于该试验片,按照JISK7078测定层间剪切强度,按照下述基准进行评价。
○:75MPa以上
×:小于75MPa
(实施例2:预浸渍体用树脂组合物(2)的制造及评价)
将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATEMR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、HEMA 66质量份、NewpolBPE-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、NewpolBPE-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、聚酰胺粒子(Arkema制“2001UD”、平均粒径5μm)11质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,得到预浸渍体用树脂组合物(2)。
另外,将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、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、聚酰胺粒子(Arkema制“2001UD”、平均粒径5μm)11质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(2)。该预浸渍体(2)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为0.94。另外,厚度为0.25mm。
(实施例3:预浸渍体用树脂组合物(3)的制造及评价)
将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATEMR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、HEMA 71质量份、NewpolBP-23P(三洋化成株式会社制:双酚A的PO加成物、羟基当量;178g/eq)48质量份、丙烯酸类粒子(积水化成品工业株式会社制“Techpolymer AFX-8”、平均粒径8μm)11质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,得到预浸渍体用树脂组合物(3)。
另外,将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、HEMA 71质量份、Newpol BP-23P(三洋化成株式会社制:双酚A的PO加成物、羟基当量;178g/eq)48质量份、丙烯酸类粒子(积水化成品工业株式会社制“Techpolymer AFX-8”、平均粒径8μm)11质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(3)。该预浸渍体(3)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为0.94。另外,厚度为0.25mm。
(实施例4:预浸渍体用树脂组合物(4)的制造及评价)
将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATEMR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、HEMA 55质量份、1,3-双羟基乙氧基苯(三井化学Fine株式会社制“DER”、羟基当量;99g/eq)38质量份、甲基丙烯酸苯氧基乙酯10质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,得到预浸渍体用树脂组合物(4)。
另外,将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、HEMA 55质量份、1,3-双羟基乙氧基苯(三井化学Fine株式会社制“DER”、羟基当量;99g/eq)38质量份、甲基丙烯酸苯氧基乙酯10质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(4)。该预浸渍体(4)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为0.95。另外,厚度为0.25mm。
(实施例5:预浸渍体用树脂组合物(5)的制造及评价)
将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATEMR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、HEMA 88质量份、NewpolBPE-100(三洋化成株式会社制:双酚A的EO加成物、羟基当量;334g/eq)51质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)4质量份混合,得到预浸渍体用树脂组合物(5)。
另外,将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATE MR-200”)50质量份、4,4’-二苯基甲烷二异氰酸酯50质量份、HEMA 88质量份、Newpol BPE-100(三洋化成株式会社制:双酚A的EO加成物、羟基当量;334g/eq)51质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)4质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(5)。该预浸渍体(5)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为0.93。另外,厚度为0.25mm。
(实施例6:预浸渍体用树脂组合物(6)的制造及评价)
将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATEMR-200”)10质量份、4,4’-二苯基甲烷二异氰酸酯90质量份、HEMA 45质量份、NewpolBPE-40(三洋化成株式会社制:双酚A的EO加成物、羟基当量;204g/eq)96质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)4质量份混合,得到预浸渍体用树脂组合物(6)。
另外,将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATE MR-200”)10质量份、4,4’-二苯基甲烷二异氰酸酯90质量份、HEMA 45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)96质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)4质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(6)。该预浸渍体(6)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为0.96。另外,厚度为0.25mm。
(比较例1:预浸渍体用树脂组合物(R1)的制作及评价)
将4,4’-二苯基甲烷二异氰酸酯100质量份、HEMA 57质量份、PNT-40(日本油脂株式会社制:季戊四醇聚氧乙烯醚、羟基当量;80g/eq)32质量份、甲基丙烯酸苯氧基乙酯19质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,得到预浸渍体用树脂组合物(R1)。
另外,将4,4’-二苯基甲烷二异氰酸酯100质量份、HEMA 57质量份、PNT-40(日本油脂株式会社制:季戊四醇聚氧乙烯醚、羟基当量;80g/eq)32质量份、甲基丙烯酸苯氧基乙酯19质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)3质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(R1)。该预浸渍体(R1)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为0.95。另外,厚度为0.25mm。
(比较例2:预浸渍体用树脂组合物(R2)的制作及评价)
将甲苯二异氰酸酯100质量份、HEMA 99质量份、Newpol BP-23P(三洋化成株式会社制:双酚A的PO加成物、羟基当量;178g/eq)82质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)4质量份混合,得到预浸渍体用树脂组合物(R2)。
另外,将甲苯二异氰酸酯100质量份、HEMA 99质量份、Newpol BP-23P(三洋化成株式会社制:双酚A的PO加成物、羟基当量;178g/eq)82质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)4质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(R2)。该预浸渍体(R2)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为0.94。另外,厚度为0.25mm。
(比较例3:预浸渍体用树脂组合物(R3)的制作及评价)
将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATEMR-200”)356质量份、HEMA 88质量份、HEMA 293质量份、苯乙烯350质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)10质量份混合,得到预浸渍体用树脂组合物(R3)。
另外,将多亚甲基多苯基多异氰酸酯与MDI的混合物(东曹株式会社制“MILLIONATE MR-200”)356质量份、HEMA 88质量份、HEMA293质量份、苯乙烯350质量份、和聚合引发剂(化药Akzo株式会社制“Trigonox 122-C80”、有机过氧化物)10质量份混合,涂布在脱模PET膜的单面,然后通过手糊法使碳纤维(三菱丽阳株式会社制“TRK979PQRW”)浸渗,使得碳纤维含量达到55%,覆盖相同的脱模PET膜,然后在45℃、24小时的条件下老化,由此制作预浸渍体(R3)。该预浸渍体(R3)中的除碳纤维以外的原料中的摩尔比(NCO/OH)为1.17。另外,厚度为0.25mm。
将实施例1中使用的预浸渍体用树脂组合物(1)变更为预浸渍体用树脂组合物(2)~(6)及(R1)~(R3),除此以外与实施例1同样地测定熔融粘度。
此外,将实施例1中使用的预浸渍体(1)变更为预浸渍体(2)~(6)及(R1)~(R3),除此以外与实施例1同样地制作成型品(2)~(6)及(R1)~(R3),进行各评价。
将上述得到的预浸渍体用树脂组合物(1)~(6)及(R1)~(R3)的评价结果示于表1及表2。
[表1]
[表2]
可确认,由实施例1~6的本发明的预浸渍体用树脂组合物得到的预浸渍体的操作性及成型性优异,所得到的成型品的耐热性、层间剪切强度优异。
另一方面,比较例1为使用季戊四醇聚氧乙烯醚代替作为本发明的必需成分的具有芳香环及氧化烯结构的多元醇(a2)的例子,可确认在120℃下不熔融,成型品的层间剪切强度差。
比较例2为没有使用作为本发明的必需成分的多异氰酸酯(a1)的例子,可确认成型品的耐热性不充分。
比较例3为没有使用作为本发明的必需成分的具有芳香环及氧化烯结构的多元醇(a2)的例子,可确认操作性及成型性不充分。
Claims (6)
1.一种预浸渍体用树脂组合物,其特征在于,其为以氨基甲酸酯(甲基)丙烯酸酯(A)及聚合引发剂(B)为必需成分的预浸渍体用树脂组合物,所述氨基甲酸酯(甲基)丙烯酸酯(A)为多异氰酸酯(a1)、多元醇(a2)与(甲基)丙烯酸羟烷基酯(a3)的反应物,所述多异氰酸酯(a1)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、及多亚甲基多苯基多异氰酸酯中的1种以上多异氰酸酯,所述多元醇(a2)具有芳香环及氧化烯结构,所述多元醇(a2)的羟基当量为90g/eq~184g/eq。
2.根据权利要求1所述的预浸渍体用树脂组合物,其中,
所述氨基甲酸酯(甲基)丙烯酸酯(A)的原料中的所述多元醇(a2)为5质量%~45质量%的范围。
3.根据权利要求1或2所述的预浸渍体用树脂组合物,其中,
所述多元醇(a2)为双酚A的氧化烯加成物。
4.根据权利要求1或2所述的预浸渍体用树脂组合物,其中,
所述(甲基)丙烯酸羟烷基酯(a3)为5质量%~50质量%的范围。
5.一种预浸渍体,其特征在于,其含有权利要求1~4中任一项所述的预浸渍体用树脂组合物及强化纤维(C)。
6.一种成型品,其特征在于,其为权利要求5所述的预浸渍体的固化物。
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