CN108778716B - 聚烯烃系树脂粘接用表面处理金属板及使用其的复合构件 - Google Patents

聚烯烃系树脂粘接用表面处理金属板及使用其的复合构件 Download PDF

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CN108778716B
CN108778716B CN201780014391.4A CN201780014391A CN108778716B CN 108778716 B CN108778716 B CN 108778716B CN 201780014391 A CN201780014391 A CN 201780014391A CN 108778716 B CN108778716 B CN 108778716B
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resin
acid
chemical conversion
polyolefin resin
adhesive layer
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CN108778716A (zh
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平野康雄
渡濑岳史
山本哲也
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Kobe Steel Ltd
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Kobe Steel Ltd
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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Abstract

本发明涉及一种聚烯烃系树脂粘接用表面处理金属板，其是在金属基板的至少一面上经由化学转化处理膜叠层有粘接剂层的聚烯烃系树脂粘接用表面处理金属板。所述化学转化处理膜是将含有酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的涂布液涂布于所述金属基板上而得到的皮膜，所述化学转化处理膜的附着量以干燥质量计为0.05～3g/m2，所述粘接剂层含有酸改性聚烯烃系树脂，所述粘接剂层的厚度为5～100μm。

Description

聚烯烃系树脂粘接用表面处理金属板及使用其的复合构件
技术领域
本发明涉及粘接性优异的聚烯烃系树脂粘接用表面处理金属板以及使用该表面处理金属板的复合构件。
背景技术
在汽车、家电制品、OA(办公自动化)机器等中使用以钢板(金属板)为代表的许多金属部件。对于这样的金属部件而言，大多数情况下是将金属板压制成形而赋予指定的形状之后，通过焊接或用螺钉固定等方式来与其它金属部件或塑料部件接合而使用。
另一方面，如果能够对金属板表面赋予与塑料的粘接性，则将该金属板压制成形后，装入于塑料成形的模具中，注入熔融塑料并冷却固化，仅通过上述操作就可以形成将金属部件与如塑料部件等树脂成形品粘接而成的金属板复合树脂成形品(以下称为复合构件)，从而可以进行构件制造工序的效率化及构件的轻量化。作为对金属板表面赋予与塑料的粘接性的方法，本申请人通过专利文献1提出了一种表面处理钢板，其特征是依次叠层有金属基板、化学转化处理膜和粘接剂层的表面处理钢板，其中，所述化学转化处理膜包含胶态二氧化硅和热固型树脂。
近年来，作为塑料，通过使用高强度且轻量的聚烯烃系树脂来实现进一步的轻量化，在专利文献1中也使用包含聚丙烯树脂的树脂成形品。专利文献1的表面处理钢板与包含聚丙烯树脂的树脂成形品粘接而成的复合构件，虽然在金属基板与树脂成形品的粘接强度(以下有时简称为粘接强度)方面实现了某种程度的提高，但是由于化学转化处理膜所包含的树脂是热固型树脂，因此有时容易引起化学转化处理膜与粘接剂层的剥离。即，在汽车的结构部件之类的要求高粘接性的用途中使用的情况下，有时不能说具有足够的粘接性。
此外，专利文献1中还提出了另一种表面处理钢板，其是通过在化学转化处理膜与粘接剂层之间设置底涂层来提高了粘接强度的表面处理钢板，但是需要在金属基板上进行3层叠层来制作表面处理钢板，制造工序变多，制造成本增高。此外，从近年来要求的构件的轻量化的观点考虑也期望减少叠层数量。
现有技术文献
专利文献
专利文献1：日本专利公开公报特开2015-110318号
发明内容
于是，考虑到上述情况，本发明提出如下的课题：以低成本提供粘接性优异的聚烯烃系树脂粘接用表面处理金属板。
本发明一个方面涉及聚烯烃系树脂粘接用表面处理金属板，其特征在于，在金属基板的至少一面上经由化学转化处理膜叠层有粘接剂层，所述化学转化处理膜是将含有酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的涂布液涂布于所述金属基板上而得到的皮膜，所述化学转化处理膜的附着量以干燥质量计为0.05～3g/m2，所述粘接剂层含有酸改性聚烯烃系树脂，所述粘接剂层的厚度为5～100μm。
具体实施方式
本发明的聚烯烃系树脂粘接用表面处理金属板，在金属基板的至少一面上经由化学转化处理膜叠层有粘接剂层。所述化学转化处理膜是将含有酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的涂布液涂布于所述金属基板上而得到的皮膜，所述化学转化处理膜的附着量以干燥质量计为0.05～3g/m2，所述粘接剂层含有酸改性聚烯烃系树脂，所述粘接剂层的厚度为5～100μm。
本发明通过利用含有酸改性聚烯烃系树脂的化学转化处理膜以及含有酸改性聚烯烃系树脂的粘接剂，来能够以低成本制造粘接性优异的表面处理金属板。本发明的表面处理金属板可以用于：汽车或家用电器制品的框体、内装或外装部件；钢制家具等的外板材；或者建筑材料等。
而且，本发明还可以提供将所述的表面处理金属板和树脂复合一体化的复合构件。
因此，本发明的复合构件可以用于汽车部件、家用电器制品、建筑材料、办公室机器等各种用途。
此外，本发明的表面处理金属板优选在金属基板的至少一面只介于化学转化处理膜来叠层粘接剂层。
以下对于本发明的实施方式进行说明。
[金属基板(钢板)]
作为本发明中使用的金属基板，没有特别限定，例如可列举：如非镀覆冷轧钢板、热浸镀锌钢板、合金化热浸镀锌钢板、电镀锌钢板等钢板；铝板；以及钛板等。其中优选热浸镀锌钢板、电镀锌钢板、铝板和钛板，更优选合金化热浸镀锌钢板。金属基板的厚度没有特别限定，为了最终制品的轻量化，优选为0.3～3.2mm左右。下文中对于使用了钢板(其为金属基板的优选例子)的实施方式进行说明，但本发明可以使用各种金属基板。
[化学转化处理膜]
化学转化处理膜可以使用包含酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的化学转化处理膜形成用涂布液来制作。
＜酸改性聚烯烃系树脂＞
本实施方式中所采用的化学转化处理膜形成用涂布液包含酸改性聚烯烃系树脂，即化学转化处理膜包含酸改性聚烯烃系树脂。通过包含酸改性聚烯烃系树脂，可以抑制化学转化处理膜与粘接剂层的剥离。酸改性聚烯烃系树脂优选包含酸改性聚丙烯树脂。
本实施方式中所采用的酸改性聚烯烃系树脂可以如下得到：使从由不饱和二元羧酸、其酸酐和酯衍生物构成的组中选择的至少1种与聚烯烃系树脂进行接枝聚合。
作为酸改性聚烯烃系树脂的原料的聚烯烃系树脂，例如可列举聚乙烯、聚丙烯、聚丁烯、聚甲基戊烯、α-烯烃与乙烯或丙烯的共聚物、乙烯-乙酸乙烯酯共聚物、乙烯-丙烯酸共聚物、乙烯-甲基丙烯酸共聚物、乙烯-马来酸酐共聚物、丙烯-马来酸酐共聚物等树脂，这些树脂可以单独使用，也可以将2种以上组合使用。从抑制化学转化处理膜与粘接剂层的剥离的观点考虑，聚烯烃系树脂优选包含聚丙烯树脂，更优选为聚丙烯树脂。
作为聚丙烯树脂，可以采用均聚丙烯(丙烯均聚物)，也可以采用丙烯与从由乙烯、其它α-烯烃和乙烯系化合物构成的组中选择的1种以上的共聚物。作为其它α-烯烃，优选碳数4～18的α-烯烃，可列举1-丁烯、异丁烯、1-戊烯、4-甲基-1-戊烯、1-己烯、1-辛烯、1-癸烯、1-十二烯等。作为聚丙烯树脂，从化学转化处理膜与粘接剂层的密合性方面考虑，特别优选均聚丙烯。
作为不饱和二元羧酸，例如可列举马来酸、富马酸、柠康酸、中康酸、衣康酸等。作为不饱和二元羧酸的酸酐，例如可列举马来酸酐、衣康酸酐、柠康酸酐等。作为不饱和二元羧酸的酯衍生物，例如可列举马来酸单甲酯等。其中优选不饱和二元羧酸的酸酐，更优选马来酸酐。不饱和二元羧酸、其酸酐或酯衍生物可以单独使用，也可以将2种以上组合使用。
酸改性聚烯烃系树脂可以通过按照常规方法使上述聚烯烃系树脂与不饱和二元羧酸、其酸酐或酯衍生物进行接枝聚合来制造。
例如，马来酸酐改性聚烯烃系树脂可以如下进行合成。作为溶媒，使用二甲苯、或者2,2,4-三甲基-1,3-戊二醇二异丁酸酯等，适当地以任意顺序或者一起加入聚丙烯树脂、马来酸酐、以及有机过氧化物(例如叔丁基过氧化-2-乙基己基碳酸酯)，通常在加热下，例如130～150℃左右，使马来酸酐与聚烯烃系树脂进行接枝聚合，由此可以得到马来酸酐改性聚烯烃系树脂。
化学转化处理膜中的酸改性聚烯烃系树脂的酸值优选为3～100mgKOH/g，更优选为5～80mgKOH/g，进一步优选为5～60mgKOH/g。如果酸值小于3mgKOH/g，则难以制造水系的化学转化处理膜形成用涂布液。另一方面，很难制作酸值超过100mgKOH/g的酸改性聚烯烃系树脂。
酸改性聚烯烃系树脂中的马来酸酐的接枝量优选为0.1～10质量％，更优选为0.3～7质量％，进一步优选为0.5～5质量％。如果接枝量小于0.1质量％，则粘接强度可能会不充分。另一方面，如果接枝量超过10质量％，则与未改性的聚烯烃系树脂的相容性可能会变差。再说，在使用2种以上的不饱和二元羧酸、其酸酐和酯衍生物的情况下，将它们的总含量作为接枝量。
作为酸改性聚烯烃系树脂，可以使用市售品。作为市售品，可列举“UNISTOLE(注册商标)”系列、日本聚丙烯公司制的“Novatec(注册商标)”系列、“Wintec(注册商标)”系列、普瑞曼聚合物公司的“Prime Polypro(注册商标)”系列等。
前述化学转化处理膜优选不含除酸改性聚烯烃系树脂以外的其它热塑性树脂，但只要是不损害本发明效果的程度则可以含有除酸改性聚烯烃系树脂以外的其它热塑性树脂。作为其它热塑性树脂，例如可列举聚苯乙烯树脂、丙烯腈-丁二烯-苯乙烯(ABS)共聚物、丙烯腈-EPDM-苯乙烯(AES)共聚物、丙烯酸系树脂、聚丁二烯、聚缩醛树脂、聚醚树脂、聚乙酸乙烯酯、聚氯乙烯、聚偏氯乙烯等，这些可以单独使用，也可以将2种以上组合使用。
前述化学转化处理膜所含有的全部树脂100质量％中，酸改性聚烯烃系树脂的含量优选为80质量％以上，更优选为90质量％以上，进一步优选为99.91质量％以上，特别优选为99.95质量％以上，最优选为100质量％(化学转化处理膜所含有的树脂仅为酸改性聚烯烃系树脂)。
化学转化处理膜形成用涂布液的固体成分100质量份中，热塑性树脂优选为30～60质量份，更优选为35～55质量份，进一步优选为40～50质量份。此外，化学转化处理膜所含有的热塑性树脂优选为30～60质量％，更优选为35～55质量％，进一步优选为40～50质量％。
＜胶态二氧化硅＞
化学转化处理膜形成用涂布液优选包含胶态二氧化硅。即，本实施方式的化学转化处理膜优选包含胶态二氧化硅。其理由在于：通过含有胶态二氧化硅，来能够具有提高耐腐蚀性的效果。作为胶态二氧化硅，可合适地使用“SNOWTEX(注册商标)”系列(日产化学工业公司制的胶态二氧化硅)的“XS”、“SS”、“40”、“N”、“UP”等。尤其可合适地使用表面积平均粒径为10～20nm左右的“SNOWTEX(注册商标)40”。在化学转化处理膜形成用涂布液的固体成分100质量份中，胶态二氧化硅的量优选为30～60质量份，更优选为35～55质量份，进一步优选为40～50质量份。此外，相对于化学转化处理膜所含有的热塑性树脂100质量份，化学转化处理膜所含有的胶态二氧化硅的量优选为50～150质量份，更优选为75～125质量份。
＜硅烷偶联剂＞
化学转化处理膜形成用涂布液优选包含硅烷偶联剂。通过包含硅烷偶联剂，可以提高化学转化处理膜对金属基板的密合性。作为硅烷偶联剂，具体例如可列举：γ-氨基丙基三甲氧基硅烷、γ-氨基丙基三乙氧基硅烷、N-(β-氨基乙基)-γ-氨基丙基三甲氧基硅烷、N-(β-氨基乙基)-γ-氨基丙基甲基二甲氧基硅烷等具有氨基的硅烷偶联剂；γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基甲基二甲氧基硅烷、γ-环氧丙氧基丙基三乙氧基硅烷、γ-环氧丙氧基甲基二甲氧基硅烷等具有环氧丙氧基的硅烷偶联剂；乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三(β-甲氧基乙氧基)硅烷等具有乙烯基的硅烷偶联剂；γ-甲基丙烯酰氧基丙基三甲氧基硅烷等具有甲基丙烯酰氧基的硅烷偶联剂；γ-巯基丙基三甲氧基硅烷、γ-巯基丙基甲基二甲氧基硅烷等具有巯基的硅烷偶联剂；γ-氯丙基甲氧基硅烷、γ-氯丙基三甲氧基硅烷等具有卤素基团的硅烷偶联剂等，其中优选具有氨基的硅烷偶联剂。这些硅烷偶联剂可以单独使用，也可以并用2种以上。其中，从使粘接性变好的观点考虑，优选具有氨基的硅烷偶联剂、具有环氧丙氧基的硅烷偶联剂，更优选具有氨基的硅烷偶联剂。在化学转化处理膜形成用涂布液的固体成分100质量份中，硅烷偶联剂的量优选为1～30质量份，更优选为3～20质量份，进一步优选为5～15质量份。
作为硅烷偶联剂，可以使用市售品，可合适地使用例如信越有机硅公司制KBM903(3-氨基丙基三甲氧基硅烷)、东丽道康宁公司制Z-6011(3-氨基丙基三乙氧基硅烷)、东丽道康宁公司制Z-6020(3-(2-氨基乙基)氨基丙基三甲氧基硅烷)等。
＜化学转化处理膜的附着量＞
化学转化处理膜的附着量以干燥质量计为0.05～3g/m2，优选为0.1～2.5g/m2，更优选为0.2～2g/m2。如果化学转化处理膜的附着量在上述范围外，则与树脂成形品的粘接强度可能会变低。
＜化学转化处理膜的形成方法＞
将含有酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的化学转化处理膜形成用涂布液涂布于金属基板的至少一面来形成化学转化处理膜。当形成化学转化处理膜时，可以在涂布液中加入其它公知的添加剂。在金属基板上形成化学转化处理膜的方法没有特别限定，可以采用以往公知的涂布方法，例如使用辊涂法、喷涂法、帘流涂布法等将化学转化处理膜用涂布液涂布于金属基板表面的单面或两面，进行加热干燥即可。加热干燥温度没有特别限定，由于化学转化处理膜形成用的涂布液为水性，因此可以在使水蒸发的100℃前后加热数十秒～数分钟左右。
[表面处理钢板]
在上述化学转化处理膜上设置由包含酸改性聚烯烃系树脂的粘接剂形成的粘接剂层，制成表面处理钢板。粘接剂层可以设置于化学转化处理膜表面的整面，也可以仅设置于化学转化处理膜表面的部分必要位置，例如可设置为若干条的线状、或若干个的点状。作为粘接剂层，优选与后述的树脂成形品的粘接性优异的层，该树脂成形品与表面处理钢板复合。
＜粘接剂＞
粘接剂包含酸改性聚烯烃系树脂，优选包含酸改性聚丙烯树脂，更优选由酸改性聚丙烯树脂组成。
粘接剂层中的酸改性聚烯烃系树脂的酸值优选为5～60mgKOH/g，更优选为10～50mgKOH/g，进一步优选为13～40mgKOH/g。如果酸改性聚烯烃系树脂的酸值在上述范围外，则粘接强度可能会变低。
作为酸改性聚烯烃系树脂，可以采用与化学转化处理膜所含有的酸改性聚烯烃系树脂同样的方法来制造。粘接剂层所含有的酸改性聚烯烃系树脂与化学转化处理膜所含有的酸改性聚烯烃系树脂可以具有相同的酸值或不同的酸值，但优选具有相同的酸值。
前述粘接剂层优选不含除酸改性聚烯烃系树脂以外的其它热塑性树脂，但只要是不损害本发明效果的程度则可以含有除酸改性聚烯烃系树脂以外的其它热塑性树脂。作为其它热塑性树脂，例如可列举聚苯乙烯树脂、丙烯腈-丁二烯-苯乙烯(ABS)共聚物、丙烯腈-EPDM-苯乙烯(AES)共聚物、丙烯酸系树脂、聚丁二烯、聚缩醛树脂、聚醚树脂、聚乙酸乙烯酯、聚氯乙烯、聚偏氯乙烯等，这些可以单独使用，也可以将2种以上组合使用。
前述粘接剂层所含有的全部树脂100质量％中，酸改性聚烯烃系树脂的含量优选为80质量％以上，更优选为90质量％以上，进一步优选为99.91质量％以上，特别优选为99.95质量％以上，最优选为100质量％(粘接剂层所含有的树脂仅为酸改性聚烯烃系树脂)。
对于粘接剂层而言，干燥后的厚度为5～100μm，优选为10～90μm。如果粘接剂层的厚度在上述范围外，则粘接强度可能会变低。
＜粘接剂层的叠层方法＞
本实施方式中，在化学转化处理膜上涂布含有酸改性聚烯烃系树脂的热熔粘接剂来叠层粘接剂层。热熔粘接剂可以采用公知的方法来涂布，例如可以采用粉末状态涂布于化学转化处理钢板的表面。此外，可以将使粘接剂溶解于有机溶剂中而得的溶液、或分散于水中而得的水分散液涂布于化学转化处理钢板。在涂布粘接剂之后，在适合于粘接剂种类的温度(例如180～230℃左右)下加热1～3分钟左右。
[复合构件]
本实施方式的表面处理钢板可以与树脂成形品(树脂层)复合而使用，即形成为在粘接剂层上设置有树脂层的复合构件而使用。这时，在需要加工的情况下，可以将化学转化处理钢板压制成形为目标形状之后设置粘接剂层，也可以将在化学转化处理钢板上设置有粘接剂层的表面处理钢板压制成形为目标形状。然后，将表面处理钢板装入注射成形机的模具中，进行合模，将熔融树脂注入模具内，使树脂冷却固化，则获得复合构件。当然，本实施方式的表面处理钢板虽然可以采用压制成形法与树脂层复合，但是从发挥注射成形的短时间且高效率这样的优点方面考虑，优选采用注射成形法。
注射成形的条件可以根据构成成形品的树脂种类而适当变更，若列举树脂成形品为聚丙烯树脂的情形的一例：可将机筒温度设为230～250℃、将模具温度设为45～55℃、将注射保持时间设为5～8秒、将冷却时间设为20～30秒左右。若在该条件下进行注射成形，则可以获得树脂层与表面处理钢板牢固粘接的本实施方式的复合构件。
＜树脂层＞
树脂层包含聚烯烃系树脂。作为聚烯烃系树脂，例如可列举聚乙烯、聚丙烯、聚丁烯、聚甲基戊烯、α-烯烃与乙烯或丙烯的共聚物、乙烯-乙酸乙烯酯共聚物、乙烯-丙烯酸共聚物、乙烯-甲基丙烯酸共聚物、乙烯-马来酸酐共聚物、丙烯-马来酸酐共聚物等树脂，这些树脂可以单独使用，也可以将2种以上组合使用。聚烯烃系树脂优选包含聚丙烯树脂，更优选仅由聚丙烯树脂组成。
为了提高复合构件的强度，在树脂层中可以包含5～60质量％左右的如玻璃纤维、碳纤维等强化纤维。此外，还可以加入各种颜料或染料、阻燃剂、抗菌剂、抗氧化剂、增塑剂、润滑剂等公知的添加剂。
[复合构件的物性]
(粘接性)
复合构件的粘接强度优选为12MPa以上，更优选为12.5MPa，进一步优选为13MPa以上，特别优选为14MPa以上。通过使用本实施方式的表面处理钢板，即使是在金属基板上仅具有化学转化处理膜和粘接剂层这2层的表面处理钢板，也可以充分提高复合构件的粘接强度。粘接强度的测定方法如后文描述。
本说明书公开了上述的各种实施方式，其主要技术总结如下。
本发明涉及一种聚烯烃系树脂粘接用表面处理金属板，其特征在于，在金属基板的至少一面上经由化学转化处理膜叠层有粘接剂层，所述化学转化处理膜是将含有酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的涂布液涂布于所述金属基板上而得到的皮膜，所述化学转化处理膜的附着量以干燥质量计为0.05～3g/m2，所述粘接剂层含有酸改性聚烯烃系树脂，所述粘接剂层的厚度为5～100μm。
在所述的聚烯烃系树脂粘接用表面处理金属板中，优选所述化学转化处理膜中的酸改性聚烯烃系树脂的酸值为3～100mgKOH/g，另外优选所述化学转化处理膜中的酸改性聚烯烃系树脂包含酸改性聚丙烯树脂。
此外，在所述的聚烯烃系树脂粘接用表面处理金属板中，优选所述粘接剂层中的酸改性聚烯烃系树脂的酸值为5～60mgKOH/g，另外优选所述粘接剂层中的酸改性聚烯烃系树脂包含酸改性聚丙烯树脂。
此外，所述金属基板优选为钢板。
此外，本发明还包含一种复合构件，在所述的表面处理金属板中的粘接剂层上设置有包含聚烯烃系树脂的树脂层，其中优选所述聚烯烃系树脂包含聚丙烯树脂。
而且，本发明还包含一种所述聚烯烃系树脂粘接用表面处理金属板的制造方法，该制造方法包括：将含有酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的化学转化处理膜形成用涂布液涂布于金属基板的至少一面而形成化学转化处理膜的工序；和，在所述化学转化处理膜上涂布含有酸改性聚烯烃系树脂的热熔粘接剂而叠层粘接剂层的工序。
实施例
以下通过实施例来进一步详述本发明，但下述实施例并不限制本发明，在不脱离本发明主旨的范围进行的变更实施全部包含于本发明中。应予说明，只要没有特别说明，份是指质量份，％是指质量％。
首先，在下文中说明实施例中使用的测定和评价方法。
＜粘接性(粘接强度)＞
在采用后述的制造方法得到的复合构件中，在25℃的气氛下，将表面处理钢板的长度方向端部与树脂层的长度方向端部用拉伸试验机的夹具夹住，以10mm/分钟的拉伸速度进行拉伸，测定了树脂层从表面处理钢板剥离时的拉伸强度，将其值作为粘接强度。其中，表面处理钢板的长度方向端部是指没有被树脂层覆盖的一侧的端部；树脂层的长度方向端部是指表面处理钢板未粘接的一侧的端部。
(实施例1)
[马来酸酐接枝聚丙烯树脂的制备]
向具备冷凝管的烧瓶中加入作为溶媒的二甲苯400ml、粒状的均聚丙烯(熔体流动速率：4g/10分钟)60g，在氮气流下，于140℃进行了加热搅拌。然后，向经搅拌的溶液中花费1小时滴加溶解有马来酸酐11g和叔丁基过氧化2-乙基己基碳酸酯4g的二甲苯40ml，其后进行了1小时反应。接着，使内容物降至室温后，投入到大量的甲基乙基酮中。最后进行过滤，得到了马来酸酐接枝聚丙烯树脂。所得的马来酸酐接枝聚丙烯树脂中的马来酸酐的接枝量为3.0质量％，所得的马来酸酐接枝聚丙烯树脂的酸值为25mgKOH/g。
[化学转化处理膜形成用涂布液]
向不锈钢制耐压容器中加入上述马来酸酐接枝聚丙烯树脂10g、三乙胺1g、丁醇10g、蒸馏水30g，在170℃下以100rpm搅拌了1小时。然后进行冷却，得到了马来酸酐接枝聚丙烯树脂水分散体。接着，向100ml高压釜中添加由上述制法制作的马来酸酐接枝聚丙烯树脂水分散体、胶态二氧化硅和硅烷偶联剂，使得以质量比(固体成分)计马来酸酐接枝聚丙烯树脂：胶态二氧化硅：硅烷偶联剂＝50：50：10，在温度140℃、搅拌速度500rpm的条件下搅拌2小时，得到了化学转化处理膜形成用涂布液。作为胶态二氧化硅使用了日产化学工业公司制SNOWTEX(注册商标)40(表面积平均粒径10～20nm)，作为硅烷偶联剂使用了信越化学工业公司制KBM903(γ-氨基丙基三甲氧基硅烷)。
[化学转化处理钢板]
在厚度1.0mm的合金化热浸镀锌钢板的表面上涂布化学转化处理膜形成用涂布液，使得以干燥质量计达到0.2g/m2，然后在100℃下加热1分钟，得到了具有化学转化处理膜的化学转化处理钢板。
[表面处理钢板]
在上述化学转化处理钢板的化学转化处理膜上用刮棒涂布机涂布酸值为25mgKOH/g的上述马来酸酐接枝聚丙烯树脂，以使厚度为20μm，然后在220℃下加热2分钟，得到了具有化学转化处理膜和粘接剂层的表面处理钢板。
[复合构件]
接着，使用注射成形机(日精树脂工业公司制PNX60)进行了注射成形。首先，将上述表面处理钢板切成100mm×25mm，放入模具中。然后，使包含20质量％玻璃纤维的聚丙烯树脂即普瑞曼聚合物公司制Prime Polypro(注册商标)V7000熔融，得到了具有100mm长×25mm宽×3mm厚的树脂层的复合构件。应予说明，以由树脂层不完全覆盖表面处理钢板的表面的方式进行了粘接，并且，树脂层与表面处理钢板以12.5mm长×25mm宽重叠(表面处理钢板的表面仅部分被树脂层覆盖)的方式进行了粘接，从而得到了复合构件。注射条件示于表2。此外，用上述的测定方法来测定了复合构件的粘接强度，其结果示于表1。
(实施例2～3、比较例1～2)
除了使化学转化处理膜的附着量为表1记载的量之外，与实施例1同样操作得到了复合构件。复合构件的粘接强度示于表1。
(实施例4～5、比较例3～4)
除了使粘接剂层为表1记载的厚度之外，与实施例1同样操作得到了复合构件。复合构件的粘接强度示于表1。
(实施例6～10、比较例5～6)
除了使化学转化处理膜的马来酸酐接枝聚丙烯树脂为表1记载的酸值之外，与实施例1同样操作得到了复合构件。复合构件的粘接强度示于表1。应予说明，上述马来酸酐接枝聚丙烯树脂的制备中，通过调节均聚丙烯和马来酸酐的加入比率来调节了树脂的酸值。
(实施例11～12、比较例7～8)
除了使粘接剂层的马来酸酐接枝聚丙烯树脂为表1记载的酸值之外，与实施例1同样操作得到了复合构件。复合构件的粘接强度示于表1。应予说明，上述马来酸酐接枝聚丙烯树脂的制备中，通过调节均聚丙烯和马来酸酐的加入比率来调节了树脂的酸值。
(比较例9、10)
作为化学转化处理膜的树脂，使用表1记载的树脂来代替马来酸酐接枝聚丙烯树脂，除此之外与实施例1同样操作得到了复合构件。复合构件的粘接强度示于表1。
Figure BDA0001783420860000111
表2
Figure BDA0001783420860000121
根据表1，可如下进行考察。
具备满足本发明构成要件的实施例1～12的表面处理钢板的复合构件的粘接强度优异。
相对于此，对于上述以外的表面处理钢板而言，如下文所详述的，不满足本发明的构成要件，不能够获得所期望的特性。
对于比较例1和2而言，由于化学转化处理膜的附着量过少，因此使用了比较例1的表面处理钢板的复合构件的粘接强度差。
对于比较例3而言，由于粘接剂层的厚度过薄，因此使用了比较例3的表面处理钢板的复合构件的粘接强度差。对于比较例4而言，由于粘接剂层的厚度过厚，因此使用了比较例4的表面处理钢板的复合构件的粘接强度差。
对于比较例5而言，由于化学转化处理膜中的酸改性聚丙烯树脂的酸值非常小，因此无法制造水系的化学转化处理膜形成用涂布液。对于比较例6而言，针对化学转化处理膜中的酸改性聚丙烯树脂的酸值非常大的树脂进行了制作，但是不能够制造酸改性烯烃树脂。
对于比较例7而言，由于粘接剂层中的酸改性聚烯烃系树脂的酸值过低，因此使用了比较例7的表面处理钢板的复合构件的粘接强度差。对于比较例8而言，由于粘接剂层中的酸改性聚烯烃系树脂的酸值过高，因此使用了比较例8的表面处理钢板的复合构件的粘接强度差。其理由推测为树脂层与粘接剂层的粘接力较弱。
比较例9～10的表面处理钢板具有不含酸改性聚烯烃系树脂的化学转化处理膜。因此，使用了比较例9～10的表面处理钢板的复合构件的粘接强度差。
本申请以2016年3月25日申请的日本国专利申请特愿2016-061676为基础，其内容包含于本申请中。
为了表示本发明，上文中参照具体实施例等通过实施方式对本发明进行了适当且充分的说明，但应该认识到本领域技术人员容易对前述实施方式进行变更和/或改良。因此，本领域技术人员实施的变更实施方式或改良实施方式，只要是没有脱离权利要求书中记载的权利要求的保护范围的水平，则该变更实施方式或该改良实施方式可解释为包含在该权利要求的保护范围内。
产业上的可利用性
本发明在涉及表面处理金属板的技术领域中具有广泛的产业上的可利用性。

Claims (7)

1.一种聚烯烃系树脂粘接用表面处理金属板，其特征在于，
在金属基板的至少一面上经由化学转化处理膜叠层有粘接剂层，
所述化学转化处理膜是将含有热塑性树脂的酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的涂布液涂布于所述金属基板上而得到的皮膜，所述化学转化处理膜的附着量以干燥质量计为0.05～3g/m2，
所述粘接剂层含有热塑性树脂的酸改性聚烯烃系树脂，所述粘接剂层的厚度为5～100μm，
所述化学转化处理膜中的酸改性聚烯烃系树脂的酸值为3～100mgKOH/g，
所述粘接剂层中的酸改性聚烯烃系树脂的酸值为5～60mgKOH/g。
2.根据权利要求1所述的聚烯烃系树脂粘接用表面处理金属板，其特征在于，所述化学转化处理膜中的酸改性聚烯烃系树脂包含酸改性聚丙烯树脂。
3.根据权利要求1所述的聚烯烃系树脂粘接用表面处理金属板，其特征在于，所述粘接剂层中的酸改性聚烯烃系树脂包含酸改性聚丙烯树脂。
4.根据权利要求1所述的聚烯烃系树脂粘接用表面处理金属板，其特征在于，所述金属基板为钢板。
5.一种复合构件，其特征在于，在权利要求1～3中任一项所述的表面处理金属板中的粘接剂层上设置有包含聚烯烃系树脂的树脂层。
6.根据权利要求5所述的复合构件，其特征在于，所述聚烯烃系树脂包含聚丙烯树脂。
7.一种权利要求1～3中任一项所述的聚烯烃系树脂粘接用表面处理金属板的制造方法，其特征在于包括：
将含有酸值为3～100mgKOH/g的热塑性树脂的酸改性聚烯烃系树脂、胶态二氧化硅和硅烷偶联剂的化学转化处理膜形成用涂布液涂布于金属基板的至少一面而形成化学转化处理膜的工序；和
在所述化学转化处理膜上涂布含有酸值为5～60mgKOH/g的热塑性树脂的酸改性聚烯烃系树脂的热熔粘接剂而叠层粘接剂层的工序。
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