JP5707582B2 - 水系金属表面処理剤及びその処理剤で処理してなる金属材料 - Google Patents
水系金属表面処理剤及びその処理剤で処理してなる金属材料 Download PDFInfo
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- JP5707582B2 JP5707582B2 JP2011157011A JP2011157011A JP5707582B2 JP 5707582 B2 JP5707582 B2 JP 5707582B2 JP 2011157011 A JP2011157011 A JP 2011157011A JP 2011157011 A JP2011157011 A JP 2011157011A JP 5707582 B2 JP5707582 B2 JP 5707582B2
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- 230000021523 carboxylation Effects 0.000 description 1
- 238000006473 carboxylation reaction Methods 0.000 description 1
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- TYAVIWGEVOBWDZ-UHFFFAOYSA-K cerium(3+);phosphate Chemical compound [Ce+3].[O-]P([O-])([O-])=O TYAVIWGEVOBWDZ-UHFFFAOYSA-K 0.000 description 1
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 description 1
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- NSYALVBBDKTCLE-UHFFFAOYSA-K chloropentamminecobalt chloride Chemical compound N.N.N.N.N.[Cl-].[Cl-].[Cl-].[Co+3] NSYALVBBDKTCLE-UHFFFAOYSA-K 0.000 description 1
- 150000001844 chromium Chemical class 0.000 description 1
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- UBFMILMLANTYEU-UHFFFAOYSA-H chromium(3+);oxalate Chemical compound [Cr+3].[Cr+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O UBFMILMLANTYEU-UHFFFAOYSA-H 0.000 description 1
- QOWZHEWZFLTYQP-UHFFFAOYSA-K chromium(3+);triformate Chemical compound [Cr+3].[O-]C=O.[O-]C=O.[O-]C=O QOWZHEWZFLTYQP-UHFFFAOYSA-K 0.000 description 1
- PPUZYFWVBLIDMP-UHFFFAOYSA-K chromium(3+);triiodide Chemical compound I[Cr](I)I PPUZYFWVBLIDMP-UHFFFAOYSA-K 0.000 description 1
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- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 1
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 229910000152 cobalt phosphate Inorganic materials 0.000 description 1
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- SRWMQSFFRFWREA-UHFFFAOYSA-M zinc formate Chemical compound [Zn+2].[O-]C=O SRWMQSFFRFWREA-UHFFFAOYSA-M 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- HTOFKHJTNDESBL-UHFFFAOYSA-L zinc tellurite Chemical compound [Zn+2].[O-][Te]([O-])=O HTOFKHJTNDESBL-UHFFFAOYSA-L 0.000 description 1
- VRGNUPCISFMPEM-ZVGUSBNCSA-L zinc;(2r,3r)-2,3-dihydroxybutanedioate Chemical compound [Zn+2].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VRGNUPCISFMPEM-ZVGUSBNCSA-L 0.000 description 1
- WDHVIZKSFZNHJB-UHFFFAOYSA-L zinc;butanoate Chemical compound [Zn+2].CCCC([O-])=O.CCCC([O-])=O WDHVIZKSFZNHJB-UHFFFAOYSA-L 0.000 description 1
- VOSQOLXQDQZVCL-UHFFFAOYSA-L zinc;chloride;hydroxide Chemical compound [OH-].[Cl-].[Zn+2] VOSQOLXQDQZVCL-UHFFFAOYSA-L 0.000 description 1
- JDLYKQWJXAQNNS-UHFFFAOYSA-L zinc;dibenzoate Chemical compound [Zn+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 JDLYKQWJXAQNNS-UHFFFAOYSA-L 0.000 description 1
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 1
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
- PEUPCBAALXHYHP-UHFFFAOYSA-L zinc;selenite Chemical compound [Zn+2].[O-][Se]([O-])=O PEUPCBAALXHYHP-UHFFFAOYSA-L 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
- 229910000350 zirconium(IV) sulfate Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
- ATYZRBBOXUWECY-UHFFFAOYSA-N zirconium;hydrate Chemical compound O.[Zr] ATYZRBBOXUWECY-UHFFFAOYSA-N 0.000 description 1
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Description
本発明に係る水系金属表面処理剤は、図1に示すように、基材である金属材料1(以下、「基材金属1」という。)の表面に、ラミネートフィルム又は樹脂塗膜3の下地用の表面処理皮膜2を形成するための処理剤である。その特徴は、水溶性又は水分散性のカチオン変性エポキシ樹脂(A)と、アミド結合、アミド基及び水酸基から選ばれる1種又は2種以上の構造単位を1mmol/g〜50mmol/g含有する水溶性又は水分散性の有機高分子(B)とを含有することにある。「含有し、」とは、水系金属表面処理剤中にカチオン変性エポキシ樹脂(A)及び有機高分子(B)以外の化合物を含んでいてもよいことを意味している。そうした化合物としては、例えば、界面活性剤、消泡剤、レベリング剤、防菌防ばい剤、着色剤等を挙げることができる。これらの化合物を、本発明の趣旨及び皮膜性能を損なわない範囲で含有することができる。
エポキシ樹脂(A)は、カチオン変性させたエポキシ樹脂を用いる。「カチオン変性」とは、エポキシ樹脂にカチオン基を有する化合物を反応させて、エポキシ樹脂の構造中に、水中でカチオン性を示すカチオン基を導入することである。また、エポキシ樹脂(A)は、水溶性又は水分散性のエポキシ樹脂を用いる。「水溶性又は水分散性」とは、水中で水溶液、エマルジョン又はディスパージョンを構成する性質のことをいう。水系金属表面処理剤が、このカチオン変性エポキシ樹脂(A)と、後述する有機高分子(B)とを所定量含むことで、この水系金属表面処理剤で処理して得られる表面処理皮膜の密着性及び耐薬品密着維持性を高めることができる。
上記単核多価フェノール化合物又は多核多価フェノール化合物にエチレンオキサイド及びプロピレンオキサイドから選ばれる1種又は2種を付加したポリグリシジルエーテル化合物;上記単核多価フェノール化合物の水添物のポリグリシジルエーテル化合物;エチレングリコール、プロピレングリコール、ブチレングリコール、ヘキサンジオール、ポリグリコール、チオジグリコール、グリセリン、トリメチロールプロパン、ペンタエリスリトール、ソルビトール、ビスフェノールA−エチレンオキサイド付加物等の多価アルコール類のポリグリシジルエーテル;
マレイン酸、フマル酸、イタコン酸、コハク酸、グルタル酸、スベリン酸、アジピン酸、アゼライン酸、セバシン酸、ダイマー酸、トリマー酸、フタル酸、イソフタル酸、テレフタル酸、トリメリット酸、トリメシン酸、ピロメリット酸、テトラヒドロフタル酸、ヘキサヒドロフタル酸、エンドメチレンテトラヒドロフタル酸等の脂肪族、芳香族又は脂環族多塩基酸のグリシジルエステル類及びグリシジルメタクリレートの単独重合体又は共重合体;
N,N−ジグリシジルアニリン、ビス(4−(N−メチル−N−グリシジルアミノ)フェニル)メタン等のグリシジルアミノ基を有するエポキシ化合物;
ビニルシクロヘキセンジエポキシド、ジシクロペンタンジエンジエポキサイド、3,4−エポキシシクロヘキシルメチル−3,4−エポキシシクロヘキサンカルボキシレート、3,4−エポキシ−6−メチルシクロヘキシルメチル−6−メチルシクロヘキサンカルボキシレート、ビス(3,4−エポキシ−6−メチルシクロヘキシルメチル)アジペート等の環状オレフィン化合物のエポキシ化物;
エポキシ化ポリブタジエン、エポキシ化スチレン−ブタジエン共重合物等のエポキシ化共役ジエン重合体;トリグリシジルイソシアヌレート等の複素環化合物;を挙げることができる。また、上記した各種化合物から選ばれる1種又は2種以上を反応させて得られる重縮合物を挙げることができる。
有機高分子(B)は、その構造中にアミド結合、アミド基及び水酸基から選ばれる1種又は2種以上の構造単位を含有している高分子化合物である。「構造単位」とは、官能基又は単一結合構造のことをいう。これらの構造単位を有する有機高分子(B)は、カチオン変性エポキシ樹脂と反応しやすくなるので、得られる表面処理皮膜の密着性及び耐薬品密着維持性を高めることができる。「含有する」とは、有機高分子(B)が他の官能基及び結合構造を有していてもよいことを意味している。
本発明に係る水系金属表面処理剤は、Mg、Al、Ca、Mn、Co、Ni、Cr(III)、Zn、Fe、Zr、Ti、Si、Sr、W、Ce、Mo、V、Sn、Bi、Ta、Te、In、Ba、Hf、Se、Sc、Nb、Cu、Y、Nd及びLaから選ばれる1種又は2種以上の元素を含む無機化合物(C)をさらに含有してもよい。中でも、Mg、Al、Ca、Mn、Cr(III)、Zn、Fe、Zr、Ti、Si、Ce、Te及びHfから選ばれる1種又は2種以上の元素を含むことがより好ましく、Cr(III)、Zr、Ti、Si、Ce及びTeから選ばれる1種又は2種以上の元素を含むことがさらに好ましい。この無機化合物(C)を含むことで、さらに耐薬品密着維持性が向上する。「含む」とは、これらの元素以外の元素を含んでいてもよいことを意味している。
硝酸アルミニウム、硫酸アルミニウム、硫酸カリウムアルミニウム、硫酸ナトリウムアルミニウム、硫酸アンモニウムアルミニウム、リン酸アルミニウム、炭酸アルミニウム、酸化アルミニウム、水酸化アルミニウム、酸化アルミニウム、フッ化アルミニウム、ヨウ化アルミニウム、酢酸アルミニウム、安息香酸アルミニウム、クエン酸アルミニウム、グルコン酸アルミニウム、セレン酸アルミニウム、蓚酸アルミニウム、酒石酸アルミニウム、乳酸アルミニウム、パルチミン酸アルミニウム等のアルミニウム塩等;
ビス(アセチルアセトナト)ジアクアカルシウム(II)、安息香酸カルシウム、クエン酸カルシウム、メタスズ酸カルシウム、セレン酸カルシウム、タングステン酸カルシウム、炭酸カルシウム、四ホウ酸カルシウム、モリブデン酸カルシウム、マレイン酸カルシウム、リンゴ酸カルシウム、ニリン酸カルシウム、フッ化カルシウム、ホスフィン酸カルシウム、硝酸カルシウム、水酸化カルシウム、酸化カルシウム、シュウ酸カルシウム、酸化カルシウム、酢酸カルシウム等のカルシウム塩等;
ビス(アセチルアセトナト)ジアクアマンガン(II)、四酸化三マンガン、酸化マンガン(II)、酸化マンガン(III)、酸化マンガン(IV)、臭化マンガン(II)、蓚酸マンガン(II)、過マンガン酸(VII)、過マンガン酸カリウム(VII)、過マンガン酸ナトリウム(VII)、リン酸二水素マンガン(II)、硝酸マンガン(II)、硫酸マンガン(II)、硫酸マンガン(III)、硫酸マンガン(IV)、フッ化マンガン(II)、フッ化マンガン(III)、炭酸マンガン(II)、酢酸マンガン(II)、酢酸マンガン(III)、硫酸アンモニウムマンガン(II)、ヨウ化マンガン(II)、水酸化マンガン(II)等のマンガン塩等又はマンガン酸塩等;
ビス(アセチルアセトナト)ジアクアコバルト(II)、トリス(アセチルアセトナト)コバルト(III)、スルファミン酸コバルト(II)、塩化コバルト(II)、クロロペンタアンミンコバルト塩化物(III)、ヘキサアンミンコバルト塩化物(III)、ジアンミンテトラニトロコバルト(III)酸アンモニウム、硫酸コバルト(II)、硫酸アンモニウムコバルト、硝酸コバルト(II)、酸化コバルト二アルミニウム、水酸化コバルト(II)、酸化コバルト(II)、リン酸コバルト、酢酸コバルト(II)、蟻酸コバルト(II)、四酸化三コバルト、臭化コバルト(II)、蓚酸コバルト(II)、セレン酸コバルト(II)、タングステン酸コバルト(II)、ヒドロキシ炭酸第一コバルト(II)、モリブデン酸コバルト(II)、ヨウ化コバルト(II)、リン酸コバルト(II)等のコバルト塩等;
二スルファミン酸ニッケル(II)、安息香酸ニッケル(II)、硝酸ニッケル(II)、硫酸ニッケル(II)、炭酸ニッケル(II)、ニッケルアセチルアセトネート(II)、塩化ニッケル(II)、ヘキサアンミンニッケル塩化物、酸化ニッケル、水酸化ニッケル(II)、酸化ニッケル(II)、酢酸ニッケル、クエン酸ニッケル(II)、コハク酸ニッケル(II)、臭化ニッケル(II)、蓚酸ニッケル(II)、酒石酸ニッケル(II)、セレン酸ニッケル(II)、ヒドロキシ炭酸ニッケル(II)、乳酸ニッケル(II)、モリブデン酸ニッケル(II)、ヨウ化ニッケル(II)、二リン酸ニッケル(II)等のニッケル塩等;
蟻酸クロム(III)、フッ化クロム(III)、硝酸クロム(III)、硫酸クロム(III)、蓚酸クロム(III)、酢酸クロム(III)、重燐酸クロム(III)、水酸化クロム(III)、酸化クロム(III)、臭化クロム(III)、ヨウ化クロム(III)等のクロム塩等;
ビス(アセチルアセトナト)亜鉛(II)、安息香酸亜鉛(II)、ヒドロキシ塩化亜鉛(II)、蟻酸亜鉛(II)、クエン酸亜鉛(II)、臭化亜鉛(II)、蓚酸亜鉛(II)、酒石酸亜鉛(II)、メタスズ酸亜鉛(II)、セレン酸亜鉛(II)、タングステン酸亜鉛(II)、フッ化亜鉛(II)、モリブデン酸亜鉛(II)、酪酸亜鉛(II)、ニリン酸亜鉛(II)、硫酸亜鉛(II)、炭酸亜鉛(II)、塩化亜鉛(II)、ヨウ化亜鉛(II)、水酸化亜鉛(II)、酸化亜鉛(II)等の亜鉛塩等;
ビス(アセチルアセトナト)ジアクア鉄(II)、トリス(アセチルアセトナト)鉄(III)、三蓚酸鉄三カリウム、蟻酸鉄(II)、四バナジン酸鉄(III)、臭化鉄(III)、酒石酸鉄(III)、乳酸鉄(II)、フッ化鉄(II)、フッ化鉄(III)、塩化鉄(II)、塩化鉄(III)、ヨウ化鉄(II)、ヨウ化鉄(III)、硫酸鉄(II)、硫酸鉄(III)、硝酸鉄(II)、硝酸鉄(III)、酢酸鉄(II)、酢酸鉄(III)、クエン酸鉄(II)クエン酸鉄(III)、グリシン鉄(II)、グリシン鉄(III)、蓚酸鉄(II)、蓚酸鉄(III)、ピコリン酸鉄(II)、ピコリン酸鉄(III)、L−フェニルアラニン鉄(II)、L−フェニルアラニン鉄(III)、マロン酸鉄(II)、マロン酸鉄(III)、水酸化鉄(II)、水酸化鉄(III)、酸化鉄(II)、酸化鉄(III)、四酸化三鉄等の鉄塩等;
ビス(アセチルアセトナト)ジアクアストロンチウム(II)、蟻酸ストロンチウム(II)、クエン酸ストロンチウム(II)タングステン酸ストロンチウム、メタスズ酸ストロンチウム、酸化ストロンチウム(IV)、酸化ストロンチウム(II)、蓚酸ストロンチウム、メタニオブ酸ストロンチウム、モリブデン酸ストロンチウム、ヨウ化ストロンチウム、硝酸ストロンチウム、硫酸ストロンチウム、炭酸ストロンチウム、酢酸ストロンチウム、塩化ストロンチウム、リン酸ストロンチウム、乳酸ストロンチウム等のストロンチウム塩等;
オキシ二蓚酸チタン二アンモニウム、オキシ二蓚酸チタン二カリウム、酸化チタン(II)、酸化チタン(III)、酸化チタン(IV)、オキシ硫酸第二チタン、塩基性リン酸チタン、臭化チタン(IV)、メタチタン酸、メタチタン酸亜鉛(II)、チタン酸アルミニウム(III)、メタチタン酸カリウム、メタチタン三コバルト(II)、チタン酸ジルコニウム、メタチタン酸ストロンチウム、メタチタン三鉄(III)、メタチタン酸銅(II)、チタン酸ナトリウム、二チタン酸ネオジム(III)、メタチタン酸バリウム、メタチタン酸ビスマス(III)、メタチタン酸マグネシウム、チタン酸マグネシウム、メタチタン酸マンガン(II)、二チタン酸ランタン(III)、メタチタン酸リチウム、ヘキサフルオロチタン(IV)酸アンモニウム、ヘキサフルオロチタン(IV)酸カリウム、ヨウ化チタン(IV)、硫酸チタン(III)、硫酸チタン(IV)、塩化チタン、硝酸チタン、硫酸チタニル、フッ化チタン(III)、フッ化チタン(IV)、ヘキサフルオロチタン酸、乳酸チタン、ペルオキソチタン酸、チタンラウレート、チタニウムアセチルアセトネート、水酸化チタン(IV)等のチタン塩等又はチタン酸塩等;
テトラキス(アセチルアセトナト)ジルコニウム(IV)、塩化酸化ジルコニウム(IV)、塩化ジルコニウム(IV)、ケイ酸ジルコニウム、酢酸酸化ジルコニウム(IV)、酸化ジルコニウム(IV)、硝酸酸化ジルコニウム(IV)、メタジルコニウム酸セシウム、メタジルコニウム酸リチウム、メタジルコニウム酸亜鉛(II)、メタジルコニウム酸アルミニウム(III)、メタジルコニウム酸カルシウム、メタジルコニウム酸コバルト(II)、メタジルコニウム酸ストロンチウム、メタジルコニウム酸銅(II)、メタジルコニウム酸ナトリウム、メタジルコニウム酸ニッケル(II)、メタジルコニウム酸バリウム、メタジルコニウム酸ビスマス(III)、メタジルコニウム酸マグネシウム、オキシ炭酸ジルコニウム、ヘキサフルオロジルコニウム(IV)酸アンモニウム、ヘキサフルオロジルコニウム(IV)酸カリウム、ヨウ化ジルコニウム、リン酸二水素酸化ジルコニウム(IV)、塩基性炭酸ジルコニウム、炭酸ジルコニウムアンモニウム、炭酸ジルコニルアンモニウム、硝酸ジルコニウム、硝酸ジルコニル、硫酸ジルコニウム(IV)、硫酸ジルコニル、ヘキサフルオロジルコニウム酸、オキシリン酸ジルコニウム、ピロリン酸ジルコニウム、リン酸二水素ジルコニル、オキシ塩化ジルコニウム、フッ化ジルコニウム、酢酸ジルコニル、酸化ジルコニウム、水酸化ジルコニウム等のジルコニウム塩等;
ヘキサフルオロケイ酸、シリカ等のケイ酸塩等;
塩化タングステン(VI)、酸化タングステン酸鉄(III)、塩化タングステン(VI)、オキシ二塩化タングステン、二酸化タングステン、三酸化タングステン、メタタングステン酸、メタタングステン酸アンモニウム、メタタングステン酸ナトリウム、パラタングステン酸、パラタングステン酸アンモニウム、パラタングステン酸ナトリウム、タングステン酸亜鉛(II)、タングステン酸カリウム、タングステン酸カルシウム、タングステン酸コバルト(II)、タングステン酸ストロンチウム、タングステン酸セシウム、タングステン酸銅(II)、タングステン酸ニッケル、タングステン酸バリウム、タングステン酸マグネシウム、タングステン酸マンガン(II)、タングステン酸リチウム、リンタングステン酸、リンタングステン酸アンモニウム、リンタングステン酸ナトリウム等のタングステン塩等又はタングステン酸塩等;
トリス(アセチルアセトナト)セリウム(III)、塩化セリウム(III)、酸化セリウム(III)、酸化セリウム(IV)、臭化セリウム(III)、蓚酸セリウム(III)、水酸化セリウム(IV)、硫酸第二セリウムアンモニウム(IV)、硫酸第一セリウムアンモニウム(III)、炭酸セリウム(III)、硫酸セリウム、酢酸セリウム(III)、硝酸セリウム(III)、硫酸セリウム(IV)、フッ化セリウム(III)、ヨウ化セリウム(III)、リン酸セリウム(III)等のセリウム塩等;
塩化モリブデン(V)、酸化モリブデン(IV)、酸化モリブデン(VI)、モリブデン酸亜鉛(II)、モリブデン酸カリウム、モリブデン酸カルシウム、モリブデン酸コバルト(II)、モリブデン酸セシウム、モリブデン酸ニッケル(II)、モリブデン酸バリウム、モリブデン酸ビスマス(III)、モリブデン酸マグネシウム、モリブデン酸リチウム、パラモリブデン酸リチウム、モリブデン酸ストロンチウム、リンモリブデン酸、リンモリブデン酸アンモニウム、リンモリブデン酸ナトリウム、モリブデン酸、モリブデン酸アンモニウム、パラモリブデン酸アンモニウム、モリブデン酸ナトリウム等のモリブデン塩等又はモリブデン酸塩等;
オキシ二塩化バナジウム、オキシ三塩化バナジウム、三塩化バナジウム、酸化バナジウム、四バナジン酸鉄(III)、臭化バナジウム(III)、オキシ蓚酸バナジウム、ヨウ化バナジウム(II)、五酸化バナジウム、メタバナジン酸、ピロバナジン酸ナトリウム、バナジン酸ナトリウム、メタバナジン酸アンモニウム、メタバナジン酸ナトリウム、メタバナジン酸カリウム、オキシ三塩化バナジウム、三酸化バナジウム、二酸化バナジウム、オキシ硫酸バナジウム、バナジウムオキシアセチルアセテート、バナジウムアセチルアセテート、リンバナドモリブデン酸等のバナジウム塩等又はバナジン酸塩等;
塩化スズ(II)、酢酸スズ(II)、蓚酸スズ(II)、酒石酸スズ(II)、酸化スズ(IV)、硝酸スズ、硫酸スズ、フッ化スズ(II)、ヨウ化スズ(II)、ヨウ化スズ(IV)、ピロリン酸スズ(II)、メタスズ酸、メタスズ酸亜鉛、メタスズ酸カルシウム、メタスズ酸ストロンチウム、メタスズ酸バリウム、メタスズ酸マグネシウム等のスズ塩又はスズ酸塩等;
安息香酸ビスマス(III)、塩化酸化ビスマス(III)、クエン酸ビスマス(III)、オキシ酢酸ビスマス(III)、酸化酒石酸ビスマス(III)、酸化ビスマス(III)、オキシ硫酸二ビスマス、臭化ビスマス(III)、酒石酸ビスマス(III)、水酸化ビスマス(III)、オキシ炭酸二ビスマス、ジルコニウム酸ビスマス(III)、オキシ硝酸ビスマス、四チタン酸ビスマス(III)、三チタン酸ビスマス(III)、フッ化ビスマス(III)、モリブデン酸ビスマス(III)、ヨウ化ビスマス(III)、硝酸ビスマス(III)、塩化ビスマス(III)、硫酸ビスマス(III)、酢酸ビスマス(III)、リン酸ビスマス(III)等のビスマス塩等;
塩化タンタル(V)、酸化タンタル(V)、臭化タンタル(V)、タンタル酸、六タンタル酸カリウム、メタタンタル酸ストロンチウム、メタタンタル酸ナトリウム、メタタンタル酸リチウム、ヨウ化タンタル(V)、タンタルオキシアセチルアセトネート、メタタンタル酸、メタタンタル酸アンモニウム、ヘプタフルオロタンタル酸カリウム等のタンタル塩等又はタンタル酸塩等;
テルル酸、メタテルル酸アンモニウム、メタテルル酸カリウム、メタテルル酸ナトリウム、ヨウ化テルル(IV)、テルル酸カリウム、テルル酸ナトリウム、亜テルル酸、亜テルル酸カリウム、亜テルル酸ナトリウム、亜テルル酸バリウム、亜テルル酸リチウム、塩化テルル(IV)、酸化テルル(IV)、臭化テルル(IV)、水酸化硝酸三酸化二テルル、亜テルル酸亜鉛等のテルル塩等又はテルル酸塩等;
トリス(アセチルアセトナト)インジウム(III)、アミド硫酸インジウム(III)、二塩化インジウム、塩化インジウム(I)、塩化インジウム(III)、酢酸インジウム(III)、臭化インジウム(III)、ヨウ化インジウム(III)、硝酸インジウム(III)、硫酸インジウム(III)、フッ化インジウム(III)、酸化インジウム(III)、水酸化インジウム(III)等のインジウム塩等;
ビス(アセチルアセトナト)ジアクアバリウム(II)、亜セレン酸バリウム、亜テルル酸バリウム、安息香酸バリウム、アルミン酸バリウム、塩化バリウム、蟻酸バリウム、クエン酸バリウム、酸化バリウム、臭化バリウム、蓚酸バリウム、酒石酸バリウム、メタジルコニウム酸バリウム、水酸化バリウム、メタスズ酸バリウム、タングステン酸バリウム、メタチタン酸バリウム、メタニオブ酸バリウム、乳酸バリウム、メタホウ酸バリウム、モリブデン酸バリウム、ヨウ化バリウム、リン酸水素バリウム、炭酸バリウム、フッ化バリウム等のバリウム塩等;
テトラキス(アセチルアセトナト)ハフニウム(IV)、塩化ハフニウム(IV)、酸化ハフニウム(IV)、ヨウ化ハフニウム(IV)、硫酸ハフニウム(IV)、硝酸ハフニウム(IV)、オキシ蓚酸ハフニウム(IV)、フルオロハフニウム酸、フルオロハフニウム酸塩、フッ化ハフニウム等のハフニウム塩等又はハフニウム酸塩等;
亜セレン酸カリウム、亜セレン酸水素カリウム、亜セレン酸三水素セシウム、亜セレン酸水素ナトリウム、亜セレン酸水素リチウム、亜セレン酸銅(II)、亜セレン酸ナトリウム、亜セレン酸バリウム、オキシ塩化セレン、塩化セレン(I)、塩化セレン(IV)、酸化セレン(IV)、セレン酸アルミニウム、セレン酸、亜セレン酸亜鉛、セレン酸カリウム、セレン酸アンモニウム、セレン酸カルシウム、セレン酸セシウム、セレン酸コバルト、セレン酸銅(II)、セレン酸ニッケル、セレン酸ナトリウム、セレン酸バリウム、セレン酸亜鉛等のセレン塩等又はセレン酸塩等;
塩化スカンジウム(III)、蟻酸スカンジウム(III)、酢酸スカンジウム(III)、硝酸スカンジウム(III)、酸化スカンジウム(III)、フッ化スカンジウム(III)、ヨウ化スカンジウム(III)、硫酸スカンジウム(III)等のスカンジウム塩等;
酸化ニオブ(II)、酸化ニオブ(V)、五(蓚酸水素)ニオブ、水酸化ニオブ(V)、ニオブオキシアセチルアセトネート、メタニオブ酸、メタニオブ酸カルシウム、メタニオブ酸ストロンチウム、メタニオブ酸バリウム、メタニオブ酸マグネシウム、メタニオブ酸リチウム、メタニオブ酸アンモニウム、メタニオブ酸ナトリウム、五塩化ニオブ等のニオブ塩等又はニオブ酸塩等;
アミド硫酸銅(II)、安息香酸銅(II)、テトラアンミン銅(II)硝酸塩、クエン酸銅(II)、酸化銅(I)、臭化銅(I)、蓚酸銅(II)、蟻酸銅(II)、酢酸銅(II)、プロピオン酸銅(II)、吉草酸銅(II)、グルコン酸銅(II)、酒石酸銅(II)、塩化銅(II)、臭化銅(II)、水酸化銅(II)、酢酸銅(II)、硝酸銅(II)、硫酸銅(II)、炭酸銅(II)、酸化銅(II)、ヒドロキシ硝酸第二銅、タングステン酸銅(II)、炭酸水酸化銅(II)、乳酸銅(II)、フッ化銅(II)、ヨウ化銅(I)等の銅塩等;
トリス(アセチルアセトナト)イットリウム(III)、塩化イットリウム(III)、蟻酸イットリウム(III)、クエン酸イットリウム(III)、酢酸イットリウム(III)、酸化イットリウム(III)、蓚酸イットリウム(III)、硝酸イットリウム(III)、炭酸イットリウム(III)、フッ化イットリウム(III)、ヨウ化イットリウム(III)、硫酸イットリウム(III)、リン酸イットリウム(III)等のイットリウム塩等;
トリス(アセチルアセトナト)ランタン(III)、塩化ランタン(III)、蟻酸ランタン(III)、酢酸ランタン(III)、酸化ランタン(III)、蓚酸ランタン(III)、硝酸ランタン(III)、炭酸ランタン(III)、フッ化ランタン(III)、二チタン酸ランタン(III)、硫酸ランタン(III)、リン酸ランタン(III)、ヨウ化ランタン(III)等のランタン塩等;
トリス(アセチルアセトナト)ネオジム(III)、塩化ネオジム(III)、蟻酸ネオジム(III)、酢酸ネオジム(III)、酸化ネオジム(III)、臭化ネオジム(III)、蓚酸ネオジム(III)、硝酸ネオジム(III)、炭酸ネオジム(III)、二チタン酸ネオジム(III)、フッ化ネオジム(III)、ヨウ化ネオジム(III)、硫酸ネオジム(III)、リン酸ネオジム(III)等のネオジウム塩等;を挙げることができる。これらの化合物は無水物であってもよいし、水和物であってもよい。また、単独で使用してもよいし、2種以上組み合わせて使用してもよい。さらに、水系金属表面処理剤溶剤中に溶解していてもよいし、分散していてもよい。
本発明に係る水系表面処理剤は、処理液中に、イソシアネート基、アルデヒド基、グリシジルエーテル基及びメチロール基から選ばれる1種又は2種以上を有する架橋性化合物(D)をさらに含有してもよい。架橋性化合物(D)を含有させることで、表面処理皮膜の緻密性が向上し、表面処理皮膜の耐薬品密着維持性をより高めることができる。
本発明に係る水系金属表面処理剤は、金属材料表面に塗布する際の作業性を良くするために、必要に応じて各種の溶剤を含有することができる。
本発明に係る水系金属表面処理剤は、界面活性剤、消泡剤、レベリング剤、防菌防ばい剤、着色剤等を、本発明の趣旨及び皮膜性能を損なわない範囲で含有することができる。
本発明に係る水系金属表面処理剤の調製方法は、特に限定されない。例えば、カチオン変性エポキシ樹脂(A)と有機高分子(B)は、必要に応じて使用することができる無機化合物(C)、必要に応じて使用することができる架橋性化合物(D)、必要に応じて使用することができるその他添加剤及び必要に応じて使用することができる溶剤と混ぜ、混合ミキサー等の攪拌機を用いて十分に混合することによって調製することができる。
本発明に係る金属材料10は、図1に示すように、基材金属1と、その表面に本発明に係る水系金属表面処理剤を塗布して形成された表面処理皮膜2を有する。「塗布」とは、後述する塗布工程によって、基材金属1の表面に水系金属表面処理剤を塗ることをいう。「有する」とは、基材金属1及び表面処理皮膜2以外に他の構成を有していてもよいことを意味している。例えば、表面処理皮膜2の上にラミネート加工によって形成された樹脂フィルム3を有していてもよい。表面処理皮膜2は、上記した本発明に係る水系金属表面処理剤を基材金属1に塗布して形成されるので、密着性及び耐薬品密着維持性に優れている。
水系金属表面処理剤を用いた金属表面の処理方法は、水系金属表面処理剤を基材金属の表面に塗布する塗布工程と、塗布工程の後、水洗することなく乾燥し、表面処理皮膜を形成する乾燥工程とによって形成することができる。
塗布工程は、水系金属表面処理剤を基材金属の表面に塗布する工程である。塗布する方法は、特に限定されず、例えば、スプレーコート、ディップコート、ロールコート、カーテンコート、スピンコート、又はこれらを組み合わせた方法を用いることができる。水系金属表面処理剤の使用条件は、特に限定されない。例えば、塗布する際の水系金属表面処理剤及び金属材料の温度は、10℃〜90℃であることが好ましく、20℃〜60℃であることがより好ましい。温度が60℃以下であると、無駄なエネルギーの使用を抑制することができる。また、塗布する時間及び塗布する量は、得られる表面処理皮膜の求められる膜厚に応じて適宜設定することができる。
乾燥工程は、塗布工程後、水洗することなく乾燥し、表面処理皮膜を形成する工程である。乾燥温度は、使用する溶剤に合わせた温度とすることができる。例えば、水を溶剤として用いた場合には、50℃〜250℃の範囲であることが好ましい。乾燥装置は特に限定されないが、バッチ式、連続式又は熱風循環式の乾燥炉、コンベアー式熱風乾燥炉又はIHヒーターを用いた電磁誘導加熱炉等を用いることができ、その風量と風速等は任意に設定することができる。
(カチオン変性エポキシ樹脂:記号Aa)
窒素ガス導入管、温度計、分水器及び攪拌装置を備えた5リットルオートクレーブにN−(2−ヒドロキシエチル)エチレンジアミン104部及びメチルイソブチルケトン400部を加え、140℃、常圧で8時間反応させた。反応中に流出した水は窒素ガスを吹き込みながら分水器で随時除去した。反応終了後、過剰のメチルイソブチルケトンを120℃、減圧下で留去した。次いで、触媒として水酸化カリウム4部を加え、エチレンオキサイド1584部とプロピレンオキサイド348部の混合物を温度130℃、圧力10kg/cm2で付加させた。反応終了後、常法により触媒を除去し、水を60部添加し、110℃で4時間加水分解を行なった。加水分解終了後、遊離したメチルイソブチルケトン及び過剰の水分を減圧下に除去し、1級アミノ基含有ポリエーテル化合物を作製した。
窒素ガス導入管、温度計、分水器及び攪拌装置を備えた2リットルフラスコに、三洋化成工業株式会社製グリシエールPP−300P(ビスフェノールAへのアルキレンオキシド付加物のポリグリシジルエーテル化合物)162部、ジャパンエポキシレジン株式会社製jER828EL(ビスフェノールAとエピクロルヒドリンとの重縮合物)1000部、ビスフェノールA440部及びテトラブチルアンモニウムブロマイド1.6部を加え、160℃でエポキシ当量800になるまで反応させた。これに、メチルイソブチルケトン450部を加え、次いで、4−エチルアミノ−1−ブタノール210部を加えて、100℃で4時間反応させ、アミノ基含有エポキシ樹脂を得た。
窒素ガス導入管、温度計、分水器及び攪拌装置を備えた反応器に、エポキシ当量188を有するビスフェノールAをベースとするエポキシ樹脂(ビスフェノールAのジグリシジルエーテル化合物)6150部、ビスフェノールA1400部、ドデシルフェノール335部、p−クレゾール470部及びキシレン441部を加え、窒素雰囲気下で125℃に加熱し、10分間反応させた。次に、130℃に加熱して、エポキシ重合触媒としてN,N’−ジメチルベンジルアミン23部を加え、エポキシ当量が880に達するまでこの温度に維持した。さらに、添加剤としてポリエーテル(BYK Chemie社製、商品名「K−2000」)90部を加え、100℃に維持し、30分後に、ブチルアルコール211部及びイソブタノール1210部を加えた。
(メチロール変性樹脂1;記号Ba)
下記化学式4のカチオン変性フェノール樹脂(化学式4中、n/m;50/50、数平均分子量;5000、含有水酸基量;7.8mmol/g)を有機高分子Baとして用いた。
下記化学式5のビスフェノール型カチオン変性フェノール樹脂(化学式5中、n/m;40/60、数平均分子量;3500、含有水酸基量;9.2mmol/g)を有機高分子Bbとして用いた。
グリセリル化キトサン(数平均分子量:1〜10万、グリセリル化度1.1、含有水酸基量;18.6mmol/g)を用いた。
鹸化度96%、粘度25mPa・S、含有水酸基量21.8mmol/gのポリビニルアルコールを有機高分子Bdとして用いた。
鹸化度99%、粘度12mPa・S、アセトアセチル化度9.8%、含有水酸基量17.0mmol/gのアセトアセチル化ポリビニルアルコールを有機高分子Beとして用いた。
2−ヒドロキシエチルアクリレート(90質量%)とアクリル酸(10質量%)との共重合体(含有水酸基量7.8mmol/g)の水溶液(不揮発分濃度15質量%、粘度70mPa・s)を有機高分子Bfとして用いた。
アクリルアミド重合体(含有アミド基量;13.9mmol/g)の水溶液(不揮発分濃度22.0質量%、粘度90mPa・s)を有機高分子Bgとして用いた。
アジピン酸とポリエチレングリコールジアミンとε−カプロラクタムのブロック重合物(分子量:1万、含有アミド結合;6.6mmol/g)を有機高分子Bhとして用いた。
用いた無機化合物(C)を以下に示す。
Cb:ジルコニウムフッ化水素酸(濃度40.0質量%)
Cc:シリカゾル(表面電荷カチオン、粒子径10〜20nm、19.0質量%、pH=4.7)
Cd:乳酸チタン(濃度44.0質量%)
Ce:非晶質ジルコニアゾル(不揮発分濃度10.0質量%、粒子径10〜30nm、pH=2.8)
Cf:ケイフッ化水素酸(濃度40.0質量%)
Cg:フッ化クロム(III)(Cr濃度1.0質量%)
Ch:フッ化鉄(III)(Fe濃度2.5質量%)
Ci;酸化セレン(IV)
Cj;酸化セリウムゾル(不揮発分濃度15%、pH=3.5)
Ck;酢酸クロム(III)
用いた架橋性化合物(D)を以下に示す。
ポリエーテル系ブロックイソシアネート水溶液(不揮発分濃度30質量%、粘度1200mPa・s、ノニオン性)を架橋性化合物Daとして用いた。
不揮発分濃度40質量%のグリオキザール水溶液を架橋性化合物Dbとして用いた。
グリセロールポリグリシジルエーテル(3官能、エポキシ当量144、粘度170mPa・S)を架橋性化合物Dcとして用いた。
カチオン変性エポキシ樹脂Aa〜Ac、有機化合物Ba〜Bh、必要に応じて無機化合物Ca〜Ck及び必要に応じて架橋性化合物Da〜Dcを所定の含有量で組み合わせ、溶剤を水として、表1〜表8に示す実施例1〜118の水系金属表面処理剤と、比較例1〜27の水系金属表面処理剤を準備した。なお、表1〜表8における「濃度」は、水系金属表面処理剤に含まれる各化合物の不揮発分濃度(質量%)を示す。また、「A濃度」、「B濃度」、「C濃度」及び「D濃度」は、それぞれ、水系金属表面処理剤中の全固形分に対するカチオン変性エポキシ樹脂(A)、有機高分子(B)、無機化合物(C)及び架橋性化合物(D)の含有量(質量%)を示す。
基材(被処理材)として用いた金属材料を以下に示す。
Al:A1100P、厚さ0.3mm
Cu:C1020P、厚さ0.3mm
Ni:純ニッケル板:(純度99質量%以上)、厚さ0.3mm
SUS:SUS304板、厚さ0.3mm
NiめっきCu:電気NiめっきCu板(厚さ0.3mm、Niめっき厚2μm)
これら金属材料から、表1〜表8の「基材」欄に示す金属材料を選択し、実施例1〜118及び比較例1〜32の基材(被処理材)として準備した。
(表面処理)
表1〜表8に示した実施例1〜118及び比較例1〜27の基材金属をファインクリーナー359E(日本パーカライジング株式会社製のアルカリ脱脂剤)の3%水溶液で65℃、1分間スプレーして脱脂した後、水洗して表面を清浄した。続いて、金属材料の表面の水分を蒸発させるために、80℃で1分間、加熱乾燥した。脱脂洗浄した金属基材の表面に、それぞれ、表1〜表8に示した実施例1〜118及び比較例1〜27の水系金属表面処理剤を#3SUSマイヤーバーを用い、バーコートによって塗布し(塗布工程)、熱風循環式乾燥炉内で180℃、1分間乾燥し(乾燥工程)、表面処理皮膜を有する金属材料を得た。なお、同種の水系金属表面処理剤を用いて表面処理した金属材料をそれぞれ2つずつ準備し、以下に示すように、表面処理皮膜の上にそれぞれ別の方法でラミネート加工を施した。
2つずつ準備した表面処理皮膜を有する金属材料の1つについて、その表面処理皮膜の上に、ヒートラミネーションによるラミネート加工を施した。他の1つの表面処理皮膜の上に、ドライラミネーションによるラミネート加工を施した。表面処理皮膜を有しない金属材料についても、2つのうち1つの片側表面にヒートラミネーションを施し、他の1つの片側表面にドライラミネーションを施した。
ヒートラミネーションによって得たポリプロピレンフィルム積層金属材料と、ドライラミネーションによって得たポリプロピレンフィルム積層金属材料とを、それぞれ絞りしごき加工試験で深絞り加工した。直径160mmに打ち抜いた被覆金属板を絞り加工(1回目)し、直径100mmのカップを作製した。続いて、そのカップを直径75mmに再度絞り加工(2回目)し、さらに直径65mmに絞り加工(3回目)し、供試材である缶を作製した。なお、1回目の絞り加工、2回目の絞り加工、3回目の絞り加工におけるしごき(薄肉化分)率は、それぞれ、5%、15%、15%であった。
(密着性)
成形加工後の缶について、ポリプロピレンフィルムの剥離の有無(以下、「初期密着性」という。)を評価した。缶が作製でき、フィルムの剥離がなく初期密着性に優れるものを「3点」とし、フィルムの一部が剥離したものを「2点」とし、フィルムが全面剥離したものを「1点」とした。また、「3点」の中で、全く剥離が見られず特に外観が良く、非常に初期密着性に優れるものを「4点」とした。評価試験の結果を表9〜表11に示す。
耐薬品密着維持性のうち、ここでは、電解液に対する密着維持性(以下、「耐電解液密着維持性」という。)について評価した。詳しくは、次のようにして、成形加工後にさらに電解液に浸漬した後の缶について、ポリプロピレンフィルムの剥離の有無を評価した。
2 表面処理皮膜
3 樹脂フィルム(ラミネートフィルム)又は樹脂塗膜
10 表面処理皮膜を有する金属材料
Claims (3)
- 水溶性又は水分散性のカチオン変性エポキシ樹脂(A)と、アミド結合、アミド基及び水酸基から選ばれる1種又は2種以上の構造単位を1mmol/g〜50mmol/g含有する水溶性又は水分散性の有機高分子(B)とを含有し、
前記カチオン変性エポキシ樹脂(A)の含有量が、全固形分に対して10質量%〜90質量%であり、
前記有機高分子(B)が、ポリビニルアルコール及びその誘導体、メチロール変性樹脂、ヒドロキシル基含有天然高分子、ヒドロキシル基及びアミド基から選ばれる1種又は2種を有する付加重合性モノマーの単独重合物又は共重合物、ポリアミドのいずれか1又は2以上を含み、当該メチロール変性樹脂が、水溶性又は水分散性のマンニッヒ変性アミノ化フェノール樹脂、メラミン樹脂、尿素樹脂のいずれかであることを特徴とする水系金属表面処理剤。 - Mg、Al、Ca、Mn、Co、Ni、Cr(III)、Zn、Fe、Zr、Ti、Si、Sr、W、Ce、Mo、V、Sn、Bi、Ta、Te、In、Ba、Hf、Se、Sc、Nb、Cu、Y、Nd及びLaから選ばれる1種又は2種以上の元素を含む無機化合物(C)をさらに含有し、当該無機化合物(C)の含有量が、全固形分に対して1質量%〜80質量%である、請求項1に記載の水系金属表面処理剤。
- 請求項1又は2に記載の水系金属表面処理剤を金属材料の表面に塗布して形成された表面処理皮膜を有することを特徴とする金属材料。
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