JP6461815B2 - 防食被膜の製造方法 - Google Patents
防食被膜の製造方法 Download PDFInfo
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- JP6461815B2 JP6461815B2 JP2015553100A JP2015553100A JP6461815B2 JP 6461815 B2 JP6461815 B2 JP 6461815B2 JP 2015553100 A JP2015553100 A JP 2015553100A JP 2015553100 A JP2015553100 A JP 2015553100A JP 6461815 B2 JP6461815 B2 JP 6461815B2
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B05D7/52—Two layers
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- B05D7/546—No clear coat specified each layer being cured, at least partially, separately
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D129/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
- C09D129/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Description
ことが今なお必要である。
(1)(A)結合剤として少なくとも1種の有機ポリマーと、(B)有機陰イオンを含む少なくとも1種の合成層状複水酸化物と、を含む防食プライマーが金属基板に直接に施され(塗布され)、且つ
(2)工程(1)で施された防食プライマーからポリマーフィルムが形成される、防食被膜の製造方法であって、
少なくとも1種の合成層状複水酸化物(B)が少なくとも1種のα−アミノ酸の有機陰イオンを含むことを特徴とする方法である。
[M2+ (1-x) M3+ x(OH)2][Ay- (x/y)]・nH2O (I)
二価金属陽イオンM2+は、Zn2+、Mg2+、Ca2+、Cu2+、Ni2+、Co2+、Fe2+、Mn2+、Cd2+、Pb2+、Sr2+及びこれらの混合物からなる群、好ましくはZn2+、Mg2+、Ca2+及びこれらの混合物からなる群、非常に好ましくはZn2+又はMg2+からなる群、から選ばれ、
三価金属陽イオンM3+は、Al3+、Bi3+、Fe3+、Cr3+、Ga3+、Ni3+、Co3+、Mn3+、V3+、Ce3+、La3+及びこれらの混合物からなる群、好ましくはAl3+、Bi3+及び/又はFe3+からなる群、より好ましくはAl3+、から選ばれ、
陰イオンAy−はα−アミノ酸の少なくとも1つの有機陰イオンを少なくとも一部として含み、
xは、0.05〜0.5の数値、より好ましくは0.15〜0.4の数値、非常に好ましくは0.25〜0.35の数値、を取り、及び
nは、0〜10の数値を取る。
亜鉛−アルミニウム及び/又はマグネシウム/アルミニウムをベースとする異なるLDHを、直接共沈法によって作製した。本発明に従って用いるLDHを、L−フェニルアラニン(Zn2+/Al3+の金属陽イオン組み合わせ)及びL−システイン(Mg2+/Al3+の金属陽イオン組み合わせ)を用いて得た。対照用に、高い効率で毒性の強い腐食防止剤として知られるクロム酸塩陰イオンを含むLDHを製造した。
3モルのNaOH溶液でpH8に調整された0.39モルのL−フェニルアラニン水溶液を、一定のメータ速度(計量添加速度)で室温窒素雰囲気でZnCl2・6H2O(0.52モル)及びAlCl3・6H2O (0.26モル)の水性混合物と、3時間以上連続撹拌しながら混合し、添加された陽イオンの量を、1.5:1のL−フェニルアラニンと三価Alとのモル比となるように選択した。pHを、3モルのNaOH溶液の添加により8に一定に維持した。金属塩の水性混合物を添加した後、室温で3時間、生成された懸濁液を撹拌し、且つエイジングした。生成された沈殿物を遠心分離し、且つ脱イオン水で4回洗浄した。生成された白い反応生成物のスラリーを、減圧下で30℃で24時間乾燥し、LDHを白い粉末として得た。
3モルのNaOH溶液でpH10に調整された0.52モルのL−システイン水溶液を、一定のメーター速度で室温で窒素雰囲気でMgCl2・6H2O(0.52モル)及びAlCl3・6H2O (0.26モル)の水性混合物と、3時間以上連続撹拌しながら混合し、添加された陽イオンの量を、2:1のL−システインと三価Alとのモル比となるように選択した。pHを、3モルのNaOH溶液の添加により10に一定に維持した。金属塩の水性混合物を添加した後、室温で3時間、生成された懸濁液を撹拌し、且つ老化した。生成された沈殿物を遠心分離し、且つ脱イオン水で4回洗浄した。生成された白い反応生成物のスラリーを、減圧下で30℃で24時間乾燥し、LDHを白い粉末として得た。LDH(一価L−システイン陰イオン:Mg2Al(OH)6(L−システイン)によって、100%の電荷補償度の理論的な最大値の場合の理論的な実験式)が41%の電荷補償度(計算中一価陰イオンと見なされるシステイン陰イオンで、ICP−OESによる定量要素分析によって測られた)を有した。
0.52モルのクロム酸ナトリウム(Na2CrO4)の水性アルカリ溶液(pH = 9.6)を、一定のメーター速度で室温窒素雰囲気でMgCl2・6H2O(0.52モル)及びAlCl3・6H2O (0.26モル)の水性混合物と3時間以上連続撹拌しながら混合し、添加された陽イオンの量を、2:1のクロム酸塩と三価Alとのモル比となるように選択した。pHを、3モルのNaOH溶液の添加により10に一定に維持した。金属塩の水性混合物を添加した後、室温で3時間、生成された懸濁液を撹拌し、且つエイジングした。生成された沈殿物を遠心分離し、且つ脱イオン水で4回洗浄した。生成された白い反応生成物のスラリーを、減圧下で30℃で24時間乾燥し、LDHを白い粉末として得た。
本発明の1つのLDH相(Zn2Al(OH)6(L−フェニルアラニン)及びMg2Al(OH)6(L−システイン)、並びに対照用LDH(Zn2Al(OH)6(1/2・CrO4))をそれぞれ含む防食プライマーを製造した。いずれの場合にも、LDH部分は、本発明の防食プライマー総量に基づき4.7質量%(該腐食防止プライマーの固形物に基づいて、10質量%に対応する)とし、かつ、それを被膜材料を製造する前にプライマー成分(表1に参照)に組み込んだ。D2)で述べるように、耐腐食性を判定するために同様に参照被膜材料を製造した。該参照被膜材料において、LDHを使用しなかった。防食プライマーはエポキシ樹脂/ポリアミン基(2C)被膜材料であった。防食プライマーの構成物質、並びにそのポリマー成分の含有量及び架橋成分の含有量は表1及び表2に記載した。基板に施される直前に、成分は3:1(ポリマー成分:架橋成分)の比率で混合した。
AA2024−T3合金(アルミニウム銅合金)で製造された基板パネルを、作製された防食プライマーを用いて被覆した。
D1)直流分極測定
α−アミノ酸の陰イオンの腐食抑制効率又は耐腐食性のテストは直流分極測定(DC分極)によって行った。公知のように、腐食過程の原理は、材料(一般的には金属表面)と、その環境との間の、金属酸化と、それによる金属陽イオンの固体材料からの出願(言い換えれば、腐食電流)を伴う電気化学反応である。DC分極測定は電気化学測定技術であり、該技術自体は公知で、例えばProgress in Organic Coatings,61 (2008) 283−290に記載されている。該方法は、電位の変化に対して持続的な走査速度で、系の電流応答を測定する。そして、腐食電流は得られる測定データから算出される。
EISは、例えば電解質溶液で覆われた表面被膜のような、異なる系のさまざまな電気化学特性を分析する(先と同様に既知)方法である。分析される系は、低振幅で周波数が連続的に変化する正弦波交流電圧に曝され、その後交流抵抗(インピーダンス量)だけではなく、付与交流電圧と、系の合成交流電流との間の相シフトも周波数の関数として測定される。評価のために、測られた周波数スペクトルは理論上の等価回路図とマッチされる。該等価回路図は、オーム性抵抗器、容量抵抗器及び誘導性抵抗器又はいわゆる「定位相」要素のような異なるインピーダンス要素の直列回路及び/又は並列回路からなる。測られたスペクトルと等価回路図(理論上のスペクトル)から得られる理論上の数学関数との間に適切な合致がある場合、実際の測定系に存在する要素は等価回路図の(理論上の)インピーダンス要素に当たる。
Rc 被膜の抵抗
Rd 基板と被膜との間の電解二重層(基板の酸化層)の抵抗
CPEc 被膜の定位相要素
CPEd 基板と被膜との間の電解二重層(基板の酸化層)の定位相要素
Claims (17)
- (1)(A)結合剤としての、重付加樹脂、重縮合樹脂及び/又は付加重合樹脂である少なくとも1種の有機ポリマーと、
(B)有機陰イオンを含む少なくとも1種の合成層状複水酸化物と、
を含む防食プライマーが金属基板に直接に施され、且つ
(2)工程(1)で施された前記防食プライマーからポリマーフィルムが形成される、防食被膜の製造方法であって、
前記少なくとも1種の合成層状複水酸化物(B)が少なくとも1種のα−アミノ酸の有機陰イオンを含むことを特徴とする方法。 - 前記防食プライマーが陰イオン安定化ポリマーを含まないことを特徴とする、請求項1に記載の方法。
- 前記防食プライマーが有機ポリマー(A)として少なくとも1種のポリビニルブチラール樹脂及び/又はエポキシ樹脂を含むことを特徴とする請求項1または2に記載の方法。
- 前記防食プライマーが有機ポリマー(A)として少なくとも1種のエポキシ樹脂と、架橋剤として少なくとも1種のポリアミンと、を含むことを特徴とする請求項3に記載の方法。
- 前記防食プライマーが二成分系であることを特徴とする請求項1から4のいずれか一項に記載の方法。
- 前記有機陰イオンを含む前記少なくとも1種の合成の層状複水酸化物(B)が下記の一般式(I)を有することを特徴とする請求項1から5のいずれか一項に記載の方法
[M2+ (1−x) M3+ x(OH)2][Ay− (x/y)]・nH2O (I)
(式中、M2+は二価金属陽イオンを表し、M3+は三価金属陽イオンを表し、Ay−は平均原子価yの陰イオンを表し、前記陰イオンは少なくとも部分的に少なくとも1種のα−アミノ酸の有機陰イオンを含み、xは0.05〜0.5の数値を取り、nは0〜10の間の数値を取る)。 - 前記二価金属陽イオンM2+が、Zn2+、Mg2+、Ca2+、Cu2+、Ni2+、Co2+、Fe2+、Mn2+、Cd2+、Pb2+、Sr2+及びこれらの混合物からなる群、好ましくはZn2+、Mg2+、Ca2+及びこれらの混合物からなる群、非常に好ましくはZn2+及び/又はMg2+からなる群、より好ましくはZn2+からなる群、から選択され、
前記三価金属陽イオンM3+が、Al3+、Bi3+、Fe3+、Cr3+、Ga3+、Ni3+、Co3+、Mn3+、V3+、Ce3+、La3+及びこれらの混合物からなる群、好ましくはAl3+、Bi3+及び/又はFe3+からなる群、より好ましくはAl3+からなる群、から選択され、
xが、0.05〜0.5の数値、より好ましくは0.15〜0.4の数値、非常に好ましくは0.25〜0.35の数値、を取り、及び
nが、0〜10の数値であることを特徴とする請求項6に記載の方法。 - 前記少なくとも1種のα−アミノ酸の有機陰イオンが、アラニン、アルギニン、アスパラギン、アスパラギン酸、システイン、シスチン、グルタミン、グルタミン酸、ヒスチジン、イソロイシン、ロイシン、リジン、メチオニン、フェニルアラニン、プロリン、セリン、トレオニン、トリプトファン、チロシン、バリン、セレノシステイン、ピロリシン及びセレノメチオニンの有機陰イオンからなる群から選択されることを特徴とする請求項1から7のいずれか一項に記載の方法。
- 前記少なくとも1種のα−アミノ酸の有機陰イオンが、1種のアミノ基とそれに対してα位に位置するカルボン酸基に加え、更に他のアミノ基、他のカルボン酸基、水酸基、チオール基、ジスルフィド基及び/又は不飽和環状ラジカルを含むα−アミノ酸の有機陰イオンからなる群から選択されることを特徴とする請求項1から7のいずれか一項に記載の方法。
- 前記少なくとも1種のα−アミノ酸の有機陰イオンが、アルギニン、アスパラギン、アスパラギン酸、システイン、シスチン、グルタミン、グルタミン酸、ヒスチジン、リジン、メチオニン、フェニルアラニン、プロリン、セリン、トレオニン、トリプトファン及びチロシンの有機陰イオンからなる群から選択されることを特徴とする請求項1から7のいずれか一項に記載の方法。
- 前記少なくとも1種のα−アミノ酸の有機陰イオンが、システイン、シスチン及びフェニルアラニンからなる群から選択されることを特徴とする請求項10に記載の方法。
- 前記有機陰イオンを含む少なくとも1種の合成層状複水酸化物が、直接共沈法或いは陰イオン交換反応により製造されることを特徴とする請求項1から11のいずれか一項に記載の方法。
- 前記有機陰イオンを含む少なくとも1種の合成層状複水酸化物の含有量が、前記防食プライマーの総量に対して2質量%〜15質量%であることを特徴とする請求項1から12のいずれか一項に記載の方法。
- 複層被膜を製造するために、前記ポリマーフィルムの形成(2)の後、
(3)少なくとも1種の他の被膜材料が施され、且つ
(4)工程(3)で施された前記他の被膜材料からポリマーフィルムが形成される
ことを特徴とする請求項1から13のいずれか一項に記載の方法。 - 前記金属基板が、アルミニウム、アルミニウム合金、より好ましくはアルミニウム銅合金、並びに非合金鋼及び合金鋼からなる群から選ばれることを特徴とする請求項1から14のいずれか一項に記載の方法。
- 請求項1から15のいずれか一項に記載の方法で被覆された被覆金属基板。
- (A)結合剤としての少なくとも1種の有機樹脂と、(B)有機陰イオンを含む少なくとも1種の合成層状複水酸化物と、を含む防食プライマーの使用方法であって、
前記少なくとも1種の合成層状複水酸化物(B)が金属基板の耐腐食性を改善するために少なくとも1種のα−アミノ酸の有機陰イオンを含む使用方法。
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- 2014-01-17 WO PCT/EP2014/050938 patent/WO2014111539A1/de active Application Filing
- 2014-01-17 CN CN201480005007.0A patent/CN105008463B/zh not_active Expired - Fee Related
- 2014-01-17 EP EP14700748.8A patent/EP2945987B1/de not_active Not-in-force
- 2014-01-17 JP JP2015553100A patent/JP6461815B2/ja not_active Expired - Fee Related
- 2014-01-17 US US14/760,823 patent/US20150376420A1/en not_active Abandoned
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EP2945987B1 (de) | 2018-05-09 |
CN105008463B (zh) | 2017-12-12 |
WO2014111539A1 (de) | 2014-07-24 |
EP2945987A1 (de) | 2015-11-25 |
CN105008463A (zh) | 2015-10-28 |
US20150376420A1 (en) | 2015-12-31 |
JP2016511300A (ja) | 2016-04-14 |
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