JPWO2019065961A1 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JPWO2019065961A1 JPWO2019065961A1 JP2019545677A JP2019545677A JPWO2019065961A1 JP WO2019065961 A1 JPWO2019065961 A1 JP WO2019065961A1 JP 2019545677 A JP2019545677 A JP 2019545677A JP 2019545677 A JP2019545677 A JP 2019545677A JP WO2019065961 A1 JPWO2019065961 A1 JP WO2019065961A1
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Classifications
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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
- C09D5/36—Pearl essence, e.g. coatings containing platelet-like pigments for pearl lustre
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
- B05D5/067—Metallic effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—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
- B05D7/50—Multilayers
- B05D7/56—Three layers or more
- B05D7/57—Three layers or more the last layer being a clear coat
- B05D7/572—Three layers or more the last layer being a clear coat all layers being cured or baked together
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
Description
下記の工程(1)〜(4):
(1)被塗物上に、ベース塗料(X)を塗装してベース塗膜を形成する工程、
(2)工程(1)で形成されるベース塗膜上に、光輝性顔料分散体(Y)を塗装して乾燥膜厚として0.01〜5μmである光輝性塗膜を形成する工程、
(3)工程(2)で形成される光輝性塗膜上に、クリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程、及び
(4)工程(1)〜(3)で形成された未硬化のベース塗膜、未硬化の光輝性塗膜及び未硬化のクリヤー塗膜を加熱することによって、これら3つの塗膜を同時に硬化させる工程、を含む複層塗膜の形成方法であって、
光輝性顔料分散体(Y)が、アルミニウムフレーク顔料(A)、光散乱粒子(B)、水酸基含有アクリル樹脂(C)、及び水を含有する複層塗膜形成方法に関する。
工程(1)は、被塗物上に、ベース塗料(X)を塗装してベース塗膜を形成する工程である。
本発明の複層塗膜形成方法において、被塗物としては、鉄、亜鉛、アルミニウム等の金属やこれらを含む合金などの金属材、及びこれらの金属による成型物、ならびに、ガラス、プラスチックや発泡体などによる成型物、フィルム等を挙げることができる。これら素材に応じて適宜、脱脂処理や表面処理して被塗物とすることができる。該表面処理としては例えばリン酸塩処理、クロメート処理、複合酸化物処理等が挙げられる。さらに、上記被塗物の素材が金属であれば、表面処理された金属素材の上にカチオン電着塗料によってカチオン電着塗膜が形成されていることが好ましい。該カチオン電着塗膜の上には中塗り塗膜が形成されていても良い。該中塗り塗膜は着色していることが下地隠蔽性及び耐候性等の点から好ましい。特に、後述するベース塗料(X)が透明の場合は、白色中塗り塗膜が形成されていることが得られる複層塗膜が耐候性及び白い金属調光沢に優れる点から好ましい。
ベース塗料(X)としては、具体的には、溶媒及び熱硬化性樹脂を主成分とする熱硬化性塗料を使用することができる。そのような熱硬化性塗料は公知である。該熱硬化性塗料には中塗り塗料と呼ばれるものも含むことができる。ベース塗料(X)は透明であっても着色されたものであっても良い。
工程(2)は、工程(1)で形成されるベース塗膜上に、光輝性顔料分散体(Y)を塗装して乾燥膜厚として0.01〜5.0μmの光輝性塗膜を形成する工程である。乾燥膜厚は好ましくは0.05〜3.0μm、さらに好ましくは0.1〜2.0μmである。
光輝性顔料分散体(Y)は、アルミニウムフレーク顔料(A)、光散乱粒子(B)、水酸基含有アクリル樹脂(C)及び水を含有する。
アルミニウムフレーク顔料(A)としては、一般にアルミニウムをボールミル又はアトライターミル中で粉砕媒液の存在下、粉砕助剤を用いて粉砕、摩砕して製造されるミリングタイプの鱗片状アルミニウム顔料と、後述する蒸着タイプの鱗片状アルミニウム顔料とのいずれを使用してもよい。ミリングタイプの鱗片状アルミニウム顔料の製造工程における粉砕助剤としては、オレイン酸、ステアリン酸、イソステアリン酸、ラウリン酸、パルミチン酸、ミリスチン酸等の高級脂肪酸のほか、脂肪族アミン、脂肪族アミド、脂肪族アルコールが使用される。粉砕媒液としてはミネラルスピリットなどの脂肪族系炭化水素が使用される。
光散乱粒子(B)は、複層塗膜のハイライト近傍での高い明度のために使用される。また、光散乱粒子(B)は、複層塗膜のハイライトからシェードまでの白さの知覚を可能にし得る。光散乱粒子(B)としては、酸化チタン、マイカ、シリカ、バリタ、ガラス、アルミナ、亜鉛華、鉛白等を挙げることができる。これらは1種を単独で又は2種以上を併用して用いることができる。該マイカ、シリカ、ガラス、アルミナは金属酸化物で被覆されていても良い。
水酸基含有アクリル樹脂(C)は、1分子中に少なくとも1個の水酸基を有するアクリル樹脂である。水酸基含有アクリル樹脂(C)は、従来から水性塗料に使用されているそれ自体既知の水溶性又は水分散性の水酸基含有アクリル樹脂を使用することができる。水酸基含有アクリル樹脂(C)は、例えば、水酸基含有重合性不飽和モノマー及び該水酸基含有重合性不飽和モノマーと共重合可能な他の重合性不飽和モノマーを、それ自体既知の方法、例えば、溶液重合などの方法により、共重合せしめることによって製造することができる。
(i) アルキル又はシクロアルキル(メタ)アクリレート: 例えば、メチル(メタ)アクリレート、エチル(メタ)アクリレート、n−プロピル(メタ)アクリレート、i−プロピル(メタ)アクリレート、n−ブチル(メタ)アクリレート、i−ブチル(メタ)アクリレート、tert−ブチル(メタ)アクリレート、n−ヘキシル(メタ)アクリレート、n−オクチル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、ノニル(メタ)アクリレート、ドデシル(メタ)アクリレート、トリデシル(メタ)アクリレート、ステアリル(メタ)アクリレート、イソステアリル(メタ)アクリレート、シクロヘキシル(メタ)アクリレート、メチルシクロヘキシル(メタ)アクリレート、t−ブチルシクロヘキシル(メタ)アクリレート、シクロドデシル(メタ)アクリレート、トリシクロデカニル(メタ)アクリレート等。
(ii) イソボルニル基を有する重合性不飽和モノマー: 例えば、イソボルニル(メタ)アクリレート等。
(iii) アダマンチル基を有する重合性不飽和モノマー: 例えば、アダマンチル(メタ)アクリレート等。
(iv) トリシクロデセニル基を有する重合性不飽和モノマー: 例えば、トリシクロデセニル(メタ)アクリレート等。
(v) 芳香環含有重合性不飽和モノマー: 例えば、ベンジル(メタ)アクリレート、スチレン、α−メチルスチレン、ビニルトルエン等。
(vii) フッ素化アルキル基を有する重合性不飽和モノマー: 例えば、パーフルオロブチルエチル(メタ)アクリレート、パーフルオロオクチルエチル(メタ)アクリレート等のパーフルオロアルキル(メタ)アクリレート;フルオロオレフィン等。
(viii) マレイミド基等の光重合性官能基を有する重合性不飽和モノマー。
(ix) ビニル化合物: 例えば、N−ビニルピロリドン、エチレン、ブタジエン、クロロプレン、プロピオン酸ビニル、酢酸ビニル等。
(x) リン酸基含有重合性不飽和モノマー: 例えば、2−アクリロイルオキシエチルアシッドホスフェート、2−メタクリロイルオキシエチルアシッドホスフェート、2−アクリロイルオキシプロピルアシッドホスフェート、2−メタクリロイルオキシプロピルアシッドホスフェート等。
(xi) カルボキシル基含有重合性不飽和モノマー: 例えば、(メタ)アクリル酸、マレイン酸、クロトン酸、β−カルボキシエチルアクリレート等。
(xii) 含窒素重合性不飽和モノマー: 例えば、(メタ)アクリロニトリル、(メタ)アクリルアミド、N,N−ジメチルアミノエチル(メタ)アクリレート、N,N−ジエチルアミノエチル(メタ)アクリレート、N,N−ジメチルアミノプロピル(メタ)アクリルアミド、メチレンビス(メタ)アクリルアミド、エチレンビス(メタ)アクリルアミド、2−(メタクリロイルオキシ)エチルトリメチルアンモニウムクロライド、グリシジル(メタ)アクリレートとアミン類との付加物等。
(xiii) 重合性不飽和基を1分子中に少なくとも2個有する重合性不飽和モノマー: 例えば、アリル(メタ)アクリレート、1,6−ヘキサンジオールジ(メタ)アクリレート等。
(xv) 分子末端がアルコキシ基であるポリオキシエチレン鎖を有する(メタ)アクリレート。
(xvi) スルホン酸基を有する重合性不飽和モノマー: 例えば、2−アクリルアミド−2−メチルプロパンスルホン酸、2−スルホエチル(メタ)アクリレート、アリルスルホン酸、4−スチレンスルホン酸等;これらスルホン酸のナトリウム塩及びアンモニウム塩等。
(xvii) 紫外線吸収性官能基を有する重合性不飽和モノマー: 例えば、2−ヒドロキシ−4−(3−メタクリロイルオキシ−2−ヒドロキシプロポキシ)ベンゾフェノン、2−ヒドロキシ−4−(3−アクリロイルオキシ−2−ヒドロキシプロポキシ)ベンゾフェノン、2,2’ −ジヒドロキシ−4−(3−メタクリロイルオキシ−2−ヒドロキシプロポキシ)ベンゾフェノン、2,2’ −ジヒドロキシ−4−(3−アクリロイルオキシ−2−ヒドロキシプロポキシ)ベンゾフェノン、2−(2’ −ヒドロキシ−5’ −メタクリロイルオキシエチルフェニル)−2H−ベンゾトリアゾール等。
(xviii) 光安定性重合性不飽和モノマー: 例えば、4−(メタ)アクリロイルオキシ−1,2,2,6,6−ペンタメチルピペリジン、4−(メタ)アクリロイルオキシ−2,2,6,6−テトラメチルピペリジン、4−シアノ−4−(メタ)アクリロイルアミノ−2,2,6,6−テトラメチルピペリジン、1−(メタ)アクリロイル−4−(メタ)アクリロイルアミノ−2,2,6,6−テトラメチルピペリジン、1−(メタ)アクリロイル−4−シアノ−4−(メタ)アクリロイルアミノ−2,2,6,6−テトラメチルピペリジン、4−クロトノイルオキシ−2,2,6,6−テトラメチルピペリジン、4−クロトノイルアミノ−2,2,6,6−テトラメチルピペリジン、1−クロトノイル−4−クロトノイルオキシ−2,2,6,6−テトラメチルピペリジン等。
(xix) カルボニル基を有する重合性不飽和モノマー: 例えば、アクロレイン、ダイアセトンアクリルアミド、ダイアセトンメタクリルアミド、アセトアセトキシエチルメタクリレート、ホルミルスチロール、4〜7個の炭素原子を有するビニルアルキルケトン(例えば、ビニルメチルケトン、ビニルエチルケトン、ビニルブチルケトン)等。
(xx) 酸無水物基を有する重合性不飽和モノマー: 例えば、無水マレイン酸等、無水イタコン酸、無水シトラコン酸等。
光輝性顔料分散体(Y)は、さらに表面調整剤(D)を含有することが好ましい。表面調整剤は、ベース塗膜面への光輝性顔料分散体(Y)の塗装時に、水に分散されたアルミニウムフレーク顔料(A)をベース塗膜面上に一様に配向するのを支援するために使用される。アルミニウムフレーク顔料(A)をベース塗膜面上に一様に配向することができれば、金属調光沢に優れ、明度変化にメリハリのある複層塗膜を得ることができる。
光輝性顔料分散体(Y)は、さらに粘性調整剤(E)を含有していても良い。粘性調整剤(E)としては、既知のものを使用できるが、例えば、シリカ系微粉末、鉱物系粘性調整剤、硫酸バリウム微粒化粉末、ポリアミド系粘性調整剤、有機樹脂微粒子粘性調整剤、ジウレア系粘性調整剤、ウレタン会合型粘性調整剤、アクリル膨潤型であるポリアクリル酸系粘性調整剤、セルロース系粘性調整剤等を挙げることができる。なかでも金属調光沢に優れた塗膜を得る観点から特に、鉱物系粘性調整剤、ポリアクリル酸系粘性調整剤、セルロース系粘性調整剤を使用することが好ましい。
光輝性顔料分散体(Y)は、アルミニウムフレーク顔料(A)、光散乱粒子(B)、水酸基含有アクリル樹脂(C)及び水を含む。該光輝性顔料分散体(Y)において各成分の配合割合は、金属調光沢に優れる塗膜を得る観点から下記の範囲内であることが好ましい。
アルミニウムフレーク顔料(A)(固形分量として):好ましくは0.1〜5.0質量部、より好ましくは0.1〜3.0質量部、さらに好ましくは0.2〜2.0質量部、
光散乱粒子(B)(固形分量として):好ましくは0.1〜40.0質量部、より好ましくは0.3〜20.0質量部、さらに好ましくは0.5〜15.0質量部、
水酸基含有アクリル樹脂(C)(固形分量として):好ましくは0.01〜5.0質量部、より好ましくは0.02〜3.5質量部、さらに好ましくは0.03〜2.0質量部、
水:好ましくは50〜99.5質量部、より好ましくは75〜96.0質量部、さらに好ましくは81〜95.0質量部。
光輝性顔料分散体(Y)は、前述の成分を混合分散せしめることによって調製される。金属調光沢に優れる塗膜を得る観点から、塗装時の固形分含有率を、光輝性顔料分散体(Y)に基づいて、好ましくは0.1〜25.0質量%、より好ましくは1.0〜20.0質量%、さらに好ましくは1.0〜9.0質量%に調整しておく。
工程(3)は、工程(2)で形成される光輝性塗膜上に、クリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程である。
クリヤー塗料(Z)は、公知の熱硬化性クリヤーコート塗料組成物をいずれも使用できる。該熱硬化性クリヤーコート塗料組成物としては、例えば、架橋性官能基を有する基体樹脂及び架橋剤を含有する有機溶剤型熱硬化性塗料組成物、水性熱硬化性塗料組成物、粉体熱硬化性塗料組成物等を挙げることができる。
水酸基含有樹脂としては、水酸基を含有するものであれば従来公知の樹脂が制限なく使用できる。該水酸基含有樹脂としては例えば、水酸基含有アクリル樹脂、水酸基含有ポリエステル樹脂、水酸基含有ポリエーテル樹脂、水酸基含有ポリウレタン樹脂などを挙げることができ、好ましいものとして、水酸基含有アクリル樹脂、水酸基含有ポリエステル樹脂を挙げることができ、特に好ましいものとして水酸基含有アクリル樹脂を挙げることができる。
ポリイソシアネート化合物は、1分子中に少なくとも2個のイソシアネート基を有する化合物であって、例えば、脂肪族ポリイソシアネート、脂環族ポリイソシアネート、芳香脂肪族ポリイソシアネート、芳香族ポリイソシアネート、該ポリイソシアネートの誘導体などを挙げることができる。
工程(4)は、工程(1)〜(3)で形成された未硬化のベース塗膜、未硬化の光輝性塗膜及び未硬化のクリヤー塗膜を加熱することによって、これら3つの塗膜を同時に硬化させる工程である。なお、光輝性顔料分散体(Y)が上記架橋剤を含まない場合でも、上層及び/又は下層からの樹脂成分の移行によって光輝性塗膜が硬化する場合がある。
また、本発明は以下の構成を採用することもできる。
(1)被塗物上に、ベース塗料(X)を塗装してベース塗膜を形成する工程、
(2)工程(1)で形成されるベース塗膜上に、光輝性顔料分散体(Y)を塗装して乾燥膜厚として0.01〜5μmである光輝性塗膜を形成する工程、
(3)工程(2)で形成される光輝性塗膜上に、クリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程、及び
(4)工程(1)〜(3)で形成された未硬化のベース塗膜、未硬化の光輝性塗膜及び未硬化のクリヤー塗膜を加熱することによって、これら3つの塗膜を同時に硬化させる工程、を含む複層塗膜の形成方法であって、
光輝性顔料分散体(Y)が、アルミニウムフレーク顔料(A)、光散乱粒子(B)、水酸基含有アクリル樹脂(C)、及び水を含有する複層塗膜形成方法。
アルミニウムフレーク顔料(A)が0.1〜5.0質量部、光散乱粒子(B)が0.1〜40.0質量部、水酸基含有アクリル樹脂が0.01〜5.0質量部、水が50〜99.5質量部である項1〜9のいずれか1項に記載の複層塗膜形成方法。
前記ベース塗膜上に形成された、光輝性顔料分散体(Y)から形成された光輝性塗膜であって、アルミニウムフレーク顔料(A)、光散乱粒子(B)、及び水酸基含有アクリル樹脂(C)を含有し、乾燥膜厚が0.01〜5μmである光輝性塗膜と、
光輝性塗膜上に形成された、クリヤー塗料(Z)を塗装してクリヤー塗膜と
を備えた複層塗膜であって、前記ベース塗膜、前記光輝性塗膜及び前記クリヤー塗膜は同時に硬化されたものである、複層塗膜。
アルミニウムフレーク顔料(A)が0.1〜50.0質量部、光散乱粒子(B)が10.0〜95.0質量部、及び水酸基含有アクリル樹脂が0.1〜30.0質量部である項13〜20のいずれか1項に記載の複層塗膜。
製造例1
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器にプロピレングリコールモノプロピルエーテル35部を仕込み85℃に昇温後、メチルメタクリレート32部、n−ブチルアクリレート27.7部、2−エチルヘキシルアクリレート20部、4−ヒドロキシブチルアクリレート10部、ヒドロキシプロピルアクリレート3部、アクリル酸6.3部、2−アクリロイルオキシエチルアシッドフォスフェート1部、プロピレングリコールモノプロピルエーテル15部及び2,2’−アゾビス(2,4−ジメチルバレロニトリル)2.3部の混合物を4時間かけて滴下し、滴下終了後1時間熟成した。その後さらにプロピレングリコールモノプロピルエーテル10部及び2,2’−アゾビス(2,4−ジメチルバレロニトリル)1部の混合物を1時間かけて滴下し、滴下終了後1時間熟成した。さらにジエタノールアミン7.4部を加え、固形分55%の水酸基含有アクリル樹脂(C−1)溶液を得た。得られた水酸基含有アクリル樹脂(C−1)は酸価が51mgKOH/g、水酸基価が52mgKOH/gであった。
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器にプロピレングリコールモノプロピルエーテル35部を仕込み85℃に昇温後、メチルメタクリレート30部、2−エチルヘキシルアクリレート20部、n−ブチルアクリレート29部、2−ヒドロキシエチルアクリレート15部、アクリル酸6部、プロピレングリコールモノプロピルエーテル15部及び2,2’−アゾビス(2,4−ジメチルバレロニトリル)2.3部の混合物を4時間かけて滴下し、滴下終了後1時間熟成した。その後さらにプロピレングリコールモノプロピルエーテル10部及び2,2’−アゾビス(2,4−ジメチルバレロニトリル)1部の混合物を1時間かけて滴下し、滴下終了後1時間熟成した。さらにジエタノールアミン7.4部を加え、固形分55%の水酸基含有アクリル樹脂(C−2)溶液を得た。得られた水酸基含有アクリル樹脂(C−2)は酸価が47mgKOH/g、水酸基価が72mgKOH/gであった。
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器にプロピレングリコールモノプロピルエーテル35部を仕込み85℃に昇温後、2−アクリロイルオキシエチルアシッドフォスフェート30部、ラウリルメタクリレート20部、n−ブチルアクリレート10部、スチレン20部、2−ヒドロキシエチルアクリレートのε−カプロラクトン付加物10部、2−ヒドロキシエチルアクリレート10部、プロピレングリコールモノプロピルエーテル15部及び2,2’−アゾビス(2,4−ジメチルバレロニトリル)2.3部の混合物を4時間かけて滴下し、滴下終了後1時間熟成した。その後さらにプロピレングリコールモノプロピルエーテル10部及び2,2’−アゾビス(2,4−ジメチルバレロニトリル)1部の混合物を1時間かけて滴下し、滴下終了後1時間熟成した。さらにジエタノールアミン7.4部を加え、固形分50%の水酸基含有アクリル樹脂(C−3)溶液を得た。得られた水酸基含有アクリル樹脂(C−3)は酸価が140mgKOH/g、水酸基価が60mgKOH/gであった。
酸化チタン分散体の製造
撹拌混合容器に、水酸基含有アクリル樹脂(C−1)6部(固形分3.3部)、JR−903(商品名、ルチル型酸化チタン顔料 テイカ社製)35部及び脱イオン水60部を入れ、均一に混合し、更に、2−(ジメチルアミノ)エタノールを添加して、pH7.5に調整した。得られた混合物を225ml容の樹脂性のビンに入れ、1.5mm径のジルコニアビーズ130部を投入して密栓し、振とう型ペイントコンディショナーを使用して120分分散した。分散後100メッシュの金網濾過を行なってジルコニアビーズを除去して、固形分66%の酸化チタン分散体1を得た。
製造例4において、水酸基含有アクリル樹脂(C−1)に替えて、水酸基含有アクリル樹脂(C−2)に変更した以外は、製造例4と同様にして、固形分66%の酸化チタン分散体2を得た。
製造例6
蒸留水 92.0部、「Hydroshine WS−3004」(商品名、水性用蒸着アルミニウムフレーク顔料、Eckart社製、固形分:10%、内部溶剤:イソプロパノール、平均粒子径D50:13μm、厚さ:0.05μm、表面がシリカ処理されている) 5.0部(固形分で0.5部)、酸化チタン分散体1 2.9部(固形分で1.9部)、「Acrysol ASE−60」(ポリアクリル酸系粘性調整剤、ダウケミカル社製、固形分:28%) 2.7部(固形分で0.76部)、表面調整剤「BYK348」(商品名、BYK社製、シリコーン系表面調整剤、接触角:13°、動的表面張力:63.9mN/m、静的表面張力:22.2mN/m、ラメラ長:7.45mm、不揮発分:100質量%) 1.0部(固形分で1.0部)、ジメチルエタノールアミン 0.3部を配合して攪拌混合し、光輝性顔料分散体(Y−1)を調製した。
表1に記載の配合とする以外は全て製造例6と同様にして光輝性顔料分散体(Y−2)〜(Y−13)を得た。
ブロックポリイソシアネート(注2):ヘキサメチレンジイソシアネ−トのイソシアヌレート体を3,5−ジメチルピラゾールでフルブロックした化合物。固形分70%、
「レオクリスタ」(注3):商品名、セルロース系粘性調整剤=セルロースナノファイバーゲル、第一工業製薬社製、固形分2%。
被塗物1
脱脂及びりん酸亜鉛処理した鋼板(JISG3141、大きさ400mm×300mm×0.8mm)にカチオン電着塗料「エレクロンGT−10」(商品名:関西ペイント社製、エポキシ樹脂ポリアミン系カチオン樹脂に架橋剤としてブロックポリイソシアネート化合物を使用したもの)を硬化塗膜に基づいて膜厚が20μmになるように電着塗装し、170℃で20分加熱して架橋硬化させ、電着塗膜を形成せしめ、被塗物1とした。
実施例1
被塗物1上に、ベース塗料(X−1)「WP−580Z N−9.0」(商品名、関西ペイント社製、ポリエステル樹脂系水性中塗り塗料、得られる塗膜のL*値:90)を回転霧化型のベル型塗装機を用いて、硬化膜厚20μmになるように静電塗装し、3分間放置し、ベース塗膜を形成した。さらに該ベース塗膜上に、前述のように作成した光輝性顔料分散体(Y−1)を、ABB社製ロボットベルを用いて、ブース温度23℃、湿度68%の条件で、乾燥塗膜として、0.2μmとなるように塗装した。3分間放置し、その後、80℃にて3分間プレヒートし、光輝性塗膜を形成した。ついで、この光輝性塗膜上に、クリヤー塗料(Z−1)「KINO6510」(商品名、関西ペイント株式会社製、水酸基/イソシアネート基硬化型アクリル樹脂・ウレタン樹脂系2液型有機溶剤型塗料)をABB社製ロボットベルを用いて、ブース温度23℃、湿度68%の条件で乾燥塗膜として、35μmとなるように塗装しクリヤー塗膜を形成した。塗装後、室温にて7分間放置した後に、熱風循環式乾燥炉内を使用して、140℃で30分間加熱し、複層塗膜を同時に乾燥せしめて試験板とした。
x=sc/sg/S*10000
x:膜厚[μm]
sc:塗着固形分[g]
sg:塗膜比重[g/cm3]
S:塗着固形分の評価面積[cm2]
表2に記載の塗料及び膜厚とする以外は全て実施例1と同様にして試験板を得た。
(X−2):「WP−522H N−8.0」(商品名、関西ペイント社製、ポリエステル樹脂系水性中塗り塗料、得られる塗膜のL*値:80)。
(X−3):「WP−522H N−7.0」(商品名、関西ペイント社製、ポリエステル樹脂系水性中塗り塗料、得られる塗膜のL*値:70)。
上記のようにして得られた各試験板について塗膜を評価し、表2にその結果を示した。
L*15値及びL*110値は、多角度分光光度計MA−68II(商品名、x−rite社製)を用いて測定した分光反射率から計算して得られた数値を使用した。
上記で得られた試験板について、光沢計(micro−TRI−gloss、BYK−Gardner社製)を用いて60°グロス値を測定した。
HG値は、Hi−light Graininess値の略称である。HG値は、塗膜面を微視的に観察した場合におけるミクロ光輝感の尺度の一つであり、ハイライトにおける粒子感を表す指標である。HG値は、次のようにして、算出される。先ず、塗膜面を、光の入射角15度/受光角0度にてCCDカメラで撮影し、得られたデジタル画像データ(2次元の輝度分布データ)を2次元フーリエ変換処理して、パワースペクトル画像を得る。次に、このパワースペクトル画像から、粒子感に対応する空間周波数領域のみを抽出して得られた計測パラメータを、更に0〜100の数値を取り、且つ粒子感との間に直線的な関係が保たれるように変換した値が、HG値である。HG値は、光輝性顔料の粒子感が全くないものを0とし、光輝性顔料の粒子感が最も大きいものを100とした値である。
試験板を40℃の温水に240時間浸漬し、引き上げ、布で水滴・汚れをふきとり、室温23℃で10分以内に、試験板の複層塗膜を素地に達するようにカッターで格子状に切り込み、大きさ2mm×2mmのゴバン目を100個作る。続いて、その表面に粘着セロハンテープを貼着し、そのテープを急激に剥離した後のゴバン目塗膜の残存状態を調べ、下記基準で耐水性を評価した。3点以上で合格である。
5点:ゴバン目塗膜が100個残存し、カッターの切り込みの縁において塗膜の小さなフチカケが生じていない。
4点:ゴバン目塗膜が100個残存するが、カッターの切り込みの縁において塗膜の小さなフチカケが生じている。
3点:ゴバン目塗膜の100個残存するが、ゴバン目塗膜の1マス単位あたり1/2未満がカケている。
2点:ゴバン目塗膜の残存数が90以上99個以下である。
1点:ゴバン目塗膜の残存数が89個以下である。
Claims (8)
- 下記の工程(1)〜(4):
(1)被塗物上に、ベース塗料(X)を塗装してベース塗膜を形成する工程、
(2)工程(1)で形成されるベース塗膜上に、光輝性顔料分散体(Y)を塗装して乾燥膜厚として0.01〜5μmである光輝性塗膜を形成する工程、
(3)工程(2)で形成される光輝性塗膜上に、クリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程、及び
(4)工程(1)〜(3)で形成された未硬化のベース塗膜、未硬化の光輝性塗膜及び未硬化のクリヤー塗膜を加熱することによって、これら3つの塗膜を同時に硬化させる工程、を含む複層塗膜の形成方法であって、
光輝性顔料分散体(Y)が、アルミニウムフレーク顔料(A)、光散乱粒子(B)、水酸基含有アクリル樹脂(C)、及び水を含有する複層塗膜形成方法。 - アルミニウムフレーク顔料(A)が蒸着アルミニウムフレーク顔料である請求項1に記載の複層塗膜形成方法。
- 光散乱粒子(B)が、酸化チタン、マイカ、シリカ、バリタ、ガラスから選ばれる少なくとも1種である請求項1または2に記載の複層塗膜形成方法。
- 光輝性顔料分散体(Y)が、さらに表面調整剤(D)を含有する請求項1ないし3のいずれか1項に記載の複層塗膜形成方法。
- 光輝性顔料分散体(Y)が、さらに粘性調整剤(E)を含有する請求項1ないし4のいずれか1項に記載の複層塗膜形成方法。
- 光輝性顔料分散体(Y)の塗装時の固形分含有率が0.1〜25.0質量%に調整される請求項1ないし5のいずれか1項に記載の複層塗膜形成方法。
- クリヤー塗料(Z)が、水酸基含有樹脂及びポリイソシアネート化合物を含有する2液型クリヤー塗料である請求項1ないし6のいずれか1項に記載の複層塗膜形成方法。
- 得られる複層塗膜に対して45度の角度から照射した光を正反射光に対して15度の角度で受光した分光反射率に基づく明度L*15が100〜150の範囲内であり、得られる複層塗膜に対して45度の角度から照射した光を正反射光に対して110度の角度で受光した分光反射率に基づく明度L*110が50〜90の範囲内である請求項1ないし7のいずれか1項に記載の複層塗膜形成方法。
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