JP6448026B2 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JP6448026B2 JP6448026B2 JP2014254401A JP2014254401A JP6448026B2 JP 6448026 B2 JP6448026 B2 JP 6448026B2 JP 2014254401 A JP2014254401 A JP 2014254401A JP 2014254401 A JP2014254401 A JP 2014254401A JP 6448026 B2 JP6448026 B2 JP 6448026B2
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Description
工程(1):水性中塗り塗料(X)を塗装して中塗り塗膜を形成する工程、
工程(2):前記工程(1)で形成された中塗り塗膜上に、水性ベース塗料(Y)を塗装してベース塗膜を形成する工程、
工程(3):前記工程(2)で形成されたベース塗膜上に、クリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、及び
工程(4):前記工程(1)〜(3)で形成された中塗り塗膜、ベース塗膜及びクリヤ塗膜を一度に加熱硬化する工程、
を順次行なう複層塗膜形成方法であって、
水性中塗り塗料(X)が、水酸基含有樹脂(A1)、親水基を有する活性メチレンブロックポリイソシアネート化合物(B1)及び顔料(C1)を含有し、
水性ベース塗料(Y)が、水酸基含有樹脂(A2)、親水基を有する活性メチレンブロックポリイソシアネート化合物(B2)及び顔料(C2)を含有し、且つ
クリヤ塗料(Z)が水酸基含有アクリル樹脂(D)及びポリイソシアネート化合物(E)を含有することを特徴とする複層塗膜形成方法に関する。
本工程では、電着塗装された被塗物上に、水性中塗り塗料(X)を塗装して中塗り塗膜を形成する。
上記水性中塗り塗料(X)としては、水酸基含有樹脂(A1)及び親水基を有する活性メチレンブロックポリイソシアネート化合物(B1)を必須の熱硬化性樹脂成分として含有し、さらに顔料(C1)を含有し、必要に応じて、他の樹脂成分、有機溶剤、増粘剤、沈降防止剤、硬化触媒、紫外線吸収剤、光安定剤、表面調整剤、消泡剤、可塑剤などを配合してなる水性液状塗料を使用することができる。なお、本明細書において、水性塗料とは溶媒の主成分が水である塗料である。
水性中塗り塗料(X)は、さらに、顔料(C1)を含有する。顔料(C1)としては、例えば、着色顔料、体質顔料、光輝性顔料などを挙げることができ、それぞれ単独でもしくは2種以上組合せて使用することができる。
工程(1)で水性中塗り塗料(X)により形成された中塗り塗膜上には、次いで、水性ベース塗料(Y)が塗装される。
上記水性ベース塗料(Y)としては、水酸基含有樹脂(A2)及び親水基を有する活性メチレンブロックポリイソシアネート化合物(B2)を必須の熱硬化性樹脂成分として含有し、さらに顔料(C2)を含有し、必要に応じて、他の樹脂成分、有機溶剤、増粘剤、沈降防止剤、硬化触媒、紫外線吸収剤、光安定剤、表面調整剤、消泡剤、可塑剤などを配合してなる水性液状塗料を使用することができる。
工程(2)で水性ベース塗料(Y)により形成されたベース塗膜上には、次いで、クリヤ塗料(Z)が塗装される。クリヤ塗料(Z)は、水酸基含有アクリル樹脂(D)及びポリイソシアネート化合物(E)を含有する。
工程(4)
以上に述べた如くして形成される中塗り塗膜、ベース塗膜及びクリヤ塗膜の3層の塗膜からなる複層塗膜は、通常の塗膜の焼付け手段により、例えば、熱風加熱、赤外線加熱、高周波加熱等により、約80〜約160℃、好ましくは約100〜約140℃の温度で約20〜約40分間程度加熱して同時に硬化させることができる。
製造例1
温度計、サーモスタット、撹拌装置、還流冷却器及び滴下装置を備えた反応容器に、脱イオン水70.7部及び「アクアロンKH−10」(商品名、第一工業製薬社製、乳化剤、有効成分97%)0.52部を仕込み、窒素気流中で撹拌混合し、80℃に昇温した。次いで、下記のモノマー乳化物のうちの全量の1%量及び濃度6%の過硫酸アンモニウム水溶液5部を反応容器内に導入し80℃で15分間保持した。その後、残りのモノマー乳化物を3時間かけて、同温度に保持した反応容器内に滴下し、滴下終了後1時間熟成した後、濃度5%の2−(ジメチルアミノ)エタノール水溶液40部を反応容器に徐々に加えながら30℃まで冷却し、100メッシュのナイロンクロスで濾過しながら排出し、固形分濃度45%の水酸基含有アクリル樹脂エマルション(I−1−1)を得た。得られた水酸基含有アクリル樹脂の酸価は12mgKOH/g、水酸基価は43mgKOH/gであった。
温度計、サーモスタット、撹拌器、還流冷却器及び滴下装置を備えた反応容器に、脱イオン水130部及び「アクアロンKH−10」0.52部を仕込み、窒素気流中で撹拌混合し、80℃に昇温した。次いで下記のモノマー乳化物(1)のうちの全量の1%量及び濃度6%の過硫酸アンモニウム水溶液5.3部を反応容器内に導入し80℃で15分間保持した。その後、残りのモノマー乳化物(1)を3時間かけて、同温度に保持した反応容器内に滴下し、滴下終了後1時間熟成を行なった。その後、下記のモノマー乳化物(2)を1時間かけて滴下し、1時間熟成した後、濃度5%のジメチルエタノールアミン水溶液40部を反応容器に徐々に加えながら30℃まで冷却し、100メッシュのナイロンクロスで濾過しながら排出し、平均粒子径100nm(サブミクロン粒度分布測定装置「COULTER N4型」(商品名、ベックマン・コールター社製)を用いて、脱イオン水で希釈し20℃で測定した)、固形分濃度30%の水酸基含有アクリル樹脂エマルション(I−1−2)を得た。得られた水酸基含有アクリル樹脂は、酸価が33mgKOH/g、水酸基価が25mgKOH/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部と2,2´−アゾビス(2,4−ジメチルバレロニトリル)1部との混合物を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溶液(I−1−3)を得た。得られた水酸基含有アクリル樹脂は酸価が47mgKOH/g、水酸基価が72mgKOH/gであった。
製造例4
温度計、サーモスタット、攪拌装置、還流冷却器及び水分離器を備えた反応容器に、トリメチロールプロパン174部、ネオペンチルグリコール327部、アジピン酸352部、イソフタル酸109部及び1,2−シクロヘキサンジカルボン酸無水物101部を仕込み、160℃から230℃まで3時間かけて昇温させた後、生成した縮合水を水分離器により留去させながら230℃で保持し、酸価が3mgKOH/g以下となるまで反応させた。この反応生成物に、無水トリメリット酸59部を添加し、170℃で30分間付加反応を行った後、50℃以下に冷却し、2−(ジメチルアミノ)エタノールを酸基に対して当量添加し中和してから、脱イオン水を徐々に添加することにより、固形分濃度45%、pH7.2の水酸基含有ポリエステル樹脂溶液(I−2−1)を得た。得られた水酸基含有ポリエステル樹脂は、酸価が35mgKOH/g、水酸基価が128mgKOH/g、重量平均分子量が13,000であった。
温度計、サーモスタット、攪拌装置、還流冷却器及び水分離器を備えた反応容器に、トリメチロールプロパン109部、1,6−ヘキサンジオール141部、ヘキサヒドロ無水フタル酸126部及びアジピン酸120部を仕込み加熱し、160℃から230℃まで3時間かけて昇温させた後、230℃で4時間縮合反応させた。次いで、得られた縮合反応生成物にカルボキシル基を付加するために、さらに無水トリメリット酸38.3部を加え、170℃で30分間反応させた後、1−オクタノール(沸点が195℃のアルコール系溶剤)で希釈し、固形分濃度70%である水酸基含有ポリエステル樹脂溶液(I−2−2)を得た。得られた水酸基含有ポリエステル樹脂は、酸価が46mgKOH/g、水酸基価が150mgKOH/g、重量平均分子量が6,400であった。
製造例6
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管、滴下装置及び除去溶媒簡易トラップを備えた反応容器に、「スミジュールN−3300」」(商品名、住化バイエルウレタン社製、ヘキサメチレンジイソシアネート由来のイソシアヌレート構造含有ポリイソシアネート、固形分約100%、イソシアネート基含有率21.8%)360部、「ユニオックスM−550」(日油社製、ポリエチレングリコールモノメチルエーテル、平均分子量 約550)60部及び2,6−ジ−tert−ブチル−4−メチルフェノール0.2部を仕込み、よく混合して、窒素気流下で130℃で3時間加熱した。次いで、酢酸エチル110部及びマロン酸ジイソプロピル252部を仕込み、窒素気流下で攪拌しながら、ナトリウムメトキシドの28%メタノール溶液3部を加え、65℃で8時間攪拌した。得られた樹脂溶液中のイソシアネート量は0.12モル/Kgであった。これに4−メチル−2−ペンタノール683部を加え、系の温度を80〜85℃に保ちながら減圧条件下で3時間かけて溶剤を留去し、ブロックポリイソシアネート化合物溶液(B−1)1010部を得た。除去溶媒簡易トラップには、イソプロパノールが95部含まれていた。得られたブロックポリイソシアネート化合物溶液(B−1)の固形分濃度は約60%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、滴下装置及び除去溶媒簡易トラップを備えた反応容器に、「スミジュールN−3300」360部、「ユニオックスM−400」(日油社製、ポリエチレングリコールモノメチルエーテル、平均分子量 約400)50部、「PEG#600」(日油社製、ポリエチレングリコール、平均分子量 約600)5部及び2,6−ジ−tert−ブチル−4−メチルフェノール0.2部を仕込み、よく混合して、窒素気流下で130℃で3時間加熱した。次いで、酢酸エチル110部及びマロン酸ジイソプロピル247部を仕込み、窒素気流下で攪拌しながら、ナトリウムメトキシドの28%メタノール溶液3部を加え、65℃で8時間攪拌した。得られた樹脂溶液中のイソシアネート量は0.11モル/Kgであった。これに4−メチル−2−ペンタノール670部を加え、系の温度を80〜85℃に保ちながら減圧条件下で3時間かけて溶剤を留去し、ブロックポリイソシアネート化合物溶液(B−2)1010部を得た。除去溶媒簡易トラップには、イソプロパノールが92部含まれていた。得られたブロックポリイソシアネート化合物溶液(B−2)の固形分濃度は約60%であった。
製造例8
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管、滴下装置及び除去溶媒簡易トラップを備えた反応容器に、「スミジュールN−3300」480部、酢酸エチル150部及びマロン酸ジイソプロピル365部を仕込み、窒素気流下で攪拌しながら、ナトリウムメトキシドの28%メタノール溶液4部を加え、65℃で8時間攪拌した。得られた樹脂溶液中のイソシアネート量は0.07モル/Kgであった。これに4−メチル−2−ペンタノール870部を加え、系の温度を90〜95℃に保ちながら減圧条件下で3時間かけて溶剤を留去し、さらに、4−メチル−2−ペンタノール120部を加えて、ブロックポリイソシアネート化合物溶液(B−3)1400部を得た。除去溶媒簡易トラップには、イソプロパノールが183部含まれていた。得られたブロックポリイソシアネート化合物溶液(B−3)の固形分濃度は約60%であった。
製造例9
製造例3で得た水酸基含有アクリル樹脂溶液(I−1−3)36部(樹脂固形分20部)、「TITANIX JR−806」(テイカ社製、商品名、ルチル型硫酸法酸化チタン)90部、「カーボンMA−100」(三菱化学社製、商品名、カーボンブラック、平均一次粒子径20nm)0.1部及び脱イオン水5部を混合し、2−(ジメチルアミノ)エタノールでpH8.0に調整した後、ペイントシェーカーで30分間分散して顔料分散ペーストを得た。
製造例9において、製造例6で得たブロックポリイソシアネート化合物溶液(B−1)の代わりに製造例7で得たブロックポリイソシアネート化合物溶液(B−2)を用いる以外は製造例9と同様にして水性中塗り塗料(X−2)を得た。
製造例9において、製造例6で得たブロックポリイソシアネート化合物溶液(B−1)の代わりに製造例8で得たブロックポリイソシアネート化合物溶液(B−3)を用いる以外は製造例9と同様にして水性中塗り塗料(X−3)を得た。
製造例3で得た水酸基含有アクリル樹脂溶液(I−1−3)36部(樹脂固形分20部)、「TIPAQUE UT−771」(石原産業社製、商品名、塩素法酸化チタン)90部、「TAROX LL−50」(チタン工業社製、商品名、黄色酸化鉄顔料)0.2部、「カーボンMA−100」(三菱化学社製、商品名、カーボンブラック、平均一次粒子径20nm)0.1部及び脱イオン水5部を混合し、2−(ジメチルアミノ)エタノールでpH8.0に調整した後、ペイントシェーカーで30分間分散して顔料分散ペーストを得た。
攪拌混合容器内において、アルミニウム顔料ペースト「CR−9800」(商品名、旭化成ケミカルズ社製、鱗片状アルミニウム顔料、金属含有量32%、平均一次粒子径7μm)20部、1−オクタノール30部、リン酸基含有樹脂溶液(*1)8部及び2−(ジメチルアミノ)エタノール0.2部を均一に混合して、光輝性顔料濃厚液(P−1)を得た。
製造例14
攪拌混合容器内において、干渉マイカ顔料「Xirallic T60−10WNTクリスタルシルバー」(商品名、メルク社製、酸化チタン被覆マイカ、固形分100%)10部、1−オクタノール35部、リン酸基含有樹脂溶液(*1)8部及び2−(ジメチルアミノ)エタノール0.2部を均一に混合して、光輝性顔料濃厚液(P−2)を得た。
製造例3で得た水酸基含有アクリル樹脂溶液(I−1−3)180部、脱イオン水360部、「サーフィノール104A」(商品名、エアープロダクツ社製消泡剤、固形分:50%)6部及び「バリファインBF−1」(商品名、堺化学工業社製、硫酸バリウム粉末、平均一次粒子径:0.05μm)250部を、ペイントコンディショナー中でガラスビーズ媒体を加えて、室温で1時間混合分散し、硫酸バリウム分散液(P−3)を得た。
製造例16
製造例2で得た水酸基含有アクリル樹脂エマルション(I−1−2)153部(樹脂固形分46部)、製造例5で得た水酸基含有ポリエステル樹脂溶液(I−2−2)29部(樹脂固形分20部)、製造例14で得た光輝性顔料濃厚液(P−2)53部、製造例15で得た硫酸バリウム分散液(P−3)32部、及び製造例6で得たブロックポリイソシアネート化合物溶液(B−1)(固形分60%)50部(樹脂固形分30部)を均一に混合し、更に、「プライマルASE−60」(商品名、ロームアンドハース社製、増粘剤)、2−(ジメチルアミノ)エタノール及び脱イオン水を加えて、pH8.0、塗料固形分25%、20℃におけるフォードカップNo.4による粘度が40秒の水性ベース塗料(Y−1)を得た。
製造例16において、製造例6で得たブロックポリイソシアネート化合物溶液(B−1)の代わりに製造例7で得たブロックポリイソシアネート化合物溶液(B−2)を用いる以外は製造例16と同様にして水性ベース塗料(Y−2)を得た。
製造例16において、製造例6で得たブロックポリイソシアネート化合物溶液(B−1)の代わりに製造例8で得たブロックポリイソシアネート化合物溶液(B−3)を用いる以外は製造例16と同様にして水性ベース塗料(Y−3)を得た。
製造例16において、製造例6で得たブロックポリイソシアネート化合物溶液(B−1)全量を「サイメル327」37部に置き換える以外は製造例16と同様にして水性ベース塗料(Y−4)を得た。
製造例20
撹拌装置、温度計、冷却管、窒素ガス導入口を備えた四ツ口フラスコにエトキシエチルプロピオネート31部を仕込み、窒素ガス通気下で155℃に昇温した。155℃に達した後、窒素ガスの通気を止め、スチレン30部、n−ブチルアクリレート37.5部、2−ヒドロキシプロピルアクリレート30部、アクリル酸2.5部及びジターシャリアミルパーオキサイド(重合開始剤)4部からなる組成配合のモノマー混合物を4時間かけて滴下した。30分後、2,2´−アゾビス(2,4−ジメチルバレロニトリル)(重合開始剤)0.5部をスワゾール1000(炭化水素系溶剤) 3部に溶解させた重合開始剤溶液を1時間かけて滴下した。ついで、155℃で窒素ガスを通気しながら2時間熟成させた後、100℃まで冷却し、酢酸ブチル29部で希釈することにより、固形分60%の水酸基含有アクリル樹脂(D−1)溶液を得た。得られた水酸基含有アクリル樹脂(D−1)は、水酸基価129mgKOH/g、酸価19mgKOH/g、重量平均分子量約12000であった。
製造例20において、スチレン30部、n−ブチルアクリレート37.5部、2−ヒドロキシプロピルアクリレート30部、アクリル酸2.5部及びジターシャリアミルパーオキサイド(重合開始剤)4部からなる組成配合のモノマー混合物を、スチレン30部、n−ブチルアクリレート40.5部、2−ヒドロキシエチルアクリレート27部、アクリル酸2.5部及びジターシャリアミルパーオキサイド(重合開始剤)4部からなる組成配合のモノマー混合物に変更する以外は、製造例20と同様にして製造することにより、固形分60%の水酸基含有アクリル樹脂(D−2)溶液を得た。得られた水酸基含有アクリル樹脂(D−2)は、水酸基価129mgKOH/g、酸価19mgKOH/g、重量平均分子量約12000であった。
製造例22
製造例20で得た水酸基含有アクリル樹脂(D−1)溶液100部(固形分60部)、「デュラネートTLA−100」(商品名、旭化成ケミカルズ社製、ポリイソシアネート化合物)40部、「BYK−300」(商品名、ビックケミー社製、表面調整剤、有効成分52%)0.2部、「TINUVIN900」(商品名、B.A.S.F.社製、ベンゾトリアゾール系紫外線吸収剤、有効成分100%)2.0部及び「TINUVIN292」(商品名、B.A.S.F.社製、ヒンダードアミン系光安定剤、有効成分100%)1.0部を均一に混合し、さらに、「スワゾール1000」(商品名、コスモ石油社製、炭化水素系溶剤)を加えて、20℃におけるフォードカップNo.4による粘度が25秒のクリヤ塗料(Z−1)を得た。
製造例22において、製造例20で得た水酸基含有アクリル樹脂(D−1)溶液の代わりに製造例21で得た水酸基含有アクリル樹脂(D−2)溶液を用いる以外は製造例22と同様にしてクリヤ塗料(Z−2)を得た。
リン酸亜鉛化成処理を施した冷延鋼板に、「エレクロンGT−10」(商品名、関西ペイント社製、カチオン電着塗料)を乾燥膜厚20μmとなるように電着塗装し、170℃で30分間加熱して硬化させて試験用被塗物とした。試験用被塗物1の表面粗度はRaが0.21であった。
実施例1
上記試験用被塗物に、上記製造例9で得た水性中塗り塗料(X−1)を、回転霧化型の静電塗装機を用いて、乾燥膜厚で25μmとなるように静電塗装し、2分間静置後、80℃で3分間プレヒートを行なった。
実施例1において、水性中塗り塗料、水性ベース塗料およびクリヤ塗料を下記表1に示す組合せとする以外は、実施例1と同様にして試験塗板を作製した。
上記実施例1〜10及び比較例1〜3で得られた各試験板について、下記の試験方法により評価を行なった。評価結果を併せて下記表1に示す。
平滑性: Wave Scan DOI(商品名、BYK Gardner社製)によって測定されるWc値を用いて評価した。Wc値は、1〜3mm程度の波長の表面粗度の振幅の指標であり、測定値が小さいほど塗面の平滑性が高いことを示す。
○:キズの大きさが小さく、電着面や素地の鋼板が露出していない
△:キズの大きさは小さいが、電着面や素地の鋼板が露出している
×:キズの大きさはかなり大きく、素地の鋼板も大きく露出している
Claims (4)
- 電着塗装された被塗物に、下記の工程(1)〜(4)、
工程(1):水性中塗り塗料(X)を塗装して中塗り塗膜を形成する工程、
工程(2):前記工程(1)で形成された中塗り塗膜上に、水性ベース塗料(Y)を塗装してベース塗膜を形成する工程、
工程(3):前記工程(2)で形成されたベース塗膜上に、クリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、及び
工程(4):前記工程(1)〜(3)で形成された中塗り塗膜、ベース塗膜及びクリヤ塗膜を一度に加熱硬化する工程、
を順次行なう複層塗膜形成方法であって、
水性中塗り塗料(X)が、水酸基含有樹脂(A1)、親水基を有する活性メチレンブロックポリイソシアネート化合物(B1)及び顔料(C1)を含有し、該化合物(B1)の親水基が数平均分子量550〜1,200のポリエチレングリコールモノメチルエーテルの使用により導入されるものであり、
水性ベース塗料(Y)が、水酸基含有樹脂(A2)、親水基を有する活性メチレンブロックポリイソシアネート化合物(B2)及び顔料(C2)を含有し、該化合物(B2)の親水基が数平均分子量550〜1,200のポリエチレングリコールモノメチルエーテルの使用により導入されるものであり、且つ
クリヤ塗料(Z)が水酸基含有アクリル樹脂(D)及びポリイソシアネート化合物(E)を含有することを特徴とする複層塗膜形成方法。 - 水性中塗り塗料(X)が、顔料(C1)として水性中塗り塗料(X)中の樹脂成分固形分総量を基準として、塩素法酸化チタンを40〜150質量%、及び黄色酸化鉄を0.01〜1質量%含有する請求項1記載の複層塗膜形成方法。
- 水性ベース塗料(Y)が、顔料(C2)として硫酸バリウムを水性ベース塗料(Y)中の樹脂成分固形分総量を基準として2〜30質量%含有する請求項1記載の複層塗膜形成方法。
- 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によって得られる塗装物品。
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