JP6833016B2 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JP6833016B2 JP6833016B2 JP2019509815A JP2019509815A JP6833016B2 JP 6833016 B2 JP6833016 B2 JP 6833016B2 JP 2019509815 A JP2019509815 A JP 2019509815A JP 2019509815 A JP2019509815 A JP 2019509815A JP 6833016 B2 JP6833016 B2 JP 6833016B2
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Classifications
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D7/50—Multilayers
- B05D7/56—Three layers or more
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D5/065—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 having colour interferences or colour shifts or opalescent looking, flip-flop, two tones
- B05D5/066—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 having colour interferences or colour shifts or opalescent looking, flip-flop, two tones achieved by multilayers
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B05D5/068—Metallic effect achieved by multilayers
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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Description
前記第1ベース塗料が、透明塗料もしくは着色塗料であり、
前記第2ベース塗料が、鱗片状光輝性顔料を含み、前記鱗片状光輝性顔料の含有量が前記第2ベース塗料中の樹脂固形分100質量部に対して10〜60質量部の範囲内であり、且つ前記第2ベース塗料中の塗料固形分濃度が第2ベース塗料の全質量に対して5〜20質量%の範囲内であり、且つ前記第2ベース塗料により形成される塗膜の膜厚が硬化塗膜に基づいて1〜8μmの範囲内である、複層塗膜形成方法に関する。
また内板用ベース塗料としては、外板用第2ベース塗料と同様の意匠となる塗料であれば特に制限なく使用でき、同じ塗料を用いても良い。
上記内板用ベース塗料としては、形成される内板塗膜面の仕上がりの観点から、鱗片状光輝性顔料を含有する塗料を好適に使用することができる。該鱗片状光輝性顔料としては、例えば、前記第2ベース塗料の説明において記載した鱗片状光輝性顔料を使用することができる。上記内板用ベース塗料が鱗片状光輝性顔料を含有する場合、該鱗片状光輝性顔料の含有量は、形成される内板塗膜面の仕上がりの観点から、内板用ベース塗料中の樹脂固形分100質量部に対して5〜60質量部の範囲内であることが好ましい。
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、脱イオン水128部、「アデカリアソープSR−1025」(商品名、ADEKA製、乳化剤、有効成分25%)2部を仕込み、窒素気流中で撹拌混合し、80℃に昇温させた。
製造例2
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溶液(b−1)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、重量平均分子量が58,000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、1,2−シクロヘキサンジカルボン酸無水物126部、及びアジピン酸120部を仕込み、160℃から230℃迄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、カルボキシル基を導入するために、無水トリメリット酸38.3部を加えて、170℃で30分間反応させた後、2−エチル−1−ヘキサノールで希釈し、固形分70%の水酸基含有ポリエステル樹脂溶液(b−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、数平均分子量が1,400であった。
製造例4
製造例2で得たアクリル樹脂溶液(b−1)180部(樹脂固形分100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(固形分3部)、及び「バリファインBF−20」(商品名、堺化学工業社製、硫酸バリウム粉末、平均粒子径0.03μm)250部を混合し、ペイントシェーカーで1時間分散して体質顔料分散液(P−1)を得た。
製造例5
製造例2で得たアクリル樹脂溶液(b−1)18部(樹脂固形分10部)、「カーボンMA−100」(商品名、三菱化学社製、カーボンブラック)10部、及び脱イオン水60部を混合し、2−(ジメチルアミノ)エタノールでpH8.2に調整した後、ペイントシェーカーで30分間分散して着色顔料分散液(P−2)を得た。
製造例6
攪拌混合容器内において、「GX−3110」(商品名、旭化成メタルズ株式会社製、アルミニウム顔料ペースト、金属含有量79%)10部、2−エチル−1−ヘキサノール35部、リン酸基含有樹脂溶液(注1)5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、鱗片状光輝性顔料分散液(P−3−1)を得た。
(注1)リン酸基含有樹脂溶液:温度計、サーモスタット、撹拌器、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、メトキシプロパノール27.5部及びイソブタノール27.5部の混合溶剤を入れ、110℃に加熱した。次いで、スチレン25部、n−ブチルメタクリレート27.5部、分岐高級アルキルアクリレート(商品名「イソステアリルアクリレート」大阪有機化学工業株式会社製)20部、4−ヒドロキシブチルアクリレート7.5部、リン酸基含有重合性モノマー(注2)15部、2−メタクリロイルオキシエチルアシッドホスフェート12.5部、イソブタノール10部、及びt−ブチルパーオキシオクタノエート4部からなる混合物121.5部を4時間かけて上記混合溶剤に加え、さらにt−ブチルパーオキシオクタノエート0.5部とイソプロパノール20部からなる混合物を1時間かけて滴下した。その後、1時間攪拌しながら熟成して固形分濃度50%のリン酸基含有樹脂溶液を得た。リン酸基含有樹脂のリン酸基による酸価は83mgKOH/g、水酸基価は29mgKOH/g、重量平均分子量は10,000であった。
(注2)リン酸基含有重合性モノマー:温度計、サーモスタット、撹拌器、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、モノブチルリン酸57.5部及びイソブタノール41部を入れ、90℃に昇温した後、グリシジルメタクリレート42.5部を2時間かけて滴下した。その後、さらに1時間攪拌しながら熟成した後、イソプロパノール59部を加えて、固形分濃度50%のリン酸基含有重合性モノマー溶液を得た。得られたモノマーのリン酸基による酸価は285mgKOH/gであった。
攪拌混合容器内において、「GX−3110」19部、2−エチル−1−ヘキサノール35部、リン酸基含有樹脂溶液(注1)9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、鱗片状光輝性顔料分散液(P−3−2)を得た。
攪拌混合容器内において、「GX−3110」38部、2−エチル−1−ヘキサノール35部、リン酸基含有樹脂溶液(注1)18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、鱗片状光輝性顔料分散液(P−3−3)を得た。
攪拌混合容器内において、「GX−3110」51部、2−エチル−1−ヘキサノール35部、リン酸基含有樹脂溶液(注1)24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、鱗片状光輝性顔料分散液(P−3−4)を得た。
攪拌混合容器内において、「GX−3110」63部、2−エチル−1−ヘキサノール35部、リン酸基含有樹脂溶液(注1)30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、鱗片状光輝性顔料分散液(P−3−5)を得た。
製造例11
製造例1で得たアクリル樹脂エマルション(a)117部(固形分35部)、製造例2で得た水酸基含有アクリル樹脂溶液(b−1)18部(固形分10部)、製造例3で得たポリエステル樹脂溶液(b−2)36部(固形分25部)、及び「サイメル251」(商品名、オルネクスジャパン社製、メラミン樹脂、固形分80%)37.5部(固形分30部)を均一に混合し、更に、「プライマルASE−60」(商品名、ダウケミカル社製、ポリアクリル酸系増粘剤)、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32%、20℃におけるフォードカップNo.4による粘度40秒の水性第1ベース塗料(1−1)を得た。また、上記水性第1ベース塗料(1−1)によって形成される厚さ10μmの硬化塗膜の波長400〜700nmにおける平均光線透過率は100%であった。
製造例11において、配合組成を後記の表1に示すものとする以外は、実施例11と同様にして、pH8.0、塗料固形分32%、20℃におけるフォードカップNo.4による粘度が40秒の水性第1ベース塗料(1−2)〜(1−6)を得た。また、各水性第1ベース塗料によって形成される厚さ10μmの硬化塗膜の波長400〜700nmにおける平均光線透過率を表1に併せて示す。
製造例17
製造例1で得たアクリル樹脂エマルション(a)117部(固形分35部)、製造例2で得た水酸基含有アクリル樹脂溶液(b−1)18部(固形分10部)、製造例3で得たポリエステル樹脂溶液(b−2)36部(固形分25部)、「サイメル251」(商品名、オルネクスジャパン社製、メラミン樹脂、固形分80%)37.5部(固形分30部)、及び製造例9で得た鱗片状光輝性顔料分散液(P−3−4)110部を均一に混合し、更に、「プライマルASE−60」(商品名、ダウケミカル社製、ポリアクリル酸系増粘剤)、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6%、20℃におけるフォードカップNo.4による粘度40秒の水性第2ベース塗料(2−1)を得た。該水性第2ベース塗料(2−1)における鱗片状光輝性顔料の含有量は、該水性第2ベース塗料(2−1)中の樹脂固形分100質量部に対して36質量部であった。
製造例17において、配合組成及び塗料固形分を後記の表2に示すものとする以外は、実施例17と同様にして、pH8.0、20℃におけるフォードカップNo.4による粘度が40秒の水性第2ベース塗料(2−2)〜(2−10)を得た。また、各水性第2ベース塗料における鱗片状光輝性顔料の含有量を、該第2ベース塗料中の樹脂固形分100質量部に対する鱗片状光輝性顔料の質量部として表2に併せて示す。
縦45cm×横30cm×厚さ0.8mmのりん酸亜鉛処理された冷延鋼板に、「エレクロンGT−10」(商品名、関西ペイント社製、熱硬化エポキシ樹脂系カチオン電着塗料)を乾燥膜厚20μmになるように電着塗装し、170℃で30分間加熱して硬化させてから、その上に中塗り塗料「アミラックTP−65−2」(商品名、関西ペイント社製、ポリエステル樹脂・アミノ樹脂系、有機溶剤型中塗り塗料)を乾燥膜厚40μmになるように塗装し、140℃で30分加熱して硬化させて、試験用被塗物とした。
実施例1
上記試験用被塗物の中塗り面の半分(I部位)の上に、製造例18で得た水性第2ベースコート塗料(2−2)を、回転霧化型のベル型塗装機「ABBカートリッジベル塗装機」(ABB社製、商品名)を用いて、乾燥膜厚3μmとなるように静電塗装し、内板用ベース塗膜相当を形成し2分間放置した。次いで上記試験用被塗物の中塗り面の内板用ベース塗膜が形成されていない半分(II部位)に隣接するように、製造例11で得た水性第1ベースコート塗料(1−1)を、回転霧化型のベル型塗装機「ABBカートリッジベル塗装機」(ABB社製、商品名)を用いて、乾燥膜厚12μmとなるように静電塗装し、第1ベース塗膜を形成した。1分間のインターバルをおいた後、該第1ベース塗膜上に、製造例18で得た水性第2ベースコート塗料(2−2)を、乾燥膜厚3μmとなるように塗装し、第2ベース塗膜を形成した。2分間のインターバルをおいた後、80℃で3分間プレヒートして、未硬化のベースコート塗膜を形成し、その上に「KINO6510」(商品名:関西ペイント株式会社、水酸基/イソシアネート基硬化型アクリルウレタン樹脂系2液型有機溶剤型塗料)を乾燥膜厚30μmとなるように塗装し、7分間放置した後、140℃で30分間加熱してこれらの全ての塗膜を同時に硬化させることにより試験板を作製した。
実施例1において、後記の表3に示す組み合わせ及び乾燥膜厚となるように、水性第1ベース塗料(1−2)〜(1−6)のいずれかを塗装して第1ベース塗膜を形成せしめた後、水性第2ベース塗料(2−1)〜(2−10)のいずれかを塗装して第2ベース塗膜を形成する以外は、実施例1と同様に操作して、実施例2〜18及び比較例1〜8の試験板を作製した。
内板塗膜面の仕上り:各試験板(I部位)の外観を目視にて評価した。
○:スプレ−ダストの塗着が認められるものの、目視では殆ど確認できず、ムラなどの違和感は全くない
△:スプレ−ダストの塗着が目視で確認することができ、ムラなどの違和感が少しある
×:スプレ−ダストの塗着が目視で確認することができ、ムラなどの違和感が明確にある。
◎:目視の角度によるメタリック感の変化が非常に大きく、フリップフロップ性に優れ、良好な光輝感を有する
○:目視の角度によるメタリック感の変化が大きく、フリップフロップ性に優れ、良好な光輝感を有する
△:目視の角度によるメタリック感の変化がやや小さく、フリップフロップ性がやや劣り、光輝感はやや劣る
×:目視の角度によるメタリック感の変化が小さく、フリップフロップ性が劣り、光輝感は劣る。
◎:極めて優れた平滑性を有する
○:優れた平滑性を有する
△:平滑性がやや劣る
×:平滑性が劣る。
Claims (7)
- 基材上に第1ベース塗料、第2ベース塗料、及びクリヤー塗料をウェットオンウェットで順次塗装することを含む、複層塗膜を形成する方法であって、
前記第1ベース塗料が、透明塗料もしくは着色塗料であり、
前記第2ベース塗料が、鱗片状光輝性顔料を含み、前記鱗片状光輝性顔料の含有量が前記第2ベース塗料中の樹脂固形分100質量部に対して10〜60質量部の範囲内であり、且つ前記第2ベース塗料中の塗料固形分濃度が前記第2ベース塗料の全質量に対して5〜20質量%の範囲内であり、且つ前記第2ベース塗料により形成される塗膜の膜厚が、硬化塗膜に基づいて1〜8μmの範囲内であり、
前記第1ベース塗料によって形成される塗膜の光線透過率が95〜100%の範囲内である、
複層塗膜形成方法。 - 前記第1ベース塗料及び前記第2ベース塗料が、
アクリル樹脂エマルション(a)、
前記アクリル樹脂エマルション(a)以外の被膜形成性樹脂(b)、及び
硬化剤(c)、
を含有する水性塗料である、請求項1記載の複層塗膜形成方法。 - 前記第2ベース塗料に含まれる前記鱗片状光輝性顔料が、アルミニウムフレーク顔料及び/又は二酸化チタン被覆鱗片状顔料である、請求項1又は2に記載の複層塗膜形成方法。
- 前記第1ベース塗料が、前記第1ベース塗料中の樹脂固形分100質量部に対して着色顔料を0.003〜20質量部含有する、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。
- 前記第1ベース塗料による塗膜の膜厚は、硬化塗膜に基づいて5〜15μmの範囲内である、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。
- 前記基材の表面が電着塗膜層又は中塗り塗膜層である、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。
- 電着塗膜又は中塗り塗膜が形成された自動車車体の内板面上に、内板用ベース塗料を塗装して内板用塗膜を形成した後、前記自動車車体の外板面上に外板用第1ベース塗料、外板用第2ベース塗料、及びクリヤ−塗料を順次塗装して外板用複層塗膜を形成することを含む、複層塗膜形成方法であって、
前記外板用第1ベース塗料が、透明塗料もしくは着色塗料であり、
前記外板用第2ベース塗料が、鱗片状光輝性顔料を含み、前記鱗片状光輝性顔料の含有量が前記外板用第2ベース塗料中の樹脂固形分100質量部に対して10〜60質量部の範囲内であり、且つ前記外板用第2ベース塗料中の塗料固形分濃度が前記外板用第2ベース塗料の全質量に対して5〜20質量%の範囲内であり、且つ前記外板用第2ベース塗料により形成される塗膜の膜厚が硬化塗膜に基づいて1〜8μmの範囲内であり、
前記第1ベース塗料によって形成される塗膜の光線透過率が95〜100%の範囲内である、
複層塗膜形成方法。
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