JP6957783B1 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JP6957783B1 JP6957783B1 JP2021537203A JP2021537203A JP6957783B1 JP 6957783 B1 JP6957783 B1 JP 6957783B1 JP 2021537203 A JP2021537203 A JP 2021537203A JP 2021537203 A JP2021537203 A JP 2021537203A JP 6957783 B1 JP6957783 B1 JP 6957783B1
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- coating film
- hydroxyl group
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- colored
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Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
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- C08G18/6216—Polymers of alpha-beta ethylenically unsaturated carboxylic acids or of derivatives thereof
- C08G18/622—Polymers of esters of alpha-beta ethylenically unsaturated carboxylic acids
- C08G18/6225—Polymers of esters of acrylic or methacrylic acid
- C08G18/6229—Polymers of hydroxy groups containing esters of acrylic or methacrylic acid with aliphatic polyalcohols
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- B05D7/572—Three layers or more the last layer being a clear coat all layers being cured or baked together
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- 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
- B05D5/065—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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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D7/57—Three layers or more the last layer being a clear coat
- B05D7/574—Three layers or more the last layer being a clear coat at least some layers being let to dry at least partially before applying the next layer
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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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
- C09D133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/062—Copolymers with monomers not covered by C09D133/06
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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
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
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Abstract
Description
工程(1):被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)を塗装して、着色塗膜を形成する工程、
工程(2):工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15〜80質量部の範囲内である光輝性顔料分散体(X)を塗装して光輝性第1ベース塗膜を形成する工程、
工程(3):工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)を塗装して、透明着色第2ベース塗膜を形成する工程、
工程(4):工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200〜350の範囲内である脂肪族トリイソシアネート化合物(z2−1)を含有するクリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、ならびに、
工程(5):前記工程(2)〜(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる工程、を含む複層塗膜形成方法。
工程(1):被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)を塗装して、着色塗膜を形成する工程、
工程(2):工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15〜80質量部の範囲内である光輝性顔料分散体(X)を塗装して光輝性第1ベース塗膜を形成する工程、
工程(3):工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)を塗装して、透明着色第2ベース塗膜を形成する工程、
工程(4):工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200〜350の範囲内である脂肪族トリイソシアネート化合物(z2−1)を含有するクリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、ならびに、
工程(5):前記工程(2)〜(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる工程、を含む複層塗膜形成方法である。
本発明の複層塗膜形成方法によれば、まず、被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)が塗装され、着色塗膜が形成される。
着色塗料(W)を適用する被塗物は、特に限定されない。該被塗物としては、例えば、乗用車、トラック、オートバイ、バス等の自動車車体の外板部;バンパー等の自動車部品;携帯電話、オーディオ機器等の家庭電気製品の外板部等を挙げることができる。これらのうち、自動車車体の外板部及び自動車部品が好ましい。
着色塗料(W)は、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する。
水酸基含有樹脂(w1)は、1分子中に少なくとも1個の水酸基を有する樹脂である。該水酸基含有樹脂(w1)としては、例えば、水酸基を有する、アクリル樹脂、ポリエステル樹脂、ポリウレタン樹脂、ポリオレフィン樹脂、ポリエーテル樹脂、ポリカーボネート樹脂、エポキシ樹脂、アルキド樹脂等の樹脂が挙げられる。これらはそれぞれ単独でもしくは2種以上組み合わせて使用することができる。
着色塗料(W)は、着色顔料(w2)を含有する。
本発明の複層塗膜形成方法によれば、次に、工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15〜80質量部の範囲内である光輝性顔料分散体(X)が塗装され、光輝性第1ベース塗膜が形成される。
水酸基含有樹脂(x1)は、1分子中に少なくとも1個の水酸基を有する樹脂である。該水酸基含有樹脂(x1)としては、例えば、水酸基を有する、アクリル樹脂、ポリエステル樹脂、ポリウレタン樹脂、ポリオレフィン樹脂、ポリエーテル樹脂、ポリカーボネート樹脂、エポキシ樹脂、アルキド樹脂等の樹脂が挙げられる。これらはそれぞれ単独でもしくは2種以上組み合わせて使用することができる。
水酸基含有アクリル樹脂(x11)は、例えば、水酸基含有重合性不飽和モノマー(a)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(b)を、それ自体既知の方法、例えば、有機溶媒中での溶液重合法、水中でのエマルション重合法等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、イソプロピル(メタ)アクリレート、n−ブチル(メタ)アクリレート、イソブチル(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、トリデシル(メタ)アクリレート、ラウリル(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: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: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: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: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。
(vi) アルコキシシリル基を有する重合性不飽和モノマー:ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリス(2−メトキシエトキシ)シラン、γ−(メタ)アクリロイルオキシプロピルトリメトキシシラン、γ−(メタ)アクリロイルオキシプロピルトリエトキシシラン等。
(vii) フッ素化アルキル基を有する重合性不飽和モノマー: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: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) カルボキシル基含有重合性不飽和モノマー:(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(メタ)アクリレート等。
(xi) 含窒素重合性不飽和モノマー:(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、グリシジル(メタ)アクリレートとアミン化合物との付加物等。
(xii) 重合性不飽和基を1分子中に2個以上有する重合性不飽和モノマー:アリル(メタ)アクリレート、エチレングリコールジ(メタ)アクリレート、1,4−ブタンジオールジ(メタ)アクリレート、ネオペンチルグリコールジ(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。
(xiii) エポキシ基含有重合性不飽和モノマー:グリシジル(メタ)アクリレート、β−メチルグリシジル(メタ)アクリレート、3,4−エポキシシクロヘキシルメチル(メタ)アクリレート、3,4−エポキシシクロヘキシルエチル(メタ)アクリレート、3,4−エポキシシクロヘキシルプロピル(メタ)アクリレート、アリルグリシジルエーテル等。
(xiv) 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。
(xv) スルホン酸基を有する重合性不飽和モノマー: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。
(xvi) リン酸基を有する重合性不飽和モノマー:アシッドホスホオキシエチル(メタ)アクリレート、アシッドホスホオキシプロピル(メタ)アクリレート、アシッドホスホオキシポリ(オキシエチレン)グリコール(メタ)アクリレート、アシッドホスホオキシポリ(オキシプロピレン)グリコール(メタ)アクリレート等。
(xvii) 紫外線吸収性官能基を有する重合性不飽和モノマー: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−[2−(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: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: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:無水マレイン酸、無水イタコン酸、無水シトラコン酸等。
光輝性顔料分散体(X)は、光輝性顔料(x2)を含有する。
本発明の複層塗膜形成方法によれば、次に、工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)が塗装され、透明着色第2ベース塗膜が形成される。
式:ヘイズ値=100*DF/(DF+PT)
水酸基含有樹脂(y1)
水酸基含有樹脂(y1)は、1分子中に少なくとも1個の水酸基を有する樹脂である。該水酸基含有樹脂(y1)としては、例えば、水酸基を有する、アクリル樹脂、ポリエステル樹脂、ポリウレタン樹脂、ポリオレフィン樹脂、ポリエーテル樹脂、ポリカーボネート樹脂、エポキシ樹脂、アルキド樹脂等の樹脂が挙げられる。これらはそれぞれ単独でもしくは2種以上組み合わせて使用することができる。
透明着色第2ベース塗料(Y)は、着色顔料(y2)を含有する。
本発明の複層塗膜形成方法によれば、次に、工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200〜350の範囲内である脂肪族トリイソシアネート化合物(z2−1)を含有するクリヤ塗料(Z)が塗装され、クリヤ塗膜が形成される。
水酸基含有アクリル樹脂(z1)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。
Tg(℃)=Tg(K)−273 (2)
各式中、W1、W2、・・は共重合に使用されたモノマーのそれぞれの質量分率、T1、T2、・・はそれぞれの単量体のホモポリマ−のTg(K)を表わす。なお、T1、T2、・・は、Polymer Hand Book(Second Edition,J.Brandup・E.H.Immergut 編)III−139〜179頁による値である。また、モノマーのホモポリマーのTgが明確でない場合のガラス転移温度(℃)は、静的ガラス転移温度とし、例えば示差走査熱量計「DSC−220U」(セイコーインスツルメント社製)を用いて、試料を測定カップにとり、真空吸引して完全に溶剤を除去した後、3℃/分の昇温速度で−20℃〜+200℃の範囲で熱量変化を測定し、低温側の最初のベースラインの変化点を静的ガラス転移温度とした。
本発明に係るクリヤ塗料(Z)は、ポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200〜350の範囲内である脂肪族トリイソシアネート化合物(z2−1)を含有する。
脂肪族トリイソシアネート化合物(z2−1)は、分子量が200〜350の範囲内であり、イソシアネート基を3個有する脂肪族ポリイソシアネート化合物である。なかでも、形成される複層塗膜の耐水性等の観点から、分子量が200〜300の範囲内であることが好ましく、230〜280の範囲内であることがより好ましい。
脂肪族トリイソシアネート化合物(z2−1)以外のポリイソシアネート化合物としては、例えば、前記脂肪族トリイソシアネート化合物(z2−1)以外の脂肪族ポリイソシアネート化合物、脂環族ポリイソシアネート化合物、芳香脂肪族ポリイソシアネート化合物、芳香族ポリイソシアネート化合物、該ポリイソシアネート化合物の誘導体等を挙げることができる。
本発明の複層塗膜形成方法によれば、次に、前記工程(2)〜(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる。
工程(1):被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)を塗装して、着色塗膜を形成する工程、
工程(2):工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15〜80質量部の範囲内である光輝性顔料分散体(X)を塗装して光輝性第1ベース塗膜を形成する工程、
工程(3):工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)を塗装して、透明着色第2ベース塗膜を形成する工程、
工程(4):工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200〜350の範囲内である脂肪族トリイソシアネート化合物(z2−1)を含有するクリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、ならびに、
工程(5):前記工程(2)〜(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる工程、を含む複層塗膜形成方法。
項21.被塗物には、カチオン電着塗料又はアニオン電着塗料である下塗り塗料が施されている項1〜20のいずれか1項に記載の複層塗膜形成方法。
1.基材の作製
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:関西ペイント株式会社製、エポキシ樹脂ポリアミン系カチオン樹脂に硬化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ることにより、被塗物とした。
水酸基含有樹脂(w1)の製造
水分散性水酸基含有アクリル樹脂(w11−1)の製造
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6%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、5%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%の水分散性水酸基含有アクリル樹脂(w11−1)を得た。得られた水分散性水酸基含有アクリル樹脂の水酸基価は43mgKOH/g、酸価は12mgKOH/gであった。
製造例2
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%の水酸基含有ポリエステル樹脂溶液(w12−1)を得た。得られた水酸基含有ポリエステル樹脂は、水酸基価が128mgKOH/g、酸価が35mgKOH/g、重量平均分子量が13000であった。
製造例3
製造例2で得た水酸基含有ポリエステル樹脂溶液(w12−1)56部(固形分25部)、「タイペーク UT−771」(商品名、ルチル型二酸化チタン顔料、石原産業社製)70部、「カーボン MA−100」(商品名、カーボンブラック顔料、三菱ケミカル社製)0.5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。次いで、得られた混合液を広口ガラスビン中に入れ、分散メジアとして直径約1.3mmφのガラスビーズを加えて密封し、ペイントシェイカーにて30分間分散して、顔料分散液(P−1)を得た。
製造例4
製造例3で得た顔料分散ペースト(P−1)131.5部、製造例1で得た水分散性水酸基含有アクリル樹脂(w11−1)44.4部(固形分20部)、「ユーコートUX−8100」(商品名、ウレタンエマルション、三洋化成工業社製、固形分35%)71.4部(固形分25部)及び「サイメル325」(商品名、メラミン樹脂、オルネクスジャパン社製、固形分80%)37.5部(固形分30部)を均一に混合した。次いで、得られた混合物に、「UH−752」(商品名、ADEKA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添加し、pH8.0、塗料固形分25%、B型粘度計を用いて20℃において回転数6rpmで測定したときの粘度が3000mPa・sの着色塗料(W−1)を得た。
コア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’−1)の製造
製造例5
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145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6%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、5%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、固形分濃度28%のコア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’−1)を得た。得られたコア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’−1)は、水酸基価が25mgKOH/g、酸価が33mgKOH/gであった。
製造例6
攪拌混合容器に、蒸留水50.1部、「レオクリスタ」(商品名、第一工業製薬社製、セルロースナノファイバー、固形分2%)25.5部(固形分0.5部)、「Dynol−604」(商品名、エボニックインダストリーズ社製、アセチレンジオール系表面調整剤、固形分100%)0.3部(固形分0.3部)、「Hydroshine WS−3001」(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)12.1部(固形分1.2部)、製造例5で得たコア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’−1)2.5部(固形分0.7部)、「TINUVIN 479−DW(N)」(商品名、BASF社製、紫外線吸収剤、固形分40%)0.3部(固形分0.1部)、「TINUVIN 123−DW(N)」(商品名、BASF社製、光安定剤、固形分50%)0.2部(固形分0.1部)、2−エチルヘキサノール0.5部、イソプロピルアルコール8.5部を添加して攪拌混合し、光輝性顔料分散体(X−1)を調整した。
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(X−2)〜(X−8)を得た。
「WBC−713T エナメルクリヤ」(商品名、関西ペイント社製、水性ベースコート塗料、透明色)に「GX−3100」(商品名、旭化成社製、アルミニウムフレーク、固形分74%、平均粒子径10μm)を添加し、合計固形分100質量部を基準として、「GX−3100」の含有量が8質量部となるように調整し、撹拌して、光輝性顔料分散体(X−9)とした。
水酸基含有アクリル樹脂溶液(y11−1)の製造
製造例15
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(y11−1)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58000であった。
製造例16
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(y12−1)を得た。得られた水酸基含有ポリエステル樹脂は、酸価が46mgKOH/g、水酸基価が150mgKOH/g、数平均分子量が1400であった。
製造例17
製造例15で得た水酸基含有アクリル樹脂溶液(y11−1)327部(固形分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(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(固形分250部)を、ペイントコンディショナー中に入れ、ガラスビーズ媒体を加えて、室温で1時間混合分散し、固形分44%の顔料分散液(P−2)を得た。
製造例15で得た水酸基含有アクリル樹脂溶液(y11−1)182部(固形分100部)、「CHROMOFINE BLUE 5206M」(商品名、大日精化工業社製、フタロシアニン系青色顔料)100部(固形分100部)及び脱イオン水450部を混合し、2−アミノ−2−メチル−1−プロパノールでpH7.5に調整した後、ペイントシェーカーで2時間分散して固形分27%の顔料分散液(P−3)を得た。
製造例15で得た水酸基含有アクリル樹脂溶液(y11−1)182部(固形分100部)、「MAROON 179 229−6438」(商品名、SUN CHEMICAL CORPORATION社製、有機ペリレン顔料)150部(固形分150部)及び脱イオン水479部を混合し、2−アミノ−2−メチル−1−プロパノールでpH7.5に調整した後、ペイントシェーカーで2時間分散して固形分31%の顔料分散液(P−4)を得た。
製造例15で得た水酸基含有アクリル樹脂溶液(y11−1)182部(固形分100部)、「Irgazin DPP Red BO」(商品名、BASF社製、ジケトピロロピロール顔料)150部(固形分150部)及び脱イオン水479部を混合し、2−アミノ−2−メチル−1−プロパノールでpH7.5に調整した後、ペイントシェーカーで2時間分散して固形分31%の顔料分散液(P−5)を得た。
製造例21
攪拌混合容器に、製造例17で得た顔料分散液(P−2)31.8部(固形分14部)、製造例5で得たコア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’−1)107.1部(固形分30部)、製造例16で得た水酸基含有ポリエステル樹脂溶液(y12−1)32.9部(固形分23部)、「ユーコートUX−310」(商品名、三洋化成社製、ウレタン樹脂水分散体、固形分含有率40%)32.5部(固形分13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、固形分含有率80%)37.5部(固形分30部)となるように添加して攪拌混合し、透明第2ベース塗料(V−1)を調製した。
製造例22
攪拌混合容器に、製造例21で得た透明第2ベース塗料(V−1)を入れ、樹脂固形分100質量部に対して「CHROMOFINE BLUE 5206M」(商品名、大日精化工業社製、フタロシアニン系青色顔料)が5質量部となるように製造例18で得た顔料分散液(P−3)を添加して、攪拌混合し、透明青色第2ベース塗料(Y−1)を調製した。
攪拌混合容器に、製造例21で得た透明第2ベース塗料(V−1)を入れ、樹脂固形分100質量部に対して「MAROON 179 229−6438」(商品名、SUN CHEMICAL CORPORATION社製、有機ペリレン顔料)が5質量部となるように製造例19で得た顔料分散液(P−4)を添加して、攪拌混合し、透明赤色第2ベース塗料(Y−2)を調製した。
製造例24
攪拌混合容器に、製造例21で得た透明第2ベース塗料(V−1)を入れ、樹脂固形分100質量部に対して「Irgazin DPP Red BO」(商品名、BASF社製、ジケトピロロピロール顔料)が5質量部となるように製造例20で得た顔料分散液(P−5)を添加して、攪拌混合し、着色赤色第2ベース塗料(V−2)を調製した。
上記で得られた透明着色第2ベース塗料(Y−1)、(Y−2)及び着色第2ベース塗料(V−2)を用い、塗膜のヘイズ値を、「濁度計COH−300A」(商品名、日本電色工業社製)にて測定した拡散光線透過率(DF)及び平行光線透過率(PT)から、次式によって計算し、評価した。
式:ヘイズ値=100*DF/(DF+PT)
塗膜は、平滑なPTFE板上に、透明着色第2ベース塗料(Y−1)、(Y−2)及び着色第2ベース塗料(V−2)のいずれかをミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として10μmの膜厚となるように塗装し、室温にて3分間放置し、熱風循環式乾燥炉内にて140℃で30分間加熱した後、PTFE板から剥離することにより得た。上記着色第2ベース塗料(V−2)は、得られた塗膜のヘイズ値が30%を超えており、本発明に係る透明着色第2ベース塗料に該当しない。
水酸基含有アクリル樹脂(z1−1)の製造
製造例25
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、「スワゾール1000」(商品名、コスモ石油社製、芳香族系有機溶剤)27部及びプロピレングリコールモノメチルエーテルアセテート5部を仕込み、窒素ガスを吹き込みながら150℃で攪拌し、この中にスチレン20部、2−ヒドロキシプロピルアクリレート32.5部、イソブチルメタクリレート46.8部、アクリル酸0.7部及びジターシャリアミルパーオキサイド(重合開始剤)6.0部からなるモノマー混合物を4時間かけて均一速度で滴下した。その後、150℃で1時間熟成させた後冷却し、さらに酢酸イソブチルを21部加えて希釈し、固形分濃度65質量%の水酸基含有アクリル樹脂(z1−1)溶液を得た。得られた水酸基含有アクリル樹脂(z1−1)の水酸基価は139mgKOH/g、酸価は5.5mgKOH/g、重量平均分子量は5,500、ガラス転移温度38℃であった。
製造例26
製造例25で得た水酸基含有アクリル樹脂(z1−1)溶液108.6部(固形分70.6部)、「BYK−300」(商品名、ビックケミー社製、表面調整剤、有効成分52%)0.4部(固形分0.2部)を均一に混合した主剤と、
硬化剤として、1,8-ジイソシアナト−4−イソシアナトメチルオクタン(固形分100%、NCO含有率50%、分子量251、粘度は23℃において8mPa・s)29.4部(固形分29.4部)とを塗装直前に均一に混合し、さらに、酢酸ブチルを加えて、20℃におけるフォードカップNo.4による粘度が30秒となるように調整してクリヤ塗料(Z−1)を得た。
表3に記載の配合とする以外は全て製造例26と同様にしてクリヤ塗料(Z−2)〜(Z−7)を得た。
(注3)「スミジュールN3300」:商品名、住化コベストロウレタン社製、ヘキサメチレンジイソシアネートのイソシアヌレート体、固形分100%、NCO含有率21.8%、
(注4)「スミジュールN3400」:商品名、住化コベストロウレタン社製、ヘキサメチレンジイソシアネートのウレトジオン体、固形分100%、NCO含有率21.8%。
試験板の作成
実施例1
(着色塗料(W)の塗装)
上記1.で作製した基材上に、上記2.で製造した着色塗料(W−1)をミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として25μmの膜厚となるように塗装し、室温にて15分間放置し、未硬化の着色塗膜を得た。
上記未硬化の着色塗膜上に、上記2.で製造した光輝性顔料分散体(X−1)をミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として1μmの膜厚となるように塗装し、室温にて2分間放置し、未硬化の光輝性第1ベース塗膜を得た。
上記未硬化の光輝性第1ベース塗膜上に、上記2.で製造した透明着色第2ベース塗料(Y−1)をミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として10μmの膜厚となるように塗装し、室温にて3分間放置した後、80℃で3分間プレヒートを行い、未硬化の透明着色第2ベース塗膜を得た。
上記未硬化の透明着色第2ベース塗膜上に、上記2.で製造したクリヤ塗料(Z−1)を、ミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として35μmとなるように塗装し、室温にて7分間放置した後、熱風循環式乾燥炉内にて140℃で30分間加熱し、着色塗膜、光輝性第1ベース塗膜、透明着色第2ベース塗膜及びクリヤ塗膜からなる複層塗膜を同時に乾燥硬化せしめて試験板を作製した。
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4に記載の塗料、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。
上記のようにして得られた各試験板について、以下の方法で塗膜を評価し、表4にその結果を示した。
(1)L*C*h表色系における彩度C*(15°)
各試験板について、「MA−68II」(商品名、x−rite社製)を使用して、L*C*h表色系における彩度C*(15°)を測定した。値が大きいほど彩度が高いことを示す。
各試験板について、「MA−68II」(商品名、x−rite社製)を使用して、IV68を測定した。値が大きいほど、輝度感が良好であることを示す。
各試験板について、「MA−68II」(商品名、x−rite社製)を使用して、SV68を測定した。値が小さいほど、光輝材の配向が良好であることを示す。
上記IV68及びSV68から下記計算式によって求められる値であり、値が大きいほどフリップフロップ性が高いことを表す。
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。A及びBが合格である。
A: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縁欠けが生じていない、
B: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縁欠けが生じており、縁欠けした残存塗膜が10個未満である、
C: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縁欠けが生じており、縁欠けした残存塗膜が10個以上である、
D:ゴバン目塗膜が90〜99個残存する、
E:ゴバン目塗膜の残存数が89個以下である。
促進耐候性試験には、JIS B 7754に規定されたスーパーキセノンウェザオメーター(商品名、スガ試験機社製)を使用し、1時間42分間のキセノンアークランプの照射と18分間の降雨条件における同ランプの照射による2時間を1サイクルとして、4000時間経過後に、上記耐水付着性試験と同様の操作を行った。A、B及びCが合格である。
Claims (13)
- 下記の工程(1)〜(5):
工程(1):被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)を塗装して、着色塗膜を形成する工程、
工程(2):工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15〜80質量部の範囲内である光輝性顔料分散体(X)を塗装して、膜厚が0.02〜7μmの範囲内である光輝性第1ベース塗膜を形成する工程、
工程(3):工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)を塗装して、透明着色第2ベース塗膜を形成する工程、
工程(4):工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200〜350の範囲内である脂肪族トリイソシアネート化合物(z2−1)を含有するクリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、ならびに、
工程(5):前記工程(2)〜(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる工程、を含む複層塗膜形成方法。 - 前記着色塗料(W)が、水性塗料である請求項1に記載の複層塗膜形成方法。
- 前記着色塗料(W)が、さらにメラミン樹脂及び/又はブロック化ポリイソシアネート化合物を含有する請求項1又は2に記載の複層塗膜形成方法。
- 前記光輝性顔料分散体(X)が、水性塗料である請求項1〜3のいずれか1項に記載の複層塗膜形成方法。
- 前記光輝性顔料分散体(X)において、前記水酸基含有樹脂(x1)が、水分散性水酸基含有アクリル樹脂(x111)を含む請求項4に記載の複層塗膜形成方法。
- 前記光輝性顔料(x2)が、蒸着アルミニウムフレーク顔料を含み、該蒸着アルミニウムフレーク顔料の含有量が、前記光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15〜55質量部の範囲内である請求項1〜5のいずれか1項に記載の複層塗膜形成方法。
- 前記光輝性顔料(x2)が、アルミニウムフレーク顔料を含み、該アルミニウムフレーク顔料の含有量が、前記光輝性顔料分散体(X)中の合計固形分100質量部を基準として、45〜80質量部の範囲内である請求項1〜5のいずれか1項に記載の複層塗膜形成方法。
- 前記透明着色第2ベース塗料(Y)が、水性塗料である請求項1〜7のいずれか1項に記載の複層塗膜形成方法。
- 前記透明着色第2ベース塗料(Y)が、さらにメラミン樹脂及び/又はブロック化ポリイソシアネート化合物を含有する請求項1〜8のいずれか1項に記載の複層塗膜形成方法。
- 前記クリヤ塗料(Z)において、ポリイソシアネート化合物(z2)のイソシアネート基の合計molと、水酸基含有アクリル樹脂(z1)の水酸基の合計molとの当量比(NCO/OH)が、1.1〜2.5の範囲内である請求項1〜9のいずれか1項に記載の複層塗膜形成方法。
- 前記透明着色第2ベース塗膜の膜厚が、3〜30μmの範囲内である請求項1〜10のいずれか1項に記載の複層塗膜形成方法。
- 前記工程(2)において、加熱硬化させた前記着色塗膜上に、光輝性顔料分散体(X)を塗装する、請求項1〜11のいずれか1項に記載の複層塗膜形成方法。
- 前記工程(2)において、未硬化の前記着色塗膜上に、光輝性顔料分散体(X)を塗装し、
前記工程(5)において、前記工程(1)〜(4)で形成される着色塗膜、光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を同時に加熱することによって、これら4つの塗膜を含む複層塗膜を一度に硬化させる請求項1〜11のいずれか1項に記載の複層塗膜形成方法。
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JP2018062634A (ja) * | 2016-10-14 | 2018-04-19 | 旭化成株式会社 | ポリイソシアネート組成物、ブロックポリイソシアネート組成物、親水性ポリイソシアネート組成物、塗料組成物、及び塗膜 |
JP2019195791A (ja) * | 2018-05-11 | 2019-11-14 | 関西ペイント株式会社 | 複層塗膜の形成方法 |
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JPWO2021193683A1 (ja) | 2021-09-30 |
EP4129493A1 (en) | 2023-02-08 |
EP4129493A4 (en) | 2024-03-27 |
WO2021193683A1 (ja) | 2021-09-30 |
CN115348902A (zh) | 2022-11-15 |
CA3172575A1 (en) | 2021-09-30 |
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