JPWO2021065401A1 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JPWO2021065401A1 JPWO2021065401A1 JP2020566003A JP2020566003A JPWO2021065401A1 JP WO2021065401 A1 JPWO2021065401 A1 JP WO2021065401A1 JP 2020566003 A JP2020566003 A JP 2020566003A JP 2020566003 A JP2020566003 A JP 2020566003A JP WO2021065401 A1 JPWO2021065401 A1 JP WO2021065401A1
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Abstract
Description
(1)被塗物上に、固形分含有率が30〜62質量%のベース塗料(X)を塗装して硬化膜厚が6〜45μmの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、固形分含有率が0.1〜10質量%の光輝性顔料分散体(Y)を塗装して硬化膜厚として0.1〜5.0μm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、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(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、上記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、
ベース塗料(X)が、ポリウレタン樹脂(A)、炭素数6〜12のアルコール(B)並びにHLBが7〜9の有機溶剤(C)を含有し、
光輝性顔料分散体(Y)が、水、鱗片状光輝性顔料(P)、樹脂エマルション(Q)及びセルロースナノファイバー(R)を含有することを特徴とする複層塗膜形成方法が提供される。
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り、被塗物上に、固形分含有率が30〜62質量%、好ましくは34〜61質量%、さらに好ましくは40〜60質量%のベース塗料(X)を塗装して硬化膜厚が6〜45μm、好ましくは8〜40μm、さらに好ましくは15〜35μmの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。
ベース塗料(X)は、ポリウレタン樹脂(A)、炭素数6〜12のアルコール(B)及びHLBが7〜9の有機溶剤(C)を含有する。
ポリウレタン樹脂(A)は、塗料に通常使用されるものであれば特に制限なく使用することができるが、水に溶解又は分散しているものが好ましく、ポリウレタン樹脂(A)が水に分散している、ポリウレタン樹脂エマルション(A−1)であることがより好ましい。該ポリウレタン樹脂エマルション(A−1)は、アクリル等の樹脂で変性されていてもよい。
HO−R−(O−C(O)−O−R)x−OH
(式中RはC1-12アルキレン基又はC1-3アルキレン−C3-8シクロアルキレン−C1-3アルキレン基を示し、xは分子の繰返し単位の数を示し、通常5〜50の整数である。複数のRは同一でも異なっていても良い)
で示される化合物等を使用することができる。これらは、ポリオールと置換カーボネート(炭酸ジエチル、ジフェニルカーボネート等)とを水酸基が過剰となる条件で反応させるエステル交換法、前記飽和脂肪族ポリオールとホスゲンを反応させるか、または必要に応じて、その後さらに飽和脂肪族ポリオールを反応させる方法等により得ることができる。
アルコール(B)としては、炭素数6〜12の範囲内であれば特に制限なく使用することができるが、金属調光沢に優れる複層塗膜を得る観点から、炭素数7〜11であることがさらに好ましい。炭素数が6よりも小さいと、ベース塗膜の粘度が低くなり、光輝性塗膜と混層し、塗膜外観が悪化する。また、炭素数が12よりも大きいと、ベース塗膜の粘度が高くなり、平滑感が悪化し、塗膜外観が損なわれる。
HLB値が7〜9の有機溶剤(C)としては、HLB値が7〜9の範囲内であれば特に制限なく使用することができるが、金属調光沢に優れる複層塗膜を得る観点から、HLB値が7.1〜8.5の範囲内であることがさらに好ましい。HLB値が7よりも小さいと、ベース塗膜の粘度が高くなり、平滑感が悪化し、塗膜外観が悪化する。また、HLB値が9よりも大きいと、ベース塗膜の極性が高くなり、光輝性塗膜と混層し、塗膜外観が損なわれる。
(式中、MHは親水基部分の分子量、Mは化合物の分子量を意味する)
上記有機溶剤(C)としては、例えば、プロピレングリコールモノメチルエーテル、エチレングリコールモノブチルエーテル、ジプロピレングリコールモノメチルエーテル、ジエチレングリコールモノブチルエーテル、及びトリプロピレングリコールモノメチルエーテルから成る群から選ばれる少なくとも一種である。これらは、単独でもしくは2種以上を組み合わせて使用することができる。該有機溶剤(C)としては、なかでも特に、ジプロピレングリコールモノメチルエーテル、ジエチレングリコールモノブチルエーテル、トリプロピレングリコールモノメチルエーテルであることが好ましく、ジプロピレングリコールモノメチルエーテルであることがさらに好ましい。
ベース塗料(X)は、金属調光沢に優れる複層塗膜を得る観点から、前記成分(A)〜(C)に加えてさらに数平均分子量が1500〜10000、好ましくは1800〜8000、さらに好ましくは2000〜6000のポリエステル樹脂(D)を含有することが好ましい。
(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−カルボキシエチルアクリレート等。
(xi)水酸基含有重合性不飽和モノマー:2−ヒドロキシエチル(メタ)アクリレート、2−ヒドロキシプロピル(メタ)アクリレート、3−ヒドロキシプロピル(メタ)アクリレート、4−ヒドロキシブチル(メタ)アクリレート等の(メタ)アクリル酸と炭素数2〜8の2価アルコールとのモノエステル化物;(メタ)アクリル酸と炭素数2〜8の2価アルコールとのモノエステル化物のε−カプロラクトン変性体;N−ヒドロキシメチル(メタ)アクリルアミド;アリルアルコール、さらに、分子末端が水酸基であるポリオキシエチレン鎖を有する(メタ)アクリレート等。
(xii)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。
(xiii)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、1,6−ヘキサンジオールジ(メタ)アクリレート等。
(xiv)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。
(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: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)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。
(xviii)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' −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。
(xix)紫外線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。
(xx)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。
(x)カルボキシル基含有重合性不飽和モノマーを好ましくは20〜50質量%、より好ましくは25〜45質量%、特に好ましくは30〜40質量%、
(v)芳香環含有重合性不飽和モノマーを好ましくは10〜60質量%、より好ましくは15〜55質量%、特に好ましくは20〜50質量%、
である。
ベース塗料(X)は、金属調光沢に優れる複層塗膜を得る観点から、前記成分(A)〜(C)に加えてさらにノニオン性親水基を有するブロックポリイソシアネート化合物(E)を含有することが好ましい。
1分子中に2以上のイソシアネート基を有するポリイソシアネート化合物(e1)は、1分子中に2以上のイソシアネート基を有する化合物であれば特に制限されず、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、及びそれらの誘導体、並びにそれらの任意の組み合わせ等が挙げられる。
ノニオン性親水基を有する活性水素含有化合物(e2)としては、例えば、ポリオキシアルキレン基を有する活性水素含有化合物が挙げられる。上記ポリオキシアルキレン基としては、例えば、ポリオキシエチレン基、ポリオキシプロピレン基、並びにそれらの任意の組み合わせ、例えば、ポリオキシエチレン(オキシプロピレン)基が挙げられる。なかでも、ブロックポリイソシアネート化合物(E)の貯蔵安定性の観点から、活性水素含有化合物(e2)は、ポリオキシエチレン基を有する活性水素含有化合物(e21)であることが好ましい。
ブロック剤(e3)としては、例えば、フェノール系、アルコール系、活性メチレン系、メルカプタン系、酸アミド系、酸イミド系、イミダゾール系、尿素系、オキシム系、カルバミン酸系、アミン系、イミン系、並びにそれらの任意の組み合わせが挙げられる。ブロック剤(e3)の具体例を、下記に示す。
フェノール、クレゾール、エチルフェノール、ブチルフェノール等、
(2)アルコール系;
エチレングリコール、ベンジルアルコール、メタノール、エタノール等、
(3)活性メチレン系;
マロン酸ジエステル、アセト酢酸エステル、イソブチリル酢酸エステル等、
(4)メルカプタン系;
ブチルメルカプタン、ドデシルメルカプタン等、
(5)酸アミド系;
アセトアニリド、酢酸アミド、ε−カプロラクタム、δ−バレロラクタム、γ−ブチロラクタム等、
(6)酸イミド系;
コハク酸イミド、マレイン酸イミド等、
(7)イミダゾール系;
イミダゾール、2−メチルイミダゾール等、
(8)尿素系;
尿素、チオ尿素、エチレン尿素等、
(9)オキシム系;
ホルムアルドオキシム、アセトアルドオキシム、メチルエチルケトオキシム、シクロヘキサノンオキシム等、
(10)カルバミン酸系;
N−フェニルカルバミン酸フェニル等
(11)アミン系;
ジフェニルアミン、アニリン、カルバゾール等、
(12)イミン系;エチレンイミン、ポリエチレンイミン等。
[ノニオン性親水基を有するブロックポリイソシアネート化合物(E11)]
ノニオン性親水基を有するブロックポリイソシアネート化合物(E11)(以下、「ブロックポリイソシアネート化合物(E11)」と称する場合がある)は、下記一般式(IV):
で示されるブロックイソシアネート基、及びノニオン性親水基を有する。
[ノニオン性親水基を有するブロックポリイソシアネート化合物(E12)]
ノニオン性親水基を有するブロックポリイソシアネート化合物(E12)(以下、「ブロックポリイソシアネート化合物(E12)」と称する場合がある)は、下記一般式(V):
で示されるブロックイソシアネート基、及びノニオン性親水基を有する。
ノニオン性親水基を有するブロックポリイソシアネート化合物(E2)(以下、「ブロックポリイソシアネート化合物(E2)」と称する場合がある)は、例えば、ブロックポリイソシアネート化合物(E)と、下記一般式(VI):
で示される2級アルコール(e4)とを反応させることによって得られる。
2級アルコール(e4)は、一般式(VI)で示される化合物であり、ブロックポリイソシアネート化合物(E)と、2級アルコール(e4)との反応性を高める観点から、R2はメチル基であることが好ましい。R3、R4及びR5は、それぞれ炭素数が多いと、得られるノニオン性親水基を有するブロックポリイソシアネート化合物(E2)の極性が低下し、他の塗料成分との相溶性が低下する場合があるため、R3は炭素数1〜3のアルキレン基であることが好ましく、そしてR4及びR5はメチル基であることが好ましい。
ノニオン性親水基を有するブロックポリイソシアネート化合物(E21)(以下、「ブロックポリイソシアネート化合物(E21)」と称する場合がある)は、例えば、下記一般式(IV):
で示されるブロックイソシアネート基及びノニオン性親水基を有するブロックポリイソシアネート化合物(E11)と、2級アルコール(e4)とを反応させることによって得られる。
で示される基に置換される。
で示されるブロックイソシアネート基、及び/又は下記一般式(II):
で示されるブロックイソシアネート基を有する。
[ノニオン性親水基を有するブロックポリイソシアネート化合物(E22)]
ノニオン性親水基を有するブロックポリイソシアネート化合物(E22)(以下、「ブロックポリイソシアネート化合物(E22)」と称する場合がある)は、例えば、一般式(V):
で示されるブロックイソシアネート基及びノニオン性親水基を有するブロックポリイソシアネート化合物(E12)と、2級アルコール(e4)とを反応させることによって得られる。
で示される基に置換される。
で示されるブロックイソシアネート基を有する。
工程(2)は、工程(1)で形成されるベース塗膜上に、固形分含有率が0.1〜10質量%、好ましくは0.5〜8質量%、さらに好ましくは1〜6質量%の光輝性顔料分散体(Y)を塗装して硬化膜厚として0.1〜5.0μm、好ましくは0.2〜3.0μm、さらに好ましくは0.3〜2.5μmの光輝性塗膜を形成する工程である。
光輝性顔料分散体(Y)は、水、鱗片状光輝性顔料(P)、樹脂エマルション(Q)及びセルロースナノファイバー(R)を含有する。
鱗片状光輝性顔料(P)としては、例えば、蒸着金属フレーク顔料、アルミニウムフレーク顔料、光干渉性顔料等を挙げることができる。これらの顔料は得られる塗膜に求められる質感によって1種又は2種以上を適宜選択して用いることができる。金属調光沢に優れた塗膜を得る観点では、蒸着金属フレーク顔料、アルミニウムフレーク顔料が好適である。一方、真珠調光沢に優れた塗膜を得る観点では、光干渉性顔料が好適である。
樹脂エマルション(Q)としては、樹脂が水性溶媒に分散されているもので、塗膜形成能を有するものであれば特に制限はなく、従来公知のものを制限なく使用することができ、その具体例としては、アクリル樹脂エマルション、アクリルシリコン樹脂エマルション、ウレタン樹脂エマルション、アクリルウレタン樹脂エマルション、ポリエステル樹脂エマルション、アルキド樹脂エマルション、オレフィン樹脂エマルション、フッ素樹脂エマルション、エポキシ樹脂エマルション、メラミン樹脂エマルション、酢酸ビニルエマルション、シリコーン樹脂エマルション、酢酸ビニル・ベオバ樹脂エマルションなどが挙げられるが、これらに限定されるわけではない。該樹脂エマルションは変性されていてもよい。これらは単独で使用しても2種以上を併用しても良い。これらの中で、金属調光沢に優れる複層塗膜を得る観点から、アクリル樹脂エマルション、ウレタン樹脂エマルション、アクリルウレタン樹脂エマルションが好ましく、特にアクリル樹脂エマルションがよい。さらに水酸基含有アクリル樹脂エマルション、水酸基含有ウレタン樹脂エマルション及び水酸基含有アクリルウレタン樹脂エマルションが好ましい。
セルロースナノファイバー(R)は、セルロースナノフィブリル、フィブリレーティドセルロース、ナノセルロースクリスタルと称されることもある。
光輝性顔料分散体(Y)は、金属調光沢に優れる複層塗膜を得る観点から、さらに湿潤剤(S)を含有することが好ましい。
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。光輝性顔料分散体(Y)は、金属調光沢に優れる複層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、0.1〜10質量%、好ましくは0.5〜8質量%、さらに好ましくは1〜6質量%に調整しておく。光輝性顔料分散体(Y)の塗装時の固形分含有率が0.1質量%より低いと、均一膜厚での塗装が困難となり、10質量%より高いと、形成された塗膜の金属調光沢が劣る。
工程(3)は、工程(2)で形成される光輝性塗膜上に、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(Z)を塗装してクリヤー塗膜を形成する工程である。
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。
IPSL≧0.32の場合、HG=500・IPSL−142.5
0.32>IPSL≧0.15の場合、HG=102.9・IPSL−15.4
0.15>IPSLの場合、HG=0
ここで、IPSL(Integration of Power Spectrum of Low Frequency)は次式によって求められる。
測定方法の詳細については、“塗料の研究”(関西ペイント技報)、No.138、2002年8月:p.8−p.24及び“塗料の研究”(関西ペイント技報)、No.132、1999年4月:p.22−p.35に記載している。粒子感のHG値が低いほど、塗膜の表面に粒子感が少なくなる。
項1.下記の工程(1)〜(4):
(1)被塗物上に、固形分含有率が30〜62質量%のベース塗料(X)を塗装して硬化膜厚が6〜45μmの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、固形分含有率が0.1〜10質量%の光輝性顔料分散体(Y)を塗装して硬化膜厚として0.1〜5.0μm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、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(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、上記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、
ベース塗料(X)が、ポリウレタン樹脂(A)、炭素数6〜12のアルコール(B)並びにHLBが7〜9の有機溶剤(C)を含有し、
光輝性顔料分散体(Y)が、水、鱗片状光輝性顔料(P)、樹脂エマルション(Q)及びセルロースナノファイバー(R)を含有することを特徴とする複層塗膜形成方法。
項2.前記アルコール(B)と前記有機溶剤(C)の含有量が、(B)/(C)の質量比で0.7〜3.0である上記項1に記載の複層塗膜形成方法。
項3.前記アルコール(B)が直鎖又は分岐鎖の脂肪族アルコールである項1又は2に記載の複層塗膜形成方法。
項4.ベース塗料(X)中の樹脂100質量部(固形分)を基準として、前記アルコール(B)を好ましくは5〜45質量部、より好ましくは10〜40質量部、さらに好ましくは15〜30質量部含有する項1〜3のいずれか1項に記載の複層塗膜形成方法。
項5.前記有機溶剤(C)が、プロピレングリコールモノメチルエーテル、エチレングリコールモノブチルエーテル、ジプロピレングリコールモノメチルエーテル、ジエチレングリコールモノブチルエーテル、及びトリプロピレングリコールモノメチルエーテルから成る群から選ばれる少なくとも一種である上記項1〜4のいずれか1項に記載の複層塗膜形成方法。
項6.ベース塗料(X)中の樹脂100質量部(固形分)を基準として、前記有機溶剤(C)を好ましくは3〜22質量部、より好ましくは5〜20質量部、さらに好ましくは8〜18質量部含有する項1〜5のいずれか1項に記載の複層塗膜形成方法。
項7.ベース塗料(X)が、さらに数平均分子量が1500〜10000のポリエステル樹脂(D)を含有する上記項1〜6のいずれか1項に記載の複層塗膜形成方法。
項8.ベース塗料(X)が、さらにノニオン性親水基を有するブロックポリイソシアネート化合物(E)を含有する上記項1〜7のいずれか1項に記載の複層塗膜形成方法。
項9.ノニオン性親水基を有するブロックポリイソシアネート化合物(E)がブロックポリイソシアネート化合物(E11)又はブロックポリイソシアネート化合物(E12)を含む項8に記載の複層塗膜形成方法。
項10.ノニオン性親水基を有するブロックポリイソシアネート化合物(E)がブロックポリイソシアネート化合物(E21)又はブロックポリイソシアネート化合物(E22)を含む項8に記載の複層塗膜形成方法。
項11.ノニオン性親水基を有するブロックポリイソシアネート化合物(E)を、ベース塗料(X)中の樹脂100質量部(固形分)を基準として、好ましくは2〜30質量部、より好ましくは4〜20質量部、さらに好ましくは7〜15質量部含有する項8〜10のいずれか1項に記載の複層塗膜形成方法。
項12.鱗片状光輝性顔料(P)が、蒸着金属フレーク顔料、アルミニウムフレーク顔料、及び光干渉性顔料のうちの1種又は2種を含む項1〜11のいずれか1項に記載の複層塗膜形成方法。
項13.樹脂エマルション(Q)がアクリル樹脂エマルション、ウレタン樹脂エマルション、又はアクリルウレタン樹脂エマルションを含む項1〜12のいずれか1項に記載の複層塗膜形成方法。
項14.光輝性顔料分散体(Y)がさらに湿潤剤(S)を含有する項1〜13のいずれか1項に記載の複層塗膜形成方法。
項15.湿潤剤(S)がアセチレンジオール系の湿潤剤を含む項14に記載の複層塗膜形成方法。
項16.前記アセチレンジオール系の湿潤剤がアセチレンジオールのエチレンオキサイド付加物である項15に記載の複層塗膜形成方法。
製造例1
温度計、サーモスタット、撹拌装置、還流冷却器及び水分離器を備えた反応容器に30.1部の水添MDIとメチルエチルケトキシム1.5部を仕込み80℃に加温し1時間攪拌して、イソシアネート反応物を得た。別容器に「UM90(1/1)」(商品名、ジオール成分が1,4−シクロヘキサンジメタノール及び1,6−ヘキサンジオールであり、1,4−シクロヘキサンジメタノールの質量/1,6−ヘキサンジオールの質量=1/1であるポリカーボネートジオール、宇部興産社製)64.1部、ジメチロールプロピオン酸4.2部を仕込み、内容物を撹拌しながら80℃まで加熱した。80℃に達した後、前記イソシアネート反応物を1時間かけて滴下した。その後、N−メチルピロリドン29.9部を添加した後、更に80℃で熟成し、ウレタン化反応を行なった。イソシアネート価が3.0以下になったら加熱をやめ、70℃でトリエチルアミン2.75部を加えた。次いで50℃を維持した状態で脱イオン水200部を1時間かけて滴下し、水分散を行うことによりウレタン樹脂エマルション(A−1)を得た。得られたウレタン樹脂エマルション(A−1)は、固形分30%、酸価19.9mgKOH/g、重量平均分子量11300で、動的光散乱法により測定した粒子径は77nmであった。
温度計、サーモスタット、攪拌装置及び還流冷却器を備えた反応容器に、ジエチレングリコールモノエチルエーテルアセテートを30部仕込み、窒素ガス通気下で145℃に昇温した後、窒素ガスの通気を止め、1段目(疎水鎖成分)として、n−ブチルアクリレート23.8部、n−ブチルメタクリレート14部、スチレン7部、2−ヒドロキシエチルメタクリレート24.5部、及びグリシジルメタクリレート0.7部、ならびに開始剤ジ−t−ブチルパーオキサイド3.0部の混合物を4時間かけて滴下した。その後、30分間、同温度で保持した。
グラフト率(%)=(1−(2段目反応完了後のエポキシ価/1段目反応完了後のエポキシ価))×100
その後、ジエチレングリコールモノエチルエーテルアセテート51部を添加して、固形分55%のグラフトアクリル樹脂の溶液を得た。得られたグラフトアクリル樹脂の重量平均分子量は15000であった。
得られたウレタン樹脂成分の重量平均分子量は20000であった。
製造例3
温度計、サーモスタット、攪拌機、加熱装置及び精留塔を具備した反応容器に、ヘキサヒドロ無水フタル酸92.9部、アジピン酸52.6部、1,6−ヘキサンジオール83.1部、ネオペンチルグリコール10.5部、2−ブチル−2−エチル−1,3−プロパンジオール32部、無水マレイン酸1.0部及びジブチル錫オキサイド0.12部を添加し、反応容器を、攪拌しながら160℃まで昇温した。次いで、内容物を160℃から240℃まで4時間かけて徐々に昇温し、精留塔を通して生成した縮合水を留去した。
反応容器を130℃まで冷却した後、反応容器に、スチレン8.7部、アクリル酸12.2部、アクリル酸−2−エチルヘキシル22.7部及びtert−ブチルパーオキシ−2−エチルヘキサノエート2.2部の混合物を、2時間かけて滴下した。
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、1,6−ヘキサンジオール82.6部、ネオペンチルグリコール12.5部、2−ブチル−2−エチル−1,3−プロパンジオール38.0部、ヘキサヒドロ無水フタル酸38.2部、アジピン酸99.3部及びジブチル錫オキサイド0.12部を添加し、内容物を、攪拌しながら160℃まで昇温させた。次いで、内容物を160℃から240℃まで4時間かけて徐々に昇温した後、内容物を240℃で4時間縮合反応させ、縮合反応生成物を得た。
製造例5
温度計、サーモスタット、攪拌装置、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%)1610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)275部及び2,6−ジ−tert−ブチル−4−メチルフェノール0.9部を添加し、内容物を混合し、そして反応容器を窒素気流下で130℃で3時間加熱した。
製造例6
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器に脱イオン水128部、及び「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7
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%の水溶性アクリル樹脂(1)溶液を得た。得られた水溶性アクリル樹脂(1)は酸価が51mgKOH/g、水酸基価が52mgKOH/gであった。
製造例8
ポリウレタン樹脂(A−1)66.7部(固形分20部)、n−オクタノール18部、n−ブタノール1部、ジプロピレングリコールモノメチルエーテル11部、ポリエステル樹脂(D−1)57.1部(固形分20部)、ポリエステル樹脂(1)14.3部(固形分10部)、ブロックポリイソシアネート(E−1)16.7部(固形分10部)、アクリルエマルション(1)66.7部(固形分20部)、「サイメル325」(商品名、日本サイテックインダストリーズ社製、メラミン樹脂、固形分80%)25部(固形分20部)、「JR−903」(商品名、ルチル型酸化チタン顔料、テイカ社製)120部、「Raven5000」(商品名、コロンビアンカーボン社製、カーボンブラック顔料)1.5部を混合容器に入れ、内容物を均一に混合し、「プライマル ASE−60」(商品名、ロームアンドハース社製、増粘剤、固形分28%)、2−(ジメチルアミノ)エタノール及び蒸留水により、pH、固形分濃度及び粘度を調整して、pH8.0、50%の固形分濃度、20℃におけるフォードカップNo.4による粘度40秒のべース塗料(X−1)を得た。
表1に記載の配合とする以外は全て製造例8と同様にしてベース塗料(X−2)〜(X−18)を得た。
「デュラネートSBN−70D」商品名、旭化成ケミカルズ社製、ピラゾールブロックポリイソシアネート化合物、固形分70%。
製造例26
攪拌混合容器に、蒸留水56.16部、「サーフィノール104A」(商品名、アセチレンジオール系湿潤剤、エアープロダクツ社製、固形分50%)1.34部(固形分0.67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)2.5部(固形分0.25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%)34部(固形分0.68部)、製造例6で製造したアクリルエマルション(1)6部(固形分1.8部)を添加して攪拌混合し、光輝性顔料分散体(Y−1)を調整した。
表2に記載の配合とする以外は全て製造例26と同様にして光輝性顔料分散体(Y−2)〜(Y−6)を得た。
「アルペースト EMR−B6360」(商品名、東洋アルミ社製、固形分48%、ノンリーフィングアルミニウムフレーク、平均粒子径D50:10.3μm、厚さ:0.19μm、表面がシリカ処理されている)、
「Xirallic T61−10 Micro Silver」(商品名、酸化チタン被覆アルミナフレーク顔料、メルク社製、一次平均粒子径:約12μm、平均厚さ:約0.3μm)、
「プライマル ASE−60」(商品名、ロームアンドハース社製、増粘剤、固形分28%)。
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。
被塗物1上に中塗り塗料「WP−522H N−5.0」(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)を硬化塗膜に基づいて膜厚が25μmになるように静電塗装し、室温にて6分間放置したものを被塗物2とした。
実施例1
被塗物1上に、ベース塗料(X−1)を回転霧化型のベル型塗装機を用いて、硬化膜厚30μm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、0.4μm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3に記載の被塗物、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。
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3にその結果を示した。
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値の式については既に記載したとおりである。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。
塗膜外観は、以下の基準に従って目視評価した。
S:ツヤ感が良好、A;ツヤ感がやや劣る、B;ツヤ感が劣る。
Claims (6)
- 下記の工程(1)〜(4):
(1)被塗物上に、固形分含有率が30〜62質量%のベース塗料(X)を塗装して硬化膜厚が6〜45μmの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、固形分含有率が0.1〜10質量%の光輝性顔料分散体(Y)を塗装して硬化膜厚として0.1〜5.0μm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、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(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、上記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、
ベース塗料(X)が、ポリウレタン樹脂(A)、炭素数6〜12のアルコール(B)並びにHLBが7〜9の有機溶剤(C)を含有し、
光輝性顔料分散体(Y)が、水、鱗片状光輝性顔料(P)、樹脂エマルション(Q)及びセルロースナノファイバー(R)を含有することを特徴とする複層塗膜形成方法。 - 前記アルコール(B)と前記有機溶剤(C)の含有量が、(B)/(C)の質量比で0.7〜3.0である請求項1に記載の複層塗膜形成方法。
- 前記有機溶剤(C)が、プロピレングリコールモノメチルエーテル、エチレングリコールモノブチルエーテル、ジプロピレングリコールモノメチルエーテル、ジエチレングリコールモノブチルエーテル、及びトリプロピレングリコールモノメチルエーテルから成る群から選ばれる少なくとも一種である請求項1又は2に記載の複層塗膜形成方法。
- ベース塗料(X)が、さらに数平均分子量が1500〜10000のポリエステル樹脂(D)を含有する請求項1〜3のいずれか1項に記載の複層塗膜形成方法。
- ベース塗料(X)が、さらにノニオン性親水基を有するブロックポリイソシアネート化合物(E)を含有する請求項1〜4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)がさらに湿潤剤(S)を含有する請求項1〜5のいずれか1項に記載の複層塗膜形成方法。
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CN105462466B (zh) * | 2014-09-26 | 2019-04-26 | 立邦涂料(中国)有限公司 | 一种高针孔极限的水性-基涂料组合物 |
CA2974183C (en) * | 2015-01-29 | 2020-09-22 | Kansai Paint Co., Ltd. | Method for forming multilayer coating film |
EP3412445B1 (en) * | 2016-02-05 | 2022-11-23 | Kansai Paint Co., Ltd | Multi-layered coating film and multi-layered coating film formation method |
EP3486291B1 (en) * | 2016-07-13 | 2022-12-07 | Kansai Paint Co., Ltd | Effect pigment dispersion |
JP6781015B2 (ja) * | 2016-11-11 | 2020-11-04 | 関西ペイント株式会社 | 複層塗膜形成方法 |
EP3542910A4 (en) * | 2016-11-18 | 2020-07-01 | Kansai Paint Co., Ltd | MULTI-LAYER COATING FILM FORMATION METHOD |
CA3044199C (en) * | 2016-11-18 | 2022-04-12 | Kansai Paint Co., Ltd. | Method for forming multilayer coating film |
CN110461955A (zh) * | 2017-03-31 | 2019-11-15 | 巴斯夫涂料有限公司 | 形成多层涂膜的方法 |
CN111615431B (zh) * | 2018-01-15 | 2022-05-06 | 关西涂料株式会社 | 多层涂膜形成方法 |
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