JP6680448B1 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JP6680448B1 JP6680448B1 JP2018231575A JP2018231575A JP6680448B1 JP 6680448 B1 JP6680448 B1 JP 6680448B1 JP 2018231575 A JP2018231575 A JP 2018231575A JP 2018231575 A JP2018231575 A JP 2018231575A JP 6680448 B1 JP6680448 B1 JP 6680448B1
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- coating film
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- resin
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Landscapes
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Abstract
Description
1.プラスチック基材上に複層塗膜を形成する塗膜形成方法であって、
工程(1):プラスチック基材上にエポキシ樹脂及びアミン化合物を含有する下塗塗料(X)を塗装して、下塗塗膜を形成する工程、
工程(2):該下塗塗膜上にポリビニルブチラール樹脂及びフェノール樹脂を含有する中塗塗料(Y)を塗装して、中塗塗膜を形成する工程、ならびに
工程(3):該中塗塗膜上にウレタンエラストマー及び芳香族ジアミン化合物を含有する上塗塗料(Z)を塗装して、上塗塗膜を形成する工程、を含む複層塗膜形成方法、
2.中塗塗料(Y)のポリビニルブチラール樹脂の重量平均分子量が10000〜100000の範囲内である上記項1に記載の複層塗膜形成方法、
3.上塗塗料(Z)のウレタンエラストマーが、オキシム化合物でブロックされた、末端イソシアネート基含有ブロック化ウレタンエラストマーである上記項1又は2に記載の複層塗膜形成方法、
4.上塗塗料(Z)の芳香族ジアミン化合物が、電子供与性基含有芳香族ジアミン化合物である上記項1〜3のいずれか一項に記載の複層塗膜形成方法、
5.上塗塗料(Z)が、さらに、アマイド化合物を含有する上記項1〜4のいずれか一項に記載の複層塗膜形成方法、
6.上記項1〜5のいずれか一項に記載の複層塗膜形成方法により塗装されたプラスチック基材物品、
を提供するものである。
プラスチック基材上に複層塗膜を形成する塗膜形成方法であって、
工程(1):プラスチック基材上にエポキシ樹脂及びアミン化合物を含有する下塗塗料(X)を塗装して、下塗塗膜を形成する工程、
工程(2):該下塗塗膜上にポリビニルブチラール樹脂及びフェノール樹脂を含有する中塗塗料(Y)を塗装して、中塗塗膜を形成する工程、ならびに
工程(3):該中塗塗膜上にウレタンエラストマー及び芳香族ジアミン化合物を含有する上塗塗料(Z)を塗装して、上塗塗膜を形成する工程、を含むことを特徴とする複層塗膜形成方法である。
プラスチック基材としては、ポリエチレン樹脂、ポリプロピレン樹脂等のポリオレフィン樹脂;ポリカーボネート、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエチレンテレフタレート/イソフタレート等のポリエステル樹脂;スチレン−ブタジエンブロック共重合体、スチレン−アクリロニトリル、アクリロニトリル−ブタジエン−スチレン(ABS)、ポリスチレン、アクリロニトリル−スチレン−アクリレート等のスチレン系樹脂、ナイロン6、ナイロン6,6、ナイロン6,10、メタキシリレンアジパミド等のポリアミド樹脂、ポリメチルメタクリレート、メチルメタクリレート・エチルアクリレート等のアクリル樹脂;ポリ塩化ビニル樹脂、塩化ビニル−酢酸ビニル等の塩化ビニリデン樹脂や、不飽和ポリエステル樹脂、フェノール樹脂、メラミン樹脂、ユリア樹脂、ポリフェニレンエーテル樹脂、ポリオキシメチレン樹脂、ポリウレタン樹脂、エポキシ樹脂等の樹脂及び各種の繊維強化プラスチック(以下、FRPと略すことがある)等のプラスチック材料を挙げることができる。上記プラスチック基材は、樹脂2種以上のハイブリッド樹脂であっても構わない。
プラスチック基材上にエポキシ樹脂及びアミン化合物を含有する下塗塗料(X)を塗装して、下塗塗膜を形成する工程、である。
本方法において下塗塗料(X)は、エポキシ樹脂及びアミン化合物を含有する塗料であれば水系、有機溶剤系いずれであってもよく、また一成分系組成物であっても多成分系組成物であってもよい。
無機系フィラーの配合量は、顔料重量濃度(PWC)が30〜80%、特に40〜65%の範囲内であることが、耐薬品性、製造安定性の観点の観点から好ましい。
工程(1)で形成された下塗塗膜上にポリビニルブチラール樹脂及びフェノール樹脂を含有する中塗塗料(Y)を塗装して、中塗塗膜を形成する工程、である。
本方法において中塗塗料(Y)は、ポリビニルブチラール樹脂及びフェノール樹脂を含有する塗料であれば水系、有機溶剤系いずれであってもよい。
ポリビニルブチラール樹脂は樹脂中のビニルブチラール単位(すなわちブチラール化度)が60〜75モル%、特に65〜70モル%の範囲内であることが密着性の観点から好ましい。
工程(2)で形成された中塗塗膜上にウレタンエラストマー及び芳香族ジアミン化合物を含有する上塗塗料(Z)を塗装して、上塗塗膜を形成する工程、である。
上塗塗料(Z)
本方法において上塗塗料(Z)は、ウレタンエラストマー及び芳香族ジアミンを含有する塗料であれば水系、有機溶剤系いずれであってもよく、また一成分系組成物であっても多成分系組成物であってもよい。
2個以上の活性水素を有する化合物としては、例えば、多価アルコール、アミン、多価フェノール等を挙げることができる。
上記電子供与性基のうち、密着性の観点からアルキル基が好ましい。
トリレンジアミン(2,3−トリレンジアミン、2,4−トリレンジアミン、2,5−トリレンジアミン、2,6−トリレンジアミン、3,4−トリレンジアミン)、ジエチルトルエンジアミン、キシレンジアミン、
芳香核にアルキル基を有するアルキル置換ジアミノジフェニルメタン(4,4´−ジアミノジフェニルメタン、2,4´−ジアミノジフェニルメタン、3,3´−ジアミノジフェニルメタン、3,4´−ジアミノジフェニルメタン)、
芳香核にアルキル基を有するアルキル置換ジアミノビフェニル(2,2´−ジアミノビフェニル、3,3´−ジアミノビフェニル)、
芳香核にアルキル基を有するアルキル置換フェニレンジアミン(o−フェニレンジアミン、m−フェニレンジアミン、p−フェニレンジアミン)、
ジアミノフェノール(2,4−ジアミノフェノール、2,5−ジアミノフェノール)、
等を挙げることができる。
下塗塗料(X1):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価2.2mmol/gのビスフェノールA骨格のエポキシ樹脂、及びマイカ顔料40(PWC)含有、硬化剤:アミン価410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比は1.0
下塗塗料(X2):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価=2.2mmol/gのビスフェノール−A骨格のエポキシ樹脂含有、及びマイカ顔料40(PWC)含有、硬化剤:アミン価=410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比=0.75
下塗塗料(X3):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価=2.2mmol/gのビスフェノール−A骨格のエポキシ樹脂含有、及びマイカ顔料40(PWC)含有、硬化剤:アミン価=410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比=1.25
下塗塗料(X4):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価=2.2mmol/gのビスフェノール−A骨格のエポキシ樹脂含有、及びマイカ顔料40(PWC)含有、硬化剤:アミン価=410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比=0.6
下塗塗料(X5):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価=2.2mmol/gのビスフェノール−A骨格のエポキシ樹脂含有、及びマイカ顔料40(PWC)含有、硬化剤:アミン価=410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比=1.4
下塗塗料(X6):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価=2.2mmol/gのビスフェノール−A骨格のエポキシ樹脂含有、及び炭酸カルシウム顔料40(PWC)含有、硬化剤:アミン価=410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比=1.0
下塗塗料(X7):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価=2.2mmol/gのビスフェノール−A骨格のエポキシ樹脂含有、及びマイカ顔料30(PWC)含有、硬化剤:アミン価=410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比=1.0
下塗塗料(X8):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価=2.2mmol/gのビスフェノール−A骨格のエポキシ樹脂含有、及びマイカ顔料70(PWC)含有、硬化剤:アミン価=410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比=1.0
下塗塗料(X9):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価5.3mmol/gのビスフェノールA骨格のエポキシ樹脂、及びマイカ顔料40(PWC)含有、硬化剤:アミン価410mgKOH/gの変性脂肪族ポリアミンアダクト、エポキシ基/アミノ基の活性水素当量比は1.0
下塗塗料(X10):溶剤系2液型塗料、主剤:固形分あたりのエポキシ価2.2mmol/gのビスフェノールA骨格のエポキシ樹脂、及びマイカ顔料40(PWC)含有、硬化剤:アミン価265mgKOH/gの脂肪族ポリアミドアミン、エポキシ基/アミノ基の活性水素当量比は1.0
<中塗塗料>
中塗塗料(Y1):フェノール樹脂AP−101(注1)60質量%及びポリビニルブチラール樹脂エスレックBM−1(注2)40質量%をメチルエチルケトン/シクロヘキサノン=1/1で混合した溶剤に溶解し、固形分を10%に調製することにより中塗塗料(Y1)を得た。
(注2)エスレックBM−1:積水化学株式会社製、ポリビニルブチラール樹脂、重量平均分子量4.0×104、水酸基34mol%、アセチル基3mol%以下、ブチラール化度65mol%、ガラス転移温度67℃
各成分の配合を表2及び表5に示す配合とする以外は中塗塗料(Y1)と同様にして、各中塗塗料(Y2)〜(Y12)を得た。中塗塗料(Y11)及び(Y12)は比較例用の中塗塗料である。
(注4)エスレックBL−1:積水化学株式会社製、ポリビニルブチラール樹脂、重量平均分子量:1.9×104、水酸基36mol%、アセチル基3mol%以下、ブチラール化度63mol%、ガラス転移温度66℃
(注5)エスレックBH−6:積水化学株式会社製、ポリビニルブチラール樹脂、重量平均分子量:9.2×104、水酸基30mol%、アセチル基3mol%以下、ブチラール化度69mol%、ガラス転移温度67℃
(注6)ショウノールCKS−3722:アイカ工業株式会社製、フェノール樹脂、重量平均分子量:2400
(注7)ショウノールCKS−937:アイカ工業株式会社製、フェノール樹脂、重量平均分子量:5000
<上塗塗料>
上塗塗料(Z1):ブロック化ウレタンエラストマー(A1)(注8)100部(固形分)、カーボンMA−100(注9)2.0部(固形分)、DISPARLON A670−20M(注10)2.0部(固形分)、ACEMATT TS−100(注11)13部(固形分)及び酢酸ブチル124.5部を混合し、サンドミルで分散を行い、分散ペーストを得た。得られた分散ペーストに、ディスパーで攪拌しながら、ポリフローNo.50EHF(注12)0.5部(固形分)、DISPARLON 1930N(注13)0.002部(固形分)、及び酢酸ブチル20部を混合することにより、固形分34.7質量%の上塗塗料(Z1)の主剤を得た。得られた上塗塗料(Z1)の主剤について、貯蔵安定性の試験を行った。表4に評価結果を示す。
(注10)DISPARLON A670−20M:楠本化成社製、脂肪酸アマイド
(注11)ACEMATT TS−100:EVONIK社製、非晶質合成シリカ
(注12)ポリフローNo.50EHF:共栄社化学社製、アクリル系表面調整剤
(注13)DISPARLON 1930N:楠本化成社製、シリコーン系消泡剤
(注14)CUREHARD MED:クミアイ化学工業社製、3,3’−ジメチル−5,5’−ジエチル−4,4’−ジアミノジフェニルメタン
(注15)ETHACURE100:ALBEMARLE社製、3,5−ジエチルトルエン−2,4−ジアミン
各成分の配合を表3〜5に示す配合とする以外は上記上塗塗料(Z1)と同様にして、固形分30質量%の各上塗塗料(Z2)〜(Z20)を得た。上塗塗料(Z20)は比較例用の上塗塗料である。
試験板の製造
試験板I(耐薬品性試験及び密着性試験用)
ブラスト処理された縦150mm×横20mm×厚さ4mmのCFRP(炭素繊維強化プラスチック)板をイソプロピルアルコールを用いて脱脂して試験用の素材とした。上記素材に上記各下塗塗料をスプレー塗装により所定の膜厚となるように塗装し、23℃で15分間セッティングした後、所定の硬化条件(温度、時間)で硬化させた。室温まで冷却後、上記各中塗塗料をスプレー塗装により所定の膜厚となるように塗装し、23℃で15分間セッティングした後、所定の硬化条件(温度、時間)で硬化させた。
ブラスト処理された縦50mm×横20mm×厚さ2mmのCFRP板をイソプロピルアルコールを用いて脱脂し、直径3mmの丸棒を用いて横20mm幅の真ん中を中心にして半分に折り曲げ加工し試験用の素材とした。上記素材に下塗塗料(X1)をスプレー塗装により硬化膜厚20μmとなるように塗装し、23℃で15分間セッティングした後、80℃で30分間硬化させた。室温まで冷却後、上記各中塗塗料をスプレー塗装により所定の膜厚となるように塗装し、23℃で15分間セッティングした後、120℃で15分間硬化させた。
上記試験板の製造で得られた各試験板を下記試験方法に従って性能評価を行った。試験結果を表1〜5に示す。なお、各試験結果において、◎、○及び○△が合格レベルである。
○:破断強度が25N以上かつ40N未満(剥離なし)
○△:剥離強度が25N以上
△:剥離強度が15N以上かつ25N未満
×:剥離強度が15N未満
耐薬品性:各試験板I1〜I14、I1G及びI101をリン酸エステル系作動油(Eastman社製)に23℃で168時間浸漬し、引き揚げたものを試験板とする以外は上記密着性の試験及び評価方法と同様にして、試験及び評価を行った。
○:60分間運転後のキズの大きさは小さいが、下地が露出している
○△:30分間運転後のキズの大きさは小さく、下地が露出していない
△:30分間運転後のキズの大きさは大きく、下地が露出している、
×:30分間運転後のキズの大きさはかなり大きく、下地も大きく露出している。
上塗塗料(Z1)及び(Z14)〜(Z16)について、以下のタレ性試験を行った。
150mm×450mm×0.3mmのイソプロピルアルコールを用いて脱脂したブリキ板を試験用の基材とした。ブリキ板下端部に幅24mm(150mm長のうち24mm分)のマスキングテープを貼り付けた後、垂直に置いた上記基材にスプレー塗装により、硬化膜厚が100〜300μmとなるように各上塗塗料を膜厚傾斜塗装し、塗装直後にマスキングテープを剥がし、基材を垂直のまま23℃で60分間セッティングした後、垂直のまま120℃で120分間硬化させることにより各試験板を得た。
○:200μm以上250μm未満
○△:150μm以上200μm未満
△:100μm以上150μm未満
×:100μm未満
各上塗塗料の評価結果は、上塗塗料(Z1)が◎、上塗塗料(Z14)が○、上塗塗料(Z15)が○△、上塗塗料(Z16)が×であった。
Claims (6)
- プラスチック基材上に複層塗膜を形成する塗膜形成方法であって、
工程(1):プラスチック基材上にエポキシ樹脂及びアミン化合物を含有する下塗塗料(X)を塗装して、下塗塗膜を形成する工程、
工程(2):該下塗塗膜上にポリビニルブチラール樹脂及びフェノール樹脂を含有する中塗塗料(Y)を塗装して、中塗塗膜を形成する工程、ならびに
工程(3):該中塗塗膜上にウレタンエラストマー及び芳香族ジアミン化合物を含有する上塗塗料(Z)を塗装して、上塗塗膜を形成する工程、を含む複層塗膜形成方法。 - 中塗塗料(Y)のポリビニルブチラール樹脂の重量平均分子量が10000〜100000の範囲内である請求項1に記載の複層塗膜形成方法。
- 上塗塗料(Z)のウレタンエラストマーが、オキシム化合物でブロックされた、末端イソシアネート基含有ブロック化ウレタンエラストマーである請求項1又は2に記載の複層塗膜形成方法。
- 上塗塗料(Z)の芳香族ジアミン化合物が、電子供与性基含有芳香族ジアミン化合物である請求項1〜3のいずれか一項に記載の複層塗膜形成方法。
- 上塗塗料(Z)が、さらに、アマイド化合物を含有する請求項1〜4のいずれか一項に記載の複層塗膜形成方法。
- 請求項1〜5のいずれか一項に記載の複層塗膜形成方法により塗装されたプラスチック基材物品。
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