JP5162097B2 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JP5162097B2 JP5162097B2 JP2006006428A JP2006006428A JP5162097B2 JP 5162097 B2 JP5162097 B2 JP 5162097B2 JP 2006006428 A JP2006006428 A JP 2006006428A JP 2006006428 A JP2006006428 A JP 2006006428A JP 5162097 B2 JP5162097 B2 JP 5162097B2
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- coating film
- electrodeposition
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- acid
- epoxy
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- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- DXNCZXXFRKPEPY-UHFFFAOYSA-N tridecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCC(O)=O DXNCZXXFRKPEPY-UHFFFAOYSA-N 0.000 description 1
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
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- Application Of Or Painting With Fluid Materials (AREA)
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Description
電着塗料として、形成される電着塗膜を105℃で3時間加熱乾燥した後、160℃で20分間加熱硬化させた時の電着塗膜の加熱減量が5重量%以下である電着塗料を使用することを特徴とする複層塗膜形成方法を提供するものである。
で示されるα−オレフィンエポキサイド;スチレンオキサイドなどの不飽和化合物の酸化物;アリルグリシジルエーテル、2−エチルヘキシルグリシジルエーテル、メチルグリシジルエーテル、ブチルグリシジルエーテル、フェニルグリシジルエーテルなどの水酸基含有化合物のグリシジルエーテル;脂肪酸のような有機酸のグリシジルエステルなどを挙げることができる。
難となることがある。
キル基、アリール基、アラルキル基又はハロゲン原子を表わし;R5は水素原子、炭
素数1〜10のアルキル基、アリール基、アラルキル基、アリル基又はハロゲン原子
を表わし;R6およびR8は同一もしくは相異なり、各々水素原子、炭素数1〜4の
アルキル基又はグリシジルオキシフェニル基を表わし;R7は水素原子、炭素数1〜
10のアルキル基、アリール基、アラルキル基、アリル基又はハロゲン原子を表わし
;
そしてnは1〜38の整数である、
で示されるエポキシ樹脂である。
ル基」は下記式(9)
タム、γ−ブチロラクタム、β−プロピオラクタムなどのラクタム系ブロック剤;アセト酢酸エチル、アセチルアセトンなどの活性メチレン系ブロック剤;メタノール、エタノール、プロパノール、ブタノール、アミルアルコール、エチ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エチルエーテル、エチレングリコールモノブチルエーテル、ジエチレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテル、ベンジルアルコール、グリコール酸メチル、グリコール酸ブチル、ジアセトンアルコール、乳酸メチル、乳酸エチルなどのアルコール系ブロック剤;ホルムアミドオキシム、アセトアルドオキシム、アセトオキシム、メチルエチルケトオキシム、ジアセチルモノオキシム、シクロヘキサンオキシムなどのオキシム系ブロック剤;ブチルメルカプタン、ヘキシルメルカプタン、t−ブチルメルカプタン、チオフェノール、メチルチオフェノール、エチルチオフェノールなどのメルカプタン系ブロック剤;酢酸アミド、ベンズアミドなどの酸アミド系ブロック剤;コハク酸イミド、マレイン酸イミドなどのイミド系ブロック剤;キシリジン、アニリン、ブチルアミン、ジブチルアミンなどのアミン系ブロック剤;イミダゾール、2−エチルイミダゾールなどのイミダゾール系ブロック剤;エチレンイミン、プロピレンイミンなどのイミン系ブロック剤等を挙げることができる。これらのうち、塗料の安定性や塗膜の硬化性などのバランスから、メチルエチルケトオキシムなどのオキシム系ブロック剤が特に好適である。
ミダゾール、1−ベンジル−2−メチルイミダゾール、2−エチルイミダゾール、2−イソプロピルイミダゾール、2−フェニル−4−ベンジルイミダゾール、1−シアノエチル−2−メチルイミダゾール、1−シアノエチル−2−エチル−4−メチルイミダゾール、1−シアノエチル−2−ウンデシルイミダゾール、1−シアノエチル−2−イソプロピルイミダゾール、1−シアノエチル−2−フェニルイミダゾール、2,4−ジアミノ−6−〔2′−メチルイミダゾリル−(1)′〕−エチル−S−トリアジン、2,4−ジアミノ−6−〔2′−エチル−4−メチルイミダゾリル−(1)′〕−エチル−S−トリアジン、2,4−ジアミノ−6−〔2′−ウンデシルイミダゾリル−(1)′〕−エチル−S−トリアジン、2−メチルイミダゾリウムイソシアヌル酸付加物、2−フェニルイミダゾリウムイソシアヌル酸付加物、1−アミノエチル−2−メチルイミダゾール、2−フェニル−4,5−ジヒドロキシメチルイミダゾール、2−フェニル−4−メチル−5−ヒドロキシメチルイミダゾール、2−フェニル−4−ベンジル−5−ヒドロキシメチルイミダゾールなどの1分子中にイミダゾール環を1個有する化合物;上記の2−フェニル−4,5−ジヒドロキシメチルイミダゾール、2−フェニル−4−メチル−5−ヒドロキシメチルイミダゾール又は2−フェニル−4−ベンジル−5−ヒドロキシメチルイミダゾールなどのヒドロキシメチル基含有イミダゾール化合物を脱水、脱ホルムアルデヒド反応により縮合させてなる1分子中にイミダゾール環を2個以上有する化合物、例えば、4,4′−メチレン−ビス−(2−エチル−5−メチルイミダゾール)などが挙げられる。
が、一般的には、硬化塗膜に基づいて10〜40μm、特に15〜25μmの範囲内が好ましい。電着塗膜は、UFロ液、工業用水、純水等で水洗することができる。
してのイミダゾール化合物、例えば、2−メチルイミダゾール、2−フェニルイミダゾール、2−エチル−4−メチルイミダゾールなどのイミダゾ−ル類、それらのシアノエチル化物、それらのトリアジン付加物、それらの水素添加物であるイミダゾリン類など;カチオン重合触媒としての芳香族スルホニウム塩、例えば、ベンジル−4−ヒドロキシフェニルメチルスルホニウムヘキサフルオロアンチモネ−ト、ベンジル−4−メトキシフェニルメチルスルホニウムヘキサフルオロアンチモネ−トなどが挙げられる。
飽和もしくは不飽和基の脂肪族二塩基酸が包含され、具体的には、例えば、コハク酸、グルタル酸、アジピン酸、ピロメリット酸、ドデカン二酸、アゼライン酸、セバシン酸、ブラシリル酸、イタコン酸、マレイン酸、シトラコン酸、エイコサン二酸など及びこれらの二塩基酸の1種もしくは2種以上の酸無水物等を挙げることができる。このうち特にドデカン二酸およびこの酸無水物が好適である。
撹拌機、温度計、滴下ロート及び還流冷却器を取付けたフラスコに、下記の成分(a1)、(a2)及び(a3)の混合物を入れ、160℃で5時間反応させた後、メチルプロパノール692部を加え、水酸基当量443、アミン価63mgKOH/g及び固形分60%の基体樹脂No.1を得た。
成分(a2): ジエタノールアミン70部、
成分(a3): エポキシ当量190のビスフェノールAジグリシジルエーテル475
部、ビスフェノールA285部、ジエタノールアミン53部及びカルビ
トール80部を混合して加熱溶解した後冷却し、130℃で3時間保持
して反応させることにより得られた生成物の全量
(注1)EHPE−3150: ダイセル化学工業(株)製、商品名、脂環式骨格にエポ
キシ基が結合してなるエポキシ基含有官能基を1分子あたり平均2個以上有する
エポキシ樹脂、エポキシ当量180。
エピコート828EL(ジャパンエポキシレジン株式会社製、商品名、エポキシ樹脂)1010部に、ビスフェノールA390部及びジメチルベンジルアミン0.2部を加え、130℃でエポキシ当量800になるまで反応させた。次に、ジメチロールブタン酸74部、ジエタノールアミン63部及びジエチレントリアミンのケチミン化物95部を加え、120℃で4時間反応させた後、エチレングリコールモノブチルエーテル330部を加え、アミン価43mgKOH/g及び固形分80%の基体樹脂No.2を得た。
サイクロマーM100(ダイセル化学工業製、商品名、3,4−エポキシシクロヘキシルメチルメタクリレート)33.4部にアゾビスジメチルバレロニトリル2部を溶解したものを、100℃に加熱したメチルイソブチルケトン10部とエチレングリコールモノブチルエーテル10部の混合溶剤中に2時間かけて滴下し、1時間熟成した後、125℃に昇温して更に1時間熟成し、エポキシ当量196及び固形分60%のエポキシ硬化剤No.1を得た。
コスモネートM−200(三井化学株式会社製、商品名、クルードMDI)270部にメチルイソブチルケトン46部を加え70℃に昇温した。さらにジエチレングリコールモノブチルエーテル281部をゆっくり加えた後、90℃に昇温した。
固形分60%の基体樹脂No.1 117部(固形分70部)、エチレングリコールモノブチルエーテルに溶解した固形分80%のEHPE−3150(注1参照)37.5部(固形分30部)及び10%ギ酸7部を混合し均一に撹拌した後、脱イオン水132.5部を強く撹拌しながら約15分かけて滴下し、固形分34%のカチオン電着用のエマルションNo.1を得た。
固形分60%の基体樹脂No.1 117部(固形分70部)、固形分60%の硬化剤No.1 50部(固形分30部)及び10%ギ酸7部を混合し均一に撹拌した後、脱イオン水120部を強く撹拌しながら約15分かけて滴下し、固形分34%のカチオン電着用のエマルションNo.2を得た。
固形分80%の基体樹脂No.2 87.5部(固形分70部)、固形分60%の硬化剤No.2 50部(固形分30部)及び10%ギ酸7部を混合し均一に撹拌した後、脱イオン水149.5部を強く撹拌しながら約15分かけて滴下し、固形分34%のカチオン電着用のエマルションNo.3を得た。
製造例1で得た60%の基体樹脂No.1 8.33部(固形分5部)に10%のギ酸4.4部を加え、さらに攪拌しながら脱イオン水15部を加える。次いで、JR−600E(注2)10部、ハイドライドPXN(注3)10部、カーボンMA−7(注4)1部、水酸化銅1部、水酸化ビスマス3部及び脱イオン水7.3部を加え、ボールミルで24時間分散処理して、固形分50.0%の顔料分散ペーストNo.1を得た。
(注2)JR−600E: テイカ社製、商品名、チタン白、
(注3)ハイドライドPXN: ジョージアカオリン社製、商品名、カオリン、
(注4)カーボンMA−7: 三菱化成社製、商品名、カーボンブラック。
製造例1で得た60%の基体樹脂No.1 8.33部(固形分5部)に10%のギ酸4.4部を加え、さらに攪拌しながら脱イオン水15部を加える。次いで、JR−600E(注2参照)10部、ハイドライドPXN(注3参照)10部、カーボンMA−7(注4参照)1部、ジオクチル錫オキサイド1部及び脱イオン水4.27部を加え、ボールミルで24時間分散処理して、固形分50.0%の顔料分散ペーストNo.2を得た。
製造例5で得た34%のエマルションNo.1 294部(固形分100部)に、製造例8で得た50%の顔料分散ペーストNo.1 60部(固形分30部)及び脱イオン水296部を加え混合して、固形分20%の電着塗料No.1を得た。
下記表2の配合内容で、製造例10と同様に操作して、電着塗料No.2を得た。
下記表2の配合内容で、製造例10と同様に操作して、電着塗料No.3を得た。
試験板(注6)の重量を測定した後、該試験板に電着塗料を電着塗装して塗膜20μmの電着塗膜を得た。次に、105℃で3時間加熱してから塗装試験板の重量を測定し塗膜重量(Y)を求めた。さらに、塗装試験板を160℃で20分間加熱した後、その重量を測定し塗膜重量(Z)を求めた。これらの塗膜重量から下記式により電着塗膜の加熱減量(X)を求めた。
ファインデックM8031(大日本インキ株式会社製、商品名、ポリエステル樹脂、水酸基価30mgKOH/g)770部、プリミドXL552(EMS−PRIMD社製、商品名、β−ヒドロキシアルキルアミド)230部及びチタン白400部をヘンシェルミキサ−でドライブレンドし、次いでブスコニーダー混練機で溶融混合分散し、冷却、粗粉砕、微粉砕を行った後、150メッシュで篩別して、粉体塗料No.1を得た。
ファインデックM8860(大日本インキ株式会社製、商品名、ポリエステル樹脂、酸
価32mgKOH/g)700部、エピコート#1002(ジャパンエポキシレジン社製、商品名、ビスフェノールAタイプのエポキシ樹脂)300部及びチタン白400部をヘンシェルミキサーでドライブレンドを行い、次いでブスコニーダー混練機で溶融混合分散し、冷却、粗粉砕、微粉砕を行った後、150メッシュで篩別して、粉体塗料No.2を得た。
試験板(注6参照)に電着塗料No.1を膜厚が20μmとなるようにして電着塗装し、25℃で20分間セッティングした後、電着塗膜面に粉体塗料No.1を静電粉体塗装機(ゲマ社製)で膜厚が50μmになるようにして塗装した。次いで、試験板の表面温度が160℃となるように加熱しながら20分間(保持時間)焼き付けを行い、試験板上に電着塗膜と粉体塗膜からなる複層塗膜No.1を形成せしめた。
下記表3に示す電着塗料及び粉体塗料ならびにセッティング/エアブロー及び焼付け硬化条件を使用し、実施例1と同様に操作して、試験板上に複層塗膜No.2〜No.6を形成せしめた。
及び稼動を必要とする)。
熱を行う必要がある(エアブロー設備又は乾燥炉の設置及び稼動を必要とする)。
稼動を必要とする。
(注8)仕上り性:
複層塗膜のワキ、ヘコミ、平滑性を目視で評価した。
(注9)防食性:
複層塗膜に、素地に達するようにナイフでクロスカット傷を入れ、これをJISZ−2371に準じて840時間耐塩水噴霧試験を行い、ナイフ傷からの錆、フクレ幅によって以下の基準で評価した。
)。
)。
(注10)60度鏡面光沢度:
複層塗膜の光沢の程度を、JIS K−5400 7.6(1990)の60度鏡面光沢度に従い、入射角及び受光角がそれぞれ60度のときの反射率を測定し、鏡面光沢度の基準面の光沢度を100としたときの百分率で表した。
試験板(注6参照)に、電着塗料No.3を膜厚が20μmとなるようにして電着塗装し、25℃で20分間セッティングした後、粉体塗料No.1を静電粉体塗装機(ゲマ社製)で膜厚が50μmになるようにして塗装した。次いで、試験板の表面温度が160℃になるようにして20分間加熱硬化を行い、試験板上に複層塗膜No.7を形成せしめた。
下記表4に示すセッティング/エアブロー/予備乾燥及び焼付け硬化条件を使用し、比較例1と同様に操作して、試験板上に複層塗膜No.8〜No.11を形成せしめた。
Claims (4)
- 金属製製品に、電着塗料を電着塗装し、セッティング又はエアブローを行った後、その未硬化の電着塗膜上に粉体塗料を塗装し、次いで形成される電着塗膜と粉体塗膜の両塗膜を同時に加熱硬化させることにより複層塗膜を形成する方法において、
電着塗料として、形成される電着塗膜を105℃で3時間加熱乾燥した後、160℃で20分間加熱硬化させた時の電着塗膜の加熱減量が5重量%以下である電着塗料を使用し、そして
粉体塗料がエポキシ樹脂、ポリエステル樹脂及びアクリル樹脂から選ばれる少なくも1種の基体樹脂を含んでなる、約120〜約160℃及び1〜120分間の焼付け条件下に硬化塗膜を形成し得る低温硬化型の熱硬化性粉体塗料である
ことを特徴とする複層塗膜形成方法。 - 電着塗膜の加熱減量が4重量%以下である電着塗料を使用する請求項1に記載の方法。
- 粉体塗料が架橋剤としてβ−ヒドロキシアルキルアミドを含んでなるものである請求項1〜3のいずれか1項に記載の方法。
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JP6859011B2 (ja) * | 2016-04-08 | 2021-04-14 | 関西ペイント株式会社 | 複層塗膜形成方法 |
JP7459042B2 (ja) * | 2021-12-24 | 2024-04-01 | 株式会社クボタ | 塗装方法 |
JP7539543B1 (ja) | 2023-06-20 | 2024-08-23 | 株式会社クボタ | 塗装方法及び塗装系 |
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