JPWO2007083803A1 - 水性中塗り塗料組成物及び複層塗膜形成方法 - Google Patents
水性中塗り塗料組成物及び複層塗膜形成方法 Download PDFInfo
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- JPWO2007083803A1 JPWO2007083803A1 JP2007555000A JP2007555000A JPWO2007083803A1 JP WO2007083803 A1 JPWO2007083803 A1 JP WO2007083803A1 JP 2007555000 A JP2007555000 A JP 2007555000A JP 2007555000 A JP2007555000 A JP 2007555000A JP WO2007083803 A1 JPWO2007083803 A1 JP WO2007083803A1
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Classifications
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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
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/348—Hydroxycarboxylic acids
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/807—Masked polyisocyanates masked with compounds having only one group containing active hydrogen with nitrogen containing compounds
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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
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- 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
- C09D133/066—Copolymers with monomers not covered by C09D133/06 containing -OH groups
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- C—CHEMISTRY; METALLURGY
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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
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- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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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
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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
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Abstract
Description
(B)メラミン樹脂及びブロックポリイソシアネート化合物からなる群より選ばれる少なくとも1種の硬化剤、並びに
(C)扁平状顔料粒子を含有する塗料組成物であって、
(A)成分及び(B)成分を含む硬化性樹脂成分の分子量分布が、分子量1,000未満の成分の含有率が30〜50重量%で、分子量100,000を超える成分の含有率が10重量%未満であり、
(C)成分の配合割合が、前記硬化性樹脂成分100重量部に対して2〜15重量部であり、且つ
当該組成物を下塗り塗膜上に塗装し、100℃で30分間予備乾燥後、145℃で30分間加熱硬化させた時の膜厚収縮率が、前記予備乾燥後の塗膜膜厚を基準にして20%以下である水性中塗り塗料組成物。
本発明の水性中塗り塗料組成物は、特定の水酸基価及び酸価を有する水酸基及びカルボキシル基含有樹脂(A)、メラミン樹脂及びブロックポリイソシアネート化合物から選ばれる少なくとも1種の硬化剤(B)及び特定量の偏平状顔料粒子(C)を含有する水性中塗り塗料組成物である。
本発明塗料組成物は、硬化性樹脂成分として、水酸基及びカルボキシル基含有樹脂(A)とメラミン樹脂及びブロックポリイソシアネート化合物から選ばれる少なくとも1種の硬化剤(B)とを含有する。また、必要に応じて、硬化性樹脂成分として、更に、1分子中に水酸基及びブロックイソシアネート基を併有するウレタン変性ポリエステル樹脂(D)を含有していてもよい。
本発明の中塗り塗料組成物においては、当該組成物を、被塗物上に形成された下塗り塗膜上に、塗装し、100℃で30分間予備乾燥後、145℃で30分間加熱硬化させた時の膜厚収縮率が、前記予備乾燥後の塗膜膜厚を基準にして20%以下であることが、必要である。この膜厚収縮率が20%を越える場合には、その中塗り塗料組成物により、電着塗膜等の下塗り塗膜表面の微小な凹凸を隠蔽して、平滑性に優れた塗膜を形成することが困難になる。即ち、下地隠蔽性が低下することになる。
水酸基及びカルボキシル基含有樹脂(A)
水酸基及びカルボキシル基含有樹脂(A)は、水酸基価が100〜200mgKOH/gであり、酸価が20〜50mgKOH/gである。本発明塗料組成物は、基体樹脂である水酸基及びカルボキシル基含有樹脂(A)が、かかる高い水酸基価を有することにより、硬化性に優れている。
水酸基及びカルボキシル基含有ポリエステル樹脂は、常法により、例えば、多塩基酸と多価アルコールとのエステル化反応によって合成することができる。
水酸基及びカルボキシル基含有アクリル樹脂は、常法に従い、例えば、ラジカル重合性モノマーを共重合することによって合成することができる。水酸基及びカルボキシル基含有アクリル樹脂としては、溶液重合法により合成される樹脂を用いることが好ましい。この重合反応に使用する有機溶剤としては、例えば、プロピレングリコール系、ジプロピレングリコール系等の親水性有機溶剤を使用するのが好ましい。
本発明塗料組成物においては、塗膜の耐チッピング性を向上させる観点から、硬化性樹脂成分として、更に、1分子中に水酸基及びブロックイソシアネート基を併有するウレタン変性ポリエステル樹脂(D)を使用することができる。
硬化剤(B)は、メラミン樹脂及びブロックポリイソシアネート化合物からなる群より選ばれる少なくとも1種の硬化剤である。
メラミン樹脂としては、具体的には、ジメチロールメラミン、トリメチロールメラミン、テトラメチロールメラミン、ペンタメチロールメラミン、ヘキサメチロールメラミン等のメチロールメラミン;これらのメチロールメラミンのアルキルエーテル化物又は縮合物;メチロールメラミンのアルキルエーテル化物の縮合物等を挙げることができる。メチロールメラミンのアルキルエーテル化は、例えば、メチルアルコール、エチルアルコール、プロピルアルコール、イソプロピルアルコール、ブチルアルコール、イソブチルアルコール、2−エチルヘキシルアルコール等のモノアルコールを用いて、公知の方法により行うことができる。
ブロックポリイソシアネート化合物は、1分子中に遊離のイソシアネート基を2個以上有するポリイソシアネート化合物のすべてのイソシアネート基をブロック剤で封鎖した化合物である。
本発明塗料組成物においては、必須成分として、偏平状顔料粒子(C)を含有する。偏平状顔料粒子(C)は、うろこのような薄く平らな形状の顔料であり、具体的には、例えば、タルク、アルミニウムフレーク、雲母フレークなどをあげることができる。これらのうち、特に、タルクが好ましい。該粒子(C)は、厚さが0.1〜2μm程度が好ましく、0.2〜1.5μm程度がより好ましい。また、その長手方向寸法が1〜100μm程度が好ましく、2〜20μm程度がより好ましい。
本発明塗料組成物においては、必要に応じて、架橋樹脂微粒子(E)を配合することにより、タレ抵抗性を向上させることができる。架橋樹脂微粒子(E)は、内部架橋された樹脂の微粒子であり、硬化反応には関与しない。また、該微粒子は、水及びテトラヒドロフラン等の有機溶剤に不溶であるため、遠心分離で沈降でき、又はろ過で除去できるため、分子量分布の測定値に影響を与えることはない。
本発明塗料組成物においては、偏平状顔料粒子(C)に加えて、必要に応じて、扁平状粒子でない顔料を配合することができる。
本発明塗料組成物においては、更に必要に応じて、硬化触媒、レオロジーコントロール剤、表面調整剤、分散剤、沈降防止剤、有機溶剤、消泡剤、紫外線吸収剤、光安定剤、酸化防止剤、防錆剤などの塗料用添加剤を適宜配合することができる。硬化触媒としては、例えば、酸触媒、有機錫化合物等を挙げることができる。また、レオロジーコントロール剤としては、例えば、増粘剤、タレ防止剤等を挙げることができる。
本発明塗料組成物は、(A)成分、(B)成分及び必要に応じて使用される(D)成分を含有する硬化性樹脂成分、並びに(C)成分に、更に必要に応じて(E)成分等の任意成分を加え、これらを水と混合し、分散せしめることにより調製することができる。水への混合及び分散にあたっては、中和剤により中和して行なうのが、水分散性を向上させる観点から好ましい。また、この混合及び分散においては、分散性向上の観点から、必要に応じて乳化剤を併用することもできる。
本発明の複層塗膜形成方法は、被塗物に、電着塗膜、中塗り塗膜、次いで上塗り塗膜を形成して、複層塗膜を形成する方法であって、中塗り塗膜を本発明の水性中塗り塗料組成物を用いて形成することを特徴とするものである。
水酸基及びカルボキシル基含有ポリエステル樹脂の製造
加熱装置、攪拌装置、温度計、還流冷却器、水分離器を備えた4つ口フラスコに、無水フタル酸28.0部、アジピン酸25.7部、ネオペンチルグリコール26.4部、トリメチロールプロパン22.9部を仕込んだ。次に、内容物を160℃から230℃まで3時間かけて昇温させた後、230℃で保持し、生成した縮合水を水分離器により留去させながら、酸価が3mgKOH/g以下になるまで反応させた。
表1に示す原料を用いて、製造例1と同様にして、水酸基及びカルボキシル基含有ポリエステル樹脂(A−2)〜(A−6)を得た。
1分子中に水酸基及びブロックイソシアネート基を併有するウレタン変性ポリエステル樹脂の製造
トリメチロールプロパン0.2モル、1,6−ヘキサンジオール0.8モル、シクロヘキシルジカルボン酸0.4モル及びアジピン酸0.3モルを反応させた後、さらに無水トリメリット酸0.05モルを付加してなるポリエステル樹脂100部に、4,4’−メチレンビス(シクロヘキシルイソシアネート)2モルとジメチロールプロピオン酸1モルを反応させてなるポリウレタン樹脂30部を、メチルエチルケトン中で反応させた。得られた反応生成物130部に含まれる水酸基の一部に、メチルエチルケトンオキシムと4,4’−メチレンビス(シクロヘキシルイソシアネート)とを等モル比で反応させてなる半ブロックポリイソシアネート化合物10部を反応せしめ、ついで脱溶剤し、ジメチルエタノールアミンをカルボキシル基に対して当量添加して中和してから、脱イオン水を徐々に添加し水分散することにより、固形分38%の1分子中に水酸基及びブロックイソシアネート基を併有するウレタン変性ポリエステル樹脂(D−1)の水分散液を得た。得られたウレタン変性ポリエステル樹脂(D−1)の水酸基価は90mgKOH/g、酸価は38mgKOH/g、NCO量は0.9%、数平均分子量は2,000であった。NCO量は、樹脂固形分100重量部に対するブロックされているNCO基の量(%)を意味する。
架橋樹脂微粒子(E)の製造
攪拌機、温度計、還流管、窒素導入管を備えた4つ口フラスコに、脱イオン水129部、アニオン界面活性剤(商品名「Newcol 707SF」、日本乳化剤製、不揮発分30%)0.8部を加え、窒素置換後、攪拌しながら82℃に保った。この中に先ず、下記のエマルション化した「モノマー混合物」5部と過硫酸アンモニウム0.3部を脱イオン水3部で溶解した混合物を添加し、20分後、残りの「モノマー混合物」と過硫酸アンモニウム0.3部を脱イオン水3部に溶解したものを4時間かけて滴下して、乳化重合を行った。これにより、固形分30%の架橋樹脂微粒子(E−1)のエマルションを得た。架橋樹脂微粒子(E−1)の平均粒子径は120nmであった。
水性中塗り塗料組成物の製造
製造例1〜6で得られたポリエステル樹脂、製造例7で得られた1分子中に水酸基及びブロックイソシアネート基を併有するウレタン変性ポリエステル樹脂、硬化剤、扁平状顔料粒子、及び製造例8で得られた架橋樹脂微粒子を、後記表2及び表3に示す配合にて、回転翼式攪拌機(商品名「デスパMH−L」、浅田鉄工(株)製)を用いて攪拌混合することにより、各水性中塗り塗料組成物No.1〜15を得た。
式(2)において、Sは塗料の固形分(wt%)を、Wは塗料の水分量(wt%)を、ρは塗料の比重(g/l)をそれぞれ示す。
実施例1〜8及び比較例1〜7で得られた各水性中塗り塗料組成物について、以下の様にして試験板を作製した。
上記で得られた各試験板について、以下の性能試験を行なった。
予備乾燥後固形分(%):上記膜厚収縮率測定の場合と同様にして、中塗り塗料組成物を塗装し、100℃で30分間の予備乾燥後、選択部位の中塗り塗着塗膜をすばやくかきとり予備乾燥後の塗着塗膜の試料とする。直径約5cmのアルミニウム箔カップに、試料約2gを測りとり、十分全体に伸ばした後、110℃で1時間乾燥させ、初期重量と110℃で1時間乾燥後の重量から予備乾燥後の塗料の固形分(%)を算出した。
Claims (13)
- (A)水酸基価が100〜200mgKOH/gで、酸価が20〜50mgKOH/gである水酸基及びカルボキシル基含有樹脂、
(B)メラミン樹脂及びブロックポリイソシアネート化合物からなる群より選ばれる少なくとも1種の硬化剤、並びに
(C)扁平状顔料粒子を含有する塗料組成物であって、
(A)成分及び(B)成分を含む硬化性樹脂成分の分子量分布が、分子量1,000未満の成分の含有率が30〜50重量%で、分子量100,000を超える成分の含有率が10重量%未満であり、
(C)成分の配合割合が、前記硬化性樹脂成分100重量部に対して2〜15重量部であり、且つ
当該組成物を下塗り塗膜上に塗装し、100℃で30分間予備乾燥後、145℃で30分間加熱硬化させた時の膜厚収縮率が、前記予備乾燥後の塗膜膜厚を基準にして20%以下である水性中塗り塗料組成物。 - 水酸基及びカルボキシル基含有樹脂(A)が、水酸基及びカルボキシル基ポリエステル樹脂及び水酸基及びカルボキシル基アクリル樹脂からなる群より選ばれる少なくとも1種である請求項1に記載の水性中塗り塗料組成物。
- 硬化剤(B)が、メラミン樹脂及びブロックポリイソシアネート化合物の混合物である請求項1に記載の水性中塗り塗料組成物。
- 硬化剤(B)が、トリアジン単核体含有率が35重量%以上で、メトキシ基/ブトキシ基のモル比率が100/0〜60/40mol%であるメチル・ブチル混合エーテル化メラミン樹脂である請求項1に記載の水性中塗り塗料組成物。
- 水酸基及びカルボキシル基含有樹脂(A)と硬化剤(B)との割合が、両者の合計固形分100重量%に基づいて、樹脂(A)が80〜65重量%で硬化剤(B)が20〜35重量%である請求項1に記載の水性中塗り塗料組成物。
- 更に、硬化性樹脂成分として、1分子中に水酸基及びブロックイソシアネート基を併有するウレタン変性ポリエステル樹脂(D)を含有する請求項1に記載の水性中塗り塗料組成物。
- 硬化剤(B)であるブロックポリイソシアネート化合物と1分子中に水酸基及びブロックイソシアネート基を併有するウレタン変性ポリエステル樹脂(D)との合計ブロックイソシアネート基の含有率が、前記硬化性樹脂成分の合計量に対して、0.02〜0.8mmol/gである請求項6に記載の水性中塗り塗料組成物。
- 水酸基及びカルボキシル基含有樹脂(A)及びウレタン変性ポリエステル樹脂(D)と硬化剤(B)との割合が、両者の合計固形分100重量%に基づいて、樹脂(A)及び樹脂(D)が85〜60重量%で硬化剤(D)が15〜40重量%である請求項6に記載の水性中塗り塗料組成物。
- 更に、平均粒子径が150nm以下の架橋樹脂微粒子(E)を含有する請求項1に記載の水性中塗り塗料組成物。
- 架橋樹脂微粒子(E)の配合割合が、前記硬化性樹脂成分100重量部に対して1〜10重量部である請求項9に記載の水性中塗り塗料組成物。
- 更に、扁平状粒子でない顔料を含有する請求項1に記載の水性中塗り塗料組成物。
- 被塗物に、下塗り塗膜、中塗り塗膜、次いで上塗り塗膜を形成して、複層塗膜を形成する方法であって、中塗り塗膜を請求項1に記載の水性中塗り塗料組成物を用いて形成することを特徴とする複層塗膜形成方法。
- 被塗物が、自動車車体である請求項12に記載の複層塗膜形成方法。
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JP5350430B2 (ja) * | 2011-04-19 | 2013-11-27 | 本田技研工業株式会社 | 水性中塗り塗料組成物 |
CN103906815B (zh) * | 2011-11-04 | 2016-08-24 | 威士伯采购公司 | 包装制品的涂料组合物 |
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CA2183187C (en) * | 1995-08-25 | 2001-01-02 | Akira Kasari | Aqueous colored base coating composition and method for forming topcoat |
JPH10231454A (ja) * | 1997-02-19 | 1998-09-02 | Nippon Paint Co Ltd | 熱硬化性水性塗料組成物およびその塗装方法 |
JP2002038104A (ja) | 2000-07-27 | 2002-02-06 | Nippon Paint Co Ltd | 中塗り塗料組成物並びに塗膜形成方法及び被塗物 |
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JP2002254024A (ja) | 2001-02-28 | 2002-09-10 | Nippon Paint Co Ltd | 塗膜形成方法及びこの方法により得られる塗膜並びに塗料組成物 |
JP2002294148A (ja) | 2001-03-30 | 2002-10-09 | Nippon Paint Co Ltd | 水性中塗り塗料組成物 |
JP3974759B2 (ja) | 2001-07-05 | 2007-09-12 | 関西ペイント株式会社 | 水性中塗り塗料 |
JP2003105257A (ja) | 2001-09-27 | 2003-04-09 | Nippon Paint Co Ltd | 水性中塗り塗料組成物 |
CN1460561B (zh) * | 2002-02-28 | 2012-01-04 | 关西涂料株式会社 | 汽车车体的涂饰方法 |
JP4139267B2 (ja) * | 2003-05-15 | 2008-08-27 | マツダ株式会社 | 塗膜形成方法 |
CA2572854A1 (en) * | 2004-07-22 | 2006-01-26 | Kansai Paint Co., Ltd. | Thermosetting water-based coating composition and method of forming coating film |
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