JP2018538388A - 架橋ポリウレタンバインダー及び特定の溶媒組成物を含む水性ベースコート材料 - Google Patents
架橋ポリウレタンバインダー及び特定の溶媒組成物を含む水性ベースコート材料 Download PDFInfo
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- JP2018538388A JP2018538388A JP2018522908A JP2018522908A JP2018538388A JP 2018538388 A JP2018538388 A JP 2018538388A JP 2018522908 A JP2018522908 A JP 2018522908A JP 2018522908 A JP2018522908 A JP 2018522908A JP 2018538388 A JP2018538388 A JP 2018538388A
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Classifications
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Abstract
【解決手段】
本発明は、水性ポリウレタン−ポリウレア分散体(PD)を含む顔料入り水性ベースコート材料であって、その分散体は、平均粒径(体積平均)が40〜2000nmでゲル分率が少なくとも50質量%の、その分散体中に存在するポリウレタン−ポリウレア粒子を有し、そのポリウレタン−ポリウレア粒子は、各々の場合に反応した形態で、
(Z.1.1)イソシアネート基を含有し、アニオン性基及び/又はアニオン性基に変換することができる基を含む、少なくとも1種のポリウレタンプレポリマー、及びまた、
(Z.1.2)2個の一級アミノ基及び1個又は2個の二級アミノ基を含む少なくとも1種のポリアミン
を含み、
特定の溶媒組成物を含む、水性ベースコート材料に関する。
本発明はまた、分散体(PD)を含むベースコート材料を使用する方法、及び、そのベースコート材料を使用して生成するマルチコートペイント系にも関する。
Description
(Z.1.1)イソシアネート基を含有し、アニオン性基及び/又はアニオン性基に変換することができる基を含む、少なくとも1種のポリウレタンプレポリマー、及びまた、
(Z.1.2)2個の一級アミノ基及び1個又は2個の二級アミノ基を含む少なくとも1種のポリアミン
を含む。
その水性ベースコート材料は、HLBが5と15の間で20℃での水溶解度が>1.5質量%の溶媒(L1)からなる群から選択される溶媒を、そのベースコート材料中に存在する溶媒(L)の総量に対して合計で9質量%未満含有し、
溶媒(L)のHLBは、次のように規定され、
HLB(L)=20×(1−M((L)の親油性画分)/M(L))、
溶媒(L)の親油性画分は、次の炭素含有基:すなわち、n=1から3であるすべてのCHn基(ただし、当該基は、
(i)OH、NH2、CO2Hに対してα位にない、
(ii)末端OH基を有するエチレンオキシド鎖に位置するエチレンオキシド単位中にない、及び/又は
(iii)−O−、NH−から選択される架橋性官能基に対してα位の環状分子又は分子部分中にない、
ことを条件とする)、
で構成される。
HLB(L)=20×(1−M((L)の親油性画分)/M(L))、
溶媒(L)の親油性画分は、次の炭素含有基:すなわち、n=1から3であるすべてのCHn基(ただし、当該基は、
(i)OH、NH2、CO2Hに対してα位にない、
(ii)末端OH基を有するエチレンオキシド鎖に位置するエチレンオキシド単位中にない、及び/又は
(iii)−O−、NH−から選択される架橋性官能基に対してα位の環状分子又は分子部分中にない、
ことを条件とする)、
で構成される。
(1)水性ベースコート材料が基材に塗布され、
(2)段階(1)において塗布されたコーティング材料からポリマーフィルムが形成され、
(3)クリアコート材料が結果として生じたベースコートフィルムに塗布され、その後、
(4)ベースコートフィルムがクリアコートフィルムとともに硬化され、
本方法は、段階(1)において使用される水性ベースコート材料が、本発明のベースコート材料であることを特徴とする。
1.固形分含量
別途指示の無い限り、下文においては固体分率とも呼ばれる固形分含量は、130℃、60分、初期質量1.0gで、DIN EN ISO 3251に従って判定した。本発明の文脈において、公式規格に対する言及がなされる場合、これは無論出願日時点において最新だった規格のバージョンのことを意味するか、その日付においては最新のバージョンが存在しない場合には、最も近い最新のバージョンのことを意味する。
以下ではNCO含有量とも呼ばれるイソシアネート含有量は、DIN EN ISO 3251、DIN EN ISO 11909、及びDIN EN ISO 14896に基づく方法で、過剰なキシレン中2%強度のN,N−ジブチルアミン溶液を、アセトン/N−エチルピロリドン(1:1、容量%)中の試料の均一な溶液に添加し、過剰なアミンを0.1Nの塩酸を用いて電位差逆滴定することによって判定した。ポリマーのNCO含有量は、固形物に基づいて、溶液中のポリマーの分率(固形分含量)によって逆算できる。
ヒドロキシル価は、R.−P.Krueger、R.Gnauck and R.Algeier、Plaste und Kautschuk、20、274(1982年)に基づいて、触媒としての4−ジメチルアミノピリジンの存在下において、室温のテトラヒドロフラン(THF)/ジメチルホルムアミド(DMF)溶液中の無水酢酸を用いて、アセチル化の後に残った過剰な無水酢酸を完全に加水分解し、水酸化カリウムのアルコール溶液を用いて酢酸の電位差逆滴定を実行することによって判定した。60分間のアセチル化時間は、すべての場合において、完全な変換を確保するのに十分であった。
酸価は、DIN EN ISO 2114に基づいて、テトラヒドロフラン(THF)/水(9容量部のTHFと1容量部の蒸留水)の均質な溶液中において、水酸化カリウムのエタノール溶液を用いて判定した。
構成成分xの中和度は、その構成成分中に存在するカルボン酸基の物質量(酸価によって決定)と、使用された中和剤の物質量とから計算した。
アミン等価質量(溶液)は、溶液のアミン含有量を判定するために役立ち、以下のように確認した。分析用の試料を室温で氷酢酸中に溶解させ、クリスタルバイオレットの存在下において、氷酢酸中0.1Nの過塩素酸に対して滴定した。試料の初期質量と過塩素酸の消費からアミン等価質量(溶液)、すなわち1モルの過塩素酸を中和するために必要な塩基性アミンの溶液の質量が得られる。
一級アミノ基のブロック度は、IR分光法によって判定した。判定は、Nexus FT IR分光計(Nicolet社より)を用いて、3310cm−1における吸収極大のIRセル(d=25mm、KBr窓)の補助で、使用されたアミンの濃度系列、及び1166cm−1における吸収極大(内部標準)に対する標準化に基づいて25℃で行った。
混合物、例えば水性分散体中の有機溶媒の量は、ガスクロマトグラフィーによって判定した(Agilent 7890A、ポリエチレングリコール相を有する50mシリカキャピラリーカラム又はポリジメチルシロキサン相を有する50mシリカキャピラリーカラム、ヘリウムキャリアガス、250℃スプリットインジェクター、40〜220℃のオーブン温度、フレームイオン化検出器、275℃の検出器温度、内部標準としてのn−プロピルグリコール)。
数平均モル質量(Mn)は、別途指示の無い限り、E.Schroeder、G.Mueller、K.F.Arndt、「Leitfaden der Polymercharakterisierung」[ポリマー特性評価の原理]、Akademie−Verlag、Berlin、47〜54頁、1982年の方法により、蒸気圧浸透圧計10.00(Knauer社より)を用いて、使用される機器の実験的較正定数を決定するためにベンゾフェノンを較正物質として用いて、50℃のトルエン中の濃度系列に対して判定した。
本発明による使用方法のための分散体(PD)中に存在するポリウレタン−ポリウレア粒子の平均粒径(体積平均)は、本発明の文脈において、光錯乱によって判定した。測定に採用したのは具体的には、光子相関分光法(PCS)であった。
本発明による使用方法のための分散体(PD)中に存在するポリウレタン−ポリウレア粒子(ミクロゲル粒子)のゲル分率は、本発明の文脈において、質量測定で判定する。ここでは、まず第一に、存在するポリマーを、水性分散体(PD)の試料(初期質量1.0g)から凍結乾燥によって単離した。凝固温度(試料の電気抵抗が、温度をさらに低下させた場合でもそれ以上さらなる変化を示さない温度)を判定した後、慣例的に5mbar〜0.05mbarの乾燥真空圧範囲で、凝固温度よりも10℃低い乾燥温度において、完全に凍結した試料をその本乾燥に供した。ポリマーの下側の加熱表面の温度を段階的に25℃まで上昇させることで、ポリマーの急速凍結乾燥を達成した。典型的には12時間の乾燥時間の後、単離されたポリマーの量(固体分率、凍結乾燥によって判定)は一定となり、凍結乾燥を延長した場合でもいかなる変化も経なかった。ポリマーの下側の表面の温度を30℃にして引き続き乾燥させ、周囲圧力を最大まで低減する(典型的には、0.05〜0.03mbar)ことで、ポリマーの最適な乾燥がなされた。
有機溶媒の水への溶解度は、20℃において以下のように判定した。当該有機溶媒及び水を好適なガラス容器内で合わせ、混合し、続いて混合物を平衡化させる。水及び溶媒の量は、平衡の後に互いから分離した2つの相が得られるように選択した。平衡させた後、水性相(すなわち、有機溶媒よりも多くの水を含有する層)からシリンジを用いて試料を採取し、この試料をテトラヒドロフランを用いて1/10の比で希釈し、ガスクロマトグラフィーによって溶媒の分率を判定した(条件については、セクション8.溶媒含有量を参照)。
ジエチレントリアミンジケチミンを、メチルエチルケトン中の部分的に中和されたm−テトラメチルキシレンジイソシアネート系ポリウレタンプレポリマーの過剰量に添加し、続いて末端一級アミノ基を架橋させ、その後水中に分散させることによる、ポリエステルウレタンウレアの本発明による使用方法のためのミクロゲルの製造
撹拌器、内蔵温度計、還流凝縮器、及び電気加熱を備えた反応容器において、570.0質量部の直鎖状ポリエステルポリオールと、27.7質量部のジメチロールプロピオン酸(GEO Speciality Chemicals社より)とを、窒素下で、344.4質量部のメチルエチルケトン中に溶解させた。この直鎖状ポリエステルジオールは、二量体化脂肪酸(Pripol(登録商標)1012、Croda社より)、イソフタル酸(BP Chemicals社より)、及びヘキサン−1,6−ジオール(BASF SE社より)から予め製造した(出発材料の質量比:二量体の脂肪酸対イソフタル酸対ヘキサン−1,6−ジオール=54.00:30.02:15.98)。この直鎖状ポリエステルジオールは、73mgKOH/g固体分率のヒドロキシル価、3.5mgKOH/g固体分率の酸価、1379g/molの算定数平均モル質量、及び蒸気圧浸透圧法によって判定した1350g/molの数平均モル質量を有した。
次いで、30.8質量部の、ジエチレントリアミンジケチミンの71.9質量%メチルイソブチルケトン希釈液を1分間にわたって混合した(プレポリマーのイソシアネート基対ジエチレントリアミンジケチミン(1個の二級アミノ基を有する)の比:5:1 mol/mol、ブロックされた一級アミノ基1個当たり2個のNCO基に相当する)。また、プレポリマー溶液への添加後に、短時間で1℃反応温度が上昇した。ジエチレントリアミンジケチミンのメチルイソブチルケトン希釈液は、メチルイソブチルケトン中の、ジエチレントリアミン(BASF SE社より)とメチルイソブチルケトンとの反応における反応水を110〜140℃で共沸除去することによって予め製造した。メチルイソブチルケトンを用いた希釈によって、124.0g/eqのアミン等価質量(溶液)への調整を実行した。IR分光法を用いて、3310cm−1における残存吸収に基づき、一級アミノ基のブロッキングを98.5%と判定した。
40℃で30分間撹拌した後、反応器の内容物を、7分間にわたって1206質量部の脱イオン水(23℃)中に分散させた。結果として生じた分散体から、45℃の減圧下においてメチルエチルケトンを蒸留し、溶媒及び水のあらゆる喪失を脱イオン水で埋め合わせて、40質量%の固形分含量を得た。
メチルエチルケトン含有量(GC): 0.3質量%
メチルイソブチルケトン含有量(GC): 0.1質量%
粘度(23℃、回転粘度計、せん断速度=1000/s):15mPa・s
酸価 17.1mgKOH/g
固形分含量
中和度(計算) 49%
pH(23℃) 7.4
粒径(光子相関スペクトロスコピー、体積平均) 156nm
ゲル分率(凍結乾燥) 83.3質量%
ゲル分率(130℃) 83.7質量%
部分的に中和されたジシクロヘキシルメタン4,4’−ジイソシアネート系ポリエステルウレタンのメチルエチルケトン溶液の分散による、架橋粒子を含まないポリエステルウレタンの分散体の製造
メチルエチルケトン含有量(GC): 0.2質量%
粘度(23℃、回転粘度計、せん断速度=1000/s):135mPa・s
酸価 19.9mgKOH/g
固形分含量
pH(23℃) 7.8
粒径(光子相関スペクトロスコピー、体積平均) 46nm
ゲル分率(凍結乾燥) −0.7質量%
ゲル分率(130℃) −0.3質量%
塗布比較のために、架橋粒子を含有しないポリウレタン分散体VD1を有する、標準水系ベースコート材料BL−V1を製造した(WO92/15405、15頁、16〜20行目に従う)。すべての本発明の水系ベースコート材料及び更なる比較例の水系ベースコート材料とは対照的に、BL−V1は塗布及び乾燥中に金属パネルから縦方向に流れてしまうことを防止するため、フィロシリケート増粘剤を含む。
カーボンブラックペーストは、25質量部の、国際特許出願WO91/15528のバインダー分散体Aにより製造したアクリル化ポリウレタン分散体、10質量部のカーボンブラック、0.1質量部のメチルイソブチルケトン、1.36質量部のジメチルエタノールアミン(脱イオン水中10%強度)、2質量部の市販のポリエーテル(Pluriol(登録商標)P900、BASF SE社より)、及び61.45質量部の脱イオン水から生成した。
レッドペーストは、40質量部の、国際特許出願WO91/15528のバインダー分散体Aにより製造したアクリル化ポリウレタン分散体、34.5質量部のCinilex(登録商標)DPPレッド、2質量部の市販のポリエーテル(Pluriol(登録商標)P900、BASF SE社より)、3質量部の1−プロポキシ−2−プロパノール及び20.5質量部の脱イオン水から生成した。
ブルーペーストは、69.8質量部の、国際特許出願WO91/15528のバインダー分散体Aにより製造したアクリル化ポリウレタン分散体、12.5質量部のPaliogen(登録商標)ブルーL6482、1.5質量部のジメチルエタノールアミン(脱イオン水中10%強度)、1.2質量部の市販のポリエーテル(Pluriol(登録商標)P900、BASF SE社より)、及び15質量部の脱イオン水から生成した。
3%ナトリウムリチウムマグネシウムフィロシリケートLaponite(登録商標)RD(Altana−Byk社より)及び3%Pluriol(登録商標)P900(BASF SE社より)の水溶液
2)流れ限界、単位μm:流れが発生したフィルム厚
3)ポップ限界、単位μm:流れが発生したフィルム厚
4)ピンホール限界、単位μm:くさび形のベースコート材料、及び二成分クリアコート材料の一定の層を塗布し、140℃の空気循環オーブン内で20分間一緒に硬化させた後に、ピンホールが発生するベースコートフィルムのフィルム厚
5)ピンホールの数:縁部の長さが30cm×50cmであるコーティングされた金属パネルのピンホール限界からのピンホールの数
3%ナトリウムリチウムマグネシウムフィロシリケートLaponite(登録商標)RD(Altana−Byk社より)及び3%Pluriol(登録商標)P900(BASF SE社より)の水溶液
ホワイトペーストは、43質量部の、国際特許出願WO91/15528のバインダー分散体Aのように製造したアクリル化ポリウレタン分散体、50質量部のチタニウムルチル2310、3質量部の1−プロポキシ−2−プロパノール及び4質量部の脱イオン水から生成した。
2)ポップ限界、単位μm:ポップが発生したフィルム厚
3)ピンホール限界、単位μm:くさび形のベースコート材料、及び二成分クリアコート材料の一定の層を塗布し、140℃の空気循環オーブン内で20分間一緒に硬化させた後に、ピンホールが発生するベースコートフィルムのフィルム厚
4)ピンホールの数:縁部の長さが30cm×50cmのコーティングされた金属パネルのピンホール限界からのピンホールの数
Claims (15)
- 水性ポリウレタン−ポリウレア分散体(PD)を含む顔料入り水性ベースコート材料であって、前記分散体は、平均粒径(体積平均)が40〜2000nmでゲル分率が少なくとも50質量%の、前記分散体中に存在するポリウレタン−ポリウレア粒子を有し、前記ポリウレタン−ポリウレア粒子は、各々の場合に反応した形態で、
(Z.1.1)イソシアネート基を含有し、アニオン性基及び/又はアニオン性基に変換することができる基を含む、少なくとも1種のポリウレタンプレポリマー、及びまた、
(Z.1.2)2個の一級アミノ基及び1個又は2個の二級アミノ基を含む少なくとも1種のポリアミン
を含み、
前記水性ベースコート材料は、HLBが5と15の間で20℃での水溶解度が>1.5質量%の溶媒(L1)からなる群から選択される溶媒を、前記ベースコート材料中に存在する溶媒(L)の総量に対して合計で9質量%未満含有し、
溶媒(L)のHLBは、次のように規定され、
HLB(L)=20×(1−M((L)の親油性画分)/M(L))、
溶媒(L)の親油性画分は、次の炭素含有基:すなわち、n=1から3であるすべてのCHn基(ただし、当該基は、
(i)OH、NH2、CO2Hに対してα位にない、
(ii)末端OH基を有するエチレンオキシド鎖に位置するエチレンオキシド単位にない、及び/又は
(iii)−O−、NH−から選択される架橋性官能基に対してα位の環状分子又は分子部分中にない、
ことを条件とする)、
で構成される、顔料入り水性ベースコート材料。 - 前記ポリウレタン−ポリウレア分散体のプレポリマー(Z.1.1)が、カルボン酸基を含む、請求項1に記載の顔料入り水性ベースコート材料。
- 前記分散体(PD)が、最大で少なくとも90質量%までのポリウレタン‐ポリウレア粒子及び水からなる、請求項1又は2に記載の顔料入り水性ベースコート材料。
- メラミン-ホルムアルデヒド樹脂、及び前記分散体(PD)中に存在する前記ポリマーとは異なる少なくとも1種のヒドロキシ官能性ポリマーをさらに含む、請求項1から3に記載の顔料入り水性ベースコート材料。
- 前記ベースコート材料が、7.8を超えるHLB及び20℃で7.7を超える水溶解度を有する溶媒(L1)からなる群から選択される溶媒を、前記ベースコート材料中に存在する前記溶媒(L)の総量に対して合計で9質量%未満含有する、請求項1から4に記載の顔料入り水性ベースコート材料。
- 水性ポリウレタン−ポリウレア分散体(PD)を含む顔料入り水性ベースコート材料であって、前記分散体は、平均粒径(体積平均)が40〜2000nmでゲル分率が少なくとも50質量%の、前記分散体中に存在するポリウレタン−ポリウレア粒子を有し、前記ポリウレタン−ポリウレア粒子は、各々の場合に反応した形態で、
(Z.1.1)イソシアネート基を含有し、アニオン性基及び/又はアニオン性基に変換することができる基を含む、少なくとも1種のポリウレタンプレポリマー、及びまた、
(Z.1.2)2個の一級アミノ基及び1個又は2個の二級アミノ基を含む少なくとも1種のポリアミン
を含み、
前記水性ベースコート材料は、前記ベースコート材料中に存在する溶媒(L)の総量に対して合計で9質量%未満のブチルグリコール、ブチルジグリコール、イソプロパノール、n−プロパノール、1−プロポキシ−2−プロパノール、イソブタノール及び/又はn−ブタノールを含有する、顔料入り水性ベースコート材料。 - 水性ポリウレタン−ポリウレア分散体(PD)を含む顔料入り水性ベースコート材料であって、前記分散体は、平均粒径(体積平均)が40〜2000nmでゲル分率が少なくとも50質量%の、前記分散体中に存在するポリウレタン−ポリウレア粒子を有し、前記ポリウレタン−ポリウレア粒子は、各々の場合に反応した形態で、
(Z.1.1)イソシアネート基を含有し、アニオン性基及び/又はアニオン性基に変換することができる基を含む、少なくとも1種のポリウレタンプレポリマー、及びまた、
(Z.1.2)2個の一級アミノ基及び1個又は2個の二級アミノ基を含む少なくとも1種のポリアミン
を含み、
前記水性ベースコート材料は、前記ベースコート材料中に存在する溶媒(L)の総量に対して合計で9質量%未満のブチルグリコールを含有する、顔料入り水性ベースコート材料。 - 15から60質量%、好ましくは30から55質量%の固形分含量を有する、請求項1から7に記載の顔料入り水性ベースコート材料。
- 1000s−1のせん断荷重の下で、23℃において40から180mPa・s、好ましくは50から150mPa・s、及びより好ましくは60から135mPa・sの粘度を有する、請求項1から8に記載の顔料入り水性ベースコート材料。
- 前記ベースコート材料の固形分含量と前記ベースコート材料中の水の分率の百分率合計が少なくとも70質量%である、請求項1から9に記載の顔料入り水性ベースコート材料。
- 前記ベースコート材料の固形分含量と前記ベースコート材料中の水の分率の百分率合計が少なくとも80質量%である、請求項1から10に記載の顔料入り水性ベースコート材料。
- 請求項1から11のいずれか一項に記載の顔料入り水性ベースコート材料を、マルチコートペイント系におけるベースコートフィルムの、保存安定性及びまた塗布特性、より具体的には、ピンホール及びポップに関する安定性を改善するために、使用する方法。
- マルチコートペイント系を生成する方法であって、前記方法において
(1) 顔料入り水性ベースコート材料を基材に塗布し、
(2) ポリマーフィルムを段階(1)で塗布したコーティング材料から形成し、
(3) 得られたベースコートフィルムにクリアコート材料を塗布し、そして
(4) 前記ベースコートフィルムを前記クリアコートフィルムと一緒に硬化させるものであり、
請求項1から11のいずれか一項に記載の顔料入り水性ベースコート材料を、段階(1)で使用する方法。 - 前記基材が硬化した電着コートフィルムでコーティングした金属基材であり、電着コートフィルムに塗布した全てのフィルムを一緒に硬化させる、請求項13に記載の方法。
- 請求項12から14のいずれか一項に記載の方法によって生成することができる、マルチコートペイント系。
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