JP2010280852A - 水性塗料用樹脂組成物、該水性塗料用樹脂組成物を配合してなる塗料 - Google Patents
水性塗料用樹脂組成物、該水性塗料用樹脂組成物を配合してなる塗料 Download PDFInfo
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- JP2010280852A JP2010280852A JP2009136492A JP2009136492A JP2010280852A JP 2010280852 A JP2010280852 A JP 2010280852A JP 2009136492 A JP2009136492 A JP 2009136492A JP 2009136492 A JP2009136492 A JP 2009136492A JP 2010280852 A JP2010280852 A JP 2010280852A
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 4
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Landscapes
- Paints Or Removers (AREA)
Abstract
【解決手段】(A)水溶性および/または水分散性樹脂、(B)オルガノシリケートおよび/またはその変性物、(C)アルコキシシリル基の加水分解縮合反応を促進させる硬化触媒、(D)酸解離定数の逆数の対数値(pKa)が7以下のヒンダードアミン系光安定剤(HALS)を含有する2液または多成分型水性塗料用樹脂組成物。
【選択図】なし
Description
前記、(D)酸解離定数の逆数の対数値(pKa)が7以下のヒンダードアミン系光安定剤(HALS)の環状アミン部の構造が次の一般式(1)または(2)である請求項1記載の2液または多成分型水性塗料用樹脂組成物。
(A)水溶性および/または水分散性樹脂を含有する基材(I)と(B)オルガノシリケートおよび/またはその変性物、(C)アルコキシシリル基の加水分解縮合反応を促進させる硬化触媒、(D)酸解離定数の逆数の対数値(pKa)が7以下のヒンダードアミン系光安定剤(HALS)、(E)分子中に反応性官能基と親水基を有する水溶性および/または水分散性硬化剤を含有してなる助剤(II)を使用前に混合して用いる2液型あるいは多成分型である請求項1または2の何れか1項に記載の2液または多成分型水性塗料用樹脂組成物。(請求項3)
前記、(D)酸解離定数の逆数の対数値(pKa)が7以下のヒンダードアミン系光安定剤(HALS)が、分子量600未満のもの(d1)と分子量600以上のもの(d2)を併用して用いる請求項1〜3の何れか1項に記載の2液または多成分型水性塗料用樹脂組成物。(請求項4)
前記、(C)アルコキシシリル基の加水分解・縮合反応を促進させる硬化触媒が、有機錫化合物、酸性リン酸エステルおよび酸性リン酸エステルとアミンの反応物の中から選ばれる1種又は2種以上であることを特徴とする請求項1〜4の何れか1項に記載の2液または多成分型水性塗料用樹脂組成物。(請求項5)
前記、(A)水溶性および/または水分散性樹脂がポリオキシアルキレン鎖を有する樹脂である請求項1〜5の何れか1項に記載の2液または多成分型水性塗料用樹脂組成物。(請求項6)
前記、(A)水溶性および/または水分散性樹脂がアルコキシシリル基含有アクリル樹脂である請求項1〜6の何れか1項記載の2液または多成分型水性塗料用樹脂組成物。(請求項7)
請求項1〜7の何れか1項記載の水性塗料用樹脂組成物を配合してなる塗料組成物。(請求項8)
基材(I)に(A)水溶性および/または水分散性樹脂に加え、(F)二酸化ケイ素、酸化アルミニウム、二酸化ジルコニウムの少なくとも3種類の表面処理を施した二酸化チタンを配合してなる請求項8記載の塗料組成物。(請求項9)
(A)水溶性および/または水分散性樹脂としては、塗膜形成能を有するものであれば特に制限なく従来公知のものを使用でき、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、フッ素樹脂エマルション、エポキシ樹脂エマルション、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、メラミン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。また、これらは単独で使用しても2種以上を併用しても良い。これらの中で形成塗膜の耐候性などの点から、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、フッ素樹脂エマルション及びウレタン樹脂エマルションよりなる群から選ばれる少なくとも1種であることが好ましい。
R5R6 (3-n)SiXn (3)
(式中、R5は重合性二重結合を有する1価有機基、R6は炭素数1〜4のアルキル基、Xは炭素数1〜4のアルコキシ基、nは2又は3)で示される有機けい素化合物で、2又は3個のアルコキシ基を有し、反応性二重結合を有する化合物である。その具体例としては、ビニルトリメトキシシラン、γ−(メタ)アクリロキシプロピルトリメトキシシラン、ビニルトリエトキシシラン、γ−(メタ)アクリロキシプロピルトリエトキシシラン、γ−(メタ)アクリロキシプロピルトリプロポキシシラン、γ−(メタ)アクリロキシプロピルトリブトキシシラン、ビニルメチルジメトキシシラン、γ−(メタ)アクリロキシプロピルメチルジメトキシシラン、ビニルメチルジエトキシシラン、γ−(メタ)アクリロキシプロピルメチルジエトキシシラン、γ−(メタ)アクリロキシプロピルメチルジプロポキシシラン、γ−(メタ)アクリロキシプロピルメチルジブトキシシランなどが上げられ、これらを1種又は2種以上併用して用いることができる。なかでも、エマルションの保存安定性の観点から、Xは炭素数2〜4が特に好ましい。
R7R8 (3-a)SiYa (4)
(式中、R7は重合性二重結合を有する1価有機基、R8は炭素数1〜4のアルキル基、Yは炭素数1〜4のアルコキシ基、aはa<nの関係を有する1又は2の整数)で示される有機けい素化合物で、1又は2個のアルコキシ基を有し、反応性二重結合を有する化合物である。その具体例としては、ビニルメチルジメトキシシラン、ビニルメチルジエトキシシラン、γ−(メタ)アクリロキシプロピルメチルジメトキシシラン、γ−(メタ)アクリロキシプロピルメチルジエトキシシラン、γ−(メタ)アクリロキシプロピルメチルジプロポキシシラン、γ−(メタ)アクリロキシプロピルメチルジブトキシシラン、ビニルジメチルメトキシシラン、ビニルジメチルエトキシシラン、γ−(メタ)アクリロキシプロピルジメチルエトキシシラン、γ−(メタ)アクリロキシプロピルジメチルメトキシシラン、γ−(メタ)アクリロキシプロピルジメチルプロポキシシラン、γ−(メタ)アクリロキシプロピルジメチルブトキシシランなどが上げられ、これらを1種又は2種以上併用して用いることができる。
オルガノシリケートは、加水分解性珪素基を含有する化合物であり、一般式(5)として現される化合物であり、エマルションに添加することにより、得られた塗膜の耐汚染性を大幅に向上させる。その具体的化合物としては、テトラメトキシシラン、テトラエトキシシラン、テトラ−n−プロポキシシラン、テトラ−i−プロポキシシラン、テトラ−n−ブトキシシラン、テトラ−i−ブトキシシラン、テトラ−t−ブトキシシラン及びそれらの部分加水分解・縮合物が例示できる。中でもエチルシリケート40、エチルシリケート48が好ましい。上記化合物は1種単独でもよく、2種以上を併用しても良い。また、同一分子中に異なったアルコキシシリル基を含有するオルガノシリケートも使用可能である。例えば、メチルエチルシリケート、メチルプロピルシリケート、メチルブチルシリケート、エチルプロピルシリケート、プロピルブチルシリケートなどである。これらの置換基の比率0〜100%の間で任意に変更可能である。また、これらのシリケートの部分加水分解・縮合物も使用可能であると記述したが、縮合度は1〜20程度が好ましい。更に好ましい縮合度の範囲は、3〜15である。
(式中、Rは同じかまたは異なり炭素数1〜4のアルキル基)
本発明の水性樹脂組成物を塗装する際にアルコキシシリル基の加水分解縮合反応を促進させる硬化触媒を添加することにより、架橋反応が促進される。硬化触媒としては、有機金属化合物、酸性触媒、塩基性触媒が使用される。
ヒンダードアミン系光安定剤(HALS)は、塗膜劣化時の生じるラジカルを補足し、無害化することで、塗膜の耐候性を向上させる化合物であり、一般的に用いられている。しかし、一般的の用いられているHALSは、酸解離定数の逆数の対数値(pKa)が高い、すなわち塩基性を示すものが多く、これらの塩基性の高いHALSをオルガノシリケートまたはその変性物を用いて耐汚染性を付与した水性塗料に添加すると、多くの場合、耐汚染性能を低下させる。ところが、pKaが7以下のHALSは、オルガノシリケートまたはその変性物を用いて耐汚染性を付与した水性塗料に添加しても、耐汚染性の低下が見られない。好ましいpKaは6.5以下、1.5以上、特に好ましいpKaは6以下2.0以上である。
一般式(1)の構造を有する市販品としては、例えば、チバ・ジャパン(株)製TINUVIN 123、TINUVIN 152、TINUVIN NOR 371 FF、TINUVIN XT855 FF、TINUVIN XT850 FF、TINUVIN 5100(株)ADEKA製アデカスタブLA−81、クラリアントジャパン(株)製Hostavin 3058 Liq.、Hostavin 3068 Liq.等が挙げられる。
TINUVIN 123:
TINUVIN 622:
分子中に反応性官能基と親水性基を有する水溶性および/または水分散性硬化剤とは、親水基、疎水基に加え、さらに反応性官能基を有するもの物質のことである。
着色に用いる白色顔料としての通常、二酸化チタンが用いられる。その二酸化チタンは光触媒反応性を有しており、塗膜劣化の原因となる。塗料用に市販されている二酸化チタンは、その光触媒反応を抑える目的や分散安定性を付与するために、各種表面処理が行われる。その表面処理の材料として、二酸化珪素、酸化アルミニウム、二酸化ジルコニウム、リン酸エステル、ポリオールなどがあげられる。
D−918、D−2667、石原産業(株)製PFC−105、ドイツ国クロノス社製KRONOS2315、KRONOS2310等があげられる。
撹拌機、還流冷却器、窒素ガス導入管および滴下ロートを備えた反応容器に、脱イオン水192重量部、Newcol−707SN(日本乳化剤(株)製:有効成分30%)0.46重量部、5%炭酸水素ナトリウム水溶液1.0重量部を仕込み、窒素ガスを導入しつつ50℃に昇温した。昇温後、7%t−ブチルハイドロパーオキサイド水溶液2.0重量部、10%Bruggolite FF−6水溶液1.4重量部、硫酸第一鉄・7水和物(0.10%)/エチレンジアミン四酢酸二ナトリウム(0.40%)混合水溶液2.8部を添加し、表1(A−1〜3)コア部記載のモノマー混合物に、アデカリアソープSR−1025((株)ADEKA製:有効成分25%)9.6重量部、アデカリアソープER−20((株)ADEKA製:有効成分75%)1.5重量部および脱イオン水50重量部を加え乳化したモノマー乳化液を160分かけて等速追加した。その間、7%t−ブチルハイドロパーオキサイド水溶液1.6重量部および2.5%Bruggolite FF−6水溶液3.2重量部を2回に分けて添加した。モノマー乳化液追加終了後、1時間後重合を行った。
合成した樹脂組成物(A−1〜3)および市販の水性樹脂組成物を用い、表2の顔料ペーストを用いて、表3に示す配合処方で塗料を作成した。
TATANIX JR−901S:テイカ(株)製(表面処理:酸化アルミニウム、二酸化ジルコニウム)
Ti−Pure R−706:デュポン(株)製(表面処理:二酸化珪素、酸化アルミニウム、ポリオール)
ゼッフルSE−310:ダイキン工業(株)製フッ素樹脂エマルション
撹拌機、還流冷却器、窒素ガス導入管を備えた容器に表4記載の原料を上から順番に投入した。投入終了後40℃に昇温し、60分撹拌し、耐汚染性付与組成物(QA−1〜8)を得た。
プログライドDMM:ダウ・ケミカル日本(株)製ジプロピレングリコールジメチルエーテル
カルボジライトV−04B:日清紡ケミカル(株)製ポリカルボジイミド
シリケート40:多摩化学工業(株)製テトラエトキシシランの部分加水分解縮合物(シリカ残存比率40%)
エンバイロジェムAD−01:日信化学工業(株)製アセチレングリコール系界面活性剤類似品
ユニルーブ70MO−10SB:日油(株)製非イオン性界面活性剤
TINUVIN 123:チバ・ジャパン(株)製ヒンダードアミン系光安定剤、pKa=4.4、分子量:737
TINUVIN 292:チバ・ジャパン(株)製ヒンダードアミン系光安定剤、pKa=8.9 分子量509
作製した基材(I)に助剤(II)を添加・攪拌混合後、6milのアプリケータを用いて、ガラス板に塗布し、室温で7日間乾燥させた。コニカミノルタ(株)製光沢計Multi−Gloss268を用い、この試験体の入射角60°の光沢値を測定した。
フレキシブル板上にSK#1000プライマー(エスケー化研(株)製、溶剤系2液エポキシ樹脂系下塗材)を塗装し、室温で1日養生後、作製した基材(I)に助剤(II)を添加・攪拌混合後、スプレーで2回塗装し、室温で7日間乾燥させた。この試験板をメタルハライドランプ灯式試験機に600時間入れた。コニカミノルタ(株)製光沢計Multi−Gloss268を用い、あらかじめ測定しておいた試験前の入射角60°の光沢値と試験後の測定値から光沢保持率を算出した。
なお、試験条件は、次の通りである。
照射 63℃ 50% 4時間 照度:85mW/cm2
結露 30℃ 98% 4時間
シャワー 照射中15分間隔に5秒
フレキシブル板上にSK#1000プライマー(エスケー化研(株)製、溶剤系2液エポキシ樹脂系下塗材)を塗装し、室温で1日養生後、作製した基材(I)に助剤(II)を添加・攪拌混合後、スプレーで2回塗装し、室温で7日間乾燥させた。この試験板を大阪府摂津市で南面45度で3カ月間曝露した。汚染性は、曝露初期のL*a*b*表色系で表される明度を色彩色差計(コニカミノルタ(株)製:CR−300)で測定し、曝露前後の明度差の絶対値(ΔL値)を汚染性の尺度とした。また、暴露後の塗膜を軽く水洗し、3時間以上乾燥させた後、水の静的接触角を測定した。
Claims (9)
- (A)水溶性および/または水分散性樹脂、(B)オルガノシリケートおよび/またはその変性物、(C)アルコキシシリル基の加水分解・縮合反応を促進させる硬化触媒、(D)酸解離定数の逆数の対数値(pKa)が7以下のヒンダードアミン系光安定剤(HALS)を含有する2液または多成分型水性塗料用樹脂組成物。
- (A)水溶性および/または水分散性樹脂を含有する基材(I)と(B)オルガノシリケートおよび/またはその変性物、(C)アルコキシシリル基の加水分解縮合反応を促進させる硬化触媒、(D)酸解離定数の逆数の対数値(pKa)が7以下のヒンダードアミン系光安定剤(HALS)、(E)分子中に反応性官能基と親水基を有する水溶性および/または水分散性硬化剤を含有してなる助剤(II)使用前に混合して用いる2液型あるいは多成分型である請求項1または2の何れか1項に記載の2液または多成分型水性塗料用樹脂組成物。
- 前記、(D)酸解離定数の逆数の対数値(pKa)が7以下のヒンダードアミン系光安定剤(HALS)が、分子量600未満のもの(d1)と分子量600以上のもの(d2)を併用して用いる請求項1〜3の何れか1項に記載の2液または多成分型水性塗料用樹脂組成物。
- 前記、(C)アルコキシシリル基の加水分解・縮合反応を促進させる硬化触媒が、有機錫化合物、酸性リン酸エステルおよび酸性リン酸エステルとアミンの反応物の中から選ばれる1種以上であることを特徴とする請求項1〜4の何れか1項に記載の2液または多成分型水性塗料用樹脂組成物。
- 前記、(A)水溶性および/または水分散性樹脂が、ポリオキシアルキレン鎖を有する樹脂である請求項1〜5の何れか1項に記載の2液または多成分型水性塗料用樹脂組成物。
- 前記、(A)水溶性および/または水分散性樹脂が、アルコキシシリル基含有アクリル樹脂である請求項1〜6の何れか1項記載の2液または多成分型水性塗料用樹脂組成物。
- 請求項1〜7の何れか1項記載の水性塗料用樹脂組成物を配合してなる塗料組成物。
- 基材(I)に(A)水溶性および/または水分散性樹脂に加え、(F)二酸化ケイ素、酸化アルミニウム、二酸化ジルコニウムの少なくとも3種類の表面処理を施した二酸化チタンを配合してなる請求項8記載の塗料組成物。
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