JP2016074751A - 水性樹脂組成物、コーティング剤及び物品 - Google Patents
水性樹脂組成物、コーティング剤及び物品 Download PDFInfo
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- JP2016074751A JP2016074751A JP2014203967A JP2014203967A JP2016074751A JP 2016074751 A JP2016074751 A JP 2016074751A JP 2014203967 A JP2014203967 A JP 2014203967A JP 2014203967 A JP2014203967 A JP 2014203967A JP 2016074751 A JP2016074751 A JP 2016074751A
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- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
Description
加熱装置、攪拌機、温度計及び還流冷却管を備えた2リットル4つ口フラスコに、メチルエチルケトン49.9質量部、ポリカーボネートポリオール(1,6−ヘキサンジオールと1,5−ペンタンジオールとジエチルカーボネートとを反応させて得られるポリカーボネートポリオール、数平均分子量2000)50質量部、2,2−ジメチロールプロピオン酸6.8質量部、1,6−ヘキサンジオール6.6質量部、ペンタエリスリトールジアクリレート(一般式(1)中のR1は、炭素原子数3のもので、重合性不飽和基を有する原子団を2つ有するものである。)11.2質量部、メチルヒドロキノン0.0022質量部、及び、2,6−tert−ブチル−p−クレゾール0.022質量部を仕込み、撹拌しながら50℃に調整した。
加熱装置、攪拌機、温度計及び還流冷却管を備えた2リットル4つ口フラスコに、1,4−ビス(3−アクリロイロキシ−2−ヒドロキシプロポキシ)ブタン(一般式(2)中のR1及びR3は炭素原子数2のもので、重合性不飽和基を有する原子団を1つ有するものであり、R2は炭素原子数4のものである。)35.6質量部、メチルヒドロキノン0.007質量部、及び、2,6−tert−ブチル−p−クレゾール0.07質量部を仕込み、攪拌しながら50℃で調整した。
温度計、窒素ガス導入管、攪拌器を備えた窒素置換された容器中で、1,6−ヘキサンジオールとネオペンチルグリコールとアジピン酸とを反応させて得られるポリエステルポリオール(数平均分子量2,000)100質量部と、1,6−ヘキサンジオール10.6質量部と、2,2−ジメチロールプロピオン酸13.4質量部と、ジシクロヘキシルメタンジイソシアネート106.3質量部とを、メチルエチルケトン98質量部に混合し、前記反応容器中の温度80℃の条件下で反応させることによって、末端にイソシアネート基を有するウレタンプレポリマーの有機溶剤溶液を得た。
温度計、窒素ガス導入管、攪拌器を備えた窒素置換された容器中で、1,6−ヘキサンジオールとネオペンチルグリコールとアジピン酸とを反応させて得られるポリエステルポリオール(数平均分子量2,000)100質量部と、1,6−ヘキサンジオール21.2質量部と、2,2−ジメチロールプロピオン酸13.9質量部と、ジシクロヘキシルメタンジイソシアネート106.3質量部とを、メチルエチルケトン93.8質量部に混合し、前記反応容器中の温度80℃の条件下で反応させることによって、末端にイソシアネート基を有するウレタンプレポリマーの有機溶剤溶液を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、N−メチル−2−ピロリドン(以下、「造膜助剤(1)」と略記する。)7質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」;1−ヒドロキシ−シクロヘキシル−フェニル−ケトンとベンゾフェノンの混合物)4質量部を混合することによって水性樹脂組成物(1)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、造膜助剤(1)0.05質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(2)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、造膜助剤(1)60質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(3)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、1,3−ブタンジオール(以下、「造膜助剤(2)」と略記する。)10質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(4)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、ソルビタンモノオレエート(以下、「造膜助剤(3)」と略記する。)1質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(5)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、造膜助剤(3)0.05質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(6)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、造膜助剤(3)60質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(7)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、ポリエーテル変性ポリジメチルシロキサン(BYK株式会社製「BYK−348」;以下、「造膜助剤(4)」と略記する。)0.5質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(4)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、造膜助剤(4)0.05質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(5)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、造膜助剤(2)60質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(10)を得た。
合成例1の不揮発分33質量%ウレタン樹脂(1)水分散体303質量部(ウレタン樹脂(1)として100質量部)、造膜助剤(1)7質量部、造膜助剤(4)0.5質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(11)を得た。
合成例2の不揮発分33質量%ウレタン樹脂(2)水分散体303質量部(ウレタン樹脂(2)として100質量部)、造膜助剤(1)7質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(12)を得た。
合成例3の不揮発分33質量%ウレタン樹脂(3)水分散体303質量部(ウレタン樹脂(3)として100質量部)、造膜助剤(1)7質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(C1)を得た。
合成例3の不揮発分33質量%ウレタン樹脂(3)水分散体303質量部(ウレタン樹脂(3)として100質量部)、造膜助剤(2)0.5質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(C2)を得た。
合成例4の不揮発分33質量%ウレタン樹脂(4)水分散体303質量部(ウレタン樹脂(4)として100質量部)、造膜助剤(1)7質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(C3)を得た。
合成例4の不揮発分33質量%ウレタン樹脂(4)水分散体303質量部(ウレタン樹脂(4)として100質量部)、造膜助剤(2)0.5質量部、及び光重合開始剤(BASFジャパン株式会社製「イルガキュア 500」)4質量部を混合することによって水性樹脂組成物(C4)を得た。
実施例及び比較例で得た各水性樹脂組成物を、塗膜の膜厚が15μmとなるように、それぞれガラス基材の表面に塗布した。前記塗布物を140℃で5分間乾燥した後、高圧水銀灯(株式会社GSユアサ製)を用いて、0.5J/cm2の紫外線を1パス照射することによって、前記ガラス基材の表面に塗膜が積層した物品を得た。
実施例及び比較例で得た各水性樹脂組成物を、塗膜の膜厚が2μmとなるように、それぞれ金属板(未処理鋼板、厚さ0.8mm)の表面に塗布した。前記塗布物を100℃で30秒間乾燥した後、高圧水銀灯(株式会社GSユアサ製)を用いて、0.5J/cm2の紫外線を1パス照射し、前記離型フィルムを除去することによって、前記金属板の表面に塗膜が積層した物品を得た。
△:塗膜の屈曲部位で、塗膜の若干のクラック、または、白いスジ状のシワが見られた。
×:塗膜の屈曲部位の全体で、塗膜の著しいクラックが見られた。
実施例及び比較例で得た水性樹脂組成物の固形分100質量部に対して光重合開始剤(1−ヒドロキシ−シクロヘキシル−フェニル−ケトンとベンゾフェノンの混合物)を4質量部配合して得た配合液を、ガラス基材上に3milのアプリケーターを用いて塗布し、60℃で10分間乾燥後、さらに高圧水銀灯を用いて0.5J/cm2照射し、その後25℃で2日間養生した塗膜を作製した。得られた塗膜の表面に、メチルエチルケトンおよびエタノールを浸み込ませたフェルトで、硬化塗膜上を往復20回ラビングした。ラビング前とラビング後の塗膜の状態を、指触及び目視により判定した。評価基準は下記の通りである。
△:若干の軟化又は光沢低下が認められる。
×:著しい軟化又は光沢低下が認められる。
実施例及び比較例で得た水性樹脂組成物の固形分100質量部に対して光重合開始剤(1−ヒドロキシ−シクロヘキシル−フェニル−ケトンとベンゾフェノンの混合物)を4質量部配合して得た配合液を、アセトンで脱脂した55質量%アルミニウム−亜鉛系合金メッキ鋼板に、バーコーターを使用して乾燥後の膜厚が約1μmになるように塗布し、雰囲気温度100℃の乾燥機に30秒間入れて乾燥し、さらに高圧水銀灯を用いて0.5J/cm2照射することによって、塗膜を作成した。その後、室温で3日間養生したものを試験片とした。
○:錆の発生及び錆に起因した塗膜の膨れや剥がれの生じた面積が、平面部全体に対して5%以上30%未満であった。
△:錆の発生及び錆に起因した塗膜の膨れや剥がれの生じた面積が、平面部全体に対して30%以上60%未満であった。
×:錆の発生及び錆に起因した塗膜の膨れや剥がれの生じた面積が、平面部全体に対して60%以上であった。
実施例及び比較例で得た水性樹脂組成物の固形分100質量部に対して光重合開始剤(1−ヒドロキシ−シクロヘキシル−フェニル−ケトンとベンゾフェノンの混合物)を4質量部配合して得た配合液を、アセトンで脱脂した55質量%アルミニウム−亜鉛系合金メッキ鋼板に、バーコーターを使用して乾燥後の膜厚が約1μmになるように塗布し、雰囲気温度100℃の乾燥機に30秒間入れて乾燥し、さらに高圧水銀灯を用いて0.5J/cm2照射することによって、塗膜を作成した。その後、室温で3日間養生したものを試験片とした。前記試験片を構成する塗膜の表面に1N塩酸をスポットで置き、180分間静置後の塗膜の劣化状態を観察した。
○:塗膜の表面に若干の黄変が見られたが実用上問題ないレベルであった。
△:塗膜の表面が著しく変色した。
×:塗膜が溶解し、基材が露出した。
実施例及び比較例で得た水性樹脂組成物の固形分100質量部に対して光重合開始剤(1−ヒドロキシ−シクロヘキシル−フェニル−ケトンとベンゾフェノンの混合物)を4質量部配合して得た配合液を、アセトンで脱脂した55質量%アルミニウム−亜鉛系合金メッキ鋼板に、バーコーターを使用して乾燥後の膜厚が約1μmになるように塗布し、雰囲気温度100℃の乾燥機に30秒間入れて乾燥し、さらに高圧水銀灯を用いて0.5J/cm2照射することによって、塗膜を作成した。その後、室温で3日間養生したものを試験片とした。
前記試験片を構成する塗膜の表面に5質量%水酸化ナトリウム水溶液をスポットで置き、20分間静置後の塗膜の劣化状態を観察した。
○:塗膜の表面の一部に若干の変色が見られたが実用上問題ないレベルであった。
△:塗膜の表面に変色が見られた。
×:塗膜が溶解し、基材が露出した。
Claims (7)
- 下記一般式(1)で示される2つ以上の重合性不飽和基を有するアルキレンジオール(a1−1)または下記一般式(2)で示される2つ以上の重合性不飽和基を有するオキシアルキレンジオール(a1−2)を含有するポリオール(a1)と、ポリイソシアネート(a2)とを反応させて得られる重合性不飽和基を有するウレタン樹脂(A)、造膜助剤(B)及び水性媒体(C)を含有することを特徴とする水性樹脂組成物。
- 前記アルキレンジオール(a1−1)がペンタエリスリトールジアクリレートである請求項1記載の水性樹脂組成物。
- 前記アルキレンジオール(a1−1)及び前記オキシアルキレンジオール(a1−2)の合計質量が、前記ウレタン樹脂(A)の製造に使用する原料の全量中に0.1〜49質量%の範囲である請求項1または2記載の水性樹脂組成物。
- 前記ポリオール(a1)が、さらにポリエステルポリオール、ポリエーテルポリオールまたはポリカーボネートポリオールを含有するものである請求項1〜3のいずれか1項記載の水性樹脂組成物。
- 前記造膜助剤(B)の含有量が、前記水性樹脂組成物中に0.1〜50質量%の範囲である請求項1〜4のいずれか1項記載の水性樹脂組成物。
- 請求項1〜5のいずれか1項記載の水性樹脂組成物を含有することを特徴とするコーティング剤。
- 請求項6記載のコーティング剤の塗膜を有することを特徴とする物品。
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