JP2014031397A - 防汚性ハードコートおよび防汚性ハードコート前駆体 - Google Patents
防汚性ハードコートおよび防汚性ハードコート前駆体 Download PDFInfo
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- JP2014031397A JP2014031397A JP2012170999A JP2012170999A JP2014031397A JP 2014031397 A JP2014031397 A JP 2014031397A JP 2012170999 A JP2012170999 A JP 2012170999A JP 2012170999 A JP2012170999 A JP 2012170999A JP 2014031397 A JP2014031397 A JP 2014031397A
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- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
【解決手段】本開示のハードコートは、ナノ粒子の混合物およびバインダーを含むハードコートであって、ナノ粒子はハードコートの全質量の40質量%〜95質量%を構成し、ナノ粒子の10質量%〜50質量%は2nm〜200nmの範囲の平均粒径を有し、ナノ粒子の50質量%〜90質量%は60nm〜400nmの範囲の平均粒径を有し、60nm〜400nmの範囲の平均粒径を有するナノ粒子の平均粒径と2nm〜200nmの範囲の平均粒径を有するナノ粒子の平均粒径の比が、2:1〜200:1の範囲であり、バインダーが多官能性フッ素化(メタ)アクリル化合物、その反応生成物、またはそれらの組み合わせを含む。
【選択図】なし
Description
HFPO−C(O)N(H)CH(CH2OC(O)CH=CH2)2;
HFPO−C(O)N(H)C(CH2CH3)(CH2OC(O)CH=CH2)2;
HFPO−C(O)NHC(CH2OC(O)CH=CH2)3;
HFPO−C(O)N(CH2CH2OC(O)CH=CH2)2;
HFPO−C(O)NHCH2CH2N(C(O)CH=CH2)CH2OC(O)CH=CH2;
HFPO−C(O)NHCH(CH2OC(O)CH=CH2)2;
HFPO−C(O)NHC(CH3)(CH2OC(O)CH=CH2)2;
HFPO−C(O)NHC(CH2CH3)(CH2OC(O)CH=CH2)2;
HFPO−C(O)NHCH2CH(OC(O)CH=CH2)CH2OC(O)CH=CH2;
HFPO−C(O)NHCH2CH2CH2N(CH2CH2OC(O)CH=CH2)2;
HFPO−C(O)OCH2C(CH2OC(O)CH=CH2)3;
HFPO−C(O)NH(CH2CH2N(C(O)CH=CH2))4CH2CH2NC(O)−HFPO;
CH2=CHC(O)OCH2CH(OC(O)HFPO)CH2OCH2CH(OH)CH2OCH2CH(OC(O)HFPO)CH2OCOCH=CH2;
HFPO−CH2O−CH2CH(OC(O)CH=CH2)CH2OC(O)CH=CH2
などが挙げられる。本開示において、HFPOとは、F(CF(CF3)CF2O)nCF(CF3)−(nは2〜15)で表されるペルフルオロエーテル部位、およびこのようなペルフルオロエーテル部位を含む化合物を意味する。
本開示のハードコートの特性を以下の方法にしたがって評価した。ハードコートは、基材にハードコート前駆体を塗布し、紫外線照射することによって形成し、基材に担持された状態で評価した。
JIS K5600−5−4(1999)に準拠して、750gのおもりを使用して基材上に形成したハードコート表面の鉛筆硬度を決定した。
ハードコートのヘーズは、JIS K 7136(2000)に準拠して、ヘーズメーターNDH−5000W(日本電色工業株式会社より入手)を使用して測定した。
接触角メーター(協和界面科学株式会社から製品名「DROPMASTER FACE」として入手)を使用し、Sessile Drop法により、ハードコート表面の水接触角を測定した。静的測定について液滴の体積を4μLとした。5回測定した平均から水接触角の値を計算した。
油性マジック(マッキー(黒)、ゼブラ株式会社より入手)を用いてハードコート上に一本の直線を引き外観を目視で観察した。インクをはじき、線にならないサンプルを良好、はじかずに線が引けるものを不良とした。
ハードコートの耐引っかき性を、摩耗抵抗試験後の光学特性および水接触角を測定することによって評価した。布帛摩耗抵抗試験では32mm幅のJIS試験用綿布帛(日本工業標準調査会より入手)を荷重500gで、スチールウール摩耗抵抗試験では32mm角の#0000スチールウールを荷重1kgでそれぞれ使用し、85mmのストローク、60サイクル/分の速さで、ハードコート表面を200回(サイクル)研磨する。図2に摩耗抵抗試験装置60(ラビングテスターIMC−157C、株式会社井元製作所より入手)の模式図を示す。ここでは、ステージ61の上に試料10を固定し、スタイラス62を介しておもり63の荷重を布帛またはスチールウール64に与え、ステージ61を往復させることによって試料の表面を研磨する。摩耗抵抗試験は、拭き取りおよび洗浄のときの引っかきを模擬している。
表面改質されたシリカゾル(「ゾル1」)を以下のように調製した。5.95gのSILQUEST A174および0.5gのPROSTABを、400gのNALCO 2329および450gの1−メトキシ−2−プロパノールの混合物にガラス瓶の中で加え、10分間室温で撹拌した。ガラス瓶を密封し、80℃のオーブン内に16時間置いた。得られた溶液から、60℃で溶液の固形分が45質量%近くになるまでロータリーエバポレーターで水を除去した。得られた溶液に200gの1−メトキシ−2−プロパノールを入れ、次に、ロータリーエバポレーターを60℃で使用して残りの水を除去した。後半のステップを2回繰り返して溶液からさらに水を取り除いた。最後に、1−メトキシ−2−プロパノールを加えることで全SiO2ナノ粒子の濃度を45質量%に調整して、75nmの平均粒径を有する表面改質SiO2ナノ粒子を含有するSiO2ゾル(以下、ゾル1という。)を得た。
表面改質されたシリカゾル(「ゾル2」)を以下のように調製した。400gのNALCO 2327、25.25gのSILQUEST A174および0.5gのPROSTABを使用した以外は、ゾル1と同様の方法で改質して、20nmの平均粒径を有する表面改質SiO2ナノ粒子を45質量%含有するSiO2ゾル(以下、ゾル2という。)を得た。
11.34gのゾル1、5.88gのゾル2、2.25gのEbecryl 4858、および0.25gのSR340を混合した。光重合開始剤として0.20gのIrgacure 2959、およびレベリング剤として0.001gのBYK−UV3500を混合物に添加した。次に、1−メトキシ−2−プロパノールを加えて固形分が50質量%になるように調整してハードコート前駆体HC−1を用意した。
11.34gのゾル1、5.88gのゾル2、2.25gのEbecryl 4858、および0.25gのSR340を混合した。防汚剤として0.17gのHFPOウレタンアクリレート、光重合開始剤として0.1gのIrgacure 2959、およびレベリング剤として0.001gのBYK−UV3500を混合物に添加した。次に、1−メトキシ−2−プロパノールを加えて固形分が50質量%になるように調整してハードコート前駆体HC−2を用意した。HFPOウレタンアクリレートは単官能性フッ素化(メタ)アクリル化合物である。
ハードコート前駆体HC−3からHC−8は、表2に記載する配合でHC−2と同様に調製した。HC−6からHC−8ではKayarad UX−5000をアクリレートオリゴマーとして使用し、HC−4、HC−5およびHC−8ではKY−1203を多官能性(メタ)アクリル化合物(防汚剤)として使用した。
PMMA基材(アクリライト L−001、100×53×2mm、三菱レイヨン株式会社より入手)を水平調節付きのステンレス鋼製テーブルの上に固定した。ハードコート前駆体HC−4を、メイヤーロッド#16を用いてPMMA基材に塗布し、60℃で5分間乾燥した。次に、Fusion UV System Inc.のH−バルブ(DRSモデル)を用いて、窒素雰囲気下、ライン速度13m/分で10回(照射量約1400mJ/cm2)紫外線を塗布面に照射した。ハードコートの厚さは約10μmであった。このようにして、例1のハードコートをPMMA基材上に形成した。
ハードコート前駆体HC−1からHC−3、HC−5からHC−8を用いて、例1と同様にハードコートをPMMA基材上に形成した。
61 ステージ
62 スタイラス
63 おもり
64 布帛またはスチールウール
Claims (9)
- ナノ粒子の混合物およびバインダーを含むハードコートであって、
前記ナノ粒子は前記ハードコートの全質量の40質量%〜95質量%を構成し、
前記ナノ粒子の10質量%〜50質量%は2nm〜200nmの範囲の平均粒径を有し、前記ナノ粒子の50質量%〜90質量%は60nm〜400nmの範囲の平均粒径を有し、60nm〜400nmの範囲の平均粒径を有するナノ粒子の平均粒径と2nm〜200nmの範囲の平均粒径を有するナノ粒子の平均粒径の比が、2:1〜200:1の範囲であり、前記バインダーが多官能性フッ素化(メタ)アクリル化合物、その反応生成物、またはそれらの組み合わせを含む、ハードコート。 - 前記ナノ粒子が表面改質ナノ粒子である、請求項1に記載のハードコート。
- 前記多官能性フッ素化(メタ)アクリル化合物が、2以上の(メタ)アクリル基を有するペルフルオロエーテル化合物である、請求項1または2のいずれかに記載のハードコート。
- 前記多官能性フッ素化(メタ)アクリル化合物が3以上の(メタ)アクリル基を有する、請求項1〜3のいずれか一項に記載のハードコート。
- 前記ナノ粒子が無機酸化物ナノ粒子であり、前記多官能性フッ素化(メタ)アクリル化合物がシロキサン単位を含む、請求項1〜4のいずれか一項に記載のハードコート。
- 前記ナノ粒子がシリカナノ粒子である、請求項5に記載のハードコート。
- 前記多官能性フッ素化(メタ)アクリル化合物が環状シロキサン単位を含む、請求項5または6のいずれかに記載のハードコート。
- 前記バインダーが紫外線吸収剤をさらに含む、請求項1〜7のいずれか一項に記載のハードコート。
- ナノ粒子の混合物およびバインダーを含むハードコート前駆体であって、
前記ナノ粒子は前記ナノ粒子および前記バインダーの合計質量の40質量%〜95質量%を構成し、
前記ナノ粒子の10質量%〜50質量%は2nm〜200nmの範囲の平均粒径を有し、前記ナノ粒子の50質量%〜90質量%は60nm〜400nmの範囲の平均粒径を有し、60nm〜400nmの範囲の平均粒径を有するナノ粒子の平均粒径と2nm〜200nmの範囲の平均粒径を有するナノ粒子の平均粒径の比が、2:1〜200:1の範囲であり、前記バインダーが多官能性フッ素化(メタ)アクリル化合物を含む、ハードコート前駆体。
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JP2012170999A JP6062680B2 (ja) | 2012-08-01 | 2012-08-01 | 防汚性ハードコートおよび防汚性ハードコート前駆体 |
KR1020157004809A KR102159140B1 (ko) | 2012-08-01 | 2013-07-30 | 방오성 하드 코트 및 방오성 하드 코트 전구체 |
PCT/US2013/052677 WO2014022363A2 (en) | 2012-08-01 | 2013-07-30 | Anti-smudge hard coat and anti-smudge hard coat precursor |
SG10201707666UA SG10201707666UA (en) | 2012-08-01 | 2013-07-30 | Anti-smudge hard coat and anti-smudge hard coat precursor |
CN201380040679.0A CN104540900B (zh) | 2012-08-01 | 2013-07-30 | 防污硬涂层和防污硬涂层前体 |
SG11201500748XA SG11201500748XA (en) | 2012-08-01 | 2013-07-30 | Anti-smudge hard coat and anti-smudge hard coat precursor |
TW102127567A TWI623595B (zh) | 2012-08-01 | 2013-07-31 | 抗污硬性塗層及抗污硬性塗層前驅物 |
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WO2016080152A1 (ja) * | 2014-11-21 | 2016-05-26 | デクセリアルズ株式会社 | 塗料組成物、及び超撥水フィルム |
JP2017128114A (ja) * | 2016-01-18 | 2017-07-27 | リケンテクノス株式会社 | ハードコート積層フィルム |
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JP7301999B2 (ja) | 2019-03-11 | 2023-07-03 | ヨアノイム リサーチ フォルシュングスゲゼルシャフト エムベーハー | オリゴマーヘキサフルオロプロピレンオキシド誘導体 |
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Also Published As
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SG11201500748XA (en) | 2015-02-27 |
SG10201707666UA (en) | 2017-10-30 |
HK1209448A1 (en) | 2016-04-01 |
KR20150040310A (ko) | 2015-04-14 |
TW201406877A (zh) | 2014-02-16 |
CN104540900B (zh) | 2017-11-17 |
JP6062680B2 (ja) | 2017-01-18 |
WO2014022363A2 (en) | 2014-02-06 |
TWI623595B (zh) | 2018-05-11 |
KR102159140B1 (ko) | 2020-09-23 |
WO2014022363A3 (en) | 2014-06-12 |
CN104540900A (zh) | 2015-04-22 |
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