JP5507849B2 - ポリマー被覆粒子の水性分散物、関連するコーティング組成物、およびコーティングされた支持体 - Google Patents
ポリマー被覆粒子の水性分散物、関連するコーティング組成物、およびコーティングされた支持体 Download PDFInfo
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- JP5507849B2 JP5507849B2 JP2008551291A JP2008551291A JP5507849B2 JP 5507849 B2 JP5507849 B2 JP 5507849B2 JP 2008551291 A JP2008551291 A JP 2008551291A JP 2008551291 A JP2008551291 A JP 2008551291A JP 5507849 B2 JP5507849 B2 JP 5507849B2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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Description
本願は、米国特許出願番号10/876,031(発明の名称「Aqueous Dispersions of Microparticles Having a Nanoparticulate Phase and Coating Compositions Containing The Same」)の一部継続出願であり、米国特許出願番号10/876,031は、米国仮特許出願番号60/482,167(2003年6月24日出願)の利益を主張する。これらの両方は、本明細書中に参考として援用される。本願はまた、米国特許出願番号10/809,764(2004年3月25日出願、発明の名称「Process For Manufacturing Powder Coating Compositions Introducing Hard to Incorporate Additives and/or Providing Dynamic Color Control」);米国特許出願番号10/809,595(2004年3月25日出願、発明の名称「Focused Heat Extrusion Process For Manufacturing Powder Coating Compositions」);および米国特許出願番号10/809,639(2004年3月25日出願、発明の名称「Apparatus For Manufacturing Thermosetting Powder Coating Compositions With Dynamic Control Including Low Pressure Injection Systems」)の一部継続出願である。これらの各々は、本明細書中に参考として援用される。
本発明は、とりわけ、ナノ粒子などのポリマー被覆粒子の水性分散物と、このような水性分散物を製造する方法と、このような方法に有用な重合性ポリマーと、このような水性分散物から形成される粉末コーティング組成物と、少なくとも一部がこのような組成物でコーティングされた支持体とに関する。
粉末コーティング組成物などのコーティング組成物は、多くの場合、得られるコーティングに対して色および/または性能特性を与える色素および/または充填剤粒子を含む。顔料粒子は、相互に親和性が高い傾向にあり、分離させない限り、ひとまとまりになり凝集体を形成する傾向がある。故に、これらの凝集体を、高剪断技法を用いて、樹脂摩砕ビヒクルおよび必要に応じて分散剤中で、粉砕または摩砕により凝集体を破壊して分散させることが多い。ナノサイズの顔料粒子を所望する際は、所望の粒径を得るために、多くの場合、さらなる粉砕が必要になる。
特定の点では、本発明は、ポリマー被覆粒子を含む水性分散物であって、これらのポリマー被覆粒子が、脆いポリマーによって被覆されている粒子を含む、水性分散物に関する。本発明はまた、このようなポリマー被覆粒子を含む粉末コーティング組成物と、少なくとも一部がこのような粉末コーティング組成物でコーティングされた支持体と、少なくとも1つのコーティング層がこのような粉末コーティング組成物から作製された少なくとも一部が多層複合被膜でコーティングされた支持体にも関する。
以下の詳細な説明において、本発明は、明示的に異なる記載がある場合を除いて、様々な別の変形とステップの順序とを想定し得ることを理解されるべきである。さらに、任意の作用実施例以外、あるいは、他に記載がある場合でも、本明細書および請求の範囲で使用する成分の量などを表すすべての数字は、すべての場合、「約」という語によって修飾されると理解されるべきである。したがって、異なる記載がない限り、以下の本明細書および添付の特許請求の範囲に記載する数値パラメータは、本発明により得られるべき所望の特性に応じて異なってもよい近似値である。少なくとも特許請求の範囲に対する均等論の適用を制限しようとするものではなく、各数値パラメータは、少なくとも報告された有効桁数に照らして、通常の丸めの技法を適用して解釈すべきものである。
X−Y−Z
を持つ化合物が挙げられ、式中、Xは、OH、SH、NH2またはNHRであり、Rは、アルキル基、アリール基、シクロアルキル基、置換アルキル基、置換アリール基および置換シクロアルキル基ならびにこれらの混合物を含み;Yは、アルキル基、アリール基、シクロアルキル基、置換アルキル基、置換アリール基および置換シクロアルキル基ならびにこれらの混合物を含み;Zは、OSO3H、COOH、OPO3H2、SO2OH、POOHおよびPO3H2ならびにこれらの混合物を含む。
(ポリウレタン分散物)
この実施例では、後に実施例2〜4のポリウレタン/ナノ顔料分散物の生成に使用したポリウレタン分散物の調製について説明する。以下に示した成分比率の混合物からポリウレタン分散物を調製した:
(ポリウレタン/ナノ顔料分散物)
この実施例では、ナノサイズのPB15:3のフタロシアニンブルー顔料分散物の調製について説明する。この分散物を以下に示した成分比率の混合物から調製した:
(ポリウレタン/ナノ顔料分散物)
この実施例では、ナノサイズのPR122のキナクリドンマゼンタ顔料分散物の調製について説明する。この分散物を以下に示した成分比率の混合物から調製した:
(ポリウレタン/ナノ顔料分散物)
この実施例では、ナノサイズのPY128のジアゾ黄色顔料分散物の調製について説明する。以下に示した成分比率の混合物からこの分散物を調製した:
(ナノ顔料分散物のドラム乾燥)
この実施例では、実施例3の液体ポリウレタン/ナノ顔料分散物を、後に粉末コーティング組成物を調製する際に使用する粉末のフィードストックへと機械的に粉砕するのに好適な乾燥材料に変換することについて説明する。上記の実施例3に記載の分散物を、ギャップが10ミルのBufolvak 6インチ×8インチのダブルドラム乾燥機セットを用いて、ドラム温度240°F、2.9rpmで回転させて乾燥させた。得られた材料は、大きな粉末に砕けやすいレース状のシートになっており、110℃で1時間測定したとき、不揮発分は、96.0%であった。
(ポリウレタン分散物)
この実施例では、その後、実施例7〜9および13のポリウレタン/ナノ顔料分散物の形成にそれぞれ用いたポリウレタン分散物の調製について説明する。このポリウレタン分散物を以下に示した成分比率の混合物から調製した:
(ポリウレタン/ナノ顔料分散物)
この実施例では、ナノサイズのPB15:3のフタロシアニンブルー顔料分散物の調製について説明する。この分散物を以下に示した成分比率の混合物から調製した:
(ポリウレタン/ナノ顔料分散物)
この実施例では、ナノサイズのPR122のキナクリドンマゼンタ顔料分散物の調製について説明する。この分散物を以下に示した成分比率の混合物から調製した:
(ポリウレタン/ナノ顔料分散物)
この実施例では、ナノサイズのPY128のジアゾ黄色顔料分散物の調製について説明する。この分散物を以下に示した成分比率の混合物から調製した:
(粉末コーティング組成物中間体の調製)
この実施例では、その後の実施例の粉末コーティング組成物を製造するのに用いる乾燥材料のコア配合物の調製について説明する。コア配合物を以下に示した比率の成分から調製した:
7EMS社製の市販品
8Estron Chemical社製の市販品
9GCA Chemical社製の市販品
10Clariant社製の市販品
11CIBA社製の市販品
12Bayer Chemical社製の市販品
13Palmer Supplies社製の市販品。
(粉末コーティング組成物の調製)
種々の粉末コーティング組成物を、実施例10の粉末コーティング組成物中間体および実施例2〜4および7〜9のポリウレタン/ナノ顔料分散物に加えて、これら分散物の様々な混合物(重量比で90:10〜10:90の範囲)から調製した。粉末コーティング組成物をそれぞれ、Coperion W&P社の30mm同時回転2軸スクリュー押出機および実施例10に記載の条件により調製した。この押出機は、米国特許出願公開第2005/0213423号;同第2005/0212159号;および同第2005/0212171号に記載されているような低圧注入システムおよび5つの独立温度制御ゾーンを備えたものであった。低圧注入システムを介して、実施例10の粉末コーティング組成物中間体を押出機に1分当たり280グラムの量で入れて、顔料分散物を押出機に1分当たり105グラムの量で入れた。ゾーン4は、揮発性蒸気を除去できるように揮発分除去口を備えていた。この押出物を冷却して、機械的粉砕システムで粒径約28〜30ミクロンまで摩砕した。
(カラーマッチングの方法)
この実施例では、液体コーティング組成物から堆積された有色被膜の色をマッチングさせる、本発明の粉末コーティング組成物の能力が改善したことを示す。この実施例では、液体コーティング組成物から作製された紫/マゼンタの有色被膜を標準皮膜とした。MA68I Multi−angle分光光度計により様々な視角で測定した色データを表1に示す。粉末コーティングAは、標準顔料しか含まない粉末コーティング組成物を用いて得られた最もよいカラーマッチングを示したものである。粉末コーティングBは、実施例2〜4および7〜9のナノ顔料分散物の組み合わせを含む粉末コーティング組成物を用いて得られた最もよいカラーマッチングを示すものである。
(ポリウレタン/ナノ顔料分散物)
この実施例では、ナノサイズのPR−179のペリレン赤顔料分散物の調製について説明する。この分散物を以下に示した成分比率の混合物から調製した:
この実施例では、2種類の粉末コーティング組成物を、実施例10に記載の成分および方法により調製した。実施例14aに関しては、Sun Chemicalから市販されているPR179顔料の3重量部を実施例10の組成物に含ませた。実施例14bについては、ポリウレタン/ナノ顔料分散物の3重量部を実施例10の組成物に含ませた。実施例14aおよび14bの粉末コーティング組成物を4インチ×12インチの電着パネルに静電気的に塗布した。このパネルを適当な高温で硬化させて、周囲温度まで冷却した。MA68I Multi−angle分光光度計を用いて種々の視角で色データを測定した。その結果を表1に示し、実施例14aとを比較した実施例14bについての値の差として報告してある。
Claims (18)
- ポリマー被覆粒子を含む水性分散物から生成された粉末コーティング組成物であって、前記ポリマー被覆粒子が、脆いポリマーによって被覆された粒子を含み、ここで、前記脆いポリマーは、(i)重合性ポリエステルポリウレタンと(ii)エチレン性不飽和モノマーとの反応生成物を含む、
ここで、前記ポリマー被覆粒子が、
(1)水性媒体中に:
(a)粒子と、
(b)エチレン性不飽和モノマーと、
(c)水分散性の重合性ポリエステルポリウレタンと
の混合物を提供することと、
(2)前記エチレン性不飽和モノマーおよび重合性ポリエステルポリウレタンを重合させて、ポリマー被覆粒子を含む水性分散物を形成することと、
(3)前記水性分散物から水を除去して、前記ポリマー被覆粒子を含む固体材料を生成することと、
(4)前記固体材料を微粒子化することと
を含む方法によって製造され、
ここで、前記ポリマー被覆粒子が脆いポリマーによって被覆される粒子を含み、ここで前記脆いポリマーが(b)および(c)の反応生成物である、
粉末コーティング組成物。 - 前記粒子は、ナノ粒子を含む、請求項1に記載の粉末コーティング組成物。
- 前記ナノ粒子は、無機ナノ粒子を含む、請求項2に記載の粉末コーティング組成物。
- 前記ナノ粒子は、コロイド状シリカ、ヒュームドシリカ、無定形状シリカ、アルミナ、コロイド状アルミナ、二酸化チタン、酸化鉄、酸化セシウム、酸化イットリウム、コロイド状イットリア、コロイド状ジルコニア、無定形状ジルコニアおよびこれらの混合物から選択される無機ナノ粒子を含む、請求項3に記載の粉末コーティング組成物。
- 前記無機ナノ粒子は、混合金属酸化物を含む、請求項3に記載の粉末コーティング組成物。
- 前記ナノ粒子は、最大ヘイズが10%である、請求項2に記載の粉末コーティング組成物。
- 前記ナノ粒子は、有機ナノ粒子を含む、請求項2に記載の粉末コーティング組成物。
- 前記有機ナノ粒子は、ペリレン、キナクリドン、フタロシアニン、イソインドリン、ジオキサジン(すなわち、トリフェンジオキサジン)、1,4−ジケトピロロピロール、アントラピリミジン、アンタントロン、フラバントロン、インダントロン、ペリノン、ピラントロン、チオインジゴ、4,4’−ジアミノ−1,1’−ジアントラキノニル、アゾ化合物、これらの置換誘導体およびこれらの混合物から選択される有機顔料を含む、請求項7に記載の粉末コーティング組成物。
- 前記重合性ポリエステルポリウレタンは、末端エチレン性不飽和を持つポリエステルポリウレタンを含む、請求項1に記載の粉末コーティング組成物。
- 末端エチレン性不飽和を持つ前記ポリエステルポリウレタンは、
(a)ポリイソシアナートと、
(b)ポリエステルポリオールと、
(c)エチレン性不飽和基および活性水素基を含む材料と
を含む反応物質から調製される、請求項9に記載の粉末コーティング組成物。 - 末端エチレン性不飽和を持つ前記ポリエステルポリウレタンは、
(d)ポリアミンと、
(e)酸官能基または酸無水物と、イソシアナート基またはヒドロキシル基と反応する官能基とを含む材料と
をさらに含む反応物質から調製される、請求項10に記載の粉末コーティング組成物。 - 前記重合性ポリエステルポリウレタンは、水分散性である、請求項1に記載の粉末コーティング組成物。
- 前記重合性ポリエステルポリウレタンは、重量平均分子量が1モル当たり40,000〜80,000グラムである、請求項1に記載の粉末コーティング組成物。
- 少なくとも一部が、請求項1に記載の粉末コーティング組成物から堆積される被膜でコーティングされた、支持体。
- 前記支持体は、金属支持体を含む、請求項14に記載の支持体。
- 少なくとも1つのコーティング層は、請求項1に記載の粉末コーティング組成物から堆積される、多層複合被膜。
- 前記粉末コーティング組成物は、
(1)押出機に
(a)請求項1に記載の水性分散物と、
(b)乾燥材料と
を含む構成成分を導入することと、
(2)前記押出機内で(a)および(b)をブレンドすることと、
(3)前記ブレンドの揮発成分を除去して押出物を生成することと、
(4)前記押出物を冷却することと、
(5)前記押出物を所望の粒径に粉砕することと
を含む方法で製造される、請求項1に記載の粉末コーティング組成物。 - 最大ヘイズが10%の複数のポリマー被覆ナノ粒子を含む粉末コーティング組成物から堆積された、色を与える非隠蔽性コーティング層で少なくとも一部がコーティングされた、反射面であって、
ここで、前記ポリマー被覆粒子が、脆いポリマーで被覆されたナノ粒子を含み、ここで、前記脆いポリマーは、(i)重合性ポリエステルポリウレタンと(ii)エチレン性不飽和モノマーとの反応生成物を含む、
反射面。
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US9328432B2 (en) | 2010-04-23 | 2016-05-03 | Pixelligent Technologies, Llc | Synthesis, capping and dispersion of nanocrystals |
US9617657B2 (en) | 2010-04-23 | 2017-04-11 | Pixelligent Technologies, Llc | Synthesis, capping and dispersion of nanocrystals |
US9856581B2 (en) | 2010-04-23 | 2018-01-02 | Pixelligent Technologies, Llc | Synthesis, capping and dispersion of nanocrystals |
US10753012B2 (en) | 2010-10-27 | 2020-08-25 | Pixelligent Technologies, Llc | Synthesis, capping and dispersion of nanocrystals |
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