JP4647494B2 - 黒色系光輝顔料およびそれを配合した化粧料、塗料組成物、樹脂組成物およびインキ組成物 - Google Patents
黒色系光輝顔料およびそれを配合した化粧料、塗料組成物、樹脂組成物およびインキ組成物 Download PDFInfo
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- JP4647494B2 JP4647494B2 JP2005514093A JP2005514093A JP4647494B2 JP 4647494 B2 JP4647494 B2 JP 4647494B2 JP 2005514093 A JP2005514093 A JP 2005514093A JP 2005514093 A JP2005514093 A JP 2005514093A JP 4647494 B2 JP4647494 B2 JP 4647494B2
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- black
- bright pigment
- glass
- coated
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Classifications
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Description
薄片ガラスに金属酸化層を形成させる手段は、本発明の目的を阻害しない限り特に限定されず、公知の被覆手段などから適宜採用される。例えば、金属酸化層がシリカで構成される層である場合、薄片ガラスを65〜75℃に加温した水の中に分散させ、ついで鉱酸ないしはカセイソーダでpH7〜9に調整した後、液温度及びpHを維持しながら珪酸ナトリウム及び鉱酸を滴下し、その後水洗、乾燥さらには焼成することにより、薄片ガラスに金属酸化層を設けることができる。
また、上記では薄片基材が薄片ガラス基材である場合を説明したが、薄片基材が金属酸化層付きガラス薄片である場合も同様にして黒色系光輝顔料を作製できる。
この薄片状黒色系光輝顔料を化粧料に配合することにより、これまでにない光輝感のある黒色を発色でき、感触も良好な化粧料を調製することができる。化粧料における薄片状黒色系光輝顔料の含有率は、1〜100質量%が適当である。1質量%未満では、黒色の発色が弱い。ルースパウダーとして使用するアイシャドー、フェースカラーなどの粉末状化粧料の場合は、使用時に肌上に存在する人脂と混ざるため、100%でもよい。
さらに、この薄片状黒色系光輝顔料を化粧料、塗料、樹脂成形体のフィラーとして利用すれば、光輝感のある黒色を呈するものとすることができ、インクのフィラーとして利用すれば光輝感のある黒色を呈する筆記ないし印刷ができる。
〔色相、輝度の評価〕
アクリル樹脂塗料(アクリルオートクリアスーパー 日本ペイント株式会社製、固形分約50質量%)に薄片状黒色系光輝顔料が樹脂中で10質量%になるように添加し、よく混合撹拌した後、隠蔽率測定紙に9ミル(9/1000インチ)隙間のアプリケーターで塗布し、乾燥させた。その塗板を、マルチアングル分光測色計(X−rite MA68II、(株)カラーテクノシステム)を使用して、角度15度における輝度L15値、色相a値、b値を測定した。その輝度L15値が高いほど輝度があり、光輝感がある。
〔隠蔽率の評価〕
上記で作製した隠蔽率測定紙の塗板につき、ミノルタ製色彩色差計CR300を用いて、白色背景でのL値(Lw)と黒色背景でのL値(Lb)を測定し、Lw値をLb値で除した数値を隠蔽指数とした。白色背景のL値と黒色背景でのL値に差がないほど(すなわち隠蔽指数が1に近いほど)隠蔽率が高いという評価である。
また、上記色相、輝度測定用の塗板を使用し、塗板を目視でも観察し、人間の目で見た場合の光輝感を判定した。目視観察は5人で行い、表1に示す基準で光輝感の印象から点数をつけてもらい、その5人の平均点を出し、表2に示したような基準で光輝感を評価した。
実施例1〜3として、Eガラス(SiO2:53質量%、Al2O3:15質量%、CaO:21質量%、MgO:2質量%、B2O3:8質量%、Na2O+K2O:0.3質量%)を1,300℃で熔融し、円筒形にブローし延伸薄膜化して冷却固化することにより、表3に示される所定の厚さにし、それを粉砕分級して、表3に示される所定の厚さ、粒度およびアスペクト比を有する薄片ガラスを製造した。また、実施例4〜7として、Cガラス(SiO2:65質量%、Al2O3:4質量%、CaO:14質量%、MgO:3質量%、B2O3:5質量%、Na2O:8質量%、K2O:1質量%)を1,200℃で熔融し、円筒形にブローし延伸薄膜化して冷却固化することにより、表3に示される所定の厚さにし、それを粉砕分級して、表3に示される所定の厚さ、粒度およびアスペクト比を有する薄片ガラスを製造した。
これらの薄片ガラス100gを1Lの精製水に添加・分散させ、恒温水槽で75℃に昇温・保持した。その溶液を希塩酸でpH3.2程度に調整した。その後、10%塩化鉄(III)溶液を添加した。この際、希水酸化ナトリウム溶液で、pHを3.2程度に維持した。これにより、薄片ガラスの表面がFe2O3で被覆された状態となる。10%塩化鉄(III)溶液の添加量は、被覆厚みがほぼ同じになるように調整した。すなわち、表3に示す母材薄片ガラスの厚みが0.7μmの場合は、10%塩化鉄(III)溶液の添加量をトータル2005g、厚みが1.3μmの場合は、10%塩化鉄(III)溶液の添加量をトータル1080g、厚みが5μmの場合は、10%塩化鉄(III)溶液の添加量をトータル281gに調整した。添加終了後、薄片ガラス懸濁溶液をろ過し、回収した残渣を乾燥したあと、600℃で2時間仮焼し、Fe2O3被覆薄片ガラスを得た。
実施例3で製造した薄片ガラス100gを、70℃に加温したイオン交換水中に分散させ、鉱酸でpH8.0に調整した後、液温度およびpHを維持しながら、珪酸ナトリウム30gを1時間かけて滴下させた。
その後、固形物をろ取し、水洗、乾燥し、600℃で焼成した。このようにして、表3に示される所定の厚さ、粒度およびアスペクト比を有するシリカ被覆薄片ガラスを製造した。このシリカ被覆薄片ガラスに実施例3と同様にしてFe2O3を被覆し、Fe2O3で被覆されたシリカ被覆薄片ガラスを製造した。
比較例1〜2として、薄片ガラスに代えて以下の表5に示すマイカを用いたこと以外、実施例1と同じ方法で黒酸化鉄を被覆し、黒色マイカを作製し、同様に評価を行った。結果を表5に示す。また、比較例3として、市販のマイカブラック(マイカに黒酸化鉄及び酸化チタンを被覆したもの:メルク社製)も同様に評価し、表5に合わせて示した。
薄片ガラス(日本板硝子(株)製 マイクログラス ファインフレークRCFFX−1040(9507)Cガラス組成 平均厚さ1.3μm 平均粒径38μm)1.2kgをイオン交換水4リットルに加え、攪拌機で攪拌して、スラリー液とした。このスラリー液に塩化スズ(II)0.5質量%水溶液を常温にて0.3リットル加えた後、5分間攪拌した。薄片ガラスを減圧ろ過で回収し、イオン交換水で水洗した。この薄片ガラスを純水4リットルに懸濁し、スラリー液とし、このスラリー液に塩化パラジウム(II)2質量%水溶液を常温にて、0.01リットル加えて、5分間攪拌した。薄片ガラスを減圧ろ過で回収し、純水で水洗した。
粒径90μm、厚み5.0μmのCガラスの薄片ガラス100gを1Lの精製水に添加・分散させ、恒温水槽で75℃に昇温・保持した。その溶液を希塩酸でpH3.2程度に調整した。その後、10%塩化鉄(III)溶液を表6に示される所定量添加した。この際、希水酸化ナトリウム溶液で、pHを3.2程度に維持した。これにより、薄片ガラスの表面がFe2O3で被覆された状態となる。添加終了後、薄片ガラス懸濁溶液をろ過し、回収した薄片ガラスを乾燥したあと、600℃で2時間仮焼し、Fe2O3被覆薄片ガラスを得た。
このFe2O3被覆薄片ガラスを、白金皿にいれ、管状炉中で水素10%−窒素90%のガスを流しながら、表6に示される所定の還元温度で2時間熱処理することにより、被覆したFe2O3を黒色のFe3O4に還元した。Fe3O4薄膜の厚みは実施例9〜11がおよそ450nm、実施例12〜14がおよそ700nmであった。
また、実施例9、10および11または実施例12、13および14を比較することにより、還元温度が順に400、500および530℃と高くなるにしたがって、色が黒くなっていることがわかる。これは、酸化鉄の還元度合いが進み、黒の吸収が強くなって、干渉色が見えなくなってきたためだと思われる。
L15値と光輝感は高く、光輝感のある暗色系顔料になっている。
実施例4で用いた、粒径40μm、厚み1.3μmの薄片ガラスを硫酸チタニル溶液中に懸濁させ、この懸濁液を加熱し1時間沸騰させることにより、薄片ガラス表面をチタニアで被覆し、濾過水洗後乾燥し、その後600℃で30分間熱処理して、チタニア被膜を備えた薄片ガラスを得た。このチタニア被覆薄片ガラスを、白金皿にいれ、管状炉中でアンモニアガスを流しながら、600℃の温度で10時間熱処理することにより、被覆したTiO2を、黒色の低次酸化チタン(TiOx、ここでxは1.7)に還元し、低次酸化チタン被覆薄片ガラスを得た。
この低次酸化チタン被覆薄片ガラスのL15値は67であり、パネリストによる光輝感評価は◎であった。なお低次酸化チタン被膜の厚みは150nmであった。
実施例16の処方中、成分(6)の(黒酸化鉄内包薄片状)黒色系光輝顔料を比較例1の酸化鉄顔料に代え、それ以外は実施例14と同様にして乳化型マスカラを作製した。
実施例16と比較例5との官能試験の結果を表11に示す。
実施例17の処方中、成分(3)の実施例5の薄片状黒色系光輝顔料を比較例2の黒酸化鉄被覆マイカに代え、それ以外は実施例17と同様にしてアイシャドーを作製した。
実施例17と比較例6との官能試験の結果を表13にまとめて示す。
実施例18の処方中、成分(4)の薄片状黒色系光輝顔料を比較例2の黒酸化鉄被覆マイカに代え、それ以外は実施例18と同様にしてアイライナーを作製した。
実施例18と比較例7との官能試験の結果を表15にまとめて示す。
実施例19の処方中、成分(10)の薄片状黒色系光輝顔料を比較例1の黒酸化鉄被覆マイカに代え、それ以外は実施例19と同様にしてネイルカラーを作製した。
実施例19と比較例8との官能試験の結果を表17にまとめて示す。
この油性スティックファンデーションは、光輝感、感触に優れていた。
この頬紅は光輝感、感触が優れていた。
[実施例23:黒塗料組成物]
以下に示す下記成分により、塗料組成物を調製した。
まず、以下の表21に示す組成を、ペイントシェーカーを用いて60分間分散させ、分散ビヒクルを作製した。
実施例23に示す塗料組成物のうち、成分(4)の薄片状黒色系光輝顔料を、比較例1の黒酸化鉄被覆マイカに代える以外は実施例23と同様にして、黒色塗料組成物を作製した。
メタクリル酸メチル共重合ビーズ98質量%、実施例7の薄片状黒色系光輝顔料2質量%をヘンシェルミキサーで攪拌混合して成形樹脂組成物を得た。これを用いて押し出し機で厚み0.5mmのアクリル樹脂成形体を作製した。この樹脂成形体は光輝感のある澄んだ黒色を呈した。
実施例24で用いた薄片状黒色系光輝顔料に代えて比較例1の黒酸化鉄被覆マイカを使用した以外は実施例24と同様にして、厚み0.5mmのアクリル樹脂成形体を作製した。この樹脂成形体は光輝感のない、マット調の黒色を呈した。
実施例24及び比較例10から分かるように、本発明に係る樹脂成形体は、光輝感、透明性のあるきれいな澄んだ黒色を呈することが分かる。
Claims (10)
- 1.3〜5.0μmの平均厚さ、1〜800μmの平均粒径および3〜500のアスペクト比を有する(a)薄片Cガラス基材または(b)金属酸化層付き薄片Cガラス基材の表面が、10nm〜1.0μmの厚みを有する四三酸化鉄および/または低次酸化チタンの薄膜で被覆されてなる黒色系光輝顔料。
- 輝度L15値が40以上である請求項1に記載の黒色系光輝顔料。
- 四三酸化鉄および/または低次酸化チタンの薄膜が、あらかじめ三二酸化鉄および/または二酸化チタンで薄片基材の表面を被覆した後、還元雰囲気中で焼成し、四三酸化鉄および/または低次酸化チタンとすることにより形成されたものである請求項1または2に記載の黒色系光輝顔料。
- 前記金属酸化層は、シリカ、酸化ジルコン、酸化亜鉛および酸化スズから選ばれた1種または2種以上の金属酸化物からなる金属酸化層である請求項1〜3のいずれか1項に記載の黒色系光輝顔料。
- 請求項1〜4のいずれか1項に記載の黒色系光輝顔料を含有する化粧料。
- 請求項1〜4のいずれか1項に記載の黒色系光輝顔料を含有する塗料組成物。
- 請求項6に記載の塗料組成物を塗布し、硬化してなる塗膜。
- 請求項1〜4のいずれか1項に記載の黒色系光輝顔料を含有する成形樹脂組成物。
- 請求項8に記載の成形樹脂組成物を成形してなる樹脂成形体。
- 請求項1〜4のいずれか1項に記載の黒色系光輝顔料を含有するインキ組成物。
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WO2013111771A1 (ja) | 2012-01-23 | 2013-08-01 | トピー工業株式会社 | 酸化鉄被覆層状ケイ酸塩顔料 |
JP2013545855A (ja) * | 2010-12-09 | 2013-12-26 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツング | 磁性顔料 |
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Also Published As
Publication number | Publication date |
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JPWO2005028566A1 (ja) | 2007-11-15 |
EP1666541B1 (en) | 2011-12-21 |
WO2005028566A1 (ja) | 2005-03-31 |
US20070032573A1 (en) | 2007-02-08 |
CN1856550A (zh) | 2006-11-01 |
KR20060090226A (ko) | 2006-08-10 |
EP1666541A1 (en) | 2006-06-07 |
EP1666541A4 (en) | 2009-03-25 |
BRPI0414602A (pt) | 2006-11-07 |
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