JP5543959B2 - 磁性ピグメントおよび磁性特性を向上するプロセス - Google Patents
磁性ピグメントおよび磁性特性を向上するプロセス Download PDFInfo
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- JP5543959B2 JP5543959B2 JP2011504050A JP2011504050A JP5543959B2 JP 5543959 B2 JP5543959 B2 JP 5543959B2 JP 2011504050 A JP2011504050 A JP 2011504050A JP 2011504050 A JP2011504050 A JP 2011504050A JP 5543959 B2 JP5543959 B2 JP 5543959B2
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- XYJRNCYWTVGEEG-UHFFFAOYSA-N trimethoxy(2-methylpropyl)silane Chemical compound CO[Si](OC)(OC)CC(C)C XYJRNCYWTVGEEG-UHFFFAOYSA-N 0.000 description 1
- UBMUZYGBAGFCDF-UHFFFAOYSA-N trimethoxy(2-phenylethyl)silane Chemical compound CO[Si](OC)(OC)CCC1=CC=CC=C1 UBMUZYGBAGFCDF-UHFFFAOYSA-N 0.000 description 1
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- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical class CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
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- 235000013343 vitamin Nutrition 0.000 description 1
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- 239000001993 wax Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Description
本出願は、2008年4月9日に出願された同じ発明の名称の、出願番号12/100,026の仮特許出願の利益を要求する。その開示は、その全体が参照され本明細書に組み入れられる。
宝石(例えばダイヤモンド、ルビー、エメラルド、トパーズ、オパール、ヒスイ)、および貴金属(例えば金、銀、白金)に加えて、真珠が数千年の間人類にとって、最も重視された所有物(または贅沢品)であった。それらの自然な美、光り輝く色および光沢に加え、それらは、しばしば安楽な社会的身分および階層を表す。その結果、驚くべきことではないが、化粧品メーキャップの傾向は、真珠、宝石および貴金属の「自然で」、「審美的な」外観を、干渉ピグメント(例えば、金属酸化物でコーティングされた雲母)のようなそれほど高価でない材料で模倣するものであった。効果ピグメントの最も一般的なタイプは、微粉にされた二酸化チタン、金属酸化物でコーティングされた雲母、金属酸化物でコーティングされたアルミナ、金属酸化物でコーティングされたシリカ、塩基性炭酸鉛、オキシ塩化ビスマスおよび天然の魚銀である。
上記および他の欠点は、基体および層を含むピグメントであって、該層がγ−Fe2O3領域およびα−Fe2O3領域を有するものの提供により克服されることができる。
0.1×10−5 m3/kg未満の磁化率を有し、Fe2O3の層を備えた板状のピグメントを提供すること;
Fe2O3のうちのいくらかまたは全部をFe3O4に還元すること;および
Fe3O4のうちのいくらかまたは全部をγ−Fe2O3へ酸化すること。
板状のピグメントの提供;
質量磁化率を増加させること;
ここで、提供されるピグメントと得られるピグメントの間の色差(ΔE*)は、約5を超えない。
板状のピグメントの提供;
質量磁化率を増加させること;
ここで、提供されるピグメントと得られるピグメントの間の色差(ΔE*)は、約5を超えない。
ピグメントの磁性特性を向上する方法は、Fe2O3の層を有し、0.1×10−5 m3/kg未満の磁化率を有する、板状のピグメントを提供する工程;
Fe2O3のうちのいくらかまたは全部をFe3O4に還元すること;およびFe3O4のうちのいくらかまたは全部をγ−Fe2O3へ酸化することを含む。
ガラスフレークの例はホウケイ酸塩である。ガラスフレークは、主としてSiO2とAl2O3からなり、ZnO、CaO、B2O3、Na2OおよびK2O、並びにFeOおよびFe2O3をさらに含むことができる。金属フレークの例としては、アルミニウム、銅、亜鉛、および展性を有する他の金属および合金があげられる。展性を有する他の金属および合金の例としては、ニッケル、マグネシウム、アルミニウム−銅合金、アルミニウム−亜鉛合金、アルミニウム−ニッケル合金およびアルミニウム−マグネシウム合金があげられる。金属フレークは、単独でまたはそれの任意の組合わせので使用されてもよい。基体は多層の材料であることができ、たとえば異なる屈折率の複数の材料を含むことができる。基体は雲母を含むことができる。真珠光沢を有するピグメントは、異なる基体の混合物を含むことができる。基体は、粒径が異なる同一または異なるフレークで作られることができる。基体の他の例は繊維である。繊維基体の例としては炭素繊維、ガラス繊維およびポリマーの繊維があげられる。
板状のピグメントの提供;
質量磁化率を増加させること;
ここで、提供されるピグメントと得られるピグメントの間の色差(ΔE*)は、約5以下である。
板状のピグメントの提供;
質量磁化率を増加させること;
ここで、提供されるピグメントと得られるピグメントの間の色差(ΔE*)は、約5以下である。
これは、酸化鉄でコーティングされた磁性ピグメントの利用可能な色範囲を、黒または茶色、または弱められた干渉色を備えた暗い色合い、たとえばColorona(登録商標)Blackstar Blue,Red,Green,および Goldのような暗い色を超えて拡張する。記載されたプロセスに基づいて、従来のブロンズ色、銅色、あずき色および他の従来の金属の真珠光沢を有するピグメントは、磁気的に整列されたコーティングに適用できる。
実施例1−磁性ブロンズ色真珠光沢を有するピグメント
触媒調製:
無水エチレングリコール(320g)およびK15 ポリビニルピロリドン(40g)は、ハウスチャイルドミキサで3000rpmで混合され、溶解された。その後、混合物は、2インチのPTFEでコーティングされた3枚羽攪拌機と窒素パージラインを備えた、PTFEでライニングされた1リットルの円筒形反応器に加えられた。セパレートビーカー内では、無水エチレングリコール(320g)および水和クロロ白金酸結晶(2g、H2PtCl6−6H2O)が均質になるまでかきまぜられた。その後、エチレングリコール混合物は酸素を除去するために10分間超音波で処理され、次に、PVP溶液を含んでいる反応容器へ投入された。追加の無水エチレングリコール(320g)が反応容器に加えられ、室温条件下でおよそ200rpmで撹拌した。その後、窒素パージラインが液表面のすぐ下までおろされ、不活性雰囲気を提供した。その後、混合物はおよそ100分でほぼ20℃から12O℃まで熱された。120℃で1時間保持した後、Pt−in−(PVP/EG)液体(液体1g当たりPt 0.75mg)が冷却され、ガラスジャーへつがれ、密封された。高度に活性の、PVP安定化白金ナノ粒子状物質で、2−10nmの範囲の平均粒径を有するものが得られた。
Fe2O3でコーティングされた天然雲母ピグメント(20g、SunPearlブロンズ、組成は表1中で示される)、およびエチレングリコールの中のPVP安定化白金触媒(4g)をポリエチレングリコール400(96g)中で分散し、一対の45度ピッチのブレードインペラーを装備した600mLスチール製Parr反応器に加えた。撹拌はおよそ800rpmで維持された。反応溶液は、容器を窒素で加圧して、ついで真空下で排出することにより、数回パージされた。十分なパージングに続いて、混合物は220℃に加熱され、水素で10.3barまで加圧され、この条件下で6時間保持された。ピグメントはろ過され、脱イオン水(4リットル)、エタノール(1リットル)ですすがれ、60−80℃で乾燥した。深く、強い色の、金色−ベージュの磁性を有し真珠光沢を有するピグメントであって、α−Fe2O3(ヘマタイト)の内側層とFe3O4(マグネタイト)の表面層を有する天然雲母で構成されるピグメントが得られた(実施例1aと呼ばれる)。
実施例1aで生成された金色−ベージュのピグメント(3.5g)は、Barnstead Thermolyne Model 1400ボックス炉を使用して、空気中で350℃で45分間加熱された。か焼は、外側のマグネタイト層をマグヘマイト(γ−Fe2O3)に変換し、輝きのある、ブロンズ色に着色された磁性を有し真珠光沢を有するピグメントを得た(実施例1b)。
ピグメント(SunPearlブロンズ、実施例1aおよび実施例1b)ドローダウンは、DAC150FVZ−Kモデル(ハウスチャイルドエンジニアリング製;Hauschild Engineering)高速ミキサーを使用して、3分間3000rpmで、Delstar DMR499のアクリルエナメルの4.5g中にピグメントを0.5g分散させることにより調製された。その後、ピグメントサスペンジョンは3ミル(約76ミクロン)のバードアプリケーターを使用して、平坦な白いカード(BYK Gardner、AG−5142)に塗布された。
円形のボタン磁石(13mmのProMAG(登録商標)ネオジム(グレード35、12,300ガウス)磁石)が、0.32cm厚のガラス板の下に置かれた。ピグメントサスペンジョンの塗布の後で硬化前に、カードがガラス板上に置かれ、円形の磁石が各コーティングの選択された部分の下に直接位置するように配置された。
調製されたすべてのピグメント、それらの対応する出発物質ピグメント、および磁気的に整列されたピグメントに対するCIELab値が、Spectraflash SF600 Plus分光光度計(9mmの開口)で測定された。表2を参照。磁気的に整列されたピグメントは、整列された円形のイメージの中心部分、最も高い磁力領域で測定された。整列されたピグメントは、磁界の適用で引き起こされた劇的な色シフトを示す。
色差(ΔE*)値は、実施例1、2および3について、それぞれSunPearlブロンズ、銅およびえび茶に関して測定された。
α−Fe2O3コーティングされた金属色調の天然雲母が、SunPearl銅(サンケミカル社)およびSunPearlえび茶(サンケミカル社)であることを除き、真珠光沢を有するピグメントが、実施例1と同じ方法で生成された。還元されて再度酸化されたSunPearl銅はそれぞれ実施例2aおよび2bであり、還元されて再度酸化されたSunPearlえび茶はそれぞれ実施例3aおよび3bである。
0.1MのHClの706.2g、38.4重量%FeCl3溶液の33.3g、192gの小球にされた尿素、および実施例1bからのピグメントの40gを含む溶液が、180rpmの撹拌下で、1リットルのジャケットを有するポット反応器へ投入された。この最初の溶液は、約1.8のpHを有していた。その後、溶液は90℃に加熱され、尿素の分解および引き続くpHの上昇を促進した。約1〜2時間の後、90℃で、溶液のpHはおよそ6.3−6.5にあがり、反応の完了を示した。作業のために、ピグメントはろ過され、水ですすがれ、65℃で乾燥された。強く色づけられた、磁性を有し、輝くオレンジの真珠光沢を有するピグメントが得られた。
Claims (1)
- 基体および層を含むピグメントであって、該層はγ−Fe2O3およびα−Fe2O3の領域を有し、該γ−Fe2O3の領域はα−Fe2O3の領域より基体から離れているピグメント。
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PCT/US2009/038199 WO2009126437A1 (en) | 2008-04-09 | 2009-03-25 | Magnetic pigments and process of enhancing magnetic properties |
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US8409342B2 (en) | 2013-04-02 |
KR101266923B1 (ko) | 2013-05-31 |
US8211225B2 (en) | 2012-07-03 |
CN101990566A (zh) | 2011-03-23 |
KR20100139136A (ko) | 2010-12-31 |
US20090255442A1 (en) | 2009-10-15 |
US20120261606A1 (en) | 2012-10-18 |
EP2285910B1 (en) | 2017-01-04 |
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