JP3426025B2 - Cosmetics containing organic-inorganic composite pigments - Google Patents
Cosmetics containing organic-inorganic composite pigmentsInfo
- Publication number
- JP3426025B2 JP3426025B2 JP08572394A JP8572394A JP3426025B2 JP 3426025 B2 JP3426025 B2 JP 3426025B2 JP 08572394 A JP08572394 A JP 08572394A JP 8572394 A JP8572394 A JP 8572394A JP 3426025 B2 JP3426025 B2 JP 3426025B2
- Authority
- JP
- Japan
- Prior art keywords
- red
- pigment
- inorganic
- organic
- sulfuric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Description
【０００１】[0001]
【産業上の利用分野】本発明は高彩度、高隠蔽性を持
ち、分散性、色調の経時安定性に優れた有機−無機複合
顔料を配合してなる化粧料に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cosmetic composition containing an organic-inorganic composite pigment having a high chroma and a high hiding property, and having excellent dispersibility and stability of color tone over time.
【０００２】[0002]
【従来の技術】一般化粧料、パウダーファンデーショ
ン、乳化型ファンデーション等のベースメークアップ料
に用いられる有色顔料としては、一般に無機顔料や有機
顔料が汎用されている。このようなベースメークアップ
料は、皮膚に塗布した際の仕上がり感を良好なものとす
るために、シミ、ソバカス等の肌のトラブルを自然にカ
バーでき、色味の発色が均一であり、経時変化で色がく
すんだりしない事が重要である。しかし、色調の面から
述べると赤色系無機顔料であるベンガラ類はそのもの自
身の彩度が低いという問題を有している。更にベンガラ
類は皮膚から分泌される皮脂や水分等により濡れると色
調が赤黒く変化してしまう。一方黄色水和酸化鉄は皮膚
から分泌される皮脂や水分により濡れると屈折率が低下
してしまう。そのためにこのような有色無機顔料を使用
したベースメークアップ料は、経時で赤黒い色調に変化
したり、光学的に下地の肌色を反映するようになるた
め、塗布色がくすんでくるという欠点を有していた。2. Description of the Related Art Inorganic pigments and organic pigments are generally used as color pigments used in base makeup materials such as general cosmetics, powder foundations and emulsion foundations. Such a base make-up agent can naturally cover skin problems such as spots and freckles in order to improve the feeling of finish when applied to the skin, and has a uniform color development, It is important that the color does not become dull due to changes. However, in terms of color tone, red iron oxides such as red iron oxide have a problem in that they themselves have low saturation. Furthermore, red iron oxide changes its color to reddish black when it is wet with oil and water secreted from the skin. On the other hand, yellow hydrated iron oxide has a reduced refractive index when it is wet with sebum or water secreted from the skin. Therefore, a base make-up material using such a colored inorganic pigment has a drawback that the coating color becomes dull because it changes to a reddish black color tone over time or optically reflects the skin color of the base. Was.
【０００３】一方、乳化型のファンデーションにおいて
は、これらのくすみ現象を防止するため有機顔料である
赤色２２６号の使用が試みられている。しかし、赤色２
２６号が親油性を示し、有色無機顔料が親水性を示す事
から、界面活性剤の選択やＨＬＢの調整が難しく、どち
らか一方が凝集し易くなるため、商品化には困難を伴っ
ていた。On the other hand, in emulsion type foundations, it has been attempted to use red pigment No. 226, which is an organic pigment, in order to prevent these dullness phenomena. But red 2
Since No. 26 shows lipophilicity and the colored inorganic pigment shows hydrophilicity, it is difficult to select a surfactant and adjust HLB, and one of them easily aggregates, which makes it difficult to commercialize. .
【０００４】又、シミ、ソバカス等の肌のトラブルのカ
バー力の面から述べると、通常カバー力のある白色顔料
として、屈折率が２．５〜２．７５の二酸化チタンが用
いられている。シミ、ソバカス等の肌のトラブルをより
きれいにカバーしようとすると二酸化チタンの処方中で
の配合量が多くなり、その結果有色無機顔料の隠蔽力を
越えてしまうと、塗布色が白っぽくなりすぎて、いわゆ
る白ボケした仕上がりとなってメークアップ料の目的か
ら外れてしまう。特にこの現象は明度が高く淡い色調の
肌色系で顕著に見られる。In terms of covering power for skin troubles such as spots and freckles, titanium dioxide having a refractive index of 2.5 to 2.75 is usually used as a white pigment having covering power. If you try to cover skin problems such as spots and freckles more beautifully, the amount of titanium dioxide will be increased in the formulation, and if the hiding power of the colored inorganic pigment is exceeded as a result, the applied color will be too whitish, The result is a so-called bokeh finish, which defeats the purpose of the makeup fee. This phenomenon is particularly noticeable in a flesh color system having a high lightness and a light color tone.
【０００５】又、美爪料に於いては美爪料に用いられる
有機顔料やパール顔料と二酸化チタンとでは比重差が大
きいため、色分かれやケーキングの原因となり、中には
再分散不可能な場合も生じるため、著しく商品価値を損
なうものであった。Further, in the nail enamel, since there is a large difference in specific gravity between the organic pigment or pearl pigment used in the nail enamel and titanium dioxide, it causes color separation or caking and cannot be redispersed therein. In some cases, the product value is significantly impaired.
【０００６】このような従来技術の欠点を改良した技術
としては、
（１）化学的方法によって水溶液化した染料に微粉砕し
た薄片状基質を加えた後、基質粒子表面に染料を沈澱、
沈着せしめる事により得られた発色性の良好な顔料を用
いる方法（特開昭６２−９１５６５号公報）。
（２）水系において基質粒子表面に顔料を析出、被覆せ
しめる事により得られた着色雲母顔料を用いる方法（特
開昭６３−２４３１６８号公報）。
（３）金属酸化物被覆雲母、雲母、セリサイト、カオリ
ン等の薄片状基質粒子上に顔料及び／又は染料粒子を液
体媒体を使用する事無く所定の高速攪拌によって薄片状
基質粒子とこれらの顔料や染料の粒子とでオーダードミ
クスチュアーを形成させて得られた彩度、分散性に優れ
且つ顔料や染料の付着安定性に優れている薄片状複合顔
料を用いる方法（特開平５−２１４２５７号公報）等が
提案されている。Techniques for improving the above-mentioned drawbacks of the prior art include (1) adding finely pulverized flaky substrates to a dye made into an aqueous solution by a chemical method, and then precipitating the dye on the surface of substrate particles,
A method of using a pigment having good colorability obtained by depositing (JP-A-62-91565). (2) A method of using a colored mica pigment obtained by depositing and coating a pigment on the surface of substrate particles in an aqueous system (JP-A-63-243168). (3) Flake-like substrate particles and pigments obtained by stirring pigments and / or dye particles on flake-like substrate particles such as mica, mica, sericite, kaolin and the like coated with metal oxide by a predetermined high speed stirring without using a liquid medium. A method of using a flaky composite pigment having excellent saturation and dispersibility, which is obtained by forming an ordered mixture with particles of a dye or a dye, and excellent adhesion stability of a pigment or a dye (JP-A-5-214257). Gazette) etc. have been proposed.
【０００７】[0007]
【発明が解決しようとする課題】しかしながら、
（１）、（２）の技術では、顔料や染料の微粒子化、分
散が未だ十分でないため、満足できる発色は得にくい。
更には処理工程において基質粒子表面に付着しなかった
或いは付着が弱かった顔料や染料は濾過工程或いは洗浄
工程において分離、脱落し、使用した顔料や染料の仕込
量に対して期待される発色性が得られない場合がある。[Problems to be Solved by the Invention] However,
According to the techniques (1) and (2), it is difficult to obtain a satisfactory color because the fine particles and the dispersion of the pigment or dye are not yet sufficient.
Furthermore, pigments or dyes that did not adhere to the surface of the substrate particles in the treatment process or were weakly adhered were separated and dropped during the filtration process or washing process, and the expected color development was found for the amount of pigment or dye used. You may not get it.
【０００８】又（３）の技術では衝撃力、圧縮力、剪断
力等の物理的手段により固着しているため、必ずしも顔
料や染料の全てが安定且つ均一に基質表面に固定される
わけではない。その上、高速攪拌により基質が粉砕され
る結果、基質の粒度分布幅が広がり、高彩度化には良い
影響を与えない。Further, in the technique (3), since the particles are fixed by physical means such as impact force, compression force and shearing force, not all the pigments and dyes are necessarily fixed stably and uniformly on the substrate surface. . In addition, as a result of the substrate being crushed by the high-speed stirring, the particle size distribution width of the substrate is widened, which does not have a favorable effect on the high saturation.
【０００９】更には基質に屈折率の低い薄片状物質を用
いているため、透明性が高く、下地色の影響を受けて高
彩度になりにくい。そのため特に化粧料の分野において
は下地である肌の形態が見え易い事と相俟って着色剤と
しての用途が大きく限定される。Furthermore, since a flaky material having a low refractive index is used as the substrate, it has high transparency and is unlikely to have high saturation due to the influence of the underlying color. Therefore, particularly in the field of cosmetics, the use as a coloring agent is greatly limited in combination with the fact that the morphology of the underlying skin is easily visible.
【００１０】そこで本発明は前記従来技術の問題点を解
決し、高彩度、高隠蔽性を持ち、分散性、色調の経時安
定性に優れた化粧料を提供する事を課題とする。[0010] Therefore, an object of the present invention is to solve the above-mentioned problems of the prior art and to provide a cosmetic having high saturation and high hiding power, and excellent dispersibility and stability of color tone over time.
【００１１】[0011]
【課題を解決するための手段】本発明者らは上記課題を
解決するため、有機顔料と高屈折率無機白色顔料を複合
化した場合の彩度と隠蔽力の変化について鋭意研究を重
ねた結果、高屈折率無機白色顔料表面に赤色２２６号を
均一且つ強固に付着させて複合化した場合には単に高屈
折率無機白色顔料と赤色２２６号とを混合した場合より
もはるかに高彩度、高隠蔽力を示す事、また処方中での
分散性、色調の経時安定性にも優れている事を見いだ
し、本発明を完成させるに至った。In order to solve the above-mentioned problems, the present inventors have conducted extensive studies on changes in saturation and hiding power when an organic pigment and a high-refractive-index inorganic white pigment are combined. In the case where Red 226 is adhered uniformly and firmly to the surface of the high refractive index inorganic white pigment to form a composite, the saturation and the hiding are much higher than those obtained by simply mixing the high refractive index inorganic white pigment and Red 226. The inventors have found that they exhibit strength, are excellent in dispersibility in a formulation, and are stable in color tone over time, and have completed the present invention.
【００１２】すなわち本発明は、屈折率２以上且つ平均
粒子径０．１〜６０μｍである無機白色顔料を赤色２２
６号で被覆した有機−無機複合顔料を配合する化粧料で
あって、該有機−無機複合顔料は、赤色２２６号が溶解
し且つ無機白色顔料が分散する硫酸を水に滴下して、該
無機白色顔料の表面に該赤色２２６号を被覆させて得ら
れたものであり、該無機白色顔料は、酸化亜鉛、酸化ジ
ルコニウム、酸化チタン（アナタース型）、酸化チタン
（ルチル型）の一種又は二種以上の組み合わせから選ば
れるものである化粧料を提供するものであり、この化粧
料は、高彩度、高隠蔽性を持ち、分散性、色調の経時安
定性に優れる。 That is, the present invention has a refractive index of 2 or more and an average value.
Inorganic white pigment having a particle size of 0.1 to 60 μm is red 22
A cosmetic containing an organic-inorganic composite pigment coated with No. 6
So, in the organic-inorganic composite pigment, red No. 226 is dissolved.
And adding sulfuric acid in which the inorganic white pigment is dispersed into the water,
Obtained by coating the surface of an inorganic white pigment with the red No. 226
The inorganic white pigment includes zinc oxide and dioxide.
Ruconium, titanium oxide (anatase type), titanium oxide
(Rutile type) or a combination of two or more
This makeup is intended to provide cosmetics
Fee, high chroma have a high hiding property, dispersibility, Ru good stability of color tone.
【００１３】以下に本発明を詳細に説明する。The present invention will be described in detail below.
【００１４】本発明に適用される、無機白色顔料を赤色
２２６号で被覆した有機−無機複合顔料は（１）赤色２
２６号を硫酸に溶解する工程と（２）赤色２２６号を溶
解した硫酸に無機白色顔料を分散させる工程と（３）赤
色２２６号を溶解し、無機白色顔料を分散させた硫酸を
水に滴下して、無機白色顔料の表面に赤色２２６号を被
覆させる工程とから製造される。The organic-inorganic composite pigment applied to the present invention, which is an inorganic white pigment coated with Red No. 226, is (1) Red 2.
No. 26 is dissolved in sulfuric acid, (2) Disperse inorganic white pigment in sulfuric acid in which red 226 is dissolved, and (3) Dissolve red 226, and sulfuric acid in which inorganic white pigment is dispersed is dropped into water. And coating the surface of the inorganic white pigment with Red No. 226.
【００１５】赤色２２６号を溶解する溶媒として硫酸以
外の酸を使用すると、概して水を相当量含有するため、
赤色２２６号を十分に溶解できない。この理由から硫酸
を用いる場合も水の含有量が１０重量％以下のものを使
用しないと赤色２２６号を完全に溶解する事は出来な
い。When an acid other than sulfuric acid is used as a solvent for dissolving Red No. 226, it generally contains a considerable amount of water.
Red 226 cannot be fully dissolved. For this reason, even when sulfuric acid is used, red 226 cannot be completely dissolved unless the water content is 10% by weight or less.
【００１６】（１）及び（２）の工程は前後しても、或
いは同時に行っても差し支えないが、赤色２２６号の溶
解状態や、無機白色顔料の分散状態が確認しやすいの
で、上記手順に従う方が好ましい。The steps (1) and (2) may be carried out before or after, or at the same time, but it is easy to confirm the dissolved state of Red No. 226 and the dispersed state of the inorganic white pigment, so follow the above procedure. Is preferred.
【００１７】この赤色２２６号を硫酸に溶解する工程及
び赤色２２６号を溶解し、無機白色顔料を分散させた硫
酸を水に滴下して、無機白色顔料の表面に赤色２２６号
を被覆させる工程においては、溶解熱により溶液の温度
が上昇するが、７０℃、更に好ましくは５０℃を越えて
上昇しないように赤色２２６号の投入速度を調節した
り、水冷、空冷等の方法で冷却する事が望ましい。７０
℃を越えると赤色２２６号の色調が本来の色調から青み
を帯びた色調に変化する上、変化した色調の再現性にも
乏しく商品価値を損ねてしまう。In the step of dissolving Red No. 226 in sulfuric acid and the step of dissolving Red No. 226 and dropping sulfuric acid in which the inorganic white pigment is dispersed into water to coat the surface of the inorganic white pigment with Red No. 226. , The temperature of the solution rises due to the heat of dissolution, but it is possible to adjust the charging speed of Red 226 so that it does not rise above 70 ° C., more preferably 50 ° C., or cool it by a method such as water cooling or air cooling. desirable. 70
When the temperature exceeds ℃, the color tone of Red No. 226 changes from the original color tone to a bluish color tone, and the reproducibility of the changed color tone is poor and the commercial value is impaired.
【００１８】被覆される無機白色顔料は屈折率が２以上
のものが好ましい。屈折率が２未満のものを用いると透
明性が強くなり、下地の形態が見えやすく且つ下地のア
ンダートーンの色味の影響を受けるため高彩度、高隠蔽
力の顔料が得られない。このような屈折率が２以上の白
色無機顔料としては、酸化亜鉛（屈折率２．０）、酸化
ジルコニウム（屈折率２．４）、アナタース型酸化チタ
ン（屈折率２．５）ルチル型酸化チタン（屈折率２．７
５）やこれらの混合物、複合物等が好適に使用できる。The inorganic white pigment to be coated preferably has a refractive index of 2 or more. When a material having a refractive index of less than 2 is used, the transparency becomes strong, and the morphology of the base is easily visible, and it is affected by the tint of the undertone of the base, so a pigment with high saturation and high hiding power cannot be obtained. Such white inorganic pigments having a refractive index of 2 or more include zinc oxide (refractive index 2.0), zirconium oxide (refractive index 2.4), anatase type titanium oxide (refractive index 2.5) rutile type titanium oxide. (Refractive index 2.7
5) or a mixture or composite of these can be preferably used.
【００１９】白色無機顔料の平均粒子径は０．１〜６０
μｍの範囲にある事が望ましい。平均粒子径が０．１μ
ｍ未満であると顔料の隠蔽力が低下する上、光学的に十
分な顔料分散状態が得にくく、６０μｍを越えると十分
な着色力が得られないだけでなく、粒子感が感じられる
ようになり、好ましくない。The average particle size of the white inorganic pigment is 0.1-60.
It is desirable to be in the range of μm. Average particle size is 0.1μ
When it is less than m, the hiding power of the pigment is lowered, and it is difficult to obtain an optically sufficient pigment dispersion state, and when it exceeds 60 μm, not only sufficient coloring power is not obtained, but also a particle feeling is felt. , Not preferable.
【００２０】以下、本発明に適用される赤色２２６号で
被覆してなる高屈折率無機白色顔料を製造例により更に
詳細に説明する。Hereinafter, the high refractive index inorganic white pigment coated with Red No. 226, which is applied to the present invention, will be described in more detail with reference to production examples.
【００２１】製造例１．ガラス容器に濃硫酸３００ｇを
秤量し、赤色２２６号（大東化成製）２０ｇを攪拌しな
がら投入し完全に溶解させた。この溶解操作の間、０〜
５℃に冷却した水を循環させたガラス性蛇管をガラス容
器内に設置して、溶液の温度は４２℃以下に保持した。
３０分攪拌を続けた後、酸化チタンＡ−１００（石原産
業製）８０ｇを投入し、更に３０分攪拌を続けて均一分
散させた。これとは別の容器に水３０００ｇと氷５００
ｇを入れた氷水を用意しておき、この中に酸化チタンを
均一分散させた赤色２２６号−濃硫酸溶液を攪拌しなが
らゆっくり注入した。注入終了時の温度は３７℃であっ
た。その後２０分間攪拌し濾過して、洗浄水のｐＨが中
性になるまで水洗、濾過を繰り返した後、８０℃で乾燥
し、粉砕して赤色２２６号被覆酸化チタン顔料を得た。Production Example 1. 300 g of concentrated sulfuric acid was weighed in a glass container, and 20 g of Red No. 226 (manufactured by Daito Kasei) was added with stirring to completely dissolve it. During this dissolution operation, 0-
A glass flexible tube in which water cooled to 5 ° C was circulated was placed in a glass container, and the temperature of the solution was kept at 42 ° C or lower.
After continuing stirring for 30 minutes, 80 g of titanium oxide A-100 (manufactured by Ishihara Sangyo Co., Ltd.) was added, and stirring was continued for 30 minutes to uniformly disperse. In a separate container, 3000g water and 500 ice cubes
Ice water containing g was prepared in advance, and a red No. 226-concentrated sulfuric acid solution in which titanium oxide was uniformly dispersed therein was slowly injected with stirring. The temperature at the end of injection was 37 ° C. Then, the mixture was stirred for 20 minutes, filtered, washed with water until the pH of the washing water became neutral, and filtered, then dried at 80 ° C. and pulverized to obtain a red 226-coated titanium oxide pigment.
【００２２】製造例２．ガラス容器に濃硫酸５００ｇを
秤量し、赤色２２６号（大東化成製）３０ｇを攪拌しな
がら投入し完全に溶解させた。この溶解操作の間、０〜
５℃に冷却した水を循環させたガラス性蛇管をガラス容
器内に設置して、溶液の温度を４８℃以下に保持した。
３０分攪拌を続けた後、酸化ジルコニウム（東ソー製）
７０ｇを投入し、更に３０分攪拌を続けて均一分散させ
た。これとは別の容器に水３０００ｇと氷５００ｇを入
れた氷水を用意しておき、この中に酸化ジルコニウムを
均一分散させた赤色２２６号−濃硫酸溶液を攪拌しなが
らゆっくり注入した。注入終了時の温度は４４℃であっ
た。その後２０分間攪拌し濾過して、洗浄水のｐＨが中
性になるまで水洗、濾過を繰り返した後、９０℃で乾燥
し、粉砕して赤色２２６号被覆酸化ジルコニウム顔料を
得た。Manufacturing Example 2. 500 g of concentrated sulfuric acid was weighed in a glass container, and 30 g of Red No. 226 (manufactured by Daito Kasei) was added with stirring to completely dissolve it. During this dissolution operation, 0-
A glass flexible tube in which water cooled to 5 ° C was circulated was placed in a glass container to keep the temperature of the solution at 48 ° C or lower.
After stirring for 30 minutes, zirconium oxide (manufactured by Tosoh)
70 g was added, and stirring was continued for further 30 minutes for uniform dispersion. Ice water containing 3000 g of water and 500 g of ice was prepared in a separate container, and a red No. 226-concentrated sulfuric acid solution in which zirconium oxide was uniformly dispersed therein was slowly added while stirring. The temperature at the end of injection was 44 ° C. Then, the mixture was stirred for 20 minutes, filtered, washed with water until the pH of the wash water became neutral, and filtered, then dried at 90 ° C. and pulverized to obtain a red No. 226-coated zirconium oxide pigment.
【００２３】製造例３．ガラス容器に濃硫酸１０００ｇ
を秤量し、赤色２２６号（大東化成製）５ｇを攪拌しな
がら投入し完全に溶解させた。この溶解操作の間、溶液
の温度は３５℃以下に保持した。３０分攪拌を続けた
後、酸化チタンＡ−１００（石原産業製）９０ｇと酸化
亜鉛５ｇを投入し、更に３０分攪拌を続けて均一分散さ
せた。これとは別の容器に水３０００ｇと氷５００ｇを
入れた氷水を用意しておき、この中に酸化チタンと酸化
亜鉛を均一分散させた赤色２２６号−濃硫酸溶液を攪拌
しながらゆっくり注入した。注入終了時の温度は５６℃
であった。その後２０分間攪拌し濾過して、洗浄水のｐ
Ｈが中性になるまで水洗、濾過を繰り返した後、６０℃
で乾燥し、粉砕して赤色２２６号被覆酸化チタン−酸化
亜鉛顔料を得た。Production Example 3. 1000g concentrated sulfuric acid in a glass container
Was weighed, and 5 g of Red No. 226 (manufactured by Daito Kasei) was added with stirring to completely dissolve it. During this dissolution operation, the temperature of the solution was kept at 35 ° C or lower. After continuing stirring for 30 minutes, 90 g of titanium oxide A-100 (manufactured by Ishihara Sangyo Co., Ltd.) and 5 g of zinc oxide were added, and stirring was continued for 30 minutes to uniformly disperse. Ice water containing 3000 g of water and 500 g of ice was prepared in a container different from this, and a red No. 226-concentrated sulfuric acid solution in which titanium oxide and zinc oxide were uniformly dispersed therein was slowly poured while stirring. The temperature at the end of injection is 56 ° C
Met. After that, stir for 20 minutes, filter, and p
After repeating washing with water and filtration until H became neutral, 60 ℃
And dried and pulverized to obtain red 226-coated titanium oxide-zinc oxide pigment.
【００２４】製造例４．ガラス容器に濃硫酸６００ｇを
秤量し、赤色２２６号（大東化成製）５０ｇを攪拌しな
がら投入し完全に溶解させた。この溶解操作の間、溶液
の温度は６２℃以下に保持した。３０分攪拌を続けた
後、酸化チタンＡ−１００（石原産業製）５０ｇを投入
し、更に３０分攪拌を続けて均一分散させた。これとは
別の容器に水３０００ｇと氷５００ｇを入れた氷水を用
意しておき、この中に酸化チタンを均一分散させた赤色
２２６号−濃硫酸溶液を攪拌しながらゆっくり注入し
た。注入終了時の温度は４８℃であった。その後２０分
間攪拌し濾過して、洗浄水のｐＨが中性になるまで水
洗、濾過を繰り返した後、４０℃で４８時間乾燥し、粉
砕して赤色２２６号被覆酸化チタン顔料を得た。Production Example 4. 600 g of concentrated sulfuric acid was weighed in a glass container, and 50 g of Red No. 226 (manufactured by Daito Kasei) was added with stirring to completely dissolve it. During this dissolution operation, the temperature of the solution was kept at 62 ° C or lower. After stirring for 30 minutes, 50 g of titanium oxide A-100 (manufactured by Ishihara Sangyo Co., Ltd.) was added, and stirring was continued for 30 minutes to uniformly disperse. Ice water containing 3000 g of water and 500 g of ice was prepared in a separate container, and a red No. 226-concentrated sulfuric acid solution in which titanium oxide was uniformly dispersed was slowly poured into the container while stirring. The temperature at the end of injection was 48 ° C. Then, the mixture was stirred and filtered for 20 minutes, washed repeatedly with water until the pH of the wash water became neutral, and then filtered, dried at 40 ° C. for 48 hours, and pulverized to obtain a red 226-coated titanium oxide pigment.
【００２５】本発明に使用される有機−無機複合顔料
は、剤型や要求される外観色により異なるが、通常化粧
料中に０．０１〜１０重量％、好ましくは０．１〜５重
量％配合される。The organic-inorganic composite pigment used in the present invention is usually 0.01 to 10% by weight, preferably 0.1 to 5% by weight in cosmetics, although it varies depending on the dosage form and the required appearance color. Be compounded.
【００２６】又、本発明に使用される有機−無機複合顔
料は、彩度、隠蔽力に優れているので、赤色２２６号を
無機白色顔料と単に併用する場合よりも、配合される赤
色２２６号の量を実質的に低減する事が出来るので、皮
膚の安全面から見ても好ましいものである。Further, since the organic-inorganic composite pigment used in the present invention is excellent in saturation and hiding power, it is better to mix Red No. 226 with the inorganic white pigment than to use it in combination. The amount can be substantially reduced, which is preferable from the viewpoint of skin safety.
【００２７】以下、実施例により本発明を更に詳細に説
明する。Hereinafter, the present invention will be described in more detail with reference to examples.
【００２８】[0028]
【実施例】製造例１〜４の赤色２２６号で被覆してなる
高屈折率無機白色顔料を使用して実施例１〜５の化粧料
を製造した。EXAMPLES The cosmetics of Examples 1 to 5 were produced using the high refractive index inorganic white pigments coated with Red No. 226 of Production Examples 1 to 4.
【００２９】
実施例１．乳化型ファウンデーション
（処方）
１．製造例１の複合顔料２．０％配合色素ペースト ２１．０
２．ステアリン酸 １．７５
３．非イオン界面活性剤 ５．０
４．トリ−２-エチルヘキサン酸グリセリン ３．０
５．ブチルパラベン ０．１
６．ＰＥＧ−４００ １．０
７．カルボキシメチルセルロースナトリウム塩 ０．１
８．メチルパラベン ０．２
９．トリエタノールアミン ０．７
１０．珪酸アルミニウムマグネシウム １．０
１１．精製水 ６６．１５
（製造法）１〜５の成分を８５℃で溶解、分散させ、油
相組成物を得た。別途１１の精製水に６〜１０の成分を
溶解、混合し８５℃まで加温して水相組成物を得た。油
相組成物に水相組成物を添加して乳化し、冷却して乳化
型ファウンデーションを得た。Example 1. Emulsion type foundation (prescription) 1. Dye paste containing 2.0% of the composite pigment of Production Example 21.0 2. Stearic acid 1.75 3. Nonionic surfactant 5.0 4. Glycerin tri-2-ethylhexanoate 3.0 5. Butylparaben 0.1 6. PEG-400 1.0 7. Carboxymethyl cellulose sodium salt 0.1 8. Methylparaben 0.2 9. Triethanolamine 0.7 10. Aluminum magnesium silicate 1.0 11. Purified water 66.15 (Production method) Components 1 to 5 were dissolved and dispersed at 85 ° C to obtain an oil phase composition. Separately, 6 to 10 components were dissolved and mixed in 11 purified water and heated to 85 ° C. to obtain an aqueous phase composition. The aqueous phase composition was added to the oil phase composition to emulsify and then cooled to obtain an emulsified foundation.
【００３０】
実施例２．頬紅
（処方）
１．タルク ６６．７５
２．セリサイト １３．０
３．カオリン １０．０
４．ミリスチン酸亜鉛 ２．０
５．炭酸マグネシウム １．０
６．製造例２の複合顔料 ０．５
７．赤色２０２号 ０．０４
８．弁柄 １．１
９．ステアリン酸 ２．５
１０．流動パラフィン ２．２
１１．ラノリン ０．６
１２．非イオン界面活性剤 ０．３
１３．ビタミンＥ ０．０１
（製造法）１〜８の成分を粉砕機で粉砕した後、ヘンシ
ェルミキサーに移し、６０℃に温度を調整した。別途９
〜１３の成分を８５℃で溶解、混合させ、ヘンシェルミ
キサーに注入して、粉体部にコーティングし、冷却した
後取り出して粉砕機で粉砕し、プレス成型して頬紅を得
た。Example 2. Blusher (prescription) 1. Talc 66.75 2. Sericite 13.0 3. Kaolin 10.0 4. Zinc myristate 2.0 5. Magnesium carbonate 1.0 6. Composite pigment of Production Example 2 0.5 7. Red No. 202 0.04 8. Rouge 1.1 9. Stearic acid 2.5 10. Liquid paraffin 2.2 11. Lanolin 0.6 12. Nonionic surfactant 0.3 13. Vitamin E 0.01 (Manufacturing method) After crushing the components of 1 to 8 with a crusher, they were transferred to a Henschel mixer and the temperature was adjusted to 60 ° C. 9 separately
The ingredients (13) to (13) were dissolved and mixed at 85 ° C., poured into a Henschel mixer, coated on the powder portion, cooled, taken out, pulverized with a pulverizer, and press-molded to obtain a blusher.
【００３１】
実施例３．リップカラー
（処方）
１．イソステアリン酸ジグリセライド １４．７
２．トリ−２−エチルヘキサン酸グリセリン ６．８
３．グリセリン脂肪酸エステル １０．８
４．マイクロクリスタリンワックス １５．６
５．ビーズワックス １．５
６．キャンデリラワックス ６．４
７．カルナバワックス ０．５
８．製造例４の複合顔料を２％含む色素ペースト ４３．７
（製造法）１〜７の成分を９０℃で混合溶解した後、８
の色素ペーストを添加、攪拌し均一に分散させて、減圧
して脱泡した。９０℃に保持しながらリップ金型に充填
し、冷却してリップカラーを得た。Example 3. Lip color (prescription) 1. Isostearic acid diglyceride 14.7 2. Glycerin tri-2-ethylhexanoate 6.8 3. Glycerin fatty acid ester 10.8 4. Microcrystalline wax 15.6 5. Bead wax 1.5 6. Candelilla wax 6.4 7. Carnauba wax 0.5 8. Dye paste containing 2% of the composite pigment of Production Example 43.7 (Production method) Components 1 to 7 were mixed and dissolved at 90 ° C., and then 8
The dye paste of (1) was added, and the mixture was stirred and uniformly dispersed. It was filled in a lip mold while maintaining at 90 ° C. and cooled to obtain a lip color.
【００３２】
実施例４．美爪料
（処方）
１．ニトロセルロース １５．０
２．アルキッド樹脂 １２．０
３．フタル酸ジブチル ６．０
４．酢酸ブチル ２３．０
５．酢酸エチル ９．０
６．エタノール ７．０
７．トルエン ２５．０
８．製造例１の複合顔料 ３．０
（製造法）１〜７の成分を混合溶解した後、これに８の
複合顔料を添加してボールミルで均一に分散させ、美爪
料を得た。Example 4. Nails (prescription) 1. Nitrocellulose 15.0 2. Alkyd resin 12.0 3. Dibutyl phthalate 6.0 4. Butyl acetate 23.0 5. Ethyl acetate 9.0 6. Ethanol 7.0 7. Toluene 25.0 8. Composite Pigment 3.0 of Production Example 1 (Production Method) After mixing and dissolving the components 1 to 7, the composite pigment of 8 was added and uniformly dispersed in a ball mill to obtain a nail enamel.
【００３３】
実施例５．水性ネイルカラー
（処方）
１．アクリルポリマーエマルション ７７．７
２．カルビトール ７．７
３．フタル酸ジエチル ３．９
４．精製水 ７．７
５．製造例３の複合顔料 ２．４
６．ベントナイト ０．４
７．防腐剤 ０．１
８．シリコーン系消泡剤 ０．１
（製造法）精製水にカルビトールとフタル酸ジエチルを
加え、これに複合顔料を分散させた後、アクリルポリマ
ーエマルションと６〜８の成分を添加し均一になるよう
攪拌混合を行った。混合後、脱気処理を行い、水性ネイ
ルカラーを得た。Example 5. Aqueous nail color (prescription) 1. Acrylic polymer emulsion 77.7 2. Carbitol 7.7 3. Diethyl phthalate 3.9 4. Purified water 7.7 5. Composite Pigment of Production Example 2.4 6. Bentonite 0.4 7. Preservative 0.1 8. Silicone antifoaming agent 0.1 (Production method) Carbitol and diethyl phthalate are added to purified water, the composite pigment is dispersed therein, and then an acrylic polymer emulsion and 6 to 8 components are added to make the mixture uniform. Stir mixing was performed. After mixing, deaeration treatment was performed to obtain an aqueous nail color.
【００３４】製造例１〜４の有機−無機複合顔料につい
て、被覆された赤色２２６号の付着安定性及び有機−無
機複合顔料の隠蔽力、彩度を、実施例１〜５の化粧料に
ついて、分散性、色調の安定性を評価した。With respect to the organic-inorganic composite pigments of Production Examples 1 to 4, the adhesion stability of the coated red No. 226 and the hiding power and chroma of the organic-inorganic composite pigments were evaluated. The dispersibility and the stability of color tone were evaluated.
【００３５】１．有機−無機複合顔料の付着安定性の評
価
精製水２００ｍｌ中に製造例１〜４の有機−無機複合顔
料６ｇを入れ、ホモミキサーで３０分間攪拌した後遠心
分離器（国産（株）製Ｈ−２００ＮＲ）を用い、９，０
００ｒｐｍで３０分間処理した後、観察したところ、下
部に沈降した有機−無機複合顔料には酸化チタンとＲ−
２２６号との分離は全く認められなかった。1. Evaluation of Adhesion Stability of Organic-Inorganic Composite Pigment Put 6 g of the organic-inorganic composite pigment of Production Examples 1 to 4 in 200 ml of purified water, stir with a homomixer for 30 minutes, and then centrifuge (H-produced by Kokusan Co., Ltd.). 200NR) and 9,0
After treatment at 00 rpm for 30 minutes, observation revealed that titanium-oxide and R-
No separation from No. 226 was observed.
【００３６】２．有機−無機複合顔料の隠蔽力の評価
製造例１〜４の有機−無機白色顔料１．０ｇを精秤し、
ひまし油１．５ｇとともにフーバーマーラーを用いて、
１５０回混練した。混練したサンプル０．５ｇを５０ｍ
ｌ容量のポリエチレン製ディスポーザブルカップに秤取
り、その中に透明ネイルエナメルラッカー１０ｇを入
れ、均一になるまで攪拌した。攪拌中に揮発したネイル
エナメルラッカーを補充して攪拌した後、隠蔽率試験紙
（日本テストパネル工業株式会社製）上に１０ｍｉｌの
ドクターブレードを用いて製膜して評価試料とした。2. Evaluation of hiding power of organic-inorganic composite pigments 1.0 g of the organic-inorganic white pigments of Production Examples 1 to 4 were precisely weighed,
Using Hoover Mahler with 1.5 g of castor oil,
Kneaded 150 times. 50 g of kneaded sample 0.5 g
10 g of a transparent nail enamel lacquer was placed in a 1-volume polyethylene disposable cup, and the mixture was stirred until uniform. The nail enamel lacquer volatilized during stirring was replenished and stirred, and then a film was formed on a concealment rate test paper (manufactured by Japan Test Panel Industry Co., Ltd.) using a doctor blade of 10 mil to obtain an evaluation sample.
【００３７】隠蔽率試験紙の製膜していない白色部と黒
色部の４００〜７００ｎｍにおける分光スペクトルの差
を１００として、製膜した白色部と黒色部の４００〜７
００ｎｍにおける分光スペクトルの差を百分率に換算し
隠蔽率を求めた。製造例１〜４の化粧料１．０ｇを隠蔽
率試験紙（日本テストパネル工業株式会社製）上に１０
ｍｉｌのドクターブレードを用いて製膜して評価試料と
し、隠蔽率試験紙の製膜していない白色部と黒色部の４
００〜７００ｎｍにおける分光スペクトルの差を１００
として、製膜した白色部と黒色部の４００〜７００ｎｍ
における分光スペクトルの差を百分率に換算し隠蔽率を
求めて評価した。Taking the difference in the spectral spectrum at 400 to 700 nm between the non-film-formed white part and the black part of the hiding rate test paper as 100, the film-formed white part and the black part 400 to 7
The concealment ratio was calculated by converting the difference in the spectrum at 00 nm into a percentage. 1.0 g of the cosmetics of Production Examples 1 to 10 was applied on a hiding rate test paper (manufactured by Nippon Test Panel Industry Co., Ltd.).
Using a mil doctor blade to form a film as an evaluation sample, the concealment rate test paper was divided into 4 parts, a white part and a black part, which were not formed.
The difference in the spectrum between 00 and 700 nm is 100
As a film, the white part and the black part of 400-700 nm
The difference between the spectral spectra at was converted into a percentage, and the hiding ratio was obtained and evaluated.
【００３８】３．有機−無機複合顔料の彩度の評価
隠蔽率試験紙に製膜した評価試料の白色部を、ミノルタ
製分光色差計ＣＭ−１０００を用いて、分光スペクトル
を測定し、Ｌ−ａ−ｂ値を算出した。3. Saturation evaluation of organic-inorganic composite pigment Concealment rate The white part of the evaluation sample formed on the test paper was measured for a spectrum using a spectrocolorimeter CM-1000 manufactured by Minolta, and the L-a-b value was measured. It was calculated.
【００３９】結果を表１に示す。The results are shown in Table 1.
【００４０】[0040]
【表１】 [Table 1]
【００４１】４．化粧料における有機−無機複合顔料の
分散性の評価
実施例１〜５に示した化粧料について光学顕微鏡で観察
した結果、いずれの化粧料もメジアン径でおよそ０．４
３〜０．４７μｍの範囲の均一な分散状態を示してお
り、凝集体は認められなかった。4. Evaluation of Dispersibility of Organic-Inorganic Composite Pigment in Cosmetics As a result of observing the cosmetics shown in Examples 1 to 5 with an optical microscope, all the cosmetics have a median diameter of about 0.4.
It showed a uniformly dispersed state in the range of 3 to 0.47 μm, and no aggregate was observed.
【００４２】５．経時に於ける化粧料の色調の安定性の
評価
上腕内側部に２×２ｃｍの大きさに実施例１〜３の化粧
料を塗布し、塗布直後及び塗布後３時間での色調の変化
をミノルタ製分光測色計ＣＭ−２００２で調べた。実施
例４、５の化粧料は爪に塗布し、同様に塗布直後及び塗
布後３時間での色調の変化をミノルタ製分光測色計ＣＭ
−２００２で調べた。5. Evaluation of stability of color tone of cosmetics over time The cosmetics of Examples 1 to 3 were applied to the inner side of the upper arm in a size of 2 × 2 cm, and the change in color tone immediately after application and after 3 hours from application was evaluated by Minolta. It was examined by a spectrophotometer CM-2002. The cosmetics of Examples 4 and 5 were applied to the nails, and similarly, the change in the color tone immediately after the application and 3 hours after the application was measured by a spectrocolorimeter CM manufactured by Minolta.
-2002.
【００４３】結果を表２に示す。The results are shown in Table 2.
【００４４】[0044]
【表２】 [Table 2]
【００４５】表１及び表２の結果に明らかなように、本
発明による化粧料は高彩度、高隠蔽性を持ち、分散性が
良く、又色調の経時安定性にも優れていた。As is clear from the results shown in Tables 1 and 2, the cosmetics of the present invention had high saturation and high hiding power, good dispersibility, and excellent stability of color tone over time.
【００４６】[0046]
【発明の効果】本発明の化粧料は、高彩度、高隠蔽性を
持ち、分散性、色調の経時安定性に優れた化粧料を提供
する。EFFECT OF THE INVENTION The cosmetic composition of the present invention provides a cosmetic composition having high saturation and high hiding power, and excellent dispersibility and stability of color tone over time.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ Ｃ０９Ｃ 3/08 Ｃ０９Ｃ 3/08 (58)調査した分野(Int.Cl.7，ＤＢ名) A61K 7/02 ─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. 7 identification code FI C09C 3/08 C09C 3/08 (58) Fields investigated (Int.Cl. 7 , DB name) A61K 7/02
Claims (4)
μｍである無機白色顔料を赤色２２６号で被覆した有機
−無機複合顔料を配合する化粧料であって、 該有機−無機複合顔料は、赤色２２６号が溶解し且つ無
機白色顔料が分散する硫酸を水に滴下して、該無機白色
顔料の表面に該赤色２２６号を被覆させて得られたもの
であり、 該無機白色顔料は、酸化亜鉛、酸化ジルコニウム、酸化
チタン（アナタース型）、酸化チタン（ルチル型）の一
種又は二種以上の組み合わせから選ばれるものであるこ
と を特徴とする化粧料。1. A refractive index of 2 or more and an average particle size of 0.1 to 60.
A cosmetic in which an organic-inorganic composite pigment obtained by coating an inorganic white pigment having a size of μm with Red No. 226 is blended , wherein the organic-inorganic composite pigment dissolves Red No. 226 and does not exist.
The sulfuric acid in which the white pigment is dispersed is added dropwise to water to give the inorganic white color.
Obtained by coating the surface of the pigment with the red No. 226
The inorganic white pigment is zinc oxide, zirconium oxide,
One of titanium (anatase type) and titanium oxide (rutile type)
Be selected from the group consisting of two or more kinds.
And cosmetics.
酸化亜鉛、酸化ジルコニウム、酸化チタン（アナタース
型）、酸化チタン（ルチル型）の二種以上の複合物から
選ばれる請求項１に記載の化粧料。2. The inorganic white pigment in the organic-inorganic composite pigment is selected from two or more composites of zinc oxide, zirconium oxide, titanium oxide (anatase type) and titanium oxide (rutile type). The listed cosmetics.
号を硫酸に溶解する工程と（２）赤色２２６号を溶解し
た硫酸に無機白色顔料を分散させる工程と（３）赤色２
２６号を溶解し、且つ無機白色顔料を分散させた硫酸を
水に滴下して、無機白色顔料の表面に赤色２２６号を被
覆させる工程とを含む製造法により製造されたものであ
る請求項１から２の何れかに記載の化粧料。3. The organic-inorganic composite pigment is (1) red 226.
No. 226 is dissolved in sulfuric acid, (2) Red 226 is dissolved in sulfuric acid in which an inorganic white pigment is dispersed, and (3) Red 2
A method of manufacturing a method comprising the steps of dissolving No. 26 and dropping sulfuric acid in which an inorganic white pigment is dispersed into water to coat the surface of the inorganic white pigment with Red No. 226. The cosmetic according to any one of 1 to 2 .
水を含む硫酸を使用して製造したものである請求項１か
ら３の何れかに記載の化粧料。Wherein organic - cosmetic according to any one of inorganic composite pigments are those produced using a sulfuric acid containing less than 10% by weight of water according to claim 1 or <br/> et 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08572394A JP3426025B2 (en) | 1994-03-30 | 1994-03-30 | Cosmetics containing organic-inorganic composite pigments |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08572394A JP3426025B2 (en) | 1994-03-30 | 1994-03-30 | Cosmetics containing organic-inorganic composite pigments |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07267824A JPH07267824A (en) | 1995-10-17 |
| JP3426025B2 true JP3426025B2 (en) | 2003-07-14 |
Family
ID=13866772
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP08572394A Expired - Fee Related JP3426025B2 (en) | 1994-03-30 | 1994-03-30 | Cosmetics containing organic-inorganic composite pigments |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3426025B2 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07268242A (en) * | 1994-03-30 | 1995-10-17 | Pola Chem Ind Inc | Organic/inorganic composite pigment and production thereof |
| JP3241535B2 (en) * | 1994-05-10 | 2001-12-25 | ポーラ化成工業株式会社 | Cosmetics containing organic-inorganic composite pigments |
| US6174533B1 (en) * | 1997-05-23 | 2001-01-16 | The Procter & Gamble Company | Skin care compositions and method of improving skin appearance |
| US5997887A (en) † | 1997-11-10 | 1999-12-07 | The Procter & Gamble Company | Skin care compositions and method of improving skin appearance |
| JP4513198B2 (en) * | 2000-10-10 | 2010-07-28 | アサヌマ コーポレーション株式会社 | Aqueous nail polish with excellent pigment admixture stability |
| JP4513199B2 (en) * | 2000-10-10 | 2010-07-28 | アサヌマ コーポレーション株式会社 | Water-based nail polish with excellent anti-fading properties |
| WO2004033563A2 (en) * | 2002-10-09 | 2004-04-22 | Ciba Specialty Chemicals Holding Inc. | Method of colouring carrier materials |
| JP6467765B2 (en) * | 2015-06-02 | 2019-02-13 | 石原産業株式会社 | Titanium oxide pigment |
-
1994
- 1994-03-30 JP JP08572394A patent/JP3426025B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07267824A (en) | 1995-10-17 |
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