JP2006193520A - Make-up cosmetic material - Google Patents

Make-up cosmetic material Download PDF

Info

Publication number
JP2006193520A
JP2006193520A JP2005363490A JP2005363490A JP2006193520A JP 2006193520 A JP2006193520 A JP 2006193520A JP 2005363490 A JP2005363490 A JP 2005363490A JP 2005363490 A JP2005363490 A JP 2005363490A JP 2006193520 A JP2006193520 A JP 2006193520A
Authority
JP
Japan
Prior art keywords
pearl pigment
metal oxide
coated
colored metal
oxide
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.)
Granted
Application number
JP2005363490A
Other languages
Japanese (ja)
Other versions
JP4791817B2 (en
Inventor
Eiichiro Misaki
栄一郎 美崎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kao Corp
Original Assignee
Kao Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kao Corp filed Critical Kao Corp
Priority to JP2005363490A priority Critical patent/JP4791817B2/en
Publication of JP2006193520A publication Critical patent/JP2006193520A/en
Application granted granted Critical
Publication of JP4791817B2 publication Critical patent/JP4791817B2/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Cosmetics (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide a make up cosmetic material able to change color feeling of the skin while giving transparent feeling, fine and bright finishing and natural luster. <P>SOLUTION: The cosmetic material contains a pearl pigment prepared by coating the surface of thin flaky powder with a colored metal or a colored metal oxide. The pearl pigment has ≤10 absolute value of a* value and b* value of the reflected light of the powder for an incident light tilting 45°to the normal line direction of the surface of the measured sample and received in the normal line direction, when the pigment is coated on the surface of synthetic black leather in 0.05 mg/cm<SP>2</SP>average amount and measured the amount of reflected lights of the pearl pigment using an S polarizing plate in an incident light side and a spectral colorimeter equipped with a P polarizing plate in a photoreception side, in the photoreception condition of 2° visual field by C light. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

本発明は、透明感を持たせつつ肌の色相感覚を変化させることができ、きめ細かい明るい仕上がりで、自然なつやを与えるメークアップ化粧料に関する。   The present invention relates to a makeup cosmetic that can change the skin hue sensation while having a transparent feeling, and gives a natural gloss with a fine and bright finish.

メークアップ化粧料は、これを塗布して肌の質感を変化させることが要求されており、拡散反射の強い粉体や鏡面反射の強い粉体などを使用して、質感の制御を行っている。例えば、拡散反射の強い粉体である酸化チタンや球状粉体を配合してマットな仕上がりを得たり、マイカ、セリサイト、タルク等の鏡面反射の強い板状粉体を配合してつやのある仕上がりを得たりしている。一方、シミ、ソバカス等の色むらをカバーするため、二酸化チタンや酸化鉄等の隠蔽力の高い顔料を配合することが行われている。   Makeup cosmetics are required to change the texture of the skin by applying this, and the texture is controlled by using powders with strong diffuse reflection and powder with strong specular reflection. . For example, titanium oxide or spherical powder, which is a powder with strong diffuse reflection, is blended to obtain a matte finish, or plate-like powder with strong specular reflection such as mica, sericite, talc, etc. is blended to give a glossy finish. Or get. On the other hand, pigments with high hiding power such as titanium dioxide and iron oxide are blended in order to cover uneven color such as spots and freckles.

しかしながら、隠蔽力の高い顔料を用いた場合には、自然な感じがなくなってしまうという問題がある。一方、隠蔽力の低い粉体で質感を調整した場合は、色むらなどのカバー力が低下する問題があった。   However, when a pigment with high hiding power is used, there is a problem that the natural feeling is lost. On the other hand, when the texture is adjusted with a powder having a low hiding power, there is a problem that the covering power such as uneven color is lowered.

近年、これらの問題を解決するため、隠蔽力が強くつや感を制御できるパール顔料を用いて肌の色相感覚を変化させることが検討されている。例えば、つやを付与するために、酸化チタン被覆パール顔料を用いた場合、正反射方向で鏡面反射によりつやを付与することができるが、鏡面反射以外の角度では、粉体そのものの白っぽい外観となってしまう。従って、顔全体などの広い範囲に化粧料を塗布すると、観察者に正対する部分はつや感があるが、正対しない部分では、白っぽい粉感が見えるため、不自然な仕上がりになってしまう傾向があった。自然なつやを得るため、特許文献1には、チタンマイカ表面をアルミナ、シリカで順次被覆した粉体が記載されている。しかし、正対しない部分での白っぽい粉感を解決できるものではない。   In recent years, in order to solve these problems, it has been studied to change the skin hue sensation using a pearl pigment that has a strong hiding power and can control glossiness. For example, when titanium oxide-coated pearl pigment is used to give gloss, it can be given gloss by specular reflection in the specular reflection direction, but at an angle other than specular reflection, the powder itself has a whitish appearance. End up. Therefore, when cosmetics are applied over a wide area such as the entire face, the part facing the viewer has a glossy feeling, but the part that does not face the face tends to have a whitish texture, which tends to result in an unnatural finish. was there. In order to obtain a natural gloss, Patent Document 1 describes a powder in which a titanium mica surface is sequentially coated with alumina and silica. However, it is not possible to solve the whitish texture at the non-facing part.

一方、例えば、酸化鉄のような有色金属酸化物を被覆したパール顔料も市販されている。特許文献2、3には、酸化鉄被覆した板状粉体の上に酸化チタンなどの無色金属酸化物を被覆した多層パール顔料が提案されているが、赤色系のパール顔料のみが得られるにすぎず、明るい魅力的な肌合いを表現することはできない。
特開2003−212722号公報 特開平7−11161号公報 特開平8−259840号公報
On the other hand, for example, a pearl pigment coated with a colored metal oxide such as iron oxide is also commercially available. Patent Documents 2 and 3 propose a multilayer pearl pigment in which a plate-like powder coated with iron oxide is coated with a colorless metal oxide such as titanium oxide, but only a red pearl pigment can be obtained. It is not too much to express a bright and attractive texture.
JP 2003-212722 A Japanese Patent Application Laid-Open No. 7-11116 JP-A-8-259840

本発明の課題は、透明感を持たせつつ肌の色相感覚を変化させることができ、きめ細かい明るい仕上がりで、自然なつやを与えるメークアップ化粧料を提供することにある。   An object of the present invention is to provide a make-up cosmetic that can change the skin hue sensation while having a transparent feeling, and gives a natural gloss with a fine and bright finish.

本発明者らは、薄片状粉体の表面を表面粗さを制御した有色金属又は有色金属酸化物で被覆し、さらに無色金属又は無色金属酸化物を被覆したパール顔料であって、特定の条件で測定した散乱光のa*値及びb*値の絶対値が10以下であるパール顔料が極めて鮮やかな発色を示し、この顔料を用いれば透明感を持たせつつ肌の色相感覚を変化させることができ、きめ細かい明るい仕上がりで、自然なつやを与えるメークアップ化粧料が得られることを見出した。   The present inventors provide a pearl pigment in which the surface of a flaky powder is coated with a colored metal or colored metal oxide having a controlled surface roughness, and further coated with a colorless metal or a colorless metal oxide, under specific conditions. Pearl pigments whose absolute value of a * and b * values of scattered light measured in (1) is 10 or less show a very vivid color, and if this pigment is used, the skin hue sensation can be changed while maintaining transparency. It was found that makeup cosmetics that give a natural gloss with a fine and bright finish can be obtained.

本発明は、薄片状粉体の表面に有色金属又は有色金属酸化物を被覆し、さらに無色金属又は無色金属酸化物を被覆したパール顔料であって、該パール顔料を黒色人工皮革表面に平均0.05mg/cm2で塗布し、入射光側にS偏光板、受光側にP偏光板を装着した分光測色計を用い、C光による2°視野の受光条件で、パール顔料の反射光量を測定したとき、測定試料面の法線方向に対して45°で入射し、法線方向で受光した粉体反射光(散乱光)のa*値及びb*値の絶対値が10以下であるパール顔料を含有するメークアップ化粧料を提供するものである。
なお、本発明において、a*値、b*値は、国際照明委員会(1976年)(CIE)で規格された色度を示す。また、ここで示したパール顔料のa*値、b*値の測定方法(図1参照)を「本発明のa*値、b*値の測定方法」という。
The present invention relates to a pearl pigment in which a surface of a flaky powder is coated with a colored metal or a colored metal oxide and further coated with a colorless metal or a colorless metal oxide, and the pearl pigment is coated on the surface of black artificial leather with an average of 0. Using a spectrocolorimeter with an S polarizing plate on the incident light side and a P polarizing plate on the light receiving side, applied at .05 mg / cm 2 , the reflected light amount of the pearl pigment is measured under the 2 ° field of view with C light. When measured, the absolute value of the a * value and b * value of powder reflected light (scattered light) incident at 45 ° with respect to the normal direction of the measurement sample surface and received in the normal direction is 10 or less. A makeup cosmetic containing a pearl pigment is provided.
In the present invention, the a * value and b * value indicate chromaticity standardized by the International Commission on Illumination (1976) (CIE). Further, the method for measuring the a * value and b * value of the pearl pigment shown here (see FIG. 1) is referred to as “the method for measuring the a * value and b * value of the present invention”.

本発明のメークアップ化粧料は、透明感を持たせつつ肌の色相感覚を変化させることができ、きめ細かい明るい仕上がりで、自然なつやを与えることができる。また、塗布時ののびなどの使用感も良好である。   The makeup cosmetics of the present invention can change the skin hue sensation while giving a clear feeling, and can give natural gloss with a fine and bright finish. Also, the feeling of use such as spreading during application is good.

本発明で用いられるパール顔料を得るための薄片状粉体は、平均粒径が2〜200μmで、平均厚さが0.01〜5μmであるのが好ましい。特に、配合適性の点から、平均粒径が2〜20μmで、平均厚さが0.05〜1μmであるのがより好ましい。ここで、平均粒径は体積平均粒径(D4)(体積分率で計算した平均粒径)を示す。測定は、レーザー回折式の粒度分布計で容易に再現性良く測定することが出来る。薄片状粉体の厚さは、原子間力顕微鏡により基準面との差を測定し相加平均したものを平均厚さとする。   The flaky powder for obtaining the pearl pigment used in the present invention preferably has an average particle diameter of 2 to 200 μm and an average thickness of 0.01 to 5 μm. In particular, from the viewpoint of suitability for blending, it is more preferable that the average particle diameter is 2 to 20 μm and the average thickness is 0.05 to 1 μm. Here, an average particle diameter shows volume average particle diameter (D4) (average particle diameter calculated by the volume fraction). Measurement can be easily performed with a laser diffraction particle size distribution meter with good reproducibility. The thickness of the flaky powder is the average thickness obtained by measuring the difference from the reference surface with an atomic force microscope and arithmetically averaging it.

かかる薄片状粉体としては、雲母、セリサイト、タルク、カオリン、スメクタイト属粘土鉱物、合成マイカ、合成セリサイト、板状二酸化チタン、板状シリカ、板状酸化アルミニウム、窒化硼素、硫酸バリウム、板状チタニア・シリカ複合酸化物等が挙げられる。これらのうち、特に雲母が、表面の平滑性の点で好ましい。   Such flaky powders include mica, sericite, talc, kaolin, smectite clay mineral, synthetic mica, synthetic sericite, plate-like titanium dioxide, plate-like silica, plate-like aluminum oxide, boron nitride, barium sulfate, plate And titania-silica composite oxide. Of these, mica is particularly preferable in terms of surface smoothness.

本発明に用いられるパール顔料おいて、薄片状粉体を被覆する有色金属としては、金、銅等が挙げられ、特に金が好ましい。有色金属酸化物としては、酸化鉄、低次酸化チタン、酸化銅、酸化コバルト、酸化クロム、酸化ニッケル等が挙げられ、特に酸化鉄が好ましい。   In the pearl pigment used in the present invention, examples of the colored metal covering the flaky powder include gold and copper, and gold is particularly preferable. Examples of the colored metal oxide include iron oxide, low-order titanium oxide, copper oxide, cobalt oxide, chromium oxide, nickel oxide and the like, and iron oxide is particularly preferable.

更に、本発明に用いられるパール顔料において、有色金属酸化物の表面を被覆する無色金属としては、チタン、ジルコニウム、亜鉛、錫、ケイ素、アルミニウム等が挙げられ、特にチタンが好ましい。無色金属酸化物としては、酸化チタン、酸化亜鉛、酸化アルミニウム等が挙げられ、特に酸化チタンが好ましい。   Further, in the pearl pigment used in the present invention, examples of the colorless metal that covers the surface of the colored metal oxide include titanium, zirconium, zinc, tin, silicon, and aluminum, with titanium being particularly preferred. Examples of the colorless metal oxide include titanium oxide, zinc oxide, aluminum oxide and the like, and titanium oxide is particularly preferable.

本発明に用いられるパール顔料は「本発明のa*値又はb*値の測定方法」に従って測定したとき、粉体反射光(散乱光)のa*値及びb*値の絶対値が10以下、好ましくは5以下のものである。
このような測色ができる測定機として、村上色彩技術研究所社製のGCMSシリーズを用いることができる。
The pearl pigment used in the present invention has an absolute value of 10 * or less of the a * value and b * value of powder reflected light (scattered light) when measured according to the “measurement method of a * value or b * value of the present invention”. , Preferably 5 or less.
A GCMS series manufactured by Murakami Color Research Laboratory Co., Ltd. can be used as a measuring machine capable of such colorimetry.

また、本発明に用いられるパール顔料は、薄片状粉体の表面を有色金属又は有色金属酸化物で被覆したものであるが、有色金属又は有色金属酸化物の表面粗さは10nm以下、好ましくは5nm以下である。有色金属又は有色金属酸化物は、特定波長の光を吸収するという特性を有するために、被覆表面の粗さが大きいと散乱色が強くなり、弱いパール光沢の発色となる。被覆表面の粗さを小さくすることにより、光の散乱が抑制されて散乱光の少ない鮮やかな発色を有する顔料が得られる。   Further, the pearl pigment used in the present invention is obtained by coating the surface of a flaky powder with a colored metal or a colored metal oxide. The surface roughness of the colored metal or the colored metal oxide is 10 nm or less, preferably 5 nm or less. Since the colored metal or the colored metal oxide has a characteristic of absorbing light of a specific wavelength, if the roughness of the coating surface is large, the scattering color becomes strong and the color of weak pearly luster is generated. By reducing the roughness of the coating surface, it is possible to obtain a pigment that suppresses light scattering and has a vivid color with little scattered light.

本発明において、表面平均粗さ(Ra)は、中心線平均粗さを示し、原子間力顕微鏡(デジタルインスツルメント社製、Nanoscope III)を用い、Scan Rate 1.0Hzで、2μm×2μmの範囲を測定したときの平均値を示すものである。測定の際、パール顔料はエタノール等の溶媒に分散させた状態で、平滑な基盤面上に付着させ、溶媒を除去することにより基盤に密着させた後、原子間力顕微鏡により測定する。   In the present invention, the surface average roughness (Ra) indicates the centerline average roughness, and is 2 μm × 2 μm at a scan rate of 1.0 Hz using an atomic force microscope (Nanoscope III, manufactured by Digital Instruments). The average value when the range is measured is shown. At the time of measurement, the pearl pigment is dispersed in a solvent such as ethanol, adhered on a smooth substrate surface, adhered to the substrate by removing the solvent, and then measured with an atomic force microscope.

また、本発明に用いられるパール顔料は、有色金属又は有色金属酸化物被覆層の光学的膜厚が15〜650nm、特に25〜650nmであることが好ましく、250nm以下、特に210nm以下であるのが好ましい。650nmを超えると、吸収層の絶対的な厚さが増すため、光吸収の影響が強くなるため、有色金属又は有色金属酸化物の固有色を活かしたパール顔料にすることが好ましい。例えば、酸化鉄では、光学的膜厚250nmを超えると、赤色のパール顔料とすることが好ましい。
ここで、光学的膜厚とは、有色金属又は有色金属酸化物の幾何学的層厚に屈折率をかけたものを示す。例えば、酸化鉄(屈折率3.0)の場合、幾何学的膜厚8〜220nmが好ましく、80nm以下、特に50nm以下であることが好ましい。散乱光を十分に抑制した場合、例えば有色金属酸化物に酸化鉄を用いると、光学的膜厚が120〜210nmの場合は干渉光が金色であり、60〜120nmの場合は干渉光が銀色である。なお、幾何学的膜厚はSEMにより測定される。
Further, in the pearl pigment used in the present invention, the optical film thickness of the colored metal or colored metal oxide coating layer is preferably 15 to 650 nm, particularly preferably 25 to 650 nm, and is preferably 250 nm or less, particularly 210 nm or less. preferable. If it exceeds 650 nm, the absolute thickness of the absorption layer increases, and the influence of light absorption becomes strong. Therefore, it is preferable to use a pearl pigment that takes advantage of the intrinsic color of a colored metal or colored metal oxide. For example, iron oxide is preferably a red pearl pigment when the optical film thickness exceeds 250 nm.
Here, the optical film thickness indicates a value obtained by multiplying the geometric layer thickness of a colored metal or colored metal oxide by a refractive index. For example, in the case of iron oxide (refractive index of 3.0), the geometric film thickness is preferably 8 to 220 nm, preferably 80 nm or less, and particularly preferably 50 nm or less. When the scattered light is sufficiently suppressed, for example, when iron oxide is used for the colored metal oxide, the interference light is gold when the optical film thickness is 120 to 210 nm, and the interference light is silver when the optical film thickness is 60 to 120 nm. is there. The geometric film thickness is measured by SEM.

更に、有色金属又は有色金属酸化物の表面を、無色金属又は無色金属酸化物で被覆して多層化すると、酸化鉄特有の色にとらわれない金色〜緑といった様々な色調の顔料を得ることができる。無色金属又は無色金属酸化物の光学的膜厚は平均180〜900nmであることが好ましい。酸化チタンの場合は、幾何学的膜厚が80〜360nmであることが好ましい。従来のパール顔料のように散乱色が強いと、これらの干渉光は散乱色に打ち消されてしまい、肉眼では観測できないが、本発明のパール顔料は散乱色が抑制されているため、被覆した有色金属又は有色金属酸化物の固有色ではない金色や緑色の干渉光も作り出すことができる。
酸化鉄等の光学的膜厚が大きい場合は、酸化鉄特有の赤色系の顔料を作る際に有利であり、散乱色を抑制することにより赤色系であっても従来の顔料より鮮やかな発色の赤色を作ることが可能となる。
Furthermore, when the surface of a colored metal or colored metal oxide is coated with a colorless metal or a colorless metal oxide to form a multilayer, pigments of various colors such as gold to green that are not bound to the color unique to iron oxide can be obtained. . The optical film thickness of the colorless metal or colorless metal oxide is preferably 180 to 900 nm on average. In the case of titanium oxide, the geometric film thickness is preferably 80 to 360 nm. If the scattering color is strong like the conventional pearl pigment, these interference lights are canceled out by the scattering color and cannot be observed with the naked eye, but the pearl pigment of the present invention suppresses the scattering color, so the coated colored Gold or green interference light that is not an intrinsic color of a metal or colored metal oxide can also be created.
When the optical film thickness of iron oxide or the like is large, it is advantageous when making red pigments unique to iron oxide. It becomes possible to make red.

更に、屈折率の関係において、薄片状粉体nsと有色金属化合物nと無色金属化合物n0の関係において、ns<n>n0となる場合は、反射率を高くでき、彩度を高めることができる。具体的には、雲母(屈折率1.58)、酸化鉄(Fe2O3)(屈折率3.01)、酸化チタン(屈折率2.5〜2.7)の組み合わせが、特に好ましい。
特に、メークアップ化粧料に用いた場合、観察者に正対する部分はつや感があるが、正対しない部分では、従来の酸化チタン被覆雲母のように白っぽい粉感が見えず、自然に赤暗くシェードする仕上がりになり、より自然な肌に近い仕上がりになる。
Further, in the relationship of refractive index, when n s <n> n 0 in the relationship between the flaky powder n s , the colored metal compound n and the colorless metal compound n 0 , the reflectance can be increased, and the saturation can be increased. Can be increased. Specifically, a combination of mica (refractive index 1.58), iron oxide (Fe 2 O 3 ) (refractive index 3.01), and titanium oxide (refractive index 2.5 to 2.7) is particularly preferable.
In particular, when used in makeup cosmetics, the part that faces the viewer is glossy, but the part that does not face the face does not have a whitish texture like conventional titanium oxide-coated mica, and is naturally reddish. The result is a shaded finish with a more natural skin finish.

本発明のパール顔料は、例えば中和滴定法を用い、有色金属酸化物前駆体水溶液の添加速度を選定することにより製造することができる。有色金属又は有色金属酸化物の表面平均粗さを小さくするために、中和滴定法が好ましい。   The pearl pigment of the present invention can be produced, for example, by using a neutralization titration method and selecting the addition rate of the colored metal oxide precursor aqueous solution. In order to reduce the surface average roughness of the colored metal or colored metal oxide, the neutralization titration method is preferable.

(製造方法1)
具体的には、薄片状粉体の水分散液に、有色金属酸化物前駆体の水溶液を、薄片状粉体100g当たりの金属イオン量が5×10-4〜12×10-4mol/minとなるように添加し、次いで、混合液にアルカリ水溶液を加えてpH5〜8とし、固体を分離した後、500〜1000℃で焼成してパール顔料を得、さらに得られたパール顔料を水に懸濁させ、無色金属の前駆体又は無色金属酸化物の前駆体の水溶液を添加し、次いで、混合液にアルカリ水溶液を加えてpH5〜8とし、固体を分離した後、500〜1000℃で焼成することにより製造することができる。
(Manufacturing method 1)
Specifically, an aqueous solution of a colored metal oxide precursor is added to an aqueous dispersion of flaky powder, and the amount of metal ions per 100 g of flaky powder is 5 × 10 −4 to 12 × 10 −4 mol / min. Then, an alkaline aqueous solution is added to the mixed solution to adjust the pH to 5 to 8, the solid is separated, and calcined at 500 to 1000 ° C. to obtain a pearl pigment. Further, the obtained pearl pigment is put into water. Suspend, add an aqueous solution of a colorless metal precursor or colorless metal oxide precursor, then add an alkaline aqueous solution to the mixture to adjust the pH to 5-8, separate the solid, and then fire at 500-1000 ° C Can be manufactured.

すなわち、まず、薄片状粉体を水に分散させ、良く撹拌して、薄片状粉体の水分散液を調製する。分散液のスラリー濃度は1〜50質量%であるのが、薄片状粉体表面を金属化合物が均一に被覆するのに好ましい。
一方、有色金属酸化物前駆体としては、硝酸第二鉄、塩化第二鉄、硫酸第二鉄等が挙げられ、これらの水溶液濃度は、20〜70質量%であるのが好ましい。
That is, first, the flaky powder is dispersed in water and stirred well to prepare an aqueous dispersion of the flaky powder. The slurry concentration of the dispersion is preferably 1 to 50% by mass so that the surface of the flaky powder is uniformly coated with the metal compound.
On the other hand, examples of the colored metal oxide precursor include ferric nitrate, ferric chloride, and ferric sulfate. The concentration of these aqueous solutions is preferably 20 to 70% by mass.

薄片状粉体の分散液を、50〜100℃、好ましくは70〜80℃に加温し、分散液に酸を加え酸性にし、更に反応液のpHを2〜4、好ましくは2.5〜3.5に保つよう、アルカリ水溶液で調整しながら、有色金属酸化物前駆体水溶液を反応混合液に加える。特に、表面粗さの小さい平滑な被覆状態を実現するためには、有色金属酸化物前駆体水溶液の添加速度を、薄片状粉体100g当たりの金属イオン量が5×10-4〜12×10-4mol/min、好ましくは8×10-4〜11×10-4mol/minとなるように添加する。この範囲の添加速度の場合に、散乱光が抑制され、より好ましい顔料を得ることができる。
なお、pHの調整に用いられるアルカリ水溶液としては、水酸化ナトリウム、水酸化カリウム、炭酸ナトリウム、炭酸カリウム、炭酸水素ナトリウム、炭酸水素カリウム等の水溶液が挙げられる。
The dispersion of flaky powder is heated to 50 to 100 ° C., preferably 70 to 80 ° C., acid is added to the dispersion, and the pH of the reaction solution is 2 to 4, preferably 2.5 to The colored metal oxide precursor aqueous solution is added to the reaction mixture while adjusting with an alkaline aqueous solution so as to maintain 3.5. In particular, in order to realize a smooth coating state with a small surface roughness, the addition rate of the colored metal oxide precursor aqueous solution is adjusted so that the amount of metal ions per 100 g of flaky powder is 5 × 10 −4 to 12 × 10. -4 mol / min, preferably 8 × 10 −4 to 11 × 10 −4 mol / min. When the addition rate is within this range, scattered light is suppressed and a more preferable pigment can be obtained.
In addition, as aqueous alkali solution used for adjustment of pH, aqueous solution, such as sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium hydrogencarbonate, potassium hydrogencarbonate, is mentioned.

添加終了後、混合液を熟成させる。その後、アルカリ水溶液を加えてpH5〜8とし、さらに熟成させる。次に、固体を分離した後、水洗によって塩を除去し、乾燥する。その後、500〜1000℃、好ましくは700〜800℃で30〜180分間焼成を行う。   After the addition is complete, the mixture is aged. Thereafter, an alkaline aqueous solution is added to adjust the pH to 5 to 8, and further ripened. Next, after separating the solid, the salt is removed by washing with water and dried. Thereafter, baking is performed at 500 to 1000 ° C., preferably 700 to 800 ° C. for 30 to 180 minutes.

次に、得られた有色金属酸化物で被覆された薄片状粉体の水分散液を調製する。分散液のスラリー濃度は1〜50質量%であるのが、有色金属酸化物で被覆された薄片状粉体を無色金属又は無色金属酸化物で均一に被覆するのに好ましい。
無色金属酸化物前駆体としては、硫酸チタン、四塩化チタン等が挙げられ、これらの水溶液濃度は、20〜60質量%であるのが好ましい。
Next, an aqueous dispersion of the flaky powder coated with the obtained colored metal oxide is prepared. The slurry concentration of the dispersion is preferably 1 to 50% by mass, so that the flaky powder coated with the colored metal oxide is uniformly coated with the colorless metal or the colorless metal oxide.
Examples of the colorless metal oxide precursor include titanium sulfate and titanium tetrachloride. The concentration of these aqueous solutions is preferably 20 to 60% by mass.

有色金属酸化物で被覆された薄片状粉体の分散液を、50〜100℃、好ましくは70〜80℃に加温し、酸を加え酸性にし、更に反応混合液のpHを1〜5、好ましくは1〜3に保つよう、アルカリ水溶液で調整ながら、無色金属酸化物前駆体の水溶液を加える。
なお、pHの調整に用いられるアルカリ水溶液としては、前記と同様のものを用いることができる。
The dispersion of the flaky powder coated with the colored metal oxide is heated to 50 to 100 ° C., preferably 70 to 80 ° C., acidified with acid, and the pH of the reaction mixture is adjusted to 1 to 5, Preferably, an aqueous solution of a colorless metal oxide precursor is added while adjusting with an alkaline aqueous solution so as to maintain a value of 1-3.
In addition, as an alkaline aqueous solution used for adjustment of pH, the thing similar to the above can be used.

添加終了後、混合液を熟成させる。その後、アルカリ水溶液を加えてpH5〜8とし、さらに熟成させる。次に、固体を分離した後、水洗によって塩を除去し、乾燥を行う。その後、500〜1000℃、好ましくは700〜800℃で30〜180分間焼成を行うことにより、本発明のパール顔料を得ることができる。   After the addition is complete, the mixture is aged. Thereafter, an alkaline aqueous solution is added to adjust the pH to 5 to 8, and further ripened. Next, after separating the solid, the salt is removed by washing with water, followed by drying. Then, the pearl pigment of this invention can be obtained by baking for 30-180 minutes at 500-1000 degreeC, Preferably 700-800 degreeC.

(製造方法2)
また、本発明で用いるパール顔料は、薄片状粉体に有色金属酸化物前駆体を被覆した後、焼成する工程を省き、無色金属又は無色金属酸化物で被覆する工程に移行して製造することもできる。すなわち、前記の製造方法1と同様に薄片状粉体の水分散液に有色金属酸化物前駆体の水溶液を添加し、次いで、アルカリ水溶液を加えてpH5〜8とした後、固体を分離し、水洗によって塩を除去する。このようにして得られた固体の表面を、製造方法1と同様の方法にて、無色金属又は無色金属酸化物で被覆し、焼成することにより、パール顔料を得ることができる。
(Manufacturing method 2)
Further, the pearl pigment used in the present invention is manufactured by coating the flaky powder with the colored metal oxide precursor, and then omitting the firing step and shifting to the step of coating with the colorless metal or the colorless metal oxide. You can also. That is, the aqueous solution of the colored metal oxide precursor is added to the aqueous dispersion of the flaky powder in the same manner as in the production method 1, and then the aqueous solution is added to adjust the pH to 5 to 8, and then the solid is separated. Remove salt by washing with water. A pearl pigment can be obtained by coating the solid surface thus obtained with a colorless metal or a colorless metal oxide in the same manner as in Production Method 1 and baking.

このようなパール顔料は、化粧持ち(持続性)向上の点からその表面を疎水化処理して用いることもできる。疎水化処理は、通常の方法に従い、疎水化処理剤で処理することにより行うことができる。
疎水化処理剤としては、シリコーン油、脂肪酸金属塩、アルキルリン酸、アルキルリン酸のアルカリ金属塩又はアミン塩、N−モノ長鎖(炭素数8〜22)脂肪族アシル塩基性アミノ酸、パーフルオロアルキル基を有するフッ素化合物などが挙げられる。
Such a pearl pigment can also be used after its surface is hydrophobized from the standpoint of improving makeup lasting (sustainability). The hydrophobizing treatment can be performed by treating with a hydrophobizing agent in accordance with a normal method.
Examples of hydrophobizing agents include silicone oil, fatty acid metal salt, alkyl phosphoric acid, alkali metal salt or amine salt of alkyl phosphoric acid, N-mono long chain (carbon number 8 to 22) aliphatic acyl basic amino acid, perfluoro Examples thereof include fluorine compounds having an alkyl group.

シリコーン油としては、例えば各種鎖状シリコーン、環状シリコーン、変性シリコーンが;脂肪酸金属塩としては、特に炭素数12〜18の脂肪酸のカルシウム、マグネシウム、亜鉛、アルミニウム等の塩が;アルキルリン酸及びその塩としては、合計炭素数8〜45のアルキル又はアルケニル基を有するモノ又はジエステル及びそのアルカリ金属塩若しくはアミン塩が;N−モノ長鎖脂肪族アシル塩基性アミノ酸としては、2−エチルヘキサノイル、カプリロイル、ラウロイル、ミリストイル、パルミトイル、ステアロイル、イソステアロイル、オレオイル、ベヘノイル、ココイル、牛脂脂肪酸アシル、硬化牛脂脂肪酸アシル等の炭素数8〜22のアシル基が塩基性アミノ酸のα位又はω位のアミノ基に結合したものが;パーフルオロアルキル基を有するフッ素化合物としては、米国特許第3632744号明細書、特開昭62−250074号公報、特開昭55−167209号公報、特開平2−218603号公報等に記載のものなどが挙げられる。   Examples of silicone oils include various chain silicones, cyclic silicones, and modified silicones; examples of fatty acid metal salts include salts of fatty acids having 12 to 18 carbon atoms such as calcium, magnesium, zinc, and aluminum; alkylphosphoric acid and its Examples of the salt include mono- or diesters having an alkyl or alkenyl group having 8 to 45 carbon atoms in total and alkali metal salts or amine salts thereof; N-mono long-chain aliphatic acyl basic amino acids include 2-ethylhexanoyl, Capyloyl, lauroyl, myristoyl, palmitoyl, stearoyl, isostearoyl, oleoyl, behenoyl, cocoyl, beef tallow fatty acyl, hard tallow fatty acyl, etc. The one attached to the group; Examples of the fluorine compound having a sulfur group include those described in US Pat. No. 3,632,744, JP-A-62-2250074, JP-A-55-167209, JP-A-2-218603, and the like. It is done.

疎水化処理量は、十分な疎水性、良好な感触の点から、パール顔料1質量部に対して疎水化処理剤0.0005〜0.2質量部、特に0.02〜0.1質量部が好ましい。   The amount of hydrophobic treatment is 0.0005 to 0.2 parts by weight, particularly 0.02 to 0.1 parts by weight, based on 1 part by weight of the pearl pigment, from the viewpoint of sufficient hydrophobicity and good feel. Is preferred.

上記のようなパール顔料は、1種以上を用いることができ、メークアップ化粧料中に0.1〜30質量%、特に0.5〜30質量%含有するのが、配合の効果を十分に発揮できるとともに、強い光沢感による不自然さを回避できるので好ましい。また、従来のパール顔料を組み合わせて使用することもできる。   One or more kinds of the pearl pigments as described above can be used, and 0.1 to 30% by mass, particularly 0.5 to 30% by mass in the makeup cosmetic is sufficient for the effect of blending. This is preferable because it can be exhibited and unnaturalness due to a strong glossiness can be avoided. Moreover, the conventional pearl pigment can also be used in combination.

本発明のメークアップ化粧料は、常法に従って製造することができ、例えば粉白粉、固形白粉、フェイスパウダー、パウダーファンデーション、油性ファンデーション、クリーム状ファンデーション、リキッドファンデーション、コンシーラー、口紅、リップクリーム、頬紅、アイシャドウ、アイライナー、アイブロウなどとすることができる。   The make-up cosmetic of the present invention can be produced according to a conventional method, for example, powder white powder, solid white powder, face powder, powder foundation, oil foundation, cream foundation, liquid foundation, concealer, lipstick, lip balm, blusher, Eye shadow, eyeliner, eyebrow, etc.

また、本発明で用いるパール顔料は、本発明のメークアップ化粧料が、粉白粉、固形白粉及びフェイスパウダーの場合は0.1〜30質量%、特に0.5〜30質量%;パウダーファンデーション及び油性ファンデーションの場合は0.1〜30質量%、特に0.5〜30質量%;クリーム状ファンデーション、リキッドファンデーション及びコンシーラーの場合は0.1〜30質量%、特に0.5〜25質量%;口紅及びリップクリームの場合は0.1〜20質量%、特に0.5〜15質量%;頬紅及びアイシャドウの場合は0.1〜30質量%、特に0.5〜25質量%;アイライナー及びアイブロウの場合は0.1〜30質量%、特に0.5〜20質量%含有されるのが好ましい。   The pearl pigment used in the present invention is 0.1 to 30% by mass, particularly 0.5 to 30% by mass when the makeup cosmetic of the present invention is powdered white powder, solid white powder and face powder; In the case of oily foundations, 0.1-30% by weight, in particular 0.5-30% by weight; in the case of creamy foundations, liquid foundations and concealers, 0.1-30% by weight, in particular 0.5-25% by weight; In the case of lipstick and lip balm, 0.1 to 20% by weight, especially 0.5 to 15% by weight; in the case of blusher and eye shadow, 0.1 to 30% by weight, in particular 0.5 to 25% by weight; eyeliner And in the case of eyebrow, it is preferable to contain 0.1-30 mass%, especially 0.5-20 mass%.

本発明のメークアップ化粧料は、さらに、25℃における粘度が1000mPa・s以下の油剤を含有することができる。特に、使用感の点から、0.1〜1000mPa・s、更に2〜500mPa・sの範囲の油剤が好ましい。   The makeup cosmetic of the present invention can further contain an oil having a viscosity at 25 ° C. of 1000 mPa · s or less. In particular, an oil agent in the range of 0.1 to 1000 mPa · s, more preferably 2 to 500 mPa · s is preferable from the viewpoint of usability.

油剤は、粘度が1000mPa・s以下であれば特に制限されず、例えば流動パラフィン、スクワラン、オリーブ油、エステル油、ジグリセライド、トリグリセライド、シリコーン油、パーフルオロアルキル基を有するフッ素系油剤等が挙げられる。これらのうち、流動パラフィン、スクワラン、エステル油、シリコーン油、パーフルオロアルキル基を有するフッ素系油剤が好ましい。   The oil agent is not particularly limited as long as the viscosity is 1000 mPa · s or less, and examples thereof include liquid paraffin, squalane, olive oil, ester oil, diglyceride, triglyceride, silicone oil, and a fluorine-based oil agent having a perfluoroalkyl group. Of these, liquid paraffin, squalane, ester oil, silicone oil, and fluorinated oils having a perfluoroalkyl group are preferred.

油剤は、1種以上を用いることができ、メークアップ化粧料中に0.5〜60質量%、特に2〜50質量%含有するのが、べたつき感のない使用感が得られるので好ましい。
また、塗布時ののびを好適にし、所期の光学特性を発揮させるため、前記パール顔料と油剤の配合比率(質量比)は1/10〜100/1であるのが好ましい。
1 or more types of oil agents can be used, and it is preferable to contain 0.5-60 mass% in makeup cosmetics, especially 2-50 mass%, since a feeling of stickiness is obtained.
Moreover, in order to make the spread at the time of application | coating suitable and to exhibit the desired optical characteristic, it is preferable that the compounding ratio (mass ratio) of the said pearl pigment and oil agent is 1 / 10-100 / 1.

本発明のメークアップ化粧料は、前記成分のほか、必要に応じて、通常の化粧料に配合されている成分、例えば、界面活性剤、水溶性高分子、他の粉体、保湿剤、防腐剤、薬剤、紫外線吸収剤、色素、無機塩又は有機酸塩、香料、キレート剤、pH調整剤、水等を含有することができる。   In addition to the above-mentioned components, the makeup cosmetic of the present invention contains components that are blended in ordinary cosmetics as necessary, for example, surfactants, water-soluble polymers, other powders, moisturizers, antiseptics. An agent, a drug, an ultraviolet absorber, a dye, an inorganic salt or an organic acid salt, a fragrance, a chelating agent, a pH adjusting agent, water, and the like can be contained.

製造例1
粒径5〜60μmの薄片状雲母80gを、1.2Lの水に加えて十分に分散させ、80℃まで昇温した後、塩酸を加えてpH3にする。次に、予め調製した硝酸第二鉄水溶液(硝酸第二鉄17質量部:水26質量部)337gを、水酸化ナトリウム水溶液を用いてpH3に保ちながら、鉄イオン濃度9×10-4mol/minの割合でゆっくりと添加する。添加終了後、水酸化ナトリウム水溶液でpH5にする。濾過し、水洗して塩を除去し、吸引濾過、乾燥し、次いで700℃で1時間焼成を行った。
得られた着色顔料は、薄片状雲母の上に、非常に微細な酸化鉄粒子が幾何学的膜厚20nmに均一に被覆されていた。被覆層の表面粗さを測定したところ、表面粗さは3.44nmであった。
次いで、前記酸化鉄被覆パール顔料80gを1.2Lの水に加えて十分に分散させ、温度を75℃まで昇温する。昇温した後に、塩酸を加えてpH1.6とする。この後、40質量%四塩化チタン水溶液を1.4g/minの速度で240g添加しながら、20質量%水酸化ナトリウム水溶液を用いてpHを1.6に維持する。その後、20質量%水酸化ナトリウム水溶液を用いて分散液をpH7まで中和する。その後、水洗によって塩を除去し、吸引濾過、乾燥して、次いで700℃で90分間焼成を行った。これにより、高彩度な金色干渉の酸化チタン/酸化鉄被覆着色パール顔料を得た。
Production Example 1
80 g of flaky mica having a particle size of 5 to 60 μm is sufficiently dispersed in 1.2 L of water, heated to 80 ° C., and hydrochloric acid is added to adjust to pH 3. Next, while maintaining 337 g of a previously prepared ferric nitrate aqueous solution (17 parts by mass of ferric nitrate: 26 parts by mass of water) at a pH of 3 using an aqueous sodium hydroxide solution, an iron ion concentration of 9 × 10 −4 mol / Slowly add at min rate. After completion of the addition, the pH is adjusted to 5 with an aqueous sodium hydroxide solution. Filtration, washing with water to remove salts, suction filtration, drying, followed by baking at 700 ° C. for 1 hour.
The obtained colored pigment was coated with very fine iron oxide particles uniformly on a flaky mica with a geometric film thickness of 20 nm. When the surface roughness of the coating layer was measured, the surface roughness was 3.44 nm.
Next, 80 g of the iron oxide-coated pearl pigment is added to 1.2 L of water and sufficiently dispersed, and the temperature is raised to 75 ° C. After raising the temperature, hydrochloric acid is added to adjust the pH to 1.6. Thereafter, while adding 240 g of 40 mass% titanium tetrachloride aqueous solution at a rate of 1.4 g / min, the pH is maintained at 1.6 using 20 mass% sodium hydroxide aqueous solution. Thereafter, the dispersion is neutralized to pH 7 using a 20% by mass aqueous sodium hydroxide solution. Then, the salt was removed by washing with water, suction filtration, drying, and then baking at 700 ° C. for 90 minutes. As a result, a highly colored gold interference titanium oxide / iron oxide coated colored pearl pigment was obtained.

製造例2
硝酸第二鉄水溶液(硝酸第二鉄17質量部:水26質量部)337gを430gに代える以外は製造例1と同様にして、酸化鉄被覆パール顔料を製造した。得られた顔料は、薄片状雲母の上に、非常に微細な酸化鉄粒子が幾何学的膜厚30nmに均一に被覆されていた。被覆層の表面粗さを測定したところ、表面粗さは4.30nmであった。
次いで、40質量%四塩化チタン水溶液の添加量を240gから200gに代える以外は製造例1と同様にして、高彩度な金色干渉の酸化チタン/酸化鉄被覆パール顔料を得た。
Production Example 2
An iron oxide-coated pearl pigment was produced in the same manner as in Production Example 1 except that 337 g of ferric nitrate aqueous solution (17 parts by mass of ferric nitrate: 26 parts by mass of water) was replaced with 430 g. In the obtained pigment, very fine iron oxide particles were uniformly coated with a geometric film thickness of 30 nm on flaky mica. When the surface roughness of the coating layer was measured, the surface roughness was 4.30 nm.
Subsequently, a titanium oxide / iron oxide-coated pearl pigment with high chroma and golden interference was obtained in the same manner as in Production Example 1 except that the amount of the 40 mass% titanium tetrachloride aqueous solution was changed from 240 g to 200 g.

製造例3
硝酸第二鉄水溶液(硝酸第二鉄17質量部:水26質量部)337gを65gに代える以外は製造例1と同様にして、酸化鉄被覆パール顔料を製造した。得られた顔料は、薄片状雲母の上に、非常に微細な酸化鉄粒子が幾何学的膜厚5nm(光学的膜厚15nm)に均一に被覆されていた。被覆層の表面粗さを測定したところ、表面粗さは3.5nmであった。
次いで、40質量%四塩化チタン水溶液の添加量を240gから305gに代える以外は製造例1と同様にして、高彩度な金色干渉の酸化チタン/酸化鉄被覆パール顔料を得た。
Production Example 3
An iron oxide-coated pearl pigment was produced in the same manner as in Production Example 1 except that 337 g of an aqueous ferric nitrate solution (17 parts by mass of ferric nitrate: 26 parts by mass of water) was replaced with 65 g. In the obtained pigment, very fine iron oxide particles were uniformly coated on a flaky mica with a geometric film thickness of 5 nm (optical film thickness of 15 nm). When the surface roughness of the coating layer was measured, the surface roughness was 3.5 nm.
Subsequently, a titanium oxide / iron oxide-coated pearl pigment with high chroma and golden interference was obtained in the same manner as in Production Example 1 except that the addition amount of the 40 mass% titanium tetrachloride aqueous solution was changed from 240 g to 305 g.

製造例4
硝酸第二鉄水溶液(硝酸第二鉄17質量部:水26質量部)337gを65gに代える以外は製造例1と同様にして、酸化鉄被覆パール顔料を製造した。得られた顔料は、薄片状雲母の上に、非常に微細な酸化鉄粒子が幾何学的膜厚5nm(光学的膜厚30nm)に均一に被覆されていた。被覆層の表面粗さを測定したところ、表面粗さは3.5nmであった。
次いで、40質量%四塩化チタン水溶液の添加量を240gから170gに代える以外は、製造例1と同様にして、高彩度な赤色干渉の酸化チタン/酸化鉄被覆パール顔料を得た。
Production Example 4
An iron oxide-coated pearl pigment was produced in the same manner as in Production Example 1 except that 337 g of an aqueous ferric nitrate solution (17 parts by mass of ferric nitrate: 26 parts by mass of water) was replaced with 65 g. In the obtained pigment, very fine iron oxide particles were uniformly coated on a flaky mica with a geometric film thickness of 5 nm (optical film thickness of 30 nm). When the surface roughness of the coating layer was measured, the surface roughness was 3.5 nm.
Subsequently, a highly saturated red interference titanium oxide / iron oxide coated pearl pigment was obtained in the same manner as in Production Example 1 except that the amount of the 40 mass% titanium tetrachloride aqueous solution added was changed from 240 g to 170 g.

試験例1
製造例1〜4及び市販の酸化チタン被覆雲母(Flamenco Gold(ENGELHARD 社)について、粉体反射光のa*値、b*値、及び被覆層の幾何学的膜厚を測定した。
(1)粉体反射光のa*値、b*値は、「本発明のa*値、b*値の測定方法」に従って測定した。分光測色計は、村上色彩技術研究所社製GCMS−4に偏光板(ポラロイド社製 型式:HN32)を設置して測定した。光源は、ナーバ社のハロゲンランプ(HLWS7)を用いた。黒色人工皮革(オカモト社製 型式:OK−7)を使用し、5cm×10cmの範囲に平均0.05mg/cm2となるようにスポンジを用いて、粉体を均一に塗布したものを測定試料として用いた。
また、幾何学的膜厚の測定は、SEMにより行った。被覆前の薄片状粉体の厚さを測定し、被覆後のパール顔料の厚さを測定することで、幾何学的膜厚とした。光学的膜厚に関しては、幾何学的膜厚に屈折率をかけたものであり、酸化鉄(Fe2O3)の屈折率は3.0、酸化チタンの屈折率は2.5を用いた。結果を表1に示す。
Test example 1
With respect to Production Examples 1 to 4 and commercially available titanium oxide-coated mica (Flamenco Gold (ENGELHARD)), the a * value, b * value of powder reflected light, and the geometric film thickness of the coating layer were measured.
(1) The a * value and b * value of the powder reflected light were measured according to “Method for Measuring a * Value and b * Value of the Present Invention”. The spectrocolorimeter was measured by installing a polarizing plate (Model: HN32 manufactured by Polaroid) on GCMS-4 manufactured by Murakami Color Research Laboratory. As the light source, a halogen lamp (HLWS7) manufactured by Nerva was used. Measurement sample using black artificial leather (model name: OK-7, manufactured by Okamoto Co., Ltd.) with a uniform powder applied using a sponge so that the average is 0.05 mg / cm 2 in a range of 5 cm x 10 cm. Used as.
The measurement of the geometric film thickness was performed by SEM. The thickness of the flaky powder before coating was measured, and the thickness of the pearl pigment after coating was measured to obtain the geometric film thickness. The optical film thickness is obtained by multiplying the geometric film thickness by the refractive index. The refractive index of iron oxide (Fe 2 O 3 ) is 3.0, and the refractive index of titanium oxide is 2.5. . The results are shown in Table 1.

(2)また、前記条件で偏光板を用いない通常の一般的な測色法(測定角度45°)で、粉体反射光のa*値、b*値を測定した。また、C*値、h値は、国際照明委員会(1976年)(CIE)で規格された彩度、色相角度を示す。結果を表2に示す。
表2の結果より、本発明で用いるパール顔料は、同じ色相角度を有する市販品に比べC*値が大きい、すなわち鮮やかであり、有色金属化合物自身の色に束縛されずに自由に干渉色を得ていることが示される。
(2) Further, the a * value and b * value of the powder reflected light were measured by a general colorimetric method (measurement angle 45 °) without using a polarizing plate under the above conditions. The C * value and h value indicate the saturation and hue angle specified by the International Commission on Illumination (1976) (CIE). The results are shown in Table 2.
From the results shown in Table 2, the pearl pigment used in the present invention has a large C * value compared to a commercial product having the same hue angle, that is, it is vivid, and it is free from interference colors without being restricted by the color of the colored metal compound itself. It is shown that

Figure 2006193520
Figure 2006193520

Figure 2006193520
Figure 2006193520

実施例1〜4、比較例1〜2
表3に示す組成の固形粉末状ファンデーションを製造し、きめ細かい仕上がり、肌色の明るさ、額部と頬側面部の塗布色の差の少なさ及び自然なつやを評価した。結果を表1に併せて示す。
Examples 1-4, Comparative Examples 1-2
Solid powdery foundations having the compositions shown in Table 3 were produced and evaluated for fine finish, brightness of skin color, little difference in coating color between the forehead and cheek side portions, and natural gloss. The results are also shown in Table 1.

(製法)
成分(1)〜(13)を撹拌混合後、(14)〜(16)を添加して混合する。これをアトマイザーで粉砕し、篩掛けした後、金皿に充填、打錠して固形粉末状ファンデーションを得た。
(Manufacturing method)
Components (1) to (13) are stirred and mixed, and then (14) to (16) are added and mixed. This was pulverized with an atomizer and sieved, and then filled in a metal pan and tableted to obtain a solid powdery foundation.

(評価方法)
各固形粉末状ファンデーションを化粧品専用パネル20名が使用し、下記の基準で評価し、その平均値で判定した。
(1)きれいな肌に見える、きめ細かい仕上がり、肌色の明るさ、自然なつや;
5点:非常に良好。
4点:良好。
3点:普通。
2点:やや不良。
1点:不良。
(Evaluation methods)
Each solid powdery foundation was used by 20 panelists dedicated to cosmetics, evaluated according to the following criteria, and judged by the average value.
(1) Looks beautiful skin, fine finish, skin color brightness, natural gloss;
5 points: Very good.
4 points: Good.
3 points: Normal.
2 points: Somewhat bad.
1 point: Defect.

(2)額部と頬側面部の塗布色の差の少なさ;
5点:差がほとんどない。
4点:差が少ない。
3点:差がややある。
2点:差がやや大きい。
1点:差が大きい。
(2) Little difference in coating color between forehead and cheek side;
5 points: There is almost no difference.
4 points: Little difference.
3 points: There is a slight difference.
2 points: The difference is slightly large.
1 point: The difference is large.

Figure 2006193520
Figure 2006193520

本発明において、「本発明のa*値、b*値の測定方法」を示す図である。In the present invention, it is a diagram showing “a * value and b * value measuring method of the present invention”.

Claims (7)

薄片状粉体の表面に有色金属又は有色金属酸化物を被覆し、さらに無色金属又は無色金属酸化物を被覆したパール顔料であって、該パール顔料を黒色人工皮革表面に平均0.05mg/cm2で塗布し、入射光側にS偏光板、受光側にP偏光板を装着した分光測色計を用い、C光による2°視野の受光条件で、パール顔料の反射光量を測定したとき、測定試料面の法線方向に対して45°で入射し、法線方向で受光した粉体反射光のa*値及びb*値の絶対値が10以下であるパール顔料を含有するメークアップ化粧料。 A pearl pigment in which a surface of a flaky powder is coated with a colored metal or a colored metal oxide and further coated with a colorless metal or a colorless metal oxide, and the pearl pigment is coated on the surface of black artificial leather with an average of 0.05 mg / cm was coated with 2, S polarizing plate on the incident light side, with a spectrophotometer equipped with a P polarizer on the light receiving side, the light receiving condition of 2 ° visual field by C light, when measuring the reflected light amount of pearl pigment, Makeup makeup containing a pearl pigment whose absolute value of a * value and b * value of powder reflected light incident at 45 ° with respect to the normal direction of the measurement sample surface and received in the normal direction is 10 or less Fee. 薄片状粉体の表面に有色金属又は有色金属酸化物を表面平均粗さ10nm以下で被覆し、さらに無色金属又は無色金属酸化物を被覆したパール顔料を含有するメークアップ化粧料。   A makeup cosmetic containing a pearl pigment in which a surface of a flaky powder is coated with a colored metal or colored metal oxide with an average surface roughness of 10 nm or less and further coated with a colorless metal or a colorless metal oxide. パール顔料の有色金属が金、又は有色金属酸化物が酸化鉄である請求項1又は2記載のメークアップ化粧料。   The makeup cosmetic according to claim 1 or 2, wherein the colored metal of the pearl pigment is gold or the colored metal oxide is iron oxide. 無色金属がチタン、又は無色金属酸化物が酸化チタンである請求項1〜3のいずれか1項記載のパール顔料を含有するメークアップ化粧料。   The makeup cosmetic containing the pearl pigment according to any one of claims 1 to 3, wherein the colorless metal is titanium or the colorless metal oxide is titanium oxide. 有色金属又は有色金属酸化物の光学的膜厚が平均15〜650nmである請求項1〜4のいずれか1項記載のパール顔料を含有するメークアップ化粧料。   The make-up cosmetic containing the pearl pigment according to any one of claims 1 to 4, wherein an average optical film thickness of the colored metal or the colored metal oxide is 15 to 650 nm. 無色金属又は無色金属酸化物の光学的膜厚が平均180〜900nmである請求項1〜5のいずれか1項記載のパール顔料を含有するメークアップ化粧料。   6. The makeup cosmetic containing the pearl pigment according to any one of claims 1 to 5, wherein an average optical film thickness of the colorless metal or colorless metal oxide is 180 to 900 nm. さらに、25℃における粘度が1000mPa・s以下の油剤を含有する請求項1〜6のいずれか1項記載のメークアップ化粧料。   Furthermore, the makeup cosmetics of any one of Claims 1-6 containing the oil agent whose viscosity in 25 degreeC is 1000 mPa * s or less.
JP2005363490A 2004-12-16 2005-12-16 Makeup cosmetics Expired - Fee Related JP4791817B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2005363490A JP4791817B2 (en) 2004-12-16 2005-12-16 Makeup cosmetics

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2004363967 2004-12-16
JP2004363967 2004-12-16
JP2005363490A JP4791817B2 (en) 2004-12-16 2005-12-16 Makeup cosmetics

Publications (2)

Publication Number Publication Date
JP2006193520A true JP2006193520A (en) 2006-07-27
JP4791817B2 JP4791817B2 (en) 2011-10-12

Family

ID=36799870

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2005363490A Expired - Fee Related JP4791817B2 (en) 2004-12-16 2005-12-16 Makeup cosmetics

Country Status (1)

Country Link
JP (1) JP4791817B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009280542A (en) * 2008-05-26 2009-12-03 Shiseido Co Ltd Composite powder, its manufacturing method and cosmetic comprising the composite powder
JP2016088911A (en) * 2014-11-10 2016-05-23 ロレアル Composition having high coating characteristics

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59212422A (en) * 1983-05-19 1984-12-01 Shiseido Co Ltd Cosmetic
JPS62285956A (en) * 1986-05-23 1987-12-11 メルク・パテント・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング Pearl gloss pigment
JPH03197413A (en) * 1989-12-26 1991-08-28 Kobayashi Kose Co Ltd Solid powdery make-up cosmetic
JPH04128211A (en) * 1990-09-20 1992-04-28 Shiseido Co Ltd Ground cosmetic
JPH0711161A (en) * 1992-10-19 1995-01-13 Mearl Corp:The Pearlescent pigment of highly vivid color
JPH08259840A (en) * 1995-03-23 1996-10-08 Shiseido Co Ltd Red-based pigment and its production
WO2004061012A2 (en) * 2002-12-31 2004-07-22 Engelhard Corporation Improved effect pigment comprising a mixture of at least 2 substrate materials
JP2005526060A (en) * 2002-03-12 2005-09-02 オヴェ カールソン コンスルト Novel composition comprising a pigment assembly comprising a mica core
JP2006508982A (en) * 2002-11-15 2006-03-16 カラー アクセス,インコーポレイティド Transparent hiding cosmetic composition

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59212422A (en) * 1983-05-19 1984-12-01 Shiseido Co Ltd Cosmetic
JPS62285956A (en) * 1986-05-23 1987-12-11 メルク・パテント・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング Pearl gloss pigment
JPH03197413A (en) * 1989-12-26 1991-08-28 Kobayashi Kose Co Ltd Solid powdery make-up cosmetic
JPH04128211A (en) * 1990-09-20 1992-04-28 Shiseido Co Ltd Ground cosmetic
JPH0711161A (en) * 1992-10-19 1995-01-13 Mearl Corp:The Pearlescent pigment of highly vivid color
JPH08259840A (en) * 1995-03-23 1996-10-08 Shiseido Co Ltd Red-based pigment and its production
JP2005526060A (en) * 2002-03-12 2005-09-02 オヴェ カールソン コンスルト Novel composition comprising a pigment assembly comprising a mica core
JP2006508982A (en) * 2002-11-15 2006-03-16 カラー アクセス,インコーポレイティド Transparent hiding cosmetic composition
WO2004061012A2 (en) * 2002-12-31 2004-07-22 Engelhard Corporation Improved effect pigment comprising a mixture of at least 2 substrate materials
JP2006522165A (en) * 2002-12-31 2006-09-28 エンゲルハード・コーポレーシヨン Color effect pigments

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009280542A (en) * 2008-05-26 2009-12-03 Shiseido Co Ltd Composite powder, its manufacturing method and cosmetic comprising the composite powder
JP2016088911A (en) * 2014-11-10 2016-05-23 ロレアル Composition having high coating characteristics

Also Published As

Publication number Publication date
JP4791817B2 (en) 2011-10-12

Similar Documents

Publication Publication Date Title
US8153163B2 (en) Pearlescent pigment
EP1110535B1 (en) Cosmetic composition containing a hollow metal oxide plate powder
EP1672037B1 (en) Pearlescent pigment
JP5085168B2 (en) Cosmetics
JP2008088317A (en) White composite powder and cosmetic incorporated with the same
JP2006299051A (en) Composite powder for coloring and cosmetic material containing the same
JP2010280607A (en) Oily cosmetic
JP2001288038A (en) Cosmetic
JP4791817B2 (en) Makeup cosmetics
JP2003002634A (en) Colored mica titanium
JP2009280542A (en) Composite powder, its manufacturing method and cosmetic comprising the composite powder
JP4791816B2 (en) Makeup cosmetics
JP4709643B2 (en) Skin impression production method
TWI388341B (en) Impression controlling agent
JP3492966B2 (en) Cosmetics
JP4440630B2 (en) Cosmetics
JP2004123682A (en) Color pigment and makeup cosmetic
CN1789342B (en) Pearlescent pigment
JP4627960B2 (en) Cosmetics
JP3723710B2 (en) Cosmetics
JP2004083423A (en) Cosmetic
KR101508192B1 (en) Manufacturing Method for used Hydro-Thermal Synthesis of the Magnesium Hydroxide on the Flat Pigment Coated with Magnesium oxide and Development for Soft Focus Cosmetics Substrate Used Method
JP2004123681A (en) Makeup cosmetic
JP2001278743A (en) Cosmetics
JP2000229809A (en) Cosmetic

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20071023

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20091014

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20091110

A601 Written request for extension of time

Free format text: JAPANESE INTERMEDIATE CODE: A601

Effective date: 20100107

A602 Written permission of extension of time

Free format text: JAPANESE INTERMEDIATE CODE: A602

Effective date: 20100113

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20100209

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A821

Effective date: 20100210

A02 Decision of refusal

Free format text: JAPANESE INTERMEDIATE CODE: A02

Effective date: 20110301

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20110601

A911 Transfer to examiner for re-examination before appeal (zenchi)

Free format text: JAPANESE INTERMEDIATE CODE: A911

Effective date: 20110622

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20110719

A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20110722

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20140729

Year of fee payment: 3

R151 Written notification of patent or utility model registration

Ref document number: 4791817

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R151

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

LAPS Cancellation because of no payment of annual fees