WO2003049707A1 - Oil-in-water emulsion containing water-swellable clay mineral and use thereof - Google Patents

Oil-in-water emulsion containing water-swellable clay mineral and use thereof Download PDF

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Publication number
WO2003049707A1
WO2003049707A1 PCT/JP2001/010882 JP0110882W WO03049707A1 WO 2003049707 A1 WO2003049707 A1 WO 2003049707A1 JP 0110882 W JP0110882 W JP 0110882W WO 03049707 A1 WO03049707 A1 WO 03049707A1
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Prior art keywords
oil
water
pigment
water emulsion
filler
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PCT/JP2001/010882
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French (fr)
Japanese (ja)
Inventor
Mika Inoue
Original Assignee
L'oreal
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Publication date
Application filed by L'oreal filed Critical L'oreal
Priority to PCT/JP2001/010882 priority Critical patent/WO2003049707A1/en
Priority to AU2002221125A priority patent/AU2002221125A1/en
Publication of WO2003049707A1 publication Critical patent/WO2003049707A1/en

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • A61K8/062Oil-in-water emulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • A61P17/16Emollients or protectives, e.g. against radiation
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • A61Q1/08Preparations containing skin colorants, e.g. pigments for cheeks, e.g. rouge
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • A61Q1/10Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations

Definitions

  • the present invention relates generally to an oil-in-water emulsion suitable for use in cosmetics and the like, and more particularly to a stable oil-in-water emulsion in which pigments and / or fillers are well dispersed.
  • the present invention also relates to a cosmetic or external preparation for skin using such an emulsion. Furthermore, the present invention also aims at improving the dispersibility of pigments and / or fillers using specific components and the stability of oil-in-water emulsions.
  • W / 0 emulsions are available in solid, creamy, and milky liquids, and are excellent in terms of good makeup and water resistance.
  • usable surfactants are sorbinyl alkyl ester, dimethicone copolyol, and polyglycerylpolyol. Ricinoleate, polyglyceryl polyhydroxyacetate
  • the W / 0 emulsion is easy to mix the pigment / filament at a high concentration, which can reduce the oiliness but does not improve the lack of freshness and the weight of elongation. .
  • the 0 / W type emulsion has a fresh feeling when used, and its growth is light. Therefore, when a cosmetic such as a foundation having a refreshing feel without an oily feeling is desired, it is desirable to use a 0 / W type emulsion.
  • 0 / W type emulsions for example,
  • the present inventors have conducted intensive studies in view of the above circumstances, and as a result, surprisingly, by using a water-swellable clay mineral as a thickener and dispersing a hydrophilic pigment and / or filler, an emulsifier It has been found that even if the amount is small, good pigment // filler dispersibility and emulsion stability can be ensured, and a 0 / W-type emulsion with a refreshing feel and a high matte effect can be obtained. It has also been found that in such a ⁇ / W emulsion, good dispersibility and stability of the pigment can be ensured even when the amount of the fatty phase is suppressed.
  • the present invention provides a relatively large amount of water compared to the conventional 0 / W type emulsion.
  • the main object of the present invention is to provide a 0 / W emulsion having excellent dispersibility and stability of the pigment and / or filler even when the pigment and / or filler is contained. It is also an object to provide a 0 / W type emulsion that has a refreshing feel and a high matte effect.
  • such an object is to provide an oil-in-water emulsion containing a fatty phase, an aqueous phase, and a surfactant, wherein the water-swellable clay mineral is contained together with a hydrophilic pigment and / or a filler to obtain a surfactant.
  • This is achieved by reducing the amount of the agent to 5% or less, preferably 4% or less, more preferably 3% or less, and even more preferably 2% or less.
  • a water-swellable clay mineral is used to thicken the water, so that a hydrophilic pigment and / or filler is added.
  • Such an oil-in-water emulsion has a reduced amount of an emulsifier and preferably a fatty phase, so that the above-mentioned problems associated with the increase in the amount of the emulsifier are of course not caused. It was found that the aforementioned problems of poor elongation to the skin, stickiness, and poor adaptation to the skin, which had occurred during the use, were also resolved.
  • FR 2 750 602 in the name of the present applicant describes a cosmetic containing water-swellable synthetic my-power as an enhancer to enhance the protective effect of an ultraviolet ray protective agent.
  • inorganic pigments having a wavelength of 5 to 100 nm can also be used.
  • the inorganic pigment used in the examples is a pigment that has been subjected to a hydrophobic surface treatment, does not use a hydrophilic pigment and / or a filler as in the present invention, and is a modified paper (regulation). 91) Does not teach or suggest that these can be dispersed stably and uniformly.
  • the formulation of the cosmetic is not limited to the 0 / W type, but also includes all types such as W / 0 type, 0 / W / 0 type, W / 0 / W type, etc.
  • the water-swelling synthetic my power has been shown to be an enhancer that enhances the protective effect of the ultraviolet protective agent, the above-mentioned effect is obtained when this material is used as a thickener in the preparation of a 0 / W emulsion. It does not teach or suggest.
  • water swelling in “water swelling clay mineral” has a meaning generally understood by those skilled in the art, and particularly, the volume of the clay mineral increases due to absorption of water. Means that.
  • the water swellability of a clay mineral can be quantified, for example, by measuring the viscosity in a state where the clay mineral is completely swelled by being dispersed in water. Water swellability is determined by adding a clay mineral to water at a concentration of 10 w / w% with stirring and uniformly swelling it all day and night in a state of uniform dispersion.
  • Still another object of the present invention is to provide a cosmetic or a skin external preparation using the above oil-in-water emulsion.
  • an object of the present invention is to reduce the amount of surfactant used to 5% by weight or less, preferably 4% by weight or less, more preferably 3% by weight or less, and most preferably 2% by weight or less.
  • Another object is to provide a method characterized by improving the dispersibility of the filler and the stability of the emulsion.
  • the oil-in-water emulsion according to a preferred embodiment of the present invention contains a fatty phase, an aqueous phase, and a surfactant, and contains a water-swellable clay mineral together with a hydrophilic pigment and / or filler.
  • the amount of the surfactant is 5% or less, preferably 4% or less, more preferably 3% or less, and even more preferably 2% or less, and is prepared using a method well known to those skilled in the art.
  • the water-swellable clay mineral used in the oil-in-water emulsion according to the present invention is not limited to a natural one, and may be a synthetic product including a partially modified natural mineral, but is preferably a layered material belonging to the genus Smectite.
  • Veegum T (trade name), Veegum HV (trade name), Veegum F (trade name), Veegum K (trade name) commercially available from Vanderbilt;
  • Hectabright AW trade name
  • Hectabright 2000 trade name
  • Bentone EW Macaroide (trade name) sold by National Lead, available from American Colloid
  • the synthetic product may be manufactured by any method, and in particular, those manufactured by three methods of a hydrothermal method, a melting method, and a solid-phase reaction method are well known and are preferably used. used.
  • Particularly preferred compositions are:
  • Synthetic smectites such as Ionite (trade name) available from Mizusawa Chemical Industries, corrected paper (Rule 91) SWN (trade name) and SAN (trade name) marketed by Corp Chemical, Laponite (trade name) marketed by Laporte, Sumecton SA (trade name) marketed by Kunimine Industries;
  • Submica E from Watscale. This is a fluorinated tetracyanite mica containing sodium in the interlayer ions and is a white powder with the following formula:
  • the water swellability of the water-swellable clay mineral suitable for the present invention can be measured with a spindle No. 2 using a viscometer RM180 RHE OMAT (RHEOMETRIC SCIE> H1FIC FELtd).
  • the viscosity reading is at least 20 Pa ⁇ s, and more preferably the viscosity reading at the spindle N 0.3 is 20 Pa ⁇ s or more.
  • the viscosities of various clay minerals are shown in the following table.
  • the water-swellable clay mineral is preferably at a concentration of about 1 to about 20% by weight, more preferably about 3 to about 1% by weight, based on the total weight of the obtained emulsion. It can be contained at a concentration of 5% by weight.
  • the hydrophilic pigment and / or filler that can be contained in the oil-in-water emulsion according to the present invention may be any of those conventionally used or usable in the field of cosmetics and dermatology. Examples thereof include extender pigments, coloring pigments, inorganic pigments such as white pigments, organic pigments, pearlescent pigments, polymer powders, and functional pigments. Hydrophilic pigment and / or The filler may be an untreated hydrophilic pigment and / or filler, or may be a hydrophilic surface-treated pigment and / or filler.
  • talc non-swelling mai force
  • kaolin calcium carbonate, magnesium carbonate, calcium anhydride, aluminum silicate, magnesium silicate, calcium silicate, aluminum oxide, barium sulfate, bengara, yellow iron oxide, Black iron oxide, chromium oxide, gunjiyou, konjiyo, carbon black, titanium oxide (amorphous or rutile and / or anamorphic type crystals), zinc oxide, mica titan, fish scale foil, bismuth oxychloride, boron nitride, Examples thereof include silk powder, natural pigments, and the like. These pigments and / or fillers are used alone or in combination of two or more.
  • pigments and / or fillers with relatively large average particle sizes are selected.
  • any treating agent may be used as long as it is conventionally used for imparting hydrophilicity to the pigment and / or filler.
  • a powder can be used, a powder that has been subjected to a surface treatment with a treating agent such as a silica treatment, an alumina treatment, a silica-alumina treatment, or a titania treatment can also be used.
  • a treating agent such as a silica treatment, an alumina treatment, a silica-alumina treatment, or a titania treatment
  • resilient treatment is suitably selected, and the treatment method itself is well known in the art.
  • the hydrophilic pigment and / or filler contained in the oil-in-water emulsion according to the present invention preferably contains 0.1 to 30% by weight, more preferably 0.5 to 10% by weight in the emulsion. Included in quantity.
  • the pigment and / or filler contained in the oil-in-water emulsion according to the present invention is basically the above-described hydrophilic pigment and / or filler, but the pigment and / or filler of the oil-in-water emulsion according to the present invention. Maintain effects such as filler dispersibility and uniformity As long as it is within the range, a pigment and / or a filler for hydrophobic treatment may be contained.
  • the amount of pigment and / or filler of this hydrophobic treatment that can be contained in the oil-in-water emulsion is preferably at most about 5% by weight, more preferably about 3% by weight.
  • any surfactant can be used as long as it has been conventionally used for emulsification of this type of oil-in-water emulsion. However, its usage is kept low.
  • the surfactant that can be used include polyoxyethylene alkyl ether, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester., Polyoxyethylene glycerin fatty acid ester, and polyoxyethylene glycerin fatty acid ester.
  • Nonionic surfactants such as oxyethylene hydrogenated castor oil and polyoxyethylene sorbitol fatty acid ester; Anionic surfactants such as sodium stearate and triethanolamine palmitate represented by fatty acid lithography Is mentioned.
  • Particularly preferred surfactants include a combination of stearic acid and Arlacel 165FL (50% glyceryl stearate + 50% PEG-100 stearic acid) manufactured by Uniqema and Sesolanol.
  • the fatty phase of the oil-in-water emulsion according to the present invention means not only a liquid oil but also a phase of any non-aqueous substance or a mixture of non-aqueous substances including a solid fat or a semi-solid oil.
  • the non-aqueous substance constituting the fatty phase i.e., the oil, may be any of vegetable, mineral, animal and / or synthetic oils as long as it has been conventionally used in the preparation of an oil-in-water emulsion. May be.
  • apogado oil olive oil, jojoba oil, oleic acid, isostearic acid, hexadecyl alcohol, oleyl alcohol, cetyl 2-ethylhexanoate, 2-ethylhexyl palmitate, myristate-2 Octyldodecyl, neopentylglycol di-2-ethylhexanoate, glycerol tri-2-ethylhexanoate, oleic acid-2-octyldodecyl, isopropyl myristate, glycerol triisostearate, 2-ethylhexane Acid diglyceride, di-paramethoxy carboxylic acid Glyceryl mono-2-ethylhexanoate dimethylpolysiloxane, dimethylpolysiloxane, methylphenylpolysiloxane, octamethylcyclote
  • the amount of fatty phase is preferably about 5 to 20% by weight, more preferably about 5% by weight, based on the total weight of the emulsion. It is preferable that the content be 15 to 15% by weight. If the amount of the fatty phase is too small, when used in cosmetics, the makeup finish is very easy to dry, pigments and / or fillers tend to be uneven, and a comfortable moist feeling cannot be obtained. Your skin will be dry. On the other hand, if the amount of the fatty phase is too large, the skin will not fit well, the oily feeling will be too heavy and the feeling will be heavy, and the stability itself will be adversely affected.
  • the aqueous phase preferably consists of water such as purified water, but in some cases, C 2-
  • the aqueous phase is preferably about 35-95% by weight, more preferably about 40-80% by weight, based on the total weight of the emulsion.
  • a water-swellable clay mineral is used as a thickening agent.
  • ordinary hydrophilic thickening agents such as carboxyvinyl polymer, acrylic copolymer, Acrylamide, polysaccharides, natural gums, etc. may be added.
  • a lipophilic thickener to the fatty phase, such as a modified clay such as bentone, a fatty acid metal salt such as aluminum stearate, or the like. Examples thereof include hydrophobic silica, ethyl cellulose, and polyethylene.
  • the oil-in-water emulsion of the present invention is preferably used as a cosmetic or a skin external preparation. Used. That is, in one embodiment of the present invention, there is provided a cosmetic or external preparation for skin consisting of the oil-in-water emulsion or containing the oil-in-water emulsion.
  • the cosmetic may be of any use, but cosmetics for make-up, skin care, and hair care are particularly preferably provided.
  • the makeup cosmetic may be a makeup of the skin of the body such as the face, lips, and eyes, or a makeup of the skin skeleton such as nails and hair. More specifically, it can take the form of a foundation, lip product, brusher, eye shadow, concealer, and the like.
  • the cosmetic or external preparation for skin may contain additives such as ordinary active ingredients to be contained in cosmetics or external products for skin.
  • Such additives include, in particular, organic solvents, softeners, antioxidants, antifree radical agents, opacifiers, stabilizers, emollients, defoamers, humectants, vitamins, fragrances, preservatives, metals
  • Conventional sequestering agents selected from ion sequestering agents, polymers, basic or acidifying agents, dyes, self-tanning agents, and any other ingredients commonly used in the cosmetic and / or dermatological fields.
  • Cosmetic and / or dermatological adjuvants Each component is contained in an aqueous phase or a fatty phase depending on the compatibility or the like.
  • a water phase, a fatty phase and a Of a water-swellable clay mineral (Submica E from Wakkale) in water hereinafter referred to as “synthetic mykadiel”.
  • Oil-in-water emulsions of the present invention (Examples 1 and 2 of the present invention) prepared by mixing and dispersing treated pigments or hydrophilic surface-treated pigments, and replacing the pigments with hydrophobic surface-treated pigments (Comparative Example 1) was prepared, and the properties of the emulsion, the dispersibility of the pigment, and the stability were compared.
  • a synthetic mica diel and a diel containing a surface-untreated pigment (Comparative Example 2), a synthetic mica diel and a diel containing a hydrophilic surface-treated pigment (Comparative Example 3), and a synthetic mica diel and a diel containing a hydrophobic surface-treated pigment (Comparative Example 2) Comparative Example 4
  • Synthesis without Using Surfactant Oil-in-Water Emulsion Containing Mica Diel and Surface Untreated Pigment (Comparative Example 5)
  • Synthetic Mica Diel without Using Surfactant and Hydrophobic Surface-treated Pigment An oil-in-water emulsion (Comparative Example 6) containing the same was prepared, and its properties and feel were similarly examined.
  • the stability was examined after storage at 45 ° C for 2 months.
  • Arlacel 165FL (manufactured by UNIQEMA)
  • Directions for use Spread an appropriate amount on skin, leave for 5 to 15 minutes, and then wipe off or rinse with water.

Abstract

An oil-in-water emulsion which comprises a fat phase, an aqueous phase, and a surfactant, and which further contains a water-swellable clay mineral incorporated therein together with a hydrophilic pigment and/or filler and has a surfactant content reduced to 5% or lower; a use of the emulsion in a cosmetic preparation or skin preparation; and a method of preparing the emulsion.

Description

明細書  Specification
水膨潤性粘土鉱物を含有する水中油型エマルシヨン及びその用途 Oil-in-water emulsion containing water-swellable clay mineral and use thereof
技術分野 Technical field
本発明は、 一般には化粧料等に用いて好適な水中油型エマルションに係り、 より詳細には、 顔料及び/又はフイラ一を良好に分散した安定な水中油型エマ ルションに関する。 本発明はまたかかるエマルシヨンを用いた化粧料又は皮膚 外用剤に関する。 更に、 特定の成分を用いる顔料及び/又はフィラーの分散性 と水中油型エマルションの安定性の改善をも対象とする。 背景技術  The present invention relates generally to an oil-in-water emulsion suitable for use in cosmetics and the like, and more particularly to a stable oil-in-water emulsion in which pigments and / or fillers are well dispersed. The present invention also relates to a cosmetic or external preparation for skin using such an emulsion. Furthermore, the present invention also aims at improving the dispersibility of pigments and / or fillers using specific components and the stability of oil-in-water emulsions. Background art
現在市場で売られているフアンデーシヨンやメークアツプ下地に代表される 高濃度の顔料及び/又はフィラーを含む化粧料の形態は、 大きく分けて 0 /W 型エマルションと、 W/ 0型エマルシヨン並びに非水系及び水系に分類される。 W/ 0型エマルシヨンは、 固形、 クリーム状、 乳液状などがあり、 化粧もちの 良さや耐水性の面で優れている。 しかしながら、 連続相が油からなるため、 油 性感が生じて、 さっぱり感に欠け、 伸びが重いという不具合があり、 使用でき る界面活性剤も、 ソルビ夕ンアルキルエステル、 ジメチコ一ンコポリオール、 ポリグリセリルポリ リシノレエート、 ポリグリセリルポリヒ ドロキシステアレ Cosmetics containing high concentrations of pigments and / or fillers, such as foundations and makeup bases currently sold in the market, can be roughly divided into 0 / W emulsions, W / 0 emulsions and non- It is classified into water system and water system. W / 0 emulsions are available in solid, creamy, and milky liquids, and are excellent in terms of good makeup and water resistance. However, since the continuous phase is composed of oil, it has an oily feeling, lacks a refreshing feeling, and has a problem that the elongation is heavy. Also, usable surfactants are sorbinyl alkyl ester, dimethicone copolyol, and polyglycerylpolyol. Ricinoleate, polyglyceryl polyhydroxyacetate
—トなどに限られている。 また、 W/ 0型エマルシヨンは、 顔料ゃフイラ一を 高濃度で配合することが容易であり、 そうすることにより、 油性感は軽減でき るが、 さっぱり感のなさや伸びの重さは改善できない。 —Limited to In addition, the W / 0 emulsion is easy to mix the pigment / filament at a high concentration, which can reduce the oiliness but does not improve the lack of freshness and the weight of elongation. .
これに対して、 0 /W型エマルシヨンは、 使用時においてみずみずしいさつ ばり感があり、 伸びも軽い。 よって、 油性感のないさっぱり した感触のファン デ一ション等の化粧料が望まれる場合には、 0 /W型エマルシヨンとすること が望ましい。 しかし、 0 /W型エマルシヨンは、 例えばファンデーションとし  On the other hand, the 0 / W type emulsion has a fresh feeling when used, and its growth is light. Therefore, when a cosmetic such as a foundation having a refreshing feel without an oily feeling is desired, it is desirable to use a 0 / W type emulsion. However, 0 / W type emulsions, for example,
訂正された用紙 (規則 91) た場合、 その感触の良さに反し、 幾つかの欠点がある。 先ず、 連続相が水相で あるため、 耐水性に劣り、 汗などに弱い。 また、 W/ 0型エマルシヨンに比べ て、 顔料ゃフイラ一を高濃度に配合し、 良好な分散性と安定性を得るのが困難 であり、 これらの特性を確保するためには、 乳化剤の量や脂肪相の量を多く し たり、 水溶性高分子を配合してエマルシヨンの粘度を増加させて顔料の凝集 · 沈降を防ぐ必要があった。 Corrected form (Rule 91) If it does, it has some drawbacks, contrary to its good feel. First, since the continuous phase is an aqueous phase, it has poor water resistance and is susceptible to sweat. Also, compared to W / 0 type emulsions, it is difficult to obtain a high dispersibility and stability by blending pigment / filament at a higher concentration. It was necessary to prevent the aggregation and sedimentation of the pigment by increasing the viscosity of the emulsion by increasing the amount of the emulsion and the fatty phase, or by adding a water-soluble polymer.
しかし、 これらの対処法では次のような問題があった。  However, these countermeasures had the following problems.
すなわち、 顔料の分散剤として働く乳化剤、 すなわち界面活性剤を増やすこ とによって、 顔料の分散性と安定性を確保する場合は、 界面活性剤によって製 品の耐水性が著しく下がり、 感触もべたついたものになってしまうという不具 合がある。  In other words, when the dispersibility and stability of the pigment are secured by increasing the emulsifier that acts as a dispersant for the pigment, that is, by increasing the surfactant, the water resistance of the product is significantly reduced by the surfactant, and the feel is also sticky. There is a problem that it becomes something.
また、 脂肪相の量を多くすると、 肌なじみが悪くなつたり、 油性感が出過ぎ て重い感触になったり、 安定性そのものにも悪影響が出た。  Also, increasing the amount of the fat phase made the skin less adaptable, became too oily to give a heavy feel, and adversely affected the stability itself.
更に、 水溶性高分子を配合する方法では、 顔料の凝集 · 沈降を防ぎうる粘度 を達成するためには、 この水溶性高分子を高配合する必要があった。 しかし、 水溶性高分子の配合量を上げれば上げるほど、 肌への伸びが悪くなり、 場合に よっては肌で伸ばすときに、 消しゴムのカスのようなものを生じることがあつ た。 更に、 感触もべたつき、 肌なじみも悪くなる傾向にある。 発明の開示  Furthermore, in the method of blending a water-soluble polymer, it was necessary to blend this water-soluble polymer in a high amount in order to achieve a viscosity that can prevent aggregation and sedimentation of the pigment. However, the higher the blending amount of the water-soluble polymer, the worse the elongation to the skin, and in some cases, when the skin was stretched, a residue like an eraser was formed. In addition, the feel tends to be sticky and the skin adaptation tends to be poor. Disclosure of the invention
本発明者らは、 上記事情に鑑みて鋭意研究を行った結果、 意外にも、 水膨潤 性粘土鉱物を増粘剤として用いて、 親水性顔料及び/又はフィラーを分散させ ることによって、 乳化剤の量を少量にしても、 良好な顔料及び/フィラーの分 散性とエマルションの安定性が確保でき、 さっぱり した感触でマツ ト効果の高 い 0 /W型エマルシヨンが得られることを見出した。 また、 このような〇/W 型エマルシヨンでは、 脂肪相の量を抑えても、 顔料の良好な分散性と安定性が 確保できることも見出された。  The present inventors have conducted intensive studies in view of the above circumstances, and as a result, surprisingly, by using a water-swellable clay mineral as a thickener and dispersing a hydrophilic pigment and / or filler, an emulsifier It has been found that even if the amount is small, good pigment // filler dispersibility and emulsion stability can be ensured, and a 0 / W-type emulsion with a refreshing feel and a high matte effect can be obtained. It has also been found that in such a 〇 / W emulsion, good dispersibility and stability of the pigment can be ensured even when the amount of the fatty phase is suppressed.
しかして、 本発明は、 従来の 0 /W型エマルシヨンと比較して、 比較的多量 の顔料及び/又はフィラーを含有させても、 顔料及び/又はフィ ラーの分散性、 安定性に優れる 0 /W型エマルシヨンを提供することを主たる目的とする。 また、 さっぱり した感触でマツ ト効果も高い 0 /W型エマルシヨンを提供す ることも目的とする。 Thus, the present invention provides a relatively large amount of water compared to the conventional 0 / W type emulsion. The main object of the present invention is to provide a 0 / W emulsion having excellent dispersibility and stability of the pigment and / or filler even when the pigment and / or filler is contained. It is also an object to provide a 0 / W type emulsion that has a refreshing feel and a high matte effect.
本発明において、 かかる目的は、 脂肪相と水相と界面活性剤とを含有する水 中油型エマルシヨンにおいて、 水膨潤性粘土鉱物を、 親水性顔料及び/又はフ イラ一と共に含有せしめて、 界面活性剤の量を 5 %以下、 好ましくは 4 %以下 より好ましくは 3 %以下、 更により好ましくは 2 %以下にすることにより、 達 成される。 しかして、 本発明では、 顔料及び/又はフイラ一を多く含む水中油 型エマルシヨンの調製において、 水膨潤性粘土鉱物を用いて水を増粘させるこ とにより、 親水性の顔料及び/又はフィラーを良好に均一に分散させたもので、 界面活性剤を低減させ、 好ましくは脂肪相の量自体も低減させたものである。 このような水中油型エマルシヨンは、 乳化剤と好ましくは脂肪相の量が低減さ れているので、 それらの増量に伴う前述の不具合を生じることがないことは無 論であるが、 水溶性高分子の使用の際に生じていた肌への伸びの悪さ、 ベたつ き、 肌なじみの悪さという前述の不具合も解消されることが知見された。  In the present invention, such an object is to provide an oil-in-water emulsion containing a fatty phase, an aqueous phase, and a surfactant, wherein the water-swellable clay mineral is contained together with a hydrophilic pigment and / or a filler to obtain a surfactant. This is achieved by reducing the amount of the agent to 5% or less, preferably 4% or less, more preferably 3% or less, and even more preferably 2% or less. Thus, in the present invention, in the preparation of an oil-in-water emulsion containing a large amount of pigment and / or filler, a water-swellable clay mineral is used to thicken the water, so that a hydrophilic pigment and / or filler is added. It is a well-dispersed one in which the surfactant is reduced, and preferably the amount of the fatty phase itself is also reduced. Such an oil-in-water emulsion has a reduced amount of an emulsifier and preferably a fatty phase, so that the above-mentioned problems associated with the increase in the amount of the emulsifier are of course not caused. It was found that the aforementioned problems of poor elongation to the skin, stickiness, and poor adaptation to the skin, which had occurred during the use, were also resolved.
上記において、 水膨潤性粘土鉱物が水系を増粘することは、 例えば、 Cosmetics & Toiletries, Vo. 104, July 1989 p.87に既に記載されている。 しかし、 この文献に は、 水膨潤性粘土鉱物を用いると、 界面活性剤の量を低く抑えた状態でも、 親 水性顔料及び/又はフイラ一を良好に分散させ 0 /W型エマルシヨンを安定化 させることができることは教示も示唆もされていない。 実際、 文献において記 載されている処方においては、 乳化剤として、 6 %のォレイ ン酸と脂肪酸石鹼 を生成させるための中和剤である トリエタノールァミン 1 %が配合されている。 また、 本出願人名義の F R 2 7 5 0 6 0 2号には、 水膨潤性合成マイ力を紫 外線防御剤の防御効果を高める増強剤として含有する化粧料が記載され、 紫外 線防御剤としては 5〜 1 0 0 n mの無機顔料も使用できることが開示されてい る。 しかし、 実施例で使用されている無機顔料は疎水性の表面処理を施した顔 料であり、 本願のような親水性顔料及び/又はフィラーを用いておらず、 よつ 訂正された用紙 (規則 91) てこれらを安定かつ均一に分散できるかは教示も示唆もしていない。 また、 化 粧料の剤型は 0 /W型に限定されるものではなく、 W/ 0型、 0 /W/ 0型、 W/ 0 /W型等全てを含むものであることから見ても、 水膨潤性合成マイ力が 紫外線防御剤の防御効果を高める増強剤となることを示しているものの、 この 材料を増粘剤として 0 /W型エマルシヨンの調製に用いたときに前述の効果が ありうることは教示も示唆もしていない。 In the above, the fact that the water-swellable clay mineral thickens the aqueous system has already been described, for example, in Cosmetics & Toiletries, Vo. 104, July 1989, p.87. However, according to this document, the use of a water-swellable clay mineral stably stabilizes the 0 / W emulsion by dispersing the hydrophilic pigment and / or filler even when the amount of the surfactant is kept low. There is no teaching or suggestion of what can be done. In fact, in the formulation described in the literature, as an emulsifier, 6% of oleic acid and 1% of triethanolamine, a neutralizing agent for producing fatty acid minerals, are blended. In addition, FR 2 750 602 in the name of the present applicant describes a cosmetic containing water-swellable synthetic my-power as an enhancer to enhance the protective effect of an ultraviolet ray protective agent. It is disclosed that inorganic pigments having a wavelength of 5 to 100 nm can also be used. However, the inorganic pigment used in the examples is a pigment that has been subjected to a hydrophobic surface treatment, does not use a hydrophilic pigment and / or a filler as in the present invention, and is a modified paper (regulation). 91) Does not teach or suggest that these can be dispersed stably and uniformly. Further, the formulation of the cosmetic is not limited to the 0 / W type, but also includes all types such as W / 0 type, 0 / W / 0 type, W / 0 / W type, etc. Although the water-swelling synthetic my power has been shown to be an enhancer that enhances the protective effect of the ultraviolet protective agent, the above-mentioned effect is obtained when this material is used as a thickener in the preparation of a 0 / W emulsion. It does not teach or suggest.
なお、 「水膨潤性粘土鉱物」 における 「水膨潤性」 なる用語は、 当業者が一 般に理解するところの意味を持つものであって、 特に粘土鉱物が水を吸収して 容積が増大することを意味する。 粘土鉱物のこの水膨潤性は、 例えば、 粘土鉱 物を水に分散させて完全に膨潤させた状態において粘度を測定することにより、 定量化できる。 しかして、 水膨潤性は、 粘土鉱物を 1 0 w/w %濃度になるよ うに水中に攪拌下で投入して均一分散させた状態で一昼夜完全膨潤させ、 室温 The term "water swelling" in "water swelling clay mineral" has a meaning generally understood by those skilled in the art, and particularly, the volume of the clay mineral increases due to absorption of water. Means that. The water swellability of a clay mineral can be quantified, for example, by measuring the viscosity in a state where the clay mineral is completely swelled by being dispersed in water. Water swellability is determined by adding a clay mineral to water at a concentration of 10 w / w% with stirring and uniformly swelling it all day and night in a state of uniform dispersion.
( 2 5 °C ) において、 例えば粘度計 R M 1 8 0 R H E 0 M A T ( RHEOMETRIC SCIENTIFIC F.E丄 td) を用いて測定した粘度 ( 2 0 0 S—1のせん断速度で、 時間 t = 1 0分で測定) が、 好ましくはスピンドル N 0 . 2で測定可能なもので、 その粘度読取値が 2 0 P a · s以上のもの、 より好ましくは、 スピンドル N o . 3での粘度読取値が 2 0 P a · s以上のものである。 (25 ° C), measured using a viscometer RM 180 RHE 0 MAT (RHEOMETRIC SCIENTIFIC FE 丄 td) (shear rate of 200 S- 1 , at time t = 10 minutes Is preferably measurable with spindle N 0.2 and has a viscosity reading of at least 20 Pa · s, more preferably a viscosity reading of spindle No. 3 of 20 More than P a · s.
更に、 本発明の他の目的は、 上記水中油型エマルシヨンを用いた化粧料又は 皮膚外用剤を提供することにもある。  Still another object of the present invention is to provide a cosmetic or a skin external preparation using the above oil-in-water emulsion.
更にまた、 本発明の目的は、 使用する界面活性剤の量を 5重量%以下、 好ま しくは 4重量%以下、 より好ましくは 3重量%以下、 最も好ましくは 2重量% 以下に抑えて、 顔料及び/又はフィラーを含有する水中油型エマルシヨンを調 製する方法において、 顔料及び/又はフィラーを親水性顔料及び/又はフィラ —とし、 更に水膨潤性粘土鉱物を添加し、 これによつて顔料及び/又はフイラ 一の分散性とエマルシヨンの安定性を改善することを特徴とする方法を提供す ることにもある。  Furthermore, an object of the present invention is to reduce the amount of surfactant used to 5% by weight or less, preferably 4% by weight or less, more preferably 3% by weight or less, and most preferably 2% by weight or less. And / or a method for preparing an oil-in-water emulsion containing a filler, wherein the pigment and / or the filler is a hydrophilic pigment and / or a filler, and a water-swellable clay mineral is further added. Another object is to provide a method characterized by improving the dispersibility of the filler and the stability of the emulsion.
本発明の更なる目的、 構成、 効果は、 以下に記載する発明の実施形態に対す る詳細な説明を読めば明確になるであろう。 訂正された用紙 (規則 91) 発明の実施の形態 Further objects, configurations, and effects of the present invention will become apparent from a detailed description of the embodiments of the present invention described below. Corrected form (Rule 91) Embodiment of the Invention
しかして、 本発明の好適な実施形態に係る水中油型エマルシヨンは、 脂肪相 と水相と界面活性剤とを含有し、 また水膨潤性粘土鉱物を、 親水性顔料及び/ 又はフィラーと共に含有し、 界面活性剤の量は 5 %以下、 好ましくは 4 %以下、 より好ましくは 3 %以下、 更により好ましくは 2 %以下とされており、 当業者 には周知の方法を用いて調製される。  Thus, the oil-in-water emulsion according to a preferred embodiment of the present invention contains a fatty phase, an aqueous phase, and a surfactant, and contains a water-swellable clay mineral together with a hydrophilic pigment and / or filler. The amount of the surfactant is 5% or less, preferably 4% or less, more preferably 3% or less, and even more preferably 2% or less, and is prepared using a method well known to those skilled in the art.
本発明に係る水中油型エマルシヨンにおいて使用される水膨潤性粘土鉱物は、 天然のものに限らず、 天然鉱物を一部変性したものを含む合成品でもよいが、 好ましくはスメクタイ ト属に属する層状ケィ酸塩鉱物であり、 1つの八面体シ 一卜が 2つの四面体シートに挟まれた 2 : 1型構造を持つ。  The water-swellable clay mineral used in the oil-in-water emulsion according to the present invention is not limited to a natural one, and may be a synthetic product including a partially modified natural mineral, but is preferably a layered material belonging to the genus Smectite. A silicate mineral with a 2: 1 type structure in which one octahedral sheet is sandwiched between two tetrahedral sheets.
このような要求に合致する天然の粘土鉱物としては以下のものが列挙される 一 モンモリロナイ ト、 例えば、 クニミネ工業から市販されている Kunipia G4 (商品名)、 Kunipia G (商品名) Kunipia F (商品名)、 Laporte社から市販され ている Gelwhite HNF sterilise (商品名) ;  The following are listed as natural clay minerals that meet such requirements. 1 Montmorillonite, for example, Kunipia G4 (trade name), Kunipia G (trade name), Kunipia F (trade name) commercially available from Kunimine Industries Gelwhite HNF sterilise (trade name) commercially available from Laporte;
- パイデライ ト ; -Paiderite;
- ノントロナイ ト ; -Nontronite;
- サボナイ ト、 例えば、 Vanderbilt社から市販されている Veegum T (商品名)、 Veegum HV (商品名)、 Veegum F (商品名)、 Veegum K (商品名) ;  -Savonites, such as Veegum T (trade name), Veegum HV (trade name), Veegum F (trade name), Veegum K (trade name) commercially available from Vanderbilt;
- ヘク トライ ト、 例えば American Colloid社から市販されている Hectabright AW (商品名)、 Hectabright 2000 (商品名)、 Bentone EW、 National Lead社より巿販さ れている Macaroide (商品名) ; -Hectolites, such as Hectabright AW (trade name), Hectabright 2000 (trade name), Bentone EW, Macaroide (trade name) sold by National Lead, available from American Colloid;
- ソ一コナイ ト ; -United States;
一 スチブンサイ ト。 One step site.
一方、 合成品は、 如何なる方法により製造したものであってもよいが、 特に 水熱法、 溶融法、 固相反応法の 3種の方法により製造されたものがよく知られ ており、 好適に使用される。 特に好ましい合成品は次のものである :  On the other hand, the synthetic product may be manufactured by any method, and in particular, those manufactured by three methods of a hydrothermal method, a melting method, and a solid-phase reaction method are well known and are preferably used. used. Particularly preferred compositions are:
一 合成スメクタイ ト、例えば水沢化学工業から市販されている Ionite (商品名)、 訂正された用紙 (規則 91) コープケミカル社から市販されている SWN (商品名)、 SAN (商品名)、 Laporte 社から市販されている Laponite (商品名)、 クニミネ工業から市販されている Sumecton SA (商品名) ; (I) Synthetic smectites, such as Ionite (trade name) available from Mizusawa Chemical Industries, corrected paper (Rule 91) SWN (trade name) and SAN (trade name) marketed by Corp Chemical, Laponite (trade name) marketed by Laporte, Sumecton SA (trade name) marketed by Kunimine Industries;
一 合成マイ力、 例えばワツケ一ル社から Submica E の商品名で市販されてい るもの。 (I) Synthetic my powers, for example, those marketed under the trade name of Submica E from Watchel.
上記の種々の粘土鉱物の中でも、 最も好ましいものは、 ワツケール社の Submica Eである。 これは、 層間イオンにナトリウムを含むフッ素四ケィ素雲母 で、 白色粉体であり、 次の示性式 :  Among the various clay minerals described above, the most preferred one is Submica E from Watscale. This is a fluorinated tetracyanite mica containing sodium in the interlayer ions and is a white powder with the following formula:
(N a 20) X (M g O) y (S i O 2) z M g F 2 (N a 20 ) X (M g O) y (S i O 2) z M g F 2
[上式中、 X、 y、 zは、 次の関係を満たす数である : [Where X, y, and z are numbers that satisfy the following relationship:
0. 1≤x≤ 0. 5  0.1 ≤ x ≤ 0.5
1. 5≤ y≤ 2  1.5 ≤ y≤ 2
3. 5≤ z≤ 4 ]  3.5 ≤ z ≤ 4]
を有している。 have.
本発明に好適な水膨潤性粘土鉱物の水膨潤性は、 前述のように、 粘度計 RM 1 8 0 RHE OMAT (RHEOMETRIC SCIE>H1FIC F.E.Ltd) を用いて、 スピンド ル N o. 2で測定可能なもので、 その粘度読取値が 2 0 P a · s以上のものが 好ましく、 より好適にはスピンドル N 0. 3での粘度読取値が 20 P a · s以 上のものである。 様々な粘土鉱物の粘度は次の表のとおりである。  As described above, the water swellability of the water-swellable clay mineral suitable for the present invention can be measured with a spindle No. 2 using a viscometer RM180 RHE OMAT (RHEOMETRIC SCIE> H1FIC FELtd). Preferably, the viscosity reading is at least 20 Pa · s, and more preferably the viscosity reading at the spindle N 0.3 is 20 Pa · s or more. The viscosities of various clay minerals are shown in the following table.
訂正された用紙 (規則 91) 粘土鉱物 成分名 商品名 会社名 スピン卜"ル 粘度 (読取値) 麵性 Corrected form (Rule 91) Clay mineral Ingredient name Trade name Company name Spindle viscosity (reading value)
No. /Pa's 可/不可 タルク LUZE NAC LUZENAC 1 測定不可 不可  No. / Pa's Available / Unavailable Talc LUZE NAC LUZENAC 1 Unavailable
15MOO (低粘度)  15MOO (low viscosity)
マイ力 MEARLMICA ENGELHARD 1 25.5 不可  My power MEARLMICA ENGELHARD 1 25.5 Not possible
MMCF  MMCF
非水膨潤性 PDM-8W トピ—工業 (株) 1 26.0 不可 合成マイ力  Non-water swellable PDM-8W Topy Industries, Ltd. 1 26.0 Not possible Synthetic
カオリン KAOLIN IMERYS 1 31.3 不可  Kaolin KAOLIN IMERYS 1 31.3 Not possible
SUPREME  SUPREME
モンモリ口ナイト GELWHITE LAPORTE 3 21.8 可  Montmorikochi Night GELWHITE LAPORTE 3 21.8 OK
HNF  HNF
サボナイト VEEGUMHV VANDERBILT 3 38.5 可 水膨潤性合成マイ力 Submica E ワツケ一ル社 4 27.7 可 合成サボナイト SUMECTON クニミネ工業 (株) 4 48.8 可  Sabonite VEEGUMHV VANDERBILT 3 38.5 Possible Synthetic water swelling power Submica E Watsukeru 4 27.7 Possible Synthetic savonite SUMECTON Kunimine Kogyo Co., Ltd. 4 48.8 Possible
-SA  -SA
注) 粘土鉱物 1 0 W/W%濃度になるように水中に、 攪拌機 (Rayneri/Groupe VMI) にて撹拌しながら振り入れ、 均一分散した後、 一昼夜完全膨張させて室温 ( 2 5°C) の条件で粘度を測定した。 粘度値は 200 S—1のせん断速度で、 時間 t = 1 0分で測定した。 Note) Clay minerals Sprinkle into water to a concentration of 10 W / W% while stirring with water using a stirrer (Rayneri / Groupe VMI), disperse uniformly, allow to expand completely for 24 hours, then room temperature (25 ° C) The viscosity was measured under the following conditions. Viscosity values were measured at a shear rate of 200 S-1 at a time t = 10 minutes.
本発明の水中油型エマルシヨンにおいて、 上記水膨潤性粘土鉱物は、 得られ るエマルションの全重量に対して好ましくは約 1〜約 2 0重量%の濃度で、 よ り好ましくは約 3〜約 1 5重量%の濃度で含有させることができる。 In the oil-in-water emulsion of the present invention, the water-swellable clay mineral is preferably at a concentration of about 1 to about 20% by weight, more preferably about 3 to about 1% by weight, based on the total weight of the obtained emulsion. It can be contained at a concentration of 5% by weight.
本発明に係る水中油型エマルションにおいて含有せしめることができる親水 性顔料及び/又はフィラーは、 化粧品及び皮膚科学の分野で従来から使用され ているものもしくは使用可能なものであれば如何なるものでも構わず、 例えば 体質顔料、 着色顔料、 白色顔料のような無機顔料、 有機顔料、 真珠光沢顔料、 高分子粉体、 機能性顔料等々を挙げることができる。 親水性顔料及び/又はフ ィラ一は、 未処理の状態で親水性の顔料及び/又はフィラーであってもよいし、 親水性の表面処理を施した顔料及び/又はフィラーであってもよい。 The hydrophilic pigment and / or filler that can be contained in the oil-in-water emulsion according to the present invention may be any of those conventionally used or usable in the field of cosmetics and dermatology. Examples thereof include extender pigments, coloring pigments, inorganic pigments such as white pigments, organic pigments, pearlescent pigments, polymer powders, and functional pigments. Hydrophilic pigment and / or The filler may be an untreated hydrophilic pigment and / or filler, or may be a hydrophilic surface-treated pigment and / or filler.
具体的には、 タルク、 非膨潤性マイ力、 カオリン、 炭酸カルシウム、 炭酸マ グネシゥム、 無水ケィ酸、 ケィ酸アルミニウム、 ケィ酸マグネシウム、 ケィ酸 カルシウム、 酸化アルミニウム、 硫酸バリウム、 ベンガラ、 黄酸化鉄、 黒酸化 鉄、 酸化クロム、 グンジヨウ、 コンジヨウ、 カーボンブラック、 酸化チタン (ァ モルファス又はルチル型及び/又はアナ夕一ゼ型結晶)、 酸化亜鉛、 雲母チタ ン、 魚鱗箔、 ォキシ塩化ビスマス、 窒化ホウ素、 シルクパウダー、 天然色素等 々を例示することができ、 これらの顔料及び/又はフイラ一は、 1種又は複数 の種類を組み合わせて使用される。  More specifically, talc, non-swelling mai force, kaolin, calcium carbonate, magnesium carbonate, calcium anhydride, aluminum silicate, magnesium silicate, calcium silicate, aluminum oxide, barium sulfate, bengara, yellow iron oxide, Black iron oxide, chromium oxide, gunjiyou, konjiyo, carbon black, titanium oxide (amorphous or rutile and / or anamorphic type crystals), zinc oxide, mica titan, fish scale foil, bismuth oxychloride, boron nitride, Examples thereof include silk powder, natural pigments, and the like. These pigments and / or fillers are used alone or in combination of two or more.
未処理の顔料及び/又はフィラーが使用される場合、 特にメークアップ化粧 料に配合することが望まれる場合には、 顔料及び/又はフィラーは比較的大な る平均粒子径を有するものが選択され、 好ましくは 0 . 1 11 から 5 0 / 111の 平均粒子径、 より好ましくは 0 . 1 mから 3 0 / mの平均粒子径、 さらによ り好ましくは 0 . 1 mから 2 0 / mの平均粒子径を有するものである。  When untreated pigments and / or fillers are used, especially when it is desired to incorporate them into make-up cosmetics, pigments and / or fillers with relatively large average particle sizes are selected. Preferably from 0.111 to 50/111 average particle size, more preferably from 0.1 m to 30 / m average particle size, even more preferably from 0.1 m to 20 / m average particle size. It has a particle diameter.
また、 親水性表面処理を施した顔料及び/又はフィラーの場合は、 処理剤と しては、 従来から顔料及び/又はフィラーに親水性を付与するために使用され ているものであれば、 如何なるものでも使用することができるが、 例えばシリ 力処理、 アルミナ処理、 シリカアルミナ処理、 チタニア処理のような処理剤に よる表面処理を施した粉体を用いることもできる。 本発明においては、 特にシ リ力処理が好適に選択され、 また処理法自体は当該技術分野において周知のも のである。  In the case of a pigment and / or filler having been subjected to a hydrophilic surface treatment, any treating agent may be used as long as it is conventionally used for imparting hydrophilicity to the pigment and / or filler. Although a powder can be used, a powder that has been subjected to a surface treatment with a treating agent such as a silica treatment, an alumina treatment, a silica-alumina treatment, or a titania treatment can also be used. In the present invention, in particular, resilient treatment is suitably selected, and the treatment method itself is well known in the art.
本発明に係る水中油型エマルシヨンに含有される上記親水性顔料及び/又は フイラ一は、 エマルシヨン中に好ましくは 0 . 1〜 3 0重量%、 更に好ましく は 0 . 5〜 1 0重量%の含有量で含まれる。  The hydrophilic pigment and / or filler contained in the oil-in-water emulsion according to the present invention preferably contains 0.1 to 30% by weight, more preferably 0.5 to 10% by weight in the emulsion. Included in quantity.
なお、 本発明に係る水中油型エマルションに含まれる顔料及び/又はフィラ 一は、 基本的には前述の親水性顔料及び/又はフィラーであるが、 本発明の水 中油型エマルションの顔料及び/又はフィラ一分散性、 均一性等の効果が維持 される範囲であれば、 疎水性処理の顔料及び/又はフィラーを含有させても構 わない。 水中油型エマルション中に含有可能なこの疎水性処理の顔料及び/又 はフイラ一の量は、 好ましくはせいぜい約 5重量%以下、 より好ましくは約 3 重量%である。 The pigment and / or filler contained in the oil-in-water emulsion according to the present invention is basically the above-described hydrophilic pigment and / or filler, but the pigment and / or filler of the oil-in-water emulsion according to the present invention. Maintain effects such as filler dispersibility and uniformity As long as it is within the range, a pigment and / or a filler for hydrophobic treatment may be contained. The amount of pigment and / or filler of this hydrophobic treatment that can be contained in the oil-in-water emulsion is preferably at most about 5% by weight, more preferably about 3% by weight.
また、 本発明において用いられる界面活性剤は、 この種の水中油型エマルシ ョンの乳化に従来から使用されているものであれば、 如何なるものでも使用す ることができるが、 前述のように、 その使用量は、 低く抑えられる。 使用され うる界面活性剤としては、 例えば、 ポリオキシエチレンアルキルエーテル、 ポ リオキシエチレン脂肪酸エステル、 ポリオキシエチレンソルビタン脂肪酸エス テル、 グリセリン脂肪酸エステル、 ポリグリセリン脂肪酸エステル.、 ポリオキ シエチレングリセリン脂肪酸エステル、 ポリオキシエチレン硬化ヒマシ油、 ポ リオキシエチレンソルビトール脂肪酸エステル等の非イオン性界面活性剤 ; ス テアリン酸ナト リウム、 パルミチン酸ト リエタノールァミン等の脂肪酸石験で 代表されるァニオン性界面活性剤等が挙げられる。 特に好適に使用できる界面 活性剤は、 ステアリン酸と Uniqema社製の Arlacel 165FL (ステアリン酸グリセ リル 5 0 % +ステアリン酸 PEG-100 5 0 % ) とセ夕ノールの組み合わせが挙げ られる。  As the surfactant used in the present invention, any surfactant can be used as long as it has been conventionally used for emulsification of this type of oil-in-water emulsion. However, its usage is kept low. Examples of the surfactant that can be used include polyoxyethylene alkyl ether, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester., Polyoxyethylene glycerin fatty acid ester, and polyoxyethylene glycerin fatty acid ester. Nonionic surfactants such as oxyethylene hydrogenated castor oil and polyoxyethylene sorbitol fatty acid ester; Anionic surfactants such as sodium stearate and triethanolamine palmitate represented by fatty acid lithography Is mentioned. Particularly preferred surfactants include a combination of stearic acid and Arlacel 165FL (50% glyceryl stearate + 50% PEG-100 stearic acid) manufactured by Uniqema and Sesolanol.
本発明に係る水中油型エマルシヨンの脂肪相は、 液体油に限らず、 固形脂又 は半固形油等を含むあらゆる非水性物質又は非水性物質の混合物の相を意味す る。 脂肪相を構成する非水性物質、 すなわち油は、 水中油型エマルシヨンの調 製において従来から使用されているものであれば、 植物性、 鉱物性、 動物性及 び/又は合成油等、 如何なるものでもよい。 例えば、 アポガド油、 ォリーブ油、 ホホバ油、 ォレイン酸、 イソステアリン酸、 へキサデシルアルコール、 ォレイ ルアルコール、 2—ェチルへキサン酸セチル、 パルミチン酸— 2—ェチルへキ シル、 ミ リスチン酸— 2—ォクチルドデシル、 ジ— 2—ェチルへキサン酸ネオ ペンチルグリコール、 ト リ一 2—ェチルへキサン酸グリセロール、 ォレイ ン酸 — 2—才クチルドデシル、 ミ リスチン酸イソプロピル、 ト リイソステアリン酸 グリセロール、 2—ェチルへキサン酸ジグリセリ ド、 ジ一パラメ トキシケィ ヒ 酸一モノー 2—ェチルへキサン酸グリセリル、 ジメチルポリシロキサン、 メチ ルハイ ドロジエンポリシロキサン、 メチルフエ二ルポリシロキサン、 ォクタメ チルシクロテトラシロキサン、 流動パラフィン、 スクワレン、 スクヮラン、 ヮ セリン、 ラノ リン、 セレシン、 マイクロクリスタリンワックス、 カルナバロゥ、 キャンデリラロウなどが挙げられ、 1種又は 2種以上を混合して用いることが できる。好ましくは、 シクロメチコーン 5重量%+ トリ(力プリル . 力プリン酸) グリセリン 5重量%の組み合わせが使用される。 本発明においては、 脂肪相の 量を、 エマルシヨンの全重量に対して好ましくは約 5〜 2 0重量%、 より好ま しくは約?〜 1 5重量%とするのが好適である。 脂肪相の量が少なすぎると、 化粧料に用いた場合に、 化粧仕上がりが非常に乾燥しやすく、 顔料及び/又は フィラーのつきがムラになりやすくなったり、 快適なしっとり感が得られず、 肌が乾いた状態になってしまう。 一方、 脂肪相の量が多すぎると、 肌なじみが 悪くなつたり、 油性感が出過ぎて重い感触になったり、 安定性そのものにも悪 影響を与える。 The fatty phase of the oil-in-water emulsion according to the present invention means not only a liquid oil but also a phase of any non-aqueous substance or a mixture of non-aqueous substances including a solid fat or a semi-solid oil. The non-aqueous substance constituting the fatty phase, i.e., the oil, may be any of vegetable, mineral, animal and / or synthetic oils as long as it has been conventionally used in the preparation of an oil-in-water emulsion. May be. For example, apogado oil, olive oil, jojoba oil, oleic acid, isostearic acid, hexadecyl alcohol, oleyl alcohol, cetyl 2-ethylhexanoate, 2-ethylhexyl palmitate, myristate-2 Octyldodecyl, neopentylglycol di-2-ethylhexanoate, glycerol tri-2-ethylhexanoate, oleic acid-2-octyldodecyl, isopropyl myristate, glycerol triisostearate, 2-ethylhexane Acid diglyceride, di-paramethoxy carboxylic acid Glyceryl mono-2-ethylhexanoate dimethylpolysiloxane, dimethylpolysiloxane, methylphenylpolysiloxane, octamethylcyclotetrasiloxane, liquid paraffin, squalene, squalane, glycine, lanolin, ceresin, micro Crystallin wax, carnavalo, candelilla wax and the like can be mentioned, and one kind or a mixture of two or more kinds can be used. Preferably, a combination of 5% by weight of cyclomethicone + 5% by weight of tri (force prill. Force pric acid) glycerin is used. In the present invention, the amount of fatty phase is preferably about 5 to 20% by weight, more preferably about 5% by weight, based on the total weight of the emulsion. It is preferable that the content be 15 to 15% by weight. If the amount of the fatty phase is too small, when used in cosmetics, the makeup finish is very easy to dry, pigments and / or fillers tend to be uneven, and a comfortable moist feeling cannot be obtained. Your skin will be dry. On the other hand, if the amount of the fatty phase is too large, the skin will not fit well, the oily feeling will be too heavy and the feeling will be heavy, and the stability itself will be adversely affected.
一方、 水相は、 好ましくは精製水等の水からなるが、 場合によっては、 C 2-On the other hand, the aqueous phase preferably consists of water such as purified water, but in some cases, C 2-
C 6低級モノアルコール及び/又はポリオ一ル、 例えばグリセロール、 ブチレン グリコール、 イソプレングリコール又はプロピレングリコールを (エマルショ ンの全重量に対して 0〜 1 5重量%) 含有することもできる。 該水相は、 エマ ルシヨンの全重量に対して、 好ましくは約 3 5〜 9 5重量%、 より好ましくは 約 4 0〜 8 0重量%である。 It may also contain C6 lower monoalcohols and / or polyols, for example glycerol, butylene glycol, isoprene glycol or propylene glycol (0 to 15% by weight relative to the total weight of the emulsion). The aqueous phase is preferably about 35-95% by weight, more preferably about 40-80% by weight, based on the total weight of the emulsion.
更に、 本発明においては、 水膨潤性粘土鉱物を増粘剤として使用しているが、 本発明の効果を損なわない範囲で、 通常の親水性増粘剤、 例えばカボキシビニ ルポリマ一、 アクリルコポリマー、 ポリアクリルアミ ド、 多糖類、 天然ガム等 を加えることも許される。 また、 場合によっては、 脂肪相に親油性増粘剤を加 えることも可能であり、 このような増粘剤としては、 ベン トーンなどの変性粘 土、 ステアリン酸アルミニウムのような脂肪酸金属塩、 疎水性シリカ、 ェチル セルロース、 ポリエチレン等を挙げることができる。  Further, in the present invention, a water-swellable clay mineral is used as a thickening agent. However, as long as the effects of the present invention are not impaired, ordinary hydrophilic thickening agents such as carboxyvinyl polymer, acrylic copolymer, Acrylamide, polysaccharides, natural gums, etc. may be added. In some cases, it is also possible to add a lipophilic thickener to the fatty phase, such as a modified clay such as bentone, a fatty acid metal salt such as aluminum stearate, or the like. Examples thereof include hydrophobic silica, ethyl cellulose, and polyethylene.
本発明の水中油型エマルションは、 好適には化粧料又は皮膚外用剤として使 用される。 すなわち、 本発明の一実施形態では、 上記水中油型エマルシヨンか らなる又は上記水中油型エマルシヨンを含有する化粧料又は皮膚外用剤が提供 される。 The oil-in-water emulsion of the present invention is preferably used as a cosmetic or a skin external preparation. Used. That is, in one embodiment of the present invention, there is provided a cosmetic or external preparation for skin consisting of the oil-in-water emulsion or containing the oil-in-water emulsion.
上記化粧料は、 如何なる用途のものでも構わないが、 特にメークアップ、 ス キンケア、 毛髪ケア用の化粧料が好適に提供される。 メークアップ化粧料は、 顔、 唇、 目等の部分のボディの皮膚のメークアップのものでも、 爪、 髪等の皮 膚骨格のメークアップのものでもよい。 更に具体的には、 ファンデーション、 唇製品、 ブラッシャー、 アイシャ ドー、 コンシ一ラー等々の形態をとりうる。 上記化粧料又は皮膚外用剤は、 化粧品又は皮膚外用製品に含有せしめられる 通常の活性成分等の添加剤を含有することができる。 かかる添加剤としては、 特に、 有機溶媒、 柔軟剤、 酸化防止剤、 抗フ リーラジカル剤、 不透明化剤、 安 定剤、 ェモリエント、 消泡剤、 保湿剤、 ビタミン類、 香料、 防腐剤、 金属ィォ ン封鎖剤、 ポリマー類、 塩基性又は酸性化剤、 染料、 自己サンタン剤、 更には 化粧品及び/又は皮膚科学の分野で通常使用されている任意の他の成分から選 択される従来の化粧品用及び/又は皮膚科学用アジュバントが挙げられる。 各 成分はそれぞれの相容性等に応じて水相又は脂肪相に含有せしめられる。  The cosmetic may be of any use, but cosmetics for make-up, skin care, and hair care are particularly preferably provided. The makeup cosmetic may be a makeup of the skin of the body such as the face, lips, and eyes, or a makeup of the skin skeleton such as nails and hair. More specifically, it can take the form of a foundation, lip product, brusher, eye shadow, concealer, and the like. The cosmetic or external preparation for skin may contain additives such as ordinary active ingredients to be contained in cosmetics or external products for skin. Such additives include, in particular, organic solvents, softeners, antioxidants, antifree radical agents, opacifiers, stabilizers, emollients, defoamers, humectants, vitamins, fragrances, preservatives, metals Conventional sequestering agents selected from ion sequestering agents, polymers, basic or acidifying agents, dyes, self-tanning agents, and any other ingredients commonly used in the cosmetic and / or dermatological fields. Cosmetic and / or dermatological adjuvants. Each component is contained in an aqueous phase or a fatty phase depending on the compatibility or the like.
このような任意に添加される成分の種類及び/又は量は、 当業者であれば本 発明の水中油型エマルションに固有の有利な特性に悪影響を及ぼさないように 留意して選択することができるものである。 実施例  The type and / or amount of such optional ingredients may be selected by those skilled in the art with care not to adversely affect the beneficial properties inherent in the oil-in-water emulsions of the present invention. Things. Example
以下、 本発明を実施例により更に詳細に説明するが、 本発明はこれちにより 限定されるものではないことは言うまでもない。 なお、 以下の表記において、 %は、 それ以外の定義を特記しない限り、 重量%を指す。 実施例 1  Hereinafter, the present invention will be described in more detail with reference to Examples, but it goes without saying that the present invention is not limited thereto. In the following notation,% indicates% by weight, unless otherwise specified. Example 1
本発明に係る水中油型エマルシヨンに使用する水膨潤性粘土鉱物と親水性顔 料及び/又はフィラーの組み合せの効果を確認するために、 水相と脂肪相と少 量の界面活性剤を混合して乳化物とし、 次に水膨潤性粘土鉱物 (ワツケール社 の Submica E ) を水に膨潤させたものを添加し (以降、 「合成マイカジエル」 と いう)、 表面未処理顔料又は親水性表面処理顔料を混合して分散させた本発明 の水中油型エマルシヨン (本発明例 1及び 2 ) を調製すると共に、 その顔料を 疎水性表面処理顔料に置換した水中油型エマルシヨン (比較例 1 ) を調製し、 エマルシヨンの性状、 顔料の分散性、 安定性を比較した。 また、 参考に、 合成 マイカジエルと表面未処理顔料を含むジエル (比較例 2 )、 合成マイカジヱル と親水性表面処理顔料を含むジヱル (比較例 3 )、 合成マイカジエルと疎水性 表面処理顔料を含むジエル (比較例 4 )、 更には界面活性剤を用いないで合成 マイカジエルと表面未処理顔料を含有させた水中油型エマルション (比較例 5 )、 界面活性剤を用いないで合成マイカジエルと疎水性表面処理顔料を含有 させた水中油型エマルシヨン (比較例 6 ) を調製し、 同様に性状、 感触を調べ た。 In order to confirm the effect of the combination of the water-swellable clay mineral and the hydrophilic pigment and / or filler used in the oil-in-water emulsion according to the present invention, a water phase, a fatty phase and a Of a water-swellable clay mineral (Submica E from Wakkale) in water (hereinafter referred to as “synthetic mykadiel”). Oil-in-water emulsions of the present invention (Examples 1 and 2 of the present invention) prepared by mixing and dispersing treated pigments or hydrophilic surface-treated pigments, and replacing the pigments with hydrophobic surface-treated pigments (Comparative Example 1) was prepared, and the properties of the emulsion, the dispersibility of the pigment, and the stability were compared. For reference, a synthetic mica diel and a diel containing a surface-untreated pigment (Comparative Example 2), a synthetic mica diel and a diel containing a hydrophilic surface-treated pigment (Comparative Example 3), and a synthetic mica diel and a diel containing a hydrophobic surface-treated pigment (Comparative Example 2) Comparative Example 4), Further, Synthesis without Using Surfactant Oil-in-Water Emulsion Containing Mica Diel and Surface Untreated Pigment (Comparative Example 5), Synthetic Mica Diel without Using Surfactant and Hydrophobic Surface-treated Pigment An oil-in-water emulsion (Comparative Example 6) containing the same was prepared, and its properties and feel were similarly examined.
また、 安定性は 4 5 °Cで 2ヶ月間保存して調べた。  The stability was examined after storage at 45 ° C for 2 months.
上記試験の結果を次表に示す。  The results of the above test are shown in the following table.
訂正された用紙 (規則 91) 本発明例 本 5§明例 比較例 比較例 比較 例 比較例 比較例 比 較例 Corrected form (Rule 91) Example of the present invention Example of this 5th example Comparative example Comparative example Comparative example Comparative example Comparative example Comparative example Comparative example
1 2 1 2 3 4 5 6 水相  1 2 1 2 3 4 5 6 Water phase
-精製水 20% 20% 20%  -Purified water 20% 20% 20%
-防腐剤 少量 少量 少量  -Preservatives small amount small amount small amount
界面活性剤  Surfactant
-ステアリン酸グリセリ /レ 50% 0.3% 0.3% 0.3%  -Glyceryl stearate / le 50% 0.3% 0.3% 0.3%
+ステアリン酸 PEG- 100 50%  + PEG-100 stearic acid 50%
(注 1 )  (Note 1)
-ステアリン酸 0. 6% 0.6% 0.6%  -Stearic acid 0.6% 0.6% 0.6%
-セタノ一ノレ 0. 5% 0. 5% 0.5%  -Setano 0.5% 0.5% 0.5%
脂肪相  Fatty phase
-デカメチルシクロペンタシ 5% 5% 5% 5% 5% ロキサン  -Decamethylcyclopentane 5% 5% 5% 5% 5% Loxane
-ト リ(カプリル カプリン 5% 5% 5% 5% 5% 酸)グリセリ ド  -Triglyceride (capryl caprin 5% 5% 5% 5% 5% acid)
合成マイ力相  Synthetic My Power Phase
-水 計 100% 計 100% 計 100% 計 100% 計 100% 計 100% 計 100% 計 100% -Water Total 100% Total 100% Total 100% Total 100% Total 100% Total 100% Total 100% Total 100%
-ナトリ ゥム及びマグネシゥ 7 % 7% 7% 10% 10% 10% 10% 10% -Natrium and magnesium 7% 7% 7% 10% 10% 10% 10% 10%
2)  2)
ムのフルォロシリケート  Fluorosilicate
表面未処理顔料  Untreated surface pigment
-未処理酸化鉄 1. 42% 1. 66% 1.42%  -Untreated iron oxide 1.42% 1.66% 1.42%
-术処理—酸 ίヒ タン 5. 58% 8. 34%  -术 Treatment-Acid-Hydrogen 5.58% 8.34%
親水性表面処理顔料  Hydrophilic surface-treated pigment
-シリカ処理酸化鉄 1. 42% 1 66%  -Silica treated iron oxide 1.42% 1 66%
-ンリ力処理一酸ィ匕チタ 5. 58% 8. 34%  -Non-strengthening treatment Ichidani Tita 5.58% 8. 34%
水性表囬処 顔料  Aqueous surface treatment pigment
•C9-15 フルォロアルコール 1. 42% 1. 66% 1. 42% リン酸処理酸化鉄  • C9-15 Fluoroalcohol 1.42% 1.66% 1.42% Phosphated iron oxide
•C9-15 フノレオ口アルコール 5. 58% 8.34% 5. 58% リン酸処理二酸化チタン  • C9-15 phenolic mouth alcohol 5.58% 8.34% 5.58% Phosphated titanium dioxide
性状 ·感触 均一、 良 均一、 良 顔料が均 均 ― 、 均 ― 、 顔料 が 顔料が均 顔料 が 好な感触 好な感触 一分散せ キ シ キ キ シ キ 均 一分 一分散 均 一分 ず シ し 、 シ し 、 散せず せず 散せず 乾燥 乾燥  Properties / Touch uniformity, good uniformity, good Pigment is average-, average-, pigment is even pigment is good pigment is good feel good feel is dispersed. Dry, dry, dry, dry, dry
安定性 良好 良好 不安定 良好 良好 不安定 不安定 不安定 Stability Good Good Unstable Good Good Unstable Unstable Unstable
(注 1 ) Arlacel 165FL( UNIQEMA社製) (Note 1) Arlacel 165FL (manufactured by UNIQEMA)
(注 2 ) Submica E ( Wackherr社製) (Note 2) Submica E (Wackherr)
訂正された用紙 (規則 91) 13 Corrected form (Rule 91) 13
Figure imgf000015_0001
Figure imgf000015_0001
(注 1 ) Arlacel 165Fし ( UNIQEMA社製)  (Note 1) Arlacel 165F (made by UNIQEMA)
(注 2 ) Submica E ( VVackherr社製) - 14 - 上記の表に示された結果から、 本発明における親水性顔料と水膨潤性粘土鉱 物の組み合わせにより得られた水中油型エマルションが、 他の組み合せによる 水中油型エマルシヨン又はジエルと比較して、 顔料の分散性と安定性、 感触等 の使用性、 マッ ト感において優れていることが分かる。 (Note 2) Submica E (VVackherr) -14-Based on the results shown in the above table, the oil-in-water emulsion obtained by the combination of the hydrophilic pigment and the water-swellable clay mineral of the present invention is compared with the oil-in-water emulsion or giel of other combinations. As a result, it was found that the pigment was excellent in dispersibility and stability, usability such as feel, and matte feeling.
実施例 2 Example 2
[フアンデ一ション]  [Foundation]
水相 A及び (B + C) 相を 6 0°Cで完全溶解させる。 タービン型ホモジナイ ザ一撹拌下で、 A相に (B + C) 相を添加し、 乳化を行う。 室温にてあらかじ め水に S UBM I CA Eを膨張させ均一分散させておいた D相を加える。 さら に顔料 E相を加え、 最終混合物を均一撹拌した。 フ ϊ一、ン =? V Completely dissolve aqueous phase A and (B + C) phase at 60 ° C. Add the (B + C) phase to the A phase under stirring with a turbine homogenizer, and emulsify. At room temperature, add the D phase in which SUBM I CAE has been swollen and dispersed uniformly in water. Further, the pigment E phase was added, and the final mixture was stirred uniformly. Off ϊ one, down =? V
A 水相  A water phase
-精製水 20%  -Purified water 20%
-防腐剤 少量  -Preservative small amount
B 界面活性剤  B surfactant
-ステアリン酸グリセリル 50% +ステアリン酸 PEG-10050%: 0. 3% -Glyceryl stearate 50% + PEG-100 stearate 50%: 0.3%
Arlacel 165FL (UNIQEMA社製) Arlacel 165FL (manufactured by UNIQEMA)
-ステアリン酸 0. 6% -0.6% stearic acid
-セ夕ノール 0. 5%-0.5%
C 脂肪相 C fatty phase
-デカメチノレシクロペン夕シロキサン 5%  -5% of decamethinolecyclopene siloxane
-トリ(力プリル/力プリン酸)ダリセリ ド 5%  -Tori (force prill / force protic acid) dariseride 5%
D 合成マイ力相  D Synthetic My Power Phase
-精製水 100%にする量 -Amount to make purified water 100%
-ナ卜リウム及びマグネシウムのフルォロシリケィ ト: 7% -Fluorosilicate of sodium and magnesium: 7%
Submica E (Wackherr社製)  Submica E (Wackherr)
E 表面未処理顔料  E Untreated surface pigment
-黄酸化鉄 0. 97% -Yellow iron oxide 0.97%
-黒酸化鉄 0. 09%-Black iron oxide 0.09%
-ベンガラ 0. 11 %-Bengala 0.11%
-酸化チタン (顔料級) 5. 83% 15 - 均一な性状で、 良好な感触のファンデーシヨンが得られた 乳液] -Titanium oxide (pigment grade) 5. 83% 15-Emulsion with uniform properties and good-feel foundation]
水相 A及び (B + C) 相を 60°Cで完全溶解させる。 タービン型ホモジナイ ザ一撹拌下で、 A相に (B + C) 相を添加し、 乳化を行う。 室温にてあらかじ め水に SUBMI CA Eを膨張させ均一分散させておいた D相を加える。 さら に顔料 E相を加え、 最終混合物を均一撹拌した。  Completely dissolve the aqueous phase A and (B + C) phase at 60 ° C. Add the (B + C) phase to the A phase under stirring with a turbine homogenizer, and emulsify. At room temperature, add SUBMI CA E to the water in advance by expanding and uniformly dispersing the SUBMI CA E in water. Further, the pigment E phase was added, and the final mixture was stirred uniformly.
Figure imgf000017_0001
油性感のない、 非常にさっぱりとした、 ベたつきのない乳液を得た。 安定性 は非常に良い。
Figure imgf000017_0001
A very light, non-greasy emulsion without an oily feeling was obtained. Stability is very good.
[スキンケアクリーム又はメーキヤップ下地クリーム] [Skin care cream or makeup base cream]
水相 A及び (B + C) 相を 60°Cで完全溶解させる。 夕一ビン型ホモジナイ - 16 - ザ一撹拌下で、 A相に (B + C ) 相を添加し、 乳化を行う。 室温にてあらかじ め水にモンモリロナイ トを膨張させ均一分散させておいた D相を加える。 さら に顔料 E相及び F相を加え、 最終混合物を均一撹拌した。 Completely dissolve the aqueous phase A and (B + C) phase at 60 ° C. Evening bottle type homogenizer -16-Add the (B + C) phase to the A phase under stirring, and emulsify. At room temperature, montmorillonite is swelled in water in advance, and the D phase that has been uniformly dispersed is added. Further, the pigment phase E and phase F were added, and the final mixture was stirred uniformly.
Figure imgf000018_0001
油性感のない、 非常にさっぱりとした、 ベたつきのないクリームを得た。 安 定性は非常に良い。 肌表面をなめらかに整えるので、 ファンデーショ ンの下地 クリームとしても使える。 [ク リーム状ほほ紅]
Figure imgf000018_0001
A very light, non-greasy cream with no oiliness was obtained. The stability is very good. It can be used as a foundation cream for foundations because it smoothes the skin surface. [Cream-like blush]
水相 A及び ( B + C ) 相を 6 0 °Cで完全溶解させる。 タービン型ホモジナイ ザ一撹拌下で、 A相に (B + C ) 相を添加し、 乳化を行う。 顕微鏡で乳化の確 認の後、 室温にてあらかじめ水に S U B M I C A Eを膨張させ均一分散させて - 17 - おいた D相を加える。 さらに顔料 E相を加え、 最終混合物を均一撹拌した, Dissolve the aqueous phase A and the (B + C) phase completely at 60 ° C. Add the (B + C) phase to the A phase and emulsify under agitating with a turbine homogenizer. After confirming the emulsification with a microscope, expand SUBMICAE in water at room temperature and disperse it uniformly. -17-Add D phase. Further, the pigment E phase was added, and the final mixture was stirred uniformly.
Figure imgf000019_0001
油性感のない、 非常にさっぱりとした、 ベたつきのないクリーム状ほほ紅を 得た。 しクリーム状アイシャ ドウ]
Figure imgf000019_0001
A very refreshing, non-greasy creamy blusher with no oiliness was obtained. Creamy aisha dough]
水相 A及び (B + C) 相を 60°Cで完全溶解させる。 夕一ビン型ホモジナイ ザ一撹拌下で、 A相に (B + C) 相を添加し、 乳化を行う。 室温にてあらかじ め水に SUBMI CA Eを膨張させ均一分散させておいた D相を加える。 さら に顔料 E相を加え、 最終混合物を均一撹拌した。 18 Completely dissolve the aqueous phase A and (B + C) phase at 60 ° C. Add the (B + C) phase to the A phase and emulsify the mixture with stirring in the evening bottle homogenizer. At room temperature, add SUBMI CA E to the water in advance by expanding and uniformly dispersing the SUBMI CA E in water. Further, the pigment E phase was added, and the final mixture was stirred uniformly. 18
Figure imgf000020_0001
油性感のない、 非常にさっぱりとした、 ベたつきのないクリーム状アイシャ ドウを得た。
Figure imgf000020_0001
A very light, non-greasy, creamy eyeshadow with no oiliness was obtained.
[クレンジングク リーム] [Cleansing cream]
水相 A及び (B + C) 相を 60°Cで完全溶解させる。 夕一ビン型ホモジナイ ザ一撹拌下で、 A相に (B + C) 相を添加し、 乳化を行う。 室温にてあらかじ め水に SUBMI CA Eを膨張させ均一分散させておいた D相を加える。 さら に顔料 E相を加え、 最終混合物を均一撹拌した。 19 Completely dissolve the aqueous phase A and (B + C) phase at 60 ° C. Add the (B + C) phase to the A phase and emulsify the mixture with stirring in the evening bottle homogenizer. At room temperature, add SUBMI CA E to the water in advance by expanding and uniformly dispersing the SUBMI CA E in water. Further, the pigment E phase was added, and the final mixture was stirred uniformly. 19
Figure imgf000021_0001
使用方法 :適量を肌に伸ばし、 汚れやメークアップと良くなじませた後、 ふき 取るか、 水で洗い流す。
Figure imgf000021_0001
Directions for use: Apply an appropriate amount to the skin, mix well with dirt and make-up, then wipe off or rinse off with water.
肌に伸ばし易く、 メークアップとのなじみも良い。 洗い流した後の肌は、 油 性感の無い、 非常にさっぱりとした、 ベたつきのない感触であった。  Easily spreads on the skin and blends well with makeup. After rinsing, the skin had a very light, non-greasy feel with no oiliness.
[洗い流しフヱイスパック] [Rinse face pack]
水相 A及び (B + C) 相を 60 °Cで完全溶解させる。 タービン型ホモジナイ ザ一撹拌下で、 A相に (B + C) 相を添加し、 乳化を行う。 顕微鏡で乳化の確 認の後、 室温にてあらかじめ水に SUBMI CA Eを膨張させ均一分散させて おいた D相を加える。 さらに顔料 E相を加え、 最終混合物を均一撹拌した。 - 20 - Completely dissolve aqueous phase A and (B + C) phase at 60 ° C. Add the (B + C) phase to the A phase under stirring with a turbine homogenizer, and emulsify. After confirming the emulsification with a microscope, add SUBMI CAE to the water in advance at room temperature. Further, phase E of pigment was added, and the final mixture was stirred uniformly. -20-
Figure imgf000022_0001
使用方法 : 適量を肌にのばし、 5〜 1 5分放置した後、 ふき取るか、 水で洗い 流す。
Figure imgf000022_0001
Directions for use: Spread an appropriate amount on skin, leave for 5 to 15 minutes, and then wipe off or rinse with water.
油性感がなく、 肌にのばしやすい。 洗い流した後、 肌はしつとりとし、 油性 感を残さないさっぱりとした感触であった。  It has no oiliness and is easy to spread on the skin. After rinsing, the skin became moist, and had a refreshing feel without leaving any oily feeling.

Claims

- 21 - 請求の範囲 -21-Claims
1 . 脂肪相と水相と界面活性剤とを含有する水中油型エマルシヨンにおいて、 水膨潤性粘土鉱物を、 親水性顔料及び/又はフィラーと共に含有せしめて、 界 面活性剤の量を 5 %以下にしたことを特徴とする水中油型エマルシヨン。 1. In an oil-in-water emulsion containing a fatty phase, an aqueous phase, and a surfactant, a water-swellable clay mineral is added together with a hydrophilic pigment and / or filler to reduce the amount of surfactant to 5% or less. An oil-in-water emulsion characterized in that:
2 . 界面活性剤の量を 1〜 3重量%、 好ましくは 0 . 1〜 2重量%としたこ とを特徴とする請求項 1に記載の水中油型エマルシヨン。 2. The oil-in-water emulsion according to claim 1, wherein the amount of the surfactant is 1 to 3% by weight, preferably 0.1 to 2% by weight.
3 . 水膨潤性粘土鉱物が層状ケィ酸塩鉱物である請求項 1又は 2に記載の水 中油型エマルション。 3. The oil-in-water emulsion according to claim 1, wherein the water-swellable clay mineral is a layered silicate mineral.
4 . 層状ケィ酸塩鉱物が、 モンモリロナイ ト、 パイデライ ト、 ノントロナイ ト、 サボナイ ト、 ヘク トライ ト、 ソーコナイ ト、 スチブンサイ ト、 合成スメク タイ ト、 合成マイ力からなる群から選択されることを特徴とする請求項 3に記 載の水中油型エマルション。 4. The layered silicate mineral is selected from the group consisting of montmorillonite, paiderite, nontronite, savonite, hectolite, sauconite, stevensite, synthetic smectite, and synthetic mylite. 4. The oil-in-water emulsion according to claim 3, wherein the oil-in-water emulsion is used.
5 . 合成マイ力が、 次の示性式 : 5. The synthetic my power has the following analytic formula:
( N a 2 O ) X (M g O ) y ( S i O 2 ) z M g F 2 (N a 2 O) X ( M g O) y (S i O 2) z M g F 2
[上式中、 X、 y、 Zは、 次の関係を満たす数である : [Where X, y, and Z are numbers that satisfy the following relationship:
0 . 1≤x≤ 0 . 5  0 .1≤x≤ 0.5
1 . 5≤y≤ 2  1.5 ≤ y ≤ 2
3 . 5≤ z≤ 4 ]  3.5 ≤ z≤ 4]
により表されるマイ力であることを特徴とする請求項 4に記載の水中油型エマ ルシヨン。 5. The oil-in-water emulsion according to claim 4, wherein the oil-in-water type emulsification is represented by:
6 . 水膨潤性粘土鉱物が、 エマルシヨ ンの全重量に対して 1〜 2 0重量%、 好ましくは 3〜 1 5重量%の濃度で存在することを特徴とする請求項 1ないし - 22 -6. The water-swellable clay mineral is present in a concentration of 1 to 20% by weight, preferably 3 to 15% by weight, based on the total weight of the emulsion. - twenty two -
5に記載の水中油型エマルション。 5. The oil-in-water emulsion according to 5.
7 . 親水性顔料及び/又はフイラ一が、 未処理顔料及び/又はフイラ一であ ることを特徴とする請求項 1ないし 6の何れか 1項に記載の水中油型エマルシ ヨン。 7. The oil-in-water emulsion according to any one of claims 1 to 6, wherein the hydrophilic pigment and / or the filler is an untreated pigment and / or a filler.
8 . 未処理顔料及び/又はフィラーが、 0 . 1〃mから 5〃mの平均粒子径 を有するものであることを特徴とする請求項 7に記載の水中油型エマルシヨン。 8. The oil-in-water emulsion according to claim 7, wherein the untreated pigment and / or filler has an average particle size of 0.1 to 5 μm.
9 . 親水性顔料及び/又はフィラーが、 親水性表面処理顔料及び/又はフィ ラーであることを特徴とする請求項 1ないし 6の何れか 1項に記載の水中油型 エマルシヨン。 9. The oil-in-water emulsion according to any one of claims 1 to 6, wherein the hydrophilic pigment and / or filler is a hydrophilic surface-treated pigment and / or filler.
1 0 . 親水性顔料及び/又はフイラ一が、 シリカにより表面処理がなされた ものであることを特徴とする請求項 9に記載の水中油型エマルシヨン。 10. The oil-in-water emulsion according to claim 9, wherein the hydrophilic pigment and / or the filler is surface-treated with silica.
1 1 . 親水性顔料及び/又はフイラ一が、 エマルシヨンの全重量に対して 1 〜 2 0重量%、 好ましくは 3〜 1 5重量の濃度で存在することを特徴とする請 求項 1ないし 1 0の何れか 1項に記載の水中油型エマルション。 Claims 1 to 1 wherein the hydrophilic pigment and / or the filler are present in a concentration of 1 to 20% by weight, preferably 3 to 15% by weight, based on the total weight of the emulsion. 0 The oil-in-water emulsion according to any one of 0.
1 2 . 脂肪相がエマルシヨンの全重量に対して 5〜 2 0重量%、 好ましくは 7〜 1 5重量%を占めることを特徴とする請求項 1ないし 1 1の何れか 1項に 記載の水中油型エマルション。 12. The water according to any one of claims 1 to 11, characterized in that the fatty phase accounts for 5 to 20% by weight, preferably 7 to 15% by weight, based on the total weight of the emulsion. Oil emulsion.
1 3 . 水相がエマルシヨンの全重量に対して 3 5〜 9 5重量%、 好ましくは 4 0〜 8 0重量%を占めることを特徴とする請求項 1ないし 1 2の何れか 1項 に記載の水中油型エマルション。 - 23 -13. The method according to claim 1, wherein the aqueous phase comprises 35 to 95% by weight, preferably 40 to 80% by weight, based on the total weight of the emulsion. Oil-in-water emulsion. - twenty three -
1 4 . 請求項 1ないし 1 3の何れか 1項に記載の水中油型エマルションから なる又は該水中油型エマルションを含有する化粧料。 14. A cosmetic comprising or containing the oil-in-water emulsion according to any one of claims 1 to 13.
1 5 . メークアップ、 スキンケアからなる群から選ばれた用途を持つ請求項 1 4に記載の化粧料。 15. The cosmetic according to claim 14, having a use selected from the group consisting of makeup and skin care.
1 6 . 請求項 1ないし 1 3の何れか 1項に記載の水中油型エマルションから なる又は該水中油型エマルシヨンを含有する皮膚外用剤。 16. An external skin preparation comprising the oil-in-water emulsion according to any one of claims 1 to 13, or containing the oil-in-water emulsion.
1 7 . 使用する界面活性剤の量を 5重量%以下に抑えて、 顔料及び/又はフ ィラーを含有する水中油型エマルションを調製する方法において、 顔料及び/ 又はフィラーを親水性顔料及び/又はフィラーとし、 更に水膨潤性粘土鉱物を 添加し、 これによつて顔料及び/又はフィラーの分散性とエマルションの安定 性を改善することを特徴とする方法。 17. A method for preparing an oil-in-water emulsion containing a pigment and / or a filler while suppressing the amount of the surfactant used to 5% by weight or less, wherein the pigment and / or the filler is a hydrophilic pigment and / or A method comprising adding a water-swellable clay mineral as a filler, thereby improving the dispersibility of the pigment and / or filler and the stability of the emulsion.
PCT/JP2001/010882 2001-12-12 2001-12-12 Oil-in-water emulsion containing water-swellable clay mineral and use thereof WO2003049707A1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1726291A1 (en) * 2005-05-25 2006-11-29 Societe L'Oreal S.A. Cosmetic rinse-off compositions comprising interferential particles

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63151351A (en) * 1986-12-16 1988-06-23 Shiseido Co Ltd Water in oil type emulsified composition
FR2750602A1 (en) * 1996-07-04 1998-01-09 Oreal Composition for protecting skin and/or hair against UV radiation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63151351A (en) * 1986-12-16 1988-06-23 Shiseido Co Ltd Water in oil type emulsified composition
FR2750602A1 (en) * 1996-07-04 1998-01-09 Oreal Composition for protecting skin and/or hair against UV radiation

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1726291A1 (en) * 2005-05-25 2006-11-29 Societe L'Oreal S.A. Cosmetic rinse-off compositions comprising interferential particles
FR2886134A1 (en) * 2005-05-25 2006-12-01 Oreal COSMETIC RINSE COMPOSITION CONTAINING INTERFERENTIAL PARTICLES

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