JP2006342140A - Water-in-oil type emulsion composition and cosmetic - Google Patents
Water-in-oil type emulsion composition and cosmetic Download PDFInfo
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- JP2006342140A JP2006342140A JP2005171621A JP2005171621A JP2006342140A JP 2006342140 A JP2006342140 A JP 2006342140A JP 2005171621 A JP2005171621 A JP 2005171621A JP 2005171621 A JP2005171621 A JP 2005171621A JP 2006342140 A JP2006342140 A JP 2006342140A
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- fine particles
- cellulose
- water
- emulsion composition
- oil
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Abstract
Description
本発明は油中水型乳化組成物に関し、より詳細には経時的安定性に優れ、滑らかで伸展性のよい油中水型乳化組成物、及びこれを用いた化粧料に関する。 The present invention relates to a water-in-oil emulsion composition, and more particularly to a water-in-oil emulsion composition that is excellent in stability over time, is smooth and has good extensibility, and a cosmetic using the same.
従来より、乳化タイプが油中水型である油中水型乳化組成物は、化粧クリームなどの化粧料、医薬用軟膏剤、バターやチーズなどの食料品、などの広い分野において用いられている（例えば、特許文献１，２）。 Conventionally, a water-in-oil emulsion composition whose emulsification type is a water-in-oil type has been used in a wide range of fields such as cosmetics such as cosmetic creams, pharmaceutical ointments, and foodstuffs such as butter and cheese. (For example, Patent Documents 1 and 2).
一般的に、油中水型乳化組成物は、分散安定性のために有機変性粘度鉱物などの増粘剤が添加されるが、これにより油中水型乳化組成物の伸びが低下しベタツキのある使用感を受けるようになり、逆に増粘剤が未添加の場合は粘度が低下し２層に分離しやすく使用時に容器を振って混合させる必要があり利便性に欠けるという問題があった。
本発明は、経時安定性に優れ、伸展性に優れて良好な使用感を有し、安全性及び使用時の利便性を併せ持つ油中水型乳化組成物を提供することを目的とする。 An object of the present invention is to provide a water-in-oil emulsion composition that has excellent stability over time, excellent extensibility, good usability, and has both safety and convenience during use.
本発明は、平均粒子径が１０〜５００ｎｍであるセルロース微粒子及びセルロース複合体微粒子の群から選ばれた少なくとも１種類の微粒子を含有することを特徴とする油中水型乳化組成物である。 The present invention is a water-in-oil emulsion composition containing at least one kind of fine particles selected from the group of cellulose fine particles and cellulose composite fine particles having an average particle size of 10 to 500 nm.
本発明の油中水型乳化組成物においては、前記セルロース微粒子及びセルロース複合体微粒子のアスペクト比Ｌ／Ｄ（ここで、Ｌはセルロース微粒子又はセルロース複合体微粒子の長径を示し、Ｄは短径を示す。）が１．３以下の微粒子であることが好ましい。 In the water-in-oil emulsion composition of the present invention, the aspect ratio L / D of the cellulose fine particles and the cellulose composite fine particles (where L is the major axis of the cellulose fine particles or cellulose composite fine particles, and D is the minor diameter) It is preferable that the fine particles are 1.3 or less.
また、本発明の油中水型乳化組成物は、無機粉体を配合してもよく、この場合は親油性界面活性剤に加えて親水性界面活性剤を含有することが好ましい。 In addition, the water-in-oil emulsion composition of the present invention may contain an inorganic powder. In this case, it is preferable to contain a hydrophilic surfactant in addition to the lipophilic surfactant.
そして、本発明は上記の油中水型乳化組成物を含んでなることを特徴とする化粧料にある。 And this invention exists in the cosmetics characterized by including said water-in-oil type emulsion composition.
本発明の油中水型乳化組成物によれば、水相でセルロース微粒子やセルロース複合体微粒子が適度の増粘作用を発現し、経時的安定性に優れ、伸展性が良くザラツキやベタツキのない良好な使用感と使用性を併せ持つことができ、これを用いた化粧料や医薬用軟膏等の乳化製品を提供することができる。 According to the water-in-oil emulsified composition of the present invention, the cellulose fine particles and cellulose composite fine particles exhibit an appropriate thickening action in the aqueous phase, have excellent temporal stability, good extensibility, and have no roughness or stickiness. It can have both good feeling and usability, and can provide emulsified products such as cosmetics and pharmaceutical ointments using the same.
本発明の油中水型（Ｗ／Ｏ）乳化組成物は、油相中に平均粒子径が１０〜５００ｎｍであるセルロース微粒子やセルロース複合体微粒子を分散させた水相を分散させることで乳化組成物の経時安定性を改善し、伸展性を向上し伸びを良好にし、さらに、無機粉体を含有するＷ／Ｏ乳化組成物においては、親油性界面活性剤に親水性界面活性剤を組み合わせることによってその作用効果をさらに向上させるものとなる。 The water-in-oil (W / O) emulsified composition of the present invention is an emulsified composition by dispersing an aqueous phase in which cellulose fine particles having an average particle diameter of 10 to 500 nm or cellulose composite fine particles are dispersed in an oil phase. Improves the aging stability of the product, improves the extensibility and makes the elongation good. In addition, in a W / O emulsion composition containing an inorganic powder, a hydrophilic surfactant is combined with a lipophilic surfactant. This further improves the effect.
本発明に用いられるセルロース微粒子としては、植物繊維から得られる天然セルロース、パルプ、精製リンターや牛乳、大豆などのタンパク質から再生される再生セルロースからなる天然由来のセルロース微粒子が用いられる。 As the cellulose fine particles used in the present invention, naturally-derived cellulose fine particles composed of natural cellulose obtained from plant fibers, pulp, purified linters, regenerated cellulose regenerated from proteins such as milk and soybean are used.
また、セルロース複合体微粒子とは、上記のセルロースに紫外線遮蔽剤、染料、顔料、シリカ化合物、香料などの機能性成分を分散または吸着させた微粒子である。 The cellulose composite fine particles are fine particles obtained by dispersing or adsorbing functional components such as an ultraviolet shielding agent, a dye, a pigment, a silica compound, and a fragrance on the cellulose.
本発明のＷ／Ｏ乳化組成物では、上記セルロース微粒子及びセルロース複合体微粒子の群から１種類または２種類以上を選択し組み合わせて使用することができる。 In the W / O emulsion composition of the present invention, one type or two or more types can be selected and used in combination from the group of cellulose fine particles and cellulose composite fine particles.
セルロース微粒子やセルロース複合体微粒子は、平均粒子径が１０〜５００ｎｍ、好ましくは１０〜２００ｎｍであり、微細で、かつ球状に近い微粒子が好ましい。前記粒子径が１０ｎｍ未満であると粒子の捕捉効率が極端に低下し、５００ｎｍを超えると乳化物の経時安定性の改善効果が悪化し好ましくない。 Cellulose fine particles and cellulose composite fine particles have an average particle diameter of 10 to 500 nm, preferably 10 to 200 nm, and are preferably fine and close to spherical particles. If the particle diameter is less than 10 nm, the particle trapping efficiency is extremely lowered, and if it exceeds 500 nm, the effect of improving the stability over time of the emulsion is deteriorated.
上記セルロース微粒子やセルロース複合体微粒子は、球状に近いものほど粒子表面が平滑でありザラツキ感が少なく、また自己凝集性が小さくなり保水性や吸油性を高めて伸展性と経時的安定性を向上することができる。この観点から、微粒子のアスペクト比Ｌ／Ｄ（ここで、Ｌはセルロース微粒子又はセルロース複合体微粒子の長径、Ｄは短径を示す）は１．３以下、好ましくは１．２以下、さらに好ましくは１．１以下である。 Cellulose fine particles and cellulose composite fine particles are more spherical and have a smoother particle surface and less graininess. Also, self-aggregation is reduced and water retention and oil absorption are improved to improve extensibility and stability over time. can do. From this point of view, the aspect ratio L / D of the fine particles (where L is the long diameter of the cellulose fine particles or cellulose composite fine particles, D is the short diameter) is 1.3 or less, preferably 1.2 or less, more preferably 1.1 or less.
なお、上記微粒子の平均粒子径は、走査型電子顕微鏡により３０００倍で拡大した画像からランダムに抽出した５０個の粒子の粒子径を測定し平均値を求めた。また、アスペクト比Ｌ／Ｄは、上記平均粒子径の測定方法に準じて粒子の長径（Ｌ）と短径（Ｄ）を測定し、その平均値からＬ／Ｄを求めた。 The average particle size of the fine particles was determined by measuring the particle size of 50 particles randomly extracted from an image magnified 3000 times with a scanning electron microscope. The aspect ratio L / D was determined by measuring the long diameter (L) and short diameter (D) of the particles according to the above average particle diameter measurement method, and calculating L / D from the average value.
本発明におけるセルロース微粒子は、例えば、無機酸水溶液にセルロースを溶解させたセルロース溶液を水または水を５０重量％以上含む凝固剤中に再沈殿させてセルロースの懸濁液を調整し、その懸濁液中のセルロースに酸加水分解処理を施し、次いでその懸濁液から酸を除去した後にビーズミル、ニーダー等の湿式磨砕機により高度粉砕処理を行うことで製造することができ、セルロース複合体微粒子は上記したようにセルロース微粒子に１種類以上の機能性成分を分散または吸着させ得ることができる。なお、セルロース微粒子を高度粉砕処理する場合には、より低濃度で処理したほうが最終乳化物の伸展性、安定性が良好である。 The cellulose fine particles in the present invention are prepared, for example, by reprecipitation of a cellulose solution obtained by dissolving cellulose in an inorganic acid aqueous solution in water or a coagulant containing 50% by weight or more of water to prepare a suspension of cellulose, Cellulose composite fine particles can be produced by subjecting cellulose in the liquid to acid hydrolysis, and then removing acid from the suspension, followed by advanced grinding with a wet mill such as a bead mill or kneader. As described above, one or more kinds of functional components can be dispersed or adsorbed on the cellulose fine particles. When cellulose fine particles are subjected to high pulverization treatment, the extensibility and stability of the final emulsion are better when treated at a lower concentration.
このセルロース微粒子やセルロース複合体微粒子を、例えばセルロース微粒子をマイクロフルタイザーにかけて所定のセルロース濃度になるように水中に分散させることで、Ｗ／Ｏ乳化組成物の水相を構成する水分散体が得られる。この場合のセルロース微粒子やセルロース複合体微粒子の配合量は水に対して０．５〜１０重量％程度であることが好ましく、０．５重量％未満では伸展性や安定性の効果が得られず、１０重量％を超えると粘度の上昇により乳化し難くなり、また分散不良を起こしやすくなり伸展性が低下し好ましくない。 By dispersing the cellulose fine particles and the cellulose composite fine particles in water so that the cellulose fine particles have a predetermined cellulose concentration, for example, by using a microfluidizer, an aqueous dispersion constituting the aqueous phase of the W / O emulsion composition is obtained. It is done. In this case, the blending amount of cellulose fine particles and cellulose composite fine particles is preferably about 0.5 to 10% by weight with respect to water, and if it is less than 0.5% by weight, the effect of extensibility and stability cannot be obtained. If it exceeds 10% by weight, it becomes difficult to emulsify due to an increase in viscosity, and it becomes difficult to cause dispersion failure, and the extensibility is lowered.
また、本発明のＷ／Ｏ乳化組成物においては、着色顔料、体質顔料、紫外線防御剤としての無機粉体、さらに、乳化剤として作用させ乳化物の安定性をよくする親油性界面活性剤を含有することができる。また、親油性界面活性剤に親水性界面活性剤を組み合わせることで乳化安定性が向上し、無機粉体を配合した系では分散性及び分散安定性を向上させることができる。 In addition, the W / O emulsion composition of the present invention contains a color pigment, an extender pigment, an inorganic powder as an ultraviolet protective agent, and a lipophilic surfactant that acts as an emulsifier and improves the stability of the emulsion. can do. Moreover, emulsification stability improves by combining a hydrophilic surfactant with a lipophilic surfactant, and dispersibility and dispersion stability can be improved in a system in which inorganic powder is blended.
無機粉体としては、例えば、タルク、マイカ、カオリン、炭酸カルシウム、酸化亜鉛、群青、オキシ塩化ビスマス、水酸化クロム、雲母チタン、酸化アルミニウム、コバルト、紺青、カーボンブラック、ケイ酸マグネシウム、酸化チタン等が挙げられる。また、油相への分散性を向上するためシリコーン処理、デキストリン脂肪酸処理等の疎水化処理された粉末が好ましい。これらの１種類または２種類以上を併用することができる。さらに、有機物粉末、金属顔料等の任意の粉末を配合してもよい。 Examples of the inorganic powder include talc, mica, kaolin, calcium carbonate, zinc oxide, ultramarine, bismuth oxychloride, chromium hydroxide, mica titanium, aluminum oxide, cobalt, bitumen, carbon black, magnesium silicate, titanium oxide, and the like. Is mentioned. Moreover, in order to improve the dispersibility to an oil phase, the powder hydrophobized, such as a silicone process and a dextrin fatty acid process, is preferable. One or more of these can be used in combination. Furthermore, you may mix | blend arbitrary powders, such as organic substance powder and a metal pigment.
親水性界面活性剤としては、ＨＬＢが８〜１８程度である界面活性剤が使用でき、中でも経時安定性を向上させる点で親水性のショ糖脂肪酸エステルが好ましく、例えばステアリン酸スクロース、オレイン酸スクロース、パルミチン酸スクロース、ラウリン酸スクロース等が挙げられる。 As the hydrophilic surfactant, a surfactant having an HLB of about 8 to 18 can be used. Among them, a hydrophilic sucrose fatty acid ester is preferable from the viewpoint of improving stability over time. For example, sucrose stearate and sucrose oleate. Sucrose palmitate, sucrose laurate and the like.
また、親油性界面活性剤としては、ＨＬＢが１〜６程度の界面活性剤が使用でき、エルカ酸スクロース、ポリステアリン酸スクロース、ジステアリン酸スクロース、ポリラウリン酸スクロース等の親油性のショ糖脂肪酸エステル、ジイソステアリン酸グリセリン、ポリエーテル変性シリコン、ペンタイソステアリン酸デカグリセリン、セスキイソステアリン酸ソルビタン、モノイソステアリン酸グリセリン、ジイソステアリン酸ポリエチレングリコール等が挙げられる。これらの親油性の界面活性剤は１種類または２種類以上を組み合わせて用いてもよい。 As the lipophilic surfactant, a surfactant having an HLB of about 1 to 6 can be used, and a lipophilic sucrose fatty acid ester such as sucrose erucate, sucrose polystearate, sucrose distearate, sucrose polylaurate, Examples include glyceryl diisostearate, polyether-modified silicon, decaglycerin pentaisostearate, sorbitan sesquiisostearate, glyceryl monoisostearate, and polyethylene glycol diisostearate. These lipophilic surfactants may be used alone or in combination of two or more.
本発明において、油相を構成する油分としては、液状、固形状、半固形状のものが使用でき、例えば、シリコーンワックス、デカメチルシクロペンタシロキサン、メチルポリシロキサン、メチルフェニルポリシロキサン等のシリコーン油、セチルイソオクタノエート、グリセリルトリヘキサノエート、イソプロピルミリステート等のエステル油、ワセリン、流動パラフィン、スクワラン等の炭化水素油、ヒマシ油、オリーブ油、椿油、ホホバ油、ラノリン等の天然動物植物油、高級アルコール、フルオロカーボン等が挙げられ、これらの１種類または２種類以上を混合して用いることができる。 In the present invention, the oil component constituting the oil phase can be liquid, solid or semi-solid, for example, silicone oil such as silicone wax, decamethylcyclopentasiloxane, methylpolysiloxane, methylphenylpolysiloxane, etc. , Ester oils such as cetyl isooctanoate, glyceryl trihexanoate, isopropyl myristate, hydrocarbon oils such as petrolatum, liquid paraffin, squalane, castor oil, olive oil, coconut oil, jojoba oil, lanolin, and other natural animal plant oils, A higher alcohol, a fluorocarbon, etc. are mentioned, These 1 type (s) or 2 or more types can be mixed and used.
また本発明では、上記成分に加えて本発明の効果を損わない範囲で通常化粧料、医薬部外品等に用いられる成分を配合することができる。このような成分としては、例えば水、油分、保湿剤、ワックス、界面活性剤、粉末、分散剤、防腐剤、香料、薬剤、紫外線吸収剤、増粘剤等が挙げられる。 Moreover, in this invention, in addition to the said component, the component normally used for cosmetics, a quasi-drug, etc. can be mix | blended in the range which does not impair the effect of this invention. Examples of such components include water, oil, moisturizer, wax, surfactant, powder, dispersant, preservative, fragrance, drug, ultraviolet absorber, thickener and the like.
例えば、油分としては、上記油相成分に用いられるものと同様の油分が使用できる。 For example, as the oil, the same oil as that used for the oil phase component can be used.
また、保湿剤としては、グリセリン、１，３−ブチレングリコール、ジプロピレングリコール、プロピレングリコール等の多価アルコール、ヒアルロン酸、コンドロイチン硫酸等の水溶性高分子、乳酸ソーダ、クエン酸ソーダ、グルタミン酸ソーダ、２−ピロリドンカルボン酸ソーダ、食塩、塩化マグネシウム等の塩類等が挙げられる。配合量としては、１〜３０重量％程度が好ましい。 Further, as the humectant, polyhydric alcohols such as glycerin, 1,3-butylene glycol, dipropylene glycol and propylene glycol, water-soluble polymers such as hyaluronic acid and chondroitin sulfate, soda lactate, soda citrate, soda glutamate, Examples thereof include salts such as sodium 2-pyrrolidonecarboxylate, sodium chloride, and magnesium chloride. As a compounding quantity, about 1 to 30 weight% is preferable.
また、界面活性剤としては、前述の他に高級脂肪酸石鹸、Ｎ−アシルアミノ酸塩等が用いられる。 Further, as the surfactant, in addition to the above, higher fatty acid soap, N-acyl amino acid salt and the like are used.
増粘剤としては、カラギーナン等植物系ガム類、デキストラン、ヒアルロン酸等の多糖類、ゼラチン、アルブミン等の蛋白類、ヒドロキシエチルセルロース等のセルロース誘導体、デンプン類、アルギン酸類、ポリビニルアルコール、ポリビニルピロリドン、カルボキシビニルポリマー、ポリエチレンオキシド等の合成高分子等がある。 Thickeners include plant gums such as carrageenan, polysaccharides such as dextran and hyaluronic acid, proteins such as gelatin and albumin, cellulose derivatives such as hydroxyethyl cellulose, starches, alginic acids, polyvinyl alcohol, polyvinylpyrrolidone, carboxy There are synthetic polymers such as vinyl polymer and polyethylene oxide.
その他の防腐剤、香料、顔料、薬剤、紫外線吸収剤等は、例示しないが化粧料に使用可能な既存物質を適宜適量とすることができる。 Other preservatives, fragrances, pigments, drugs, ultraviolet absorbers and the like are not exemplified, but existing substances that can be used in cosmetics can be appropriately adjusted.
本発明のＷ／Ｏ乳化組成物は、油相と水相との比率は特に限定されないが、好ましくは重量比で油相：水相＝５０〜１０：５０〜９０、より好ましくは油相：水相＝４０〜２０：６０〜８０である。油相が１０重量％未満では安定な乳化物を得ることが困難となり、５０重量％を超えると油分によるベタツキによって使用感が低下する。 In the W / O emulsified composition of the present invention, the ratio of the oil phase to the aqueous phase is not particularly limited, but the oil phase: water phase = 50 to 10:50 to 90, more preferably the oil phase: Aqueous phase = 40-20: 60-80. If the oil phase is less than 10% by weight, it is difficult to obtain a stable emulsion, and if it exceeds 50% by weight, the feeling of use is reduced due to stickiness due to oil.
このＷ／Ｏ乳化組成物は、例えば、スクワラン、デカメチルシクロペンタシロキサン、メトキシケイヒ酸オクチルなどの油分に酸化チタンや酸化亜鉛などの無機粉体、親油性界面活性剤を含む油相成分を８０℃程度で加熱溶解させ均一化した油相部を形成し、水相部として、例えばセルロース濃度１．５％のセルロース微粒子分散水溶液に親水性界面活性剤や１，３−ブチレングリコールなどの保湿剤を投入して８０℃程度に加熱溶解させ、水相に油相を加えながらホモミキサーなどで撹拌し脱気、冷却し乳化物を収容して得られる。 This W / O emulsified composition comprises, for example, an oil phase component containing an inorganic component such as titanium oxide or zinc oxide and a lipophilic surfactant in an oil component such as squalane, decamethylcyclopentasiloxane, octyl methoxycinnamate, and the like. A uniform oil phase is formed by heating and dissolving at about 0 ° C., and as the aqueous phase, a humectant such as a hydrophilic surfactant or 1,3-butylene glycol is added to a cellulose fine particle dispersion aqueous solution having a cellulose concentration of 1.5%. The mixture is heated and dissolved at about 80 ° C., stirred with a homomixer while adding the oil phase to the aqueous phase, degassed and cooled to contain the emulsion.
本発明の化粧料は、前記Ｗ／Ｏ乳化組成物をセルロース微粒子として化粧料中に０．５〜１０重量％含むものであり、安全な天然由来のセルロース類を含有することで市場に好まれ、経時安定性に優れるとともにザラツキやベタツキ感がなく伸展性の良い化粧料として、例えば、メイクアップ化粧料、日焼け止め乳液、保湿クリーム、乳化ファンデーション、ヘアクリームなどの乳化化粧料、クリーム製剤などの医薬軟膏品などを提供するものとなる。 The cosmetic of the present invention contains 0.5 to 10% by weight of the W / O emulsion composition as cellulose fine particles in the cosmetic and is preferred by the market because it contains safe naturally-derived cellulose. As cosmetics that are excellent in stability over time and have no roughness or stickiness, such as makeup cosmetics, sunscreen emulsions, moisturizing creams, emulsified foundations, hair creams and other emulsified cosmetics, cream formulations, etc. It provides pharmaceutical ointments and the like.
以下に本発明を実施例に基づいてさらに詳細に説明するが、本発明はこれらによって何ら限定されるものではない。なお、配合量は重量％である。 Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited thereto. In addition, a compounding quantity is weight%.
表１に示すセルロース微粒子に関する実施例１〜６、比較例１〜３、及び表２に示すセルロース複合体微粒子に関する実施例７の各Ｗ／Ｏ乳化組成物を、下記成分を用いて表に記載の配合量で下記の方法により調整し、各Ｗ／Ｏ乳化組成物の伸展性（伸び試験）と経時安定性について下記の試験方法に従い評価した。結果を表１、２に示す。 Each W / O emulsion composition of Examples 1 to 6 relating to the cellulose fine particles shown in Table 1, Comparative Examples 1 to 3 and Example 7 relating to the cellulose composite fine particles shown in Table 2 is described in the table using the following components. Was adjusted by the following method, and the extensibility (elongation test) and stability over time of each W / O emulsion composition were evaluated according to the following test method. The results are shown in Tables 1 and 2.
［表１の成分］
・デカメチルシクロペンタシロキサン：信越化学工業（株）ＫＦ９９５
・スクワラン：スクアテック（株）スーパースクワラン
・メトキシケイヒ酸オクチル：アイエスピージャパン（株）エスカロール５５７
・酸化チタン：石原産業（株）ＴＴＯ−５５（Ｃ）
・酸化亜鉛：三好化成（株）ＳＡＳ−ＵＦＺＯ−４５０（１３％）
・ショ糖脂肪酸エステル（ＨＬＢ＝２）：第一工業製薬（株）ショ糖脂肪酸エステルＲ−２０
・ジイソステアリン酸グリセリン：日本エマルジョン（株）ＥＭＡＬＥＸ ＤＩＧＳ−２ＥＸ
・セルロース微粒子分散液（１）：セルロース微粒子；平均粒子径２０ｎｍ、Ｌ／Ｄ＝１．０５、濃度４％の分散水溶液
・セルロース微粒子分散液（２）：セルロース微粒子；平均粒子径２０ｎｍ、Ｌ／Ｄ＝１．０５、濃度１．５％の分散水溶液
・セルロース微粒子分散液（３）：セルロース微粒子；平均粒子径５５０ｎｍ、Ｌ／Ｄ＝１．０５、濃度４％の分散水溶液
・セルロース微粒子分散液（４）：セルロース微粒子；平均粒子径２０ｎｍ、Ｌ／Ｄ＝１．４０、濃度４％の分散水溶液
・精製水：イオン交換水
・１，３−ブチレングリコール：協和発酵ケミカル（株）
・ショ糖脂肪酸エステル（ＨＬＢ＝１５）：第一工業製薬（株）ショ糖脂肪酸エステルＳ−１６０
・有機変性ベントナイト：Elementis Specialities社 ベントン３８Ｖ
[Ingredients in Table 1]
Decamethylcyclopentasiloxane: Shin-Etsu Chemical Co., Ltd. KF995
・ Squalane: Squatech Co., Ltd. Super Squalane ・ Octyl methoxycinnamate: ES Japan Co., Ltd. Escalol 557
・ Titanium oxide: Ishihara Sangyo Co., Ltd. TTO-55 (C)
・ Zinc oxide: Miyoshi Kasei Co., Ltd. SAS-UFZO-450 (13%)
-Sucrose fatty acid ester (HLB = 2): Daiichi Kogyo Seiyaku Co., Ltd. Sucrose fatty acid ester R-20
・ Glycerin diisostearate: Nippon Emulsion Co., Ltd. EMALEX DIGS-2EX
Cellulose fine particle dispersion (1): Cellulose fine particles; average particle size 20 nm, L / D = 1.05, dispersion aqueous solution with 4% concentration Cellulose fine particle dispersion (2): Cellulose fine particles; average particle size 20 nm, L / D D = 1.05, 1.5% concentration aqueous dispersion / cellulose fine particle dispersion (3): cellulose fine particles; average particle size 550 nm, L / D = 1.05, 4% concentration aqueous dispersion / cellulose fine particle dispersion (4): Cellulose fine particles; average particle diameter 20 nm, L / D = 1.40, 4% concentration dispersion aqueous solution / purified water: ion-exchanged water / 1,3-butylene glycol: Kyowa Hakko Chemical Co., Ltd.
Sucrose fatty acid ester (HLB = 15): Daiichi Kogyo Seiyaku Co., Ltd. Sucrose fatty acid ester S-160
・ Organic modified bentonite: Elementis Specialities Benton 38V
［表１のＷ／Ｏ乳化組成物の調整方法］
表１記載の各Ｗ／Ｏ乳化組成物は、表記載の配合量（重量％）に従い、油分としてデカメチルシクロペンタシロキサン、スクワラン、メトキシケイヒ酸オクチルの混合物に酸化チタン、酸化亜鉛、ショ糖脂肪酸エステル（ＨＬＢ＝２）、ジイソステアリン酸グリセリンをそれぞれ混合して８０℃で加熱溶解させ均一化した油相部を形成し、セルロース微粒子分散水液（１）〜（４）に１，３−ブチレングリコール、ショ糖脂肪酸エステル（ＨＬＢ＝１５）、有機変性ベントナイトをそれぞれ投入して８０℃に加熱溶解させ水相部とし、水相に油相を加えながらホモミキサーで撹拌し、必要に応じて精製水を加えて調整し、脱気、冷却し乳化物を作製した。
[Method for preparing W / O emulsion composition of Table 1]
Each W / O emulsion composition described in Table 1 is a mixture of decamethylcyclopentasiloxane, squalane and octyl methoxycinnamate as an oil component in accordance with the blending amount (% by weight) described in the table, and titanium oxide, zinc oxide and sucrose fatty acid. Esters (HLB = 2) and glyceryl diisostearate are mixed together and heated and dissolved at 80 ° C. to form a uniform oil phase, and 1,3-butylene glycol is added to cellulose fine particle dispersions (1) to (4). , Sucrose fatty acid ester (HLB = 15), and organically modified bentonite were added to each, heated and dissolved at 80 ° C. to form an aqueous phase, stirred with a homomixer while adding an oil phase to the aqueous phase, and purified water as needed Was added, adjusted, degassed and cooled to prepare an emulsion.
［表２の成分］
・シリコーン処理酸化チタン：大東化成工業（株）ＳＩ０１−４ ＴＴＯ−Ｓ−１
・シリコーン処理タルク：三好化成（株）ＳＡ−ＪＡ−６８Ｒ
・スクワラン：スクアテック（株）スーパースクワラン
・デカメチルシクロペンタシロキサン：信越化学工業（株）ＫＦ９９５
・ポリエーテル変性ジメチルシロキサン：信越化学工業（株）ＫＦ６０１５
・グリセリン：阪本薬品工業（株）
・塩化ナトリウム：ナカライテスク（株）
・精製水：イオン交換水
[Ingredients in Table 2]
Silicone-treated titanium oxide: Daito Kasei Kogyo Co., Ltd. SI01-4 TTO-S-1
・ Silicone-treated talc: Miyoshi Kasei SA-JA-68R
・ Squalane: Squatech Co., Ltd. Super Squalane ・ Decamethylcyclopentasiloxane: Shin-Etsu Chemical Co., Ltd. KF995
Polyether modified dimethylsiloxane: Shin-Etsu Chemical Co., Ltd. KF6015
・ Glycerin: Sakamoto Pharmaceutical Co., Ltd.
・ Sodium chloride: Nacalai Tesque
・ Purified water: Ion exchange water
なお、セルロース複合体微粒子は、セルロース微粒子（平均粒子径２０ｎｍ、Ｌ／Ｄ＝１．０５）の懸濁液中に下記顔料をセルロース微粒子：顔料＝９：１（重量比）で分散させた懸濁液をスプレードライ法で造粒し、乾燥させ、シリコーン処理黒酸化鉄／セルロース複合体微粒子、シリコーン処理ベンガラ／セルロース複合体微粒子、及びシリコーン処理黄酸化鉄／セルロース複合体微粒子を調製した。 The cellulose composite fine particles are suspensions of the following pigments dispersed in a suspension of cellulose fine particles (average particle diameter 20 nm, L / D = 1.05) at a cellulose fine particle: pigment = 9: 1 (weight ratio). The suspension was granulated by a spray drying method and dried to prepare silicone-treated black iron oxide / cellulose composite fine particles, silicone-treated bengara / cellulose composite fine particles, and silicone-treated yellow iron oxide / cellulose composite fine particles.
［顔料］
・シリコーン処理黒酸化鉄：三好化成（株）ＳＡ−ＢＬ−１００
・シリコーン処理ベンガラ：三好化成（株）ＳＡ−ベンガラ七宝
・シリコーン処理黄酸化鉄：三好化成（株）ＳＡ−ＬＬ−ＸＬＯ
[Pigment]
Silicone-treated black iron oxide: Miyoshi Kasei SA-BL-100
・ Silicone-treated Bengala: Miyoshi Kasei Co., Ltd. SA-Bengara Cloisonne ・ Silicone-treated yellow iron oxide: Miyoshi Kasei Co., Ltd. SA-LL-XLO
［表２のＷ／Ｏ乳化組成物の調整方法］
表２記載の実施例７のＷ／Ｏ乳化組成物は、（１）油分としてのスクワラン、デカメチルシクロペンタシロキサン及びポリエーテル変性ジメチルシロキサンの混合物に、シリコーン処理酸化チタン、シリコーン処理タルク、シリコーン処理黒酸化鉄／セルロース複合体微粒子、シリコーン処理ベンガラ／セルロース複合体微粒子、及びシリコーン処理黄酸化鉄／セルロース複合体微粒子を加えて均一に分散させる。（２）精製水の一部にグリセリン及び塩化ナトリウムを溶解する。（３）前記（１）を撹拌しながら前記（２）を加え、精製水の残部を加え、ホモミキサーで５０００ｒｐｍで５分間の撹拌処理して乳化物を作製した。
[Method for preparing W / O emulsion composition of Table 2]
The W / O emulsion composition of Example 7 described in Table 2 was prepared by (1) mixing a mixture of squalane, decamethylcyclopentasiloxane and polyether-modified dimethylsiloxane as an oil component with silicone-treated titanium oxide, silicone-treated talc, and silicone-treated. Black iron oxide / cellulose composite fine particles, silicone-treated bengara / cellulose composite fine particles, and silicone-treated yellow iron oxide / cellulose composite fine particles are added and dispersed uniformly. (2) Dissolve glycerin and sodium chloride in a part of purified water. (3) While stirring (1) above, the above (2) was added, the remainder of the purified water was added, and the mixture was stirred with a homomixer at 5000 rpm for 5 minutes to prepare an emulsion.
［試験方法］
１．伸び試験
各Ｗ／Ｏ乳化組成物を５名のパネルによる官能試験を行い、顔面でのＷ／Ｏ乳化組成物の伸び状態を７段階の絶対評価基準、評価６：非常に良い、評価５：良い、評価４：やや良い、評価３：普通、評価２：やや悪い、評価１：悪い、評価０：非常に悪い、に従い評点し、５名の平均値で下記の通り評価した。
◎：非常によい；平均値が５点を超える。
○：良い；平均値が５点以下、３点を超える。
△：やや悪い；平均値が３点以下、１点を超える。
×：悪い；平均値が１点以下。
[Test method]
1. Elongation test Each W / O emulsion composition was subjected to a sensory test with a panel of five people, and the elongation state of the W / O emulsion composition on the face was evaluated in 7 stages of absolute evaluation criteria, evaluation 6: very good, evaluation 5: Evaluation was made according to Good, Evaluation 4: Slightly Good, Evaluation 3: Normal, Evaluation 2: Slightly bad, Evaluation 1: Bad, Evaluation 0: Very bad, and the average value of five persons was evaluated as follows.
A: Very good; average value exceeds 5 points.
○: Good; average value is 5 points or less and 3 points or more.
Δ: Slightly bad; average value is 3 points or less and 1 point or more.
X: Poor; average value is 1 point or less.
２．安定性試験
各Ｗ／Ｏ乳化組成物をガラス製サンプル瓶に充填し、４０℃で１ヶ月放置した後、組成物の分離状態を目視にて観察し、下記の基準に従い評価した。
◎：全く分離が認められない。
○：ほとんど分離が認められない。
△：わずかに分離が認められる。
×：完全に分離している。
2. Stability test Each W / O emulsion composition was filled in a glass sample bottle and allowed to stand at 40 ° C. for 1 month, and then the separated state of the composition was visually observed and evaluated according to the following criteria.
(Double-circle): Separation is not recognized at all.
○: Almost no separation is observed.
Δ: Slight separation is observed.
X: Completely separated.
表に示す結果より、本発明に係る実施例１〜７のＷ／Ｏ乳化組成物は、伸展性、経時安定性が共に良好でありザラツキやベタツキを抑えて化粧料として好適であることが分かる。しかし、界面活性剤としてショ糖脂肪酸エステルに代えてジイソステアリン酸グリセリンを用いた実施例５では経時変化による安定性低下の傾向が若干見られた。
From the results shown in the table, it can be seen that the W / O emulsion compositions of Examples 1 to 7 according to the present invention have good extensibility and stability over time, and are suitable as cosmetics with reduced roughness and stickiness. . However, in Example 5 in which glyceryl diisostearate was used instead of sucrose fatty acid ester as a surfactant, there was a slight tendency for stability to decrease with time.
これに対し、セルロース微粒子を含まない比較例１のＷ／Ｏ乳化組成物では、伸展性、経時安定性共に劣り、また増粘剤として従来の有機変性ベントナイトを用いた比較例２は伸展性が悪くベタツキやすくなる。一方、セルロース微粒子の粒子径が５００ｎｍを超える比較例３は、伸展性が不十分となり、また経時変化による分離が大きく見られた。 On the other hand, the W / O emulsion composition of Comparative Example 1 containing no cellulose fine particles is inferior in both extensibility and stability over time, and Comparative Example 2 using conventional organic modified bentonite as a thickener has extensibility. It becomes worse and sticky. On the other hand, in Comparative Example 3 in which the particle diameter of the cellulose fine particles exceeded 500 nm, the extensibility was insufficient, and separation due to a change with time was seen greatly.
本発明のＷ／Ｏ乳化組成物は、メイクアップ化粧料、日焼け止め乳液、保湿クリーム、乳化ファンデーション、ヘアクリームなどの乳化化粧料、及びクリーム製剤などの医薬軟膏品などに好適に使用することができる。
The W / O emulsified composition of the present invention can be suitably used for makeup cosmetics, sunscreen emulsions, moisturizing creams, emulsified foundations, hair creams and other emulsified cosmetics, and pharmaceutical ointments such as cream preparations. it can.
Claims (4)
A cosmetic comprising the water-in-oil emulsion composition according to any one of claims 1 to 3.
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| JP2008208045A (en) * | 2007-02-23 | 2008-09-11 | Shiseido Co Ltd | Water-in-oil type emulsion composition |
| JP2013544852A (en) * | 2010-12-10 | 2013-12-19 | エヌエス テクノロジーズ プロプライエタリー リミテッド | Methods for forming miniemulsions and their use for delivering bioactive agents |
| JP2016183202A (en) * | 2010-12-10 | 2016-10-20 | エヌエス テクノロジーズ プロプライエタリー リミテッドＮｓ Ｔｅｃｈｎｏｌｏｇｉｅｓ Ｐｔｙ Ｌｔｄ | Methods for forming miniemulsions and use thereof for delivering bioactive agents |
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