JP7420341B2 - Oil-in-water emulsion composition - Google Patents
Oil-in-water emulsion composition Download PDFInfo
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- JP7420341B2 JP7420341B2 JP2019194419A JP2019194419A JP7420341B2 JP 7420341 B2 JP7420341 B2 JP 7420341B2 JP 2019194419 A JP2019194419 A JP 2019194419A JP 2019194419 A JP2019194419 A JP 2019194419A JP 7420341 B2 JP7420341 B2 JP 7420341B2
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- oil
- water emulsion
- emulsion composition
- mass
- powder
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- UJMBCXLDXJUMFB-UHFFFAOYSA-K trisodium;5-oxo-1-(4-sulfonatophenyl)-4-[(4-sulfonatophenyl)diazenyl]-4h-pyrazole-3-carboxylate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-UHFFFAOYSA-K 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 description 1
Landscapes
- Cosmetics (AREA)
Description
本発明は、水中油型エマルション組成物に関する。 The present invention relates to oil-in-water emulsion compositions.
水中油型エマルションは、水に油を分散させたエマルションであり乳化物とも呼ばれる。水中油型エマルションとしては、油を可視サイズ（約５０μｍ以上）で分散させた水中油型巨大エマルションも知られており、その特徴的な外観により化粧水や美容液などの化粧品に用いられる。しかし、一般的な水中油型エマルションに比べ、油滴の粒子サイズが大きい水中油型巨大エマルションでは、クリーミングや合一などの不安定化が起こりやすく、油滴の分散状態の安定化が課題である。 An oil-in-water emulsion is an emulsion in which oil is dispersed in water, and is also called an emulsion. As oil-in-water emulsions, oil-in-water giant emulsions in which oil is dispersed in a visible size (approximately 50 μm or more) are also known, and are used in cosmetics such as lotions and serums due to their characteristic appearance. However, compared to general oil-in-water emulsions, oil-in-water giant emulsions with larger oil droplets are more prone to destabilization such as creaming and coalescence, and stabilizing the dispersion state of oil droplets is an issue. be.
水中油型巨大エマルションの調製には、平均粒子径が２０μｍ以下の薄片化層状ケイ酸塩粉体に、疎水基をもつ第４級アンモニウムイオンを結合することにより、層状ケイ酸塩粉体の層間に疎水基を結合してなる有機変性層状ケイ酸塩粉体を用いる手法（特許文献１）が報告されている。また、シリカポーラスグラスを用いる手法（非特許文献１）、マイクロチャネルを用いる手法（非特許文献２）、固形油分と流動油分を用いて安定化する手法（非特許文献３）などを用いて水中油型巨大エマルションを調製することが検討されている。 To prepare an oil-in-water macroemulsion, exfoliated layered silicate powder with an average particle size of 20 μm or less is bonded with quaternary ammonium ions having a hydrophobic group to form an interlaminar layer of the layered silicate powder. A method using an organically modified layered silicate powder formed by bonding a hydrophobic group to (Patent Document 1) has been reported. In addition, we have investigated methods using silica porous glass (Non-Patent Document 1), microchannels (Non-Patent Document 2), stabilization using solid oil and fluid oil (Non-Patent Document 3), etc. The preparation of oil-based macroemulsions has been considered.
シリカポーラスグラスやマイクロチャネル乳化を用いた手法では、少量の界面活性剤を用い、５０μｍ程度までの比較的サイズの大きいエマルションを調製できる。しかしながら乳化粒子の安定性や量産性において課題があった。また界面活性剤を用いることから、界面活性剤由来のべたつきや皮膚刺激もまた課題であった。一方、固形油分と流動油分を用いて安定化する手法では、数ｍｍ程度の巨大エマルションを調製できるが、用いる流動油分の極性によって適切な固形油分の選択が必要であるため、安定な巨大エマルションを得るために煩雑な検討が必要であるという課題があった。また固形油分を用いるために肌へ塗布した後の使用感が重たいという課題があった。 With methods using silica porous glass or microchannel emulsification, relatively large emulsions up to about 50 μm in size can be prepared using a small amount of surfactant. However, there were problems with the stability and mass production of emulsified particles. Furthermore, since a surfactant is used, stickiness and skin irritation caused by the surfactant are also issues. On the other hand, with the stabilization method using solid oil and fluid oil, it is possible to prepare a giant emulsion of several millimeters in size. There was a problem in that complicated studies were required to obtain the results. Furthermore, since it uses a solid oil, there is a problem in that it feels heavy after being applied to the skin.
また、近年は、水中油型巨大エマルションに様々な機能を持たせることも検討されている。例えば、着色した油滴を有する水中油型巨大エマルションや、機能性粉体を含む油滴を有する水中油型巨大エマルションの開発が望まれている。 Furthermore, in recent years, it has been considered to provide various functions to oil-in-water giant emulsions. For example, it is desired to develop oil-in-water giant emulsions having colored oil droplets and oil-in-water giant emulsions having oil droplets containing functional powders.
本発明は、このような従来技術に鑑みてなされたものであり、粉体を含有した油相（油滴）を可視可能なサイズで分散した、安定性に優れた水中油型巨大エマルション組成物を提供することを課題とする。 The present invention has been made in view of such prior art, and provides a highly stable oil-in-water giant emulsion composition in which a powder-containing oil phase (oil droplets) is dispersed in a visible size. The challenge is to provide the following.
本発明者は、上記課題を解決すべく鋭意検討した結果、後述する成分（Ａ）～（Ｄ）を必須成分として含むことで、粉体を含有した油相（油滴）を可視可能なサイズで分散することができ、かつ乳化粒子の安定性が高い水中油型巨大エマルション組成物が得られることを見出し、本発明を完成するに至った。
具体的に、本発明は、以下の構成を有する。
As a result of intensive studies to solve the above problems, the present inventor has determined that by including components (A) to (D) described below as essential components, the oil phase (oil droplets) containing powder can be made into a size that makes it visible. The present inventors have discovered that it is possible to obtain an oil-in-water giant emulsion composition that can be dispersed in water and has highly stable emulsified particles, and have completed the present invention.
Specifically, the present invention has the following configuration.
［１］ 下記成分（Ａ）～（Ｄ）を含む水中油型エマルション組成物であって、油滴の平均粒子径が５０μｍ以上である、水中油型エマルション組成物。
（Ａ）微細繊維状セルロース
（Ｂ）液状油及び半固形油から選択される少なくとも１種
（Ｃ）粉体
（Ｄ）水
［２］ さらに成分（Ｅ）として増粘多糖類を含む、［１］に記載の水中油型エマルション組成物。
［３］ 微細繊維状セルロースの平均繊維幅が１０００ｎｍ以下である、［１］又は［２］に記載の水中油型エマルション組成物。
［４］ 微細繊維状セルロースが、リンオキソ酸基、カルボキシ基及びカルボキシメチル基から選択される少なくとも１種を有する、［１］～［３］のいずれかに記載の水中油型エマルション組成物。
［５］ 油滴の平均粒子径が５０００μｍ以下である、［１］～［４］のいずれかに記載の水中油型エマルション組成物。
［６］ 増粘多糖類が、ヒドロキシエチルセルロース及びグアーガムから選択される少なくとも１種である、［２］～［５］のいずれかに記載の水中油型エマルション組成物。
［７］ さらに成分（Ｆ）として分散剤を含む、［１］～［６］のいずれかに記載の水中油型エマルション組成物。
［８］ 分散剤の含有量が、水中油型エマルション組成物の全質量に対して０質量％超え２．０質量％以下である、［７］に記載の水中油型エマルション組成物。
［９］ 水中油型エマルション組成物における、（Ａ）微細繊維状セルロースの含有率をａとし、（Ｂ）液状油及び半固形油から選択される少なくとも１種の含有率をｂとし、（Ｅ）増粘多糖類の含有率をｃとした場合、ａ：ｂで表される質量比率が、１：１～１：４００であり、かつ、ａ：ｃで表される質量比率が、３０：１～１：２である、［２］～［８］のいずれかに記載の水中油型エマルション組成物。
[1] An oil-in-water emulsion composition containing the following components (A) to (D), wherein the average particle diameter of oil droplets is 50 μm or more.
(A) Fine fibrous cellulose (B) At least one selected from liquid oil and semi-solid oil (C) Powder (D) Water [2] Further containing a thickening polysaccharide as component (E) [1 The oil-in-water emulsion composition described in ].
[3] The oil-in-water emulsion composition according to [1] or [2], wherein the average fiber width of the fine fibrous cellulose is 1000 nm or less.
[4] The oil-in-water emulsion composition according to any one of [1] to [3], wherein the fine fibrous cellulose has at least one selected from phosphorus oxoacid groups, carboxy groups, and carboxymethyl groups.
[5] The oil-in-water emulsion composition according to any one of [1] to [4], wherein the average particle diameter of the oil droplets is 5000 μm or less.
[6] The oil-in-water emulsion composition according to any one of [2] to [5], wherein the thickening polysaccharide is at least one selected from hydroxyethyl cellulose and guar gum.
[7] The oil-in-water emulsion composition according to any one of [1] to [6], further comprising a dispersant as component (F).
[8] The oil-in-water emulsion composition according to [7], wherein the content of the dispersant is more than 0% by mass and 2.0% by mass or less based on the total mass of the oil-in-water emulsion composition.
[9] In the oil-in-water emulsion composition, (A) the content of fine fibrous cellulose is a, (B) the content of at least one selected from liquid oil and semi-solid oil is b, and (E ) When the content of polysaccharide thickener is c, the mass ratio represented by a:b is 1:1 to 1:400, and the mass ratio represented by a:c is 30: The oil-in-water emulsion composition according to any one of [2] to [8], which has a ratio of 1 to 1:2.
本発明によれば、粉体を含有した油相（油滴）を可視可能なサイズで分散することができ、かつ乳化粒子の安定性が高く、かつ、油相中に粉体を分散した水中油型巨大エマルション組成物を提供することができる。 According to the present invention, the oil phase (oil droplets) containing powder can be dispersed in a visible size, the stability of the emulsified particles is high, and the powder is dispersed in the oil phase. An oil-based macroemulsion composition can be provided.
（水中油型エマルション組成物）
本発明は、下記成分（Ａ）～（Ｄ）を含む水中油型エマルション組成物に関する。ここで、水中油型エマルション組成物中に含まれる油滴の平均粒子径は５０μｍ以上である。
（Ａ）微細繊維状セルロース
（Ｂ）液状油及び／又は半固形油から選択される少なくとも１種
（Ｃ）粉体
（Ｄ）水
本発明の水中油型エマルション組成物は、さらに（Ｅ）増粘多糖類及び／又は（Ｆ）分散剤を含んでもよい。
なお、本明細書において、油滴の平均粒子径が５０μｍ以上の水中油型エマルション組成物を、水中油型巨大エマルション組成物ともいう。
(Oil-in-water emulsion composition)
The present invention relates to an oil-in-water emulsion composition containing the following components (A) to (D). Here, the average particle diameter of oil droplets contained in the oil-in-water emulsion composition is 50 μm or more.
(A) Fine fibrous cellulose (B) At least one selected from liquid oil and/or semi-solid oil (C) Powder (D) Water The oil-in-water emulsion composition of the present invention further comprises (E) It may also contain a mucopolysaccharide and/or (F) a dispersant.
In this specification, an oil-in-water emulsion composition in which the average particle diameter of oil droplets is 50 μm or more is also referred to as an oil-in-water macroemulsion composition.
本発明において、水中油型エマルション組成物とは、乳化粒子を含む組成物であって、該乳化粒子の平均粒子径は５０μｍ以上である。本発明の水中油型エマルション組成物は、水中に油滴が分散しているエマルションであるので、乳化粒子は、水中に分散する油滴である。すなわち、本発明の水中油型エマルション組成物における油滴の平均粒子径は５０μｍ以上である。 In the present invention, the oil-in-water emulsion composition is a composition containing emulsified particles, and the average particle diameter of the emulsified particles is 50 μm or more. Since the oil-in-water emulsion composition of the present invention is an emulsion in which oil droplets are dispersed in water, the emulsified particles are oil droplets dispersed in water. That is, the average particle diameter of oil droplets in the oil-in-water emulsion composition of the present invention is 50 μm or more.
水中油型エマルション組成物において、油滴中には粉体が包含されている。すなわち、水中油型エマルション組成物は、微細繊維状セルロースと、粉体を包含する油滴と、水とを含む、なお、油滴は液状油及び／又は半固形油から選択される少なくとも１種から構成される。 In an oil-in-water emulsion composition, powder is included in the oil droplets. That is, the oil-in-water emulsion composition contains fine fibrous cellulose, oil droplets containing powder, and water, and the oil droplets include at least one type selected from liquid oil and/or semi-solid oil. It consists of
水中油型エマルション組成物における油滴の平均粒子径は、５０～５０００μｍであることが好ましく、５０～４０００μｍであることがより好ましく、５０～３５００μｍであることがさらに好ましい。ここで、油滴の平均粒子径は、以下のようにして測定される値である。まず、水中油型エマルション組成物を５０ｍＬスクリュー管に入れ、定規と共に写真撮影する。撮影した画像を適切な倍率で拡大し、１画像に付き１００個以上の粒子の粒子径を計測する。計測した値と拡大倍率により実際の粒子径を算出し、その平均値を平均粒子径とする。 The average particle size of oil droplets in the oil-in-water emulsion composition is preferably 50 to 5000 μm, more preferably 50 to 4000 μm, and even more preferably 50 to 3500 μm. Here, the average particle diameter of oil droplets is a value measured as follows. First, an oil-in-water emulsion composition is placed in a 50 mL screw tube, and a photograph is taken with a ruler. The photographed image is enlarged at an appropriate magnification, and the particle diameters of 100 or more particles per image are measured. The actual particle diameter is calculated from the measured value and the magnification, and the average value is defined as the average particle diameter.
一般的な乳化粒子は、外観が不透明で白色（平均粒子径１～数１０μｍ）であるか、もしくは青白色（平均粒子径０．１～１μｍ）である。一方で、本発明の水中油型エマルションにおいては、油滴の平均粒子径が５０μｍ以上であり、かつ油滴中に後述する粉体が包含されるため、図１に示されるように、油滴を目視で確認することができ、微細な油滴が密集した特徴的な外観を呈する。 Typical emulsified particles have an opaque and white appearance (average particle diameter of 1 to several tens of μm) or bluish-white (average particle diameter of 0.1 to 1 μm). On the other hand, in the oil-in-water emulsion of the present invention, the average particle diameter of the oil droplets is 50 μm or more, and the oil droplets contain the powder described below, so as shown in FIG. It can be visually confirmed and has a characteristic appearance of densely packed fine oil droplets.
本発明の水中油型エマルション組成物における界面活性剤の含有量は、水中油型エマルション組成物の全質量に対して１．０質量％以下であることが好ましい。本発明において、界面活性剤は粉体の分散剤として良好な発色を得るために用いられる場合があるが、用いる粉体の種類によっては、界面活性剤は実質的に配合されなくてもよい。 The content of surfactant in the oil-in-water emulsion composition of the present invention is preferably 1.0% by mass or less based on the total mass of the oil-in-water emulsion composition. In the present invention, a surfactant may be used as a powder dispersant to obtain good color development, but depending on the type of powder used, the surfactant may not be substantially incorporated.
（（Ａ）成分）
本発明の水中油型エマルション組成物は、（Ａ）微細繊維状セルロースを含む。本明細書では、微細繊維状セルロースを（Ａ）成分と呼ぶこともある。
((A) component)
The oil-in-water emulsion composition of the present invention contains (A) fine fibrous cellulose. In this specification, fine fibrous cellulose is sometimes referred to as component (A).
（Ａ）成分の微細繊維状セルロースは、セルロースを含む繊維原料から製造される。セルロースを含む繊維原料としては、とくに限定されないが、入手しやすく安価である点からパルプを用いることが好ましい。パルプとしては、たとえば木材パルプ、非木材パルプ、および脱墨パルプが挙げられる。（Ａ）成分の微細繊維状セルロースは、パルプ等を原料としており、持続可能資源である。 The fine fibrous cellulose of component (A) is produced from a fiber raw material containing cellulose. The fiber raw material containing cellulose is not particularly limited, but it is preferable to use pulp because it is easily available and inexpensive. Pulps include, for example, wood pulp, non-wood pulp, and deinked pulp. The fine fibrous cellulose of component (A) is made from pulp or the like and is a sustainable resource.
微細繊維状セルロースは、たとえば繊維幅が１０００ｎｍ以下である微細繊維状セルロースである。なお、微細繊維状セルロースの繊維幅は、たとえば電子顕微鏡観察などにより測定することが可能である。 The fine fibrous cellulose is, for example, a fine fibrous cellulose having a fiber width of 1000 nm or less. Note that the fiber width of the fine fibrous cellulose can be measured by, for example, electron microscopic observation.
微細繊維状セルロースの平均繊維幅は、たとえば１０００ｎｍ以下である。微細繊維状セルロースの平均繊維幅は、たとえば２ｎｍ以上１０００ｎｍ以下であることが好ましく、２ｎｍ以上１００ｎｍ以下であることがより好ましく、２ｎｍ以上５０ｎｍ以下であることがさらに好ましく、２ｎｍ以上１０ｎｍ以下であることがとくに好ましい。なお、微細繊維状セルロースは、たとえば単繊維状のセルロースである。 The average fiber width of the fine fibrous cellulose is, for example, 1000 nm or less. The average fiber width of the fine fibrous cellulose is, for example, preferably 2 nm or more and 1000 nm or less, more preferably 2 nm or more and 100 nm or less, even more preferably 2 nm or more and 50 nm or less, and 2 nm or more and 10 nm or less. is particularly preferred. Note that the fine fibrous cellulose is, for example, monofilament cellulose.
微細繊維状セルロースの繊維長は、とくに限定されないが、たとえば０．１μｍ以上１０００μｍ以下であることが好ましく、０．１μｍ以上８００μｍ以下であることがより好ましく、０．１μｍ以上６００μｍ以下であることがさらに好ましい。繊維長を上記範囲内とすることにより、微細繊維状セルロースの結晶領域の破壊を抑制できる。また、微細繊維状セルロースのスラリー粘度を適切な範囲とすることも可能となる。なお、微細繊維状セルロースの繊維長は、たとえばＴＥＭ、ＳＥＭ、ＡＦＭによる画像解析より求めることができる。 The fiber length of the fine fibrous cellulose is not particularly limited, but for example, it is preferably 0.1 μm or more and 1000 μm or less, more preferably 0.1 μm or more and 800 μm or less, and preferably 0.1 μm or more and 600 μm or less. More preferred. By setting the fiber length within the above range, destruction of the crystalline region of the fine fibrous cellulose can be suppressed. Further, it is also possible to set the slurry viscosity of the fine fibrous cellulose within an appropriate range. The fiber length of the fine fibrous cellulose can be determined, for example, by image analysis using TEM, SEM, or AFM.
微細繊維状セルロースの軸比（繊維長／繊維幅）は、とくに限定されないが、たとえば２０以上１００００以下であることが好ましく、５０以上１０００以下であることがより好ましい。 The axial ratio (fiber length/fiber width) of the fine fibrous cellulose is not particularly limited, but is preferably, for example, 20 or more and 10,000 or less, more preferably 50 or more and 1,000 or less.
本実施形態における微細繊維状セルロースは、たとえば結晶領域と非結晶領域をともに有していることが好ましい。結晶領域と非結晶領域をともに有し、かつ軸比が高い微細繊維状セルロースは、好ましく用いられる。なお、本実施形態における微細繊維状セルロースはＩ型結晶構造を有していることが好ましい。 The fine fibrous cellulose in this embodiment preferably has, for example, both crystalline regions and amorphous regions. Fine fibrous cellulose having both crystalline and non-crystalline regions and a high axial ratio is preferably used. In addition, it is preferable that the fine fibrous cellulose in this embodiment has an I-type crystal structure.
本実施形態における微細繊維状セルロースは、イオン性置換基を有していることが好ましく、イオン性置換基としてアニオン性基を有することがより好ましい。イオン性置換基としてのアニオン性基としては、たとえばリンオキソ酸基、カルボキシ基、カルボキシメチル基、スルホン基等を挙げることができる。中でも、微細繊維状セルロースは、リンオキソ酸基、カルボキシ基及びカルボキシメチル基から選択される少なくとも１種を有することが好ましく、リンオキソ酸基を有することが特に好ましい。なお、本明細書においては、リンオキソ酸基には、リンオキソ酸基に由来する置換基が含まれ、カルボキシ基には、カルボキシ基に由来する置換基が含まれる。リンオキソ酸基に由来する置換基としては、例えば、リンオキソ酸基の塩、リンオキソ酸エステル基などの置換基が含まれ、カルボキシ基に由来する置換基には、カルボキシ基の塩、カルボン酸エステル基などの置換基が含まれる。なお、リンオキソ酸基は、たとえば、亜リン酸基（ホスホン酸基）であってもよい。 The fine fibrous cellulose in this embodiment preferably has an ionic substituent, and more preferably has an anionic group as the ionic substituent. Examples of the anionic group as an ionic substituent include a phosphorus oxoacid group, a carboxy group, a carboxymethyl group, and a sulfone group. Among these, the fine fibrous cellulose preferably has at least one selected from phosphorus oxoacid groups, carboxy groups, and carboxymethyl groups, and particularly preferably has phosphorus oxoacid groups. In addition, in this specification, a phosphorus oxoacid group includes a substituent derived from a phosphorus oxoacid group, and a carboxy group includes a substituent derived from a carboxyl group. Examples of substituents derived from a phosphorus oxo acid group include salts of a phosphorus oxo acid group, substituents such as a phosphorus oxo acid ester group, and substituents derived from a carboxy group include salts of a phosphorus oxo acid group, carboxylic acid ester groups, etc. This includes substituents such as. Note that the phosphorus oxo acid group may be, for example, a phosphorous acid group (phosphonic acid group).
微細繊維状セルロースは、セルロースを含む繊維原料に対して解繊処理を行うことで得られるものであってもよい。また、微細繊維状セルロースとしては、市販品を用いることもできる。微細繊維状セルロースの市販品としては、アウロ・ヴィスコTM ＣＳ（王子ホールディングス社製、リン酸ナトリウム処理微細繊維状セルロース２質量％含有スラリー）、レオクリスタ（第一工業製薬社製、カルボン酸処理微細繊維状セルロース２質量％含有スラリー）、セレンピア（日本製紙社製、カルボキシメチル化処理微細繊維状セルロース８８質量％以上含有スラリー）、ＢｉＮＦｉ－ｓ（スギノマシン社製、未処理微細繊維状セルロース２質量％含有スラリー）等を挙げることができる。 The fine fibrous cellulose may be obtained by subjecting a fiber raw material containing cellulose to a fibrillation treatment. Moreover, a commercially available product can also be used as the fine fibrous cellulose. Commercial products of fine fibrous cellulose include Auro Visco TM CS (manufactured by Oji Holdings, slurry containing 2% by mass of fine fibrous cellulose treated with sodium phosphate), and RheoCrysta (manufactured by Daiichi Kogyo Seiyaku Co., Ltd., carboxylic acid treated fine fiber). Serenpia (manufactured by Nippon Paper Industries, slurry containing 88% by mass or more of carboxymethylated fine fibrous cellulose), BiNFi-s (manufactured by Sugino Machine Co., Ltd., slurry containing 2% by mass of untreated fine fibrous cellulose) containing slurry), etc.
本発明の水中油型エマルション組成物は、上述したような微細繊維状セルロースを含むため、粉体を分散した油滴（乳化粒子）の分散安定性を高めることができる。 Since the oil-in-water emulsion composition of the present invention contains the above-mentioned fine fibrous cellulose, it can improve the dispersion stability of oil droplets (emulsified particles) in which powder is dispersed.
（Ａ）成分の含有量は、水中油型エマルション組成物の全質量に対して、０．０３～２．０質量％であることが好ましく、０．０５～１．０質量％であることがより好ましい。（Ａ）成分の含有量を上記範囲内とすることにより、水中油型エマルション組成物中の乳化粒子（油滴）の分散安定性をより効果的に高めることができる。 The content of component (A) is preferably 0.03 to 2.0% by mass, more preferably 0.05 to 1.0% by mass, based on the total mass of the oil-in-water emulsion composition. More preferred. By controlling the content of component (A) within the above range, the dispersion stability of emulsified particles (oil droplets) in the oil-in-water emulsion composition can be more effectively enhanced.
（（Ｂ）成分）
本発明の水中油型エマルション組成物は、（Ｂ）成分として、液状油及び半固形油から選択される少なくとも１種を含む。なお、本明細書において、半固形油とは、融点が４５℃以下で、室温でペースト状の油剤である。
((B) component)
The oil-in-water emulsion composition of the present invention contains at least one selected from liquid oil and semi-solid oil as component (B). In addition, in this specification, a semi-solid oil is an oil agent with a melting|fusing point of 45 degreeC or less and a paste-form at room temperature.
液状油及び半固形油から選択される少なくとも１種は、４５℃で液状の油剤であることが好ましい。液状油又は半固形油の具体例としては、スクワランや流動パラフィン等の炭化水素油、イソオクタン酸セチルやトリエチルヘキサノイン等のエステル油、ジイソノニルエーテルやジカプリリルエーテル等のエーテル油、オリーブ油やホホバ油、シア脂等の動植物油、ジフェニルジメチコンやジフェニルシロキシフェニルトリメチコン等のシリコーン油、ポリパーフルオロメチルイソプロピルエーテルなどのフッ素油、アスタキサンチンやリコピン等の油溶性有効成分、メトキシケイヒ酸エチルヘキシルやオクトクリレン等の紫外線吸収剤、油溶性ビタミン類、精油、香料等があげられるが、好ましくは炭化水素油、植物油、シリコーン油、油溶性有効成分、油溶性ビタミン類、香料等を挙げることができる。これらは、１種または２種以上を組合せて用いることができる。 At least one selected from liquid oil and semi-solid oil is preferably an oil agent that is liquid at 45°C. Specific examples of liquid oils or semi-solid oils include hydrocarbon oils such as squalane and liquid paraffin, ester oils such as cetyl isooctanoate and triethylhexanoin, ether oils such as diisononyl ether and dicaprylyl ether, olive oil and jojoba oil, Animal and vegetable oils such as shea butter, silicone oils such as diphenyl dimethicone and diphenylsiloxyphenyl trimethicone, fluorine oils such as polyperfluoromethyl isopropyl ether, oil-soluble active ingredients such as astaxanthin and lycopene, and ultraviolet rays such as ethylhexyl methoxycinnamate and octocrylene. Examples include absorbents, oil-soluble vitamins, essential oils, fragrances, etc., and preferably hydrocarbon oils, vegetable oils, silicone oils, oil-soluble active ingredients, oil-soluble vitamins, fragrances, etc. These can be used alone or in combination of two or more.
本発明の水中油型エマルション組成物における、（Ｂ）成分の含有量は、水中油型エマルション組成物の全質量に対して、０．１～５０．０質量％であることが好ましく、０．５～３０．０質量％であることがより好ましい。（Ｂ）成分の含有量を上記範囲内とすることにより、水中油型エマルション組成物中の乳化粒子（油滴）の分散安定性をより効果的に高めることができる。 The content of component (B) in the oil-in-water emulsion composition of the present invention is preferably 0.1 to 50.0% by mass, and 0.1 to 50.0% by mass, based on the total mass of the oil-in-water emulsion composition. More preferably, it is 5 to 30.0% by mass. By controlling the content of component (B) within the above range, the dispersion stability of emulsified particles (oil droplets) in the oil-in-water emulsion composition can be more effectively enhanced.
（（Ｃ）成分）
本発明の水中油型エマルション組成物は、（Ｃ）成分として、粉体を含む。粉体は表面未処理粉体もしくは表面処理粉体のいずれであってもよい。
((C) component)
The oil-in-water emulsion composition of the present invention contains powder as component (C). The powder may be either a surface-untreated powder or a surface-treated powder.
表面未処理粉体の具体例としては、酸化チタン、ベンガラ、黄酸化鉄、黒色酸化鉄、酸化亜鉛、酸化セリウム、マンガンバイオレット、コバルトバイオレット、酸化クロム、水酸化クロム、チタン酸コバルト、群青、紺青、酸化マグネシウム、酸化ジルコニウム、タルク、カオリン、絹雲母（セリサイト）、白雲母、金雲母、合成雲母、紅雲母、黒雲母、パーミ キュライト、シリカ、炭酸カルシウム、炭酸マグネシウム、ケイ酸マグネシウム、ケイ酸アルミニウム、ケイ酸バリウム、ケイ酸カルシウム、硫酸バリウム、硫酸カルシウム、リン酸カルシウム、ヒドロキシアパタイト、窒化ホウ素、パール顔料、オキシ塩化ビスマス、アルミナ、水酸化アルミニウムなどの無機顔料や、赤色３号、赤色１０号、赤色１０６号、赤色２０１号、赤色２０２号、赤色２０４号、赤色２０５号、赤色２２０号、赤色２２６号、赤色２２７号、赤色２２８号、赤色２３０号、赤色４０１号、赤色４０５号、赤色５０５号、黄色４号、黄色５号、黄色２０２号、黄色２０３号、黄色２０５号、黄色４０１号、橙色２０１号、橙色２０３号、橙色２０４号、橙色２０５号、橙色２０６号、橙色２０７号、青色１号、青色２号、青色２０１号、青色４０４号、緑色３号、緑色２０１号、緑色２０４号、緑色２０５号などの有機色素や、クロロフィルやβ－カロチンなどの天然色素や、ミリスチン酸亜鉛、パルミチン酸カルシウム、ステアリン酸アルミニウムなどの金属石鹸や、ナイロンパウダー、セルロースパウダー、ポリエチレンパウダー、ポリメタクリル酸メチルパウダー、ポリスチレンパウダー、アクリルパウダー、シリコーンパウダー等の有機粉体が挙げられる。表面未処理粉体は化粧品用のものであることが好ましく、この場合、用いられる表面未処理粉体は特に限定されるものではない。 Specific examples of surface-untreated powders include titanium oxide, red iron oxide, yellow iron oxide, black iron oxide, zinc oxide, cerium oxide, manganese violet, cobalt violet, chromium oxide, chromium hydroxide, cobalt titanate, ultramarine, and deep blue. , magnesium oxide, zirconium oxide, talc, kaolin, sericite, muscovite, phlogopite, synthetic mica, red mica, biotite, permiculite, silica, calcium carbonate, magnesium carbonate, magnesium silicate, silicic acid Inorganic pigments such as aluminum, barium silicate, calcium silicate, barium sulfate, calcium sulfate, calcium phosphate, hydroxyapatite, boron nitride, pearl pigment, bismuth oxychloride, alumina, aluminum hydroxide, Red No. 3, Red No. 10, Red No. 106, Red No. 201, Red No. 202, Red No. 204, Red No. 205, Red No. 220, Red No. 226, Red No. 227, Red No. 228, Red No. 230, Red No. 401, Red No. 405, Red No. 505 No. 4, Yellow No. 5, Yellow No. 202, Yellow No. 203, Yellow No. 205, Yellow No. 401, Orange No. 201, Orange No. 203, Orange No. 204, Orange No. 205, Orange No. 206, Orange No. 207, Organic pigments such as Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 404, Green No. 3, Green No. 201, Green No. 204, Green No. 205, natural pigments such as chlorophyll and β-carotene, and myristic acid. Examples include metal soaps such as zinc, calcium palmitate, and aluminum stearate, and organic powders such as nylon powder, cellulose powder, polyethylene powder, polymethyl methacrylate powder, polystyrene powder, acrylic powder, and silicone powder. The surface-untreated powder is preferably for cosmetics, and in this case, the surface-untreated powder used is not particularly limited.
表面処理粉体は、上述の表面未処理粉体を母粉体とし、シリコーン類、アルキルシラン類、アルキルチタネート類、フッ素化合物類、アミノ酸化合物類、脂肪酸化合物類などの化合物で処理されたものを言う。すなわち、表面処理粉体は、上述した化合物によって母粉体が被覆処理されてなる粉体である。また、表面処理粉体としては、従来公知の各種表面処理を施した粉体を用いることができる。また、その際の表面処理に上記の化合物以外の成分を用いることもできる。なお、表面処理粉体としては、複数の表面処理を組み合わせた粉体を用いることもできる。粉体としては、表面未処理粉体、表面処理粉体を問わず、１種または２種以上を組合せて用いることができる。 Surface-treated powder is one that uses the above-mentioned surface-untreated powder as a base powder and is treated with compounds such as silicones, alkylsilanes, alkyl titanates, fluorine compounds, amino acid compounds, and fatty acid compounds. To tell. That is, the surface-treated powder is a powder obtained by coating a base powder with the above-mentioned compound. Further, as the surface-treated powder, powders subjected to various conventionally known surface treatments can be used. Moreover, components other than the above-mentioned compounds can also be used for the surface treatment at that time. Note that, as the surface-treated powder, a powder obtained by combining a plurality of surface treatments can also be used. The powder may be either surface-untreated powder or surface-treated powder, and may be used alone or in combination of two or more.
粉体の一次平均粒子径は、５～１０００μｍであることが好ましく、１０～５００μｍであることがより好ましい。粉体の一次平均粒子径を上記範囲内とすることにより、粉体を含有した油相（油滴）を可視可能なサイズで分散させやすくなり、かつ乳化粒子の安定性をより効果的に高めることができる。 The primary average particle diameter of the powder is preferably 5 to 1000 μm, more preferably 10 to 500 μm. By setting the primary average particle diameter of the powder within the above range, it becomes easier to disperse the oil phase (oil droplets) containing the powder in a visible size, and the stability of the emulsified particles is more effectively enhanced. be able to.
本発明の水中油型エマルション組成物における、（Ｃ）成分の含有量は、水中油型エマルション組成物の全質量に対して、０．０１～５０．０質量％であることが好ましく、０．５～３５．０質量％であることがより好ましい。（Ｃ）成分の含有量を上記範囲内とすることにより、水中油型エマルション組成物中の乳化粒子（油滴）の分散安定性をより効果的に高めることができる。 The content of component (C) in the oil-in-water emulsion composition of the present invention is preferably 0.01 to 50.0% by mass, and 0.01 to 50.0% by mass, based on the total mass of the oil-in-water emulsion composition. More preferably, it is 5 to 35.0% by mass. By controlling the content of component (C) within the above range, the dispersion stability of emulsified particles (oil droplets) in the oil-in-water emulsion composition can be more effectively enhanced.
（（Ｄ）成分）
本発明の水中油型エマルション組成物は、（Ｄ）成分として、水を含む。水は、ナトリウム、カリウム等のアルカリ金属に由来するアルカリ金属イオンを含まないか、アルカリ金属イオン量ができるだけ少ないものが好ましく、イオン交換水、蒸留水、逆浸透膜によるろ過水等を用いることが好ましい。
((D) component)
The oil-in-water emulsion composition of the present invention contains water as component (D). It is preferable that the water does not contain alkali metal ions derived from alkali metals such as sodium and potassium, or that the amount of alkali metal ions is as small as possible, and it is preferable to use ion-exchanged water, distilled water, water filtered through a reverse osmosis membrane, etc. preferable.
本発明の水中油型エマルション組成物における、（Ｄ）成分の含有量は、水中油型エマルション組成物の全質量に対して、４０～９９．９質量％であることが好ましく、６０～９９．０質量％であることがより好ましい。 The content of component (D) in the oil-in-water emulsion composition of the present invention is preferably 40 to 99.9% by mass, and 60 to 99.9% by mass, based on the total mass of the oil-in-water emulsion composition. More preferably, it is 0% by mass.
（（Ｅ）成分）
本発明の水中油型エマルション組成物は、（Ｅ）成分として、増粘多糖類をさらに含んでもよい。
((E) component)
The oil-in-water emulsion composition of the present invention may further contain a thickening polysaccharide as component (E).
本発明における増粘多糖類は、増粘性の多糖類であれば特に制限されず、増粘多糖類としては、例えば、キサンタンガム、カラギーナン、グアーガム、ローカストビーンガム、タマリンドガム、グルコマンナン、ジェランガム、スクシノグリカン、ペクチン、アラビアガム、ペクチン、アルギン酸、プルラン、スクレロチウムガム、カチオン化でんぷん、カチオン化グアーガム、クインスシード、寒天、メチルセルロース、ヒドロキシエチルセルロース、ヒドロキシプロピルメチルセルロースステアロキシエーテル、カルボキシメチルセルロース、ヒドロキシプロピルメチルセルロース等が挙げられる。これらのうち、ヒドロキシエチルセルロース及びグアーガムから選択される少なくとも１種は増粘性、分散性の観点から好ましく用いられる。増粘多糖類は、１種のみを用いてもよく、２種以上を混合して用いてもよい。 The thickening polysaccharide in the present invention is not particularly limited as long as it is a thickening polysaccharide, and examples of the thickening polysaccharide include xanthan gum, carrageenan, guar gum, locust bean gum, tamarind gum, glucomannan, gellan gum, and sugar thickening polysaccharide. Sinoglycan, pectin, gum arabic, pectin, alginic acid, pullulan, sclerotium gum, cationized starch, cationized guar gum, quince seed, agar, methylcellulose, hydroxyethylcellulose, hydroxypropyl methylcellulose stearoxy ether, carboxymethylcellulose, hydroxypropyl methylcellulose etc. Among these, at least one selected from hydroxyethyl cellulose and guar gum is preferably used from the viewpoint of thickening property and dispersibility. Only one type of thickening polysaccharide may be used, or two or more types may be used in combination.
本発明の水中油型エマルション組成物が増粘多糖類を含む場合、（Ｅ）成分の含有量は、水中油型エマルション組成物の全質量に対して、０．０１～０．５質量％であることが好ましく、０．０２～０．３質量％であることがより好ましい。 When the oil-in-water emulsion composition of the present invention contains a polysaccharide thickener, the content of component (E) is 0.01 to 0.5% by mass based on the total mass of the oil-in-water emulsion composition. It is preferably 0.02 to 0.3% by mass, and more preferably 0.02 to 0.3% by mass.
（（Ｆ）成分）
本発明の水中油型エマルション組成物は、（Ｆ）成分として分散剤をさらに含んでもよい。
((F) component)
The oil-in-water emulsion composition of the present invention may further contain a dispersant as component (F).
分散剤は、粉体を分散できる成分であれば特に制限されず、分散剤としては、例えば、モノイソステアリン酸ソルビタン、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、モノイソステアリン酸ジグリセリン、ポリリシノレイン酸ポリグリセリルー６、ポリリシノレイン酸ポリグリセリルー１０、ペンタイソステアリン酸ポリグリセリルー１０、ペンタオレイン酸ポリグリセリルー１０、ポリヒドロキシステアリン酸、シリコーン系界面活性剤等が挙げられる。分散剤は１種のみを用いてもよく、２種以上を混合して用いても良い。 The dispersant is not particularly limited as long as it is a component that can disperse powder, and examples of the dispersant include sorbitan monoisostearate, sorbitan sesquiisostearate, glyceryl monoisostearate, diglyceryl monoisostearate, and polyglyceryl polyricinoleate. -6, polyglyceryl 10 polyricinoleate, polyglyceryl 10 pentaisostearate, polyglyceryl 10 pentaoleate, polyhydroxystearic acid, and silicone surfactants. Only one type of dispersant may be used, or two or more types may be used in combination.
本発明の水中油型エマルション組成物が分散剤を含む場合、（Ｆ）成分の含有量は、水中油型エマルション組成物の全質量に対して、０質量％超え５質量％以下であることが好ましく、０質量％超え２質量％以下であることがより好ましい。 When the oil-in-water emulsion composition of the present invention contains a dispersant, the content of component (F) may be more than 0% by mass and not more than 5% by mass based on the total mass of the oil-in-water emulsion composition. It is preferably more than 0% by mass and more preferably 2% by mass or less.
（成分比率）
水中油型エマルション組成物における、（Ａ）微細繊維状セルロースの含有率をａとし、（Ｂ）液状油及び半固形油から選択される少なくとも１種の含有率をｂとし、（Ｅ）増粘多糖類の含有率をｃとした場合、ａ：ｂで表される質量比率が、１：１～１：４００であり、かつ、ａ：ｃで表される質量比率が、３０：１～１：２であることが好ましい。
(component ratio)
In the oil-in-water emulsion composition, (A) the content of fine fibrous cellulose is a, (B) the content of at least one selected from liquid oil and semi-solid oil is b, and (E) thickening. When the polysaccharide content is c, the mass ratio represented by a:b is 1:1 to 1:400, and the mass ratio represented by a:c is 30:1 to 1. :2 is preferable.
（任意成分）
さらに、本発明の水中油型エマルション組成物には、本発明の効果を損なわない範囲で通常化粧料や皮膚外用剤に配合される公知の成分を含有することができる。公知の成分としては、ロウ類、保湿剤、増粘剤、色剤、高級アルコール、高級脂肪酸、糖、高分子化合物、生理活性成分、経皮吸収促進剤、溶媒、防腐剤、ｐＨ調整剤、キレート剤、抗酸化剤等が挙げられるがこれらに限定されるものではない。
(optional ingredient)
Furthermore, the oil-in-water emulsion composition of the present invention may contain known ingredients that are commonly incorporated into cosmetics and skin preparations to the extent that the effects of the present invention are not impaired. Known ingredients include waxes, humectants, thickeners, coloring agents, higher alcohols, higher fatty acids, sugars, polymer compounds, physiologically active ingredients, transdermal absorption enhancers, solvents, preservatives, pH adjusters, Examples include, but are not limited to, chelating agents, antioxidants, and the like.
（用途）
本発明の水中油型エマルション組成物は、スキンケア化粧料、ヘアケア化粧料、ボディ用化粧料、その他の化粧料、皮膚外用剤、入浴剤、メイクアップ化粧料等に用いることができ、これに限定されるものではない。
(Application)
The oil-in-water emulsion composition of the present invention can be used in skin care cosmetics, hair care cosmetics, body cosmetics, other cosmetics, external skin preparations, bath salts, makeup cosmetics, etc., but is limited thereto. It is not something that will be done.
（水中油型エマルション組成物の製造方法）
本発明の水中油型エマルション組成物は、成分（Ａ）、（Ｄ）、（Ｅ）を混合して、第１相を得る工程と、成分（Ｂ）、（Ｃ）を混合して第２相を得る工程と、第１相と第２相を混合する工程とを含むことが好ましい。このような製造工程を経ることにより、粉体を含有した油相（油滴）を可視可能なサイズで分散した水中油型エマルション組成物を得ることができる。
(Method for producing oil-in-water emulsion composition)
The oil-in-water emulsion composition of the present invention includes a step of mixing components (A), (D), and (E) to obtain a first phase, and a step of mixing components (B) and (C) to obtain a second phase. Preferably, the method includes the steps of obtaining a phase and mixing the first phase and the second phase. By going through such a manufacturing process, it is possible to obtain an oil-in-water emulsion composition in which the oil phase (oil droplets) containing powder is dispersed in a visible size.
以下に本発明の実施例を挙げて、本発明についてさらに詳しく説明するが、本発明はこれに限定されるものではない。なお、以下の例において、配合量の記載は特に断りのない限り質量％を意味する。 EXAMPLES The present invention will be described in more detail below with reference to Examples, but the present invention is not limited thereto. In addition, in the following examples, the description of the blending amount means mass % unless otherwise specified.
（実施例１－１、１－２及び比較例１－１、１－２：微細繊維状セルロースと増粘多糖類との比較評価
１．試料の調製
表１に示す第１相と第２相を構成する各成分をそれぞれ測りとり、第１相を構成する各成分を均一になるまで撹拌した。第２相を構成する各成分を撹拌し均一分散した。次に、第１相に第２相を添加し、パドルミキサーによって撹拌し、均質化して水中油型エマルション組成物を得た。表中の各成分の数値は質量％を示す。
(Examples 1-1, 1-2 and Comparative Examples 1-1, 1-2: Comparative evaluation of fine fibrous cellulose and thickening polysaccharide 1. Preparation of samples First phase and second phase shown in Table 1 Each component constituting the first phase was measured and stirred until it became uniform.The components constituting the second phase were stirred and uniformly dispersed.Next, the second phase was added to the first phase. The phases were added, stirred with a paddle mixer, and homogenized to obtain an oil-in-water emulsion composition.The numerical values for each component in the table indicate mass %.
２．油滴の平均粒子径の測定方法
実施例１－１と１－２及び比較例１－１と１－２の水中油型エマルション組成物をそれぞれ５０ｍＬスクリュー管に入れ、定規とともに写真撮影した。撮影した画像を適切な倍率で拡大し、１画像につき１００個以上の油滴の粒子径を計測した。計測した値と拡大倍率より実際の油滴の粒子径を算出し、算出した１００個以上の値を平均したものを油滴の平均粒子径とした。
2. Method for Measuring Average Particle Size of Oil Droplets The oil-in-water emulsion compositions of Examples 1-1 and 1-2 and Comparative Examples 1-1 and 1-2 were each placed in a 50 mL screw tube and photographed with a ruler. The captured images were enlarged at an appropriate magnification, and the particle diameters of 100 or more oil droplets were measured for each image. The actual particle size of the oil droplet was calculated from the measured value and the magnification, and the average of 100 or more calculated values was taken as the average particle size of the oil droplet.
３．安定性の評価方法
実施例１－１と１－２及び比較例１－１と１－２の水中油型エマルション組成物を４５℃の恒温槽に３ヶ月間放置した。その後、室温へ戻したサンプルについて目視による外観観察を行った。外観観察は以下に示す評価基準により油滴粒子の均一性について評価した。
＜評価基準：油滴粒子の均一性＞
Ａ：油滴粒子の合一やクリーミング、粉体の沈降は認められない
Ｂ：油滴粒子の合一やクリーミングは認められないが、わずかな粉体の沈降が認められる
Ｃ：油滴粒子の合一やクリーミングが認められる、もしくは粉体の沈降が認められる
－：調製翌日に分離または粉体が沈降したため評価未実施
3. Stability evaluation method The oil-in-water emulsion compositions of Examples 1-1 and 1-2 and Comparative Examples 1-1 and 1-2 were left in a constant temperature bath at 45° C. for 3 months. Thereafter, the sample was returned to room temperature and visually observed for appearance. In the appearance observation, the uniformity of the oil droplet particles was evaluated using the evaluation criteria shown below.
<Evaluation criteria: Uniformity of oil droplet particles>
A: No coalescence or creaming of oil droplet particles or sedimentation of powder is observed. B: No coalescence or creaming of oil droplet particles is observed, but slight sedimentation of powder is observed. C: No coalescence of oil droplet particles is observed. Coalescence or creaming is observed, or powder sedimentation is observed -: Evaluation not performed because separation or powder sedimentation occurred the day after preparation.
４．結果
実施例で得られた水中油型エマルション組成物においては、油滴中に粉体が含有されていた。リン酸ナトリウム処理微細繊維状セルロースを０．３質量％含む実施例１－１では粉体を含有した油滴の分散安定性に優れていた。グアーガムを用いた実施例１－２では、リン酸ナトリウム処理繊維状セルロースの含有量が０．１５質量％であっても、粉体を含有した油滴の分散安定性に優れていた。一方、グアーガムや（アクリル酸ヒドロキシエチル／アクリロイルジメチルタウリンＮａ）コポリマーを単独で用いた比較例１－１および比較例１－２では、調製直後の油滴の平均粒子径が大きく、翌日には分離が認められた。その結果、粉体を含む油滴は観察されなかった。なお、実施例１－１の外観写真を図１に示す。
4. Results In the oil-in-water emulsion compositions obtained in Examples, powder was contained in the oil droplets. Example 1-1 containing 0.3% by mass of sodium phosphate-treated fine fibrous cellulose had excellent dispersion stability of oil droplets containing powder. In Example 1-2 using guar gum, the dispersion stability of oil droplets containing powder was excellent even when the content of the sodium phosphate-treated fibrous cellulose was 0.15% by mass. On the other hand, in Comparative Examples 1-1 and 1-2, in which guar gum or (hydroxyethyl acrylate/Na acryloyl dimethyltaurine) copolymer was used alone, the average particle size of the oil droplets immediately after preparation was large, and the oil droplets separated the next day. was recognized. As a result, no oil droplets containing powder were observed. Incidentally, an external photograph of Example 1-1 is shown in FIG.
（実施例２－１～２－３：界面活性剤有無の評価）
１．試料の調製と評価方法
表２に示す各成分を使用して、実施例１－１と同様の方法で水中油型エマルション組成物を調製し、実施例１－１と同様の方法で評価を行った。表中の各成分の数値は質量％を示す。
(Examples 2-1 to 2-3: Evaluation of presence or absence of surfactant)
1. Sample preparation and evaluation method Using each component shown in Table 2, an oil-in-water emulsion composition was prepared in the same manner as in Example 1-1, and evaluated in the same manner as in Example 1-1. Ta. The numerical value of each component in the table indicates mass %.
ＦＰＤ－Ｃ－ＷＨＩＴＥ：ハイドロゲンジメチコン、タルク（東色ピグメント社製）、
ＦＰＤ－Ｃ－Ｄａ－Ｙｅｌｌｏｗ：酸化鉄、ハイドロゲンジメチコン、タルク（東色ピグメント社製）、
ＦＰＤ－Ｃ－Ｄａ－Ｒｅｄ：酸化鉄、ハイドロゲンジメチコン、タルク（東色ピグメント社製）、
ＦＰＤ－Ｃ－Ｄａ－Ｂｌａｃｋ：酸化鉄、ハイドロゲンジメチコン、タルク（東色ピグメント社製）、
ＴＡＲＯＸ Ｒ－５１６Ｐ：酸化鉄（チタン工業社製）、
ＴＡＲＯＸ ＬＬ－１００Ｐ：酸化鉄（チタン工業社製）、
ＴＡＲＯＸ ＢＬ－１００Ｐ：酸化鉄（チタン工業社製）、
ＭＰ－１１３１：酸化チタン、水酸化Ａｌ（テイカ社製）
FPD-C-WHITE: Hydrogen dimethicone, talc (manufactured by Toshiki Pigment Co., Ltd.),
FPD-C-Da-Yellow: iron oxide, hydrogen dimethicone, talc (manufactured by Toshiki Pigment Co., Ltd.),
FPD-C-Da-Red: iron oxide, hydrogen dimethicone, talc (manufactured by Toshiki Pigment Co., Ltd.),
FPD-C-Da-Black: iron oxide, hydrogen dimethicone, talc (manufactured by Toshiki Pigment Co., Ltd.),
TAROX R-516P: Iron oxide (manufactured by Titan Kogyo Co., Ltd.),
TAROX LL-100P: Iron oxide (manufactured by Titan Kogyo Co., Ltd.),
TAROX BL-100P: Iron oxide (manufactured by Titanium Industries),
MP-1131: Titanium oxide, Al hydroxide (manufactured by Teika)
２．結果
実施例で得られた水中油型エマルション組成物においては、油滴中に粉体が含有されていた。また、いずれも安定性は良好であった。
2. Results In the oil-in-water emulsion compositions obtained in Examples, powder was contained in the oil droplets. In addition, all had good stability.
実施例３：ファンデーション
第１相 アウロ・ヴィスコＣＳ ７．５０（質量％）
グアーガム ０．０５
プロパンジオール ３．００
防腐剤 適量
水 残部
第２相 アルミナ、シラン処理酸化チタン １．７３
シラン処理酸化鉄（黄色） ０．２０
シラン処理酸化鉄（赤） ０．０４
シラン処理酸化鉄（黒） ０．０３
スクワラン ３．００
ポリヒドロキシステアリン酸 ０．０５
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は９９７μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 3: Foundation phase 1 Auro Visco CS 7.50 (mass%)
Guar gum 0.05
Propanediol 3.00
Preservative Appropriate amount Water Remainder 2nd phase Alumina, silanized titanium oxide 1.73
Silanized iron oxide (yellow) 0.20
Silanized iron oxide (red) 0.04
Silanized iron oxide (black) 0.03
Squalane 3.00
Polyhydroxystearic acid 0.05
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 997 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例４：化粧下地
第１相 アウロ・ヴィスコＣＳ ２．５００（質量％）
タマリンドガム ０．００２
１，３－ブチレングリコール ３．０００
防腐剤 適量
水 残部
第２相 シリコーン処理マイカ ５．０００
シリコーン処理タルク ５．０００
ジメチコン １０．０００
（合計） １００．０００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は１０８７μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 4: Makeup base phase 1 Auro Visco CS 2.500 (mass%)
Tamarind gum 0.002
1,3-butylene glycol 3.000
Preservative Appropriate amount Water Remainder 2nd phase Silicone treated mica 5.000
Silicone treated talc 5.000
Dimethicone 10.000
(Total) 100.000
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 1087 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例５：日焼け止め
第１相 アウロ・ヴィスコＣＳ ７．５（質量％）
グアーガム ０．３
ジプロピレングリコール １０．０
防腐剤 適量
水 残部
第２相 水酸化アルミニウム、脂肪酸処理微粒子酸化チタン ２．０
シリカ、脂肪酸処理微粒子酸化亜鉛 ２．０
（カプリル酸／カプリン酸）グリセリル ４．０
ポリヒドロキシステアリン酸 ０．３
（合計） １００．０
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は１０２０μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 5: Sunscreen Phase 1 Auro Visco CS 7.5 (mass%)
Guar gum 0.3
Dipropylene glycol 10.0
Preservative Appropriate amount Water Remainder 2nd phase Aluminum hydroxide, fatty acid treated fine particle titanium oxide 2.0
Silica, fatty acid treated fine particle zinc oxide 2.0
(Caprylic acid/Capric acid) Glyceryl 4.0
Polyhydroxystearic acid 0.3
(Total) 100.0
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 1020 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例６：化粧下地
第１相 アウロ・ヴィスコＣＳ ７．５０（質量％）
ヒドロキシプロピルメチルセルロースステアロキシエーテル ０．０５
プロピレングリコール ７．００
防腐剤 適量
水 残部
第２相 水酸化アルミニウム処理酸化チタン １．７３
未処理酸化鉄（黄色） ０．２０
未処理酸化鉄（赤） ０．０４
未処理酸化鉄（黒） ０．０３
マカデミアナッツ油 ３．００
ポリヒドロキシステアリン酸 ０．０５
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は１２１８μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 6: Makeup base phase 1 Auro Visco CS 7.50 (mass%)
Hydroxypropyl methyl cellulose stearoxy ether 0.05
Propylene glycol 7.00
Preservative Appropriate amount Water Remainder 2nd phase Aluminum hydroxide treated titanium oxide 1.73
Untreated iron oxide (yellow) 0.20
Untreated iron oxide (red) 0.04
Untreated iron oxide (black) 0.03
Macadamia nut oil 3.00
Polyhydroxystearic acid 0.05
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 1218 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例７：プライマー
第１相 アウロ・ヴィスコＣＳ ７．５０（質量％）
グアーガム ０．３０
１，３－ブチレングリコール １５．００
防腐剤 適量
水 残部
第２相 酸化チタン、マイカ（パール剤） ０．１５
エチルヘキサン酸セチル １．００
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は９５７μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 7: Primer phase 1 Auro Visco CS 7.50 (mass%)
Guar gum 0.30
1,3-butylene glycol 15.00
Preservative Appropriate amount Water Remainder 2nd phase Titanium oxide, mica (pearl agent) 0.15
Cetyl ethylhexanoate 1.00
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 957 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例８：ファンデーション
第１相 セレンピア ０．２０（質量％）
グアーガム ０．０５
プロパンジオール ７．００
防腐剤 適量
水 残部
第２相 レシチン処理酸化チタン １．７３
レシチン処理酸化鉄（黄色） ０．２０
レシチン処理酸化鉄（赤） ０．０４
レシチン処理酸化鉄（黒） ０．０３
パルミチン酸エチルヘキシル ３．００
ポリヒドロキシステアリン酸 ０．０５
（合計） １００．００
※セレンピア：カルボキシメチル化処理微細繊維状セルロース８８質量％含有スラリー（日本製紙社製）
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は１０６３μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 8: Foundation phase 1 Serenpia 0.20 (mass%)
Guar gum 0.05
Propanediol 7.00
Preservative Appropriate amount Water Remainder 2nd phase Lecithin-treated titanium oxide 1.73
Lecithin-treated iron oxide (yellow) 0.20
Lecithin-treated iron oxide (red) 0.04
Lecithin-treated iron oxide (black) 0.03
Ethylhexyl palmitate 3.00
Polyhydroxystearic acid 0.05
(Total) 100.00
*Selenpia: Slurry containing 88% by mass of carboxymethylated fine fibrous cellulose (manufactured by Nippon Paper Industries)
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 1063 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例９：ファンデーション
第１相 レオクリスタ ８．００（質量％）
グアーガム ０．０５
ジプロピレングリコール ５．００
防腐剤 適量
水 残部
第２相 アミノ酸処理酸化チタン １．７３
アミノ酸処理酸化鉄（黄色） ０．２０
アミノ酸処理酸化鉄（赤） ０．０４
アミノ酸処理酸化鉄（黒） ０．０３
パルミチン酸エチルヘキシル ３．００
ポリヒドロキシステアリン酸 ０．０５
（合計） １００．００
※レオクリスタ：カルボン酸処理微細繊維状セルロース２質量％含有スラリー（第一工業製薬社製）
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は１２６７μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 9: Foundation phase 1 RheoCrysta 8.00 (mass%)
Guar gum 0.05
Dipropylene glycol 5.00
Preservative Appropriate amount Water Remainder 2nd phase Amino acid treated titanium oxide 1.73
Amino acid treated iron oxide (yellow) 0.20
Amino acid treated iron oxide (red) 0.04
Amino acid treated iron oxide (black) 0.03
Ethylhexyl palmitate 3.00
Polyhydroxystearic acid 0.05
(Total) 100.00
*LeoCrysta: Slurry containing 2% by mass of carboxylic acid-treated fine fibrous cellulose (manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd.)
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 1267 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例１０：チーク
第１相 アウロ・ヴィスコＣＳ ８．５０（質量％）
グアーガム ０．１０
ヘキサンジオール ３．００
ジグリセリン ５．００
防腐剤 適量
水 残部
第２相 酸化チタン ０．２５
酸化鉄 １．５０
赤２０２ ０．１２
黄４ ４．００
イソステアリン酸ソルビタン ０．５０
トリエチルヘキサノイン １０．００
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は９８２μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 10: Teak 1st phase Auro Visco CS 8.50 (mass%)
Guar gum 0.10
Hexanediol 3.00
Diglycerin 5.00
Preservative Appropriate amount Water Remainder 2nd phase Titanium oxide 0.25
Iron oxide 1.50
Red 202 0.12
Yellow 4 4.00
Sorbitan isostearate 0.50
Triethylhexanoin 10.00
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 982 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例１１：チーク
第１相 アウロ・ヴィスコＣＳ ８．００（質量％）
ジェランガム ０．０５
ペンチレングリコール ３．００
グリセリン ５．００
防腐剤 適量
水 残部
第２相 酸化チタン ２．５０
酸化鉄 ０．２５
赤２０１ ０．１０
シクロペンタシロキサン １０．００
ＰＥＧ－１０ジメチコン ０．５０
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は１０９２μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 11: Teak 1st phase Auro Visco CS 8.00 (mass%)
gellan gum 0.05
Pentylene glycol 3.00
Glycerin 5.00
Preservative Appropriate amount Water Remainder 2nd phase Titanium oxide 2.50
Iron oxide 0.25
Red 201 0.10
Cyclopentasiloxane 10.00
PEG-10 dimethicone 0.50
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 1092 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例１２：アイシャドウ
第１相 アウロ・ヴィスコＣＳ １０．００（質量％）
キサンタンガム ０．０５
プロピレングリコール １０．００
防腐剤 適量
水 残部
第２相 合成金雲母 ５．００
マイカ、酸化チタン、コンジョウ（パール剤） ５．００
パルミチン酸エチルヘキシル １０．００
ポリヒドロキシステアリン酸 ０．１０
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は１０７１μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 12: Eyeshadow first phase Auro Visco CS 10.00 (mass%)
Xanthan gum 0.05
Propylene glycol 10.00
Preservative Appropriate amount Water Residual second phase Synthetic phlogopite 5.00
Mica, titanium oxide, powder (pearl agent) 5.00
Ethylhexyl palmitate 10.00
Polyhydroxystearic acid 0.10
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 1071 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例１３：アイシャドウ
第１相 アウロ・ヴィスコＣＳ ７．５０（質量％）
キサンタンガム ０．０７
ジプロピレングリコール ８．００
防腐剤 適量
水 残部
第２相 酸化鉄、酸化チタン、マイカ（パール剤） ７．００
マイカ、酸化チタン、カルミン（パール剤） ３．００
シア脂 １．００
パルミチン酸エチルヘキシル １２．００
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は８１７μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 13: Eyeshadow first phase Auro Visco CS 7.50 (mass%)
Xanthan gum 0.07
Dipropylene glycol 8.00
Preservatives Appropriate amount Water Remainder 2nd phase Iron oxide, titanium oxide, mica (pearl agent) 7.00
Mica, titanium oxide, carmine (pearl agent) 3.00
Shea butter 1.00
Ethylhexyl palmitate 12.00
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 817 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例１４：アイライナー
第１相 アウロ・ヴィスコＣＳ ７．５０（質量％）
ヒドロキシエチルセルロース ０．０５
ヘキサンジオール ８．００
ポリビニルピロリドン ０．５０
防腐剤 適量
水 残部
第２相 カーボンブラック ７．００
トリエチルヘキサノイン ４．００
イソステアリン酸 ３．００
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は８１７μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 14: Eyeliner first phase Auro Visco CS 7.50 (mass%)
Hydroxyethyl cellulose 0.05
Hexanediol 8.00
Polyvinylpyrrolidone 0.50
Preservative Appropriate amount Water Residual second phase Carbon black 7.00
Triethylhexanoin 4.00
Isostearic acid 3.00
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 817 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例１５：アイライナー
第１相 アウロ・ヴィスコＣＳ ８．００（質量％）
プロピレングリコール ７．００
防腐剤 適量
水 残部
第２相 リンゴ酸ジイソステアリル ７．００
赤２２６ ０．３０
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は９２０μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 15: Eyeliner first phase Auro Visco CS 8.00 (mass%)
Propylene glycol 7.00
Preservative Appropriate amount Water Remainder 2nd phase Diisostearyl malate 7.00
Red 226 0.30
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 920 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
実施例１６：ファンデーション
第１相 アウロ・ヴィスコＣＳ ８．００（質量％）
ヒドロキシエチルセルロース ０．１０
ジプロピレングリコール ３．００
防腐剤 適量
水 残部
第２相 フッ素処理酸化チタン １．８０
フッ素処理酸化鉄（黄色） ０．２０
フッ素処理酸化鉄（赤） ０．０５
フッ素処理酸化鉄（黒） ０．０２
ポリパーフルオロイソプロピルエーテル ３．００
（合計） １００．００
調製方法：実施例１－１に同じ。
結果：油滴の平均粒子径は１０２０μｍであった。水中油型エマルション組成物においては、油滴中に粉体が含有されており、４５℃・３カ月保管後も油滴の分散安定性は良好であった。
Example 16: Foundation phase 1 Auro Visco CS 8.00 (mass%)
Hydroxyethyl cellulose 0.10
Dipropylene glycol 3.00
Preservative Appropriate amount Water Remainder 2nd phase Fluorine-treated titanium oxide 1.80
Fluorine treated iron oxide (yellow) 0.20
Fluorine treated iron oxide (red) 0.05
Fluorine treated iron oxide (black) 0.02
Polyperfluoroisopropyl ether 3.00
(Total) 100.00
Preparation method: Same as Example 1-1.
Results: The average particle size of the oil droplets was 1020 μm. In the oil-in-water emulsion composition, powder was contained in the oil droplets, and the dispersion stability of the oil droplets was good even after storage at 45° C. for 3 months.
本発明品の水中油型エマルション組成物は化粧料として利用することができる。 The oil-in-water emulsion composition of the present invention can be used as a cosmetic.
Claims (8)
下記成分（Ａ）の含有量が前記水中油型エマルション組成物の全質量に対して０．０３～２．０質量％であり、
下記成分（Ｂ）の含有量が前記水中油型エマルション組成物の全質量に対して０．１～５０．０質量％であり、
下記成分（Ｃ）の含有量が前記水中油型エマルション組成物の全質量に対して０．０１～５０．０質量％であり、
前記水中油型エマルション組成物中に含まれる界面活性剤の含有量が１．０質量％以下であり、
油滴の平均粒子径が５０μｍ以上である、水中油型エマルション組成物。
（Ａ）平均繊維幅が１０００ｎｍ以下であり、イオン性置換基を有する微細繊維状セルロース
（Ｂ）炭化水素油、エーテル油、動植物油、シリコーン油及びフッ素油から選択される少なくとも１種
（Ｃ）粉体
（Ｄ）水 An oil-in-water emulsion composition containing the following components (A) to (D),
The content of the following component (A) is 0.03 to 2.0% by mass based on the total mass of the oil-in-water emulsion composition,
The content of the following component (B) is 0.1 to 50.0% by mass based on the total mass of the oil-in-water emulsion composition,
The content of the following component (C) is 0.01 to 50.0% by mass based on the total mass of the oil-in-water emulsion composition,
The content of surfactant contained in the oil-in-water emulsion composition is 1.0% by mass or less,
An oil-in-water emulsion composition in which the average particle size of oil droplets is 50 μm or more.
(A) Fine fibrous cellulose having an average fiber width of 1000 nm or less and having ionic substituents; (B) at least one selected from hydrocarbon oils, ether oils, animal and vegetable oils, silicone oils, and fluorine oils;
(C) Powder (D) Water
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| JP2010138074A (en) | 2007-04-13 | 2010-06-24 | Dai Ichi Kogyo Seiyaku Co Ltd | Aqueous dispersion and aqueous cosmetic |
| JP2010168338A (en) | 2009-01-23 | 2010-08-05 | Daito Kasei Kogyo Kk | Oil-in-water type cosmetic |
| JP2014169266A (en) | 2013-03-01 | 2014-09-18 | Daito Kasei Kogyo Kk | Oil-in-water type cosmetic |
| JP2016074660A (en) | 2014-10-08 | 2016-05-12 | 堺化学工業株式会社 | Oil-in-water emulsion cosmetic and production method thereof |
| JP2017048142A (en) | 2015-09-01 | 2017-03-09 | 王子ホールディングス株式会社 | Cosmetic |
| WO2018212223A1 (en) | 2017-05-19 | 2018-11-22 | 株式会社 資生堂 | Oil-in-water emulsion composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010138074A (en) | 2007-04-13 | 2010-06-24 | Dai Ichi Kogyo Seiyaku Co Ltd | Aqueous dispersion and aqueous cosmetic |
| JP2010168338A (en) | 2009-01-23 | 2010-08-05 | Daito Kasei Kogyo Kk | Oil-in-water type cosmetic |
| JP2014169266A (en) | 2013-03-01 | 2014-09-18 | Daito Kasei Kogyo Kk | Oil-in-water type cosmetic |
| JP2016074660A (en) | 2014-10-08 | 2016-05-12 | 堺化学工業株式会社 | Oil-in-water emulsion cosmetic and production method thereof |
| JP2017048142A (en) | 2015-09-01 | 2017-03-09 | 王子ホールディングス株式会社 | Cosmetic |
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