JP2009203200A - Oil-in-water emulsified composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a thickening oil-in-water emulsified composition which is free from stickiness and kinkiness and excellent in emulsion stability. <P>SOLUTION: The oil-in-water emulsified composition comprises an aqueous phase containing agar microgel with an average particle size of 10-50 μm, an oily phase dispersed in the aqueous phase as emulsified particles with an average size of 1-5 μm and a powder component dispersed in the oily phase, wherein the total content of the microgel and the oily phase stands at 60-80 mass% based on the composition. In the above composition, it is preferable that the agar microgel contains one or more substances selected from succinoglycan, carboxymethylcellulose, xanthan gum and acrylamide. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to an oil-in-water emulsified composition and a method for producing the same, and more particularly to an oil-in-water emulsified composition containing a microgel and improvement of its usability.

Conventionally, as a thickening method for cosmetics, a method using a polysaccharide such as xanthan gum, a hydrophilic synthetic polymer such as polyacrylic acid, a clay mineral such as bentonite, or the like as a thickening agent is known.
However, when a polysaccharide such as xanthan gum is used as a thickening agent, although stability in a system in which a drug component and various salts are simultaneously blended is excellent, there is a problem in terms of usability such as a sticky feeling. In addition, when a hydrophilic synthetic polymer such as polyacrylic acid is used, there is no stickiness, a refreshing feeling is obtained, and the usability is good, but since salt resistance and ion resistance are low, drug components and salts When a large amount of is added, there is a problem that the viscosity of the system is lowered. Furthermore, when clay minerals such as bentonite are used as a thickener, there is a problem in terms of usability such as a squeaky feeling.
For such problems, it has been reported that a thickener obtained by microgelling a hydrophilic compound having gelling ability such as agar greatly contributes to the usability and stability of cosmetics (Patent Document 1). ).
On the other hand, in an oil-in-water emulsion composition, a fine particle powder is dispersed and blended in the inner oil phase, and a general thickener such as succinoglycan, xanthan gum and acrylamide is blended in the outer water phase. There is known a technique for thickening the emulsion and stably dispersing the fine particle powder in the aqueous phase simultaneously with the emulsified particles (Patent Documents 2 to 4).
Japanese Patent No. 3531735 Japanese Patent Laid-Open No. 2004-210698 JP 2005-225771 A JP 2005-247722 A

However, the oil-in-water emulsified composition obtained by blending the above thickener has a problem of usability due to the stickiness and kinking derived from the thickener, and the stringiness. Furthermore, when inorganic powder fine particles are blended in the inner oil phase of the oil-in-water emulsion composition, salts may be eluted from the fine particles over time to act on the thickener, thereby reducing the viscosity.
Moreover, although the said microgel has shown high evaluation about the usability, such as thickening as a thickener, stickiness, and long-term stability (no water separation), when applied to an oil-in-water emulsion composition There is still room for study regarding the influence on the dispersibility of the emulsified particles and the stability to the inorganic powder component.
The present invention has been made in view of the above problems, and an object of the present invention is to provide a thickened oil-in-water emulsion composition that is free from stickiness and distortion and has excellent emulsification stability.

As a result of intensive studies by the present inventors to solve the above problems, an oil-in-water emulsion composition containing an agar microgel having a specific particle size and emulsified particles in a specific mass range has excellent usability, And it discovered that very high emulsion stability was exhibited, and came to complete this invention.
That is, the oil-in-water emulsion composition according to the present invention is dispersed in the aqueous phase as an aqueous phase containing an agar microgel having an average particle diameter of 10 to 100 μm and emulsified particles having an average particle diameter of 0.5 to 10 μm. It contains an oil phase and a powder component dispersed in the oil phase, and the total content of the microgel and the oil phase is 60 to 80% by mass with respect to the composition.
In the oil-in-water emulsion composition, the microgel preferably contains one or more selected from succinoglycan, carboxymethylcellulose, xanthan gum, and acrylamide.
Furthermore, the method for producing an oil-in-water emulsion composition according to the present invention includes the following steps (I) to (III).
(I) A step of heating and dissolving agar in an aqueous solvent, and pulverizing it after cooling to produce an agar microgel;
(II) a step of mixing and dispersing the powder component in the oil phase component, and adding the dispersion to the aqueous phase component to produce an emulsion;
(III) A step of mixing the agar microgel of (I) and the emulsion of (II).
In the production method, it is preferable that in the step (I), at least one selected from succinoglycan, carboxymethylcellulose, xanthan gum, and acrylamide is blended in the aqueous solvent.

  According to the present invention, it is possible to obtain a thickened oil-in-water emulsified composition excellent in usability that does not cause stickiness or twist during use. Further, the composition has high stability, and does not cause water separation with time and viscosity reduction due to outflow of inorganic powder.

Hereinafter, the present invention will be described in detail.
The basic components of the oil-in-water emulsion composition according to the present invention include an aqueous phase containing an agar microgel, emulsified particles (oil phase) dispersed in the aqueous phase, and a powder component dispersed in the emulsified particles. It is.
First, each component of the oil-in-water type emulsion composition concerning this invention is demonstrated.
<Agar Microgel>
In the present invention, the agar microgel indicates a solidified agar crushed into micron units. As agar, any natural or commercially available product can be used without limitation as long as it has agarose having a high gelling power as a main component. Examples of commercially available agar include Ina Agar PS-84, Z-10, AX-30, AX-100, AX-200, T-1, S-5, and M-7 (manufactured by Ina Food Industry Co., Ltd.). Etc. can be used suitably. Further, purified agarose may be used as the agar.

Subsequently, the production of the microgel will be described.
Agar dissolves in water or an aqueous component, and is then allowed to cool and solidify to form a gel. Agar can be dissolved in water or aqueous components by mixing, heating, or the like.
Gelation (solidification) is carried out by stopping heating and leaving it to a temperature lower than the gelation temperature (solidification temperature) after dissolution.

The aqueous component is not particularly limited as long as it is an aqueous component that can be used in the cosmetics and pharmaceutical fields. For example, glycols such as 1,3-butylene glycol and propylene glycol, and lower alcohols such as ethanol and propanol. In addition, it is possible to contain components that are generally blended as an aqueous phase component of cosmetics. Specific examples include chelating agents such as metaphosphate and edetate, pH adjusting agents, preservatives, and the like, but are not limited thereto.
In the conventional oil-in-water emulsion composition, for example, when a large amount of a humectant such as glycerin is added to the aqueous phase, stickiness or the like tends to occur. On the other hand, in the oil-in-water emulsified cosmetic according to the present invention, a humectant is blended as an aqueous component of the microgel, so that a large amount can be blended without giving the system stickiness. Similarly, a component that has been difficult to be blended or blended in a large amount due to a problem with characteristics or compatibility with other components, for example, a drug such as arginine can be blended in the microgel. Thereby, the oil-in-water type emulsion composition of this invention can be provided with additional functions, such as moisture retention, according to a compounding component.

The gel strength of the gel is not particularly limited as long as the gel itself can maintain its shape and can obtain the microgel of the next step. In the invention, gels having a considerably high gel strength can be used. For example, gels having a jelly strength of 1,000 g / cm ² (day cold water measurement) or less can be used. A microgel can be obtained even with a considerably weak gel strength of about 30 g / cm ² . From the viewpoint of improving usability, a jelly strength of around 100 g / cm ² is preferable.
From the viewpoint of the jelly strength, the agar preferably has a concentration in water or an aqueous component of 0.5 to 3%. The oil-in-water emulsion composition preferably contains about 20 to 60% by mass of water or an aqueous component as a constituent of the agar microgel and about 0.1 to 2% by mass of agar.

In the present invention, it is preferable to blend one or more hydrophilic thickening compounds selected from succinoglycan, carboxymethylcellulose, xanthan gum, acrylamide, or salts thereof into the agar gel. In particular, succinoglycan or a salt thereof is preferred.
By blending the hydrophilic thickening compound in the agar gel, it is possible to improve the characteristic stickiness and spinnability that occur when the compound is blended directly into the aqueous phase, the warp that occurs during application, and the like. Further, the gel strength of the agar gel is improved, and sedimentation and water separation over time of the emulsified particles in the composition are suppressed.

In addition, since the hydrophilic thickening compound has low salt resistance, it is conventionally known that when blended into a composition together with inorganic powder particles, the viscosity is lowered by the action of the eluted salt from the particles. On the other hand, in the present invention, since the hydrophilic thickener compound is blended in the agar gel having high salt resistance, the thickening compound is not easily subjected to the action of such an elution salt.
Furthermore, since the hydrophilic thickening compound does not have a gelling ability, it is possible to adjust the gel strength of the agar gel by blending them. That is, the gel strength decreases by increasing the blending ratio of the hydrophilic thickening compound.
The blending amount of the hydrophilic thickening compound varies depending on the use of the oil-in-water emulsion composition to which the agar microgel is applied, but is preferably 0.5 to 2% by mass with respect to all the components of the agar microgel. If the blending amount is less than 0.5% by mass relative to the agar microgel, sufficient dispersion stability may not be imparted to the composition, and if it exceeds 2% by mass, stickiness may occur.

Subsequently, the formed agar gel is crushed with a homogenizer, a disper, a mechanical stirrer, etc., and a desired microgel is obtained.
The degree of crushing can be adjusted according to the purpose as long as the obtained microgel is within the above particle size range. When smoother usability is required, it should be sufficiently crushed by high-speed stirring to make a fine particle size microgel. On the other hand, when tactile feel of the microgel itself is required, the degree of crushing is reduced by light stirring. Use a microgel with a slightly larger particle size.
In particular, in the present invention, it is preferable to prepare such that the average particle size of the microgel is 10 to 100 μm. If the average particle size of the microgel is less than 10 μm, it is difficult to exhibit gelation ability. If the average particle size exceeds 100 μm, the difference in particle size between the microgel and the emulsified particles becomes too large. Becomes difficult.

The viscosity of the microgel thus obtained can be appropriately adjusted according to the use of the oil-in-water emulsion composition to be blended, but it is a B-type viscometer at an agar concentration of about 0.5 to 2% with respect to water or an aqueous component. The thing of about 2,000-1,000,000 mPa * s is preferable by the measurement by (rotational speed 0.6rpm, 25 degreeC).

<Water phase component>
A water phase component is a component which comprises the outer water phase of an oil-in-water emulsion composition, and consists of water and / or a water-soluble component. Examples of the water-soluble component include lower alcohols and polyhydric alcohols.
Examples of the lower alcohol include ethanol, propanol, isopropanol, isobutyl alcohol, t-butyl alcohol and the like.

Examples of the polyhydric alcohol include divalent alcohols (for example, ethylene glycol, propylene glycol, trimethylene glycol, 1,2-butylene glycol, 1,3-butylene glycol, tetramethylene glycol, 2,3-butylene glycol, Pentamethylene glycol, 2-butene-1,4-diol, hexylene glycol, octylene glycol, etc.); trivalent alcohol (eg, glycerin, trimethylolpropane, etc.); tetravalent alcohol (eg, 1,2,6) Pentaerythritol such as hexanetriol); pentavalent alcohol (such as xylitol); hexavalent alcohol (such as sorbitol, mannitol); polyhydric alcohol polymer (such as diethylene glycol, dipropylene glycol, triethylene glycol) ,polypropylene Glycol, tetraethylene glycol, diglycerin, polyethylene glycol, triglycerin, tetraglycerin, polyglycerin, etc.); divalent alcohol alkyl ethers (for example, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene) Glycol monophenyl ether, ethylene glycol monohexyl ether, ethylene glycol mono 2-methylhexyl ether, ethylene glycol isoamyl ether, ethylene glycol benzyl ether, ethylene glycol isopropyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, etc.) ; Dihydric alcohol alkyl ester Tellurium (for example, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol butyl ether, diethylene glycol methyl ethyl ether, triethylene glycol monomethyl ether, triethylene glycol monoethyl ether, propylene glycol monomethyl ether , Propylene glycol monoethyl ether, propylene glycol monobutyl ether, propylene glycol isopropyl ether, dipropylene glycol methyl ether, dipropylene glycol ethyl ether, dipropylene glycol butyl ether, etc.); divalent alcohol Ether esters (eg, ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol monobutyl ether acetate, ethylene glycol monophenyl ether acetate, ethylene glycol diazinate, ethylene glycol disuccinate, diethylene glycol monoethyl ether acetate, diethylene glycol) Monobutyl ether acetate, propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, propylene glycol monopropyl ether acetate, propylene glycol monophenyl ether acetate, etc .; glycerin monoalkyl ethers (eg, xyl alcohol, ceralkyl alcohol) Sugar alcohol (for example, sorbitol, maltitol, maltotriose, mannitol, sucrose, erythritol, glucose, fructose, amylolytic sugar, maltose, xylitolose, amylolytic reducing alcohol, etc.); Solid; Tetrahydrofurfuryl alcohol; POE-Tetrahydrofurfuryl alcohol; POP-butyl ether; POP / POE-butyl ether; Tripolyoxypropylene glycerin ether; POP-glycerin ether; POP-glycerin ether phosphate; POP / POE-pentaneerythritol Examples include ether and polyglycerin.
The blending amount of the water phase component in the oil-in-water emulsion composition is usually preferably 20 to 40% by mass with respect to the oil-in-water emulsion composition.

<Oil phase component>
The oil phase component is a component constituting the emulsified particles (inner oil phase) of the oil-in-water emulsion composition, and the emulsified particles have a structure in which a powder component is dispersed.
Examples of the oil phase component according to the present invention include liquid oils such as avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil , Sasanqua oil, castor oil, flaxseed oil, safflower oil, cottonseed oil, enoy oil, soybean oil, peanut oil, teaseed oil, kaya oil, rice bran oil, snail oil, Japanese kiri oil, jojoba oil, germ oil, triglycerin Etc.
Examples of the solid fat include cacao butter, palm oil, horse fat, hydrogenated palm oil, palm oil, beef tallow, sheep fat, hydrogenated beef tallow, palm kernel oil, pork fat, beef bone fat, owl kernel oil, hydrogenated oil, cattle Leg fats, moles, hydrogenated castor oil and the like.

  Examples of waxes include beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax, ibota wax, whale wax, montan wax, nuka wax, lanolin, kapok wax, lanolin acetate, liquid lanolin, sugar cane wax, lanolin fatty acid isopropyl, hexyl laurate, and reduced lanolin. , Jojoballow, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid polyethylene glycol, POE hydrogenated lanolin alcohol ether, and the like.

  Examples of the hydrocarbon oil include liquid paraffin, ozokerite, squalane, pristane, paraffin, ceresin, squalene, petrolatum, microcrystalline wax, and the like.

  Examples of the higher fatty acid include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, undecylenic acid, toluic acid, isostearic acid, linoleic acid, linolenic acid, eicosapentaenoic acid (EPA), docosahexaenoic acid ( DHA) and the like.

  Examples of the higher alcohol include linear alcohols (eg, lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol); branched chain alcohols (eg, monostearyl glycerin ether (batyl alcohol)) 2-decyltetradecinol, lanolin alcohol, cholesterol, phytosterol, hexyl decanol, isostearyl alcohol, octyldodecanol, etc.).

  Synthetic ester oils include isopropyl myristate, cetyl octanoate, octyldodecyl myristate, isopropyl palmitate, butyl stearate, hexyl laurate, myristyl myristate, decyl oleate, hexyl decyl dimethyloctanoate, cetyl lactate, myristyl lactate Lanolin acetate, isocetyl stearate, isocetyl isostearate, cholesteryl 12-hydroxystearate, ethylene glycol di-2-ethylhexanoate, dipentaerythritol fatty acid ester, monoisostearate N-alkyl glycol, neopentyl glycol dicaprate, apple Acid diisostearyl, di-2-heptylundecanoic acid glycerin, tri-2-ethylhexanoic acid trimethylolpropane, triisostearic acid trimethylo Propane, tetra-2-ethylhexanoate pentaerythritol, glycerol tri-2-ethylhexanoate, glycerol trioctanoate, glycerol triisopalmitate, trimethylolpropane triisostearate, cetyl 2-ethylhexanoate, 2-ethylhexyl palmi Tate, glyceryl trimyristate, glyceride tri-2-heptylundecanoate, castor oil fatty acid methyl ester, oleyl oleate, acetoglyceride, 2-heptylundecyl palmitate, diisobutyl adipate, N-lauroyl-L-glutamic acid-2 -Octyldodecyl ester, di-2-heptylundecyl adipate, ethyl laurate, di-2-ethylhexyl sebacate, 2-hexyldecyl myristate, 2-hexyldecyl palmitate, 2-hexyldecyl adipate , Diisopropyl sebacate, 2-ethylhexyl succinate, and triethyl citrate.

  Examples of the silicone oil include linear polysiloxanes (for example, dimethylpolysiloxane, methylphenylpolysiloxane, diphenylpolysiloxane, etc.); cyclic polysiloxanes (for example, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexyl). Silicone resins, silicone rubber, various modified polysiloxanes (amino-modified polysiloxane, polyether-modified polysiloxane, alkyl-modified polysiloxane, fluorine-modified polysiloxane, etc.), acrylic silicone And the like.

<Powder component>
Further, the present invention has a structure in which the powder component is dispersed in the emulsified particles. The powder component is not particularly limited as long as it can be dispersed in the emulsified particles, that is, the oil phase component. However, in consideration of the dispersibility in the oil phase and the ultraviolet absorption effect thereof, the powder component is particularly subjected to a hydrophobic treatment. The use of inorganic powder is preferred.
Examples of the hydrophobized powder include, for example, the surface of inorganic powder particles such as silicones such as methyl hydrogen polysiloxane and dimethyl polysiloxane, dextrin fatty acid ester, higher fatty acid, higher alcohol, fatty acid ester, metal soap, alkyl phosphorus. Hydrophobic acid ether, fluorine compound, or hydrocarbons such as squalane, paraffin, etc. that have been hydrophobized by a wet method using a solvent, a gas phase method, a mechanochemical method, etc., or after coating inorganic powder particles with silica And those subjected to hydrophobic treatment with an alkyl-modified silane coupling agent or the like.

Examples of the inorganic powder particles to be hydrophobized include, for example, titanium oxide, zinc oxide, talc, mica, sericite, kaolin, titanium mica, black iron oxide, yellow iron oxide, bengara, ultramarine blue, bitumen, chromium oxide, Examples thereof include chromium hydroxide. In the present invention, it is particularly preferable to include hydrophobized fine particle titanium dioxide and / or hydrophobized fine particle zinc oxide.
In the present invention, it is particularly preferable to apply a hydrophobized powder obtained by treating a silane coupling agent-treated powder (OTS ^™ or the like) obtained by treating inorganic powder particles with octyltriethoxysilane or the like with a cationic surfactant. .
In the present invention, considering the feature of dispersing in the oil phase component, it is preferable that the average particle size of the powder component is smaller than that of the emulsified particles. Moreover, it is preferable that the compounding quantity is 20-50 mass% with respect to all the oil phase components. If the blending amount is less than 20% by mass, a sufficient ultraviolet absorption effect may not be obtained. If the blending amount exceeds 50% by mass, the powder cannot be uniformly dispersed in the oil phase, and the particles are aggregated or into the water phase. May be allowed to escape.

The oil-in-water emulsified composition according to the present invention can be easily obtained by adding an oil phase component in which the above-described powder component is dispersed to the water phase component to emulsify, and adding an agar microgel to the obtained emulsion. Can be manufactured.
Specifically, the oil phase component including the powder component is appropriately crushed with a bead mill or the like and then dissolved by heating. Subsequently, the oil phase component is added with stirring to a mixture of water phase components heated to the same degree to obtain an emulsion. The emulsion is cooled to room temperature, agar microgel prepared in advance is added thereto, and stirred and mixed to obtain a uniform oil-in-water emulsion composition.

That is, in the oil-in-water emulsion composition of the present invention, the emulsion particles are stabilized by dispersing the agar microgel particles and the emulsion particles (oil phase) in the composition, and packing both particles closely into the composition. To maintain a dispersed state. In addition, agar microgel exhibits moderate thixotropy due to friction between gels, preventing aggregation and coalescence of the particles without interfering with the mobility of emulsified particles dispersed between the microgels, and moderate thickening in the system. Is granted.
Agar microgel does not thicken by developing a network structure in the composition like conventional thickeners such as succinoglycan, xanthan gum and acrylamide, and trapping moisture in the composition. In addition, there is no stickiness (spinning property) or twisting due to the characteristics of the polymer. Moreover, since agar with high salt resistance is used for the microgel, there is no decrease in viscosity due to the influence of salt.

  It is more preferable to prepare the emulsified particles so that the particle size is approximately the same as the microgel particle size or slightly smaller than the microgel. If there is a significant difference between the particle size of the emulsified particles and the particle size of the microgel, the microgel particles and the emulsified particles tend to be difficult to pack sufficiently densely in a uniformly dispersed state. In the present invention, the average particle size of the emulsified particles according to the particle size of the agar microgel particles is 0.5 to 10 μm. By setting the emulsified particles in this particle size range, the agar microgel and the emulsified particles take a close-packed structure in the composition. The particle size of the emulsified particles can be easily adjusted by, for example, the type of emulsifier to be selected and the stirring speed during emulsification.

  Further, in order for the agar microgel and the emulsified particles having the above particle diameter to be closely packed in the composition, the agar microgel particles and the emulsified particles may be contained in a total of 60 to 80% by mass with respect to the composition. preferable. When the blending amount of both particles is lower than 60% by mass, the particle filling rate in the composition is lowered, and sufficient emulsification stability may not be obtained. When the blending amount exceeds 80% by mass, the microgel and the emulsified particles are difficult to uniformly disperse in the composition.

  In addition, it is also possible to mix | blend a suitable powder component with agar microgel instead of an emulsified particle, and to disperse | distribute this powder component stably in a composition. In particular, since the hydrophilic powder is easily compatible with the microgel particles, sedimentation of the powder in the composition can be suppressed and excellent dispersibility can be maintained. Such an improvement in the dispersibility of the powder is considered to contribute greatly to the manifestation of SPF, transparency and the like of the powder component.

In the oil-in-water emulsion composition of the present invention, in addition to the above-described components, components that can be usually blended in cosmetics and pharmaceuticals can be appropriately blended within a range that does not impair the effect.
There are no restrictions on the components that can be added, but various surfactants, humectants, monosaccharides, oligosaccharides, organic amines, UV absorbers, antioxidants, preservatives (such as ethyl paraben and butyl paraben), and whitening agents ( For example, placenta extract, saxifrage extract, arbutin, tranexamic acid, potassium 4-methoxysalicylate, etc., various extracts (eg ginger, buckwheat, auren, shikon, birch, loquat, carrot, aloe, mallow, iris, grape , Loofah, lily, saffron, senkyu, ginger, hypericum, onionis, garlic, red pepper, chimpi, red snapper, button, seaweed, etc.) , Cholesterol derivatives, etc.), antiseborrheic agents (eg Dokishin such, thianthol, etc.), perfumes, dyes, and the like.

The oil-in-water emulsion composition according to the present invention can be made into a cosmetic by appropriately blending the above components. The form and dosage form of such cosmetics are not particularly limited. For example, in the form of aqueous, liquid, gel, cream, etc., moisturizing cream, massage cream, cosmetic liquid, lotion, milk, makeup cosmetics, It can be suitably applied to sun care products, hair cosmetics such as hair set agents and hair creams, hair dyes, body care products and the like.
Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited thereto. Unless otherwise specified, all compounding amounts are expressed in mass%.

An oil-in-water emulsion composition was produced according to the formulation shown in Table 1 below, and the stability and usability of each sample were evaluated. The results are shown in Table 1 below. In addition, the manufacturing method and evaluation criteria of a composition are as follows.
<Manufacturing method>
(Test Example 1)
Water-phase component 1 (1) to (2) and (8) to (9) are dissolved by heating, cooled to room temperature, and microgelled with a homomixer. The oil phase components (10) to (14) were mixed and dispersed and crushed with a bead mill, and then added to the aqueous phase component 2 in which (15) to (21) were dissolved by heating while applying a homomixer. Furthermore, the aqueous phase component 1 prepared in advance was added with stirring at room temperature to obtain an oil-in-water emulsion composition. The average particle size of the microgel in the composition was 30 to 50 μm, and the average particle size of the emulsified particles was 1 to 2 μm.
(Test Examples 2 to 6)
Water phase component 1 (1), (3) to (9), and water phase component 2 (15) to (21) were dissolved with heating and stirring, and oil phase components (10) to (14) were mixed. After dispersion and crushing with a bead mill, the mixture was added to the aqueous phase component while applying a homomixer to obtain an oil-in-water emulsion composition. The average particle size of the emulsified particles was 1 to 3 μm.

<Evaluation criteria>
Each sample obtained by the above manufacturing method was evaluated according to the following criteria. The results are shown in Table 1.
(Dispersion stability)
The dispersion state of the emulsified particles in each sample after 1 hour of preparation was visually observed and evaluated according to the following evaluation criteria.
○: The emulsified particles are uniformly dispersed.
Δ: Some sedimentation or coalescence of emulsified particles is observed.
X: The emulsified particles settle or coalesce and the oil phase is separated.
(Stability over time (no water separation))
The degree of water separation after storage for 1 month at 40 ° C. was visually observed and evaluated according to the following evaluation criteria.
A: No water separation is observed.
○: Almost no water separation is observed.
Δ: Slight oozing of water is observed.
X: Exudation of water is seen.
(Sticky)
Each panel was actually used by 20 panelists, and the stickiness and freeness during coating were evaluated according to the following criteria.
A: 18 or more responded that there was no stickiness (spreading) during application.
○: 15-17 respondents answered that there was no stickiness (spreading) during application.
Δ: 6 to 14 people answered that there was no stickiness (spreading) during application.
×: 5 or less responded that there was no stickiness (spreading) during application.
(Various)
A: 18 or more responded that no sag was observed during application.
○: 15-17 respondents answered that no sag was observed during application.
Δ: 6 to 14 people answered that no sag was observed during application.
X: 5 or less responded that no sag was observed during application.

(Table 1)

As can be seen from Table 1, when microgelled agar was used as the thickener, a good feeling of use without stickiness and kink was obtained (Test Example 1). On the other hand, Test Examples 2 to 4 thickened with sodium carboxymethylcellulose, succinoglycan, and xanthan gum were slightly superior in dispersion stability, but had a significant stickiness and twist.
In Test Examples 5 and 6 using acrylamide and polyacrylic acid, the emulsified particles were not uniformly dispersed. This is because when acrylamide or polyacrylic acid is used, the salt elutes from the inorganic powder fine particles (hydrophobized titanium oxide) into the aqueous phase over time, which acts on the thickener to lower the viscosity. it is conceivable that. On the other hand, in the test example using a thick salt-resistant thickener such as agar, it is considered that sedimentation of the emulsified particles was prevented over a long period of time without being affected by the elution salt.
Therefore, in an oil-in-water emulsion composition, it was recognized that emulsified particles can be uniformly dispersed without causing stickiness or twisting by blending an agar microgel. Moreover, it was suggested that the stability over time of emulsification is maintained even in a system in which inorganic powder is blended by blending a thickener having high salt resistance.

Next, the stability and usability of the oil-in-water emulsion compositions having the formulations shown in Table 2 below were evaluated, and the incorporation of succinoglycan, which had particularly high temporal stability in the above test, was examined. The results are shown in Table 2 below. In addition, the manufacturing method of a composition is as follows, and the evaluation criteria followed the said test.
(Manufacturing method)
The aqueous phase component 1 (1) to (5) was dissolved by heating, cooled to room temperature, and microgelled with a homomixer. The oil phase components (6) to (10) were mixed and dispersed and crushed with a bead mill, and then added to the water phase component 2 in which (11) to (17) were heated and dissolved while applying a homomixer. Further, the aqueous phase component 1 prepared in advance was added with stirring at room temperature. The average particle size of the microgel in the composition was 30 to 60 μm, and the average particle size of the emulsified particles was 1 to 3 μm.

(Table 2)

  As shown in Test Examples 1, 7, and 8 in Table 2 above, as glycerin was added to the agar microgel, the water separation phenomenon tended to be eliminated, but at the same time, the stickiness during application increased. It became. On the other hand, as shown in Test Examples 9 to 11, a composition in which succinoglycan showing high stability against water separation is blended with an agar microgel has both non-stickiness and stability over time regardless of the amount of glycerin added. It had been.

Subsequently, the above-described evaluation test was performed on the oil-in-water emulsion composition having the formulation shown in Table 3 below, and the addition of various thickening polymers to the microgel was examined. The results are shown in Table 3 below.
(Manufacturing method)
Water phase component 1 (1) to (9) was dissolved by heating, then cooled to room temperature, and microgelled with a homomixer. The oil phase components (10) to (15) were mixed and dispersed and crushed with a bead mill, and then added to the aqueous phase component 2 in which (16) to (21) were dissolved by heating while applying a homomixer. Further, the aqueous phase component 1 prepared in advance was added with stirring at room temperature. The average particle size of the microgel in the composition was 30 to 50 μm, and the average particle size of the emulsified particles was 1 to 3 μm.

(Table 3)

As shown in Test Examples 9 and 12 to 14 in Table 3, even when sodium carboxymethylcellulose, xanthan gum, and acrylamide were used in combination with the agar microgel, as in the case where succinoglycan was added, good without stickiness. Stability could be obtained. However, in Test Example 15 in which polyacrylate was blended, a uniform emulsion could not be obtained.
From the above results, in the present invention, it is preferable to add any of succinoglycan, carboxymethylcellulose, xanthan gum, and acrylamide to the agar microgel, and particularly succinoglycan is preferable.

<Amount of agar microgel and emulsified particles>
Subsequently, the above-described evaluation test was performed on the oil-in-water emulsion composition having the formulation shown in Table 4 below, and the blending amounts of the microgel and the emulsion particles were examined. The results are shown in Table 4 below. In addition, “microgel and oil phase” in Table 4 represents the total blending amount in the composition of the aqueous phase component 1 constituting the microgel and the oil phase component constituting the oil phase.
(Manufacturing method)
The aqueous phase component 1 (1) to (5) was dissolved by heating, cooled to room temperature, and microgelled with a homomixer. The oil phase components (6) to (10) were mixed, dispersed and crushed by a bead mill, and then added to the aqueous phase component 2 in which (16) to (21) were dissolved by heating while applying a homomixer. Further, the aqueous phase component 1 prepared in advance was added with stirring at room temperature. The average particle size of the microgel in the composition was 40 to 70 μm, and the average particle size of the emulsified particles was 1 to 3 μm.

(Table 4)

As shown in Table 4 above, excellent dispersion stability and stability over time were observed in Test Examples 17 to 19 in which the total blending amount of the microgel and the oil phase with respect to the composition was 60 to 80% by mass. On the other hand, in Test Example 16 in which the blending amount was 50% by mass and Test Example 20 in which 90% by mass was present, both dispersion stability and stability over time were inferior.
Therefore, in this invention, it is preferable that the compounding quantity of the agar microgel and the emulsified particle (oil phase) with respect to a composition is 60-80 mass%.

Hereinafter, although the suitable Example of the cosmetics using the composition of this invention is shown, this invention is not limited to these Examples at all.

Formulation Example 1: Suncut oil-in-water emulsion
(mass%)
(1) Hydrophobized titanium dioxide 5
(2) Acrylic silicone 1
(3) POE-modified methylpolysiloxane 1
(4) Decamethylpentacyclosiloxane 10
(5) Octyl paramethoxycinnamate 5
(6) PEG-60 hydrogenated castor oil 2
(7) Dynamite glycerin 6
(8) Agar 0.3
(9) Succinoglycan 0.3
(10) Ethanol 5
(11) Ion exchange water Residue (Production method)
A part of (8), (9), and (11) was heated and dissolved, then cooled to room temperature, and microgelled with a homomixer. (1) to (5) were mixed and dispersed and crushed with a bead mill, and then added to the aqueous phase in which the remainder of (6), (7), and (11) was dissolved by heating while applying a homomixer. Further, a microgel comprising a part of (8), (9), and (11) was added with stirring at room temperature, and (10) was added. The average particle size of the microgel in the composition was 40 to 60 μm, and the average particle size of the emulsified particles was 1 to 2 μm.

Formulation Example 2: Oil-in-water emulsion foundation
(mass%)
(1) Hydrophobized titanium dioxide 10
(2) Hydrophobized talc 3
(3) Hydrophobized yellow iron oxide 0.8
(4) Hydrophobized black iron oxide 0.16
(5) Hydrophobized Bengala 0.36
(6) Acrylic silicone 1
(7) POE-modified methylpolysiloxane 1
(8) Decamethylpentacyclosiloxane 10
(9) Octyl paramethoxycinnamate 5
(10) PEG-60 hydrogenated castor oil 2
(11) Dynamite glycerin 6
(12) Agar 0.3
(13) Xanthan gum 0.3
(14) Ethanol 5
(15) Ion exchange water Residue (Production method)
A part of (11) to (13) and (15) was heated and dissolved, then cooled to room temperature, and microgelled with a homomixer. (1) to (9) were mixed, dispersed and crushed with a bead mill, and then added to the aqueous phase in which the remainder of (10) and (15) was dissolved by heating while applying a homomixer. Further, a microgel composed of the remainder of (11) to (13) and (15) was added with stirring at room temperature, and (14) was added. The average particle size of the microgel in the composition was 50 to 70 μm, and the average particle size of the emulsified particles was 1 to 5 μm.

Formulation example 3: UV protection whitening serum
(mass%)
(1) Hydrophobized titanium dioxide 5
(2) ABA-type POE-modified methylpolysiloxane 1
(3) POE-modified methylpolysiloxane 1
(4) Decamethylpentacyclosiloxane 10
(5) Octyl paramethoxycinnamate 5
(6) PEG-100 hydrogenated castor oil 2
(7) Dynamite glycerin 6
(8) Agar 0.3
(9) Carboxymethylcellulose sodium 0.3
(10) Ethanol 6
(11) Citric acid appropriate amount (12) Sodium citrate appropriate amount (13) Ascorbic acid glycoside 2
(14) Caustic potash appropriate amount (15) Ion exchange water Residual (Production method)
A part of (7) to (9) and (15) was heated and dissolved, then cooled to room temperature, and microgelled with a homomixer. (1) to (5) are mixed, dispersed and crushed by a bead mill, and then subjected to a homomixer to the aqueous phase obtained by heating and dissolving the remainder of (6), (11) to (14) and (15). Added. Further, a microgel composed of the remainder of (7) to (9) and (15) was added with stirring at room temperature, and (14) was added. The average particle size of the microgel in the composition was 50 to 70 μm, and the average particle size of the emulsified particles was 1 to 5 μm.

  None of the above cosmetics were sticky or kinky, had a fresh and fresh feel, and had excellent dispersion stability and stability over time.

Claims (4)

An aqueous phase containing an agar microgel having an average particle size of 10 to 100 μm;
An oil phase dispersed in the aqueous phase as emulsified particles having an average particle size of 0.5 to 10 μm;
A powder component dispersed in the oil phase,
The oil-in-water emulsion composition, wherein the total content of the microgel and the oil phase is 60 to 80% by mass with respect to the composition.   The oil-in-water emulsion composition according to claim 1, wherein the agar microgel contains one or more selected from succinoglycan, carboxymethylcellulose, xanthan gum, and acrylamide. The manufacturing method of the oil-in-water type emulsion composition characterized by including the following process (I)-(III).
(I) A step of heating and dissolving agar in an aqueous solvent, and pulverizing it after cooling to produce an agar microgel;
(II) a step of mixing and dispersing the powder component in the oil phase component, and adding the dispersion to the aqueous phase component to produce an emulsion;
(III) A step of mixing the agar microgel of (I) and the emulsion of (II).   In the said process (I), 1 or more types selected from succinoglycan, carboxymethylcellulose, a xanthan gum, and acrylamide are mix | blended in an aqueous solvent, The manufacture of the oil-in-water-type emulsion composition of Claim 3 characterized by the above-mentioned. Method.