HK1141713B - Oil-in-water emulsion composition and method for producing the same - Google Patents

Description

Oil-in-water type emulsion composition and method for producing the same

Related application

The present application claims priority from Japanese patent application No. 2007-116809 applied on 26.4.2007, the contents of which are hereby incorporated by reference.

Technical Field

The present invention relates to an oil-in-water emulsion composition, and particularly to an oil-in-water emulsion composition having excellent emulsion stability and a method for producing the same.

Background

An oil-in-water emulsion used in cosmetics and the like stably mixes an aqueous component and an oily component by emulsification of an added surfactant.

On the other hand, with the increase in consumers who pay more attention to safety in recent years, there is an increasing demand for oil-in-water type emulsions which do not contain a surfactant which may be irritating in a small amount or in a content which does not have such irritation, due to extremely allergic users.

Pickering emulsions (Pickering emulsions) have been known in the past which are prepared by adsorbing a powder on an interface without using a surfactant. Many studies have been reported so far for the preparation of pickering emulsions (for example, non-patent document 1), and their application to the field of cosmetics has been proposed (patent documents 1 and 2).

In recent years, a stable oil-in-water emulsion composition has been obtained by emulsifying an oil phase containing an amphiphilic substance such as ceramide by using a specific cationic surfactant and a polyhydric alcohol in combination with a powder (see patent document 3).

Patent document 1: japanese patent No. 2656226

Patent document 2: japanese Kohyo publication No. 2001-518111

Patent document 3: japanese laid-open patent publication No. 2006-36763

Non-patent document 1: B.Binks et al, Advances in Colloid and interface science 100-

Disclosure of Invention

However, it is very difficult to prepare an oil-in-water type pickering emulsion having stability against temperature or stirring under various environments, which is necessary for applying the emulsion to cosmetics.

Further, in patent document 3, an amphiphilic substance is essential, and a surfactant and a liquid crystal structure (α gel) are formed, whereby the system is stabilized, but there is a tendency that the system is sticky in terms of usability. In order to obtain a pickering emulsion, a technique of blending a trace amount of an amphiphilic substance has been reported so far (for example, Mukul M, Sharma et al, Journal of Colloid and interface science 157, 244-253, (1993)), but it is difficult to obtain a product satisfying sufficient stability as a cosmetic, and there is a problem in a new use touch such as stickiness of a preparation due to the amphiphilic substance.

The present invention has been made in view of the above problems, and an object of the present invention is to provide an oil-in-water emulsion composition having excellent emulsion stability, less sticky feeling, and low skin irritation, and a simple method for producing the same.

As a result of intensive studies to achieve the above object, the present inventors have found that an oil-in-water emulsion having a specific structure formed from specific amounts of a powder, an oil phase component, an aqueous phase component, and a cationic surfactant containing 2 alkyl groups having a chain length in a specific range has excellent emulsion stability, no sticky feeling, and low irritation, and have completed the present invention.

Further, the present inventors have found that the oil-in-water type emulsion composition can be easily obtained without separately treating the powder by incorporating the cationic surfactant treatment to the powder into the preparation step of the emulsion composition in the preparation of the emulsion composition.

That is, the first aspect of the present invention is an oil-in-water emulsion composition containing (a) 1 to 20% by mass of a powder component, (b) 0.001 to 0.5% by mass of a cationic surfactant having two alkyl chains with 12 to 22 carbon chains, (c) an oil phase component, and (d) an aqueous phase component, and having a structure in which powder particles of (a) are adsorbed on oil droplets dispersed in an aqueous phase.

The oil-in-water emulsion composition is characterized in that the cationic surfactant (b) is adsorbed on the powder particles (a).

The oil-in-water emulsion composition preferably contains the cationic surfactant (b) in an amount of 0.001 to 0.1% by mass in total.

In the oil-in-water emulsion composition, the cationic surfactant (b) is preferably dimethyldialkylammonium chloride.

The oil-in-water emulsion composition preferably contains 1 or 2 or more kinds selected from succinoglycan, xanthan gum and acrylamide as the aqueous phase component of (d).

The oil-in-water emulsion composition preferably contains 0.001 to 0.5 mass% of a hydrophilic surfactant in an aqueous phase.

Further, the method for producing the oil-in-water emulsion composition is characterized by comprising the following steps (a) and (B).

(A) A step of dispersing a powder component and a cationic surfactant having 2 alkyl chains with carbon chains of 12 to 22 in an aqueous phase component,

(B) and (A) mixing the dispersion with an oil phase component.

The method for producing the oil-in-water emulsion composition is characterized by further comprising the following step (C).

(C) And (B) adding and mixing a hydrophilic surfactant after the step (B).

A second aspect of the present invention is a skin external preparation for sunscreen, which comprises the oil-in-water emulsion composition described above, and further comprises a hydrophobized powder dispersed in the oil phase component of (c).

In the oil-in-water type sunscreen skin external preparation, it is preferable that the hydrophobized powder contains a hydrophobized particulate titanium dioxide and/or a hydrophobized particulate zinc oxide.

A third aspect of the present invention is a cosmetic composition containing the oil-in-water emulsion composition, further containing a hydrophobized powder dispersed in the oil phase component of (c), wherein 50% by mass or more of the oil phase component is a silicone oil.

In the cosmetic composition, the hydrophobized powder preferably contains 1 or 2 or more kinds selected from the group consisting of hydrophobized fine particulate titanium dioxide, red iron oxide, yellow iron oxide, black iron oxide, and aluminum oxide.

Further, the cosmetic composition preferably contains 1 or 2 or more kinds of acrylic silicone represented by the following general formula (I).

(chemical formula 1)

(wherein R is an alkyl group having 10 to 20 carbon atoms, a + b + c is 1, a, b and c are each 0.2 or more, and d is an integer of 5 to 100.)

Further, the cosmetic composition preferably contains 1 or 2 or more kinds of both-terminal silicone-modified glycerin represented by the following general formula (II).

(chemical formula 2)

(in the above formula, R1 represents a C1-12 linear or branched alkyl group or a phenyl group, R2 represents a C2-11 alkylene group, m represents 10-120, and n represents 1-11.)

A fourth aspect of the present invention is a hair cosmetic for hair styling, which contains the oil-in-water emulsion composition, wherein the oil-phase component of (c) of the oil-in-water emulsion composition contains 1 to 30% by mass of a solid oil component and 1 to 30% by mass of a liquid oil component.

In the hair cosmetic composition for hair styling, the powder component of (a) preferably contains silica.

According to the present invention, an oil-in-water emulsion composition having excellent emulsion stability can be obtained easily. Further, by blending the above composition, a sunscreen skin external preparation, a cosmetic composition and a hair cosmetic for hair styling having high functionality can be obtained.

Drawings

FIG. 1 is a phase diagram of dialkylmethylammonium chloride in a two-component system with water.

FIG. 2 shows the preparation of silica-coated titanium oxide by changing the amount of dimethyldistearylammonium chloride: 3 wt%, oil content: 47 wt%, water: the residual amount of the oil-in-water emulsion composition is shown by measuring the zeta potential of the silica-coated titanium oxide powder dispersed in water together with dimethyldistearylammonium chloride.

Detailed Description

The following describes specific embodiments of the present invention.

First, an oil-in-water type emulsion composition according to a first embodiment of the present invention will be described.

The oil-in-water emulsion composition of the present invention contains a specific amount of a cationic surfactant having 2 alkyl groups of a specific chain length, in addition to the oil phase, the water phase and the powder components which constitute the conventional pickering emulsion.

(double-chain cationic surfactant)

The alkyl chain of the double-chain cationic surfactant of the present invention may be linear or branched, and may be different. Examples of the double-chain type cation contained in the oil-in-water emulsion of the present invention include dimethyl dilauryl ammonium chloride, diethyl dilauryl ammonium chloride, dipropyl dilauryl ammonium chloride, dimethyl dipalmityl ammonium chloride, diethyl dipalmityl ammonium chloride, dipropyl dipalmityl ammonium chloride, dimethyl dicetyl ammonium chloride, diethyl dicetyl ammonium chloride, dipropyl dicetyl ammonium chloride, dimethyl distearyl ammonium chloride, diethyl distearyl ammonium chloride, dipropyl distearyl ammonium chloride, dimethyl di (behenyl) ammonium chloride, diethyl di (behenyl) ammonium chloride, dipropyl di (behenyl) ammonium chloride, distearyl dimethyl ammonium chloride, dipalmitoyl ethyl dimethyl ammonium chloride, distearyl ethyl hydroxyethyl methyl ammonium methyl sulfate (distearoyl hydroxyethyl methyl ammonium methyl sulfate), Dipalmitoylethyl hydroxyethylmethyl ammonium methosulfate (dipalmitoylethyl hydroxyethylammonium methosulfate), and the like.

The length of the alkyl chain of the double-chain cationic surfactant in the oil-in-water emulsion composition of the present invention is preferably 12 to 22. When the amount is less than 12, the emulsifying power and the emulsion stability are problematic, and when the amount exceeds 22, the sticky feeling is increased, which causes a problem in terms of handling.

The length of the alkyl chain of the double-chain cationic surfactant is more preferably 16 to 20. The double-chain cationic surfactant of the oil-in-water emulsion composition of the present invention is preferably dimethyldialkylammonium chloride.

The amount of the double-chain cationic surfactant to be incorporated in the oil-in-water emulsion composition of the present invention is 0.001 to 0.5% by mass, preferably 0.001 to 0.1% by mass, based on the total amount of the emulsion. When the amount of the double-chain cationic surfactant is too large, the composition becomes a gel and sticky, and the feeling of use tends to be reduced.

In general, when a surfactant of the above-mentioned level is blended, a trace amount thereof exceeds an amount which functions as an emulsifier in an emulsion composition, but exhibits an extremely excellent emulsion stabilizing function in a pickering emulsion having the structure of the present invention. In addition, the irritation was also extremely low.

(powder component)

Examples of the powder component contained in the oil-in-water type emulsion composition of the present invention include inorganic powders (for example, talc, kaolin, mica, sericite (sericite), muscovite, phlogopite, synthetic mica, lepidolite, biotite, vermiculite, magnesium carbonate, calcium carbonate, aluminum silicate, barium silicate, calcium silicate, magnesium silicate, strontium silicate, metal tungstate, magnesium, silica, zeolite, barium sulfate, sintered calcium sulfate (calcined gypsum), calcium phosphate, fluorapatite, hydroxyapatite, ceramic powder, etc.), metal soaps (for example, zinc myristate, calcium palmitate, aluminum stearate), boron nitride, etc.), organic powders (for example, titanium dioxide, zinc oxide, etc.), inorganic red pigments (for example, iron titanate, etc.), inorganic violet pigments (for example, mangoviole, cobalt violet, etc.), inorganic green pigments (for example, chromium oxide, chromium hydroxide, cobalt titanate, etc.), inorganic blue pigments (e.g., ultramarine blue, prussian blue, etc.), pearlescent pigments (e.g., titanium oxide-coated mica, titanium oxide-coated bismuth oxychloride, titanium oxide-coated talc, colored titanium oxide-coated mica, bismuth oxychloride, perlite, etc.), metal powder pigments (e.g., aluminum powder, copper powder, etc.), organic pigments such as zirconium, barium, or aluminum lake (e.g., organic pigments such as red 201, red 202, red 204, red 205, red 220, red 226, red 228, red 405, orange 203, orange 204, yellow 205, yellow 401, and blue 404, red 3, red 104, red 106, red 227, red 230, red 401, red 505, orange 205, yellow 4, yellow 5, yellow 202, yellow 203, orange 205, yellow 203, yellow 104, red 106, red 227, red 230, red 401, red 505, orange 205, yellow 4, yellow 5, yellow 202, yellow 203, blue 203, Green No. 3, blue No. 1, etc.), natural pigments (e.g., chlorophyll, β -carotene, etc.), etc., and the like, may be used alone or in combination of 2 or more. In addition, a composite powder obtained by coating a powder with a metal oxide or the like, or a modified powder obtained by treating the surface of a powder with a compound or the like can also be used.

In the present invention, silica, titanium dioxide, zinc oxide, or a composite powder containing these is preferably used, and silica-coated zinc oxide and silica-coated titanium oxide are particularly preferable from the viewpoints of skin compatibility, usability, uv shielding effect, and emulsion stability.

The particle size of the powder is not particularly limited, but is preferably 1 to 200nm in view of ease of handling and emulsion stability when incorporated into an aromatic cosmetic.

The amount of the powder component to be incorporated in the oil-in-water emulsion of the present invention is preferably 1 to 20% by mass, and particularly preferably 1 to 10% by mass, based on the total amount of the oil-in-water emulsion composition. If the blending amount is less than 1% by mass, emulsification may not be sufficiently performed, and if it exceeds 20% by mass, sticky feeling tends to be improved.

(oil phase component)

The oil phase component contained in the oil-in-water emulsion composition of the present invention includes the following components.

Examples of the liquid oil and fat include avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg butter oil, sesame oil, persic oil, wheat germ oil, camellia oil, castor oil, linseed oil, safflower oil, cottonseed oil, perilla oil, soybean oil, peanut oil, tea seed oil, coconut oil, rice bran oil, china tung oil, japanese tung oil, jojoba oil, germ oil, and triglycerin.

Examples of the solid fat and oil include cacao butter, coconut oil, horse fat, hydrogenated coconut oil, palm oil, beef tallow, mutton tallow, hydrogenated beef tallow, palm kernel oil, lard, beef bone fat, beeswax kernel oil, hydrogenated oil, beef foot fat, beeswax, hydrogenated castor oil, and the like.

Examples of the waxes include beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax (bayberry wax), insect wax, spermaceti wax, montan wax, bran wax, lanolin, kapok wax, lanolin acetate, liquid lanolin, sugar cane wax, isopropyl lanolin fatty acid ester, hexyl laurate, reduced lanolin, jojoba wax, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid polyethylene glycol, and POE hydrogenated lanolin alcohol ether.

Examples of the hydrocarbon oil include liquid paraffin, natural ceresin, squalane, pristane, paraffin, purified ceresin, squalene, vaseline, and microcrystalline wax.

Examples of the higher fatty acid include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, undecylenic acid, tall oil acid (ト - ル acid), isostearic acid, linoleic acid, linolenic acid, eicosapentaenoic acid (EPA), and docosahexaenoic acid (DHA).

Examples of the higher alcohol include a straight-chain alcohol (e.g., lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, etc.), a branched-chain alcohol (e.g., monostearyl glyceryl ether (batyl alcohol), 2-decyltetradecyl alcohol, lanolin alcohol, cholesterol, phytosterol, hexyldodecanol, isostearyl alcohol, octyldodecanol, etc.), and the like.

Examples of the synthetic ester oil include isopropyl myristate, cetyl octanoate, octyldodecyl myristate, isopropyl palmitate, butyl stearate, hexyl laurate, myristyl myristate, decyl oleate, hexyldecyl dimethyloctanoate, cetyl lactate, myristyl lactate, lanolin acetate, isocetyl stearate, isocetyl isostearate, cholesteryl 12-hydroxystearate, ethylene glycol di-2-ethylhexanoate, dipentaerythritol fatty acid ester, N-alkylethylene glycol monoisostearate (モノイソステアリル acid N- アルキルグリコ - ル), neopentyl glycol didecanoate, diisostearyl malate, di-2-heptylundecyl glyceride, trimethylolpropane tri-2-ethylhexanoate, trimethylolpropane triisostearate, trimethylolpropane myristate, isopropyl myristate, hexyl myristate, decyl myristate, hexyl lactate, lanolin, isopropyl stearate, isocetyl isostearate, ethylene glycol diisostearyl stearate, glycerol di-2-heptylundecanoate, Pentaerythritol tetra-2-ethylhexanoate, glycerol tri-2-ethylhexanoate, glycerol trioctanoate, glycerol triisopalmitate, trimethylolpropane triisostearate, cetyl 2-ethylhexanoate, 2-ethylhexyl palmitate, glycerol trimyristate, glycerol tri-2-heptyl undecanoate, methyl ricinoleate, oleyl oleate, acetyl glycerol, 2-heptyl undecyl palmitate, diisobutyl adipate, 2-octyl dodecyl N-lauroyl-L-glutamate, di-2-heptyl undecyl adipate, ethyl laurate, di-2-ethylhexyl sebacate, 2-hexyl decanomyristate, 2-hexyl decanopalmitate, glycerol tri-2-ethylhexanoate, glycerol tri-2-heptyl undecanoate, methyl ricinoleate, oleyl oleate, acetyl glycerol, 2-heptyl undecyl palmitate, diisobutyl adipate, 2-octyl dodecanoate, di-2-heptyl undecyl adipate, ethyl laurate, di-2-ethylhexyl sebacate, 2-hexyl decanoate, 2-hexyldecyl adipate, diisopropyl sebacate, 2-ethylhexyl succinate, triethyl citrate, and the like.

Examples of the silicone oil include chain polysiloxanes (e.g., dimethylpolysiloxane, methylphenylpolysiloxane, diphenylpolysiloxane, etc.), cyclic polysiloxanes (e.g., octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, etc.), silicone resins having a three-dimensional network structure, silicone rubbers, various modified polysiloxanes (e.g., amino-modified polysiloxane, polyether-modified polysiloxane, alkyl-modified polysiloxane, fluorine-modified polysiloxane, etc.), acrylic silicones, and the like.

(Water phase component)

In the present invention, the aqueous phase component contains, in addition to water, a lower alcohol, a polyhydric alcohol, and the like.

Examples of the lower alcohol include ethanol, propanol, isopropanol, isobutanol, and tert-butanol.

Examples of the polyhydric alcohol include dihydric alcohols (e.g., ethylene glycol, propylene glycol, trimethylene glycol, 1, 2-butanediol, 1, 3-butanediol, tetramethylene glycol, 2, 3-butanediol, pentamethylene glycol, 2-butene-1, 4-diol, hexanediol, octanediol, etc.), trihydric alcohols (e.g., glycerin, trimethylolpropane, etc.), tetrahydric alcohols (e.g., pentaerythritol, such as 1, 2, 6-hexanetriol, etc.), pentahydric alcohols (e.g., xylitol, etc.), hexahydric alcohols (e.g., sorbitol, mannitol, etc.), polyhydric alcohol polymers (e.g., diethylene glycol, dipropylene glycol, triethylene glycol, polypropylene glycol, tetraethylene glycol, diglycerol, polyethylene glycol, triglycerol, tetraglycerol, polyglycerols, etc.), glycol alkyl ethers (e.g., ethylene glycol monomethyl ether, propylene glycol ether, propylene, 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.), glycol alkyl ethers (e.g., 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.), glycol ether esters (e.g., ethylene glycol monomethyl ether acetate, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, etc.), ethylene glycol monoethyl ether acetate, ethylene glycol monobutyl ether acetate, ethylene glycol monophenyl ether acetate, ethylene glycol diadipate, 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.), glycerol monoalkyl ethers (e.g., chimyl alcohol, batyl alcohol, etc.), sugar alcohols (e.g., sorbitol, maltitol, maltotriose, mannitol, sucrose, erythritol, glucose, fructose, amylolytic sugars, maltose, xylose, amylolysis, etc. reducing alcohols), Glysolid (グリソリツド), tetrahydrofurfuryl alcohol, POE-tetrahydrofurfuryl alcohol, POP-butyl ether, POP-POE-butyl ether, polyoxypropylene glyceryl ether, POP-glycerol ether, POP-glycerol ether phosphoric acid, POP-POE-pentaerythritol ether, polyglycerol, and the like.

In the oil-in-water type emulsion composition of the present invention, it is particularly preferable to blend a thickener having salt resistance, particularly succinoglycan, xanthan gum or acrylamide, in order to impart stability against sedimentation and creaming of emulsion oil droplets with time and further stability against aggregation of powder. When a general thickener is used, there is a possibility that salts slowly eluted from the hydrophobized powder into the aqueous phase with the lapse of time act on the thickener to lower the viscosity, but when a thickener having excellent salt resistance such as succinoglycan is used, the sedimentation of emulsified particles can be prevented for a long period of time without being affected by the eluted salts.

The preferred amount of the thickener when added is preferably 0.01 to 5% by mass based on the total amount of the external preparation for skin.

The oil-in-water type emulsion composition of the present invention contains the above components to form a so-called pickering emulsion.

Pickering emulsion (Pickering emulsion) is known as an O/P/W type emulsion in which an oil phase is uniformly dispersed in an aqueous phase by fine particles (Powder) in an oil-in-water type dispersion. In the present invention, a cationic surfactant having a specific structure is applied to the emulsion to enhance the emulsion stability by the powder.

The structure of the oil-in-water emulsion composition according to the present invention will be described below based on the production method thereof.

In the preparation method of the present invention, it is necessary to preliminarily prepare a cationic surfactant having two alkyl chains with carbon chains of 12 to 22 as an aqueous dispersion having a lamellar liquid crystal structure before the emulsification step. Similarly, the powder component is uniformly dispersed in water in advance before emulsification.

As a specific method, for example, a powder component and a cationic surfactant are added to water, and a uniform aqueous dispersion of a layered structure and powder is formed by a homomixer, ultrasonic treatment, or the like. Alternatively, the powder component and the cationic surfactant may be dispersed in a part of water and then mixed. In these steps, other aqueous phase components may also be added and mixed.

The cationic surfactant with two alkyl chains with 12-22 carbon chains used in the invention forms a lipophilic-associated lamellar liquid crystal structure in water within a wide concentration and temperature range. For example, dialkylmethylammonium chloride is known to have a liquid crystal structure shown in fig. 1 at a low concentration in a two-component system with water. In the present invention, it is particularly preferable that the cationic surfactant is in a state corresponding to a water/liquid crystal stable dispersion phase (water/liquid crystal dispersion) in fig. 1, that is, a state in which a small lamellar structure of the cationic surfactant is dispersed in water.

When the cationic surfactant in the lamellar liquid crystal state is dispersed in the same water system as the powder component, the hydrophilic group of the positively charged liquid crystal is generally adsorbed on the surface of the negatively charged powder particle. It is considered that by dispersing the surfactant particles by an appropriate treatment, a dispersion of numerous liquid-crystalline surfactant powder particles is produced.

FIG. 2 shows the preparation of silica-coated titanium oxide by changing the amount of dimethyldistearylammonium chloride: 3 wt%, oil content: 47 wt%, water: the residual amount of the oil-in-water emulsion composition is shown by measuring the zeta potential of the silica-coated titanium oxide powder dispersed in water together with dimethyldistearylammonium chloride. As shown in fig. 2, as the concentration of the cationic surfactant increases, the zeta potential, which indicates the surface potential of the powder, moves in the positive direction, and therefore it is presumed that dimethyldistearylammonium chloride having a cationic group is adsorbed onto the surface of the powder. As is clear from fig. 2, the higher the cationic surfactant is blended with the powder, the larger the adsorption amount is, but if the blending amount is too high, the phase inversion may be water-in-oil type at the time of emulsification. Therefore, in the present invention, the ratio of the specific cationic surfactant to the powder component depends on other formulation components, but is preferably about 5: 0.001 to 5: 1.

After the above-mentioned step, the oil-in-water type emulsion composition according to the present invention can be obtained by adding an oil phase component to the obtained dispersion of the cationic surfactant-adsorbed powder particles and emulsifying the mixture with an emulsifying machine or the like. The addition of the oil phase component may be carried out under heating as necessary, and may be carried out in advance by a treatment such as pre-crushing depending on the state of the oil phase component.

That is, the present invention is an O/P/W type emulsion in which an oil phase is uniformly dispersed in an aqueous phase by fine particles having a specific cationic surfactant adsorbed thereon.

It is considered that the added oil component enters the lipophilic group-associated portion of the lamellar liquid crystal adsorbed on the powder, and forms oil droplets adsorbing the powder particles at the interface with the aqueous phase. It is presumed that, at this time, the adsorption of the oil droplets by the powder is enhanced by the action of the specific cationic surfactant, and a composition having excellent emulsion stability can be obtained as compared with a conventional O/P/W emulsion in which oil droplets are dispersed only by the adsorption force of the powder.

It is considered that the emulsion composition of the present invention has a structure in which powder particles are adsorbed on oil droplets dispersed in an aqueous phase, and a cationic surfactant is further adsorbed on the powder particles.

In the method for producing the oil-in-water type emulsion composition according to the present invention, as described above, it is preferable that the specific cationic surfactant in a liquid crystal state is adsorbed to the powder in advance before emulsification of the aqueous phase and the oil phase is performed. The addition of the cationic surfactant during or after emulsification does not provide a sufficient improvement in the emulsified state and emulsion stability.

(other Components)

The oil-in-water composition according to the present invention may contain a hydrophilic surfactant and/or a lipophilic surfactant in an amount that does not impair the pickering emulsion. The hydrophilic surfactant contributes to the elimination of the rough feeling accompanying the emulsification of the powder and the improvement of the skin-friendly feeling, and the lipophilic surfactant contributes to the improvement of the stability of the emulsion over time.

When the hydrophilic surfactant is blended, it is preferable to form an O/P/W emulsion from the above-mentioned essential components and then add and mix the hydrophilic surfactant to the external aqueous phase of the emulsion. The amount of the hydrophilic surfactant added at this time is preferably 0.001 to 0.5% by mass based on the composition. By adding the hydrophilic surfactant in a low blending amount after the emulsification step, the rough feeling due to the emulsion can be relieved without causing the surfactant to act on the structure of the O/P/W type emulsion.

Examples of the hydrophilic surfactant that can be blended include glycerin or polyglycerin fatty acid esters, propylene glycol fatty acid esters, POE sorbitan fatty acid esters, POE sorbitol fatty acid esters, POE glycerin fatty acid esters, POE alkyl ethers, POE alkylphenyl ethers, POE-POP alkyl ethers, POE castor oil or POE hydrogenated castor oil derivatives, POE beeswax-lanolin derivatives, alkanolamides, POE propylene glycol fatty acid esters, POE alkylamines, POE fatty acid amides, polyoxyethylene alkyl ether sulfates, alkylamides, and the like, and 1 or a combination of 2 or more of these may be blended.

The lipophilic surfactant may be added as an oil phase component during the preparation of the O/P/W emulsion. When the lipophilic surfactant is blended, the amount of the lipophilic surfactant is in a range in which the lipophilic surfactant does not function as an emulsifier, that is, about 0.01 to 5% by mass relative to the composition. The O/P/W emulsion according to the present invention has a structure in which, as described above, a powder of lamellar liquid crystal having a specific cationic surfactant adsorbed on the surface thereof is emulsified in advance, thereby forming oil droplets having high stability in which the powder particles are adsorbed on the surface thereof by the surfactant. Therefore, the lipophilic surfactant dissolved in the oil does not affect the powder emulsification even when added in a small amount as an oil phase component, and the lipophilic surfactant itself hardly participates in the emulsification. On the other hand, an emulsion having high stability over time can be obtained by dissolving a lipophilic surfactant in emulsified oil droplets (oil phase).

Examples of the lipophilic surfactant which can be blended include sorbitan fatty acid esters such as sorbitan monooleate, sorbitan monoisostearate, sorbitan monopalmitate, sorbitan sesquioleate, sorbitan trioleate and diglycerin sorbitan penta-2-ethylhexanoate, glycerol or polyglycerol fatty acid esters such as glycerol monoerucate, glycerol sesquioleate, glycerol monostearate, diglycerol monostearate and glycerol monostearate malic acid, lipophilic sucrose fatty acid esters such as sucrose polyerucate, sucrose polyacylate and sucrose polyisostearate, propylene glycol fatty acid esters such as propylene glycol monostearate, hydrogenated castor oil derivatives, glycerol alkyl ethers, polyether-modified silicones, cetyl alcohol, stearyl alcohol, and the like, Aliphatic alcohols such as behenyl alcohol, and the like, and 1 or a combination of 2 or more thereof may be used.

Further, the oil-in-water emulsion composition of the present invention may be prepared by a conventional method by blending components generally used in cosmetics and quasi drugs, in addition to the above components, in such an amount that the effects thereof are not impaired. The ingredients that can be blended are not limited, and examples thereof include a humectant, a monosaccharide, an oligosaccharide, an organic amine, an ultraviolet absorber, an antioxidant, a preservative (e.g., ethyl p-hydroxybenzoate, butyl p-hydroxybenzoate), a whitening agent (e.g., saxifrage extract, arbutin, tranexamic acid, 4-methoxysalicylate), various extracts (e.g., ginger, phellodendron, coptis, gromwell, white birch, loquat, carrot, aloe, mallow, iris, grape, luffa, lily, saffron, chuanxiong rhizome, pinecone, hypericum perforatum, formononetin, garlic, capsicum, tangerine peel, angelica, peony, seaweed, etc.), an activator (e.g., panthenyl ethyl ether, nicotinamide, biotin, pantothenic acid, royal jelly, cholesterol derivatives, etc.), an antiseborrheic agent (e, pyridoxine, dimethyl thianthrene, etc.), a perfume, etc, Pigments, and the like.

Examples of the humectant include, in addition to the polyhydric alcohol, chondroitin sulfate, hyaluronic acid, mucopolysaccharide sulfate, カロニン acid (charonin acid), atelocollagen (atelocollagen), cholesterol-12-hydroxystearate, sodium lactate, bile acid salts, dl-pyrrolidone carboxylate, short-chain soluble collagen, diglycerol (EO) PO adduct, rosa roxburghii extract, achillea millefolium extract, and melilotus officinalis extract.

Examples of the monosaccharide include a three-carbon sugar (e.g., D-glyceraldehyde, dihydroxyacetone, etc.), a four-carbon sugar (e.g., D-erythrose, D-erythrulose, D-threose, erythritol, etc.), a five-carbon sugar (e.g., L-arabinose, D-xylose, L-lyxose, D-arabinose, D-ribose, D-ribulose, D-xylulose, L-xylulose, etc.), a six-carbon sugar (e.g., D-glucose, D-talose, D-psicose, D-galactose, D-fructose, L-galactose, L-mannose, D-tagatose, etc.), a seven-carbon sugar (e.g., heptose, heptulose, etc.), an eight-carbon sugar (e.g., octulose, etc.), a deoxy sugar (e.g., 2-deoxy-D-ribose, D-galactose, L-mannose, D-tagatose, etc.), a D-arabinose (e.g, 6-deoxy-L-galactose, 6-deoxy-L-mannose, etc.), amino sugars (e.g., D-glucosamine, D-galactosamine, sialic acid, aminouronic acid, muramic acid, etc.), uronic acids (e.g., D-glucuronic acid, D-mannuronic acid, L-guluronic acid, D-galacturonic acid, L-iduronic acid, etc.), etc.

Examples of the oligosaccharide include sucrose, gentiotriose, umbelliferose, lactose, psyllium sugar, iso-perillaose, α -trehalose, raffinose, perillaose, umbilicin, stachyose, and verbascose.

Examples of the amino acid include neutral amino acids (e.g., threonine and cysteine), basic amino acids (e.g., hydroxylysine), and the like. Examples of the amino acid derivative include sodium acyl sarcosinate (sodium lauroyl sarcosinate), acyl glutamate, sodium acyl β -alanine, glutathione, pyrrolidone carboxylic acid, and the like.

Examples of the organic amine include monoethanolamine, diethanolamine, triethanolamine, morpholine, triisopropanolamine, 2-amino-2-methyl-1, 3-propanediol, and 2-amino-2-methyl-1-propanol.

As the ultraviolet absorber of the organic compound, for example, benzoic acid-based ultraviolet absorbers (for example, p-aminobenzoic acid (hereinafter abbreviated as PABA), PABA monoglyceride, N-dipropoxypPABA ethyl ester, N-diethoxypPABA ethyl ester, N-dimethylpPABA butyl ester, N-dimethylpPABA ethyl ester and the like), anthranilic acid-based ultraviolet absorbers (for example, N-acetylanthranilic acid homoaminobenzoic acid)Esters, etc.), salicylic acid-based ultraviolet absorbers (e.g., amyl salicylate, salicylic acid)High in ester and salicylic acidEsters, octyl salicylate, phenyl salicylate, benzyl salicylate, p-isopropanolphenyl salicylate, etc.), cinnamic acid-type ultraviolet absorbers (e.g., octyl cinnamate, ethyl-4-isopropyl cinnamate, methyl-2, 5-diisopropyl cinnamate, ethyl-2, 4-diisopropyl cinnamate, methyl-2, 4-diisopropyl cinnamate, etc.), cinnamic acid-type ultraviolet absorbers (e.g., ethyl cinnamate, ethyl-4-isopropyl cinnamate, p-isopropyl salicylate, etc.), cinnamic acid-type ultraviolet absorbers, cinnamic acid esters, cinnamic acidIsopropyl cinnamate, propyl-p-methoxycinnamate, isopropyl-p-methoxycinnamate, isopentyl-p-methoxycinnamate, octyl-p-methoxycinnamate (2-ethylhexyl-p-methoxycinnamate), 2-ethoxyethyl-p-methoxycinnamate, cyclohexyl-p-methoxycinnamate, ethyl- α -cyano- β -phenyl cinnamate, 2-ethylhexyl- α -cyano- β -phenyl cinnamate, glyceryl mono-2-ethylhexanoyl-di-p-methoxycinnamate, etc.), benzophenone-based ultraviolet absorbers (e.g., 2, 4-dihydroxybenzophenone, 2' -dihydroxy-4-methoxybenzophenone, methyl benzophenone, methyl methacrylate, ethyl, 2, 2 ' -dihydroxy-4, 4 ' -dimethoxybenzophenone, 2 ', 4, 4 ' -tetrahydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-4 ' -methylbenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonate, 4-phenylbenzophenone, 2-ethylhexyl-4 ' -phenyl-benzophenone-2-carboxylate, 2-hydroxy-4-n-octoxybenzophenone, 4-hydroxy-3-carboxybenzophenone, etc.), 3- (4 ' -methylbenzylidene) -d, l-camphor, 3-benzylidene-d, l-camphor, 2-phenyl-5-methylbenzoxazole, 2, 2-hydroxy-5-methylphenylbenzotriazole, 2- (2 ' -hydroxy-5 ' -tert-octylphenyl) benzotriazole, 2- (2 ' -hydroxy-5 ' -methylphenylbenzotriazole, dibenzylidene azine (dibenzaladine), diantimonyl methane, 4-methoxy-4 ' -tert-butylbenzoyl methane, 5- (3, 3-dimethyl-2-norbornyl) -3-pentan-2-one, and the like.

Examples of the ultraviolet absorber of the inorganic compound include titanium oxide, zinc oxide, iron oxide, cerium oxide, and composite powder containing these.

Examples of the antioxidant auxiliary include phosphoric acid, citric acid, ascorbic acid, maleic acid, malonic acid, succinic acid, fumaric acid, cephalin, hexametaphosphate, phytic acid, and ethylenediaminetetraacetic acid.

The formulation of the oil-in-water emulsion composition of the present invention is not limited, and can be appropriately determined into a cosmetic liquid form, an emulsion form, a cream form, a gel form, and the like, depending on the formulation components, the intended use, and the like.

Next, a skin external preparation for sunscreen according to a second embodiment of the present invention will be described. In general, in an external preparation for skin for ultraviolet protection, an organic ultraviolet protection agent as an oil agent and a powdery inorganic ultraviolet protection agent are blended in a base. Although a water-in-oil emulsion composition is widely used as a base in terms of blending a large amount of these ultraviolet protective agents, there is a possibility that a skin external preparation having such a structure may not give a good feeling of use because of a strong unpleasant oily feeling and powdery feeling.

On the other hand, if an oil-in-water emulsion composition is used as a base material, an external skin preparation having a delicate and refreshing feeling can be obtained due to the characteristics of the composition, but it is difficult to sufficiently blend the ultraviolet ray protection agent and maintain emulsion stability. Further, the conventional oil-in-water type sunscreen skin external preparation has a problem that it is inferior in water resistance to the water-in-oil type sunscreen skin external preparation and is easily peeled off by sweat or sebum.

Accordingly, the present inventors have further studied the properties of the oil-in-water emulsion composition according to the present invention and found that an oil-in-water sunscreen skin external preparation having excellent emulsion stability and little roughness can be obtained by blending the composition.

The components of the oil-in-water emulsion composition to be incorporated in the external preparation for skin for sunscreen of the present invention are as described above. The external skin preparation for sunscreen according to the present invention is obtained by dispersing a hydrophobized powder in the oil phase component of the oil-in-water emulsion composition.

Examples of the hydrophobized powder dispersed in the oil phase component include a powder obtained by hydrophobizing the surface of inorganic powder particles with a siloxane such as methylhydrogenpolysiloxane or dimethylpolysiloxane, a dextrin fatty acid ester, a higher fatty acid, a higher alcohol, a fatty acid ester, a metal soap, an alkyl phosphate ether, a fluorine compound, or a hydrocarbon such as squalane or paraffin by a wet method, a vapor phase method, a mechanochemical method, or the like using a solvent, and a powder obtained by coating inorganic powder particles with silica and then hydrophobizing the inorganic powder particles with an alkyl-modified silane coupling agent or the like.

Examples of the inorganic powder particles subjected to the hydrophobic treatment include titanium oxide, zinc oxide, talc, mica, sericite, kaolin, mica titanium, iron oxide black, iron oxide yellow, iron oxide red, ultramarine, prussian blue, chromium oxide, chromium hydroxide, and the like. In the present invention, it is particularly preferable to contain hydrophobized fine particulate titanium oxide and/or hydrophobized fine particulate zinc oxide.

In view of the properties of the present invention in which the hydrophobized powder is dispersed in an oil phase component, the average particle diameter is preferably smaller than that of emulsified particles in the oil phase. In particular, when it is considered that a hydrophobized powder is used as an ultraviolet scattering agent, it is preferable to use a powder having an average particle diameter of 100nm or less in the external preparation for sunscreen skin according to the present invention.

The skin external preparation for sunscreen of the present invention may be prepared by appropriately blending, in addition to the above essential components, other components as long as the effects are not impaired, according to the method for producing the oil-in-water type emulsion composition of the present invention. For example, a desired external preparation for skin for sun protection can be obtained by adding a powder component and a specific cationic surfactant to a part of water, mixing the mixture under heating, adding the rest of water and a water phase component, mixing the mixture, and then adding and mixing an oil phase component in which a hydrophobic powder is dissolved and stirred in advance under heating.

The formulation of the cosmetic composition may be appropriately determined in the form of a lotion, emulsion, cream, gel, etc., depending on the formulation components, the intended use, etc.

The third embodiment of the present invention is a cosmetic composition.

Conventionally, various powders have been blended in cosmetic products for imparting functions such as coloring skin or hair, concealing freckles, etc., protecting skin from ultraviolet rays, and absorbing sweat or sebum. On the other hand, when such a powder is blended into an emulsion composition, a technique is required to prevent aggregation of emulsion particles or aggregation and sedimentation of fine powder particles due to aging, temperature change, or the like, and to provide sufficient dispersion stability of the powder.

Further, the oil-in-water type emulsion composition has a delicate and refreshing feeling in use, and is preferable for cosmetics such as an emulsion, a cream, and an emulsion type foundation. Although silicone oils are widely used to provide such a preferable feeling of use and high water repellency, oils having a high proportion of silicone oils having low compatibility with other oil components such as hydrocarbons require much effort in selecting an optimal surfactant, and it is difficult to stably emulsify the oil. In particular, when a silicone surfactant is used for emulsification of silicone oil, it is necessary to blend a large amount of the surfactant for stabilization, and there is a problem that the composition has a sticky feeling due to the surfactant.

Accordingly, the present inventors have further studied the properties of the oil-in-water emulsion composition of the present invention, and have found that an oil-in-water cosmetic composition having excellent emulsion stability and less stickiness can be obtained by blending the composition.

The components of the oil-in-water emulsion composition to be incorporated in the cosmetic composition according to the present invention are as described above. The cosmetic composition according to the present invention is obtained by dispersing a hydrophobized powder in an oil phase component of the oil-in-water emulsion composition.

Examples of the hydrophobized powder dispersed in the oil phase component include a powder obtained by hydrophobizing the surface of inorganic powder particles with a solvent using a siloxane such as methylhydrogenpolysiloxane or dimethylpolysiloxane, a dextrin fatty acid ester, a higher fatty acid, a higher alcohol, a fatty acid ester, a metal soap, an alkyl phosphate ether, a fluorine compound, or a hydrocarbon such as squalane or paraffin, or a powder obtained by coating inorganic powder particles with silica and then hydrophobizing the inorganic powder particles with an alkyl-modified silane coupling agent.

Examples of the inorganic powder particles subjected to the hydrophobic treatment include titanium oxide, zinc oxide, talc, mica, sericite, kaolin, mica titanium, iron oxide black, iron oxide yellow, iron oxide red, ultramarine, prussian blue, chromium oxide, chromium hydroxide, and the like. In the present invention, particularly, hydrophobized fine particulate titanium dioxide, red iron oxide, yellow iron oxide, black iron oxide and/or aluminum oxide is preferably contained. The powder thus hydrophobized has high water resistance to sebum, sweat, and the like, and thus has good cosmetic durability, and by dispersing these in the oil phase component of the oil-in-water emulsion composition, a composition having good feeling of use during application and excellent properties after application can be obtained.

In view of the properties of the present invention in which the hydrophobized powder is dispersed in an oil phase component, the average particle diameter is preferably smaller than that of emulsified particles in the oil phase. In particular, in the cosmetic composition according to the present invention, it is preferable to use a powder having an average particle diameter of 100nm or less.

The cosmetic composition according to the present invention contains 50% by mass or more of a silicone oil with respect to the oil phase component in an oil-in-water emulsion composition as an essential component.

Examples of the silicone oil which can be suitably used in the present invention include chain polysiloxanes (e.g., dimethylpolysiloxane, methylphenylpolysiloxane, diphenylpolysiloxane, etc.), cyclic polysiloxanes (e.g., octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, etc.), silicone resins which form a three-dimensional network structure, silicone rubbers, various modified polysiloxanes (e.g., amino-modified polysiloxane, polyether-modified polysiloxane, alkyl-modified polysiloxane, fluorine-modified polysiloxane, etc.), acrylic siloxanes, and the like, and these can be blended alone or in combination of 2 or more kinds.

In the present invention, an acrylic silicone represented by the following general formula (I) is preferably used.

(chemical formula 3)

In the general formula (I), R is an alkyl group having 10 to 20 carbon atoms. Further, a + b + c is 1, a, b, and c are all 0.2 or more, and d is an integer of 5 to 100.

In the present invention, it is preferable to blend both terminal siloxane-modified glycerin represented by the following general formula (II).

(chemical formula 4)

In the above formula, R1 is a C1-12 linear or branched alkyl group or a phenyl group, and R2 is a C2-11 alkylene group. In addition, m is 10 to 120, and n is 1 to 11.

The silicone oils represented by the above general formulae (I) and (II) may be blended singly or in combination.

The oil phase of the oil-in-water emulsion composition contained in the cosmetic composition of the present invention may contain, in addition to a specific amount of silicone oil, an oil component usually used in cosmetics, such as liquid oils and fats, waxes, hydrocarbon oils, higher fatty acids, higher alcohols, and synthetic ester oils.

The cosmetic composition according to the present invention may be prepared by appropriately blending, in addition to the above essential components, other components within a range not impairing the effects thereof, according to the above method for producing an oil-in-water emulsion composition of the present invention. For example, a desired cosmetic composition can be obtained by adding a powder component and a specific cationic surfactant to a part of water, mixing the mixture under heating, adding the rest of water and a water phase component, mixing the mixture, and then adding and mixing an oil phase component in which a hydrophobic powder is dissolved by heating in advance and stirred under heating.

The formulation of the cosmetic composition may be appropriately determined in the form of a lotion, emulsion, cream, gel, etc., depending on the formulation components, the intended use, etc.

A fourth aspect of the present invention is a hair cosmetic for hair styling.

Conventionally, hair styling agents suitable for hair are required to have hair styling properties, as well as non-stickiness and high moisture resistance when used. For example, as a general technique for improving hair-setting properties or moisture resistance, it is considered to increase the viscosity of a product by adjusting the amount of a solid oil agent or the like. However, although the hair styling property is improved, the hair-sticking feeling is often increased.

On the other hand, it is known that the stickiness can be improved by applying an oil-in-water emulsion to a hair styling agent, but it is difficult to achieve both selection of an oil agent for optimizing hair styling properties and stable emulsification as an emulsion.

Accordingly, the present inventors have further studied the properties of the oil-in-water type emulsion composition of the present invention, and have found that a hair styling cosmetic composition having excellent emulsion stability, excellent hair styling performance and moisture resistance, and less sticky feeling can be obtained by blending the composition.

The components of the oil-in-water emulsion composition to be blended in the hair cosmetic composition for hair styling according to the present invention are as described above. In the present invention, the solid oil content is 1 to 30% by mass and the liquid oil content is 1 to 30% by mass, based on the total components constituting the present invention.

In the present invention, the solid oil refers to an oil that is solid at room temperature and is generally used in cosmetics. Examples of such oil components include solid oils and fats such as cocoa butter, coconut oil, horse oil, hydrogenated coconut oil, palm oil, beef tallow, mutton fat, hydrogenated beef tallow, palm kernel oil, lard, beef bone oil, wood wax kernel oil, hydrogenated oil, neatsfoot oil, wood wax, hydrogenated castor oil, beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax, insect wax, spermaceti, montan wax, bran wax, lanolin, kapok wax, lanolin acetate, sugarcane wax, isopropyl lanolate, hexyl laurate, reduced lanolin, jojoba wax, POE lanolin, shellac wax, lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, POE hydrogenated lanolin alcohol ether, waxes such as polyethylene wax, paraffin wax, purified ozokerite, vaseline, microcrystalline wax (lunacera), hydrocarbon waxes such as natural ceresin wax, cetyl alcohol, cetostearyl alcohol, stearyl alcohol, and the like, Higher alcohols such as behenyl alcohol, fatty acid glycerol ethers such as monostearyl glycerol ether (batyl alcohol), fatty acid glycerol esters such as acetyl glycerol and tri-2-heptyl glyceryl undecanoate, and the like, and 1 or 2 or more of these may be used in combination.

The amount of the solid oil component to be blended in the hair styling cosmetic composition of the present invention is 1 to 30% by mass, more preferably 2 to 15% by mass, based on the total components. If the amount of the solid oil is less than 1% by mass, the hair styling ability may be insufficient, and if it exceeds 30% by mass, the hair becomes sticky.

The liquid oil component used in the present invention refers to an oil component that is liquid at room temperature and is generally used in cosmetics. Examples of such oil components include avocado oil, evening primrose oil, camellia oil, turtle oil, macadamia nut oil, sunflower oil, almond oil, corn oil, mink oil, olive oil, rapeseed oil, egg butter, sesame oil, peach kernel oil, wheat germ oil, camellia oil, castor oil, linseed oil, safflower oil, cottonseed oil, perilla oil, soybean oil, peanut oil, tea seed oil, coconut oil, rice bran oil, china tung oil, japanese tung oil, jojoba oil, liquid oils such as germ oil, cetyl octanoate, cetyl 2-ethylhexanoate, hexyl dimethyl octanoate, ethyl laurate, hexyl laurate, isopropyl myristate, 2-hexyldecyl myristate, myristyl myristate, octyldodecyl myristate, isopropyl palmitate, 2-ethylhexyl palmitate, 2-hexyldecyl palmitate, and the like, 2-heptylundecyl palmitate, butyl stearate, isocetyl isostearate, decyl oleate, dodecyl oleate, oleyl oleate, myristyl lactate, cetyl lactate, diisostearate malate, cholesteryl 12-hydroxystearate, methyl ricinoleate, 2-octyldodecyl N-lauroyl-L-glutamate, 2-ethylhexyl succinate, diisobutyl adipate, 2-hexyldecyl adipate, di-2-heptylundecyl adipate, diisopropyl sebacate, di-2-ethylhexyl sebacate, ethylene glycol di-2-ethylhexanoate, neopentyl glycol didecanoate, neopentyl glycol dicaprylate, acetyl glycerol, di-2-heptylundecyl glyceride, glyceryl di-2-heptylundecyl oleate, glyceryl di-N-lauryl oleate, glyceryl di-2-heptylundecyl oleate, glyceryl di-2-ethylhexoate, Silicone oils such as ester oils including glyceryl trioctoate, glyceryl tri-2-ethylhexanoate, glyceryl trimyristate, glyceryl triisopalmitate, glyceryl tri-2-heptylundecanoate, trimethylolpropane tri-2-ethylhexanoate, trimethylolpropane triisostearate, pentaerythritol tetraoctanoate, and pentaerythritol tetra-2-ethylhexanoate, hydrocarbon oils such as liquid paraffin, natural ceresin, squalene, squalane, polybutene, and polybutene, chain polysiloxanes such as dimethylpolysiloxane, methylphenylpolysiloxane, and diphenylpolysiloxane, cyclic polysiloxanes such as octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, and dodecamethylcyclohexasiloxane, and various modified polysiloxanes such as amino-modified polysiloxane, polyether-modified polysiloxane, alkyl-modified polysiloxane, and fluorine-modified polysiloxane, one of them may be used 1 or 2 or more in combination.

The amount of the liquid oil component to be blended in the hair styling cosmetic composition of the present invention is 1 to 30% by mass, more preferably 5 to 20% by mass, based on the total components. If the amount of the liquid oil component is less than 1% by mass, the hair styling ability may be insufficient, and if it exceeds 30% by mass, stickiness may occur.

In the hair cosmetic composition for hairstyling according to the present invention, it is preferable to blend silicon dioxide, titanium dioxide, zinc oxide, or a composite powder containing these as a powder component of the oil-in-water emulsion composition as an essential component. Silica is particularly preferably used from the viewpoint of transparency and non-whitening after coating.

The particle size of the powder is not particularly limited, but is preferably 1 to 100nm in view of ease of handling when incorporated into a cosmetic and emulsion stability.

The hair cosmetic composition for hair styling according to the present invention can be prepared by appropriately blending, in addition to the above essential components, other components as long as the effects thereof are not impaired, according to the method for producing the oil-in-water type emulsion composition of the present invention. For example, a desired hair cosmetic for hair styling can be obtained by adding a powder component and a specific cationic surfactant to a part of water, mixing them under heating, adding the rest of water and a water phase component, mixing them, and then adding an oil phase component containing a solid oil component and a liquid oil component, which are dissolved in advance under heating, to the mixture under heating.

The formulation of the cosmetic composition may be appropriately determined in the form of a lotion, emulsion, cream, gel, etc., depending on the formulation components, the intended use, etc.

Example 1

The present invention will be described in more detail with reference to the following examples, but the technical scope of the present invention is not to be construed as being limited by these examples. In the present example, "mass%" or "%" indicating the amount to be blended means mass% based on the total amount of the composition unless otherwise specified.

First, the evaluation method used in the present example will be explained.

Evaluation (1): emulsion stability (appearance)

The appearance of the emulsion was visually observed within 1 day after the emulsion was prepared.

O: the sample was homogeneous and no oil slick (oil slick き) or agglomeration of the powder was observed.

And (delta): the sample was approximately uniform, but slight oil slick and the like were found.

X: the samples were not homogeneous or significant oil phase separation, powder agglomeration was found.

Evaluation (2): emulsion stability (emulsion particle)

When the sample is observed with an optical microscope,

o: the emulsified particles were uniform and no aggregation or aggregation was found.

And (delta): the emulsified particles were almost uniform, but were found to be slightly aggregated or coagulated.

X: the emulsified particles are not homogeneous and significant aggregation or agglomeration is found.

Evaluation (3): skin irritation test

On the inner side of the upper arm of 10 subjects, a closing mottled closure (lateral パツチ) was performed for 24 hours, and then the average value was calculated based on the following criteria.

No abnormalities were found at all.

Slight redness was found.

Redness was found.

Redness and pimples were found.

The evaluation criteria of the "skin irritation test" are as follows.

Very good: the average value of 10 subjects was 0 or more and less than 0.15

O: the average value of 10 subjects was 0.15 or more and less than 0.2

And (delta): the average value of 10 subjects was 0.2 or more and less than 0.3

X: the average value of 10 subjects was 0.3 or more

Evaluation (4): evaluation of tacky feeling at the time of coating

The actual use test of each sample was conducted by 10 subjects specified. The evaluation criteria are as follows.

Very good: the subjects 8 or more considered that the coating had no sticky feeling

O: the subjects were 6 or more and less than 8 and were considered to have no sticky feeling during application

And (delta): the subjects 3 or more and less than 6 were considered to have no sticky feeling during application

X: less than 3 subjects considered no sticky sensation in the application

An oil-in-water emulsion containing the compounding composition shown in table 1 was prepared by the following method, and the evaluation tests of the above-mentioned evaluations (1) to (4) were carried out for each sample.

[ Table 1]

(preparation method)

The aqueous phase components glycerin, succinoglycan and the powder component silica-coated zinc oxide were added to purified water and mixed. To this, stearyltrimethylammonium chloride or dimethyldistearylammonium chloride, which was additionally dispersed in purified water, was added and heat-sonicated. After the powder components were uniformly dispersed, the remaining oil phase components were added and mixed uniformly by a mixer to obtain an oil-in-water type emulsion composition.

As is clear from table 1, in test example 1 in which only the powder was blended, the emulsifiability was significantly poor. Although the emulsifying property was good, the test example 2 in which a small amount of the single-chain cationic active agent was added tended to have high skin irritation and high sticky feeling. On the other hand, in test example 3 in which the cationic active agent having 2 long-chain alkyl groups was added, all of the emulsifying property, the skin irritation, and the sticky feeling were good.

Next, in order to examine the preferable blending amount of the powder, an oil-in-water type emulsion containing the blending composition shown in table 2 was prepared by a conventional method, and the above evaluation tests of evaluations (1) to (4) were performed for each sample.

[ Table 2]

(preparation method)

The aqueous phase components glycerin, succinoglycan and the powder component silica-coated zinc oxide were added to purified water and mixed. Dimethyl distearyl ammonium chloride additionally dispersed in purified water was added thereto, and heat sonication was performed. After the powder components were uniformly dispersed, the remaining oil phase components were added and mixed by a mixer until uniform to obtain an oil-in-water type emulsified composition.

As is clear from Table 2, in test examples 5 to 7, the emulsions exhibited excellent emulsion stability, low sticky feeling, and low skin irritation. On the other hand, the emulsion of test example 4 containing 0.1 mass% of the powder was slightly inferior in emulsion stability, and the sticky feeling of test example 8 containing 30 mass% of the powder was strong.

Therefore, the oil-in-water emulsion of the present invention is preferably blended in an amount of 1 to 20% by mass based on the total amount of the emulsion.

Next, in order to examine a preferable blending amount of the cationic surfactant having 2 long chain alkyl groups, an oil-in-water emulsion containing the blending composition described in table 3 was prepared by a conventional method, and the above evaluation tests of evaluations (1) to (4) were performed on each sample.

[ Table 3]

(preparation method)

The aqueous phase components glycerin, succinoglycan and the powder component silica-coated zinc oxide were added to purified water and mixed. Dimethyl distearyl ammonium chloride additionally dispersed in purified water was added thereto, and heat sonication was performed. After the powder components were uniformly dispersed, the remaining oil phase components were added and mixed by a mixer until uniform to obtain an oil-in-water type emulsified composition.

As is clear from Table 3, in test examples 10 to 12, the emulsions exhibited excellent emulsion stability, low sticky feeling, and low skin irritation. On the other hand, the emulsion of test example 9 in which 0.0005 mass% of the cationic surfactant was blended was poor in emulsion stability, and the emulsion of test example 13 in which 1 mass% of the cationic surfactant was blended was slightly poor in skin irritation and strong in sticky feeling.

Therefore, the oil-in-water emulsion of the present invention is preferably such that the amount of the cationic surfactant is 0.001 to 0.5% by mass based on the total amount of the emulsion.

Subsequently, an oil-in-water emulsion containing the compounding composition shown in table 4 was prepared by a conventional method, and the above-described evaluation tests (1) to (4) were performed on each sample.

[ Table 4]

(preparation method)

The aqueous phase components glycerin, succinoglycan and the powder component silica-coated zinc oxide were added to purified water and mixed. Dimethyl distearyl ammonium chloride additionally dispersed in purified water was added thereto, and heat sonication was performed. After the powder components were uniformly dispersed, the remaining oil phase components were added and mixed by a mixer until uniform to obtain an oil-in-water type emulsified composition.

As is clear from Table 4, in test examples 15 to 17, the emulsions exhibited excellent emulsion stability, low sticky feeling, and low skin irritation. On the other hand, the emulsion of test example 14 having a chain length of 10 had poor emulsifiability, and the sticky feeling was improved as the chain length extended to 18 to 22 (test examples 16 to 17).

Therefore, the oil-in-water emulsion of the present invention preferably has a chain length of 2 alkyl groups of the cationic active agent of 12 to 22.

Further, with respect to the oil-in-water type emulsion composition, the change with time of emulsion stability due to the blending of succinoglycan, xanthan gum or acrylamide was evaluated. The evaluation method is as follows.

Evaluation (5): stability over time

An oil-in-water type emulsion composition containing the compounding composition shown in table 5 below was prepared, and the state of the emulsion after 1 month from the preparation was visually observed for the compositions of the respective test examples.

Very good: the composition remains emulsified as prepared.

O: some settling of the emulsion was found, but the composition remained approximately emulsified.

And (delta): the emulsified particles were found to settle and the particles aggregated.

X: the emulsified particles in the composition settle and aggregate, and the oil phase is completely separated.

[ Table 5]

(preparation method)

The aqueous phase component glycerin, succinoglycan, xanthan gum, acrylamide or polyacrylate and the powder component silica-coated zinc oxide were added to purified water and mixed. Dimethyl distearyl ammonium chloride additionally dispersed in purified water was added thereto, and heat sonication was performed. After the powder components were uniformly dispersed, the remaining oil phase components were added and mixed by a mixer until uniform to obtain an oil-in-water type emulsified composition.

As is clear from Table 5, the stable emulsified state was maintained for a long period of time in test examples 18 to 20 in which succinoglycan, xanthan gum or acrylamide was added. On the other hand, in test example 21 in which another thickener was added and test example 22 in which no thickener was added, the stability with time was slightly lowered.

Therefore, in the oil-in-water emulsion composition of the present invention, it is preferable to blend 1 or more of succinoglycan, xanthan gum and acrylamide.

The method for producing the oil-in-water emulsion composition of the present invention was studied. Emulsion compositions having the formulations shown in table 6 were prepared by the following respective preparation methods, and the emulsion state thereof was evaluated. The results are shown in Table 7.

Preparation method

(test example 23)

A dispersion in which an aqueous phase component and a powder component are uniformly dispersed in a part of purified water is mixed with a dispersion in which a surfactant component is uniformly dispersed in the remaining part of purified water, and the mixture is heated to 70 ℃ and subjected to ultrasonic treatment. Adding oil phase component heated to 70 deg.C, and emulsifying with emulsifying machine to obtain composition.

(test example 24)

Mixing the water phase component and the powder component, heating to 70 deg.C and performing ultrasonic treatment. An oil phase component and a surfactant component heated to 70 ℃ were added thereto, and emulsified with an emulsifying machine to obtain a composition.

(test example 25)

Stirring the powder and surfactant in appropriate amount of ethanol, and volatilizing ethanol to obtain surfactant treated powder. Mixing the surfactant treated powder with the water phase component, heating to 70 deg.C and performing ultrasonic treatment. Adding oil phase component heated to 70 deg.C, and emulsifying with emulsifying machine to obtain composition.

Evaluation method

Evaluation (1): emulsion stability (appearance)

The appearance of the emulsion was visually observed within 1 day after the preparation of the emulsion.

O: the sample was homogeneous and no oil slick or powder agglomeration was observed.

And (delta): the sample was approximately uniform, but slight oil slick and the like were found.

X: the samples were not homogeneous or significant oil phase separation, powder agglomeration was found.

Evaluation (2): emulsion stability (emulsion particle)

When the sample is observed with an optical microscope,

o: the emulsified particles were uniform and no aggregation or aggregation was found.

And (delta): the emulsified particles were almost uniform, but were found to be slightly aggregated or coagulated.

X: the emulsified particles are not homogeneous and significant aggregation or agglomeration is found.

[ Table 6]

[ Table 7]

As shown in table 7, test example 23, in which a specific cationic surfactant in a state of being dispersed in water was mixed with a powder component and then emulsified with an oil phase component, exhibited excellent emulsion stability.

On the other hand, in test example 24 in which the cationic surfactant was added at the time of emulsification of the aqueous phase and the oil phase without passing through the above-mentioned steps, stable emulsification was not obtained, and aggregation or aggregation of oil droplets or powder was observed. Further, in test example 25 in which the powder and the cationic surfactant were not treated in water but separately treated in ethanol, the emulsion stability was poor.

As is clear from comparison between test example 23 and test example 24, stable emulsions were obtained by dispersing a specific cationic surfactant in water to form a lamellar liquid crystal, adsorbing the lamellar liquid crystal on powder particles, and emulsifying the powder particles. Further, as is clear from comparison between test example 23 and test example 25, a composition having high emulsion stability can be easily prepared by treating the powder with a specific cationic surfactant that forms a lamellar liquid crystal in water.

Emulsion stability was evaluated for a composition obtained by mixing 50 parts by weight of a dispersion of the surface-treated powder obtained by each method described below and 50 parts by weight of an oil phase component (liquid paraffin) under heating at 70 ℃.

(test example 26)

0.1 part by weight of dimethyldistearylammonium chloride and 6 parts by weight of silica-coated zinc oxide were dispersed in 100 parts by weight of water, and ultrasonic treatment was carried out under heating.

(test example 27)

To a solution prepared by dissolving 0.1 part by weight of stearic acid in 100 parts by weight of ethanol, 6 parts by weight of silica-coated zinc oxide was added, and the mixture was stirred and mixed under heating.

(test example 28)

0.1 part by weight of glycerin monostearate was uniformly dispersed in 100 parts by weight of water, and 6 parts by weight of silica-coated zinc oxide was added and dispersed, followed by ultrasonic treatment under heating.

[ Table 8]

As shown in test example 26, an O/P/W emulsion composition having excellent stability can be obtained by performing powder treatment with dimethyldistearylammonium chloride in water and performing powder emulsification with an oil phase component using the obtained treated powder dispersion.

On the other hand, stearic acid, which is a general hydrophobizing agent for powder, is difficult to be powder-treated in water due to its properties, and is therefore treated in ethanol (test example 27). Therefore, the dispersion of the treated powder cannot be directly emulsified with the oil phase component. It was found that the treatment powder was emulsified by dispersing again the powder in water, but the emulsion stability of the obtained composition was inferior to that of test example 26.

In addition, in test example 28, although the treated powder was formed by glycerin monostearate in water and the powder emulsification was possible by using this dispersion, the emulsion stability of the obtained composition was inferior to that of test example 26.

As described above, the oil-in-water type emulsion composition according to the present invention can be obtained by using a cationic surfactant having 2 long-chain alkyl groups as a treatment agent for the powder to be emulsified, treating the powder in water, and mixing the resulting dispersion of the treated powder with the oil phase component as it is. That is, the oil-in-water type emulsion composition of the present invention can be easily and continuously carried out from the surface treatment of the powder to the emulsification by the powder by using the cationic surfactant having a specific structure as the treating agent for the powder, and has high emulsion stability.

Further, compositions in which a hydrophilic surfactant (PEG-60 hydrogenated castor oil) was further added to the formulation of table 6 in the following blending amounts and methods were evaluated. The results are shown in Table 9.

Preparation procedure of the composition

(A) A dispersion in which an aqueous phase component and a powder component were uniformly dispersed in a part of purified water was mixed with a dispersion in which a surfactant component (dimethyl distearyl ammonium chloride) was uniformly dispersed in the remaining part of the purified water, and the mixture was heated to 70 ℃ and subjected to ultrasonic treatment.

(B) An oil phase component heated to 70 ℃ is added to the dispersion, and emulsified by an emulsifying machine.

Method for adding hydrophilic surfactant

(test example 29)

In the step (B), a hydrophilic surfactant (PEG-60 hydrogenated castor oil) was added and mixed in an amount of 0.01 mass% to the total amount of the components after emulsification.

(test example 30)

In the step (B), a hydrophilic surfactant (PEG-60 hydrogenated castor oil) was added and mixed to the total amount of the components in an amount of 1 mass% after emulsification.

(test example 31)

In the step (a), a hydrophilic surfactant (PEG-60 hydrogenated castor oil) was added and mixed as an aqueous component in an amount of 0.01 mass% to the total components.

(test example 32)

In the step (a), a hydrophilic surfactant (PEG-60 hydrogenated castor oil) was added as an aqueous phase component in an amount of 1 mass% based on the total components.

Evaluation method

Evaluation (1): emulsion stability (appearance)

The appearance of the emulsion was visually observed within 1 day after the preparation of the emulsion.

O: the sample was homogeneous and no oil slick or powder agglomeration was observed.

And (delta): the sample was approximately uniform, but slight oil slick and the like were found.

X: the samples were not homogeneous or significant oil phase separation, powder agglomeration was found.

Evaluation (2): emulsion stability (emulsion particle)

When the sample is observed with an optical microscope,

o: the emulsified particles were uniform and no aggregation or aggregation was found.

And (delta): the emulsified particles were almost uniform, but were found to be slightly aggregated or coagulated.

X: the emulsified particles are not homogeneous and significant aggregation or agglomeration is found.

Evaluation (3): skin irritation test

The blocking patches were applied to the inner upper arms of 10 subjects for 24 hours, and the average values were calculated based on the following criteria.

No abnormalities were found at all.

Slight redness was found.

Redness was found.

Redness and pimples were found.

The evaluation criteria of the "skin irritation test" are as follows.

Very good: the average value of 10 subjects was 0 or more and less than 0.15

O: the average value of 10 subjects was 0.15 or more and less than 0.2

And (delta): the average value of 10 subjects was 0.2 or more and less than 0.3

X: the average value of 10 subjects was 0.3 or more

Evaluation (4): skin substantivity after coating

The actual use test of each sample was conducted by 10 subjects specified. The evaluation criteria are as follows.

Very good: the skin affinity after coating was considered to be good by 8 or more subjects

O: the skin affinity after application was considered good by 6 subjects or more and less than 8 subjects

And (delta): the skin affinity after coating was considered good by 3 or more and less than 6 subjects

X: less than 3 subjects considered good skin affinity after application

[ Table 9]

As is clear from table 9, test example 29 in which 0.01 mass% of the hydrophilic surfactant was added after the emulsification step exhibited a significant improvement in skin compatibility while maintaining the same low skin irritation as test example 23 in which no hydrophilic surfactant was added. However, test example 30 in which 1 mass% of the hydrophilic surfactant was added by the same addition method was inferior to test example 29 in skin irritation.

On the other hand, in the compositions of test examples 31 and 32 in which the hydrophilic surfactant was added at the time of powder treatment, no improvement in skin affinity was observed, but as in the case of test examples 29 and 30, deterioration in skin irritation was observed due to an increase in the amount added.

This is because, when the hydrophilic surfactant is added after the sufficient emulsification of the powder, the powder is already adsorbed on the surface of the emulsified oil droplets, and there is no room for the hydrophilic surfactant to act on the interface. Therefore, it is considered that the hydrophilic surfactant is sufficiently dissolved and dispersed in the external aqueous phase, and contributes to improvement of skin compatibility. On the other hand, when a hydrophilic surfactant is added during the surface treatment of the powder, the surfactant acts on the interface in the subsequent emulsification step, and therefore the skin affinity effect cannot be exhibited in the aqueous phase.

Thus, the oil-in-water emulsion composition according to the present invention is improved in skin compatibility after application by blending a hydrophilic surfactant in a range that does not affect the emulsification step and skin irritation. Further, as a result of further investigation, the amount of the hydrophilic surfactant exhibiting such an effect is 0.001 to 0.5% by mass, preferably 0.01 to 0.5% by mass, based on the composition.

The following examples are given for the formulation of the oil-in-water emulsion composition of the present invention, but the present invention is not limited thereto. The oil-in-water emulsion compositions obtained by the following formulation examples all had high emulsion stability, low sticky feeling, and low skin irritation.

< formulation example 1> emulsion

(mass%)

Phase A

Squalane 4.0

Oleic acid oleyl ester 2.5

Sorbitan sesquioleate 0.8

Evening primrose oil 0.2

Fragrance 0.1

Phase B

1, 3-butanediol 1.5

Ethanol 2.0

Silica (10nm) 5.0

Dimethyl distearyl ammonium chloride 0.05

Proper amount of purified water

Phase C

Xanthan gum 0.1

Proper amount of purified water

Phase D

Carboxyvinyl Polymer 0.2

0.1 part of potassium hydroxide

L-arginine L-aspartate 0.01

PEG-100 hydrogenated Castor oil 0.05

Ethylenediaminetetraacetate 0.05

Proper amount of preservative

Purified water residue

(preparation method)

Heating phase B to 70 deg.C, dispersing thoroughly with mixer or ultrasonic wave, adding phase C, adding phase A, emulsifying with emulsifier, and adding phase D to obtain emulsion.

< formulation example 2> ultraviolet protective emulsion

(mass%)

Phase A

Squalane 4.0

Octyl methoxy cinnamate 8.0

Cyclopenta dimethyl siloxane 5.0

Fragrance 0.1

Phase B

1, 3-butanediol 1.5

Ethanol 2.0

Silica-coated Zinc oxide (30nm)3.0

Dimethyl distearyl ammonium chloride 0.015

Proper amount of purified water

Phase C

Succinoglycan 0.2

Glycerol 3.0

PEG-60 hydrogenated Castor oil 0.01

L-arginine L-aspartate 0.01

Ethylenediaminetetraacetate 0.05

Proper amount of preservative

Purified water balance

(preparation method)

The phase B is heated to 70 ℃ and dispersed by a mixer or ultrasonic waves, and then the homogeneously dissolved phase C is added. Adding phase A heated to 70 deg.C into phase B heated to 70 deg.C, and emulsifying with emulsifying machine. It was cooled to give an emulsion.

< prescription example 3> Foundation make-up

(mass%)

Phase A

Cetyl alcohol 3.5

Deodorized lanolin 4.0

Jojoba oil 5.0

Vaseline 2.0

Squalane 6.0

Pyridoxine tripalmitate 0.1

Proper amount of preservative

Fragrance 0.3

Phase B

Mica 5.0

Dimethyl distearyl ammonium chloride 0.015

Proper amount of purified water

Phase C

Propylene glycol 10.0

POE (30) docosyl ether 0.02

Blended powder 12.0

Ethylenediaminetetraacetic acid trisodium 0.5

Purified water balance

(preparation method)

Heating phase B to 70 deg.C, dispersing with emulsifier, adding heated phase A, and emulsifying with emulsifier. Finally, phase C was added and the emulsion was cooled using a heat exchanger to give a foundation.

The oil-in-water emulsion compositions of formulation examples 1 to 3 were all excellent in emulsion stability and free from skin irritation and stickiness.

Example 2

The sunscreen skin external preparation according to the present invention was studied. In the present example, "mass%" or "%" indicating the amount to be blended means mass% based on the total amount of the composition unless otherwise specified.

First, the evaluation method used in the present example will be described.

Evaluation (1): emulsion stability (emulsion particle)

When the appearance of the sample was observed with an optical microscope within 1 day after the preparation of the emulsion,

o: the emulsified particles were uniform and no aggregation or aggregation was found.

And (delta): the emulsified particles were almost uniform, but were found to be slightly aggregated or coagulated.

X: the emulsified particles are not homogeneous and significant aggregation or agglomeration is found.

Evaluation (2): rotation test

The sample was put into a 50ml sample tube (diameter 3cm), rotated at 45rpm for 4 hours at room temperature, and the emulsion stability was evaluated by a microscope. The evaluation criteria are as follows.

O: the emulsified particles were uniform and no aggregation was observed.

And (delta): the emulsified particles were approximately uniform, but were found to be slightly aggregated.

X: the emulsified particles were not homogeneous and significant aggregation was found.

Evaluation (3): roughness after use

With respect to the presence or absence of roughness after the use of the sample, 10 subjects were exclusively used to carry out the actual use test. The evaluation criteria are as follows.

Very good: the subjects 8 or more considered no rough feeling after use

O: the subjects were 6 or more and less than 8 and considered to have no rough feeling after use

And (delta): the subjects had 3 or more and less than 6 subjects considered no rough feeling after use

X: less than 3 subjects considered no rough feeling after use

Evaluation (4): evaluation of tacky feeling at the time of coating

The actual use test of each sample was conducted by 10 subjects specified. The evaluation criteria are as follows.

Very good: the subjects 8 or more considered that the coating had no sticky feeling

O: the subjects were 6 or more and less than 8 and were considered to have no sticky feeling during application

And (delta): the subjects 3 or more and less than 6 were considered to have no sticky feeling during application

X: less than 3 subjects considered no sticky sensation in the application

An external preparation for skin for sunscreen having a compounding composition shown in table 10 was prepared, and evaluation tests of the above-described evaluations (1) to (4) were performed on each sample.

[ Table 10]

(preparation method)

Heating phase A to 70 deg.C, dispersing with ultrasonic wave, and adding uniformly dissolved phase B. Adding phase C heated to 70 deg.C into phase B heated to 70 deg.C, emulsifying with emulsifying machine, and cooling to room temperature.

As shown in table 10, in test example 33 using the powder without the cationic surfactant, the emulsifiability was significantly poor. In addition, in test example 34 in which only 1 chain cationic surfactant was added, the emulsion stability due to the rotation was lowered. On the other hand, test example 35, in which a cationic surfactant having 2 long chain alkyl groups was added, showed excellent results in any of the items.

In test 36 in which no powder component (silica-coated zinc oxide) was blended, the emulsion stability was significantly inferior to that in test 35, and in test 37 in which no hydrophobized powder was included in the oil phase, a rough feel was observed after use, and stickiness tended to occur during application. In test example 38 in which hydrophilic titanium dioxide was blended instead of the hydrophobized powder, a remarkable rough feeling and sticky feeling were found.

It is thus found that the oil-in-water sunscreen skin external preparation according to the present invention has excellent emulsion stability by containing an oil-in-water emulsion composition containing (a) a powder component, (b) a cationic surfactant having 2 alkyl chains with carbon chains of 12 to 22, (c) an oil phase component, and (d) an aqueous phase component. Further, by blending the hydrophobized powder to the oil phase component, the rough feeling after use and the sticky feeling during coating are improved.

Next, in order to examine a preferable blending amount of the powder used for emulsification, an external preparation for sunscreen skin having a blending composition shown in table 11 was prepared, and the evaluation tests of the above evaluations (1) to (4) were performed for each sample.

[ Table 11]

(preparation method)

Heating phase A to 70 deg.C, dispersing with ultrasonic wave, and adding uniformly dissolved phase B. Adding phase C heated to 70 deg.C into phase B heated to 70 deg.C, emulsifying with emulsifying machine, and cooling to room temperature.

As is clear from Table 11, in test examples 40 to 42, the compositions exhibited excellent emulsion stability, and almost no rough feeling or sticky feeling was observed. On the other hand, in test example 39 in which 0.5 mass% of the powder was blended, the emulsion stability was poor, and in example 43 in which 30 mass% of the powder was blended, the rough feeling and sticky feeling were strong.

Therefore, the amount of the powder to be incorporated in the external preparation for skin for sunscreen of the present invention is preferably 1 to 20% by mass based on the total amount of the external preparation.

Next, in order to examine a preferable blending amount of the cationic surfactant having 2 long-chain alkyl groups, an oil-in-water type sunscreen skin external preparation having a blending composition described in table 12 was prepared, and the above evaluation tests of evaluations (1) to (4) were performed for each sample.

[ Table 12]

(preparation method)

Heating phase A to 70 deg.C, dispersing with ultrasonic wave, and adding uniformly dissolved phase B. Adding phase C heated to 70 deg.C into phase B heated to 70 deg.C, emulsifying with emulsifying machine, and cooling to room temperature.

As shown in Table 12, the compositions of test examples 45 to 47 exhibited excellent emulsion stability, and neither coarse feeling nor sticky feeling was observed. On the other hand, example 44 in which 0.0005 mass% of the cationic surfactant was blended and test example 48 in which 1 mass% of the cationic surfactant was blended exhibited significantly poor emulsion stability.

Therefore, in the external skin preparation for sunscreen according to the present invention, the amount of the cationic surfactant having 2 alkyl chains with 12 to 22 carbon chains is preferably 0.001 to 0.5% by mass based on the total amount of the components.

Next, an external preparation for skin for sunscreen having a compounding composition shown in table 13 was prepared, and evaluation tests of the above evaluations (1) to (4) were performed on each sample.

[ Table 13]

(preparation method)

Heating phase A to 70 deg.C, dispersing with ultrasonic wave, and adding uniformly dissolved phase B. Adding phase C heated to 70 deg.C into phase B heated to 70 deg.C, emulsifying with emulsifying machine, and cooling to room temperature.

As shown in table 13, test examples 50 and 51 showed good results in both evaluation items. On the other hand, the emulsion stability of example 49 in which the cationic surfactant having a chain length of 10 was blended was poor, and as shown in test example 52, when the cationic surfactant having a chain length of 22 or more was blended, the emulsion stability during rotation was lowered, and the rough feeling and sticky feeling were increased.

Therefore, in the external skin preparation for sunscreen according to the present invention, the cationic surfactant preferably has a 2-alkyl chain length of 12 to 22.

Examples of the formulation of the external preparation for skin for sunscreen of the present invention are given below, but the present invention is not limited thereto. The oil-in-water sunscreen skin external preparation obtained by the following formulation examples has high emulsion stability and water resistance, low rough feeling and sticky feeling, and low skin irritation.

< formulation example 1> sunscreen emulsion

(mass%)

Phase A

Squalane 4.0

Oleic acid oleyl ester 2.5

Sorbitan sesquioleate 0.8

Evening primrose oil 0.2

Hydrophobicized titanium dioxide 3.0

Fragrance 0.1

Phase B

1, 3-butanediol 1.5

Ethanol 2.0

Silica (10nm) 5.0

Dimethyl distearyl ammonium chloride 0.05

Proper amount of purified water

Phase C

Xanthan gum 0.1

Proper amount of purified water

Phase D

Carboxyvinyl Polymer 0.2

0.1 part of potassium hydroxide

PEG-100 hydrogenated Castor oil 0.01

L-arginine L-aspartate 0.01

Ethylenediaminetetraacetate 0.05

Proper amount of preservative

Purified water balance

(preparation method)

Heating phase B to 70 deg.C, dispersing thoroughly with mixer or ultrasonic wave, adding phase C, adding phase A, emulsifying with emulsifier, and adding phase D to obtain emulsion.

< formulation example 2> ultraviolet protective emulsion

(mass%)

Phase A

Squalane 4.0

Octyl methoxy cinnamate 8.0

Cyclopenta dimethyl siloxane 5.0

Hydrophobized zinc oxide 5.0

Fragrance 0.1

Phase B

1, 3-butanediol 1.5

Ethanol 2.0

Silica-coated Zinc oxide (30nm)3.0

Distearoylethyl dimethyl ammonium chloride 0.015

Proper amount of purified water

Phase C

Succinoglycan 0.2

Glycerol 3.0

POE (20) docosanol 0.02

L-arginine L-aspartate 0.01

Ethylenediaminetetraacetate 0.05

Proper amount of preservative

Purified water balance

(preparation method)

The phase B is heated to 70 ℃ and dispersed by a mixer or ultrasonic waves, and then the homogeneously dissolved phase C is added. Adding phase A heated to 70 deg.C into phase B heated to 70 deg.C, and emulsifying with emulsifying machine. It was cooled to give an emulsion.

< prescription example 3> sunscreen foundation

(mass%)

Phase A

Cetyl alcohol 3.5

Deodorized lanolin 4.0

Jojoba oil 5.0

Vaseline 2.0

Squalane 6.0

Pyridoxine tripalmitate 0.1

Hydrophobicized titanium dioxide 3.0

Proper amount of preservative

Fragrance 0.3

Phase B

Mica 5.0

Dimethyl distearyl ammonium chloride 0.015

Proper amount of purified water

Phase C

Propylene glycol 10.0

PEG-100 hydrogenated Castor oil 0.05

Blended powder 12.0

Ethylenediaminetetraacetic acid trisodium 0.5

Purified water balance

(preparation method)

Heating phase B to 70 deg.C, dispersing with emulsifier, adding heated phase A, and emulsifying with emulsifier. Finally, phase C was added and the emulsion was cooled using a heat exchanger to give a foundation.

Example 3

The cosmetic composition according to the present invention was studied. In the present example, "mass%" or "%" indicating the amount to be blended means mass% based on the total amount of the composition unless otherwise specified.

First, the evaluation method used in the present example will be described.

Evaluation (1): formulation stability

The appearance was visually observed for the state after the prepared emulsion was stored at 50 ℃ for 1 month, and further, the state of the emulsion was observed with an optical microscope. The evaluation criteria are as follows.

O: no change in appearance was observed, and further, the emulsified particles were uniform and no aggregation or aggregation was observed.

And (delta): no change in appearance was observed, but aggregation or aggregation of the emulsified particles was observed.

X: the separation of the oil phase was visually observed.

Evaluation (3): sticky feeling after use

With respect to the presence or absence of sticky feeling after the use of the sample, 10 subjects were exclusively used to carry out the actual use test. The evaluation criteria are as follows.

Very good: the above 8 subjects considered no sticky feeling after use

O: the subjects were 6 or more and less than 8 and were considered to have no sticky feeling after use

And (delta): the subjects had no sticky feeling after use, and 3 or more and less than 6 subjects had no sticky feeling

X: less than 3 subjects considered no sticky feeling after use

Evaluation (3): evaluation of tenderness feeling at the time of coating

The actual use test of each sample was conducted by 10 subjects specified. The evaluation criteria are as follows.

Very good: more than 8 subjects considered to have a tender feeling when applied

O: the subjects 6 to less than 8 considered tender feeling in application

And (delta): the subjects 3 or more and less than 6 considered tender feeling in application

X: less than 3 subjects considered tender when applying

Cosmetic compositions containing the blend compositions shown in Table 14 were prepared, and the evaluation tests of the above-described evaluations (1) to (3) were carried out on the respective samples.

[ Table 14]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. The mixture to which phase B was added, emulsified with an emulsifier, and cooled.

As shown in table 14, in test example 53 in which only the hydrophilic powder was blended without containing the cationic surfactant, and in test example 54 in which only the cationic surfactant was blended, the emulsifiability was significantly poor. In contrast, test example 55, which contained a cationic surfactant and a hydrophilic powder, exhibited good stability, no stickiness, and a moist feeling.

Further, the composition of test example 56 emulsified with the hydrocarbon surfactant had poor formulation stability, exhibited a sticky feeling, and had no tender feeling. In test example 57 using a silicone surfactant, the formulation stability was improved compared to that of the case of the hydrocarbon surfactant, but the sticky feeling and the tender feeling were still poor.

As described above, the cosmetic composition according to the present invention has excellent emulsion stability by containing an oil-in-water emulsion composition containing (a) a powder component, (b) a cationic surfactant having 2 alkyl chains with a carbon chain of 12 to 22, (c) an oil phase component, and (d) an aqueous phase component. Further, by blending the hydrophobized powder to the oil phase component, the rough feeling after use and the sticky feeling during coating are improved.

Next, the following study was conducted on the oil phase component of the cosmetic composition of the present invention.

That is, cosmetic compositions containing the blend compositions shown in table 15 were prepared, and the above evaluations (2) and (3) were performed for each sample.

[ Table 15]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. The mixture to which phase B was added, emulsified with an emulsifier, and cooled.

As shown in Table 15, the compositions of test examples 58 to 61, in which the oil phase contained 50% by mass or more of silicone oil relative to the oil phase component, had no sticky feeling and had delicate touch. In particular, when an acrylic silicone having a specific structure (test example 58), both terminal silicone-modified glycerin (test example 59), or both of them (test example 60) were blended, it was found that the usability was remarkably improved. On the other hand, in test example 62 in which the amount of the silicone oil blended is less than 50% by mass relative to the oil phase component, the sample was significantly sticky and did not feel delicate.

As described above, in the cosmetic composition according to the present invention, it is preferable that the oil phase component contains at least 50% by mass of a silicone oil, and the incorporation of an acrylic silicone having a specific structure and/or both terminal silicone-modified glycerin is particularly preferable in terms of improvement in usability.

Next, in order to examine a preferable blending amount of the powder used for emulsification, cosmetic compositions having blending compositions shown in table 16 were prepared, and the evaluation tests of the above evaluations (1) to (3) were performed for each sample.

[ Table 16]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. The mixture to which phase B was added, emulsified with an emulsifier, and cooled.

As shown in table 16, the cosmetic compositions of test examples 64 to 66 had excellent preparation stability and were also excellent in terms of no stickiness and delicate feeling. On the other hand, in test example 63 in which the amount of the powder component (silica-coated zinc oxide) involved in the emulsification was 0.5 mass%, the formulation stability was poor, and the composition of example 67 in which the same powder component was added in an amount of 30 mass% was strong in stickiness and poor in delicate feeling.

Therefore, in the cosmetic composition according to the present invention, the amount of the powder component is preferably 1 to 20% by mass based on the composition.

Next, in order to examine a preferable blending amount of the cationic surfactant having 2 long chain alkyl groups, cosmetic compositions having the blending compositions shown in table 17 were prepared, and the evaluation tests of the above evaluations (1) to (3) were performed for each sample.

[ Table 17]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. The mixture to which phase B was added, emulsified with an emulsifier, and cooled.

As is clear from table 17, the cosmetic compositions of test examples 69 to 71 exhibited excellent formulation stability and were also excellent in terms of non-stickiness and delicate feeling. On the other hand, the preparation stability was significantly reduced in example 68 in which 0.0005 mass% of dimethyldistearylammonium chloride was blended and in test example 72 in which 1 mass% was blended.

Therefore, in the cosmetic composition according to the present invention, the cationic surfactant having 2 alkyl chains with carbon chains of 12 to 22 is preferably blended in an amount of 0.001 to 0.5% by mass based on the composition.

Next, cosmetic compositions containing the blend compositions shown in table 18 were prepared, and the evaluation tests of the above-described evaluations (1) to (3) were performed on the respective samples.

[ Table 18]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. The mixture to which phase B was added, emulsified with an emulsifier, and cooled.

As shown in table 18, the compositions of test examples 74 and 75 showed good results in both evaluation items. On the other hand, the formulation stability of the composition of example 73 using dimethyldialkylammonium chloride with an alkyl chain length of 10 was significantly low and was not use-tolerant. The composition of example 76 having an alkyl chain length of 22 was excellent in formulation stability, but was slightly sticky and tender.

Therefore, in the cosmetic composition according to the present invention, the cationic surfactant preferably has a 2-alkyl chain length of 12 to 22.

Examples of the formulation of the cosmetic composition of the present invention are given below, but the present invention is not limited to these examples. The cosmetic compositions obtained by the following formulation examples all had high formulation stability, low sticky feeling, and delicate feeling.

< formulation example 1> oil-in-water type emulsion foundation

(mass%)

(1) Hydrophobized titanium dioxide 10.0

(2) Hydrophobicized talc 3.0

(3) Hydrophobized iron oxide yellow 0.8

(4) Hydrophobized iron oxide Black 0.15

(5) Hydrophobized iron oxide Red 0.36

(6) Both terminal siloxane-modified glycerin of the general formula (II) 3.0

(7) PEG-10 Dimethylpolysiloxane 0.5

(8) Decamethylcyclopentasiloxane 10.0

(9) Squalane 4.0

(10) Dipropylene glycol 5.0

(11) Silica (10nm) 3.0

(12) Distearoyl diethylammonium chloride 0.03

(13) Proper amount of purified water

(14) Xanthan gum 0.3

(15) Carboxymethyl cellulose 0.2

(16) Ethanol 2.0

(17) Ethylenediaminetetraacetate 0.1

(18) Proper amount of preservative

(19) PEG-60 hydrogenated Castor oil 0.01

(20) Purified water balance

(preparation method)

The oil-in-water type emulsion foundation can be obtained by mixing (10) to (13), heating to 70 ℃, fully dispersing with a homomixer or ultrasonic waves, adding the oil phases (1) to (9) dispersed and broken in advance with a bead mill, emulsifying with an emulsifying machine, adding (14) to (20), and uniformly dispersing.

< formulation example 2> oil-in-water type emulsion foundation

(mass%)

(1) Hydrophobized titanium dioxide 10.0

(2) Hydrophobicized talc 3.0

(3) Hydrophobized iron oxide yellow 0.8

(4) Hydrophobized iron oxide Black 0.15

(5) Hydrophobized iron oxide Red 0.36

(6) Both terminal siloxane-modified glycerin of the general formula (II) 3.0

(7) PEG-10 Dimethylpolysiloxane 0.5

(8) Decamethylcyclopentasiloxane 15.0

(9) Octyl methoxy cinnamate 5.0

(10) Ochrinklin 2.0

(11) Glycerol 3.0

(12)1, 3-butanediol 4.0

(13) Silica-coated Zinc oxide (30nm) 5.0

(14) Distearoyl dimethyl ammonium chloride 0.05

(15) Proper amount of purified water

(16) Succinoglycan 0.3

(17) Carboxymethyl cellulose 0.2

(18) Proper amount of preservative

(19) PEG-100 hydrogenated Castor oil 0.03

(20) Purified water balance

(preparation method)

The oil-in-water emulsion foundation is obtained by mixing (11) to (15), heating to 70 ℃, sufficiently dispersing the mixture with a homomixer or ultrasonic waves, slowly adding the oil phases (1) to (10) dispersed and crushed in advance with a bead mill, emulsifying the mixture with an emulsifier, and uniformly dispersing the mixture by adding (16) to (20).

< formulation example 3> oil-in-water type gel foundation

(mass%)

(1) Hydrophobized titanium dioxide 10.0

(2) Hydrophobized iron oxide yellow 0.8

(3) Hydrophobized iron oxide Black 0.15

(4) Hydrophobized iron oxide Red 0.36

(5) Acrylic siloxane of formula (I) 1.0

(6) PEG-10 Dimethylpolysiloxane 0.5

(7) Isostearic acid 0.2

(8) Decamethylcyclopentasiloxane 12.0

(9) Cetyl octanoate 3.0

(10) Glycerol 3.0

(11) Dipropylene glycol 4.0

(12) Silica-coated titanium oxide (10nm) 3.0

(13) Distearoyl dimethyl ammonium chloride 0.15

(14) Proper amount of purified water

(15) Xanthan gum 0.2

(16) Agar powder 1.5

(17) Ethylenediaminetetraacetate 0.1

(18) Proper amount of preservative

(19) POE (20) docosanol 0.01

(20) Purified water balance

(preparation method)

Mixing (11) - (14), heating to 70 deg.C, fully dispersing with homomixer or ultrasonic wave, slowly adding oil phase (1) - (10) dispersed and crushed with bead mill, and emulsifying with emulsifier. Then, after uniformly dispersing at 90 ℃ in advance, the cooled (15) to (20) were added to obtain an oil-in-water gel foundation.

Example 4

The following studies were made on the hair styling cosmetic according to the present invention. In the present example, "mass%" or "%" indicating the amount to be blended means mass% based on the total amount of the composition unless otherwise specified.

First, the evaluation method used in the present example will be described.

Evaluation (1): emulsion stability (emulsion particle)

When the appearance of the sample was observed with an optical microscope within 1 day after the preparation of the emulsion,

o: the emulsified particles were uniform and no aggregation or aggregation was found.

And (delta): the emulsified particles were almost uniform, but were found to be slightly aggregated or coagulated.

X: the emulsified particles are not homogeneous and significant aggregation or agglomeration is found.

Evaluation (2): force of whole hair

For the hair styling ability of the samples, the actual use test was conducted by 10 specialized subjects. The evaluation criteria are as follows.

Very good: the subjects 8 above considered that the hair styled in a natural state with natural hair flow could be maintained.

O: the subjects 6 or more and less than 8 were considered to be able to maintain the natural state of hair with natural hair flow.

And (delta): the subjects 3 or more and less than 6 considered to be able to maintain the natural state of hair with natural hair flow.

X: less than 3 subjects considered a natural state of hair lift with natural hair flow.

Evaluation (3): moisture resistance

After applying a sample to a hair piece, shaping the hair piece into curly hair and naturally drying the hair piece, the hair piece was stored in a container adjusted to have a relative humidity of 90% and a temperature of 25 ℃ for 24 hours, and 10 subjects evaluated the shape and feel of the hair piece according to the following criteria.

Very good: moisture resistance was judged to be present in 8 or more subjects.

O: the moisture resistance was judged in 6 subjects or more and less than 8 subjects.

And (delta): the moisture resistance was judged in 3 or more and less than 6 subjects.

X: less than 3 subjects were judged to have moisture resistance.

Evaluation (4): evaluation of tacky feeling at the time of coating

The actual use test of each sample was conducted by 10 subjects specified. The evaluation criteria are as follows.

Very good: the subjects 8 or more considered that the sticky feeling was not caused when the coating was applied

O: the subjects were 6 or more and less than 8 and considered to have no sticky feeling when applied

And (delta): the subjects 3 or more and less than 6 considered no sticky feeling at the time of application

X: less than 3 subjects considered no sticky feeling on application

Hair cosmetics for hair styling containing the blend compositions shown in table 19 were prepared, and the above-described evaluation tests (1) to (4) were performed on each sample.

[ Table 19]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. Adding phase B heated to 80 deg.C, emulsifying with emulsifying machine, and cooling.

As shown in table 19, both test example 77 in which the hydrophilic powder (silica-coated titanium dioxide, silica) was emulsified and test example 78 in which the hydrophilic powder was emulsified with dimethyldistearylammonium chloride had significantly poor emulsion stability. On the other hand, test example 79 in which emulsification was performed using both dimethyldistearylammonium chloride and a hydrophilic powder had high emulsion stability, and exhibited good usability with respect to all of hair styling ability, moisture resistance, and no stickiness.

In addition, the composition of test example 80 emulsified only with the hydrocarbon surfactant PEG-60 hydrogenated castor oil had poor emulsion stability and was not sufficient in use.

Accordingly, the hair cosmetic for hair styling according to the present invention preferably contains an oil-in-water emulsion composition containing (a) a powder component, (b) a cationic surfactant having 2 alkyl chains with a carbon chain of 12 to 22, (c) an oil phase component, and (d) an aqueous phase component.

Next, in order to examine the preferable blending amount of the powder used for emulsification, hair styling cosmetic compositions containing the blending compositions shown in table 20 were prepared, and the evaluation tests of the above evaluations (1) to (4) were performed for each sample.

[ Table 20]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. Adding phase B heated to 80 deg.C, emulsifying with emulsifying machine, and cooling.

As shown in table 20, the hair styling cosmetic compositions of test examples 82 to 84 exhibited excellent emulsion stability and high evaluation in all of hair styling power, moisture resistance and non-sticky feeling. On the other hand, the emulsion stability of test example 81 in which the amount of the powder components (silica-coated zinc oxide, silica) involved in the emulsion was 0.5 mass% was poor, and the usability of the composition of example 85 in which the powder components were 30 mass% was significantly poor.

Therefore, the hair cosmetic composition for hair styling according to the present invention preferably contains the powder component in an amount of 1 to 20% by mass based on the composition.

Next, in order to examine a preferable blending amount of the cationic surfactant having 2 long chain alkyl groups, hair cosmetic preparations for hair styling containing the blending composition described in table 21 were prepared, and the evaluation tests of the above evaluations (1) to (4) were performed for each sample.

[ Table 21]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. Adding phase B heated to 80 deg.C, emulsifying with emulsifying machine, and cooling.

As shown in Table 21, the hair styling cosmetics of test examples 87 to 89 exhibited high emulsion stability and were excellent in hair styling power, moisture resistance and sticky feeling. On the other hand, example 86 in which the amount of dimethyl distearyl ammonium chloride blended was 0.0005 mass% was poor in emulsion stability, and test example 90 in which the amount blended was 1 mass% was poor in emulsion stability and usability.

Therefore, in the hair cosmetic composition for hair styling according to the present invention, the cationic surfactant having an alkyl chain having 2 carbon atoms of 12 to 22 is preferably blended in an amount of 0.001 to 0.5% by mass based on the composition.

Next, hair styling cosmetic compositions containing the blend compositions shown in table 22 were prepared, and the evaluation tests of the above-described evaluations (1) to (4) were carried out for the respective samples.

[ Table 22]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. Adding phase B heated to 80 deg.C, emulsifying with emulsifying machine, and cooling.

As shown in table 22, the compositions of test examples 92 and 93 exhibited good results in any of the evaluation items. On the other hand, the composition of example 91 using dimethyldialkylammonium chloride with an alkyl chain length of 10 had significantly low emulsion stability and was not durable to use. The composition of example 94 having an alkyl chain length of 22 had insufficient formulation stability and usability.

Therefore, in the hair cosmetic composition for hair styling according to the present invention, the cationic surfactant preferably has a 2-alkyl chain length of 12 to 22.

Next, in order to examine the preferable oily components in the present invention, hair styling cosmetic compositions containing the blend compositions shown in table 23 were prepared, and the evaluation tests of the above evaluations (2) to (4) were performed for each sample.

[ Table 23]

(preparation method)

Phase A was heated to 70 ℃ and dispersed by sonication. Adding phase B heated to 80 deg.C, emulsifying with emulsifying machine, and cooling.

As shown in table 23, in test example 95 in which only the solid oil component was blended as the oil phase component, the sticky feeling was high, and in test example 96 in which only the liquid oil component was blended, the hair-styling performance was poor. On the other hand, the composition of test example 97 containing appropriate amounts of the solid oil component and the liquid oil component showed excellent results in all the items.

On the other hand, in test examples 98 and 99 in which a large amount of solid oil or liquid oil was blended, usability was inferior to that of test example 97.

Therefore, in the hair cosmetic composition for hair styling of the present invention, it is preferable to blend appropriate amounts of the solid oil component and the liquid oil component as the oil phase component.

Further, as a result of further investigation, the amounts of the solid oil and the liquid oil to be blended are preferably 1 to 30% by mass, respectively, based on the total amount of the components.

Examples of the hair styling cosmetic formulation of the present invention are given below, but the present invention is not limited to these examples. The hair styling cosmetic compositions obtained by the following formulation examples all had high emulsion stability, low sticky feeling, and excellent hair styling performance and moisture resistance.

< prescription example 1> Hair wax

(mass%)

(A phase)

Liquid paraffin 10.0

Microcrystalline wax 5.0

Carnauba wax 5.0

Pentaerythritol tetra-2-ethylhexanoate 3.0

(phase B)

1, 3-butanediol 7.0

Silica-coated Zinc oxide (30nm)3.0

Dimethyl distearyl ammonium chloride 0.03

Silica (10nm) 1.0

Proper amount of purified water

(C phase)

Triethanolamine 0.3

Ethanol 2.0

Carboxyvinyl Polymer 0.2

Proper amount of p-hydroxybenzoate

Proper amount of 3 sodium ethylene diamine tetraacetate

PEG-100 hydrogenated Castor oil 0.05

Purified water balance

(preparation method)

Phase B was heated to 70 ℃ and dispersed by sonication. Adding phase A heated to 80 deg.C, emulsifying with emulsifying machine, adding phase C, and cooling.

< prescription example 2> Hair wax

(mass%)

(A phase)

Liquid paraffin 10.0

Microcrystalline wax 10.0

Dimethylpolysiloxane 4.0

Stearyl alcohol 2.0

Carnauba wax 3.0

Pentaerythritol tetra-2-ethylhexanoate 2.0

Proper amount of perfume

(phase B)

Propylene glycol 8.0

Silica-coated Zinc oxide (30nm) 2.0

Dimethyl distearyl ammonium chloride 0.07

Silica (10nm) 2.0

Proper amount of purified water

(C phase)

Succinoglycan 0.2

Glycerol 3.0

L-arginine L-aspartate 0.01

Ethylenediaminetetraacetate 0.05

Proper amount of preservative

POE (20) docosanol 0.02

Purified water balance

(preparation method)

Phase B was heated to 70 ℃ and dispersed by sonication. Adding phase A heated to 80 deg.C, emulsifying with emulsifying machine, adding phase C, and cooling.

Claims (13)

1. An oil-in-water emulsion composition comprising:

(a) 1 to 20 mass% of a powder component selected from the group consisting of silica, titanium dioxide, zinc oxide and composite powders containing these,

(b) 0.001 to 0.5 mass% of a cationic surfactant having 2 alkyl chains with 12 to 22 carbon chains selected from the group consisting of dimethyl dilauryl ammonium chloride, diethyl dilauryl ammonium chloride, dipropyl dilauryl ammonium chloride, dimethyl dipalmyl ammonium chloride, diethyl dipalmyl ammonium chloride, dimethyl distearyl ammonium chloride, dipropyl distearyl ammonium chloride, dimethyl behenyl ammonium chloride, diethyl behenyl ammonium chloride, dipropyl behenyl ammonium chloride, distearyl ethyl dimethyl ammonium chloride, dipalmitoyl ethyl hydroxyethyl methyl ammonium methyl sulfate, and dipalmitoyl ethyl hydroxyethyl methyl ammonium methyl sulfate,

(c) An oil phase component containing an oil component selected from the group consisting of liquid oils and fats, waxes, hydrocarbon oils, higher fatty acids, higher alcohols, synthetic ester oils, and silicone oils,

(d) Contains 1 or more than 2 kinds of water phase components selected from succinoglycan, xanthan gum and acrylamide,

has a structure in which the powder particles of (a) are adsorbed onto oil droplets dispersed in an aqueous phase, and contains 0.001 to 0.5 mass% of a hydrophilic surfactant to the aqueous phase of the composition,

the composition is manufactured by the steps of,

(A) a step of dispersing a powder component and a cationic surfactant having 2 alkyl chains with carbon chains of 12 to 22 in an aqueous phase component,

(B) a step of mixing the dispersion and an oil phase component after the step (A).

2. The oil-in-water emulsion composition according to claim 1, wherein (b) a cationic surfactant is adsorbed to the powder particles of (a).

3. The oil-in-water emulsion composition according to claim 1 or 2, wherein the cationic surfactant of (b) is added in a total amount of 0.001 to 0.1% by mass.

4. The oil-in-water type emulsion composition according to claim 1 or 2, wherein the cationic surfactant of (b) is dimethyldialkylammonium chloride selected from the group consisting of dimethyldilaurylammonium chloride, dimethyldipalmitylammonium chloride, dimethyldistearylammonium chloride, and dimethyldidodecylammonium chloride.

5. The method for producing an oil-in-water emulsion composition according to claim 1 or 2, comprising the following steps (A) and (B),

(A) a step of dispersing a powder component and a cationic surfactant having 2 alkyl chains with carbon chains of 12 to 22 in an aqueous phase component,

(B) a step of mixing the dispersion and an oil phase component after the step (A).

6. The process according to claim 5, further comprising the step (C),

(C) and (B) adding and mixing a hydrophilic surfactant after the step (B).

7. An external preparation for skin for sunscreen comprising the oil-in-water emulsion composition according to claim 1 or 2,

and a hydrophobized powder containing a hydrophobized particulate titanium oxide and/or a hydrophobized particulate zinc oxide dispersed in the oil phase component of (c).

8. A cosmetic composition comprising the oil-in-water emulsion composition according to claim 1 or 2,

further comprises a hydrophobized powder containing 1 or 2 or more kinds selected from the group consisting of a hydrophobized fine particulate titanium dioxide, an iron oxide red, an iron oxide yellow, an iron oxide black and an aluminum oxide dispersed in the oil phase component of (c),

and 50% by mass or more of the oil phase component is a silicone oil.

9. The cosmetic composition according to claim 8, comprising 1 or 2 or more kinds of acrylic siloxanes represented by the following general formula (I),

in the above formula, R is an alkyl group having 10 to 20 carbon atoms, a + b + c is 1, a, b and c are all 0.2 or more, and d is an integer of 5 to 100.

10. The cosmetic composition according to claim 8, which comprises 1 or 2 or more kinds of both-terminal silicone-modified glycerin represented by the following general formula (II),

in the above formula, R1 is a C1-12 linear or branched alkyl group or a phenyl group, R2 is a C2-11 alkylene group, m is 10-120, and n is 1-11.

11. A hair cosmetic composition for hair styling, comprising the oil-in-water emulsion composition according to claim 1 or 2,

the oil phase component (c) contains 1 to 30 mass% of solid oil and 1 to 30 mass% of liquid oil with respect to the total composition components.

12. The hair cosmetic for hair styling according to claim 11, wherein the powder component of (a) contains silica.

13. The oil-in-water emulsion composition according to claim 1, further comprising (C),

(C) and (B) adding and mixing a hydrophilic surfactant after the step (B).