JPH10114624A - Solid aqueous cosmetic - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a solid aqueous cosmetic containing a sucrose fatty acid diester, a water-soluble anionic surfactant and agar and excellent in water resistance, portability and usability such as refrigerant, moist touch and youthfulness. SOLUTION: This solid aqueous cosmetic contains 0.5-15wt.% of a sucrose fatty acid diester, 0.05-15wt.% of agar and a water-soluble ionic surfactant. The water-soluble surfactant is preferably a >=12C fatty acid soap, and is contained in an amount of 0.2-15wt.% based on the sucrose fatty acid diester. The solid aqueous cosmetic preferably further contains 30-95wt.% of water, 0.5-10wt.% of a surfactant except the ionic surfactant, 1-30wt.% of an oil and 1-40wt.% of a powdery material as essential components. The cosmetic can be prepared into solid skin lotions, solid emulsions, solid beauty creams, make-up foundations, rouges, eye shadows, eye liners, sun care products, body cosmetics, etc. This cosmetic is a remarkable solid aqueous cosmetic excellent in water resistance and water repellency.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a solid water-based cosmetic which is excellent in usability such as refreshing feeling, moisture feeling, freshness and the like, and excellent in water resistance and excellent in portability.

[0002]

2. Description of the Related Art Conventionally, solid cosmetics represented by foundations and the like have a high need for the market because they are particularly excellent in portability, but most of the dosage forms are powder type and oil type. And the types containing water were limited. In addition, even in those containing water, most of the dosage forms are solidified water-in-oil type liquid cosmetics, and since these have water in the internal phase, a large amount of water is not blended. It was difficult. On the other hand, the oil-in-water type is difficult to solidify because the external phase is water, and only a few are currently on the market.

[0003]

The water-in-oil type has advantages such as easy solidification, but it is difficult to mix a large amount of water. Refreshing feeling
There are many disadvantages such as lack of moisture and skin care. On the other hand, in the case of the oil-in-water type, since there are few suitable solidifying agents corresponding to the wax in the water-in-oil type, the shape is mostly liquid or creamy. Had a problem. Also,
For example, there is known an oil-in-water type solid cosmetic using a thickening polysaccharide such as agar which is a typical water solidifying agent (JP-A-5-178723). Alternatively, there is a problem that the sponge is poorly removed, so that there is still a considerable problem in solidifying oil-in-water type cosmetics.

[0004] One of the major drawbacks of oil-in-water type cosmetics is that there is a major problem in the ability to retain on the skin and the like. In other words, when the cosmetic is applied on the skin, the base is water-based and therefore has low water resistance. For example, it is easily peeled off by operations such as cooking, and it is difficult to maintain the effect for a long time. Met. On the other hand, in the winter, dry, open air conditions, water work, etc. tend to cause cracks, red tinge, rough skin, etc. Cosmetics containing various drugs are used for prevention and treatment of these, but water-based creams etc. -There was a problem that the effect was limited due to poor retention on the skin.

[0005]

Means for Solving the Problems The present inventors have paid attention to the above points, and have conducted intensive studies to obtain cosmetics excellent in usability, water resistance and portability. As a result, agar and sucrose fatty acid were obtained. By using a diester and a water-soluble ionic surfactant in combination, it is possible to solidify to improve portability while having the benefits of water-based cosmetics such as a refreshing feeling and a moist feeling, by using a finger or a sponge. The inventors have found that cosmetics having improved water resistance and good water resistance can be obtained, and have completed the present invention.

[0006] That is, the present invention is a solid aqueous cosmetic containing sucrose fatty acid diester, a water-soluble ionic surfactant and agar.

Hereinafter, the configuration of the present invention will be described in detail. The agar used in the present invention is agarose, ie, [4-0]
-(Β-D-galactopyranosyl) -3,6-anhydro-L-galactose] as a main component, and is a so-called “agar” generally used for foods and the like. There are no limitations on the source algae, production method, and the like. Further, the agar may be subjected to a chemical treatment, a physical treatment, or a treatment with a microorganism or an enzyme for the purpose of adjusting the hardness of the agar, improving the removal in a product system, and the like. And about the compounding quantity of the agar in this invention, 0.05-1 in the whole composition
0.0% by weight, and particularly preferably in the range of 0.5 to 5.0% by weight. If the amount of agar is less than 0.05% by weight,
There is a problem in maintaining the form in the container. If the content exceeds 10.0% by weight, the content becomes too hard, and the removal with a finger or a sponge becomes worse.

As for water, 30.0 to 9% of the total composition
When blended at 5.0% by weight, especially at 50.0 to 80.0% by weight, excellent usability and portability can be obtained.

In the sucrose fatty acid diester of the present invention, the fatty acid is a saturated or unsaturated, linear or branched one having 12 to 22 carbon atoms, and the two fatty acids may be the same or different. Good. Examples of such fatty acids include stearic acid, oleic acid, palmitic acid, behenic acid, isostearic acid and the like. The blending amount of the sucrose fatty acid diester is 0.5 to 15.
0% by weight. If the content is less than 0.5% by weight, satisfactory water resistance cannot be obtained, and if the content exceeds 15.0% by weight, the content becomes hard and the removal with a finger or a sponge becomes poor.

In the present invention, even if other sucrose fatty acid esters (for example, monoester and triester) are contained as impurities in the sucrose fatty acid diester, the coating film has water repellency and water resistance. An aqueous cosmetic can be obtained. The monoester content is up to 30.0% by weight, preferably 20.0% by weight or less, more preferably 10.0% by weight or less. If the monoester content is high, an aqueous cosmetic that forms a coating film having water repellency and water resistance cannot be obtained. The content of triesters (including polyesters equal to or higher than triesters) is at most 40.0% by weight, preferably 30.0% by weight or less, more preferably 20.0% by weight or less. If the triester content is high, it is difficult to achieve dispersion or oil-in-water emulsification, and if achieved, the stability is reduced. In the total sucrose fatty acid ester, the sucrose fatty acid diester needs to be 50.0% by weight or more, preferably 60.0% by weight or more, more preferably 70.0% by weight or more.
0.0% by weight or more.

However, when a monoester and a triester coexist as impurities and the ratio of the monoester to the triester is in the range of 1: 3 to 1:20, the content of the diester is 50.0% by weight. %, And in this case, the content of the diester is 35.0% by weight or more, preferably 40.0% by weight or more.

Sucrose fatty acid diester is extremely dispersed in water even at a temperature higher than Tc (solid-liquid transition temperature of hydrate (temperature at which the hydrophobic chain of a hydrated surfactant changes from a solid state to a liquid state)). In order to obtain an oil-in-water emulsified composition, it is difficult to disperse the diester.
It is necessary to incorporate 5.0% by weight of the ionic surfactant, and the preferred amount is 0.3 to 10.0% by weight, more preferably 0.5 to 5.0% by weight. Further, 0.01 to 5.0% by weight is usually added to the total amount of the cosmetic. If the amount of the water-soluble ionic surfactant is too large, dispersion or oil-in-water emulsification can be easily achieved,
No water-repellent and water-resistant coating film is formed.

The ionic surfactants used in the present invention are those generally used for cosmetics and include, for example, fatty acid soaps (sodium laurate, sodium palmitate, etc.) and higher alkyl sulfates (lauryl). Sodium sulfate, potassium lauryl sulfate, etc.)
・ Alkyl ether sulfate (POE lauryl sulfate triethanolamine, POE lauryl sodium sulfate, etc.) ・ N-acyl sarcosine salt (lauroyl sarcosine sodium, etc.) ・ Higher fatty acid amide sulfonate (N-myristoyl-N-methyltaurine sodium) ,
Palm oil fatty acid sodium methyl tauride, sodium lauryl methyl tauride, etc.), phosphate salt (P
OE sodium oleyl ether phosphate, POE stearyl ether phosphoric acid, etc.), sulfosuccinate (di-2-
Sodium ethylhexyl sulfosuccinate, monolauroyl monoethanolamide polyoxyethylene sodium sulfosuccinate, sodium lauryl polypropylene glycol sulfosuccinate, etc., alkylbenzene sulfonates (sodium linear dodecylbenzenesulfonate, linear dodecylbenzenesulfonate triethanolamine, linear dodecylbenzene) Sulfonic acid etc.) ・ N-
Acyl glutamates (sodium N-lauroyl glutamate, disodium N-stearoyl glutamate, monosodium N-myristoyl-L-glutamate), higher fatty acid ester sulfates (hardened coconut oil fatty acid sodium glycerin sulfate, etc.), POE alkyl ether carboxylic acid Acid salt, POE alkyl allyl ether carboxylate, α-olefin sulfonate, higher fatty acid ester sulfonate, secondary alcohol sulfate, higher fatty acid alkylolamide sulfate,
Sodium lauroyl monoethanolamidosuccinate
Anionic surfactants such as N-palmitoyl aspartate ditriethanolamine and sodium caseinate; alkyl trimethyl ammonium salts (such as stearyl trimethyl ammonium chloride and lauryl trimethyl ammonium chloride); dialkyl dimethyl ammonium salts (such as distearyl dimethyl ammonium chloride); alkyl Pyridinium salts (poly [N, N-dimethyl-3,5-methylenepiperidinium chloride], cetylpyridinium chloride, etc.)
Alkyl quaternary ammonium salts, alkyl dimethyl benzene ammonium salts, alkyl isoquinolinium salts, dialkyl morphonium salts, POE alkylamines, alkylamine salts, polyamine fatty acid derivatives, amyl alcohol fatty acid derivatives, quaternary ammonium salts (benzalco chloride And a cationic surfactant such as benzethonium chloride).

Preferred ionic surfactants are anionic surfactants and cationic surfactants.
One or more of these are used in combination. Among them, particularly preferred are fatty acid soaps having 12 or more carbon atoms, and preferred counter ions include sodium, potassium, triethanolamine, ammonia and the like.

In addition, surfactants other than ionic surfactants can be included. Examples of such surfactants include imidazoline amphoteric surfactants (2-undecyl-N,
N, N- [hydroxyethylcarboxymethyl] -2-
Imidazoline sodium, 2-cocoyl-2-imidazolinium hydroxide-1-carboxyethyloxy 2
Amphoteric surfactants such as sodium salts) and betaine-based amphoteric surfactants (such as 2-heptadodecyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, laurylmethyl acetate betaine, alkyl betaine, amido betaine and sulfobetaine). Activators, sorbitan fatty acid esters (sorbitan monooleate, sorbitan monoisostearate, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate,
Sorbitan sesquioleate, sorbitan trioleate, diglycerol sorbitan penta-2-ethylhexylate, diglycerol sorbitan tetra-2-ethylhexylate, etc., glycerin or polyglycerin fatty acids (glycerin mono-cottonseed oil, glycerin monoerucate, sesquiolein, Acid glycerin, glyceryl monostearate, diglycerin monostearate α, α
-Glycerin pyroglutamate oleate, monosteering lyserine malic acid, etc.) propylene glycol fatty acid esters (propylene glycol monostearate, propylene glycol monolaurate, etc.), hydrogenated castor oil derivatives, glycerin alkyl ethers, POE
Sorbitan fatty acid esters (POE sorbitan monooleate, POE sorbitan monostearate, POE
Sorbitan monolaurate, POE sorbitan tetraoleate, etc.) / POE sorbitol fatty acid esters (P
OE sorbit monolaurate, POE sorbit monooleate, POE sorbit pentaoleate, PO
E-Sorbit monostearate, etc.) POE glycerin fatty acid esters (POE glycerin monostearate, POE glycerin monoisostearate, POE glycerin triisostearate, etc.) POE fatty acid esters (POE monooleate, POE distearate, polyethylene isostearate) Glycol etc.) ・ P
OE alkyl ethers (POE lauryl ether, P
OE oleyl ether, POE stearyl ether, P
OE behenyl ether, POE octyl dodecyl ether, POE cholestanol ether, etc.) POE alkyl phenyl ethers (POE octyl phenyl ether, POE nonyl phenyl ether, POE dinyl phenyl ether, etc.) POE-POP alkyl ethers (POE-POP) Cetyl ether, POE-POP2-
Decyl tetradecyl ether, POE-POP monobutyl ether, POE-POP hydrogenated lanolin, POE-P
OP glycerin ether, etc.) ・ Tetra POE-Tetra P
OP ethylenediamine condensates / POE castor oil or hydrogenated castor oil derivatives (POE castor oil, POE hydrogenated castor oil, POE hydrogenated castor oil monoisostearate, PO
E-hardened castor oil triisostearate, POE-hardened castor oil monopyroglutamic acid monoisostearate diester, POE-hardened castor oil maleic acid, etc.) / POE beeswax-lanolin derivative (POE sorbit beeswax, etc.)
・ Alkanolamides (coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, fatty acid isopropanolamide, etc.) ・ POE propylene glycol fatty acid ester ・ POE alkylamine ・ POE fatty acid amide ・ sucrose fatty acid ester ・ POE nonylphenylformaldehyde condensate ・ alkyl Nonionic surfactants such as ethoxydimethylamine oxide and trioleyl phosphate can be used. One or more of these may be selected and used. The content of the surfactant other than the ionic surfactant is 0.5 to 10.0% by weight in the solid aqueous cosmetic.

The oil component used in the present invention is generally used for cosmetics and has high skin safety. For example, liquid oils such as avocado oil, camellia oil, turtle oil, macadamia nut oil, mink oil, olive oil, Rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil, sasanqua oil, castor oil, linseed oil, safflower oil,
Solid oils such as cottonseed oil, soybean oil, peanut oil, teaseed oil, rice bran oil, jojoba oil, germ oil, triglycerin, glycerin trioctanoate, glycerin tripalmitate, etc. ·Palm oil·
Beeswax, sheep butter, hardened beef tallow, palm kernel oil, lard, beef tallow, beef tallow, hardened oil, hardened oil, beef leg oil, moles, hardened castor oil, beeswax, candelilla wax, cotton wax, carnauba wax・ Bayberry wax ・ Ibotaro wax ・ Whale wax ・ Montan wax ・ Nukarou ・ Lanolin ・ Kapok wax ・ Lanolin acetate ・ Liquid lanolin ・ Sugar cane wax ・ Lanoline fatty acid isostearyl ・ Hexyl laurate ・ Reduced lanolin ・ Jojobarou ・ Hard lanolin ・ Seraclow ・ Polyoxyethylene Lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid polyethylene glycol, etc., as liquid hydrocarbons such as liquid paraffin, ozokerite, squalane, pristane, etc.
Higher fatty acids such as paraffin, ceresin, squalene, vaseline, and microcrystalline wax, such as lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, 12-hydroxystearic acid, undecylenic acid, tolic acid, isostearic acid, Higher alcohols such as linoleic acid, linoleic acid, eicosapentaenoic acid and docosahexaenoic acid, such as lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, monostearyl glycerin ether, and 2-decyltetradecinol・ Lanolin alcohol ・ cholesterol ・ phytosterol ・ hexyldecanol ・ isostearyl alcohol ・
Octyldodecanol and other ester oils such as isopropyl myristate, cetyl octanoate, octyldodecyl myristate, isopropyl palmitate, butyl stearate, hexyl laurate, myristyl myristyl, decyl oleate, hexyldecyl dimethyloctanoate, cetyl lactate Myristyl lactate / lanolin lactate / isocetyl stearate / isocetyl isostearate /
Cholesteryl di-2-hydroxystearate di-2-
Ethyl hexyl ethyl glycol / dipentaerythritol fatty acid ester / monoisostearic acid-N-
Alkyl glycol, neopentyl glycol dicaprate, diisostearyl malate, glycerin di-2-heptylundecanoate, trimethylolpropane tri-2-ethylhexylate, trimethylolpropane triisostearylate, pentaerythritol tetra-2-ethylhexylate -Glycerin tri-2-ethylhexylate-trimethylolpropane triisostearate-cetyl 2-ethylhexanoate-2-ethylhexyl palmitate-glycerin trimmyristate-tri-2-
Heptylundecanoic acid glyceride, castor oil fatty acid methyl ester, oleic acid oil, cetostearyl alcohol, acetoglyceride, 2-heptylundecyl palmitate, diisobutyl adipate, N-lauroyl-L-glutamic acid-2-octyldodecyl ester, adipic acid Di-2-heptylundecyl ethyl laurate sebacate di-2-ethylhexyl myristate 2-hexyldecyl palmitate 2-hexyldecyl adipate 2-hexyldecyl diisopropyl sebacate 2-ethylhexyl succinate Ethyl acetate, butyl acetate, amyl acetate, triethyl citrate, etc., as silicones such as dimethylpolysiloxane, methylphenylpolysiloxane, methylhydrogenpolysiloxane, decamethyl Silicone resin, silicone rubber or the like to form a polysiloxane-dodecamethyl polysiloxane tetramethyl hydrogen polysiloxane three-dimensional network structure, and the like, but not limited to the above components. The content of these oils is 1.0 to 30.0% by weight, preferably 5.0 to 20.0% by weight in the solid aqueous cosmetic.

The powders used in the present invention are those generally used for cosmetics, and include talc, kaolin, mica, sericite, muscovite, phlogopite, synthetic mica, rhodolite and biotite.・ Lithia mica ・ Vermiculite ・ Magnesium carbonate ・ Calcium carbonate ・ Aluminum silicate ・ Barium silicate ・ Calcium silicate ・ Magnesium silicate ・ Strontium silicate ・ Metal salt ・ Magnesium ・ Silica ・ Zeolite ・ Barium sulfate ・ Calcium sulfate ・Inorganic powders such as calcined gypsum, calcium phosphate, fluoroapatite, hydroxyapatite, ceramic powder, metal soap (zinc myristate, calcium palmitate, aluminum stearate), boron nitride, polyamide resin powder, polyethylene powder, polymeta Organic powders such as methyl acrylate powder, polystyrene powder, styrene-acrylic acid copolymer resin powder, benzoguanamine resin powder, polytetrafluoroethylene powder, and cellulose powder; inorganic white pigments such as titanium dioxide and zinc oxide; and iron oxide Inorganic red pigments such as (Bengara) and iron titanate, inorganic brown pigments such as γ-iron oxide, inorganic yellow pigments such as yellow iron oxide and loess, black iron oxide, carbon black, and lower titanium oxide Inorganic black pigments, inorganic purple pigments such as mango violet and cobalt violet,
Inorganic green pigments such as chromium oxide / chromium hydroxide / cobalt titanate, inorganic blue pigments such as ultramarine / dark blue, titanium oxide coated mica / titanium oxide coated bismuth oxychloride / titanium oxide coated talc / colored titanium oxide coated mica / Pearl pigments such as bismuth oxychloride and fish scale, metal powder pigments such as aluminum powder and copper powder, Red No. 201, Red No. 202, Red No. 204, Red No. 205, Red No. 220, Red No. 226, Red No. 228. Red 405 / Orange 203 / Orange 2
Organic pigments such as No. 04 / Yellow 205 / Yellow 401 / Blue 404, Red No.3 / Red No.104 / Red No.106 /
Red 227, Red 230, Red 401, Red 50
No. 5, orange 205, yellow 4, yellow 5, yellow 202
Organic pigments such as zirconium, barium and aluminum lakes such as No. 203, yellow No. 203, green No. 3 and blue No. 1, and natural pigments such as chlorophyll and β-carotene.
One or more of these may be arbitrarily selected and used. In the present invention, these powders may be subjected to a hydrophobic treatment in order to improve the hydrophobicity of these powders. Examples of the hydrophobic substance used in the hydrophobizing treatment include metal soaps, fats and oils, waxes, silicone compounds, fluorine compounds, hydrocarbons, fatty acid esters, and the like. The content of these powders in the solid aqueous cosmetic is preferably 1.0 to 40.0% by weight, more preferably 5 to 30.0% by weight.

The solid aqueous cosmetic composition of the present invention may further comprise, if necessary, a humectant, a preservative, an antioxidant,
It is possible to use ultraviolet absorbers, lower alcohols, polyhydric alcohols, fragrances, drugs and the like under qualitative and quantitative conditions that do not impair the effects of the present invention. In addition, a cooling agent such as 1-menthol, camphor, a salicylic acid derivative, or a tranexamic acid derivative may be contained in order to improve the refreshing sensation, which is a characteristic of the aqueous cosmetics.

The solid aqueous cosmetic of the present invention is obtained by dispersing and dissolving sucrose fatty acid diester, a water-soluble ionic surfactant, and agar in water. It can be applied to products such as emulsions, solid serums, makeup bases, foundations, blushers, eye shadows, eye liners, sun care products, body cosmetics, and the like.

[0020]

Next, the present invention will be described in detail with reference to examples. The present invention is not limited by this.
In addition, the compounding amount is wt% unless otherwise specified. First,
A production example of a sucrose fatty acid diester characteristic of the present invention will be described.

Production Example 1 Purification of Sucrose Stearic Acid Diester (1) In a 1 L beaker, 100 g of commercially available sucrose stearic acid ester containing about 30% of diester was weighed.
A mixture of 855 ml of methanol and 45 ml of water is added, and the sample is dissolved once near the boiling point of the solvent. Then, add 4
After keeping the temperature at 4 ° C and separating into two layers, the upper layer (solution phase) is separated. The main component of the lower layer (solid phase) is a triester, and the upper layer mainly contains a monoester and a diester. (2) Methanol concentration of about 80 (V / V)
%, The temperature is raised to 60 ° C., a precipitate is formed at 25 ° C., and the precipitate is collected. The upper layer is mainly composed of monoester, and the precipitate is mainly composed of diester. (3) The precipitate obtained in (2) was dissolved in 720 ml of methanol, 180 ml of water was added to the solution, and the mixture was stirred.
To generate a precipitate, and the precipitate is collected. (4) By repeating the operation of (3), a composition containing about 80% or more of sucrose stearic acid diester was obtained. Ingredients other than sucrose stearic acid diester were sucrose fatty acid monoester, triester, stearic acid, sodium stearate and the like. In addition,
The yield based on the starting sucrose fatty acid ester was about 33%.

Production Example 2 Purification of sucrose oleic acid mono- and diesters (1) In a 1 L beaker, 50 g of a commercially available sucrose oleic acid ester containing about 70% of a monoester was weighed, and 760 ml of methanol and 190 ml of water were weighed. The mixed solution is added and dissolved, and the mixture is allowed to stand at −20 ° C., and after two-phase separation, a precipitated portion (lower layer) is separated. Here, the upper layer is mainly composed of monoester, and the precipitate (lower layer) is mainly composed of a mixture of diester and triester. (2) 760 ml of methanol and 19
0 ml of the mixed solution is added to dissolve the mixture, and the mixture is allowed to stand at −20 ° C., and then subjected to two-phase separation again to separate a precipitated portion. This operation is repeated twice. Here, upper layer is monoester, precipitate (lower layer)
Has a diester and a triester as main components. (3) The upper layer obtained in (1) and (2) was concentrated to obtain sucrose oleate monoester. The purity of the sucrose oleate monoester was about 95%, and the yield was about 65% based on the raw sucrose oleate. (4) The lower layer obtained in (1) and (2) is dissolved in a 97% methanol solution, and left at room temperature to separate the upper layer. (5) The upper layer obtained in (4) was concentrated and dried to obtain sucrose oleic acid diester. The purity of the sucrose oleic diester was 65% or more, and the yield based on the raw sucrose oleic ester was about 25%.

Production Example 3 Purification of sucrose stearic acid diester by column chromatography (1) Using 400 ml of chloroform as a solvent, 200 g of commercially available silica gel for column chromatography was swollen, filled in a column chromatography tube, and prepared according to Production Method 1. About 10 g of the obtained crude sucrose stearic acid diester is added. (2) Elution is performed sequentially using the following solvents. Methanol: chloroform = 8:92 (volume ratio) 1
L methanol: chloroform = 15: 85 (volume ratio) 1
L methanol: chloroform = 25: 75 (volume ratio) 1
The L eluate was fractionated by 70 ml, and sucrose stearic acid diester was confirmed by gas chromatography and TLC for each fraction.
When the diester fraction was concentrated, about 4 g of sucrose stearic diester could be collected.

Production Example 4 Purification of sucrose oleic acid diester by column chromatography (1) Using 400 ml of chloroform as a solvent, 200 g of commercially available silica gel for column chromatography was swollen, filled in a column chromatography tube, and prepared according to Production Method 2. About 10 g of the obtained crude sucrose oleic acid diester is added. (2) Elution is performed sequentially using the following solvents. Methanol: chloroform = 6:94 (volume ratio) 1
L methanol: chloroform = 12: 88 (volume ratio) 1
L methanol: chloroform = 20: 80 (volume ratio) 1
The L eluate was fractionated in 70 ml portions, and sucrose oleate diester was confirmed by gas chromatography and TLC for each fraction. When the diester fraction was concentrated, about 2.5 g of sucrose oleic acid diester could be collected.

Production Example 5 Purification of sucrose stearic acid diester (1) In a 1 L beaker, 100 g of commercially available sucrose stearic acid ester containing about 30% of diester was weighed,
A mixture of 800 ml of methanol and 100 ml of water is added, and the sample is dissolved once at a temperature near the boiling point of the solvent.
Thereafter, a precipitate was formed at 35 ° C., and the precipitate was fractionated to obtain a composition containing about 40% of sucrose stearic diester and about 50% of sucrose stearic triester. Ingredients other than sucrose stearic acid diester and sucrose stearic acid triester include sucrose stearic acid monoester, stearic acid,
It was sodium stearate. The yield based on the raw material stearic acid ester was about 75%.

Example 1, Comparative Examples 1-4 An emulsified foundation (Example 1, Comparative Examples 1-2, 4) having the formulation shown in Table 1 was prepared by the following method, and a commercially available emulsion foundation having the formulation shown in Table 2 was prepared. At the same time as the solid emulsified foundation (water-in-oil emulsified type, Comparative Example 3), a sensory evaluation was performed according to the following evaluation methods and evaluation criteria. Table 3 shows the results. The sucrose oleic acid diester used was purified in Production Example 4.

(Preparation of Example 1 and Comparative Examples 1-2, 4) The components (1)-(8) were mixed by heating, and mixed and ground (9)-(15) were added thereto, followed by homomixing. And uniformly dispersed.
Separately, (16) to (21) were prepared by heating (oil phase), and the aqueous phase and the oil phase were mixed and emulsified by a homomixer, and then filled in a container and cooled to obtain a solid emulsified foundation.

(Production method of Comparative Example 3) (1) to (9) were heated and dissolved, and then mixed and pulverized (10) to (15) were added thereto and uniformly dispersed with a homomixer. After adding (16) and (17) to the mixture and mixing and emulsifying with a homomixer, the mixture was filled in a container and cooled to obtain a solid emulsified foundation.

(Evaluation Method and Evaluation Criteria) (1) Retention of Form in Container When the emulsion foundation filled in a dish-shaped container was stored at 50 ° C. for one month, the fluidity was confirmed as ×. Those that were not performed were marked with ○.

(2) Removal of foundation, refreshing sensation, moist feeling, freshness, lack of film feeling after application, and make-up (water resistance) Sensory evaluation was conducted by 10 professional panelists according to the following criteria.

A: Very good. ：: Somewhat good. Δ: Somewhat bad. X: Very bad.

[0032]

[Table 1] Component Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 4 ─────────────────────────────────── (1) Purified water Residue Residue Residue Residue (2) Propylene Glycol 10.0 10.0 10.0 10.0 (3) Sodium stearate 0.1 0.1 0.1 − (4) Coolant appropriate amount appropriate amount appropriate amount appropriate amount (5) agar 2.5 2.5 − 1.0 (6) sucrose oleic diester 5.0 − 5.0 − (7) triethanolamine − − − 0.2 (8) Carboxyvinyl polymer − − − 1.2 (9) Talc 3.0 3.0 3.0 − (10) Titanium dioxide 5.0 5.0 5.0 − (11) Fluorine compound treated talc − − − 3.0 (12) Fluorine compound treated titanium dioxide − − − 5.0 (13) Bengala 0.5 0.5 0.5 0.5 (14) Yellow iron oxide 1.4 1.4 1.4 1.4 (15) Black iron oxide 0.1 0.1 0.1 0.1 (16) Stearic acid − − − 2 .0 (17) Isohexadecyl alcohol 7.0 7.0 7.0 7.0 (18) Liquid lanolin 2.0 2.0 2.0 2.0 (19) Liquid paraffin 8.0 8.0 8.0 8.0 (20) Preservatives proper amount proper amount proper amount proper amount (21) Flavor proper amount proper amount proper amount proper amount ── ─────────────────────────────────

[0033]

[Table 2] Component Comparative Example 3 ────────────────────────── (1) Dimethylpolysiloxane 10.0 (2) Decamethylcyclopentasiloxane 15.0 (3) Squalane 3.0 (4) Glycerin trioctanoate 1.0 (5) Polyoxyethylene-modified dimethylpolysiloxane 3.0 (6) Solid paraffin 5.0 (7) Carnauba wax 3.0 (8) Preservatives qs (9) Fragrance qs (10) Silicone treated titanium oxide 10.0 (11) silicone Treated Bengala 0.36 (12) Silicone-treated iron oxide yellow 0.8 (13) Silicone-treated black iron oxide 0.16 (14) Talc 11.68 (15) Sericite 7.0 (16) Purified water Residue (17) 1,3-butylene glycol 4.0 ── ────────────────────────────────

[0034]

[Table 3] ──────────────────────────────── Example Comparative example Evaluation item ──────── ──────────── 1 1 2 3 4 ──────────────────────────────── Container Retention of form inside ○ ○ × ○ ○ Removal of foundation ○ △ △ ◎ △ Cool feeling ◎ ◎ ◎ × ◎ Moist feeling ◎ ◎ ◎ × ◎ Freshness ◎ ◎ ◎ × ◎ No film feeling after application ○ × ○ ◎ △ Makeup (water resistant) ◎ × ◎ ◎ × ────────────────────────────────

As is clear from Table 3, Comparative Example 1 has almost the same refreshing sensation, moist feeling, and freshness as Example 1, and there is no problem in maintaining the form in the container. There are problems with lack of film feeling, lack of foundation, and stickiness (water resistance). Comparative Example 2 had the same advantages as Comparative Example 1, but had a problem in maintaining the form in the container, and was insufficient as a solid aqueous cosmetic. Although Comparative Example 3 solved the disadvantages of Comparative Examples 1 and 2, it lacked a refreshing sensation, moistness, and freshness because it was a water-in-oil emulsion type.
Comparative Example 4 is a solid cosmetic according to the existing technology (Japanese Patent Application Laid-Open No. 5-178723), but has the same drawbacks as Comparative Example 1. On the other hand, Example 1 was a solid emulsification foundation of an oil-in-water type emulsification type, which was unusual in that the usability was good and the shape retention in the container was satisfactory.

Example 2 Solid lotion (1) Purified water residue (2) Sorbit 4.0% by weight (3) Dipropylene glycol 6.0 (4) Polyethylene glycol 1500 5.0 (5) Sucrose stearic acid Diester 2.0 (6) Agar 4.0 (7) Potassium stearate 0.1 (8) Ethanol 10.0 (9) Coolant appropriate amount (10) Flavor appropriate amount (11) Preservative appropriate amount (12) Chelating agent appropriate amount (13) Appropriate amount of anti-browning agent (14) Appropriate amount of buffering agent (Preparation method) Take a part of (1) and use (2)-(5), (7) and (12)-
Add (14) and dissolve. (9) to (11) are added to (8), dissolved, and added to the above solution and mixed. Add (6) to the rest of (1),
The solution dissolved by heating was added and cooled to obtain a solid lotion.

Example 3 Solid emulsion (1) Purified water residue (2) Ethanol 5.0% by weight (3) Glycerin 4.0 (4) 1,3-butylene glycol 4.0 (5) Agar 3.5 (6) Sucrose stearic acid diester 2.5 (7) Stearic acid triethanolamine salt 0.2 (8) Coolant appropriate amount (9) Cetyl alcohol 1.0 (10) Beeswax 0.5 (11) Vaseline 2. 0 (12) Squalane 6.0 (13) Dimethylpolysiloxane 2.0 (14) Preservative proper amount (15) Flavor proper amount (Production method) Add (2) to (8) to (1) and heat and dissolve at 70 ° C And
Those prepared by heating (9) to (15) to 70 ° C. were added, mixed, and cooled to obtain a solid emulsion.

Example 4 Makeup Base (1) Purified Water Residue (2) Propylene Glycol 10.0% by Weight (3) Agar 2.5 (4) Sucrose Oleic Acid Diester 4.0 (5) Potassium Oleate 2 (6) Appropriate amount of cooling agent (7) Isohexadecyl alcohol 7.0 (8) Liquid lanolin 2.0 (9) Liquid paraffin 8.0 (10) Preservatives appropriate amount (11) Flavoring appropriate amount (production method) (1) The components (1) to (6) are mixed by heating at 70 ° C.
Keep at ° C (aqueous phase). Separately, (8) to (11) were prepared by heating at 70 ° C. (oil phase), the aqueous phase and the oil phase were mixed and emulsified by a homomixer, and then filled into a container and cooled to obtain a solid makeup base. .

Example 5 Blush (1) Purified Water Residue (2) Propylene Glycol 10.0% by Weight (3) Agar 2.5 (4) Sucrose Oleic Diester 5.0 (5) Sodium Oleate 0.1 (6) Appropriate amount of cooling agent (7) Talc 7.0 (8) Titanium dioxide 2.0 (9) Iron oxide (red) 0.3 (10) Red No. 202 0.5 (11) Isohexadecyl alcohol 0 (12) Liquid lanolin 2.0 (13) Liquid paraffin 8.0 (14) Preservative proper amount (15) Flavor proper amount (Production method) Heat and mix each component of (1) to (6) at 70 ° C, Then, (7) to (10) mixed and ground are added, and the mixture is uniformly dispersed with a homomixer and kept at 70 ° C. (aqueous phase). Separately from (11) to (15)
The mixture was heated at 0 ° C. (oil phase), and the aqueous phase and the oil phase were mixed and emulsified by a homomixer, filled in a container and cooled to obtain a solid emulsified blusher.

Example 6 Eye Shadow (1) Purified Water Residue (2) 1,3-butylene glycol 5.0% by weight (3) Glycerin 1.0 (4) Preservative Appropriate amount (5) Agar 3.0 (6) ) Sucrose oleic acid diester 4.0 (7) Potassium oleate 0.1 (8) Coolant appropriate amount (9) Talc 10.0 (10) Kaolin 2.0 (11) Color pigment 5.0 (12) Myristin Isopropyl acid 8.0 (13) Propylene glycol monolaurate 3.0 (14) Perfume Appropriate amount (Production method) Each component of (1) to (8) was heated and mixed at 70 ° C, and mixed and pulverized (9) to Add (11), uniformly disperse with a homomixer, and maintain at 70 ° C. (aqueous phase). Separately from (12) to (14)
The mixture was heated at 0 ° C. (oil phase), and the aqueous phase and the oil phase were mixed and emulsified by a homomixer, and then filled in a container and cooled to obtain a solid emulsified eye shadow.

Example 7 Lipstick (1) Purified water residue (2) 1,3-butylene glycol 5.0% by weight (3) Glycerin 1.0 (4) Preservative appropriate amount (5) Agar 3.0 (6) Sucrose stearic acid diester 4.0 (7) Potassium stearate 0.1 (8) Titanium dioxide 4.5 (9) Red 201 No. 0.5 (10) Red 202 No. 2.0 (11) Red 223 0 1 (12) Isopropyl myristate 8.0 (13) Propylene glycol monolaurate 3.0 (14) Liquid paraffin 3.0 (15) Candelilla wax 5.0 (16) Perfume appropriate amount (production method) (1)- The components of (7) were heated and mixed at 70 ° C., and the mixed and pulverized (8) to (11) were added thereto, uniformly dispersed with a homomixer, and kept at 70 ° C. (aqueous phase). Separately, (12)-(16)
The mixture was heated at 0 ° C. (oil phase), and the aqueous phase and the oil phase were mixed and emulsified by a homomixer, and then filled in a container and cooled to obtain an emulsified lipstick.

Example 8 Solid lotion (1) Purified water residue (2) Sorbit 4.0% by weight (3) Dipropylene glycol 6.0 (4) Polyethylene glycol 1500 5.0 (5) Sucrose stearic acid Diester 1.5 (6) Sucrose stearic acid monoester 0.2 (7) Sucrose stearic acid triester 0.1 (8) Agar 4.0 (9) Potassium stearate 0.1 (10) Ethanol 10. 0 (11) Suitable amount of freshener (12) Suitable amount of fragrance (13) Suitable amount of preservative (14) Suitable amount of chelating agent (15) Suitable amount of anti-browning agent (16) Suitable amount of buffer agent (Preparation method) 2)-(7), (9) and (14)-
Add (16) and dissolve. (11) to (13) are added to (10), dissolved, and added to the above solution and mixed. (8) was added to the remainder of (1), and the solution obtained by heating and dissolving was added, followed by cooling to obtain a solid lotion.

[0043]

As described above, the solid aqueous cosmetic of the present invention has usability (coolness, moisture, freshness, etc.) which was difficult to achieve with conventional solid cosmetics.
Moreover, it is a dosage form with excellent portability, and has water repellency,
It is an unprecedented breakthrough solid water-based cosmetic with excellent water resistance.

Claims (3)

[Claims] 1. A solid aqueous cosmetic comprising sucrose fatty acid diester, a water-soluble ionic surfactant and agar. 2. A water-soluble ionic interface containing 0.5 to 15.0% by weight of sucrose fatty acid diester based on the total amount of the cosmetic and 0.05 to 10.0% by weight of agar based on the total amount of the cosmetic. The activator is used in an amount of 0.2 to 1 based on the sucrose fatty acid diester.
The solid aqueous cosmetic according to claim 1, which contains 5.0% by weight. 3. The water-soluble ionic surfactant has 1 carbon atom.
3. The solid aqueous cosmetic according to claim 1, which is two or more fatty acid soaps.