JP2002309283A - METHOD FOR SUPPRESSING beta-CRYSTALLIZATION OF FATTY ACID MONOGLYCERIDE AND EMULSIFIED COMPOSITION - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain an emulsified composition which can sufficiently suppress the β-crystallization of a fatty acid monoglyceride and excels in not only an external appearance and a feeling of use but also emulsification stability. SOLUTION: A method for suppressing the β-crystallization of the fatty acid monoglyceride comprises stirring and mixing a water-swelling clay mineral and the fatty acid monoglyceride to modify the water-swelling clay mineral with the fatty acid monoglyceride. The emulsified composition can be obtained by incorporating the water-swelling clay mineral and the fatty acid monoglyceride modified product obtained by mixing and modifying the water- swelling clay mineral with the fatty acid monoglyceride.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a method for suppressing β-type crystallization of fatty acid monoglyceride and an emulsified composition, and more particularly to a method and an emulsion capable of effectively suppressing β-type crystallization of fatty acid monoglyceride. The present invention relates to an emulsion composition having excellent stability.

[0002]

2. Description of the Related Art Fatty acid monoglycerides include sub-α,
It is known that the α-form is preferable to have crystal polymorphs called α and β and to obtain good emulsifying properties and foamability. However, for example, it is difficult to maintain the α-form in the emulsified composition, and there is a problem that the composition changes to a stable β-form and large crystals are formed, so that the appearance and usability of the composition deteriorate.

As a countermeasure against such a problem, a higher alcohol or a propylene glycol fatty acid ester has been used, but there are problems such as a bad smell and a bad texture of the cream, and the problem has not been solved.

Japanese Patent Application Laid-Open No. 55-59106 discloses that an oil-in-water emulsion composition obtained by reacting and emulsifying a basic amino acid with a higher fatty acid having 14 to 22 carbon atoms or beeswax contains α-monoglyceryl. An oil-in-water emulsion composition in which crystallization of a higher fatty acid is suppressed by blending an ether. JP-A-5-56757 discloses a method for producing an emulsified foaming agent powder in which crystallization is suppressed by propylene glycol fatty acid ester. JP-A-11-290669 proposes an emulsified composition in which the growth of β-type crystals of fatty acid monoglyceride is suppressed by the combined use of 12-hydroxystearic acid monoglyceride, and these proposals all disclose fatty acid monoglyceride. Stable emulsification of fatty acid monoglyceride with good appearance and usability and stable β-type crystallization Emulsified composition was not intended is obtained.

[0005]

DISCLOSURE OF THE INVENTION The present invention has been made in view of the above circumstances, and a method for effectively suppressing β-type crystallization of fatty acid monoglyceride, and a method for suppressing β-type crystallization of fatty acid monoglyceride, It is an object of the present invention to provide an emulsified composition capable of preparing an emulsion having good appearance and feeling of use and excellent emulsification stability by utilizing the emulsifying property of the fatty acid monoglyceride, which has been suppressed from becoming emulsified.

[0006]

Means for Solving the Problems and Embodiments of the Invention As a result of intensive studies to achieve the above object, the present inventor has found that
As shown in Examples described later, when the fatty acid monoglyceride is mixed and modified with a water-swellable clay mineral, β-type crystallization of the fatty acid monoglyceride can be suppressed, and thus the fatty acid monoglyceride is mixed with the water-swellable clay mineral. By using the modified water-swellable clay mineral / fatty acid monoglyceride modified product, it has been found that an emulsified composition having not only excellent appearance and usability but also excellent emulsification stability can be obtained, and the present invention has been made. Reached.

That is, the present invention provides (1) a water-swellable clay mineral and a fatty acid monoglyceride which are stirred and mixed, and the fatty acid monoglyceride is modified with the water-swellable clay mineral to obtain β-type crystallization of the fatty acid monoglyceride. A method for suppressing β-type crystallization of fatty acid monoglyceride, characterized by suppressing water content, and (2) blending a water-swellable clay mineral / fatty acid monoglyceride modified product obtained by mixing and modifying a fatty acid monoglyceride with a water-swellable clay mineral. An emulsified composition is provided.

Hereinafter, the present invention will be described in more detail. The method for suppressing β-type crystallization of a fatty acid monoglyceride according to the present invention comprises stirring and mixing a water-swellable clay mineral and a fatty acid monoglyceride to form the water-swellable clay mineral. By mixing and modifying the fatty acid monoglyceride, the β-type crystallization of the fatty acid monoglyceride is suppressed, and the emulsified composition of the present invention is a water-swellable clay in which the β-type crystallization of the fatty acid monoglyceride is suppressed by the method. It contains modified mineral and fatty acid monoglyceride.

Here, the type of the water-swellable clay mineral used in the present invention is not particularly limited as long as it is commonly used in cosmetics and the like. Examples of the water-soluble clay mineral include natural or synthetic water-swellable clay minerals such as montmorillonite, saponite, hectorite, beidellite, nontronite, stevensite, sauconite, bentonite, and the like. The above can be used in appropriate combinations. In the case of the present invention, among these, montmorillonite, hectorite, bentonite and the like are particularly preferable.

As the fatty acid monoglyceride used in the present invention, the kind of the constituent fatty acid is not particularly limited, but the constituent fatty acid is preferably a linear saturated fatty acid, and the constituent fatty acid has 12 to 22 carbon atoms. , Especially 14-20
Is more preferable. More specifically, the constituent fatty acids are lauric acid, myristic acid,
Fatty acid monoglycerides such as palmitic acid, stearic acid, arachidic acid, behenic acid and the like are mentioned.
The species can be used alone or in combination of two or more.

Here, if the water swellable clay mineral / modified fatty acid monoglyceride in which the β-type crystallization of fatty acid monoglyceride is suppressed by the method for suppressing β-type crystallization of fatty acid monoglyceride of the present invention, the fatty acid monoglyceride used Regardless of the purity of the emulsion, a stable emulsion composition can be obtained, but in order to obtain an emulsion composition having a better appearance, the purity must be 40% or more, more preferably 40 to 1
It is preferred to use 00%, more preferably 50-100% fatty acid monoglycerides. If the purity is less than 40%, the particles of the emulsified composition may become coarse as a whole.

In the present invention, the ratio of the water-swellable clay mineral to the fatty acid monoglyceride is not particularly limited, but is usually water-swellable clay mineral / fatty acid monoglyceride (mass ratio) = 20/1 to 1 / 3, especially 10/1 ~
It is preferred to use at a ratio of 1/2. When the ratio of the water-swellable clay mineral to the fatty acid monoglyceride is larger than 20/1, the ratio of the water-swellable clay mineral increases, so that the viscosity of the emulsified composition becomes extremely high and the usability may be deteriorated. In addition, when the ratio is less than 1/3 and the ratio of fatty acid monoglyceride increases, it may be difficult to sufficiently obtain the effect of suppressing β-type crystal growth.

The method of the present invention for inhibiting β-type crystallization of fatty acid monoglyceride involves mixing and modifying the fatty acid monoglyceride with a water-swellable clay mineral, and the mixing conditions for mixing and modifying are not particularly limited. Although not preferred, preferred stirring devices include stirring blades capable of performing total mixing, for example, a stirring tank equipped with a propeller, a turbine, a disperser, and the like, a kneader, an azihomomixer, a unimixer, and the like. The peripheral speed (m / s) of the stirrer during mixing and denaturation is:
It is preferable to mix at 0.5 m / s or more, especially 1-1.
It is particularly preferable to carry out mixed denaturation at 5 m / s. When the peripheral speed is less than 0.5 m / s, the fatty acid monoglyceride may be easily crystallized in β-form due to insufficient modification. The mixing time can be appropriately set depending on the type of the stirrer, the purpose and use of the emulsified composition, and is usually 20 to 1
It is desirable to mix for 20 minutes, especially 30 to 100 minutes.

In the method for suppressing β-type crystallization of fatty acid monoglyceride of the present invention, it is possible to mix together components which do not hinder the modification during the above-mentioned mixed modification. For example, olive oil, jojoba oil, castor oil, coconut oil, corn oil, rapeseed oil,
Squalane, oleic acid, lauric acid, myristic acid,
Isostearic acid, palmitic acid, isopropyl myristate, butyl stearate, isopropyl palmitate, octyldodecyl myristate, cetyl octanoate, octyldodecyl myristate, hexyl laurate, myristyl myristate, decyl oleate, 2-hexyldecyl myristate And oils such as 2-hexyldecyl palmitate, and the amount of these can be appropriately selected within a range that does not impair the effects of the present invention.

In the present invention, the fact that the fatty acid monoglyceride has been modified with a water-swellable clay mineral can be confirmed by disappearance of the peak pattern of the fatty acid monoglyceride by, for example, X-ray diffraction.

The emulsified composition of the present invention contains a water-swellable clay mineral / fatty acid monoglyceride modified product obtained by mixing and modifying the fatty acid monoglyceride with a water-swellable clay mineral as described above. The amount of the water-swellable clay mineral / fatty acid monoglyceride modified product in the emulsion composition is not particularly limited, and can be appropriately selected depending on the components of the composition, applications, dosage forms, and the like. It is preferably from 0.1 to 20% by mass, particularly preferably from 0.5 to 10% by mass, based on the total amount of the substance. If the amount of the water-swellable clay mineral / modified fatty acid monoglyceride is less than 0.1% by mass, a stable emulsion may not be prepared. Also, if the amount is more than 20% by mass,
The viscosity of the composition may be high, and the feeling of use may be poor.

The content of the fatty acid monoglyceride or the water-swellable clay mineral in the emulsified composition of the present invention is not particularly limited. 10% by mass, more preferably 0.2 to 8% by mass, and the above water so as to be 0.1 to 12% by mass, more preferably 0.2 to 10% by mass of the total amount of the composition as the water-swellable clay mineral. When a modified swelling clay mineral and fatty acid monoglyceride are blended,
More preferred. If the content of the fatty acid monoglyceride is too small, emulsification may be difficult, and if it is too large, formulation design may be restricted. On the other hand, if the content of the water-swellable clay mineral is too small, the β-type crystallization of the fatty acid monoglyceride may not be sufficiently suppressed, and if it is too large, there may be a limitation in formulation design.

The use and purpose of the emulsified composition of the present invention are not particularly limited.
It can be widely applied as a quasi-drug, especially as a composition for external use. More specifically, cosmetics can be widely applied in the form of facial cleanser, milky lotion, cream, serum, pack, and the like. In addition, makeup cosmetics can be widely applied to forms such as foundations.
Furthermore, if it is a medicine or a quasi-drug, it can be widely applied to various ointments and the like. When used for the scalp, it can be widely applied to forms such as emulsified hair tonics and emulsified hair lotions. These dosage forms and forms are not limited to those described above, and the dosage form and form are not particularly limited as long as they are the emulsion composition of the present invention.

The emulsified composition of the present invention includes surfactants, oils, alcohols / polyhydric alcohols, water-soluble polymer compounds, and preservatives which are used in ordinary emulsified compositions as long as the effects of the present invention are not impaired.・ Antibacterial agent, antioxidant, ultraviolet absorber,
Powder, humectant, viscosity modifier, vitamins, amino acids,
A normal amount of a plant extract, an active ingredient, a pH adjuster, a pigment, a fragrance, an inorganic salt, a solubilizing agent, a pearl appearance-imparting agent, etc., can be added. These types are not particularly limited, but examples include the following.

Surfactants that can be used in the present invention include, for example, sodium cetyl sulfate, POE lauryl ether phosphoric acid, sodium lauryl phosphate, triethanolamine palmitate, sodium N-acylglutamate, soap base, sodium laurate Fatty acid soaps such as sodium stearate, sodium palmitate, sodium lauryl sulfate, potassium lauryl sulfate, POE triethanolamine lauryl sulfate, PO
E Sodium lauryl sulfate, sodium lauroyl sarcosine, N-myristoyl-N-methyl taurine sodium, coconut oil fatty acid methyl tauride sodium, lauryl methyl tauride sodium, POE sodium oleyl ether phosphate, POE stearyl ether phosphate, di-2 -Sulfosuccinates such as sodium ethylhexyl sulfosuccinate, monolauroyl monoethanolamide POE sodium sulfosuccinate, lauryl polypropylene glycol sodium sulfosuccinate, linear sodium dodecylbenzenesulfonate, linear sodium dodecylbenzenesulfonate triethanolamine, linear dodecylbenzenesulfone Acid, monosodium N-lauroylglutamate, disodium N-stearoylglutamate, N-milli Toyl -L- monosodium glutamate, hydrogenated coconut oil fatty acid glycerin sodium sulfate, turkey red oil, POE alkyl ether carboxylic acids, P
OE alkyl allyl ether carboxylate, α-olefin sulfonate, higher fatty acid ester sulfonate,
Anionic surfactants such as secondary alcohol sulfates, higher fatty acid alkylolamide sulfates, sodium lauroyl monoethanolamide succinate, N-palmitoyl aspartate ditriethanolamine, sodium caseinate, stearyl dimethyl benzyl ammonium chloride, stearyl chloride Alkyl trimethylammonium salts such as trimethylammonium and lauryltrimethylammonium chloride, distearyldimethylammonium dialkyldimethylammonium chloride, alkyl such as poly (N, N'-dimethyl-3,5-methylenepiperidinium) chloride and cetylpyridinium chloride Pyridinium salt, alkyl quaternary ammonium salt, alkyldimethylbenzylammonium salt, alkylisoquinolinium salt, dialkylmoly Phonium salts, POE alkylamines, alkylamine salts, polyamine fatty acid derivatives, amyl alcohol fatty acid derivatives, cationic surfactants such as benzalkonium chloride, benzethonium chloride, alkylaminoethylene glycine chloride solution, lecithin, 2-undecyl-N- ( Hydroxyethylcarboxymethyl) -2-
Imidazoline sodium, 2-cocoyl-2-imitazolinium hydroxide-1-carboxyethyloxy 2
Sodium salt, 2-heptadecyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine,
Amphoteric surfactants such as betaine lauryldimethylaminoacetate, alkylbetaine, amidobetaine and sulfobetaine, sucrose fatty acid ester, polyethylene glycol monostearate, POE coconut fatty acid monoethanolamide, POE polyoxypropylene glycol, POE castor oil, POE Lanolin, sorbitan monostearate, POE sorbitan monopalmitate, sorbitan monooleate, sorbitan monoisostearate, sorbitan monolaurate, sorbitan monopalmitate,
Sorbitan monostearate, sorbitan sesquioleate, sorbitan trioleate, diglycerol sorbitan penta-2-ethylhexylate, diglycerol sorbitan tetra-2-ethylhexylate, glycerin mono-cottonseed oil fatty acid, glycerin monoerucate, glycerin sesquioleate, α, α'-oleic acid glyceryl pyroglutamate, glycerin monostearate malic acid, propylene glycol monostearate, hydrogenated castor oil derivatives, glycerin alkyl ether, POE / methyl polysiloxane copolymer, POE sorbitan monooleate, POE-sorbitan mono Stearate, PO
E-sorbitan monooleate, POE-sorbitan tetraoleate, POE-sorbit monolaurate,
POE-Sorbit monooleate, POE oleyl ether, POE-Sorbit pentaoleate, POE
-Sorbit monostearate, POE-glycerin monostearate, POE-glycerin monoisostearate, POE-glycerin triisostearate, PO
E monooleate, POE distearate, POE monodioleate, ethylene glycol distearate, P
OE lauryl ether, POE stearyl ether, P
POE alkyl ethers such as OE behenyl ether, POE2-octyldodecyl ether, POE cholestanol ether, POE octyl phenyl ether, P
OE nonyl phenyl ether, POE dinonyl phenyl ether, Pluronic, POE polyoxypropylene cetyl ether, POE polyoxypropylene 2-decyltetradecyl ether, POE polyoxypropylene monobutyl ether, POE polyoxypropylene hydrogenated lanolin, POE・ Polyoxypropylene glycerin ether, Tetronic, POE hydrogenated castor oil, P
OE hydrogenated castor oil monoisostearate, POE hydrogenated castor oil triisostearate, POE hydrogenated castor oil monopyroglutamic acid monoisostearate diester, P
OE hardened castor oil maleic acid, POE sorbite beeswax, coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, fatty acid isopropanolamide, P
Examples include nonionic surfactants such as OE propylene glycol fatty acid ester, POE alkylamine, POE fatty acid amide, POE nonylphenylformaldehyde condensate, alkylethoxydimethylamine oxide, and trioleyl phosphoric acid.

Oils include olive oil, jojoba oil, castor oil, cocoa butter, camellia oil, coconut oil, wood wax, grape seed oil, avocado oil, mink oil, egg yolk oil, hardened oil, evening primrose oil, turtle oil, macadamia nut oil, Corn oil, rapeseed oil, sesame oil, persic oil, wheat germ oil, sasanqua oil, linseed oil, safflower oil, cottonseed oil, eno oil,
Soybean oil, peanut oil, teaseed oil, kaya oil, rice bran oil, cinnamon oil, Japanese kiri oil, germ oil, triglycerin, glycerin trioctanoate, glycerin triisopalmitate, horse oil, hydrogenated coconut oil, palm oil, tallow , Sheep fat, hardened beef tallow, palm kernel oil, lard, beef bone fat, oil and fats such as mokuro tachibana oil, beef foot oil, hardened castor oil, spermaceti, beeswax, lanolin, carnauba wax, candelilla wax, cotton wax , Bayberry wax, ibota wax, montan wax, bran wax, kapok wax, lanolin acetate, liquid lanolin, sugar cane wax, lanolin fatty acid isopropyl, hexyl laurate, reduced lanolin, jojoba wax, hard lanolin, shellac wax, polyoxyethylene (POE) lanolin alcohol ether, POE Lanolin alcohol acetate, POE cholester Over ether, lanolin fatty acid polyethylene glycol, waxes such as POE hydrogenated lanolin alcohol ether, liquid paraffin, ceresin,
Squalane, microcrystalline wax, paraffin wax, petrolatum, ozokerite, squalene, pristane, hydrocarbons such as paraffin, stearic acid,
Oleic acid, lauric acid, myristic acid, isostearic acid, palmitic acid, behen (behenine) acid, 12-hydroxystearic acid, undecylenic acid, tolic acid, linoleic acid, linoleic acid, eicosapentaenoic acid (EP
A), fatty acids such as docosahexaenoic acid (DHA), cetanol, stearyl alcohol, lanolyl alcohol, octyldodecanol, hexyldecanol, lauryl alcohol, cetyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetstearyl alcohol, monostearyl glycerin ether (Bacyl alcohol), 2-decyltetradecinol, cholesterol, phytosterol, alcohols such as isostearyl alcohol, isopropyl myristate, butyl stearate, isopropyl palmitate, octyldodecyl myristate, cholesterol oleate, cetyl octanoate, myristic acid Octyldodecyl, hexyl laurate, myristyl myristate,
Decyl oleate, hexyl decyl dimethyl octoate, cetyl lactate, myristyl lactate, lanolin acetate, isocetyl stearate, isocetyl isostearate,
Cholesteryl 1,2-hydroxystearylate, di-2
-Ethylene glycol ethylhexylate, dipentaerythritol fatty acid ester, monoisostearic acid N-
Alkyl glycol, neopentyl glycol isocaprate, diisostearyl malate, glycerin di-2-heptylundecanoate, trimethylolpropane tri-2-ethylhexylate, trimethylolpropane triisostearate, pentaneerythritol tetra-2-ethylhexylate, Glycerin tri-2-ethylhexylate, trimethylolpropane triisostearate, cetyl-2-ethylhexanoate, 2-ethylhexyl palmitate, glycerin trimyristate, glyceride tri-2-heptylundecanoate, methyl ester of castor oil fatty acid, Oleyl oleate, cetostearyl alcohol, acetoglyceride, 2-heptylundecyl palmitate, diisobutyl adipate, N
-Lauroyl-L-glutamic acid-2-octyldodecyl ester, di-2-heptylundecyl adipate,
Ethyl laurate, di-2-ethylhexyl sebacate, 2-hexyldecyl myristate, palmitic acid 2
Esters such as hexyldecyl, 2-hexyldecyl adipate, diisopropyl sebacate, 2-ethylhexyl succinate, ethyl acetate, butyl acetate, amyl acetate, triethyl citrate; silicone oils such as dimethylpolysiloxane and methylphenylpolyester; Siloxane,
Higher alkoxy-modified silicones such as methyl hydrogen polysiloxane, octamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, and stearoxysilicone, alkyl-modified silicones, higher fatty acid ester-modified silicones, and higher fatty acid ether-modified silicones.

As alcohols and polyhydric alcohols,
Ethanol, lower alcohols such as isopropanol, sorbitol, xylitol, sugar alcohols such as maltose, propylene glycol, dipropylene glycol,
1,3-butylene glycol, hexylene glycol,
Glycerin, diglycerin, polyethylene glycol and the like can be mentioned.

Examples of the water-soluble polymer compound include plant polymer compounds such as gum arabic, galactan, guar gum, carrageenan, pectin, quince, locust bean gum, and microbial polymers such as xanthan gum, dextran, succinoglucan, and pullulan. Compounds, collagen, casein, animal polymer compounds such as gelatin, methylcellulose, hydroxypropyl methylcellulose,
Cellulosic polymer compounds such as carboxymethylcellulose, polyvinyl methyl ethers, vinyl polymer compounds such as carboxyvinyl polymers; polyacrylates;
Acrylic polymer compounds such as polymethacrylate and polyacrylamide are exemplified.

As preservatives and antibacterial agents, alkyl paraoxybenzoate, benzoic acid, sodium benzoate,
Sorbic acid, potassium sorbate, phenoxyethanols, salicylic acid, benzalkonium chloride and the like.

Examples of the antioxidant include tocopherol, butylhydroxyanisole, dibutylhydroxytoluene and the like.

Examples of the ultraviolet absorber include aminobenzoic acid derivatives such as p-aminobenzoic acid, ethyl p-aminobenzoate, glyceryl p-aminobenzoate, and amyl p-dimethylaminobenzoate; ethylene glycol salicylate;
Salicylic acid derivatives such as dipropylene glycol salicylate, octyl salicylate, myristyl salicylate, methyl diisopropylcinnamate, ethyl p-methoxycinnamate, isopropyl p-methoxycinnamate, 2-ethylhexyl p-methoxycinnamate, p- Cinnamic acid derivatives such as butyl methoxycinnamate, 2-hydroxy-4-
Benzophenone derivatives such as methoxybenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid, 2,2′-dihydroxy-4-methoxybenzophenone, azole compounds such as urocanic acid and ethyl urocanate, or 4-t- Butyl-4'-methoxybenzoylmethane and the like.

As the powder, talc, kaolin, zinc oxide, titanium oxide, magnesium oxide, silica, mica,
Examples include zeolite, magnesium silicate, petal-like silica, mica titanium, silk, nylon powder, polyethylene powder, polystyrene powder, polymethacrylate, and crosslinked polyacrylic acid.

Examples of the humectant include glycerin,
1,3-butylene glycol, propylene glycol,
Polyhydric alcohols such as sorbitol, polyethylene glycol, dipropylene glycol, hexylene glycol, xylitol and maltitol, NMF components such as amino acids, sodium lactate and sodium pyrrolidone carboxylate, hyaluronic acid, atelocollagen, short-chain soluble collagen, mucopolysaccharide , Mucoitin sulfate, chondroitin sulfate, etc., water-soluble high molecular substances such as common rose extract, Achillea millefolium extract, melilot extract, coenzyme A, oxidized coenzyme A, coenzyme H, urocanic acid, cholesteryl-12-hydroxystea Rate, sodium lactate, bile salts, d, l-pyrrolidone carboxylate, diglycerin (EO) PO adduct and the like.

Examples of the viscosity modifier include sodium alginate, xanthan gum, aluminum silicate, quince seed extract, tragacanth gum, starch, soluble starch, cationized cellulose, carboxyvinyl polymer, polyvinyl alcohol, karaya gum, carob gum, dextrin, pectic acid. Sodium, sodium alginate, tamarind gum, dialkyldimethylammonium cellulose sulfate, aluminum magnesium silicate and the like.

Examples of vitamins include vitamin A, vitamin B, vitamin C, vitamin D, vitamin E, vitamin F, vitamin K, vitamin P, vitamin K, vitamin U, carnitine, ferulic acid, γ-oryzanol, α -Lipoic acid, orotic acid and their components or derivatives retinol acetate, riboflavin acetate, pyridoxine dioctanoate, L-ascorbic acid dipalmitate, L-ascorbic acid-2-sodium sulfate, phosphorus L-ascorbic acid Acid ester, DL-tocopherol-L-ascorbic acid dipotassium phosphate dipotassium, pantothenyl ethyl ether, D-pantothenyl alcohol, acetyl pantothenyl ethyl ether, ergocalciferol, cholecalciferol,
Nicotinic acids such as nicotinic acid, nicotinamide and benzyl nicotinate; α-tocopherol, tocopherol acetate, nicotinic acid-DL-α-tocopherol, DL-α-tocopherol succinate, biotin and the like.

Examples of the amino acid include glycine, alanine, valine, leucine, isoleucine, serine, threonine, phenylalanine, tyrosine, tryptophan, cystine, cysteine, methionine, proline, hydroxyproline, aspartic acid, glutamic acid, arginine, histidine, and lysine. And its derivatives.

Examples of the plant extract include oak extract, spinach extract, sicon extract, peonies extract, assembly extract, birch oil extract, and the like.
Sage extract, loquat extract, carrot extract, aloe extract, mallow extract, iris extract, grape extract, yokuinin extract, loofah extract, lily extract, saffron extract, senkyu extract, ginger extract Extract components, hypericum extract components, ononis extract components, rosemary extract components, garlic extract components, capsicum extract components, chimneys, corns, and the like. Examples of crude drugs include, for example, magnolia, sandalwood, valerian, scallop, scallop, spruce, spruce, squash, squirrel, squirrel, aloe, carrot, keihi, peonies, peppermint, mint, squirrel, matsubusa, swordfish, falcon , Oak, fennel, cockscomb, ganpi, chamomile, radish, willow, camphor, elderberry, sokuzu, nakinata koju, Japanese hornbeam, sekisho,
Artemisia, Hypericum perforatum, Yuzu, Daidai, peach, honey locust, loquat, honeysuckle, yorigusa, bodaige, horse chestnut, yarrow, hop, rosemary, cabano,
Pine, yarenzura, lantana, licorice, foxglove, marronnier and the like. These may be powders or extracted extracts.

Examples of the active ingredient include glycyrrhizic acid derivatives, glycyrrhetinic acid derivatives, salicylic acid derivatives, anti-inflammatory agents such as hinokitiol, zinc oxide, allantoin, royal jelly, photosensitizers, cholesterol derivatives, and the like.
Activators such as calf blood extract, ellagic acid, kojic acid, placenta extract, glutathione, saxifrage extract, whitening agents such as arbutin, nonylate warenylamide, nicotinic acid benzyl ester, nicotinic acid-β-butoxyethyl ester, Capsaicin, zingerone, cantaris tincture, ittamol, caffeine, tannic acid, α-borneol, tocopherol nicotinate, inositol hexanicotinate, cyclandate, cinnarizine, trazoline, acetylcholine, verapamil, cepharanthin,
blood circulation promoters such as γ-oryzanol; antiseborrheic agents such as pyrocton olamine, sulfur and thiantole; and hair growth ingredients such as pentadecanoic acid monoglyceride and minoxidil.

The preparation method of the emulsified composition of the present invention is not particularly limited, and it can be prepared according to a conventional method of a usual emulsified composition. The above water-swellable clay mineral / fatty acid monoglyceride modified product is obtained by mixing and modifying with a mineral, and the modified product and the above-mentioned optional component are appropriately mixed as necessary and the oil phase is stirred and mixed at an appropriate temperature to obtain the above-mentioned optional component. An emulsion composition can be prepared by gradually stirring and mixing the above oil phase at an appropriate temperature in an aqueous phase appropriately dissolved according to the above, and the thus obtained emulsion composition has an appearance It is not only excellent in the feeling of use but also excellent in emulsion stability.

[0035]

The present invention will be described more specifically with reference to the following examples and comparative examples, but the present invention is not limited to the following examples. In addition, in the following tables, the compounding amount is represented by mass%.

First, a method for modifying a fatty acid monoglyceride with a water-swellable clay mineral in the following examples will be described.

[Modification method] When fatty acid monoglyceride was heated at a temperature higher than the melting point (melting point + 5 ° C or higher), smectite (bentonite: Kunimine Kogyo Co., Kunipia F) was added as a water-swellable clay mineral. Using a stirring tank equipped with a disper, denaturation was performed by stirring and mixing at a peripheral speed of 3 m / s for 30 minutes.

[Confirmation of Crystal Inhibiting Effect] The inhibitory effect of the water-swellable clay mineral on the β-type crystallization of fatty acid monoglyceride was confirmed by X-ray diffraction. The measurement was performed using a sample horizontal X-ray diffractometer RINT2100 manufactured by Rigaku Corporation, and the X-ray source was CuKα (4
0 kV, 20 mA) at a measurement temperature of 25 ° C. and a scan speed of 4 ° C./min. Using pentadecanoic acid monoglyceride as a representative of fatty acid monoglyceride,
The following three points prepared by the above modification method were measured.
As a result, as shown in FIG. 1, since the peak pattern of the fatty acid monoglyceride disappeared due to the modification, the fatty acid monoglyceride alone easily became a β-type crystal, and the crystal peak remained, but was modified with the water-swellable clay mineral. It can be seen that crystallization became difficult due to this. In the graph of FIG. 1, the peak patterns are pentadecanoic acid monoglyceride only, pentadecanoic acid monoglyceride / smectite (bentonite: manufactured by Kunimine Industries,
Kunipia F) (mixed modified product) (mass ratio) = 1/1, pentadecanoic acid monoglyceride / smectite (bentonite: manufactured by Kunimine Industries, Kunipia F) (mass ratio) = 1 /
2 is a peak pattern of the mixed modified product of No. 2.

[Examples 1 to 7] The fatty acid monoglycerides shown in Table 1 were modified with smectite (bentonite: Knipine F, manufactured by Kunimine Kogyo Co., Ltd.) by the above modification method, and the oil phase was mixed at 75 ° C. Further, the aqueous phase shown in Table 1 was changed to 6
The mixture was mixed and dissolved at 0 ° C. with a stirrer. Thereafter, the aqueous phase is put into a mixing tank equipped with a homomixer, and the oil phase is gradually stirred and mixed at 75 ° C. Then, the fragrances shown in Tables 6 to 8 are added on the way, and further mixed to obtain a beauty liquid (emulsion composition). Product).

Comparative Example 1 Fatty acid monoglycerides shown in Table 1 were added to an oil phase and mixed at 75.degree. The aqueous phases shown in Table 1 were mixed and dissolved at 60 ° C. with a stirrer. Thereafter, the aqueous phase is put into a mixing tank equipped with a homomixer, and the oil phase is gradually emulsified and mixed at 75 ° C. Then, the fragrances shown in Tables 6 to 8 are added on the way, and further mixed to obtain a beauty liquid (emulsion composition). Product).

Comparative Example 2 Fatty acid monoglycerides shown in Table 1 were added to the oil phase and mixed at 75.degree. Further, smectite (bentonite: Kunipia F, manufactured by Kunimine Industries) shown in Table 1 was added to the aqueous phase, and mixed and dissolved at 60 ° C. with a stirrer. Thereafter, the aqueous phase was charged into a mixing tank equipped with a homomixer, and the oil phase was gradually emulsified and mixed at 75 ° C.
The fragrance shown in No. 8 was added and further mixed to obtain a serum (emulsion composition).

With respect to each of the essences (emulsion compositions) of Examples 1 to 7 and Comparative Examples 1 and 2, crystal precipitation of fatty acid monoglyceride and emulsion stability were evaluated according to the following evaluation methods. The results are also shown in Table 1.

<Evaluation Method of Crystal Precipitation of Emulsion Composition> Each cosmetic (emulsion composition) was placed in a 50 ml vial bottle and placed at 5 ° C.
After storage for one week under low temperature conditions, it was observed with a position scanning microscope whether fatty acid monoglyceride crystals were precipitated in the composition, and crystal precipitation was evaluated based on the following evaluation criteria.
This was used as an index of the β-type crystal inhibitory effect of the fatty acid monoglyceride by the above modification.

Evaluation criteria ：: No crystals were observed at all. Δ: Slight crystals observed X: Many crystals of 0.5 mm or more were observed.

<Method of Evaluating Stability of Emulsion Composition> Each cosmetic (emulsion composition) was placed in a 50 ml vial bottle,
After storage for one month under the high temperature condition, whether separation had occurred was visually observed and evaluated based on the following evaluation criteria.

Evaluation criteria ：: No separation was observed at all. Δ: Slight separation observed X: Separated layer of 1 cm or more was observed.

[0047]

[Table 1]

[Examples 8 to 12] The fatty acid monoglycerides shown in Table 2 were modified with smectite (bentonite: Kunimine F, Kunipia F) by the above modification method.
It was added to the oil phase shown in Table 2 and mixed at 80 ° C. Further, after the aqueous phase shown in Table 2 was heated and melted at 70 ° C., the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 80 ° C .; A fragrance having the composition shown in Nos. 6 to 8 was added and cooled to room temperature to obtain a skin cream (emulsion composition).

Comparative Example 3 Fatty acid monoglycerides shown in Table 2 were added to the oil phase and mixed at 80.degree. Further, after the aqueous phase shown in Table 2 was heated and melted at 70 ° C., the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 80 ° C .; A fragrance having the composition shown in Nos. 6 to 8 was added and cooled to room temperature to obtain a skin cream (emulsion composition).

Comparative Example 4 Fatty acid monoglycerides shown in Table 2 were added to the oil phase and mixed at 80.degree. Further, smectite (bentonite: Knipine F, manufactured by Kunimine Industries) shown in Table 2 was added to the aqueous phase, and mixed and dissolved at 70 ° C. with a stirrer. Thereafter, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually emulsified and mixed at 70 ° C.
Was added and further mixed to obtain a skin cream (emulsion composition).

The skin creams (emulsion compositions) of Examples 8 to 12 and Comparative Examples 3 and 4 were evaluated for crystal precipitation of fatty acid monoglyceride and emulsion stability according to the evaluation methods described above. The results are also shown in Table 2.

[0052]

[Table 2]

[Examples 13 to 17] The fatty acid monoglycerides shown in Table 3 and smectite (bentonite: Kunimine F, Kunipia F) shown in Table 3 were modified by the above-mentioned modification method, and added to the oil phase shown in Table 3 at 80 ° C. And mixed. Further, after the aqueous phase shown in Table 3 was heated and dissolved at 70 ° C, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 80 ° C. A fragrance having the composition shown in Nos. 6 to 8 was added, and the mixture was cooled to room temperature to obtain a hair restorer (emulsion composition).

Comparative Example 5 Fatty acid monoglycerides shown in Table 3 were added to the oil phase and mixed at 80.degree. Further, after the aqueous phase shown in Table 3 was heated and dissolved at 70 ° C, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 80 ° C. A fragrance having the composition shown in Nos. 6 to 8 was added, and the mixture was cooled to room temperature to obtain a hair restorer (emulsion composition).

Comparative Example 6 Fatty acid monoglycerides shown in Table 3 were added to an oil phase and mixed at 80 ° C. In addition, smectite (bentonite: Kunipia F, manufactured by Kunimine Industries Co., Ltd.) shown in Table 3 was added to the aqueous phase, and mixed and dissolved at 70 ° C. with a stirrer. Thereafter, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually emulsified and mixed at 80 ° C.
The fragrance shown in No. 8 was added and further mixed to obtain a hair restorer (emulsion composition).

With respect to the hair restorers (emulsion compositions) of Examples 13 to 17 and Comparative Examples 5 and 6, crystal precipitation of fatty acid monoglyceride and emulsion stability were evaluated according to the evaluation methods described above. The results are also shown in Table 3.

[0057]

[Table 3]

[Examples 18 to 22] The fatty acid monoglycerides shown in Table 4 were modified with smectite (bentonite: Kunimine Kogyo Co., Kunipia F) by the above modification method.
It was added to the oil phase shown in Table 4 and mixed at 75 ° C. Further, after the aqueous phase shown in Table 4 was heated and dissolved at 70 ° C., the aqueous phase was charged into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 75 ° C., and then cooled while cooling. A fragrance having the composition shown in Nos. 6 to 8 was added, and the mixture was cooled to room temperature to obtain a bath liquid (emulsion composition).

Comparative Example 7 Fatty acid monoglycerides shown in Table 4 were added to an oil phase and mixed at 75 ° C. Further, after the aqueous phase shown in Table 4 was heated and dissolved at 70 ° C., the aqueous phase was charged into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 75 ° C., and then cooled while cooling. A fragrance having the composition shown in Nos. 6 to 8 was added, and the mixture was cooled to room temperature to obtain a bath liquid (emulsion composition).

Comparative Example 8 Fatty acid monoglycerides shown in Table 4 were added to an oil phase and mixed at 75 ° C. In addition, smectite (bentonite: Knipine F, manufactured by Kunimine Industries) shown in Table 4 was added to the aqueous phase, and mixed and dissolved at 70 ° C. with a stirrer. Thereafter, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually emulsified and mixed at 75 ° C.
Add the perfume shown in (1) and further mix to make a bath solution (emulsion composition)
I got

The bath solutions (emulsified compositions) of Examples 18 to 22 and Comparative Examples 7 and 8 were evaluated for crystal precipitation of fatty acid monoglyceride and emulsion stability according to the evaluation methods described above. The results are shown in Table 4.

[0062]

[Table 4]

Examples 23 to 26 The fatty acid monoglycerides shown in Table 5 were modified with smectite (bentonite: Kunimine F, Kunipia F) by the above modification method.
It was added to the oil phase shown in Table 5 and mixed at 75 ° C. After heating and dissolving the aqueous phase shown in Table 5 at 70 ° C, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 75 ° C. Add a fragrance having the composition shown in Nos. 6 to 8 and cool to room temperature.
A V care agent (emulsion composition) was obtained.

Comparative Example 9 Fatty acid monoglycerides shown in Table 5 were added to an oil phase and mixed at 75 ° C. After heating and dissolving the aqueous phase shown in Table 5 at 70 ° C, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 75 ° C. A fragrance having a composition shown in Nos. 6 to 8 was added, and the mixture was cooled to room temperature to obtain a water-in-oil type UV care agent (emulsion composition).

Comparative Example 10 Fatty acid monoglycerides shown in Table 5 were added to an oil phase and mixed at 75 ° C. In addition, smectites shown in Table 5 (bentonite: manufactured by Kunimine Industry Co., Ltd.)
Kunipia F) was added to the aqueous phase, and mixed and dissolved at 70 ° C. with a stirrer. Thereafter, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually emulsified and mixed at 75 ° C.
To 8 were further added and mixed to obtain a water-in-oil type UV care agent (emulsion composition).

[Examples 27 to 29] The fatty acid monoglycerides shown in Table 5 were modified with smectite (bentonite: Kunimine F, Kunipia F) by the above modification method.
It was added to the oil phase shown in Table 5 and mixed at 75 ° C. After heating and dissolving the aqueous phase shown in Table 5 at 70 ° C, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 75 ° C. Add a fragrance having the composition shown in Nos. 6 to 8 and cool to room temperature.
A V care agent (emulsion composition) was obtained.

Comparative Example 11 Fatty acid monoglycerides shown in Table 5 were added to an oil phase and mixed at 75 ° C. After heating and dissolving the aqueous phase shown in Table 5 at 70 ° C, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually stirred and mixed at 75 ° C. A fragrance having the composition shown in Nos. 6 to 8 was added, and the mixture was cooled to room temperature to obtain an oil-in-water type UV care agent (emulsion composition).

Comparative Example 12 Fatty acid monoglycerides shown in Table 5 were added to an oil phase and mixed at 75 ° C. In addition, smectites shown in Table 5 (bentonite: manufactured by Kunimine Industry Co., Ltd.)
Kunipia F) was added to the aqueous phase, and mixed and dissolved at 70 ° C. with a stirrer. Thereafter, the aqueous phase was put into a mixing tank equipped with a homomixer, and the oil phase was gradually emulsified and mixed at 75 ° C.
To 8 were further added and mixed to obtain an oil-in-water type UV care agent (emulsion composition).

Examples 23 to 29 and Comparative Examples 9 to 12
With respect to the UV care agent (emulsion composition), crystal precipitation of fatty acid monoglyceride and emulsion stability were evaluated in accordance with the above evaluation method. The results are also shown in Table 5.

[0070]

[Table 5]

[0071]

[Table 6]

[0072]

[Table 7]

[0073]

[Table 8]

[0074]

According to the present invention, a β-type crystallization of fatty acid monoglyceride can be sufficiently suppressed, and an emulsified composition having not only excellent appearance and feeling of use but also excellent emulsification stability can be obtained. Therefore, the present invention is particularly useful for emulsified compositions, particularly external compositions, used as skin cosmetics, hair cosmetics, various pharmaceuticals, quasi-drugs, etc., utilizing the emulsifying properties of fatty acid monoglycerides.

[Brief description of the drawings]

FIG. 1 is a graph of X-ray diffraction confirming the formation of a water-swellable clay mineral / modified fatty acid monoglyceride and the effect of suppressing β-type crystallization in Examples of the present invention.

Continuation of the front page (51) Int.Cl. ⁷ Identification code FI Theme coat II (reference) A61K 7/48 A61K 7/48 7/50 7/50 C11C 3/00 C11C 3/00 (72) Inventor Satsuki Miyauchi Tokyo 1-3-7, Honjo, Sumida-ku, Tokyo F-term in Lion Corporation (reference) 4C083 AA112 AA122 AB172 AB212 AB242 AB432 AB442 AC022 AC072 AC102 AC122 AC212 AC302 AC312 AC352 AC421 AC422 AC432 AC482 AC532 AC542 AC842 AD072 AD092 AD152 AD172 AD352 AD472 AD472 AD532 AD662 CC01 CC05 CC19 CC25 CC31 DD31 EE03 EE06 4H059 AA12 BA34 BB02 BB03 DA24 EA01 EA11

Claims (2)

[Claims] Claims: 1. A water-swellable clay mineral and a fatty acid monoglyceride are stirred and mixed to modify the fatty acid monoglyceride with the water-swellable clay mineral, thereby suppressing β-type crystallization of the fatty acid monoglyceride. For suppressing β-type crystallization of fatty acid monoglycerides. 2. An emulsified composition comprising a water-swellable clay mineral / fatty acid monoglyceride modified product obtained by mixing and modifying a fatty acid monoglyceride with a water-swellable clay mineral.