JP5088766B2 - Oil fine dispersion composition - Google Patents

Description

  The present invention relates to a finely dispersed composition of oil in which an oil phase containing a solid oil is stably dispersed as fine particles in an aqueous phase, a method for producing the same, and a skin external preparation containing such a finely dispersed composition of oil. It is about.

  The oily ingredient is coated with a thin film of high-molecular substances such as gelatin and collagen, as well as emulsion preparations in which liquid oily ingredients are dispersed in an aqueous solution using various surfactants. Oil-based capsules, microcapsules, etc. are used in various fields. However, in skin preparations such as skin lotions and creams, for example, in conventional emulsion preparations, when applied to the skin, moisture and liquid oil are in contact with the skin at the same time. There was a problem that the penetration into the skin was hindered and the effect could not be fully exhibited. In addition, oil-based capsules and microcapsules, when applied to the skin, leave the polymer material used as the capsule coating material on the skin, causing a sense of incongruity and foreign matter. Not suitable for formulation.

  Therefore, a capsule-containing composition is proposed in which an oil component containing an amphiphilic substance that is solid at room temperature is dispersed in an aqueous solvent as an oil capsule having an average particle size of 100 μm or more (Patent Document 1). The composition for external use containing such oil-based capsules has the advantage that spherical particles are visible and visually novel, and has no foreign matter feeling when applied to the skin, but the particle size of the capsule particles is 100 μm. The oil capsules are large and have a small surface area, so that the familiarity is not sufficient, and there is a problem that a finger is bad at the time of use. Moreover, when the stirring speed in the stirring step was increased to reduce the particle size, floating separation of the oil component occurred, and a stable and uniform oil fine dispersion could not be formed.

On the other hand, a finely dispersed wax composition is disclosed in which a solid or semi-solid wax at room temperature is stabilized by blending with a nonionic surfactant and an amphoteric surfactant (Patent Document 2). And 3) were not suitable for application to basic cosmetics, etc., because it was necessary to formulate a specific surfactant combination for stabilization.
JP 2003-73230 A Japanese Patent Laid-Open No. 10-324617 JP-A-11-263915

  In view of the circumstances as described above, the present invention stably disperses an oil phase containing a solid oil as fine particles in an aqueous solution without the need for blending a surfactant into a stable fine dispersion composition of oil. It is intended to provide. Another object of the present invention is to provide a skin external preparation excellent in stability, usability, and feeling of use, which contains such a finely dispersed composition of oil.

  The present invention adds an oil phase containing a solid oil component and a liquid oil component to a water phase at a temperature higher than the melting point of the solid oil component and higher than the melting point of the solid oil component containing the water-soluble thickener, and a mixture thereof. Can be stably dispersed as fine particles in an aqueous phase without adding a surfactant by shear mixing to a temperature below the melting point of the solid oil component. When a finely dispersed composition of oil having an average primary particle size of 0.1 to 30 μm, produced by such a method, is applied to the skin, it has good finger fit and smoothness, and is moist and fluffy. It is based on the discovery of superiority. In an aqueous phase containing a water-soluble thickener, the solid oil that has been crystallized (solidified) forms particles so as to include other oil components, and the particles are immediately finely pulverized into fine particles by shearing force. Therefore, a stable and uniform finely dispersed composition of oil can be produced without producing oil agglomerates and suspended matters.

  The oil finely dispersed composition of the present invention comprises an oil phase containing a solid oil component and a liquid oil component, and an aqueous phase containing a water-soluble thickener, and the oil phase has an average maximum size of primary particles of 0. .1-30 μm fine particles are dispersed in the aqueous phase, and the solid oil is crystallized in the fine particles. Preferably, the average maximum dimension of the primary particles is 1 to 15 μm. By dispersing the oil phase as fine particles having such dimensions, stability and usability can be further improved.

  In the present specification, “solid oil” refers to a solid or semi-solid oil at room temperature (25 ° C.), and “liquid oil” refers to an oil that is liquid at room temperature (25 ° C.).

  From the viewpoint of stability, usability and feeling of use, the oil phase preferably contains 10 to 50% by mass of solid oil and 50 to 90% by mass of liquid oil based on the total mass of the oil phase. Preferably, it contains 10 to 20% by mass of solid oil and 80 to 90% by mass of liquid oil based on the total mass of the oil phase. Moreover, it is preferable that the compounding quantity of an oil phase is 1-20 mass% with respect to the total mass of a composition.

  The solid oil preferably contains one or more selected from the group consisting of candelilla wax and higher alcohols having 16 or more carbon atoms. By blending such a solid oil component, usability and usability can be further enhanced.

  Furthermore, the oil phase preferably contains a lipophilic gelling agent. When a lipophilic gelling agent is blended in the oil phase, the skin feel when applied to the skin is soft and excellent in touch.

  The water-soluble thickener preferably contains carboxyvinyl polymer or agar. When such a water-soluble thickener is blended in the aqueous phase, it is particularly excellent in stability, usability and usability.

  The external preparation for skin of the present invention is characterized by containing the above finely dispersed composition of oil. By blending the above finely dispersed composition of oil, it is possible to provide an external preparation for skin that has good finger contact and skin familiarity, and is also moist and fluffy.

  The method for producing a finely dispersed composition of oil according to the present invention includes a solid oil component and an oil phase containing a liquid oil component at a temperature higher than the melting point of the solid oil component and the melting point of the solid oil component containing the water-soluble thickener. Adding to the aqueous phase at a high temperature; and shearing the mixture of the oil phase and the aqueous phase to a temperature not higher than the melting point of the solid oil to disperse the oil phase as fine particles in the aqueous phase. It is characterized by including; By carrying out shear mixing to a temperature below the melting point of the solid oil component, a stable finely dispersed composition of oil can be prepared without forming floating or agglomerated oily components.

  The average maximum size of the primary particles of the fine particles in the oil fine dispersion composition obtained by the production method of the present invention is preferably 0.1 to 30 μm, more preferably 1 to 15 μm. Such a finely dispersed composition of oil is particularly excellent in stability, usability, and feeling of use, is well-familiar when applied to the skin, and is excellent in fluffy and moist feeling.

  In this specification, “shear mixing” means mixing while applying a shearing force. For example, the shear mixing is preferably performed by a high-speed shearing dispersion device such as a homomixer, a homodisper, a flow jet mixer, an ultramixer, or a colloid mill, or a high-pressure shearing dispersion device such as a homogenizer.

  It is preferable to further include a step of stirring after the dispersing step. A more uniform and stable oil fine dispersion composition can be prepared. The stirring step can be performed by, for example, a propeller mixer, a paddle mixer, an anchor mixer, a gate mixer, or a planetary mixer.

  In the oil finely dispersed composition of the present invention, the oil phase containing a solid oil and a liquid oil is dispersed as fine particles having an average maximum size of 0.1 to 30 μm in a water phase containing a water-soluble thickener. Therefore, it is very stable over a long period of time, and is excellent in usability and usability. When the finely dispersed composition of the present invention is applied to the skin as an external preparation, since the oil phase in which the fine particles are formed does not inhibit the penetration of moisture into the skin, it can initially impart freshness to the skin, and gradually the fine oil particles. Since the oil phase covers the entire skin by crushing, the skin can finally be moistened. Furthermore, by making the oil phase fine, finger contact and skin familiarity are improved, and the oil phase can be uniformly applied on the skin. Furthermore, there is no stickiness because it contains a solid oil.

  The method for producing a finely dispersed composition of oil according to the present invention includes a solid oil component and an oil phase containing a liquid oil component at a temperature higher than the melting point of the solid oil component and the melting point of the solid oil component containing the water-soluble thickener. Addition to the aqueous phase at a high temperature, and the mixture is shear-mixed to a temperature below the melting point of the solid oil, so that fine particles of oil containing solid oil that has been crystallized (solidified) without forming suspended matter or aggregates Can be stably dispersed in the aqueous phase.

  The oil finely dispersed composition of the present invention is composed of an oil phase containing a solid oil and a liquid oil and an aqueous phase containing a water-soluble thickener, and the oil phase has an average primary particle size of 0 in the primary phase. .Dispersed in the aqueous phase as fine particles of 1 to 30 μm. More preferably, the average maximum dimension of the primary particles is 1 to 15 μm. When the average maximum dimension of the primary particles is less than 0.1 μm, the stability is deteriorated, and when it exceeds 30 μm, the finger and the familiarity with the skin are deteriorated. In the finely dispersed oil composition of the present invention, the fine oil particles may be partially aggregated (unified).

  In this specification, the average maximum size of primary particles means the average value of the maximum size of individual oil particles, and 50 particles randomly selected using an optical micrograph of the finely dispersed composition. Obtained by the average value of the maximum dimensions.

  The shape of the oil fine particles is not particularly limited and may be irregular, and may be any shape such as a wedge shape, a barrel shape, an irregular spherical shape, a spherical shape, etc. However, the irregularly shaped particles have a larger surface area of the particles, and the skin conforms better when applied to the skin as an external preparation. Depending on the conditions of shear mixing during production, particles having different shapes are formed.

  In the oil finely dispersed composition of the present invention, the solid oil is crystallized (solidified) to form fine particles so as to surround the liquid oil. The solid oil component is mainly present at the interface between the oil phase and the water phase, but may be partially present inside the fine particles together with other oil components. Moreover, a liquid oil part may exist in the interface of an oil phase and a water phase partially. The presence of crystallized solid oil at the interface between the oil phase and the aqueous phase so as to surround the liquid oil prevents the oil phase from inhibiting the penetration of moisture into the skin when applied to the skin as an external preparation. In addition, the oil phase can be stably dispersed in the aqueous phase without adding a surfactant.

  The solid oil used in the present invention is not particularly limited as long as it is a solid or semi-solid oil component at room temperature (25 ° C.). For example, solid paraffin, microcrystalline wax, ceresin, bees wax, barico wax, polyethylene wax, Silicon wax, behenyl alcohol, stearyl alcohol, cetyl alcohol, batyl alcohol, carnauba wax, beeswax, candelilla wax, jojoballow, lanolin, shellac wax, whale wax, moscow, myristic acid, palmitic acid, stearic acid, behenic acid, 12-hydroxystearin Acid, cacao butter, hydrogenated castor oil, hydrogenated palm oil, palm oil, hydrogenated palm oil, polyethylene powder, petroleum jelly, various water-added animal and vegetable oils, fatty acid monocarboxylic acid lanolin alcohol ester And the like. In particular, a solid oil component having a melting point of 45 to 75 ° C is preferable, and a solid oil component having a melting point of 50 to 70 ° C is more preferable. If a solid oil component having a melting point lower than 45 ° C. is used, the stability of the finely dispersed composition may be deteriorated. If a solid oil component having a melting point higher than 75 ° C. is used, the aqueous phase for preparing the composition for external use Mixing and melting at a temperature higher than the standard temperature (75 ° C.) for mixing and melting the oil phase is required, and the processing becomes complicated. Examples of such solid oil include, but are not limited to, for example, higher alcohols having 16 or more carbon atoms such as cetyl alcohol (16 carbon atoms), stearyl alcohol (18 carbon atoms), behenyl alcohol (22 carbon atoms), Or candelilla wax is mentioned. Furthermore, the higher alcohol is more preferably a linear saturated higher alcohol having no unsaturated bond and having 18 or more carbon atoms. In particular, behenyl alcohol or candelilla wax is preferred in that melting of the particles at a high temperature is suppressed as much as possible and versatility is recognized.

  The solid oil components as described above can be used alone or in combination of two or more in the present invention.

  The blending amount of the solid oil is preferably 10 to 50% by mass and more preferably 10 to 20% by mass with respect to the total mass of the oil phase. When the blending amount of the solid oil in the oil phase is less than 10% by mass, the stability of the dispersion composition tends to deteriorate, and when the blending amount of the solid oil exceeds 50% by mass, it is applied to the skin. There is a tendency to become less crushed and to become less familiar with the skin.

  In the oil finely dispersed composition of the present invention, the liquid oil component forms fine particles together with the crystallized solid oil component, making it easy to crush the oil particles on the skin and to improve the familiarity with the skin. The solid oil alone makes the oil particles hard and does not stretch on the skin, resulting in poor usability and usability.

  The liquid oil used in the present invention is not particularly limited as long as it is an oily component that is liquid at room temperature (25 ° C.). For example, olive oil, avocado oil, camellia oil, macadamia nut oil, evening primrose oil, jojoba oil, rapeseed oil, egg yolk Oil, sesame oil, castor oil, safflower oil, cottonseed oil, soybean oil, teaseed oil, rice bran oil, wheat germ oil, germ oil, peanut oil, sunflower oil, almond oil, corn oil, turtle oil, mink oil, persic oil , Sasanqua oil, linseed oil, eno oil, kaya oil, Japanese drill oil, medfoam oil, squalene, squalane, vegetable squalane, jojoba alcohol, liquid paraffin, polybutene, hydrogenated polyisobutene, isocetyl isostearate, di-2-ethyl Ethylene glycol hexanoate, cetyl 2-ethylhexanoate, tri-2-ethylhexane Trimethylolpropane, tetra-2-ethylhexanoic acid pentaerythritol, cetyl octanoate, pentaerythryl tetraoctanoate, tri-2-heptylundecanoic acid glyceride, diisobutyl adipate, 2-hexyldecyl sebacate, glycerin trioctanoate, Glycerol triisopalmitate, diisostearyl malate, isopropyl myristate, 2-octyldodecyl oleate, hexyldecyl dimethyloctanoate, 2-hexyldecyl myristate, myristyl myristate, octyldodecyl myristate, isopropyl palmitate, 2 -Ethylhexyl palmitate, 2-hexyldecyl palmitate, 2-heptylundecyl palmitate, butyl stearate, isocetyl stearate, oleic acid Sil, dodecyl oleate, oleyl oleate, myristyl lactate, cetyl lactate, cholesteryl 12-hydroxystearylate, castor oil fatty acid methyl ester, 2-ethylhexyl succinate, 2-hexyldecyl adipate, di-2-heptylunadipate Decyl, diisopropyl sebacate, di-2-ethylhexyl sebacate, neopentyl glycol dicaprate, neopentyl glycol dioctanoate, glycerin tri-2-ethylhexanoate, glyceryl trimyristate, glyceride tri-2-heptylundecanoate, tri Trimethylolpropane isostearate, glyceryl tri-2-ethylhexanoate, dimethicone, dimethylpolysiloxane, methylphenylpolysiloxane, octamethylcyclotetrasiloxane, Decamethylcyclopentasiloxane, glyceryl trioctanoate, glyceryl triisopalmitate, triglycerin, oleic acid, tall oil fatty acid, isostearic acid, lauryl alcohol, oleyl alcohol, isostearyl alcohol, octyldodecanol, methylpolysiloxane, methylphenylpoly Siloxane, methyl hydrogen polysiloxane, cyclic polysiloxane, isopropyl myristate, isopropyl palmitate, hexyl laurate, oleyl oleate, decyl oleate, octyldodecyl myristate, hexyldecyl dimethyloctanoate, diethyl phthalate, phthalic acid Examples include dibutyl, dioctyl succinate, fluorine-modified oil, trioctanoin, and tripropylene glycol dipivalate. In particular, dimethicone, pentaerythrityl tetraoctanoate, or jojoba alcohol is preferably blended as a liquid oil because it is familiar to the skin when applied to the skin as an external preparation.

  The liquid oil as described above can be used in the present invention alone or in combination of two or more.

  The blending amount of the liquid oil is preferably 50 to 90% by mass and more preferably 80 to 90% by mass with respect to the total mass of the oil phase. When the blending amount of the liquid oil in the oil phase is less than 50% by mass, it tends to be difficult to crush when applied to the skin, and the skin conformability tends to deteriorate, and when it exceeds 90% by mass, the stability of the dispersion composition Tend to get worse.

  It is preferable to further blend a lipophilic gelling agent in the oil phase. The lipophilic gelling agent can adjust the hardness so as to be suitable for reducing the solidification power of the solid oil and smashing and stretching the oil particles on the skin.

  The lipophilic gelling agent used in the present invention is not particularly limited as long as it can reduce the solidification power of the solid oil blended together. For example, metal soap, lipophilic bentonite, amino acid derivative, dextrin fatty acid ester Sucrose fatty acid esters, benzylidene derivatives of sorbitol, and the like. Examples of the metal soap include aluminum stearate in which a hydroxyl group remains, magnesium stearate, zinc myristate, and the like. Examples of the lipophilic bentonite include dimethylbenzyl dodecyl ammonium montmorillonite clay and dimethyl dioctadecyl ammonium montmorillonite clay. Examples of amino acid derivatives include N-lauroyl-L-glutamic acid and α, γ-di-n-butylamine. Examples of dextrin fatty acid esters include dextrin palmitate, dextrin oleate, dextrin stearate, and the like. Examples of the sucrose fatty acid ester include those in which 3 or less of 8 hydroxyl groups are esterified with a higher fatty acid, and the higher fatty acid is stearic acid or palmitic acid. Examples of the benzylidene derivative of sorbitol include monobenzylidene sorbitol, dibenzylidene sorbitol, and the like. In particular, dextrin palmitate is most preferable in terms of stability and usability. The dextrin fatty acid ester is not particularly limited, but is commercially available from Chiba Flour Milling Co., Ltd. under trade names such as “Leopearl KL” and “Leopearl KE”.

  The above lipophilic gelling agents can be used in the present invention alone or in combination of two or more.

  The blending amount of the lipophilic gelling agent varies depending on the use and desired feeling of use and is not particularly limited, but is preferably 0.01 to 5% by mass, more preferably based on the total mass of the oil phase. It is 0.03 to 2% by mass.

  Further, as necessary, UV absorbers such as sterols, octyl paramethoxycinnamate, 2-hydroxy-4-methoxybenzophenone, vitamin A and derivatives thereof, vitamin D and derivatives thereof, vitamin E and derivatives thereof, vitamins Vitamins such as K and its derivatives, animal and plant extracts, oil-soluble drugs, pigments, fragrances and the like may be incorporated into the oil phase, and the surface of water-soluble drug crystals such as vitamin C and arbutin are hydrophobic. What has been subjected to chemical treatment may be dispersed in the oil phase. Furthermore, you may mix | blend an oil-soluble chemical | medical agent in an oil phase.

  The blending amount of the oil phase in the finely dispersed oil composition of the present invention varies depending on the use and desired feeling of use and is not particularly limited, but is 1 to 20% by mass with respect to the total mass of the composition. Is preferable, and more preferably 3 to 10% by mass. When the amount of the oil phase is less than 1% by mass, it may not be sufficiently moist when applied to the skin as an external preparation, and when it exceeds 20% by mass, stickiness may occur.

  The oil finely dispersed composition of the present invention contains a water-soluble thickener in the aqueous phase. The water-soluble thickener increases the viscosity of the composition and helps to stably disperse the oil particulates in the aqueous phase. Moreover, it plays the role which adjusts the viscosity of a composition to the viscosity suitable for use.

  The water-soluble thickener used in the present invention is not particularly limited as long as it can thicken an aqueous solvent. For example, gum arabic, gum tragacanth, galactan, carob gum, guar gum, caraya gum, carrageenan, pectin , Plant polymers such as agar, quince seed (malmello), algae colloid (brown algae extract), microbial polymers such as dextran, succinoglucan, pullulan, animal polymers such as collagen, casein, albumin, gelatin, Methyl cellulose, nitrocellulose, ethyl cellulose, methyl hydroxypropyl cellulose, hydroxyethyl cellulose, cellulose sodium sulfate, hydroxypropyl cellulose, sodium carboxymethyl cellulose, crystalline cellulose, cellulose powder, etc. Cellulose polymers, alginic acid polymers such as sodium alginate, propylene glycol ester alginate, vinyl polymers such as polyvinyl alcohol, polyvinyl methyl ether, polyvinyl pyrrolidone, carboxyvinyl polymer, alkyl-modified carboxyvinyl polymer, polyoxyethylene polymer Molecule, polyoxyethylene polyoxypropylene copolymer polymer, acrylic polymer such as sodium polyacrylate, polyethyl acrylate, polyacrylamide, polyethyleneimine, cationic polymer, bentonite, aluminum magnesium silicate, laponite, hectorite, Examples thereof include inorganic water-soluble polymers such as silicic anhydride. In particular, the alkyl-modified carboxyvinyl polymer has a surface activity and also has an action of preventing aggregation and coalescence of large particles, so that it is particularly suitable for use in the oil fine dispersion composition of the present invention. It is a thickener. The alkyl-modified carboxyvinyl polymer is an alkyl methacrylate copolymer and is commercially available, for example, under the trade names CARBOPOL 1342, PEMULEN TR-1, and PEMULEN TR-2 (BF Goodrich). In addition, when agar is used as the water-soluble thickener, a new feeling of use that cannot be obtained by using other water-soluble thickeners can be brought about. Furthermore, you may use the thickener which consists of a microgel as described in Unexamined-Japanese-Patent No. 2004-43785 in this invention.

  The water-soluble thickeners as described above can be used alone or in combination of two or more in the present invention.

  The blending amount of the water-soluble thickener in the aqueous phase varies depending on the type of water-soluble thickener, application, desired usability, etc., and is not particularly limited. It is 0.01-1.0 mass%, More preferably, it is 0.05-0.5 mass%.

  Furthermore, in addition to common aqueous solvents such as water, ethanol, glycerin, dipropylene glycol, 1,3-butylene glycol and the like in the aqueous phase, other water-soluble components such as, for example, , Arbutin, ascorbic acid and its derivatives, water-soluble drugs such as tranexamic acid and its derivatives, ultraviolet absorbers, chelating agents, pH adjusting agents, preservatives, dyes, fragrances and the like.

  The oil finely dispersed composition of the present invention is stable even if it does not contain a surfactant, and preferably contains no surfactant from the viewpoints of stability, skin irritation and usability. Any surfactant may be included in the oil phase or the aqueous phase as long as the above objective can be achieved. The blending amount of the surfactant is preferably 10% by mass or less, more preferably 5% by mass or less, and further preferably 2% by mass or less with respect to the total mass of the composition. When the amount of the surfactant is increased, the temporal stability of the finely dispersed composition of the oil of the present invention tends to deteriorate and stickiness tends to occur.

  The finely dispersed composition of the oil of the present invention can be used in any form as long as the object can be achieved, and the most suitable application aspect includes a skin external preparation. In this specification, “external preparation for skin” means a composition applied to the outer skin (including scalp and hair), and includes, for example, cosmetics, pharmaceuticals, quasi drugs, and the like.

  The finely dispersed composition of the oil of the present invention may be used as it is as an external preparation for skin, or may be used as an element added in the production process of a general external preparation for skin. When used as an element, the dosage form is arbitrary, for example, aqueous solution system, solubilization system, emulsification system, oil liquid system, gel system, paste system, ointment system, aerosol system, water-oil two-layer system, water -Includes any dosage form, such as three layers of oil-powder.

  The product form and use of the external preparation for skin of the present invention are also arbitrary, and for example, it can be used as an external preparation for facial, body or hair such as lotion, milky lotion, cream and pack.

  Further, in addition to the finely dispersed composition of the oil, a moisturizer, an emulsifier, an ultraviolet absorber, a fragrance, an antioxidant, an antiseptic / antifungal agent, and an extender are appropriately added as necessary within the range not impairing the effects of the present invention. In addition, it may contain other optional components that are usually used in external preparations for skin, such as cosmetics and pharmaceuticals, such as coloring agents such as coloring pigments, pH adjusting agents, and the like.

  The blending amount of the fine dispersion composition of the oil in the external preparation for skin of the present invention varies depending on its use and product form and is not particularly limited, but is preferably 0.01 with respect to the total mass of the external preparation for skin. -100 mass%, More preferably, it is 0.1-100 mass%.

  The oil finely dispersed composition of the present invention comprises a water phase containing a solid oil and a liquid oil at a temperature higher than the melting point of the solid oil and higher than the melting point of the solid oil containing the water-soluble thickener. It can be prepared by adding to the phase and shear mixing the mixture to a temperature below the melting point of the solid oil.

  Usually, a mixture of oily components heated to a temperature of around 70 ° C. and liquefied is directly injected from the lower part of the aqueous phase into an aqueous phase having the same temperature using, for example, an injection means such as a liquid feed pump. The oil phase is introduced into the aqueous phase. When such injection is carried out from the upper part of the aqueous phase, the oily component immediately floats and separates, and it may be difficult to form a uniform dispersion of fine particles.

  Next, for example, by shear mixing to a temperature below the melting point of the solid oil, such as about 40 ° C. to 50 ° C., the oil particles formed so that the solid oil is crystallized to include other oil components are sheared. Grind to form a fine dispersion of oil. Thereby, the oil phase containing the solid oil as water is preferably formed as fine particles having an average primary particle size of 0.1 to 30 μm, more preferably 1 to 15 μm, without causing floating or agglomeration of oily components. It can be stably dispersed in the phase. The shear mixing may be performed while the oil phase is added to the aqueous phase, or the shear mixing may be started immediately after completion of the addition without shear mixing during the addition. Further, at the time of shear mixing, for example, the mixture may be sheared and mixed using ice or the like, or may be sheared and mixed while naturally cooling at room temperature. In this specification, “shear mixing to a temperature below the melting point of the solid oil” means that shear mixing is started from a temperature higher than the melting point of the solid oil, and the temperature of the mixture of the oil phase and the aqueous phase is It means that shear mixing is performed continuously or intermittently until the temperature becomes lower than the melting point. For example, the production method of the present invention also includes a case where, after shear mixing to a temperature near the melting point of the solid oil component, shear mixing is once stopped and shear mixing is performed again at a temperature equal to or lower than the melting point of the solid oil component.

Shear mixing can be performed using any device capable of mixing while applying shear force. For example, the shear mixing can be performed by a high-speed shearing dispersion device such as a homomixer, a homodisper, a flow jet mixer, an ultramixer, a colloid mill, or a high-pressure shearing dispersion device such as a homogenizer, but the object of the present invention can be achieved. As long as it is, shear mixing may be performed using any other apparatus. Among these, a more homogeneous and stable oil fine dispersion composition can be prepared by shear mixing using a homomixer. The rotational speed when using a high-speed shearing dispersion device or the pressure when using a high-pressure shearing dispersion device varies depending on the type and power of the device used, and is not particularly limited. For example, a high-speed shearing dispersion device such as a homomixer is used. The rotation speed in this case is preferably 500 to 15,000 rpm, more preferably 1,000 to 10,000 rpm, and further preferably 4,000 to 9,000 rpm. If the rotational speed of the high-speed shear disperser is less than 500 rpm, oil fine particles having the expected size may not be formed. Even if the rotational speed is increased beyond 10,000 rpm, the effect of atomization can be further increased. Can not. Moreover, the pressure when using a high-pressure shear dispersion device such as a homogenizer is preferably 50 to 1000 kgf / cm ² , more preferably 100 to 500 kgf / cm ² , and further preferably 200 to 400 kgf / cm ² . If the pressure of the high-pressure shear disperser is less than 50 kgf / cm ² , oil fine particles with the expected dimensions may not be formed. Even if the pressure exceeds 1000 kgf / cm ² , the effect of atomization can be further increased. I can't.

  The shear mixing time varies depending on the time required to bring the temperature of the mixture of the oil phase and the liquid phase to a temperature equal to or lower than the melting point of the solid oil component, and is not particularly limited, but is preferably 1 minute to 60 minutes, more The time is preferably 2 minutes to 30 minutes, more preferably 3 minutes to 10 minutes.

  Furthermore, after the dispersion step by shear mixing, it is preferable to stir the dispersion in order to increase homogeneity and stability. The stirring is usually performed at a relatively low rotational speed of, for example, about 10 to 1500 rpm, more preferably about 20 to 300 rpm, for example, 30 minutes to 10 hours, more preferably 1 hour to 4 hours, for example, a propeller mixer, paddle mixer, anchor mixer. , A low speed stirring device such as a gate mixer or a planetary mixer.

  EXAMPLES Hereinafter, although an Example is given and this invention is demonstrated concretely, this invention is not limited to the following Example.

Using the same formulation shown in Table 1, oil dispersion compositions were prepared under the following dispersion treatment conditions (Examples 1 to 4 and Comparative Examples 1 to 5), and the dispersion composition was subjected to the following evaluation method. The particle shape, dispersion state, average maximum size, stability over time, usability (finger finger, familiarity with skin) and feeling of use (moist feeling, fluffy feeling) were evaluated.

Example 1
HM4500 / 50 ° C
Using a homomixer (manufactured by Tokushu Kika Co., Ltd.) at a rotational speed of 9000 rpm, the liquid oil phase melted by heating to about 70 ° C. to 75 ° C. is converted into an aqueous phase heated to about 70 ° C. After the addition, the homomixer was rotated to 4500 rpm and further cooled to 50 ° C. over 2.5 minutes in ice water while further shear mixing. The homomixer was stopped, and then cooled to 30 ° C. with stirring at 150 rpm using a propeller mixer (manufactured by HEIDON).

Example 2
HM4500 / 40 ° C
After adding the liquid oil phase melted by heating to about 70 ° C. to 75 ° C. while shear mixing at a rotational speed of 9000 rpm using a homomixer, the water phase heated to about 70 ° C. The mixture was further cooled to 40 ° C. over 5 minutes in ice water while further rotating and mixing at a rotational speed of 4500 rpm. The homomixer was stopped and then cooled to 30 ° C. with stirring at 150 rpm using a propeller mixer.

Example 3
HM9000 / 50 ° C
The liquid oil phase melted by heating to about 70 ° C. to 75 ° C. is added to the aqueous phase heated to about 70 ° C. while shear mixing using a homomixer at a rotation speed of 9000 rpm, and then rotated at 9000 rpm. While further shear mixing with a homomixer at the speed, the mixture was cooled to 50 ° C. over 2.5 minutes in ice water. The homomixer was stopped and then cooled to 30 ° C. with stirring at 150 rpm using a propeller mixer.

Example 4
HM9000 / 40 ° C
The liquid oil phase melted by heating to about 70 ° C. to 75 ° C. is added to the aqueous phase heated to about 70 ° C. while shear mixing using a homomixer at a rotation speed of 9000 rpm, and then rotated at 9000 rpm. The mixture was further cooled to 40 ° C. over 5 minutes in ice water while further shear mixing with a homomixer at the speed. The homomixer was stopped and then cooled to 30 ° C. with stirring at 150 rpm using a propeller mixer.

Comparative Example 1
PM175 / 70 ° C
While stirring at a rotational speed of 175 rpm using a propeller mixer, a liquid oil phase heated to about 70 ° C. to 75 ° C. and melted is added to an aqueous phase heated to about 70 ° C., and then the propeller mixer is rotated. The mixture was cooled to 30 ° C. in ice water while stirring at a speed of 150 rpm.

Comparative Example 2
PM300 / 70 ° C
While stirring at a rotational speed of 300 rpm using a propeller mixer, a liquid oil phase heated to about 70 ° C. to 75 ° C. and melted is added to an aqueous phase heated to about 70 ° C., and then the propeller mixer is rotated. The mixture was cooled to 30 ° C. in ice water while stirring at a speed of 150 rpm.

Comparative Example 3
PM500 / 70 ° C
While stirring at a rotational speed of 500 rpm using a propeller mixer, a liquid oil phase heated to about 70 ° C. to 75 ° C. and melted is added to an aqueous phase heated to about 70 ° C., and then the propeller mixer is rotated. The mixture was cooled to 30 ° C. in ice water while stirring at a speed of 150 rpm.

Comparative Example 4
HM4500 / 70 ° C
While stirring at a rotational speed of 4500 rpm using a homomixer, the liquid oil phase melted by heating to about 70 ° C. to 75 ° C. is added to the aqueous phase heated to about 70 ° C., and then the homomixer is stopped. Then, it was cooled to 30 ° C. while stirring at 150 rpm using a propeller mixer.

Comparative Example 5
HM9000 / 70 ° C
While stirring at a rotational speed of 9000 rpm using a homomixer, the liquid oil phase melted by heating to about 70 ° C. to 75 ° C. is added to the aqueous phase heated to about 70 ° C., and then the homomixer is stopped. Then, it was cooled to 30 ° C. while stirring at 150 rpm using a propeller mixer.

Evaluation of Particle Shape, Dispersion State and Average Maximum Size The shape, dispersion state and average maximum size of oil particles in the dispersion composition were scaled from the top by spreading a 3 g sample on a 55 mmφ petri dish and observing with an optical microscope. At the same time, the images were captured with a digital camera and evaluated using optical micrographs. The average maximum dimension was determined by reading the maximum dimension of 50 randomly selected particles from a scale (one scale 2.5 μm) and calculating the average value. In FIG. 1, the optical microscope photograph immediately after manufacture of the dispersion composition created by each dispersion processing conditions of Examples 1-4 is shown.

Evaluation of stability over time The stability over time of the dispersion composition was evaluated according to the following evaluation criteria using optical micrographs of the composition after standing at each temperature for 3 months:
○: No change in particle aggregation
Δ: Particle aggregation slightly increased ×: Particle aggregation significantly increased

FIG. 2 shows an optical microscope of the dispersion composition prepared under the dispersion treatment conditions of Example 1 immediately after production and after standing at −5 ° C., 0 ° C., room temperature (RT), 37 ° C., and 50 ° C. for 3 months. Show photos.

Evaluation of Usability and Feeling of Use Evaluation of usability (finger feeling, familiarity with skin) and feel of use (moist feeling, fluffy feeling) of the finely dispersed composition was conducted by a sensory test using a professional panel. Each sample was applied to the forearm of 20 female panels and evaluated according to the following criteria:
(Finger)
○: 15 or more panel evaluated as easy to remove with fingers Δ: 6 to 14 panel evaluated as easy to remove with fingers ×: 5 or less panels evaluated as easy to remove with fingers

(Skin familiarity)
○: 15 or more panels evaluated as being familiar with skin Δ: 6 to 14 panels evaluated as being familiar with skin ×: 5 or less panels evaluated as being easy to adjust to skin

(Moist feeling)
○: 15 or more panel evaluated as having a moist feeling on the skin after application. Δ: 6 to 14 panel having been evaluated as having a moist feeling on the skin after application. ×: The skin after application has a moist feeling. No more than 5 panels

(Feeling plump)
○: 15 or more panel evaluated as having fluffy feeling after application Δ: 6 to 14 panel having been evaluated as having fluffy feeling after application ×: Skin after application having fluffy feeling No more than 5 panels

The evaluation results are shown in Table 2.

  In the finely dispersed compositions of oils of Examples 1 to 4 subjected to shear mixing to a temperature equal to or lower than the melting point of the solid oil (40 ° C. or 50 ° C.), the average maximum size of the particles is in the range of 0.1 to 30 μm. Yes, after aggregation for 3 months at 50 ° C, no aggregation occurs, stability over time is good, and when applied to the skin (finger, skin familiarity) and feeling (moist feeling, fluffy feeling) are also excellent It was. On the other hand, the finely dispersed composition of the oils of Comparative Examples 1 to 3 which were only subjected to stirring with a low-speed stirring device (propeller mixer) without being subjected to shear mixing, Particles could not be created, the fingers were not well-familiar and could not give the skin a plump feeling. In addition, the oil finely dispersed compositions of Comparative Examples 4 and 5 in which shear mixing was performed only at a temperature higher than the melting point of the solid oil component, the oil particles formed in a liquid state were made fine by shearing force and the particles were small. However, immediately after the small particles aggregated and joined together, aggregated debris was generated, which was very uneven. The stability over time and the familiarity with the skin were poor, and the skin was not able to give a plump feeling.

Next, using the same formulation shown in Table 3, an oil dispersion composition prepared according to the method of the present invention (Example 5) and a composition prepared by low-speed stirring with a conventional propeller mixer (Comparative Example) In 6), the usability and usability were compared and evaluated.

Example 5
Using a homomixer (manufactured by Tokushu Kika Co., Ltd.) at a rotational speed of 9000 rpm, the liquid oil phase melted by heating to about 70 ° C. to 75 ° C. is converted into an aqueous phase heated to about 70 ° C. After the addition, the mixture was cooled to 40 ° C. over 5 minutes in ice water while shear mixing at 9000 rpm. The homomixer was stopped, and then cooled to 30 ° C. with stirring at 150 rpm using a propeller mixer (manufactured by HEIDON).

Comparative Example 6
While stirring at a rotation speed of 180 rpm using a propeller mixer, a liquid oil phase heated to about 70 ° C. to 75 ° C. and melted is added to water heated to about 70 ° C., and then the remaining components are added. Then, the propeller mixer was cooled to 30 ° C. in ice water while further stirring with a rotation speed of 150 rpm.

  In FIG. 3, the optical micrograph of the particle | grains in each prepared dispersion composition is compared and shown. One scale of the scale is 2.5 μm. The particles in the composition of Example 5 prepared by the method of the present invention had a maximum particle size of about 2.5 to 12.5 μm and were wedge-shaped, whereas the particles in the composition of Comparative Example 6 Was a large sphere with a particle size of about 0.1 to 0.5 mm.

Comparative evaluation of usability and feeling of use Seven skin care panels were allowed to evaluate the following evaluation criteria by comparing the compositions of Example 5 and Comparative Example 6 for various items relating to usability and feeling of use:

-2: Comparative example 6 is remarkably superior -1: Comparative example 6 is slightly superior 0: Same level 1: Example 5 is slightly superior 2: Example 5 is remarkably superior ing

The average value of scoring of 7 panelists for each item is obtained and shown in the graph of FIG.

  Even with the same formulation, the finely dispersed composition of oil prepared by the method of the present invention is superior in finger feeling, moist feeling, and fluffy feeling, particularly compared to the composition of the comparative example prepared by the conventional method. In addition, it was evaluated that the overall evaluation was superior to that of the comparative example.

  Hereinafter, other embodiments of the finely dispersed composition of the oil of the present invention will be shown as examples. In addition, all compounding quantities are represented by the mass% with respect to the formulation whole quantity.

Example 6
Agar Formulation Prepared based on the following formulation (Table 4) and manufacturing method using agar as a water-soluble thickener:

(Production method)
Using a homomixer (manufactured by Tokushu Kika Co., Ltd.) at a rotational speed of 9000 rpm, a liquid oil phase heated to 70 ° C. to 75 ° C. is applied to a 70 ° C. aqueous phase in which agar is dissolved for 1 minute. After the addition, the rotation speed of the homomixer was set to 4500 rpm, and the mixture was further cooled to 55 ° C. in ice water while further shear mixing. The homomixer was stopped, allowed to cool until the agar was completely solidified, and then shear mixed at 4500 rpm for 10 minutes using a homomixer.

  The finely dispersed oil composition of this example is a uniform composition of spherical particles having an average particle diameter of about 12.5 μm, has good temporal stability, and is excellent in finger contact and skin familiarity. Furthermore, it is a non-sticky composition, has a very good feeling in use, and has a high palatability.

Example 7
Microgel formulation (1)
A microgel (see Japanese Patent Application Laid-Open No. 2004-43785) was used as a water-soluble thickener and was prepared based on the following formulation (Table 5) and production method:

(Production method)
Using a homomixer (manufactured by Tokushu Kika Co., Ltd.) at a rotational speed of 9000 rpm, the liquid oil phase melted by heating to about 70 ° C. to 75 ° C. is converted into an aqueous phase heated to about 70 ° C. After the addition, the homomixer was rotated at 6500 rpm and further cooled to 45 ° C. over 8 minutes in ice water while further shear mixing.

  The finely dispersed oil composition of this example is a uniform composition of spherical particles with a partial defect having an average maximum dimension of about 22.5 μm, good stability over time, and softness per skin after application. Excellent.

Example 8
Microgel formulation (2)
A microgel (see JP 2004-43785 A) was used as a water-soluble thickener and was prepared based on the following formulation (Table 6) and manufacturing method:

(Production method)
Using a homomixer (manufactured by Tokushu Kika Co., Ltd.) at a rotational speed of 9000 rpm, the liquid oil phase melted by heating to about 70 ° C. to 75 ° C. is converted into an aqueous phase heated to about 70 ° C. After the addition, the mixture was shear-mixed at 9000 rpm to 55 ° C. while being cooled in ice water, shear-mixed at 55 ° C. to 50 ° C. at 6000 rpm, and further shear-mixed at 4500 rpm at 50 ° C.

  The oil finely dispersed composition of this example is a uniform composition of rod-shaped particles having an average maximum dimension of about 17.5 μm, good stability over time, and excellent softness per skin after application. ing.

  FIG. 5 shows optical micrographs of the finely dispersed oil compositions prepared in Examples 6 to 8.

  Below, the formulation example of the skin external preparation of this invention is shown as an Example. All are prepared by the same method as in Example 1. In addition, all compounding quantities are represented by the mass% with respect to the formulation whole quantity.

Example 9
Formulation Example 1: Emulsion (KOH neutralized)

Example 10
Formulation Example 2: Latex (AMPD neutralization)

Example 11
Formulation Example 3: Emulsion (Arginine Neutralization / Refreshing Type with Less Moisturizer)

Example 12
Formulation Example 4: Emulsion (AMPD neutralization / moisturizing agent and oil-free type with low blending amount)

Example 13
Formulation example 5: emulsion (AMPD neutralization / refreshing type with less oil content)

Example 14
Formulation Example 6: Hydrogenated polyisobutene formulation (usable rich type)

Example 15
Formulation Example 7: Alcohol-containing formula (refreshing type)

Example 16
Formulation Example 8: Solid oil rich formula (hard use type)

Example 17
Formulation Example 9: Behenyl alcohol formulation (soft type)

Example 18
Formulation Example 10: Acrylic / alkyl methacrylate copolymer formulation

Example 19
Formulation Example 11: Simple Formula

  Any of the above-mentioned external preparations for skin of Examples 9 to 19 (Prescription Examples 1 to 11) contains fine oil particles having an average primary particle size of 0.1 to 30 μm, and has good stability, usability and Excellent usability.

Optical micrographs of oil fine dispersion compositions of Examples 1 to 4 Optical micrograph showing stability over time of oil fine dispersion composition of Example 1 at each temperature Optical micrographs comparing the size of the particles in the compositions of Example 5 and Comparative Example 6 The graph which shows the comparative evaluation result of the usability and the usability of the compositions of Example 5 and Comparative Example 6 Optical micrographs of oil fine dispersion compositions of Examples 6-8

Claims (12)

A finely dispersed composition of oil, comprising an oil phase containing a solid oil and a liquid oil, and an aqueous phase containing a water-soluble thickener, and does not contain a surfactant, and the oil phase is lipophilic It contains a gelling agent and is dispersed in the aqueous phase as fine particles having an average primary particle size of 0.1 to 30 μm. In the fine particles, the solid oil is crystallized to form an oil phase and an aqueous phase. A finely dispersed composition of oil, characterized by being present at the interface . The finely dispersed composition of oil according to claim 1, wherein an average maximum dimension of the primary particles is 1 to 15 μm. The finely dispersed composition of oil according to claim 1 or 2, wherein the oil phase contains 10 to 50% by mass of solid oil based on the total mass of the oil phase. 4. The finely dispersed oil composition according to claim 3, wherein the oil phase contains 10 to 20% by mass of solid oil based on the total mass of the oil phase. The finely dispersed composition of oil according to any one of claims 1 to 4, wherein a blending amount of the oil phase is 1 to 20% by mass with respect to a total mass of the composition. The oil according to any one of claims 1 to 5, wherein the solid oil contains one or more selected from the group consisting of candelilla wax and higher alcohols having 16 or more carbon atoms. Fine dispersion composition. The finely-dispersed composition of oil according to any one of claims 1 to 6, wherein the water-soluble thickener contains carboxyvinyl polymer or agar. The skin external preparation containing the fine dispersion composition of the oil of any one of Claim 1 to 7. A method for producing a finely dispersed oil composition, wherein an oil phase containing a solid oil and a liquid oil is higher than a melting point of the solid oil and higher than a melting point of the solid oil containing a water-soluble thickener. Adding to the aqueous phase at temperature;
A step of shear- mixing the mixture of the oil phase and the aqueous phase to a temperature below the melting point of the solid oil by a high-speed shearing dispersion device or a high-pressure shearing dispersion device to disperse the oil phase as fine particles in the aqueous phase; and
A step of further stirring after the dispersing step ;
The oil phase contains a lipophilic gelling agent;
The oil phase and aqueous phase do not contain a surfactant ,
The average maximum dimension of the primary particles of the fine particles is 0.1 to 30 μm . The manufacturing method according to claim 9 , wherein an average maximum dimension of primary particles of the fine particles is 1 to 15 μm. The manufacturing method according to claim 9 or 10 , wherein the shear mixing is performed by a homomixer, a homodisper, a flow jet mixer, an ultramixer, a colloid mill, or a homogenizer. The stirring step, a propeller mixer, a paddle mixer, anchor mixer, gate mixer or a planetary and performing the mixer, The method according claim 9 to 11 any one.