JP2013006822A - Emulsified product, and method for producing the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an emulsified product having improved characteristics (especially dampish feeling or film feeling on skin or hair when being used as a cosmetic, texture of skin or the like), and to provide a method for producing the same.SOLUTION: In this emulsified product, the inner phase contains a water holding oil, and at least a part thereof is an oil phase in the lyotropic spherical liquid crystal state, and the outer phase is an aqueous phase, and contains O/W emulsion containing closed vesicles formed from an amphiphilic substance for forming closed vesicles spontaneously or particles of a polycondensation polymer having a hydroxy group. The O/W emulsion can maintain the emulsified state by interposition of the closed vesicles and/or the particles on the interface between the aqueous phase and the oil phase.

Description

  The present invention relates to an emulsion and a method for producing the emulsion.

  Conventionally, when a functional oil base or functional granules are emulsified and dispersed in water, a surfactant is selected according to the required HLB of the functional oil base and the properties of the granule surface, and emulsified and dispersed. . Since the emulsifier has insufficient thermal stability and stability over time, a wide variety of surfactants are mixed and used (see Non-Patent Documents 1 to 4, etc.).

  By the way, emulsions are often used in cosmetics applied to skin and hair in anticipation of a moisturizing effect due to oil phase components. Currently, the oil phase components and surfactants are appropriately selected according to the required properties.

“Emulsion Science” Edited by P.I. Sherman, Academic Press Inc. (1969) "Microemulsions-Theory and Practice" Edited by Leon M. et al. price, Academic Press Inc. (1977) "Emulsification / Solubilization Technology" Recommended, Engineering Book Publishing (1976) "Development Technology of Functional Surfactants" CM Publishing (1998)

  However, the conventional emulsion has a limit to the extent that the characteristics can be improved. In particular, when conventional emulsions are used in cosmetics, it is difficult to improve characteristics such as film feeling on skin and hair and skin texture.

  The present invention has been made in view of the above circumstances, and has improved properties (particularly moist feeling and film feeling on skin and hair when used in cosmetics, skin texture, etc.). It aims at providing the manufacturing method of an emulsion and an emulsion.

  The inventors of the present invention provide an oil phase in which an emulsifier including a closed endoplasmic reticulum formed from an amphiphilic substance having self-organization ability and a polycondensation polymer that has been granulated contains a water-holding oil agent and is in a lyotropic spherical liquid crystal state. The present inventors have found that it can be formed and have completed the present invention. Specifically, the present invention provides the following.

  (1) The inner phase is an oil phase containing a hydrated oil and at least partly in the form of lyotropic spherical liquid crystals, the outer phase is an aqueous phase, and is formed by an amphiphilic substance that spontaneously forms closed vesicles. An emulsion comprising an O / W emulsion comprising particles of a closed condensation vesicle or a polycondensation polymer having a hydroxyl group.

  (2) The emulsion according to (1), wherein the O / W emulsion maintains an emulsified state by interposing the closed vesicles and / or the particles at an interface between the water phase and the oil phase. .

  (3) The emulsion according to (2), wherein a fluidized state at room temperature is realized by interposing the closed vesicles and / or the particles at an interface between the aqueous phase and the oil phase.

  (4) The emulsion according to any one of (1) to (3), which is used in cosmetics applied to skin or hair.

  (5) The emulsion according to any one of (1) to (4), wherein an average particle size of the inner phase is 1.0 μm or more.

  (6) The emulsion according to any one of (1) to (5), wherein the ratio of the oil phase in the lyotropic spherical liquid crystal state is 80% or more in the inner phase having a cross-sectional major axis of 1.0 μm or more.

  (7) The emulsion according to any one of (1) to (6), wherein a liquid oil component is contained in an amount of less than 10% by mass with respect to the emulsion separately from the water-holding oil.

  (8) The emulsion according to any one of (1) to (7), wherein a blending amount of the water-holding oil is more than 10% by mass with respect to the emulsion.

  (9) The emulsified product according to any one of (1) to (8), wherein the hydrated oil agent contains a higher alcohol.

  (10) A cosmetic comprising the emulsion according to any one of (1) to (9) and applied to skin or hair.

(11) A layered body of a bilayer film of an amphiphile is dispersed in water, or a polycondensation polymer having a hydroxyl group is made into single particles in water, and the closed vesicle formed by the amphiphile or the heavy Forming an emulsifier dispersion containing condensation polymer particles;
A step of forming an O / W emulsion by mixing the emulsifier dispersion and an oil agent containing a water-holding oil agent at a temperature equal to or higher than the melting point of the water-holding oil agent.

  (12) The method for producing an emulsion according to (11), wherein in the step of forming the O / W emulsion, the amount of the liquid oil component contained in the oil is less than 10% by mass with respect to the emulsion.

  (13) The method for producing an emulsion according to (11) or (12), wherein in the step of forming the O / W emulsion, a blending amount of the water-holding oil is more than 10% by mass with respect to the emulsion.

  (14) The method for producing an emulsion according to any one of (11) to (13), wherein the closed vesicles or the particles in the emulsifier dispersion exhibit an average particle diameter of 8 nm to 800 nm.

  (15) A method for producing a cosmetic comprising a step of processing the emulsion produced by the method according to any one of (11) to (14) into a cosmetic.

  (16) The process for producing a cosmetic according to (15), wherein the processing step includes a step of diluting the emulsion with water.

  (17) The method for producing a cosmetic according to (15) or (16), wherein the processing step includes a step of adding an emulsion of a liquid oil component to the emulsion.

  (18) To the lyotropic spheroidization of the liquid crystal in the oil phase containing a water-containing oil agent of particles of a polycondensation polymer having closed vesicles and / or hydroxyl groups formed by amphiphiles that spontaneously form closed vesicles Use of.

  According to the present invention, the hydrated oily agent in the internal phase is formed into a lyotropic spherical liquid crystal by containing particles of a closed vesicle formed by an amphiphile that spontaneously forms a closed vesicle or a polycondensation polymer particle having a hydroxyl group. Thus, the properties of the emulsion (particularly, moist feeling and film feeling on the skin and hair when used in cosmetics, skin texture, etc.) can be improved.

It is the all-optical micrograph (a) of the emulsion which concerns on Example 1 of this invention, and the polarization micrograph (b) in the same visual field. It is the all-optical micrograph (a) of the emulsion which concerns on Example 2 of this invention, and the polarization micrograph (b) in the same visual field. It is the all-optical micrograph (a) of the emulsion which concerns on a comparative example, and the polarization micrograph (b) in the same visual field. It is the all-optical micrograph (a) of the emulsion which concerns on Example 3 of this invention, and the polarization micrograph (b) in the same visual field. It is the all-optical micrograph (a) of the emulsion which concerns on Example 4 of this invention, and the polarization micrograph (b) in the same visual field. It is the all-optical micrograph (a) of the emulsion which concerns on Example 5 of this invention, and the polarization micrograph (b) in the same visual field. It is the all-optical micrograph (a) of the emulsion which concerns on Example 6 of this invention, and the polarization micrograph (b) in the same visual field.

  Hereinafter, although embodiment of this invention is described, these do not limit this invention.

  The emulsion according to the present invention includes particles of a closed vesicle or a polycondensation polymer having a hydroxyl group formed of an amphiphile that spontaneously forms a closed vesicle, the internal phase includes a water-containing oil agent, and at least A part is an oil phase in the state of a lyotropic spherical liquid crystal, and an outer phase contains an O / W emulsion that is an aqueous phase. The water-holding oil has a property of taking a liquid crystal structure, but when it comes into contact with water, it may solidify soon and not take a liquid crystal structure. However, in the present invention, closed vesicles or polycondensation polymer particles are present at the interface between the water phase and the oil phase, so that the water-containing oil mixed with water at room temperature (specifically, 25 ° C.). The liquid state is realized by suppressing solidification, thereby realizing the liquid crystal state, and the hydrated oil agent is emulsified spherically by van der Waals force in the process, so that the lyotropic spherical liquid crystal can be formed. This effect is unique to three-phase emulsification with closed endoplasmic reticulum or polycondensation polymer particles and cannot be obtained with conventional surfactants.

  The lyotropic spherical liquid crystal is formed by overlapping spherical layers of lamellar liquid crystal, and can exhibit the characteristics of lamellar liquid crystal over the entire outer periphery. For this reason, the emulsion according to the present invention is suitably used for cosmetics applied to the skin or hair, and gives excellent properties with respect to moist feeling, film feeling, skin texture, etc. on the skin and hair. Can do.

  In the lyotropic spherical liquid crystal, the shape of the inner phase observed in the all-optical micrograph of the emulsion is substantially circular (a perfect circle, an ellipse, or a shape close to it). It is identified by confirming Nicole. The lyotropic spherical liquid crystal is a spherulite of the conventionally known thermotropic liquid crystal (the black crossed Nicol in the polarization micrograph is observed only in the internal phase where the liquid crystal direction and the irradiation direction of the polarization accidentally have a predetermined relationship. The probability is significantly different from that of a lyotropic spherical liquid crystal).

  The internal phase in the emulsion may be at least partially in the state of lyotropic spherical liquid crystals, and not all of the internal phases may be lyotropic spherical liquid crystals. However, it is preferable that the ratio of the oil phase in the state of lyotropic spherical liquid crystal is 80% or more in the inner phase having a cross-sectional major axis of 1.0 μm or more, more preferably in view of sufficiently obtaining the above effect. 85% or more. The “longitudinal major axis of 1.0 μm or more” here refers to the sectional major axis of the inner phase in the field of view of the all-optical microscope. As will be described later, since the inner phase with an excessively small particle size cannot emit white light due to interference light under visible light, the proportion of the inner phase in the state of the lyotropic spherical liquid crystal in the population not including such an inner phase is better. , Which reflects the performance of the emulsion with high accuracy.

  The O / W emulsion is preferably one that maintains an emulsified state by the presence of closed vesicles and / or the above particles at the interface between the aqueous phase and the oil phase. Thereby, even if the environment (composition, concentration, temperature, etc.) of the outer phase changes, the inner phase is protected and changes in the liquid crystal structure are suppressed. This state is confirmed by observing the emulsion with a transmission electron microscope (TEM) (for example, Japanese Patent No. 3855203).

  In order for the lyotropic spherical liquid crystal to give the above characteristics, the optical path difference due to the liquid crystal needs to be an integral multiple of the wavelength (this causes white light emission due to interference light), and accordingly the liquid crystal needs to have a corresponding thickness. . For this reason, when used under visible light as in the cosmetics described above, the particle size of the internal phase constituting the liquid crystal needs to be at least twice the wavelength of visible light (390 nm) (780 nm).

  From another viewpoint, in order to maximize the characteristics of the oil agent of the emulsion, the emulsion particles are sufficiently broken by an external force during application or the like, and the water-holding oil agent in the internal phase is uniformly applied (for example, skin, hair) It is desirable to spread to. When the particle diameter of the inner phase is too small, the external force is not sufficiently applied to the emulsion particles, and it is difficult to sufficiently break the emulsion particles. Therefore, the average particle size of the inner phase is preferably 1.0 μm or more, more preferably 3.0 μm or more, and most preferably 5.0 μm or more. As a result, the above properties (especially moist and filmy feeling on the skin and hair when used in cosmetics, skin texture, etc.) are further improved and spread to the application target (good elongation) ) Will improve dramatically. Further, from the viewpoint of balance between ease of production and the above effect, the average particle diameter of the inner phase is not particularly limited, but may be 20 μm or less, 15 μm or less, and 10 μm or less. The average particle size of the inner phase is measured with a laser diffraction / scattering particle size distribution analyzer (SALD2100, Shimadzu Corporation) in a state where the viscosity of the emulsion is sufficiently low (diluted if necessary).

  The water-holding oil agent is not particularly limited, and may be an oil-soluble substance that has one or more polar groups in the molecule and is liquid or pasty or solid at room temperature. For example, fatty acids such as isostearic acid, isopalmitic acid, oleic acid, palmitoleic acid, linoleic acid, ricinoleic acid, lanolin derivatives such as lanolin, lanolin alcohol, hydrogenated lanolin alcohol, cetanol, hexyldecanol, isostearyl alcohol, stearyl alcohol, octyl Examples include higher alcohols such as dodecanol, oleyl alcohol, cetostearyl alcohol, and behenyl alcohol, and fatty acid esters and fatty acid oligomer esters derived from animal and vegetable oils such as cholesterol derivatives and phytosterol derivatives, which may be one or more of these. Examples of the cholesterol derivative and phytosterol derivative include macadamia nut oil fatty acid cholesteryl, macadamia nut oil fatty acid phytosteryl, lanolin fatty acid cholesteryl, and cholesteryl 12-hydroxystearate. Of these, higher alcohols are particularly preferred because of their high melting point and low stickiness.

  Since the lyotropic spherical liquid crystal based on the water-repellent oil gives the desired properties, it is preferable that the amount of the water-hydrate oil is sufficiently large. As described above, in the emulsion of the present invention, since the solidification of the water hydrated oil is highly suppressed, the blending amount of the water hydrated oil can be sufficiently increased, and is not particularly limited. It is preferably more than 10% by mass, more preferably 15% by mass or more and 20% by mass or more. In addition, each compounding quantity in this invention is the content measured by the quantity which actually mix | blended or gas chromatography.

  The internal phase may contain an oil other than the water-holding oil depending on the performance required for the emulsion. However, in the present invention, since the solidification of the water-holding oil is suppressed as described above, it is not necessary to use a liquid oil component (for example, mineral oil) to suppress the solidification of the water-holding oil. Since the liquid oil component (for example, mineral oil) often inhibits the hydrated oil agent from forming lyotropic spherical liquid crystals, it may contain the liquid oil component in an amount of less than 10% by mass relative to the emulsion. Preferably, more preferably 9 mass% or less, 8 mass% or less, 7 mass% or less, 6 mass% or less, 5 mass% or less, 4 mass% or less, 3 mass% or less, 2 mass% or less, 1 mass% or less, 0% by mass.

  However, a liquid oil component (for example, mineral oil) may be necessary for the purpose of performing a specific function as a component of cosmetics. In this case, it is preferable to prepare an O / W emulsion in which the inner phase is a liquid oil component (for example, mineral oil) separately from the O / W emulsion in which the inner phase is a hydrated oil, and to mix them. . In the emulsion produced through such a method, as a result, the blending amount of the liquid oil component may be 10% by mass or more based on the emulsion, but the lyotropic spherical liquid crystal of the water-holding oil is already sufficient. Since it is formed, there is no particular problem.

  The amphiphilic substance that spontaneously forms a closed endoplasmic reticulum is not particularly limited, but is a polyoxyethylene hydrogenated castor oil derivative represented by the following general formula 1, or a dialkylammonium derivative represented by the general formula 2: Examples thereof include derivatives of halogenated salts of trialkylammonium derivatives, tetraalkylammonium derivatives, dialkenylammonium derivatives, trialkenylammonium derivatives, or tetraalkenylammonium derivatives.

General formula 1

  In the formula, E, which is the average added mole number of ethylene oxide, is 3 to 100. If E is excessive, the type of good solvent that dissolves the amphiphilic substance is limited, and thus the degree of freedom in producing hydrophilic nanoparticles is narrowed. The upper limit of E is preferably 50, more preferably 40, and the lower limit of E is preferably 5.

General formula 2

  In the formula, R 1 and R 2 are each independently an alkyl group or alkenyl group having 8 to 22 carbon atoms, R 3 and R 4 are each independently hydrogen or an alkyl group having 1 to 4 carbon atoms, and X is F, Cl, Br or I.

  As the amphiphile, phospholipids, phospholipid derivatives, etc., in particular, those in which a hydrophobic group and a hydrophilic group are ester-bonded may be employed.

  As the phospholipid, among the structures represented by the following general formula 3, DLPC (1,2-Dilauroyl-sn-glycero-3-phospho-rac-1-choline) having a carbon chain length of 12, DMPC (1,2-Dimyristol-sn-glycero-3-phospho-rac-1-choline), DPPC with a carbon chain length of 16 (1,2-Dipalmitoyyl-sn-glycero-3-phospho-rac-1-choline) Can be adopted.

General formula 3

  In addition, among the structures represented by the following general formula 4, DLPG (1,2-Diilauroyl-sn-glycero-3-phospho-rac-1-glycerol) Na salt or NH4 salt, carbon chain of carbon chain length 12 Na or NH4 salt of DMPG having a length of 14 (1,2-Dimyristol-sn-glycero-3-phospho-rac-1-glycerol), DPPG having a carbon chain length of 16 (1,2-Dipalmitoyyl-sn-glycero-3) -Phospho-rac-1-glycerol) Na salt or NH4 salt may be employed.

Formula 4

  Further, lecithin such as egg yolk lecithin or soybean lecithin may be employed as the phospholipid.

  The polycondensation polymer having a hydroxyl group may be either a natural polymer or a synthetic polymer, and may be appropriately selected according to the use of the emulsifier. However, natural polymers are preferable from the viewpoint of safety and generally inexpensive, and sugar polymers described below are more preferable from the viewpoint of excellent emulsifying function. The particles include both single particles of the polycondensation polymer and those in which the single particles are connected, but do not include aggregates (having a network structure) before being formed into single particles.

  The sugar polymer is a polymer having a glucoside structure such as cellulose and starch. For example, those produced by microorganisms with some sugars among monosaccharides such as ribose, xylose, rhamnose, fucose, glucose, mannose, glucuronic acid, gluconic acid, xanthan gum, gum arabic, guar gum, caraya gum, carrageenan , Pectin, fucoidan, quinseed gum, tranto gum, locust bean gum, galactomannan, curdlan, gellan gum, fucogel, casein, gelatin, starch, collagen and other natural polymers, methylcellulose, ethylcellulose, methylhydroxypropylcellulose, carboxymethylcellulose, Hydroxymethylcellulose, hydroxypropylcellulose, sodium carboxymethylcellulose, propylene glycol alginate, cellulose Crystals, starch-acrylic acid sodium graft polymer, semi-synthetic polymers such as hydrophobic hydroxypropylmethylcellulose, polyvinyl alcohol, polyvinyl pyrrolidone, carboxyvinyl polymer, polyacrylic acid salts, synthetic polymers such as polyethylene oxide can be cited.

  The closed vesicles and particles have an average particle size of about 8 nm to 800 nm before the formation of the emulsion, but in the O / W emulsion structure, the average particle size is about 8 nm to 500 nm. In addition, the particle | grains of the polycondensation polymer which have the closed endoplasmic reticulum of an amphiphile and a hydroxyl group may contain only one, or both. When both are included, for example, separately emulsified emulsions may be mixed.

The above emulsion is a closed endoplasmic reticulum formed of an amphiphilic substance by dispersing a bilayer film of an amphiphilic substance in water, or by making a polycondensation polymer having a hydroxyl group into water into single particles. Forming an emulsifier dispersion comprising polycondensation polymer particles;
The emulsifier dispersion is mixed with an oil agent containing a water-holding oil agent at a temperature equal to or higher than the melting point of the water-holding oil agent to form an O / W emulsion.

  By sufficiently forming closed vesicles or polycondensation polymer particles, an oil phase in a lyotropic spherical liquid crystal state having a sufficient particle size can be obtained. As such a method, the above-mentioned amphiphilic substance and / or polycondensation polymer having a hydroxyl group is added to a dispersion medium (that is, water) and stirred for a long time. After dissolution, the solution may be mixed with water (for example, see JP-A-2006-241424). As a result, the above-mentioned characteristics (particularly moist feeling and film feeling on skin and hair when used in cosmetics, skin texture, etc.) are further improved, and spread to the application target (good elongation) ) Will improve dramatically. Specifically, the above step is preferably performed until the closed vesicles or particles in the emulsifier dispersion exhibit an average particle diameter of 8 nm to 800 nm.

  In the single particle formation, granules containing a conjugate of polycondensation polymer particles are dispersed in water to prepare a dispersion, then the granules are swollen, and hydrogen bonds derived from the granules are further broken under reversible conditions. Thus, it is preferable to produce a relaxed product in which the higher-order structure of the conjugate is relaxed, and after a while, cleave the hydrogen bond in the conjugate and separate the polycondensation polymer particles in water. Without this process, it is difficult to sufficiently obtain polycondensation polymer particles (single particles to several single particles) (see Comparative Example).

  In the step of forming the O / W emulsion, the blending amount of the liquid oil component contained in the oil is preferably less than 10% by mass with respect to the emulsion. Thereby, inhibition of lyotropic spherical liquid crystal formation by a liquid oil component is suppressed. When a large amount of the liquid oil component is required, it is preferable to separately prepare an emulsion of the liquid oil component and mix it with the emulsion of the present invention.

  In the step of forming the O / W emulsion, the blending amount of the water-containing oil agent is preferably more than 10% by mass with respect to the emulsion. Thereby, the characteristic (especially moist feeling on the skin and hair when used for cosmetics, a film feeling, skin texture, etc.) can be further improved.

  Moreover, after forming the O / W emulsion, it is preferable to gradually cool the emulsion so as not to inhibit the liquid crystal formation of the internal phase. Although it does not specifically limit, What is necessary is just to cool at the speed | rate about 30-120 degreeC per hour.

  The present invention includes a cosmetic that contains the above emulsion and is applied to the skin or hair. The cosmetic according to the present invention contains closed vesicles formed by an amphiphilic substance that spontaneously forms closed vesicles or particles of a polycondensation polymer having a hydroxyl group, so that the water-holding oil in the internal phase is lyotropic. A spherical liquid crystal is formed, and thereby the properties of the emulsion (particularly, moist feeling on the skin and hair when used in cosmetics, film feeling, skin texture, etc.) can be improved.

  Specific forms of cosmetics are not particularly limited, but skin cosmetics such as creams, emulsions, lotions, cosmetics, facial cleansers, cleansings, body soaps, shampoos, rinses, conditioners, treatments, styling agents, permanents -It may be a cosmetic product for hair such as a color pre- and post-treatment agent, or a product (so-called miscellaneous goods) that is not subject to the Pharmaceutical Affairs Law in a dosage form similar to cosmetics. According to the request | requirement with respect to cosmetics, cosmetics may contain another component suitably in addition to an emulsion.

  The manufacturing method of the cosmetics which concern on this invention has the process of processing the emulsion manufactured by the above method into cosmetics. Processing is not particularly limited, and may be performed as appropriate. Specifically, the processing step may include a step of diluting the emulsion with water. In the case of a surfactant, when water is added to the O / W emulsion, the surfactant that has been reversibly adsorbed to the oil phase is detached, the emulsified state becomes unstable, and the liquid crystal structure is destroyed. However, in the present invention, closed vesicles or polycondensation polymer particles are irreversibly adhered to oil and emulsified, so that the emulsified state is stable and the liquid crystal structure is maintained regardless of the presence or absence of dilution. This makes it possible to produce a cosmetic product in which the emulsion is produced so that the oil has a high concentration, the emulsion is distributed, etc., and appropriately diluted when the cosmetic product is produced.

  Moreover, the process to process may have the process of adding the emulsion of a liquid oil component (for example, mineral oil) to the above-mentioned emulsion. As described above, the liquid oil component may be required in cosmetics, but when emulsified together with the water-holding oil, the lyotropic spherical liquid crystal formation of the water-holding oil is inhibited. Accordingly, by mixing an emulsion of a liquid oil component (for example, mineral oil) with an emulsion of a hydrated oil agent, a necessary amount of the liquid oil component can be used while enjoying the effect of the lyotropic spherical liquid crystal. .

  The present invention also relates to a liquid lyotropic oil phase liquid crystal containing a hydrated oil of particles of a polycondensation polymer having closed vesicles and / or hydroxyl groups formed by amphiphiles that spontaneously form closed vesicles. Also includes use for spheronization.

<Example 1>
To 139.0 g of water, 1.0 g of lecithin was added and stirred. 100 g of this stirring solution was heated to 80 ° C., 40 g of warm water was added, and 60 g of cetanol at 80 ° C. was further added. This liquid was stirred with a homomixer at 6000 rpm, 80 ° C. for 10 minutes to carry out emulsification. Thereafter, the mixture was allowed to cool for 15 minutes, and further cooled to 35 ° C. with water to prepare an emulsion.

  FIG. 1 is an all-optical micrograph (a) in the same visual field (magnification 200 times) and a polarized light micrograph (b) in the same visual field of the emulsion prepared in this example. In (a), most of the inner phase observed in a circular cross section shows black crossed Nicols in (b), and it is recognized that lyotropic spherical liquid crystals are formed. In the inner phase having a cross-sectional major axis of 1.0 μm or more, the ratio of the oil phase in the state of lyotropic spherical liquid crystal was 93%. Moreover, about the said emulsion, the average particle diameter computed with the laser diffraction scattering type particle size distribution analyzer (Shimadzu Corporation SALD2100) was 10 micrometers.

<Example 2>
An emulsified product was prepared in the same manner as in Example 1 except that the emulsification was allowed to stand at 70 ° C. for 5 minutes without using a homomixer.

  FIG. 2 is an all-optical micrograph (a) in the same visual field (magnification 200 times) and a polarized light micrograph (b) in the same visual field of the emulsion prepared in this example. A part of the inner phase observed in a circular cross section in (a) shows black crossed Nicols in (b), and it is recognized that a lyotropic spherical liquid crystal is formed. In the inner phase having a cross-sectional major axis of 1.0 μm or more, the ratio of the oil phase in the lyotropic spherical liquid crystal state was 92%. Moreover, about the said emulsion, the average particle diameter computed with the laser diffraction scattering type particle size distribution analyzer (Shimadzu Corporation SALD2100) was 1 micrometer.

(Comparative example)
To 139.9 g of water at 80 ° C., 0.1 g of Alcacylan was added and stirred. To 100 g of this stirring solution, 60 g of cetanol at 80 ° C. was added. This liquid was stirred with a homomixer at 6000 rpm and 80 ° C. for 5 minutes for emulsification. Thereafter, the mixture was cooled to 40 ° C. over 10 minutes while stirring at 4000 rpm, and further water-cooled to 25 ° C. to prepare an emulsion.

  FIG. 3 is an all-optical micrograph (a) in the same visual field (magnification 200 times) and a polarized light micrograph (b) in the same visual field of the emulsion prepared in this comparative example. In (a), the inner phase itself separated from the outer phase was not observed so much, and in (b), black crossed Nicols were not confirmed. From this, it can be seen that in this comparative example, particles of the polycondensation polymer were not formed, and as a result, the lyotropic spherical liquid crystal formation of the water hydrated oil did not occur.

[Evaluation]
6 panellas were allowed to apply about 0.5 g of each emulsion to the skin of the inner part of the forearm, and evaluated at that time and afterwards in 3 stages (○: good, △: normal, ×: bad) It was. The results are shown in Table 1.

  Moreover, about 0.5 g of each emulsion was applied to the hair to each of the panelists described above, and the feeling of use at that time and thereafter was evaluated. The results were the same as in Table 1.

  From the above results, the so-called three-phase emulsification forms the lyotropic spherical liquid crystal in the internal phase, and the properties of the emulsion (especially moist on the skin and hair when used in cosmetics) It was found that the feeling, film feeling, skin texture, etc.) can be improved. In particular, by sufficiently forming closed vesicles or polycondensation polymer particles that contribute to three-phase emulsification, an internal phase having a large particle diameter can be formed, thereby improving the above-described characteristics and improving It was also found that the spread (goodness of elongation) improved dramatically.

<Example 3>
An emulsion was prepared in the same procedure as in Example 1 except that the cooling after the emulsion formation was performed by cooling with water while stirring all the steps without cooling. FIG. 4 is an all-optical micrograph (a) in the same visual field (magnification 200 times) and a polarized light micrograph (b) in the same visual field of the emulsion prepared in this example. A part of the inner phase observed in a circular cross section in (a) shows black crossed Nicols in (b), and it is recognized that a lyotropic spherical liquid crystal is formed. The ratio of the emulsified inner phase itself is small, and the ratio of the oil phase in the lyotropic spherical liquid crystal state is only 30% in the inner phase having a cross-sectional major axis of 1.0 μm or more. From this, it was found that gradually cooling after the emulsion formation is important for emulsification and formation of lyotropic spherical liquid crystals. Table 2 shows the results of evaluating the prepared emulsion in the same procedure as in Example 1.

<Examples 4 to 6>
In Example 4, the amount of water was 159.0 g and the amount of cetanol was 40 g. In Example 5, the amount of water was 179.0 g, and the amount of cetanol was 20 g. An emulsion was prepared by the procedure. In Example 6, an emulsion was prepared in the same procedure as in Example 1 except that stearyl alcohol was used instead of cetanol. Table 2 shows the results of evaluating the prepared emulsion in the same procedure as in Example 1.

  FIGS. 5-7 is the all-optical micrograph (a) in the same visual field (200-times multiplication factor) of the emulsion prepared in Examples 4-6, respectively, and the polarization micrograph (b) in the same visual field. In any of FIGS. 5 to 7, most of the inner phase observed in a circular cross section in (a) shows black crossed Nicols in (b), and it is recognized that lyotropic spherical liquid crystals are formed. In the inner phase having a cross-sectional major axis of 1.0 μm or more, the ratio of the oil phase in the lyotropic spherical liquid crystal state was 90% in Examples 4 and 5, and 91% in Example 6. Moreover, about the said emulsion, the average particle diameter computed with the laser diffraction scattering type particle size distribution analyzer (Shimadzu Corporation SALD2100) was 5 micrometers in Example 4 and 5, and was 10 micrometers in Example 6.

  From the comparison of Examples 1 and 3, in the internal phase having a cross-sectional major axis of 1.0 μm or more, the ratio of the oil phase in the state of lyotropic spherical liquid crystals is high, so that smoothness, good elongation, film feeling, skin feel It was found that the characteristics such as texture can be further improved.

  From Example 6, it was found that although cetanol is preferable, various water hydrating oils can be used in the present invention. Further, from the comparison of Examples 1, 4 and 5, the large amount of the water-holding oil can improve properties such as moist feeling and skin texture, and more than 10% with respect to the emulsion. It was found that the film feeling can be further improved.

Claims (18)

  The inner phase is an oil phase that contains a water hydrated oil and is at least partially in the form of lyotropic spherical liquid crystals, and the outer phase is an aqueous phase, closed by an amphiphile that spontaneously forms closed vesicles. An emulsion containing an O / W emulsion containing particles of a polycondensation polymer having an endoplasmic reticulum or a hydroxyl group.   The emulsion according to claim 1, wherein the O / W emulsion maintains an emulsified state by interposing the closed vesicles and / or the particles at an interface between the aqueous phase and the oil phase.   The emulsion of Claim 2 which implement | achieved the fluid state at room temperature by the said closed endoplasmic reticulum and / or the said particle | grain interposing in the interface of the said water phase and the said oil phase.   The emulsion according to any one of claims 1 to 3, which is used in a cosmetic applied to skin or hair.   The emulsion according to any one of claims 1 to 4, wherein an average particle size of the inner phase is 1.0 µm or more.   The emulsion according to any one of claims 1 to 5, wherein a ratio of the oil phase in a lyotropic spherical liquid crystal state is 80% or more in the inner phase having a cross-sectional major axis of 1.0 µm or more.   The emulsion according to any one of claims 1 to 6, which contains a liquid oil component in an amount of less than 10% by mass with respect to the emulsion separately from the hydrated oil.   The emulsified product according to any one of claims 1 to 7, wherein a blending amount of the water-holding oil is more than 10% by mass with respect to the emulsified product.   The emulsified product according to any one of claims 1 to 8, wherein the hydrated oil agent contains a higher alcohol.   A cosmetic comprising the emulsion according to claim 1 and applied to skin or hair. A bilayer membrane of an amphiphile is dispersed in water, or a polycondensation polymer having a hydroxyl group is made into single particles in water, and the closed vesicle formed of the amphiphile or the polycondensation polymer Forming an emulsifier dispersion containing particles;
A step of forming an O / W emulsion by mixing the emulsifier dispersion and an oil agent containing a water-holding oil agent at a temperature equal to or higher than the melting point of the water-holding oil agent.   The method for producing an emulsion according to claim 11, wherein, in the step of forming the O / W emulsion, a liquid oil component containing less than 10% by mass relative to the emulsion is used as the oil agent in addition to the water-holding oil agent. .   The method for producing an emulsion according to claim 11 or 12, wherein in the step of forming the O / W emulsion, a blending amount of the water-containing oil agent is more than 10% by mass with respect to the emulsion.   The method for producing an emulsion according to any one of claims 11 to 13, wherein the closed vesicles or the particles in the emulsifier dispersion exhibit an average particle diameter of 8 nm or more and 800 nm or less.   The manufacturing method of cosmetics which has the process of processing the emulsion manufactured by the method in any one of Claim 11 to 14 into cosmetics.   The method for producing a cosmetic according to claim 15, wherein the processing step includes a step of diluting the emulsion with water.   The method for producing a cosmetic according to claim 15 or 16, wherein the processing step includes a step of adding an emulsion of a liquid oil component to the emulsion.   Use of particles of polycondensation polymers having closed vesicles and / or hydroxyl groups formed by amphiphiles that spontaneously form closed vesicles in the lyotropic spheroidization of liquid crystals of the oil phase containing a hydrated oil agent.