KR102589703B1 - Method for manufacturing interface emulsification ability-reinforced composite emulsion composition for ultra-high-density nano particles and a cosmetic composition including ultra-high-density nano particles manufactured thereby - Google Patents

Abstract

The present invention relates to particles comprising an anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant as components for emulsifying two or more liquids, a dispersed phase containing the components, and a continuous layer surrounding the dispersed phase. It relates to an emulsion formulation containing a phase, wherein the anionic surfactant and the amphoteric surfactant adjust the physical distance between the surfactants at the outer interface of the dispersed phase particles, improving the integrity of the dispersed phase particles, and the first nonionic surfactant It improves the stability of the dispersed phase particles by relaxing the interface through a combination of surfactants at the inner interface of the dispersed phase particles, and is used in emulsion formulations containing dispersed phase particles with a higher density and smaller and uniform size, and cosmetic compositions and skin containing the same. A composition for external use is provided.

Description

Method for manufacturing interface emulsification ability-reinforced composite emulsion composition for ultra-high-density nanoparticles and cosmetic composition containing ultra-high-density nanoparticles produced thereby nano particles and a cosmetic composition including ultra-high-density nano particles manufactured thereby}

The present invention relates to particles comprising an anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant as components for emulsifying two or more liquids, a dispersed phase containing the components, and a continuous layer surrounding the dispersed phase. It relates to an emulsion formulation comprising a phase.

Emulsification refers to a phenomenon in which one liquid among two immiscible liquids is dispersed in the form of fine particles in the other liquid, and a mixture in this state is called an emulsion.

Depending on the dispersion type, oil-in-water type (hydrophilic emulsion, Oil in Water, O/W type), water-in-oil type (lipophilic emulsion, Water in Oil, W/O type), multiple type (multiple emulsion, O/W/ Type O or W/O/W).

The size of particles in an emulsion generally has a size distribution of several nm to several tens of ㎛, and microemulsions with a size distribution of several ㎛ to several tens of ㎛ are thermodynamically unstable and are subject to flocculation, sedimentation, and corrosion. It has a tendency to separate through various pathways such as creaming, Ostwald ripening, and coalescence, and thus has low stability.

A liquid-liquid dispersion system in which the average diameter of the particles of the dispersed phase is 20 to 500 nm is called a nano emulsion, and when the size of the particles of the dispersed phase decreases to nano size, the emulsion changes in kinetic terms due to Brownian motion between particles. The stability of the product can be greatly improved, and the small particle size has the advantage of effectively delivering active ingredients to the skin.

Nanotechnology is a technology with great potential in the cosmetics market and is widely used in the industrial field. In the field of cosmetics manufacturing, nanotechnology is being applied to improve the delivery performance of effective substances by controlling the size of the structure that plays a role in delivering effective ingredients into the skin to be smaller than the size of the cells that make up the skin. In addition, by forming the structure in the form of a multi-layer liquid crystal film similar to the lipid structure of the skin, effective ingredients that are vulnerable to external environments such as air, moisture, light, and temperature can be more stabilized, and the skin delivery effect can also be improved.

Accordingly, interest in nanoemulsion technology is increasing, and recently, a high-pressure emulsification method that provides strong shear force by adjusting ultra-high pressure within an emulsifier, or a composition consisting of a three-component system of water, oil, and nonionic surfactant As the temperature rises, the hydrogen bond between ethylene oxide, the hydrophilic group of the nonionic surfactant, and water decreases, and the inversion temperature emulsification method, which uses the principle that the hydrophilic nature decreases, is being applied to nanoemulsion manufacturing technology.

The use of an emulsifier is essential in emulsion formulations, and the selection and content control of the emulsifier used to maintain appropriate viscosity and form a stable emulsion without separation phenomena such as coalescence or agglomeration by combining the oil phase and aqueous phase components with each other is also important. More importantly, the selection and content control of the emulsifier are more important in order to achieve the stability of nanoemulsions with small particle sizes. However, the technology for realizing the size of the dispersed phase particles and the stability of the emulsion formulation has not been accurately identified.

Under this background, there is a need for an emulsion formulation in which the dispersed phase particles are small, uniform, high density, and stable in nano size through a combination of emulsifiers.

Korean registered patent 10-1827486

One aspect is to provide particles comprising an anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant as ingredients for emulsifying two or more liquids.

Another aspect includes a dispersed phase comprising an anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant, and comprising a second nonionic surfactant; and a continuous phase surrounding the dispersed phase.

Another aspect is to provide a cosmetic composition comprising the emulsion formulation.

Another aspect is to provide a composition for external skin application containing the emulsion preparation.

One aspect provides particles comprising an anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant as ingredients for emulsifying two or more liquids.

In one embodiment, the anionic surfactant and the amphoteric surfactant improve the integrity of the particle by controlling the physical distance between the surfactant at the outer interface of the particle, and the first nonionic surfactant is the first nonionic surfactant of the particle. The safety of the particles may be improved by relaxing the interface through a combination of surfactants at the inner interface.

The anionic surfactant and the amphoteric surfactant may improve the integrity of the particle by making the physical bond distance between the surfactant at the outer interface closer and forming the particle size smaller.

More specifically, when the anionic surfactant approaches the amphoteric surfactant, the adjacent surface of the amphoteric surfactant is charged with a partial positive charge, and an attractive force acts due to electrostatic interaction with the anionic surfactant. The physical bond distance between the surfactants at the outer interface may be adjusted to improve particle integrity.

In one embodiment, the anionic surfactant and the amphoteric surfactant may enhance the emulsifying ability of the outer interface of the particle, and the first nonionic surfactant may enhance the emulsifying ability of the inner interface of the particle.

Strengthening the emulsifying ability of the outer interface may be achieved by controlling the physical bond distance between the anionic surfactant and the amphoteric surfactant at the outer interface of the particle, thereby improving the integrity of the particle.

Strengthening the emulsifying ability of the inner interface may be that the first nonionic surfactant improves the stability of the particle by relaxing the interface through a combination of various surfactants at the inner interface of the particle.

The interface may refer to an interface between two or more substances, liquids, liquid phases, or continuous phases.

The emulsification ability may mean the ability to mix two or more immiscible substances, liquids, liquid phases, or continuous phases, and to disperse and contain one or more dispersed phases without being separated in one or more continuous phases.

The enhanced emulsification ability may mean that the dispersed phase particles are stabilized without being separated from the continuous phase even at a smaller size. Depending on the enhanced emulsification ability, the size of the dispersed phase particles may be 50 nm to 100 nm.

Strengthening the emulsifying ability of the interface may mean having the effect of strengthening the emulsifying ability by relaxing the boundary of the interface.

Another aspect includes a dispersed phase comprising an anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant, and comprising a second nonionic surfactant; and a continuous phase surrounding the dispersed phase.

The emulsion formulation may refer to a formulation in which two or more immiscible liquids are dispersed in one or more continuous phases as one or more dispersed phases through an emulsifier (for example, a surfactant), an emulsifying aid, etc.

The interface, emulsifying ability, emulsifying ability strengthening, and emulsifying ability strengthening of the interface are the same as mentioned above.

The emulsion formulation may be an oil-in-water emulsion (O/W (oil-in-water) emulsion) formulation, a water-in-oil emulsion (W/O (water-in-oil) emulsion) formulation, or a multiple emulsion (W/O/W) formulation. (water-in-oil-in-water) emulsion, O/W/O (oil-in-water-in-oil) emulsion, or multiple emulsion).

In an oil-in-water emulsion, an aqueous component may be contained on the outside of the dispersed phase particles and an oily component may be contained on the inside, and in a water-in-oil emulsion, an oily component may be contained on the outside of the dispersed phase particles and an aqueous component may be contained on the inside. In a medium-sized emulsion, the dispersed phase particles may contain an aqueous or oil-based component on the outside and an oil-based or aqueous component on the inside.

In one embodiment, the anionic surfactant and the amphoteric surfactant improve the integrity of the sprayed particles by controlling the physical distance between the surfactants at the outer interface of the dispersed phase particles, and the first nonionic surfactant may improve the safety of the dispersed phase particles by relaxing the interface through a combination of surfactants at the inner interface of the dispersed phase particles.

The anionic surfactant and the amphoteric surfactant may improve the integrity of the sprayed particles by making the physical bonding distance between the surfactants at the outer interface closer, thereby forming the dispersed phase particles into a smaller size.

More specifically, when the anionic surfactant approaches the amphoteric surfactant, the adjacent surface of the amphoteric surfactant is charged with a partial positive charge, and an attractive force acts on the amphoteric surfactant through electrostatic interaction with the anionic surfactant. The physical bond distance between the surfactants at the outer interface may be adjusted to improve the integrity of the dispersed phase particles.

Strengthening the emulsifying ability of the inner interface may be that the first nonionic surfactant improves the stability of the dispersed phase particles by relaxing the interface through a combination of various surfactants at the inner interface of the dispersed phase particles.

In one embodiment, the anionic surfactant and the amphoteric surfactant may enhance the emulsifying ability of the outer interface of the dispersed phase.

Strengthening the emulsifying ability of the outer interface of the dispersed phase may be achieved by controlling the physical bond distance between the anionic surfactant and the amphoteric surfactant at the outer interface of the dispersed phase particles, thereby improving the integrity of the dispersed phase particles.

Specifically, the anionic surfactant and the amphoteric surfactant may increase density by increasing the physical bond distance on the outside of the emulsifier located at the interface of the dispersed phase (e.g., the portion in contact with the continuous phase component). . By increasing the density, dispersed phase particles with high density, smaller and more uniform sizes can be formed with high stability.

In one embodiment, the first nonionic surfactant may enhance the emulsifying ability of the inner interface of the dispersed phase.

Strengthening the emulsifying ability of the inner interface of the dispersed phase may be that the first nonionic surfactant improves the stability of the dispersed phase particles by relaxing the interface through a combination of various surfactants at the inner interface of the dispersed phase particles.

More specifically, the first nonionic surfactant may relax the interface inside the emulsifier located at the interface of the dispersed phase (for example, the part in contact with the dispersed phase component) to improve the safety of the dispersed phase particles and increase density. there is. By increasing the density, dispersed phase particles with high density, smaller and more uniform sizes can be formed with high stability.

In one embodiment, the emulsion formulation may include the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant.

More specifically, the emulsion formulation includes a dispersed phase comprising an anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant, and a second nonionic surfactant; And it may be an emulsion formulation comprising a continuous phase surrounding the dispersed phase.

In one embodiment, the anionic surfactant and the amphoteric surfactant may enhance the emulsifying ability of the outer interface of the dispersed phase, and the first nonionic surfactant may enhance the emulsifying ability of the inner interface of the dispersed phase, The anionic surfactant and the amphoteric surfactant increase the density of the outside of the emulsifier located at the interface of the dispersed phase (for example, the portion in contact with the continuous phase component), so that the first nonionic surfactant is used in the dispersed phase. By increasing the density of the inside of the emulsifier located at the interface (for example, the part in contact with the dispersed phase component), dispersed phase particles with higher density and smaller and more uniform sizes can be formed with high stability.

In one embodiment, the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant are administered to two or more liquids and an emulsion formulation containing dispersed phase particles, which are ultra-highly concentrated particles, is formed through a high-temperature vacuum emulsification step. Through the second concentration step, an emulsion formulation containing ultra-high density nanoparticles of the dispersed phase with smaller particle size and increased density can be formed. One or more of the liquids may be highly concentrated liquids through a primary concentration step prior to the high-temperature vacuum emulsification step.

The primary concentration step, high-temperature vacuum emulsification step, and secondary concentration step will be described in detail in the emulsion production method below.

In one embodiment, the dispersed phase particles may have a diameter of 50 to 100 nm. More specifically, the diameter of the dispersed phase particles is 50 to 100 nm, 55 to 70 nm, 70 to 100 nm, 45 to 60 nm, 65 to 90 nm, 50 to 90 nm, 50 to 80 nm, 50 to 70 nm, 50 to 65 nm, 50 to 60 nm, 45 to 100nm, 45 to 90nm, 45 to 80nm, 45 to 70nm, 45 to 65nm, 45 to 55nm, 45 to 50nm, 55 to 100nm, 55 to 65nm, 55 to 60nm, 55 to 50nm, 60 to 100nm, 60 to 60nm It may be 90 nm, 60 to 70 nm, 60 to 65 nm, 65 to 100 nm, 65 to 80 nm, 65 to 70 nm, 70 to 90 nm, or 70 to 80 nm.

According to one embodiment, in the emulsion formulation, the anionic surfactant and the amphoteric surfactant enhance the emulsifying ability of the outer interface of the dispersed phase, and the first nonionic surfactant enhances the emulsifying ability of the inner interface of the dispersed phase. strengthening, and the second nonionic surfactant is an emulsifier, and may be an emulsion formulation.

In one embodiment, the surfactant relaxes the interface of two or more substances, liquids, liquid phases, or continuous phases to mix immiscible liquids, and is dispersed without separation in one or more continuous phases as one or more dispersed phases. It may be a compound that makes it possible or emulsifies it.

The surfactant may include, but is not limited to, one or more selected from the group consisting of cationic surfactants, anionic surfactants, amphoteric surfactants, nonionic surfactants, and saponified surfactants.

In one embodiment, the anionic surfactant may refer to a surfactant containing an anionic functional group that can act as an acid within one molecule.

The anionic surfactants include sodium stearoyl glutamate, sodium cocoyl sarcosinate, potassium cetyl phosphate, sodium laureth sulfate, disodium laureth sulfosuccinate, sodium lauryl sulfate, ammonium laureth sulfate, and ammonium lauryl sulfate. , Sodium C14-16 Olefin Sulfonate, Potassium Cocoyl Glycinate and Sodium Cocoyl Isethionate, Sodium Methyl Cocoyl Taurate, Alkyl Phosphate, Alkyl Taurate, Sulfosuccinate, Alkyl Sulfate, Sarcosinate. , alkyl ether sulfate, isethionate, alkyl ether carboxylate, sodium lauryl sulfate, ammonium lauryl sulfate, magnesium lauryl sulfate, triethanolamine lauryl sulfate, sodium polyoxyethylene lauryl sulfate and ammonium polyoxyethylene lauryl sulfate. It may be one or more selected from the group consisting of, but is not limited to, sodium stearoyl glutamate, sodium cocoyl sarcosinate, potassium cetyl phosphate, or a combination thereof.

In one embodiment, the anionic surfactant may be included in an amount of 0.01 to 1% by weight based on the total weight of the emulsion formulation. Specifically, the anionic surfactant is used in an amount of 0.01 to 1% by weight, 0.1 to 0.4% by weight, 0.01 to 0.7% by weight, 0.01 to 0.5% by weight, 0.01 to 0.4% by weight, 0.01 to 0.3% by weight, 0.01 to 0.01% by weight, based on the total weight of the emulsion formulation. 0.2% by weight, 0.01 to 0.1% by weight, 0.05 to 1% by weight, 0.05 to 0.7% by weight, 0.05 to 0.5% by weight, 0.05 to 0.4% by weight, 0.05 to 0.3% by weight, 0.05 to 0.2% by weight, 0.05 to 0.1% by weight %, 0.1 to 1% by weight, 0.1 to 0.7% by weight, 0.1 to 0.5% by weight, 0.1 to 0.3% by weight, 0.1 to 0.2% by weight, 0.2% by weight, 0.2 to 1% by weight, 0.2 to 0.7% by weight, 0.2 to 0.5% by weight, 0.2 to 0.4% by weight, 0.2 to 0.3% by weight, 0.2% by weight, 0.2 to 1% by weight, 0.2 to 0.7% by weight, 0.2 to 0.5% by weight, 0.2 to 0.4% by weight, 0.2 to 0.3% by weight, 0.3% by weight, 0.3 to 1% by weight, 0.3 to 0.5% by weight, 0.3 to 0.4% by weight, 0.4% by weight, 0.4 to 1% by weight, 0.4 to 0.5% by weight, 0.5 to 1% by weight or 0.5 to 0.7% by weight. may be included.

In one embodiment, the amphoteric surfactant may refer to a surfactant containing a cationic functional group and an anionic functional group that can act as both an acid and a base in one molecule.

The amphoteric surfactants include cocobetaine, sodium cocoamphoacetate, disodium cocoamphodiacetate, lauramidopropyl betaine, cocamidopropyl betaine, and 2-heptadecyl-N-carboxymethyl-N-hydroxyethyl. Midazolinium Betaine, Lauryldimethylamino Acetic Acid Betaine, Alkyl Betaine, Amide Betaine, Sulfobetaine Lauryl Hydroxulsteine, 2-Undecyl-N,N,N-(Hydroxyethylcarboxymethyl) It may be one or more selected from the group consisting of -2-imidazoline sodium and 2-cocoyl-2-imidazolinium hydroxide-1-carboxyethyloxy disodium, but is not limited thereto, and is preferably It may be cocobetaine, sodium cocoamphoacetate, or a combination thereof.

The amphoteric surfactant may be included in an amount of 0.01 to 0.5% by weight based on the total weight of the emulsion formulation. Specifically, the amphoteric surfactant is 0.01 to 0.5% by weight, 0.03 to 0.1% by weight, 0.01 to 0.3% by weight, 0.01 to 0.1% by weight, 0.01 to 0.05% by weight, 0.02 to 0.5% by weight, 0.02 to 0.02% by weight, based on the total weight of the emulsion preparation. 0.3% by weight, 0.02 to 0.1% by weight, 0.02 to 0.05% by weight, 0.03 to 0.5% by weight, 0.03 to 0.3% by weight, 0.03 to 0.05% by weight, 0.05% by weight, 0.05 to 0.5% by weight, 0.05 to 0.3% by weight, It may be included in 0.05 to 0.1% by weight, 0.1 to 0.5% by weight, 0.1 to 0.3% by weight, 0.2 to 0.5% by weight, 0.2 to 0.3% by weight, or 0.3 to 0.5% by weight.

In one embodiment, the nonionic surfactant may refer to a surfactant containing a hydrophilic functional group and a hydrophobic functional group that does not dissociate into ions within the molecule.

In the present invention, the nonionic surfactant includes a first nonionic surfactant and a second nonionic surfactant.

The first nonionic surfactant may enhance the emulsifying ability of the inner interface of the dispersed phase in the emulsion formulation. Specifically, the first nonionic surfactant may be used to strengthen the emulsifying ability of the inner interface of the dispersed phase in the emulsion formulation. This may be to increase the density of the part that is in contact with. The second nonionic surfactant may function as an emulsifier in the emulsion formulation.

In the production of an emulsion formulation, the first nonionic surfactant may be added together with the anionic surfactant and the amphoteric surfactant, and the second nonionic surfactant may be added in addition to the first nonionic surfactant. It may be added as an emulsifier or emulsifying ingredient in an emulsion preparation.

The first nonionic surfactant may be added in the water phase or oil phase production step in emulsion production, or may be added in the high temperature vacuum emulsification step, and the second nonionic surfactant may be added in the water phase or oil phase production step in emulsion production. It may be added to the step, or it may be added to the first concentration step before the high-temperature vacuum emulsification step. However, it is not limited to this.

The first nonionic surfactant may be added by mixing with the anionic surfactant and the amphoteric surfactant in the process of emulsifying the dispersed phase and the continuous phase containing the second nonionic surfactant.

The nonionic surfactants include polyglyceryl-2 sesquiisostearate, polyglyceryl-4 isostearate, glyceryl stearate, lauryl glucoside, decyl glucoside and coco-glucoside, and PEG-40 hydrogenated caster. Oil, cocamide methyl MEA, polyethylene glycol monostearate, PEG-100 stearate, PEG-40 stearate, PEG-20 stearate, PEG-60 hydrogenated castor oil, PEG- 40 Hydrogenated castor oil, polysorbate 60, polyglyceryl-4 caprate, cetearyl olivate, sorbitan olivate, cetearyl alcohol, behenyl alcohol, batyl alcohol, arachidyl alcohol, myristyl alcohol , C14-22 Alcohol, Butyl Glucoside, C10-16 Alkyl Glucoside, C12-18 Alkyl Glucoside, C12-20 Alkyl Glucoside, Caprylyl Glucoside, Caprylyl/Capryl Glucoside, Octyldodecyl Glucoside, Arachidyl Glucoside, La Uryl dimethyl amine oxide, palm oil alkyl dimethyl amine oxide, lauric acid diethanol amide, palm oil fatty acid diethanol amide, palm oil fatty acid monoethanol amide, polyoxyethylene lauryl ether, polyoxyethylene nonylphenyl ether, octyldodeceth-16, sorbate It may be one or more selected from the group consisting of sorbitan sesquioleate, sorbitan tristearate, sorbitan monooleate, sorbitan monostearate, and diethylene glycol monolaurate, but is not limited thereto, Preferably, the first nonionic surfactant may be polyglyceryl-2 sesquiisostearate, polyglyceryl-4 isostearate, glyceryl stearate, or a combination thereof.

The first nonionic surfactant may be included in an amount of 0.01 to 0.5% by weight based on the total weight of the emulsion formulation. Specifically, the first nonionic surfactant is 0.01 to 0.5% by weight, 0.05 to 0.2% by weight, 0.01 to 0.3% by weight, 0.01 to 0.2% by weight, 0.01 to 0.1% by weight, 0.02 to 0.5% by weight, based on the total weight of the emulsion formulation. 0.02 to 0.3% by weight, 0.02 to 0.2% by weight, 0.02 to 0.1% by weight, 0.03 to 0.5% by weight, 0.03 to 0.3% by weight, 0.03 to 0.2% by weight, 0.03 to 0.1% by weight, 0.05% by weight, 0.05 to 0.5% by weight %, 0.05 to 0.3% by weight, 0.05 to 0.1% by weight, 0.1% by weight, 0.1 to 0.5% by weight, 0.1 to 0.3% by weight, 0.1 to 0.2% by weight, 0.2 to 0.5% by weight, 0.2 to 0.3% by weight or 0.3 to 0.3% by weight. It may be included at 0.5% by weight.

In one embodiment, the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant may be included in the emulsion formulation at a weight ratio of 4:0.5 to 2:1 to 3. Specifically, the anionic surfactant and the first nonionic surfactant have a weight ratio of 4:0.5 to 2:1 to 3, a weight ratio of 4:1:2, 4 : weight ratio of 0.5:2, weight ratio of 4:2:2, weight ratio of 4:1:1, weight ratio of 4:1:3, weight ratio of 4:0.5 to 1:1 to 3, 4:0.5 to 1:1 Weight ratio of 4:0.5 to 1:2 to 3, 4:1 to 2:1 to 3, 4:1 to 2:1 to 2, 4:1 to 2:2 to 3 It may be included in the emulsion formulation at a weight ratio of 4:0.5 to 2:1 to 2, or a weight ratio of 4:0.5 to 2:2 to 3.

By including the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant in the above weight ratio in the emulsion formulation, dispersed particles with high density and smaller, uniform sizes can be formed with high stability.

For example, if the amphoteric surfactant is included in less than the above weight ratio, the effect of strengthening the emulsification ability of the outer interface of the dispersed phase particles (e.g., the part in contact with the continuous phase component) is weak, and the stability of the dispersed phase particles may decrease. . For example, in oil-in-water emulsion formulations, the oily components inside the dispersed phase particles may be discharged to the outside of the particles or the high temperature long-term stability may decrease. If the amphoteric surfactant is included in more than the above weight ratio, the hardness may increase over time or a gelling phenomenon may occur due to the excessive amount of emulsifier.

Also, as an example, if the first nonionic surfactant is included in less than the above weight ratio, the effect of strengthening the emulsification ability of the inner interface of the dispersed phase particles (for example, the part in contact with the dispersed phase component) may be weak, and the stability of the dispersed phase particles may decrease. there is. For example, in oil-in-water emulsion formulations, the oily components inside the dispersed phase particles may be discharged to the outside of the particles or the long-term stability at high temperatures may decrease. If the first nonionic surfactant is included in more than the above weight ratio, the hardness may increase over time or a gelling phenomenon may occur due to the excessive amount of emulsifier.

Another aspect is to provide a method for preparing the emulsion formulation.

The method of preparing the emulsion formulation includes mixing the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant at high temperature and vacuum in the process of emulsifying the dispersed phase and the continuous phase containing the second nonionic surfactant. It may be manufactured by emulsifying under the following conditions.

In one embodiment, the manufacturing method includes preparing an aqueous phase part; Primary concentration step; High temperature vacuum emulsification step; And it may include a secondary concentration step.

Specifically, each of the above steps may be as follows.

The step of preparing the aqueous phase may be performed by mixing components constituting the aqueous phase (e.g., purified water, etc.). Specifically, the components constituting the water phase can be mixed in a vacuum emulsification tank capable of temperature control and stirring, and then heated to dissolve and homogenize each component. At this time, the heating temperature may be 60 to 90°C, specifically 70 to 85°C, but is not limited thereto.

The aqueous phase may further include polyol. Polyols can act as humectants, specifically, supplying or maintaining moisture in the skin. For example, polyols are from the group consisting of glycerin, butylene glycol, propanediol, dipropylene glycol, and pentylene glycol. It may include one or more selected types, but is not limited thereto.

The aqueous phase may contain 0.01 to 30% by weight of polyol, and specifically 10 to 20% by weight. If the water phase contains less than 5% by weight of polyol based on the total weight of the composition, the moisturizing power may be reduced, and if the polyol contains more than 30% by weight of the total weight of the composition, the feeling of use may be reduced, such as providing a slippery and sticky feeling. You can.

The aqueous phase may further include a thickener. The thickener can play a role in stably forming the formulation of the composition while stably controlling the viscosity. For example, thickeners include Carbomer, Poloxamer, Xanthan Gum, Caprylic/Capric Triglyceride*Polyurethane-11, Mannan, and Gellan Gum. Gum), Carrageenan, Ceratonia Siliqua (Carob) Gum and Hydroxyethylcellulose, Acrylates/C10-30 Alkyl Acrylate Crosspolymer and Acrylic It may include one or more selected from the group consisting of Ammonium Acryloyldimethyltaurate/VP Copolymer, etc., but is not limited thereto.

In one embodiment, the aqueous phase may contain a thickener in an amount of 0.01 to 2.0% by weight, specifically 0.2 to 1.0% by weight, based on the total weight of the composition. If the water phase contains less than 0.01% by weight of the thickener based on the total weight of the composition, the formulation stability may be reduced, such as when the viscosity is not properly formed or phase separation occurs, and if the thickener is included in an amount exceeding 2.0% by weight based on the total weight of the composition, the viscosity may not be properly formed or phase separation may occur. If it is included, the feeling of use may be reduced, such as providing a thick and sticky feeling, or emulsification with the oily part may not occur.

In one embodiment, the first concentrating step may be performed by concentrating the oil phase containing lipids and amphipathic components (eg, surfactants). Specifically, the first concentrating step includes preparing the oil phase portion by mixing the components constituting the oil phase portion; and compressing the oil phase portion.

Specifically, in the step of preparing the oil phase, the components constituting the oil phase (for example, lipids, amphiphilic components, or emulsifiers, etc.) are mixed in an oil phase dissolution tank capable of temperature control and stirring, and then heated to dissolve each component. Can be dissolved and homogenized. At this time, the heating temperature may be 60 to 90°C, specifically 70 to 85°C, but is not limited thereto.

The lipid is a component similar to the component that makes up the skin structure, and can allow the composition and the active ingredients within the composition to effectively penetrate and be delivered to the skin through interaction with intercellular lipids.

In one embodiment, the oily part may contain 0.1 to 15% by weight of the lipid relative to the total weight of the composition, specifically 0.5 to 10% by weight, and more specifically 1 to 3% by weight. can do. If the oil phase contains less than 0.1% by weight of lipids relative to the total weight of the composition, formulation stability may be reduced, such as phase separation, and if lipids are included in excess of 15% by weight relative to the total weight of the composition, excessive hardness may be formed. Ultrafine particles may not be formed or the feeling of use may be reduced.

In one embodiment, the lipid may include a low melting point lipid having a melting point of 55°C or lower. For example, low melting point lipids include Myristyl Myristate, Cetyl Palmitate, Hydrogenated Olive Oil Lauryl Esters, and Astrocaryum murumuru seed butter. ) and shea butter, but is not limited thereto.

In one embodiment, the oil phase may include 0.1 to 7% by weight of low melting point lipid, specifically 0.5 to 5% by weight, and more specifically 1 to 3% by weight, based on the total weight of the composition. It can be included. When the oil phase contains the low melting point lipid within the above content range, ultrafine particles with the most appropriate hardness, viscosity, and size can be formed.

In one embodiment, the lipid may further include one or more waxes selected from vegetable wax, animal wax, mineral wax, and synthetic wax, but is not limited thereto. Specifically, the additionally included lipid may be a wax having a melting point in the range of 50 to 80°C. Waxes with a melting point in the range of 50 to 80°C can improve the stability of ultrafine particles and provide excellent oiliness and moisture retention.

For example, vegetable waxes include Candelilla Wax, Carnauba Wax, Rice Bran Wax, Cotton Wax, Chinese Insect Wax, Sugar Cane Wax, Jojoba Wax, Butyrospermum Parkii (Shea) Butter, Sunflower Wax, Hydrogenated Vegetable Oil and Hydrogenated Olive Oil Stearyl Esters) may include, but are not limited to, one or more types selected from the group consisting of Esters.

For example, animal wax may include, but is not limited to, lanolin, and mineral wax may include ozokerite, ceresin wax, and microcrystalline wax. , multi wax, paraffin wax, etc., but is not limited thereto.

For example, synthetic waxes include polyethylene wax, POE (polyoxyethylene) lanolin alcohol ether wax, POE Lanolin Alcohol Acetate Wax, and POE cholesterol ether wax. (POE Cholesterol Ether Wax), lanolin fatty acid polyethylene glycol wax, and POE hydrogenated lanolin alcohol ether wax, etc. may include one or more selected from the group, but are not limited thereto.

The lipid included in the oil phase may further include one or more lipids selected from C10-C30 higher fatty alcohols and C10-C30 higher fatty acids. Specifically, the lipid may include a higher fatty alcohol of C10-C30. C10-C30 higher fatty alcohols have high solubility in the oil phase, so they can be uniformly dispersed within the oil phase, can be used as an emulsification aid, and can provide a smooth application feeling as they melt on the skin.

Specifically, higher fatty alcohols of C10-C30 include Cetearyl Alcohol, Cetyl Alcohol, Stearyl Alcohol, Cetostearyl Alcohol, and Behenyl Alcohol. ), Lauryl Alcohol, Oleyl Alcohol, Isostearyl Alcohol, Cholesterol, Octyldodecanol, Hexyldecanol, etc. It may include one or more types selected from, but is not limited to this.

Specifically, the higher C10-C30 fatty acids are Lauric Acid, Stearic Acid, Hydroxystearic Acid, Oleic Acid, and Behenic Acid. It may include one or more selected from the group consisting of Acid, Myristic Acid, and Palmitic Acid, but is not limited thereto.

In one embodiment, the amphiphilic component is a material that has both a hydrophilic portion and a lipophilic portion, and the hydrophilic component is oriented outside the core of the particle and the lipophilic portion is oriented inside the core to form stable ultrafine particles. can play a role. Additionally, the amphipathic component can serve to further stabilize the exterior of ultrafine particles with a lipid core.

Specifically, the amphipathic components are Poloxamer 235, Poloxamer 338, Poloxamer 407, Poloxamer 188, bis-(carboxyceramide NP), and Poloxamer. It may include one or more selected from the group consisting of 407 (Bis-(Carboxy Ceramide NP) Poloxamer407) and Polyurethane-15 (Polyurethane-15), but is not limited thereto.

In one embodiment, the oil phase may include an amphiphilic component in an amount of 0.01 to 5.0% by weight, specifically 0.01 to 1.0% by weight, and more specifically 0.1 to 0.5% by weight, based on the total weight of the composition. It can be included. If the oil phase contains less than 0.01% by weight of the amphiphilic component relative to the total weight of the composition, the density of the active ingredient in the particle may be lowered or the stability of the particle may be reduced, and if the amphiphilic component exceeds 5.0% by weight relative to the total weight of the composition, the density of the active ingredient within the particle may decrease or the stability of the particle may be reduced. If included, it may provide a sticky finish and deteriorate the feeling of use.

In one embodiment, the oil phase portion may further include an emulsifier. Emulsifiers can serve to stably disperse the substances constituting the composition within the composition. The emulsifier may include the second nonionic surfactant.

In one embodiment, the emulsifier is Cetearyl Olivate/Sorbitan Olivate, Glyceryl Stearate, PEG-40 Stearate, PEG -100 Stearate (PEG-100 Stearate), PEG-150 Stearate, PEG-40 Distearate, PEG-100 Distearate , PEG-150 Distearate, Cetearyl Olivate, Sorbitan Laurate, Sorbitan Palmitate, Sorbitan Laurate ), Sorbitan Palmitate, Sorbitan Stearate, Sorbitan Olivate, Sorbitan Trioleate, Laureth-4, Laureth-4 23 (Laureth-23), Ceteth-2, Ceteth-10, Ceteth-20, Steareth-2, Steareth- 10, Steareth-20, Oleth-2, Oleth-10, Oleth-20, polyglyceryl -3 Diisostearate (Polyglyceryl-3 Diisostearate) and polyglyceryl-4 oleate (Polyglyceryl-4 Oleate), etc. may include one or more selected from the group, but are not limited thereto.

In one embodiment, the oil phase part may contain an emulsifier in an amount of 0.5 to 10% by weight, specifically 2 to 6% by weight, based on the total weight of the composition. If the oil phase contains less than 0.5% by weight of the emulsifier based on the total weight of the composition, emulsification of the water phase and the oil phase may not occur and an appropriate formulation may not be formed, and if the emulsifier contains more than 10% by weight of the total weight of the composition, If the hardness is excessive, ultrafine particles may not be formed or the feeling of use may be reduced.

In one embodiment, the oil phase portion may further include oil. The oil constitutes the base of the oil phase. For example, the oil may include one or more oils selected from ester oils, vegetable oils, hydrocarbon oils, and silicone oils, but is not limited thereto.

Specifically, ester oils include Caprylic/Capric Triglyceride, ethylhexylstearate, Isopropyl Palmitate, Octyldodecyl Myristate, Isopropyl Myristate, Butyloctyl Salicylate, Coco-Caprylate/Caprate, Hexyl laurate, Dicaprylyl Carbonate carbonate), Diisostearyl malate, Butylene glycol dicaprylate/dicaprate, Decyl Cocoate, Dicaprylyl Carbonate ), Cetylethylhexanoate, Triethylhexanoin, Dicetearyl dimer dilinoleate, Polyglyceryl-2 Triisostearate, and It may include one or more selected from the group consisting of pentaerythrityl tetraisostearate, etc., but is not limited thereto.

Specifically, vegetable oils include Castor Oil, Olive Oil, Jojoba Oil, Persea Gratissima (Avocado) Oil, Macadamia Ternifolia Seed Oil, and Meadow Oil. It may contain one or more types selected from the group consisting of meadowfoam seed oil, etc., and hydrocarbon oils include polybutene, hydrogenated polyisobutene, and mineral oil. , Hydrogenated Polydecene, Squalane, etc., but is not limited thereto.

Specifically, silicone oils include Methylphenyl Polysiloxane, Decamethylcyclopentasiloxane, Methyl Trimethicone, Cyclomethicone, Phenyl Trimethicone, and Dimethicone. It may include one or more types selected from the group consisting of Dimethicone, etc., but is not limited thereto.

In one embodiment, the oil phase may contain 5 to 20% by weight of oil, and specifically 7 to 10% by weight, based on the total weight of the composition. If the oil phase contains less than 5% by weight of oil based on the total weight of the composition, the moisturizing power may be reduced, and if the oil contains more than 20% by weight of the total weight of the composition, the feeling of use may decrease or emulsification of the water phase and the oil phase may occur. You may not lose.

In one embodiment, in the subsequent step of compressing the oil phase, the oil phase may be primarily concentrated by applying pressure to the oil phase in which the components constituting the oil phase are mixed and uniformly dissolved.

Specifically, primary concentration of the oil phase can be performed using a high-pressure emulsifier. A microfluidizer can be used as a high-pressure emulsifier, but it is not limited to this, and any device for high-pressure emulsification commonly used in the industry can be used.

Specifically, the primary concentration of the oil phase may be performed at a temperature of 40 to 60°C and a pressure of 500 to 900 bar, specifically at a temperature of 50 to 60°C and a pressure of 700 to 900 bar, but is limited thereto. That is not the case. When primary concentration is performed under the above temperature and pressure conditions, damage to the active ingredient can be minimized, the possibility of a drop in the titer of the active ingredient and rancidity can be prevented, and the oily phase can be appropriately concentrated.

Specifically, the number of repetitions of the step of compressing the oily phase can be set variously in consideration of the degree of concentration of the oily phase. For example, the step of compressing the oily part may be performed once, but is not limited to this, and may be repeated two or more times depending on the embodiment to which the present invention is applied.

In one embodiment, the high-temperature vacuum emulsification step may be performed by mixing the prepared water phase, the first concentrated oil phase, and the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant. there is.

Specifically, the primary concentrated oil phase and the anionic surfactant, amphoteric surfactant, and first nonionic surfactant are added to the vacuum emulsification tank containing the aqueous phase, and stirred for 1 to 30 minutes to emulsify the aqueous phase and the oil phase. You can. At this time, high-temperature vacuum emulsification of the water phase and the oil phase is performed at a temperature of 60 to 90 ° C. (preferably a temperature of 70 to 85 ° C.), 0.05 MPa to 0.15 MPa (preferably, 0.06 MPa to 0.09 MPa), and 4,000 to 7,000 rpm. It may be performed while maintaining the conditions, but is not limited to this.

Depending on the embodiment, other additional ingredients may be added in the step of preparing the water phase, the first concentration step, or the high temperature vacuum emulsification step. Additional ingredients include, for example, functional ingredients such as stabilizers, thickeners, antioxidants, sunscreens, pigments, fragrances, and preservatives, or effective ingredients that are effective in moisturizing, whitening, improving wrinkles, improving elasticity, improving skin barrier, and skin regeneration. Ingredients may be included, but are not limited thereto. For example, the active ingredients are ethylhexylglycerin, hydroxyacetophenone, vitamin A, vitamin B, vitamin C, vitamin E, vitamin derivatives, collagen, ceramide, peptide, and adenosine. , Arbutin, Hyaluronic Acid, Chondroitin Sulfate, alpha-bisabolol, Guaiazulene, Coenzyme Q10, useful Oil SolubleLicorice (Glycyrrhiza) Extract, Hydroxydecyl Ubiquinone, Betaine, Allantoin, Urea, Niacinamide, Adenosine and Tranek It may include one or more selected from the group consisting of tranexamic acid, etc., but is not limited thereto.

For example, if the additional ingredient is a fat-soluble ingredient, the additional ingredient may be first mixed in the oil phase and then mixed and emulsified with the water phase to stabilize the lipid core. Additionally, for example, if the additional component is a water-soluble component, the additional component may be first mixed in the water phase and then mixed and emulsified with the oil phase to stabilize the lipid core. However, it is not limited to this, and additional ingredients may be added additionally after the oil phase and the water phase are mixed.

In the high-temperature vacuum emulsification step, emulsified dispersed particles may be formed in the water phase. Specifically, emulsified dispersed particles containing active ingredients including lipids, functional ingredients, skin nutritional ingredients, etc. may be formed inside the particles.

In particular, as the oil phase is first concentrated before emulsification, a larger amount of material is filled in the same volume of the particles, allowing the active ingredient to be stably maintained at a high density within the particles.

In addition, in the high-temperature vacuum emulsification step after primary concentration, the anionic surfactant and the amphoteric surfactant can improve the integrity of the particles by controlling the physical distance between the surfactants at the outer interface of the dispersed phase particles. The first nonionic surfactant can improve the safety of the particles by relaxing the interface through a combination of surfactants at the inner interface of the dispersed phase particles. Through this, dispersed phase particles with higher density and smaller and more uniform sizes can be formed with high stability.

In one embodiment, after the high-temperature vacuum emulsification step, a step of stabilizing the emulsified mixture by cooling while stirring may be further included. Specifically, the mixture can be stabilized by stirring the emulsified mixture using a paddle at a temperature of 30 to 50°C. As this stabilizing step is performed, the emulsified particles can be distributed more uniformly and densely within the composition.

In one embodiment, after the high-temperature vacuum emulsification step, the secondary concentration step may be performed by concentrating the emulsified mixture. Specifically, the mixture can be secondary concentrated by adding the high-temperature vacuum emulsified mixture and subjecting it to pressure. For example, secondary concentration of the mixture can be performed using a high-pressure emulsifier. A microfluidizer can be used as a high-pressure emulsifier, but it is not limited to this, and any device for high-pressure emulsification commonly used in the industry can be used.

Specifically, in the secondary concentration step, the emulsified dispersed phase particles generated in the high-temperature vacuum emulsification step are divided to form ultra-high density nano-sized nanoparticles. Specifically, by first concentrating the oil phase and emulsifying it together with the aqueous phase in the high-temperature vacuum state, the dispersed phase particles in which the active ingredient is supported at high density are secondarily concentrated, thereby allowing the dispersed phase particles to be split once more.

Specifically, the ultra-high density nanoparticles may have a particle size of 50 to 100 nm. That is, as the secondary concentration step is performed, hard capsule-like particles with a pore size of about 0.001 to 0.01 may be formed. Particles formed in such a very fine size contain a high density of active ingredients inside, so the particle density is high, hard, and highly stable, enabling effective delivery of the active ingredient into the body and preventing loss of the active ingredient during the delivery process. It can be prevented.

Specifically, the secondary concentration step may be performed at a temperature of 60 to 80°C and a pressure of 1,200 to 1,600 bar, specifically at a temperature of 65 to 75°C and a pressure of 1,300 to 1,500 bar, but is limited thereto. It's not like that. When secondary concentration is performed under the above temperature and pressure conditions, sufficiently broken particles can be obtained.

Specifically, the number of repetitions of the secondary concentration step can be set variously in consideration of the size of the split particles. For example, the secondary concentration step may be repeated two or three times, but is not limited thereto, and may be performed once or repeated four or more times depending on the embodiment to which the present invention is applied.

Specifically, after the secondary concentration step, a step of stabilizing the secondary concentrated mixture by cooling while stirring may be further included. For example, the mixture can be stabilized by stirring the secondary concentrated mixture using a paddle at a temperature of 30 to 45°C. As this stabilizing step is performed, high-density ultrafine particles can be distributed more uniformly and densely within the composition.

In this way, the present invention is a double concentration in which the oil phase is first concentrated, then the first concentrated oil phase and the water phase are emulsified at high temperature and vacuum with the anionic surfactant, amphoteric surfactant, and nonionic surfactant, and then concentrated for the second time. It has the characteristic of using a system. In other words, the present invention using a double concentration system uses the anionic surfactant, amphoteric surfactant, and nonionic surfactant during the emulsification process, compared to the case where concentration is performed a total of once or when concentration is performed a total of two times. By adding an activator and emulsifying it under the high temperature and vacuum conditions, a larger amount of material can be filled in the same volume, producing a highly stable ultra-high-density nanoparticle composition in a dispersed phase of smaller and uniform size containing very dense particles. can do.

In addition, the present invention manufactures an ultra-high-density nanoparticle composition in which active ingredients such as lipids, functional ingredients, skin care ingredients, etc. are supported at high density in the particles, thereby improving the elasticity of the formulation and having excellent particle stability because the particles are hard. can do.

In addition, the present invention is effective because the particle size can be formed very finely compared to the case where concentration is performed a total of 1 time or a total of 2 times, so the skin penetration rate is very excellent and loss of the active ingredient is prevented during the delivery process. Ultra-high-density nanoparticle compositions that maximize the delivery efficiency of ingredients can be manufactured.

The ultra-high-density nanoparticle composition may include particles in which the active ingredient is densely contained within the particles and has a particle size of 50 to 100 nm. These particles can have excellent skin permeability because they are composed of a microscopic size of about 0.001 to 0.01 of the pore size.

In one embodiment, the ultra-high-density nanoparticle composition may be manufactured using the double concentration and high-temperature vacuum emulsification system and have the same effect as above.

In the above manufacturing method, two or more liquids may be included, and the anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant are administered to the two or more liquids, and the ultra-highly concentrated particles are formed through the high-temperature vacuum emulsification step. An emulsion formulation containing dispersed phase particles can be formed, and through the secondary concentration step, an emulsion formulation containing ultra-high density nanoparticles of the dispersed phase with smaller particle size and increased density can be formed. One or more of the liquids may be highly concentrated liquids through the first concentration step before the high-temperature vacuum emulsification step.

In one embodiment, through the above manufacturing method, an emulsion formulation in which the size of the dispersed particles is reduced and the density is increased can be formed.

In the above production method, in the high-temperature vacuum emulsification step, the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant are administered to two or more liquids to form a dispersed phase with high density and a smaller and more uniform size. An emulsion formulation containing ultra-high density nanoparticles can be formed with high stability.

In the above manufacturing method, the role, effect, ingredients, weight percentage and weight ratio of the anionic surfactant, amphoteric surfactant, and first nonionic surfactant are as described above.

Another aspect provides a cosmetic composition comprising the emulsion formulation.

The cosmetic composition may be a cosmetic composition containing the ultra-high density nanoparticles. The ultra-high density nanoparticles may be manufactured by the above manufacturing method.

The term “cosmetic composition” refers to an article used on the human body to clean and beautify the human body, add attractiveness, brighten the appearance, or maintain or promote the health of skin and hair.

The cosmetic composition may be an emulsion formulation. Additionally, the cosmetic composition can be manufactured in any formulation commonly manufactured in the technical field to which the present invention pertains. For example, it may be formulated as emulsion, lotion, cream, paste, solution, suspension, oil, wax, pack, foundation, etc., but is not limited thereto. More specifically, nutritional cream, massage cream, milk lotion, essence, eye cream, sun lotion, sunscreen, makeup primer, makeup base, BB cream, emulsion foundation, pack, stick product or balm type product. It can be prepared as a dosage form.

The cosmetic composition contains additional ingredients commonly used in cosmetics, such as thickeners, dispersants, fragrances, fillers, preservatives, preservatives, stabilizers, neutralizers, humectants, emollients, ultraviolet absorbers, disinfectants, emulsifiers, antioxidants, and pH adjusters. , organic and inorganic pigments, fragrances, sweeteners, vitamins, coolants, antiperspirants, free-radical scavengers, metal ion sequestrants, functional ingredients and mixtures thereof. You can. A person skilled in the art will be able to select any additional ingredients and/or their amounts such that the advantageous properties of the compositions according to the present disclosure are not or substantially not adversely affected by the envisaged additions.

When the cosmetic composition according to the present invention is a cream or gel formulation, it may further include animal oil, vegetable oil, wax, paraffin, starch, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc, or zinc oxide as carrier ingredients. You can.

When the cosmetic composition is in the form of a solution or emulsion, the solvent, solvating agent, or emulsifying agent may be water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, propylene glycol, glycerol aliphatic ester, polyethylene glycol, or fatty acid of sorbitan. It may further include ester, etc.

When the cosmetic composition is a suspension formulation, the carrier ingredients include water, a liquid diluent such as ethanol or propylene glycol, a suspending agent such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol ester, and polyoxyethylene sorbitan ester, and microcrystalline It may further include cellulose, aluminum metahydroxide, bentonite, agar, or tracant.

The cosmetic composition may be used alone or in combination, or may be used in combination with other cosmetic compositions other than the present invention. In addition, the cosmetic composition according to the present invention can be used according to conventional usage methods, and the number of times of use can be varied depending on the user's skin condition or taste.

Another aspect provides a composition for external skin application including the emulsion formulation.

The composition for external skin application may be a cream, gel, ointment, skin emulsifier, skin suspension, transdermal delivery patch, drug-containing bandage, lotion, or a combination thereof. The skin external preparations include ingredients commonly used in external skin preparations such as cosmetics and medicines, such as aqueous ingredients, oil-based ingredients, powder ingredients, alcohols, moisturizers, thickeners, ultraviolet absorbers, whitening agents, preservatives, antioxidants, surfactants, and fragrances. , colorants, various skin nutrients, or a combination thereof may be appropriately mixed according to need. The skin external composition contains metal sequestrants such as disodium edetate, trisodium edetate, sodium citrate, sodium polyphosphate, sodium metaphosphate, and gluconic acid, caffeine, tannin, belafamil, licorice extract, glablidin, and calin. Hot water extract of fruit, various herbal medicines, drugs such as tocopherol acetate, glytylitinic acid, tranexamic acid and its derivatives or salts, vitamin C, magnesium ascorbate phosphate, ascorbate glucoside, arbutin, kojic acid, glucose, fructose, Sugars such as trehalose can also be appropriately mixed. The skin includes all skin areas of the body, including the face, hands, arms, legs, feet, chest, stomach, back, buttocks, and scalp.

The anionic surfactant and the amphoteric surfactant of the present invention improve the integrity of the dispersed phase particles by controlling the physical distance between the surfactants at the outer interface of the dispersed phase particles, and the first nonionic surfactant is used at the inner interface of the dispersed phase particles. By relaxing the interface through a combination of surfactants, the stability of the dispersed phase particles is improved, providing an emulsion formulation with high density and containing dispersed phase particles of smaller and more uniform size.

1 shows that the anionic surfactant and the amphoteric surfactant control the physical distance between the surfactants at the outer interface of the dispersed phase particles, improving particle integrity, and the first nonionic surfactant is used at the inner interface of the dispersed phase particles. A schematic diagram shows how to improve the safety of particles by relaxing the interface through a combination of activators.
Figure 2 shows the median and average values of dispersed phase particle diameters in Examples 1 and 2.
Figure 3 shows the diameter distribution of dispersed phase particles in Examples 1 and 2.

Below, preferred embodiments are presented to aid understanding of the present invention. However, the following examples are provided only to make the present invention easier to understand, and the content of the present invention is not limited by the following examples. The embodiments may be subject to various changes, and the embodiments are not limited to the embodiments disclosed below and may be implemented in various forms.

The terms or words used in the specification and claims of the present invention are not to be construed as limited to their ordinary or dictionary meanings, and the inventor may appropriately define the concept of terms to explain his or her invention in the best way. It must be interpreted as meaning and concept consistent with the technical idea of the present invention based on principles.

Throughout the specification of the present invention, when a part is said to "include" a certain component, this means that it does not exclude other components but may further include other components, unless specifically stated to the contrary. .

Throughout the specification of the present invention, “A and/or B” means A or B, or A and B.

Experimental Example 1. Emulsion formulation preparation and stability evaluation

1.1 Manufacturing of oil-in-water emulsion formulation

Examples 1 and 2 were prepared respectively according to the compositions disclosed in Table 1 below. In Table 1 below, the content of each component is expressed in weight percent.

More specifically, the preparation of Examples 1 and 2 includes preparing an aqueous phase; Primary concentration step; High temperature vacuum emulsification step; and proceeded to the second concentration step.

In the aqueous phase preparation step, purified water, moisturizer, thickener, and preservative were mixed in an emulsification tank capable of temperature control and stirring, and then heated at a temperature of 60 to 90° C. to dissolve and homogenize each component.

In the primary concentration step, the emulsifier (second nonionic surfactant) and emulsification aid (higher alcohol) are mixed in an oil phase emulsification tank capable of temperature control and stirring, and then heated at a temperature of 60 to 90°C to separate each component. The oil phase was prepared by dissolving and homogenizing, and the prepared oil phase was concentrated at a temperature of 40 to 60°C and a pressure of 500 to 900 bar.

In the high-temperature vacuum emulsification step, the primary concentrated oil phase, anionic surfactant, amphoteric surfactant, and first nonionic surfactant are added to the vacuum emulsification tank in which the water phase is accommodated, and the temperature is 60 to 90° C. (preferably was high-temperature vacuum emulsification at a temperature of 70 to 85°C), a vacuum of 0.05 MPa to 0.15 MPa (preferably, 0.06 MPa to 0.09 MPa), and 4,000 to 7,000 rpm.

In the secondary concentration step, the emulsified compound was concentrated at a temperature of 60 to 80 ° C. and a pressure of 1,200 to 1,600 bar, and then cooled to a temperature of 35 ° C. to prepare an emulsion containing ultra-high density nanoparticles. .

role Ingredient name Example 1 Example 2 anionic surfactant Sodium Stearoyl Glutamate 0.2 0.2 amphoteric surfactant Coco-Betaine 0.05 0.025 First nonionic surfactant Polyglyceryl-sesquiisostearate 0.1 0.1 ratio 4:1:2 4:0.5:2 Second nonionic surfactant Cetearyl Olivate/Sorbitan Olivate 3 3 Glyceryl Stearate One One Emulsifying aid (higher alcohol) Cetaryl alcohol 1.5 1.5 Oil-moisturizer Caprylic/Capric Triglyceride 10 10 Ethylhexylstearate 5 5 water-moisturizer glycerin 15 15 thickener carbomer 0.1 0.1 Floxamer 0.05 0.05 xanthan gum 0.05 0.05 Caprylic/Capric Triglyceride*Polyurethane-11 0.01 0.01 antiseptic Ethylhexylglycerin 0.1 0.1 Hydroxyacetophenone 0.3 0.3 solvent Purified water To 100 To 100

1.2 Safety evaluation of oil-in-water emulsion formulation

The size and safety of ultra-high density nanoparticles in the emulsion dispersion phase of Examples 1 and 2 prepared in Experimental Example 1.1 were evaluated.

Specifically, the particle size (diameter) was analyzed using dynamic lightscattering (DLS), and the results are shown in Table 2, Figures 2, and 3. Specifically, the particle size was measured using the HORIBA nanoparticle size analyzer (Particle Size Analyzer, SZ-100) using the measurement method of ISO 22412:2017. .

In the case of stability, it was confirmed by visual evaluation, and the results are shown in Table 3 below.

Example 1 Example 2 Particle size (diameter, nm) 55-70 70-100

Example 1 Example 2 stability ○ ○

※ The evaluation criteria for formulation stability are as follows:

○: Nanoparticle formation, uniform particle distribution;

×: Nanoparticle non-formation, layer separation phenomenon, gelling phenomenon, or oil discharge.

1 shows that an anionic surfactant and an amphoteric surfactant control the physical distance between the surfactants at the outer interface of the dispersed phase particles, improving the integrity of the particles, and the first nonionic surfactant is used at the inner interface of the dispersed phase particles. A schematic diagram shows how to improve the safety of particles by relaxing the interface through a combination of activators.

Figure 2 shows the median and average values of dispersed phase particle diameters in Examples 1 and 2.

Figure 3 shows the diameter distribution of dispersed phase particles in Examples 1 and 2.

As shown in Table 2, Table 3, and Figures 2 and 3, the anionic surfactant and the amphoteric surfactant adjust the physical distance between the surfactants at the outer interface of the dispersed phase particles, improving the integrity of the particles, The first nonionic surfactant improves the safety of the particles by relaxing the interface through a combination of surfactants at the inner interface of the dispersed phase particles, thereby producing ultrahigh-density dispersed nanoparticles with a uniform distribution of nano sizes in both Examples 1 and 2. It was formed with high stability.

Experimental Example 2. Emulsion formulation preparation and safety evaluation depending on whether or not an emulsifier is included

2.1 Manufacturing of oil-in-water emulsion formulation with or without emulsifier

Example 1 and Comparative Examples 1 to 3 were prepared according to the compositions disclosed in Table 4 below. In Table 4 below, the content of each component is expressed in weight percent.

The specific manufacturing method is the same as Experimental Example 1.1, except that in the high-temperature vacuum emulsification step, in Comparative Example 1, an anionic surfactant was not added, and in Comparative Example 2, an amphoteric surfactant was not added. In Comparative Example 3, the first nonionic surfactant was not added.

role Ingredient name Example 1 Comparative Example 1 Comparative example 2 Comparative Example 3 anionic surfactant Sodium Stearoyl Glutamate 0.2 Not included 0.17 0.17 Amphoteric surfactant Coco-Betaine 0.05 0.17 Not included 0.17 First nonionic surfactant Polyglyceryl-sesquiisostearate 0.1 0.17 0.17 Not included Second nonionic surfactant Cetearyl Olivate/Sorbitan Olivate 3 3 3 3 Glyceryl Stearate One One One One Emulsifying aid (high-grade alcohol) Cetaryl alcohol 1.5 1.5 1.5 1.5 Oil-moisturizer Caprylic/Capric Triglyceride 10 10 10 10 Ethylhexylstearate 5 5 5 5 water-moisturizer glycerin 15 15 15 15 thickener carbomer 0.1 0.1 0.1 0.1 Floxamer 0.05 0.05 0.05 0.05 xanthan gum 0.05 0.05 0.05 0.05 Caprylic/Capric Triglyceride*Polyurethane-11 0.01 0.01 0.01 0.01 antiseptic Ethylhexylglycerin 0.1 0.1 0.1 0.1 Hydroxyacetophenone 0.3 0.3 0.3 0.3 solvent Purified water To 100 To 100 To 100 To 100

2.2 Stability evaluation of oil-in-water emulsion formulation with or without emulsifier

The safety of Example 1 and Comparative Examples 1 to 3 prepared in Experimental Example 2.1 was evaluated.

In the case of stability, it was evaluated by visual inspection, and the results are shown in Table 5 below.

Example 1 Comparative Example 1 Comparative example 2 Comparative example 3 stability ○ × × ×

※ The evaluation criteria for formulation stability are as follows:

○: Nanoparticle formation, uniform particle distribution;

×: Nanoparticle non-formation, layer separation phenomenon, gelling phenomenon, or oil discharge.

As shown in Table 5, in Comparative Examples 1 to 3, an unstable emulsion formulation was formed. In Comparative Example 1, dispersed particles were not formed, in Comparative Example 2, layer separation between the oil phase and water phase of the formulation was confirmed, and in Comparative Example 3, oil was discharged.

These results show that when anionic surfactants, amphoteric surfactants, and nonionic surfactants according to one embodiment are used as emulsifiers, an emulsion formulation containing uniformly dispersed ultra-high density nanoparticles of 50 to 100 nm is formed. it means.

Experimental Example 3. Emulsion formulation preparation and safety evaluation according to emulsifier ratio

3.1 Preparation of oil-in-water emulsion formulation according to emulsifier ratio

Example 1 and Comparative Examples 4 to 6 were prepared according to the compositions disclosed in Table 6 below. In Table 6 below, the content of each component is expressed in weight percent.

The specific manufacturing method was the same as Experimental Example 1.1, except that in the high-temperature vacuum emulsification step, the weight ratio of the anionic surfactant, the amphoteric surfactant, and the second nonionic surfactant in the formulation was different.

role Ingredient name Example 1 Comparative Example 4 Comparative Example 5 Comparative Example 6 Comparative example 7 anionic surfactant Sodium Stearoyl Glutamate 0.2 0.2 0.2 0.2 0.2 amphoteric surfactant Coco-Betaine 0.05 0.005 0.15 0.05 0.05 First nonionic surfactant Polyglyceryl-sesquiisostearate 0.1 0.1 0.1 0.005 0.2 ratio 4:1:2 4:0.1:2 4:3:2 4:1:0.1 4:1:4 Second nonionic surfactant Cetearyl Olivate/Sorbitan Olivate 3 3 3 3 3 Glyceryl Stearate One One One One One Emulsifying aid (high-grade alcohol) Cetaryl alcohol 1.5 1.5 1.5 1.5 1.5 Oil-moisturizer Caprylic/Capric Triglyceride 10 10 10 10 10 Ethylhexylstearate 5 5 5 5 5 water-moisturizer glycerin 15 15 15 15 15 thickener carbomer 0.1 0.1 0.1 0.1 0.1 Floxamer 0.05 0.05 0.05 0.05 0.05 xanthan gum 0.05 0.05 0.05 0.05 0.05 Caprylic/Capric Triglyceride*Polyurethane-11 0.01 0.01 0.01 0.01 0.01 antiseptic Ethylhexylglycerin 0.1 0.1 0.1 0.1 0.1 Hydroxyacetophenone 0.3 0.3 0.3 0.3 0.3 solvent Purified water To 100 To 100 To 100 To 100 To 100

3.2 Safety evaluation of oil-in-water emulsion formulation according to emulsifier ratio

The safety of Example 1 and Comparative Examples 4 to 7 prepared in Experimental Example 3.1 was evaluated.

In the case of stability, it was evaluated by visual inspection, and the results are shown in Table 7 below.

Example 1 Comparative example 4 Comparative Example 5 Comparative Example 6 Comparative Example 7 stability ○ × × × ×

※ The evaluation criteria for formulation stability are as follows:

○: Nanoparticle formation, uniform particle distribution;

×: Nanoparticle non-formation, layer separation phenomenon, gelling phenomenon, or oil discharge.

As shown in Table 7, in Comparative Examples 4 to 7, an unstable emulsion formulation was formed. In Comparative Example 4, the effect of improving the integrity of the particles by adjusting the physical distance between the surfactants at the outer interface (the part in contact with the continuous phase component) of the dispersed phase particles of the amphoteric surfactant was weak, so that the internal oil of the oil phase particles was weak. was discharged, and in the case of Comparative Example 5, the hardness increased over time due to the excessive amount of emulsifier, and in the case of Comparative Example 6, the inner interface of the dispersed phase particles of the nonionic surfactant (the part in contact with the dispersed phase component) through the combination of surfactants at the interface. The effect of improving the safety of the particles by alleviating was weak, so long-term stability at high temperatures was low, and in the case of Comparative Example 7, it was confirmed that a gelling phenomenon occurred due to an excessive amount of emulsifier.

These results show that when anionic surfactants, amphoteric surfactants, and nonionic surfactants according to one embodiment are used as emulsifiers and are contained in the formulation at a weight ratio of 4:0.5 to 2:1 to 3, 50 to 50 This means that an emulsion containing ultra-high density nanoparticles in a uniformly dispersed phase of 100 nm is formed.

Claims (14)

delete delete a dispersed phase comprising an anionic surfactant, an amphoteric surfactant, and a first nonionic surfactant, and comprising a second nonionic surfactant; and
An emulsion formulation comprising a continuous phase surrounding the dispersed phase,
An emulsion formulation wherein the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant are included in a weight ratio of 4:0.5 to 2:1 to 3. The emulsion formulation according to claim 3, wherein the particles of the dispersed phase have a diameter of 50 to 100 nm. The method of claim 3, wherein the anionic surfactant and the amphoteric surfactant are such that when the anionic surfactant approaches the amphoteric surfactant, an adjacent surface of the amphoteric surfactant is charged with a partial positive charge, thereby forming the anionic surfactant. By controlling the physical bond distance between the surfactants at the outer interface of the dispersed phase particles by applying an attractive force due to electrostatic interaction with, the size of the dispersed phase particles is made smaller, thereby improving the integrity of the dispersed phase particles, and the first Nonionic surfactants relax the boundary of the interface through polyglyceryl-2 sesquiisostearate, polyglyceryl-4 isostearate, glyceryl stearate, or a combination thereof at the inner interface of the dispersed phase particles. Improving the safety of the emulsion formulation, wherein the second nonionic surfactant is an emulsifier. The emulsion formulation according to claim 3, wherein the anionic surfactant includes at least one from the group consisting of sodium stearoyl glutamate, sodium cocoyl sarcosinate, and potassium cetyl phosphate. The emulsion formulation of claim 3, wherein the amphoteric surfactant includes coco-betaine, sodium cocoamphoacetate, or a combination thereof. The emulsion formulation of claim 3, wherein the first nonionic surfactant includes at least one from the group consisting of polyglyceryl-2 sesquiisostearate, polyglyceryl-4 isostearate, and glyceryl stearate. . delete The emulsion formulation of claim 3, wherein the second nonionic surfactant includes cetearyl olivate/sorbitan olivate, glyceryl stearate, or a combination thereof. The method of claim 3, wherein in the process of emulsifying the dispersed phase and the continuous phase containing the second nonionic surfactant, the anionic surfactant, the amphoteric surfactant, and the first nonionic surfactant are mixed and emulsified under vacuum. This is an emulsion formulation. The method of claim 3, wherein O/W (oil-in-water) emulsion, W/O (water-in-oil) emulsion, W/O/W (water-in-oil-in-water) emulsion, O/W An emulsion formulation, which is an oil-in-water-in-oil (/O) emulsion or multiple emulsion. A cosmetic composition comprising the emulsion formulation of claim 3. A composition for external application for skin comprising the emulsion formulation of claim 3.