KR102120789B1 - Nano-emulsion cosmetic composition stabilized oil of high content - Google Patents

Abstract

The present invention relates to a translucent oil-in-water (O/W) nanoemulsion cosmetic composition having excellent stability including high-content oil (5 to 30%), and more specifically, pre-emulsion by applying an emulsifier. It relates to a nano-emulsion cosmetic composition having a low-viscosity (less than 5000 cps) physical properties having a semi-transparent appearance by passing through a high pressure homogenizer after making it secondary.

Description

Nano-emulsion cosmetic composition stabilized oil of high content

The present invention relates to a nanoemulsion cosmetic composition that stabilizes a high content of oil.

Emulsion refers to a liquid-liquid dispersion system in which one or more liquid phases that are not mixed in one liquid phase are dispersed, and generally has a size distribution of several μm to several tens of μm.

Macroemulsions having such a particle size are thermodynamically unstable, and eventually separated by various routes such as floculation, sedimentation, creming, particle growth (Ostwald ripening) and coalescence. It has the property to be.

At this time, when the size of the dispersed phase emulsion particles is reduced to nano-scale, the brown's motion between particles can significantly improve the stability of the emulsion in terms of kinetics, and it is possible to manufacture a low-viscosity emulsion with a high content of the inner phase. In addition to being able to make cosmetics with various feelings of use, it has the advantage of being able to effectively deliver active ingredients to the skin due to its small particle size.

In general, although there is a slight difference according to the literature, a nano-emulsion (Flockhart, IR etc, Nanoemulsions derived from lanolin show promising drug delivery properties, J. Pharm.pharmac ., 50(Supplement)1998, 141).

Several attempts have been made to produce nanoemulsions with fine, low-viscosity particles, and among them, a phase-in-phase emulsification method or a high-pressure emulsification method has been used.

Among them, the phase-inversion emulsification method decreases the hydrogen bond between the hydrophilic group of the nonionic surfactant and ethylene oxide and water as the temperature of the composition composed of the three-component system of water, oil, and nonionic surfactant decreases, thereby reducing the hydrophilic property. It is an emulsification method using the principle (Inter. J. Cosmet. Sci. 1994, 16, 84-92). At this time, the composition composed of the three-component system will form an O/W type emulsion below a certain temperature, and a W/O type emulsion above a certain temperature. This temperature is called "PIT (Phase Inversion Temperature)".

In addition, a high-pressure emulsification method of manufacturing a nanoemulsion using a high-pressure emulsifier was used, but there was also a limitation in implementing a semi-transparent formulation by applying a high content of oil to a low-viscosity formulation such as lotion.

As described above, efforts have been made to make the particles fine and uniform, but these methods alone have many technical limitations in manufacturing a cosmetic having a desired viscosity, nano-sized particle production, and high-content oil while having a semi-transparent appearance. In fact, it has not been used much in the productive aspect.

Stefan Schultz and Joachim Ulrich, High pressure homogenizations as a process for emulsion formation, Chem engineering & Technology, 27, 361-368 (2004) Wan Goo Cho, Nanoemulsions: a Novel Vehicle for Cosmetics, J. Soc. Cosmet. Scientists Korea, 37, 1-21 (2011) MYu Koroleva, E V Yurtov, Nanoemulsions: the properties, methods of preparation and promising applications, Russian Chemical Reviews, 81, 21-43 (2012)

Accordingly, the present inventors applied a high-pressure emulsifier Bi-Pass emulsification method while using a polyglyceryl-based emulsifier or a PEG-based stearate emulsifier, so that the average size of the emulsified particles is very small, and it is excellent in stability, but also contains translucent oil. The present invention was completed by developing a low-viscosity O/W-type nanoemulsion cosmetic composition showing an appearance.

Therefore, the object of the present invention is water; Polyglyceryl-based emulsifiers or PEG-based stearate emulsifiers; At least one high-content oil selected from the group consisting of silicone oil, ester oil and hydrocarbon oil; And a polyol or polyol derivative; to provide a translucent oil-in-water (O/W) nanoemulsion cosmetic composition.

In addition, another object of the present invention is to provide a method for producing a translucent oil-in-water (O/W) nanoemulsion cosmetic composition.

As a means for solving the above problems, the present invention is water; Polyglyceryl-based emulsifiers or PEG-based stearate emulsifiers; At least one oil selected from the group consisting of silicone oil, ester oil and hydrocarbon oil; And polyol or a polyol derivative; provides a translucent oil-in-water (O/W) nanoemulsion cosmetic composition comprising a.

As another means for solving the above problems, the present invention

1) mixing water and a polyol or a polyol derivative;

2) mixing one or more oils selected from the group consisting of silicone oils, ester oils and hydrocarbon oils, and polyglyceryl-based emulsifiers or PEG-based stearate emulsifiers,

3) Mixing the mixture of 1) and the mixture of 2) and emulsifying at high pressure.

It provides a method for producing a translucent oil-in-water (O/W) nanoemulsion cosmetic composition comprising a cosmetic composition.

According to the present invention, it is possible to provide a translucent nanoemulsion having a high oil content through a method using a combination of an existing emulsification method and a high pressure emulsification method. Through this, there is a limit to solubilization of a large amount of oil, so it is possible to overcome the limitation of the existing low-viscosity cosmetic composition that realizes a feeling of use with a small amount of oil and a large amount of polymer and moisturizer. Through this, not only can a cosmetic composition having various feelings of use be produced, but the size of the emulsified particles is small, which has an advantage of effectively delivering an active ingredient to the skin.

1 shows the nanoemulsion particle size of Example 1.
Figure 2 is a photo confirming the stability of the nano-emulsion of Example 1 before the high pressure emulsifier passed, after the first pass, after the second pass through transparency.
3 is a photograph confirming the transparency of Comparative Examples 1 to 3.

The present invention is water; Polyglyceryl-based emulsifiers or PEG-based stearate emulsifiers; At least one high-content oil selected from the group consisting of silicone oil, ester oil and hydrocarbon oil; And polyol or a polyol derivative; relates to a translucent oil-in-water (O/W) nanoemulsion cosmetic composition comprising a.

The polyglyceryl-based emulsifier may be, for example, polyglyceryl 10-stearate, polyglyceryl-3-caprate, polyglyceryl-3-diisostearate, polyglyceryl-3 methylglucose distearate, etc. , But is not limited to this.

The PEG-based stearate emulsifier may be one or more selected from the group consisting of PEG-n stearate having a polymerization degree of 3 to 90, but is not limited thereto.

The polyglyceryl-based emulsifier or PEG-based stearate emulsifier may be included in an amount of 1 to 10% by weight based on the total weight of the cosmetic composition. If it is out of the above range, the cosmetic composition may not have hardness or may have an opaque appearance.

The oil used in the present invention is not particularly limited as long as it is commonly used in preparing an oil-in-water emulsion composition, but may be, for example, one or more selected from the group consisting of silicone oil, ester oil and hydrocarbon oil. .

The silicone oil is dimethicone, cyclomethicone, polydimethylsiloxane, methylphenylpolysiloxane, methylcyclopolysiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, tetradecamethylhexasiloxane and octamethyltri It may be one or more selected from the group consisting of siloxane, but is not limited thereto.

The ester-based oil is triethylhexanoin, cetylethylhexanoate, cetyloctanoate, cetylisooctanoate, octyldodecyl myristate, pentaerythritol tetraethylhexanoate, isopropyl palmitate, iso It may be one or more selected from the group consisting of propyl myristate, caprylic/capric triglyceride, butylene glycol dicaprylate/dicaprate, tocopherol acetate and dicaprylic carbonate, but is not limited thereto.

The hydrocarbon-based oil may be at least one selected from the group consisting of paraffin, ceresin and microcrystalline wax, but is not limited thereto.

The oil may be included in 5 to 30% by weight based on the total weight of the composition. At this time, "the content of oil" means the total amount of the oil phase component that does not contain an emulsion stabilizer, and if the content of the oil is less than 5% by weight, it is easy to see the existing skin-type cosmetic composition and the appearance and feeling of use without much difference. It is possible to implement, and if it exceeds 30% by weight, the emulsifying particles may become large and the emulsification stability may be deteriorated.

In the present invention, a high-content oil is used, and it is characterized in that a translucent emulsion formulation stabilized even when 5% by weight or more is used. Stability/semi-transparency, etc. were not secured when performed with the existing technology, and the existing technology is usually used in nanoemulsions as a composition having an oil content of less than 5%, that is, a low content.

As the polyol or a derivative thereof, glycerin, a monovalent or divalent alcohol, or a mixture thereof may be used. More specifically, it may be at least one selected from the group consisting of butylene glycol, glycerin, propylene glycol, dipropylene glycol, propanediol, hexanediol, and the like, and mixtures thereof. Specifically, the polyol or polyol derivative included in the composition according to the present invention may be, for example, a mixture of glycerin and 1,2-hexanediol, but is not limited thereto.

The polyol or polyol derivative may include 1 to 30% by weight based on the total weight of the composition. If the content thereof is less than 5% by weight, the skin moisturizing effect may be insufficient, and if it exceeds 30% by weight, there is a problem that a feeling of use and skin irritation may be caused.

In some cases, the composition according to the present invention may further include a pigment, a fragrance, a preservative, or a thickener as an auxiliary component used in preparing an oil-in-water nanoemulsion composition, wherein the content of the auxiliary component is, for example, a composition It may be 0 to 20% by weight based on the total weight.

Water used in the present invention can be used as the balance of the above composition based on the total composition weight.

In addition, the nanoemulsion according to the present invention is not particularly limited as long as it has a low viscosity enough to achieve the desired dispersibility in order to increase the content of the inner phase and effectively deliver the active ingredient, for example, 5000 cps or less, specifically As it may have a viscosity of 3000 cps or less, more specifically 2000 cps or less. The'low viscosity' emulsion includes all of the emulsions belonging to the aforementioned viscosity range from the case where the viscosity is very small and the viscosity cannot be experimentally measured, and the viscosity range when the viscosity is not experimentally measured is 0. , For example, may have a viscosity of 0 to 5000 cps, specifically 1 to 3000 cps, and more specifically 5 to 2000 cps.

The emulsion is not particularly limited as long as it has a nano-size and improves the stability of the emulsion while producing a low-viscosity emulsion, for example, the average size may be 250 nm or less, specifically 200 nm or less. The emulsion may have any size that falls within the above average size range, but may have, for example, an average size of 10 to 250 nm, specifically 20 to 200 nm. At this time, the particle size distribution may be very narrow, for example, 10 to 250 nm, specifically 50 to 150 nm, and through this, it is possible to provide a nanoemulsion composition which is not only excellent in terms of stability, but also light in use. have.

The emulsion composition may exhibit a translucent appearance. When the conventional emulsification method or simply the high pressure emulsification method is applied, it is easy to realize the appearance of white turbidity or suspension, but it is difficult to express a translucent appearance. However, the emulsion composition according to the present invention has a semi-transparent appearance of a low-viscosity skin type and can realize a nutritious inversion feeling through a high content of oil.

The cosmetic composition according to the present invention is not particularly limited in its formulation, but can be used for skin, mucous membranes, scalp or hair, for example, softening, longevity, lotion, cream, pack, gel, patch or spray ( Mist) and other basic cosmetics; Color cosmetics such as lipstick, makeup base, or foundation; Cleaning agents such as shampoo, conditioner, body cleanser, toothpaste or mouthwash; Hair dressing agents such as hair tonic, gel or mousse; Or it may be formulated as a cosmetic composition for hair, such as wool or hair dye. In addition, it can be widely applied as medicines and quasi-drugs such as lotions, ointments, gels, creams, patches or sprays.

In addition, the present invention provides a method for preparing a translucent oil-in-water (O/W) nanoemulsion cosmetic composition in which the composition is applied with an emulsification method and a high pressure emulsification method.

Specifically, the present invention

1) mixing water and a polyol or a polyol derivative;

2) mixing one or more oils selected from the group consisting of silicone oils, ester oils and hydrocarbon oils, and polyglyceryl-based emulsifiers or PEG-based stearate emulsifiers,

3) Mixing the mixture of 1) and the mixture of 2) and emulsifying at high pressure.

It may include a method of manufacturing a translucent oil-in-water (O/W) nanoemulsion cosmetic composition comprising a.

In addition, the ingredients mentioned in the above manufacturing method may be applied to the same content as the cosmetic composition.

The high pressure emulsification is preferably performed under a pressure of 500 to 2500 bar, and when it is less than 500 bar, transparency and stability of the appearance cannot be expected, and thus there is a problem in forming a correct nanoemulsion, and when it exceeds 2500 bar, it is unreasonable to a high pressure emulsifier. Can be a problem for continuous production.

In addition, when the high pressure emulsification is performed two or more times, particles having an average particle size of 20 to 250 nm stabilized can be obtained.

Hereinafter, examples and the like will be described in detail to help understanding of the present invention. However, the embodiments according to the present invention may be modified in various other forms, and the scope of the present invention should not be interpreted as being limited to the following examples. The embodiments of the present invention are provided to more fully describe the present invention to those skilled in the art.

Example 1 and Comparative Examples 1-3: Preparation of oil-in-water nanoemulsion cosmetic composition

Examples 1 and Comparative Examples 1 to 3 according to each component and content shown in Table 1 to prepare a cosmetic composition in the following way.

As shown in Table 1, first, each raw material of 1 part was weighed, stirred with a disper, and heated (75°C). Next, each raw material of 2 parts was weighed/stirred, heated (75° C.), mixed with 1 part, and stirred at 3000 rpm for 5 minutes using a Homo-mixer. 3 parts of raw materials were added at 50°C, stirred under the same conditions (3000 rpm/5 minutes), and cooled to 30°C. The M-110P Microfluidizer ^® high pressure emulsifier was used twice and passed under conditions of 1000 bar and cooled to 30°C.

Here, unlike the Homo-mixer used in the existing emulsification system, the point of using a high pressure emulsifier is different from the existing emulsification process.

Through this process change, the physical or physicochemical properties of the emulsifying particles can be changed.

division

(weight%) Raw material name Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 1 part water to 100 to 100 to 100 to 100 glycerin 8 8 8 8 1,2-hexanediol 2 2 2 2 2 part Polyglyceryl-10 stearate 5 0 0 0 Polysorbate 60 0 5 0 0 Sorbitan stearate/PEG-40 stearate 0 0 5 0 lecithin 0 0 0 5 Cetyl Ethyl Hexanoate 5 5 5 5 Dimethicone 5 5 5 5 3 part ethanol 5 5 5 5 Spices 0.1 0.1 0.1 0.1

Experimental Example 1: Stability evaluation

Attached Figure 1 shows the nanoemulsion particle size of Example 1 in which the high pressure emulsifier 2 pass after Homo-Mix. The results show that the average particle size is around 100 nm. In general, when the particle size is less than 200 nm, the appearance is translucent and has a bluish characteristic, so it is easy to visually determine whether the nanoemulsion is well prepared. In addition, in the evaluation of formulation stability, it can be determined that stability is maintained when the translucent appearance persists as in the case immediately after preparation. Here, the particle size was measured using a particle size analyzer (Submicron Particle Sizer NICOMP 380).

Here, the size of the particles can be changed according to the experimental conditions (composition content and the number of times the high pressure emulsifier passes). Such particle size measurement can be used as another reliable method for determining the stability of the formulation in addition to the method that is easily determined by the naked eye.

Experimental Example 2: Transparency check

The emulsion of Example 1 was prepared, and the transparency after storage at 40° C. for 30 days was visually observed, and the results are shown in FIG. 2.

In addition, in the case of Comparative Examples 1 to 3 in which the high-pressure emulsifier was passed twice, the opaque appearance could be confirmed unlike the Examples, and the results are shown in FIG. 3.

Experimental Example 3: Viscosity check

The viscosity of the product is measured with a Brookfield DV-E viscometer and is expressed in cps (centi poise). The viscosity of the sample measured in this experiment is shown in Table 2 below.

Experimental Example 4: Usability Confirm

Emulsion compositions of Example 1 and Comparative Examples 1 to 3 were applied to the back of each hand once (approximately 0.5 ml) to provide various sensibility qualities such as appearance, spreadability, moisture, oiliness, stickiness, adhesion, absorbency, post-use feeling, and persistence. It is possible to evaluate the overall product satisfaction. The usability/characteristics of the examples and comparative examples are shown in Table 2 below.

division Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 Exterior Translucent opacity opacity opacity Viscosity (cps) 800 cps 7500 cps 5500 cps 6500 cps Usability/Features Usability change
Changes in usability starting with rich moisture and finishing with rich oily Sticky emulsion that feels more oily than moisture The soft spread is good, but
Sticky emulsion Emulsion with a very sticky finish stability stability
See Figure 2 Instability
See Figure 3 Instability
See Figure 3 Instability
See Figure 3

Claims (15)

water,
Polyglyceryl 10-stearate emulsifier,
At least one oil selected from the group consisting of silicone oil, ester oil and hydrocarbon oil, and
Polyols or polyol derivatives,
Does not contain emulsifiers and thickeners other than polyglyceryl 10-stearate,
The emulsifier is contained in 1 to 5% by weight based on the total weight of the composition,
The oil is included in 5 to 30% by weight based on the total weight of the composition,
Semi-transparent oil-in-water (O/W) nanoemulsion cosmetic composition having a particle size distribution of 10-250 nm.
delete delete delete According to claim 1,
The silicone oil is dimethicone, cyclomethicone, polydimethylsiloxane, methylphenylpolysiloxane, methylcyclopolysiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, tetradecamethylhexasiloxane and octamethyltri At least one cosmetic composition selected from the group consisting of siloxanes.
According to claim 1,
The ester-based oil is triethylhexanoin, cetylethylhexanoate, cetyloctanoate, cetylisooctanoate, octyldodecyl myristate, pentaerythritol tetraethylhexanoate, isopropyl palmitate, iso At least one cosmetic composition selected from the group consisting of propyl myristate, caprylic/capric triglyceride, butylene glycol dicaprylate/dicaprate, tocopherol acetate and dicaprylic carbonate.
According to claim 1,
The hydrocarbon-based oil is a cosmetic composition of at least one selected from the group consisting of paraffin, ceresin and microcrystalline wax.
delete According to claim 1,
The polyol or a derivative thereof is at least one cosmetic composition selected from the group consisting of glycerin, monovalent or divalent alcohol, and mixtures thereof.
According to claim 1,
The polyol or a derivative thereof is a cosmetic composition comprising 1 to 30% by weight based on the total weight of the composition.
According to claim 1,
The emulsion is a cosmetic composition having a viscosity of 0 to 5000 cps.
According to claim 1,
Nano emulsion is a cosmetic composition having an average particle size of 10 to 250 nm.
1) mixing water and a polyol or a polyol derivative;
2) mixing one or more oils selected from the group consisting of silicone oil, ester oil and hydrocarbon oil and polyglyceryl 10-stearate emulsifier,
3) Mixing the mixture of 1) and the mixture of 2), and performing high pressure emulsification two or more times under a pressure of 500 to 2500 bar.
Including,
Does not contain emulsifiers and thickeners other than polyglyceryl 10-stearate,
The emulsifier is contained in 1 to 5% by weight based on the total weight of the composition,
The oil is included in 5 to 30% by weight based on the total weight of the composition,
Method of manufacturing a semi-transparent oil-in-water (O/W) nanoemulsion cosmetic composition having a particle size distribution of 10-250 nm.
delete delete

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