KR20210153853A - Stabilizing method of rice bran wax and cosmetic composition containing the stabilized rice bran wax - Google Patents

Abstract

The present invention relates to a method for stabilizing rice bran wax and a cosmetic composition containing a nanoemulsion stabilized with a high content of rice bran wax, specifically, to prepare a stable nanoemulsion containing a high content of rice bran wax without the use of an emulsifier or surfactant and technology to use it as a cosmetic. According to the present invention, it is possible to prepare a cosmetic composition excellent in long-term stability without separation and particle destruction at high and low temperatures because it contains a high content of rice bran wax and has excellent emulsion stability and constant flowability.

Description

Stabilizing method of rice bran wax and a cosmetic composition containing a nanoemulsion in which a high content of rice bran wax is stabilized {Stabilizing method of rice bran wax and cosmetic composition containing the stabilized rice bran wax}

The present invention relates to a method for stabilizing rice bran wax and a cosmetic composition containing a nanoemulsion stabilized with a high content of rice bran wax, specifically, to prepare a stable nanoemulsion containing a high content of rice bran wax without the use of an emulsifier or surfactant and technology to use it as a cosmetic.

In general, in the manufacture of moisturizing cosmetics, active ingredients to increase the skin's moisturizing power are used. Humectants that absorb moisture or occlusive moisturizers that prevent moisture evaporation by forming a shielding film are used to remove moisture from the stratum corneum. A method of increasing the water retention of water is widely used. Most of the humectants are polyols, such as glycerin, propylene glycol, butylene glycol, propanediol, and polyethylene glycol. And lipid components such as ceramides or essential fatty acids and lipid complexes are used as occlusive moisturizers, which are known to have the advantage of excellent moisturizing power, but they can be used only in the composition of specific raw materials, so there is a problem that it is difficult to use them universally .

Conventionally, Korean Patent Publication No. 10-2015-0019669 "Oil-in-water emulsified cosmetic composition containing high content of butter" discloses a technique for stabilizing a high content of butter as an oil-in-water cosmetic using a high molecular weight polymer, but the polymer There is a problem in that the feeling of use is limited by the polymer and the low-temperature stability is weak. In addition, Korean Patent Laid-Open No. 10-2014-0123295 "Cosmetic composition containing transparent ceramide emulsion" includes an emulsion composition in which anionic surfactant is used and ceramide is stabilized by treatment with a high-pressure homogenizer, but the anionic surfactant causes severe skin irritation. There is a problem in applying a high content. In addition, Korean Patent Laid-Open No. 10-2017-0003189 "Multilayer Ceramide Lamella Structure Containing Fatty Acid and Neutralizing Agent" discloses a ceramide stabilization technology using a lamellar liquid crystal using a solid fatty acid. It is difficult to form an emulsion, and there is a problem of precipitation due to change over time at low temperature.

On the other hand, recently, moisturizing cosmetics are being developed to suppress the use of chemical substances that can be harmful to the skin and to maintain skin moisture by using natural substances derived from plants as raw materials. As one of these natural moisturizing cosmetics, plant-derived wax or butter is used. Butter is a fat extract of a plant fruit or seed, and has a melting point close to human body temperature.

The present inventors have endeavored to develop cosmetics that maintain skin moisture by stably containing these natural cosmetics in a high content, and have studied how to select rice bran wax as a natural cosmetic and use it effectively. The cosmetic composition containing a high content of rice bran wax exhibited a very excellent advantage of forming a shielding film on the skin during application to prevent moisture evaporation and impart gloss. However, waxes having a high melting point including rice bran wax had a problem in that recrystallization occurred at a low temperature.

As a result of research to solve this problem, the present inventors prepared rice bran wax as a primary emulsion using a specific liquid fatty acid and a neutralizing agent, and treated it again with a high pressure homogenizer to prepare a nano emulsion. However, the present invention was completed by confirming that it was possible to prepare a cosmetic that was stable without a change in viscosity at room temperature or low temperature.

Therefore, an object of the present invention is to provide a method for stabilizing rice bran wax in which rice bran wax is prepared as a primary emulsion using a liquid fatty acid and a neutralizer, and this is treated again with a high-pressure homogenizer to produce a nano-emulsion.

In addition, another object of the present invention is to provide a nanoemulsion that is manufactured by the above stabilization method and is stable without viscosity change at high temperature, room temperature, or low temperature even if a high content of rice bran wax is included.

Another object of the present invention is to provide a cosmetic composition containing the nanoemulsion and exhibiting an excellent moisturizing effect and skin luster effect.

According to the present invention in order to achieve the above object, A) mixing the oil phase part containing 10 to 50% by weight of rice bran wax and 0.1 to 5.0% by weight of isostearic acid by stirring at 70 to 80 ℃; B) mixing the aqueous phase part containing 0.1 to 0.5% by weight of a neutralizing agent and purified water at 70 to 80° C. by stirring; C) preparing a primary emulsion by mixing the oil phase part and the aqueous phase part and stirring with a homomixer; And D) passing the primary emulsion through a high pressure homogenizer (Micro Fluidizer) 2-3 times under a pressure of 1,000 to 1,500 bar and cooling to prepare a nano-emulsion There is provided a method of stabilizing rice bran wax.

The neutralizing agent is at least one selected from the group consisting of tromethamine, triethanolamine, sodium hydroxide, potassium hydroxide and arginine.

According to the present invention in order to achieve the above other object, there is provided a nanoemulsion prepared by the stabilization method.

According to the present invention in order to achieve the above another object, there is provided a cosmetic composition in which the nanoemulsion is contained in an amount of 0.1 to 90% by weight based on the total weight of the cosmetic composition. The cosmetic composition is characterized in that it has excellent skin moisturizing effect and skin luster effect.

According to the present invention, it is possible to manufacture a cosmetic with excellent stability at high and low temperatures because it has excellent emulsification stability and constant flowability while containing a high content of rice bran wax without the use of a surfactant. The cosmetic composition containing it exhibits excellent skin moisturizing and skin luster effect when applied to the skin.

1 shows a particle size distribution diagram of a nanoemulsion prepared according to an embodiment of the present invention.
2 shows a particle size distribution diagram of a nanoemulsion prepared according to a comparative example of the present invention.
Figure 3 shows the micrographs before and after passing through the high pressure homogenizer of the emulsion prepared according to an embodiment of the present invention.

Hereinafter, the present invention will be described in more detail.

The present invention is technically characterized in that rice bran wax, which is an excellent moisturizing cosmetic, is effectively stabilized without using a surfactant and used as a cosmetic.

Rice bran wax (Rice Bran Wax) is obtained by separating and refining rice bran oil from Oryza sativa L., and the main component is myricyl lignocerate. Pale yellow to brown flakes or lumps with a characteristic odor. As a surface film forming agent, it is used as a moisture evaporation barrier agent. In addition, it contains a large amount of antioxidants such as tocopherol and oryzanol, and contains active ingredients such as phytosterol and phospholipids, which can help strengthen the skin barrier and lower cholesterol. In addition, there is a paper stating that it does not go rancid easily due to its high antioxidant content and that compared to rice bran extract and vitamin C, the whitening effect due to the antioxidant effect is excellent. Korea, Vol.37, No.2, June 2011. 153 ~159)

According to the present invention, A) 10 to 50% by weight of rice bran wax and 0.1 to 5.0% by weight of isostearic acid by stirring and mixing the oil phase part at 70 to 80 ℃; B) mixing the aqueous phase part containing 0.1 to 0.5% by weight of a neutralizing agent and purified water at 70 to 80° C. by stirring; C) preparing a primary emulsion by mixing the oil phase part and the aqueous phase part and stirring with a homomixer; And D) passing the primary emulsion through a high pressure homogenizer (Micro Fluidizer) 2-3 times under a pressure of 1,000 to 1,500 bar and cooling to prepare a nano-emulsion There is provided a method of stabilizing rice bran wax.

First, a primary emulsion containing rice bran wax is prepared and stabilized using a liquid fatty acid and a neutralizer. Specifically, the oil phase part containing 10 to 50% by weight of rice bran wax and 0.1 to 5.0% by weight of isostearic acid, a liquid fatty acid, based on the total weight of the composition for preparing an emulsion is prepared by stirring and mixing at 70 to 80°C. In addition, the aqueous phase part containing 0.1 to 0.5% by weight of the neutralizing agent and purified water is prepared by stirring and mixing at 70 to 80 ℃. A primary emulsion is prepared by mixing the prepared oil phase part and water phase part and stirring with a homomixer. According to one embodiment of the present invention, the primary emulsion is prepared by stirring at 3,000 to 5,000 rpm for 10 to 20 minutes using a homomixer.

At this time, the rice bran wax is included in an amount of 10.0 to 50.0% by weight, preferably 20 to 40% by weight, based on the total weight of the composition for forming an emulsion. If the content of the rice bran wax is less than 10% by weight, it is difficult to exert the maximum activity, and if it exceeds 50% by weight, the feeling of use may deteriorate due to too much oily feeling, and formulation stability may be unstable.

Iso-stearic acid, a liquid fatty acid used for stabilizing rice bran wax, has a chemical formula of C ₁₈ H ₃₆ O ₂ and is a branched aliphatic acid having 18 carbons, and is saturated with lauric acid, palmitic acid, stearic acid, etc. Since fatty acids exist in a liquid phase at room temperature compared to a solid at room temperature, they have better stability at low temperatures and are adsorbed to the interface to provide a stable nanoemulsion.

The isostearic acid is included in an amount of 0.1 to 5.0% by weight, preferably 0.5 to 5.0% by weight, based on the total weight of the composition for forming an emulsion. At this time, if the content of isostearic acid is less than 0.1% by weight, emulsion stability may be problematic, and if it exceeds 5.0% by weight, precipitation may occur due to excess fatty acid, and there is a problem in that the feeling of use becomes heavy.

When at least one selected from the group consisting of tromethamine, triethanolamine, sodium hydroxide, potassium hydroxide and arginine is used as the neutralizing agent, tromethamine is preferably used.

The primary emulsion prepared in this way is passed through a high-pressure homogenizer (Micro Fluidizer) 2-3 times under a pressure of 1,000 to 1,500 bar and cooled to about 30° C. to prepare a nano-emulsion to further stabilize it.

The nanoemulsion prepared by the above stabilization method in which the primary emulsion is formed using isostearic acid, a liquid fatty acid, and tromethamine, a neutralizer, is treated with a high-pressure homogenizer, and exhibits a uniform particle size distribution, and contains a high content of rice bran wax. However, it showed excellent stability at low as well as high temperature.

The nanoemulsion may be contained in an amount of 0.1 to 90% by weight based on the total weight of the cosmetic composition. The cosmetic composition exhibits an excellent skin moisturizing effect and skin luster effect.

In the cosmetic composition, components included in conventional emulsified cosmetic compositions, that is, antioxidants, polyhydric alcohols, various vitamins, stimulants, softeners, fragrances, etc. may be selected and added to the cosmetic composition.

The cosmetic composition of the present invention may be prepared in any conventionally prepared formulation, for example, lotion, cream, essence, cleansing foam, cleansing water, pack, body lotion, body oil, body gel, shampoo, conditioner, hair conditioners, hair gels, foundations, lipsticks, mascaras, makeup bases, and the like.

[Example]

Hereinafter, the configuration and operation of the present invention will be described in more detail through preferred embodiments of the present invention. However, the following examples are provided to aid understanding of the present invention, and the scope of the present invention is not limited thereto.

Examples 1 to 3: Preparation of rice bran wax-stabilized nano-emulsion

According to the composition of Table 1 below, an oil-in-water nanoemulsion for stabilizing rice bran wax was prepared by the following method.

After measuring the raw materials in Table 1 below, the aqueous phase and oil phase parts were each stirred and mixed, and dissolved by heating to 75°C. The water phase part and the oil phase part were mixed and stirred at 3,000 rpm for 10 minutes using a homomixer to obtain an opaque liquid primary emulsion. Then, it passed through a high pressure homogenizer (Micro Fluidizer, M/F) three times under a pressure of 1,500 bar and cooled to 30° C. to obtain a nanoemulsion.

Comparative Examples 1 to 2: Preparation of rice bran wax-stabilized nano-emulsion

According to the composition of Table 1 below, an oil-in-water nanoemulsion for stabilizing rice bran wax was prepared in the same manner as in Examples.

Example 4: Preparation of rice bran wax stabilized emulsion

According to the composition of Table 1 below, an oil-in-water emulsion for stabilizing rice bran wax was prepared by the following method.

After measuring the raw materials in Table 1 below, the aqueous phase and oil phase parts were each stirred and mixed, and dissolved by heating to 75°C. The water phase part and the oil phase part were mixed and stirred at 3,000 rpm for 10 minutes using a homomixer to obtain an opaque liquid emulsion.

Comparative Example 3: Preparation of rice bran wax stabilized emulsion

According to the composition of Table 1 below, an oil-in-water emulsion for stabilizing rice bran wax was prepared by the following method.

After measuring the raw materials in Table 1 below, the aqueous phase and oil phase parts were each stirred and mixed, and dissolved by heating to 75°C. The water phase part and the oil phase part were mixed and stirred at 3,000 rpm for 10 minutes using a homomixer to obtain an opaque liquid emulsion.

division ingredient Example comparative example One 2 3 4 One 2 3 paid rice bran wax 30.0 30.0 30.0 30.0 30.0 30.0 30.0 propanediol 30.0 30.0 30.0 30.0 30.0 30.0 30.0 isostearic acid 0.5 2.0 5.0 2.0 0.05 - 10.0 stearic acid - - - - - 2.0 - tocopherol 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Awards tromethamine 0.01 0.2 0.5 0.2 0.1 0.2 1.0 pentylene glycol 2.0 2.0 2.0 2.0 2.0 2.0 2.0 Purified water To 100 To 100 To 100 To 100 To 100 To 100 To 100 M/F processing O O O X O O X

Test Example 1: Evaluation of properties and stability

The properties of the emulsions prepared in Examples and Comparative Examples were confirmed and shown in Table 2 below.

In addition, high-temperature stability and low-temperature stability were evaluated by the following method, and the results are shown in Table 2 below.

The high temperature stability was recorded by visual observation and microscopic observation of discoloration, discoloration, oxidation, and separation for 4 weeks at 45℃, and the low temperature stability was measured by visual inspection for discoloration, discoloration, oxidation, crystallization and precipitation at -10℃ for 4 weeks at -10℃. It was evaluated by observation and by observing and recording the particles under a microscope.

Example comparative example One 2 3 4 One 2 3 appearance milky white viscous liquid milky white viscous liquid milky white viscous liquid milk white
viscous fluid separation milk white
creamy milk white
creamy Particle size immediately after manufacturing (nm) 127 139 112 587 92, 321 114, 769 105, 534, 2459 High temperature stability result (4 weeks) Good Good Good Good separation Good Good Low temperature stability result (4 weeks) Good Good Good slightly suspended particle destruction particle destruction
(precipitation) particle destruction
(precipitation)

As shown in Table 2, as a result of measuring the particle size immediately after preparation, the Examples showed small and even particle distribution, while the Comparative Examples showed non-uniform particle size. Also, in Examples 1 to 4, the final milky white color A nanoemulsion type oil-in-water composition was prepared as a viscous liquid of After that, the particle size started to increase, and after 4 weeks, it was precipitated at low temperature. Comparative Example 3 became a high-viscosity creamy state immediately after emulsification, and emulsification by a high-pressure homogenizer could not proceed.

In addition, Example 4 has the same composition as Example 2, but a composition that does not pass through a high-pressure homogenizer, has good phase stability, but has a larger particle size than that treated with a high-pressure homogenizer, and has poor low-temperature stability.

Through these results, in order to obtain a composition containing a high content of rice bran wax, excellent stability at high and low temperatures, and a small emulsion particle size and uniformly distributed composition, isostearic acid, a liquid fatty acid, and tromethamine, a neutralizing agent, must be contained in a specific ratio. and high pressure homogenizer treatment was found to be important.

Test Example 2: Confirmation of particle distribution

The particle distribution immediately after the preparation of Examples and Comparative Examples is shown in FIGS. 1 and 2 , respectively. In addition, micrographs of particles before and after the emulsion of Example 2 passed through a high-pressure homogenizer are shown in FIG. 3 .

1 to 3, the nanoemulsions of Examples 1 to 3 prepared by forming a primary emulsion using isostearic acid, a liquid fatty acid, and tromethamine, a neutralizing agent, and then treating with a high-pressure homogenizer are fine and uniform. The particle size distribution is shown.

Formulation Example 1: Preparation of softening lotion

A softening lotion containing the nanoemulsion prepared in the above Example was prepared according to the composition of Table 3 below. Raw materials 1 to 8 were heated and mixed at 50°C. Raw materials 9 to 14 were put into a separate dissolution tank, completely dissolved, mixed, and finally, raw material 15 was added to uniformly disperse and aged for 1 day.

number ingredient content (wt%) function One Purified water To 100 solvent 2 Disodium EDITEA 0.01 sequestering agent 3 Butylene Glycol 10.00 moisturizer 4 glycerin 10.00 moisturizer 5 xanthan gum 0.05 thickener 6 hyaluronic acid 0.02 moisturizer 7 Citric Acid 0.01 pH regulator 8 sodium citrate 0.03 pH regulator 9 PEG-60 Hydrogenated Castor Oil 0.20 solubilizer 10 tocopherol 0.05 antioxidant 11 Phenoxyethanol 0.50 preservative 12 Ethylhexylglycerin 0.05 moisturizer 13 1,2-Hexanediol 0.50 moisturizer 14 incense 0.10 flavoring agent 15 Nanoemulsion (Example 2) 20.0 skin improver

Formulation Example 2: Lotion Preparation

A lotion containing the nanoemulsion prepared in the above Example was prepared according to the composition of Table 4 below. Raw materials 1 to 8 were heated and mixed at 85°C. Raw materials 9 to 16 were sequentially added, stirred at 3000 rpm for 10 minutes, cooled to 45° C., and raw materials 17 to 20 were sequentially added and sufficiently stirred.

number ingredient content (wt%) function One Purified water To 100 solvent 2 Disodium EDITEA 0.01 sequestering agent 3 Butylene Glycol 8.00 moisturizer 4 glycerin 5.00 moisturizer 5 xanthan gum 0.07 thickener 6 hyaluronic acid 0.01 moisturizer 7 Carbomer 0.05 thickener 8 tromethamine 0.05 pH adjuster 9 cetostearyl alcohol 1.50 softener 10 behenyl alcohol 1.20 softener 11 Glyceryl Monostearate 0.50 emulsifier 12 Hydrogenated Lecithin 0.20 emulsifier 11 Cyclopentasiloxane 1.00 preservative 13 squalane 0.50 softener 14 Neopentyl glycol diheptanoate 1.50 moisturizer 15 Hydrogenated Poly (C6-14 Olefin) 1.50 softener 16 tocopheryl acetate 0.20 antioxidant 17 1,2-Hexanediol 2.00 moisturizer 18 Ethylhexylglycerin 0.05 moisturizer 19 incense 0.10 flavoring agent 20 Nanoemulsion (Example 2) 20.0 skin improvement agent

Formulation Example 3: Preparation of water-in-oil cream

A water-in-oil cream containing the nanoemulsion prepared in the above Example was prepared according to the composition of Table 5 below. Raw materials 1 to 8 were heated and mixed at 85° C., and then raw materials 9 to 16 were sequentially added and stirred at 3000 rpm for 10 minutes. After cooling to 45° C., the raw materials 17 to 20 were sequentially added and sufficiently stirred.

number ingredient content (wt%) function One Purified water To 100 solvent 2 Disodium EDITEA 0.01 sequestering agent 3 Butylene Glycol 8.00 moisturizer 4 glycerin 5.00 moisturizer 5 xanthan gum 0.07 thickener 6 hyaluronic acid 0.01 moisturizer 7 Carbomer 0.05 thickener 8 tromethamine 0.05 pH adjuster 9 cetostearyl alcohol 3.00 softener 10 behenyl alcohol 2.00 softener 11 Glyceryl Monostearate 0.50 emulsifier 12 Hydrogenated Lecithin 1.00 emulsifier 11 Polyglyceryl-3 methylglucose distearate 2.00 preservative 13 squalane 5.00 softener 14 Neopentyl glycol diheptanoate 3.00 moisturizer 15 Hydrogenated Poly (C6-14 Olefin) 3.00 softener 16 tocopheryl acetate 0.20 antioxidant 17 1,2-Hexanediol 2.00 moisturizer 18 Ethylhexylglycerin 0.05 moisturizer 19 incense 0.20 flavoring agent 20 Nanoemulsion (Example 2) 10.0 skin improvement agent

Formulation Example 4: Oil-in-water cream preparation

An oil-in-water cream containing the nanoemulsion prepared in the above Example was prepared according to the composition of Table 6 below. Oil phase raw materials 7 to 11 were mixed in the main dissolution tank. After completely dissolving the raw materials 1 to 6 in a separate dissolution tank in order, the main dissolution tank is slowly stirred while stirring, and the mixture is stirred until the end while confirming that viscosity is formed. Then, raw material 12 was added and completed.

number ingredient content (wt%) function One Purified water To 100 solvent 2 Disodium EDIT 0.01 sequestering agent 3 allantoin 0.05 emollient 4 sodium chloride 0.80 stabilizer 5 Butylene Glycol 10.0 moisturizer 6 Nanoemulsion (Example 2) 20.0 skin improvement agent 7 Quaternium-18 Hectorite 1.50 thickener 8 Cyclodimethicone 10.0 softener 9 Sorbitan sesquioleate 0.50 emulsifier 10 Cyclopentasiloxane/dimethicone crosspolymer 2.00 softener 11 Cetyl PG / PG-10 Dimethicone 2.00 emulsifier 12 incense 0.20 flavoring agent

In general, when preparing an oil-in-water cream, it is not easy to apply a high-temperature melting point wax such as rice bran wax, but a cosmetic composition of an oil-in-water cream containing 6% rice bran wax could be easily and stably prepared.

Formulation Example 5: Shampoo Preparation

The shampoo containing the nanoemulsion prepared in the above Example was prepared in a conventional manner according to the composition of Table 7 below.

division content (wt%) function Purified water To 100 solvent Sodium Laureth Sulfate 30.00 Surfactants Sodium Lauryl Sulfate 15.00 Surfactants Lauryl Glucoside 10.00 Surfactants Sodium Cocoyl Glucoside 5.00 Surfactants Decyl Glucoside 2.00 Surfactants propanediol 1.00 moisturizer Poloxamer 407 0.70 thickener panthenol 0.50 skin improvement agent Polyquaternium-10 0.30 thickener hydroxyacetophenone 0.10 preservative Disodium EDIT 0.02 sequestering agent Spices 0.15 flavoring agent glycerin 0.50 moisturizer Nanoemulsion (Example 2) 10.00 skin improvement agent

Claims (6)

A) mixing the oil phase part containing 10 to 50% by weight of rice bran wax and 0.1 to 5.0% by weight of isostearic acid by stirring at 70 to 80° C.;
B) mixing the aqueous phase part containing 0.1 to 0.5% by weight of a neutralizing agent and purified water at 70 to 80° C. by stirring;
C) preparing a primary emulsion by mixing the oil phase part and the aqueous phase part and stirring with a homomixer; and
D) Passing the primary emulsion through a high pressure homogenizer (Micro Fluidizer) 2 to 3 times under a pressure of 1,000 to 1,500 bar, and cooling the rice bran wax stabilization method comprising the step of preparing a nano-emulsion. The method of claim 1, wherein the neutralizing agent is at least one selected from the group consisting of tromethamine, triethanolamine, sodium hydroxide, potassium hydroxide and arginine. A nanoemulsion prepared by the stabilization method of claim 1 or 2. A cosmetic composition in which the nanoemulsion of claim 3 is contained in an amount of 0.1 to 90% by weight based on the total weight of the cosmetic composition. [Claim 5] The cosmetic composition according to claim 4, wherein the cosmetic composition is for skin moisturizing. [Claim 5] The cosmetic composition according to claim 4, wherein the cosmetic composition is for skin luster.

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