KR100673786B1 - Emulsion type cosmetic compositions containing oil and emulsifier having fluorine - Google Patents

Abstract

The present invention relates to an emulsified cosmetic composition that can be effectively used in cosmetics by making oil phase and water phase containing fluorinated oil with a fluorinated emulsifier to form uniform, fine and highly stable emulsion particles using a high pressure homogenizer.

The emulsified composition of the present invention is made by emulsifying the fluorinated oil having a high moisturizing and protective effect on the skin with a fluorinated emulsifier and a high pressure device to make the emulsified particles small. It is excellent, and the composition ratio of a raw material can be changed widely compared with general emulsification, and various physical properties can be obtained, and it can use it suitably as a base of cosmetics. Therefore, the present invention has an effect of providing an emulsified cosmetic composition having excellent emulsification stability and good smooth feel and providing skin safety, excellent protection and moisturizing power.

Emulsifying Composition, Fluorine Oil, Emulsifier, High Pressure Homogenizer

Description

Emulsion type cosmetic compositions containing oil and emulsifier having fluorine}

The present invention relates to an emulsified cosmetic composition to which a fluorinated emulsifier is applied as an emulsifier using a high pressure homogenizer, and a method of manufacturing the same. More particularly, the present invention relates to an emulsified cosmetic composition which can be effectively used in cosmetics by making oil phase and water phase containing fluorinated oil with a fluorinated emulsifier to form uniform, fine and highly stable emulsion particles using a high pressure homogenizer.

In general, the general emulsified composition increases the stability of the oil phase, water, polyhydric alcohol, etc., in which oil phase components such as liquid paraffin, petrolatum, synthetic esters, higher fatty acids, higher alcohols, silicone oils, and lanolin derivatives are properly blended with viscosity and usability. Emulsion composition was prepared by selecting an appropriate emulsifier and emulsifying it with a conventional mixer by applying a water-soluble polymer as a thickener. Most of the raw materials used in the cosmetic composition is relatively safe for the skin because it is applied to the skin, and as the emulsifier, nonionic surfactants having relatively low skin irritation have been mainly used. However, when emulsifying with a general homomixer while applying a nonionic surfactant, it is difficult to make small and fine emulsion particles, and it is very difficult to apply to a low viscosity emulsion products (Patent No. 1990-007396).

Fluorine-based compounds generally have very unique properties. In other words, it has very strong hydrophobicity, thermal stability, oxidative stability is increased, and non-adhesiveness and very low friction property in terms of surface properties. Therefore, by using a compound having such properties in cosmetics, it is possible to make a product with a light feeling by using not only increased water resistance but also low frictional properties. However, since fluorine compounds have a very strong hydrophobicity, it is known that it is very difficult to prepare an emulsion that is insoluble in almost all solvents and is widely used in cosmetics. Was one of. The present inventors have conducted a lot of research to obtain an emulsion composition which is safe and safe for skin while using a small amount of fluorine-based emulsifier while the particles are uniform, fine and low viscosity. Among them, the most effective method is to use a fluorinated emulsifier as the main emulsifier and to use a high-pressure homogenizer to produce uniform and very fine emulsions of the desired quality, and to easily emulsify oily parts containing fluorinated oils. Can be. Fluorine-based emulsifiers are emulsifiers substituted with hydrogen of a general emulsifier, such as potassium perfuluro carboxylate, potassium perfuluroalkyl carboxylate perfuluroalkyl phosphate, trimethyl ammonium perfuluroalkylate, perfuluroalkyl betaine and Polyoxyethylene perpuluolo alcohol and the like. Fluorinated oils are perpulouropolymethylether, perfulurinated polyether or polyoxyperfuluroalkanes, and are currently being actively researched in artificial blood (Art. Cells, Blood Subs., And Immob.Biotech., 25 (1 & 2), 43-52 (1997)) Although fluorine-based emulsifiers are used industrially as fiber spinning agents, they are not yet used in cosmetics.

The present invention is based on the above facts, and the present inventors earnestly studied to solve the problems described above, and as a result, the emulsion cosmetic composition of the present invention contains 1 to 50% by weight of fluorinated oil as an oily component. The content of the fluorinated emulsifier is 0.5 to 5% by weight, and the content of the polyhydric alcohol and the aqueous phase component is 5 to 60% by weight for the purpose of reinforcing the emulsifying ability. Through the present invention was found to be stable, safe, moisturizing, excellent skin protection effect and good feeling to complete the present invention. The light feeling and skin protection effect of the emulsified cosmetic composition of the present invention can be inferred from the properties of the fluorine-based oil and has excellent moisturizing power by inhibiting the evaporation of moisture from the skin by forming a strong barrier film on the skin, In addition, the fluorine-based compound is very stable and can be used for artificial blood, and thus its safety can be predicted.

In general, the emulsified particle size in the emulsification is highly dependent on the ability to lower the interfacial tension by the emulsifier and the mechanical force during emulsification. However, fluorine compounds are more hydrophobic than ordinary oils and require a high pressure homogenizer with strong force.                     

Hereinafter, each component of the emulsion cosmetic composition of the present invention and a high pressure homogenizer (Homogenizer) which is a manufacturing method will be described in detail. The high pressure homogenizer is emulsified using a high pressure, and is first stirred with a general stirrer or a homomixer. It refers to the second emulsification by passing the emulsion through a high pressure homogenizer. At this time, the pressure is manufactured at a high pressure of 50 to 2500 atmospheres. The process of atomization of the particles is to pass the emulsion from a high pressure to an atmospheric pressure of 1 atmosphere. It refers to the process of making emulsified particles small by pressure fluctuation, cavitation, and impact force. As a method of preparing emulsions, it can be said that the homogenizer is 10,000 times larger than the general homomixer in terms of energy (Encyclopedia of Emulsion Technology, Vol 1 page 97 (1983)). As for the preferable pressure in this invention, it is suitable to let it pass at least once at 200-900 atmospheres. Here, the most preferable emulsion particle size distribution is about 100 ~ 300 micrometer (㎛) of the average size of the primary emulsified by the general homomixer, and after the primary emulsification by the general homomixer, the secondary emulsification is performed by the high pressure homogenizer method. If the average particle size is 1 ~ 10 ㎛ and the viscosity is equal to water or more than 10,000cps or less.

The oil phase component of the emulsified composition in the present invention is perfuluropolymethylether, perfulurinated polyether or polyoxyperfuluroalkane having a structural formula as follows, and an oil having a molecular weight of about 1500 to 7000 is used.

X-CH ₂ CF ₂ O- (CF ₂ CF ₂ O) p- (CF ₂ O) qCF ₂ CH ₂ -X

p / q = 0.5-3                     

X = -OH

-(OCH ₂ CH ₂ ) nOH

-(OCH ₂ CH ₂ ) nO-PO (OH) ₂ where n = 1-2

The emulsifier used in the present invention will be described in detail through Table 1 below.

Characteristics of Fluorine Emulsifiers rescue Potassium Perfulurocarboxylate Potassium perfluorofluoroalkyl carboxylate Perfluorouroalkyl phosphate Trimethylammoniumperfuluroalkylate Polyoxyethylene fur pullo alcohol Perpulouroalkyl betaine Specific gravity (25 ℃) 1.07 1.08 1.11 1.09 1.09 1.00 Kraft temperature (℃) 20 <0 <0 <0 <0 Surface Tension (0.01%) (0.1%) (dyne / cm, 25 ℃) 31.0 18.6 39.5 37.4 20.3 15.8 16.5 16.2 18.0 17.0 19.0 17.0 Interfacial Tension (0.1%) / Cyclohexane 10.5 37.1 10.9 10.2 8.8 9.8 Ionic nature Negative ion Negative ion Negative ion Cation Amphoteric Non-ion

In addition, examples of the aqueous phase component of the present invention include polyhydric alcohols such as ethylene glycol, glycerin, propylene glycol, 1.3.butylene glycol, dipropylene glycol, erythritol, sorbitol, lower alcohols such as ethyl alcohol and isopropyl alcohol, water, and the like. have.

To the emulsified cosmetic composition of the present invention, ingredients such as higher alcohols, higher fatty acids, vitamins, and other active ingredients, sunscreens, antioxidants, preservatives, fragrances, colorants, and the like, which are commonly used in cosmetics, can be added.
Examples and Comparative Examples

Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 Pupuloolo Polymethyletherel 30.0 30.0 30.0 30.0 30.0 30.0 30.0 Perpuluorinated polyether 30.0 30.0 Polyoxy perfluoroalkanes 30.0 30.0 30.0 30.0 Potassium Perfuluro Carboxylate 1.0 1.0 1.0 1.0 1.0 1.0 Potassium perfluorofluoroalkyl carboxylate 1.0 Perpulouroalkyl phosphate 1.0 Trimethylammonium Perfuluroalkylate 1.0 Polyoxyethylene Perfulo Alcohol 1.0 1.0 1.0 1.0 Squalane 20.0 Liquid paraffin 10.0 Polyoxyethylene (40) Cured Castor Oil 1.0 Purified water to 100 to 100 to 100 to 100 to 100 to 100 to 100 to 100 to 100 to 100 to 100 to 100 to 100 to 100 Concentrated glycerin 10.0 10.0 10.0 10.0 10.0 10.0 10.0 10.0 10.0 10.0 10.0 10.0 20.0 40.0 antiseptic q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. incense q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. q.s. High pressure device handling (bar) Processing Processing Processing Processing 400 400 600 900 400 400 400 400 400 400

In the preparation method of the embodiment, the fluorinated emulsifier and the fluorine oil are mixed at a weight ratio shown in Table 2 above, and heated and stirred at 50 ° C. to make it uniform. In a separate mixer, the water phase component is mixed in the weight ratio shown in Table 2 above, and the oil phase component having 50 ° C. is added to the water phase while stirring and warming to 50 ° C., followed by emulsification (primary emulsification) and cooling. Secondary emulsification passes through a high pressure homogenizer and the pressure is 50-2500 atm, usually at 500 atm once. In the preparation method of Comparative Example 1-3, the fluorinated emulsifier and the fluorine oil are mixed at the weight ratio shown in Table 2 above, and heated and stirred at 50 ° C to make it uniform. In a separate mixer, the water phase components are mixed in the weight ratio shown in Table 2 above, and the oil phase components having a temperature of 50 ° C. are added to the water phase while being heated and stirred at 50 ° C., emulsified and cooled.

stability

Stability evaluation was conducted at 50 ℃, 0 ℃, and cycle (-10 ℃ <1 day> → 45 ℃ <1 day> → -10 ℃ <1 day>…) for 1 month after observing the condition to separate oil and particles. The change in size and the like were evaluated.

Stability test result Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 50 ℃ × O △ O ◎ ◎ ◎ O O ◎ ◎ O ◎ ◎ 0 ℃ × O △ O O ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ Cycle × △ △ O △ ◎ ◎ O △ ◎ ◎ O ◎ ◎

◎ Very good O Good △ Slightly separated × Completely separated

Particle size distribution

The particle size and the degree of distribution were measured after preparation using a commonly used particle sizer machine.

Particle Average Size and Results Comparative Example / Example Particle Average Size (μm) Comparative Example 1 17 Comparative Example 2 30 Comparative Example 3 Dozens Comparative Example 4 3-6 Example 1 1-3 Example 2 2-5 Example 3 2-5 Example 4 3-5 Example 5 2-5 Example 6 2-5 Example 7 5 Example 8 2-5 Example 9 3-7 Example 10 2-5

As shown in Tables 3 and 4, the emulsion particles were also very large and unstable when prepared in a general manner as in Comparative Examples. The effect of pressure on the production of emulsions using homogenizers is that the higher the pressure, the more fine the particles and the more fluidized the emulsion.The higher the pressure, the smaller the particle size is. In consideration of this, preferably 500 atm is suitable.

Feeling

Forty to fifty panelists in their twenties to forties of the emulsified cosmetic composition prepared in Comparative Examples and Examples judged the feeling of use as a result of sensory evaluation by product evaluation.                     

 Usability evaluation result Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 grade 3.4 3.8 3.6 2.4 4.0 4.7 4.7 4.7 4.8 4.1 4.7 4.6 4.7 4.1

As shown in Table 5, even in the case of the comparative composition and the example, the preference was different depending on the presence and pressure of the high pressure treatment. The reason is that when the high pressure is not treated, the particles are large and the viscosity is high, which imposes a burden on the skin. However, the high pressure treated emulsion has fluidity and the particles are small and fine, so there is no burden on the skin. In addition, it showed an excellent usability advantage compared to the case of the general emulsion.

Moisturizing

Forty to twenty to forty panelists of the emulsified cosmetic composition prepared in Comparative Examples and Examples were evaluated for the moisturizing power by the product evaluation by the sensory evaluation as follows.

Moisturizing ability evaluation result Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 grade 4.0 3.9 3.8 2.3 4.5  4.1 4.0 4.2 4.3 4.2 4.0 4.2 4.9 4.9

As shown in Table 6, Comparative Examples 1, 2 and 3 prepared according to the general emulsification method showed a slightly lower level of moisturizing power than Example, but Comparative Example 4 and Examples showed a significant difference in moisturizing power.

safety

The stimulation such as edema was visually confirmed after 48 hours of application of 15 μg of each sample to the arms of 50 panelists in the 20s to 40s of the emulsion cosmetic composition prepared as in Comparative Examples and Examples.

Safety evaluation result Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 grade 0.06 0.1 0.08 0.08 0.02 0.02 0.02 0.02 0.0 0.04 0.0 0.02 0.02 0.04

Results of the safety evaluation of Table 7 Comparative Examples or Examples Although it is relatively safe for the skin, the examples prepared by the high pressure using a homogenizer was shown to be safer on the skin than the comparative examples prepared generally.

As can be seen through the above examples and comparative examples, the emulsion cosmetic composition of the present invention is a composition of emulsified fluorine-based oil having a high moisturizing, protective effect on the skin with a fluorine-based emulsifier and emulsified particles using a high pressure device It is made small and has excellent emulsification stability, safety on skin, usability in use, and moisturizing power. The composition ratio of raw materials can be changed in a wide range compared to general emulsification, so that various physical properties can be obtained. Therefore, the present invention has an effect of providing an emulsified cosmetic composition having excellent emulsification stability and good smooth feel and providing skin safety, excellent protection and moisturizing power.

Claims (4)

1 to 50% by weight of fluorinated oil, 0.5 to 5% by weight of fluorinated emulsifier, 5-60% by weight of polyhydric alcohol and purified water, and emulsified one or more times at 200 to 900 atmospheres using a high pressure homogenizer. Emulsified cosmetic composition. The emulsified cosmetic composition according to claim 1, wherein the fluorine-based oil is perfuluropolymethylether, perfulurinatedpolyether or polyoxyperfuluroalkane. The method of claim 1, wherein the fluorinated emulsifier is potassium perfuluro carboxylate, potassium perfuluroalkyl carboxylate, perfuluroalkyl phosphate, trimethyl ammonium perfuluroalkylate, perfuluroalkyl betaine or polyoxyethylen perfulo. Emulsified cosmetic composition, characterized in that the alcohol. The emulsion cosmetic according to any one of claims 1 to 3, wherein the average particle size of the emulsion cosmetic composition is 1 to 10 micrometers (µm) and the viscosity is equal to or higher than water and 10,000 cps or less. Composition.