KR101727527B1 - Manufacturing method of aqueous dispersions containing titanium dioxide and zinc oxide and cosmetic composition for protecting containing thereof - Google Patents

Abstract

The present invention relates to a process for preparing an aqueous dispersion of an inorganic ultraviolet screening agent and a cosmetic composition containing the same, and more particularly, to a process for preparing an aqueous dispersion of an inorganic ultraviolet screening agent, comprising a preliminary dispersing step of adding an inorganic ultraviolet screening agent to a dispersing agent- Dispersing the wetted water dispersion using a continuous bead mill of 0.05 to 5 mm, wherein the inorganic ultraviolet screening agent is titanium dioxide, zinc oxide or a mixture thereof, and the dispersant is a polyglyceryl- Rate, and the dispersion medium is purified water.
According to the present invention, it is possible to overcome disadvantages such as feeling of use and whitish appearance when titanium dioxide or zinc oxide itself is used as cosmetics such as hydrophilic type bibby cream, suncare, foundation and white cream. In addition, when the aqueous dispersion of titanium dioxide or zinc oxide according to the present invention is contained in the cosmetic composition, there is a useful effect that the ultraviolet ray shielding effect, stability and usability are excellent.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for preparing an aqueous dispersion of an inorganic sunscreen agent and a cosmetic composition containing the same, and a cosmetic composition containing the same. BACKGROUND ART < RTI ID = 0.0 >

The present invention relates to a process for producing an aqueous dispersion of an inorganic UV-blocking agent and a cosmetic composition containing the same, and more particularly to a cosmetic composition containing an inorganic UV-blocking agent such as titanium dioxide or zinc oxide, The present invention relates to a process for producing an aqueous dispersion of an inorganic UV-blocking agent and a cosmetic composition containing the same, which is excellent in stability, safety and usability, and is excellent in transparency by improving whiteness.

In general, ultraviolet rays are classified according to the wavelength and the effect on the human body, and if they are overexposed, they are known to cause various diseases and cancer. Ultraviolet rays are the ultraviolet rays (UV-A), which causes premature aging of the skin and blackening of the skin, the mid-wave ultraviolet (UV-B), which makes the skin burn, (UV-C) that is not transmitted to the ground by absorption of light by the ozone layer or directly destroying living organisms.

In the past, long wavelength ultraviolet light has been a welcome trend because of its high effectiveness in treating inflammation. Recently, it has been regarded as a boundary object by promoting skin aging by protein denaturation, capillary expansion and hexane (DNA) destruction.

On the other hand, the mid-wave ultraviolet rays, which are mostly absorbed in the epidermis of the skin, are called harmful ultraviolet rays because they rapidly act on the epidermis and cause burns. The long wavelength ultraviolet rays reach the skin all year round, but because they do not have any subjective symptoms, the skin becomes old without knowing oneself.

In ultraviolet cosmetics, an inorganic ultraviolet scattering agent and an organic ultraviolet absorbing agent are used as an ultraviolet screening agent.

Organic ultraviolet absorbers mainly absorb the mid-wave ultraviolet light, whereas inorganic ultraviolet light absorbers mainly scatter long-wavelength ultraviolet light. The ultraviolet absorber absorbs ultraviolet rays and protects the skin by changing energy such as reverse, vibration, fluorescence, and radical. On the other hand, ultraviolet scattering agents block ultraviolet rays by the refractive index of light of inorganic pigments.

Examples of the inorganic ultraviolet scattering agent include metal oxides such as titanium dioxide, zinc oxide, and cerium oxide, and their complexes. Of these, titanium dioxide and zinc oxide are popular.

The titanium dioxide exists in two structures, anatase and rutile, and the physical differences according to crystal structure and crystal structure are as follows. Anatase is a crystal in which crystal units are connected to each other at their vertexes, and Rutile is a crystal in which crystal units are connected to each other at their side edges.

Comparison of physical properties according to crystal structure of titanium dioxide division Anatase Rutile color Black, yellow, blue Black, reddish brown (coarse crystal), yellow (thin crystal) transparency opacity Transparency decision Tetragonal Tetragonal Stripe color White Brown Hardness 5.5 to 6 6 to 6.5 importance 3.8 to 3.9 4.2 Band Cap Energy 3.23 eV 3.02 eV Usage Photocatalytic material White paint, pigment

The titanium dioxide having the above physical properties is not only very physically stable but also has a very high refractive index of about 2.5 to 2.8 and a small particle size, and thus has excellent chemical properties such as whiteness, hiding power and tinting strength, Sunscreen, white cream, and base makeup products, it is possible to have a sunscreen effect and a skin correcting effect only by applying the skin.

In addition, when zinc oxide is used together, it enhances the advantages of titanium dioxide, and it also has excellent light, heat, and chemical resistance. Titanium dioxide and zinc oxide are hydrophilic type babe cream, suncare (sun cream, sun lotion etc.) And is widely used as a white pigment in a cosmetic composition containing an aqueous dispersion such as cream.

However, despite these effects, titanium dioxide and zinc oxide show a rough feeling when applied to cosmetics due to strong cohesion between the particles, and the whiteness of the titanium dioxide and zinc oxide indicates that the skin whitening phenomenon There is a problem that the application as a cosmetic is limited and the use and use amount thereof is limited.

In order to improve this, a stabilized oil dispersion of titanium dioxide and zinc oxide, which are inorganic ultraviolet screening agents, is prepared in Korean Patent No. 10-1210371 '' Method for producing stabilized oil dispersion of inorganic ultraviolet screening agent and cosmetic composition containing the same ' . In addition, a stabilized oil dispersion of titanium dioxide and zinc oxide was also prepared in Korean Patent No. 10-0758819, "High Concentration and High Dispersion Ultraviolet-shielding Composition ".

However, none of these prior art patents have produced stabilized oil dispersions, and no stabilized aqueous dispersions have been prepared. Therefore, until now, the application of titanium dioxide and zinc oxide to a hydrophilic type cosmetic composition still has a rough texture, a feeling of use and a whitish appearance.

KR 10-1210371 B1 KR 10-0758819 B1

Accordingly, it is an object of the present invention to overcome the above-described problems of using titanium dioxide and zinc oxide in a hydrophilic type cosmetic, and it is an object of the present invention to provide a titanium dioxide or a zinc oxide by using a bead mill to prepare polyglyceryl- And dispersing the titanium dioxide and the zinc oxide in a uniform particle size by preparing an aqueous dispersion in which the titanium dioxide and the zinc oxide are dispersed in purified water which is a dispersion medium.

In addition, titanium dioxide and zinc oxide are dispersed in a uniform particle size to improve the whiteness of an aqueous dispersion, improve transparency, and provide an aqueous dispersion of an inorganic sunscreen agent having excellent ultraviolet shielding effect and excellent stability, safety and usability And a cosmetic composition using the same.

The method for producing an aqueous dispersion of an inorganic UV-blocking agent according to the present invention comprises a preliminary dispersion step of adding an inorganic UV-ray shielding agent to a dispersion medium and a dispersion medium mixed solution and stirring the mixture with an agitation mixer to wet the aqueous dispersion, And dispersing the mixture using a bead mill apparatus, wherein the inorganic UV blocking agent is titanium dioxide, zinc oxide or a mixture thereof, the dispersing agent is polyglyceryl-4 caprate, and the dispersion medium is purified water .

The dispersing step may include a first dispersion step of dispersing the wet aqueous dispersion using a 0.2-0.5 mm bead mill apparatus and a second dispersion step of dispersing the primary dispersion aqueous dispersion using a 0.05-0.2 mm bead mill And a step of dispersing the particles.

The inorganic UV blocking agent is characterized by being titanium dioxide coated with hydrated silica, zinc oxide coated with triethoxycaprylylsilane, or a mixture thereof.

Wherein the stabilizer further comprises at least one stabilizer selected from the group consisting of butylene glycol, 1, 2-hexanediol, and caprylhydroxamic acid, and the antifoaming agent is simethicone .

Wherein the temperature of the preliminary dispersion step is 20 to 30 ° C, the temperature of the dispersion step is 30 to 40 ° C, and 1 to 400 parts by weight of the inorganic ultraviolet screening agent is mixed with 100 parts by weight of the dispersant and the dispersion medium mixture solution do.

The cosmetic composition according to the present invention is characterized by containing an aqueous dispersion prepared according to the above-described production method in an amount of 0.1 to 50% by weight based on the total weight of the cosmetic composition.

According to the present invention, it is possible to overcome disadvantages such as feeling of use and whitish appearance when titanium dioxide or zinc oxide itself is used as cosmetics such as hydrophilic type bibby cream, suncare, foundation and white cream.

In addition, when the aqueous dispersion of titanium dioxide or zinc oxide according to the present invention is contained in the cosmetic composition, there is a useful effect that the ultraviolet ray shielding effect, stability and usability are excellent.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a process chart for producing an aqueous dispersion of an inorganic UV blocking agent according to the present invention. FIG.
2 is a view showing a coating method of titanium dioxide according to the present invention.
3 is a view showing a coating method of zinc oxide according to the present invention.
4 is a SEM photograph of Example 1 according to the present invention.
5 is a SEM photograph of Example 2 according to the present invention.
6 is a SEM photograph of Comparative Example 1 according to the present invention.
7 is a SEM photograph of Comparative Example 2 according to the present invention.
8 is a graph showing a particle distribution diagram of Example 1 according to the present invention.
9 is a graph showing a particle distribution diagram of Example 2 according to the present invention.
10 is a graph showing a particle distribution diagram of Comparative Example 1 according to the present invention.
11 is a graph showing a particle distribution diagram of Comparative Example 2 according to the present invention.
12 is a photograph showing the stability after 90 days in RT of Example 1 and Comparative Example 1 according to the present invention.
13 is a photograph showing stability after 90 days in RT of Example 2 and Comparative Example 2 according to the present invention.
14 is a graph of ultraviolet blocking index of Formulation Example 1 according to the present invention.
FIG. 15 is a graph of UV blocking index of Comparative Formulation Example 1 according to the present invention. FIG.
16 is a graph of UV blocking index of Formulation Example 2 according to the present invention.
FIG. 17 is a graph of UV blocking index of Comparative Formulation Example 2 according to the present invention. FIG.
FIG. 18 is a graph of UV blocking index of Formulation Example 3 according to the present invention. FIG.
FIG. 19 is a graph of UV blocking index of Comparative Formulation Example 3 according to the present invention. FIG.
Fig. 20 is a graph of UV blocking index of Formulation Example 4 according to the present invention. Fig.
FIG. 21 is a graph showing UV blocking index of Comparative Formulation Example 4 according to the present invention. FIG.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will now be described in detail with reference to the accompanying drawings.

The method for producing an aqueous dispersion of an inorganic sunscreen agent according to the present invention comprises the steps of: adding an inorganic ultraviolet screening agent to a dispersing agent and a dispersion medium mixed solution and stirring the same with an agitator to wet the dispersion; Wherein the inorganic UV-blocking agent is titanium dioxide, zinc oxide or a mixture thereof, the dispersing agent is polyglyceryl-4-caprate, and the dispersion medium is Purified water.

More preferably, the dispersing step comprises a first dispersion step of dispersing the wet aqueous dispersion using a 0.2-0.5 mm bead mill, and a first dispersion step of dispersing the first dispersion aqueous dispersion using a 0.05-0.2 mm bead mill And a second dispersion step of dispersing the dispersion liquid.

Here, the preliminary dispersion step and the primary and secondary dispersion steps can be performed automatically as the system shown in FIG. And, the bead mill device used in the dispersion step is an apparatus for dispersing high energy, and can operate a continuous cooling system. The reason why the bead mill device is used in the range of 0.05 to 5 mm is that the smaller the size of the bead is, the more the undifferentiated acid becomes, and the speed is preferably 1200 to 1800 rpm. This is because, if the speed is out of the above range, the product is not separated evenly and the separation phenomenon of the product occurs. It is more preferable to use a bead mill apparatus of 0.2 to 0.5 mm for primary dispersion and a bead mill apparatus of 0.05 to 0.2 mm for secondary dispersion for uniform dispersion.

Herein, the inorganic ultraviolet screening agent may be titanium dioxide, zinc oxide or a mixture thereof, as well as coated titanium dioxide, zinc oxide or a mixture thereof.

At this time, it is preferable that the titanium dioxide is hydrate silica and the zinc oxide is triethoxycaprylylsilic acid because the coating can produce a more excellent aqueous dispersion.

As shown in FIG. 2, 100 parts by weight of titanium dioxide and 200 to 400 parts by weight of water are mixed and dispersed, and 20 to 30 parts by weight of hydrated silica is mixed with the hydrate silica. (300 to 400 rpm, stirring for 1 hour), washed twice, dried at 60 DEG C for 3 days, and atomized at 10,000 to 15,000 rpm to obtain titanium dioxide coated with hydrated silica.

As a method of coating zinc oxide with triethoxycaprylylsilic acid, zinc oxide is dissolved by dissolving metal zinc, vaporized and oxidized to prepare zinc oxide, and then zinc oxide is subjected to acid leaching, precipitation reaction, filtering and drying , And heat-treated to produce activated zinc oxide. Then, 100 parts by weight of the activated zinc oxide is surface-treated with 3 to 5 parts by weight of triethoxycaprylylsilane, milled and dried, and finely divided to obtain zinc oxide coated with triethoxycaprylylsilic acid .

The method of coating these particles is well known in the field to which this technique belongs, and therefore, a detailed description thereof will be omitted.

And a stabilizer and an antifoaming agent in the preliminary dispersion step, wherein the stabilizer is at least one selected from the group consisting of butylene glycol, 1, 2-hexanediol, and caprylhydroxamic acid, There is no restriction, however.

It is preferable that the temperature of the preliminary dispersion step is 20 to 30 ° C and the temperature of the dispersion step is 30 to 40 ° C because the modification of the coating material of the inorganic UV- Thereby causing the final product to discolor and turn off, thereby keeping the temperature constant.

The inorganic ultraviolet screening agent may be blended in an amount of 1 to 400 parts by weight of the inorganic ultraviolet screening agent per 100 parts by weight of the dispersing agent and the dispersion medium mixed solution. The stabilizing agent may be added in an amount of 1 to 20 parts by weight and the defoaming agent may be added in an amount of 1 to 20 parts by weight If the amount of the inorganic ultraviolet screening agent is too small, the ultraviolet screening agent will not act as an ultraviolet screening agent. If the amount is too large, dispersion will not occur easily.

In addition, since the dispersion step can be repeated two or more times, a more uniform dispersion can be produced by dispersion over a plurality of times.

On the other hand, the stabilized aqueous dispersion prepared by the same method as described above can be incorporated into a hydrophilic type bibby cream, sun cream, foundation, sun care, whitening cream and makeup cosmetic composition. By weight, which is a content considering the formulation, spreadability, etc. of the cosmetic composition.

Hereinafter, the present invention will be described in more detail with reference to the following Examples and Test Examples.

(Example 1) Preparation of aqueous dispersion type titanium dioxide

First, fine particle titanium dioxide having an average particle diameter of 10 mu m was coated as in the process of Fig. As a treatment method thereof, 100 g of the titanium dioxide was dispersed in 300 g of water, 24 g of hydrated silica was added thereto, and the mixture was stirred at 400 rpm for 1 hour and washed twice. After that, Dried, and atomized at 10,000 to 15,000 rpm to obtain coated titanium dioxide.

Then, 41 g of the obtained titanium dioxide was mixed with 5 g of polyglyceryl-4 caprate as a dispersant, 1.5 g of butylene glycol, a stabilizer, 1.5 g of 1-2 hexanediol, 1.5 g of caprylhydroxamic acid, g and purified water of 47.85 g. The mixture was thoroughly agitated and dispersed with an agitator, followed by primary dispersion with a 0.3 mm automatic bead mill, followed by secondary dispersion with a 0.1 mm automatic bead mill to prepare aqueous dispersion titanium dioxide. Here, the temperature at the time of stirring and the temperature at the time of primary and secondary bead mill dispersion were both 30 占 폚 in an agitator.

(Example 2) Production of water dispersible zinc oxide

First, fine particle zinc oxide having an average particle diameter of 10 mu m was coated as in the process of Fig. As the treatment method, 48 g of zinc oxide was activated by acid leaching, precipitation reaction, filtering, drying and heat treatment, and the activated zinc oxide was surface-treated with 2 g of triethoxycaprylylsilic acid, and milled, Zinc oxide was obtained.

Then, 50 g of the obtained zinc oxide was mixed with 7 g of polyglyceryl-4 caprate as a dispersant, 2 g of butylene glycol, a stabilizer, 2 g of 1-2 hexanediol, 2 g of caprylhydroxamic acid, 2.2 g of a defoamer, 34.8 g, and dispersed sufficiently with an agitator to disperse the dispersion. The dispersion was firstly dispersed with a 0.3 mm automatic bead mill and then dispersed with a 0.1 mm automatic bead mill to prepare dispersed zinc oxide. Here, the temperature at the time of stirring and the temperature at the time of primary and secondary bead mill dispersion were both 30 占 폚 in an agitator.

(Comparative Example 1)

The same procedure as in Example 1 was carried out, but without using a continuous automatic bead mill, the titanium dioxide water dispersion was prepared by homogeneously dispersing with an agitator at 1,800 to 2,000 rpm for about 2 to 3 hours.

(Comparative Example 2)

A zinc oxide aqueous dispersion was prepared in the same manner as in Example 2 except that the continuous automatic bead mill was not used and uniformly dispersed in an agitator at 18,000 to 2,000 rpm for about 2 to 3 hours.

(Test Example 1)

In order to confirm the dispersion state of the titanium dioxide and zinc oxide aqueous dispersion according to the present invention, the above Examples 1 and 2 and Comparative Examples 1 and 2 were observed with an electron microscope. The results are shown in Figs. 4 to 7 (Fig. 4 is a SEM photograph of Example 1, Fig. 5 is a SEM photograph of Example 2, Fig. 6 is Comparative Example 1, and Fig. 7 is a SEM photograph of Comparative Example 2). As can be seen from Figs. 4 to 7, the dispersion states of Comparative Example 1 and Comparative Example 2 in which bead mills were not used were not complete, and it was confirmed that a part of titanium dioxide and zinc oxide particles were aggregated. On the other hand, it was confirmed that the dispersion state of Examples 1 and 2 treated with bead mill was remarkably improved.

8 to 11 are graphs of particle distribution diagrams of Examples 1 and 2 and Comparative Examples 1 and 2. It can be seen that the particles of Examples 1 and 2 are uniformly dispersed and smaller in size than Comparative Examples 1 and 2 there was.

(Test Example 2)

The stability of Example 1 and Example 2 were tested as follows. The aqueous dispersions of Examples 1 and 2 and Comparative Examples 1 and 2 were mixed at room temperature (RT), 4 占 폚, CT (Cycling Test: -4 to +40 占 폚 once a day), 37 占 폚, 50 占 폚 After 90 days of storage, the stability was visually measured. The experimental results are shown in the following Table 2 and Figs. 12 and 13 (Fig. 12 is a comparative photograph of Example 1 and Comparative Example 1, and Fig. 13 is a comparative photograph of Example 2 and Comparative Example 2).

Test results of Test Example 2. division
7 days 30 days 90 days Example 1 Comparative Example 1 Example 2 Comparative Example 2 Example 1 Comparative Example 1 Example 2 Comparative Example 2 Example 1 Comparative Example 1 Example 2 Comparative Example 2 RT ○ ○ ○ ○ ○ △ ○ △ ○ × ○ × 4 ℃ ○ ○ ○ ○ ○ △ ○ △ ○ × ○ × CT ○ △ ○ △ ○ × △ × ○ × △ × 37 ℃ ○ △ ○ × ○ × ○ × ○ × ○ × 50 ℃ ○ × ○ × ○ × ○ × ○ × ○ ×

?: Stable,?: Slightly separated, X: Separated

As can be seen from the above Table 2 and FIGS. 12 and 13, it can be confirmed that the cells of Examples 1 and 2 were stable for 90 days or more than those of Comparative Examples 1 and 2.

(Test Example 3)

To evaluate the skin irritation related to the safety of the composition according to the present invention, a human skin patch test was conducted. Propylene glycol and purified water were sprayed for 24 hours in a predetermined amount (about 40 占 퐂) as the aqueous dispersions of Examples 1 and 2 and Comparative Examples 1 and 2 and the control group, respectively, at the upper bosom of 30 healthy women. Subsequently, the skin irritation was measured by removing it, and the skin reaction was again examined after 24 hours and 48 hours. The criteria for skin irritation and the degree of irritation are as follows, and the results are shown in Table 3 below.

Criteria - - No erythema or specific symptoms

+ -: slightly reddish from the surroundings

+: Significantly reddened than surrounding

++: more reddened and bulging than ambient

(Stimulus calculation formula)

Test results of Test Example 3. division Number of subjects When Judgment result Stimulus (%)
++ + + - - Example 1

30 people Immediately after removal 0 people 0 people 1 person 29 people 3.33 30 people After 24 hours 0 people 0 people 2 people 28 people 6.67 30 people After 48 hours 0 people 0 people 2 people 28 people 6.67 Example 2

30 people Immediately after removal 0 people 0 people 1 person 29 people 3.33 30 people After 24 hours 0 people 0 people 1 person 29 people 3.33 30 people After 48 hours 0 people 0 people 2 people 28 people 6.67 Comparative Example 1

30 people Immediately after removal 0 people 0 people 2 people 28 people 6.67 30 people After 24 hours 0 people 1 person 1 person 28 people 9.68 30 people After 48 hours 0 people 0 people 2 people 28 people 6.67 Comparative Example 2

30 people Immediately after removal 0 people 0 people 2 people 28 people 6.67 30 people After 24 hours 0 people 1 person 1 person 28 people 9.68 30 people After 48 hours 0 people 0 people 2 people 28 people 6.67 Propylene glycol 30 people Immediately after removal 0 people 2 people 4 people 26 people 25.00 30 people After 24 hours 0 people 2 people 4 people 26 people 25.00 30 people After 48 hours 0 people 2 people 4 people 26 people 25.00 Purified water

30 people Immediately after removal 0 people 0 people 0 people 29 people 0.00 30 people After 24 hours 0 people 0 people 0 people 30 people 0.00 30 people After 48 hours 0 people 0 people 0 people 30 people 0.00

As can be seen from the above Table 3, the aqueous dispersion of the present invention proved to have little skin irritation.

(Formulation Example 1 and Comparative Formulation Example 1)

Formulation Example 1 and Comparative Formulation Example 1 were made into formulations of Bibi Cream (whitening, wrinkle-functioning, SPF 50+, PA ++++) with the prescription shown in Table 4 below.

Formulation Example 1 and Comparative Formulation Example 1 Raw material name Formulation Example 1 Comparative Formulation Example 1 The aqueous dispersion of Comparative Example 1 0 10 The aqueous dispersion of Comparative Example 2 0 10 The aqueous dispersion of Example 1 10 0 The aqueous dispersion of Example 2 10 0 To a solution of < RTI ID = 0.0 & 7.5 7.5 Bis-ethylhexyloxyphenol methoxyphenyltriazine 2 2 Octocrylene 2 2 Cetearyl alcohol 1.5 1.5  Polyglyceryl-3 methyl glucoside distearate 2 2 Glyceryl stearate / phage-100 stearate 1.5 1.5 Cyclopentasiloxane / cyclohexasiloxane 8 8 Dimethicone 0.5 0.5  Hydrogenated coconut oil One One Cyclomethicone / dimethicone crosspolymer 0.5 0.5 Tocopheryl acetate 0.1 0.1 Disodium iodide 0.05 0.05 Arbutin 2.0 2.0 Adenosine 0.04 0.04 Allantoin 0.1 0.1 Panthenol 0.1 0.1 Butylene glycol 5 5 glycerin 2 2 Betaine 0.5 0.5 1,2-hexanediol / butyleneglycol / caprylic hydroxamic acid 0.8 0.8 Sodium hyaluronate / phenoxyethanol One One  Phenoxyethanol 0.25 0.25 Sodium acrylate / sodium acryloyldimethyltaurate copolymer / isohexadecane / polysorbate 80 1.5 1.5 Spices 0.25 0.25 Black iron oxide 0.25 0.25 Yellow iron oxide 0.6 0.6 Red iron oxide 0.25 0.25 Purified water 38.71 38.71

(Formulation Example 2 and Comparative Formulation Example 2)

Formulation Example 2 and Comparative Formulation Example 2 were formulated into sunflower (SPF 50+, PA ++++) formulations as shown in Table 5 below.

Formulation Example 2 and Comparative Formulation Example 2 Raw material name Formulation Example 2 Comparative Formulation Example 2 The aqueous dispersion of Comparative Example 1 0 10 The aqueous dispersion of Comparative Example 2 0 15 The aqueous dispersion of Example 1 10 0 The aqueous dispersion of Example 2 15 0 To a solution of < RTI ID = 0.0 & 7.5 7.5 Bis-ethylhexyloxyphenol methoxyphenyltriazine 2.5 2.5 Octocrylene 2.5 2.5 Cetearyl alcohol 1.5 1.5  Polyglyceryl-3 methyl glucoside distearate 2 2 Glyceryl stearate / phage-100 stearate 1.5 1.5 Cyclopentasiloxane / cyclohexasiloxane 8 8 Dimethicone 0.5 0.5  Hydrogenated coconut oil One One Cyclomethicone / dimethicone crosspolymer 0.5 0.5 Tocopheryl acetate 0.1 0.1 Disodium iodide 0.05 0.05 Allantoin 0.1 0.1 Panthenol 0.1 0.1 Butylene glycol 5 5 glycerin 2 2 Betaine 0.5 0.5 1,2-hexanediol / butyleneglycol / caprylic hydroxamic acid 0.8 0.8 Sodium hyaluronate / phenoxyethanol One One  Phenoxyethanol 0.25 0.25 Sodium acrylate / sodium acryloyldimethyltaurate copolymer / isohexadecane / polysorbate 80 1.2 1.2 Spices 0.25 0.25 Purified water 36.15 36.15

(Formulation Example 3 and Comparative Formulation Example 3)

Formulation Example 3 and Comparative Formulation Example 3 were formulated into formulations (whitening, wrinkle-improving, SPF 50+, PA ++++) with the prescription as shown in Table 6 below.

Formulation Example 3 and Comparative Formulation Example 3 Raw material name Formulation Example 3 Comparative Formulation Example 3 The aqueous dispersion of Comparative Example 1 0 20 The aqueous dispersion of Comparative Example 2 0 5 The aqueous dispersion of Example 1 20 0 The aqueous dispersion of Example 2 5 0 To a solution of < RTI ID = 0.0 & 7.5 7.5 Bis-ethylhexyloxyphenol methoxyphenyltriazine 3 3 Octocrylene One One Cetearyl alcohol 2.5 2.5  Polyglyceryl-3 methyl glucoside distearate 2 2 Glyceryl stearate / phage-100 stearate One One Cyclopentasiloxane / cyclohexasiloxane 7 7 Dimethicone One One  Hydrogenated coconut oil 2 2 Cyclomethicone / dimethicone crosspolymer 0.5 0.5 Tocopheryl acetate 0.1 0.1 Disodium iodide 0.05 0.05 Arbutin 2.0 2.0 Adenosine 0.04 0.04 Allantoin 0.1 0.1 Panthenol 0.1 5 Butylene glycol 5 4 glycerin 4 0.5 Betaine 0.5 0.5 1,2-hexanediol / butyleneglycol / caprylic hydroxamic acid 0.8 0.8 Sodium hyaluronate / phenoxyethanol One One  Phenoxyethanol 0.25 0.25 Sodium acrylate / sodium acryloyldimethyltaurate copolymer / isohexadecane / polysorbate 80 1.2 1.2 Spices 0.25 0.25 Black iron oxide 0.25 0.25 Yellow iron oxide 0.7 0.7 Red iron oxide 0.3 0.3 Purified water 30.46 30.46

(Formulation Example 4 and Comparative Formulation Example 4)

Formulation Example 4 and Comparative Formulation Example 4 were prepared in the form of a white cream (whitening, SPF 10, PA ++) in the formulations shown in Table 7 below.

Formulation Example 4 and Comparative Formulation Example 4 Raw material name Formulation Example 4 Comparative Formulation Example 4 The aqueous dispersion of Comparative Example 1 0 10 The aqueous dispersion of Comparative Example 2 0 One The aqueous dispersion of Example 1 10 0 The aqueous dispersion of Example 2 One 0 Arbutin 2 2 Cetearyl alcohol 2.5 2.5  Polyglyceryl-3 methyl glucoside distearate 2 2 Glyceryl stearate / phage-100 stearate One One Squalane 2 2 Cetyl hexanoate 3 3 Caprylic / capric triglyceride 2 2 Meadow Foam Seed Oil 2 2 Cyclopentasiloxane / cyclohexasiloxane 4 4 Dimethicone One One  Hydrogenated coconut oil One One Tocopheryl acetate 0.1 0.1 Disodium iodide 0.05 0.05 Allantoin 0.1 0.1 Panthenol 0.1 0.1 Butylene glycol 5 5 glycerin 5 5 Betaine 0.5 0.5 1,2-hexanediol / butyleneglycol / caprylic hydroxamic acid 0.8 0.8 Sodium hyaluronate / phenoxyethanol One One  Phenoxyethanol 0.25 0.25 Sodium acrylate / sodium acryloyldimethyltaurate copolymer / isohexadecane / polysorbate 80 One One Spices 0.25 0.25 Purified water 52.35 52.35

(Test Example 4)

In order to observe the effect of the improvement of the transparency of the titanium dioxide and zinc oxide aqueous dispersion according to the present invention on the reduction of the whitish phenomenon, the whitening phenomenon of the cosmetic composition of Example 1, Comparative Example 1, Formulation Example 2 and Comparative Formulation Example 2 Were measured.

In the measurement method, 0.50 g of each of Example 1, Comparative Example 1, Formulation Example 2 and Comparative Formulation Example 2 was uniformly applied (30 mu m) to a transparent glass plate and black artificial leather, (L: 24.27, a: -0.20, b: -0.43) for measuring the degree of concealment, and then measured for whiteness using a color limiter. The experimental results are shown in Table 8 below.

Lab is an international standardized color system standardized by CIE (Commission Internationale del'Eclairage, International Lighting Commission). L value refers to lightness which is bright and dark. The value a means the relationship between green and red. If you go to the negative side, it means green. If you go toward the positive side, it means red. The value b means blue and yellow. If you go towards negative, it means blue. Here, the larger the value of L, the stronger the opacity is, and the darker the background, the closer it is to white.

Test results of Test Example 4. division Example 1 Comparative Example 1 Formulation Example 2 Comparative Formulation Example 2 L 43.22 46.51 38.18 40.79 a +0.85 +0.25 +0.51 +0.18 b -6.01 -3.04 -4.26 -2.00

As can be seen from the above Table 8, it was confirmed that the whitening effect of the cosmetic composition of Formulation Example 2 was improved compared with the cosmetic composition of Comparative Formulation Example 2, and the whitening effect was greatly reduced.

(Test Example 5)

In general, titanium dioxide on a powder is a material having a high hiding power due to a high refractive index of about 2.5 to 2.8 and a very small particle size, and when it is contained in a product such as bibby cream, suncare (sunscreen and the like), foundation and white cream, The UV protection effect is obtained only by application.

To confirm whether titanium dioxide or zinc oxide dispersed in polyglyceryl-4 caprate as a dispersant according to the present invention and purified water as a dispersion medium exhibit the same effect as above, a transparent plastic tape (Transpore Tape; 3M, USA) After applying the cosmetic composition of Forms 1 to 4 and Comparative Formulation Examples 1 to 4 at a dose of 2 mg / cm 2, the ultraviolet blocking effect was measured with a UV detector (SPF 290 Analyzer). The results are shown in Table 9 and Figs. 14 to 21 (Fig. 14 shows Formulation Example 1, Fig. 15 shows Comparative Formulation Example 1, Fig. 16 shows Formulation Example 2, Fig. 17 shows Comparative Formulation Example 2, 19 is Comparative Formulation Example 4, Fig. 20 is Formulation Example 4, and Fig. 21 is a measurement result of Comparative Formulation Example 4).

Test results of Test Example 5. division Formulation Example 1 compare
Formulation Example 1 2 Formulation Example compare
Formulation Example 2 Formulation Example 3 compare
Formulation Example 3 Formulation Example 4 compare
Formulation Example 4 SPF Value 55.31 45.03 55.96 46.83 50.78 43.1 9.92 7.02 PA value ++++
(33.66) ++++
(22.65) ++++
(30.42) ++++
(23.87) ++++
(22.78) ++
(5.55) ++
(5.55) ++ (4.17)

From the results of Table 9 and Figs. 14 to 21, it can be seen from the results of Table 9 and Figs. 14 to 21 that in the case of the formulation according to the present invention, ultraviolet ray blocking index is about 15.0-20.0% higher than that of the comparative formulation containing powder- And the blocking index was high.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the same is by way of illustration and example only and is not to be construed as limiting the scope of the present invention. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.

Claims (6)

A preliminary dispersing step of adding an inorganic ultraviolet screening agent to a dispersing agent and a dispersion medium mixed solution, stirring the same with an agitator to effect wetting,
And a dispersing step of dispersing the wetted water dispersion using a continuous bead mill of 0.05 to 5 mm,
The inorganic ultraviolet screening agent may be selected from the group consisting of titanium dioxide, zinc oxide, a mixture of titanium dioxide and zinc oxide, titanium dioxide coated with hydrated silica, zinc oxide coated with triethoxycaprylylsilane, disodium dioxide coated with hydrated silica A mixture of zinc oxide coated with titanium and triethoxycaprylylsilane,
The dispersant is polyglyceryl-4 caprate,
Wherein the dispersion medium is purified water,
Wherein the dispersing step comprises:
A primary dispersion step of dispersing the wet aqueous dispersion using a 0.2-0.5 mm bead mill apparatus and a secondary dispersion step of dispersing the primary dispersion aqueous dispersion using a 0.05-0.2 mm bead mill In addition,
A stabilizer and an antifoaming agent in said preliminary dispersion step,
Wherein the stabilizer is at least one of butylene glycol, 1, 2-hexanediol, and caprylhydroxamic acid, and the antifoaming agent is simethicone.
delete delete delete The method according to claim 1,
Wherein the temperature of the preliminary dispersion step is 20 to 30 ° C, the temperature of the dispersion step is 30 to 40 ° C, and 1 to 400 parts by weight of the inorganic ultraviolet screening agent is mixed with 100 parts by weight of the dispersant and the dispersion medium mixture solution By weight based on the total weight of the aqueous ultraviolet absorber.
The cosmetic composition according to any one of claims 1 to 5, wherein the aqueous dispersion is contained in an amount of 0.1 to 50% by weight based on the total weight of the cosmetic composition.

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