KR102203667B1 - Sunscreen composition providing improved skin coverage and cosmetic composition containing the same - Google Patents

Abstract

The present invention relates to a technology for preparing a UV-blocking composition with improved UV-blocking and skin coverage using titanium dioxide particles having a particle diameter of 50-100 nm, and using the same as a cosmetic, and according to the present invention, titanium having a particle diameter of 50-100 nm A sunscreen composition comprising 30.0 to 50.0 wt% of dioxide, 1.0 to 10.0 wt% of alkyl silane, 30.0 to 50.0 wt% of silicone oil, and 10.0 to 20.0 wt% of a surfactant and a sunscreen cosmetic composition containing the same Is provided.

Description

Sunscreen composition providing improved skin coverage and cosmetic composition containing the same}

The present invention relates to a composition for blocking UV rays with improved skin coverage and a cosmetic composition containing the same, and specifically, to prepare a composition with improved UV protection and skin coverage by using fine particle titanium dioxide having a particle diameter of 50 to 100 nm, It relates to the technology used as.

Inorganic sunscreens are widely used in sunscreen cosmetic compositions because they have a high sunscreen effect. However, when applied, consumers have felt uncomfortable when using it because it causes a stiff feeling and cloudiness in the skin. Accordingly, microparticle inorganic UV blockers have been developed and used to block UV rays, improve whiteness, and improve feeling of use. In particular, titanium dioxide (TiO ₂ ) is classified into pigments, sunscreens, and particulate sunscreens according to their size.

In recent years, titanium dioxide for UV protection is used as raw materials of 50 nm or less to improve the feeling of use, prevent whitening, and improve UV protection efficacy, but there is a problem that it does not exhibit satisfactory skin coverage when used as a cosmetic. Therefore, it is cumbersome and has the disadvantage of thickening the makeup since it is necessary to use makeup cosmetics again after applying sunscreen. Accordingly, in recent years, attempts have been made to use pigment-grade titanium dioxide in a cosmetic composition for UV protection to improve skin coverage along with UV protection effect, but dispersion was difficult due to the high content. When preparing a titanium dioxide dispersion as an inorganic UV blocking agent, dispersion was performed using a three-stage roll mill or a continuous bead mill, but it was difficult to secure long-term stability through this.

Therefore, the present inventors prepared a composition for UV protection with excellent skin coverage and UV protection effect, and in a research process for using it as a cosmetic, various dispersion methods were applied to various sizes of dispersants to prepare a UV protection composition. As a result, when fine particles of titanium dioxide having a particle diameter of 50 to 100 nm are coated and dispersed with a ring mill-type batch bead mill, a UV-blocking composition that improves skin coverage and maintains an excellent UV-blocking effect for a long time can be obtained. By confirming the present invention was completed.

(001) Korean Patent Publication No. 10-2010-0013719 (2010.02.10.) (002) Korean Patent Application Publication No. 10-2016-0144779 (December 16, 2016)

An object of the present invention is to provide a composition for blocking ultraviolet rays having excellent skin coverage and maintaining ultraviolet blocking capacity for a long time.

Another object of the present invention is to provide a sunscreen cosmetic composition containing the sunscreen composition.

In addition, another object of the present invention is to provide a method for preparing the UV-blocking composition.

According to the present invention in order to achieve the above object, 50 to 100 nm particle diameter titanium dioxide 30.0 to 50.0 wt%, alkyl silane (Alkyl Silane) 1.0 to 10.0 wt%, silicone oil 30.0 to 50.0 wt%, and surfactant 10.0 to 20.0 wt% There is provided a composition for blocking ultraviolet rays consisting of %.

Preferably, the alkyl silane is triethoxycaprylylsilane, and contains 9.5% by weight or more based on the weight of the titanium dioxide.

The silicone oil is selected from the group consisting of cyclopentasiloxane, cyclohexasiloxane, dimethicone, diphenyldimethicone, diphenylsiloxyphenyltrimethicone, simethicone, phenyltrimethicone and methyltrimethicone. Is at least one, more preferably cyclopentasiloxane.

The surfactants are PEG-11 methyl ether dimethicone, PEG/PP-20/22 butyl ether dimethicone, PEG-3 dimethicone, PEG-10 dimethicone, PEG-12 di Methicone, PEG/PP-18/18 dimethicone, lauryl PEG-9 polydimethylsiloxyethyldimethicone, PEG-9 polydimethylsiloxyethyldimethicone, cetyl PEG/ PPG-10/1 dimethicone, lauryl polyglyceryl-3 polydimethylsiloxyethyldimethicone, polyglyceryl-3 polydimethylsiloxyethyldimethicone, lauryl PEG-10 tris( It is at least one selected from the group consisting of trimethylsiloxy)silylethyldimethicone and cetyldiglyceryltris(trimethylsiloxy)silylethyldimethicone, more preferably PEG-10dimethicone.

The UV blocking composition is obtained by dispersing in a ring mill batch type bead mill.

According to the present invention in order to achieve the above other object, there is provided a sunscreen cosmetic composition containing 0.1 to 20% by weight of the sunscreen composition based on the total weight of the cosmetic composition.

According to the present invention in order to achieve the another object, (A) coating a titanium dioxide having a particle diameter of 50 ~ 100nm with an alkylsilane; (B) adding the coated titanium dioxide while mixing and stirring the dispersant and the solvent, and mixing by stirring for 30 to 60 minutes; And (C) transferring the mixture to a ring mill type batch bead mill and dispersing the mixture by stirring for 1 to 2 hours with an internal mixer of 1000 to 1100 rpm and an external mixer of 100 to 200 rpm at 30 to 40°C. Is provided.

Preferably, the alkylsilane in step (A) is triethoxycaprylylsilane.

The solvent is selected from the group consisting of cyclopentasiloxane, cyclohexasiloxane, dimethicone, diphenyldimethicone, diphenylsiloxyphenyltrimethicone, simethicone, phenyltrimethicone and methyltrimethicone. At least one, more preferably cyclopentasiloxane.

The dispersant is PEG-11 methyl ether dimethicone, PEG/PP-20/22 butyl ether dimethicone, PEG-3 dimethicone, PEG-10 dimethicone, PEG-12 dimethicone Ticon, PEG/PP-18/18 dimethicone, lauryl PEG-9 polydimethylsiloxyethyldimethicone, PEG-9 polydimethylsiloxyethyldimethicone, cetyl PEG/P Sebum-10/1 dimethicone, lauryl polyglyceryl-3 polydimethylsiloxyethyldimethicone, polyglyceryl-3 polydimethylsiloxyethyldimethicone, lauryl PEG-10 tris (tri It is at least one selected from the group consisting of methylsiloxy)silylethyldimethicone and cetyldiglyceryltris(trimethylsiloxy)silylethyldimethicone, more preferably PEG-10dimethicone.

The UV-blocking composition according to the present invention has excellent skin coverage and is stable, so that the UV-blocking effect lasts for a long time, so it can be usefully used as a sun-blocking cosmetic.

1 is a schematic diagram showing the operating principle of a continuous bead mill and a batch bead mill.
2 is a micrograph of a composition for blocking UV rays prepared according to an embodiment of the present invention.
3 is a photograph showing a difference in transparency of a composition for blocking ultraviolet rays according to the size of titanium dioxide.
Figure 4 is a photograph showing the stability of the composition for blocking UV according to an embodiment of the present invention.

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

According to the present invention, a composition for UV protection comprising 30.0 to 50.0 wt% of titanium dioxide having a particle diameter of 50 to 100 nm, 1.0 to 10.0 wt% of alkyl silane, 30.0 to 50.0 wt% of silicone oil, and 10.0 to 20.0 wt% of a surfactant Is provided.

In the present invention, titanium dioxide having a particle diameter (median volume particle diameter) of 50 to 100 nm (more than 50 nm and 100 nm or less) is used as a dispersant in order to improve skin coverage with UV blocking effect. If it exceeds 100 nm, the white turbidity may become severe, and if it is less than 50 nm, the transparency increases and the covering power decreases.

Since the UV blocking effect is directly related to the dispersibility of the dispersion, in the present invention, the dispersoid titanium dioxide is coated with an alkyl silane to improve dispersibility. According to an embodiment of the present invention, the alkyl silane is triethoxycaprylylsilane. The alkyl silane as a coating base material is preferable because it is more excellent in dispersibility when it is contained in an amount of 9.5% by weight or more based on the weight of the dispersant titanium dioxide.

The silicone oil is selected from the group consisting of cyclopentasiloxane, cyclohexasiloxane, dimethicone, diphenyldimethicone, diphenylsiloxyphenyltrimethicone, simethicone, phenyltrimethicone and methyltrimethicone. Is at least one, more preferably cyclopentasiloxane.

The surfactants are PEG-11 methyl ether dimethicone, PEG/PP-20/22 butyl ether dimethicone, PEG-3 dimethicone, PEG-10 dimethicone, PEG-12 di Methicone, PEG/PP-18/18 dimethicone, lauryl PEG-9 polydimethylsiloxyethyldimethicone, PEG-9 polydimethylsiloxyethyldimethicone, cetyl PEG/ PPG-10/1 dimethicone, lauryl polyglyceryl-3 polydimethylsiloxyethyldimethicone, polyglyceryl-3 polydimethylsiloxyethyldimethicone, lauryl PEG-10 tris( It is at least one selected from the group consisting of trimethylsiloxy)silylethyldimethicone and cetyldiglyceryltris(trimethylsiloxy)silylethyldimethicone, more preferably PEG-10dimethicone.

On the other hand, the persistence of the UV blocking effect is directly related to dispersion stability. The composition for blocking ultraviolet rays of the present invention is characterized in that it is obtained by dispersing in a ring mill type batch bead mill to ensure dispersion stability.

Compared to the case of dispersing using a three-stage roll mill or a continuous bead mill, which has been used in the production of a conventional UV blocking composition, long-term dispersion stability was more excellent when the composition was prepared by dispersing with a ring mill batch bead mill. . In the case of using a three-stage roll mill, there is a problem that the number of processes is infinitely long depending on the union state of titanium dioxide, so production efficiency is degraded, and the continuous bead mill has a limitation in dispersion efficiency, making it difficult to obtain uniform results.

In order to overcome this limitation, in the present invention, a batch bead mill was selected, and among them, a dispersion was manufactured using a ring mill type batch bead mill having excellent efficiency by rotating in reverse to the basket outside the bead (see FIG. 1). It was confirmed that the ring mill type batch bead mill exhibits more excellent dispersion stability when using beads of 0.9 mm or more, more preferably 0.9 to 1.2 mm in a condition filled with 70% of the volume of the ring mill.

In order to achieve another object of the present invention, there is provided a sunscreen cosmetic composition containing 0.1 to 20% by weight of the sunscreen composition based on the total weight of the cosmetic composition.

In this case, the sunscreen cosmetic composition may further include other inorganic and organic sunscreen agents. As the inorganic UV blocking agent, zinc oxide coated with alkyl silane and having a particle diameter of 50 to 100 nm may be used.

The organic sunscreens include ethylhexylmethoxycinnamate, octocrylene, octylmethoxycinnamate, butylmethoxydibenzoylmethane, benzophenone, avobenzene, octyltrizone, and bis-ethylhexyloxyphenolmethoxyphenyltri At least one selected from the group consisting of azine may be used.

Since the UV-blocking cosmetic composition has excellent UV-blocking effect and skin coverage, it has the advantage of not having to separately use other makeup cosmetics.

[Example]

Hereinafter, the present invention will be described in more detail through Examples and Test Examples.

These examples are for illustrative purposes only, and it will be apparent to those of ordinary skill in the art that the scope of the present invention is not limited by these examples.

Examples 1-5: Preparation of UV blocking composition

A composition for blocking UV rays was prepared according to the composition of Table 1 below.

First, titanium dioxide was dry-coated with triethoxycaprylylsilane. Disperse PEG-10 dimethicone as a dispersant and cyclopentasiloxane as a solvent using a mixer (Heungbu Tech, Ekatomixer) at room temperature for 30 to 40 minutes at a speed of 1200 to 1300 rpm, then dry coating while stirring at the same speed Titanium dioxide was added and continued for 30 minutes, and then transferred to a ring mill type batch bead mill and stirred at 30 to 40°C with an internal mixer of 1000 to 1100 rpm and an external mixer of 100 rpm for 1 hour, followed by filtration through a 100 mesh filter.

Comparative Examples 1-4: Preparation of UV-blocking composition

According to the composition of Table 1 below, a UV blocking composition was prepared in the same manner as in the above Example. In Comparative Example 1, titanium dioxide not coated with an alkylsilane was used.

ingredient Comparative example Example One 2 3 4 One 2 3 4 5 Titanium dioxide (15nm) - 41.0 - - - - - - - Titanium dioxide (80nm) 45.0 - - - 44.0 43.0 42.0 41.0 39.0 Titanium dioxide (150nm) - - 41.0 - - - - - - Titanium dioxide (200nm) - - - 41.0 - - - - - Triethoxycaprylylsilane - 4.0 4.0 4.0 1.0 2.0 3.0 4.0 6.0 Cyclopentasiloxane 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 PEG 10-Dimethicone 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0

Test Example 1: Comparison of dispersing power of titanium dioxide

The dispersion power of each composition prepared according to the above Examples and Comparative Examples was measured with a microscope. The compositions of Examples 1 to 5 and Comparative Example 1 were observed under a microscope, and the results are shown in FIG. 2.

As can be seen in FIG. 2, black spots are observed in the composition of Comparative Example 1 in which the alkyl silane coating is not applied, which represents titanium dioxide aggregated without being dispersed.

In the compositions of other examples, it can be seen that the dispersibility is improved, and it can be seen that the dispersibility of Examples 4 and 5 is the most excellent. In Examples 1 to 5, the dispersing power increases in proportion to the increase in the amount of coating agent to the weight of the dispersant titanium dioxide, but in Examples 4 and 5, the content of the coating agent for titanium dioxide is about 9.5% by weight or more. You can see the same thing.

Test Example 2: UV blocking effect test

The UV blocking effect of the UV blocking composition of the above Examples and Comparative Examples was confirmed.

In-vitro SPF and PA were measured for the compositions prepared according to the compositions of Comparative Examples 1 to 4 and Example 4. The UV blocking measurement experiment was performed using a solar protection factor (SPF) analyzer (SPF-290AS, SOLAR LIGHT, USA). On the PMMA plate, 0.0325 g of the material to be measured is uniformly spread over the entire surface and dried at room temperature for 30 minutes. The dried PMMA plate was inserted into the SPF analyzer, and the values of SPF and PA were measured by selecting 9 random locations for UV in the 290-400 nm wavelength range. The results are shown in Table 2.

Comparative example Example One 2 3 4 4 SPF 33 48 26 20 130 PA 28 45 21 16 96

As can be seen from the SPF and PA measurement results in Table 2, both SPF and PA had the highest results in Example 4, and the results were large in the order of Comparative Example 2, Comparative Example 1, Comparative Example 3, and Comparative Example 4. In particular, the results of Example 4 were found to be remarkably high in PA. This shows a result consistent with the dispersion power test result of Test Example 1.

Test Example 3: Comparison of skin coverage

Skin coverage was observed with respect to the composition prepared according to the composition of Comparative Examples 2 to 4 and Example 4. 3 is a photograph comparing the transparency by applying the compositions of Comparative Examples 2 to 4 and Example 4 to the skin.

As can be seen in Figure 3, the composition of the smallest titanium dioxide (Comparative Example 2) is the most transparent, it can be seen that the skin coverage of the composition of Example 4 is greatly improved.

Examples 6 to 8: Preparation of UV blocking composition

A composition for blocking ultraviolet rays was prepared by different dispersion methods for the composition of Example 4.

Zirconium beads having different sizes of 0.3 mm (Example 6), 0.6 mm (Example 7), and 0.9 mm (Example 8) respectively in a ring mill batch type bead mill commonly used in paint and semiconductor fields were ring milled. A composition for blocking ultraviolet rays was prepared by dispersing under conditions filled with 70% of the volume.

Specifically, in order to manufacture using a ring mill batch type bead mill (ARMSTEC, RRG-100), zirconium beads dried at 50°C for 48 hours were filled to 70% of the volume of the basket, and the mixed composition was added to 30-40 It was prepared by stirring for 1 hour with an internal mixer 1000-1100rpm and an external mixer 100rpm at °C and then filtered through a 100mesh filter.

Comparative Examples 5-7: Preparation of UV blocking composition

With respect to the composition of Example 4, a composition for blocking ultraviolet rays was prepared by different dispersion equipment. For UV protection by using a three-stage roll mill (Comparative Example 5), a continuous bead mill (Comparative Example 6), and a basket-type batch bead mill (Comparative Example 7), which have been used in the production of the conventional UV blocking composition The composition was prepared.

Specifically, the composition for UV protection of Comparative Example 5 was prepared by dispersing once at a rate of 2500 g/min at room temperature using a three-stage roll mill (Light Yong Machine, TRM-14").

Using a continuous bead mill (Nipponcoke&engineering, SC100), the mixture was stirred at 30 to 40°C and 3000 rpm and dispersed at a rate of 500 g/min to prepare a UV-blocking composition of Comparative Example 6.

Using a basket-type batch bead mill (Unitec, U-mill basket type 300L), 0.5mm zirconium beads were filled to 70% of the basket volume, and dispersed under the conditions of 30~40℃, 1000rpm, 1 hour, A composition for blocking ultraviolet rays was prepared.

Test Example 4: UV blocking effect test

The UV-blocking effect of the UV-blocking compositions of Examples and Comparative Examples was confirmed by the same method as in Test Example 2. The results are shown in Table 3 below.

Comparative example Example 5 6 7 6 7 8 SPF 102 114 126 130 130 130 PA 66 80 92 96 96 96

The composition of the example prepared using the ring mill batch type bead mill exhibits better SPF and PA values, indicating that the dispersibility is better. The three-stage roll mill exhibited the lowest dispersibility, and the continuous bead mill showed a large result deviation due to the inconsistent number of times the composition passed through the mill, and the dispersing power was also not excellent, resulting in low SPF and PA values. Among the batch bead mills, both the basket method and the ring mill method showed better dispersion results, and the best dispersion results were obtained in the examples using the ring mill method batch bead mill.

Test Example 5: Dispersion Stability Test

The stability of the UV-blocking compositions of Examples and Comparative Examples was evaluated. The compositions prepared in Examples 6 to 8 and Comparative Examples 5 to 7 were stored at 45° C., and then the condition after 30 days was observed. The results are shown in FIG. 4.

As can be seen in Figure 4, in the case of the composition of Comparative Example 5 using a three-stage roll mill, Comparative Example 6 using a continuous bead mill, and Comparative Example 7 using a basket-type batch bead mill, a phase separation phenomenon appeared in terms of long-term stability. Showed undesirable results.

In the case of the compositions of Examples prepared by dispersing with a ring mill batch bead mill by varying the size of the beads, in the compositions of Examples 6 and 7 dispersed by using 0.3 mm and 0.6 mm, respectively, the phase separation phenomenon was observed after 30 days. Appearance could be confirmed. When using beads of less than 0.9mm, it was found that coalescence occurred due to insufficient dispersant capable of maintaining the dispersing power of the titanium dioxide dispersed too small. It was confirmed that the UV-blocking composition of Example 8 obtained by dispersing a 0.9 mm-sized bead in the condition filled with 70% of the volume of the ring mill exhibited a stable state even after 30 days, and thus had the best long-term stability.

Formulation Example 1: Preparation of sunscreen lotion

A sunscreen lotion containing the sunscreen composition of Example 4 was prepared by a conventional method according to the composition of Table 4 below.

Raw material Content (% by weight) UV protection composition (Example 4) 15.0 Lauryl PEG-9 polydimethylsiloxyethyl dimethicone 3.0 Squalane 0.5 PEG-10 Dimethicone/Vinyl Dimethicone Crosspolymer 4.0 Butylene Glycol 2.0 glycerin 1.0 Sodium chloride 1.0 Phenoxyethanol a very small amount Spices a very small amount Purified water Balance

Although the specific embodiments have been listed as described above, it is clear that these specific techniques are only preferred embodiments and are not intended to limit the scope of the present invention to those of ordinary skill in the art. Therefore, it will be said that the substantial scope of the present invention is defined by the appended claims and their equivalents.

Claims (9)

delete delete delete delete delete delete (A) coating titanium dioxide having a particle size of 50-100 nm with triethoxycaprylylsilane;
(B) adding the coated titanium dioxide while mixing and stirring the dispersant and the solvent, and mixing by stirring for 30 to 60 minutes; And
(C) Transfer the mixture to a ring mill batch bead mill filled with 0.9 to 1.2 mm beads to 70% of the ring mill volume, and stir for 1 to 2 hours with an internal mixer 1000 to 1100 rpm and an external mixer 100 to 200 rpm at 30 to 40 °C Method for producing a UV-blocking composition comprising the step of dispersing. delete A sunscreen cosmetic composition containing 0.1 to 20% by weight of the sunscreen composition prepared by the method of claim 7 based on the total weight of the cosmetic composition.

Images