KR100744945B1 - Composition for blocking of Ultraviolet Radiation Comprising Multi-layer Encapsulated Titanium Dioxide and Silica Sol as Active Ingredient and Manufacturing Process Thereof - Google Patents

Abstract

The present invention relates to a sunscreen composition containing titanium dioxide and silica sol encapsulated in a multilayer as an active ingredient and a method for producing the same. The sunscreen composition of the present invention is excellent in the sunscreen ability and excellent in the usability can be usefully used to prepare a sunscreen cosmetics.

Titanium Dioxide, Silica Sol, Sun Protection, Hybrid-Encapsulation

Description

Composition for blocking of Ultraviolet Radiation Comprising Multi-layer Encapsulated Titanium Dioxide and Silica Sol as Active Ingredient and Manufacturing Process Thereof}

1 is an optical microscope photograph of pure titanium dioxide used in Example 1. FIG.

2 is an optical microscope photograph of pure silica used in Example 1. FIG.

3 is an optical microscope photograph of the titanium dioxide / silica composite particles of Example 1. FIG.

4 is an optical microscope photograph of zirconia surface-treated titanium dioxide / silica composite particles of Example 5. FIG.

5 is a particle size measurement graph of the titanium dioxide / silica composite particles of Example 1. FIG.

FIG. 6 is a graph of absorbance of titanium dioxide (UV TITAN M170, TTO S-1 and Titan P25) and titanium dioxide / silica composite particles of Example 1. FIG.

The present invention relates to a sunscreen composition, a manufacturing method thereof and a cosmetic composition for sunscreen comprising the sunscreen composition as an active ingredient.

Cosmetics are broadly classified into basic cosmetics, makeup cosmetics, hair cosmetics, and sun care products.

Recently, as the ozone layer is destroyed due to environmental pollution such as automobile smoke and factory heat, the exposure to ultraviolet rays is intensified, and the skin damage such as sun burn, blackening and erythema by ultraviolet rays is accelerated day by day. There is a need for development of a product that protects the skin from ultraviolet rays. In particular, as life improves, the demand for protecting skin from ultraviolet rays as well as leisure activities such as skiing, golf, and sea bathing are increasing day by day, and the demand for protecting skin from ultraviolet rays is increasing day by day. Research is ongoing.

Conventional sunscreens for protecting the skin with ultraviolet light include (i) inorganic sunscreens such as titanium dioxide and zinc white, and (ii) Ethylhexyl Methoxycinnamate, butyl methoxydibenzoyl. Methane (Butyl Methoxydibenzoylmethane), Octyl triazone, Glycery PABA, Drometizole, Benzophenone-3, Benzophenone-4, Benzophenone-4 Benzophenone-8, Cinoxate, Octocrylene, Ethylhexyl Dimethyl PABA, 2-phenylbenzimidazole-5-sulfonic acid, octyl Organic sunscreens such as Salicylate (Ethylhexyl Salicylate) and Homosalate (Homosalate) are classified and commonly used. The reason why the organic sunscreen is mixed with the inorganic sunscreen is that the organic sunscreen absorbs the ultraviolet rays by absorbing the ultraviolet rays, that is, it is classified into a substance that can easily block UVA and a substance that can easily block UVB by λmax. This is because the UV blocking material blocks ultraviolet rays by scattering and reflecting ultraviolet rays. Therefore, in order to effectively block ultraviolet rays, organic and inorganic sunscreens should be mixed appropriately.

In other words, in order to effectively block UV rays, it is inevitable that an inorganic sunscreen agent is incorporated into the sun care product. Among them, titanium dioxide effectively blocks the UVB region and has been widely used as sun care products are also used as a substitute for makeup bases. Inorganic sunscreens include metal oxides such as titanium dioxide, zinc oxide, and cerium oxide, and have been widely used because of their excellent UV protection and safety. Among these, titanium dioxide is widely used in makeup cosmetics as well as UV protection products due to its low price and high coverage.

However, titanium dioxide has high photoactivity, which irritates the skin, causes whitening phenomenon when applied to the skin, forms complexes when mixed with certain organic ultraviolet materials, lowers the titer, and the structure (Morphology) Tetrahedral (Tetrahedral) has the disadvantage of rough use.

Therefore, in order to solve the above problems, studies on particles of titanium dioxide (US Pat. No. 6,123, 927) in order to effectively block ultraviolet rays with a minimum amount of the compound, applying a suitable amount of alumina and silica to titanium dioxide (Dopping), Surface treatment with saponification reaction using fatty acids such as stearic acid and oleic acid, surface treatment with silicon and alkylsilane, compounding method of coating titanium dioxide on talc, inorganic powder and titanium dioxide or organic resin and titanium dioxide A method of preparing a powder by simple mixing, a method of hydrolyzing titanium alkoxide by the sol-gel method to impregnate the surface or the inside of the substrate, and a method of impregnating titanium dioxide have been researched and developed. The method of surface modification with metal salts, silicones and silanes is the most common method to improve spreading and smoothness, and slightly improve dispersibility, but the problem of whitening phenomenon that is weak when applied to skin due to low transparency It exists as it is, and there exists a problem of colliding with a specific organic sunscreen. The method of coating alumina and silica on titanium dioxide also solves the activity of titanium dioxide to some extent, but problems such as dispersibility, transparency problem, and whitening still remain. Finally, a method of making titanium dioxide particles by hydrolysis using silica or polymethacrylate with teus, etc., and a method of combining and hybridizing pre-formed titanium dioxide particles with a resin (Japanese Patent Laid-Open No. 2001-00280147) Although the former has a weak UV blocking index due to poor formation of titanium dioxide particles, the latter has a limitation in improving transparency and improving usability, but increasing the amount of inorganic materials such as titanium dioxide. There is still a problem of lowering the titer by forming a complex with a specific organic sunscreen.

Throughout this specification, numerous patent documents are referenced and their citations are shown in parentheses. The disclosure of the cited patent documents is incorporated herein by reference in their entirety, and the level of the technical field to which the present invention belongs and the contents of the present invention are more clearly explained.

Thus, the present inventors improve the visible light transmittance to minimize whitening phenomenon when applied to the skin, improve the UV blocking ability, decrease the photocatalytic activity to improve safety and light stability, and furthermore, with a specific organic sunscreen As a result of repeated studies to solve the complex problem to facilitate the formulation of the sun care product, as well as to inexpensive product, the present invention was completed by confirming that the composition of the present invention solves the above problems.

Accordingly, an object of the present invention is to provide a sunscreen composition comprising (a) an inorganic sunscreen and (b) an inorganic silica sol as an active ingredient, wherein the sunscreen composition comprises 2 to 20 layers of the inorganic sunscreen on an inorganic silica sol. It is to provide a sunscreen composition characterized in that the formulation of the hybrid-encapsulated multiparticulates in a multilayer.

In addition, another object of the present invention to provide a method for producing the sunscreen composition.

In addition, another object of the present invention to provide a cosmetic composition for sunscreen comprising the sunscreen composition as an active ingredient.

Other objects and advantages of the present invention will become apparent from the following detailed description and claims.

According to an aspect of the present invention, the present invention provides a sunscreen composition comprising (a) an inorganic sunscreen agent and (b) an inorganic silica sol as an active ingredient, wherein the sunscreen composition comprises two inorganic sunscreens on an inorganic silica sol. It provides a sunscreen composition, characterized in that the formulation of the hybrid-encapsulated multiparticulates in a multilayer of 20 to 20 layers.

The inorganic sunscreen agent included in the sunscreen composition of the present invention has an average particle size of 20 to 40 nm, titanium dioxide having a spherical shape, zinc white or cerium oxide, an average particle size of 15 to 25 nm, It is preferable that it is titanium dioxide which is not surface-treated.

In conventional sunscreen cosmetic formulations, in contrast to the use of needles (needles) to enhance transparency and effectively block ultraviolet rays, in the present invention, as an active ingredient that acts as a sunscreen, it is close to a sphere for easy encapsulation. It has a length / thickness ratio of 2/3 to 1/1 in shape, and uses pure titanium dioxide that is not complexed with alumina, silica, etc., to be combined with silica, and not surface-treated with fatty acid metal salts, alkylsilanes, and silicon. It is characterized by. In a preferred embodiment of the present invention, titanium dioxide having an average particle size of 25 nm was used.

In addition, the inorganic silica sol included in the sunscreen composition of the present invention is preferably a compound having a structure of the formula (1) by sol-forming silica alkoxide.

Wherein M is silica, R is an alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl, pentyl, hexyl, heptyl and octyl, n is an integer from 3 to 8.

It is preferable that the said silica alkoxide is tetra ethyl oxo silicate or tetra methyl oxo silicate, and it is more preferable that it is tetra ethyl oxo silicate.

The composition for a sunscreen of the present invention is characterized in that the inorganic sunscreen has a formulation of hybrid-encapsulated multiparticulate particles in an inorganic silica sol in multiple layers.

Hereinafter, as used herein, the term 'hybrid-encapsulated multiparticulate' refers to a multiparticulate having a form of a capsule by silica sol coating a surface of titanium dioxide located at the center thereof, and again a 'titanium dioxide-silicazole' in the capsule. Titanium dioxide-silica sol-'coated in multiple layers. Hybrid-encapsulated multiparticulate means a multiparticulate multiparticulate capsule composed of titanium dioxide and silica sol.

In more detail, the sunscreen composition of the present invention is to form a hybrid-encapsulated composite particles by coating titanium dioxide having a sunscreen action with the silica sol formed above, multi-layered to effectively block ultraviolet rays by increasing the content of titanium dioxide Hybrid-capsules were formed, and hybrid-capsules were formed in 2 to 20 layers to have an appropriate average particle size. In particular, when titanium dioxide having an average particle size of 20 to 40 nm is simply impregnated with silica having an average particle size of 2 to 5 nm, the average particle size of the composite particles is 20 to 1000 nm, but hybrid-capsules are multilayered. The average particle size of the finally formed composite particles increases in size from 1 to 6 ㎛. By increasing the average particle size of the composite particles in this way, the usability and spreadability of titanium dioxide can be eliminated and the usability can be increased by reducing the friction coefficient.

Hybrid-capsules prepared in consideration of UV-blocking ability, transparency and usability in a multi-layered composite particle, that is, the sunscreen composition of the present invention preferably has an average particle size of 1 to 6 ㎛, more preferably 3 to 5 ㎛ Do.

It is preferable that the composition ratio of the said inorganic type sunscreen agent / inorganic silica sol contained in the composition for sunscreen of this invention is 85-70 / 15-30, It is more preferable that it is 80-70 / 20-30. When the amount of the inorganic sunscreen, preferably titanium dioxide, included in the composition for the sunscreen is 70% or less, the effect of UV protection is low due to the low UV protection effect, and when the weight is 85% or more, the UV protection effect is excellent. Failure to hybridize encapsulation with silica leads to roughness and cloudiness, making it unsuitable for use as a sunscreen.

In addition, the sunscreen composition of the present invention may further comprise (i) a hydrophobic material selected from the group consisting of silicone materials, such as methicone and dimethicone, alkylsilanes and amino acids, or (ii) dimethicone copolyols or phospholipids. Hydrophilic material is surface coated. The hydrophobic material or hydrophilic material surface-coated in the sunscreen composition of the present invention is not limited to the components described above as the components used to facilitate dispersion, it is usually selected from any of the components used in cosmetic formulations Can be used.

When using a hydrophobic material to facilitate dispersion in the sunscreen composition and considering compatibility with the organic sunscreen, the hydrophobic material is preferably included 1 to 7% by weight relative to the total weight of the sunscreen composition. In a preferred embodiment of the invention triethoxysilane was used to coat the sunscreen composition.

In addition, the present invention

(i) stirring silica alkoxide, alcohol and water under a base atmosphere to produce a stable silica sol;

(ii) preparing a hybrid-encapsulated titanium dioxide / silica composite particle by coating the silica sol prepared in step 1 on titanium dioxide having an average particle size of 20 to 40 nm; And

(iii) repeating steps 1 and 2 two to twenty times to provide a method for preparing a composition for a sunscreen composition comprising the step of preparing hybrid-encapsulated silica / titanium dioxide composite particles in a multilayer.

Method for producing a composition for sunscreen of the present invention is (i) a hydrophobic material selected from the group consisting of silicone materials, such as methicone and dimethicone, alkylsilanes and amino acids or (ii) dimethicone copolyols or phospholipids Surface coating of the hydrophilic material can be further performed.

Referring to the production method of the present invention in more detail as follows.

(i) stirring silica alkoxide, alcohol and water under a base atmosphere to produce a stable silica sol

The silica alkoxide used in this step is not particularly limited in its kind, but using silica substituted with an alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl, pentyl, hexyl, heptyl and octyl groups It is preferable. Specifically, for example, tetra-ethylolsosilicate or tetra-methylolsosilicate, and the like, in the preferred embodiment of the present invention was used tetra-ethylolsosilicate.

In addition, the alcohol used in this step is used to make a stable sol by controlling the reaction rate, and methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, butyl alcohol, pentyl alcohol, hexyl alcohol, heptyl alcohol and octyl alcohol. It is preferably selected from the group consisting of.

Meanwhile, in this step, ammonia water is used to make a base atmosphere and proceed with the reaction with silica sol, and it is preferable to use ammonia water diluted to 10%, 20%, 30%, 40% or 50%.

The silica sol preparation step of the present invention is illustrated by the following process.

Wherein M is silica, R is an alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl, pentyl, hexyl, heptyl and octyl, n is an integer from 3 to 8.

(ii) preparing a hybrid-encapsulated titanium dioxide / silica composite particle by coating the silica sol prepared in step 1 on titanium dioxide having an average particle size of 20 to 40 nm.

In the step, water and alcohol are added to titanium dioxide having an average particle size of 20 to 40 nm, ammonia water is added, a nitrogen atmosphere is formed, and the stable silica sol prepared in step (i) is used by using a micro syringe. By dropping one by one so that the silica is coated on the titanium dioxide. This step produces a hybrid-encapsulated titanium dioxide / silica composite particle in a monolayer having an average particle size of 20 to 1000 nm as mentioned above.

(iii) repeating steps 1 and 2 two to twenty times to produce hybrid-encapsulated silica / titanium dioxide composite particles in multiple layers.

In this step, the hybrid capsules are multilayered by repeating the steps 1 and 2 several times to produce multiparticulates having an average particle size of 1 to 6 µm, preferably 3 to 5 µm. It is preferable to repeat steps 1 and 2 two to twenty times to allow the hybrid-capsules to be multilayered, but may be appropriately adjusted according to the reaction conditions. The particle size shows the secondary parabola convex upward as the basicity increases by the base strength, and the optimal size condition can be found in the basicity at the vertex of the convex parabolic upward.

In addition, polyethylene glycol or ethylene glycol may be used to prevent secondary aggregation of the composite particles, and 0.1 to 3.0% of a surfactant having a HLB (Hydrophic / Lipophilc Balanace) 5 to 13 such as polysorbate may be used as an adhesive. Can be.

In addition, the steps of (i) to (iii) may be carried out to filter, wash, dry and calcined the composite powder prepared, (i) silicone materials, such as methicone and dimethicone, alkylsilane and Surface coating a hydrophobic material selected from the group consisting of amino acids or (ii) hydrophilic materials such as dimethicone copolyols or phospholipids.

The surface coating of the composite powder with a hydrophobic material or a hydrophilic material is a step in which the product is lipophilic and at the same time has a smooth usability, thereby facilitating formulation when the final product is included in the cosmetic and manufactured. Preferably, the hydrophobic or hydrophilic material is included in an amount of 1 to 7 wt% based on the total weight of the final prepared sunscreen composition. In a preferred embodiment of the present invention, as a hydrophobic material for coating the composite powder, it was coated with silicone oil, such as methicone, dimethicone, triethoxysilane.

The sunscreen composition of the present invention and the sunscreen composition prepared by the method described above have an angle of repose suitable for use as a cosmetic and have excellent spreadability, and the coefficient of friction is reduced to reduce roughness when used.

In addition, the sunscreen composition of the present invention is excellent in the ability to block UV rays, UVB as well as the effect of blocking the UVA region, very low photoactivation is a composition that is stable for use in cosmetics, as well as low absorption in the ultraviolet region, Absorption of visible light region is also low and does not show turbidity effect.

The sunscreen composition of the present invention having excellent usability and excellent UV blocking effect can be usefully used for all cosmetics used for the purpose of blocking UV rays.

The present invention also provides a sunscreen cosmetic composition comprising the sunscreen composition at 0.1 to 20.0% by weight.

The sunscreen cosmetic composition of the present invention comprises the sunscreen composition or the sunscreen composition prepared by the method of the present invention as an active ingredient 0.1 to 20.0% by weight. If the amount is less than the sunscreen effect is weak, when used above the content is excellent in the sunscreen effect, but may cause skin irritation or poor compatibility with other sunscreen ingredients and formulation formation.

The cosmetic composition of the present invention contains, as an active ingredient, ingredients commonly used in cosmetic compositions in addition to the sunscreen composition, and include, for example, conventional auxiliaries such as antioxidants, stabilizers, solubilizers, vitamins, pigments and perfumes, and carriers. Include.

Cosmetic compositions of the present invention may be prepared in any formulation conventionally prepared in the art and include, for example, solutions, suspensions, emulsions, pastes, gels, creams, lotions, powders, soaps, surfactant-containing cleansing , Oils, powder foundations, emulsion foundations, wax foundations, sprays, and the like, but are preferably formulated in powder form. More specifically, it may be prepared in a formulation selected from the group consisting of two-way cake, face powder, compact, makeup base, skin cover, eye shadow, cheek color, lipstick, lip gloss, lip fix, and eyebrow pencil.

When the formulation of the present invention is a paste, cream or gel, animal oils, vegetable oils, waxes, paraffins, starches, trachants, cellulose derivatives, polyethylene glycols, silicones, bentonites, silicas, talc or zinc oxide may be used as carrier components. Can be.

When the formulation of the present invention is a powder or a spray, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder may be used, in particular in the case of a spray, additionally chlorofluorohydrocarbon, propane Propellant such as butane or dimethyl ether.

When the formulation of the present invention is a solution or emulsion, a solvent, solubilizer or emulsifier is used as the carrier component, such as water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1 Fatty acid esters of, 3-butylglycol oil, glycerol aliphatic ester, polyethylene glycol or sorbitan.

When the formulation of the present invention is a suspension, liquid carrier diluents such as water, ethanol or propylene glycol, suspending agents such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol ester and polyoxyethylene sorbitan ester, microcrystals Soluble cellulose, aluminum metahydroxy, bentonite, agar or tracant and the like can be used.

When the formulation of the present invention is a surfactant-containing cleansing, the aliphatic alcohol sulfate, aliphatic alcohol ether sulfate, sulfosuccinic acid monoester, isethionate, imidazolinium derivative, methyltaurate, sarcosinate, fatty acid as carrier components Amide ether sulfates, alkylamidobetaines, aliphatic alcohols, fatty acid glycerides, fatty acid diethanolamides, vegetable oils, lanolin derivatives or ethoxylated glycerol fatty acid esters and the like can be used.

Hereinafter, the present invention will be described in more detail with reference to Examples. These examples are only for illustrating the present invention in more detail, it will be apparent to those skilled in the art that the scope of the present invention is not limited by these examples in accordance with the gist of the present invention. .

Example 1

60 g of titanium dioxide (Daegusa, Titan P-25) with an average particle size of 25 nm was placed in the reactor Aggglomaster, and 2500 g of water was added while rotating at 1000 rpm at an elevation of 0.5 m / min. After adding 100 g of methanol and 20 g of acetone, 30 g of 30% diluted ammonia water was added and stirred. When heated to 55 ° C. under nitrogen, 210 g of TEOS (tetra ethyl ortho silicate) was added dropwise dropwise using a micro syringe, inserted over 2 hours, and stirred for 12 hours. It was filtered and washed and dried at 50 ° C.

After repeating the above process 2 to 3 times, it was heated to 550 ℃ and burned at high temperature to burn the organic material unsuitable for use in cosmetics. Then 100 g of the mixture was taken and placed in a 1 L round bottom flask equipped with a stirrer and thermometer together with 500 g of water to warm to 50 ° C.

Then, 2.5 g of triethoxysilane and 12.5 g of alcohol were taken and stirred in a 50 ml beaker for wet surface treatment with silicone, alkylsilane, and the like. When the heating was over to 50 ℃ put the prepared triethoxysilane and alcohol and warmed up to 100 ℃. When it became 100 degreeC, it was made to react for 24 hours in this state.

Example 2

Composite particles were prepared in the same manner as in Example 1, except that the temperature of the calcination process was adjusted to 700 to 750 ° C.

Example 3

In the same procedure as in Example 1, except that the average particle size was 20-40 nm instead of the titanium dioxide of Example 1, and pure titanium dioxide (Teica, Japan, TiO ₂ MT 500B) was not used. Composite particles were prepared.

Example 4

The same procedure as in Example 1, except that titanium dioxide (Ishihara Sangyo, Japan, TTO-V4), first surface-treated with alumina instead of titanium dioxide, was used. To prepare a composite particle.

Example 5

A composite particle was prepared in the same manner as in Example 1, except that titanium dioxide (Ishihara Sangyo, Japan, TTO-S-1) surface-treated with zirconia was used instead of the titanium dioxide of Example 1.

Example 6

A composite particle was prepared in the same manner as in Example 1, except that ceria (Nanotech, Ceria) having an average particle size of 20-60 nm was used instead of the titanium dioxide of Example 1.

Experimental Example 1 Observation of Form of Composite Particles

In order to confirm that the titanium dioxide / silica composite particles prepared in Example were properly formed, the shape of the composite particles was observed using an optical microscope. To compare the formation of the composite particles, the form of pure silica and pure titanium dioxide was observed as a comparison group. The optical microscope observation results are shown in FIGS. 1 to 4.

As a result, the pure titanium dioxide of FIG. 1 was in a spherical tetrahedral form, scattered light, appeared to be somewhat rough because the titanium dioxide was not uniformly dispersed and not impregnated-hybrid, and FIG. 2 Pure silica was in spherical form, transmitted light, and polished particles. On the other hand, it was found that the composite particles of Example 1 in which pure titanium dioxide was impregnated and hybridized to silica were changed into a gentle spherical shape of titanium dioxide (FIG. 3). However, the composite particles of Example 5, in which zirconia surface-treated titanium dioxide was impregnated-hybridized, had a lower sphericity, more spreadability (below angle of refraction), and photo discoloration than those of Example 1 (FIG. 4).

Experimental Example 2 Measurement of Average Particle Size of Composite Particles

The average particle size of various titanium dioxide and silica sol / titanium dioxide composite particles was measured using SALD-2001 (Shimadzu, Japan). The average particle size was measured using titanium particles or silica sol / titanium dioxide composite particles aggregated by the surrounding moisture to form tertiary particles. The average particle size measurement results are shown in Table 1 below, and the particle size distribution of the composite particles of Example 1 of the present invention is shown graphically in FIG. 5.

Average particle size of the composite particles sample Average particle size (primary particle μm) Degusa Titan P-25 0.25 Tayca TiO ₂ MT 500B (Tyaca) 0.35 TTO S-1 (Ishiharo Sankyo) 2.05 Silica 3.69 Titanium Dioxide with Silica and Dimethicone Surface Treatment (Kemira M-170) 0.78 Composite Particles of Example 1 2.50 Composite Particles of Example 5 3.60

As shown in Table 1, the composite particles of Example 1 of the present invention had an average particle size of 2.5 μm, and showed a particle size distribution as shown in FIG. 5.

Experimental Example 3 Flowability of Composite Particles

The angle of repose was checked to determine the flowability of pure titanium dioxide and composite particles. The flowability is usually determined by measuring the angle of repose or kinetic friction coefficient, in the present invention by measuring the angle of repose to determine the flow of the composite particles. In general, the smaller the angle of repose, the better the flowability. The angle of repose was measured by the injection angle method, which measures the angle between the conical and horizontal planes of the powders accumulated through a funnel of a certain height.

Repose angle of composite particles sample Repose angle ( ^o ) Degusa Titan P-25 55-60 Tayca TiO ₂ MT 500B (Tyaca) 60-60 TTO S-1 (Ishiharo Sankyo) 50-55 Silica 35-40 Talc 50-55 Titanium Dioxide with Silica and Dimethicone Surface Treatment (Kemira M-170) 40-50 Composite Particles of Example 1 35-40 Composite Particles of Example 5 40-45

Not comparable to titanium dioxide, similar to pure silica, and typically the ideal angle of repose in cosmetic materials is known to be 30-40 ^° . As shown in Table 2, the angle of repose of the optimum conditions for imparting the flowability and smooth feel of the powder was derived. Therefore, the composite particles of Example 1 of the present invention was found that the angle of repose is 35-40 ^o , the optimum angle in terms of spreadability by reducing the angle of repose compared to the raw material titanium dioxide (Degusa Titan P-25).

Experimental Example 4: UV blocking ability of the composite particles

In order to check the UV-blocking ability of the composite particles prepared in the present invention, pure titanium dioxide, the composite particles of Example 1 and commercialized samples were wetted with 5% in petrolatum and taped at 2 mg / Cm ² (SPF Analyzer tape) ) Was measured using SPF Analyzer 290 (Optometri).

UV protection ability of composite particles Item P-25 MT 500B TTO-S-1 M-170 Example 1 Example 2 Example 5 SPF / Standard Deviation 17.53 /3.09 13.12 /3.86 11.85 /4.03 13.78 /3.86 8.95 /2.22 8.92 /2.13 5.27 /1.27 UVA / UVB 0.57 0.747 0.596 0.526 0.555 0.562 0.57

As shown in Table 3, the composite particles of Example 1 prepared using pure titanium dioxide have a UV blocking index SPF of 8.95, which is slightly lower than that of other titanium dioxide, but this is pure water contained in the composite particles. As a result of showing that the content of titanium dioxide is less than that of other titanium dioxide, it can be seen that it has excellent UV blocking ability similarly to other titanium dioxide not compounded.

In addition, the ultraviolet ray blocking ability of the composite particles of Example 1 using pure titanium dioxide was 57.0%, the ultraviolet ray blocking ability of the composite particles of Example 2 prepared by increasing the temperature of the firing process compared to Example 1 was 34.03% It was found that the ultraviolet rays of the composite particles of the present invention is excellent.

As shown in the UVA / UVB ratio, the composite particles of Example 1 were excellent in shielding effect not only in the UVB but also in the UVA region, and similar to the pure titanium dioxide content ratio and the raw materials. In particular, the composite particles of Example 5 had the same input ratio as the composite particles of Example 1 at the time of manufacture, but the process of encapsulating-hybridized with silica was not as good as that of Example 1 because titanium dioxide was first complexed with zirconia. And it was found.

Experimental Example 5: Photoactivation degree of the composite particles

In order to check the light activation of the composite particles of the present invention, the sample was wetted with 5% petrolatum, and then the standard value was measured using a color difference meter (Minolta CR 300), and a wavelength similar to sunlight using a spectrophotometer. After irradiating with artificial light for 6 hours, the color light was irradiated, the artificial light was irradiated, and light activation was checked by comparing color values before and after irradiation, and the results are shown in Table 4 below.

In the following table, L represents lightness, A and B represent redness, and the chroma value (ΔE) was calculated by the following equation.

Light activation of composite particles sample Wetting early After investigation ΔE L A B l ^* a ^* b ^* Titan P-25 96.99 0.75 5.52 75.4 2.79 12.06 22.65 MT 500B 94.22 1.9 2.14 71.79 4.12 19.66 28.54 TTO S-1 95.5 1.33 0.17 83.2 0.82 20.26 23.56 M-170 97.19 0.89 0.08 90.30 2.14 5.91 9.11 Example 1 91.04 1.31 2.18 91.78 1.89 1.6 1.07 Example 5 90.50 1.78 0.4 86.50 1.70 1.03 4.05

As shown in Table 4, the light activation degree of the sample of Example 1 is the lowest, and the light stability is excellent, in particular, titanium dioxide (p-25) and titanium dioxide surface-treated with zirconia (TTO S- Compared with 1) and alkylsilane (M-170), it was found that the light stability was much better. In general, when the saturation (ΔE) value is 1 or less, it is difficult to distinguish the human vision.

Experimental Example 6: Whitening Degree of Composite Particles

When applied to the skin, the absorbance was measured using IR (infrared ray) to check the whitening phenomenon that became bluish or bluish. The visible light region is 400-800 nm and high absorption in this region is known to cause bleaching.

Through the absorbance graph of FIG. 6, the composite particles of the present invention have high absorbency in the 280-320 nm region, which is an ultraviolet blocking region, and have excellent ultraviolet redundancy effect. It can be seen that the phenomenon rarely causes.

As described in detail above, the composition of the present invention is to hybridize encapsulated titanium dioxide in multiple layers with silica sol to solve the roughness of the existing sunscreen, improve safety and stability, improve dispersibility, and By improving the compatibility of the excellent UV blocking ability and usability can be easily used in the manufacture of cosmetics for UV protection.

Having described the specific part of the present invention in detail, it is apparent to those skilled in the art that the specific technology is merely a preferred embodiment, and the scope of the present invention is not limited thereto. Thus, the substantial scope of the present invention will be defined by the appended claims and equivalents thereof.

Claims (13)

An inorganic sunscreen having an average particle size of 20 to 40 nm is hybrid-encapsulated into 2 to 20 layers by an inorganic silica sol, and a hydrophobic material or dimethic agent selected from the group consisting of methicone or dimethicone, alkylsilane and amino acid as a silicone material A sunscreen composition comprising composite particles having an average particle size of 1 to 6 μm, surface-coated with a hydrophilic material selected from chicon copolyol or phospholipid. delete The sunscreen composition of claim 1, wherein the inorganic sunscreen is titanium dioxide, zinc oxide or cerium oxide having a spherical property, and has an average particle size of 15-25 nm. The sunscreen composition according to claim 3, wherein the titanium dioxide is titanium dioxide which is not surface treated. According to claim 1, wherein the inorganic silica sol is a sunscreen composition, characterized in that the compound having a structure of formula (1) prepared by mixing silica alkoxide, alcohol and water. <Formula 1>

Wherein M is silica, R is an alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl, pentyl, hexyl, heptyl and octyl, n is an integer from 3 to 8. 6. The sunscreen composition according to claim 5, wherein the silica alkoxide is tetra ethyl oxo silicate or tetra methyl oxo silicate. The sunscreen composition according to claim 1, wherein the composition ratio of the inorganic sunscreen agent / inorganic silica sol contained in the sunscreen composition is 85-70 / 15-30. delete delete (i) stirring silica alkoxide, alcohol and water under a base atmosphere to produce a stable silica sol; (ii) preparing a hybrid-encapsulated titanium dioxide / silica composite particle by coating the silica sol prepared in step 1 on titanium dioxide having an average particle size of 20 to 40 nm; (Iii) repeating steps 1 and 2 two to twenty times to produce hybrid-encapsulated silica / titanium dioxide composite particles in multiple layers; And (Iii) a hydrophobic material or dimethicone copolyol or phospholipid selected from the group consisting of methicone or dimethicone, alkylsilanes and amino acids as a silicone material on the surface of the hybrid-encapsulated silica / titanium dioxide composite particle Method for producing a composition for sunscreen comprising the step of coating with a hydrophilic material. delete A sunscreen cosmetic composition comprising 0.1 to 20.0 wt% of the sunscreen composition of any one of claims 1, 3, 5, 6 or 7. 13. The cosmetic composition of claim 12, wherein the cosmetic composition is a formulation selected from the group consisting of two-way cake, face powder, compact, makeup base, skin cover, eye shadow, cheek color, lipstick, lip gloss, lip fix, and eyebrow pencil. Cosmetic composition for UV protection.

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