KR101436540B1 - Uv protecting cosmetic composition comprising titania nano rod - Google Patents

Abstract

TECHNICAL FIELD The present invention relates to a cosmetic composition for ultraviolet ray shielding comprising a nano-rod-shaped titania.
According to the present invention, by including the nano-rod-shaped titania as the ultraviolet screening agent component through the shape modification of the inorganic ultraviolet screening agent, it is possible to minimize whitening phenomenon caused by the high refractive index of the conventional inorganic ultraviolet screening agent, And provides a covering force for security, and improves the feeling of being hurt by the agglomeration of these inorganic ultraviolet screening agents. In addition, the cosmetic composition for protecting ultraviolet rays of the present invention may further comprise a titanium dioxide nano powder or an organic ultraviolet ray blocking agent in the form of a nano-rod-like titania as the ultraviolet screening agent component, The synergy effect of ultraviolet ray blocking can be realized through the light stability by the titania.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a UV-blocking cosmetic composition containing titania

The present invention relates to a cosmetic composition for ultraviolet shielding comprising a nano-rod-shaped titania, and more particularly, to a cosmetic composition for ultraviolet shielding comprising a nano- The high refraction index of the ultraviolet screening agent can compensate for the whitening phenomenon that occurs when the skin is applied, and it can improve the feeling of use due to the agglomeration of the inorganic blockers. The titanium nano- Nano powder or organic ultraviolet screening agent, thereby providing a synergistic effect of ultraviolet ray blocking through the light stability by the nano-rod-shaped titania.

Currently, cosmetics for ultraviolet rays, the most approved cosmetics in the domestic functional cosmetics market, are expected to expand rapidly due to the problem of skin damage caused by ultraviolet rays due to destruction of the ozone layer.

However, in the suncare market, the annual growth rate of over 20% per year for the past three years, but more than 90.0% of raw materials are dependent on overseas imports. Although the growth rate of raw material imports is increasing due to the expansion of the market in the future, it is not able to secure new materials and products capable of international competitiveness.

Most UV-blocking agents sold on the market have been continuously pointed out that the by-products generated by photo-degradation adversely affect the skin, and studies are under way to reduce such photodegradation.

Conventional ultraviolet screening agents may be used to impart synergistic effects by mixing different types of ultraviolet screening agents in the same product or effectively block ultraviolet screening agents using a stabilized ultraviolet screening agent at a specific wavelength or encapsulate or form a complex And a method of imparting stability.

The ultraviolet screening agent to be obtained through the above-mentioned method must (a) be capable of absorption over a whole range of 280 to 320 nm, (b) be stable to heat or light, (c) It should be absent. Also, (d) should not be absorbed too quickly into the skin, (e) must be neutral, and (f) must meet the requirements for easy dissolution in appropriate media.

In order to meet these requirements, the ultraviolet screening agents currently used in the cosmetics industry can be broadly divided into organic ultraviolet screening agents and inorganic ultraviolet screening agents.

First, organic sunscreen agents have problems in optical stability and cause irritant contact dermatitis in sensitive skin, which is absorbed into the skin or causes serious problems in stability due to photoreaction products. Therefore, there are many restrictions on the use of most organic UV-blocking agents.

On the other hand, titanium dioxide, which is a typical example of an inorganic UV blocking agent, has a fine size (<100 nm) distribution and effectively blocks ultraviolet rays from a wide area (280-400 nm) through scattering, reflection, etc., It is most widely used because it shows a natural feeling.

However, once titanium oxide or zinc oxide absorbs ultraviolet rays due to its photocatalytic activity, it may cause degradation of organic substances contained in the ultraviolet screening agent by forming oxygen or oxygen radicals on the surface of titanium dioxide, It may cause damage.

In addition, inorganic sunscreen agents have a high refractive index and thus have a large effect of scattering ultraviolet rays, but they cause discomfort due to a feeling of weariness when applied to the skin and make the skin white and shiny with turbidity on the skin.

These inorganic ultraviolet screening agents are over-dispersed in nanoscale, and are highly susceptible to penetration into the skin, and thus stability problems are pointed out. That is, it may cause skin irritation and skin damage due to the photocatalytic activity due to free radicals, and the particle size due to the secondary agglomeration of particles may increase, and ultraviolet blocking ability may decrease with time.

Nevertheless, most sunscreen products absorb or reflect ultraviolet rays using the organic or inorganic ultraviolet screening agents described above, and utilize the advantages of each of them to shield ultraviolet rays.

Therefore, it is necessary to improve the physical properties of the currently used blocking agent. For example, a method of coating aluminum oxide (Al ₂ O ₃ ) and silicon oxide (SiO ₂ ) on the surface of titanium dioxide has been reported to improve the disadvantage of titanium dioxide due to photocatalytic activity [ Thin Solid Films 2005 , 475 , pp 171-177, Technol . 2006 , 24 (5) , pp 275-281].

Accordingly, the present inventors have made efforts to solve the problems of conventional ultraviolet screening agents, particularly inorganic ultraviolet screening agents, and as a result, they have found that by including nano-rod-shaped titania as a typical ultraviolet screening agent component through shape modification of an inorganic ultraviolet screening agent, The present inventors have completed the present invention by minimizing whitening whitening during skin application, realizing light stability, and confirming the synergistic effect when water is combined with other UV blocking agents.

An object of the present invention is to provide a cosmetic composition for ultraviolet ray shielding comprising a nano-rod-shaped titania as an ultraviolet screening agent component.

Another object of the present invention is to provide a method for producing titania in the shape of a nano-rod.

Another object of the present invention is to provide a colorant comprising the nano-rod-shaped titania.

In order to achieve the above object, the present invention provides a cosmetic composition for ultraviolet ray shielding comprising ultraviolet shielding titania as a component of an ultraviolet ray blocking agent in an inorganic cosmetic composition for ultraviolet ray shielding.

In the present invention, the nano-rod-shaped titania contained as the ultraviolet blocking agent component is anhydrous titania nanorod which is heat-treated from a hydrogen tantanate (H ₂ Ti ₅ O ₁₁ ) nanotube; Or surface modified anhydrous titania nanorods.

The surface-modified titania nanorods may be made of aluminum oxide (Al ₂ O ₃ ), dimethicones, cyclomethicones, inorganic materials, silicone oils, and ester oils. One of which is coated on the surface of the titania nano rod.

In the cosmetic composition for protecting ultraviolet rays of the present invention, it is preferable that the ultraviolet screening agent component contains 0.0001 to 30% by weight of titania in the form of nanorods relative to the weight of the whole composition.

In addition, in the cosmetic composition for protecting ultraviolet rays of the present invention, the ultraviolet screening agent component may further include titanium nioxide nanoparticles in the form of a nano-rod, 0 to 70 parts by weight of a non-nano-rod-shaped titanium dioxide nano powder per 100 parts by weight of the titania.

In the cosmetic composition for protecting ultraviolet rays of the present invention, the ultraviolet screening agent component

The nano-rod-shaped titania may further include an organic UV-blocking agent, and more preferably 10 to 200 parts by weight of the organic UV-blocking agent may be added to 100 parts by weight of the nano-rod-shaped titania.

The present invention relates to a process for producing hydrogentanetanate (H ₂ Ti ₅ O ₁₁ ) nanotubes by hydrothermal synthesis of titanium dioxide nanoparticles and heat-treating the hydrogentanetanate nanotubes produced at 300 to 800 ° C. to form nanorods a provides a process for the preparation of titania (TiO _2).

Further, the present invention provides a colorant comprising nano-rod-shaped titania prepared from the above-mentioned production method.

The present invention provides a cosmetic composition for ultraviolet shielding comprising a nano-rod-shaped titania as an ultraviolet screening agent component, thereby improving the whitening phenomenon of the inorganic ultraviolet screening agent, the photoactive skin irritation caused by free radicals and the skin damage problem.

In other words, the cosmetic composition for protecting ultraviolet rays of the present invention complements the phenomenon of whitening whitening due to the high refractive index of the conventional inorganic ultraviolet screening agent through shape modification of the inorganic ultraviolet screening agent, It is possible to improve the feeling of being used.

In addition, the cosmetic composition for protecting ultraviolet rays of the present invention may further comprise titanium dioxide nano powder or organic ultraviolet ray blocking agent in the form of nano-rod-like titania, The synergy of ultraviolet shielding can be given through stability.

Accordingly, the cosmetic composition for protecting ultraviolet rays of the present invention can impart a covering function to the skin which is not a general inorganic ultraviolet screening agent, thereby complementing the skin disadvantage.

1 is a SEM measurement result of the nano-rod-shaped titania of the present invention,
FIG. 2 shows the HR TEM measurement result of the nano-rod-shaped titania of the present invention,
FIG. 3 shows the results of the avobenzone potency test according to the UV irradiation of the cosmetic composition for UV screening of the present invention,
Fig. 4 shows the result of discoloration test after light irradiation of the cosmetic composition for UV screening of the present invention,
5 is a result of turbidity test of the cosmetic composition for protecting ultraviolet rays of the present invention,
FIG. 6 is a process flow chart of the nano-rod-shaped titania manufacturing method of the present invention,
7 is a schematic view showing a process of converting the hydrogentanatanite nanotubes of the present invention into titania nanorods.

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

The present invention provides a cosmetic composition for ultraviolet ray shielding comprising a nano rod titania as an ultraviolet screening agent component in the cosmetic composition for blocking ultraviolet rays of the present invention.

In this specification, the term 'nano-rod shape' refers to fine primary particles having a thickness of several tens of nanometers (1 nm of 1 billionths of a meter) and length of several micrometers, in which atoms connected by polygonal rings form a long rod.

In the present specification, the term 'titania' refers to synthetic gemstones composed of titanium oxide, but in the present specification refers to crystallized titanium oxide.

In the present specification, the term "titania" in the form of a nanorod means that the crystallized titanium oxide is connected with a polygonal ring to crystallize the shape of the long rod.

In the present invention, as the nano-rod-shaped titania, preferably, titanium dioxide nano powder is mixed with titanic anhydride nanorods thermally treated from hydrogentanetanate (H ₂ Ti ₅ O ₁₁ ) nanotubes produced by hydrothermal synthesis, The modified anhydrous titania nanorods are selected for use.

FIG. 1 shows the SEM measurement results of the nano-rod-shaped titania of the present invention, and FIG. 2 shows the nano rod shape as a result of HR TEM measurement of the nano-rod-shaped titania.

Also, as the nano-rod-shaped titania of the present invention, the term "surface modification" in surface-modified titania nano-rods means that the surface of a specific material is covered with another material to convert the physical properties of the specific material into properties of other materials .

Accordingly, in the present invention, any one selected from the group consisting of aluminum oxide (Al ₂ O ₃ ), dimethicones, cyclomethicones, inorganic materials, silicone oils, and ester oils But not limited to, surface modification.

In the preferred cosmetic composition for protecting ultraviolet rays of the present invention, the ultraviolet screening agent component may contain 0.0001 to 30% by weight, more preferably 10 to 15% by weight, based on the weight of the entire composition, of nano- By weight and 12 to 13% by weight. At this time, if the content of titania in the form of nano-rods exceeds 30% by weight, the feeling of use becomes heavy, and the white turbidity becomes serious, which is inferior to the sunscreen product.

In the preferred cosmetic composition for protecting ultraviolet rays of the present invention, as the ultraviolet screening agent component, the nano-rod-shaped titania may further include a non-nano-rod-shaped titanium dioxide nano powder.

Preferably, 0 to 70 parts by weight, more preferably 1 to 10 parts by weight, and most preferably 3 to 10 parts by weight of titanium dioxide nano powder in the form of a non-nano rod are added to 100 parts by weight of the nano- To 5 parts by weight.

At this time, if the non-nano-rod-shaped titanium dioxide nano powder is contained in an amount exceeding 70 parts by weight, it is not preferable because the advantages of the Naro rod are offset.

In another preferred cosmetic composition for protecting ultraviolet rays of the present invention, the nano-rod-shaped titania as the ultraviolet screening agent component may further include an organic ultraviolet screening agent. Preferably, 100 parts by weight of the nano- And 10 to 200 parts by weight of an organic UV blocking agent. At this time, the organic UV blocking agent content range is set to a range for achieving a synergistic effect when the ultraviolet blocking agent component is a mixed type, and the nano rod-shaped titania stabilizes the conventional organic UV blocking agent component so as to realize the optical stability.

The organic UV blocking agent preferably used in the present invention includes ethylhexyl methoxycinnamate, octocrylene, avobenzene, butylmethoxydibenzoylmethane, oxybenzone, octyltriazone, menthyl anthranilate, 3,4- Methylbenzylidene Kempfer or bis-ethylhexyloxyphenol methoxyphenyltriazine, or a mixture of two or more thereof, and most preferably any one of ethylhexylmethoxycinnamate or octocrylene, or a mixture thereof But is not limited thereto.

FIG. 3 shows the results of potency test of avobenzone according to irradiation of ultraviolet rays of the cosmetic composition for protecting ultraviolet rays according to the present invention. When the ultraviolet ray blocking agent is contained in the nanorodic titania, the initial recovery rate The synergy effect of light stability can be confirmed from the result of keeping constant.

Fig. 4 is a graph showing the result of discoloration after light irradiation of the cosmetic composition for protecting ultraviolet rays of the present invention. As a result, color change can not be observed even after one week elapsed after irradiation with ultraviolet rays (280-400 nm) for 24 hours. Thus, cosmetic compositions for ultraviolet shielding comprising nano-rod-shaped titania as the ultraviolet screening agent component of the present invention show no discoloration without the octocrylene component conventionally used for the prevention of photodecomposition, so that the nano- It also helps to prevent discoloration due to photolysis.

Fig. 5 shows the results of turbidity test of the cosmetic composition for protecting ultraviolet rays according to the present invention. As a result, it is possible to confirm excellent transparency through surface modification of turbidity peculiar to titanium dioxide (TiO ₂ ).

Especially. In the ultraviolet screening cosmetic composition of the present invention, the nano-rod-shaped titania is constituted of an organic / inorganic composite material containing an organic ultraviolet screening ingredient as an ultraviolet screening agent component, thereby providing excellent SPF boosting effect due to synergy effect [ 5].

It will be appreciated that the UV-blocking cosmetic composition of the present invention may further contain an aqueous phase component, an oily component, an oily component, and a solvent component in addition to the nano-rod-shaped titania. As a specific example, 0.3 to 0.5% by weight of the incrementing agent; 0.4 to 0.5% by weight of an emulsifier; 0.9 to 1.1% by weight of a hydrocarbon-based high saturated fatty alcohol; 6.4 to 6.6 wt% of ester oil; 1.0 to 7.5% by weight of an organic sunscreen agent; And a remaining amount of purified water.

The incrementing agent may be any one selected from the group consisting of xanthan gum, ammonium acryloyldimethyltaurate and Vipico polymers, or a mixture of two or more thereof.

Examples of the emulsifier include polysorbate 60, lanolin, sorbitan oil vase, Carnauba wax, olive liquid, lecithin, stearic acid, borax, ceteth, solvolysizer, cetyl alcohol, A polysorbate 80, a Sorbitan Stearate, a Polyoxyetylene Phytosterol and a Hydrogenated Soybean Phospholipid, or a mixture of two or more thereof may be used. And most preferably polysorbates, but it is not limited thereto and can be selected according to the formulation of the ultraviolet screening agent to be produced.

The hydrocarbon-based higher saturated fatty alcohols may be any one of behenyl alcohol, Cetearyl alcohol, and stearyl alcohol, or a mixture of two or more thereof, But are not limited to, allyl alcohol.

In addition, the ester oil may be any one of cetylaryl octanoate, dicapricarbonate, and glyceryl stearate, or a mixture of two or more thereof.

A feature of the present invention is an emulsified emulsion comprising an oil component containing an aqueous component containing purified water, the thickener, and the emulsifier, a hydrocarbon-based higher saturated fatty alcohol, and an ester oil, It is possible to exhibit a great synergy effect of ultraviolet ray blocking even when the cosmetic composition is prepared by using water resistance and other UV blocking agents.

In addition to the nano-rod-shaped titania, the cosmetic composition for protecting ultraviolet rays of the present invention may further contain a known substance required according to the cosmetic composition formulation.

Accordingly, in accordance with an embodiment of the present invention, the cosmetic composition of the present invention can be used as a cosmetic composition containing glycerin, butylene glycol, polyoxyethylene hardened castor oil, tocopheryl acetate, citric acid, panthenol, squalane, sodium citrate and allantoin Further comprising at least one auxiliary component selected from the group consisting of glycerin, polyoxyethylene hydrogenated castor oil, tocopheryl acetate, squalane and sodium citrate, and at least one auxiliary component selected from the group consisting of butylene glycol, At least one component selected from the group consisting of panthenol and allantoin, and most preferably at least one component selected from the group consisting of glycerin, butylene glycol, polyoxyethylene hydrogenated castor oil, tocopheryl acetate, citric acid, panthenol, squalane, Lt; RTI ID = 0.0 &gt; allantoin &lt; / RTI &gt;

Since the cosmetic composition of the present invention is basically applied to the skin, it can be provided with reference to the cosmetic composition of the related art, for example, as a solution, a suspension, an emulsion, a paste, a gel, a cream, a lotion, But are not limited to, surfactant-containing cleansing, oils, powder foundations, emulsion foundations, wax foundations and sprays.

More specifically, it can be manufactured in the form of a soft lotion, a nutritional lotion, a nutritional cream, a massage cream, an essence, an eye cream, a cleansing cream, a cleansing foam, a cleansing water, a pack, a spray or a powder.

When the formulation of the present invention is a paste, cream or gel, an animal oil, vegetable oil, wax, paraffin, starch, tracant, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc or zinc oxide may be used as the carrier component .

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 as a carrier component. In the case of a spray, in particular, / Propane or dimethyl ether.

When the formulation of the present invention is a solution or an emulsion, a solvent, a dissolving agent or an emulsifying agent is used as a carrier component, and examples thereof include water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, , 3-butyl glycol oil, glycerol aliphatic ester, polyethylene glycol or sorbitan fatty acid esters.

When the formulation of the present invention is a suspension, a carrier such as water, a liquid diluent such as ethanol or propylene glycol, a suspension such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol ester and polyoxyethylene sorbitan ester, Crystalline cellulose, aluminum metahydroxide, bentonite, agar, or tracant may be used.

When the formulation of the present invention is an interfacial active agent-containing cleansing, the carrier component may include aliphatic alcohol sulfate, aliphatic alcohol ether sulfate, sulfosuccinic acid monoester, isethionate, imidazolinium derivative, methyltaurate, sarcosinate, fatty acid amide Ether sulfates, alkylamidobetaines, aliphatic alcohols, fatty acid glycerides, fatty acid diethanolamides, vegetable oils, lanolin derivatives, or ethoxylated glycerol fatty acid esters.

In addition, the present invention provides a method for producing titania of nano-rod shape.

FIG. 6 is a process flow chart of the nano-rod-shaped titania manufacturing method, which can be produced by a hydrothermal synthesis method (hydrothermal synthesis method) from titanium dioxide nano powder.

The hydrothermal synthesis method (hydrothermal synthesis method) in the present invention refers to a method of hydrothermally synthesizing a nano-rod-like titania in the presence of high-temperature water, particularly at high temperature and high pressure, Synthesis or modification reaction, that is, synthesis using a hydrothermal reaction.

Scheme 1

_{H 2 Ti 4 O 9 · H} 2 O → 4 / 5H 2 Ti 5 O 11 → 2TiO 2 + H 2 O ↑

More specifically, the titanium dioxide nano-powder is stirred in an aqueous solution of 10M sodium hydroxide (NaOH) for 1 to 4 hours, and hydrothermally synthesized by using an autoclave at a temperature of preferably 130 to 160 ° C, most preferably 150 ° C (H ₂ Ti ₅ O ₁₁ ). The resulting precipitate was washed with a 0.1 M aqueous HCl solution until the pH became less than 7.0, to remove Na ⁺ ions, washed several times with distilled water to remove Cl ^- ions, and dried in an oven at about 80 ° C Synthesize hydrogentanitate nanotubes.

Thereafter, the hydrogentanatitanate nanotube is heat-treated at preferably 300 to 800 ° C, more preferably 400 to 600 ° C, and most preferably 500 ° C to obtain nano-rod-shaped titania (TiO ₂ ) .

FIG. 7 is a schematic view showing a shape modification process of converting the hydrogentanatanite nanotubes of the present invention into titania nanorods. FIG.

Furthermore, the present invention provides a colorant comprising titania in the form of a nanorod.

The colorant of the present invention can be applied to a makeup base or a point makeup product in which such characteristics are required, depending on the properties of the above-described nano-rod-shaped titania, such as light stability, water resistance, photolysis prevention property, and transparency.

In the present specification, the properties of the nano-rod-shaped titania as the coloring agent application are overlapped with the use of the ultraviolet screening agent described above, so detailed description thereof will be omitted.

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

The present invention is intended to more specifically illustrate the present invention, and the scope of the present invention is not limited to these embodiments.

PREPARATION EXAMPLE 1 Preparation of Titania Nanorod 1

1,250 ml of 10 M NaOH aqueous solution was added to 125 g of titania nano powder (P25 Evonik Degussa) and stirred for 4 hours, followed by hydrothermal synthesis at 150 ° C in an autoclave apparatus to obtain a precipitate. The precipitate was washed with 0.1 M HCl aqueous solution until it became slightly acidic to pH 7.0 or lower to remove Na ⁺ ions, and then washed several times with distilled water to remove Cl ^- ion. The final washing process was performed using ethanol, followed by drying in an oven at 80 ° C to synthesize a hydrotentitanate nanotube.

The synthesized hydrogen titanate nanotubes were heat-treated at 400 ° C to prepare water-removed titania nano-rods.

PREPARATION EXAMPLE 2 Titania Nanorod Production 2

The titania nano-rods were prepared in the same manner as in Example 1 except that the hydrogel titanate nanotubes prepared in Example 1 were heat-treated at 500 ° C.

At this time, as shown in Fig. 7, the nanotube shape of the hydrogen titanate is converted into the nanorod shape by the heat treatment.

&Lt; Example 1 > Preparation of cosmetic composition for UV screening

As shown in the following Table 1 , a cosmetic composition for UV screening was prepared, and the titania nanododes prepared in Preparation Example 1 were included.

More specifically, as the phase A, which is an aqueous phase component for producing a base, purified water, suntan com (KELCO), ammonium acryloyldimethyltaurate / Vpicopolymer, 1,3-butylene glycol (SKCCHEM.), The amount of Bait 60 (CRODA) (water phase component) was precisely weighed and weighed in a container. The thickening agent was uniformly dispersed in the water phase using a NATIONAL SS MOTOR and dissolved by heating at 85 ° C or higher.

Thereafter, as the phase B as an oily component, a mixture of behenyl alcohol (KOKYUALCOHOL), cetearyl octanoate (BASF (COGNIS)), dicapryl carbonate (BASF (COGNIS)) and glyceryl stearate , A titania nanorod prepared according to Preparation Example 1 and a C-phase as an inorganic UV-blocking agent component composed of BASF (CIVASPECIALTY) Avobenzone) were prepared.

Then, methyl methacrylate crosspolymer (MICROPOL INC, D phase) was precisely weighed as a powder, mixed, and heated to 85 ° C or higher. The B, C, and D phases were slowly mixed in phase A while maintaining 85 ° C and homogenized using a homomixer (PRIMIX). Next, the fragrant component (E-phase) was precisely weighed, and the contents were cooled to 35 DEG C and filled in a container.

&Lt; Comparative Example 1 > Preparation of cosmetic composition for ultraviolet screening

In Example 1, in place of the titania nanododes, a conventional titanium dioxide (SACHTLEBEN) was added to the C-phase component as the inorganic UV- TiO ₂ ) powder was used instead of the TiO ₂ powder.

&Lt; Comparative Example 2 > Preparation of cosmetic composition for ultraviolet screening

The procedure of Example 1 was repeated except for using a component composed of abbenzone (BASF (CIVASPECIALTY), Avobenzone) and ethylhexylmethoxycinnamate in place of the C-phase component as the inorganic UV blocking agent component. .

&Lt; Comparative Example 3 > Preparation of cosmetic composition for ultraviolet screening

In the same manner as in Example 1, except that in Example 1, components made of avobenzone (BASF (CIVASPECIALTY) Avobenzone) and octocrylene (MURCK) were used instead of the C-phase component as the inorganic UV- Respectively.

The physical properties of the cosmetic composition prepared in Example 2 and Comparative Examples 1 to 3 were tested through Experimental Examples 4 to 5.

Example 2: Preparation of cosmetic composition for ultraviolet screening

Example 1 was carried out in the same manner as in Example 1, except that the titania nanododes prepared in Production Example 2 were used as the C-phase component as the inorganic UV blocking agent component.

&Lt; Experimental Example 1 >

The shape of the titania nano-rods prepared in Preparation Example 1 was monitored using a scanning electron microscope (SEM).

As a result, as shown in FIG. 1, when the titania nano-rods prepared in Production Example 1 were enlarged to 100,000 times, nano-rod bundles were observed.

The results of measurement using a high-resolution transmission electron microscope (HR TEM) are shown in FIG.

As a result, the shape of the titania nano-rods prepared in Production Example 1 was observed.

&Lt; Experimental Example 2 > The avobenzone potency test

The ultraviolet screening compositions prepared in Example 1 and Comparative Examples 1 to 3 were subjected to an avobenzone potency test after irradiation with ultraviolet light. The HPLC analysis conditions were as follows:

Column: Symmetry C18 Reversed phase column of 5 占 퐉 占 4.6 占 150 mm

- mobile phase: a mixture of tetrahydrofuran, water and acetonitrile

Detection: 305 nm

- Flow rate: 1.0 ml / min

- Test conditions: UV source: exposure 208-400 nm UVA / UVB irradiation, solar simulator: 250 ~ 765 W / m ² Xenon lamp by Atlas

FIG. 3 is a graph showing the results of avobenzone potency test according to the ultraviolet irradiation time for the ultraviolet screening composition prepared in Example 1 and Comparative Examples 1 to 3, wherein the ultraviolet screening composition prepared in Example 1 was the most It is a stable formulation. Thus, the ultraviolet-shielding composition of Example 1 used the titania nano-rod material, so that the initial recovery rate remained constant even after the ultraviolet irradiation time elapsed. Accordingly, it has been confirmed that the titania nano-rod material stabilizes the conventional organic UV-blocking agent, abbenzone, so as to realize the optical stability.

<Experimental Example 3> Color change test after UV Irradiation

The ultraviolet screening composition prepared in Example 1 and Comparative Example 3 was irradiated with ultraviolet rays (280 to 400 nm) for 24 hours, stored at 25 ° C for one week, and then subjected to weathering test to observe the discoloration test.

FIG. 4 is a photograph of the discoloration test result of ultraviolet ray blocking composition of the present invention after irradiation with ultraviolet rays.

As a result, the UV blocking compositions prepared in Example 1 and Comparative Example 3 did not exhibit any apparent color change with the naked eye.

The above results show that the ultraviolet screening composition of Example 1 is comparable to the result of Comparative Example 3 containing an octocrylene component for preventing photodegradation among conventional sunscreen components by using a titania nano rod component, It is confirmed that it plays a role to prevent the discoloration caused by.

Example 3: Preparation of cosmetic composition for ultraviolet screening

As shown in the following Table 2 , titania nano-rods prepared in Preparation Example 1 and avobenzone, an organic UV-ray blocking agent, were used as ultraviolet screening agent components, and other components were weighed and mixed and heated to 85 ° C or higher. The mixture was gradually mixed at 85 ° C and homogenized using a homomixer (PRIMIX). Next, the contents of the fragrance were precisely poured, and the contents were cooled to 35 DEG C and filled in a container.

Example 4: Preparation of cosmetic composition for ultraviolet screening

As shown in the following Table 2 , except that the titania nanowire and the titanium dioxide (TiO ₂ ) powder prepared in Preparation Example 1 were used as the ultraviolet screening agent component, Was prepared.

EXPERIMENTAL EXAMPLE 4 SPF Boosting Effect

The SPF boosting effect was tested on the cosmetic composition for UV screening prepared in Example 3 and Comparative Examples 4 to 6.

As a result, in Comparative Example 5 of Comparative Examples, it was confirmed that the use of a mixture of avobenzone and octocrylene among the organic ultraviolet screening agents helped maintain the blocking ability of avobenzone. However, in the composition of Example 3, organic and inorganic ultraviolet The ultraviolet shielding composition of Example 3 containing the organic / inorganic composite material containing the component showed the best SPF boosting effect due to the synergistic effect.

&Lt; Experimental Example 5 >

The whiteness degree test of the cosmetic composition for UV screening prepared in Example 3 and Comparative Example 4 was carried out.

As can be seen in the photograph of FIG. 5, the result of the composition of Comparative Example 4 on the right side of the photograph shows a transparent result in the case of the composition of Example 3 on the left side of the photograph, as opposed to a tangible result. The above ultraviolet barrier composition of Example 3, which shows the above transparent result, confirms that the turbidity inherent to titanium dioxide (TiO ₂ ) has been overcome through the property change.

&Lt; Experimental Example 6 > Water resistance test

The water resistance test was carried out using the UV-blocking cosmetic composition prepared in Example 3 under the conditions shown in Table 4 below.

The following Table 4 shows the results of water resistance test of the cosmetic composition for UV screening of Example 3 by applying a coating amount of 2 mg / cm ² using a transpore tape having an area of 70.7 x 70.7 mm The in vitro test was carried out at 23 to 28 DEG C for about 20 minutes and then dried for 20 minutes twice.

The result of the water resistance, that is, to have water resistance ratio was calculated by the following equation and the results are shown in Table 5.

&Quot; (1) &quot;

Water resistance ratio = (SPF i i -1) / (SPF i -1) x 100

In the above, SPF i is the water-resistant ultraviolet barrier index of each sample, and SPF i is the ultraviolet barrier index of each sample.

At this time, when the water resistance ratio is 50% or more, it is judged that the water resistance is effective.

From the results shown in Table 5, the UV-blocking cosmetic composition of Example 3 had an average water resistance ratio of about 67%, confirming excellent water resistance characteristics.

As described above, the present invention provides a UV-blocking cosmetic composition comprising nano-rod-shaped titania as an ultraviolet blocking agent component.

The cosmetic composition for protecting against ultraviolet rays of the present invention complements the phenomenon of whitening whitening due to the high refractive index of a conventional inorganic ultraviolet screening agent through shape modification of the inorganic ultraviolet screening agent, Improved feeling.

In addition, the cosmetic composition for protecting ultraviolet rays of the present invention may further comprise titanium dioxide nano powder or organic ultraviolet ray blocking agent in the form of nano-rod-like titania, By providing the synergy effect of ultraviolet ray shielding through stability, it is possible to provide a function of covering the skin disadvantages and shielding the skin by forming the covering power of the skin which is not in general inorganic ultraviolet ray blocking agent.

Further, the present invention provides a method for producing titania of nano-rod shape, and provides the use of nano-rod-shaped titania obtained therefrom as a colorant.

While the invention has been shown and described with reference to certain exemplary embodiments thereof, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (8)

An ultraviolet screening cosmetic composition comprising a nano rod-shaped titania in which titanium oxide crystallized is connected by a polygonal ring, and an ultraviolet screening agent component composed of an organic / inorganic composite material containing an organic ultraviolet screening component. The method according to claim 1, wherein the nano-rod-shaped titania is thermally treated from a hydrogen titanate (H ₂ Ti ₅ O ₁₁ ) nanotube; Or a surface-modified titania nanorod;
Wherein the surface-modified titania nanorods are selected from the group consisting of aluminum oxide (Al ₂ O ₃ ), dimethicones, cyclomethicones, silicone oils, and ester oils. Wherein the cosmetic composition is one coated with an ultraviolet ray. delete The cosmetic composition for protecting ultraviolet rays according to claim 1, wherein the nano rod-like titania component is contained in an amount of 0.0001 to 30% by weight based on the total weight of the composition. The cosmetic composition for ultraviolet blocking according to claim 1, wherein 0 to 70 parts by weight of titanium dioxide nano powder in the form of a non-nano rod is further contained in 100 parts by weight of the nano-rod-shaped titania. The cosmetic composition for protecting ultraviolet rays according to claim 1, wherein 10 to 200 parts by weight of an organic UV-blocking agent is contained in 100 parts by weight of the nano-rod-shaped titania. (H ₂ Ti ₅ O ₁₁ ) nanotubes are produced by hydrothermal synthesis of titanium dioxide nanoparticles, and hydrogentanethanates (H ₂ Ti ₅ O ₁₁ )
(TiO ₂ ) having a nanorod structure in which titanium oxide is crystallized by annealing the generated hydrogentanatitanate nanotubes at 300 to 500 ° C. in a polygonal loop. A colorant comprising nano-rod-shaped titania produced from the manufacturing method of claim 7.

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