KR100520841B1 - Pulverulent body for makeup and the process for the same, and cosmetic composition containing the same - Google Patents

Abstract

The present invention relates to a composite makeup cosmetic powder composed of silica / titanium dioxide / barium sulfate, a preparation method thereof, and a cosmetic composition containing the powder. More specifically, the composite makeup cosmetic powder comprises the steps of: (1) preparing a porous silica containing disodium distil biphenyl disulfonate as a fluorescent dye; (2) reacting the titanium dioxide sol with the plate-like barium sulfate; And (3) dispersing the reaction slurry of step (2) while adjusting the pH, and preparing the composite makeup cosmetic powder by reacting by adding the silica of step (1).

The cosmetic composition using the composite makeup cosmetic powder prepared above improves the clarity and spreadability of the makeup, increases the usability and skin adhesion, and effectively hides problems such as skin wrinkles and pores.

Description

Powder for composite makeup cosmetics, preparation method thereof and cosmetic composition containing same {Pulverulent body for makeup and the process for the same, and cosmetic composition containing the same}

The present invention relates to a composite makeup cosmetic powder composed of silica / titanium dioxide / barium sulfate, a preparation method thereof, and a cosmetic composition containing the powder. More specifically, the composite makeup cosmetic powder comprises the steps of: (1) preparing a porous silica containing disodium distil biphenyl disulfonate as a fluorescent dye; (2) reacting the titanium dioxide sol with the plate-like barium sulfate; And (3) dispersing the reaction slurry of step (2) while adjusting the pH, and preparing the composite makeup cosmetic powder by reacting by adding the silica of step (1).

In general, make-up cosmetics should be applied to the surface of the skin, such as proper concealment, color expression, UV protection, and excellent persistence of the cosmetic effect, and should have a good feeling such as skin adhesion, skin flexibility. In addition, it should be excellent in water resistance such as not being erased by water, sweat, etc., and excellent formulation stability.

Meanwhile, in addition to the above general functions, powders using optical scattering effects have been developed to improve skin wrinkles. As a specific example, "light scattering reflective composites in which talc is coated with an acrylic polymer" (中 村 直 生, 高 順 賀 豊 高., J. Soc . Cosmet . Chem . Jpn ., 21, 119 (1987)) is effective as a fine wrinkle . It is applied to the shading part of the pores, etc., so that the inner shadow is scattered and reflected by the external rays to make it shine brightly. In addition, composite powders coated with mica surface with particulate silica [特 開平 4-803119], and composite powders coated with zirconium oxide and aluminum oxide on the surface of silica containing ultrafine titanium oxide [特 開平 9-67232, 特]開平 8-217673].

However, the above-mentioned special coating powders for improving fine wrinkles are an invention in which the scattering reflection effect of light, which is an optical characteristic, is applied to the visible region, and is not suitable for the effective absorption scattering reflection of the ultraviolet region present in life. .

On the other hand, as a material for inducing natural makeup, a double-treatment of titanium dioxide, a high refractive index material, with silica, a low refractive index material, is used as a sandwich [Hirochika Nishimura, Research & development of summer foundation, Fragrance Journal, 25, (8), 42. 49 (1997)] and zinc oxide luminescent powders that produce natural skin clarity by analyzing the skin emission spectrum of natural skin condition. [ Fragrance , Fragrance Journal, 22, (2), 11-16 (1994)]. However, the zinc oxide inorganic light-emitting body is natural and can produce a natural skin with a sense of transparency, but due to the strong texture of the unique texture of the zinc oxide powder may be a burden on the skin during use.

In order to solve the above problems, the present inventors have studied components that can effectively conceal skin wrinkles and pores while inducing natural makeup, and have silica, titanium dioxide, and barium sulfate containing ultraviolet absorbing fluorescent dyes. When the composite makeup cosmetic powder is prepared and included in the cosmetic composition, the present invention has been found to be able to effectively hide skin wrinkles, pores, etc. as well as exhibit excellent transparency and feeling in use.

Accordingly, it is an object of the present invention to provide a composite makeup cosmetic powder composed of silica, titanium dioxide and barium sulfate that effectively conceal skin wrinkles, pores, as well as excellent usability and transparency.

In addition, another object of the present invention is to provide a method for producing the composite makeup cosmetic powder.

In addition, another object of the present invention is to provide a cosmetic composition containing the composite makeup cosmetic powder.

In order to achieve the above object, the composite make-up cosmetic powder of the present invention is characterized by consisting of silica, titanium dioxide and barium sulfate containing a UV absorbing fluorescent dye. In addition, the composite makeup cosmetic powder is (1) preparing a porous silica containing disodium distil biphenyl disulfonate as a fluorescent dye; (2) reacting the titanium dioxide sol with the plate-like barium sulfate; And (3) dispersing the reaction slurry of step (2) while adjusting the pH, and preparing the reaction by adding the silica of step (1).

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

The ultraviolet absorbing fluorescent material used in the present invention refers to a material that expresses strong blue fluorescence when exposed to sunlight. That is, it is a material that absorbs light in the ultraviolet portion (330-380 nm) of sunlight and expresses fluorescence in the short wavelength region (400-450 nm) of the visible portion, and means a fluorescent brightener, a fluorescent brightener, a fluorescent brightening agent, or an optical It is called variously as Brightener, but is used as Fluorescent Brightener in Color Index.

In particular, the disodium distil biphenyl disulfonate used as an ultraviolet absorbing fluorescent material in the present invention is represented by the structure of the following formula (1), the following planar structure has a conjugated double bond as a general colored dye, There is no strong electron aspirator such as -NO ₂ or -N = N-, which is different from ordinary colored dyes.

In the structure of Chemical Formula 1, the electrons of the double bond portion of the benzene ring are excited by absorption of ultraviolet rays and are excited by the excitation singlet state, and then return to a low single state, thereby showing a fluorescence phenomenon.

Hereinafter, the manufacturing method of the composite makeup cosmetic powder of the present invention will be described in detail for each step.

(1) preparing a porous silica containing a disodium distil biphenyl disulfonate, which is an ultraviolet absorbing fluorescent dye, in a slurry form;

First, 99.75 to 99.94% by weight of silica is added to a four-necked reactor based on the total weight of the composition, dispersed in a fixed amount of purified water and dispersed for 20 minutes in a slurry state. Next, using an acid solution such as sulfuric acid and hydrochloric acid or an alkaline solution such as potassium hydroxide and sodium hydroxide, the pH of the reaction solution is adjusted to 5.0 to 10.0, followed by redispersion, followed by disodium distilbibiphenyldisulfonate at room temperature. Into the reaction kiln at 0.06 to 0.25% by weight, the mixture was stirred for 30 minutes and then cooled to room temperature.

The silica prepared in this step is a spherical porous synthetic silica, which is a synthetic silica having an average particle diameter of 1 to 3 µm, a specific surface area of 63 m 2 / g, and an oil absorption of 120 ± 20 ml / 100 g. In addition, the silica induces a light makeup with a natural feeling with a clear feeling when applying the skin, and has the ability to control sebum as a porous structure.

(2) reacting the titanium dioxide sol with the plate-like barium sulfate;

First, 87 to 90% by weight of barium sulphate is added to a four-necked reactor with a quantitative amount of water based on the total weight of the composition, and then dispersed for 30 minutes to form a slurry. Next, titanium dioxide is solvated under acidic solution of sulfuric acid, hydrochloric acid or the like, or alkaline solution of potassium hydroxide, sodium hydroxide, etc. while maintaining the pH at 5-10. Next, titanium dioxide sol is added to the barium sulfate slurry and reacted at 80 ° C. for 30 minutes.

The plate-shaped barium sulphate has a specific gravity of 4.0 to 4.5, a particle size of 10 to 20 µm, a refractive index of 1.63, and is characterized by being almost transparent upon encountering oil. In addition, although the adhesion is excellent and slightly heavy feeling, it has the characteristics of a calm appearance and usability. On the other hand, the titanium dioxide having a size of 0.01 μm to 0.1 μm treated on the barium sulfate surface has a large number of particles per unit weight, and exhibits high visible light scattering ability and induces clear makeup.

(3) dispersing the reaction slurry of step (2) while adjusting the pH, and preparing the composite makeup cosmetic powder by reacting by adding the silica of step (1);

First, 80% by weight of the slurry of step (2) is dispersed while adjusting to pH 5.0 to 10.0, and then the silica sludge of step (1) is added and reacted at 80 ° C. for 30 minutes. Next, after the reaction was cooled to room temperature and aged for 24 hours, and then washed several times with water, filtered, dried at 120 ℃ again, calcined and ground to prepare a composite makeup cosmetic powder.

The composite makeup cosmetic powder prepared in the above step not only has an excellent wrinkle concealing effect, but also a small amount of UV-blocking effect can be expected to increase the transparency of the skin make-up to induce natural makeup and has excellent use and adhesion.

In addition, the composite makeup cosmetic powder of the present invention can be prepared in a formulation of a makeup product containing 1 to 50% by weight, specific examples of the formulation include a foundation, a two-way cake, a face powder and the like. In the preparation of the makeup formulation, the content of the composite make-up cosmetic powder is preferably 1 to 50% by weight based on the total weight of the composition, which is less than 1% by weight can not exhibit a sufficient concealing effect and exceeds 50% by weight of the skin This is because there is a possibility of causing problems such as adhesion, molding state, usability.

Hereinafter, although an Example and a comparative example are given and this invention is demonstrated in detail, this invention is not limited only to these examples.

Example 1 Preparation of Composite Makeup Cosmetic Powder

(1) Preparation of Silica Containing Ultraviolet Absorption Fluorescent Dye

99.94% by weight of porous silica (Airlite C53, Chemland Co. Ltd) was added to a sand dune reactor, and 6-10 times the weight of silica was quantitatively added and dispersed for 30 minutes to prepare a slurry. Next, the pH was adjusted to 5-10 with 40% aqueous sulfuric acid solution, and then 0.06% by weight of disodium distilbibiphenyldisulfonate (Tinopal CBS-X, Ciba Co. Ltd) was added at 80-90 ° C for 30 minutes. Reaction at After completion of the reaction, the mixture was cooled to room temperature, left for at least 12 hours and aged to prepare silica containing an ultraviolet absorbing fluorescent dye.

(2) Treatment of titanium dioxide sol with plate-like barium sulphate

87.0% by weight of plate shaped Barium Sulfate HL (NIHON KOKEN KOGYO Co. Ltd.) was prepared and added to a sand dune reactor, and the pH was 5.0 to 10.0 with 40% aqueous sulfuric acid solution and potassium hydroxide. Eusolex T, Merck Co. Ltd.) was dissolved, and then 13.0% by weight of titanium dioxide sol was added to the barium sulfate, followed by reaction for 30 minutes while maintaining a temperature of 80 ° C.

(3) Preparation of composite makeup cosmetic powder

80% by weight of the slurry of (2) was added to a sand dune reactor and 20% by weight of the silica of step (1) was added at 80 ° C. while maintaining a pH of 5.0 to 10.0 using a 40% aqueous sulfuric acid solution and potassium hydroxide. The reaction was carried out for 30 minutes. After the reaction, the mixture was cooled to room temperature and aged for 24 hours. After washing with water several times, the mixture was filtered, dried at 120 ° C., and ground to prepare a composite makeup cosmetic powder.

[Test Example 1]

In order to measure the fluorescence characteristics of the powder prepared in Example 1, UV-VIS Spectrophotometer (Perkin Elamer / Lamda 16) and Fluorescence Spectrometer (ISSK 2 / K2 Multifrequency cross-correla) was used.

1) First, by using a UV-VIS Spectrophotometer (Perkin Elamer / Lamda 16) to measure the ultraviolet absorbance of the ultraviolet absorbing fluorescent dye disodium distil biphenyl disulfonate was measured in the ultraviolet region. Next, 1 g of the sample of Example 1 was dissolved by adding ethanol, and then filtered. The filtrate was put into a quartz cell having a layer length of 10 mm x 10 mm, and ethanol was measured as a blank test solution. The results are shown in Figure 1 below.

2) On the other hand, using a Fluorescence Spectrometer (ISSK 2 company / K2 Multifrequency cross-correla) was measured by treating the sample in the same manner as in (1). In addition, the standard solution was made separately to verify the fluorescence generation spectrum using the control solution, the results are shown in Figure 2 below.

As can be seen in FIGS. 1 and 2, the fluorescence luminosity of the powder of the present invention was measured using a wavelength of 350 nm measured using a UV-Vis Spectrophotometer as an excitation wavelength. As described above, it was confirmed that blue color fluorescence of 400-450 nm appeared. In addition, as confirmed in FIG. 2, it was confirmed that the powder of the present invention exhibits a practical spectral distribution by exhibiting a wavelength of 400 to 450 nm, which is a spectral range in which the skin surface looks healthy while being transparent.

Test Example 2 Wrinkle concealment, clarity, feeling and adhesion sensory test

In order to check the wrinkle concealment, clarity, feeling of use and adhesion of the silica / plate-like barium sulfate composite makeup cosmetic powder prepared in Example 1, 20 female panels 20 to 35 years old were covered with wrinkles through transparency test. Relative assessments of feelings of use, adhesion and adhesion were conducted.

First, after applying the powder of Example 1 to the skin of each person's hand several times, wrinkle concealment, clarity, feeling and adhesion were determined in five steps according to the following evaluation criteria and the average value of the evaluation value is shown in Table 1 below. .

<Evaluation Criteria>

5: Very good 4: Excellent 3: Normal 2: Slightly poor 1: Poor

Wrinkle concealment Feeling Transparent Adhesion Example 1 4.70 4.40 4.50 3.80

As can be seen in Table 1, when the powder of the present invention was used, it was confirmed that the results of the overall excellent results in the wrinkle improvement effect, clarity, usability and adhesion of the skin surface.

Formulation Example 1 and Comparative Example 1

Formulation Example 1 and Comparative Example 1 were prepared as a liquid foundation formulation with the composition of Table 2 below.

No Name Formulation Example 1 (wt%) Comparative Example 1 (% by weight) One Composite powder of Example 1 4.00 - 2 Glycerin Monostearate 1.50 1.50 3 Sorbitol monooleate 1.50 1.50 4 Monostearic acid polyoxyethylene glycerine 1.00 1.00 5 Stearic acid 1.50 1.50 6 Cetyl alcohol 0.50 0.50 7 Cetearyl Octanoate 10.00 10.00 8 Cyclomethicone 5.00 5.00 9 Dextrin palmitate 0.30 0.30 10 Propylene glycol 5.00 5.00 11 Carboxy Vinyl Polymer 0.10 0.10 12 Iron oxides Quantity Quantity 13 Titanium oxide 5.00 5.00 14 antiseptic Quantity Quantity 15 Spices Quantity Quantity 16 Purified water to 100 to 100

<Production method>

Formulation Example 1 ; The components 10, 12, 13 were added to the colloid mill, and then passed through three times while adjusting the scale to 3, 2, 1, and washed with a part of the component 16 and put into the manufacturing part. Next, prepare the ingredients 16 in a separate container, while slowly adding the ingredients 11 and 14 uniformly while stirring with a homo mixer, and put into the manufacturing unit, heated to 80 ~ 85 ℃ and then put into the manufacturing unit to operate the emulsifier The components 1 to 9 were emulsified for 10 minutes while heating to 80 to 85 ° C. After emulsification, the mixture was cooled to 45 ° C. while stirring using a stirrer, and then ingredients 14 were added, cooled to 25 ° C., and then floated to prepare.

Comparative Example 1 ; It was prepared in the same manner as in Formulation Example 1, except that the powder of Example 1 was not contained.

Formulation Example 2 and Comparative Example 2

Formulation Example 2 and Comparative Example 2 were prepared in the formulation of Two-way Cake with the composition of Table 3 below.

No Upper division Name Formulation Example 2 (wt%) Comparative Example 2 (% by weight) One A Nylon Powder 5.00 5.00 2 Mica 20.00 20.00 3 kaoline 5.00 5.00 4 Silica 5.00 5.00 5 Zinc stearate 2.00 2.00 6 Iron oxides Quantity Quantity 7 Titanium oxide 7.00 7.00 8 Composite powder of Example 1 10.00 - 9 Talc to 100 to 100 10 B Dimethicone 5.00 5.00 11 antiseptic Quantity Quantity 12 Spices Quantity Quantity

<Production method>

Formulation Example 2 ;

1) A is added to the Henschel mixer and mixed and stirred at a constant speed.

2) Mix and stir while spraying B on A phase.

3) Mixing A and B The mixed bulk is pulverized three times with an atomizer.

4) The semi-finished product is sifted and aged in airtight storage for 2 days, and then molded (tableted).

Comparative Example 2 ; It was prepared in the same manner as in Formulation Example 2, except that the powder of Example 1 was not contained.

Formulation Example 3 and Comparative Example 3

Formulation Example 3 and Comparative Example 3 was prepared as a face powder formulation in the composition of Table 4 below.

Name Formulation Example 3 (wt%) Comparative Example 3 (wt%) A  Mica 20.00 20.00  2. nylon powder 10.00 10.00  3. Silica 5.00 5.00  4. Heavy Magnesium Carbonate 3.00 3.00  5. Zinc Stearate 3.00 3.00  6. Composite powder of Example 1 10.00 -  7. Talc to 100.0 to 100.0  8.Iron Oxides Quantity Quantity B  9. Preservative Quantity Quantity  10. Spices Quantity Quantity

<Production method>

Formulation Example 3 and Comparative Example 3; It was prepared in the same manner as in Formulation Example 2 and Comparative Example 2.

[Test Example 3]

In order to confirm the visual effect of the wrinkle concealment and clarity of the formulation example, the test subject was allowed to apply Formulation 2 to the eyes, and before and after the application was observed. The results are shown in Figures 3a to b below.

As confirmed in Figure 3, using the cosmetic composition containing the composite makeup cosmetic powder of the present invention was confirmed that it is possible to conceal the wrinkles around the eyes and natural cosmetic with a sense of transparency.

[Test Example 4]

In order to check the skin wrinkle concealment, clarity, feeling and adhesion of the formulation examples 1 to 3 and Comparative Examples 1 to 3, the four items were applied to 50 women aged 25 to 35 years and then to the following five steps. It judged and the result is shown to the following Tables 5-7.

<Evaluation Criteria>

5: Very good 4: Excellent 3: Normal 2: Slightly poor 1: Poor

division Wrinkle concealment Transparent Feeling Wheat adhesion Formulation Example 1 47 30 40 39 Comparative Example 1 3 20 10 11

division Wrinkle concealment Transparent Feeling Wheat adhesion Formulation Example 2 48 41 40 37 Comparative Example 2 2 9 10 13

division Wrinkle concealment Transparent Feeling Wheat adhesion Formulation Example 3 48 41 41 37 Comparative Example 3 2 9 9 13

As can be seen in Tables 5 to 7, Formulation Examples 1 to 3 containing the composite makeup cosmetic powder of the present invention is excellent in wrinkle improvement effect compared to Comparative Examples 1 to 3 and excellent in all aspects of transparency, feeling, adhesion It was confirmed that the preference.

As described above, when the makeup cosmetic composition was prepared using a composite makeup cosmetic powder composed of silica / titanium dioxide / plate-like barium sulfate containing the ultraviolet-absorbing fluorescent dye of the present invention, the wrinkle concealing effect and transparency were improved. It was confirmed that there is an excellent improvement effect in terms of use, skin adhesion, and the like.

1 is a graph showing ultraviolet absorbance of disodium distil biphenyl disulfonate as an ultraviolet absorbing fluorescent dye.

2 is an analysis result of the fluorescence intensity of the composite makeup cosmetic powder of the present invention.

Figure 3 is a photograph before the application of the skin of the formulation example 2 of the present invention (a) and after application (b).

Claims (4)

A composite makeup cosmetic powder comprising silica, titanium dioxide and barium sulfate containing disodium distil biphenyl disulfonate as an ultraviolet absorbing fluorescent dye. (1) 99.75 to 99.94% by weight of silica is dispersed in purified water with respect to the total weight of the composition and dispersed for 20 minutes in a slurry state, and then, the acid solution or alkaline solution is adjusted to pH 5.0 to 10.0 and redispersed. Preparing a porous silica containing an ultraviolet absorbing fluorescent dye by adding 0.06 to 0.25% by weight of disodium distilbiphenyl disulfonate as an ultraviolet absorbing fluorescent dye at room temperature and stirring for 30 minutes; (2) 87 to 90% by weight of a panic acid-type barium sulfate based on the total weight of the composition was added together with water, dispersed for 30 minutes to form a slurry, and the titanium dioxide was maintained at pH 5-10 under an acid solution or an alkaline solution. Adding a doped titanium dioxide sol while reacting at 80 ° C. for 30 minutes; And (3) 80% by weight of the reaction slurry of the step (2) was dispersed while adjusting to pH 5.0 ~ 10.0, and then the silica of step (1) was added to react for 30 minutes at 80 ℃ to prepare a composite makeup cosmetic powder Steps. delete A makeup cosmetic composition comprising the composite makeup cosmetic powder according to claim 1 in an amount of 1 to 50% by weight, based on the total weight of the composition.