KR20080011542A - Cosmetic composition containing preprocessed carbon black - Google Patents

Abstract

A cosmetic composition comprising carbon black pre-treated with polyol is provided to solve the problems of a conventional carbon black such as lumping or scattering of powder, improve a black color of the composition due to even dispersion and maximize softness by using powder having large surface area. A cosmetic composition comprises carbon black pre-treated with polyol as a black pigment, where the pre-treatment is done by soaking the carbon black in the polyol, agitating, heating and emulsifying it, the content of the carbon black is 0.01-80 wt.% regarding the total weight of the composition and the content of the polyol is 0.1-10 wt.% regarding the total weight of the composition. The cosmetic composition further comprises powder having surface area of 100-800 m^2/g.

Description

Cosmetic composition containing pretreated carbon black {Cosmetic composition containing preprocessed carbon black}

The present invention relates to a cosmetic composition comprising pretreated carbon black, and more particularly, by using pretreated carbon black in polyol to improve the dispersion of the medium to increase the sharpness of the black, with a thin particle arrangement due to the even dispersion It relates to a cosmetic composition having a soft applicability. In addition, when a powder having a large specific surface area is mixed with the composition, a cosmetic composition having a further enhanced soft feel is produced.

Carbon black is mainly used in eye cosmetic compositions such as mascara, eyebrows, eyeliners and eyeshadows. In particular, mascara consists of 73 ± 8.5㎛ thick, 5.22 ± 0.86㎛ long and 102.8 ± 20.0 black hairs on average, and it is applied to the eyelashes to raise the eyelashes to make the eyes clear. . The early mascara was a solid mixture of sodium stearate and carbon black, which was applied using a brush soaked in water.However, nowadays, vegetable ester waxes or hydrocarbon waxes are applied with high-safety polymers having appropriate plasticity and It is mixed and emulsified. As mentioned above, the purpose of mascara is to sharpen the eyes. To do this, you can think of how to make your eyebrows thicker or longer to deepen your eyes, and how to curl to make your eyes cooler.In addition, you can create a visually darker eye by sharpening the black color of the contents. have. In this case, the eyes can be made thick even when they have the same coating amount, so there is an advantage in that a clear eye can be made without lumping or burdening eyes.

Carbon black is a very fine pigment having a particle size of several tens of nanometers and is obtained by incombusting hydrocarbon gas or oil. Carbon black is used to color, stabilize the contents and color the plastics and coatings. Carbon black, which has the advantage of superior black color compared to iron oxide or titanium oxide, which shows other black colors, has been used in food, medicine and cosmetics until the 1960s. However, carbon black began to be questioned for its safety, especially in the US because of the possibility of eluting polynuclear aromatic hydrocarbons (PNA's or PAH's) such as 3,4-benzoanthracene, a carcinogen. Esau has been regulated since 1976. The regulation was licensed for use only in D & C Black # 2, a carbon black refined by CTFA in 2004 in the United States.

Looking at the technology using the conventional carbon black, there is a composition patent (application number: 1987-040667) combining a conventional makeup material, 5 to 95% silica and 5 to 95% fibrous polyethylene. It claims to include carbon black as only one term of the pigment together with iron oxide, chromium oxide and titanium oxide as a claim, but it does not introduce the advantages of carbon black itself. Another patent for invention of effective eyebrows is 0.1 to 2.0% water soluble polymer (e.g. carboxy vinyl polymer), 10 to 30% water soluble resin (e.g. vinyl acetate-vinylpyrrolidone polymer) and 0.1 to 10.0% There is a patent (application number: 1997-115262) which uses the dye fiber (the nylon fiber colored with carbon black, 0.1-5.0 mm in length, and 0.1-9.0 denier). This patent uses fibers to express effective eyebrows and uses a black pigment as a coating to color the fibers. Another patent is a patent for dyeing inks for eyebrow pencils or gray hair (application number: 1994-298024), which contains pigments and oils based on carbon black fiber powder from 0.1 to 1.0 mm, especially over 500 micrometers in length. In this case, the carbon black fiber can be used for multi-faceted and non-planar, thinning effect. In addition, carbon black is used incidentally to produce the color of the fiber, and there is no detailed description of the advantages of carbon black in addition to the method of handling the carbon black or color. Lastly, it is about solid cosmetics such as eyeliner and eyebrow, and it is a patent that improves the shape retention and improves the feeling by using pore kaolin, bentonite, carbon black, graphite or carbide (application number: 1985-038463), both formulations deal only with dispersion formulations and do not address the use and benefits of emulsion types. As such, the existing patents are not for carbon black powder, but for patents for fibers colored with carbon black or for manufacturing solid solid makeup products.

Thus, the present inventors, while studying the cosmetic composition using the carbon black, when using the carbon black pre-treated with a polyol, it is easy to disperse in the emulsified formulation, and can increase the sharpness of the black by even dispersion, and also soft It has been found that a cosmetic composition with a feeling of use can be prepared, and furthermore, the present invention has been found to exhibit a much softer feeling when applied using a powder having a large specific surface area in the composition.

It is therefore an object of the present invention to provide a cosmetic composition comprising carbon black pretreated with a polyol.

In order to achieve the above object, the present invention provides a cosmetic composition comprising a carbon black pre-treated with a polyol as a black pigment.

In addition, the cosmetic composition provides a cosmetic composition, characterized in that further adding a powder having a specific surface area of 100m ² / g ~ 800m ² / g.

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

D & C Black # 2, a high-purity carbon black used in place of iron oxide in the present invention, has a specific surface area of 200-260 m ² / gram, a weight loss of less than 2%, an ash content of less than 0.15%, and a PHA's content of 500 ppb or less, which is a US FDA-approved requirement. LCp Unipure LC 902 and Geotech Midnight Black were used as raw materials satisfying benzo pyridine of 5 ppb or less and dibenzatracin 5 ppb.

The carbon black is preferably contained in 0.01 to 80% by weight of the total weight of the composition, most preferably 0.5 to 20% by weight. When the content of the carbon black exceeds 80% by weight, the stirrer may not be properly operated due to the increase in viscosity during manufacture, and thus it may not be dispersed. Such a composition that is not properly dispersed cannot be emulsified and layer separation occurs.

Examples of the polyol for wetting the carbon black include glycerin, propylene glycol, 1,3 butylene glycol, butylene glycol, and polyethylene glycol having a liquid phase at a normal temperature of 200 to 600. In addition, pentylene glycol and hexylene Polyols having a high average molecular weight such as glycol and the like can be considered, but these are not suitable for cosmetics because of their irritation and smell, and when the molecular weight is higher than 1000, it is difficult to wet carbon black because they have a semi-solid or solid phase. The content of the polyol is different depending on the content of carbon black to be used.If you want to use 5% by weight of carbon black soaked in 1,3 butylene glycol at 50% by weight, 5% by weight of butylene glycol is formulated. Will be used within. In order to use the carbon black dye, since the polyol is added together, it is necessary to pay attention to the content of the polyol that is carefully wetted according to the formulation. If it is intended to be used in creamy formulations, the use of excess polyols of more than 10% by weight can give a tight feeling, while formulations that require moisture sustainability, such as mascara, can contain more than 10% by weight of polyols with high hydroxyl groups (-OH). When used, it is difficult to prevent smearing. Therefore, the polyol is preferably contained in 0.1 to 10% by weight of the total weight of the composition. In the case where the carbon black is used without pretreatment in a polyol, when the carbon black is dispersed in a medium of 1% or more, the carbon black does not mix with the medium and turns white so that the dispersion itself cannot proceed.

Table 1 shows the presence or absence of dispersibility when the carbon black was not pretreated with the polyol and when pretreated.

Pretreatment (Polyol) X (none) ○ (glycerine) ○ (propylene glycol) ○ (1,3-butylene glycol) Dispersibility of Carbon Black X ○ ○ ○

○: well dispersed in the medium

X: Not distributed

As shown in Table 1, it can be seen that the dispersion itself cannot proceed if the carbon black is not pretreated with the polyol in advance.

Compared to the sample using iron oxide, the sample using carbon black, which is pretreated, is not only dark in color but also fine in size of 20 to 30 nm, so that a fine dispersion and emulsification surface can be created. It exhibits smooth spreadability, especially at the time of application, and the use (powderability) can be further increased by using a powder having a specific surface area of 100 m ² / g or more. When the powder is used to further improve applicability, a powder having a size of 1 to 3 micrometers or less or a specific surface area of 100 to 800 m ² / g is preferable. More preferably, a powder having a specific surface area of 300 m ² / g to 800 m ² / g is advantageous. For example, Sunsphere series, which is a silica series from Asahi Glass, is advantageous, among which H-32, H-52, H-122, H33, and H53 having a large specific surface area and oil absorption are particularly effective. . Among the Godball series of Suzuki Oil Industry Co., Ltd., B-6c, B-25c, E-6c, D-11c, and E-16c are preferred, such as porous and hollow methacrylate (PMMA) and polytetrafluoroethylene ( PTEE), Jurymer MB1, silica, alumina, aluminosilicate (Sunsil 130 / 200-260 m ² / g) and Silica Beads (SB 260 m ² / g) with high specific surface areas are recommended. Powders having a large specific surface area are advantageous as described above for smooth spreadability, and their content is preferably 0.1 to 5.0% by weight based on the total weight of the composition. At less than 0.1% by weight, the shear thinning effect, which causes soft spreadability, is difficult to see, because the amount of powder is too small compared to the whole system, which is inadequate to change the overall feeling. In the case of more than%, the large specific surface area is not suitable because the powder itself is difficult to be entangled and dispersed by catching oil, wax polyol, water, etc. in the formulation. In the case of using the powder having a large specific surface area, the content of which the viscosity is increased by the powder is easily pushed out by the stress (Stress), thereby making it possible to feel an excellent usability (appliability) when applying the cosmetic contents.

Hereinafter, although an Example and a test example are given and this invention is demonstrated in detail, this invention is not limited by these.

Table 2 shows the structures of Examples 1 to 6 and Comparative Example 1 as preparation examples of mascara. Examples 1 and 2 are carbon blacks manufactured by LCW, respectively, and mascara is prepared using only 1/10 (1% by weight) and 1/5 (2% by weight) of iron oxide, and Examples 3 and 4 are carbons manufactured by Geotech. Mascara was prepared using only black (1/10 (1% by weight), 1/5 (2% by weight)) of iron oxide. In addition, Example 5, 6 adds silica powder with a large specific surface area, using 2 weight% of carbon black by Geotech. Comparative Example 1 is prepared as 10% by weight of iron oxide which is a pigment mainly used as a control for comparing the color and spreadability with Examples 1 to 6.

Examples 1 to 6 and Comparative Example 1 Ingredient Name Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative Example 1 1.Purified water to 100 to 100 to 100 to 100 to 100 to 100 to 100 2.butylene glycol 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.glycerine 5.0 5.0 5.0 5.0 5.0 5.0 5.0 4.hydroxyethyl cellulose 0.5 0.5 0.5 0.5 0.5 0.5 0.5 5.ethanol 2.0 2.0 2.0 2.0 2.0 2.0 2.0 6.acrylate copolymer 15.0 15.0 15.0 15.0 15.0 15.0 15.0 7.Unipure LC902 (LCW) 1.0 2.0 - - - - - 8.Midnight Black (Geotech) - - 1.0 2.0 2.0 2.0 - 9.iron oxide - - - - - -  10.0 10.Cellulose Fiber 2.0 2.0 2.0 2.0 - - 2.0 11.Sunsphere H51 - - - - 2.0 - - 12.Godball B-25c - - - - - 2.0 - 13.Sorbitan Oliveate 5.0 5.0 5.0 5.0 5.0 5.0 5.0 14.Beswax 10.0 10.0 10.0 10.0 10.0 10.0 10.0 15.stearyl alcohol 2.5 2.5 2.5 2.5 2.5 2.5 2.5 16.Kanauba 2.0 2.0 2.0 2.0 2.0 2.0 2.0 17.preservative Quantity Quantity Quantity Quantity Quantity Quantity Quantity

The carbon blacks used in Examples 1 to 6 of Table 2 were 10 to 80% by weight of the carbon black to the total weight of the polyol as a pretreatment, so that the carbon black was well wetted with the polyol for 1 to 120 hours. Stirred.

When the content of the carbon black is less than 10% by weight based on the total weight of the polyol, the polyol, which is inevitably added together with the carbon black, enters nine times or more, which may affect the sustainability or feel of the formulation. In the case of more than 80% by weight of the carbon black relative to the carbon black powder can not be sufficiently wetted, can not be properly pretreated.

The time is determined by the amount of carbon black to be wetted and the amount of polyol used at this time. If you want to soak 100 g of carbon black in 100 g of 1,3 butylene glycol, it will take about 10 to 50 hours. If the time is shorter than this, the carbon black is not sufficiently wetted in the polyol, and the stirring itself is difficult, and even if the stirring is difficult, the dispersion in the formulation is difficult and the emulsification is broken. On the other hand, if you want to moisten a smaller amount of carbon black, for example, about 10g in 100g butylene glycol, can be emulsified cleanly by stirring after 5 hours. Thus, the time required to wet the carbon black in the polyol is determined by the amount of the carbon black and the content of the polyol used. If you want to wet carbon black in an amount of 10 to 80 g at 10 to 80% by weight in polyol, it will take about 1 to 120 hours.

How to stir after this is divided by the weight ratio of carbon black to polyol, if less than 20% by weight Agi-Mixer or Paddle Mixer (Homo-Mixer) ) Is advantageous and can effectively stir when using a roll mill. If the carbon black is 20 wt% or more with respect to the polyol, it is difficult to stir with an Agi-Mixer, Paddle Mixer, or Homo-Mixer, and must be stirred using a roll mill.

<Production method>

1) The components 1-6 were heated to 70 degreeC.

2) Pretreated carbon black (Examples 1 to 6) or iron oxide powder was added to 1) as prescribed and stirred.

3) Components 13-17 were heated to 75 ° C.

4) The emulsion was added to 2) above while slowly emulsifying and cooled to 35 ° C.

5) It was filled in a mascara container.

Test Example 1 Color Comparison Test

In order to compare the colors of Examples 1 to 4 and Comparative Example 1, the color was measured according to the following method and the results are shown in Table 3 below.

The mascara contents were sufficiently inserted into 1 cm crystal cells, and the brightness and saturation of the contents were measured using a Xenon flash spectrophotometer of Hunter Lab. The value representing the brightness value is represented by L *, and the smaller the value, the higher the black color. The value of a is red and green. It has a positive value and has a larger absolute value. The red value has a larger value. The b value is a yellow and blue value. If the absolute value is large while having a positive value, the yellow value is more yellow. If the absolute value is large and has a negative value, the value b is more blue.

Item Example 1 Example 2 Example 3 Example 4 Comparative Example 1 L * 8.11 6.81 6.96 5.44 16.27 A -0.25 -0.62 0.05 0.21 -0.76 B -1.43 -1.43 -0.95 -0.08 -3.94

As shown in Table 3, when carbon black is used instead of the iron oxide (Comparative Example 1), which is mainly used, it was found that a much darker color can be expressed even with only 1/10 of the iron oxide. In particular, the color was the most excellent in Example 4 using the carbon black of Geotech Co., Ltd. When using the Geotech pigment, especially when used at 2% by weight, the hardness is about twice as high as using 2% of the LCW pigment It has a disadvantage that it is rubbed on.

Test Example 2 Usability Test (Viscosity Data at the Time of Application)

The viscosity data at the time of application | coating was measured in order to know the usability of the said Examples 1-6 and Comparative Example 1. The instrument uses an AR2000 Rheometer, and the accessory used was designed to measure high viscosities such as cream or mascara due to its short radius, and the instrument was used at a radius of 1 cm and an inclination angle of 1 °. Viscosity at shear rate 1000 (1 / s) was measured. In general, the delivery rate when applying cosmetics is reported as 1 ~ 1000 (1 / s), the viscosity at this time is the value of the resistance to movement when the fluid moves, the larger the value, the more difficult to enter the force to prevent movement. On the contrary, when the viscosity is low, the resistance that hinders this movement is small and can flow easily. Therefore, the small value of the viscosity at the time of application means that the contents spread easily in the application direction.

Table 4 below shows the viscosity values measured at delivery rates of 1000 (1 / s) for Examples 1-6 and Comparative Example 1. In addition, the evaluation of the usability for the application of the mascara during the application was performed.

Item Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative Example 1 Viscosity (Pas) 0.52 0.70 0.78 0.67 0.13 0.23 8.24 Usability Evaluation ○ ○ △ ○ ◎ ◎ ×

◎: Very smooth coating

○: Apply gently when applied

△: normal

×: stiff

When carbon black is 1/10 smaller in size than iron oxide and a force is applied to the contents, the rearrangement of the contents occurs more easily than in the contents using iron oxide, and for this reason, the viscosity at the transfer rate of 1000 (1 / s) is easily lowered. You can spread the contents and you can see that the applicability improves eventually. As shown in Table 4, in Examples 1 to 4, the spreadability was better when the content was low in the case of LCW (Examples 1 and 2), but rather in the case of Geotech (Examples 3 and 4) The spreadability was better at 2% than at 1% when the viscosity value was low.

Example 5 is the addition of Sunsphere Series H-51, a porous silica from Asahi glass of 800 m ² / g. The average size of the silica is 5 micrometers, larger than carbon black, but due to the large specific surface area, It can contain a lot of content. However, when the delivery rate is large, the contents can be easily discharged out, resulting in a large drop in viscosity depending on the delivery rate. When the powder contains such a large specific surface area, it has a lower resistance to movement in the transmission rate of 1000 (1 / s), and thus the spreadability feels better. Example 6 is an example in which Godball B-25c, which is a hollow silica of Suzuki oil-containing, was carried out instead of H-51. The Godball series is a hollow or porous silica series with a large surface area of 100 to 800 m ² / g and an average particle size of 0.5 to 150 micrometers. As a result of the measurement, Example 6, like Example 5, showed a low viscosity at a transmission rate of 1000 (1 / s) and had excellent spreadability. On the other hand, the viscosity at the transmission rate of 1000 (1 / s) of Comparative Example 1 using iron oxide is about 10 to 80 times larger than Examples 1 to 6 using carbon black, indicating that the value has a large resistance to movement In the case of Comparative Example 1 was confirmed that it has a disadvantage that it is not easily spread when applied. The spreadability through the value of this viscosity was also in agreement with the usability evaluation for spreadability through the panel.

As shown in Table 4, compared with Comparative Example 1, Examples 1 to 6 all had a low viscosity value at a transmission rate of 1000 (1 / s) was confirmed to show a smooth application, especially as in Examples 5, 6 It was found that the use of silica with a large specific surface area could result in a softer feel.

Test Example 3 Eye Stimulation Test

In order to test the eye irritation of the mascara prepared with the compositions of Examples 1 to 6 and Comparative Example 1, an eye stimulation test using an egg (HETCAM-HEN'S EGG TEST ON THE CHORIOALLANTOIC MEMBRANE) was performed. The test method used the test method defined in the CTFA SAFETY TESTING GUIDELINES. When white eggs are hatched at 37 ± 0.5 degrees and 55 ± 7% for 10 days, when air is observed, select only eggs with well-developed Chorioallantoic membranes (CAMs), remove eggshells and egg shells, and thin the test substance on a parafilm. After spreading, the test substance was applied downward to the CAM for a predetermined time (30 seconds) and washed with physiological saline to evaluate the reaction. The results were evaluated according to the evaluation criteria in the preliminary experiment of Table 5. The evaluation by HET-CAM was expressed as the sum <S> of each observation item H, L, and C (Hemorrhage, Lysis, Coagulation), and the S value was obtained by the stimulation index.

Reference substance Judgment Response pattern Score 0.5% Texapon ASV Weak Hemorrhage and lysis 1 (0 if no response) 1.0% Texapon ASV Moderate 2 5.0% Texapon ASV Strong 3

The test was carried out six times, and the results are summarized in Table 6 below. In the following Table 6, the average stimulus score is less than 6 is "◎" as the light stimulation (SLIGHTLY IRRITATING), "6" is 6 to 12 is "O" as the middle stimulation (MOERATELY IRRITATING) "IR" is irritating (IRRITATING) "△ ", Greater than 16 are marked with" X "as SEVERELY IRRITATING, respectively.

Test substance HET-CAM test results Example 1 ◎ Example 2 ◎ Example 3 O Example 4 O Example 5 O Example 6 O Comparative Example 1 O

As shown in Table 6, compared with Comparative Example 1 of the existing mascara product, Examples 1 to 6 according to the present invention showed a level of stimulation not much different. Therefore, it can be seen that the cosmetic composition of the present invention can be used safely without any irritation to the eyes like conventional products.

As described above, the present invention facilitates the manufacturing operation by improving the agglomeration or dusting of the existing carbon black through the pretreatment of the carbon black, and improves the black color of the cosmetic composition due to even dispersion, furthermore the specific surface area The large powder was used to maximize the softness of the even dispersion of carbon black.

Claims (8)

A cosmetic composition comprising carbon black pretreated with a polyol as a black pigment. The cosmetic composition according to claim 1, wherein the pretreatment is performed by soaking carbon black in a polyol, stirring, heating, and emulsifying. According to claim 1, wherein the carbon black is a cosmetic composition, characterized in that contained in 0.01 to 80% by weight relative to the total weight of the composition. The cosmetic composition according to claim 1, wherein the polyol is contained in an amount of 0.1 to 10% by weight based on the total weight of the composition. The cosmetic composition according to any one of claims 1 to 3, wherein the carbon black is pretreated by stirring at 10 to 80% by weight based on the total weight of the polyol. The cosmetic composition according to any one of claims 1 to 3, wherein the carbon black is pretreated by stirring for 1 to 120 hours with the polyol. The cosmetic composition according to any one of claims 1 to 4, further comprising a powder having a specific surface area of 100 m ² / g to 800 m ² / g. The cosmetic composition according to claim 7, wherein the powder is contained in an amount of 0.1 to 5.0% by weight based on the total weight of the composition.