KR20040100280A - Manufacturing Method of Pigments Composition Containing Silkpowder - Google Patents

Abstract

PURPOSE: Provided is a manufacturing method of a pigment composition containing silkpowder as a moisturizing material by ring mill. Therefore, make-up base or foundation containing the pigment composition has moisturizing effect, skin safety and excellent coloring effect, and gives good feeling in use. CONSTITUTION: The manufacturing method of a pigment composition containing silkpowder comprises the steps of: pre-dispersing one of chromium oxide green and iron oxide, and titaniumdioxide, silkpowder, methylmethacrylate crosspolymer and cyclomethicone at room temperature at 1500 rpm for 15 minutes; and dispersing them at 1000 rpm for 50 minutes using a ring mill.

Description

Manufacturing Method of Pigment Composition Containing Silk Powder {Manufacturing Method of Pigments Composition Containing Silkpowder}

The present invention relates to a method for producing a cosmetic pigment composition containing a silk powder as a moisturizing substance, in order to improve the dispersibility of a pigment base containing a silk powder dispersed using a ring mill (Ring Mill) in a particle size The present invention relates to a method for preparing a silk powder-containing pigment composition for make-up cosmetics having improved adhesion and moisturizing power to skin by minimizing particle size.

Silk powder is a natural protein produced by silkworms from mulberry, which is a natural plant, and has been used as a clothing material since ancient times because it has excellent moisturizing and dyeing properties, and has a unique luster and feel.

Such silk is synthesized and secreted from the silk gland of 5th-age silkworms, and exists in a kind of solution called liquid dog in the silkworm body. The liquid dog is coated with the protein sericin, which is spun from the earth and sand to form a fiber and cocoons.

The main constituents of cocoon fibers are 70-80% of fibroin and 20-30% of sericin covering them, and when treated with hot water or alkali, sericin is easily dissolved and finally gives the silk a unique luster.

The amino acid composition of fibroin is about 40% glycine, about 25% alanine and about 13% serine, and its molecular structure is a single glycine-cross-linked -GAGXGA- (G: glycine, A: alanine, X: other Amino Acids) are arranged regularly.

Fibroin has excellent moisturizing and systemic properties and has a soft texture. It has been used as a powder raw material for makeup products for a long time. The hydrolyzate is mainly used in hair care along with hydrolysates of other proteins, collagen or keratin. It has been used in products.

Thus, look specifically at the example of the prior art applied to the silk powder or silk protein cosmetics as follows.

Korean Patent Publication No. 1999-68624 discloses a hair care composition for hair and perm containing silk protein and cysteine as a hair protector together with a humectant, a dye, a coloring agent and the like.

In addition, the Republic of Korea Patent Publication No. 2002-96607 is a cosmetic composition that has a low-molecular silk protein prepared by hydrolysis using proteolytic enzymes to improve the product safety and long-term storage stability while improving the moisturizing effect without stickiness when using Attempts have been made to provide.

In addition, the Republic of Korea Patent Registration No. 170572 discloses a method for producing a composite pigment for coloring cosmetics having improved cosmetic sustainability and high affinity by coating a silk protein with an anionic polymer and a skin lipid-like component in a spherical powder.

However, in these prior arts, the silk powder or silk protein was used as it is, or coated on the composite powder. When the silk powder is mixed and used according to a general cosmetic manufacturing process, the particle size is relatively large. There was a problem that the skin could not be uniformly coated, and when the silk protein is coated on the composite powder as in the Korean Patent Registration No. 170572, it may be deteriorated due to being adsorbed on the surface of the powder for a long time and the actual cosmetics. In the process of manufacturing the product has been a problem that the silk protein is separated from the outside and the moisturizing component is not evenly delivered to the skin.

Therefore, in order to minimize the size of the dispersed silk powder particles by dispersing the silk powder-containing pigment base by using a ring mill device, it is possible to achieve a good dispersion of the pigment, is uniformly applied on the skin, the color expression is good and the feeling of use of color products It is now possible to manufacture improved color products that have been greatly improved.

The present invention is to overcome the problems of the prior art, by minimizing the particle size of the dispersed silk powder so that the dispersion can be made well when the pigment is dispersed, it is uniformly applied on the skin, the color expression is good and the feeling of use of the color product This significantly improved improved color tone product can be produced, which significantly improves the disadvantages of existing products in moisturizing power, safety, particle size and dispersion and product properties, ie viscosity and color. It is to provide a method for producing a pigment composition for.

To this end, the present invention, the titanium dioxide, silk powder, chromium oxide green or iron oxide, methyl methacrylate crosspolymer, cyclomethicone is dispersed at room temperature for 15 minutes at 1500 rpm using a disper and a ring mill It provides a method for producing a cosmetic pigment composed of a secondary dispersion step of dispersing at 1000 rpm for 50 minutes.

1 is a graph showing the particle size distribution of Examples 1 and 2 and Comparative Examples 1 and 2 of the present invention;

2 is a diagram showing the color comparison of Examples 1, 2 and Comparative Examples 1, 2 of the present invention,

Figure 3 is a diagram showing a comparison of the moisturizing power of Examples 1 and 2 of the present invention and Comparative Examples 1 and 2.

The present invention is to minimize the size of the dispersed particles by using a method for dispersing the pigment base containing the moisturizing silk powder in the size of the particles, thereby increasing the moisturizing power and greatly improve the adhesion and dispersibility to the skin, the silk powder-containing ring mill treatment It relates to a method for producing a cosmetic composition.

The color products that have been commonly used up to now, including those containing silk powder, have a weak point that they are very tightly adhered to the skin due to the large size of dispersed pigment particles and poor pigment dispersion.

The present inventors have been struggling to overcome such disadvantages of the existing products, that is, the disadvantages of large particle size of silk powder and silk protein coating powder, lack of dispersion, uneven application on the skin during use, color tone When cosmetics are produced by dispersing active ingredients, including silk powder, by using a ring mill, the particle size becomes fine and dispersion is made well. Therefore, it can be uniformly applied on the skin during use, so that color expression and feeling are improved. This invention was completed.

In view of this, the present invention, by ring milling the pigment base containing the moisturizing material silk powder to disperse to the particle size to minimize the size of the dispersed particles, the moisturizing power is increased and adhesion to the skin and dispersibility is greatly improved color It can be said that it is related with the manufacturing method of the pigment composition containing the silk powder excellent in expression.

Ring Mill is a kind of Bead Mill which disperses the mixture by using Zirconia beads as a dispersion medium.The Bead is 0.3mm in diameter of Zirconia and uses 80% of the total volume and the Zirconia Bead to be processed. Tens of thousands collide at 1000rpm to refine the powder, including the pigment in the dispersion, in the present invention, Model No. RG-100 was used.

Hereinafter, with reference to the accompanying drawings, and production examples and test examples to explain in more detail the manufacturing method of the present invention, but is not intended to limit the present invention to this.

1 is a graph showing the particle size distribution of Examples 1 and 2 and Comparative Examples 1 and 2 of the present invention, Figure 2 is a diagram showing the color comparison of Examples 1 and 2 and Comparative Examples 1 and 2 of the present invention. 3 is a diagram showing a comparison of the moisturizing power of Examples 1 and 2 and Comparative Examples 1 and 2 of the present invention.

In the method for preparing a cosmetic composition of the present invention, as shown in the following preparation example, disperse titanium dioxide (TiO ₂ ), chromium oxide green (Cr ₂ O ₃ ), methacrylate acrylate crosspolymer and cyclomethicone together with silk powder. The pre-dispersion process is carried out for 15 minutes at 1500 rpm and the same contents are dispersed into particles for 50 minutes at 1000 rpm with a ring mill to make fine powder silk pigment-containing pigment composition for the preparation of color cosmetics.

Preparation Example 1 Preparation of Pigment Composition

After the basis weight according to the composition of Table 1 and pre-dispersed at 1500 rpm for 15 minutes with a disper at room temperature, the same contents were dispersed in a ring mill for 50 minutes at 1000 rpm as Example 1, and the composition of Table 1 After weighing according to the predispersion at room temperature for 15 minutes with a disperser at 1500 rpm for 15 minutes, this was treated three times using a three-stage roller instead of a ring mill as a comparative example 1 to prepare a silk powder-containing pigment composition of the makeup base formulation.

The 3-stage roller is a device that disperses the contents while rotating three cylinders for good dispersion. It is a device that is often used in the process of dispersing pigments in the manufacture of makeup cosmetics. The dispersion time of the pigment was determined to be 50 minutes, because the dispersion was observed under a microscope and showed the best dispersion effect at 50 minutes.

In addition, as a silk powder, CAS (Chemical Abstracts Service) No. : 9009-99-8 was used as the methacrylate acrylate crosspolymer having a molecular formula of (C ₁₀ H ₁₄ O _{4 ′} C ₈ H ₈ O ₂ ) _X , and cyclomethicone was used as the following molecular formula. .

On the other hand, when using the iron oxide instead of chromium oxide green in the composition of Table 1 can be prepared a pigment composition for the formulation formulation, as described above, the method for producing a pigment composition of the present invention by changing a part of its composition, that is, all makeup cosmetics, that is, color cosmetics It is applicable to the preparation of the composition.

No Name Example 1 (% by weight) Comparative Example 1 (% by weight) One Titanium dioxide 1.0-10.0 1.0-10.0 2 Silk Powder 0.01 to 10.0 0.01 to 10.0 3 Chromium Oxide Green 0.01 to 5.0 0.01 to 5.0 4 Methyl methacrylate crosspolymer 0.1-2.0 0.1-2.0 5 Cyclomethicone To 100 To 100

Manufacturing method

Example 1

The components 1 to 5 were predispersed at 1500 rpm for 15 minutes with a disper at room temperature, and then dispersed at 50 rpm for 2 minutes at 1000 rpm using a ring mill to prepare a pigment composition.

Comparative Example 1

The components 1 to 5 were predispersed at 1500 rpm for 15 minutes with a disper at room temperature, and then treated three times using a three-stage roller to disperse secondarily to prepare a pigment composition.

Using a particle sizer (Particle Sizer, Model Mastersizer 2000, Malvern, UK), the size of the dispersed particles was measured 30 times with respect to Example 1 and Comparative Example 1 prepared as described above, the average value of the results 2 is shown. The unit of Table 2 is a micrometer (μm).

Item Example 1 Comparative Example 1 Average particle size 2.565 5.623

As shown in the results of Table 2, although the pigment composition was made with the same composition, it can be seen that there is a difference in the size of the particles, in particular, Example 1 is dispersed by showing that the particles are very small than Comparative Example 1 It was found that the state was made of fine particles.

On the other hand, the distribution of the particle size measured for Example 1 and Comparative Example 1 is shown graphically in Figure 1, the microdispersion particles of Example 1 of the present invention is not only small in size, but also the distribution of particle size By forming a narrower range compared to 1, it was made into more uniform particles, and thus, the moisturizing component of the silk powder could be spread evenly on the skin, thereby increasing the moisturizing property.

Preparation Example 2 Preparation of Cosmetic Composition

Using the pigment composition prepared in Example 1 and Comparative Example 1, according to the composition and preparation method of Table 3 below, using Example 1 cosmetic composition of Example 2 of the makeup base formulation, using Comparative Example 1 To prepare a cosmetic composition of Comparative Example 2 of the makeup base formulation. The units in Table 3 are by weight.

No. ingredient Example 2 Comparative Example 2 One Ozokerite 1.2 1.2 2 Calcium stearate 0.68 0.68 3 Cyclomethicone 16 16 4 Cetyl Dimethicone Copolyol 1.7 1.7 5 Sorbitan sesquioleate 0.1 0.1 6 Dimethicone Crosspolymer-3 9.0 9.0 7 Sorbitan isostearate 0.3 0.3 8 Hexyllaurate 3.38 3.38 9 Tocopheryl Acetate 0.03 0.03 10 Butylene glycol dicaprylamide / dicaprate 1.0 1.0 11 Octylmethoxycinnamate 3.0 3.0 12 Example 1 25.0 - 13 Comparative Example 1 - 25.0 14 Butylene Glycol 4.0 4.0 15 Triethanolamine q.s q.s 16 Trisodium IDT 0.02 0.02 17 Purified water To 100 To 100 18 antiseptic q.s q.s 19 incense q.s q.s

Manufacturing method

1) The oily ingredients, i.e. components 1 to 11, are added to the main kiln and mixed and dissolved for 20 minutes at 20 rpm with a paddle mixer while warming to 70-75 ° C.

2) Example 1 (12) is added to the oil phase component of 1) and Example 1 (13) is added to Comparative Example 2, and mixed and dispersed for 10 minutes at 2500 rpm with a homomixer.

3) The aqueous phase component, i.e., components 14 to 17, is introduced into the aqueous phase bath and warmed to 70 to 75 ° C to completely dissolve.

4) The water phase component of 3) in the state of 70 to 75 ° C was introduced into the main kiln of 2), emulsified at 3500 rpm for 10 minutes using a homomixer, cooled to 45 ° C, and then additives, that is, components 18 and 19 It completes at 35 degreeC, stirring.

Thus prepared Example 2 and Comparative Example 2 using a particle size analyzer (Particle Sizer, Model Mastersizer 2000, Malvern, UK) to measure the size of the dispersed particles by 30 times the number of iterations and the average value of the results are shown in Table 4 below It was. The unit of Table 4 is micrometer (micrometer).

Item Example 2 Comparative Example 2 Average particle size 6.12 14.56

As shown in the results of Table 4, as in the case of Example 1 and Comparative Example 1, which is a pigment composition, there was also a difference in the size of the particles of Example 2 and Comparative Example 2 prepared as an actual cosmetic using them In particular, it can be seen that, in Example 2, the particles are much smaller than Comparative Example 1, so that the dispersed state is made of fine particles.

On the other hand, the distribution of the particle size measured for Example 2 and Comparative Example 2 is shown graphically in Figure 1, the microdispersion particles of Example 2 of the present invention is not only small in size, but also the distribution of the particle size is Comparative Example By forming a narrower range compared to 2, it was made into more uniform particles, and thus, it could be expected that the moisturizing ingredients of silk powder and silk protein were spread evenly on the skin to increase moisturizing properties.

Hereinafter, the performance as a cosmetic was tested using the cosmetic composition of the makeup base formulation prepared as Example 2 and Comparative Example 2.

Test Example 1 Safety Test

Patch tests were conducted to test the safety of the makeup base formulation cosmetics containing the micronized composition prepared by Example 2 of the present invention. 11 subjects (female age 28.7 years old) participated in the test and applied 10µg of the sample to the area of 2 × 2cm ² of each subject's left arm and closed it with a patch and then swelled after 48 hours. Observation was made by visual observation, and the number of subjects corresponding to each degree of stimulation is shown in Table 5 below.

Sample Erythema, itching Swelling No irritation Example 2 - - 11

As a result of the safety test, there was no subject showing the irritation or side effect symptoms with respect to the cosmetic composition of Example 2. That is, it can be seen that the composition of Example 2 of the fine particle dispersion particles prepared using the ring mill improved the safety of the silk powder as a cosmetic by not showing irritation symptoms such as erythema, itching, and swelling.

Test Example 2 Moisturizing Effect Test

The moisturizing effect was tested using Example 2 and Comparative Example 2.

Participants were 20 women in their late 20s to late 40s (mean age: 32.3 years) with no adverse effects on cosmetic use and good health.

The test is a three-time measurement of moisture and oil content after application of the sample of Example 2 and Comparative Example 2, and the measurement of the moisture and oil before application of the sample to the area of 2 × 2 cm ² of the left arm of each subject and the application of 10 μg each. One minute after application, four hours later and six hours later, moisture and oil were measured.

Moisture measurement was performed using Sebumeter SM 825 (Courage & Khazaka, GmbH, Cologne, Germany) to measure the relative capacity of moisture content by measuring the capacitance according to the water content with the highest insulation coefficient in the skin. The average value measured at the time point before application, after 1 hour, after 4 hours, and after 6 hours was used.

For the measurement of oil content, Sebumeter SM 815 (Courage & Khazaka, GmbH, Cologne, Germany) was used to measure the average amount of oil (sebum) secreted on the skin surface.

Table 6 below shows the average value of the measured values.

moisture Oil Before application 1 hour later 4 hours later 6 hours later Before application 1 hour later 4 hours later 6 hours later Example 2 22.6 32.7 31.0 29.6 2.2 38.3 22.3 11.3 Comparative Example 2 22.6 29.9 27.5 26.3 2.2 34.4 19.2 7.8

As shown in the results of Table 6, it can be seen that Example 2 has a higher value of oil and moisture even after the time compared to Comparative Example 2, which can be used to prepare the pigment composition containing the silk powder in the form of fine particles. It was judged that it was possible to improve the moisturizing power by being able to prepare a cosmetic composition of the powdered makeup base formulation accordingly.

Test Example 3 Color and Viscosity Test

Viscosity and color were measured for Examples 1 and 2 and Comparative Examples 1 and 2 of the present invention to test the quality as a cosmetic.

Viscosity test, the viscosity of the dispersed particles of Examples 1 and 2 and Comparative Examples 1 and 2 using a viscosity measuring instrument (Model; Brooks, USA, Spindle No. 4, Speed 6) up to 8 days after manufacture 1 The average value measured once was recorded and the color was evaluated by measuring the color using a spectrophotometer (Nippon Denshoku, Model No. NF-333, Japan).

The average of the results is shown in Table 7 below. The viscosity unit of Table 7 is cPs (Centipoise) and the color is expressed as L ^* , a ^* , b ^* values according to USC notation, where L ^* represents the brightness of the color and a ^* represents the red side of-. The green side is shown, and b ^* is the coefficient which shows the yellow side of + side, and the blue side of side.

Item Example 1 Comparative Example 1 Example 2 Comparative Example 2 Viscosity 737 22 24,917 20,957 color L ^* value 83.27 83.95 80.93 83.66 a ^* value -8.27 -6.02 -8.94 -6.78 b ^* value 6.32 1.98 7.19 4.56

As can be seen from the results shown in Table 7, the pigment composition of Example 1 and the cosmetic composition of Example 2 prepared using a ring mill were prepared using the pigment composition of Comparative Example 1, which was prepared using a three-stage roller. Compared to the cosmetic composition of Comparative Example 2, Example 1 measured about 715 cPs higher than Comparative Example 1, and Example 4,000 was about 4,000 cPs higher than Comparative Example 2, and in the case of color, Examples 1 and 2 were comparative examples. It can be seen that the colors appeared darker toward green and blue than 1 and 2, because it was determined that Examples 1 and 2 were composed of particles finer than Comparative Examples 1 and 2.

In particular, the color and viscosity characteristics were determined that each composition is composed of finer microparticles, so that the silk powder component can be uniformly applied on the skin, which is a very large amount of cosmetics capable of uniformly delivering each active ingredient to the skin. It can be said to be a characteristic that influences important performance.

By completing the present invention as described above, a pre-dispersion step of dispersing titanium dioxide, silk powder, chromium oxide green or iron oxide, methyl methacrylate crosspolymer, cyclomethicone at 1500 rpm for 15 minutes using a disper at room temperature, A method for producing a cosmetic pigment composed of a secondary dispersion process of dispersing 50 minutes at 1000 rpm using a ring mill can be provided.

By the completion of the present invention, the final product obtained by minimizing the particle size of the silk powder-containing pigment composition is uniformly applied on the skin, the color is well expressed and the feeling is significantly improved. In addition, a method for preparing a pigment composition for cosmetics containing silk powder, which significantly improves the disadvantages of the existing products in moisture retention, safety, dispersibility, and physical properties of the product, that is, viscosity and color, can be provided.

Claims (2)

In the manufacturing method of the pigment composition for makeup cosmetics containing a silk powder, A pre-dispersion process of dispersing any one of chromium oxide green and iron oxide, titanium dioxide, silk powder, methylmethacrylate crosspolymer and cyclomethicone at 1500 rpm for 15 minutes at room temperature with a disper; Characterized in that consisting of a secondary dispersion process for dispersing the ring mill at 1000 rpm for 50 minutes, Manufacturing method. The method of claim 1, 0.01 to 5.0 wt% of chromium oxide green and iron oxide, 1.0 to 10.0 wt% of titanium dioxide, and 0.01 to 10.0 wt% of silk powder, and 0.1 to 2.0 wt% of methylmethacrylate crosspolymer based on the final pigment composition. %, Cyclomethicone is used in an amount such that the total of the total components is 100% by weight, Manufacturing method.