KR102211958B1 - Manufacturing method of powder composition dispersed by particulate process and a powder composition manufactured thereby - Google Patents

Abstract

The present invention provides a micronized, homogenized powder composition that can be included in a cosmetic composition, and by using this, a cosmetic composition with improved excellent adhesion, high coverage, long lasting, and soft feeling of use can be prepared. By using the powder composition of the present invention, it is possible to express smooth skin by effectively filling the unevenness of the skin such as wrinkles and pores, it is possible to evenly cover the skin without cloudiness, and excellent skin adhesion.

Description

Manufacturing method of powder composition dispersed by particulate process and a powder composition manufactured thereby}

The present invention relates to a method for preparing a powder composition contained in a cosmetic composition and a powder composition prepared through the method, and specifically, to a method for improving the micronization and homogenization effect of the powder composition particles, and a powder composition prepared therethrough will be.

The makeup cosmetic composition should be applied gently when applied to the skin, has excellent skin adhesion and covering effect, should not be shiny even after time, and should maintain excellent skin stability. These properties are greatly influenced by the powder contained in cosmetics.

In general, a widely known emulsified or oil-dispersible makeup cosmetic composition uses various types of powders, and has various input and dispersion processes. As one method, there is a method of mixing powder, pulverizing an atomizer, and then directly putting it into a cosmetic manufacturing facility to disperse it.This has a disadvantage that a lot of powder dust is generated during the manufacturing process and color control is difficult during manufacturing. There is a problem that the micronization and homogenization effect is not great. As another method, there is a method of mixing the powder with a solvent to make a powder composition using equipment such as a roll mill or a bead mill, and dispersing it by putting it into a cosmetic manufacturing facility, which is described above. Compared to the first method, there is an advantage that powder dust is not generated and color adjustment is possible during manufacturing. However, there is a risk in handling the manufacturing equipment when manufacturing the powder composition, and the quality of the powder composition is not uniform depending on the manufacturing conditions, so there is a disadvantage that when using cosmetics manufactured using the powder composition, agglomeration occurs.

Korean Patent Registration 10-1634595B Korean Patent Registration 10-0473262B

In order to solve the above problems, the present invention provides a powder composition included in a cosmetic that provides excellent skin adhesion and coverage, long lasting and soft feeling by increasing the fineness and homogenization effect of particles, and a method of manufacturing the same.

The present invention is a method for producing a cosmetic composition comprising an inorganic pigment powder, the step of mixing the solvent and the inorganic pigment powder (S1); Dispersing the mixture of the solvent and powder prepared through the step S1 with a high pressure disperser under a pressure of 600 to 1500 bar (S2); And mixing (S3) an oil phase component, an aqueous phase component, or a mixture of an oil phase component and an aqueous phase component in the dispersion prepared through the S2 step, wherein the solvent is aqueous, oily, or aqueous and oily mixture It provides a method of manufacturing a cosmetic composition, which is a solvent. In particular, the step of high-pressure dispersion with the high-pressure disperser (S2) is characterized in that it is repeated three or more times. In addition, the cosmetic composition of the present invention may be prepared by additionally mixing a dispersant in the step (S1) of mixing the powder and the solvent.

The present invention also provides a cosmetic composition prepared through the above method.

By applying a micronized and homogenized powder composition to a cosmetic composition, it is intended to provide cosmetics with improved excellent adhesion, high coverage, long lasting, and soft feeling of use. By using a micronized and homogenized powder composition, it is possible to express smooth skin by effectively filling in irregularities in the skin such as wrinkles and pores, and to cover the skin evenly without cloudiness. In addition, since the micronized powder has a large surface area, it has a high oil absorption ability, so it adheres to the skin faster and thinner.

1 is a photograph observed with a microscope after dispersing a powder composition including particulate titanium dioxide under a pressure of 600 bar using a high pressure disperser. (a) is dispersed once with a high pressure disperser, (b) is dispersed twice, and (c) is dispersed three times.
2 is a photograph observed with a microscope after dispersing a powder composition containing titanium dioxide fine particles by agitation Mix.
3 is a comparative graph of particle size analysis when a powder composition including particulate titanium dioxide is stirred and mixed, dispersed using a 3-stage Roll Mill, and dispersed by pressure (300, 600, 1500 bar) using a high pressure disperser.
4 is a photograph observed with a microscope after dispersing a powder composition containing titanium dioxide under a pressure of 600 bar using a high pressure disperser. (a) is dispersed once with a high pressure disperser, (b) is dispersed twice, and (c) is dispersed three times.
5 is a photograph observed with a microscope after dispersing a powder composition containing titanium dioxide by stirring and mixing.
6 is a comparative graph of particle size analysis when a powder composition containing titanium dioxide is stirred and mixed, dispersed using a three-stage roll mill, and dispersed by pressure (300, 600, 1500 bar) using a high-pressure disperser.
7 shows a result of a sensory test of a makeup cosmetic composition including a powder composition prepared by different dispersion processes.
8 is a result of measuring the average melanin level before and after application of the makeup cosmetic composition of the present invention and the comparative example composition.
9 is a photograph of the skin surface before and after application of the inventive makeup cosmetic composition and the comparative example composition.

The present invention relates to a method for preparing a powder composition applied to a cosmetic composition and a powder composition prepared therethrough, and provides excellent skin adhesion and coverage, long lasting and soft feeling by increasing the micronization and homogenization effect of the powder composition particles. It is characterized.

In this specification, a solvent is a liquid used to dissolve a substance, and may be an aqueous solvent, an oil solvent, or a mixed solvent of aqueous and oil, and a liquid that can be appropriately selected and used by a person skilled in the art. Means.

In the present specification, when preparing an oil-in-water cosmetic, the oily component means a component capable of preparing an oily composition by combining it with an oily agent. In addition, an aqueous phase component means a component capable of preparing an aqueous phase composition by combining it with an aqueous medium such as water when preparing an oil-in-water cosmetic.

The method for preparing a powder composition of the present invention comprises the steps of mixing a powder (Powder) and a solvent (Solvent) (S1); And after mixing in the step S1, dispersing using a high-pressure homogenizer (S2).

In the present invention, dispersion is a suspension in which a solid in the form of a powder is dispersed in a liquid, and a strong energy is applied to the material so that the particle size is refined and dispersed. Therefore, the step of dispersing using the high-pressure disperser (S2) aims to micronize and homogenize the particles by allowing the powder to pass through a system of high pressure.

The dispersion step using a high pressure disperser is characterized in that it proceeds under a pressure of 600 to 1500 bar. Below 600 bar, the powder refining effect is not large, and as the pressure increases, the refining effect increases, but when it exceeds 1500 bar, the difference is insignificant. The dispersing step using a high-pressure disperser is characterized in that it is dispersed three or more times. The micronization effect increases as the number of dispersion increases, but the difference is insignificant when the dispersion is dispersed more than three times.

In the present invention, the powder composition refers to a composition prepared by mixing a powder and a solvent and then dispersing it through a high-pressure disperser, and the solvent is for dispersing the powder and may be an oily or aqueous solution, or a mixed solvent thereof. . Further, in the powder composition of the present invention, a dispersant may be added to improve the stability of the composition by preventing the dispersed powder from agglomeration again.

In the powder composition, the powder is titanium dioxide, particulate titanium dioxide, zinc oxide, yellow iron oxide (CI 77492), red iron oxide (CI 77491), black iron oxide ( Black Iron Oxide, CI 77499), ultramarine (CI 77007), chromium oxide green (Chromium Oxide Green, CI 77288) may be one or more selected from the group consisting of inorganic pigment powders. Powder can be mixed and used by appropriately selecting the content and content according to the UV blocking effect, coverage, color development, etc., which are expressed when applied to the skin.

In addition, the powder is triethoxycaprylylsilane, lauroyl lysine, disodium stearoyl glutamate, isopropyl titanium triisostearate (Isopropyl Titanium Triisostearate). It may be coated with one or more coating materials selected from the group consisting of.

The solvents include Cyclopentasiloxane, Cyclohexasiloxane, Dimethicone 1CS-100CS, Phenyl Trimethicone, Diphenylsiloxy Phenyl Trimethicone), Caprylyl Methicone, Methyl Trimethicone, Isononyl Isononanoate, Isododecane, Isohexadecane, C12-15 Alkyl Benzoate (C12-15 Alkyl Benzoate), Caprylic/Capric Triglyceride, Octyldodecanol, Butylene Glycol, Glycerin, Purified Water Water) may be one or more selected from the group consisting of.

The dispersant is PEG-10 Dimethicone, Cetyl PEG/PPG-10/1 Dimethicone, Lauryl PEG-9 Polydimethicone Siloxyethyldimethicone (Lauryl PEG-9 Polydimethylsiloxyethyl Dimethicone), PEG-9 Polydimethylsiloxyethyl Dimethicone, Lauryl PEG-8 Dimethicone ), Lauryl PEG/PPG-18/18 Methicone, Sebum/PP-19/19 Dimethicone (PEG/PPG-19/19 Dimethicone), Bis -PEG/PPG-14/14 Dimethicone, PEG/PPG-18/18 Dimethicone (PEG/PPG-18/18 Dimethicone), PEG/ PPG-20/20 Dimethicone (PEG/PPG-20/20 Dimethicone), Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone, Polyglyceryl-4 isostearate ( Polyglyceryl-4 Isostearate) Sorbitan Isostearate, Sorbitan Sesquioleate, Polypropylsilsesquioxane, Acrylate/Ethylhexylacrylate/Dimethicone Methacrylate It may be one or more selected from the group consisting of copolymers (Acrylates/Ethylhexyl Acrylate/Dimethicone Methacrylate Copolymer).

The inorganic pigment powder composition of the present invention may be included in preparing an emulsion-type, water-dispersion or oil-dispersion cosmetic composition by mixing with an oily component and/or an aqueous phase component, and the cosmetic composition comprising the powder composition comprises powder and a solvent. Mixing step (S1); After mixing in the step S1, dispersing using a high-pressure disperser (S2); And mixing the powder and the solvent dispersed in step S2 with an oily component, an aqueous phase component, or a mixture of an oily phase and an aqueous phase component (S3).

The cosmetic composition, for example, when the cosmetic composition includes both an oily component and an aqueous phase component, may contain 10 to 40% by weight of a powder composition based on the total weight of the cosmetic composition, and the oily component is 10 to 40% by weight, It is preferable that the component contains 20 to 60% by weight.

The powder composition of the present invention may be included in a cosmetic composition for a specific use according to an appropriate selection of a person skilled in the art, and, for example, may be included in a cosmetic composition for makeup or skin care. In addition, the cosmetic composition may additionally include additional additives such as fragrances and preservatives, but is not limited thereto.

Hereinafter, the present invention will be described in more detail through test examples and examples. In particular, the effect of dispersion using a high-pressure disperser will be examined with reference to the drawing. However, since these examples are for illustrative purposes only, the scope of the present invention is not construed as being limited by these examples.

This is an enlarged photograph of a powder composition dispersed by agitation mix after mixing with cyclopentasiloxane and PEG-10 dimethicone.

Comparing FIGS. 1 and 2, it can be seen that the powder composition (FIG. 1) dispersed using a high-pressure disperser has much smaller powder particles and is homogenized and dispersed.

3 is a particle size comparison analysis graph comparing particle sizes of powder compositions dispersed in different processes after mixing a powder composition including particulate titanium dioxide in the same composition as described above. Particle size analysis was carried out by Malvern's analyzer. In FIG. 3, it was confirmed that the powder composition dispersed using a high-pressure disperser has a smaller average and standard deviation of the powder particle size compared to the agitation mixed powder composition and the powder composition dispersed using a 3-stage Roll Mill. I can. In particular, it can be seen that when the high pressure disperser is applied, the average particle size decreases as the pressure increases. Therefore, when the powder is dispersed using a high-pressure disperser, the particle size can be uniformly distributed, so it is possible to cover smoothly when applying a cosmetic composition including the same to the skin. , It is easy to maintain quality even in mass production. In addition, as the pressure increases during high-pressure dispersion, the average particle size decreases. In particular, since the average particle size is very small at 600 bar or more, adhesion can be remarkably improved.

Test example 2. According to the dispersion process Titanium dioxide Comparison of dispersion state of powder composition

Figure 4 is a microscopic enlarged photograph of a powder composition prepared by dispersing titanium dioxide, cyclopentasiloxane, and PEG-10 dimethicone under a pressure of 600 bar using a high-pressure disperser, and Figure 5 is an enlarged photograph of a powder composition prepared by dispersing titanium dioxide, cyclopentasiloxane, and PEG-10 dimethicone. It is a microscopic enlarged photograph of a powder composition prepared by mixing with Easy-10 Dimethicone and then dispersing by stirring and mixing.

Comparing FIG. 4 and FIG. 5, it can be seen that the powder composition (FIG. 4) dispersed using a high-pressure disperser has much smaller powder particles and is homogenized and dispersed.

6 is a particle size comparison analysis graph comparing particle sizes of powder compositions dispersed in different processes after mixing a composition containing titanium dioxide in the same composition as described above. Compared to the agitation mixed powder composition and the powder composition using a three-stage roll mill, the particles of the powder composition dispersed using a high pressure disperser can be confirmed to be distributed smaller, and the pressure will increase when the high pressure disperser is applied. It can be seen that the average and standard deviation of the particle size is smaller as the particle size increases.

Test example 3. Make-up containing powder compositions with different dispersion processes Cosmetic Preparation of the composition

(1) Preparation of Example 1

A makeup cosmetic composition was prepared by mixing a powder composition, an oily component, and an aqueous phase component as shown in Table 1 below.

Specifically, in the makeup cosmetic composition of Example 1, powder, solvent, and dispersant were mixed and dispersed three times using a high-pressure disperser at a pressure of 600 bar to prepare a powder composition, and then the oily components were mixed and dispersed with a homomixer. After mixing the water-phase components and dispersing it with a homomixer.

Based on the total weight of the makeup cosmetic composition, the powder composition was prepared by mixing 29.5% by weight, the oily component 35.5% by weight, and the water phase component 35% by weight. At this time, the powder composition contained 17.8% by weight of powder, 11% by weight of cyclopentasiloxane, and 0.7% by weight of PG-10 dimethicone based on the total weight of the makeup cosmetic composition. Specifically, the powder contained in the powder composition is a mixture of particulate titanium dioxide, titanium dioxide, yellow iron oxide, red iron oxide, and black iron oxide powder.

(2) Preparation of Example 2

Prepared by dispersing the powder composition of [Table 1] three times using a high-pressure disperser in the same manner as in Example 1, but applying a pressure of 1000 bar, mixing the oil phase component and dispersing it with a homomixer, and mixing the aqueous phase component It was prepared by dispersing in a homomixer.

(3) Preparation of Comparative Example 1

The powder, solvent, and dispersant of Table 1 are mixed and dispersed using a roll mill, and then the oil phase component is mixed and dispersed with a homomixer, and the aqueous phase component is mixed and dispersed with a homomixer.

(4) Preparation of Comparative Example 2

Unlike Examples 1 and 2 and Comparative Example 1, a makeup cosmetic composition of Comparative Example 2 was prepared by mixing the components of the following [Table 2] without a dispersion process.

Test Example 4. Evaluation of the makeup cosmetic composition prepared in Test Example 3

(1) sensory evaluation

About Example 1, Example 2, Comparative Example 1, and Comparative Example 2 prepared in Test Example 4, sensory evaluation (5-point scale method) was performed. Adhesion, thickness, coverage, durability, finish, and darkening were evaluated as very good 5 points, good 4 points, normal 3 points, bad 2 points, and very bad 1 points, and the evaluation results are shown in FIG. 7. In this evaluation, the sense of thickness refers to the sense of thickness of the formulation that is sensed when first applied to the skin, and when applied thinly and evenly, it is evaluated close to 5 points. Darkening refers to a phenomenon in which darkening is oxidized in the air or combined with sweat and oil on the skin when a certain time elapses after makeup, and is evaluated closer to 5 points as there is no darkening phenomenon.

As a result of the sensory evaluation, the makeup cosmetic composition including the powder composition using the high pressure disperser of Examples 1 and 2 in all items such as adhesion, thickness, coverage, lasting power, finish, and darkening was compared to the makeup of Comparative Examples 1 and 2. It received higher evaluation than the cosmetic composition.

(2) Comparison and evaluation of adhesion cover efficacy

The adhesion cover efficacy of Example 1 and Comparative Example 1 prepared in Test Example 3 was compared and evaluated through Average Melanin level.

For 5 adults with an average age of 25.6 years, after washing their face, they were allowed to rest for 30 minutes under the same conditions, and then evaluated. Each substance was applied to the test areas on both sides of the tester's face, including the border of both lower eyelids and the border of the nose, but for the same area area, Example 1 was 16 ul (80 %), Comparative Example 1 was applied with 20 ul.

For the test site, an Antera 3D (miravex, UK) camera was used to measure the average melanin level before application of each substance, and after applying each substance, the average melanin level was measured (FIG. 8(a)). Using the measured value, the average melanin level increase or decrease rate was calculated according to Equation 1 below (FIG. 8(b)).

(X: Average Melanin level of the measurement site before product use,

Y: Average Melanin level of the measurement area after using the product)

In addition, photographs were taken before and after applying the makeup cosmetic composition of Example 1 and Comparative Example 1 in the same manner as above (FIG. 9).

As can be seen from FIG. 8(b), the increase/decrease rate of the Average Melanin level of Example 1 is about -11.2%, and the increase/decrease rate of the Average Melanin level of Comparative Example 1 is about -10.8%. This means that the 16 ul applied Example 1 and the 20 ul applied Comparative Example 1 are closely covered to a similar degree or somewhat superior to reduce melanin production. In addition, as can be seen in FIG. 9, it can be seen that when all of the five testers apply Example 1, the covering power is more excellent in a photograph. In other words, it means that the makeup cosmetic composition of Example 1 of the present invention can exhibit excellent coverage even with a smaller application amount (80% compared to Comparative Example 1).

Claims (13)

As a method for producing a cosmetic composition comprising an inorganic pigment powder,
A step (S1) including a first step of mixing a solvent and an inorganic pigment powder and a second step of dispersing the mixed mixture under high pressure with a high pressure disperser under a pressure of 600 to 1500 bar (S1); And
Including the step (S2) of mixing the dispersion prepared through the step S1, an oil phase component, an aqueous phase component, or a mixture of an oil phase component and an aqueous phase component,
The solvent is an aqueous, oily, or aqueous and oily mixed solvent, a method for producing a cosmetic composition.
The method of claim 1,
The second process of high-pressure dispersing with the high-pressure disperser of step S1 is to repeat the high-pressure dispersing three or more times.

The method of claim 1,
The inorganic pigment powder is titanium dioxide, particulate titanium dioxide, zinc oxide, yellow iron oxide, red iron oxide, black iron oxide, ultramarine (Ultramarine), chromium oxide green (Chromium Oxide Green) is at least one selected from the group consisting of, a method for producing a cosmetic composition.
The method of claim 1,
The solvents include Cyclopentasiloxane, Cyclohexasiloxane, Dimethicone 1CS-100CS, Phenyl Trimethicone, Diphenylsiloxy Phenyl Trimethicone), Caprylyl Methicone, Methyl Trimethicone, Isononyl Isononanoate, Isododecane, Isohexadecane, C12-15 Alkyl Benzoate (C12-15 Alkyl Benzoate), Caprylic/Capric Triglyceride, Octyldodecanol, Butylene Glycol, Glycerin, Purified Water Water) is one or more selected from the group consisting of, a method for producing a cosmetic composition.
The method according to claim 1 or 2,
The first step of mixing the solvent and inorganic pigment powder of step S1 is to disperse at high pressure after additionally mixing the solvent and the inorganic pigment powder with a dispersant.

The method of claim 5,
The dispersant is PEG-10 Dimethicone, Cetyl PEG/PPG-10/1 Dimethicone, Lauryl PEG-9 Polydimethicone Siloxyethyldimethicone (Lauryl PEG-9 Polydimethylsiloxyethyl Dimethicone), PEG-9 Polydimethylsiloxyethyl Dimethicone, Lauryl PEG-8 Dimethicone ), Lauryl PEG/PPG-18/18 Methicone, Sebum/PP-19/19 Dimethicone (PEG/PPG-19/19 Dimethicone), Bis -PEG/PPG-14/14 Dimethicone, PEG/PPG-18/18 Dimethicone (PEG/PPG-18/18 Dimethicone), PEG/ PPG-20/20 Dimethicone (PEG/PPG-20/20 Dimethicone), Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone, Polyglyceryl-4 isostearate ( Polyglyceryl-4 Isostearate) Sorbitan Isostearate, Sorbitan Sesquioleate, Polypropylsilsesquioxane, Acrylate/Ethylhexylacrylate/Dimethicone Methacrylate Copolymer (Acrylates/Ethylhexyl Acrylate/Dimethicone Methacrylate Copolymer) is at least one selected from the group consisting of, a method for producing a cosmetic composition.
A mixture of a solvent and inorganic pigment powder; And as a cosmetic composition comprising an oily component, an aqueous component, or an oily component and an aqueous component,
The solvent is an aqueous, oily, or aqueous and oily mixed solvent,
The mixture of the solvent and inorganic pigment powder is dispersed under high pressure with a high pressure disperser under a pressure of 600 to 1500 bar, cosmetic composition.
The method of claim 7,
The mixture of the solvent and powder is dispersed with a high pressure disperser three or more times, the cosmetic composition.
The method of claim 7,
The powder is titanium dioxide, particulate titanium dioxide, zinc oxide, yellow iron oxide, red iron oxide, black iron oxide, ultramarine ), chromium oxide green (Chromium Oxide Green) is one or more selected from the group consisting of, a cosmetic composition.
The method of claim 7,
The solvents include Cyclopentasiloxane, Cyclohexasiloxane, Dimethicone 1CS-100CS, Phenyl Trimethicone, Diphenylsiloxy Phenyl Trimethicone), Caprylyl Methicone, Methyl Trimethicone, Isononyl Isononanoate, Isododecane, Isohexadecane, C12-15 Alkyl Benzoate (C12-15 Alkyl Benzoate), Caprylic/Capric Triglyceride, Octyldodecanol, Butylene Glycol, Glycerin, Purified Water Water) is one or more selected from the group consisting of, a cosmetic composition.
The method according to claim 7 or 8,
The mixture of the solvent and the powder is that the dispersant is additionally mixed, the cosmetic composition.
The method of claim 11,
The dispersant is PEG-10 Dimethicone, Cetyl PEG/PPG-10/1 Dimethicone, Lauryl PEG-9 Polydimethicone Siloxyethyldimethicone (Lauryl PEG-9 Polydimethylsiloxyethyl Dimethicone), PEG-9 Polydimethylsiloxyethyl Dimethicone, Lauryl PEG-8 Dimethicone ), Lauryl PEG/PPG-18/18 Methicone, Sebum/PP-19/19 Dimethicone (PEG/PPG-19/19 Dimethicone), Bis -PEG/PPG-14/14 Dimethicone, PEG/PPG-18/18 Dimethicone (PEG/PPG-18/18 Dimethicone), PEG/ PPG-20/20 Dimethicone (PEG/PPG-20/20 Dimethicone), Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone, Polyglyceryl-4 isostearate ( Polyglyceryl-4 Isostearate) Sorbitan Isostearate, Sorbitan Sesquioleate, Polypropylsilsesquioxane, Acrylate/Ethylhexylacrylate/Dimethicone Methacrylate Copolymer (Acrylates/Ethylhexyl Acrylate/Dimethicone Methacrylate Copolymer) is at least one selected from the group consisting of, a cosmetic composition.
The method of claim 7,
The cosmetic composition is an emulsified, oil-dispersible, or water-dispersible cosmetic composition.

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