KR101281527B1 - Silicone gel composition and method for preparing globular particle therefrom - Google Patents

Abstract

The present invention is dimethicone / vinyl dimethicone crosspolymer silica powder 10 to 40% by weight, cyclomethicone 10 to 50% by weight, dipropylene glycol 5 to 20% by weight, glycerin 5 to 20% by weight, butylene glycol 5 to 30 A silicone gel composition comprising 10% by weight and 10-20% by weight of water and a method for producing silicon-containing spherical particles therefrom.

Description

Silicone gel composition and method for producing spherical particles therefrom {SILICONE GEL COMPOSITION AND METHOD FOR PREPARING GLOBULAR PARTICLE THEREFROM}

The present invention is dimethicone / vinyl dimethicone crosspolymer silica powder 10 to 40% by weight, cyclomethicone 10 to 50% by weight, dipropylene glycol 5 to 20% by weight, glycerin 5 to 20% by weight, butylene glycol 5 to 30 A silicone gel composition comprising 10% by weight and 10-20% by weight of water and a method for producing silicon-containing spherical particles therefrom.

Recently, consumers have demanded for efficacy along with aesthetic functions in cosmetics. Cosmetic developers are working to create effective products that are multifunctional and easy to use. For example, creams, lotions and color cosmetics should be easy to spread and comfortable to use without the unpleasant feeling or greasy.

Silicone is a popular material in skin care products. This versatile material has the ability to provide a variety of properties and unique aesthetics, for example wetting, diffusion and emolliency properties are known. As technology continues to evolve, silicon offers increasingly versatile and high performance characteristics. Silicone elastomers are the latest performance-enhanced silicone materials. The unique skin feel of silicone elastomers is a dry, soft and silky powder. The most important characteristic of silicone elastomers in skin care applications is their ability to absorb various oils and sebum. Developed as the first silicone elastomer for personal care applications is an elastomer powder made by freeze grinding of the cured silicone elastomer. Since then, various silicone elastomers have been developed. Product offerings of silicone elastomers include anhydrous gels and powders in their pure form, and may also be provided through an aqueous suspension.

One of the most recent of these silicone elastomers is dimethicone / vinyl dimethicone crosspolymer silica. Dimethicone / vinyl dimethicone crosspolymer silica is a spherical silicone elastomer coated with silica and has a diameter of about 1-10 μm. In addition to the function of absorbing sebum, it can provide the advantage of masking wrinkles of the face, and its spherical structure can impart free-flowing properties without aggregation. Dimethicone / Vinyl Dimethicone Crosspolymer Silica is an elastic powder that can give skin smoothness when applied to cosmetics, improve the spreadability of products, and absorb oil compared to conventional cosmetic oil absorbent materials. Is very good. In order to apply such dimethicone / vinyl dimethicone crosspolymer silica in a powder state practically to a cosmetic emulsion, it is necessary to convert the powder form into a translucent gel phase so that it can be easily used in cosmetic compositions of various formulations. There is a strong demand for the development of gel compositions containing applicable dimethicone / vinyl dimethicone crosspolymer silica.

Accordingly, the present invention is to provide a silicone gel composition that can be easily applied to various cosmetic formulations.

Another object of the present invention is to provide a method for producing silicon-containing spherical particles from a silicone gel composition.

In order to achieve the above object, the present invention is dimethicone / vinyl dimethicone crosspolymer silica powder 10 to 40% by weight, cyclomethicone 10 to 50% by weight, dipropylene glycol 5 to 20% by weight, glycerin 5 to 20% by weight To provide a silicone gel composition comprising 5 to 30% by weight of butylene glycol and 10 to 20% by weight of water.

In addition, in order to achieve the above another object, adding a silicone gel composition according to the invention 10 parts by weight to 40 parts by weight of water and then emulsified; Adding 0.01 to 5 parts by weight of a polymer encapsulating agent to the emulsion obtained in the above step and then mixing the emulsion; And it provides a method for producing a silicon-containing spherical particles comprising the step of dropping the mixture obtained in the above step into the aqueous polyvalent cation salt.

Hereinafter, the present invention will be described in detail.

According to one aspect of the invention dimethicone / vinyl dimethicone crosspolymer silica powder 10 to 40% by weight, cyclomethicone 10 to 50% by weight, dipropylene glycol 5 to 20% by weight, glycerin 5 to 20% by weight, butylene A silicone gel composition is provided comprising 5 to 30 weight percent glycol and 10 to 20 weight percent water.

The silicone gel composition of the present invention comprises 10 to 40% by weight of dimethicone / vinyl dimethicone crosspolymer (and) silica powder. Dimethicone / vinyl dimethicone crosspolymer silica, marketed by Dow Corning under the trade name 9701 Cosmetic Powder, is a spherical silicone elastomer coated with silica (SiO ₂ ). Dimethicone / vinyl dimethicone crosspolymer silica powders are excellent in their ability to absorb oil and sebum, as well as provide free-flowing properties without flocculation due to their spherical morphology. Dimethicone / vinyl dimethicone crosspolymer silica can be applied to various cosmetics such as foundation, makeup base and body cream. In the silicone gel composition of the present invention, when dimethicone / vinyl dimethicone crosspolymer silica is included in less than 10% by weight, there may be a problem that the gel is not formed but is formed only as a flowable liquid. It may not form and the powder itself may not aggregate.

The silicone gel composition of the present invention contains 10 to 50% by weight of cyclomethicone. Cyclomethicone helps to liquefy the powder with silicone fluid. In the silicone gel composition of the present invention, when cyclomethicone is included in less than 10% by weight, the powder may not be well dispersed, and when included in more than 50% by weight, the powder may be completely changed into a liquid phase.

The silicone gel composition of the present invention contains 5 to 20% by weight of dipropylene glycol. Dipropylene glycol in the silicone gel composition of the present invention facilitates the dispersion of the cyclomethicone oil phase powder in the water phase. In the silicone gel composition of the present invention, when dipropylene glycol is included in less than 5% by weight may not be properly dispersed in the water phase, when contained in more than 20% by weight may have a problem that the powder is liquefied.

The silicone gel composition of the present invention contains 5 to 20% by weight of glycerin. Glycerin in the silicone gel composition of the present invention serves to adjust the viscosity. In the silicone gel composition of the present invention, when glycerin is contained in less than 5% by weight, it may be a liquid without viscosity, and when included in excess of 20% by weight, there may be a problem in that the viscosity is too high.

The silicone gel composition of the present invention contains 5 to 30% by weight of butylene glycol. Butylene glycol in the silicone gel composition of the present invention aids in the dispersion of the powder. If butylene glycol is included in less than 5% by weight in the silicone gel composition of the present invention may not properly disperse the powder, if contained in more than 30% by weight may have a problem that the powder is liquefied.

The silicone gel composition of the present invention contains 10 to 20% by weight of water. In the silicone gel composition of the present invention, when the water is included in less than 10% by weight, the transparency of the silicone gel is lowered, the gel may be clouded, and when included in more than 20% by weight, the silicone gel may not be formed.

The silicone gel composition of the present invention is a semi-transparent gel, and because it is a silicone-in-water type, the feeling of use is lighter than that of a conventional silicone type of water-in-silicone, and the conventional type remains oily. It feels more moisturized than that, and is immediately removed by water at the time of cleansing. In addition, the silicone gel composition of the present invention is easy to disperse in water by using a variety of polyols, can compensate for the lack of moisture when using only silicon powder, it is possible to make a gel having a variety of viscosities.

According to another aspect of the invention, adding 10 to 40 parts by weight of water to 100 parts by weight of the silicone gel composition according to the present invention and then emulsified;

Adding 0.01 to 5 parts by weight of a polymer encapsulating agent to the emulsion and then mixing the emulsion; And

Provided is a method for producing a silicon-containing spherical particle comprising the dropwise addition of the mixture to an aqueous polyvalent cation salt.

If 10 to 40 parts by weight of water is added to 100 parts by weight of the silicone gel composition according to the present invention, and then less than 10 parts by weight of water is added in the emulsifying step, there may be a problem that the transparency becomes worse, and the amount is added in excess of 40 parts by weight. The emulsion may not form properly. Emulsification can be carried out using conventional methods known in the art, for example using a high pressure microfluidizer.

When the polymer encapsulating agent is added to less than 0.01 part by weight in the step of adding the polymer encapsulating agent to the formed emulsion and then mixing, the capsule is not formed or the hardness of the capsule is weak and can be easily broken, more than 5 parts by weight added The hardness of the capsule may be too high. The polymer encapsulating agent may preferably be used alginate, agar, cellulose-based compound, gelatin, gum arabic, polyvinylacetate (PVA), chitosan, carrageenan or guar gum. Alginate salts are most preferably sodium alginate. As the cellulose-based compound, for example, methyl cellulose, ethyl cellulose or hydroxypropyl cellulose may be used.

In the step of dropwise addition of the mixture to the aqueous solution of polyvalent cation salt, the polyvalent cation salt may preferably be calcium chloride (CaCl ₂ ), barium chloride (BaCl ₂ ) or aluminum chloride (AlCl ₃ ). The concentration of the polyvalent cation salt aqueous solution is preferably 0.01 to 1 mol. The dropwise addition of the mixture of the emulsion and the polymer encapsulating agent to the aqueous polyvalent cation salt solution may be performed, for example, by dropping the mixture into a polyvalent cation salt aqueous solution after loading the mixture in a syringe. In order to control the size of the spherical particles (beads) or to produce the spherical particles in a more uniform size, an encapsulation unit may be used. For example, an encapsulation system commercially available from Nisco Engineering AG, Switzerland may be used. Can be used. The size of the spherical particles in the present invention can be variously adjusted according to its needs, but is preferably about 100 to 3,000 ㎛.

The silicone gel composition or silicone-containing spherical particles according to the present invention can be applied to cosmetic compositions of various formulations such as lotions, creams, essences, and the like, and can also be used in personal care such as skin care compositions, body care compositions, hair care compositions, etc. personal care) compositions. Silicon-containing spherical particles may not only provide visual aesthetics due to their unique appearance, but may also serve as encapsulation to aid in the stability or transdermal delivery of other active ingredients.

The silicone gel composition according to the present invention can be easily applied to cosmetic compositions and personal care compositions of various formulations in a silicone-in-water type, and the silicone-containing spherical particles prepared therefrom are unique as well as the efficacy of silicone. In addition to providing visual aesthetics by appearance, it also plays an encapsulation role.

1 is a photograph of a cream prepared using the silicone gel composition and the silicon-containing spherical particles of the present invention.
2 is a photograph taken of the spherical particles of Example 10 using an optical microscope.

Hereinafter, the present invention will be described in detail with reference to examples. However, the examples are given for the purpose of helping understanding of the present invention, and thus the scope of the present invention is not limited thereto.

Example  1: Preparation of Silicone Gel Composition

The A component of Table 1 was introduced into the vessel and then mixed at room temperature for 5 minutes using a Henschel mixer. The B components were then introduced and mixed for 5 minutes using a Henschel mixer to prepare a translucent silicone gel composition.

Example  2: Preparation of Silicon-Containing Spherical Particles

A component of Table 2 was introduced into the container, and then mixed at room temperature for 5 minutes using a Henschel mixer. The B components were then introduced and mixed for 5 minutes using a Henschel mixer to prepare a translucent silicone gel composition. Water (C) was added to the obtained silicone gel composition, followed by three consecutive passes at 1,000 bar in a high pressure homogenizer, followed by sodium alginate (D). Spherical particles (beads) were prepared by dropwise addition to a beaker containing 0.1 M calcium chloride (CaCl ₂ ) solution.

Example  3 and Comparative example : Preparation of Lotion and General Lotion comprising Silicone Gel Composition

A lotion and a general lotion including a silicone gel composition were prepared in the following composition of Table 3.

Example  4: comprising the silicone gel composition Body lotion  Produce

To prepare a body lotion using a silicone gel composition in the composition of Table 4.

Example  5: Preparation of a Cream Including a Silicone Gel Composition

To prepare a cream using a silicone gel composition in the composition of Table 5.

Example  6: Preparation of Essences Containing Silicone Gel Composition

Essence was prepared using the silicone gel composition in the composition of Table 6 below.

Example  7: Preparation of cream using silicone gel composition and silicone containing spherical particles

Essences were prepared using GPC liposomes in the composition of Table 7 below. The prepared essence was photographed and shown in FIG. 1.

Example  8: Preparation of Essences Containing Silicon-Containing Spherical Particles

Essence was prepared using the silicon-containing spherical particles in the composition of Table 8.

Example  9: comprising silicone gel composition BB ( Blemish Balm ) Preparation of Cream

A component of Table 9 was prepared by treating three times with a three-stage roller dispersion mixing apparatus, and then, B components were added to the manufacturing unit, heated to 70-80 ° C., and then the A components treated with the three-stage roller dispersion mixing apparatus were added. And dispersed. The C components were prepared by dissolving them in a separate container, and heated to 80-85 ° C. while stirring with a homo mixer to emulsify for 10 minutes. After emulsification, the mixture was stirred using a stirrer, cooled to 25 ° C., then floated to prepare.

Example  10: comprising a silicone gel composition BB ( Blemish Balm ) Preparation of Spherical Particles Using Cream

A component of Table 2 was introduced into the container, and then mixed at room temperature for 5 minutes using a Henschel mixer. The B components were then introduced and mixed for 5 minutes using a Henschel mixer to prepare a translucent silicone gel composition. Water (C) was added to the obtained silicone gel composition, followed by three consecutive passes at 1,000 bar in a high pressure homogenizer, followed by sodium alginate (D) and BB cream (E) prepared in Example 9. Spherical particles (beads) were prepared by dropwise addition to a beaker with 0.1 M calcium chloride (CaCl ₂ ) solution using Cut System (VCS). The prepared spherical particles were photographed with an optical microscope (Olympus BX50) and are shown in FIG. 2.

Experimental Example  1: of silicone gel composition Feeling  Sensory evaluation

The lotion containing the silicone gel composition of Example 3 and the general lotion of the comparative example were tested for 20 female panels 20 to 60 years old. When good was 10 points, bad was calculated as 0 points. The results are shown in Table 11 below.

As can be seen in Table 11, the lotion containing the silicone gel composition was found to be superior in all evaluation items, such as absorption into the skin, spreadability or soft feeling compared to the general lotion.

Experimental Example  2: determination of changes in retinol content

In preparing the essence of Example 8, 0.02% of retinol added to spherical particles and 0.02% of retinol added to a general emulsion were stored at 25 ° C., shading conditions and 40 ° C., light exposure conditions. , Retinol content was quantitatively analyzed for about one month by HPLC method under the following conditions. The result is shown in Table 12, the numerical value outside parentheses is 25 degreeC and light-shielding conditions, and the numerical value in parentheses is 40 degreeC and light exposure conditions.

Column: C18 (3.9 × 150 mm, 5 μm)

Mobile phase: methanol: water = 90: 10

Flow rate: 1.0 ml / min

Detector: UV 325 nm

As can be seen from Table 12, the essence containing the silicon-containing spherical particles of the present invention was found to have excellent stability compared to the general essence.

Experimental Example  3: Percutaneous  Absorption Promotion Effect Experiment

Female hairless guinea pigs (strain IAF / HA-hrBR) of about 8 weeks were used. The abdominal skin of the guinea pig was excised and mounted on a Franz-type diffusion cell (Lab fine instruments, Korea). 50 mM phosphate buffer (pH 7.4, 0.1 M NaCl) was added to the Receptor vessel (5 ml) of the Franz-type diffusion cell, and then the diffusion cell was mixed and dispersed at 32 ° C. and 600 rpm. The spherical particles were included. 50 μl of the essence and the transparent emulsion in the form of a general emulsion were placed in a donor container. Absorption and diffusion were carried out according to the scheduled time, and the skin where absorption and diffusion occurred was 0.64 cm ² . After the diffusion of the active ingredient is completed, the emulsion remaining on the skin is not washed away with dried kimwipes or 10 ml of ethanol, and the active ingredient is absorbed using a tip-type homogenizer. After the diffused skin was changed, retinol absorbed into the skin was extracted using 4 ml of dichloromethane. The extract was then filtered through a 0.45 μm nylon membrane filtration membrane, and the content was measured by HPLC under the following conditions.

Column: C18 (3.9 × 150 mm, 5 μm)

Mobile phase: methanol: water = 90: 10

Flow rate: 1.0 ml / min

Detector: UV 325 nm

As can be seen in Table 13, it was confirmed that the silicon-containing spherical particles of the present invention plays an important role in the encapsulation as well as the visual effect, and excellent in the percutaneous absorption effect.

Claims (8)

Dimethicone / vinyl dimethicone crosspolymer silica powder 10-40 wt%, cyclomethicone 10-50 wt%, dipropylene glycol 5-20 wt%, glycerin 5-20 wt%, butylene glycol 5-30 wt% and Silicone gel composition comprising 10 to 20% by weight of water. Adding 10 to 40 parts by weight of water to 100 parts by weight of the silicone gel composition of claim 1, followed by emulsification;
To the emulsion obtained in the above step, 0.01 to 5 parts by weight of a polymer encapsulating agent selected from the group consisting of alginic acid salt, agar, cellulose-based compound, gelatin, gum arabic, polyvinylacetate (PVA), chitosan, carrageenan and guar gum was added. Then mixing; And
Method for producing a silicon-containing spherical particles comprising the step of dropping the mixture obtained in the above step into an aqueous polyvalent cation salt. delete The method of claim 2 wherein the alginic acid salt is sodium alginate. The method of claim 2, wherein the cellulose-based compound is methyl cellulose, ethyl cellulose or hydroxypropyl methyl cellulose. The method of claim 2, wherein the polyvalent cation salt is calcium chloride (CaCl ₂ ), barium chloride (BaCl ₂ ) or aluminum chloride (AlCl ₃ ). A silicon-containing spherical particle produced by the method of claim 2. A cosmetic composition comprising the silicone gel of claim 1 or the silicon-containing spherical particles of claim 7.

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