WO2017057886A1 - Composite powder in which porous polymer is impregnated with scoria powder particles, cosmetic composition containing same, and process for producing same - Google Patents

Abstract

The present invention relates to a composite powder of scoria powder and a porous polymer. More particularly, the present invention relates to a composite powder (scoria sphere) in which the surface and the inside of a porous polymer are uniformly impregnated with scoria powder particles prepared by spraying in one-step a dispersion in which scoria powder is dispersed in a solution in which a polymer is dissolved; a cosmetic composition containing the same; and a process for producing the same. When the scoria impregnated powder, of the present invention, in which the porous polymer is uniformly impregnated with the scoria powder particles, is formulated as a cosmetic composition, the porous polymer supplements the sebum absorption performance of the scoria miniaturized in a micro size, and thus the sebum absorption power is greatly improved.

Description

Volatile powder powder particles impregnated with a porous polymer, a cosmetic composition containing the same, and a preparation method thereof

This application claims the benefit of priority based on Korean Patent Application No. 10-2015-0137327 of September 30, 2015 and Korean Patent Application No. 10-2016-0122454 of September 23, 2016. All content disclosed in the literature is included as part of this specification.

The present invention relates to a composite powder of volcanic pine powder and porous polymer, and more particularly, volcanic pine powder particles prepared by spraying a dispersion in which volcanic pine powder is dispersed in a solution in which a polymer is dissolved in a single step. The present invention relates to a composite powder (Scoria sphere) evenly impregnated on the surface and the inside of the porous polymer, a cosmetic composition containing the same, and a preparation method thereof.

Volcanic clusters (Scoria) are known as a kind of natural ceramics. When the volcano erupts, the first erupted lava solidifies, producing a lava mixed with gas first, and in the process a volcanic cluster of porous structures containing numerous fine holes is created.

It is found in Jeju Island in Korea, and it is called Song-Yi or Song-Yi-Suk in the dialect of Jeju. The physical properties of volcanic oysters are weakly alkaline, with a pH of 7.2 to 7.8, and are porous. They have a reddish brown color, yellow brown color, black color and gray color depending on the minerals they contain.

Meanwhile, 5α-Reductase, which is present in testosterone-reactive tissues such as sebaceous glands, hair follicles, prostate, and epididymis, reduces testosterone, one of the male hormones, to dihydrotestosteron (DHT). It is an enzyme involved in Testosterone is involved in skeletal muscle growth and spermatogenesis, and dihydrotestosterone is known to be involved in the tissues in acne, sebum and prostatic hyperplasia (Diane et al; J. Invest Dermatol. 775-778, 1995. Bruchovsky , N et al; JBC 243, 2112-2121, 1968). In addition, in the sebaceous glands of the skin, testosterone is converted into dihydrotestosterone by 5α-reductase, binds to a receptor protein in the cytoplasm, enters the nucleus, activates sebaceous gland cells, and promotes differentiation of sebum in sebaceous glands. (Diane et al; J. Invest Dermatol. 105; 209-214).

In this regard, Applicant has disclosed in Korean Patent Publication No. 1414196 of volcanic clusters that effectively inhibits the activity of 5α-reductase, thereby affecting sebum control, pore reduction, and skin trouble.

In addition, volcanic clusters contain a large amount of natural minerals, and their own far-infrared emissivity is high, so the physical properties are known to be excellent in antibacterial and deodorizing properties, and volcanic clusters contain a lot of natural minerals. Its use is increasing with various cosmetic ingredients such as antibacterial and antibacterial.

Volcanic ash is a kind of volcanic debris, which is a porous material with large particles, but is usually pulverized into small particles when used as a material for cosmetics. However, when crushed to a micro size for the cosmetic material, the porous structure is destroyed and sebum absorption performance is lost. In addition, due to the crystalline structure of the rough feeling of use can not be avoided, the volcanic powder is not required to be directly exposed to the skin, but a porous composite powder structure excellent in sebum absorption performance is required.

[Preceding technical literature]

Korean Patent Publication No. 1414196 "Cosmetic composition containing volcanic stone clusters"

In order to solve the above problem, it is possible to coat the surface of the volcanic ash powder with polymer materials, but it is not possible to solve the disadvantage of inferior dispersibility due to the aggregation of particles by sebum. In addition, the volcanic pine powder and the porous raw material can be used separately in the formulation, but there is a problem in that the volcanic pine powder having a coarse crystalline structure is directly exposed to the skin, thereby greatly decreasing the feeling of use. In addition, although there is an emulsion polymerization method as a technique for making a porous polymer, there is no precedent success case due to technical limitations in preparing the porous polymer and impregnating the inorganic powder, and even if it is possible to manufacture, the surface is not easy to remove the surfactant. It is difficult to control the physical properties.

In order to solve this problem, in the present invention, after dispersing the volcanic ash powder in a solution in which the polymer is dissolved, the dispersion is sprayed by one-step spray spraying or electro-spraying. Disclosed are a volcanic pine-impregnated powder (Scoria sphere) in which volcanic pine powder particles are evenly impregnated with a porous polymer, a cosmetic composition containing the same, and a method of preparing the same. The particles of the volcanic ash powder are 5 to 20 μm, and may be impregnated with 10 to 90% by weight, preferably 50 to 90% by weight, based on the total weight of the composite powder. The porous polymer is polymethyl methacrylate [PMMA: poly- (methyl methacrylate)], polyvinylpyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)], poly -L-lactic acid [PLLA: poly- (L-lactic acid)], polyethylene oxide [PEO: poly- (ethylene oxide)], polypropylene oxide [PPO: poly- (propylene oxide)], polydimethylsiloxane [PDMS: poly- (dimethyl siloxane)], polylactic glycolic acid [PLGA: poly- (lactic-co-glycolic acid)], polystyrene [PS: poly styrene] and one or more selected from the group thereof The specific volume is preferably 0.5-5 cm ³ / g.

When the volcanic pine powder impregnated with the volcanic pine powder particles of the present invention evenly impregnated with a cosmetic composition as a cosmetic composition, the sebum oil absorption performance of the volcanic pine micronized to micro size is complemented by the porous polymer to improve the sebum adsorption power. Greatly improved.

In addition, when the spray drying or electro-spraying process is introduced to prepare the volcanic scouring sphere of the present invention, spherical porosity in a single process can be avoided by using an emulsifier that is irritating to the skin. It can be impregnated evenly on the polymer surface and inside.

In addition, by impregnating the coarse crystalline powder of volcanic powder into the spherical porous polymer, the spreadability, spreadability and softness are improved, and the aggregation phenomenon is eliminated.

1 is a scanning electron microscope (SEM) image of the volcanic cluster powder applied to the present invention.

FIG. 2 is a scanning electron microscope (SEM) image of a volcanic scotch sphere (Scoria sphere) sphere of the present invention.

Figure 3 is a scanning electron microscope (SEM) image of the cut surface of the volcanic scotch impregnated powder (Scoria sphere) of the present invention.

FIG. 4 is an image obtained by quantitatively and qualitatively analyzing each element included in a Scoria sphere of the present invention with an energy dispersive X-ray (EDX) analyzer.

5 is an oil absorption (mL / g) test results of the volcanic scouring powder (Scoria sphere) of the present invention.

The present invention relates to a composite powder of a volcanic pine powder and a porous polymer, and more particularly, after the volcanic pine powder is dispersed in a solution in which the polymer is dissolved, spray drying or electro-spraying is performed. Compound powder (hereinafter referred to as volcanic pine-impregnated powder, Scoria sphere) in which volcanic powder powder particles are uniformly impregnated on the surface and inside of porous polymer by spraying the dispersion by one-step, cosmetic composition containing the same and preparation thereof It is about a method. In the present invention, the term 'impregnation' means a state in which other powder particles are uniformly dispersed and penetrated between the inside of the powder particles to be a mother, and in the past, the surface of the powder particles is coated with other powder particles or supported by the pores of the powder surface. It is different from. Hereinafter, the present invention will be described in detail.

Scoria powder

Volcanic pine used as an active ingredient in the present invention (Scoria) is a kind of volcanic ash that exists only in Jeju Island in Korea, and is known to be produced when generating parasitic volcanoes (rising) across Jeju, and the reserve in Jeju Island is about 20 billion m ³ It is estimated to be an almost infinite resource. Volcanic ash is a natural material capable of combating E. coli with 92-93% of far-infrared radiation, 97% deodorization rate and 99.9% antibacterial fungus in its natural state.

Volcanic ash of the present invention can be obtained by a conventional method in the art, the production method is not particularly limited. For example, volcanic clusters collected in areas not contaminated with pesticides may be obtained by pulverizing various particle sizes according to the use to remove impurities and dry heat sterilizing at a temperature of 150 ° C. or higher.

However, in the present invention, the particles of the volcanic ash powder usable as the cosmetic composition are preferably processed to have an average particle diameter of 0.1 to 2 μm. If the thickness exceeds 2 μm, the effect of the volcanic ash powder is insignificant. If the thickness is less than 0.1 μm, the surface of the spherical volcanic ash-impregnated powder (Scoria sphere) is roughened, and thus the feeling of use is reduced.

Porous polymer

In the present invention, the porous polymer impregnated with the volcanic ash powder particles is a spherical powder having oil absorption and sebum absorption.

As the porous polymer, polymethyl methacrylate [PMMA: poly (methyl methacrylate)] was used as an embodiment, but in addition, polyvinylpyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)], poly-L-lactic acid [PLLA: poly- (L-lactic acid)], polyethylene oxide [PEO: poly- (ethylene oxide)], polypropylene oxide [PPO: poly- (propylene oxide) )], Polydimethylsiloxane [PDMS: poly- (dimethyl siloxane)], polylactic glycolic acid [PLGA: poly- (lactic-co-glycolic acid)], polystyrene [PS: poly styrene] and copolymers thereof It may be selected from the group, but is not limited thereto.

Since the porous polymer is spherical in shape, it is easy to mix when manufacturing various cosmetic formulations, and the spherical fine particles are rolled on the skin, thereby providing excellent feeling of application such as spreadability when applying the skin and having characteristics of a spherical surface. Due to light scattering prevention effect and improvement of makeup persistence, it is commonly used in basic cosmetics for sebum control and makeup products for skin tone correction.

Volcanic Pine Impregnated Powder

The volcanic cluster impregnated powder (Scoria sphere) of the present invention, that is, the composite powder in which the volcanic cluster powder particles are impregnated evenly on the surface and the inside of the porous polymer is preferably an average particle diameter of 5 ~ 20 ㎛. This particle size is related to the oil absorption and the feeling of use, and if the particle size is less than 5 μm, there may be a problem that the stability of the cosmetics is agglomerated with each other. If the particle size exceeds 20 μm, the particle size is applied to the cosmetic composition and applied to the skin. You may feel unpleasant by the usability.

The content of volcanic cluster powder in the volcanic cluster impregnated powder may be impregnated with 10 to 90% by weight relative to the total volcanic cluster impregnated powder weight, but impregnated with 50 to 90% by weight, the effect of volcanic cluster powder and the effects of skin application. Most preferable in a feeling.

In addition, the volcanic cluster impregnated powder can control the pore characteristics according to the manufacturing process conditions. Controllable pore characteristics include average pore size, porosity and total pore area. Specifically, the average pore size may be 15 to 800 nm, more preferably 250 to 600 nm, and the porosity may be 40 to 85%, and more preferably 50 to 75%. In addition, the total pore area may be 1 to 100 m ² / g, more preferably 5 to 80 m ² / g.

Volcanic cluster-impregnated powders having such characteristics may cause an oil absorption increase effect due to their pore size and porosity. The oil absorption amount can be explained by the intrusion volume of mercury described later. The mercury infiltration volume of the volcanic pine-impregnated powder according to the present invention is measured in the range of 0.5-5 cm ³ / g, which can be regarded as oil absorption with high confidence level.

Conventional porous polymers have a relatively large specific surface area due to a single-size mesoporous structure, but have a low average pore size and porosity, whereas the volcanic pine-impregnated powder of the present invention is multi-porous. Porous channels are formed due to the porous, micro + meso + macro structure, which is more advantageous for oil absorption by capillary action.

The present invention provides a porous volcanic cluster impregnated powder in one-step by spray drying or electrospraying a polymer dispersion obtained by dispersing volcanic cluster powder in a polymer solution. It is possible to impregnate the powder evenly on and in the porous polymer surface. At this time, it is desirable to exclude the emulsifier in order to maximize the oil absorption capacity and to implement super water-repellent. The detailed steps of spray drying and electrospray are not particularly limited in the present invention and follow a known method. The composite powder thus prepared may be lyophilized to sufficiently remove the solvent to maintain the spherical particle shape.

However, it is preferable that the solvent of the polymer solution is a polymethyl methacrylate (PMMA) to use a mixed solvent of dichloromethane (DCM) and hexanol (Hexanol), the mixing ratio of dichloromethane (DCM) and hexanol (Hexanol) The weight ratio can be selected from 9: 1 to 7: 3. Since hexanol plays a role of forming pores of porous polymers, if the proportion of hexanol is less than 10% by weight of the total solvent, the pore size is too small. .

Cosmetic composition

The image cluster impregnated powder according to the present invention can be preferably applied to a cosmetic composition. At this time, the cosmetic composition preferably contains 2 to 80% by weight of the volcanic ash-impregnated powder based on the total weight of the composition. If less than 2% by weight indicates a problem that the oil absorption is lowered, if it exceeds 80% by weight will have a problem that affects the stability of the formulation is poor stability.

In addition, the cosmetic composition containing volcanic pine-impregnated powder according to the present invention is a fatty substance, an organic solvent, a dissolving agent, a thickening agent, a gelling agent, a softening agent, an antioxidant, a suspending agent, a stabilizing agent, a foaming agent, a fragrance, an interface. Common to active agents, water, ionic or nonionic emulsifiers, fillers, metal ion sequestrants, chelating agents, preservatives, vitamins, blockers, wetting agents, essential oils, dyes, pigments, hydrophilic or lipophilic active agents, lipid vesicles or cosmetics It may contain adjuvants conventionally used in the cosmetic or dermatological field, such as any other ingredients used as. Such adjuvants are introduced in amounts generally used in the cosmetic or dermatological arts.

The cosmetic composition containing volcanic pine-impregnated powder according to the present invention may be formulated containing a cosmetically or dermatologically acceptable medium or base. These are all formulations suitable for topical application, for example emulsions, suspensions, microemulsions, microcapsules, microgranules or ionic (liposomes) obtained by dispersing an oil phase in solutions, gels, solids, pasty anhydrous products, aqueous phases and It may be provided in the form of a nonionic vesicle dispersant or in the form of a cream, skin, lotion, powder, ointment, spray, pack, or cone stick. It can also be used in the form of a foam or in the form of an aerosol composition further containing a compressed propellant. These compositions can be prepared according to conventional methods in the art.

For example, the cosmetic composition may be any one of skin, lotion, cream, serum, emulsion, essence, powder, foundation, spray, more preferably a mask pack, a sheet pack, a sleep pack, a wash off pack, a peel off pack, or the like. It can be formulated as, but is not particularly limited in the formulation, it can be selected and changed appropriately as desired.

Hereinafter, the present invention will be described in more detail with reference to examples and drawings. However, the present invention is not limited by the following examples, and it can be apparent to those skilled in the art that various changes or modifications can be made within the technical idea of the present invention.

In order to prepare the volcanic pine-impregnated powder of the present invention, the composition of the following <Table 1> is prepared.

Volcanic Cluster Powder	Bio Land Manufacturing, Jeju Volcanic Stone Cluster
Poly (methyl methacrylate) (PMMA)	LG PMMA Manufacturer
Dichloromethane anhydrous (DCM)	Manufactured by Sigma-Aldrich, Purity> 99.8%
Hexanol (1-hexanol)	Manufactured by Sigma-Aldrich, Purity> 99%

< Example  1> Spray-Drying

1) 40 g of PMMA is dissolved in 1 L of a solvent (DCM: Hexanol = 9: 1, wt%).

2) 40g volcanic cluster powder is added to PMMA solution and dispersed using homogenizer.

3) The PMMA solution in which the volcanic ash powder is dispersed is spray-dried under the conditions of the following <Table 2>.

Internal humidity	30% or more
Internal temperature	Keep at room temperature
Internal pressure	20atm
Feed rate	20%
Aspirator	70%

4) The PMMA solution in which the volcanic ash powder is dispersed is continuously stirred through the stirrer during spray drying.

5) The spray dried volcanic ash powder / PMMA composite powder particles are sufficiently washed and then lyophilized to completely remove the remaining solvent.

< Example  2> electrospray ( Electro  Spraying)

1) 0.4 g of PMMA is dissolved in 10 mL of a solvent (DCM: Hexanol = 9: 1, wt%).

2) 0.4 g of volcanic ash powder is added to PMMA solution and dispersed using an ultrasonic grinder.

3) The PMMA solution in which the volcanic ash powder is dispersed is electrosprayed under the conditions of the following <Table 3>.

Internal humidity	30% or more
Internal temperature	Keep at room temperature
Distance	15 cm
Feed rate	0.01 mL / min
Voltage	10 kV

4) After sufficiently washing the electrosprayed volcanic ash powder / PMMA composite powder particles, they are lyophilized to completely remove the remaining solvent.

The volcanic cluster-impregnated powders to be described below were experimented with those prepared according to the spray drying method of Example 1.

< Experimental Example  1> Scanning electron microscope SEM ) image

FIG. 1 is a scanning electron microscope (SEM) image of volcanic cluster powder, and FIG. 2 is a spherical shape of volcanic cluster impregnated powder impregnated evenly on the surface and inside of a polymethyl methacrylate (PMMA) particle of the volcanic cluster powder. Sphere) and scanning electron microscope (SEM) images of the cut plane. As shown in FIG. 1, polymethyl methacrylate (PMMA) particles as shown in FIGS. 2 and 3 by spray-drying or electrospraying a volcanic pine powder, which is an amorphous coarse structure having no porosity, is introduced by spray drying or electrospray. It is possible to impregnate the surface and inside evenly.

< Experimental Example  2> energy dispersive X-ray ( EDX : Energy Dispersive  X-ray Analysis

FIG. 4 is an image obtained by quantitatively and qualitatively analyzing each element included in the volcanic ash-impregnated powder of the present invention with an energy dispersive X-ray (EDX) analyzer. The distribution of the main components of silicon (Si), iron (Fe), aluminum (Al) element can be confirmed, and thus the volcanic cluster powder was uniformly impregnated throughout the polymethyl methacrylate (PMMA).

< Experimental Example  3> Oil absorption  Test

After weighing 1 g of volcanic pine-impregnated powder using a scale and petri dish, drop the triglyceride oil, which has properties similar to sebum of the human body, using dropper to measure the oil absorption required until the volcanic pine-impregnated powder is wet. Measured. At this time, use a spatula (Spatula) to mix the oil so that the wet well.

As shown in Figure 5, the oil absorption of the volcanic matsutake impregnated powder is 1.6mL / g, it can be seen that the oil absorption increased more than five times compared to 0.3mL / g of the oil absorption of the volcanic ash raw material powder. This is an effect generated by maintaining a large pore size and a high porosity, even though the volcanic pine-impregnated powder of the present invention contains 50% by weight of volcanic pine powder.

Claims (14)

1. A composite powder in which volcanic powder powder particles are impregnated into a porous polymer.
2. The method of claim 1,

   The composite powder, characterized in that the average particle diameter of the volcanic cluster powder is 0.1 ~ 2 ㎛.
3. The method of claim 1,

   The volcanic ash powder is composite powder, characterized in that impregnated with 50 to 90% by weight relative to the total weight of the composite powder.
4. The method of claim 1,

   The porous polymer may be polymethylmethacrylate, polyvinylpyrrolidone, polycaprolactone, poly-L-lactic acid, polyethylene oxide, polypropylene oxide, polydimethylsiloxane, polylactic glycolic acid, polystyrene, and air thereof Composite powder, characterized in that at least one selected from the group of coalescence.
5. The method of claim 1,

   The composite powder, characterized in that the average particle diameter of the sphere is 5 ~ 20 ㎛.
6. The method of claim 1,

   Porosity of the composite powder is a composite powder, characterized in that 40 to 85%.
7. The method of claim 1,

   The composite powder, characterized in that the average pore size of the composite powder is 15 ~ 800nm.
8. A method for producing a composite powder in which a volcanic pine powder particle is impregnated into a porous polymer, characterized by spray drying a dispersion obtained by dispersing a volcanic pine powder in a polymer solution.
9. The method of claim 8,

   The solvent of the polymer solution is a method for producing a composite powder, characterized in that a mixed solvent of dichloromethane and hexanol.
10. The method of claim 9,

    Method for producing a composite powder, characterized in that the weight ratio of the dichloromethane and hexanol is 9: 1 to 7: 3.
11. A method for producing a composite powder in which volcanic pine powder particles are impregnated into a porous polymer, characterized in that the dispersion is dispersed by dispersing the volcanic pine powder in a polymer solution.
12. The method of claim 11,

    The solvent of the polymer solution is a method for producing a composite powder, characterized in that a mixed solvent of dichloromethane and hexanol.
13. The method of claim 12,

    Method for producing a composite powder, characterized in that the weight ratio of the dichloromethane and hexanol is 9: 1 to 7: 3.
14. Cosmetic composition containing the composite powder of any one of Claims 1-7.

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