WO2017057918A1 - Ultravoilet radiation screening cosmetic composition and preparation method therefor - Google Patents

Abstract

The present invention relates to: an ultraviolet radiation screening cosmetic composition in which a ring-mill base comprising inorganic powder particles is ring-mill-dispersed, wherein the average particle size of the inorganic powder particles is 5-2,000 nm; and a preparation method therefor.

Description

Cosmetic composition for UV protection and its manufacturing method

The present invention relates to a cosmetic composition for sunscreen and a method of manufacturing the same.

This application claims the benefit of the filing date of Korean Patent Application No. 10-2015-0137946 filed with the Korean Intellectual Property Office on September 30, 2015, the entire contents of which are incorporated herein.

Inorganic sunscreen cosmetics are widely used in the market using inorganic powder particles, which have no controversy to the human body, unlike organic sunscreen cosmetics.However, when the size of inorganic powder particles is large, a so-called white clouding phenomenon occurs in which the skin becomes white. There is a problem.

In addition, the inorganic powder particles of the inorganic sunscreen cosmetic is preferably a small particle size in order to reduce the clouding phenomenon, but if the inorganic powder particles are small in size due to the characteristics of the inorganic powder particles, it is easy to aggregate in the formulation. Inorganic powder particles have a problem that whitening occurs when applied to the skin, but the UV protection ability is poor.

Therefore, the development of inorganic anti-vibration cosmetics that can reduce the clouding phenomenon and improve the ability to block UV rays is required, but the conventional method for mixing powders or apparatuses used for dispersing powder in the manufacture of cosmetics nanometer level size Since it is difficult to disperse the particles, it is difficult to secure high dispersibility, and even if the dispersibility is increased, it is difficult to maintain a stable formulation for a long time while maintaining high dispersibility.

The present invention is to provide a method for dispersing a cosmetic composition capable of improving the dispersibility of the fine inorganic powder particles, suppressing cloudiness during application of the skin, and improving the UV blocking ability, and a cosmetic composition prepared by such a dispersion method.

The present invention provides a cosmetic composition for blocking UV rays by ring-milling a ring mill base including inorganic powder particles, wherein the average particle size of the inorganic powder particles is 5 nm to 2000 nm.

In addition, the present invention is a ring mill mixing step of mixing the inorganic powder particles, and ring beads 5 nm to 2000 nm; And a ring mill dispersion step of stirring the ring mill base.

The present invention can provide a cosmetic composition exhibiting excellent ultraviolet blocking ability while ring-dispersing the ring mill base including the inorganic powder particles, thereby improving the dispersibility of the fine inorganic powder particles and suppressing the clouding phenomenon when applying the skin.

1 is a photograph of the dispersion state after the preparation of Comparative Example 1 prepared in Reference Example 3.

FIG. 2 is a photograph of a dispersion state of Example 4 prepared in Reference Example 3. FIG.

The cosmetic composition for sunscreen according to the present invention and a manufacturing method thereof will be described in detail.

Names of compounds mentioned in this specification, unless stated otherwise, are listed in the International Cosmetic Ingredient Dictionary (ICID) published by the Cosmetic, Toiletry and Fragrance Association (CTFA), INCI (International Nomenclature Cosmetic). Ingredient) means a compound corresponding to the name, and if the name does not exist among INCI Names, it means a compound according to the IUPAC nomenclature established by the International Union of Pure and Applied Chemistry (IUPAC). In the absence of a compound according to the IUPAC nomenclature, a compound corresponding to the name of a compound commonly used in the art.

The cosmetic composition for sunscreen according to the present invention is prepared by ring mill dispersion of a ring mill base, and the ring mill base will be described in detail as follows.

The ring mill dispersion will be described in detail as follows.

Ring mill mixing step of mixing the inorganic powder particles and ring beads (S10)

In one embodiment of the present invention, the average diameter of the ring beads is 0.1 mm to 3.0 mm. If the average straightness of the ring bead is less than 0.1 mm, dispersion may not be performed well, and if it is more than 3.0 mm, dispersion may not be performed well.

In one embodiment of the present invention, the ring beads are beads made of zirconia, beads made of tungsten carbide, or a combination thereof.

remind Ring mill  Bass Stirring Ring mill  Dispersion step (S20)

In one embodiment of the present invention, the ring mill dispersion step is carried out at a temperature of 20 ℃ to 100 ℃. If the temperature is less than 20 ° C, physical dispersion may not be good, and if it is above 100 ° C, the components in the ring mill base may be denatured.

In one embodiment of the present invention, the stirring speed of the ring mill base is 100 rpm to 1000 rpm. If the stirring speed is less than 100 rpm, no dispersion is made, if the stirring speed is more than 1000 rpm, performance may occur in the stirring device.

In one embodiment of the present invention, the ring mill dispersion step is carried out for 30 to 120 minutes. If the execution time of the ring mill dispersion step is less than 30 minutes, the dispersion may not be sufficient, and if it is more than 120 minutes, the components in the ring mill base may be denatured by the temperature rise, and the yield of the ring mill base is reduced.

EMBODIMENT OF THE INVENTION Hereinafter, the ring mill base which concerns on this invention is demonstrated concretely.

Ring mill  Base

1) inorganic powder particles

The ring mill base according to the present invention comprises inorganic powder particles, wherein the average particle size of the inorganic powder particles is 5 nm to 2000 nm. When the average particle size of the inorganic powder particles is less than 5 nm, the UV blocking effect is weak, and when the average particle size is larger than 2000 nm, light scatters in a broad wavelength range including a visible light region, and white clouding occurs due to scattering of light in the visible light region. cause.

In one embodiment of the present invention, the inorganic powder particles are any one or more selected from the group consisting of zinc oxide, titanium dioxide, cerium oxide and zirconium dioxide.

In one embodiment of the invention, the inorganic powder particles are aluminum hydroxide, stearic acid, triethoxycaprylsilane, alumina, silica, aluminum stearate, isostearic acid, polyhydroxy-stearic acid , Hydrogendimethicone, simethicone, methicone, PEG-10 dimethicone, perfluorooctyltriethoxysilane, manganese dioxide, sodium metaphosphate, sodium polyacrylate and triethoxysilylethyl polydimethylsiloxy It further comprises any one or more selected from the group consisting of seven hexyl dimethicone.

In one embodiment of the present invention, the content of the inorganic powder particles, based on the total weight of the composition, 5% to 80% by weight, preferably 20% to 70% by weight.

2) Thickener

In one embodiment of the present invention, the ring mill base is disteadimonium hectorite, stearalconium hectorite, trihydroxystearin, vinyl dimethicone / methicone silsesquioxane crosspolymer, polymethylsilses quoxane, It further comprises any one or more thickeners selected from the group consisting of silica, polymethylmethacrylate, talc and mica. The thickener can properly maintain the viscosity of the ring mill base to suppress the deposition of inorganic powder particles in the ring mill base, thereby extending the shelf life of the cosmetic composition for sunscreen.

In one embodiment of the present invention, the content of the thickener is 0.1 to 10% by weight, preferably 0.5 to 2% by weight relative to the total weight of the composition.

3) Dispersion

In one embodiment of the present invention, the ring mill base is alcohol benzoate of 12 to 15 carbon atoms, cyclopentasiloxane, caprylic / capric triglyceride, dimethicone, dicaprylylcarbonate, isopropyl myristate and octyl It further comprises any one or more dispersion medium selected from the group consisting of dodecanol.

In one embodiment of the present invention, the content of the dispersion medium is 20% to 90% by weight based on the total weight of the composition.

4) Dispersant

In one embodiment of the present invention, the ring mill base is an acrylate / ethylhexyl acrylate / dimethicone methacrylate copolymer, liglyceryl-3 polyricinoleate, polyhydroxystearic acid, polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone, Cetyl Fiji / Fiji-10 / 1 Dimethicone, Fiji-10 Dimethicone, Lauryl Fiji-9 Polydimethylsiloxyethyl Dimethicone, Bis-Pig / Fiji-14 / 14 dimethicone, Fiji-30 dipolyhydroxystearate and polyglyceryl-2dipolyhydroxystearate further comprises any one or more dispersants selected from the group consisting of.

In one embodiment of the present invention, the content of the dispersant is 0.5% to 20% by weight based on the total weight of the composition.

Hereinafter, the ultraviolet-ray cosmetic composition in which the above-mentioned ring mill base is ring mill-dispersed is demonstrated concretely.

UV-rays Cosmetics  Composition

In one embodiment of the present invention, the viscosity of the cosmetic composition is 3000 to 100,000 cps.

In one embodiment of the present invention, the SPF of the cosmetic composition is 10 to 60.

As used herein, “SPF” is determined by the “COLIPA International Sun Protection Factor Test Method” (COLIPA, May 2006), wherein the skin after standardized application of the light blocking agent The increase in redness threshold (minimum erythema dose, MED) is determined as a function of irradiation time.

The composition according to the present invention may contain other ingredients in addition to the above-mentioned materials within the range not impairing the main effect, preferably giving a synergistic effect to the main effect. In addition, the composition according to the present invention may further include colorants, moisturizers, emollients, ultraviolet absorbers, preservatives, fungicides, antioxidants, pH adjusters, flavoring agents, cooling agents or limiting agents widely used in the art. The compounding quantity of the said component can be selected easily by a person skilled in the art within the range which does not impair the objective and effect of this invention.

In one embodiment of the present invention, the composition may be formulated containing a cosmetically or dermatologically acceptable medium or base.

In one embodiment of the present invention, the formulation of the composition is any one selected from the group consisting of water-in-oil type, oil-in-water type and oil-dispersed type.

In one embodiment of the present invention, the formulation of the composition is impregnated into a foamed polymer foam. More preferably, the foamed polymer foam is a foamed urethane foam.

When the composition is impregnated into the foamed polymer foam, dispersion stability in which the aqueous phase component and the oil phase component are not separated is increased.

Hereinafter, an Example is given and this invention is demonstrated in detail. However, these embodiments are only intended to describe the present invention in detail, and the scope of the present invention is not limited by these embodiments.

Reference Example 1 Preparation of Ring Mill Base

To prepare a ring mill base by mixing the Preparation Examples 1 to 3 in the composition of Table 1 below.

For Preparation Examples 1 and 2, after mixing components 3 to 6 of Table 1 in an oil state, wetting the components 1 and 2 of Table 1 in a powder state, and then mixed with the mixed components 3 to 6 Ring mill base was prepared.

In the case of Preparation Example 3, components 3 to 6 of Table 1, which are in an oil state, were mixed and then dispersed in an azimixer together with Component 7 of Table 1 below. Components 1 and 2 of Table 1, which are in a powder state, were wetted and then mixed with the dispersed components 3 to 7 to prepare a ring mill base.

ingredient	Ingredient Name	Composition (Unit: g)
		Preparation Example 1	Preparation Example 2	Preparation Example 3
One	Fine particle titanium oxide * aluminum hydroxide * stearic acid (titanium dioxide * aluminum hydroxide * stearic acid)	30	33	30
2	Zinc Oxide * Triethoxycaprylylsilane	25	27	25
3	C12-15 alcohols benzoate	26.5	21.5	25.7
4	Fiji-10 dimethicone	2.5	2.5	2.5
5	Acrylate / ethylhexyl acrylate / dimethicone methacrylate copolymer * cyclopentasiloxane	8	8	8
6	Polyhydroxystearic acid * lecithin * ethylhexyl palmitate * isopropyl palmitate * isostearic acid * polyglyceryl-3 polylysinoleate	8	8	8
7	Disteadimonium hectorite	-	-	0.8

Reference Example 2 Dispersion of Ring Mill Base and Measurement of Its Viscosity

The ring mill bases of Preparation Examples 1 to 3 were each ring mill dispersed by rotating with a 500 rpm agitator at a temperature of 30 ° C. to 80 ° C. for 1 hour in a container containing zirconia beads having an average diameter of 230 nm, thereby dispersing the composition of Examples 1 to 3. Prepared.

The viscosity of the composition of Examples 1 to 3 prepared above was measured using Spindle Number No. 64, No. 29 and spindle speed (SPM) measured by a BROOKFIELD viscosity measuring instrument (BROOKFIELD RVDV-III ULTRA (Serial No. RY6521152) set to 12 rpm) and is shown in Table 2 below.

division	Example 1	Example 2	Example 3
Viscosity (cps)	6000	60000	45000

As shown in Table 2, in the case of Example 1 containing about 55% by weight of inorganic sunscreen showed a low viscosity of 6000 cps it can be seen that the dispersion was well, in the case of Example 2 also dispersed with an appropriate viscosity It can be seen that the well, in the case of Example 3, by including a thickener, it can be confirmed that the inorganic sunscreen with high density is prevented from being deposited over time.

In addition, in Example 1, it is difficult to float the inorganic powder particles in the formulation due to the low viscosity, and some occurrence of the caking phenomenon, which is a deposition phenomenon in which the inorganic powder particles settle and agglomeration phenomenon due to deposition, occurs. , Even though the viscosity is lower than that of Example 2, it was confirmed that the inorganic powder particles do not sink and the formulation remains stable by forming a network in the oil phase and floating the inorganic powder due to the disteadimonium hectorite as a component.

Reference Example 3 Preparation of Sunscreen Composition

ingredient	Ingredient Name	Example 4 and Comparative Example 1 (unit: g)
One	C12-15 alcohols benzoate	11.65
2	Fine particle titanium oxide * aluminum hydroxide * stearic acid (titanium dioxide * aluminum hydroxide * stearic acid)	12
3	Zinc Oxide * Triethoxycaprylylsilane	10
4	Fiji-10 dimethicone	One
5	Acrylate / ethylhexyl acrylate / dimethicone methacrylate copolymer * cyclopentasiloxane	3
6	Polyhydroxystearic acid * lecithin * ethylhexyl palmitate * isopropyl palmitate * isostearic acid * polyglyceryl-3 polylysinoleate	3
7	Disteadimonium hectorite	0.35
8	Cyclopentasiloxane * cyclohexasiloxane	26.5
9	Lauryl Fig-9 Polydimethylsiloxyethyl Dimethicone	1.5
10	Disteadimonium hectorite	One
11	Purified water	24.05
12	Disodium ID	0.05
13	Sodium chloride (ICID), sodium chloride (KP)	0.5
14	Butylene Glycol	5
15	Phenoxyethanol	0.4

For Example 4, the oil mill was prepared by mixing the ring mill base in which the components 1 to 7 of Table 1 were dispersed together with the components 8 to 10. The aqueous phase in which the components 11 to 15 of Table 1 were mixed was slowly mixed with the prepared oil phase, and emulsified at 7000 rpm for 10 minutes to prepare a sunscreen composition.

In the case of Comparative Example 1, components 3 to 15 were mixed and then wet and mixed with components 1 and 2 in powder form, and the oil phase was prepared by dispersing for 10 minutes at 7000 rpm with a homo mixer. Thereafter, the aqueous phase in which the components 11 to 15 were mixed was slowly mixed with the prepared oil phase, and emulsified at 7000 rpm for 10 minutes to prepare a sunscreen composition.

 Test Example 2 Measurement of Viscosity and Formulation Stability

Comparative Example 1 and Example 4 prepared in Reference Example 3 were taken after the dispersion state, and are shown in FIGS. 1 and 2, respectively.

Looking at Figure 1, unlike the formulation of Comparative Example 1 that can observe the amorphous inorganic powder particles present in a state of being aggregated in a size of 20 μm or more, looking at Figure 2, the formulation of Example 4 is fine in the inorganic powder particles You can see that it is distributed in size.

In addition, in Example 4 and Comparative Example 1 prepared in Reference Example 3, the viscosity was measured under the same conditions as those measured in Reference Example 2, respectively. 4 is shown. The criterion for determining that the formulation remains stable is that the following agglomeration and oil separation do not occur in the formulation.

1. Agglomeration-The glossiness of the appearance is reduced, and when the glass plate is pushed, the surface of the particles is irregular. Check for foreign body when applying skin.

2. Separation of oil-Take out from 45 ℃ thermostat (manufactured by JISCO Co.) and Cycle machine (LTI-1001SD manufactured by EYELA Co., Ltd.) repeatedly changing the temperature range from -10 ℃ to 45 ℃. Transparent oil sash on the skin. (The formulation is white so can be distinguished)

		Comparative Example 1	Example 4
Viscosity (cps)		80000	17000
Stability	45 ℃ thermostat	7 days	60 days
	Cycle device	14 days	90 days

Looking at the results of Table 4, Comparative Example 1 to which homo mixing is applied in the same composition is compared with Example 4 to which the ring mill dispersion is applied, the inorganic sunscreen is not properly dispersed, the phenomenon of aggregation in the formulation is accelerated, oil of the trauma It doesn't mix very well and you can see the separation happen.

On the other hand, in the case of Example 4 to which the ring mill dispersion is applied, it is excellent in stability, and compared with Comparative Example 1 to which homo mixing is applied, it can be confirmed that the viscosity is about 1/5 lower, and from this, excellent applicability can be expected.

Reference Example 4 Preparation of Sunscreen Composition

Example 5 was prepared in the same manner as in Example 4 of Reference Example 3, except that the composition was performed as in Table 5, and Comparative Example 2 was prepared by the same procedure as Comparative Example 1 of Reference Example 3 (However, the ring mill base was Components 1 to 4).

In Example 5, the oil mill was prepared by mixing the ring mill base in which the components 1 to 4 in Table 1 were dispersed together with the components 8 to 10. The aqueous phase in which the components 11 to 15 of Table 1 were mixed was slowly mixed with the prepared oil phase, and emulsified at 7000 rpm for 10 minutes to prepare a sunscreen composition.

In the case of Comparative Example 1, components 4 and 8 to 15 were mixed and then mixed by wetting the components 1 and 2 in powder form, and dispersed in a homo mixer at 7000 rpm for 10 minutes to prepare an oil phase. Thereafter, the aqueous phase in which the components 11 to 15 were mixed was slowly mixed with the prepared oil phase, and emulsified at 7000 rpm for 10 minutes to prepare a sunscreen composition.

ingredient	Ingredient Name	Example 5 and Comparative Example 2 (unit: g)
One	Fine particle titanium oxide * aluminum hydroxide * stearic acid (titanium dioxide * aluminum hydroxide * stearic acid)	8
2	Zinc Oxide * Triethoxycaprylylsilane	8
3	Ethylhexylmethoxycinnamate	7
4	Ethylhexyl salicylate	4
8	Cyclopentasiloxane * cyclohexasiloxane	26.5
9	Lauryl Fig-9 Polydimethylsiloxyethyl Dimethicone	1.5
10	Disteadimonium hectorite	One
11	Purified water	24.05
12	Disodium ID	0.05
13	Sodium chloride (ICID), sodium chloride (KP)	0.5
14	Butylene Glycol	5
15	Phenoxyethanol	0.4

<Test Example 4> UV protection

In order to measure the UV blocking index, the amount of ultraviolet light emitted to the test site was measured using the IL1733 radiometer and SED 240 probe, except for the spine of 12 subjects including 6 males and 6 females. It was adjusted to 100mj / ㎠ to irradiate with a solar simulator (Solar simulater; 81293 (Xenon UV Lamp 1KW, unfiltered)) lamp. Minimal erythema amount (Minimal Erythema Dosa: MED) was confirmed 24 hours after UV irradiation. In order to confirm the UV blocking effect of the sample to uniformly apply the sample to the same site, such as the subject of Example 1 and Comparative Examples 1 and 2 of Preparation Example 1 to a thickness of 2㎛ / ㎠ It was left to dry for 15 minutes. The UV irradiation window was attached to the sample application sites of Comparative Examples 2 and 5 and fixed, and the other parts except the irradiation window were blocked with UV using a leather and a towel, and UV was irradiated. Based on the subject's MED, SPF 50 and the predicted sample were started with SPF 15-40 and dose, and gradually increased UV dose. Minimum erythema amount was determined after 24 hours of ultraviolet irradiation, and the UV blocking effect was calculated according to Equation 1 below.

[Equation 1]

UV protection effect of the sample (SPF) = (minimum erythema of the sample coated area) / (minimum erythema of the sample uncoated area)

	Comparative Example 2	Example 5
SPF measurement	38	57.5

Looking at Table 6, it can be seen that in the same composition, compared to Comparative Example 2 to which homo mixing is applied, Example 5 to which the ring mill dispersion is applied improves the SPF measured value by 1.5 times.

Claims (5)

1. A sunscreen cosmetic composition comprising a ring mill dispersion of a ring mill base containing inorganic powder particles,

   Cosmetic particle composition having an average particle size of the inorganic powder particles is 5 nm to 2000 nm.
2. The method of claim 1,

   The inorganic powder particles are any one or more selected from the group consisting of zinc oxide, titanium dioxide, cerium oxide and zirconium dioxide.
3. The method of claim 1,

   The ring mill base is disteadimonium hectorite, stearalconium hectorite, trihydroxystearin, vinyl dimethicone / methicone silsesquioxane crosspolymer, polymethylsilses quoxane, silica, polymethyl methacrylate, talc And a cosmetic composition further comprises any one or more thickeners selected from the group consisting of mica.
4. The method of claim 1,

   The content of the thickener is 0.1% by weight to 10% by weight relative to the total weight of the composition.
5. A ring mill mixing step of mixing the inorganic powder particles, which are 5 nm to 2000 nm, and the ring beads; And

   Method of producing a cosmetic composition for sunscreen comprising a; ring mill dispersion step of stirring the ring mill base.

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