KR102417771B1 - Water-dispersible titanium dioxide composite powder - Google Patents

Abstract

The present invention relates to a titanium dioxide surface-treated hydrophobic with an alkoxy silane; nonionic surfactants having an HLB of 12 to 18; and lipids having an HLB of 1 to 5; to a water-dispersible titanium dioxide composite powder prepared by pulverizing a mixture comprising a milling process.

Description

Water-dispersible titanium dioxide composite powder

The present invention relates to a water-dispersible titanium dioxide composite powder having a complexion improvement effect and excellent skin stability, and an oil-in-water cosmetic composition comprising the same.

The water-in-oil (W/O) cosmetic composition generally applied in the existing cosmetic field is an external oil phase that is a continuous phase of titanium dioxide (TiO ₂ ) for pigments in order to give an immediate complexion improvement effect (white turbidity). The emulsion formulation was stabilized using a surfactant having a low hydrophile-lipophile balance (HLB). In this case, titanium dioxide for pigment is contained in the external oil phase as a continuous phase, which has the advantage of having excellent formulation stability and skin stability.

However, the water-in-oil formulation has excellent water resistance and thus has excellent makeup durability, but has poor skin burden such as stickiness and oiliness, spreadability, and spreadability.

Therefore, when changing the formulation to oil-in-water (O/W), it is possible to realize a light, moist, soft feeling and high moisture, while titanium dioxide for pigment used for complexion improvement effect is used at the emulsion interface. There was a problem that deteriorated the stability of the formulation and caused skin irritation.

Accordingly, there is a continuous demand for the development of a cosmetic composition with reduced skin irritation while maintaining a complexion improvement effect, excellent feeling of use, and high moisture.

As a similar prior document on improving skin irritation, Korean Patent Application Laid-Open No. 2012-0043167 is presented.

Korean Patent Publication No. 2012-0043167 (2012.05.03)

An object of the present invention is to provide a water-dispersible titanium dioxide composite powder having a complexion improvement effect and excellent skin stability, and an oil-in-water cosmetic composition comprising the same.

The present invention relates to a titanium dioxide surface-treated hydrophobic with an alkoxy silane; nonionic surfactants having an HLB of 12 to 18; and lipids having an HLB of 1 to 5; to a water-dispersible titanium dioxide composite powder prepared by pulverizing a mixture comprising a milling process.

In addition, another aspect of the present invention relates to an oil-in-water cosmetic composition comprising a water-dispersible titanium dioxide composite powder.

The water-dispersible titanium dioxide composite powder according to the present invention uses titanium dioxide treated with a hydrophobic surface with an alkoxy silane to maintain the skin complexion improvement effect (white turbidity), and to allow water dispersion by milling process. Although titanium dioxide is used, skin irritation can be remarkably reduced, and during the milling process, titanium dioxide, a nonionic surfactant having an HLB of 12 to 18, and a lipid having an HLB of 1 to 5 are mixed and dispersed in an oil-in-water formulation. It has the advantage of being able to maintain a very stable formulation even with

Hereinafter, the water-dispersible titanium dioxide composite powder according to the present invention will be described in detail with reference to the accompanying drawings. The drawings introduced below are provided as examples so that the spirit of the present invention can be sufficiently conveyed to those skilled in the art. Accordingly, the present invention is not limited to the drawings presented below and may be embodied in other forms, and the drawings presented below may be exaggerated to clarify the spirit of the present invention. Also, like reference numerals refer to like elements throughout.

At this time, if there is no other definition in the technical terms and scientific terms used, it has the meaning commonly understood by those of ordinary skill in the art to which this invention belongs, and the gist of the present invention in the following description and accompanying drawings Descriptions of known functions and configurations that may be unnecessarily obscure will be omitted.

The present invention enables water dispersion by milling the hydrophobic surface-treated titanium dioxide for pigments with surfactants and lipids having different hydrophile-lipophile balance (HLB) to ensure formulation stability when applied to oil-in-water cosmetic compositions, , to a water-dispersible titanium dioxide composite powder that can reduce skin irritation.

In detail, the water-dispersible titanium dioxide composite powder according to an embodiment of the present invention includes: titanium dioxide surface-treated with an alkoxy silane hydrophobic; nonionic surfactants having an HLB of 12 to 18; and lipids having an HLB of 1 to 5; may be prepared by pulverizing a mixture comprising a milling process.

As described above, by using titanium dioxide treated with hydrophobic surface with alkoxy silane, the effect of improving skin complexion (white turbidity) is maintained, and by processing it in a milling process to enable water dispersion, skin irritation is reduced despite the use of the same amount of titanium dioxide. In the milling process, titanium dioxide, a nonionic surfactant having an HLB of 12 to 18, and a lipid having an HLB of 1 to 5 are mixed and used together, so that the formulation can be maintained very stably even when dispersed in an oil-in-water formulation. .

In an example of the present invention, the water-dispersible titanium dioxide composite powder may contain 40 to 50% by weight of titanium dioxide, 1 to 10% by weight of a nonionic surfactant, and 30 to 40% by weight of lipids based on the total weight. When milling in the above range, the composite powder may have excellent water dispersion performance, and thus, excellent formulation stability and skin safety can be secured when preparing an oil-in-water cosmetic composition.

In an example of the present invention, titanium dioxide is used for an immediate skin complexion improvement effect, and the alkoxysilane coated on the surface of titanium dioxide is used in oil-in-water formulations through hydrophobic interactions with the hydrophobic group of the surfactant. It can play a role in helping to stably exist on the interface between water and water. Specifically, the alkoxy silane may satisfy Formula 1 below.

[Formula 1]

In Formula 1, R ₁ may be C1-C3 alkyl, R ₂ may be C1-C18 alkyl, alkenyl or alkynyl, and R ₃ may be —H, C1-C3 alkyl. and n may be a real number of 1-3.

More specifically, in one non-limiting embodiment, vinyltrimethoxysilane, vinyltriethoxysilane, 2-(3,4 epoxycyclohexyl)ethyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane 3-Glycidoxypropylmethyldiethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-acryloxypropyltrimethoxysilane, N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane , 3-Aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, 3-ureidopropyltriethoxysilane 3-isocyatatepropyltriethoxy It may be any one or two or more selected from silane, trimethoxycaprylylsilane, and triethoxycaprylylsilane.

However, when the surface-treated titanium dioxide is applied to the oil-in-water formulation as it is without milling treatment, the titanium dioxide is located at the interface of the formulation, impairs the stability of the dispersed phase, and may cause skin irritation. It is preferable to perform a milling process so that it can be dispersed in water. At this time, by properly adjusting the milling process conditions, the effect of improving the complexion by titanium dioxide for pigments may not be inhibited, and the water dispersion performance of the titanium dioxide composite powder may be more effectively secured. In one embodiment, the average particle diameter of titanium dioxide before the milling process may be several to several tens of μm, and more specifically, 1 to 20 μm. The average particle diameter of titanium dioxide fine particles after the milling process may be smaller than the average particle diameter of titanium dioxide before the milling process as it is pulverized by the milling process, and more specifically, may be 0.5 to 15 μm, but is not necessarily limited thereto.

In addition, water dispersion performance can be further improved by milling titanium dioxide, a nonionic surfactant, and a lipid together. If non-ionic surfactants and lipids are not used, the fine particles of titanium dioxide are not well dispersed in the aqueous phase and sedimentation occurs during dispersion in water, or the particles of titanium dioxide agglomerate, which can impair the stability of the composition. .

In one embodiment of the present invention, nonionic surfactants and lipids having different HLBs may be used together during the milling process. Specifically, as described above, the HLB of the nonionic surfactant may be 12 to 18, and the HLB of the lipid may be 1 to 5. As such, by mixing and using two materials having different HLBs, the water dispersion stability of the composite powder can be improved when dispersed in an oil-in-water formulation. More preferably, the HLB of the nonionic surfactant may be 13 to 17, and the HLB of the lipid may be 1 to 3.

The nonionic surfactant has an HLB of 12 to 18, and may be used without particular limitation as long as it is commonly used in the art, for example, an alkylene oxide adduct type, a polyhydric alcohol type, an alkylene oxide adduct-polyhydric alcohol type or a mixture thereof. More specifically, in one non-limiting embodiment, the alkylene oxide adduct type is laureth-7, laureth-9, laureth-23, cetes-10, cetes-20, isoceteth-20, Ceteareth-12, Ceteareth-20, Ceteareth-25, Ceteareth-30, Steareth-10, Steareth-20, Oleth-10, Oleth-20, PEG-20 Stearate, PEG-30 Stear any one or two or more selected from the rate and PEG-40 stearate, and the polyhydric alcohol type may be any one or two or more selected from glycerol, 1,2-propylene glycol, sorbitol, butylene glycol and hexylene glycol, , The alkylene oxide adduct-polyhydric alcohol type is polysorbate 20, polysorbate 40, polysorbate 60, polysorbate 80, PEG-20 glyceryl isostearate, PEG-40 castor oil, PEG-40 - It may be any one or two or more selected from hydrogenated castor oil and PEG-60-hydrogenated castor oil, but is not necessarily limited thereto.

The lipid may be used without particular limitation as long as it has an HLB of 1 to 5 and is commonly used in the art, but may be, for example, a phospholipid. More specifically, in one non-limiting embodiment, the phospholipid is a C14-C20 phosphatidyl choline-based acyl group, a C14-C20 phosphatidyl ethanolamine-based, C14-C20 phosphatidylserine-based, carbon number C14-C20 phosphatidic acid, C14-C20 phosphatidylglycerol, C14-C20 phosphatidylinositol, C14-C20 rhizophosphatidylcholine, aliphatic C14-C20 sphingo It may be any one or two or more selected from the myelin series and hydrides thereof, but is not necessarily limited thereto.

As a preferred example, the nonionic surfactant may be an alkylene oxide adduct-polyalcohol type, and the lipid may be a phosphatidyl choline-based phospholipid having a C14-C20 acyl group. As a particularly preferred example, the use of polysorbate 80 as the nonionic surfactant and hydrogenated lecithin as the lipid may be advantageous in securing excellent formulation stability and light, moist and soft feel.

In an example of the present invention, the hydrophobic surface-treated titanium dioxide can be made water-dispersible by processing the milling process with a nonionic surfactant and lipids, thus securing formulation stability when applied to oil-in-water formulations, and It can reduce irritation. In detail, the milling process is not particularly limited as long as it is a method commonly performed in the art, and in one non-limiting example, roll milling, ball milling, bead milling, art Attrition milling (Attrition Milling), planetary milling (Planetary Milling), jet milling (Zet Milling) and may be any one or two or more selected from the ring mill (Ring mill).

In an example of the present invention, the milling process is not particularly limited, but it is good to control the milling process conditions for titanium dioxide, nonionic surfactant, and lipid components used. In one embodiment, the milling process may be performed at 8000 to 10000 rpm for 60 to 90 minutes, but is not necessarily limited thereto.

In addition, the present invention relates to an oil-in-water cosmetic composition comprising a water-dispersible titanium dioxide composite powder, and it is possible to realize a light, moist, soft feeling and high moisture feeling.

In detail, the oil-in-water cosmetic composition according to an embodiment of the present invention comprises: titanium dioxide surface-treated hydrophobic with alkoxy silane; nonionic surfactants having an HLB of 12 to 18; and lipids having an HLB of 1 to 5; may include a water-dispersible titanium dioxide composite powder prepared by pulverizing a mixture comprising a milling process.

As described above, by milling the hydrophobic surface-treated titanium dioxide, it can be effectively dispersed in the external aqueous phase, which is the continuous phase of the oil-in-water cosmetic composition, and excellent formulation stability and skin safety can be ensured.

In the oil-in-water cosmetic composition according to an example, the water-dispersible titanium dioxide composite powder may be contained in 0.1 to 10% by weight of the total composition, preferably in 0.5 to 5% by weight, more preferably in 1 to 3% by weight. can be The complexion improvement effect is excellent in the above range, and skin irritation can be significantly reduced.

Such an oil-in-water cosmetic composition can be used for basic makeup such as skin, lotion or essence, makeup base, foundation, BB cream, or concealer, or functional makeup such as sunscreen.

In one embodiment, when used for sunscreen, the oil-in-water cosmetic composition may further include a sunscreen, and the sunscreen may be an organic sunscreen, an inorganic sunscreen, or a mixture thereof. Organic sunscreens are homosalate, ethylhexyl salicylate, phenylbenzimidazole sulfonic acid, octocrylene, ethylhexyl methoxycinnamate, ethylhexyl palmitate, butylmethoxydibenzoylmethane, 4-methylbenzylidene camphor. , isoamyl-p-methoxycinnamate and bis-ethylhexyloxyphenol methoxyphenyltriazine, etc., may be any one or two or more, and the inorganic sunscreen is any one selected from titanium dioxide, zinc oxide, iron oxide, etc. It may be two or more, but is not necessarily limited thereto. The content of the sunscreen is not particularly limited, but may be 1 to 25% by weight, preferably 5 to 20% by weight, based on the total weight of the composition.

Other oil-in-water cosmetic compositions include surfactants, antioxidants, stabilizers, pH adjusters, preservatives, bactericides, and pigments commonly used in the art according to the purpose of the cosmetic composition within the range that does not reduce formulation stability and skin safety. , and may further include a fragrance or pearl agent.

Hereinafter, the water-dispersible titanium dioxide composite powder and oil-in-water cosmetic composition according to the present invention will be described in more detail through Examples. However, the following examples are only a reference for describing the present invention in detail, and the present invention is not limited thereto, and may be implemented in various forms. Also, unless otherwise defined, all technical and scientific terms have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein is for the purpose of effectively describing particular embodiments only and is not intended to limit the invention. Also, the singular forms used in the specification and appended claims may also be intended to include the plural forms unless the context specifically dictates otherwise. In addition, the unit of additives not specifically described in the specification may be weight %.

[Production Example 1]

Milling 50% by weight of titanium dioxide (CI 77891), 20% by weight of butylene glycol, 10% by weight of polysorbate 80, 10% by weight of aluminum hydroxide, 5% by weight of hydrogenated lecithin and 5% by weight of triethoxycaprylylsilane A titanium dioxide composite powder was prepared by grinding and mixing in the process.

[Comparative Preparation Example 1]

Titanium dioxide (CI 77891) 76.9% by weight, aluminum hydroxide 15.4% by weight, and triethoxycaprylylsilane 7.7% by weight were mixed to prepare a titanium dioxide composite powder.

[Comparative Preparation Example 2]

50% by weight of titanium dioxide (CI 77891), 20% by weight of butylene glycol, 10% by weight of polysorbate 80, 10% by weight of aluminum hydroxide, 5% by weight of hydrogenated lecithin and 5% by weight of triethoxycaprylylsilane are mixed Thus, a titanium dioxide composite powder was prepared, but the milling process was not performed.

[Comparative Preparation Example 3]

Titanium dioxide composite powder was prepared by mixing 52.6 wt% of titanium dioxide (CI 77891), 21.1 wt% of butylene glycol, 10.5 wt% of polysorbate 80, 10.5 wt% of aluminum hydroxide and 5.3 wt% of triethoxycaprylylsilane did

[Example 1 and Comparative Examples 1 to 3]

A sunscreen was prepared by mixing the titanium dioxide composite powder prepared in Preparation Example 1 or Comparative Preparation Examples 1 to 3 according to the composition (% by weight) shown in Table 1 below.

[Table 1]

[Skin Stability Test]

A skin irritation test was performed on 33 panelists (10 males, 23 females) with an average age of 26.6 years using the C-HPIT 2003(3) method. The sunscreens prepared in Example 1 and Comparative Examples 1 to 3 were applied to the skin and cheekbones under the eyes, respectively, and after 20 minutes, the degree of skin irritation was measured and quantified, and the results are shown in Table 2. At this time, the higher the level of stimulation, the stronger the degree of skin irritation.

[Table 2]

[Formulation stability test]

After leaving the sunscreens prepared in Example 1 and Comparative Examples 1 to 3 at room temperature (25° C.) for 30 days, the state of the formulation was evaluated, and the results are shown in Table 3.

[Table 3]

As described above, in the present invention, specific matters and limited examples and comparative examples have been described, but these are provided to help a more general understanding of the present invention, and the present invention is not limited to the above examples, and the present invention is not limited to the above examples. Various modifications and variations are possible from these descriptions by those of ordinary skill in the art.

Therefore, the spirit of the present invention should not be limited to the described embodiments, and not only the claims described below, but also all of the claims and all equivalents or equivalent modifications to the claims will be said to belong to the scope of the spirit of the present invention. .

Claims (11)

titanium dioxide surface-treated hydrophobically with alkoxy silane; nonionic surfactants having an HLB of 12 to 18; and a lipid having an HLB of 1 to 5; is a water-dispersible titanium dioxide composite powder prepared by pulverizing a mixture comprising a milling process,
The nonionic surfactant is an alkylene oxide adduct type, a polyhydric alcohol type, an alkylene oxide adduct-polyhydric alcohol type, or a mixture thereof,
The alkylene oxide adduct type is laureth-7, laureth-9, laureth-23, cetes-10, cetes-20, isoceteth-20, ceteareth-12, ceteareth-20, ceteareth Any one selected from -25, ceteareth-30, steareth-10, steareth-20, oleth-10, oleth-20, PEG-20 stearate, PEG-30 stearate and PEG-40 stearate or two or more,
The polyhydric alcohol type is any one or two or more selected from glycerol, 1,2-propylene glycol, sorbitol, butylene glycol and hexylene glycol,
The alkylene oxide adduct-polyhydric alcohol type is polysorbate 20, polysorbate 40, polysorbate 60, polysorbate 80, PEG-20 glyceryl isostearate, PEG-40 castor oil, PEG-40- any one or two or more selected from hydrogenated castor oil and PEG-60-hydrogenated castor oil,
The lipid is a C14-C20 phosphatidyl choline-based acyl group, a C14-C20 phosphatidyl ethanolamine-based, C14-C20 phosphatidylserine-based, C14-C20 phosphatidic acid-based, carbon number Any one selected from C14-C20 phosphatidylglycerol, C14-C20 phosphatidylinositol, C14-C20 lysophosphatidylcholine, aliphatic C14-C20 sphingomyelin, and hydrides thereof Or two or more water-dispersible titanium dioxide composite powder.
The method of claim 1,
The powder is a water-dispersible titanium dioxide composite powder containing 40 to 50% by weight of titanium dioxide, 1 to 10% by weight of a nonionic surfactant, and 30 to 40% by weight of a lipid based on the total weight.
delete delete delete delete The method of claim 1,
The milling process is any one or two or more water-dispersible titanium dioxide composite powder selected from roll milling, ball milling, bead milling, attrition milling, planetary milling, jet milling and ring milling.
8. The method of claim 7,
The milling process is a water-dispersible titanium dioxide composite powder that is performed for 60 to 90 minutes at 8000 to 10000 rpm.
An oil-in-water cosmetic composition comprising the water-dispersible titanium dioxide composite powder according to any one of claims 1, 2, 7 and 8.
10. The method of claim 9,
The water-dispersible titanium dioxide composite powder is an oil-in-water cosmetic composition contained in an amount of 0.1 to 10% by weight of the total composition.
10. The method of claim 9,
The composition is an oil-in-water cosmetic composition for UV protection.