KR101047694B1 - Solid oil-in-water type cosmetic composition having a volatilization stability and excellent moisture retention - Google Patents

Abstract

The present invention relates to a solid oil-in-water cosmetic composition, and more particularly, to a polyoxyalkylene addition organopolysiloxane including lauryl fiji-9 polydimethylsiloxyethyldimethicone as a surfactant or the polyoxyalkylene addition valent By containing a mixture of nopolysiloxane and a hydrophobic surfactant, the present invention relates to a solid oil-in-water cosmetic composition that prevents shrinkage, surface cracking, and change of feeling caused by volatilization in the water phase, thereby providing a fresh, light usability and excellent moisturizing effect.

Volatilization stability * Moisturizing * Solid (cake) * Lauryl Fiji-9 Polydimethylsiloxyethyldimethicone * Emulsion

Description

Oil-in-water solid cosmetic composition with higher stability against evaporation of internal phase (water) as well as outstanding moisturizing effect}

The present invention relates to a solid oil-in-water cosmetic composition, and more particularly, to a polyoxyalkylene addition organopolysiloxane including lauryl fiji-9 polydimethylsiloxyethyldimethicone as a surfactant or the polyoxyalkylene addition valent The present invention relates to a solid oil-in-water cosmetic composition which contains a mixture of nopolysiloxane and a hydrophobic surfactant to prevent shrinkage, surface cracking, and change in feeling caused by volatilization in the water phase, thereby providing a fresh, light usability and excellent moisturizing effect.

Solid (cake) cosmetics are prepared by a method of solidifying by molding in a plate or a container using a large amount of wax or oil thickener and mixtures thereof to maintain the cake or stick form in the oily ingredients. The oil cake or stick manufactured in this way has the advantage of being easy to carry and use, and to form a cosmetic film with excellent water repellency, while the feeling of use is very heavy and waxy due to the large amount of wax used to maintain the oil component and form. (Eoly), and face had a drawback over time.

Many techniques have been researched and developed to remedy this disadvantage. For example, U.S. Patent No. 5,725,845 discloses a stick type matt finish cosmetic composition, and U.S. Patent No. 5,266,321 discloses a method for improving bleeding or lifting while maintaining a high oil content using a silicone gel. Although the Korean Patent Laid-Open Publication No. 2003-0050532 attempts to improve the cosmetic composition using a volatile oil and an excessive amount of powder, there is a problem of inferior high temperature fluidity during molding and the use of excess volatile oil and powder. As the skin is pulled over time, the used powder agglomerates to the skin, causing the skin to become white. As a technology developed to improve these disadvantages, US Patent Nos. 5,645,903 and 5,362,482 disclose oil-in-water emulsified and water-in-oil emulsified solid cosmetic compositions, respectively. Although they have been disclosed, special care has to be taken even when using closed containers due to the problem that the water in the inner water is volatilized or the surface is cracked during use.

In order to solve the problem of shrinkage or cracking by lowering the volatility of the contents, the present inventors analyze what components are volatilized first when contracting and cracking the surface in a solid (cake) oil-in-water cosmetic and volatile components and solid (cake) oil-in-water cosmetic In-depth study of the relationship between the stability and the results showed that even in the case of solid (cake) oil-in-water emulsions containing large amounts of volatile silicones, the components that primarily affect the shrinkage and cracking of the contents are those It was confirmed that the water phase, not silicon, and the volatility of the water phase was closely related to the interfacial tension between the water phase and the oil phase. That is, in order to improve the shrinkage or surface cracking of the solid (cake) oil-in-water emulsion, it is necessary to use a surfactant that can effectively lower the energy of the interface by adsorbing at the interface between the inner and outer oil phases. The present inventors have studied various types of surfactants and found that polyoxyalkylene-added organopolysiloxanes including lauryl fig-9 polydimethylsiloxyethyldimethicone or polyoxyalkylene-added organopolysiloxanes and hydrophobic surfactants When using the mixture as a surfactant it was found that even if it contains a large amount of water phase to minimize the energy of the water-based interface to provide an initial moisture feeling without shrinkage or surface cracking of the contents to complete the present invention.

Accordingly, it is an object of the present invention to provide a stable solid (cake) oil-in-water cosmetic composition that can simultaneously moisturize with moisture and light usability without contraction or surface cracking of the inner phase.

In order to achieve the above object, in the present invention, a hydrophobic interface with a polyoxyalkylene addition organopolysiloxane or a polyoxyalkylene addition organopolysiloxane including lauryl fig-9 polydimethylsiloxyethyldimethicone as a surfactant A solid oil-in-water cosmetic composition containing a mixture of active agents is provided.

The solid oil-in-water cosmetic composition according to the present invention minimized the energy of the aqueous-oil-based interface to prevent shrinkage, surface cracking, and feeling change of contents caused by volatilization in the aqueous phase, thereby providing a fresh and light usability and excellent moisturizing effect.

The solid oil-in-water cosmetic composition according to the present invention contains a surfactant, an oil, an oil thickener, a cosmetic powder, and water.

Surfactants used in the present invention include polyoxyalkylene addition organopolysiloxane including lauryl fig-9 polydimethylsiloxyethyldimethicone or a mixture of the polyoxyalkylene addition organopolysiloxane and a hydrophobic surfactant. have.

The amount of the surfactant is preferably 0.01 to 10 parts by weight based on 100 parts by weight of the composition. If it exceeds 10 parts by weight, the stickiness is increased and the feeling of use is worsened. When the content is less than 0.01 parts by weight, the volatilization stability may be lowered.

The polyoxyalkylene addition organopolysiloxane comprising lauryl fig-9 polydimethylsiloxyethyldimethicone used in the present invention has the structure of formula (I):

Hydrophobic surfactants used in the present invention include sorbitan sesquioleate, sorbitan isostearate and sorbitan sesquiisostearate, which may be lauryl fiji-9 polydimethylsiloxyethyldimethicone. When used in combination with the containing polyoxyalkylene addition organopolysiloxane, the mixing ratio is preferably 0.1: 1 to 1: 0.1 by weight.

Oils used in the present invention include silicone oils, hydrocarbon-based oils, higher fatty acids, higher fatty acid esters, higher alcohols, vegetable oils and mixtures thereof, the content of which is 5 to 80 parts by weight based on 100 parts by weight of the composition desirable. If the content is less than 5 parts by weight, the moisturizing effect is inferior, and if it exceeds 80 parts by weight, the form may collapse and flow at a high temperature, as well as the water content is low, the overall feeling of use becomes heavy.

As the volatile silicone oil used in the present invention, it is preferable to use a cyclomethicone silicone oil represented by the following Chemical Formula 2, such as octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane.

In addition, the cosmetic composition according to the present invention includes a non-volatile silicone oil containing dimethicone and polypetrinylmethicone as an oil for improving the moisturizing effect or feeling; Hydrocarbon-based oils including squalane, liquid paraffin, and hydrogenated C6-14 olefin polymers; Higher fatty acids; Higher fatty acid esters including butyleneglycoldicaprylate-dicaprate, C14-18 alkylethylhexanoate, dicaprylylcarbonate, cetyloctanoate and octyldodecyl myristate; Higher alcohols; Vegetable oils including meadowfoam seed oil, olive oil and jojoba oil; And sunscreen oils including ethylhexylmethoxycinnamate, octylsalicylate, ethylhexyltriazine and bis-ethylhexyloxyphenol methoxyphenyltriazine, and the like, but are not limited thereto.

Since the solid oil-in-water cosmetic composition according to the present invention must maintain its form without flowing in the temperature range (for example, minus 20 to 50 ℃) used by customers, for this purpose, a solid wax having a high melting point is used as an oil thickener. do. Solid wax used in the present invention is composed of a linear or branched hydrocarbon having 25 to 52 carbon atoms, specifically, petroleum wax such as paraffin wax and microcrystalline wax; Mineral waxes such as ozokerite and ceresin; Natural waxes such as carnauba wax and candelilla wax, and the like, and these may be used alone or in combination. The amount of the oil thickener is preferably 2 to 20 parts by weight based on 100 parts by weight of the composition. If the content of the thickener is less than 2 parts by weight, it is difficult to make a solid (cake) formulation, and if it exceeds 20 parts by weight, it is too hard and does not apply well.

Cosmetic powders used in the present invention include talc, mica, sericite, silica, polymethyl methacrylate, nylon, synthetic mica, titanium dioxide, zinc oxide and titanated mica, the content of which is a composition 0 to 50 parts by weight are preferred based on 100 parts by weight. The solid oil-in-water cosmetic provided by the present invention may not contain a cosmetic powder according to the purpose of use, and when the content of the cosmetic powder exceeds 50 parts by weight, the feeling is too powdery so that the skin is easily pulled out after application. Occurs.

The solid oil-in-water cosmetic composition according to the present invention is not particularly limited in its formulation, but is not only skin care cosmetics such as solid balm, eye stick, cleansing balm and sunscreen balm, but also cosmetics such as makeup base and foundation, etc. Can be formulated.

Hereinafter, the present invention will be described in more detail with reference to Examples and Test Examples. However, the scope of the present invention is not limited to the following experimental examples, test examples and the like.

[Examples 1-3 and Comparative Examples 1-4]

The solid (cake) oil-in-water emulsions of Examples 1 to 3 and Comparative Examples 1 to 4 were prepared according to the compositions shown in Table 1 below.

division Compounding Ingredients (wt%) Example Comparative example One 2 3 One 2 3 4 Paid
ingredient Decamethylcyclopentasiloxane 30 30 30 30 30 30 30 Ceresin 3 3 3 3 3 3 3 Candelilla wax 3 3 3 3 3 3 3 Polyoxyalkylene addition organopolysiloxane including lauryl fig-9 polydimethylsiloxyethyldimethicone 2 0.5 0.5 - - - - Cetyl Fiji / Fiji -10/1 dimethicone - One 0.5 2 One 0.5 - Sorbitan sesquioleate - 0.5 1.0 - One 1.5 2 Awards
ingredient Purified water Balance Balance Balance Balance Balance Balance Balance glycerin 5 5 5 5 5 5 5 Butylene glycol 5 5 5 5 5 5 5

<Manufacturing Method>

1) The oily ingredients were mixed and warmed to 75 to 80 ° C and completely dissolved.

2) The aqueous phase components were mixed and dissolved, and then heated to 70 ° C.

3) The oil phase component of 1) was emulsified by gradually adding the water phase component of 2) while stirring at 7000 rpm using a homogenizer. At this time, the temperature was maintained at 70 ° C.

4) After the addition of the aqueous phase component was continued stirring for 3-5 minutes and then degassed and poured into a container to cool to 30 ℃ to complete the solid (cake) oil-in-water emulsion.

[Test Example 1] Volatile Stability of Ibam with Solid (Cake) Water-Based Oils According to the Composition of Surfactants

The solid (cake) oil-in-water emulsions prepared in Examples 1 to 3 and Comparative Examples 1 to 4 were placed in a thermostatic bath at 30 ° C and 45 ° C, and the weight change was performed for 1 week, 2 weeks and 3 weeks without the cap of the container being closed. The surface state was checked to evaluate the volatilization stability of the contents.

<Measurement of Volatilization of Contents>

Volatility of contents = (weight of initial contents-weight of contents over time) / weight of initial contents × 100

Storage temperature (℃)
(without cap) Volatility Stability
(Shrink / split surface) 1 week 2 weeks 3 weeks Example 1 30 0.4 1.1 1.4 Good 45 1.3 2.8 5.7 Good Example 2 30 0.65 1.11 1.38 Good 45 2.1 4.34 7.99 Good Example 3 30 1.0 1.8 2.4 Good 45 5.4 12.8 17.8 Good Comparative Example 1 30 8.9 15.4 30.89 Shrink 45 24.1 46.7 70.2 Contraction / Crack Comparative Example 2 30 7.5 13.5 29.8 Shrink 45 19.0 36.3 59.0 Contraction / Crack Comparative Example 3 30 3.6 7.77 13.4 Good 45 7.3 18.88 31.1 Shrink Comparative Example 4 30 10.99 28.09 60.28 Contraction / Crack 45 20.1 54.8 73.4 Contraction / Crack

As shown in the results of Table 2 above, Examples 1 to 1 containing polyoxyalkylene addition organopolysilonic acid containing lauryl fiji-9 polydimethylsiloxyethyldimethicone and a hydrophobic surfactant together In the case of 3, although the cap was left open, it was confirmed that even at 30 ° C and 45 ° C, the volatilization of the contents was low, and it was prepared as a stable solid (cake) oil-in-water emulsion type that does not cause problems such as shrinkage or surface cracking.

[Examples 4 to 6 and Comparative Examples 5 to 8]

The solid (cake) oil-in-water type sunscreen of Examples 4-6 and Comparative Examples 5-8 was prepared according to the composition shown in Table 3 below.

division Compounding Ingredients (wt%) Example Comparative example 4 5 6 5 6 7 8 Paid
ingredient Decamethylcyclopentasiloxane 20 20 20 20 20 20 20 Ceresin 3 3 3 3 3 3 3 Candelilla wax 3 3 3 3 3 3 3 Octylmethoxycinnamate ^{1 )} 7 7 7 7 7 7 7 Isoamyl-p-methoxycinnamate ^{1 )} 2 2 2 2 2 2 2 Bisethylhexyloxyphenol methoxyphenyl triazine ^{1 )} 3 3 3 3 3 3 3 Polyoxyalkylene addition organopolysiloxane including lauryl fig-9 polydimethylsiloxyethyldimethicone 2 0.5 0.5 - - - - Cetyl Fiji / Fiji -10/1 dimethicone - One 0.5 2 One 0.5 - Sorbitan sesquioleate - 0.5 1.0 - One 1.5 2 Dicaprylylcarbonate 4 4 4 4 4 4 4 powder Titanium oxide 5 5 5 5 5 5 5 Awards
ingredient Purified water Balance Balance Balance Balance Balance Balance Balance glycerin 5 5 5 5 5 5 5 Butylene glycol 5 5 5 5 5 5 5

* ¹⁾ : organic sunscreen

<Manufacturing Method>

1) The oily ingredients except for the sunscreen were mixed and warmed to 75-80 ° C., and then completely dissolved.

2) Titanium oxide was dispersed for 5 minutes while stirring the oil phase component of 1) at 7000 rpm using a homogenizer.

3) The aqueous phase components were mixed and dissolved, and then heated to 70 ° C.

4) While the oil phase component of 2) was stirred at 7000 rpm using a homogenizer, the water phase component of 3) was gradually added to emulsify, and the temperature was maintained at 70 ° C.

5) After the addition of the aqueous phase component was continued stirring for 3-5 minutes and then degassed and poured into a container to cool to 30 ℃ to complete the solid (cake) oil-in-water sunscreen.

[Test Example 2] Volatilization Stability of Solid (Cake) Oil-in-water Sunscreen According to the Composition of Surfactant

In the same manner as in Test Example 1, the volatilization stability of the solid (cake) oil-in-water sunscreens prepared in Examples 4 to 6 and Comparative Examples 5 to 8 was evaluated, and the results are shown in Table 4.

Storage temperature (℃)
(without cap) Volatility Stability
(Shrink / split surface) 1 week 2 weeks 3 weeks Example 4 30 2 3.8 5.1 Good 45 7.8 12.9 18.4 Good Example 5 30 2.1 3.24 6.43 Good 45 7.5 13.1 17.3 Good Example 6 30 1.2 2.1 3.4 Good 45 6.4 12.3 19.8 Good Comparative Example 5 30 9.7 18.4 35.89 Shrink 45 34.1 56.7 76.2 Contraction / Crack Comparative Example 6 30 7.5 13.5 29.8 Shrink 45 19.0 39.3 69.0 Contraction / Crack Comparative Example 7 30 3.3 9.77 21.4 Good 45 8.3 22.88 35.1 Shrink Comparative Example 8 30 15.99 38.09 63.28 Contraction / Crack 45 30.1 58.8 88.4 Contraction / Crack

As shown in the results of Table 4 above, even in the case of the solid (cake) oil-in-water sunscreen, polyoxyalkylene addition organopolysilonic acid containing lauryl Fiji-9 polydimethylsiloxyethyldimethicone and hydrophobic thereof It was found that Examples 4 to 6 contained together with the surfactant had an excellent effect of preventing shrinkage and surface cracking compared to the Comparative Examples.

Example 7 and Comparative Examples 9 to 10

To prepare a solid (cake) oil-in-water sunscreen of Example 7 and Comparative Examples 9 to 10 according to the composition shown in Table 5.

division Compounding Ingredients (wt%) Example 7 Comparative Example 9 Comparative Example 10 Paid
ingredient Decamethylcyclopentasiloxane 30 30 30 Ozokerite 3 3 3 Carnauba Wax 3 3 3 Dimethicone 3 3 3 Hexyllaurate 2 2 2 Polyoxyalkylene addition organopolysiloxane including lauryl fig-9 polydimethylsiloxyethyldimethicone 2 - - Cetyl Fiji / Fiji -10/1 dimethicone - 2 - Sorbitan isostearate - - 2 Dicaprylylcarbonate 4 4 4 Dimethicone / Dimethicone Vinyl Dimethicone Crosspolymer 5 5 5 powder Titanium oxide 7 7 7 Ferric oxide 0.2 0.2 0.2 Hydrated ferric oxide 1.3 1.3 1.3 Silica 5 5 5 Awards
ingredient Purified water Balance Balance Balance glycerin 2 2 2 Butylene glycol 5 5 5

<Manufacturing Method>

1) The oily ingredients except for the sunscreen were mixed and warmed to 75-80 ° C., and then completely dissolved.

2) The powder component was dispersed for 5 minutes while stirring the oil phase component of 1) at 7000 rpm using a homogenizer.

3) The aqueous phase components were mixed and dissolved, and then heated to 70 ° C.

4) While the oil phase component of 2) was stirred at 7000 rpm using a homogenizer, the water phase component of 3) was gradually added to emulsify, and the temperature was maintained at 70 ° C.

5) After the addition of the aqueous phase component was continued stirring for 3-5 minutes and then degassed and poured into a container to cool to 30 ℃ to complete the solid (cake) oil-in-water sunscreen.

[Test Example 3] Volatilization Stability of Solid (Cake) Oil-in-water Sunscreen According to the Composition of Surfactant

The volatilization stability of the solid (cake) oil-in-water type sunscreen prepared in Example 7 and Comparative Examples 9 to 10 was evaluated in the same manner as in Test Example 1, and the results are shown in Table 6.

Storage temperature (℃)
(without cap) Volatility Stability
(Shrink / split surface) 1 week 2 weeks 3 weeks Example 7 30 0.2 0.78 1.48 Good 45 1.12 1.8 3.7 Good Comparative Example 9 30 5.9 17.4 35.89 Shrink 45 14.1 36.7 54.2 Contraction / Crack Comparative Example 10 30 6.5 17.5 31.8 Shrink 45 18.3 29.9 57.4 Contraction / Crack

As shown in the results of Table 6, Example 7 according to the present invention was found to have an excellent effect of preventing the shrinkage or surface cracking compared to the comparative examples.

Example 8 and Comparative Example 11

To prepare a solid (cake) oil-in-water emulsion of Example 8 and Comparative Example 11 in the same manner as in Example 1 according to the composition shown in Table 7.

division Compounding Ingredients (wt%) Example 8 Comparative Example 11 Paid
ingredient Decamethylcyclopentasiloxane 15 5 Ceresin 3 - Candelilla wax 3 - Butylene glycol dicaprylate dicaprate 5 5 Cetyloctanoate 5 5 Meadowfoam Seed Oil 5 5 Squalene 5 5 Polyoxyalkylene addition organopolysiloxane including lauryl fig-9 polydimethylsiloxyethyldimethicone 2 - Cetyl Fiji / Fiji -10/1 dimethicone - 1.5 Sorbitan sesquioleate - 0.5 Awards
ingredient Purified water Balance Balance glycerin 5 5 Butylene glycol 5 5

Test Example 4 Skin Moisturizing Effect of Solid (Cake) Oil-in-water Emulsion

In order to investigate the skin moisturizing effect of the solid (cake) oil-in-water emulsion according to the present invention, 50 adults and men and women in their 20s and 30s who complain of dryness or dry skin are prepared in Example 8 and Comparative Example 11 After applying one cosmetic composition to the inside of the face and forearm, the skin moisture content was measured using a corneometer (CM820 courage Khazaka electronic GmbH, Germany) for 24 hours. The skin moisture content was measured using a conniometer at a constant temperature and humidity condition (24 ° C. and 40% humidity) before application, and the change was measured after 12 hours and 24 hours, and the results are shown in Table 8 below. Shown in

[Measurement of Koniometer]

Principle: The moisture level was measured by measuring the amount of moisture in the skin's epidermis using a sensor and quantifying the amount of moisture.

1) The probe of the Koniometer was placed on the skin area to be measured.

2) When the probe is pressed on the skin, the electrical conductivity of the skin is quantified through the sensor and displayed on the screen.

3) Repeated measurements were made with different measurement sites.

4) After measuring once, wipe the sensor with a tissue such as Kimwipe and measure again.

Skin moisture content (%) of solid (cake) oil-in-water emulsions and ordinary oil-in-water emulsions over time sample Before application 12 hours later 24 hours later Example 8 26 48 45 Comparative Example 11 26 26 27

In the results of Table 8, in the solid (cake) oil-in-water emulsion according to the present invention, it was confirmed that the moisturizing power lasts more than 24 hours and the skin moisture content increase effect is also very good.

In addition, when using the Example 8 and Comparative Example 11, the questionnaire for the freshness, moisture and moisturizing feeling was conducted to the test subjects at the end of the test. The survey was to display the satisfaction with the degree of freshness, moisture and moisturizing very good, good, moderate and poor, and the results are shown in Table 9 below.

Usability (freshness, moisture, moisture) questionnaire sample Respondents Very good Good usually Inadequate Example 8 Freshness 16 25 7 2 Moisture 6 26 18 0 Moisturizing 24 21 5 0 Comparative Example 11 Freshness 8 18 24 0 Moisture 5 29 14 2 Moisturizing 10 11 27 2

In the results of Table 9, it was found that the solid (cake) oil-in-water emulsion according to the present invention has superior moisture retention compared to general oil-in-water emulsions, and has excellent usability in terms of freshness and moisture.

Claims (7)

A solid oil-in-water cosmetic composition represented by the following formula (1) as a surfactant and containing a polyoxyalkylene addition organopolysiloxane comprising lauryl fig-9 polydimethylsiloxyethyldimethicone: [Formula 1]

The solid oil-in-water cosmetic composition according to claim 1, wherein the composition further comprises a hydrophobic surfactant selected from the group consisting of sorbitan sesquioleate, sorbitan isostearate and sorbitan sesquiisostearate. . The method of claim 2, wherein the mixing ratio of the polyoxyalkylene addition organopolysiloxane and the hydrophobic surfactant including the lauryl fig-9 polydimethylsiloxyethyldimethicone is 0.1: 1 to 1: 0.1 by weight. Solid oil-in-water cosmetic composition. The oil-in-water cosmetic composition according to claim 1, further comprising 5 to 80 parts by weight of oil, 2 to 20 parts by weight of solid wax, 0 to 50 parts by weight of cosmetic powder and water. Composition. The method of claim 4, wherein the oil comprises: a volatile silicone oil comprising octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane; Nonvolatile silicone oils including dimethicone and polypetrinylmethicone; Hydrocarbon-based oils including squalane, liquid paraffin, and hydrogenated C6-14 olefin polymers; Higher fatty acids; Higher fatty acid esters including butyleneglycoldicaprylate-dicaprate, C14-18 alkylethylhexanoate, dicaprylylcarbonate, cetyloctanoate and octyldodecyl myristate; Higher alcohols; Vegetable oils including meadowfoam seed oil, olive oil and jojoba oil; And a sunscreen oil comprising ethylhexylmethoxycinnamate, octylsalicylate, ethylhexyltriazine, and bis-ethylhexyloxyphenol methoxyphenyltriazine. The method of claim 4, wherein the solid wax is a petroleum wax including paraffin wax and microcrystalline wax; Mineral waxes including ozokerite and ceresin; Solid oil-in-water cosmetic composition, characterized in that selected from the group consisting of natural wax including carnauba wax and candelilla wax. The method of claim 4, wherein the cosmetic powder is selected from the group consisting of talc, mica, sericite, silica, polymethylmethacrylate, nylon, synthetic mica, titanium dioxide, zinc oxide and titanated mica. Solid oil-in-water cosmetic composition.