High-power sunscreen lotion and preparation method thereof
By using a silicone oil-in-water emulsion formula and a three-dimensional network sunscreen film technology, the problems of heavy skin feel and sun protection gaps in sunscreen products have been solved, achieving a highly efficient and even sun protection effect and a lightweight and easy-to-apply user experience.
Patent Information
- Application Number
- CN202511761035.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-26
- Publication Date
- 2026-02-06
AI Technical Summary
Existing sunscreen products often feel sticky and heavy on the skin, leading consumers to apply insufficient amounts, resulting in substandard sun protection. Furthermore, the addition of powder can create gaps in sun protection.
It adopts a silicone oil-in-water emulsion formulation, which contains a continuous oil phase, a dispersed aqueous phase and a solid phase component to form a three-dimensional network sunscreen film. It uses porous silica to load chemical sunscreen agents and silane film-forming polymers, combined with silicone-surfaced physical sunscreen agents to ensure uniform distribution and water resistance.
With a thin application amount (1mg/cm2), the SPF value is not less than 50, achieving efficient and uniform UVA/UVB protection, avoiding sun protection gaps, and possessing a lightweight and easy-to-spread skin feel, as well as sweat and water resistance.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of cosmetics, in particular, to a high-fold sunscreen cream and a preparation method thereof. BACKGROUND
[0002] At present, the demand of consumers for sunscreen products is changing from single sunscreen function to multi-effect skin care, scene segmentation and safety upgrade, especially the demand for high-fold sunscreen products with light and thin skin feel is increasing.
[0003] The regulations in China stipulate that the UVB sunscreen index of sunscreen products can only be marked as SPF50+. Due to the regulations in human sunscreen test, the application amount is (2.00±0.05) mg / cm 2 Under such circumstances, the sunscreen product has a sticky, heavy and thick skin feel. Therefore, in the actual use of sunscreen products, the actual application thickness of consumers is probably small, which results in insufficient sunscreen protection effect. SUMMARY
[0004] The purpose of the embodiments of the present application is to provide a high-fold sunscreen cream and a preparation method thereof.
[0005] In a first aspect, the present application provides a high-fold sunscreen cream, which is a water-in-silicone emulsion; the high-fold sunscreen cream comprises: a continuous oil phase, a dispersed water phase, a solid phase component and a film former; the mass ratio of the water phase to the oil phase is 1:10-1:1; The continuous oil phase comprises silicone oil and a chemical sunscreen agent, the chemical sunscreen agent includes an oil-soluble chemical sunscreen agent; the dispersed water phase comprises water and a water-soluble chemical sunscreen agent; the solid phase component is dispersed in the continuous oil phase; the solid phase component includes a silicon surface treated physical sunscreen agent and a powder composite sunscreen agent; the powder composite sunscreen agent is a composite particle in which a chemical sunscreen agent is loaded on porous silica; and the film former is a silane film forming polymer dissolved or swollen in the continuous oil phase; The film former, the continuous oil phase and the solid phase component together form a three-dimensional network, so that a continuous, uniform and water-resistant sunscreen film can be formed on the skin surface after application and drying; and when the application amount of the sunscreen cream is 1 mg / cm 2 , the in vitro SPF value is not less than 50.
[0006] The above technical solution, the film forming agent, the continuous oil phase, and the solid phase component together form a three-dimensional network, so that after being applied and dried, a continuous, uniform, and water-resistant sunscreen film can be formed on the skin surface; it can ensure that the sunscreen is evenly distributed on the skin surface, avoiding the local protection weakness (i.e., "sunscreen leaks") caused by the agglomeration or uneven dispersion of traditional formulations. By using porous silica loaded with chemical sunscreen composite particles, the powder that was traditionally only used to improve skin feel and could become a "leak" is transformed into an active ingredient that has both sunscreen function and improves the smoothness of the application. The water-in-silicone emulsion itself has the characteristics of a smooth and breathable skin feel. The combination of the silicone system and the composite powder improves the smooth and easy-to-push texture of the product, solves the technical problem of "high SPF thick and sticky", so that the sunscreen emulsion has an in vitro SPF value of not less than 50 when the application amount is 1 mg / cm 2 .
[0007] Further, the chemical sunscreen in the oil phase covers a specific wave band, the chemical sunscreen in the water phase supplements the coverage, and the physical sunscreen provides broad-spectrum UVA / UVB protection and scattering. The powder composite sunscreen further supplements and enhances. This design of the synergistic cooperation of the oil phase, the water phase, and the solid phase ensures seamless coverage of the UVA and UVB wave bands, and the protection effect is more comprehensive and reliable.
[0008] Further, the mass ratio of the water phase to the oil phase is 1:10 to 1:1; a water-in-oil system can be formed. Further, the three-dimensional network formed by the film forming agent, the continuous oil phase, and the solid phase component also helps the long-term stable suspension of the solid phase component.
[0009] Using silicon-treated nano-zinc oxide and silicon-treated nano-titanium dioxide has better sunscreen effect, and forms mutual supplementation of the sunscreen range with the chemical sunscreen, and using cyclopentasiloxane as a dispersant for such silicon-treated powder or composite powder is more conducive to the dispersion of the powder in the system, and better sunscreen effect can be achieved.
[0010] In other embodiments of the present application, the above-mentioned silicon surface-treated physical sunscreen includes at least one of silicon-treated nano-zinc oxide and silicon-treated nano-titanium dioxide.
[0011] In other embodiments of the present application, in the powder composite sunscreen, the porous silica loaded chemical sunscreen includes methoxy cinnamic acid ethylhexyl ester.
[0012] In other embodiments of the present application, the silane film forming polymer includes trimethylsiloxysilicate.
[0013] In other embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least one of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, oxybenzone, or bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0014] In other embodiments of the present application, the water-soluble chemical sunscreen agent includes phenyl benzimidazole sulfonic acid.
[0015] In a second aspect, the present application provides a method for preparing a high-multiplying sunscreen cream, comprising: mixing the silicone oil, the oil-soluble chemical sunscreen agent, the silicone surface-treated physical sunscreen agent, and the film-forming agent, heating and homogeneously dispersing to obtain a uniform continuous oil phase premix; mixing the water, the water-soluble chemical sunscreen agent, and the pH adjusting agent, completely dissolving and adjusting the pH to 7.5-7.8 to obtain an aqueous phase premix; under stirring, slowly adding the aqueous phase premix to the continuous oil phase premix to perform homogenization emulsification to form a primary emulsion; adding the powder composite sunscreen agent to the primary emulsion, stirring and homogeneously dispersing to uniformly disperse in the emulsion.
[0016] In other embodiments of the present application, the preparation of the continuous oil phase premix includes: first premixing the silicone surface-treated physical sunscreen agent with part of the silicone oil and the dispersing agent, homogeneously activating, and then combining with other oil phase components.
[0017] In other embodiments of the present application, the speed of homogenization is 3000 rpm-5000 rpm, and the time is 3-10 minutes.
[0018] In other embodiments of the present application, the temperature when the aqueous phase is added to the oil phase is 70°C-80°C.
[0019] In other embodiments of the present application, the temperature of the material body is reduced to below 40°C when the powder composite sunscreen agent is added.
[0020] In other embodiments of the present application, the pH adjusting agent includes aminomethyl propanol.
[0021] In other embodiments of the present application, the following raw materials are included in the mass percentage: Triethoxycaprylylsilane surface treated nano zinc oxide: 6-12%; cyclopentasiloxane: 10-15%; polyglyceryl-3 polydimethylsiloxyethyl dimethicone: 0.1-2%; cetyl PEG / PPG-10 / 1 dimethicone: 2-4%; sorbitan olivate: 0.1-3%; film forming agent: 1-5%; hydrogenated polydimethylsiloxane surface treated nano titanium dioxide: 1-5%; isododecane: 2-6%; disteardimonium hectorite: 0.1-1%; dibutyl adipate: 2-10%; tocopheryl acetate: 0.1-0.5%; farnesol: 0.1-0.5%; methoxycinnamic acid ethylhexyl ester: 5-9%; ethylhexyl salicylate: 2-5%; homosalate: 1-5%; ethylhexyl triazone: 1-5%; diethylamino hydroxybenzoyl hexyl benzoate: 3-8%; bis-ethylhexyloxyphenol methoxyphenyl triazine: 1-5%; phenylbenzimidazole sulfonic acid: 0.1-5%; amino methyl propanol: 0.1-1.67%; powder composite sunscreen: 1-10%; balance water. DETAILED DESCRIPTION
[0022] In order to make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments of the present application.
[0023] Therefore, the following detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but merely represents the selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative work fall within the scope of protection of the present application.
[0024] In conventional sunscreen products, the addition amount of sunscreen is generally large, which makes the product feel oily, thick, and not easy to apply. Therefore, adding various powders to improve the application feeling of the product is a common choice for many sunscreen products. However, the addition of powders also causes a sunscreen gap, especially in the case of thin application, the powder is neither an internal phase nor an external phase, and does not have sunscreen performance, so the point sunscreen performance of the powder is insufficient.
[0025] Based on the above research, the embodiments of the present application provide a high-fold sunscreen cream, which is a water-in-silicon emulsion; the high-fold sunscreen cream comprises: a continuous oil phase, a dispersed water phase, a solid phase component, and a film forming agent; the mass ratio of the water phase to the oil phase is 1:10~1:1; The continuous oil phase comprises silicone oil and chemical sunscreen agents, the chemical sunscreen agents including oil-soluble chemical sunscreen agents; the dispersed water phase comprises water and water-soluble chemical sunscreen agents; the solid phase component is dispersed in the continuous oil phase; the solid phase component comprises a physical sunscreen agent with a silicon surface treatment, and a powder composite sunscreen agent; the powder composite sunscreen agent is a composite particle in which a porous silica is loaded with a chemical sunscreen agent; and the film-forming agent is a silane film-forming polymer that is dissolved or swelled in the continuous oil phase; The film-forming agent, the continuous oil phase and the solid phase component together form a three-dimensional network, so that after being applied and dried, a continuous, uniform and water-resistant sunscreen film is formed on the surface of the skin; and the sunscreen cream has an in-vitro SPF value of not less than 50 when the application amount is 1 mg / cm 2 .
[0026] In the above technical solution, the outer phase (oil phase) and the inner phase (water phase) cover the sunscreen. In the high-multiplying sunscreen cream of the present application, the powder composite sunscreen agent not only improves the application performance of the product, but also realizes the gap sunscreen coverage between the powders, so that the often neglected sunscreen gaps in the sunscreen product are filled, and the sunscreen performance is greatly improved. The silane film-forming polymer film-forming agent has good affinity for silica; it also has good affinity for the physical sunscreen agent with a silicon surface treatment, so that the above-mentioned chemical sunscreen agent, the physical sunscreen agent with a silicon surface treatment and the silicon powder composite sunscreen agent are better applied to the skin, realizing thin application and uniform coverage of the skin, realizing waterproof and sweat-resistant sunscreen while thin application and high-efficiency sunscreen. The selection of the powder composite sunscreen agent also improves the smoothness of the material and the application performance of the material, and also has the effect of filling fine lines and lightening fine lines.
[0027] Under the condition of thin application of 1.0 mg / cm 2 , which is much lower than the national standard test amount (2.0 mg / cm 2 ), the in-vitro SPF value is still not less than 50. The problem of sharp decline in sunscreen effect caused by insufficient actual application amount due to sticky skin feel of the consumer is effectively solved.
[0028] Further, the film-forming agent, the continuous oil phase, and the solid phase component together form a three-dimensional network, so that after being applied and dried, a continuous, uniform, and water-resistant sunscreen film can be formed on the surface of the skin; it can ensure that the sunscreen is evenly distributed on the surface of the skin, avoiding the local protection weakness (i.e., "sunscreen leaks") caused by the traditional formula due to the agglomeration or uneven dispersion of the powder. The essence of the water-in-silicone emulsion and the cross-linking and curing of the silane film-forming polymer make the sunscreen film have excellent resistance to sweat and water flushing, suitable for outdoor and sports scenes. By using composite particles of porous silica loaded with chemical sunscreen, the powder that may only improve skin feel in the traditional formula is transformed into an active ingredient that has both sunscreen function and improves the smoothness of application. The water-in-silicone emulsion itself has the characteristics of refreshing skin feel and good breathability. The combination of the silicone system and the composite powder improves the smooth and easy-to-push texture of the product, solving the technical problem of "high SPF sunscreen thickness, heavy and sticky".
[0029] Further, the chemical sunscreen in the oil phase covers a specific waveband, the chemical sunscreen in the water phase supplements the coverage, and the physical sunscreen provides broad-spectrum UVA / UVB protection and scattering. The powder composite sunscreen further supplements and enhances. This design of the synergistic cooperation of the oil phase, the water phase, and the solid phase ensures seamless coverage of the UVA and UVB wavebands, and the protection effect is more comprehensive and reliable.
[0030] The mass ratio of the water phase to the oil phase is 1:10 to 1:1, which can form a water-in-silicone shake emulsion type. Further, the three-dimensional network formed by the film-forming agent, the continuous oil phase, and the solid phase component also helps the long-term stable suspension of the solid phase component.
[0031] Further optionally, in some embodiments of the present application, the mass ratio of the water phase to the oil phase is 1:10, 1:9, 1:8, 1:7, 1:6, 1:5, 1:4, 1:3, 1:2, 1:1, or a range between any two of the foregoing values.
[0032] Further optionally, in some embodiments of the present application, the mass ratio of the water phase to the oil phase is 1:9 to 1:1; further optionally, in some embodiments of the present application, the mass ratio of the water phase to the oil phase is 1:8 to 1:1; further optionally, in some embodiments of the present application, the mass ratio of the water phase to the oil phase is 1:7 to 1:1; further optionally, in some embodiments of the present application, the mass ratio of the water phase to the oil phase is 1:5 to 1:1.
[0033] Further optionally, for example, in some embodiments of the present application, the sunscreen emulsion has an in vitro SPF value of 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, or a range between any two of the foregoing values, when the application amount is 1 mg / cm 2
[0034] Further, in some embodiments of the present application, the physical sunscreen agent with a silicon surface treatment includes at least one of a triethoxycaprylylsilane surface-treated nano-zinc oxide or a hydrogenated polydimethylsiloxane surface-treated nano-titanium dioxide.
[0035] Illustratively, in some embodiments of the present application, the physical sunscreen agent with a silicon surface treatment is any one of a triethoxycaprylylsilane surface-treated nano-zinc oxide or a hydrogenated polydimethylsiloxane surface-treated nano-titanium dioxide. Alternatively, in some embodiments of the present application, the physical sunscreen agent with a silicon surface treatment is a mixture of a triethoxycaprylylsilane surface-treated nano-zinc oxide and a hydrogenated polydimethylsiloxane surface-treated nano-titanium dioxide; optionally, in some embodiments of the present application, the mixture can include the respective ingredients in any ratio.
[0036] Further, in some embodiments of the present application, the chemical sunscreen agent loaded on porous silica in the powder composite sunscreen agent includes at least one of ethylhexyl methoxy cinnamate.
[0037] Further, in some embodiments of the present application, the silane-based film-forming polymer includes trimethylsiloxysilicate.
[0038] Further, in some embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least one of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, dioxybenzone, or bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0039] Illustratively, in some embodiments of the present application, the oil-soluble chemical sunscreen agent is any one of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, dioxybenzone, or bis-ethylhexyloxyphenol methoxyphenyl triazine. Alternatively, in some embodiments of the present application, the oil-soluble chemical sunscreen agent is a mixture of ethylhexyl methoxy cinnamate and ethylhexyl salicylate; alternatively, in some embodiments of the present application, the oil-soluble chemical sunscreen agent is a mixture of homosalate and ethylhexyl triazone; alternatively, in some embodiments of the present application, the oil-soluble chemical sunscreen agent is a mixture of dioxybenzone and bis-ethylhexyloxyphenol methoxyphenyl triazine. The respective ingredients in each of the above mixtures can be mixed in any ratio.
[0040] Further optionally, in some embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least two of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, dioxybenzone, or bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0041] Further optionally, in some embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least three of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, dioxybenzone, or bis-ethylhexyloxyphenol methoxyphenol triazine.
[0042] Further optionally, in some embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least four of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, dioxybenzone, or bis-ethylhexyloxyphenol methoxyphenol triazine.
[0043] Further optionally, in some embodiments of the present application, the water-soluble chemical sunscreen agent includes phenyl benzimidazole sulfonic acid.
[0044] Some embodiments of the present application provide a method for preparing a high-multiple sunscreen cream, comprising: mixing the silicone oil, the oil-soluble chemical sunscreen agent, the silicone surface-treated physical sunscreen agent, and the film-forming agent, heating and homogeneously dispersing to obtain a uniform continuous oil phase premix; mixing the water, the water-soluble chemical sunscreen agent, and the pH adjusting agent, completely dissolving and adjusting the pH to 7.5-7.8 to obtain an aqueous phase premix; slowly adding the aqueous phase premix to the continuous oil phase premix under stirring to perform homogenization emulsification to form a primary emulsion; adding the powder composite sunscreen agent to the primary emulsion, stirring and homogeneously dispersing to uniformly disperse in the emulsion.
[0045] In the above technical solution, the aqueous phase is slowly added to the oil phase for emulsification to obtain a water-in-oil emulsion, which has excellent water resistance. The high-multiple sunscreen cream obtained by the present application has a "silicone oil-in-water shake shake emulsion dosage form".
[0046] Further optionally, for example, in some embodiments of the present application, the above mixing the water, the water-soluble chemical sunscreen agent, and the pH adjusting agent, completely dissolving and adjusting the pH to 7.5, 7.6, 7.7, 7.8, or a range between any two of the foregoing values to obtain an aqueous phase premix.
[0047] Further, in some embodiments of the present application, the method for preparing a high-multiple sunscreen cream comprises the following steps: Step S1, preparing a continuous oil phase premix.
[0048] Further, in some embodiments of the present application, the step of preparing a continuous oil phase premix comprises: The silicone oil, the oil-soluble chemical sunscreen agent, the physical sunscreen agent of silicon surface treatment, and the film forming agent are mixed, heated and homogeneously dispersed to obtain a uniform continuous oil phase premix.
[0049] Further optionally, in some embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least one of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, DEA-methoxy cinnamate, or bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0050] Further optionally, in some embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least two of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, DEA-methoxy cinnamate, or bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0051] Further optionally, in some embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least three of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, DEA-methoxy cinnamate, or bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0052] Further optionally, in some embodiments of the present application, the oil-soluble chemical sunscreen agent includes at least four of ethylhexyl methoxy cinnamate, ethylhexyl salicylate, homosalate, ethylhexyl triazone, DEA-methoxy cinnamate, or bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0053] Exemplarily, in some embodiments of the present application, the high SPF sunscreen cream includes, in percentage by mass, ethylhexyl methoxy cinnamate: 5-9%; ethylhexyl salicylate: 2-5%; homosalate: 1-5%; ethylhexyl triazone: 1-5%; DEA-methoxy cinnamate: 3-8%; and bis-ethylhexyloxyphenol methoxyphenyl triazine: 1-5%.
[0054] Exemplarily, in some embodiments of the present application, the high-factor sunscreen cream comprises, in percentage by mass: ethylhexyl methoxy cinnamate: 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, or a range between any two of the numbers; ethylhexyl salicylate: 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or a range between any two of the numbers; homosalate: 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or a range between any two of the numbers; ethylhexyl triazone: 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or a range between any two of the numbers; oxybenzone: 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, or a range between any two of the numbers; bis-ethylhexyloxyphenol methoxyphenyl triazine: 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or a range between any two of the numbers.
[0055] Further optionally, in some embodiments of the present application, the silicone oil described above comprises: a silicone oil and an auxiliary solvent.
[0056] Further optionally, in some embodiments of the present application, the silicone oil described above comprises: cyclopentasiloxane.
[0057] Further optionally, in some embodiments of the present application, the silicone oil described above is added in an amount of 10%-15% by mass. Exemplarily, in some embodiments of the present application, the silicone oil described above is added in an amount of 10%, 11%, 12%, 13%, 14%, 14.5%, 15%, or a range between any two of the numbers.
[0058] Further optionally, in some embodiments of the present application, the auxiliary solvent described above comprises: isododecane.
[0059] Further optionally, in some embodiments of the present application, the isododecane described above is added in an amount of 2%-6% by mass. Exemplarily, in some embodiments of the present application, the isododecane described above is added in an amount of 2%, 3%, 4%, 5%, 5.5%, 6%, or a range between any two of the numbers.
[0060] Further optionally, in some embodiments of the present application, the physical sunscreen agent with a silicon surface treatment described above comprises: at least one of a triethoxysilane surface-treated nano-zinc oxide, a dimethicone surface-treated nano-titanium dioxide.
[0061] Exemplarily, in some embodiments of the present application, the high SPF sunscreen cream comprises, in percentage by mass, 6-12% of triethoxysilane surface-treated nano zinc oxide; 1-5% of hydrogenated polydimethylsiloxane surface-treated nano titanium dioxide. Exemplarily, the high SPF sunscreen cream comprises, in percentage by mass, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, or a range between any two of the aforementioned values, of triethoxysilane surface-treated nano zinc oxide; 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or a range between any two of the aforementioned values, of hydrogenated polydimethylsiloxane surface-treated nano titanium dioxide.
[0062] Further optionally, in some embodiments of the present application, the film-forming agent comprises: a silane film-forming polymer. Exemplarily, the film-forming agent comprises: trimethylsiloxysilicate.
[0063] Further optionally, in some embodiments of the present application, the film-forming agent comprises: a solvent; optionally, exemplarily, in some embodiments of the present application, the film-forming agent comprises: a mixture of cyclotetrasiloxane and trimethylsiloxysilicate, each of the raw materials in the mixture can be mixed in a 1:1 ratio.
[0064] Further optionally, in some embodiments of the present application, the high SPF sunscreen cream comprises, in percentage by mass, 1%-5% of a mixture of cyclotetrasiloxane and trimethylsiloxysilicate; exemplarily, the high SPF sunscreen cream comprises, in percentage by mass, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or a range between any two of the aforementioned values, of the mixture of cyclotetrasiloxane and trimethylsiloxysilicate.
[0065] Further optionally, in some embodiments of the present application, the preparation of the continuous oil phase premix comprises: first premixing the silicon surface-treated physical sunscreen agent with part of the silicone oil and the dispersant, and then combining with other oil phase components after high-shear homogenization activation.
[0066] Further optionally, exemplarily, the aforementioned dispersant comprises: polyglyceryl-3 polydimethylsiloxyethyl dimethicone.
[0067] Further optionally, the aforementioned dispersant is added in an amount of 0.1%-2% in percentage by mass; exemplarily, the aforementioned dispersant is added in an amount of 0.1%, 0.11%, 0.12%, 0.15%, 0.16%, 0.18%, 2%, or a range between any two of the aforementioned values, in percentage by mass.
[0068] Further optionally, after high shear homogenization activation, the homogenization speed is 3000 rpm-5000 rpm, and the time is 3-10 minutes; for example, the homogenization speed is 3000 rpm, 3200 rpm, 3500 rpm, 3800 rpm, 4000 rpm, 3200 rpm, 3500 rpm, 3800 rpm, 5000 rpm, or a range between any two of the foregoing values, and the time is 3, 4, 5, 6, 7, 8, 9, 10 minutes.
[0069] Step S2, preparing an aqueous phase premix.
[0070] Further optionally, in some embodiments of the present application, water, water-soluble chemical sunscreen, and pH adjuster are mixed, completely dissolved, and adjusted to a pH of 7.5-7.8 to obtain an aqueous phase premix.
[0071] For example, in some embodiments of the present application, the water-soluble chemical sunscreen includes phenyl benzimidazole sulfonic acid.
[0072] Further optionally, in some embodiments of the present application, the high-factor sunscreen cream includes 1%-5% phenyl benzimidazole sulfonic acid by mass percentage. For example, the high-factor sunscreen cream includes 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or a range between any two of the foregoing values, of phenyl benzimidazole sulfonic acid by mass percentage.
[0073] Further optionally, in some embodiments of the present application, the pH adjuster includes aminomethyl propanol.
[0074] Further optionally, in some embodiments of the present application, the aminomethyl propanol is added in an amount of 0.1%-1.67% by mass percentage.
[0075] Further optionally, in some embodiments of the present application, the mass ratio of phenyl benzimidazole sulfonic acid to aminomethyl propanol is 3:1.
[0076] For example, the mass ratio of phenyl benzimidazole sulfonic acid to aminomethyl propanol is 3:1, 2:1, 1:1, 1:2, 1:3, or a range between any two of the foregoing values.
[0077] In the above technical solution, by controlling the aminomethyl propanol to be added in an amount of 0.1%-1.67% by mass percentage, the pH of the system can be ensured to be in a range of 7.5-7.8.
[0078] Step S3, mixing.
[0079] Further optionally, in some embodiments of the present application, the aqueous phase premix is slowly added to the continuous oil phase premix under stirring to perform homogenization emulsification to form a primary emulsion. Further optionally, in some embodiments of the present application, the temperature when the aqueous phase is added to the oil phase is 70-80°C; for example, the temperature when the aqueous phase is added to the oil phase is 70°C, 71°C, 72°C, 73°C, 74°C, 75°C, 76°C, 77°C, 78°C, 79°C, 80°C, or a range between any two of the aforementioned values.
[0080] Step S4, compounding.
[0081] Further optionally, in some embodiments of the present application, the powder composite sunscreen is added to the colostrum, stirred and homogeneously dispersed, so as to be uniformly dispersed in the emulsion.
[0082] Further optionally, in some embodiments of the present application, the powder composite sunscreen is a composite particle of porous silica loaded with a chemical sunscreen; further optionally, in some embodiments of the present application, the chemical sunscreen loaded by the porous silica in the powder composite sunscreen includes ethylhexyl methoxy cinnamate.
[0083] Further optionally, in some embodiments of the present application, the addition amount of silica / ethylhexyl methoxy cinnamate is 1-10% by mass percentage. For example, in some embodiments of the present application, the addition amount of silica / ethylhexyl methoxy cinnamate is 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, or a range between any two of the aforementioned values.
[0084] Further optionally, in some embodiments of the present application, the temperature of the material body is reduced to below 40°C when the powder composite sunscreen is added.
[0085] For example, the temperature of the material body is reduced to 40°C, 39°C, 38°C, 35°C, 32°C, 30°C, or a range between any two of the aforementioned values when the powder composite sunscreen is added.
[0086] The present application contains physical sunscreens, chemical sunscreens, and powder composite sunscreens. The optimized combination of sunscreens used in the present application covers the protection range of UVA and UVB bands. The present application realizes the improvement of sunscreen performance by the selection of silicon-based film-forming agents and composite powders. The sunscreen cream of the present application has the skin feel of lightness, thinness, and easy application, and the effect of high sunscreen. Even in the case of thin application, it still has a high sunscreen effect.
[0087] The features and performance of the present application are further described in detail below in conjunction with examples: A high sunscreen cream is provided, and the compositions of various embodiments and comparative examples are shown in Table 1 below: Table 1 (wt%)
[0088] The preparation method of each example, comparative sample in the above table is as follows: Manufacturing process: (1) Homogeneously disperse 1, 2, 3, 4, 5, 6, 7, 8, 10 in the emulsifying pot, and activate for later use; the homogenization speed is 3000 rpm; (2) Add 11, 12, 13, 14, 15, 16, 17, 18, 19 into the emulsifying pot, and heat to completely dissolve; (3) Dissolve 20, 21, 22 completely, and adjust the pH to 7.5-7.8 for later use; (4) Add 1-10 into the emulsifying pot, and homogeneously disperse; the homogenization speed is 3000 rpm; (5) Slowly add 20-22 into the emulsifying pot under stirring, homogenize and emulsify, and cool down; the temperature is reduced below 40℃; the homogenization speed is 400 rpm; (6) Add 23, 25 into the emulsifying pot, stir and homogeneously disperse; the homogenization speed is 3000 rpm; (7) Take samples, and discharge after passing the inspection.
[0089] The performance of the sunscreen cream prepared in each example and comparative example is tested: I. Sunscreen performance test The test method is as follows: 1. Sample plate preparation 1.1 Prepare several PMMA plates (≥4 pieces), with an area of 25 cm 2 One of them is a blank plate, and the rest are sample plates.
[0090] 1.2 Use a balance with an accuracy of 0.0001 to weigh the test sample on the sample plate, and disperse 0.025±0.0005 grams, corresponding to a thickness of 1 mg / cm 2 .
[0091] 1.3 Wear rubber gloves, pre-soak, and evenly apply the sample plate within a short period of time.
[0092] 1.4 Place the evenly coated sample sheet in a dark place and dry for 15-20 minutes.
[0093] 1.5 Open the software operation shortcut key, and the interface shows CONNECT in the lower bar, indicating that the software can be used.
[0094] 2. Method selection 2.1 Select Study on the interface, then click Method.
[0095] 2.2 Select Method for testing.
[0096] 2.3 Test parameter settings 2.3.1 Select the number of plates required for testing.
[0097] 2.3.2 Select the number of locations per plate.
[0098] 2.3.3 Select the number of blank scans.
[0099] 2.3.4 Leave other fields blank, and click OK.
[0100] 2.4 Blank scan Click the button in the middle of the interface, and follow the English prompts to perform a blank scan. First, scan the blank PMMA plate without sample, and set the initial scan number as the default blank value.
[0101] 2.5 Sample scan 2.5.1 Place the sample-coated PMMA plate in the instrument, and select the first location. Click Location1 as prompted by the software.
[0102] 2.5.2 Then use the X-Y positioning platform to move the sample to the second location, and click Location2…, and so on until all locations are tested.
[0103] 2.5.3 Then test the second sample-coated plate, and then the third plate, and so on until all plates are tested.
[0104] 2.5.4 Record the SPF and UVAPF values of each plate, and calculate the average values.
[0105] 2.6 End of test Turn off the computer and the instrument power.
[0106] The test results are shown in Table 2.
[0107] Table 2
[0108] The current standard test dosage in the art is 0.05±0.0005 grams, corresponding to a thickness of 2 mg / cm 2 The dosage in the present application is 0.025±0.0005 grams, corresponding to a thickness of 1 mg / cm 2The sun protection factor (SPF) values of the various embodiments can reach 68-100, and the UVAPF values can reach 12-20 under the condition of thin coating.
[0109] Further, under the condition of thin coating of 1 mg / cm 2 The sun protection factor (SPF) values and the UVAPF values of the various comparative examples are all lower than those of the various embodiments.
[0110] Therefore, it is shown that the embodiment scheme of the present application can effectively improve the sunscreen effect under the condition of thin coating.
[0111] Further, it can be seen from the comparison between Comparative Example 2 and Embodiment 1 that the content of silica and ethylhexyl methoxy cinnamate in Comparative Example 2 is the same as that in Embodiment 1, and under this premise, the SPF of Comparative Example 2 sharply decreases (from 68 to 45). Therefore, it can be seen that the present application realizes the improvement of sunscreen leakage points, the maintenance of the integrity of the sunscreen film, and the improvement of the sunscreen effect by compounding the powder composite sunscreen agent.
[0112] Further, all the embodiments: under the condition of thin coating (1 mg / cm 2 ), the SPF values are still very high. This shows that even if the coating is very thin, the sunscreen film does not have obvious weak points, which proves the characteristics of "continuous uniformity" and "no leakage" of the sunscreen film formed by the present application.
[0113] II. Waterproof and sweat-resistant effect test Equipment requirements: 250ML beaker, 200ML water, fixed speed 100RPM, water temperature maintained at 23℃-32℃, and water quality should be fresh. Record the water temperature, room temperature and relative humidity.
[0114] Test method: Test of general water resistance of sunscreen cosmetics If the product claims to have water resistance, the indicated SPF value should be the SPF value measured after the product has undergone the following 40-minute water resistance test: 1. Perform water resistance test on the PMMA plate tested above 2. Label the sample plate, lay it flat at the bottom of the water tank, and stir the water in the tank at a fixed speed. After 40 minutes, take it out and dry it for 15-20 minutes before testing the SPF value, following the above test method.
[0115] 3. Record the test results and calculate the average value.
[0116] The test results are shown in Table 3 below.
[0117] Table 3
[0118] The waterproof and sweat-resistant effect SPF values of each comparative example are lower than each embodiment. Thus, it is illustrated that the embodiment scheme of the application can effectively improve the waterproof and sweat-resistant effect.
[0119] III. Test the skin feel refreshing effect 1. Test purpose: The test aims to evaluate the basic skin feel and differences of the tested cosmetic.
[0120] 2. Test design: The forearm skin is selected for positioning and applying the product to evaluate the differences of specific skin feel indicators.
[0121] 3. Test environment: stable temperature and humidity, temperature (20-24) ℃, humidity (50±10)% 4. Test materials: Paper towel, disposable sterile syringe, pathological grade microscope slide, timer, wet wipe 5. Test method: 5.1 Volunteer requirements 5.1.1 Inclusion criteria: 5.1.1.1 Age between 18 and 40 years old, trained personnel (except pregnant or lactating women).
[0122] 5.1.1.2 No serious systemic disease, no immunodeficiency or autoimmune disease, and no skin cosmetic treatment or other tests that may affect the results on the test site.
[0123] 5.1.1.3 No active allergic disease.
[0124] 5.1.1.4 No highly allergic constitution.
[0125] 5.1.1.5 No open wounds or lesions on the test site.
[0126] 5.1.1.6 Trained and qualified in sensory evaluation.
[0127] 5.1.2 Exclusion criteria: 5.1.2.1 Pregnant or lactating women. (For female subjects) 5.1.2.2 Subjects with eczema, dermatitis, or scars on the back of the hand that may affect the test results.
[0128] 5.1.2.3 Unable to understand the training content and test questionnaire.
[0129] 5.1.2.4 Unable to cooperate with the test.
[0130] 5.1.3 Withdrawal criteria: Subjects who, in the opinion of the investigator, are not suitable to continue the study due to adverse events or other reasons during the study will be withdrawn from the study, and the reason for withdrawal will be recorded.
[0131] 5.2 Evaluation method: Table 4
[0132] 5.3 Subjects: 6 people were included, 0 people dropped out, 6 people were effective, 0 men and 6 women; the minimum age was 25 years old, the maximum age was 39 years old; the average age was 31.00±6.16 years old. The voluntary selection criteria.
[0133] 5.4 Test steps: 5.4.1 Volunteers clean the test site in the sensory evaluation laboratory, and understand the evaluation indicators and evaluation methods of this test under the guidance of the technician.
[0134] 5.4.2 In use (immediately-5 circles): take a sample (0.1 ml) with a 1 ml syringe and place it in the designated area of the left / right arm, and use the first segment of the right / left index finger and middle finger to make 5 circles (circle diameter 5 cm) at a speed of one circle per second; 5.4.3 In use (30 circles): continue to make circles at a speed of one circle per second to 30 circles, and evaluate the product by vision and touch; 5.4.4 After use (immediately): continue to make circles at a speed of one circle per second, and evaluate the product by vision and touch after completely absorbed (no product residue visible on the skin surface) or the product absorption is saturated (product residue is still visible on the skin surface); 5.4.5 After use (5 minutes after use): wait for 5 minutes after the product is completely absorbed, and evaluate the product by vision and touch.
[0135] 5.5 Sample use method: 5.5.1 The product should be randomly distributed in the designated area of the left and right arms, and ensure that the distribution area of the product is statistically balanced; 5.5.2 The subject washes both hands before testing, and then gently wipes the test area with a wet paper towel three times (wiping method: gently slide the folded wet paper towel from the elbow to the wrist, and do not apply pressure when wiping), and then use a dry paper towel to dry the moisture on the skin in the same way; 5.5.3 The sensory evaluation assistant positions the test area according to the number of samples, and then assigns the samples to the subjects, who evaluate the product according to the evaluation indicators and methods of the test questionnaire and comparison.
[0136] 5.6 Test site: single forearm (randomly applied according to random table) 5.7 Sample amount: 0.1ml / R = 5cm (0.1ml sample amount in a circle with a diameter of 5cm) The test results are shown in Table 5 below: Table 5 Freshness score
[0137] The sample of each embodiment has a freshness score of 10-14 after 5 minutes. Thus, it is shown that the sample of the embodiment scheme of the application has excellent freshness effect.
[0138] Four, stability test 1. Stability test samples: Example 1, Example 2, Example 3, Example 4, Example 5 products; 2. Test method: internal control standard (light for 1 month, high and low temperature test for 3 months), higher than national standard, industry standard; 3. The test results are shown in Table 6 below.
[0139] Table 6
[0140] The results of the above table show that the application has good stability in product application.
[0141] Five, safety test 1. Number of test persons: 30 persons, 5 men and 25 women; minimum age: 23 years old, maximum age: 44 years old; average age 35±15 years old; 2. Test method: patch test for Example 1-5. Select qualified patch tester, use closed patch test method, place about 0.020-0.025mL of the test material in the patch tester, apply medical tape to the back of the test subject, remove the test material after 24 hours, and observe the skin reaction at 0.5, 24 and 48 hours after removing the patch, respectively. Record the results according to the skin reaction grading standard in the “Cosmetic Safety Technology Standard” (2015 edition).
[0142] 3. The evaluation criteria are shown in Table 7.
[0143] Table 7 Evaluation criteria
[0144] After measurement, the closed patch test results of human skin showed that according to Table 7, among the 30 people, 0 cases had positive reactions, and according to the “Cosmetic Safety Technology Standard” (2015 edition), the batch of test materials (Example 1, Example 2, Example 3, Example 4, Example 5) would not cause skin adverse reactions in this batch of test subjects.
[0145] The above descriptions are only the preferred embodiments of the present application, and are not intended to limit the present application. The present application can have various modifications and changes for those skilled in the art. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A high-SPF sunscreen lotion, characterized in that, The high-SPF sunscreen emulsion is a water-in-silicone emulsion; the high-SPF sunscreen emulsion comprises: a continuous oil phase, a dispersed aqueous phase, a solid phase component, and a film-forming agent; the mass ratio of the aqueous phase to the oil phase is 1:10 to 1:1; The continuous oil phase comprises silicone oil and chemical sunscreens, including oil-soluble chemical sunscreens; the dispersed aqueous phase comprises water and water-soluble chemical sunscreens; the solid phase component is dispersed in the continuous oil phase; the solid phase component includes a silicone-surfaced physical sunscreen and a powder composite sunscreen; the powder composite sunscreen is a porous silica composite particle loaded with chemical sunscreens; the film-forming agent is a silane-based film-forming polymer dissolved or swollen in the continuous oil phase; The film-forming agent, the continuous oil phase, and the solid phase components together form a three-dimensional network, enabling the formation of a continuous, uniform, and water-resistant sunscreen film on the skin surface after application and drying. Furthermore, the sunscreen lotion, when applied at a concentration of 1 mg / cm³, provides a complete sun protection solution. 2 At that time, its in vitro SPF value is not less than 50.
2. The high-SPF sunscreen lotion according to claim 1, characterized in that, The physical sunscreen agent with silicon surface treatment includes at least one of: nano zinc oxide with triethoxyoctylsilane surface treatment and nano titanium dioxide with hydrogenated polydimethylsiloxane surface treatment.
3. The high-SPF sunscreen lotion according to claim 1, characterized in that, In the powder composite sunscreen, the porous silica-loaded chemical sunscreen includes: ethylhexyl methoxycinnamate.
4. The high-SPF sunscreen lotion according to claim 1, characterized in that, The silane-based film-forming polymers include: trimethylsiloxysilicate.
5. The high-SPF sunscreen lotion according to any one of claims 1-4, characterized in that, The oil-soluble chemical sunscreen agents include at least one of the following: ethylhexyl methoxycinnamate, ethylhexyl salicylate, humosalidinyl methoxyphenol triazine, diethylamino hydroxybenzoyl hexyl benzoate, or bis-ethylhexyloxyphenol methoxyphenyl triazine.
6. The high-SPF sunscreen lotion according to any one of claims 1-4, characterized in that, The water-soluble chemical sunscreen agent includes: phenylbenzimidazole sulfonic acid.
7. The method for preparing the high-SPF sunscreen lotion according to any one of claims 1-6, characterized in that, include: Silicone oil, oil-soluble chemical sunscreen, silicone-treated physical sunscreen, and film-forming agent are mixed, heated, and homogenized to obtain a uniform continuous oil-phase premix. Water, water-soluble chemical sunscreen, and pH adjuster are mixed, completely dissolved, and the pH is adjusted to 7.5-7.8 to obtain an aqueous premix. Under stirring, the aqueous premix is slowly added to the continuous oil premix for homogenization and emulsification to form a primary emulsion; Add the powdered composite sunscreen agent to the colostrum, stir and homogenize to disperse it evenly in the emulsion.
8. The preparation method according to claim 7, characterized in that, The preparation of the continuous oil phase premix includes: first, premixing the silicone surface-treated physical sunscreen agent with a portion of silicone oil and dispersant, then homogenizing and activating it, and finally combining it with other oil phase components.
9. The preparation method according to claim 7, characterized in that, The homogenization process is carried out at a speed of 3000 rpm - 5000 rpm for 3-10 minutes. Optionally, the temperature at which the aqueous phase is added to the oil phase is 70℃-80℃; Optionally, the temperature of the powdered composite sunscreen agent is reduced to below 40°C when it is added; Optionally, the pH adjuster includes: aminomethylpropanol.
10. The preparation method according to claim 7, characterized in that, The product comprises the following raw materials by weight percentage: Triethoxyoctylsilane surface-treated nano-zinc oxide: 6-12%; Cyclopentasiloxane: 10-15%; Polyglycerol-3 polydimethylsiloxane: 0.1-2%; Cetyl PEG / PPG-10 / 1 polydimethylsiloxane: 2-4%; Sorbitan oleate: 0.1-3%; Film-forming agent: 1-5%; Hydrogenated polydimethylsiloxane surface-treated nano-titanium dioxide: 1-5%; Isododecane: 2-6%; Distearate dimethylammonium lithium montmorillonite: 0.1-1%; Dibutyl adipate: 2-10%; Tocopheryl acetate: 0.1-0.5%; Bisabolol: 0.1-0.5%; Ethylhexyl methoxycinnamate: 5-9%; Ethylhexyl salicylate: 2-5%; Homosalate: 1-5%; Ethylhexyl triazine: 1-5%; Diethylamino hydroxybenzoyl hexyl benzoate: 3-8%; Bis-ethylhexyloxyphenol methoxyphenyl triazine: 1-5%; Phenylbenzimidazole sulfonic acid: 0.1-5%; Aminomethylpropanol: 0.1-1.67%; Powdered compound sunscreen: 1-10%; Balance: water.
Citation Information
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