Transparent sunscreen composition as well as preparation method and application thereof

Abstract

The invention relates to a transparent sunscreen composition as well as a preparation method and application thereof, and belongs to the technical field of sunscreen spray. The scheme of the invention provides a composition capable of being used for preparing a sun-screening spray without a boosting agent. The composition is prepared from the following components in parts by weight: 20 to 35 parts of emollient, 15 to 23 parts of sun-screening agent, 0.5 to 8 parts of film-forming agent, 0.1 to 2 parts of dibutyl ethyl hexanoyl glutamine and 30 to 50 parts of ethanol. According to the scheme, through scientific matching and component synergistic effect, the multiple advantages of high sunscreen, fresh skin feeling, excellent film forming, transparent texture, propellant-free spray form and the like are achieved, particularly, the limitation of a traditional ethanol system sunscreen product is broken through, and remarkable innovativeness and market competitiveness are achieved.

Description

Technical Field

[0001] The present application relates to a transparent sunscreen composition, a preparation method thereof and an application, belonging to the technical field of sunscreen sprays. Background Art

[0002] Exposure to ultraviolet radiation can easily cause skin redness, aging, reduce enzymatic and non-enzymatic antioxidants in the skin, and damage the natural protection mechanism in the skin, resulting in DNA damage and potential skin cancer. In order to effectively protect against ultraviolet radiation, it is necessary to use sunscreen products for sun protection, which is crucial for maintaining the health and appearance of the skin.

[0003] Common preparations of sunscreen products include lotions, sprays, gels, etc. Among them, sunscreen sprays have the advantages of convenient use and good use experience, and are gradually favored by consumers. For the sunscreen sprays in the prior art, in order to achieve the sunscreen effect, the viscosity of some products' sunscreen systems is relatively high, and it is necessary to add a propellant as a spray aid. On the one hand, the skin feel experience is poor, and on the other hand, there is also an explosion risk; some products do not add a propellant. However, in order to facilitate atomization, the sunscreen effect of the sunscreen system is poor, and it is difficult for the SPF to reach 50.

[0004] It can be seen that the main advantage of the sunscreen spray in the prior art that does not require adding a propellant as a spray aid is good skin feel, but the film-forming effect is poor and it is easy to slide off the skin. In addition, limited by the sunscreen system in the formula, it is difficult to achieve a good sunscreen effect.

[0005] Chinese Patent CN 118717546 A discloses a transparent sunscreen spray and a preparation method thereof, which avoid the environmental and health risks of traditional propellants. However, the addition of dimethyldistearylammonium lithium montmorillonite and silica easily causes the material to stratify and the spray to be uneven, and destroys the transparency of the spray. In addition, the particle characteristics of dimethyldistearylammonium lithium montmorillonite and silica may block the nozzle, affecting the uniformity and fineness of the spray, resulting in unstable spraying effect. And silica may cause the material to stratify or precipitate during storage, affecting the long-term stability of the product, increasing the difficulty of quality control and shortening the shelf life.

[0006] Chinese Patent CN 118750417 A discloses a two-phase transparent sunscreen spray, a preparation method thereof and an application, which adopts a layered system. It has the problem that the sliding property of the sprayed material is strong after shaking, resulting in easy rapid sliding of the spray during use, unable to be evenly applied on the skin surface, causing uneven sunscreen effect. In addition, if the sliding property of the spray liquid is strong and difficult to control, it may lead to uneven particle sizes of the sprayed particles, affecting the fineness of the spray, resulting in uneven coverage layer after spraying, excessive spray in some areas while insufficient spray in other areas, thus affecting the protection effect.

[0007] In addition, the layered system of two-way transparent spray usually results in a relatively high concentration of sunscreen ingredients (such as chemical sunscreens) in one layer of the spray and a relatively low concentration in the other layer. Even after shaking, the sunscreen ingredients may not be completely evenly distributed in the spray liquid, leading to insufficient sunscreen protection in some areas and poor sunscreen effect.

[0008] The layered system contains oily ingredients and aqueous ingredients, and there is a problem of unstable film-forming effect. As a result, the film layer after spraying is weak, the sunscreen effect cannot last for a long time, and it is easy to fall off due to friction or sweat, reducing the durability of sunscreen protection.

[0009] No emulsifier is added in this patent system, which can avoid the possible irritation to the skin caused by some surfactants, but it will increase the technical difficulty in the production process. In the absence of emulsifiers, the stability of the product, the spray effect, and the stability during long-term storage will all face more challenges. During large-scale production, in order to ensure that the spray effect and composition of each bottle of spray are consistent under the same conditions, more stringent process control is required, resulting in an increase in production costs and technical difficulties.

[0010] Therefore, it is urgent to optimize the sunscreen system in the existing sunscreen sprays to provide a transparent sunscreen spray product with good skin feel, uniform and stable texture, a sunscreen SPF of 50, and no need to add boosters. Summary of the Invention

[0011] To solve the above problems, a transparent sunscreen composition, its preparation method and application are provided. In this application, by adopting a sunscreen system with an ethanol solvent, the viscosity of the sunscreen composition is below 10 cst, achieving a refreshing and non-greasy skin feel, being easy to spray and having a good film-forming effect, and being able to ensure that the sunscreen SPF value is above 50, reaching the PA+++ level, solving the problem that it is difficult to have both a good skin feel, sunscreen effect and film-forming effect in the existing transparent sunscreen system, and having strong market competitiveness.

[0012] This application provides a transparent sunscreen composition. By weight, the transparent sunscreen composition includes: 20 - 35 parts of emollient, 15 - 23 parts of sunscreen agent, 0.5 - 8 parts of film-forming agent, 0.1 - 2 parts of dibutyl ethylhexanoyl glutamine, and 30 - 50 parts of ethanol;

[0013] The emollient includes one or more of isopropyl myristate, polydimethylsiloxane, dicaprylyl carbonate, C12-15 alkyl benzoate, cyclopentasiloxane, isononyl isononanoate, and squalane;

[0014] The sunscreen agent includes one or more of bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane, homosalate, diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, polysiloxane-15, cresol triazone, and diethylhexyl butamido triazone;

[0015] The film-forming agent includes one or more of trimethylsilyloxy silicate, acrylate / octylacrylamide copolymer, VP / acrylate / lauryl methacrylate copolymer, dibutyl lauroyl glutamate, and VP / eicosene copolymer.

[0016] Optionally, the SPF of the transparent sunscreen composition is not less than 50.

[0017] Optionally, the viscosity of the transparent sunscreen composition is not higher than 20 cps.

[0018] Optionally, the average particle size of the atomized particles after spraying the transparent sunscreen composition is not higher than 100 μm.

[0019] Optionally, the sunscreen agent includes one or more of bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, ethylhexyl salicylate, and polysiloxane-15.

[0020] Optionally, the sunscreen agent includes:

[0021] 0.1 - 2 parts of bis-ethylhexyloxyphenol methoxyphenyl triazine, 1 - 7 parts of diethylamino hydroxybenzoyl hexyl benzoate, 0.5 - 10 parts of ethylhexyl methoxycinnamate, 0.1 - 5 parts of ethylhexyl triazone, 0.5 - 4 parts of octocrylene, 1 - 5 parts of ethylhexyl salicylate, and 0.5 - 3 parts of polysiloxane-15.

[0022] Optionally, the transparent sunscreen agent composition includes: 0.1 - 2 parts of bis-ethylhexyloxyphenol methoxyphenyl triazine, 1 - 7 parts of diethylamino hydroxybenzoyl hexyl benzoate, 0.5 - 10 parts of ethylhexyl methoxycinnamate, 0.1 - 5 parts of ethylhexyl triazone, 0.5 - 4 parts of octocrylene, 1 - 5 parts of ethylhexyl salicylate, 0.5 - 3 parts of polysiloxane-15, 1 - 15 parts of dicaprylyl carbonate, 0.5 - 7 parts of isopropyl myristate, 0.1 - 3 parts of polydimethylsiloxane, 0.5 - 7 parts of C12-15 alkyl benzoate, 30 - 50 parts of ethanol, 0.01 - 1 part of dibutyl ethylhexanoyl glutamine, and 0.5 - 3 parts of acrylate / octylacrylamide copolymer.

[0023] Optionally, the transparent sunscreen composition further includes fragrance and / or whitening active ingredients.

[0024] The present application provides a method for preparing a transparent sunscreen composition, and the preparation method includes the following steps:

[0025] 1) Weigh the raw materials to be used and set them aside for later use;

[0026] 2) Dissolve ethanol, diethylhexyl acetylglutamine, and acrylate / octylacrylamide copolymer until transparent and free of particles for later use;

[0027] 3) Add bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, ethylhexyl salicylate, polysiloxane-15, dicaprylyl carbonate, and C12-15 alkyl benzoate to the main pot, start the stirrer, and heat the main pot to 80-85 °C. After the material is evenly dispersed and free of particles, set it aside for later use;

[0028] 4) When the temperature drops to 55-65 °C, add tetrahydrocurcumin to the main pot and stir until evenly mixed and free of particles; add isopropyl myristate and polydimethylsiloxane and stir evenly for later use;

[0029] 5) When the temperature drops to 36-40 °C, add the ethanol solution, fragrance, and tetraisopalmitoyl ascorbate dissolved in step 2) and stir until evenly mixed;

[0030] 6) Let it stand and cool to room temperature to obtain the transparent sunscreen composition.

[0031] The present application provides the use of the above-mentioned transparent sunscreen composition in the preparation of a booster-free sunscreen spray.

[0032] The beneficial effects of the present application include but are not limited to:

[0033] 1) The solution of the present application is based on an ethanol system, having the advantages of a refreshing and non-greasy skin feel. Using ethanol as the main solvent, compared with traditional sunscreen products, it can volatilize quickly, keep the skin refreshing and non-greasy, and also improve the comfort of use in hot environments. It is especially suitable for use on oily skin or in hot and humid environments. In addition, due to the good solubility of ethanol, the use of high-molecular emulsifiers can be reduced, thereby further reducing the stickiness of the formula and improving the skin feel.

[0034] 2) The main challenge in the prior art for ethanol systems is that it is difficult for sunscreen components to form a uniform film, and the problem of uneven distribution of sunscreen agents is likely to occur. The solution of the present application optimizes the film-forming effect based on an ethanol system. Specifically, through the synergistic cooperation of diethylhexyl acetylglutamine and acrylate / octylacrylamide copolymer, the sunscreen formula of the present application can still form a uniform and stable protective layer without the use of thickeners, achieving an excellent SPF50 sunscreen effect.

[0035] In an ethanol system, dibutyl ethylhexanoyl glutamine is used in combination with a sunscreen system. The distribution uniformity of the sunscreen is better, and a stable protective film can be formed on the skin surface, thereby improving the sunscreen persistence. In addition, it can also enhance the stability of the sunscreen. Specifically, through the amide group in its molecular structure, hydrogen bonds are formed with the polar groups in the sunscreen, thereby enhancing the adhesion of the sunscreen on the skin surface and improving the persistence and uniformity of the sunscreen film.

[0036] Further, when acrylate / octylacrylamide copolymer is used in combination, a transparent protective film can be formed on the skin surface to prevent the sunscreen from being washed away by sweat or moisture. This raw material is well compatible with the dibutyl ethylhexanoyl glutamine, sunscreen system and ethanol system, improving the uniformity and transparency of the film-forming process.

[0037] 3) The present application also scientifically formulates the sunscreen, which can effectively enhance the SPF50 protection. Specifically, the chemical sunscreens used include bis-ethylhexyloxyphenol methoxyphenyl triazine (BEMT), diethylamino hydroxybenzoyl hexyl benzoate (DHHB), ethylhexyl methoxycinnamate (OMC), ethylhexyl triazone (EHT), octocrylene (OCR), ethylhexyl salicylate (EHS), polysiloxane-15 (PS-15). The combination of this sunscreen system can achieve broad-spectrum protection: among them, BEMT has excellent UVA and UVB absorption capabilities and excellent photo-stability. When compounded with other sunscreens, it can improve the overall protection performance; DHHB mainly targets the long wavelength of UVA and can effectively prevent photoaging. When combined with BEMT, it forms a strong UVA protection system; OMC, EHS, octocrylene, EHT, etc. target the UVB band, enhancing the UVB protection ability of the sunscreen product and preventing sunburn. The selected sunscreen system in the present application can synergistically enhance the effects of each component. Through scientific proportioning, each component stabilizes each other, improves the photo-stability and reduces degradation, thereby improving the sunscreen persistence and making the SPF50 sunscreen effect more persistent and reliable.

[0038] 4) Traditional high-sunscreen formulations often contain physical sunscreens such as titanium dioxide or zinc oxide, or components such as emulsifiers and thickeners, which are prone to turbidity or whitening. However, the present application completely relies on a chemical sunscreen system, does not add any physical sunscreens and film-forming agents, and optimizes the solubility and film-forming properties of the sunscreen, making the entire formulation present a transparent aqueous solution texture with a clear appearance and little impact on the natural skin color.

[0039] In the formulation, ethanol synergizes with the film-forming agent. The low viscosity and high volatility of ethanol enable the sunscreen agent and the film-forming agent to be evenly dispersed in the solution, forming a transparent appearance. The transparency of acrylate / octylacrylamide copolymer in the ethanol system further ensures the high transparency of the product and avoids the common white residue problem of traditional sunscreen products. The combination of dibutyl ethylhexanoyl glutamine and acrylate / octylacrylamide copolymer components has good transparency and does not affect the overall appearance of the product, ensuring that no white marks are left on the skin after use.

[0040] 5) The solution of this application realizes the spray function without a booster through the low viscosity and high volatility of the ethanol system and combines with an efficient film-forming technology. The spraying process is delicate and uniform, and the average particle size of the droplets after spraying is 50 - 80 microns, with a uniform distribution, ensuring the uniformity and high efficiency of the sunscreen film. Compared with traditional spray products containing boosters, this product is not only safer and more convenient to use, but also provides a more comfortable skin feel and higher environmental friendliness, fully demonstrating its unique technical advantages and market competitiveness.

[0041] 6) The product of this application has a wide range of applications and obvious market advantages. It is suitable for all skin types, especially for oily skin and consumers in hot regions, and can avoid the greasy and heavy sunscreen experience. Its transparent texture suits all skin tones and does not cause whitening, meeting the demand for "invisible sunscreen" in Asian and European and American markets. Moreover, it can be prepared in a spray form, which is more convenient to use and suitable for outdoor, sports, airplane, high-speed rail and other scenarios, further expanding the application scope of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] The drawings described herein are used to provide a further understanding of this application and form a part of this application. The schematic embodiments of this application and their descriptions are used to explain this application and do not constitute an improper limitation to this application. In the drawings:

[0043] Figure 1 is a schematic diagram of the product of the transparent sunscreen composition related to Example 1 of this application;

[0044] Figure 2 is a particle size distribution result diagram related to Test Example 6 of this application;

[0045] Figure 3 is a light transmittance detection result diagram related to Test Example 7 of this application;

[0046] Figure 4 is a turbidity detection result diagram related to Test Example 7 of this application;

[0047] Figure 5 is a preliminary sample result diagram of the transparent sunscreen spray related to Comparative Example 1 of this application;

[0048] Figure 6 This is the result diagram after 5 hours of sedimentation of the transparent sunscreen spray involved in Comparative Example 1 of this application. Detailed implementation mode

[0049] The present application will be described in detail below in conjunction with embodiments. However, the present application is not limited to these embodiments. Unless otherwise specified, the raw materials and reagents in the embodiments of the present application are all purchased through commercial channels.

[0050] The solution of the present application will be described below through specific embodiments.

[0051] Embodiment 1

[0052] This embodiment provides a transparent sunscreen composition, and its specific components and compositions are shown in Table 1 below.

[0053] Table 1 Composition table of the transparent sunscreen composition in Embodiment 1

[0054] Component Name Content (parts) Function Bis-ethylhexyloxyphenol methoxyphenyl triazine 2 Sun protection agent Diethylamino hydroxybenzoyl hexyl benzoate 5 Sun protection agent Ethylhexyl methoxycinnamate 9 Sun protection agent Ethylhexyl triazone 2 Sun protection agent Octocrylene 2 Sun protection agent Ethylhexyl salicylate 4 Sun protection agent Polysiloxane-15 2 Sun protection agent Isopropyl myristate 5 Emollient Polydimethylsiloxane 2 Emollient Dioctyl carbonate 9 Emollient C12-15 alkyl benzoate 5 Emollient Dibutyl ethylhexanoyl glutamine 1 Thickening agent Acrylates / octylacrylamide copolymer 2 Film-forming agent Ethanol 49.15 Solvent Tetrahexyldecyl ascorbate 0.1 Whitening agent Tetrahydrocurcumin 0.15 Skin protectant Fragrance 0.6 Aromatic agent

[0055] The preparation method of this transparent sunscreen composition is as follows:

[0056] 1) Weigh the raw materials to be used and set aside.

[0057] 2) Dissolve ethanol, diethylhexyl 2-ethylhexanoylglutamate, and acrylate / octylacrylamide copolymer until transparent and particle-free for standby.

[0058] 3) Add bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, ethylhexyl salicylate, polysiloxane-15, dicaprylyl carbonate, and C12-15 alkyl benzoate to the main pot, start the stirrer, and heat the main pot to 83 °C. After the material is evenly dispersed and particle-free, set aside.

[0059] 4) When the temperature drops to 60 °C, add tetrahydrocurcumin to the main pot and stir until it is uniform and particle-free; add isopropyl myristate and polydimethylsiloxane and stir evenly for standby.

[0060] 5) When the temperature drops to 38 °C, add the ethanol solution, essence, and tetraisopalmitoyl ascorbate dissolved in the second step and stir until uniform.

[0061] 6) Let it stand and cool to room temperature to obtain this transparent sunscreen composition.

[0062] 7) Take samples for testing. After passing the test, discharge and let it stand for 48 hours to obtain this transparent sunscreen composition. The product picture is as Figure 1 shown.

[0063] Embodiment 2

[0064] This embodiment provides a transparent sunscreen composition, and its specific ingredients and composition are shown in Table 2 below.

[0065] Table 2 Composition Table of the Transparent Sunscreen Composition in Example 2

[0066] Component Name Content (parts) Function Bis-ethylhexyloxyphenol methoxyphenyl triazine 2 Sun protection agent Diethylamino hydroxybenzoyl hexyl benzoate 5 Sun protection agent Ethylhexyl methoxycinnamate 3 Sun protection agent Ethylhexyl triazone 1.5 Sun protection agent Octocrylene 4 Sun protection agent Ethylhexyl salicylate 4.5 Sun protection agent Polysiloxane-15 0.5 Sun protection agent Isopropyl myristate 7 Emollient Polydimethylsiloxane 0.1 Emollient Dioctyl carbonate 1 Emollient C12-15 alkyl benzoate 7 Emollient Dibutyl ethylhexanoyl glutamine 0.6 Thickening agent Acrylates / octylacrylamide copolymer 2 Film-forming agent Ethanol 30 Solvent Tetrahexyldecyl ascorbate 0.1 Whitening agent Tetrahydrocurcumin 0.15 Skin protectant Fragrance 0.6 Aromatic agent

[0067] The preparation method of this transparent sunscreen composition is as follows:

[0068] 1) Weigh the raw materials to be used and set them aside for later use;

[0069] 2) Dissolve ethanol, dibutyl ethylhexanoyl glutamine, and acrylate / octylacrylamide copolymer until transparent and free of particles for later use;

[0070] 3) Add bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, ethylhexyl salicylate, polysiloxane-15, dicaprylyl carbonate, and C12-15 alkyl benzoate to the main pot, start the stirrer, and heat the main pot to 85°C. After the material is evenly dispersed and free of particles, set it aside for later use;

[0071] 4) When the temperature drops to 65°C, add tetrahydrocurcumin to the main pot and stir until it is evenly distributed and free of particles; add isopropyl myristate and polydimethylsiloxane and stir evenly for later use;

[0072] 5) When the temperature drops to 40°C, add the ethanol solution, fragrance, and tetraisopalmitoyl ascorbate dissolved in the second step and stir until evenly distributed;

[0073] 6) Let it stand and cool to room temperature to obtain this transparent sunscreen composition.

[0074] 7) Take samples for testing. After passing the test, discharge the material and let it stand for 48 hours to obtain this transparent sunscreen composition.

[0075] Example 3

[0076] This embodiment provides a transparent sunscreen composition, and its specific ingredients and composition are shown in Table 3 below.

[0077] Table 3 Composition Table of the Transparent Sunscreen Composition in Example 3

[0078] Component Name Content (parts) Function Bis-ethylhexyloxyphenol methoxyphenyl triazine 0.5 Sun protection agent Diethylamino hydroxybenzoyl hexyl benzoate 3 Sun protection agent Ethylhexyl methoxycinnamate 9.5 Sun protection agent Ethylhexyl triazone 4 Sun protection agent Octocrylene 0.5 Sun protection agent Ethylhexyl salicylate 3 Sun protection agent Polysiloxane-15 3 Sun protection agent Isopropyl myristate 0.5 Emollient Polydimethylsiloxane 3 Emollient Dioctyl carbonate 15 Emollient C12-15 alkyl benzoate 0.5 Emollient Dibutyl ethylhexanoyl glutamine 0.3 Thickening agent Acrylates / octylacrylamide copolymer 2 Film-forming agent Ethanol 50 Solvent Tetrahexyldecyl ascorbate 0.1 Whitening agent Tetrahydrocurcumin 0.15 Skin protectant Fragrance 0.6 Aromatic agent

[0079] The preparation method of this transparent sunscreen composition is as follows:

[0080] 1) Weigh the raw materials to be used and set them aside for later use;

[0081] 2) Dissolve ethanol, dibutyl ethylhexanoyl glutamine, and acrylate / octylacrylamide copolymer until transparent and free of particles for later use;

[0082] 3) Add bis - ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl benzoate hexyl ester, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, ethylhexyl salicylate, polysiloxane - 15, dicaprylyl carbonate, and C12 - 15 alkyl benzoate into the main pot, start the stirrer, and heat the main pot to 80 °C. After the material is evenly dispersed and there are no particles, set it aside for later use;

[0083] 4) When the temperature drops to 55 °C, add tetrahydrocurcumin into the main pot and stir until it is evenly dispersed and there are no particles; add isopropyl myristate and polydimethylsiloxane, and stir evenly for later use;

[0084] 5) When the temperature drops to 36 °C, add the ethanol solution, essence, and tetraisopalmitoyl ascorbate dissolved in the second step, and stir until evenly mixed;

[0085] 6) Let it stand and cool to room temperature to obtain the transparent sunscreen composition.

[0086] 7) Take samples for testing. After passing the test, discharge the material and let it stand for 48 hours to obtain the transparent sunscreen composition.

[0087] Example 4

[0088] This example is basically the same as Example 1, except that it does not contain dibutyl ethylhexanoyl glutamine.

[0089] Example 5

[0090] This example is basically the same as Example 1, except that dibutyl ethylhexanoyl glutamine is replaced with an equal amount of dibutyl lauroyl glutamate.

[0091] Example 6

[0092] This example is basically the same as Example 1, except that acrylate / octylacrylamide copolymer is replaced with an equal amount of VP / eicosene copolymer.

[0093] Example 7

[0094] This example is basically the same as Example 1, except that dibutyl ethylhexanoyl glutamine is replaced with an equal amount of xanthan gum.

[0095] Example 8

[0096] This example is basically the same as Example 1, except that dibutyl ethylhexanoyl glutamine is replaced with an equal amount of VP / acrylate / lauryl methacrylate copolymer.

[0097] Example 9

[0098] This example is basically the same as Example 1, except that dibutyl ethylhexanoyl glutamine is replaced with an equal amount of polyvinylpyrrolidone.

[0099] Test Example 1

[0100] The products of Examples 1-9 were observed for stability for 90 days, and the results are shown in Table 4 below.

[0101] Table 4 Stability test results

[0102]

[0103] According to the stability results in Table 4, Examples 5-9 could not pass the stability test, and precipitation occurred under extreme temperature conditions, indicating that the physical stability of the products was poor under high and low temperature environments. The formation of precipitation affected the appearance, usability, and efficacy of the products, resulting in the products of Examples 5 and 6 not meeting the market standards. Examples 1-4 showed good stability under extreme conditions.

[0104] Test Example 2

[0105] Experimental animals and breeding environment: Japanese white rabbits with big ears, male, ordinary grade, provided by Beijing Jinmuyang Experimental Animal Breeding Co., Ltd. [License number: SCXK(Jing)2020-0003, Quality certificate number: 110333241100207077], a total of 4 animals, with a body weight of 2.5-3 kg. The animals were acclimatized in the ordinary environment animal house for 3 days, and after completing animal quarantine and confirming the health of the animals, the experiment was carried out. The temperature in the animal house was 20.7-21.2 °C, the relative humidity was 40-43%, the light was alternated between light and dark for 12 hours, and the experimental animal use license number was: SYXK(Jing)2024-0053. The animal feed was purchased from Keao Xieli (Tianjin) Feed Co., Ltd., license number: SCXK(Jin)2020-0004, quality certificate number: 1209162500039029, and the drinking water was tap water.

[0106] Test method: 24 hours before the test, the hair on both sides of the spine of the animals was removed, and the hair removal area was 3 cm × 3 cm on the left and right. 0.5 mL of the test substance was applied to the left skin, and the application area was 2.5 cm × 2.5 cm. It was applied once a day for 14 consecutive days, and the right skin was used as a control. Starting from the second day, the hair was removed before each application, and it was washed with warm water to remove the residual test substance. The results were observed 1 hour later, and the control area and the test area were treated in the same way. The skin irritation / corrosion test was scored according to the "Technical Specifications for Cosmetics Safety" (2015 Edition), Chapter 6 Toxicology Test Methods 4, and the average score of each animal per day was calculated according to the following formula. The skin irritation intensity was determined according to the highest average score.

[0107]

[0108] Table 5 Results of multiple skin irritation tests on Japanese white rabbits with large ears in Examples 1 and 4

[0109]

[0110] According to the test results, the multiple skin irritation results of Example 1 and Example 4 on Japanese white rabbits with large ears were non-irritating.

[0111] Test Example 3

[0112] Positive substance: 2,4-dinitrochlorobenzene, batch number: STBG2582V, manufacturer: Sigma, solvent: 80% ethanol, induction concentration: 2.0%, excitation concentration: 0.5%. Experimental animals: 40 ordinary-grade Dunkin Hartley guinea pigs, half male and half female, weighing 300 - 350 g, provided by Beijing Jinmuyang Experimental Animal Breeding Co., Ltd., license number: SCXK(Beijing)2020 - 0003, quality certificate number: 110333241100203486. The animals were acclimated in the ordinary environment animal house for 3 days, and after completing animal quarantine and confirming the health of the animals, the test was carried out. The temperature of the animal house was 21.1 - 22.4 °C, the relative humidity was 38 - 45%, the light was alternated between light and dark for 12 hours, and the experimental animal use license number was SYXK(Beijing)2024 - 0053. The animal feed was purchased from Kaoao Xieli (Tianjin) Feed Co., Ltd., license number: SCXK(Tianjin)2020 - 0004, quality certificate number: 1209162500039029, and the drinking water was tap water.

[0113] Test method: For the guinea pigs in the test group, the test substance was used for induction and excitation treatment. The positive control group was given 2,4-dinitrochlorobenzene for induction and excitation treatment, with an induction concentration of 2.0% and an excitation concentration of 0.5%. The negative control group was treated with deionized water for induction and the test substance for excitation. The hair on the left side of the guinea pigs' backs within a range of 2 cm × 2 cm was shaved 24 hours before the test. Inductive contact: 0.2 mL of the test substance was applied to the depilated area on the left side of the animals, covered with two layers of gauze and one layer of cellophane, and then sealed and fixed with non-irritating adhesive tape for 6 hours. The same method was repeated on the 7th day and the 14th day. Excitation contact: 14 days after the last induction, 0.2 mL of the test substance was applied to the depilated area on the right side of the animals (depilated 24 hours before contact) within a range of 2 cm × 2 cm, then covered with two layers of gauze and one layer of cellophane, and sealed and fixed with non-irritating adhesive tape for 6 hours. The skin reaction was observed at 24 hours and 48 hours after excitation contact, and the sensitization intensity of the test substance was judged according to the "Skin Allergy Test" in the "Cosmetics Safety Technical Specifications" (2015 edition).

[0114] Table 6 Results of skin allergy test on guinea pigs (BT method)

[0115]

[0116] Note: ① The starting weight and ending weight are expressed as mean ± SD; ② In the skin reaction intensity column, the proportion of animals with a skin reaction score of 0, 1, 2, or 3 out of the total number of test animals should be filled in. Date of positive control test: July 19, 2024 - August 23, 2024.

[0117] According to the test results, for the guinea pig skin allergy test of Example 1 and Example 4, the number of animals with an erythema edema score ≥ 2 was 0, the sensitization rate was 0%, and no skin allergy was observed.

[0118] Test Example 4

[0119] Negative control: Blank control. Subjects: A total of 38 cases were included in the human patch test, of which 3 cases dropped out. Actually, 35 subjects completed the test, including 10 males and 25 females, aged 22 to 41 years, with an average age of 27.2 ± 4.57 years.

[0120] Patch test method: Select qualified patch test equipment. Using the closed patch test method, place approximately 0.020 mL - 0.025 mL (liquid) of the test substance in the patch tester, and apply a low - sensitization tape externally to the flexor side of the subject's forearm. Remove the test substance after 24 hours, and observe the skin reaction at 0.5, 24, and 48 hours after removal. Record the results according to the skin reaction grading standard of the skin closed patch test in Chapter 7, Human Safety Test Methods, Annex 2 of the Cosmetics Safety and Technical Specifications (2015).

[0121] Table 7 Results of Cosmetics Human Skin Patch Test

[0122]

[0123] The results of the human skin patch test showed that among 35 subjects, there were 35 negative reactions and 0 positive reactions, indicating that Examples 1 and 4 have good safety.

[0124] Test Example 5

[0125] Detection method: The subject takes the prone position and the back is irradiated. The minimum erythema dose (MED value) of the subject's skin to ultraviolet irradiation is predicted 24 hours before the detection. According to the prediction result, the ultraviolet irradiation dose is adjusted for detecting the sample. On the day of detection, first select a normal skin area of 7 cm × 7 cm on the subject's back, and evenly apply the sample to be detected or the standard control product at a sample dosage of (2.00 ± 0.05) mg / cm2 in the above area. Then select an appropriate ultraviolet irradiation dose and irradiate in three cases: ① The subject's skin is not coated with the sample; ② The control standard product is coated; ③ The test sample is coated. Observe the experimental results 16 - 24 hours later and record the MED values in the three cases respectively.

[0126] Calculation method of SPF value: The SPF value of the sample or standard product for protecting a single subject is expressed by the following formula:

[0127]

[0128] The calculation of the individual SPF value requires accuracy to one decimal place. Calculate the arithmetic mean of the SPF values of the sample for protecting all subjects, and take the integer part as the SPF value of the tested sample.

[0129] Table 8 Detection results of Example 1

[0130]

[0131] According to the test results, the average SPF value of Example 1 is 57.7.

[0132] Table 9 Detection results of Example 4

[0133]

[0134] According to the test results, the average SPF value of Example 4 is 15.6.

[0135] According to the above results, it can be seen that the SPF of Example 1 is significantly improved compared with Example 4. It can be seen that the addition of dibutyl ethylhexanoyl glutamine not only significantly improves the film-forming effect, but also significantly increases the SPF value of the product by optimizing the distribution, adhesion and stability of the sunscreen agent, making it significantly higher than the formula without adding this component.

[0136] And the experimenters found that other similar additives are difficult to play such an obvious improvement role as dibutyl ethylhexanoyl glutamine. For specific details, refer to the detection results of Examples 5, 7, 8, and 9 below.

[0137] Table 10 Detection results of Example 5

[0138]

[0139] Table 11 Test Results of Example 7

[0140]

[0141] Table 12 Test Results of Example 8

[0142]

[0143] Table 13 Test Results of Example 9

[0144]

[0145] Dibutylethylhexanoylglutamine, as a thickening and stabilizing raw material, is originally mostly used in ointment products to improve the hardness and transparency of ointments. However, in the solution of this application, it has achieved unexpected technical effects, and other components with similar effects cannot achieve similar effects.

[0146] In the solution of this application, dibutylethylhexanoylglutamine plays a key role in the film-forming process through its unique molecular structure (long-chain alkyl and amide groups): 1) It can form a uniform and dense film on the skin surface, ensuring the uniform distribution of the sunscreen and avoiding inconsistent protection effects caused by uneven local concentrations; 2) Its amide group forms hydrogen bonds with the cutin proteins on the skin surface and the polar groups in the sunscreen, significantly enhancing the adhesion and persistence of the sunscreen film and reducing the loss of the sunscreen caused by friction or sweat.

[0147] In the solution of this application, through the use of dibutylethylhexanoylglutamine and in combination with other components such as the sunscreen system, the film-forming effect of the entire system can be significantly improved. This film-forming effect not only enhances the uniformity and density of the sunscreen film but also directly enhances the stability and reliability of the SPF value, significantly improving the sunscreen effect and solving the technical problem that the sunscreen ability of the ethanol sunscreen system in the prior art cannot be improved.

[0148] Test Example 6

[0149] This product uses an ethanol system as a solvent and combines the film-forming technologies of dibutylethylhexanoylglutamine and acrylate / octylacrylamide copolymer to achieve a spray function without a booster.

[0150] The low viscosity and high volatility of ethanol enable the material to be easily atomized through the fine nozzle of the spray device to form a uniform and delicate spray. The rapid evaporation characteristic of ethanol ensures that the material can quickly form a uniform sunscreen film on the skin surface after spraying. The spray is delicate and uniform, without an obvious feeling of liquid droplets when spraying, and the skin feel is fresh and non-greasy. Since there is no need for a booster, it avoids the cold feeling or irritation caused by the propellant in traditional spray products, making it more comfortable to use.

[0151] After spraying, the material quickly forms a transparent, uniform and dense sunscreen film on the skin surface, with the sunscreen evenly distributed to ensure an efficient sunscreen effect (SPF50).

[0152] To verify the atomization effect of the spray, the experimenters detected the particle size after spraying using the laser diffraction method. The detection results are as Figure 2 shown.

[0153] The average particle size of the droplets after spraying is 50 - 80 microns, belonging to the fine atomization range, ensuring the uniformity and coverage of the spray. The particle size distribution range is narrow (30 - 110 microns), indicating that the spray droplets are of uniform size, avoiding the problems of large droplets or uneven atomization commonly found in traditional spray products. Compared with traditional spray products containing propellants, the atomization effect of this product is more delicate and uniform, and there is no additional irritation or discomfort caused by the propellant.

[0154] Test Example 7

[0155] To verify the transparency and uniformity of the sample, the transmittance of Example 1 was detected. The transmittance of the sample in the visible light range was tested by ultraviolet-visible spectrophotometry; the degree of light scattering of the sample was tested by a turbidimeter to evaluate its turbidity. The lower the turbidity, the better the transparency and uniformity of the sample. The test results are as Figure 3 and Figure 4 shown, where there is no significant difference in the transmittance detection data of Examples 1, 2, and 3. Example 1 is used for illustration.

[0156] According to the detection results, Example 1 has almost no light absorption or scattering in the visible light range and has good transparency; in the turbidity test, there are no obvious particles or suspended substances in Examples 1 - 3, and they have good uniformity.

[0157] Test Example 8

[0158] The viscosity of the sample of Test Example 1 was tested. Specifically, the viscosity of the sample was tested using a rotational viscometer with a No. 1 rotor and a rotation speed set at 60 rpm.

[0159] The detection results are as follows: the torque of the sample of Example 1 is 4.9%, and the viscosity is 4.9 mPa·s. The torque of the compared deionized water is 2.4%, and the viscosity is 2.3 mPa·s.

[0160] The test results show that the viscosity of the sample is slightly higher than that of deionized water, but it is still in the low viscosity range, showing excellent fluidity.

[0161] The low-viscosity property of the product of this application enables it to easily achieve a delicate and uniform atomization effect through a spraying device, quickly form a uniform sunscreen film on the skin surface after spraying, and at the same time avoid the sticky feeling of traditional high-viscosity sunscreen products, providing a refreshing use experience.

[0162] Compared with deionized water, the viscosity of the sample is slightly higher but still maintains excellent fluidity, giving it unique advantages as a spray product, including rapid film formation, easy application, and a refreshing skin feel, significantly enhancing the user experience and product performance.

[0163] Comparative Example 1

[0164] This comparative example is a reproduction of the prior art patent CN118717546A. When conducting the prior art transparent sunscreen spray and its preparation method, the experiment was carried out according to the formula and process described in the patent, focusing on the effects of lithium magnesium stearate montmorillonite and silica on the stability of the material, spray performance, and transparency. The results of the obtained products are as Figure 5 and 6 shown.

[0165] The experimenters found that the material showed a certain fluidity and low transparency in the initial stage after preparation. However, in the spray test, due to the particle characteristics of lithium magnesium stearate montmorillonite and silica, the spray uniformity and fineness were poor, and nozzle clogging occurred, resulting in unstable spray effects.

[0166] In the storage stability test, the material showed stratification and precipitation when stored statically at 25°C, and obvious solid precipitation appeared at the bottom, indicating that the particle characteristics of silica and lithium magnesium stearate montmorillonite destroyed the homogeneity and long-term stability of the material.

[0167] The viscosity test results showed that the viscosity of the material was too high (80 mPa·s), the fluidity was poor, and the use experience for spray products needed to be optimized.

[0168] Experimental Example 1

[0169] Before determining the sunscreen system of this application's solution, the experimenters further screened and optimized the combination of the ethanol system and film-forming agents. Some representative screened samples are shown in Table 14 below, and the test results are shown in Table 15 below.

[0170] Table 14 Optimization and Screening of the Sunscreen System

[0171]

[0172] Table 15 Sample Test Results

[0173]

[0174] During the one-week stability observation, samples 2, 4, and 5 were all unstable, while samples 1, 3, and 6 showed excellent stability.

[0175] In the SPF test, the SPF value of sample 6 was only 38, which did not meet the project requirements.

[0176] In the sensory test, sample 1 had a refreshing texture without obvious greasiness, the skin was smooth after application, and there was no white residue or heaviness; sample 3 had a relatively heavy texture, a serious sense of oiliness after application, and obvious oiliness. By sensory comparison, the texture of sample 1 was better than that of sample 3, and finally the sunscreen agent system was determined to be the combination of sample 1.

[0177] As described above, it is only the embodiments of the present application. The protection scope of the present application is not limited by these specific embodiments, but is determined by the claims of the present application. For those skilled in the art, various changes and modifications can be made to the present application. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A transparent sunscreen composition, characterized in that, By weight parts, the transparent sunscreen composition comprises: 20 - 35 parts of emollient, 15 - 23 parts of sunscreen agent, 0.5 - 8 parts of film-forming agent, 0.1 - 2 parts of dibutyl ethylhexanoyl glutamine and 30 - 50 parts of ethanol; The emollient includes one or more of isopropyl myristate, polydimethylsiloxane, dicaprylyl carbonate, C12-15 alkyl benzoate, cyclopentadimethylsiloxane, isononyl isononanoate, squalane; The sunscreen agent includes one or more of bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane, homosalate, diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, polysiloxane-15, methylene bis-benzotriazolyl tetramethylbutylphenol, diethylhexyl butamido triazone; The film-forming agent includes one or more of trimethylsilyoxysilicate, acrylate / octylacrylamide copolymer, VP / acrylate / lauryl methacrylate copolymer, dibutyl lauroyl glutamate, VP / eicosene copolymer; 2. The transparent sunscreen composition according to claim 1, wherein The SPF of the transparent sunscreen composition is not less than 50.

3. The transparent sunscreen composition according to claim 1, characterized in that, The viscosity of the transparent sunscreen composition is not higher than 20 cps.

4. The transparent sunscreen composition according to claim 1, characterized in that, The average particle size of the atomized particles after spraying the transparent sunscreen composition is not higher than 100 μm.

5. The transparent sunscreen composition according to claim 1, wherein The sunscreen agent includes one or more of bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, ethylhexyl salicylate, polysiloxane-15; 6. The transparent sunscreen composition according to claim 5, characterized in that, The sunscreen agent includes: 0.1 - 2 parts of bis-ethylhexyloxyphenol methoxyphenyl triazine, 1 - 7 parts of diethylamino hydroxybenzoyl hexyl benzoate, 0.5 - 10 parts of ethylhexyl methoxycinnamate, 0.1 - 5 parts of ethylhexyl triazone, 0.5 - 4 parts of octocrylene, 1 - 5 parts of ethylhexyl salicylate, 0.5 - 3 parts of polysiloxane-15; 7. The transparent sunscreen composition according to claim 1, characterized in that, The transparent sunscreen agent composition includes: 0.1 - 2 parts of bis-ethylhexyloxyphenol methoxyphenyl triazine, 1 - 7 parts of diethylamino hydroxybenzoyl hexyl benzoate, 0.5 - 10 parts of ethylhexyl methoxycinnamate, 0.1 - 5 parts of ethylhexyl triazone, 0.5 - 4 parts of octocrylene, 1 - 5 parts of ethylhexyl salicylate, 0.5 - 3 parts of polysiloxane-15, 1 - 15 parts of dicaprylyl carbonate, 0.5 - 7 parts of isopropyl myristate, 0.1 - 3 parts of polydimethylsiloxane, 0.5 - 7 parts of C12-15 alkyl benzoate, 30 - 50 parts of ethanol, 0.01 - 1 part of dibutyl ethylhexanoyl glutamine, 0.5 - 3 parts of acrylate / octylacrylamide copolymer; 8. The transparent sunscreen composition according to claim 1, characterized in that, The transparent sunscreen composition further includes essence and / or whitening efficacy components.

9. A method for preparing a transparent sunscreen composition, characterized in that, The preparation method includes the following steps: 1) Weigh the raw materials to be used and set aside; 2) Dissolve ethanol, dibutyl ethylhexanoyl glutamine and acrylate / octylacrylamide copolymer until transparent and particle-free and set aside; 3) Add bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl hexyl benzoate, ethylhexyl methoxycinnamate, ethylhexyl triazone, octocrylene, ethylhexyl salicylate, polysiloxane-15, dicaprylyl carbonate, and C12-15 alkyl benzoate into the main pot, start the stirrer, and heat the main pot to 80-85 °C. After the material is evenly dispersed and there are no particles, set it aside for later use; 4) When the temperature drops to 55-65 °C, add tetrahydrocurcumin into the main pot and stir until it is evenly dispersed and there are no particles; add isopropyl myristate and polydimethylsiloxane, and stir evenly for later use; 5) When the temperature drops to 36-40 °C, add the ethanol solution, essence, and tetraisopalmitoyl ascorbate dissolved in step 2), and stir until evenly mixed; 6) Let it stand and cool to room temperature to obtain the transparent sunscreen composition.

10. Use of the transparent sunscreen composition according to any one of claims 1 to 8 in the preparation of a booster-free sunscreen spray.

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