Sunscreen composition, application and sunscreen product

Abstract

The invention belongs to the field of daily chemicals, and discloses a preparation method of a sunscreen composition, which comprises the following steps: step 1, mixing and dispersing sodium stearoyl glutamate, a part of a thickener, a part of an alcohol solvent and a part of water; step 2, adding a sun-screening agent into the mixture obtained in the step 1; 3, grinding the mixture obtained in the step 2; 4, emulsifying and homogenizing the residual thickening agent, the residual alcohol solvent, the residual water and the mixture obtained in the step 3; the sun-screening agent contains methylene bis (benzotriazolyl) tetramethyl butyl phenol; the weight ratio of the sodium stearoyl glutamate to the methylene bis-benzotriazolyl tetramethyl butyl phenol is (2-7): (45-55). According to the sunscreen composition disclosed by the invention, wide experimental verification shows that the sodium stearoyl glutamate and the methylene bis-benzotriazolyl tetramethyl butyl phenol have obvious sunscreen synergy. Meanwhile, the invention also discloses the composition and application thereof.

Description

Technical Field

[0001] The present invention relates to the daily chemical field, and specifically to a sunscreen composition, use, and sunscreen product. Background Art

[0002] In the prior art, the sun protection performance of sunscreen agents can be enhanced by different sunscreen synergists. A relatively typical one is a powdery synergist, such as HDI / trimethylolhexyl lactone cross-linked polymer and / or lauroyl lysine (CN118105315A, Sunscreen Synergist, Oil Composition, Care Composition, Use, and Preparation Method), or a sunscreen synergist derived from plants, such as plant root extract and hesperidin (CN115487103A, A Sunscreen Synergist Composition Derived from Plants and Its Application);

[0003] The following is a solution that uses an emulsifier as a sunscreen synergist:

[0004] Publication No. CN115337227A, a technical solution with the theme of a sunscreen composition and its application, mentions using sodium bis(lauroylglutamyl)lysine and PEG-240 / HDI copolymer bis-decyltetradecyl polyethylene glycol-20 ether to enhance inorganic sunscreen agents; its mechanism is to enhance the sunscreen effect by promoting the suspension of inorganic particles through emulsifiers;

[0005] Publication No. CN117338622A, a technical solution with the theme of a sunscreen composition and its preparation method and application, mentions using sodium stearoyl glutamate in the aqueous phase, and achieving improved stability of the obtained sunscreen composition, reduced emulsion particle size, and avoidance of delamination or oil separation, etc., and thus enhanced sunscreen performance by using different emulsifiers, namely hydrogenated lecithin, phytosterol, batyl alcohol, and sodium stearoyl glutamate, in the alcohol phase, aqueous phase, and oil phase.

[0006] In the prior art, for sunscreen agents involving an emulsion system, there are relatively many requirements for emulsifiers, and it is difficult for a general emulsion system to effectively enhance the sun protection of sunscreen agents, especially chemical sunscreen agents.

[0007] The technical problem to be solved in this case is: how to screen sunscreen agents and emulsifiers to achieve sun protection enhancement in most stable emulsion systems. Summary of the Invention

[0008] The object of the present invention is to provide a preparation method of a sunscreen composition. Through extensive experimental verification, it is found that there is an obvious sunscreen synergy between sodium stearoyl glutamate and methylene bis-benzotriazolyl tetramethylbutylphenol. The synergy mechanism lies in that sodium stearoyl glutamate can be regarded as a liquid crystal emulsifier. By grinding, sodium stearoyl glutamate shows a liquid crystal state, and the formed liquid crystal structure has birefringence, achieving an improvement in the sun protection effect of methylene bis-benzotriazolyl tetramethylbutylphenol.

[0009] Meanwhile, the present invention also discloses the composition and its use.

[0010] To achieve the above object, the present invention provides the following technical solutions:

[0011] A preparation method of a sunscreen composition, characterized by comprising the following steps:

[0012] Step 1: Mix and disperse sodium stearoyl glutamate, part of the thickener, part of the alcohol solvent, and part of the water;

[0013] Step 2: Add a sunscreen agent to the mixture obtained in Step 1;

[0014] Step 3: Grind the mixture obtained in Step 2;

[0015] Step 4: Emulsify and homogenize the remaining thickener, the remaining alcohol solvent, the remaining water, and the mixture obtained in Step 3;

[0016] The sunscreen agent contains methylene bis - benzotriazolyl tetramethylbutylphenol;

[0017] The weight ratio of sodium stearoyl glutamate to methylene bis - benzotriazolyl tetramethylbutylphenol is 2 - 7:45 - 55.

[0018] The mechanism of the sun protection synergistic effect of the present invention is as follows:

[0019] Sodium stearoyl glutamate can be regarded as a kind of liquid crystal emulsifier. Through grinding, sodium stearoyl glutamate shows a liquid crystal state, and the formed liquid crystal structure has birefringence, realizing the improvement of the sun protection effect of methylene bis - benzotriazolyl tetramethylbutylphenol; this characteristic enables it to show excellent emulsification effect at low dosages. Therefore, sodium stearoyl glutamate can not only be used as an emulsifier, but also form a liquid crystal structure in the formulation, thereby improving the stability and performance of the product, enhancing the dispersibility and stability of the sunscreen agent. At the same time, it can form an interfacial layer between the oily component and the aqueous component, evenly encapsulating the sunscreen agent in the emulsion, reducing the aggregation and precipitation of the sunscreen agent. This can ensure the uniform distribution of the sunscreen agent on the skin, forming a continuous protective film, thereby improving the sun protection effect, and can improve its stability and solubility in the formulation, thus enhancing the sun protection effect.

[0020] In the above sunscreen composition, the total amount of sodium stearoyl glutamate and methylene bis - benzotriazolyl tetramethylbutylphenol is equivalent to 47 - 62 wt% of the total amount of the product obtained in Step 4.

[0021] In the above sunscreen composition, the weight ratio of sodium stearoyl glutamate to methylene bis - benzotriazolyl tetramethylbutylphenol is 3 - 6:48 - 52.

[0022] In the above sunscreen composition, the sunscreen agent further includes one or more combinations of ethylhexyl methoxycinnamate, ethylhexyl salicylate, ethylhexyl triazone, homosalate, and octocrylene.

[0023] In the above sunscreen composition, the weight ratio of sodium stearoyl glutamate to the sunscreen agent is 2-7:45-65.

[0024] In the above sunscreen composition, the alcohol solvent is one or more combinations of glycerin, butylene glycol, and propylene glycol;

[0025] The dosage of the alcohol solvent is 1.5-4 wt%.

[0026] The thickener is one or more combinations of xanthan gum, carbomer, and hydroxypropyl methylcellulose; the dosage of the thickener is 0.3-1 wt%.

[0027] In the present invention, 30-60 wt% of the thickener, 30-60 wt% of the alcohol solvent, and 30-60 wt% of water are used in step 1, and the remaining part is used in step 4;

[0028] The grinding is carried out using a sand mill, and the rotation speed of the sand mill is 1000 rpm; the flow rate of the material in the sand mill is 4000 L / 3 h.

[0029] Meanwhile, the present invention also discloses a sunscreen composition prepared by using any one of the above methods.

[0030] Meanwhile, the present invention also discloses the use of the sunscreen composition prepared by using any one of the above in preparing a sunscreen product.

[0031] Finally, the present invention also discloses a sunscreen product containing any one of the above sunscreen compositions.

[0032] In the above sunscreen product, the dosage of the sunscreen composition in the sunscreen product is 1-20 wt%.

[0033] In the above sunscreen product, the dosage form of the sunscreen product is water-in-oil sunscreen milk, oil-in-water sunscreen milk, water-in-oil sunscreen cream, oil-in-water sunscreen cream, or sunscreen spray

[0034] Compared with the prior art, the beneficial effects of the present invention are:

[0035] 1. By combining the use of sodium stearoyl glutamate and methylene bis - benzotriazolyl tetramethylbutylphenol, the sun protection property of methylene bis - benzotriazolyl tetramethylbutylphenol can be effectively improved. This combination can be applied to most sun protection emulsion systems, with little restriction on the type of emulsifier, and can improve the wide applicability of the formulation.

[0036] 2. The liquid crystal effect of sodium stearoyl glutamate in the present invention has a promoting effect on most chemical sunscreens. However, for the amplitude of the promoting effect, methylene bis - benzotriazolyl tetramethylbutylphenol is the most significant. Detailed implementation mode

[0037] Next, the technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the scope of protection of the present invention.

[0038] Description of raw material sources:

[0039] Mixed sunscreen 1: Ethylhexyl methoxycinnamate, Ethylhexyl salicylate, and the weight ratio of the two is 5:4;

[0040] Mixed sunscreen 2: Ethylhexyl methoxycinnamate, Homosalate, and the weight ratio of the two is 5:3;

[0041] Mixed sunscreen 3: Ethylhexyl salicylate, Homosalate, and the weight ratio of the two is 4:3.

[0042] The sun protection values of the above - mentioned mixed sunscreens 1 to 3 and methylene bis - benzotriazolyl tetramethylbutylphenol of the present invention do not show significant differences.

[0043] AFSK: Potassium cetyl phosphate;

[0044] HR - S1 emulsifier: Water, Potassium lauryl phosphate, and the concentration of Potassium lauryl phosphate is 48 wt%.

[0045] The formula of the sun protection lotion is as shown in Table 1 below, and all subsequent cases will be implemented according to this formula table;

[0046] Table 1 Sun protection lotion formula table

[0047]

[0048]

[0049] The formulation preparation process is as follows: (1) Weigh the Phase A into a beaker according to the proportion, homogenize it for 10 minutes, keep it at 85°C for standby after mixing evenly. (2) Weigh the Phase B into another beaker, heat it to 85 - 95°C and dissolve it evenly for standby. (3) Weigh the Phase D into another beaker, heat it to 85°C and dissolve it evenly for standby. (4) Pour the prepared Phase B into the beaker of Phase A, homogenize it for 15 minutes, stir and cool down to 60°C after homogenizing evenly, add the Phase C and continue to stir, then add the prepared Phase D and E after cooling down to 45°C. (5) After adding all phases, stir for another 5 minutes to complete the preparation.

[0050] The test method for the sun protection value is as follows:

[0051] According to the property that ultraviolet absorbers and blockers in sunscreen cosmetics can block ultraviolet rays, apply the sunscreen cosmetics on special tapes, irradiate them with ultraviolet rays of different wavelengths, measure the absorbance values of the samples, and directly evaluate the sun protection effect based on the measured values. Due to the use of a 125-watt continuous xenon light source with high stability, the intensity value of the irradiation light source in the experiment remains consistent, ensuring the accuracy of the experiment. The X-Y automatic sampling control workbench is adopted to avoid the errors caused by manual sampling. The software is easy to operate and can obtain the desired SPF value and the critical wavelength value of PA in a very short time. Application: Measurement of the SPF value of cosmetics, sunscreen products, ultraviolet-proof fabrics, photosensitive emulsions, etc.

[0052] The First Part: Preparation and Performance Test of Sunscreen Compositions

[0053] The preparation method of the sunscreen composition is as follows:

[0054] Step 1: Mix and disperse sodium stearoyl glutamate, part of the thickener, part of the alcohol solvents, and part of the water.

[0055] Step 2: Add the sunscreen agent to the mixture in Step 1.

[0056] Step 3: Grind the mixture obtained in Step 2, the rotation speed of the sand mill is 1000 rpm, and the circulation flow rate is 4000 L / 3 h.

[0057] Step 4: Emulsify and homogenize the remaining thickener, the remaining alcohol solvents, the remaining water and the mixture obtained in Step 3, the homogenization pressure is 150 MPa, and the time is 0.5 h.

[0058] The dosages of the above substances can refer to Table 2; the proportions of the thickener, alcohol solvents, and water allocated in Step 1 can be seen in the allocation ratio column in Table 2.

[0059] Table 2 Compound Table of Sodium Stearoyl Glutamate and Different Sunscreen Agents Unit wt%

[0060]

[0061]

[0062] Referring to the preparation method of Example 2 above, a combination of the relatively typical liquid crystal emulsifier hydrogenated lecithin, HR-S1 and sunscreen is used to prepare the composition, and the specific formula can be referred to Table 3; in Table 3, AFSK is a common emulsifier, and it is reported that it can form a liquid crystal phase under relatively harsh processes. In the present invention, it is only used as a common emulsifier.

[0063] The ratio of the thickener, alcohol solvent, and water allocated in Step 1 is 50%;

[0064] Table 3 Compound table of different emulsifiers and different sunscreens Unit wt%

[0065]

[0066]

[0067] Comparative Example 16

[0068] The formula is the same as that of Example 2, and the preparation method is as follows:

[0069] Step 1: Mix and disperse sodium stearoyl glutamate, part of the thickener, part of the alcohol solvent, and part of the water;

[0070] Step 2: Add the sunscreen methylene bis-benzotriazolyl tetramethylbutylphenol to the mixture obtained in Step 1;

[0071] Step 3: Emulsify and homogenize the mixture obtained in Step 2;

[0072] Step 4: Emulsify and homogenize the remaining thickener, the remaining alcohol solvent, the remaining water and the mixture obtained in Step 3;

[0073] The homogenization pressure in Step 3 and Step 4 is 150 MPa, and the homogenization time is 0.3 h and 0.5 h respectively.

[0074] Comparative Example 17

[0075] The formula is the same as that of Comparative Example 4, and the preparation method is as follows:

[0076] Step 1: Mix and disperse AFSK, part of the thickener, part of the alcohol solvent, and part of the water;

[0077] Step 2: Add the sunscreen methylene bis-benzotriazolyl tetramethylbutylphenol to the mixture obtained in Step 1;

[0078] Step 3: Emulsify and homogenize the mixture obtained in Step 2;

[0079] Step 4: Emulsify and homogenize the remaining thickener, the remaining alcohol solvent, the remaining water and the mixture obtained in Step 3;

[0080] The homogenization pressure for Steps 3 and 4 is 150 MPa, and the homogenization times are 0.3 h and 0.5 h respectively.

[0081] Comparative Example 18

[0082] The formulation is the same as that of Comparative Example 8, and the preparation method is as follows:

[0083] Step 1: Mix and disperse the HR-S1 emulsifier, a part of the thickener, a part of the alcohol solvent, and a part of the water;

[0084] Step 2: Add the sunscreen agent methylene bis-benzotriazolyl tetramethylbutylphenol to the mixture obtained in Step 1;

[0085] Step 3: Emulsify and homogenize the mixture obtained in Step 2;

[0086] Step 4: Emulsify and homogenize the remaining thickener, the remaining alcohol solvent, the remaining water and the mixture obtained in Step 3;

[0087] The homogenization pressure for Steps 3 and 4 is 150 MPa, and the homogenization times are 0.3 h and 0.5 h respectively.

[0088] Comparative Example 19

[0089] The formulation is the same as that of Comparative Example 12, and the preparation method is as follows:

[0090] Step 1: Mix and disperse hydrogenated lecithin, a part of the thickener, a part of the alcohol solvent, and a part of the water;

[0091] Step 2: Add the sunscreen agent methylene bis-benzotriazolyl tetramethylbutylphenol to the mixture obtained in Step 1;

[0092] Step 3: Emulsify and homogenize the mixture obtained in Step 2;

[0093] Step 4: Emulsify and homogenize the remaining thickener, the remaining alcohol solvent, the remaining water and the mixture obtained in Step 3;

[0094] The homogenization pressure for Steps 3 and 4 is 150 MPa, and the homogenization times are 0.3 h and 0.5 h respectively.

[0095] Table 4 Results of sunscreen performance tests

[0096]

[0097]

[0098] Result analysis:

[0099] 1. As can be seen from Examples 1 to 5, a stable emulsion system can be formed with 2 wt% of sodium stearoyl glutamate. An increase in its dosage will not have an obvious impact on the sunscreen SPF value; an increase in the dosage of methylene bis - benzotriazolyl tetramethylbutylphenol will lead to an increase in the sunscreen value.

[0100] 2. As can be seen from Examples 6 to 9, the use of other sunscreens can further increase the sunscreen value of the formulation, but the increase amplitude is limited due to the limitation of their usage amounts;

[0101] 3. As can be seen from Comparative Examples 1 - 3, Example 2, and Comparative Examples 4 - 7, in the common emulsifier AFSK, there is little difference in the sunscreen performance of most sunscreens and the sodium stearoyl glutamate system. Among them, the gain effect of the mixed sunscreen 2 in the sodium stearoyl glutamate system is relatively significant. In terms of the gain amplitude, methylene bis - benzotriazolyl tetramethylbutylphenol is significantly better than the mixed sunscreen 2;

[0102] 4. As can be seen from Example 2, Comparative Examples 1 - 3, and Comparative Examples 8 - 11, for the typical liquid crystal emulsifier HR - S1, the gain effect on the mixed sunscreen 1 and the mixed sunscreen 3 is significantly greater than that in the sodium stearoyl glutamate system; as can be seen from Example 2, Comparative Examples 1 - 3, and Comparative Examples 12 - 15, for the typical liquid crystal emulsifier hydrogenated lecithin, the gain effect on the mixed sunscreen 1 and the mixed sunscreen 3 is significantly greater than that in the sodium stearoyl glutamate system;

[0103] 5. As can be seen from Example 2 and Comparative Examples 16 to 19, AFSK, the liquid crystal emulsifier HR - S1, and hydrogenated lecithin all show relatively similar sunscreen effects after homogenization and grinding. For sodium stearoyl glutamate, its sunscreen gain effect is better, probably because it has better ability to form liquid crystals.

[0104] Based on the analysis of the above results, generally speaking, using a liquid crystal emulsifier can increase the sunscreen value of most sunscreens due to its birefringence. When using sodium stearoyl glutamate and methylene bis - benzotriazolyl tetramethylbutylphenol to form an emulsified sunscreen system and apply it to the formulation, a more obvious sunscreen effect can be achieved; the reason is that: sodium stearoyl glutamate has stronger emulsification stability and the formed liquid crystal phase has better birefringence. At the same time, due to its stability and coating property, it can spread more evenly, improving the sunscreen effect; in addition, methylene bis - benzotriazolyl tetramethylbutylphenol can better adapt to the above characteristics of sodium stearoyl glutamate and show better effects.

[0105] Part 1: Safety Test of the Sunscreen Composition

[0106] Apply the composition of Example 3 to the application formulation in Table 1 for a skin patch test.

[0107] The experimental method is as follows:

[0108] Select qualified patch test equipment. Using the occlusive patch test method, place about 0.020 g - 0.025 g (solid) or 0.020 mL - 0.025 mL (liquid) of the test substance in the patch tester, and apply it to the flexor side of the forearm of the subject with a low-allergy tape. After 24 hours, remove the test substance, and observe the skin reaction at 0.5, 24, and 48 hours after removal respectively. Record the results according to the skin reaction grading standard in the currently effective technical specification.

[0109] Skin reaction grading standard for skin occlusive patch test:

[0110]

[0111] The experimental results are shown in Table 5 below;

[0112] Table 5 Patch test table

[0113]

[0114]

[0115] From the above experiments, it can be seen that the formula of the present invention has a high safety factor and is non-irritating to the human body.

Claims

1. A method for preparing a sunscreen composition, characterized in that: The steps include: Step 1: Mix and disperse sodium stearoyl glutamate, part of thickener, part of alcohol solvent and part of water; Step 2: Add sunscreen to the mixture in step 1; Step 3: Grinding the mixture obtained in step 2; Step 4: emulsifying and homogenizing the remaining thickener, the remaining alcohol solvent, the remaining water and the mixture obtained in step 3; The sunscreen contains methylene bis-benzotriazolyl tetramethylbutylphenol; The weight ratio of the sodium stearoyl glutamate to the methylene bis-benzotriazolyl tetramethylbutylphenol is 2-7:45-55.

2. The preparation method according to claim 1, characterized in that: The total amount of the sodium stearoyl glutamate and methylene bis-benzotriazolyl tetramethylbutylphenol is equivalent to 47-62 wt % of the total amount of the product obtained in step 4.

3. The preparation method according to claim 1, characterized in that: The weight ratio of the sodium stearoyl glutamate to the methylene bis-benzotriazolyl tetramethylbutylphenol is 3-6:48-52.

4. The preparation method according to claim 1, characterized in that: The sunscreen agent also includes one or more combinations of ethylhexyl methoxycinnamate, ethylhexyl salicylate, ethylhexyl triazone, homosalate, and octocrylene.

5. The preparation method according to claim 4, characterized in that: The weight ratio of the sodium stearoyl glutamate to the sunscreen is 2-7:45-65.

6. The preparation method according to claim 1, characterized in that: The alcohol solvent is one or more combinations of glycerol, butylene glycol, and propylene glycol; The alcohol solvent is used in an amount of 1.5 to 4 wt %; The thickener is one or more combinations of xanthan gum, carbomer, and hydroxypropyl methylcellulose; the amount of the thickener is 0.3-1wt%; The grinding is carried out by using a sand mill, the rotation speed of the sand mill is 1000 rpm; the flow rate of the material in the sand mill is 4000 L / 3h.

7. A sunscreen composition, characterized in that: The method is prepared by any one of claims 1 to 6.

8. Use of the sunscreen composition according to claim 7 in preparing sunscreen products.

9. A sunscreen product, characterized in that: Contains the sunscreen composition as claimed in claim 7.

10. The sunscreen product according to claim 9, characterized in that: The amount of the sunscreen composition in the sunscreen product is 1-20wt%; the dosage form of the sunscreen product is water-in-oil sunscreen lotion, oil-in-water sunscreen lotion, water-in-oil sunscreen cream, oil-in-water sunscreen cream or sunscreen spray.

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